CN109627356A - A kind of preparation method based on shrimp shell production chitosan - Google Patents
A kind of preparation method based on shrimp shell production chitosan Download PDFInfo
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- CN109627356A CN109627356A CN201811516931.1A CN201811516931A CN109627356A CN 109627356 A CN109627356 A CN 109627356A CN 201811516931 A CN201811516931 A CN 201811516931A CN 109627356 A CN109627356 A CN 109627356A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0006—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
- C08B37/0024—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid beta-D-Glucans; (beta-1,3)-D-Glucans, e.g. paramylon, coriolan, sclerotan, pachyman, callose, scleroglucan, schizophyllan, laminaran, lentinan or curdlan; (beta-1,6)-D-Glucans, e.g. pustulan; (beta-1,4)-D-Glucans; (beta-1,3)(beta-1,4)-D-Glucans, e.g. lichenan; Derivatives thereof
- C08B37/0027—2-Acetamido-2-deoxy-beta-glucans; Derivatives thereof
- 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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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0003—General processes for their isolation or fractionation, e.g. purification or extraction from biomass
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Abstract
The invention discloses a kind of preparation methods based on shrimp shell production chitosan, the following steps are included: collecting shrimp shell, dried after being cleaned up shrimp shell with tap water, crushing obtains shrimp shell meal, shrimp shell meal is taken to be placed in purified water, acid solution is added dropwise in whipping process, until bubble-free generates, filtering, collect solid powder, it is washed to neutrality, is obtained except the shrimp shell meal after minerals, what is obtained heats except the shrimp shell meal after minerals is placed in lye.Acid solution is added dropwise during stirring shrimp shell meal/purifying water mixed liquid, make acid solution enter after mixed liquor quickly with mineral qualitative response, it can not only accurately determine the reaction time, and mixture system is avoided to be constantly in stronger acidity, the problem of making chitin degrade under acid catalysis, ensure the relative molecular weight distribution of chitin product in relatively narrow range, so that it is guaranteed that the relative molecular weight distribution of chitosan product in relatively narrow range, improves the application value of chitosan product.
Description
Technical field
The present invention relates to chitosan preparation technical field, specially a kind of preparation method based on shrimp shell production chitosan.
Background technique
Chitosan is also known as chitosan, is by the chitin in the shell-fish arthropod shell such as shrimp, crab by de-
The organic compound that acetyl effect obtains is unique alkaline polysaccharide in natural polysaccharide, has blood compatibility, safety, micro-
The excellent performances such as biological degradability are widely used in weaving, medicine, papermaking, cosmetics, food industry and biotechnology field.
Currently, existing prepare in the technique of chitosan by raw material of shrimp shell, handled using diluted acid and diluted alkaline prawn shell,
Shrimp shell after processing is used directly as the chitin of production chitosan, however still can be residual in the shrimp shell after soda acid processing
There are part inorganic salts, these inorganic salts can not be removed in concentrated base pyrolytic process, inorganic salt blended in chitosan, be made
The ash content of chitosan product is higher, reduces the content of chitosan in product, and chitin obtains shell by concentrated base pyrolysismethod
Glycan, chitin and chitosan is easy to degrade in concentrated base, so that chitosan unstable product quality, range of molecular weight distributions
Wide, application value is low.
Summary of the invention
In view of the deficiencies of the prior art, it the present invention provides a kind of preparation method based on shrimp shell production chitosan, solves
It is existing to be prepared in the technique of chitosan by raw material of shrimp shell, it is handled using diluted acid and diluted alkaline prawn shell, after handling
Shrimp shell directly as production chitosan chitin use, however soda acid processing after shrimp shell in still can remain part without
Machine salt, these inorganic salts can not be removed in concentrated base pyrolytic process, inorganic salt blended in chitosan, make chitosan product
Ash content it is higher, reduce the content of chitosan in product, and chitin obtains chitosan, chitin by concentrated base pyrolysismethod
It can degrade in concentrated base with chitosan, so that chitosan unstable product quality, range of molecular weight distributions is wide, application value
The problem of bottom.
To achieve the above object, the invention provides the following technical scheme: a kind of preparation side based on shrimp shell production chitosan
Method, comprising the following steps:
(1) shrimp shell pre-processes: collecting shrimp shell, dries after being cleaned up shrimp shell with tap water, crushing obtains shrimp shell meal.
