CN106633120B - A kind of preparation method of chitosan crosslinked alcohol soluble protein - Google Patents
A kind of preparation method of chitosan crosslinked alcohol soluble protein Download PDFInfo
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- C08B37/003—Chitin, i.e. 2-acetamido-2-deoxy-(beta-1,4)-D-glucan or N-acetyl-beta-1,4-D-glucosamine; Chitosan, i.e. deacetylated product of chitin or (beta-1,4)-D-glucosamine; Derivatives thereof
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Abstract
A kind of preparation method of chitosan crosslinked alcohol soluble protein, belongs to new material technology field.The present invention is using dried rice slag or wheat protein powder or corn protein powder and chitosan as raw material, by the step of preparing alcohol soluble protein solution, preparation chitosan solution, preparing chitosan crosslinked alcohol soluble protein reaction solution and prepare chitosan crosslinked alcohol soluble protein copolymer, crosslinking rate is prepared up to 55~65% chitosan crosslinked alcohol soluble protein copolymer of yellowish-brown.The present invention makes chitosan form schiff bases by glutaraldehyde with alcohol soluble protein by connect, and crosslinking rate is high, cross-linked stable is good；Cross-linking products have the characteristics that good skin-friendly, antibiotic property and thermo forming；The cross-linking reaction mild condition, easy to operate, raw materials used to be easy to get, low production cost is environmentally protective, and the chitosan crosslinked alcohol soluble protein prepared can be widely applied to the fields such as weaving, clothes, food.
Description
One, technical field
The invention belongs to new material technology fields, and in particular to a kind of preparation method of chitosan crosslinked alcohol soluble protein.
Two, background technology
New material industry is the strategic emerging industries of state key development, is the base of all strategic emerging industries development
Plinth and guide.And the new type natural polymer composite for synthesizing alternative fossil resources then becomes Research Emphasis and hot spot, is
One of the main flow direction of polymeric material field future development, thus dive with very important urgent, scientific and application
Power.
Chitosan system chitin N- deacetylation products, structure be 2- acetylaminohydroxyphenylarsonic acid 2- deoxidation-D- glucopyranoses and
The linear polymer that 2- amino -2- deoxidation-D- glucopyranoses pass through β-(Isosorbide-5-Nitrae) glucosides key connection.Chitin and chitosan has
There are numerous unique physicochemical properties and bioactivity, such as cationic polyelectrolyte, multifunctional groups reactivity, antibacterial
Property, film forming, biocompatibility and biodegradability etc., amino, hydroxyl, acetylamino, oxygen are contained in molecular structure
Bridge and pyranoid ring isoreactivity group rich in electronics can occur hydrolysis, alkylation, be acylated, carboxymethyl under given conditions
The chemical reactions such as change, sulfonation, nitrification, halogenation, oxidation, reduction, condensation and complexing.At present chitosan and its derivative medicine,
The numerous areas such as food, functional material, cosmetics, agricultural, environmental protection, household chemicals base biotechnology show wide application
Foreground.But the chitosan and its derivative disadvantage that there is also brittleness is big, irritation is strong, modification need to be modified to it, side
It can be used for more extensive field or place.
Alcohol soluble protein is primarily present in the seed of plant, its name is obtained because being dissolved in 50~90% ethanol solution.Due to richness
Not soluble in water containing glutamine residue, alcohol soluble protein is currently only used for doing the coated fertilizer of tablet or for making daily use chemicals original
Material or feedstuff, purposes and its limited, added value is extremely low.
Chitosan and alcohol soluble protein are rich in free primary amine groups, and glutaraldehyde is a kind of common bifunctional reagent, is contained
There are two aldehyde radical, aldehyde radical is conducive to the attack of nucleopilic reagent, and theoretically, under optimum conditions, the aldehyde radical on glutaraldehyde can
Schiff base structure is formed with the glutamy amido of alcohol soluble protein and the free primary amino group of chitosan, forms new polymers, it should
New polymers has heat not only in conjunction with the advantageous property of chitosan and alcohol soluble protein, especially antibiotic property and film forming
Machine-shaping and degradable new function can be used for preparing the wider field such as textile fabric.Therefore, synthesis chitosan is repaiied
The alcohol soluble protein base novel composite material of decorations is necessary.
