Large-scale clean production method for enteromorpha polysaccharide

22-07-2015 дата публикации
Номер:
CN104788580A
Принадлежит: Third Institute of Oceanography SOA
Контакты:
Номер заявки: 18-10-20150188
Дата заявки: 16-04-2015

[1]

Technical Field

[2]

The invention belongs to the field of biological extraction separation technology, in particular to a polysaccharide Entermorpha the large-scale clean production method.

[3]

Background Art

[4]

Enteromorpha)   is the enteromorpha is the Chlorophyta, Ulvales, shi Chunke multi-cell eukaryote, is a large-scale marine chlorophycean. In widely distributed Entermorpha our coastal, a major types (  prolifera   Enteromorpha) Entermorpha, (  intestinalis Enteromorpha) intestinal Entermorpha, and (Enteromorphalinza), and (  clathrata Enteromorpha)strip enteromorphaflat enteromorpha (  compressa   Enteromorpha), and the like. With extremely strong Entermorpha anti-contravariance growth ability, from 2007 to 2014 years, a row of eight years past sea Entermorpha chlorophycean disasters outbreak of a large-scale, a serious impact on the water quality and the urban environment, to huge negative impact on Society.

[5]

A Entermorpha rich in carbohydrate, protein, low fat quality of marine algae, Entermorpha comprising in 40%   sugar, 9%-14%   protein, 32%-36%   ash, 6.7% -  9%   moisture, about 2%   fat [Aguilera   M,   Casas   M,   Carrillo   S,   et   al.   Chemical   composition   and   microbiological   assays   of   marine   alage   Enteromorpha   spp.   as   a   potental   food   source.   J   Food   Comp,   2005,   18 (1): 79-88.]. Waters he Qing Entermorpha Tunghai analysis of China's such as the main component is a polysaccharide and coarse fiber, the dried moss occupies the river bank 63.9%, the protein content is 27%, fat 0.9% [ he Qing , hu Xiaobo , seedling zhou Zhi , and the like. Tunghai chlorophycean and nutrient component analysis and evaluation. Marine science, 2006, 30 (1): 34-38]. Further study finds that, polysaccharide Entermorpha with immunomodulatory, anti-oxidation, anti-tumor, anti-aging, anti-radiation, reducing blood lipid, and moisturizing and the like function of a plurality of biological activity, as the glycan structure and active research, polysaccharide Entermorpha researchers at home and abroad has become hot.

[6]

At the same time because of rich in protein Entermorpha, minerals, pigments, and the like various components, therefore, need to adopt in addition to protein, in addition to salt, decolourizations and the like only after separation and purification steps to obtain a high content of polysaccharide Entermorpha. In addition to protein Sevage method of the traditional method, trifluoro trichlorethane law , trichloro acetic acid method, enzymatic, and the like, these in addition to protein method requires the use of a large number of chemical reagent or enzyme, high-cost and pollution, it is difficult to meet the requirement of mass production. A commonly used method for desalination of dialysis, negative and positive ion exchange resin and the like, wherein the dialysis method the efficiency is low, the need of space occupying relatively large. Commonly used decoloring method with ion exchange method, oxidation method, said metal complex, these decoloring method need of a large amount of use of acid-base or heavy metal, will cause serious environmental pollution. Therefore, there is an urgent need for the development of scale in the tundra from river bank polysaccharide preparation Entermorpha clean production process, waste, improve the economic and social benefit.

[7]

Content of the invention

[8]

The purpose of this invention is for the preparation of polysaccharide Entermorpha the defects existing in the prior art, to provide a raw material from Entermorpha Entermorpha preparing high content of the polysaccharide in the large-scale clean production method.

