PROCEDURE FOR the PRODUCTION OF ALKYLATED n AND/OR AMINO, AMMONIUM OR SPIROBICYCLI GROUPS OF AMMONIUM of HALTIGEN, INTERLACED POLYMERS

The invention concerns a technical procedure for the production of alkylated Nbzw. Amino, Ammoniumoder spirobicyclischen or groups of ammonium of haltiger, interlaced polymers, which are used for example in the medicine for the lowering of the Cholesterinspiegels by connection of bile acids and/or by bile acid salts, as for instance Colesevelam hydrochloride. The production of these polymers takes place thereby in several steps, like networking, cutting, alkylation up, washing with several wash steps between the individual stages and drying process. So far from the state of the art, as for instance from WHERE 98/43653; WHERE 99/33452; WHERE 99/22721; US 5,496,545; EP 0 90g 768; WHERE 99/34786; WHERE 98/29107; WHERE 00/32656, WHERE 02/22695, polymer Preprints 2000, 41 (1), 735 u.s.w, well-known procedures for the production of alkylated, interlaced Nbzw. Amino, Ammoniumoder spirobicyclische groups of ammonium haltigen polymers, for example by networking of Polyallylaminhydrochlorid with epichlorohydrin, and following alkylation, approximately with (6-Bromhexyl) - tri methyl ammonium bromide and 1-Bromdecan, suffer from the circumstance not to be suitable for a production process in the technical yardstick. With the first process step, which leads networking an uncontrolled hardening by precipitation in the reaction boiler to the formation of a polymer block, whereby damages at the equipment can occur, for example at the agitator. Additionally high requirements exist concerning an efficient load intermediate cleaning to technical gelling equipment. Cutting the hardened raw gel up takes place according to state of the art in relatively uncontrolled way, approximately via Zerrühren of the gel body in a container. Since after this step unequally large particles are present, a homogeneity is with the following chemical reactions and does not ensure wash steps, what to increased by-product formation and worse wash efficiency leads. A possibility for the production of Partikelchen with the desired mechanical characteristics is according to state of the art the suspension polymerization, however additional solvents are necessary for this procedure. Washing of raw gel serves mainly for the distance of the inorganic salt formed in preceded the step and taken place according to conditions the technology by means of water and possibly in the following with an alcohol, like isopropanol or methanol. It has very an unfavorable effect that raw gels pour very strongly with water (5 - 40 subject) and it thus around large volume and uneconomic process steps acts. Additionally making more difficult the very bad filtration achievements of these gels affect themselves. Since the water in the subsequent step (alkylation) disturbs, it is displaced with some procedures by isopropanol. Thus however an additional solvent during the process emerges, which brings among other things the implementation to a separate Lösungsrnittelaufarbeitung with itself. The drying process of the raw gel in the water-damp condition is described according to state of the art as very laborious with typical drying times of 1 week. Isopropanol-damp raw gel is easier under acceptance of the disadvantage of an additionally necessary solvent already described to dry. Apart from the general disadvantage of a drying process as aufwändigen process step, still its high oxidation sensitivity comes to carrying with the RohgeI drying process. Raw gel contains contrary to the alkylated final product unprotonierte amino groups, which form by-products with traces of oxygen. The following step is alkylation for example with Bromodecan and (6-Brom-hexyl) - tri methyl ammonium bromide. During the production of (6-Brom-hexyl) - tri methyl ammonium bromide are according to state of the art, like in Synth. Commun. (1999), 29 (14), 2393-2398 described, the yields with 78% low, the response times with 24 hours very long and the used solvents, as in this case tetrahydrofurane, which is inclined during a solvent processing very strongly to the peroxide formation, process-technically disadvantageous and besides expensively. Other manufacture methods as in A. Gray et al., J. To. Chem. Soc. 77, 3648 (1955) descriptive, wise better raw yields up, have however the disadvantage that likewise are enough for response time the high surplus of Dibromhexan (1.5 subject), necessary by one day, and the use of benzene as solvent, which is harmful both for humans and environment. Due to the low quality of the raw product must be recrystallized here in addition from tert butanol, which draws an additional expenditure for a solvent processing. 