The existing method for preparing chitosan derivatives, such as " chitosan-is bright for University Of Chongqing's Master's thesis disclosed in 2006
The MTGase of glue copolymer is catalyzed and synthesized and is characterized ", method disclosed in the paper is to use commercially available thick microorganism transglutamin-ase 9
Enzyme powder (MTGase) is raw material, is first purified to commercially available thick MTGase, is then catalyzed chitosan by the MTGase of purifying
Primary amino group is reacted with gelatin glutamy amido generation transglutamin-ase 9 and is crosslinked, and the disadvantages of this method is：1. since MTGase is
Protein, so its catalytic action condition has certain limitations, especially when containing inhibitor (or deactivator) in catalyst system and catalyzing,
The catalysis activity of enzyme will be weakened significantly, thus its cross-linking efficiency is poor；2. the higher price of enzyme carries out pure by using commercially available thick enzyme
Change extraction, but its purification process heavy workload, process is cumbersome, is unfavorable for realizing industrialization.
In another example application No. is CN200610034875.9, entitled " enzymolyzed wheat mucedin and polysaccharide cross-linked polymerics
Method " patent of invention, which disclose a kind of methods of enzymolyzed wheat mucedin and polysaccharide cross-linked polymeric, including：
(1) wheat gluten protein digests；(2) enzymolyzed wheat mucedin and polysaccharide copolymerzation with cross-linking, obtain copolymer；(3) separation copolymerization
Object is centrifuged off insoluble part, obtains soluble fraction, soluble fraction is concentrated into a concentration of 25~30%, spray drying.It should
The shortcomings that method is：1. being crosslinked using ultrasonic wave auxiliary law, reaction is not easily controlled, has side reaction, and microwave is anti-
It answers device expensive, laboratory can only be limited in and synthesized on a small scale, it is difficult to large-scale industrial production；2. egg in wheat gluten
White matter content is 70% or so, still contains much starch, and after enzymolyzed wheat mucedin, also much starch does not utilize still,
Waste vast resources；3. using phosphate buffer solution come enzymolyzed wheat mucedin, the processing of phosphate buffer solution can increase
Cost, and pollute the environment.
Three, invention content
The purpose of the present invention is for the existing shortcoming for preparing carbohydrate cross-linked proteins derivative method, provide one kind
The preparation method of chitosan crosslinked alcohol soluble protein prepares chitosan crosslinked alcohol soluble protein with the present invention and not only maintains alcohol soluble protein
Good compatibility, and good antibiotic property is also added, the chitosan crosslinked alcohol soluble protein prepared has antibacterial, pro-skin
Etc. characteristics, can be applied to the fields such as weaving, clothes, food.
The present invention cardinal principle be：Contain a large amount of hydrophilic hydroxyl groups and amino using chitosan, in alcohol soluble protein strand
Also contain a large amount of free amine group, these amino there are a lone pair electrons, have very strong nucleophilicity, and glutaraldehyde is a kind of common
Bifunctional reagent, containing there are two aldehyde radical, aldehyde radical is conducive to the attack of nucleopilic reagent, and chitosan on alcohol soluble protein
Amino has very strong nucleophilicity, therefore the aldehyde radical on dialdehyde substance can form schiff bases with the amino of chitosan and alcohol soluble protein
Structure, to which chitosan and alcohol soluble protein to be successfully crosslinked, crosslinking is mainly intermolecular generation.
