낮은 바인더 함량과 낮은 외부 표면적을 갖는 X 제올라이트로 만들어진 제올라이트 흡착제, 상기 흡착제의 제조 방법 및 그것의 용도

The present invention according to adsorption number

The, main number number 1 according to, the present invention refers to number it rises, light based on number and non-adsorbing it rises, light based phase number relates to, said adsorption number is:

- 30 m² . g^-1 Hereinafter, preferably 20 m² . g^-1 Hereinafter in external surface,

At least one number number it rises, light based on this [thu - X types of FAU structure it rises, including,

According to standard ASTM D 4284 - 83 - into the gear distribution determined by mercury (mercury intrusion) dV/dLogD_Hg Represented by microscopic pores diameter as distributions, where D_Hg The apparent pore diameter and V is volume and is microscopic pores, including its mode boundaries in 100 nm - 250 nm, said pore diameter distribution.

In a preferred embodiment form there is, adsorption number type [ni[ni] wool month (unimodal) distribution of a fore diameter distribution into the slide groove.

Terms "type [ni[ni] wool month distribution" big distribution having a single peak. The, type [ni[ni] wool month distribution characterized by a diameter and which has a single peak, the value of the diameter in the upper end of this with a peak "mode" or "a prevailing value" distributed are known to most frequent value by a goniophotometer. Distribution of peaks separated by a trough (trough) when 2, suitable for a bimodal distribution (bimodal).

The present invention refers to bimodal or even multimodal (multimodal) distributions, i.e. concentration zone to be several of values separated by the discontinuity points not related to distribution. Such distributions having different diameters for various gun [phyul [syen pressurizes presence that is unique to disclosed.

Advantageously, nitrogen at a temperature of 77 K (N₂ ) Formed in the adsorption are evaluated by a method from a t - plot, the present invention according to adsorption number micro pore volume 0. 200 cm³ . g^-1 Greater than. The formed in the nitrogen adsorption, time 9 - 16 time period of time at a temperature of 300 °C - 450 °C, preferably 400 °C in 10 hours, vacuum (P < 6. 7 × 10^-4 Pa) to a degassing after, measured substrate.

Advantageously, the present invention according to 2 weight % - 8% by weight to the gross weight of the adsorption number the absorption number it rises, light based on a level of non-number comprises. Form there is another preferred embodiment of the present invention, adsorption number is barium, or barium and potassium comprises.

The outer surface of the of the present invention number number 9 - 16 time it rises, light based adsorption at a temperature of 300 °C - 450 °C is time period of time, preferably 10 hours in 400 °C, vacuum (P < 6. 7 × 10^-4 Pa) to a degassing after, from nitrogen adsorption method at a temperature of 77 K are calculated through t - formed in the plot. It rises, FAU number used in the same manner as the external surface area of the aggregation of determining light measured substrate. External surface area of the m² The entire porous surface exceeds a BET surface exhibits a portion of unit/g (microporous surface + S BET=external surface).

According to the preferred embodiments, barium oxide (BaO) expressed, barium (Ba) content of the present invention number it rises, light based adsorption number, the total weight of the adsorption number contrast, exceeds 10% by weight, preferably greater than 15% by weight, very preferably exceeds 20% by weight, further preferably exceeds 23% by weight, or even greater than 33% by weight, advantageously, 23% - 42% by weight of the total weight of the adsorbent of the number contrast barium content weight, 30 weight % - 40% by weight and typically, includes the boundary.

In another preferred according to one embodiment, potassium oxide (K₂ O) expressed, it rises, potassium (K) content of the present invention number number number 25% by weight of the total weight of the adsorbent of the adsorption based light contrast less than, preferably 0 - 20% by weight, further preferably 0 - 15% by weight, very preferably 0 - 10% by weight and, includes the boundary.

In a further preferred embodiment form there is, barium oxide (BaO) and oxidation potassium (K₂ O) represented in a total content other than alkali metal or alkali earth ion oxide, barium and potassium ions other than alkali metal or alkali earth the overall content, relative to the total weight of the adsorption number, and 0 - 5%, includes the boundary.

Advantageously, the present invention according to number it rises, light based adsorption number is, 0. 15 cm³ . g^-1 - 0. 5 cm³ . g^-1 , Preferably 0. 20 cm³ . g^-1 - 0. 40 cm³ . g^-1 , Very preferably 0. 20 cm³ . g^-1 - 0. 35 cm³ . g^-1 Of, mercury according to standard ASTM D 4284 - 83 33 macropores and maul parcel [e and to the measured total volume (volume sum volume of macropores maul parcel [e) with, including said values ranges are understood to all boundaries.

A preferred embodiment of the present invention form there is, it rises, light based adsorption number is number macro pressurizes, comprising the maul parcel [e in addition with micro pores. The terms "macro pressurizes", pressurizes the idea exceeds 50 nm diameter means other. Terms "maul parcel [e" diameters, boundaries pressurizes to 2 nm - 50 nm in means other. The terms "micro pressurizes", diameter less than 2 nm are big microscopic pores.

In addition, adsorption of the present invention is advantageously boundaries number including 0. 2 - 1, very preferably 0. 6 - 1 of (macropores volume)/(volume + macropores maul parcel [e volume) ratio.

In conjunction with the present invention, nitrogen at a temperature of 77 K (N₂ ) Formed in the micro pore volume plot method was assessed by adsorption from t - 0. 200 cm³ . g^-1 Excess, preferably 0. 205 cm³ . g^-1 - 0. 300 cm³ . g^-1 , More preferably 0. 205 cm³ . g^-1 - 0. 290 cm³ . g^-1 In addition it rises, light based adsorption number is preferably in number.

In conjunction with the present invention, sized mechanical strength 1. Less than 6 mm for agglomeration and methods are measured by Shell method series SMS 1471 - 74. It rises, light based adsorption number defined number prior measured makes this mechanical strength generally 1. 5 mpa - 4 mpa, preferably 1. 7 mpa - 4 mpa, more preferably 1. 8 mpa - 4 mpa, and most preferably 2 mpa - 4 mpa, includes the boundary.

In a further preferred embodiment form there is, the present invention according to number it rises, light based adsorption number boundary is intermediate 1. 00 - 1. 50, preferably 1 to boundaries. 05 - 1. 50, more preferably 1 to boundaries. 15 - 1. 50 atomic ratio of Si/Al.

X FAU structure and types of number in light it rises,, it is known in particular 2 sub groups it rises, MSX number it rises, current typically LSX number method and apparatus which is excellent in the admit configured of vehicle from the outside. It rises, sprouts LSX number about 1 atomic ratio of Si/Al MSX number with it rises, sprouts, about 1 comprising boundaries. 05 - about 1. 15 atomic ratio of Si/Al. In a preferred embodiment form there is, at least one FAU number it rises, sprouts, boundaries to 1. 15 - 1. 50 atomic ratio of Si/Al it rises, light X having number are disclosed. In another preferred embodiment form there is, at least one number about 1 atomic ratio Si/Al having it rises, LSX type of number it rises, light X in among others light.

It rises, light based adsorption of the present invention number in number, form there is a preferred embodiment, the terms "types of FAU number X it rises, light" coincidence it rises, this [thu X types of FAU number components, such hierarchical (hierarchically) it rises, sprouts are porous and said number, i.e. X types of hierarchical porous number it rises, light (or HPX number it rises, light), it rises, light (or HPMSX) MSX types of hierarchical porous number types of hierarchical porous number LSX and it rises, light (or HPLSX) and, in particular boundaries than to 1. 00 - 1. 50, preferably 1. 05 - 1. 50, more preferably 1 to boundaries. 05 - 1. 40, further preferably 1 to boundaries. 15 - 1. 40 atomic ratio of Si/Al FAU number having a hierarchical porous it rises, light among others.

