CN103374081A - Method for preparing high-viscosity and high-deacetylation-degree chitosan - Google Patents
Method for preparing high-viscosity and high-deacetylation-degree chitosan Download PDFInfo
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- CN103374081A CN103374081A CN 201210113768 CN201210113768A CN103374081A CN 103374081 A CN103374081 A CN 103374081A CN 201210113768 CN201210113768 CN 201210113768 CN 201210113768 A CN201210113768 A CN 201210113768A CN 103374081 A CN103374081 A CN 103374081A
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Abstract
The invention discloses a method for preparing high-viscosity and high-deacetylation-degree chitosan. The method is characterized by comprising the following steps of: adding sodium hydroxide solution and chitin into a reaction kettle, controlling the temperature at 90-100 DEG C, controlling the temperature at 0.1-2 Mpa, and reacting for 5-7 hours; and removing an alkali liquid, adding purified water to wash for several times until the pH is 7, and drying to obtain the high-viscosity and high-deacetylation-degree chitosan. Compared with the prior art, the method for preparing high-viscosity and high-deacetylation-degree chitosan has the advantages that the cost is low, the steps are few, the industrialization is liable, the deacetylation degree of a prepared product can reach above 95%, and the viscosity of the prepared product can reach 2000 mpa; and the practicality is good, and good economic benefits and social effects can be generated.
Description
Technical field
The present invention relates to chitosan, be specifically related to a kind of method for preparing the high viscosity chitosan with high deacetylation degree.
Background technology
Chitosan (chitosan) is to be obtained through deacetylation by the chitin (chitin) that nature extensively exists, chemical name is Chitosan (1-4)-2-amino-B-D glucose, has widely to use in the numerous areas such as medicine, food, chemical industry, makeup, water treatment, METAL EXTRACTION and recovery, biochemistry and biomedical engineering.In the existing method for preparing chitosan, prepared Viscosity of Chitosan is low, and deacetylation is not high yet, can not satisfy user demand fully.
Summary of the invention
Goal of the invention: for the deficiencies in the prior art, the purpose of this invention is to provide a kind of method for preparing the high viscosity chitosan with high deacetylation degree, cost is low, step is few so that it has, be easy to the advantages such as industrialization, and the product of preparation has the viscosity height, the deacetylation high.
Technical scheme: in order to realize the foregoing invention purpose, the technical solution used in the present invention is as follows:
A kind of method for preparing the high viscosity chitosan with high deacetylation degree: add sodium hydroxide solution and chitin in reactor, 90 ~ 100 ℃ of temperature controls, pressure control react 5 ~ 7h at 0.1 ~ 2Mpa; Venting alkali lye washs to pH7 for several times with purified water, and blowing is drying to obtain the high viscosity chitosan with high deacetylation degree.
The concentration of sodium hydroxide solution is 45 ~ 55%g/g.
The L/kg of sodium hydroxide solution and chitin is 4 ~ 6:1.
Method of the present invention is reacted under condition of high voltage, has avoided long-time reaction to cause the chitosan molecule fracture, reduced viscosity, and deacetylation can reach more than 95% simultaneously, and common only has 90%.The Viscosity of Chitosan that usual way is produced only has 1000mpa, and the Viscosity of Chitosan of producing in this way reaches 2000mpa..
Beneficial effect: compared with prior art, the method for preparing the high viscosity chitosan with high deacetylation degree of the present invention, cost is low, step is few, be easy to industrialization, and the product of preparation has deacetylation and can reach more than 95%, and viscosity reaches 2000mpa.Have good practicality, can produce good economic benefit and social effect.
Embodiment
The present invention is further illustrated below in conjunction with specific embodiment.