The object of the present invention is achieved like this：A kind of preparation method of chitosan crosslinked alcohol soluble protein, with dried rice
Slag or wheat protein powder or corn protein powder and chitosan are raw material, by preparing alcohol soluble protein solution, preparing chitosan solution, system
It standby chitosan crosslinked alcohol soluble protein reaction solution and the step of preparing chitosan crosslinked alcohol soluble protein copolymer, prepares crosslinking rate and reaches
55~65% chitosan crosslinked alcohol soluble protein copolymer of yellowish-brown.Its specific processing step is as follows：
(1) alcohol soluble protein solution is prepared
Dried rice slag or wheat protein powder or corn protein powder are scattered in the ethanol solution that volumetric concentration is 70~85%,
30~40min of stir process under the rotating speed of 100~120r/min, wherein dried rice slag or wheat protein powder or corn protein powder
It is 1: 8~10 (kg/L) that quality, which is the ratio between 70~85% volume of ethanol solution with volumetric concentration,.It is taken out after the completion of processing
Filter collects filtrate respectively and filter residue is used to prepare feed addictive to the filter residue of collection；It is 50 in temperature to the filtrate of collection
~60 DEG C, vacuum degree be 0.09~0.1MPa under conditions of be concentrated in vacuo, until concentrate without ethanol flavor when stop, then plus
Enter ethylene glycol to be handled, processing time is 20~30min, and wherein the volume ratio of concentrate and ethylene glycol is 1: 2~4 (L/L).
After the completion of processing, that is, alcohol soluble protein solution is prepared, is used to prepare chitosan crosslinked alcohol soluble protein reaction solution.
(2) chitosan solution is prepared
The ratio between the HCL aqueous solution volumes for being 0.5~1.5% according to chitosan mass and mass fraction are 1: 20~40 (kg/
The chitosan that molecular weight is 30~50KDa is dissolved in the HCL aqueous solutions, according still further to chitosan by ratio L) under stiring
The ratio between quality and ethylene glycol volume are the ratio of 1: 5~15 (kg/L), and ethylene glycol is added, and after mixing, that is, it is poly- to prepare shell
Sugar juice prepares chitosan crosslinked alcohol soluble protein reaction solution for lower step.
(3) chitosan crosslinked alcohol soluble protein reaction solution is prepared
It is first 1: 1~3 according to the ratio between volume of chitosan solution and alcohol soluble protein solution after the completion of (1) and (2) step
(L/L) ratio, two kinds of solution that (1) and (2) step is prepared are uniformly mixed, according still further to glutaraldehyde and chitosan solution body
The ratio between product is the ratio of 1: 100~200 (L/L), and glutaraldehyde solution, the quality percentage of glutaraldehyde wherein in glutaraldehyde solution is added
A concentration of 25%~50%.Then 40~50 DEG C are warming up to, 1~2h is reacted, just prepares chitosan crosslinked alcohol soluble protein reaction
Liquid prepares chitosan crosslinked alcohol soluble protein copolymer for lower step.
(4) chitosan crosslinked alcohol soluble protein copolymer is prepared
After the completion of (3) step, chitosan crosslinked alcohol soluble protein reaction solution prepared by (3) step is pumped into vacuum filter
It is filtered, collects filtrate and filter residue respectively.To the filtrate of collection, for recycling ethylene glycol；To the filter residue of collection, with volume hundred
Divide a concentration of 80~95% ethyl alcohol washing, the ratio between the ethyl alcohol volume that wherein filter residue quality is 80~95% with concentration expressed in percentage by volume
For 1: 6~8 (kg/L).It is pumped into vacuum filter and is filtered again after the completion of washing, collect filtrate and filter residue respectively.To receiving
The filtrate of collection, contains unreacted alcohol soluble protein, and can be used for lower batch after recycling ethyl alcohol prepares alcohol soluble protein solution；Filter to collection
Slag, be sent into vacuum drying chamber in, carried out under conditions of temperature is 50~60 DEG C, vacuum degree is 40~50Pa vacuum drying 24~
30h, that is, prepare filemot chitosan crosslinked alcohol soluble protein copolymer, and total recovery rate reaches 56.3%~64.8%.
