CN110746520A - Novel efficient preparation method for chitosan production - Google Patents
Novel efficient preparation method for chitosan production Download PDFInfo
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- CN110746520A CN110746520A CN201911221984.5A CN201911221984A CN110746520A CN 110746520 A CN110746520 A CN 110746520A CN 201911221984 A CN201911221984 A CN 201911221984A CN 110746520 A CN110746520 A CN 110746520A
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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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- 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
- C08B37/0003—General processes for their isolation or fractionation, e.g. purification or extraction from biomass
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Abstract
The invention relates to the technical field of chitosan preparation, and discloses novel chitosan, which comprises the following raw materials, by weight, 2-5 parts of shrimp shell powder, 150 parts of 7% HCL solution 120-containing organic solvent, 150 parts of 10% NAOH solution 120-containing organic solvent, 12-15 parts of 95% ethanol solution, 12-15 parts of absolute ethyl alcohol and 60-100 parts of 50% NAOH solution.
Description
Technical Field
The invention relates to the technical field of chitosan preparation, in particular to a novel efficient preparation method for chitosan production.
Background
The chitosan is a chitin N-deacetylation product, is stable in chemical property, is soluble in dilute acid and is almost insoluble in water and organic solvents under the action of internal and external hydrogen bonds, so that the application and development of the chitosan are limited to a great extent, and the water-soluble chitosan is low-molecular-weight chitosan capable of being directly soluble in water, has the functions of being easily absorbed by a human body, resisting tumors, regulating blood fat, improving the immunity of the human body and the like, and has high safety and potential antibacterial property.
At present, the preparation process method of the domestic high-quality chitosan is far behind that of developed countries in the western world, reports on the aspects of the preparation and the antibacterial property of the water-soluble chitosan are also rare, consistent results are not obtained, and in the food and medicine industry, the food spoilage, the drug resistance of pathogenic microorganisms and the side effect of traditional antibiotic drugs caused by microbial pollution lead people to urgently hope to find a food preservative and an antibacterial drug which are efficient, non-toxic, wide in action spectrum, economical and practical to solve the problems, for example, Chinese patent CN 101284884B discloses a preparation method of temperature-sensitive chitosan derivative-hydroxybutyl chitosan, the method takes 1 and 2-butylene oxide as etherifying agents and alkalizing chitosan, chemical modification is carried out under certain conditions controlled under an isopropanol system, and the obtained water-soluble hydroxybutyl chitosan has good water solubility, meanwhile, the chitosan prepared by the method has general viscosity and higher production cost, and the problem is solved by providing a novel efficient preparation method for producing chitosan.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides a novel efficient preparation method for chitosan production, which has the advantages of high viscosity and low production cost, and solves the problems of common viscosity and high production cost of the prepared chitosan.
(II) technical scheme
In order to achieve the aim of good antibacterial effect, the invention provides the following technical scheme: the novel chitosan comprises the following raw materials in parts by weight: 2-5 parts of shrimp shell powder, 150 parts of 7% HCL solution 120-ion, 150 parts of 10% NAOH solution 120-ion, 12-15 parts of 95% ethanol solution, 12-15 parts of absolute ethanol and 60-100 parts of 50% NAOH solution.
Preferably, the feed comprises the following raw materials in parts by weight: 2 parts of shrimp shell powder, 120 parts of 7% HCL solution, 120 parts of 10% NAOH solution, 12 parts of 95% ethanol solution, 12 parts of absolute ethanol and 60 parts of 50% NAOH solution.
Preferably, the feed comprises the following raw materials in parts by weight: 5 parts of shrimp shell powder, 150 parts of 7% HCL solution, 150 parts of 10% NAOH solution, 15 parts of 95% ethanol solution, 15 parts of absolute ethanol and 100 parts of 50% NAOH solution.
Preferably, the feed comprises the following raw materials in parts by weight: 3.5 parts of shrimp shell powder, 135 parts of 7% HCL solution, 135 parts of 10% NAOH solution, 13.5 parts of 95% ethanol solution, 13.5 parts of absolute ethanol and 80 parts of 50% NAOH solution.