The present invention refers to in addition at least one porous layer 2 are as defined just it rises, rotary cutter having mixtures including number it rises, light based adsorption number FAU number without using a tool.

The term "hierarchical porous number it rises, light" number to maul parcel [e and having both micro pressurizes it rises, light, i.e. microporous and maul soda worker adult it rises, this [thu big number. The terms "resulting mesoporous number it rises, light", it rises, light based microporous number as described US 7 e.g. together with porosity rate determining are micro (TEM) easily identifiable by using transmission electron microscope observation (maul soda production rate) are the internal cavity of the nano having this [thu it rises, number components, transmission electron microscopy (TEM) by observations are, determining number are filled (i.e., non-maul small porosity) number it rises, light based it rises, light crystals or filled number of aggregate (aggregates) or an aggregate of it rises, light crystals or checked whether the resulting mesoporous determining resulting mesoporous determining nephrophathy.

In the crystalline structure of the present invention number it rises, light based adsorption number X types of FAU number it rises, rotary cutter having (that are publicly known to one skilled in the field of the XRD abbreviation) x - ray is increased by identifiable disclosed.

In another preferred embodiment form there is, FAU structure other than it rises, light infrastructure is not number, preferably equal number other than X structure of the present invention number it rises, light based adsorption number is in the engine it rises, light infrastructure is increased by x - line are detected.

The FAU structure other than "FAU structure other than it rises, light infrastructure number is not" representing one or more number it rises, light based phases, 5% by weight to boundaries than, preferably less than 2% by weight to boundaries by big. Determined by XRD (it became the after alcoholic beverage techniques) to the gross weight of the expressed in a mass fraction of the adsorption number.

In particular it rises, light based on determining the number of interconnected (NZP) non number for use in bath method ensure agglomerated and binder, "aggregate" or "number it rises, light based aggregate" herein terms in the terms of the present invention such as described above are used instead of "number it rises, light based adsorption number" occasionally.

In the present invention, the term "binder" of the present invention number it rises, light based adsorption number (or agglomerated number it rises, light based material) agglomerated binder by big number in determining light it rises, ensure combinations. The binder is that it does not have a crystalline structure after calcination in addition it rises, light based on determining number in number and with light it rises, hereinafter, a gaseous inert binder is often, more accurately adsorption and ion exchange inert toward other controller.

In a further preferred embodiment form there is, it rises, FAU number X number it is this [thu it rises, types of this [thu preferably, at least 85% by weight of the present invention adsorbed it rises, rotary cutter having mass fraction of the total weight of FAU number number preferably remains at least 90 weight % contrast, consists of the remainder of the number it rises, light based on 100% preferably non (NZP). According to one aspect in particular advantageous, it rises, rotary cutter having mass fraction of the FAU number, number of the present invention adsorbed total weight of contrast, 92 weight % - 98% by weight, weight % - 98% by weight and preferably 94, and boundaries, it rises, light based on the remainder of the number preferably non consists of 100%.

As already indicated, the present invention according to the number of adsorption number it rises, benzoarylureido abbreviation (crystallization degree) in the field of light (are) XRD x - ray diffraction analysis provides one skilled that are determined by the publicly known disapproval.

In a preferred embodiment form there is, the present invention according to number it rises, light based adsorption number is, boundary intermediate 7. 7% hereinafter, preferably 0 - 7. 7%, preferably 3. 0% - 7. 7%, more preferably 3. 5% - 6. 5%, advantageously 4. 5% - 6. Of 0%, and an ignition loss (loss on ignition) measured at 950 °C according to standard NF EN 196 - 2 has.

With the description herein specify not, 1 950 °C displayed in time ratio is performed based on calcined, calcined equivalent solid component weight ratio counted are disclosed.

The present invention according to a process for adsorption number number high pressure liquid coolant

The present invention according to number of the present invention relates to a process for adsorption number number it rises, light based main number is other high pressure liquid coolant, said process at least:

A) 20 m² . g^-1 Excess, preferably boundaries 20 m including² . g^-1 - 200 m² . g^-1 , More preferably boundaries 40 m including² . g^-1 - 150 m² . g^-1 Of, measured by nitrogen adsorption, that having a outer surface, clay or clay binder is preferably at least 80% of maximum 5% with the addition of a mixture including number and, in addition allow drying and calcination of agglomerated material after formation of the aggregates and the amount of water having, at least one FAU number it rises, light, preferably X number of decisions during the coagulation step it rises, rotary cutter having FAU type;

B) optionally at least one structured in the presence of number, step a) acquired in aggregates all or part of this [thu aqueous base solution by contacting it with said binder it rises, step number;

C) optionally be present selectively structured industry association step number number;

D) a barium or barium potassium ions by contacting with a solution of step b) or c) the agglomerates of cation exchange (are);

E) potassium by contacting with a solution of step d) selective cation exchanging additional aggregate;

F) at a temperature of 50 °C - 150 °C, step d) or e) acquired in aggregates cleaning and drying; and

G) 100 °C - 400 °C, preferably at a temperature of 200 °C - 300 °C, in particular oxygen, nitrogen, air, drying and/or decarbonization acid air, or alternatively drying and/or decarbonization specialty gas such as oxygen-depleted air, the oxidation and/or inert gas stream of step f) by activating the present invention according to number acquired in aggregates generating it rises, light based adsorption number comprising the following steps.

A preferred embodiment form of the present invention number number number it rises, light based adsorption process for high pressure liquid coolant, said step a) the drying of agglomerates in generally carried out in a temperature of 50 °C - 150 °C, dried agglomerates of calcination at generally higher temperature than 150 °C, typically 180 °C - 800 °C, in preferentially 200 °C - 650 °C, hours, e.g. 2 - 6 hours time in particular oxygen, nitrogen, air, drying and/or decarbonization sulphonic air, or alternatively drying and/or decarbonization sulphonic gas such as oxygen-depleted air, carried out in a stream of oxidation and/or inert gas.

Form there is one embodiment of the present invention, agglomeration step (step a) it rises, rotary cutter having determinations are used during intermediate 1 micro m - 20 micro m boundary FAU number, more preferably boundaries to 1. 5 micro m - 20 micro m, a boundary intermediate priority 1. 8 micro m - 10 micro m, including better boundaries 2 micro m - 10 micro m, more preferably has a number average diameter of 2 micro m - 8 micro m to boundaries.

In the synthesized, terms "number average diameter" or "size" is preferred in particular number for determining light it rises, are used without. The scale for measuring method which the carry enumerated encoded.

In a preferred embodiment form there is a, number of sprouts FAU it rises, defined above are useful as advantageously preferably boundaries to 1. 00 - 1. 50, preferably 1. 05 - 1. 50, more preferably 1. 05 - 1. 40, more preferably 1. 10 - 1. 40, further preferably 1. 15 - 1. 40 atomic ratio of Si/Al.

A proper prior, the aforementioned process steps a) determining used in external surface area of the time period of time at a temperature of 300 °C - 450 °C time of 9 - 16, preferably 10 hours in 400 °C, vacuum (P < 6. 7 × 10^-4 Pa) to a degassing after, from nitrogen adsorption method at a temperature of 77 K are calculated through t - formed in the plot.

In a preferred embodiment form there is a, step a) it rises, sprouts FAU number used in hierarchical porous FAU number it rises, light among others. High external surface area it rises, rotary cutter having determinations are out-of-one skilled art hierarchical porous FAU number according to various publicly known method, e.g. described by Inayat synthetic (Angew. Chem. Int. Ed. , (2012), 51, 1962 - 1965) obtained according may be filled.