The present invention is after adopting the above technical scheme, mainly have the following effects：
1, the present invention makes chitosan form schiff bases by glutaraldehyde with alcohol soluble protein by connect, and crosslinking rate is high, crosslinking is steady
Qualitative good, cross-linking products have good skin-friendly；
2, using alcohol soluble protein ethylene glycol solution and chitosan HCl/water solution, ethylene glycol is miscible with water, in liquid-liquid reactions
Under the conditions of, resistance to mass tranfer is relatively low, and chitosan is easy to be reacted with alcohol soluble protein, and crosslinking rate is up to 55~65%；
3, since chitosan has antibiotic property, crosslinking rate is high, and antimicrobial sites are more, therefore antibiotic property is strong.Such as the chitosan
Crosslinking alcohol soluble protein copolymer reaches 41.7% to the antibiotic property of Escherichia coli；
4, the cross-linking reaction mild condition, easy to operate, raw materials used to be easy to get, low production cost is environmentally protective, prepares
The chitosan crosslinked alcohol soluble protein gone out can be widely applied to the fields such as weaving, clothes, food, have huge society and economy valence
Value；
5, the chitosan crosslinked alcohol soluble protein copolymer melting range is 162~163 DEG C, has the characteristics of thermo forming, can
It is used to prepare the wider field such as textile fabric.
Four, specific implementation mode
With reference to embodiment, it further illustrates the present invention.
Embodiment 1
A kind of preparation method of chitosan crosslinked alcohol soluble protein, specific processing step are as follows：
(1) alcohol soluble protein solution is prepared
Dried rice slag is scattered in the ethanol solution that volumetric concentration is 70%, under the rotating speed of 100r/min at stirring
30min is managed, it is 1: 8 (kg/L) that the quality Yu volumetric concentration of wherein dried rice slag, which are the ratio between 70% volume of ethanol solution,.
It is filtered after the completion of processing, collects filtrate respectively and filter residue is used to prepare feed addictive to the filter residue of collection；To collecting
Filtrate, be concentrated in vacuo under conditions of temperature is 50 DEG C, vacuum degree is 0.09MPa, until concentrate without ethanol flavor when
Only, ethylene glycol is then added to be handled, the volume ratio of processing time 20min, wherein concentrate and ethylene glycol are 1: 2 (L/
L).After the completion of processing, that is, alcohol soluble protein solution is prepared, is used to prepare chitosan crosslinked alcohol soluble protein reaction solution.
(2) chitosan solution is prepared
The ratio between HCL aqueous solution volumes for being 0.5% according to chitosan mass and mass fraction are the ratio of 1: 20 (kg/L),
The chitosan that molecular weight is 30~50KDa is dissolved under stiring in the HCL aqueous solutions, according still further to chitosan mass and second two
The ratio between alcohol volume is the ratio of 1: 5 (kg/L), and ethylene glycol is added and prepares chitosan solution after mixing, is used for lower step
Prepare chitosan crosslinked alcohol soluble protein reaction solution.
(3) chitosan crosslinked alcohol soluble protein reaction solution is prepared
It is first 1: 1 (L/L) according to the ratio between volume of chitosan solution and alcohol soluble protein solution after the completion of (1) and (2) step
Ratio, two kinds of solution that (1) and (2) step is prepared are uniformly mixed, according still further to glutaraldehyde and chitosan solution volume it
Than the ratio for 1: 100 (L/L), glutaraldehyde solution is added, wherein the mass percentage concentration of glutaraldehyde is in glutaraldehyde solution
25%.Then 40 DEG C are warming up to, 1h is reacted, just prepares chitosan crosslinked alcohol soluble protein reaction solution, it is poly- to prepare shell for lower step
Sugar crosslinking alcohol soluble protein copolymer.