2 RKs 411,463 B with alkylation concerns a heterogeneous reaction, with which the particle size and also the particle size distribution of the assigned raw gel play a large role. With past alkylating procedures is not considered to this circumstance, so that during the diffusion-controlled reactions uncontrolled quantities of halogenhaltigen by-products, as for example for instance Chlordecan and/or Chloroquat, and when using methanol as solvents in combination with aqueous caustic soda solution of by-products, like Methoxydecan and/or Methoxyquat u.s.w, to develop. A further disadvantage of usual alkylating procedures are the unsatisfactory alkylating yields and are enough for response times. With the procedures after state of the art partly also extremely long filtration times (e.g. 24 hours) arise with the following wash steps due to the different particle size. In addition the considerable portion of volatile organic impurities from the polymers and/or gels must be eliminated afterwards by several alcohol/NaCI laundry or alcohol laundry. Since the swelling behaviour of the gels varies during the individual wash steps relatively strongly and the Trockensubstanzgehalt of gels is generally very small (between 8 - 40%), is the arrangement and the selection of the wash mechanisms of special importance, in order to keep on the one hand the throughput small highly and around on the other hand the solvent consumption of the washing solutions. The solvent preparation represents a further point. Task of the available invention was therefore it, a procedure for the production of alkylated Nbzw. Amino, ammonium or spirobicyclische groups of ammonium more haltiger to find interlaced gels and/or polymers which are suitable for a production process in the technical yardstick. A goal were in particular technical processes for the production of raw gels (networking), their washing, drying process and alkylation, production of quaternären halogen alkyl ammonium salts, as for instance (6-Brom-hexyl) - tri methyl ammonium bromide, as well as the consistent vote of these processes one on the other, in order to finally come to as simple and efficient a manufacture process under guarantee of the quality requirements (as small a formation of by-products as possible) and high yield as possible. Unexpectedly this task could be solved by a manufacture process, with not only optimal single steps to the networking, raw gel cutting, gel washing and AIkylierung was found, but also equal a whole step and a solvent to be completely eliminated could. The subject of the invention is from there a procedure for the production of alkylated Nbzw. Amino, ammonium or spirobicyclische or groups of ammonium of haltiger, interlaced polymer gels, which are characterized by the fact that a) in the networking step an aqueous solution of a polymer at a temperature from 0 to 90°C to a pH value of 7.5-14 is stopped, afterwards the appropriate cross linkage material is metered and under agitating pre+interlaced and the vorvernetz.te polymer for complete hardening by precipitation into a hardening container is transferred, on which b) the hardened raw gel into a defined form is cut, c) with methanol batchweise in static or agitated bed is then washed and directly afterwards to d) in methanol alkylation by addition one or several Alkylatoren at a temperature from 5 to 90°C and a pressure from 1 to 3 bar, addition of a base and if necessary Reprotonierung is continuously washed effected, on which the alkylated gel e) first by means of methanol/NaCI laundry batchweise in static or agitated bed or continuously and afterwards f) by means of NaCI laundry and concluding water wash with entsalztem water batchweise in static or agitated bed or. With the procedure according to invention alkylated, interlaced, Nbzw become. Amino, Ammoniumoder spirobicyclische groups of ammonium haltige polymers manufactured. With these polymers it acts around polymers, for example in WHERE 00/32656, WHERE 00/38664, WHERE 99/33452, WHERE 99/22721, WHERE 98/43653, WHERE 02/22696, US 5,624,963 and US 5,496,545, as well as in polymer Preprints 2000, 