(2) minerals are removed: taking shrimp shell meal to be placed in purified water, acid solution is added dropwise in whipping process, until bubble-free generates,
Filtering collects solid powder, is washed to neutrality, obtains except the shrimp shell meal after minerals.
(3) it removing protein and lipid: is heated what step (1) obtained except the shrimp shell meal after minerals is placed in lye, then
Filtering collects shrimp shell meal, is beaten with purified water, is washed till neutrality, the shrimp shell meal after obtaining isolating protein and lipid；
(4) it decolourizes: the shrimp shell meal after isolating protein and lipid that step (2) obtains being placed in hydrogen peroxide and is beaten, filter,
Shrimp shell meal is collected, purified water mashing is primary, obtains chitin crude product；
(5) it purifies: the chitin crude product that step (4) obtains is placed in LiCl/DMAC mixed solution simultaneously stirring and dissolving, mistake
Filtrate is collected in filter, is beaten and is cleaned with purified water after filter vacuum concentration is done, obtains chitin powder.
(6) deacetylated: the chitin powder that step (5) obtains being added in the mixed solution of methanol/sodium hydroxide and is heated
Reflux, cooled and filtered obtain solid powder, and solid powder mashing is washed to neutrality, the solid was filtered powder, drying
After obtain thick chitosan；
(7) purify: the thick chitosan that step (6) obtains being dissolved in diluted acid and obtains mixed solution, titrated with diluted alkaline described in
Filter cake is added in purified water after being beaten and filters by mixed solution to pH=7~8.5, filtering, and filtration cakes torrefaction obtains white powder,
That is chitosan.
Further, the shrimp shell meal crushed in the step (1) is the sieving of 80 mesh.
Further, in the step (2), the volume of the purified water is three times of shrimp shell meal quality, and the acid solution is
The hydrochloric acid of 5mol/L.
Further, in the step (3), the lye is the sodium hydroxide solution of 1mol/L, and volume used is shrimp
Five times of shell silty amount, the heating operation are that 1h is boiled in heating.
Further, in the step (4), the volume of the hydrogen peroxide is three times of shrimp shell meal quality.
Further, in the step (5), the volume of the LiCl/DMAC mixed solution is three times of shrimp shell meal quality,
The volume of DMAC is the thirtyfold of LiCl mass in the LiCl/DMAC mixed solution.
Further, in the step (6), the volume of methanol/sodium hydroxide mixed solution is five times of shrimp shell meal quality,
In the methanol/sodium hydroxide mixed liquor, the volume of methanol is 100 times of sodium hydroxide quality, and described being heated to reflux is 75
DEG C reflux one hour.
Further, after the step (6), the method that thick chitosan uses (6) is carried out again deacetylated.
Further, in the step (7), the diluted acid is the aqueous acetic acid of 0.01g/mL, and the diluted alkaline is
The sodium bicarbonate aqueous solution of 0.01g/ml.
It has the beneficial effect that:
(1) acid solution is added dropwise during stirring shrimp shell meal/purifying water mixed liquid, make acid solution enter after mixed liquor quickly with
Mineral qualitative response can not only accurately determine the reaction time, and mixture system is avoided to be constantly in stronger acidity, make first
The problem of shell element is degraded under acid catalysis, it is ensured that the relative molecular weight distribution of chitin product in relatively narrow range, from
And the relative molecular weight distribution for ensuring chitosan product improves the application value of chitosan product in relatively narrow range.
(2) chitin crude product is dissolved using LiCl/DMAC mixed solution, chitin crude product is refined, remove first
Residual ash in shell element, avoids ash content from being mixed into chitosan product during chitin synthesizes chitosan, and it is poly- to improve shell
The content of chitosan in sugar product.
(3) replace concentrated base using methanol/sodium hydroxide mixed solution, it is deacetylated in chitin to reduce chitin and chitosan
Base produces the degree of degradation during chitosan, it is ensured that the relative molecular weight distribution of chitosan product improves in relatively narrow range
The application value of chitosan product.
Detailed description of the invention
Fig. 1 is process flow chart of the invention.
Specific embodiment
Based on the embodiments of the present invention, those of ordinary skill in the art are obtained without making creative work
The every other embodiment obtained, shall fall within the protection scope of the present invention.
The present invention provides a kind of technical solution: a kind of preparation method based on shrimp shell production chitosan, comprising the following steps:
(1) shrimp shell pre-processes: collecting shrimp shell, dries after being cleaned up shrimp shell with tap water, crushing obtains shrimp shell meal.