In addition, and by seeding (seeding) SiO/or synthetic mixture₂ /Al₂ O₃ Non-, like carbon and alkali sodium content synthetic operating conditions or alternatively by adjusting the publicly known art provides one skilled of the existing method of determining post-processes by synthesis number decisions during the high pressure liquid coolant according to said write it rises, FAU number can be.

Post-process are generally that deallumination solids undergoing at least as acid, may include the processing, e.g., D. Like Verboekend (Adv. Funct. Mater. , 22, (2012), 916 - 928 page) as addressed by, sodium hydroxide (NaOH) in order to stand-alone aluminum based residue number at least twice of said acid followed by washing, or alternatively, for example, taught application WO2013/106816 as, action of acid and acid number combination by action of improving effectiveness of structured processes it rises, light network (network) number is a number of already-formed consists of atoms from industry.

The number (i.e., other than post-synthesis processes) for the direct synthesis of rotary cutter having it rises, processes preferably and generally comprising the one or more structured number or sacrificial template.

Used may be any publicly known art provides one skilled sacrificial templates described those types and in particular application WO 2007/043731 disapproval. In a preferred embodiment form there is, sacrificial template is advantageously bonded organosilane, it will be burnt preparation of dimethyl - [3 - (tree maul [thok[thok] sour reel) propyl] ammonium chloride for a desired period, it will be burnt dimethyl [3 - (tree maul [thok[thok] sour reel) propyl] ammonium chloride process, accumulation of [3 - (tree maul [thok[thok] sour reel) propyl] thread d methyl ammonium chloride, [3 - (tree maul [thok[thok] sour reel) propyl] jade [thil ammonium chloride, N - [3 - (tree maul [thok[thok] sour reel) propyl] aniline, 3 - [2 - (2 - aminoethyl amino) ethylamino] propyl the tree maul [thok it will be sour, column, N - [3 - (tree maul [thok[thok] sour reel) propyl] - N' - (4 - vinyl benzyl) ethylenediamine, [thok at the time of tree - 3 - (2 - imidazolin - 1 - yl) propyl silane, 1 - [3 - (tree maul [thok[thok] sour reel) propyl] urea, N - [3 - (tree maul [thok[thok] sour reel) propyl] ethylene diamino mill a, [3 - (diethylamino) propyl] trimethoxysilane, (3 - writing city [til[til] jade hour pro it will bloom) trimethoxysilane, 3 - (tree maul [thok[thok] sour reel) propyl methacrylate, [2 - (cyclo fragrance) ethyl] tree [thok it will be sour, column, [thok it will be sour in thread tree, column of boron atoms, the tree maul which will be burnt [thok it will be sour, column process, (3 - aminopropyl) trimethoxysilane, (3 - mercapto cop toe pro it will bloom) trimethoxysilane and (3 - chloro-propyl) trimethoxysilane, and in addition at least one mixture selected from all ratio among these 2.

Among the aforementioned sacrificial template, it will be burnt preparation of [3 - (tree maul [thok[thok] sour reel) propyl] dimethyl ammonium chloride, or most preferably TPOAC in particular.

In addition, higher molar mass sacrificial templates, e.g. PPDA (polymer poly - d the d methyl ammonium which will inform), PVB (polyvinyl butyral) and maul parcel [e thereof in order of diameter increases and other publicly known to the field used to oligomeric compounds may be filled.

In a preferred embodiment of the present invention is provided a process, number intended to volatile in the presence of the sacrificial template number bath, such as described above, a step of determining rotary cutter having at least one hierarchical porous FAU number it rises, aggregation) carried out in.

This number according to the publicly known method for making out-of-one skilled art, e.g. calcination may be performed by, non-number limited manner, a number of sacrificial template in the stream of oxidation and/or inert gas it rises, light determining calcination, in particular oxygen, nitrogen, air, drying and/or decarbonization sulphonic air, drying and/or decarbonization sulphonic selectively oxygen-depleted air into such a gas, at a temperature of greater than 150 °C one or more, typically in 180 °C - 800 °C, in preferentially 200 °C - 650 °C, hours, e.g. 2 - 6 is carried out during the time disapproval. The nature of the gas, temperature increase causes lamps (ramps) and a continuous temperature stages and its duration are adapted according to the nature of the sacrificial template will.

Additional steps of the present invention number number number number sacrificial template industry selective adsorption process for a high pressure liquid coolant can be carried out at any time during it rises, light based disapproval. The, said sacrificial template for placing a number of advantageously agglomeration step a) before, or alternatively step a) performed by determining number of calcination of calcined during adsorption number following it rises, light disapproval.

However, step a) aggregation of porous base material obtained according to another method of the present invention out of the way power to it rises, rotary cutter having aggregation not FAU number are disclosed.

It rises, rotary cutter having the synthesis generally alkaline medium FAU types of number (sodium hydroxide and the Na⁺ Cation) occurs in. The most it rises, rotary cutter having determinations are obtained FAU number, or even entirely comprises sodium cations. However, step a) if selective number sacrificial template embodiment carried out before step before or after the wetting ability, one or more times between Na domain of cation exchange to the use of out of the way of the present invention undergoes a decisions not disclosed. In this case, step d) and optionally exchange e) is selective resulting in the slot disapproval.

Step a) in the present invention according to number of FAU number it rises, rotary cutter having crystals used in scanning electron microscope (SEM) and adsorption FAU number measured by viewing it rises, rotary cutter having determining size substrate.

The out-of-one skilled in the art for aggregation and formed (step a) according to any publicly known techniques, in particular extrusion, compact, granulating plate, granulating drum aggregation, atomization in NaCl techniques performed according to at least one of disapproval.

It rises, 92 parts by weight of binder (hereinafter defined reference) and number used aggregation number 8 - 15 - 85 parts by weight of it rises, for parts by weight ratio rotary cutter having a slotted parts by weight of binder are disclosed.

Step a) after, the cyclone and/or screening for most fine agglomerated adsorption number by number can also be volatile and/or too coarse aggregates, e.g., extrudates may be filled and a sense number by comminution screened or when displayed. The adsorption number is obtained, beads, in the form of extrusion machines or the like, preferably boundaries to 0. 2 mm - 2 mm, in particular 0. 2 mm - 0. 8 mm, preferably 0. 40 mm - 0. The volume mean diameter of 65 mm, or length has (when not spherical it longest dimension).

Thus, the present invention may be used in conjunction with the binder of the existing method provides one skilled the art may be selected from publicly known binders, preferably selected from a mixture of clay and clay disapproval.

Clays is preferably kaolin, the car it raises but this [thu, me grow this [thu, state d chi, halloysite, child [phel person [thu, sepiolite, montmorillonite, bentonite, production of and metakaolin, all ratio among these 2 in addition at least one chosen from mixtures.

Preferably, step a) used in the aggregation binder, preferably kaolin, the car it raises but this [thu, me grow this [thu, d chi state, group of halloysite and metakaolin, it rises, this [thu painter it is skillful and comprising at least one number selected from clay and mixtures thereof. Preferably kaolin and most typically are used. Step a) bentonite in addition binder used in aggregation, such as other mineral binder may contain child [phel person [thu may be filled. The terms "this [thu painter it is skillful number it rises, clay", usually through action of aqueous base solution can be converted into a mixture of big number it rises, [thu[thu] clay or clay.

Step a) optionally addition in number, the publicly known to one skilled in the art for any number it rises, light synthesis expert type of silica source, e.g. colloidal silica, diatomite, perlite, fly ash, sand, or other different types of solid silica may be disclosed.

Step a) during, it rises, light crystals in addition number, include the addition of one or more binder in addition number may be filled. Priority number is added at the top, e.g. lignin, starch, carboxymethylcellulose, surfactants (cationic, anionic, non-ionic or amphiphilic) and number molecules, this rheological (rheology) by changing a number and/or adhesion it rises, light/clay paste or in particular for the operation of the final adsorption number gives a satisfactory characteristics in macro porosity rate hereinafter intended to substrate.