[9]

In order to realize the purpose of this invention, the solution of the invention is:

[10]

Polysaccharide Entermorpha of a large-scale clean production method, comprising the following steps:

[11]

1) grinding: Entermorpha used to dry the raw material into a crushing enteromorpha powder ;

[12]

2) extracting: enteromorpha powder after pulverization in the reactor, heating 20-60 times of water, control pH value is 6-13, the extraction temperature 60-100 the [...] , extraction time is 1-4 hours, to obtain the polysaccharide extract Entermorpha;

[13]

3) solid-liquid separation: centrifugal removing solid impurities extracted solution;

[14]

4) a primary microfiltration process: the tubular ceramic micro-filtration membrane to remove impurity to clarify the centrifugate;

[15]

5) two-stage ultrafiltration process: the feed flow path wide roll type ultra-filtration membrane to a type ceramic microfiltration process further concentrated to percolate, in addition to protein, in addition to salt and decolourizations;

[16]

6) drying: the two-stage ultrafiltration concentrate obtained after spray drying, the total sugar content of greater than 80%, protein content of less than 10%, ash content of less than 5% of the polysaccharide Entermorpha solid.

[17]

The step 3 is the speed 3000-13000rpm continuous flow centrifuge to remove solid impurities of the extraction liquid.

[18]

The step 4 of the ceramic micro-filtration membrane pore size 0.2-1.4 the  m, the ceramic film of the active layer is made of aluminum oxide or zirconium oxide or titanium oxide, is the highest tolerable temperature the 90 [...] , operating temperature 20-70   °C, the operating pressure is 0.1-0.6   MPa, the concentration multiple is 3-20 times, adding multiple is 0.3-1.5 times.

[19]

The step 5 is a roll type ultrafiltration membrane with molecular weight retention 30-200   KDa, the feed flow passage is 1-5   mm, operating temperature the 20-50 [...] , the operating pressure is 0.3-1   MPa, the concentration multiple is 5-30 times, adding multiple is 0.5-2 times.

[20]

The raw materials are selected from at least one of the following: Entermorpha, enterohaemorrhagic Entermorpha, and, or strip enteromorphaflat enteromorpha.

[21]

The invention effectively solves the problem that the polysaccharide Entermorpha traditional low separating efficiency in the production process, the production cost is high, pollution, it is difficult to scale to promote application shortcoming. The invention has the advantages of simple process flow high-efficiency, high separation selectivity, low energy consumption, avoiding the secondary pollution effectively and is easy to be industrialized amplifying, and the like, is especially suitable for low-value resource reuse and industrial production eliminating environmental pollution.

[22]

Mode of execution

[23]

The invention discloses a polysaccharide Entermorpha the large-scale clean production method, comprising the following steps:

[24]

1) grinding: Entermorpha used to dry the raw material into a crushing enteromorpha powder , raw materials are selected from at least one of the following: Entermorpha, enterohaemorrhagic Entermorpha, and, strip enteromorpha , such as flat enteromorpha ;

[25]

2) extracting: enteromorpha powder after pulverization in the reactor, heating 20-60 times of water, control pH value is 6-13, the extraction temperature 60-100 the [...] , extraction time is 1-4 hours, to obtain the polysaccharide extract Entermorpha;

[26]

3) solid-liquid separation: adopting rotating speed 3000-13000rpm continuous flow centrifuge to remove solid impurities extracted solution;

[27]

4) a primary microfiltration process: the tubular ceramic micro-filtration membrane to remove impurity to clarify the connectors, the ceramic micro-filtration membrane pore size 0.2-1.4 the  m, the ceramic film of the active layer is made of aluminum oxide or zirconium oxide or titanium oxide, is the highest tolerable temperature the 90 [...] , operating temperature the 20-70 [...] , the operating pressure is 0.1-0.6 MPa, the concentration multiple is 3-20 times, adding multiple is 0.3-1.5 times;

[28]

5) two-stage ultrafiltration process: the feed flow path wide roll type ultra-filtration membrane to a type ceramic microfiltration process further concentrated to percolate, in addition to protein, in addition to salt and decolourizations, the coiling-type ultra-filtration membrane is for molecular weight 30-200   KDa, the feed flow passage is 1-5   mm, operating temperature the 20-50 [...] , the operating pressure is 0.3-1   MPa, the concentration multiple is 5-30 times, adding multiple is 0.5-2 times;

[29]

6) drying: the two-stage ultrafiltration concentrate obtained after spray drying, the total sugar content of greater than 80%, protein content of less than 10%, ash content of less than 5% of the polysaccharide Entermorpha solid.