41 (1), 735 is descriptive. For the procedure according to invention in particular kationische polymers are suitable. To the kationischen polymers among other things such polymers, which contain an amine N atom, belong as for instance to RK 41 1 463 B primary, secondary or tertiary groups of amines or salts of it, quaternäre groups of ammonium and/or spirobicyclische groups of ammonium. Additional kationische groups contain Amidino, Guanidino, Imino etc. The kationische polymer is characterised by the fact that it exhibits a positive load at the physiological pH value. Examples of suitable kationische polymers contain Polyvinylamine, Polyallylamine, Polydiallylamine, Polyvinylimidazole, Polydiallylalkylamine, Polyethylenimine etc., as well as polymers containing out for example WHERE the 00/32656, side 7f. ; WHERE 98/43653, side 4f. ; US 5.496.545, column 2 to 4; US 5,624,963; WHERE u.s.w, admitted 98/29107, repeating units. According to invention the polymers used for the procedure exhibit further negatively charged Gegenionen. This Gegenionen can be organic or inorganic ions or combinations of it. Suitable Gegenionen contains likewise from the state of the art already quoted admitted Gegenionen. Examples of suitable inorganic ions are halides, in particular chloride, phosphates, Phosphite, carbonates, Bicarbonate, sulfates, Bisulfate, hydroxides, nitrates, Persulfate, sulfites and sulfides. Examples of suitable organic ions are acetates, Ascorbate, Benzoate, Lactat, Fumarat, Maleat, Pyruvat, CIT rate, Dihydrogencitrate, hydraulic gene CIT rate, Propionat, Butyrat, oxalates, Succinate, Tartrate, Cholate etc. With the first process step according to invention the polymers, which will receive by polymerization of the appropriate monomers in accordance with the state of the art can, are interlaced. Suitable cross linkage materials contain from literature places already quoted admitted cross linkage materials. Examples of it are epichlorohydrin, Succinyldichlorid, ethyl diamine, Toluoldiisocyanat, Diacrylate, Dimethacrylate, until acrylamideacrylamide until acrylamides, Dichlorethan, Dichlorpropan, U.S, W, preferred the networking on 2 reactors are divided, whereby the problems, like uncontrolled hardening by precipitation in the reaction boiler, arising in accordance with the state of the art, are avoided. In a suitable mixture reactor, preferentially also high-polished high-grade steel surface with installed CIP nozzles (CIP = clean into place), an aqueous solution of the appropriate polymer, as for instance 50% a ige Polyallylaminhydrochlorid solution according to invention with water and caustic soda solution, prefers 30% industrial union to 60% industrial union, mixed. A pH value of 7.5 - 14 is stopped. Preferentially a pH value of 9,5 is - 10.6 and particularly preferential from 9,8 to 10,4. The mixture temperature is with 0 to 90°C, preferentially with 5 - 30 °C and particularly preferentially with 1015°C. Subsequently, this reaction mixture is transferred preferentially into a suitable gelling reactor and the appropriate cross linkage material, as for instance epichlorohydrin, is chargiert for networking. To the Vorvernetzung the reaction mixture 1 to 240 minutes, prefers 10 to 120 minutes and particularly prefers 15 to 30 minutes agitated. To short agitating leads to a two-phase reaction mixture and in the consequence to an inhomogenous product, while to long agitating leads to the uncontrolled hardening by precipitation in the gelling boiler. The before-interlaced mixture is then filled up into suitable hardening containers and hardened in accordance with state of the art by standing to leave. The gelling reactor and also before-interlaced gel the pipings come into contact are cleaned according to invention with water. The gelling reactor possesses for the purpose of an efficient cleaning prefers a high-polished high-grade steel surface as well as CIP nozzles. In step b) the hardened raw gel into a defined form is cut. Cutting the raw gel up into a defined form, prefers in cubes with an edge length of 1 to 3 mm, and with defined particle size distribution effected prefers in accordance with the Austrian patent application A 1630/2001. The homogeneity necessary for the following reaction steps and wash steps is ensured by cutting up into a defined form according to invention. In step c) the cut raw gel batchweise according to invention in the static or in agitated bed