Preferentially, however non-exclusive manner, methyl cellulose and their derivatives, lignosulfonate, poly car [lu luck thread obstetrics carboxylic acid nose Polymer, their amine one derivatives and their salts, in particular alkaline salts are ammonium salts referred disapproval. 0 - 5% by weight to the gross weight of number number added to the absorption device, preferably 0. 1 weight % - 2% by weight at a rate of multiple myelomas are included.

It rises, light based adsorption number number of SEM observations are, for example, adsorption or other amorphous phase including other non-number number of agglomerated binder can diffuse to the presence on it rises, light based.

Step a) included for calcination, properties of gases, and a continuous temperature stages and in addition duration are in particular number of special uses of each of the increasing temperature lamps be sacrificial template according to the nature of the agglomeration step a) adapted according to the nature of the binder used in will.

Similarly, it rises, number this [thu step b) is carried out according to the method described in the prior art may be any well-known and to allow a user to one skilled art step, an aqueous solution of sodium hydroxide or potassium hydroxide is used alkaline aqueous solution is possibly, most in particular preferably use of sodium hydroxide. Generally, the concentration of the alkaline solution it rises, this [thu number 0. 5 M - 5 M are disclosed.

It rises, number this [thu preferably higher than the room temperature, for example room temperature (about 20 °C) between this [thu number it rises, and alkaline solution boiling point temperature, e.g. at a temperature of approximately 80 °C - 100 °C carried out furnace. It rises, this [thu - the duration of the process number decoding generally several hours, usually about 1 - 8 time time are disclosed.

One embodiment of the present invention is provided a process, at least a portion of step b it rises, binder aggregation number this [thu) is out-of-one skilled art according to the publicly known method, e.g. by calcination in the presence of at least one structured number intended to volatile number or sacrificial template may be performed, the presence of structured number number resulting mesoporous it rises, light based aggregate so as to obtain a resin of the present invention has the purpose of maul soda production rate at a specified level of the agglomerates.

Structured sacrificial template properties of any number or kind of the publicly known art provides one skilled in particular porous layer may be selected from the aforementioned number for the synthesis rotary cutter having it rises, disapproval.

The amount of structured number, the presence of this [thu it rises, number in it, according to the desired maul soda production rate may be varied within a broad is within, clay (are) of a predetermined advantageously 0. 1 weight % - 50% by weight, preferably 0. 1 weight % - 33% by weight, more preferably 1 weight % - 30% by weight, 5% - 30% by weight weight advantageously are disclosed.

It rises, number this [thu step b) for selectively introducing a portion of the trough and the flocculated binder during the resulting mesoporous number intended to converting it rises,, selective number of special number structured step c) is out-of-one skilled art any publicly known means, in particular, generally exceeds 150 °C, typically 180 °C - 650 °C, performed by heat treatment at a temperature of 200 °C - 600 °C preferentially disapproval. In this case, g activating step performed at high temperatures) is structured to permit number of every other number in addition, advantageously step g) during activation of said structured number number number in step e and a sense substantially wetting ability) to eliminate a possible causes.

The aforementioned cation exchange steps d) and e) is, in accordance with the out-of-one skilled art publicly known standard method, high barium content, i.e. adsorption number representing the total mass of barium in relation when weight, preferably greater than 10%, preferably greater than 15%, very preferably exceeds 20%, further preferably exceeds 23%, or even greater than 33% - 100 °C to quickly obtain content to room temperature, preferably 80 °C - 100 °C barium salt aqueous solution at a temperature of, for example barium chloride (BaCl₂ ) And/or potassium salt (KCl) and/or barium and potassium salt and, step a) carried out by contacting the adsorption number obtained from clear.

Advantageously, the total weight of the adsorbent of the heat exchanger represented number 23 weight % - 42% by weight barium content including contrast boundaries, 30% - 40% by weight weight typically are disclosed. Exchanging a large excess barium ions for cations rotary cutter having it rises, preferably number, typically approximately 10 - 12 excess amount, advantageously by continuous exchange preferably working.

Step e) (step b) before and/or after selective potassium exchange is barium exchange may be disclosed. In addition step a) already includes a barium or potassium ions or barium and potassium ions (step a) it rises, FAU number before barium or potassium or barium and potassium coalescer decisions during the rotary cutter having ion, it rises, FAU types of disclosure number is not present cation, sodium cation typically pre-exchange), steps d) and/or e) can be decided (otherwise be).

The applicant, surprisingly, the number of hierarchical porous cation exchange step is difficult it rises, light determining relative brittle that is likely to contain said porous layer number (or mass flow rate of the exchanged once number related to adsorption) of determining light it rises, micro pore volume and external surface will not affect the inherent properties of effect on the observed.

After cation exchange step (are), then generally and preferably water washing is carried out, then the number of obtained adsorption drying 369. Drying (step f) followed by activation method according to the publicly known art is made out-of-one skilled, e.g. generally 100 °C - 400 °C, preferably carried out at a temperature of 200 °C - 300 °C. Accomplished during activation are determined according to desired ignition loss of time. Generally few minutes - hours time, typically 1 - 6 time time are disclosed.

Use of the present invention according to adsorption number

In the present invention refers to in addition synthesized is described, FAU types of number method based on decisions it rises, rotary cutter having of the existing method, for use in particular listed, adsorption material advantageously replace the use of the aforementioned number it rises, light based adsorption number as adsorption are disclosed:

The papermaking fraction●C8 aromatic isomers, in particular the separation of xylene,

●knit with [thol base n, n d ethyl [thol base, such as substituted toluene diamine toluene isomers are separated,

Separation of cresol●,

Separation of●polyhydric alcohol such as glucose.

According to another main number, as defined in the present invention refers to at least one number on it rises, light based adsorption number xylene isomers for process using gas or liquid phase separation are disclosed.

The present invention refers to in particular para - xylene adsorbing material such as using it rises, light based adsorption number number as defined above, having from 8 carbon atoms para - aromatic isomers fractions of feedstock processed picture on the magnesium alloy are disclosed.

Thus, the desired product (para - xylene) (disposed (batch) mode) by pre-adsorption liquid chromatography, advantageously simulating moving bed unit continuous mode, i.e. simulation with parallel flow reflux or simulation, in particular separated warm than simulating disapproval.

Industrial simulation simulated moving bed adsorption unit acting as backflow mode operating conditions are generally as follows:

The number of bed●: 4 - 24;

Number of zones●: of at least 4 as zone, each feed point (stream of processed feedstock stream or desorption number) and drawing point is located between the (raffinate stream of stream of or extract);

●100 °C - 250 °C, preferably 140 °C - 190 °C temperature;

A process temperature xylene (when selected as desorption number is toluene or toluene)●heater pressure between pressure unit 3 mpa industry;

●0. 7 - 2. 5, preferably 0. 7 - 2. 0, e.g. stand-alone adsorption the unit 0. 9 - 1. 8, in combination with adsorption crystallization unit the unit 0. 7 - 1. 4 desorbing number/feedstock flow rate ratio;

●recirculation rate: 2 - 12, preferably 2. 5 - 6;

Between two injection cycle time corresponding to a given bed desorption number●: advantageously 4 - 25 minutes.

US 2 are patent, US 5 and US 5 event of disapproval referenced in this regard.

Generally, industrial simulation-current adsorption operating conditions may include, generally 0. 8 - 7 in recirculation rate under the outside number are the same and the facsimile and operated to in a mode backflow conditions. US 4 and are referenced in this US 4 patent disapproval.