(2) minerals are removed: taking shrimp shell meal to be placed in purified water, acid solution is added dropwise in whipping process, until bubble-free generates,
Filtering collects solid powder, is washed to neutrality, obtains except the shrimp shell meal after minerals.
(3) it removing protein and lipid: is heated what step (1) obtained except the shrimp shell meal after minerals is placed in lye, then
Filtering collects shrimp shell meal, is beaten with purified water, is washed till neutrality, the shrimp shell meal after obtaining isolating protein and lipid；
(4) it decolourizes: the shrimp shell meal after isolating protein and lipid that step (2) obtains being placed in hydrogen peroxide and is beaten, filter,
Shrimp shell meal is collected, purified water mashing is primary, obtains chitin crude product；
(5) it purifies: the chitin crude product that step (4) obtains is placed in LiCl/DMAC mixed solution simultaneously stirring and dissolving, mistake
Filtrate is collected in filter, is beaten and is cleaned with purified water after filter vacuum concentration is done, obtains chitin powder.
(6) deacetylated: the chitin powder that step (5) obtains being added in the mixed solution of methanol/sodium hydroxide and is heated
Reflux, cooled and filtered obtain solid powder, and solid powder mashing is washed to neutrality, the solid was filtered powder, drying
After obtain thick chitosan；
(7) purify: the thick chitosan that step (6) obtains being dissolved in diluted acid and obtains mixed solution, titrated with diluted alkaline described in
Filter cake is added in purified water after being beaten and filters by mixed solution to pH=7~8.5, filtering, and filtration cakes torrefaction obtains white powder,
That is chitosan.
Further, the shrimp shell meal crushed in the step (1) is the sieving of 80 mesh, increases the specific surface area of shrimp shell, is increased
The area for having added shrimp shell to contact with diluted acid shortens the reaction time to increase the speed that shrimp shell is reacted with diluted acid, reduces chitin
Palliating degradation degree.
Further, in the step (2), the volume of the purified water is three times of shrimp shell meal quality, and the acid solution is
The hydrochloric acid of 5mol/L in the mixed liquor that acid droplet is added to purified water and shrimp shell meal, is kept away while reacting acid solution with shrimp shell meal
Exempt from the problem of mixture system is constantly in stronger acidity, chitin is made to degrade under acid catalysis, it is ensured that chitin produces
The relative molecular weight distribution of product is in relatively narrow range.
Further, in the step (3), the lye is the sodium hydroxide solution of 1mol/L, and volume used is shrimp
Five times of shell silty amount, the heating operation are that 1h is boiled in heating, will not shadow with 1mol/L sodium hydroxide solution processing shrimp shell meal
Ring the viscosity of chitosan product, it is ensured that relative molecular weight of chitosan is unaffected.
Further, in the step (4), the volume of the hydrogen peroxide is three times of shrimp shell meal quality, utilizes hydrogen peroxide
The pigment in shrimp shell meal is removed, the color of chitosan product is improved, improves the quality of chitosan product.
Further, in the step (5), the volume of the LiCl/DMAC mixed solution is three times of shrimp shell meal quality,
The volume of DMAC is the thirtyfold of LiCl mass in the LiCl/DMAC mixed solution, forms network using chitin and lithium ion
The characteristic purification chitin that object is dissolved in DMAC is closed, the purity of chitin is improved, reduces the content of ash content in chitin, from
And improve the quality of chitosan product.
Further, in the step (6), the volume of methanol/sodium hydroxide mixed solution is five times of shrimp shell meal quality,
In the methanol/sodium hydroxide mixed liquor, the volume of methanol is 100 times of sodium hydroxide quality, and described being heated to reflux is 75
DEG C reflux one hour, accelerates methanol to react with chitin using the sodium hydroxide of catalytic amount, keep chitin completion deacetylated.
Further, after the step (6), thick chitosan is carried out using the method for (6) deacetylated again, it is poly- increases shell
The deacetylation of sugar, improves the purity of chitosan.
Further, in the step (7), the diluted acid is the aqueous acetic acid of 0.01g/mL, and the diluted alkaline is
The sodium bicarbonate aqueous solution of 0.01g/ml, further refines chitosan, increases the quality of chitosan.