exclusively with methanol is washed. The step effected thereby at a temperature of 1 °C to 65 °C, preferentially with 5 to 60°C, particularly prefers with 10 to 40°C. The raw gel laundry (step c) taken place after cutting the block gel due to the compressibility of the gel prefers according to invention in an agitating boiler or in a RührfilterAT 411,463 B nutsche, whereby particularly prefer the solvent supply been made from the ground of the agitating boiler or Rührfilternut and the exhaust of the used up Waschmediums by an immersion tube, until a certain limit value at water is reached. If necessary can be also agitated in case of the ground supply. The supply of the solvent can be made however also by head into the agitating boiler or into Rührfilternut. The raw gel washing takes place according to invention exactly with the solution means, i.e. with methanol, in which also alkylation is accomplished. Unexpectedly become by washing also excluding methanol in relation to the state of the art (for example polymer Preprints 2000, 41 (1), page 735-736) still further advantages obtained: By washing according to invention with methanol instead of with water and afterwards with isopropanol, the strong swelling of the raw gel in the water is avoided. Further become large volume and uneconomic process steps, which are necessary when using water, and bad filtration achievements of the gels poured in water avoided. By the elimination of isopropanol from the process the otherwise necessary solvent processing for isopropanol is void. Contrary to the simple distillation of methanol the processing of isopropanol is process engineering only very with difficulty and aufwändig feasible. In addition a diaphragm procedure is necessary or a E×traktivdestillation. An additional solvent processing in the comparison to the state of the art is not necessary, since methanol is again contained of alkylation already in the subsequent step. According to invention the wash achievement is increased by washing by saving of the quantity of the entirely necessary washing solution compared to above mentioned state of the art. Further when washing through exhaust of the supernatant washing liquid by means of immersion tube from the wash boiler contrary to the use of conventional filtration apparatuses, like centrifuge or Filternut, equipment and charge time one saves. In accordance with the state of the art the drying process of the raw gel takes place following washing. A drying process of the raw gel according to invention becomes redundant in connection with the use of the same solvent described above, both during the raw gel washing and with alkylation. Thus again substantial savings at equipment, handling and charge time result. In the next step the alkylation of the raw gel (step d) takes place. At the time of the execution of the technical alkylating reaction are crucial the employment grain size defined by gel with the appropriate mechanical characteristics, and close particle size distribution. Further the process must be so laid out that these characteristics are lost with no step. In addition it is to be preserved necessarily the gel before mechanical load, as for example as possible by drastic reduction of agitating times. Unexpectedly in the technical plant with certain operations, only very short necessary agitating times within the minute range were determined. It found that a short obligation mixture is always necessary by means of agitators, when and after bringing in of raw materials and reagents, afterwards however the convection mixture by return flow cooking is sufficient. During alkylation according to invention to the gel suspension stirred up in methanol the appropriate AIkylatoren is admitted. By Alkylatoren reactants are to be understood, those, if they are converted with an interlaced polymer, cause that an alkyl group or a derivative of it, as for instance a substituted alkyl group etc., is bound kovalent to or several of the N-atoms in the polymer. Suitable Alkylatoren is thereby connections of the formula RX, which an alkyl group or an alkyl derivative with 1 to 24 C-flavours exhibit (R), which and/or to a group of outlets (X) is bound, as she already admits from the state of the art already quoted is. R is therefore a linear, branched or cyclischer alkyl residue with 1 to 24 C-atoms, preferential with 4 to 20 C-atoms, or an alkyl derivative, as for instance a c1 - C20 -, prefers C4 - C20 - group of hydroxyalkyls, CT-C20 - Aralkylgruppe, c1 - C20 -, C4 - C20 - group of alkyl ammonium or C - prefers C20, prefers C4 - C20 - Alkylamidogruppe. X is an electrical file group of outlets, for example from the group of the halides, like RK 411,463 B for instance chloride, bromide, fluoride, iodide or for example a group of outlets such as Epoxy, Tosylat, Mesylat or Triflat. The Alkylator can contain thereby one or more groups of outlets. Examples of preferential Alkylatoren are c1 - C24 - alkyl halides, as for instance n-butyl halide, n-Hexylhalogenid, n-Decylhalogenid, n-Dodecylhalogenid, n-Tetradecylhalogenid, n-Octadecylhalogenid, etc., c1 - C24 - Dihalogenalkane, as for instance 1,10-Dihalogendecan, etc., C - C24 - hydroxyalkyl halides, as for instance 11-Halogen-l-undecanol, etc., c1 - C24 - Aralkylhalogenide, as for instance benzyle halide, substituted benzyle halides, etc., c1 - C24 - Alkylepoxyammoniumsalze, as for instance Glycidylpropyl trimethyl ammonium salt, etc., C - C24 - Epoxyalkylamide, as for instance n (2,3Epoxypropan) butyramid, n (2,3-Epoxypropan) hexane amide, etc., C - C24 - halogen alkyl ammonium salts, as for instance (4-Halogenbutyl) - tri methyl ammonium salt, (6-Halogenhexyl) - tri methyl ammonium salt, (8-Halogenoctyl) - tri methyl ammonium salt, (10-Halogendecyl) - trimethylammoniu msalz, (12-Halogendodecyl) - tri methyl ammonium salt, etc. Preferential Alkylatoren is Bromdecan and 6-Brom-hexyl-trimethylammonium-bromid. With the alkylating reaction one or more Alkylatoren can be added. The Alkylatoren is used with the procedure according to invention depending upon desired alkylating degree. The synthesis of Colesevelam hydrochloride is to supply for example a polymer structure, with which approximately 12% of the amines of the Polyallylamingerüstes interlace, approximately to % with of the amines of the Polyallylamingerüstes with Decylgruppen and approximately 34% of the amines of the Polyallylamingerüstes with Trimethylammonium hexyl groups provided is, as well as approximately 14% of the amines of the Polyallylamingerüstes as primary amines to exist remain (polymer Preprints 2000, 41 (1), 735-736). The determination of the different alkylating degrees can be determined very simply compared with a selected reference substance by analysis of the C/N relationship and the number of free amines (titratable amines). The addition of the Alkylatoren takes place at a temperature between 5 and 90°C and with a pressure from 1 - 3 bar. Before or after the addition for example the gel on 25 to 90°C, suspended in methanol, can be heated up, preferentially on 35 to 65°C and particularly preferentially on boiling temperature of methanol. Preferred the agitator of the alkylating boiler is switched on during the heating phase for the indulgence of the gel only periodically (e.g. every 30 minutes) and only in each case for short time (e.g. 2 - 3 minutes). After addition or the Alkylatoren is still through-mixed the reaction mixture, whereby the mixing time prefers between 1 and 60 minutes, 5 to 50 minutes and particularly prefers 10 to 40 minutes lies. Subsequently, with the addition at base one begins. As a base for this NaOH, KOH, NH4 OH, are suitable LiOH, approx. (OH) 2, Ba (OH) 2, close and NaNH2 as a function of the used solvent. Preferred NaOH is used. The addition of the base effected prefers in several portions. Preferred for the indulgence of the gel the agitator of the alkylating boiler is switched on only during the Chargierung of the base and for short time thereafter (e.g. 10 minutes). In particular it was found that the convective mixing due to the return flow cooking during possible longer post-reaction times (type. 8 - 10 hours) completely is sufficient. The alkylating reaction is terminated, if at least 95 to 99% the Alkylatoren is abreacted, which takes place according to invention in the comparison to the state of the art around 30% faster. After end of the reaction the gel in methanol is reprotoniert by addition of an acid. Preferred for the indulgence of the gel the agitator of the alkylating boiler is switched on only during the Chargierung of the acid and for short time thereafter (e.g. 10 minutes). As acids for the Reprotonierung are suitable all mineral acids and organic acids, which lead to the Gegenionen already stated. These are for example HCI, HBr, H2 SO4, H3 PO4, HNO3 u.s.w, as well as formic acid, acetic acid, oxalic