(4) chitosan crosslinked alcohol soluble protein copolymer is prepared
After the completion of (3) step, chitosan crosslinked alcohol soluble protein reaction solution prepared by (3) step is pumped into vacuum filter
It is filtered, collects filtrate and filter residue respectively.To the filtrate of collection, for recycling ethylene glycol；To the filter residue of collection, with volume hundred
Divide a concentration of 80% ethyl alcohol washing, the ratio between the ethyl alcohol volume that wherein filter residue quality is 80% with concentration expressed in percentage by volume is 1: 6
(kg/L).It is pumped into vacuum filter and is filtered again after the completion of washing, collect filtrate and filter residue respectively.Filter to collection
Liquid, contains unreacted alcohol soluble protein, and can be used for lower batch after recycling ethyl alcohol prepares alcohol soluble protein solution；To the filter residue of collection, send
Enter in vacuum drying chamber, is dried in vacuo for 24 hours, that is, prepared yellowish-brown under conditions of temperature is 50 DEG C, vacuum degree is 40Pa
The chitosan crosslinked alcohol soluble protein copolymer of color, total recovery rate reach 56.3%.
Embodiment 2
A kind of preparation method of chitosan crosslinked alcohol soluble protein, specific processing step are as follows：
(1) alcohol soluble protein solution is prepared
Wheat protein powder is scattered in the ethanol solution that volumetric concentration is 80%, the stir process under the rotating speed of 110r/min
35min, it is 1: 9 (kg/L) that the quality Yu volumetric concentration of wherein wheat protein powder, which are the ratio between 80% volume of ethanol solution,.It has handled
It is filtered after, collects filtrate respectively and filter residue is used to prepare feed addictive to the filter residue of collection；To the filtrate of collection,
It is concentrated in vacuo, is stopped when until concentrate is without ethanol flavor, then under conditions of temperature is 55 DEG C, vacuum degree is 0.095MPa
Ethylene glycol is added to be handled, the volume ratio of processing time 25min, wherein concentrate and ethylene glycol are 1: 3 (L/L).Processing
After the completion, that is, alcohol soluble protein solution is prepared, chitosan crosslinked alcohol soluble protein reaction solution is used to prepare.
(2) chitosan solution is prepared
The ratio between HCL aqueous solution volumes for being 1% according to chitosan mass and mass fraction are the ratio of 1: 30 (kg/L), will
Molecular weight is that the chitosan of 30~50KDa is dissolved under stiring in the HCL aqueous solutions, according still further to chitosan mass and ethylene glycol
The ratio between volume is the ratio of 1: 10 (kg/L), and ethylene glycol is added and prepares chitosan solution after mixing, is used for lower step
Prepare chitosan crosslinked alcohol soluble protein reaction solution.
(3) chitosan crosslinked alcohol soluble protein reaction solution is prepared
It is first 1: 2 (L/L) according to the ratio between volume of chitosan solution and alcohol soluble protein solution after the completion of (1) and (2) step
Ratio, two kinds of solution that (1) and (2) step is prepared are uniformly mixed, according still further to glutaraldehyde and chitosan solution volume it
Than the ratio for 1: 150 (L/L), glutaraldehyde solution is added, wherein the mass percentage concentration of glutaraldehyde is in glutaraldehyde solution
50%.Then 45 DEG C are warming up to, 1.5h is reacted, just prepares chitosan crosslinked alcohol soluble protein reaction solution, shell is prepared for lower step
Glycan is crosslinked alcohol soluble protein copolymer.
(4) chitosan crosslinked alcohol soluble protein copolymer is prepared
After the completion of (3) step, chitosan crosslinked alcohol soluble protein reaction solution prepared by (3) step is pumped into vacuum filter
It is filtered, collects filtrate and filter residue respectively.To the filtrate of collection, for recycling ethylene glycol；To the filter residue of collection, with volume hundred
Divide a concentration of 90% ethyl alcohol washing, the ratio between the ethyl alcohol volume that wherein filter residue quality is 90% with concentration expressed in percentage by volume is 1: 7
(kg/L).It is pumped into vacuum filter and is filtered again after the completion of washing, collect filtrate and filter residue respectively.Filter to collection
Liquid, contains unreacted alcohol soluble protein, and can be used for lower batch after recycling ethyl alcohol prepares alcohol soluble protein solution；To the filter residue of collection, send
Enter in vacuum drying chamber, carries out vacuum drying 27h under conditions of temperature is 55 DEG C, vacuum degree is 45Pa, that is, prepare yellowish-brown
The chitosan crosslinked alcohol soluble protein copolymer of color, total recovery rate reach 61.6%.