Desorption number is, formed with a plurality of desorption solvent such as toluene feedstock having a boiling point lower than the desorption solvent having a boiling point of - diethylbenzene (PDEB) feedstock is higher than such as are disclosed. Advantageously, desorption is formed with a plurality number toluene - diethylbenzene among others.

C8 - aromatic fractions containing xylene adsorption parameters to the selectivity of the number for the present invention according to adsorption, measured at its ignition loss is preferably 7 950 °C. 7% hereinafter, preferably 0 - 7. 7%, very preferably 3. 0% - 7. 7%, more preferably 3. 5% - 6. 5%, further preferably 4. 5% - 6% and, boundaries when optimum comprising are disclosed.

Water content feedstock and/or desorption number streams among the influent stream constituted by, e.g. feedstock and/or desorption number streams preferentially adding water to a wavelength of 20 ppm - 150 ppm.

It rises, light based adsorption number includes an improved mass transfer characteristics of the present invention number para - xylene selectivity of optimized characteristics while at the same time, to keep the maximum adsorbent, preferably para - xylene for simulating types of backflow of liquid phase separation process for use in preserve the high degree of mechanical strength.

Most in particular, the present invention according to number it rises, light based adsorption number 14 is greater than combined index (CI) exceeds 15 and generally with, this CI value compared to prior art adsorption number observed to completely in which an inhibin receptor.

CI index defined by the following formula:

Here

"Selectivity" - and para - xylene with meta - xylene and exhibits a selectivity between parameters,

"Capacity" parameter being represented -% xylene adsorb (cm column³ C adsorbed per_8- Aromatic cm³ )

Para - xylene column length - "EHTP" parameter is measured at theoretical plates exhibits equivalent height (expressed in %).

Various parameters includes the following conditions tests performed in liquid phase in the junction (breakthrough) one of the techniques:

- Adsorption temperature 175 °C and,

Circulating liquid test temperature (flow/column cross-section) is 1 - surface speeds. 3 cm. s^-1 And,

- D ethyl benzene and para - desorption solvent used,

The composition of feedstock - as follows:

●para - xylene: 45% by weight

●meta - xylene: 45% by weight

●isooctane: 10% by weight (this non-selective volume used as removed from the tracker for estimating not involved).

According to another aspect, the present invention refers to such as xylene isomers for gaseous or liquid phase separation prior defined in processes, exceeds 14, preferably greater than 15 having at least one number combination index (CI) use of it rises, light based adsorption number are disclosed.

In uses, it rises, light based adsorption number is said at least one number, including boundaries, advantageously 1. Exceeds 5 mpa, preferably 1. 7 mpa - 4 mpa, more preferably 1. 8 mpa - 4 mpa, most preferably 2 mpa - 4 mpa mechanical strength. In conjunction with the present invention, sized mechanical strength 1. Less than 6 mm for agglomeration and methods through a series SMS 1471 - 74 Shell method are disclosed.

Characterization techniques

It rises, number determining particle size of light

The present invention according to number of aggregation (step a) it rises, light crystals and it rises, light based adsorption number used FAU number determining an estimate of the scanning electron microscope (SEM) of number average diameter contained by using observation carried out.

Samples to estimate the size of in determining light it rises, number, less magnification of Figure 5000 series of phases are taken other. Determining the diameter of at least 200 of private software then measured by use of a substrate. Accuracy is approximately 3%.

It rises, light based adsorption number number of - Si/Al ratios and replaced chemical analysis:

The aforementioned steps a) to e) are publicly known to one skilled in the art for chemical analysis element of the final product obtained after the various analysis techniques may be followed according to disapproval. Among described, wavelength dispersion spectrometer (WDXRF), e.g. Bruker yarn number Tiger S8 machine described x ray fluorescent by chemical analysis techniques referred as standard NF EN ISO 12677:2011 disapproval.

X ray fluorescent is, away from elemental composition of the sample, in the range of photo luminescent (photoluminescence) spectral techniques using non-destructive x line atom are disclosed. X ray beam electron bombardment or by atoms of the excited atoms generally returns to the ground state after CLK3 specific radiation. X ray fluorescent spectrum is extremely dependent on the chemoselective chemical element to advantage, this number and precise determination both quantitatively and qualitatively under public affairs substrate. 0. 4% by weight of less than conventional measuring the fire rapidly each oxide obtained after correction are disclosed.

Such number of chemical analysis elements between the ratio Si/Al number used adsorbent of the adsorption number of atomic ratio Si/Al number bath during checking step c both in addition it rises, rotary cutter having) and selection steps d) may check for diffuse to the described ion exchange quality. In the description of the invention, the measurement of atomic ratio Si/Al the fire rapidly ± 5% are disclosed.

It rises, light based adsorption number number remaining after a removal for replacement ion exchange quality is sodium oxide, Na₂ O relative molar number. More accurately, barium ions heat exchange diagram, BaO molar number combinations (BaO + Na₂ O + K₂ O) between ratio estimation value by evaluating the molar number. Similarly, potassium oxide potassium ion exchange diagram, K₂ O molar number combinations (BaO + K₂ O + Na₂ O) between ratio estimation value by evaluating the molar number. The content of various oxides to the gross weight of a given number anhydride it rises, light based adsorption number as weight percent charcoal large substrate.

It rises, light based adsorption number number size:

Aggregation and formation step a) it rises, light based adsorption number obtained after the volume mean diameter of a determination of the number, camera samples in front of objective lens for passing conveyor belt, standard ISO 13322 - 2:2006 according to number of the sample particle size distribution analysis carried out by imaging by adsorption.

The volume mean diameter is then standard ISO 9276 - 2: by applying 2001 are calculated from the particle size distribution. In the synthesized, terms "volume mean diameter" or "size" number is it rises, light based adsorption number are completed. In the size range of accuracy of the present invention adsorption number nearly 0. 01 mm are disclosed.

The mechanical strength of it rises, light based adsorption number number:

As described in the present invention it rises, light based adsorption bed of coffee strength number number, associated with a yarn commercially available by Vinci Technologies BCS tester machine, Shell method SMS1471 provided 74 series (series SMS1471 provided 74 Shell method Catalyst bulk grinding intensity decision. Compression - sheave method) According to characterizing other. This method is intended to characterize the 3 mm - 6 mm of catalyst initially 425 method based on the use of micro m screen, this in particular separation diffuse to the fine component are generated during grinding. 425 micro m the use of screen 1. Particles having a diameter greater than 6 mm but still subjected to suitable, characterization of grain size number should tailored along which it is desired to adsorption.

Generally in the form of extrudates or beads of the present invention conventional adsorption number boundary intermediate 0. 2 mm - 2 mm, in particular 0. 2 mm - 0. 8 mm, preferably 0. 40 mm - 0. The volume mean diameter of 65 mm or length, i.e. in the case of non-spherical adsorption number has a longest dimension. As a result, 100 micro m Shell method mentioned in standard SMS 1471 - 74 are used instead of micro m screen screen 425.

Measuring protocol as follows: HTML (100 micro m) pre-screening and is at least 2 hours (300 °C Shell method mentioned in standard SMS 1471 - 74 instead) 250 °C pre-dried in an oven to a 20 cm³ Agglomerated number known to the internal cross-adsorption of sample is placed inside a metal cylinder. Agglomerated adsorption number to better spread the force exerted by the piston to 5 cm³ Steel beads through the bed, the sample irradiated by the piston increased force imparted substrate (1 installation. 6 mm diameter beads having a diameter of less than 2 mm for the use of particles of spherical in shape). Oil acquired in various pressure stages fine screening (100 micro m suitable screen) separated by a weighing with each other.