Embodiment one: collecting shrimp shell, 60 DEG C of baking oven drying is put into after cleaning up shrimp shell using tap water, by drying
Shrimp shell crushed 80 mesh mesh screens and obtain shrimp shell meal, weighs 100g shrimp shell meal and is put into beaker, and 300ml purified water is added into beaker and stirs
It mixes uniformly, the hydrochloric acid of 5mol/L is added dropwise, until there is no bubble generations in mixed liquor, the shrimp shell meal after filtering out except minerals,
Shrimp shell meal with purified water mashing cleaning to neutrality, after filtering out except minerals.Single port will be added except the shrimp shell meal after minerals
In round-bottomed flask, and the sodium hydroxide solution of 500ml 1mol/L is added, single necked round bottom flask is heated using heating mantle, makes alkali
Liquid flows back one hour, cooling, the shrimp shell meal after filtering out isolating protein and lipid, with water mashing cleaning to neutrality.By isolating protein
And the shrimp shell meal after lipid and 300ml hydrogen peroxide are added in beaker and are beaten one hour for 35 DEG C of water-bath, filter out chitin crude product, are used in combination
Purified water mashing is primary.10g LiCl is dissolved in 300ml DMAC and is configured to LiCl/DMAC mixed solution, measures 300ml
LiCl/DMAC mixed solution is placed in a beaker, and chitin crude product is added in beaker and in 50 DEG C of stirred in water bath half an hour, mistake
Filtrate is collected in filter, and filtrate is concentrated and is done, and twice with water mashing cleaning, chitin powder is collected in filtering.Chitin powder is added
Enter to be heated to reflux in the mixed solution of 500ml methanol/sodium hydroxide one hour, cooled and filtered obtains solid powder.To round bottom
5g sodium hydroxide and 500ml methanol are added in flask, and round-bottomed flask is added in solid powder, is heated to reflux one hour, it is cooling
After thick chitosan is obtained by filtration, thick chitosan is dissolved in diluted acid and obtains mixed solution, titrates the mixed solution extremely with diluted alkaline
Filter cake is added in purified water and is beaten by pH=7.5, filtering, filters, and filter cake is put into vacuum oven and is less than in vacuum degree
0.1MPa is dried in vacuo three hours under temperature 60 C, obtains white Chitosan powder 7.9g, detected, and chitosan sample is made
Moisture content be 3.8%, content of ashes 0.27%, deacetylation 95.7%, range of molecular weight distributions are 90-110 ten thousand
Dalton.
Embodiment two: collecting shrimp shell, 60 DEG C of baking oven drying is put into after cleaning up shrimp shell using tap water, by drying
Shrimp shell crushed 80 mesh mesh screens and obtain shrimp shell meal, weighs 100g shrimp shell meal and is put into beaker, and 300ml purified water is added into beaker and stirs
It mixes uniformly, the hydrochloric acid of 5mol/L is added dropwise, until there is no bubble generations in mixed liquor, the shrimp shell meal after filtering out except minerals,
Shrimp shell meal with purified water mashing cleaning to neutrality, after filtering out except minerals.Single port will be added except the shrimp shell meal after minerals
In round-bottomed flask, and the sodium hydroxide solution of 500ml 1mol/L is added, single necked round bottom flask is heated using heating mantle, makes alkali
Liquid flows back one hour, cooling, the shrimp shell meal after filtering out isolating protein and lipid, with water mashing cleaning to neutrality.By isolating protein
And the shrimp shell meal after lipid and 300ml hydrogen peroxide are added in beaker and are beaten one hour for 35 DEG C of water-bath, filter out chitin crude product, are used in combination
Purified water mashing is primary.10g LiCl is dissolved in 300ml DMAC and is configured to LiCl/DMAC mixed solution, measures 300ml
LiCl/DMAC mixed solution is placed in a beaker, and chitin crude product is added in beaker and in 50 DEG C of stirred in water bath half an hour, mistake
Filtrate is collected in filter, and filtrate is concentrated and is done, and twice with water mashing cleaning, chitin powder is collected in filtering.Chitin powder is added
Enter to be heated to reflux in the mixed solution of 500ml methanol/sodium hydroxide one hour, cooled and filtered obtains solid powder.To round bottom
20g sodium hydroxide and 500ml methanol are added in flask, and round-bottomed flask is added in solid powder, is heated to reflux one hour, it is cooling
After thick chitosan is obtained by filtration, thick chitosan is dissolved in diluted acid and obtains mixed solution, titrates the mixed solution extremely with diluted alkaline
Filter cake is added in purified water and is beaten by pH=7.5, filtering, filters, and filter cake is put into vacuum oven and is less than in vacuum degree
0.1MPa is dried in vacuo three hours under temperature 60 C, obtains white Chitosan powder 7.2g, detected, and chitosan sample is made
Moisture content be 4.1%, content of ashes 0.23%, deacetylation 96.7%, range of molecular weight distributions are 80-110 ten thousand
Dalton.