Embodiment 1
Drop into the sodium hydroxide solution of 2500L concentration 50%g/g in the 3000L glassed steel reaction vessels, toward wherein adding chitin 500kg, closed reactor is opened steam and is warming up to 90 ℃, keeps reacting kettle inner pressure in 0.2Mpa, at 90 ~ 100 ℃ of insulation 6h.After insulation finished, venting alkali lye was squeezed into purified water unlatching stirring and is washed, repeatedly wash more than three times, until PH reaches 7, and blowing.Then dry, namely obtain the high viscosity chitosan, after testing, deacetylation can reach more than 95%, and Viscosity of Chitosan reaches 2000mpa..
Embodiment 2
Drop into the sodium hydroxide solution of 2400L concentration 45%g/g in the 3000L glassed steel reaction vessels, toward wherein adding chitin 400kg, closed reactor is opened steam and is warming up to 90 ℃, keeps reacting kettle inner pressure in 0.2Mpa, at 90 ~ 100 ℃ of insulation 5h.After insulation finished, venting alkali lye was squeezed into purified water unlatching stirring and is washed, repeatedly wash more than three times, until PH reaches 7, and blowing.Then dry, namely obtain the high viscosity chitosan, after testing, deacetylation can reach more than 95%, and Viscosity of Chitosan reaches 2000mpa..
Embodiment 3
Drop into the sodium hydroxide solution of 2000L concentration 55%g/g in the 3000L glassed steel reaction vessels, toward wherein adding chitin 500kg, closed reactor is opened steam and is warming up to 90 ℃, keeps reacting kettle inner pressure in 0.2Mpa, at 90 ~ 100 ℃ of insulation 7h.After insulation finished, venting alkali lye was squeezed into purified water unlatching stirring and is washed, repeatedly wash more than three times, until PH reaches 7, and blowing.Then dry, namely obtain the high viscosity chitosan, after testing, deacetylation can reach more than 95%, and Viscosity of Chitosan reaches 2000mpa..
Claims (3)
1. method for preparing the high viscosity chitosan with high deacetylation degree is characterized in that: add sodium hydroxide solution and chitin in reactor, 90 ~ 100 ℃ of temperature controls, pressure control be at 0.1 ~ 2Mpa, reaction 5 ~ 7h; Venting alkali lye washs to pH7 for several times with purified water, and blowing is drying to obtain the high viscosity chitosan with high deacetylation degree.
2. the method for preparing the high viscosity chitosan with high deacetylation degree according to claim 1, it is characterized in that: the concentration of sodium hydroxide solution is 45 ~ 55%g/g.
3. the method for preparing the high viscosity chitosan with high deacetylation degree according to claim 1, it is characterized in that: the L/kg of sodium hydroxide solution and chitin is 4 ~ 6:1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201210113768 CN103374081A (en) | 2012-04-18 | 2012-04-18 | Method for preparing high-viscosity and high-deacetylation-degree chitosan |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201210113768 CN103374081A (en) | 2012-04-18 | 2012-04-18 | Method for preparing high-viscosity and high-deacetylation-degree chitosan |
Publications (1)
| Publication Number | Publication Date |
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| CN103374081A true CN103374081A (en) | 2013-10-30 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN 201210113768 Pending CN103374081A (en) | 2012-04-18 | 2012-04-18 | Method for preparing high-viscosity and high-deacetylation-degree chitosan |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103709269A (en) * | 2013-12-27 | 2014-04-09 | 中国科学院海洋研究所 | Method for preparing chitosan with ultrahigh deacetylation degree |
| CN113024686A (en) * | 2021-02-02 | 2021-06-25 | 吉林农业大学 | Preparation method of chitosan |
-
2012
- 2012-04-18 CN CN 201210113768 patent/CN103374081A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103709269A (en) * | 2013-12-27 | 2014-04-09 | 中国科学院海洋研究所 | Method for preparing chitosan with ultrahigh deacetylation degree |
| CN113024686A (en) * | 2021-02-02 | 2021-06-25 | 吉林农业大学 | Preparation method of chitosan |
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| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20131030 |