The invention aims to solve another technical problem of providing a novel efficient preparation method for producing chitosan, which comprises the following steps:
1)1) taking 2-5 parts of shrimp shell powder and 150 parts of 7% HCL solution 120-5 parts, adding 2-5 parts of shrimp shell powder into 60-75 parts of 7% HCL solution, soaking and stirring at room temperature for 20-24h, then filtering, and removing filtrate to obtain solid A;
2) washing the fixed product A prepared in the step 1) with distilled water for several times until the product is neutral, then soaking the solid product A in 60-75 parts of 10% NAOH solution at the constant temperature of 40-60 ℃ for 20-24h, then filtering, and removing the filtrate to obtain a fixed product B;
3) washing the fixed product B prepared in the step 2) with distilled water for several times until the fixed product B is neutral, then performing decalcification and deproteinization treatment on the fixed product B by using 60-75 parts of 7% HCl solution and 60-75 parts of 10% NAOH solution respectively, then filtering, and removing filtrate to obtain crude chitin;
4) soaking the crude chitin prepared in the step 3) in 12-15 parts of 95% ethanol solution for 20-24h, filtering the solution the next day, soaking the filtered solid in 12-15 parts of absolute ethanol for 20-24h, filtering the solution, washing the filtered solid with warm distilled water for several times until the solid is neutral, and finally drying the solid by electrothermal blowing at 80-110 ℃ to prepare fine chitin;
5) soaking the fine chitin prepared in the step 4) in 60-100 parts of 50% NAOH solution at 60-65 ℃ for 6-8h, cooling at room temperature, standing overnight, filtering the fine chitin the next day, washing the filtered fixed chitin with hot water to be neutral, and drying the chitin by electric heating air blast at 80-110 ℃ to obtain the chitosan.
(III) advantageous effects
Compared with the prior art, the invention provides a novel efficient preparation method for chitosan production, which has the following beneficial effects:
the novel efficient preparation method for producing the chitosan is characterized in that the method is provided with the shrimp shell powder, a common once short-time high-temperature boiling method is changed into a long-time medium-temperature intermittent soaking method according to the physicochemical properties of the lobster shells to prepare the chitosan with high deacetylation degree, the quality index of the food-grade chitosan is reached, in the experimental process, the chitosan is treated at low-concentration strong acid and strong alkali at medium temperature for a long time, the breakage of β -1, 4-glycosidic bonds of the chitosan can be reduced, the high-viscosity chitosan is prepared, the decolorized ethanol is recovered by a distillation method, the concentrated alkali liquor used for deacetylation is utilized, and the concentrated alkali liquor is diluted after recovery for secondary deproteinization and is recycled, so that the production cost is effectively reduced.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The first embodiment is as follows: the novel chitosan comprises the following raw materials in parts by weight: 2 parts of shrimp shell powder, 120 parts of 7% HCL solution, 120 parts of 10% NAOH solution, 12 parts of 95% ethanol solution, 12 parts of absolute ethanol and 60 parts of 50% NAOH solution.
The invention aims to solve another technical problem of providing a novel efficient preparation method for producing chitosan, which comprises the following steps:
1) taking 2 parts of shrimp shell powder and 120 parts of 7% HCl solution, adding 2 parts of shrimp shell powder into 60 parts of 7% HCl solution, soaking and stirring at room temperature for 20 hours, then filtering, and removing filtrate to obtain solid A;
2) washing the fixed product A prepared in the step 1) with distilled water for several times until the product is neutral, then soaking the solid product A with 60 parts of 10% NAOH solution at the constant temperature of 40 ℃ for 20 hours, then filtering, and removing the filtrate to obtain a fixed product B;
3) washing the fixed product B prepared in the step 2) with distilled water for several times until the fixed product B is neutral, then respectively carrying out decalcification and deproteinization treatment on 60 parts of 7% HCl solution and 60 parts of 10% NAOH solution, then filtering, and removing the filtrate to obtain crude chitin;
4) soaking the crude chitin prepared in the step 3) in 12 parts of 95% ethanol solution for 20h, filtering the solution the next day, soaking the filtered solid in 12 parts of absolute ethanol for 20h, filtering the solution, washing the filtered solid with warm distilled water for several times until the solid is neutral, and finally drying the solid by electric heating air blast at 80 ℃ to prepare fine chitin;
5) soaking the fine chitin prepared in the step 4) in 60 parts of 50% NAOH solution at 60 ℃ for 6 hours, cooling at room temperature and standing overnight, filtering the fine chitin the next day, washing the filtered fine chitin with hot water to be neutral, and drying the fine chitin by using electrothermal blowing at 80 ℃ to obtain the chitosan.
