CN1205233C - Carboxymethyl chitin, its preparing method and usage - Google Patents
Carboxymethyl chitin, its preparing method and usage Download PDFInfo
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- CN1205233C CN1205233C CN 03118437 CN03118437A CN1205233C CN 1205233 C CN1205233 C CN 1205233C CN 03118437 CN03118437 CN 03118437 CN 03118437 A CN03118437 A CN 03118437A CN 1205233 C CN1205233 C CN 1205233C
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- chitin
- chitosan
- carboxymethyl chitin
- carboxymethyl
- sodium hydroxide
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Abstract
The present invention discloses carboxymethyl chitin which has good moisture absorption and moisture preservation performance, chitosan and a preparation method thereof. The method comprises the following steps: chitin used as raw material is thoroughly alkalized in sodium hydroxide solution; chloroacetic acid is added to isopropyl alcohol solution; at the room temperature, the reaction is carried out for 3 to 8 hours; after the reaction is finished, a product is regulated to be neutral with diluted hydrochloric acid, and required 6-O-CM-chitin is obtained; 6-O-CM-chitin is deacetylated with mixed solution of alkali and alcohol, and 6-O-CM-chitosan is prepared. The method is simple and is easily operated. The prepared carboxymethyl chitin and the chitosan have the same moisture absorption and moisture preservation effect as hyaluronic acid. Because sources of the carboxymethyl chitin and the chitosan are abundant, and the price is low, the carboxymethyl chitin and the chitosan can replace the hyaluronic acid to be used in cosmetics and clinical medicine, and the carboxymethyl chitin and the chitosan have the good development prospect.
Description
Technical field
The present invention relates to a kind of preparation method of carboxymethyl chitin.
Background technology
Hyaluronic acid is described as " gold of preserving moisture ", because its good performance of keeping humidity is widely used in makeup and clinical medicine.Though hyaluronic acid is very wide in distributed in nature, total amount seldom costs an arm and a leg.
Summary of the invention
Problem to be solved by this invention provides a kind of preparation method who possesses the carboxymethyl chitin of good moisture absorption, performance of keeping humidity, the inexpensive alternative hyaluronic acid of gained carboxymethyl chitin (carboxymethyl chitin, chitosan) is as wetting Agent for Printing Inks, and the preparation method is simple.
Carboxymethyl chitin in the technical scheme provided by the invention (carboxymethyl chitin, chitosan), carboxymethyl 60%-90% is substituted in chitinous C-6 position, and molecular weight is 1.0 * 10
5-1.0 * 10
6, degree of substitution by carboxymethyl is 0.6-1.0.
The invention provides the preparation method of above-mentioned carboxymethyl chitin, get the fully alkalization in sodium hydroxide solution of 50-80g chitin, add the 300-500ml Virahol, add the 80-120g Mono Chloro Acetic Acid again, room temperature reaction 3-8 hour, reaction finishes after product and transfers to neutrality with dilute hydrochloric acid, obtains the carboxymethyl chitin (6-O-CM-chitin) of 6 required replacements.6-O-CM-chitin uses the mixing solutions deacetylation of alkali and alcohol again, makes the cm-chitosan (6-O-CM-chitosan) of 6 replacements.
Above-mentioned chitin in-20-0 ℃ freezing 4-12 hour, adds Virahol in sodium hydroxide solution fully after the alkalization again after thawing.
Above-mentioned raw materials THE MOLECULAR WEIGHT OF CHITIN 3.0 * 10
5-1.0 * 10
6, concentration sodium hydroxide is 50-70% (W/W).
Alkali is NaOH or KOH in the mixing solutions of above-mentioned alkali and alcohol, and the concentration of alkali is 20-40% (W/W).
Technology of the present invention is simply effective.The carboxymethyl chitin and the chitosan of preparation are inexpensive, its moisture absorption, moisture retention and hyaluronic acid quite or be better than hyaluronic acid, alternative hyaluronic acid is used for makeup and clinical medicine.
Embodiment
Embodiment 1: getting molecular weight is 5.0 * 10
5The fully alkalization in the sodium hydroxide solution of (weight percent, down with) 60% of 50 gram chitins, freezing 12 hours in-20 ℃.Add the 500ml Virahol after thawing, add the 100g Mono Chloro Acetic Acid again, room temperature reaction 5 hours, reaction finishes after product and transfers to neutrality with dilute hydrochloric acid.Again that product is water-soluble, dialyse after 5 days, obtain the carboxymethyl chitin (6-O-CM-chitin) of 6 required replacements with acetone precipitation.Its moisture absorption, moisture retention are listed in the table 1.