acid, citric acid, Brenztraubensäure, maleic acid, fumaric acid, Propionsäure, tartaric acid etc. Wishing case can take place the Reprotonierung of the alkylated gel however also at the end of one or several Methanolund/or methanol/salt, for example NaCI, - laundry. The methanol/sodium chloride laundry in step e) can take place according to invention after alkylation, 6 RKs 411,463 B as descriptive for the raw gel laundry. Particularly preferentially washing takes place in a wash tower or an agitating boiler, whereby the gel cake is present after filtration of the gel suspension in static or agitated bed and the methanol/sodium chlorid solution is made from the ground and the exhaust by an immersion tube, until a certain limit value at organic by-products is reached. As soon as this is reached, can be filtered if necessary the gel cake up to dry ones. If necessary the gel cake in a continuously operated washing column can be washed (figure 1). In order to exchange afterwards the bromide ions of the quaternären ammonium groupings with chloride ions, according to invention washing with a sodium chlorid solution after the methanol/sodium chloride laundry (step f) takes place. Particularly preferred a sodium chlorid solution is used, which exhibits a smaller concentration than 2 molecular (0,1 - 1,9 molecular), in order to cause due to the density variation between the gel particles filled with organic solvent and the sodium chlorid solution no Aufschwimmen. If necessary also a sodium chlorid solution of higher concentration (to concentrated sodium chlorid solution) can be used, in order to steer aimed a Aufschwimmen of the gel particles and thus washing the against the current in a column. Applying the sodium chlorid solution on the gel bed effected prefers by spraying, since thereby despite a considerable contraction and thus cracking in the gel bed an efficient washing is ensured. The prints of the washing solution on the gel cakes can be accomplished likewise, however more washing solution one needs. The water washing effected prefers in similar way, like the sodium chloride washing by spraying. In case of the water wash however the entire Waschmedium can be applied on the gel bed and pressed by the gel cake. Natriumchloridund water washing can take place however also via suspension laundry into Rührfilternut or in an agitating boiler. The last wash step effected then prefer on Filternut, a band filter or a centrifuge. If necessary the NaCIund water washing can take place continuously via use of in series of switched columns (figure 1). By the procedure according to invention, which becomes from the steps according to invention networking in two separated reaction boilers under adherence to of a special pH value and a special temperature, cuts of the gel into a defined form, washing with alcohol under exhaust of the supernatant washing solution by means of immersion tube and alkylation the disadvantages of the past from the state of the art admitted procedures avoided. A special advantage is void a drying step before the alkylating step, necessary in accordance with state of the art. In addition by the gel washing the according to invention, with consideration of of the physical-chemical characteristics of the gel, became in the comparison to the state of the art (polymer Preprints 2000, 41 (1), 735) a Waschverfahren found, with which the solvent consumption and the mixture of the used solvents can be kept high minimum and the throughput per unit volume. The result is that the WaschIösungsmittelmenge which can be used can be doubled over up to 66% be reduced and the throughput. The gel wash procedure is the subject of the available invention therefore likewise. A further advantage of the total procedure according to invention is the higher total throughput by reduction of the response time around approx. 30% (of approx. 