Bulk crushing strength (MPa) modulus of elasticity in the magazine pressure unit passes through the screen and are determined by the pressure of the sample exceeds a preset threshold value for the amount of fine minutes 0. 5 weight % raised to an other. This value is, the bed adsorption number obtained in accordance with the force exerted on the mass of an graphs display by using the fine minutes 0. 5 mass % accumulated fine minutes are obtained by interpolation. Mechanical bulk crushing strength is typically able to 0 kPa - generally and some ten MPa. 3 mpa - 3. 2 mpa are disclosed. Accuracy is made 0. Less than 1 mpa.

It rises, light based adsorption number number number of it rises, light based on:

It rises, light based on the content of non-number (NZP), e.g. aggregation binder and other other amorphous on content is calculated for added are:

NZP=100 - Σ (ZP),

The meaning of the present invention in an amount of total number of fractions it rises, light X ZP here exhibits.

It rises, light based adsorption number number number of it rises, light based fractions of mass amount

It rises, adsorption number number contained in the identification of x - ray diffraction (XRD) carried out by means of light fractions. This analysis carried out Bruker brand machine. It rises, light based adsorption number crystalline phases present in ICDD database the identification number by comparison sheets and carried out. For example, barium 6003 and X type number 38 - 0234 ("number it rises, light X, (Ba)") once it rises, rotary cutter having presence ICDD sheet to obtain a diffraction morality line identified by the comparison of will. It rises, light based fractions number amount of mass, which takes reference as a reference peak intensities, peak intensities of diffraction from evaluation with each other (the same chemical properties of number it rises, sprouts contemplated adsorption number of conditions the same cation processing conditions tend to 100% crystalline as well as is). 2 θ angular zone to the peaks may be 9° - 37° until crystallization of the strongest peaks, i.e., each 11° - 13°, 22° - 26°, 31° - 33° 2 θ angular range of peaks observed in are disclosed.

Micro pore volume and an outer surface

In addition micro pore volume and number of the present invention crystals it rises, light based adsorption number by measuring adsorption number crystallization of diagram, reference the same (the same cationic processing conditions it rises, light or theoretical 100% crystalline number number it rises, light) evaluated by compared with each other. Opposing surfaces of the micro pore volume determined from measurement of the adsorption of liquefied gas such as nitrogen at a temperature.

Before adsorption, it rises, light based sample number (either an adsorbent of the same number determining admitting,) the vacuum (P < 6. 7 × 10^-4 Pa) encoded in time to a time period of time 9 - 16 300 °C - 450 °C molten glass. 77 K formed in the nitrogen adsorption measurements of then 0. 002 - 1 non-P/P₀ Measuring points of relative pressure of at least 35 takes, from Micromeritics ASAP 2020 M carried out in machine.

Micro pore volume and external surface is, by t - plot method, standard ISO 15901 - 3:2007 - type type (Harkins-a Jura equation) by applying the statistical thickness (t) under [khin through opposing surfaces obtained by calculating determined from. External surface area of the micro pore volume, a linear regression slope from each y - from the axis to the origin, 0. 45 nm - 0. T of 57 nm obtained by linear regression in plot of points with each other. Micro pore volume per gram of liquid adsorbate adsorption anhydride evaluated number cm³ Represented. External surface area of the adsorption anhydride per gram of m number² Represented.

Macropores and maul parcel [e volume, microscopic pores and grain density distributions in mercury 33

Macropores and grain density measured by a mercury press maul parcel [e volume and porosity measurement (porosimetry) 2000. From Micromeritics Autopore^® 9500 mercury pressure pad is formed with microscopic pores and to macropores and maul parcel [e when used to determine volume of distribution analysis.

Standard ASTM D 4284 - 83 method described by referring machine manual experiments (the ignition loss of publicly known) pre-weighing the sample adsorption number (number it rises, light based particulate material may be measured) a porosity measurement window and then, after first the gas grudge which burns (at least 10 minutes 30 facilitate the micro mHg), a given pressure (0. 0036 mpa) then the mercury cell and filling the pores of a fore network 400 mpa mercury penetration to the sample in order to gradually increases the pressure in applying consists of. Each pressure stage in the mercury penetration pore volume increment (dV) is recorded. The number of pressure stages typically 0. 0036 mpa - 0. 2 mpa and approximately 15, 0. Approximately 90 2 mpa - 400 mpa are disclosed.

Pressure applied to the appearance pore diameter (D_Hg ) Relationship between, cylindrical pressurizes, between the wall of the contact angle of mercury surface tension of mercury 140° pressurizes and 485 dynes/cm are set by the target value. Pressure applied to the mercury are introduced according to an accumulated amount is recorded. All of the mercury filling voids temperatures value 0. 2 mpa is set, exceeds this value are deemed pressurizes mercury penetration of the granular material. Then, grain volume (Vg) is the pressure (0. 2 mpa) subtracted from the accumulated mercury from porosity by volume measure volume, and this difference anhydride equivalent mass of particulate material, i.e. an ignition loss of a mass of said material can be modified for a divided by the calculated substrate.

The inverse of grain volume (Vg) and grain density, cm³ Expressed in gram of number per anhydride adsorption.

Macropores volume granular material, having a diameter greater than 50 nm corresponding to included volume apparent pressurizes, 0. 2 mpa - 30 mpa introduced at a pressure of mercury is accumulated volume is defined. Pressure of mercury is introduced granular material 30 mpa - 400 mpa maul parcel [e volume cumulative volume is defined.

In the synthesized, cm³ . g^-1 Represented, it rises, light based adsorption number by connecting a number of volume and mass of mercury the macropores maul parcel [e volume and sample as anhydrous equivalent, i.e. an ignition loss of a mass of said material can be modified for a measured substrate.

Microscopic pores diameter distribution apparent pore diameter determined mercury 33 pressurizes (D_Hg ) Blocking unit volume distribution dV/dLogD_Hg Represented. dV/dLogD_Hg Values, an apparent pore diameter corresponding in both of the respective pressure stage in the value calculated from the mercury penetration pore volume increment (dV) are disclosed.

It rises, light based adsorption number number of ignition loss:

An ignition loss of standard NF EN 196 - 2 (April 2006) as described in the oxidizing ambient air at a temperature of 950 °C ± 25 °C by calcination of the sample determined. Measuring a standard deviation 0. Less than 1%.

Liquid phase adsorption characterization of junction:

The described techniques used to characterize porous solid molecules liquid phase adsorption, adsorbent components of grade implantation study each of junction as response curve defining, by Ruthven The principle of adsorption and adsorption processes (8 9 field and an, John Wiley & Sons, 1984) as described junction publicly known techniques are disclosed. Average discharge time (instantaneous number 1) analysis of the junction curves number information and are in addition to the amount adsorbed under public affairs selectivity, i.e. able to diffuse to the separation factor between two of adsorbent components 2.

The introduction of the non-absorbent and non-selective volume estimation used as tracer are recommended for. Analysis of the dispersion of junction curves (instantaneous number 2), direct measurements of mass transfer between adjacent dispersion for legal entity, a limited number of ideal stirring virtual reactors (theoretical stages) by column display able to diffuse to the equivalent height based on theoretical plates.

In the embodiment are:

In the embodiment A: Hierarchical porous FAU number it rises, rotary cutter having synthesis

High external surface area FAU number etc. it rises, sprouts Inayat papers (Angew. Chem. Int. Ed. , (2012), 51, 1962 - 1965) directly synthesized according.

Step 1): 300 rpm Archimedean screw in an agitated reactor growth gel number bath

Sodium hydroxide (NaOH) in 300 rpm stirring rate 25 min or 25 °C 119g, 128g of alumina trihydrate (Al₂ O₃ It 3H₂ O, 65. 2% by weight of Al₂ O₃ Containing) and 195. 5g water containing aluminate solution, 25 °C in 565. 3g sodium silicate, 55. 3g of NaOH and 1997. 5g containing silicate solution by mixing water, heating jacket, temperature probe and a stainless - steel reactor with stirrer gel encoded number growing in a bath.