Embodiment 2: getting molecular weight is 1.0 * 10
670 the gram chitins in 65% sodium hydroxide solution fully the alkalization, freezing 8 hours in-20 ℃.Add the 500ml Virahol after thawing, add the 120g Mono Chloro Acetic Acid again, room temperature reaction 7 hours, reaction finishes after product and transfers to neutrality with dilute hydrochloric acid.Obtain the carboxymethyl chitin (6-O-CM-chitin) of 6 required replacements.With the aqueous isopropanol deacetylation of 6-O-CM-chitin, make required 6-O-CM-chitosan again with 30% alkali (NaOH).Its moisture absorption, moisture retention are listed in the table 1.
Embodiment 3: getting molecular weight is 1.0 * 10
650 gram chitins in 55% sodium hydroxide solution fully after the alkalization, add the 500ml Virahol, add the 80g Mono Chloro Acetic Acid again, room temperature reaction 8 hours, reaction finishes after product and transfers to neutrality with dilute hydrochloric acid, obtains the carboxymethyl chitin (6-O-CM-chitin) of 6 required replacements.With the aqueous isopropanol deacetylation of 6-O-CM-chitin, make required 6-O-CM-chitosan again with 40% alkali (KOH).Its moisture absorption, moisture retention are listed in the table 1.
Comparative example 1
(N-CM-chitosan) compares with the cm-chitosan that replaces on the nitrogen position, and its moisture absorption, moisture retention are also listed in the table 1.
Comparative example 2
With molecular weight is 1 * 10
46-O-CM-chitin compare, its moisture absorption, moisture retention are listed in the table 1.
Comparative example 3
Get hyaluronic acid and compare, moisture absorption, moisture retention are listed in the table 1.
Table 1
| Embodiment 1 | Embodiment 2 | Embodiment 2 | Comparative Examples 1 | Comparative Examples 2 | Comparative Examples 3 | |
| RH81% rate of moisture absorption (%) | 48 | 50 | 40 | 35 | 60 | 56 |
| The RH43% rate (%) of preserving moisture | 240 | 220 | 180 | 180 | 50 | 240 |
Claims (3)
1. the preparation method of carboxymethyl chitin, it is characterized in that: get the fully alkalization in sodium hydroxide solution of 50-80g chitin, add the 300-500ml Virahol, add the 80-120g Mono Chloro Acetic Acid again, room temperature reaction 3-8 hour, reaction finishes after product and transfers to neutrality with dilute hydrochloric acid, obtains the carboxymethyl chitin of 6 required replacements.
2. method according to claim 1 is characterized in that: chitin in-20-0 ℃ freezing 4-12 hour, adds Virahol in sodium hydroxide solution fully after the alkalization again after thawing.
3. method according to claim 1 and 2 is characterized in that: raw material THE MOLECULAR WEIGHT OF CHITIN 3.0 * 10
5-1.0 * 10
6, concentration sodium hydroxide is 50-70wt%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03118437 CN1205233C (en) | 2003-01-09 | 2003-01-09 | Carboxymethyl chitin, its preparing method and usage |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03118437 CN1205233C (en) | 2003-01-09 | 2003-01-09 | Carboxymethyl chitin, its preparing method and usage |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1431230A CN1431230A (en) | 2003-07-23 |
| CN1205233C true CN1205233C (en) | 2005-06-08 |
Family
ID=4790772
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 03118437 Expired - Fee Related CN1205233C (en) | 2003-01-09 | 2003-01-09 | Carboxymethyl chitin, its preparing method and usage |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1205233C (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101701042B (en) * | 2009-03-28 | 2011-11-30 | 中国科学院海洋研究所 | Carboxymethyl chitosan thiourea resin and preparation method and application thereof |
| CN106366213B (en) * | 2016-08-25 | 2019-05-10 | 浙江澳兴生物科技有限公司 | The industrialized process for preparing of O-CMC |
| CN109734519A (en) * | 2019-03-15 | 2019-05-10 | 招远市金虹精细化工有限公司 | A kind of nutrient solution and its application method for administering grassland desertification |
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2003
- 2003-01-09 CN CN 03118437 patent/CN1205233C/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN1431230A (en) | 2003-07-23 |
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