Embodiment 3
A kind of preparation method of chitosan crosslinked alcohol soluble protein, specific processing step are as follows：
(1) alcohol soluble protein solution is prepared
Corn protein powder is scattered in the ethanol solution that volumetric concentration is 85%, under the rotating speed of 120r/min at stirring
40min is managed, it is 1: 10 (kg/L) that the quality Yu volumetric concentration of wherein corn protein powder, which are the ratio between 85% volume of ethanol solution,.
It is filtered after the completion of processing, collects filtrate respectively and filter residue is used to prepare feed addictive to the filter residue of collection；To collecting
Filtrate, be concentrated in vacuo under conditions of temperature is 60 DEG C, vacuum degree is 0.1MPa, until concentrate without ethanol flavor when
Only, ethylene glycol is then added to be handled, the volume ratio of processing time 30min, wherein concentrate and ethylene glycol are 1: 4 (L/
L).After the completion of processing, that is, alcohol soluble protein solution is prepared, is used to prepare chitosan crosslinked alcohol soluble protein reaction solution.
(2) chitosan solution is prepared
The ratio between HCL aqueous solution volumes for being 1.5% according to chitosan mass and mass fraction are the ratio of 1: 40 (kg/L),
The chitosan that molecular weight is 30~50KDa is dissolved under stiring in the HCL aqueous solutions, according still further to chitosan mass and second two
The ratio between alcohol volume is the ratio of 1: 15 (kg/L), and ethylene glycol is added and prepares chitosan solution after mixing, is used for down
Step prepares chitosan crosslinked alcohol soluble protein reaction solution.
(3) chitosan crosslinked alcohol soluble protein reaction solution is prepared
It is first 1: 3 (L/L) according to the ratio between volume of chitosan solution and alcohol soluble protein solution after the completion of (1) and (2) step
Ratio, two kinds of solution that (1) and (2) step is prepared are uniformly mixed, according still further to glutaraldehyde and chitosan solution volume it
Than the ratio for 1: 200 (L/L), glutaraldehyde solution is added, wherein the mass percentage concentration of glutaraldehyde is in glutaraldehyde solution
25%.Then 50 DEG C are warming up to, 2h is reacted, just prepares chitosan crosslinked alcohol soluble protein reaction solution, it is poly- to prepare shell for lower step
Sugar crosslinking alcohol soluble protein copolymer.
(4) chitosan crosslinked alcohol soluble protein copolymer is prepared
After the completion of (3) step, chitosan crosslinked alcohol soluble protein reaction solution prepared by (3) step is pumped into vacuum filter
It is filtered, collects filtrate and filter residue respectively.To the filtrate of collection, for recycling ethylene glycol；To the filter residue of collection, with volume hundred
Divide a concentration of 95% ethyl alcohol washing, the ratio between the ethyl alcohol volume that wherein filter residue quality is 95% with concentration expressed in percentage by volume is 1: 8
(kg/L).It is pumped into vacuum filter and is filtered again after the completion of washing, collect filtrate and filter residue respectively.Filter to collection
Liquid, contains unreacted alcohol soluble protein, and can be used for lower batch after recycling ethyl alcohol prepares alcohol soluble protein solution；To the filter residue of collection, send
Enter in vacuum drying chamber, carries out vacuum drying 30h under conditions of temperature is 60 DEG C, vacuum degree is 50Pa, that is, prepare yellowish-brown
The chitosan crosslinked alcohol soluble protein copolymer of color, total recovery rate reach 64.8%.