[30]

Example a:

[31]

The 50 kg Entermorpha enteromorpha powder used to dry, then adding 1500 kilograms of pure water, the extraction temperature control in the 70 [...] , stirring 4 hours, to obtain the polysaccharide extract Entermorpha;

[32]

Adopting rotating speed 10000   rpm continuous flow centrifuge to remove solid impurities of the above-mentioned extract solution;

[33]

The aperture is 1.4   µm tubular ceramic membrane of the continuous flow centrifuge to clarify the centrifugate edulcoration, the ceramic film of the active layer is made of alumina, the operating temperature of the 60 [...] , the operating pressure is 0.2   MPa, the concentration multiple is 4 times, adding multiple is 1.5 times;

[34]

With molecular weight of 200   kDa rolling hyperfilltration to a type ceramic microfiltration process for concentrating liquid permeable, in addition to protein, in addition to salt and decolourizations, the feed flow passage is 2   mm, the operating temperature of the 40 [...] , the operating pressure is 0.3   MPa, the concentration multiple is 10 times, adding multiple is 0.5 times;

[35]

The two-stage ultrafiltration concentrate obtained after spray drying, the total sugar content of greater than 90%, protein content of less than 5%, ash content of less than 5% of the polysaccharide Entermorpha solid.

[36]

Example b:

[37]

The 100 kg Entermorpha enteromorpha powder used to dry, then adding 5000 kilograms of pure water, using sodium hydroxide to adjust pH value to 9, the extraction temperature control in the 80 [...] , stirring 2 hours, to obtain the polysaccharide extract Entermorpha;

[38]

Adopting rotating speed 8000   rpm continuous flow centrifuge to remove solid impurities of the above-mentioned extract solution;

[39]

The aperture is 0.8   µm tubular ceramic membrane of the continuous flow centrifuge to clarify the centrifugate edulcoration, the ceramic film of the active layer is made of zirconia, the operating temperature of the 65 [...] , the operating pressure is 0.3   MPa, the concentration multiple is 10 times, adding multiple is 1 times;

[40]

With a molecular weight of 150   kDa rolling hyperfilltration to a type ceramic microfiltration process for concentrating liquid permeable, in addition to protein, in addition to salt and decolourizations, the feed flow passage is 1.5   mm, the operating temperature of the 40 [...] , the operating pressure is 0.35   MPa, the concentration multiple is 15 times, adding multiple is 0.5 times;

[41]

The two-stage ultrafiltration concentrate obtained after spray drying, the total sugar content of greater than 85%, protein content of less than 8%, ash content of less than 5% of the polysaccharide Entermorpha solid.

[42]

Example three:

[43]

The 150 kg Entermorpha enteromorpha powder used to dry, then adding 6000 kilograms of pure water, using sodium hydroxide to adjust pH value is 10, the extraction temperature control in the 90 [...] , stirring 1 hour, to obtain the polysaccharide extract Entermorpha;

[44]

Adopting rotating speed 12000   rpm continuous flow centrifuge to remove solid impurities of the above-mentioned extract solution;

[45]

The aperture is 0.5   µm tubular ceramic membrane of the continuous flow centrifuge to clarify the centrifugate edulcoration, the ceramic film of the active layer is made of titanium oxide, the operating temperature of the 70 [...] , the operating pressure is 0.35   MPa, the concentration multiple is 6 times, adding multiple is 1 times;

[46]

With molecular weight cut-off of 100   kDa rolling hyperfilltration to a type ceramic microfiltration process for concentrating liquid permeable, in addition to protein, in addition to salt and decolourizations, the feed flow passage is 2   mm, the operating temperature of the 45 [...] , the operating pressure is 0.4   MPa, the concentration multiple is 12 times, adding multiple is 1 times;

[47]

The two-stage ultrafiltration concentrate obtained after spray drying, the total sugar content of greater than 85%, protein content of less than 8%, ash content of less than 5% of the polysaccharide Entermorpha solid.