Embodiment three: collecting shrimp shell, 60 DEG C of baking oven drying is put into after cleaning up shrimp shell using tap water, by drying
Shrimp shell crushed 80 mesh mesh screens and obtain shrimp shell meal, weighs 100g shrimp shell meal and is put into beaker, and 300ml purified water is added into beaker and stirs
It mixes uniformly, the hydrochloric acid of 5mol/L is added dropwise, until there is no bubble generations in mixed liquor, the shrimp shell meal after filtering out except minerals,
Shrimp shell meal with purified water mashing cleaning to neutrality, after filtering out except minerals.Single port will be added except the shrimp shell meal after minerals
In round-bottomed flask, and the sodium hydroxide solution of 500ml 1mol/L is added, single necked round bottom flask is heated using heating mantle, makes alkali
Liquid flows back one hour, cooling, the shrimp shell meal after filtering out isolating protein and lipid, with water mashing cleaning to neutrality.By isolating protein
And the shrimp shell meal after lipid and 300ml hydrogen peroxide are added in beaker and are beaten one hour for 35 DEG C of water-bath, filter out chitin crude product, are used in combination
Purified water mashing is primary.10g LiCl is dissolved in 300ml DMAC and is configured to LiCl/DMAC mixed solution, measures 300ml
LiCl/DMAC mixed solution is placed in a beaker, and chitin crude product is added in beaker and in 50 DEG C of stirred in water bath half an hour, mistake
Filtrate is collected in filter, and filtrate is concentrated and is done, and twice with water mashing cleaning, chitin powder is collected in filtering.Chitin powder is added
Enter to be heated to reflux in the mixed solution of 500ml methanol/sodium hydroxide one hour, cooled and filtered obtains solid powder.To round bottom
40g sodium hydroxide and 500ml methanol are added in flask, and round-bottomed flask is added in solid powder, is heated to reflux one hour, it is cooling
After thick chitosan is obtained by filtration, thick chitosan is dissolved in diluted acid and obtains mixed solution, titrates the mixed solution extremely with diluted alkaline
Filter cake is added in purified water and is beaten by pH=7.5, filtering, filters, and filter cake is put into vacuum oven and is less than in vacuum degree
0.1MPa is dried in vacuo three hours under temperature 60 C, obtains white Chitosan powder 7.4g, detected, and chitosan sample is made
Moisture content be 3.3%, content of ashes 0.26%, deacetylation 96.3%, range of molecular weight distributions are 80-100 ten thousand
Dalton.
It should be noted that, in this document, relational terms such as first and second and the like are used merely to a reality
Body or operation are distinguished with another entity or operation, are deposited without necessarily requiring or implying between these entities or operation
In any actual relationship or order or sequence.Moreover, the terms "include", "comprise" or its any other variant are intended to
Non-exclusive inclusion, so that the process, method, article or equipment including a series of elements is not only wanted including those
Element, but also including other elements that are not explicitly listed, or further include for this process, method, article or equipment
Intrinsic element.
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
A variety of variations, modification, replacement can be carried out to these embodiments without departing from the principles and spirit of the present invention by understanding
And modification, the scope of the present invention is defined by the appended.
Claims (9)
1. a kind of preparation method based on shrimp shell production chitosan, which comprises the following steps:
(1) shrimp shell pre-processes: collecting shrimp shell, dries after being cleaned up shrimp shell with tap water, crushing obtains shrimp shell meal.
(2) minerals are removed: taking shrimp shell meal to be placed in purified water, acid solution is added dropwise in whipping process, until bubble-free generates, mistake
Filter collects solid powder, is washed to neutrality, obtains except the shrimp shell meal after minerals.