Claims (1)
1. a kind of preparation method of chitosan crosslinked alcohol soluble protein, it is characterised in that specific processing step is as follows：
(1) alcohol soluble protein solution is prepared
Dried rice slag or wheat protein powder or corn protein powder are scattered in the ethanol solution that volumetric concentration is 70~85%,
30~40min of stir process under the rotating speed of 100~120r/min, the wherein matter of dried rice slag or wheat protein powder or corn protein powder
It is 1: 8~10kg/L that amount, which is the ratio between 70~85% volume of ethanol solution with volumetric concentration, is filtered after the completion of processing, point
Not Shou Ji filtrate and filter residue feed addictive is used to prepare to the filter residue of collection；It is 50~60 in temperature to the filtrate of collection
DEG C, vacuum degree be 0.09~0.1MPa under conditions of be concentrated in vacuo, until concentrate without ethanol flavor when stop, second is then added
Glycol is handled, and processing time is 20~30min, and the wherein volume ratio of concentrate and ethylene glycol is 1: 2~4L/L, has been handled
Cheng Hou prepares alcohol soluble protein solution, be used to prepare chitosan crosslinked alcohol soluble protein reaction solution；
(2) chitosan solution is prepared
The ratio that the ratio between the HCL aqueous solution volumes for being 0.5~1.5% according to chitosan mass and mass fraction are 1: 20~40kg/L
Example, by molecular weight be 30~50KDa chitosan be dissolved under stiring in the HCL aqueous solutions, according still further to chitosan mass with
The ratio between ethylene glycol volume is the ratio of 1: 5~15kg/L, and ethylene glycol is added and prepares chitosan solution after mixing, uses
Chitosan crosslinked alcohol soluble protein reaction solution is prepared in lower step；
(3) chitosan crosslinked alcohol soluble protein reaction solution is prepared
It is first 1: 1~3L/L's according to the ratio between volume of chitosan solution and alcohol soluble protein solution after the completion of (1) and (2) step
Ratio, two kinds of solution that (1) and (2) step is prepared are uniformly mixed, according still further to the ratio between glutaraldehyde and chitosan solution volume
For the ratio of 1: 100~200L/L, glutaraldehyde solution is added, wherein the mass percentage concentration of glutaraldehyde is in glutaraldehyde solution
25%~50%, 40~50 DEG C are then warming up to, 1~2h is reacted, just prepares chitosan crosslinked alcohol soluble protein reaction solution, be used for
Lower step prepares chitosan crosslinked alcohol soluble protein copolymer；
(4) chitosan crosslinked alcohol soluble protein copolymer is prepared
After the completion of (3) step, chitosan crosslinked alcohol soluble protein reaction solution prepared by (3) step is pumped into vacuum filter and is carried out
It filters, filtrate and filter residue is collected respectively, to the filtrate of collection, for recycling ethylene glycol；It is dense with volume basis to the filter residue of collection
Degree washs for 80~95% ethyl alcohol, and the ratio between the ethyl alcohol volume that wherein filter residue quality is 80~95% with concentration expressed in percentage by volume is 1:
6~8kg/L is pumped into vacuum filter after the completion of washing and is filtered again, collects filtrate and filter residue, the filter to collection respectively
Liquid, contains unreacted alcohol soluble protein, and can be used for lower batch after recycling ethyl alcohol prepares alcohol soluble protein solution；To the filter residue of collection, send
Enter in vacuum drying chamber, 24~30h of vacuum drying carried out under conditions of temperature is 50~60 DEG C, vacuum degree is 40~50Pa,
Filemot chitosan crosslinked alcohol soluble protein copolymer is prepared, total recovery rate reaches 56.3%~64.8%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610911293.8A CN106633120B (en) | 2016-10-19 | 2016-10-19 | A kind of preparation method of chitosan crosslinked alcohol soluble protein |
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