Example two: the novel chitosan comprises the following raw materials in parts by weight: 5 parts of shrimp shell powder, 150 parts of 7% HCL solution, 150 parts of 10% NAOH solution, 15 parts of 95% ethanol solution, 15 parts of absolute ethanol and 100 parts of 50% NAOH solution.
The invention aims to solve another technical problem of providing a novel efficient preparation method for producing chitosan, which comprises the following steps:
1) taking 5 parts of shrimp shell powder and 150 parts of 7% HCL solution, adding 5 parts of shrimp shell powder into 75 parts of 7% HCL solution, soaking and stirring at room temperature for 24 hours, then filtering, and removing filtrate to obtain solid A;
2) washing the fixed product A prepared in the step 1) with distilled water for several times until the product is neutral, then soaking the solid product A with 75 parts of 10% NAOH solution at the constant temperature of 60 ℃ for 24 hours, then filtering, and removing the filtrate to obtain a fixed product B;
3) washing the fixed product B prepared in the step 2) with distilled water for several times until the fixed product B is neutral, then respectively carrying out decalcification and deproteinization on 75 parts of 7% HCl solution and 75 parts of 10% NAOH solution, then filtering, and removing the filtrate to obtain crude chitin;
4) soaking the crude chitin prepared in the step 3) in 15 parts of 95% ethanol solution for 24 hours, filtering the solution the next day, soaking the filtered solid in 15 parts of absolute ethanol for 24 hours, filtering the solution, washing the filtered solid with warm distilled water for several times until the solid is neutral, and finally drying the solid by electric heating air blast at 110 ℃ to prepare the fine chitin;
5) soaking the fine chitin prepared in the step 4) in 100 parts of 50% NAOH solution at 65 ℃ for 8h, cooling at room temperature, standing overnight, filtering the solution the next day, washing the filtered fixed part with hot water to neutrality, and drying the washed fixed part with 110 ℃ electric heating forced air to obtain the chitosan.
Example three: the novel chitosan comprises the following raw materials in parts by weight: 3.5 parts of shrimp shell powder, 135 parts of 7% HCL solution, 135 parts of 10% NAOH solution, 13.5 parts of 95% ethanol solution, 13.5 parts of absolute ethanol and 80 parts of 50% NAOH solution.
The invention aims to solve another technical problem of providing a novel efficient preparation method for producing chitosan, which comprises the following steps:
1) taking 3.5 parts of shrimp shell powder and 135 parts of 7% HCL solution, adding 3.5 parts of shrimp shell powder into 67.5 parts of 7% HCL solution, soaking and stirring at room temperature for 22 hours, then filtering, and removing filtrate to obtain solid A;
2) washing the fixed product A prepared in the step 1) with distilled water for several times until the product is neutral, then soaking the solid product A with 67.5 parts of 10% NAOH solution at the constant temperature of 50 ℃ for 22 hours, then filtering, and removing the filtrate to obtain a fixed product B;
3) washing the fixed product B prepared in the step 2) with distilled water for several times until the fixed product B is neutral, then performing decalcification and deproteinization treatment on 67.5 parts of 7% HCl solution and 67.5 parts of 10% NAOH solution respectively, filtering, and removing the filtrate to obtain crude chitin;
4) soaking the crude chitin prepared in the step 3) in 13.5 parts of 95% ethanol solution for 22h, filtering the solution the next day, soaking the filtered solid in 13.5 parts of absolute ethanol for 22h, filtering the solution, washing the filtered solid with warm distilled water for several times until the solid is neutral, and finally drying the solid by electric heating blast at 95 ℃ to prepare fine chitin;
5) soaking the fine chitin prepared in the step 4) in 80 parts of 50% NAOH solution at 62.5 ℃ for 7h, cooling at room temperature, standing overnight, filtering the solution the next day, washing the filtered fixed solution with hot water to neutrality, and drying the washed fixed solution with 95 ℃ electric heating air blast to obtain the chitosan.