(3) removing protein and lipid: heating except the shrimp shell meal after minerals is placed in lye by what step (1) obtained, then filter,
Shrimp shell meal is collected, is beaten with purified water, is washed till neutrality, the shrimp shell meal after obtaining isolating protein and lipid；
(4) it decolourizes: the shrimp shell meal after isolating protein and lipid that step (2) obtains being placed in hydrogen peroxide and is beaten, filter, collect
Shrimp shell meal, purified water mashing is primary, obtains chitin crude product；
(5) it purifies: the chitin crude product that step (4) obtains being placed in LiCl/DMAC mixed solution simultaneously stirring and dissolving, is filtered,
Filtrate is collected, is beaten and is cleaned with purified water after filter vacuum concentration is done, obtain chitin powder.
(6) deacetylated: the chitin powder that step (5) obtains is added in the mixed solution of methanol/sodium hydroxide and is heated to reflux,
Cooled and filtered obtains solid powder, solid powder mashing is washed to neutrality, the solid was filtered powder obtains after dry
Thick chitosan；
(7) it purifies: the thick chitosan that step (6) obtains being dissolved in diluted acid and obtains mixed solution, titrate the mixing with diluted alkaline
Filter cake is added in purified water after being beaten and filters by solution to pH=7~8.5, filtering, and filtration cakes torrefaction obtains white powder, i.e. shell
Glycan.
2. a kind of preparation method based on shrimp shell production chitosan as described in claim 1, it is characterised in that: the step
(1) shrimp shell meal crushed in is the sieving of 80 mesh.
3. a kind of preparation method based on shrimp shell production chitosan as described in claim 1, it is characterised in that: the step
(2) in, the volume of the purified water is three times of shrimp shell meal quality, and the acid solution is the hydrochloric acid of 5mol/L.
4. a kind of preparation method based on shrimp shell production chitosan as described in claim 1, it is characterised in that: the step
(3) in, the lye is the sodium hydroxide solution of 1mol/L, and volume used is five times of shrimp shell meal quality, the heating behaviour
1h is boiled as heating.
5. a kind of preparation method based on shrimp shell production chitosan as described in claim 1, it is characterised in that: the step
(4) in, the volume of the hydrogen peroxide is three times of shrimp shell meal quality.
6. a kind of preparation method based on shrimp shell production chitosan as described in claim 1, it is characterised in that: the step
(5) in, the volume of the LiCl/DMAC mixed solution is three times of shrimp shell meal quality, in the LiCl/DMAC mixed solution
The volume of DMAC is the thirtyfold of LiCl mass.
7. a kind of preparation method based on shrimp shell production chitosan as described in claim 1, it is characterised in that: the step
(6) in, the volume of methanol/sodium hydroxide mixed solution is five times of shrimp shell meal quality, the methanol/sodium hydroxide mixed liquor
In, the volume of methanol is 100 times of sodium hydroxide quality, and described being heated to reflux flows back one hour for 75 DEG C.
8. a kind of preparation method based on shrimp shell production chitosan as described in claim 1, it is characterised in that: the step
(6) after, the method that thick chitosan uses (6) is carried out again deacetylated.
9. a kind of preparation method based on shrimp shell production chitosan as described in claim 1, it is characterised in that: the step
(7) in, the diluted acid is the aqueous acetic acid of 0.01g/mL, and the diluted alkaline is the sodium bicarbonate aqueous solution of 0.01g/ml.
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Cited By (5)
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|---|---|---|---|---|
| CN110746659A (en) * | 2019-11-14 | 2020-02-04 | 广东医科大学 | Natural preservative film and preparation method thereof |
| CN111393541A (en) * | 2020-04-13 | 2020-07-10 | 扬州日兴生物科技股份有限公司 | Enzymatic refining process of chitosan |
| CN111574288A (en) * | 2020-05-30 | 2020-08-25 | 江苏福砳生物环保科技有限公司 | Foliar fertilizer and preparation method thereof |
| CN112341551A (en) * | 2020-11-05 | 2021-02-09 | 广东广纳安疗科技有限公司 | Chitosan substance with ultralow endotoxin and preparation method thereof |
| CN113527535A (en) * | 2020-04-21 | 2021-10-22 | 钱能胜 | Method for preparing chitosan from shrimp heads, shrimp shells and crab shells |
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| WO2021244003A1 (en) * | 2020-05-30 | 2021-12-09 | 江苏福砳生物环保科技有限公司 | Foliar fertilizer and preparation method therefor |
| CN112341551A (en) * | 2020-11-05 | 2021-02-09 | 广东广纳安疗科技有限公司 | Chitosan substance with ultralow endotoxin and preparation method thereof |
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