Chemical isoolefins growth gel as follows: 3. 48 Na₂ O/Al₂ O₃ /3. 07 SiO₂ /180 H₂ O. 25 minutes stirring 300 rpm in the homogenizing 25 °C growth gel is carried out.

Step 2): introduction of structured number reaction medium

During 60% MeOH solution of TPOAC 27. 3g is 300 rpm stirring rate are introduced into the reaction medium (TPOAC/Al₂ O₃ Molar ratio=0. 04). 5 minutes after homogenizing, the stirring speed resulting in low 50 rpm.

Step 3): maturation step

The reaction medium is continued to 22 hours in 25 °C 50 rpm then the stir, crystallization is then disclosure with each other.

Step 4): crystallization

The stirring speed into a 50 rpm, reactor jacket 80 °C 80 medium is set to a value reactor 75 °C min or to nominal temperature substrate. 72 75 °C in at least two stages has been completed, reaction medium cooled by cycling a cold water through the jacket to maintain crystallinity.

Step 5): filtration/washing

The solids recovered using neutral pH (permuted water) applied after sintering water cleaned substrate.

Step 6): drying/calcination

In order to characterize the product, drying is carried out in an oven 90 °C to 8 hours, 22% by weight of the dried product is an ignition loss are disclosed.

A stand-alone (water) and the micro-porosity rate structured number number necessary to release both the dried product of calcination temperature profile maul soda production rate next carried out: 200 °C increased until 30 minutes, then 200 °C 1 time in at least two stages, then increased to the 550 °C 3 time, finally 550 °C 1 in at least two stages. 5 time.

X - ray diffraction (XRD analysis) obtained determinations are equal by determining a few identified with each other. Solid chemical analysis atomic ratio Si/Al=1. 24 a number under public affairs substrate. The resulting mesoporous number it rises, light (or hierarchical porous number it rises, light) obtained determination of the mean diameter of the number of 4. 5 micro m are disclosed.

10 hours after degassing under vacuum at 400 °C 77 K formed in the nitrogen adsorption method micro pore volume and external surface area of the plot measured according to t - from, each, expressed per gram of dry adsorption number 0. 260 cm³ . g^-1 And 90 m² . g^-1 Are disclosed.

In the embodiment B: Atomic ratio Si/Al=1. 25, 1. 0=1 Na/Al atomic ratio of number average diameter and having it rises, light X number determining micro m non-maul small porosity of synthesis

3 molar composition. 5 Na₂ O - 2. 8 SiO₂ - Al₂ O₃ - 130 H₂ Next reagent O of gel are: sodium silicate, sodium aluminate and water bath by encoded number. Gel time 35 °C and 20 in maturation, a determination 4 100 °C carried out in time.

X-ray diffraction (XRD analysis) determinations are obtained after filtration and washing by determining a few are identified as being equal. Solid chemical analysis atomic ratio Si/Al=1. 25 number a under public affairs substrate. The mean diameter of the number of number determining light it rises, 1. 0 micro m are disclosed. 10 hours after degassing under vacuum at 400 °C 77 K formed in the nitrogen adsorption method micro pore volume and external surface area of the plot measured according to t - from, each, expressed per gram of dry adsorption number 0. 345 cm³ . g^-1 And 2 m² . g^-1 Are disclosed.

It rises, light based adsorption number number number of bath

In the embodiment described procedures are homogenous mixture A or B number bath and it rises, NaX number prepared by the number of determinations are according 1600g rotary cutter having, allowing a mixture of extrusion with the amount of, and brand Klebosol 350g of kaolin (calcined equivalent)^® 30 (30% by weight of SiO₂ And 0. 5% of Na₂ O) of colloidal silica to a commercially available 130g agglomerated substrate. The paste extrusion before an ignition loss of 44% are disclosed. 1 diameter. 6 mm in extrudates are formed. In the extrudates are stored at 80 °C ventilation type oven dried substrate. In the 550 °C extrudates are then calcined in nitrogen stream after 2 hours, drying, after 2 hours in a stream of air to a calcined 550 °C decarbonization sulphonic, 0. 4 mm in equivalent diameter grinding thereby to recover the spaced with each other.

In the embodiment 1: (Comparison example)

Type X number it rises, light, 1. 0 number of micro m it rises, light crystals, and non-number types of binder having this [thu it rises, it rises, light based adsorption number number number of ground in the form of kaolin crude

In the embodiment B produced by powder granules obtained from (200 g) is 0 in step 4 of 95 °C. 5 M barium chloride using a solution exchange with each other. In each stage, the volumetric ratio of the mass of the solid to solution 20 ml. g^-1 4 every time exchanges and continuous with each other. Each exchange between, a stand-alone number exceeds the solids are cleaning several times in order to salt in solid amount. It is then time to a nitrogen stream at a temperature of 250 °C 2 activated substrate.

5 barium exchange diagram and the ignition loss of 97%. 4% are disclosed. 10 hours after degassing under vacuum at 400 °C 77 K formed in the nitrogen adsorption method micro pore volume and external surface area of the plot measured according to t - from, each, 0. 226 cm³ . g^-1 And 16. 7 m² . g^-1 Are disclosed.

Measured by mercury porosity measurements and total volume of macropores maul parcel [e 0. 32 cm³ . g^-1 Are disclosed. The volume fraction of the total volume of macropores and maul parcel [e macro pressurizes 0. 87 are disclosed.

Pore diameter distribution determined from analysis were performed mercury adsorption number 33 pressurizes an apparent diameter (D_Hg ) According to volume distribution dV/dLogD_Hg To exhibits. Distribution is controlled in a lambda value in the region of 350 nm peak corresponding macro pressurizes a special distribution type [ni[ni] wool month's desire.

In addition the description of the invention are measured according to the method number it became at the time of in mechanical strength. 0. 5% fine component necessary for obtaining pressure is 2. 2 mpa are disclosed.

In the embodiment 2: (Comparison example)

X types of number it rises, light, 1. 0 number of micro m it rises, light crystals, and number it rises, this [thu kaolin types of binder having grinding forms of number it rises, light based adsorption number number of bath

In the embodiment B produced by powder granules obtained from (200 g) is adjusted at a temperature of 100 °C ± 1 °C jacket with glass reactor disposed, concentration of 1 M aqueous sodium hydroxide 1. 5 L is then added 3 hours stirring the reaction medium to each other.

Then, the agglomerated continuous cleaning operation after reactor water 3 times cleaned in an emptying other. Cleaning efficiency, 10. 0 - 10. 5 ensure by measuring pH in final washing water are disclosed.

The aggregates of 95 °C 0 in step 4. 5 M barium chloride using a solution exchange with each other. In each stage, the volumetric ratio of the mass of the solid to solution 20 ml. g^-1 4 every time exchanges and continuous with each other. Each exchange between, a stand-alone number excess amount in order that the solid salt are cleaning several times. Then, it is time to a stream of nitrogen at a temperature of 250 °C 2 activated substrate.

5 barium exchange diagram and the ignition loss of 97%. 3% are disclosed. 10 hours after degassing under vacuum at 400 °C 77 K formed in the nitrogen adsorption method micro pore volume and external surface area of the plot measured according to t - from, each, 0. 249 cm³ . g^-1 And 5 m² . g^-1 Are disclosed.

Measured by mercury porosity measurements and total volume of macropores maul parcel [e 0. 29 cm³ . g^-1 Are disclosed. The volume fraction of the total volume of macropores and maul parcel [e macro pressurizes 0. 97 are disclosed.