[48]

[49]

Example four:

[50]

The 200 kg Entermorpha enteromorpha powder used to dry, then adding 10000 kilograms of pure water, using sodium hydroxide to adjust pH value to 11, the extraction temperature control in the 90 [...] , stirring 1 hour, to obtain the polysaccharide extract Entermorpha;

[51]

Adopting rotating speed 8000   rpm continuous flow centrifuge to remove solid impurities of the above-mentioned extract solution;

[52]

The aperture is 0.4   µm tubular ceramic membrane of the continuous flow centrifuge to clarify the centrifugate edulcoration, the ceramic film of the active layer is made of alumina, the operating temperature of the 70 [...] , the operating pressure is 0.3   MPa, the concentration multiple is 5 times, adding multiple is 1 times;

[53]

With a molecular weight of 50   kDa rolling hyperfilltration to a type ceramic microfiltration process for concentrating liquid permeable, in addition to protein, in addition to salt and decolourizations, the feed flow passage is 3   mm, the operating temperature of the 45 [...] , the operating pressure is 0.5   MPa, the concentration multiple is 15 times, adding multiple is 0.5 times;

[54]

The two-stage ultrafiltration concentrate obtained after spray drying, the total sugar content of greater than 90%, protein content of less than 5%, ash content of less than 5% of the polysaccharide Entermorpha solid.

[55]

Of the above, is only example of execution of this invention, and the technical scope of the present invention to do any restriction, of the invention is therefore based on the technical essence to the above-mentioned embodiment for any slight modification of the, equivalent to change and modification, are still belongs to the within the scope of technical scheme of the invention.



[1]

The invention discloses a large-scale clean production method for enteromorpha polysaccharide. According to the method, large-scale clean production of the enteromorpha polysaccharide is realized by using enteromorpha as raw materials through the steps of smashing, extracting, solid-liquid separation, tubular ceramic microfiltration, roll type ultrafiltration and spray-drying. The method has the advantages that a technological process is simple and efficient, protein removal, desalting and decoloration can be realized synchronously, separation selectivity is high, energy consumption is low, secondary pollution is effectively avoided, industrialized enlargement is facilitated, and the method is especially suitable for low-value resource development and utilization and industrial production requiring to eliminate environmental pollution.



1. Polysaccharide Entermorpha of a large-scale clean production method, comprising the following steps:

1) grinding: Entermorpha used to dry the raw material into a crushing enteromorpha powder ;

2) extracting: enteromorpha powder after pulverization in the reactor, heating 20-60 times of water, control pH value is 6-13, the extraction temperature 60-100 the [...] , extraction time is 1-4 hours, to obtain the polysaccharide extract Entermorpha;

3) solid-liquid separation: centrifugal removing solid impurities extracted solution;

4) a primary microfiltration process: the tubular ceramic micro-filtration membrane to remove impurity to clarify the centrifugate;

5) two-stage ultrafiltration process: the feed flow path wide roll type ultra-filtration membrane to a type ceramic microfiltration process further concentrated to percolate, in addition to protein, in addition to salt and decolourizations;

6) drying: the two-stage ultrafiltration concentrate obtained after spray drying, the total sugar content of greater than 80%, protein content of less than 10%, ash content of less than 5% of the polysaccharide Entermorpha solid.

2. Polysaccharide Entermorpha of a method for producing large-scale clean according to Claim 1, characterized in that the step 3 is the speed 3000-13000rpm continuous flow centrifuge to remove solid impurities of the extraction liquid.

3. Polysaccharide Entermorpha of a method for producing large-scale clean according to Claim 1, characterized in that the stated step 4 ceramic micro-filtration membrane aperture of 0.2-1.4 the  m, the ceramic film of the active layer is made of aluminum oxide or zirconium oxide or titanium oxide, is the highest tolerable temperature the 90 [...] , operating temperature 20-70   °C, the operating pressure is 0.1-0.6   MPa, the concentration multiple is 3-20 times, adding multiple is 0.3-1.5 times.

4. Polysaccharide Entermorpha of a method for producing large-scale clean according to Claim 1, characterized in that the stated step 5 is a roll type ultrafiltration membrane with molecular weight retention 30-200   KDa, the feed flow passage is 1-5   mm, operating temperature the 20-50 [...] , the operating pressure is 0.3-1   MPa, the concentration multiple is 5-30 times, adding multiple is 0.5-2 times.

5. Polysaccharide Entermorpha of a method for producing large-scale clean as in Claim 1, 2, 3 or Claim 4, characterized in that the stated step 1 raw materials are selected from at least one of the following: Entermorpha, enterohaemorrhagic Entermorpha, and, or strip enteromorphaflat enteromorpha.