The invention has the advantages that the novel efficient preparation method for producing the chitosan has the advantages that the common one-time short-time high-temperature boiling method is changed into the long-time medium-temperature intermittent soaking method according to the physicochemical properties of the lobster shells of the lobsters to prepare the chitosan with high deacetylation degree, the quality index of the food-grade chitosan is reached, in the experimental process, the strong acid and strong base with low concentration are used for long-time treatment at medium temperature, the breakage of β -1, 4-glycosidic bonds of the chitosan can be reduced, the high-viscosity chitosan can be prepared, the decolored ethanol is recovered by a distillation method, the concentrated alkali liquor used for deacetylation is utilized, and the concentrated alkali liquor is diluted for secondary deproteinization after recovery and recycled, the production cost is effectively reduced, and the problems that the prepared chitosan has common viscosity and high production cost are solved.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (5)
1. The novel chitosan is characterized by comprising the following raw materials in parts by weight: 2-5 parts of shrimp shell powder, 150 parts of 7% HCL solution 120-ion, 150 parts of 10% NAOH solution 120-ion, 12-15 parts of 95% ethanol solution, 12-15 parts of absolute ethanol and 60-100 parts of 50% NAOH solution.
2. The novel chitosan according to claim 1, which is characterized by comprising the following raw materials in parts by weight: 2 parts of shrimp shell powder, 120 parts of 7% HCL solution, 120 parts of 10% NAOH solution, 12 parts of 95% ethanol solution, 12 parts of absolute ethanol and 60 parts of 50% NAOH solution.
3. The novel chitosan according to claim 1, which is characterized by comprising the following raw materials in parts by weight: 5 parts of shrimp shell powder, 150 parts of 7% HCL solution, 150 parts of 10% NAOH solution, 15 parts of 95% ethanol solution, 15 parts of absolute ethanol and 100 parts of 50% NAOH solution.
4. The novel chitosan according to claim 1, which is characterized by comprising the following raw materials in parts by weight: 3.5 parts of shrimp shell powder, 135 parts of 7% HCL solution, 135 parts of 10% NAOH solution, 13.5 parts of 95% ethanol solution, 13.5 parts of absolute ethanol and 80 parts of 50% NAOH solution.
5. A novel efficient preparation method for chitosan production is characterized by comprising the following steps:
1) taking 2-5 parts of shrimp shell powder and 150 parts of 7% HCL solution 120-containing liquid, adding 2-5 parts of shrimp shell powder into 60-75 parts of 7% HCL solution, soaking and stirring at room temperature for 20-24h, then filtering, and removing filtrate to obtain solid A;
2) washing the fixed product A prepared in the step 1) with distilled water for several times until the product is neutral, then soaking the solid product A in 60-75 parts of 10% NAOH solution at the constant temperature of 40-60 ℃ for 20-24h, then filtering, and removing the filtrate to obtain a fixed product B;
3) washing the fixed product B prepared in the step 2) with distilled water for several times until the fixed product B is neutral, then performing decalcification and deproteinization treatment on the fixed product B by using 60-75 parts of 7% HCl solution and 60-75 parts of 10% NAOH solution respectively, then filtering, and removing filtrate to obtain crude chitin;
4) soaking the crude chitin prepared in the step 3) in 12-15 parts of 95% ethanol solution for 20-24h, filtering the solution the next day, soaking the filtered solid in 12-15 parts of absolute ethanol for 20-24h, filtering the solution, washing the filtered solid with warm distilled water for several times until the solid is neutral, and finally drying the solid by electrothermal blowing at 80-110 ℃ to prepare fine chitin;
5) soaking the fine chitin prepared in the step 4) in 60-100 parts of 50% NAOH solution at 60-65 ℃ for 6-8h, cooling at room temperature, standing overnight, filtering the fine chitin the next day, washing the filtered fixed chitin with hot water to be neutral, and drying the chitin by electric heating air blast at 80-110 ℃ to obtain the chitosan.
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CN111888320A (en) * | 2020-08-19 | 2020-11-06 | 福建农林大学 | Essence hair mask of chitin in lobster shells and preparation method thereof |
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