Pore diameter distribution apparent pore diameter determined from analysis were performed mercury adsorption number 33 (D_Hg ) According to volume distribution dV/dLogD_Hg (1 also reference) to exhibits. Distribution is controlled corresponding to the area of 360 nm in concerning the special distribution peak in macropores type [ni[ni] wool month's desire.

It rises, light based on content non-number, the same as the barium exchange it rises, light decisions during the rough disclosure number reference, when measured by XRD, 5% by weight are disclosed.

In addition the description of the invention are measured according to the method number it became at the time of in mechanical strength. 0. 5% fine component necessary for obtaining pressure is 2. 5 mpa are disclosed.

In the embodiment 3: (Comparison example)

HPX types of number it rises, light, 4. 5 micro m number of it rises, light crystals, and non-number types of binder having this [thu it rises, it rises, light based adsorption number number number of ground in the form of kaolin crude

In the embodiment A produced by powder granules obtained from (200 g) is 0 in step 4 of 95 °C. 7 M barium chloride using a solution exchange with each other. In each stage, the volumetric ratio of the mass of the solid to solution 20 ml. g^-1 4 every time exchanges and continuous with each other. Each exchange between, a stand-alone number exceeds the solids are cleaning several times in order to salt in solid amount. It is then time to a nitrogen stream at a temperature of 250 °C 2 activated substrate.

5 barium exchange diagram and the ignition loss of 97%. 5% are disclosed. 10 hours after degassing under vacuum at 400 °C 77 K formed in the nitrogen adsorption method micro pore volume and external surface area of the plot measured according to t - from, each, 0. 192 cm³ . g^-1 And 70 m² . g^-1 Are disclosed.

Measured by mercury porosity measurements and total volume of macropores maul parcel [e 0. 33 cm³ . g^-1 Are disclosed. The volume fraction of the total volume of macropores and maul parcel [e macro pressurizes 0. 6 are disclosed.

In addition the description of the invention are measured according to the method number it became at the time of in mechanical strength. 0. 5% fine component necessary for obtaining pressure is 2. 1 mpa are disclosed.

Pore diameter distribution were performed mercury adsorption number 33 in Figure 1 determined from analysis apparent pore diameter (D_Hg ) According to volume distribution dV/dLogD_Hg To exhibits. The area of distribution and macropores show a peak and shoulders, in the area of about 55 nm to about 140 nm mode number 1 number 2 modes bimodal distribution in very small and macropores green substrate.

In the embodiment 4 (The instruction executing the present invention):

4. 5 micro m size HPX types of crystals, and this [thu number it rises, kaolin types of binder having grinding forms of number it rises, light based adsorption number number of bath

In the embodiment A produced by powder granules obtained from (200 g) is adjusted at a temperature of 100 °C ± 1 °C jacket with glass reactor disposed, concentration of 1 M aqueous sodium hydroxide 1. 5 L is then added 3 hours stirring the reaction medium to each other.

Then, the agglomerated continuous cleaning operation after reactor water 3 times cleaned in an emptying other. Cleaning efficiency, 10. 0 - 10. 5 ensure by measuring pH in final washing water are disclosed.

The aggregates of 95 °C 0 in step 4. 5 M barium chloride using a solution exchange with each other. In each stage, the volumetric ratio of the mass of the solid to solution 20 ml. g^-1 4 every time exchanges and continuous with each other. Each exchange between, a stand-alone number excess amount in order that the solid salt are cleaning several times. Then, it is time to a stream of nitrogen at a temperature of 250 °C 2 activated substrate.

5 barium exchange diagram and the ignition loss of 96%. 3% are disclosed. 10 hours after degassing under vacuum at 400 °C 77 K formed in the nitrogen adsorption method micro pore volume and external surface area of the plot measured according to t - from, each, 0. 260 cm³ . g^-1 And 12 m² . g^-1 Are disclosed.

Measured by mercury porosity measurements and total volume of macropores maul parcel [e 0. 29 cm³ . g^-1 Are disclosed. The volume fraction of the total volume of macropores and maul parcel [e macro pressurizes 0. 9 are disclosed.

Pore diameter distribution determined from analysis of Figure 1 to perform mercury adsorption number 33 apparent pore diameter (D_Hg ) According to volume distribution dV/dLogD_Hg To exhibits. Distribution is controlled in a lambda value in the region of 190 nm peak corresponding macro pressurizes a special distribution type [ni[ni] wool month's desire.

Figure 1 in the embodiment 2 in the embodiment 4 to the adsorption of mercury to perform number 33 curves determined from analysis distributions exhibits microscopic pores.

It rises, light based on non-number the same as the barium content exchange it rises, light decisions during the rough disclosure number reference, when measured by XRD, 5% by weight are disclosed.

In addition the description of the invention are measured according to the method number it became at the time of in mechanical strength. 0. 5% fine component necessary for obtaining pressure is 2. 5 mpa are disclosed.

In the embodiment 5:

Test (front chromatography) is then sent to the adsorption efficiency of junction number estimate adsorbed carried out in number. The test used in the amount of about 34g adsorption number are disclosed.

Curves junction for obtaining procedure is as follows:

With sheave●inserted into test bench for filling and column;

Filled●desorption solvent at room temperature;

A gradual increase of a sorbing temperature in the stream of solvent●(5 cm³ . Min^-1 );

A sorbing temperature●stopped after 30 cm³ . Min^-1 Of solventInjection;

Feedstock /●to inject feedstock substituted (permutation) solvent (30 cm³ . Min^-1 );

The introduction of the feedstock into the●then a period of time sufficient to thermodynamic equilibrium (i.e., zero (zero) until the concentration of the solvent during the effluent liquor) being maintained.

●junction of the effluent liquor collection and analysis.

Desorption solvent used para - diethylbenzene among others. The composition of feedstock as follows:

●para - xylene: 45% by weight,

●ethylbenzene: 45% by weight,

●isooctane: 10% by weight (this non-selective volume used as removed from the tracker for estimating not involved).

175 °C adsorption temperature tests carried out. Liquid feedstock be held on the pressure is sufficient, i.e. 1. 5 mpa are disclosed. Circulating liquid test temperature surface speeds (flow/column cross-section) with respect to all tests occur is approximately 1. 3 cm. s^-1 Are disclosed.

The selectivity of the material balance is calculated by meta - xylene parametric - xylene are disclosed. For table 1 encoded number ball junction results to:

Symbol description table (key)

●PX=para - xylene; MX=meta - xylene

●% represented adsorb (adsorbed C₈ - Aromatic cm³ /Cm column³ )

% Para - xylene measured theoretical plates●EHTP=column length expressed in equivalent height

●

In the embodiment 1 and 2 are compared to results obtained to adsorption of number, reflected by a height equivalent of a theoretical plate significantly reduced, which leads to a significant adsorption of mass transfer in number in the embodiment 4 and improvements are found.

In the embodiment 3 compared to results obtained to adsorption of number, para - xylene to meta - xylene (+ 17%) and which leads to a significant increase in the embodiment 4 which leads to a significant improvement in selectivity of adsorbent for adsorption of number are found.

Such parameters, capacity, selectivity and EHTP combination both CI index selectivity, capacity and mass transfer between negotiation under control can be mixed: higher index can comprise, negotiation better disclosed. Based on HPX decisions during the adsorption number, i.e. in the embodiment 3 and 4 (in the embodiment 4 is the instruction executing the present invention) are calculated in the number 1 and number 2 in the embodiment is adsorption of adsorption of CI indexes are calculated in the characteristic index varies very significantly superior to that the components on the substrate.

The present invention according to in the embodiment 4 is obtained in adsorption of the highest calculated CI index number, as a result, the adsorbing number will most efficient separation of para - xylene.

The present invention according to number it rises, light based adsorption number is good mechanical strength, good para - xylene adsorption selectivity, high adsorbent and adsorption number rapid delivery of the molecules in combination other.