20 h, and/or 26 h in accordance with state of the art on 14-16 h). Example 1: Interlaced technical production one with Epichiorhydrin Polyallylaminhydrochlorides, alkylation and washing: a) Networking: In the mixing tank g 1 under agitating 320.2 kg demineralized water and 236.0 kg of 50% ige Polyallylaminhydrochlorid solution were submitted. Subsequently, with caustic soda solution (50% industrial union) a pH value was stopped between 9,8 - 10.4. The received mixture was agitated 20 minutes with 20 °C, cooled down on 13 °C and transferred then into the gelling reactor R2. There under agitating 2.36 kg RK 411,463 B RST epichlorohydrin were chargiert and 20 minutes for homogenization were further-agitated. For hardening by precipitation contents of R2 were filled up into a barrel. The curing time amounted to 18 hours. The gelling reactor was rinsed with 50 kg demineralized water, in order to avoid the unwanted hardening of gel remainders in the reactor. The yield amounted to 625 kg raw gel (100%). b) Cuts and c) wash the hardened raw gel: 1400 kg hardened raw gel were cut in the pure area by means of gel cut apparatus into the reactor R3 (right parallelepipeds with approx. 2 x 2 x 2 mm of edge length). For suspending 2920 kg methanol were chargiert, which transfers gel 20 minutes stirred up and the suspension into the wash boiler R4. The wash mother liquor was expressed over an immersion tube. Altogether 3 washing with methanol were accomplished. d) Alkylation: The washed methanol-damp raw gel was suspended in the reactor R4 in 1200 kg methanol and transferred in the AIkylierungskessel R5. To this agitated suspension a solution was chargiert by 376 kg (6-Bromhexyl) - tri methyl ammonium bromide in 220 kg methanol, as well as 260 kg 1-Bromdecan. The reaction mixture in R5 was heated on 60 °C, whereby to the mixing with optimum mechanical indulgence of the gel particles the agitator only all minutes for 2 - 3 minutes was switched on. With 60 - 70 °C under agitating 53 kg of caustic soda solution (50%) were admitted and afterwards still further 10 minutes were agitated, before the reaction mixture became to leave 2 hours under return flow cooking. In this way altogether 4 portions of caustic soda solution were chargiert. The post-reaction took place during the following 8 hours return flow cooking with 60 - 70 °C with switched off agitator. Reprotonierung: Contents of R5 were cooled down under agitating on 40 °C, 240 kg concentrated hydrochloric acid (34% industrial union) and the agitator was chargiert was switched off after further 10 minutes. Wash the alkylated gel: The received gel suspension was transferred into the wash reactor R6 and shifted 4 times under agitating with 1680 kg each methanol and 255 kg of NaCI solution (10.9%) and filtered off after 20 of minütiger agitating time over an immersion tube. Subsequently, the gel cake on Drucknut (F1) 6 times was washed to each of 3000 kg demineralized water with 1800 - 3000 kg of NaCI solution (10.9%) and 6 times with ever 1800 -. Drying process: The damp gel was dried according to the state of the art up to a drying loss of maximally 3%. 1750 kg (100%) became product with a Trockensubstanzgehalt of max. 4% receive. Solvent regeneration: The distillation of methanol took place in two stages. The first stage in the column K1 was a Vordestillation with sourly stopped feed for the distance of volatile basic amines (allyl amine). In the collecting main B1 the basic methanolic filtrates from the wash boiler R4 with the sour filtrates from R5 were mixed and &lt before the task on K1 by means of sulfuric acid on a pH; 2 posed. The Vordestillat consisted of a mixture methanol I water. This was separated in the second stage with the column K2. A comparison example for the production of Coleveselam is after state of the art in the literature polymer Preprints 2000, 41 (1), page 735-736. Example 2: C) raw gel laundry comparison attempt walked in accordance with state of the art (see also regulation in polymer Preprints 2000; 41 (1), 735): In order to manufacture 677 g dried and washed raw gel, for SuspensionsAT 411,463 B production were admitted to the cut up gel by 5300 g (approx. 4300 g correspond to raw gel in accordance with procedures according to invention) of 10 litres water. Subsequently, the gel was washed by means of suspension laundry with 10, 15 and 20 litres water to 3 time, whereby in each case 1 hour was agitated. Subsequently, with 17 I Ispopronal was washed and the gel after filtration on Filtemut was dried. The yield amounted to 680 G. Raw gel laundry in accordance with procedures according to invention: a): 4300 g of the cut raw gel were washed to 3 time with 8600 g each methanol via suspension laundry. Subsequently, the gel was dried, whereby one received 662 g of easy-yellowish granulates. b): 4300 g of the cut raw gel were washed to 3 time with 8600 g each methanol via suspension laundry. After filtration the received filter cakes by 4268 g directly for the next reaction step (alkylation) one used. c): 4300 g of the cut raw gel were washed in such a way with 27000 g methanol that under agitating the methanol quantity of the ground of the agitating boiler was pumped by the gel suspension. The supernatant solution was sucked off by means of immersion tube. The received gel suspension of 6380 g was used directly for a next reaction step (alkylation). Table 1: Confrontation of the used wash quantities with same wash efficiency: Ständ of the technology a) b) c) kg water; 17 I isopropanol 25,8 kg methanol 25,8 kg methanol 27 kg methanol example 3: E walked) Methanol /NaCI laundry: Vergleichsbeispie/: State of the art (see also regulation in polymer Preprints 2000; 41 (1), 735): In order to manufacture 727 g dried Colesevelam hydrochloride, the reprotonierte gel was washed with 15.92 kg methanol via Suspensionsoder displacement laundry. Methanol/NaCI laundry in accordance with procedures according to invention: a): Based on the beginning with a size of 1900 g raw gel (approx. 730 g correspond to dried Colesevelam hydrochloride) 3 suspension laundry with 5 kg each (in sum kg) was accomplished methanol. b): On the beginning with a size of 1900 g raw gel (approx. 730 g correspond to dried Colesevelam hydrochloride) 3 suspension laundry with 4,4 kg each (in sum 13,2 kg) became based methanol/NaCI (87/13 Gew,% = 90/10 Vol%; 2M NaCI solution) accomplished. c): On the beginning with a size of 1900 g raw gel (approx. 730 g correspond to getrocknerem Colesevelam hydrochloride) 5 suspension laundry with 2,1 kg each (in sum 10,5 kg) became based methanol/NaCl (87/13 Gew,% = 90/10 Vol%; 2M NaCI solution) so accomplished that after setting off leave surplus methanol over the gel cake to the gel suspension by means of immersion tube one sucked off. d): Based on the beginning with a size of 1900 g raw gel (approx. 730 g correspond to dried Colesevelam hydrochloride) was in such a way washed the gel from the ground that in sum only 5,3 kg methanol/NaCl (87/13 Gew, % = 90/10 Vol%) were used, in order to manufacture a specification-fair product. Table 2: Confrontation of the used wash quantities with same wash efficiency: 9 RKs 411,463 B state of the art 'a) b) c) d) 15,9 kg methanol 15,0 kg methanol/NaCI 13,2 kg methanol/NaCl 10,5 kg methanol/NaCI 5,3 kg methanol/NaCI example 4: F) NaCl laundry walked: State of the art (see also regulation in polymer Preprints 2000; 41 (1), 735): In order to manufacture 727 g dried Colesevelam hydrochloride, the reprotonierte became after gel effected MeOHbzw. MeOH/NaCI laundry washed with 43.2 kg 2M of aqueous NaCI solution via Suspensionsoder displacement laundry. a): Based on the beginning with a size of 1900 g raw gel (approx. 730 g correspond to dried Colesevelam hydrochloride) 6 laundry with 5,3 kg each (in sum 32 kg) was accomplished 2M of aqueous NaCI solution, whereby after each wash step completely one filtered off. b): Based on the beginning with a size of 1900 g raw gel (approx. 730 g correspond to dried Colesevelam hydrochloride) was in such a way washed the gel by spraying with aqueous 2M NaCILösung that in sum only 20,5 kg of solvent were used, in order to manufacture a specification-fair product. Table 3: Confrontation of the used wash quantities with same wash efficiency: State of the art 43,2 2M NaCI solution a) 32,0 2M NaCI solution b) 20,5 2M NaCI solution example 5: Water wash: State of the art (see also regulation in polymer Preprints 2000; 41 (1), 735): In order to manufacture 727 g dried Colesevelam hydrochloride, the reprotonierte gel was washed after effected MeOHund NaCI laundry water entionisiertem with 44 kg via Suspensionsoder displacement laundry. a): Based on the beginning with a size of 1900 g raw gel (approx. 730 g correspond to dried Colesevelam hydrochloride) 6 laundry with 4,97 kg each (in sum 29,8 kg) was accomplished entionisiertem water, whereby after each wash step completely one filtered off. b): Based on the beginning. with a size of 1900 g raw gel (approx., hydrochloride corresponds to 730 g dried Colesevelam) was washed in such a way the gel by spraying or applying with entionisiertem water that in sum only 13,2 kg of solvent were used, in order to manufacture a specification-fair product. Table 4: Confrontation of the used wash quantities - task was it to achieve the same wash efficiency: State of the art 44,0 kg entionisiertes water a) 29,8 kg entionisiertes water b) 13,2 kg entionisiertes water