CN1056853C - Method for prepn. of chitose - Google Patents
Method for prepn. of chitose Download PDFInfo
- Publication number
- CN1056853C CN1056853C CN96101077A CN96101077A CN1056853C CN 1056853 C CN1056853 C CN 1056853C CN 96101077 A CN96101077 A CN 96101077A CN 96101077 A CN96101077 A CN 96101077A CN 1056853 C CN1056853 C CN 1056853C
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- CN
- China
- Prior art keywords
- shrimp
- clear water
- chitosan
- rinsing
- hours
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
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- 238000000034 method Methods 0.000 title abstract description 4
- LKAPTZKZHMOIRE-KVTDHHQDSA-N (2s,3s,4s,5r)-3,4-dihydroxy-5-(hydroxymethyl)oxolane-2-carbaldehyde Chemical compound OC[C@H]1O[C@H](C=O)[C@@H](O)[C@@H]1O LKAPTZKZHMOIRE-KVTDHHQDSA-N 0.000 title 1
- LKAPTZKZHMOIRE-UHFFFAOYSA-N chitose Natural products OCC1OC(C=O)C(O)C1O LKAPTZKZHMOIRE-UHFFFAOYSA-N 0.000 title 1
- 241000238557 Decapoda Species 0.000 claims abstract description 32
- 229920001661 Chitosan Polymers 0.000 claims abstract description 19
- 238000002360 preparation method Methods 0.000 claims abstract description 7
- 229910017053 inorganic salt Inorganic materials 0.000 claims abstract description 6
- 235000013372 meat Nutrition 0.000 claims abstract description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 33
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 23
- 239000000463 material Substances 0.000 claims description 14
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 11
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 10
- 230000007935 neutral effect Effects 0.000 claims description 8
- MBLBDJOUHNCFQT-LXGUWJNJSA-N aldehydo-N-acetyl-D-glucosamine Chemical compound CC(=O)N[C@@H](C=O)[C@@H](O)[C@H](O)[C@H](O)CO MBLBDJOUHNCFQT-LXGUWJNJSA-N 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 6
- 229960000583 acetic acid Drugs 0.000 claims description 5
- 230000006196 deacetylation Effects 0.000 claims description 5
- 238000003381 deacetylation reaction Methods 0.000 claims description 5
- 239000012362 glacial acetic acid Substances 0.000 claims description 5
- 150000003839 salts Chemical class 0.000 claims description 5
- 238000007654 immersion Methods 0.000 claims description 3
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 2
- 229910052791 calcium Inorganic materials 0.000 claims description 2
- 239000011575 calcium Substances 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 238000002791 soaking Methods 0.000 claims description 2
- 239000002994 raw material Substances 0.000 abstract description 7
- 238000006116 polymerization reaction Methods 0.000 abstract description 5
- 230000036541 health Effects 0.000 abstract description 3
- 230000001363 autoimmune Effects 0.000 abstract description 2
- 230000004060 metabolic process Effects 0.000 abstract description 2
- 125000000218 acetic acid group Chemical group C(C)(=O)* 0.000 abstract 1
- 230000003544 deproteinization Effects 0.000 abstract 1
- 230000009758 senescence Effects 0.000 abstract 1
- 239000002253 acid Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 3
- 150000001412 amines Chemical class 0.000 description 3
- 235000009508 confectionery Nutrition 0.000 description 3
- 241000131500 Chionoecetes opilio Species 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 201000011510 cancer Diseases 0.000 description 2
- 201000010099 disease Diseases 0.000 description 2
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 2
- 239000000428 dust Substances 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 229920002521 macromolecule Polymers 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 241000238424 Crustacea Species 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- 206010028980 Neoplasm Diseases 0.000 description 1
- 241001533364 Portunus trituberculatus Species 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000003712 anti-aging effect Effects 0.000 description 1
- 230000001093 anti-cancer Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 229960002442 glucosamine Drugs 0.000 description 1
- 231100001261 hazardous Toxicity 0.000 description 1
- 230000003053 immunization Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000004089 microcirculation Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000001473 noxious effect Effects 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 235000014102 seafood Nutrition 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 230000004083 survival effect Effects 0.000 description 1
Landscapes
- Polysaccharides And Polysaccharide Derivatives (AREA)
- Cosmetics (AREA)
Abstract
The present invention relates to chitosan, particularly to a preparation method of chitosan. The present invention is characterized in that shrimp and crab resources produced in China are utilized; heads are removed, meat is peeled, and shells are reserved; through rinsing operation, deproteinization, inorganic salt removal, acetyl removal/polymerization, dryness and grinding operation, the chitosan is obtained. The present invention has the characteristics that the method is simple, and the quality of finished products conforms to requirements. The present invention provides a large quantity of raw material which can resist senescence, can promote metabolism of a human body, can regulate microcirculatory of a human body and can strengthen autoimmune for health care and medical treatment.
Description
What the present invention relates to is a kind of chitosan, concretely, relate to be a kind of principal constituent be the poly-grape amine candy (preparation method of the macromolecular compound of α-N-Glucosamine).
Chitosan of the present invention has been widely used in body-care and medical aspect, becomes the high-new technology products in the rotten world of current wind, and is described as the 6th kind of living matter of human survival.This be because chitosan have multiple function to the human body beneficial: it can promote human body metabolism, delay senility; It also can prevent and the treatment effect of malignant tumors and play by adjusting and the improvement to the microcirculation in human body function.Existing result of study is verified chitosan of the present invention has good anticancer, control the cancer effect, and be applied to medical treatment.
Chitosan of the present invention can improve and improve constantly the autoimmune function of human body, and the effect that plays diseases prevention, cures the disease, it plays a role in health care in the many hazardous and noxious substances of human body internal adsorption owing to itself be a kind of macromolecular compound of positively charged.Therefore the attention object that multi-purpose formulation, health-care product just become many logists on the our times is further developed and developed to chitosan.
The main raw material of chitosan is the shell of the Crustacean in the ocean, as crab, shrimp etc.Main production country is at present: Japan, Korea S, the U.S., Canada and some countries of Europe.The raw material that they utilized mainly is the red pawl crab of Hokkaido, Japan and Alaska snow crab, because this kind animal chitosan content on one's body is higher, general extraction yield can reach 30-40wt%.
China is a maritime nation, and a large amount of sea-food resources is also arranged, but does not have the red pawl crab in Hokkaido and Alaska snow crab, but China is coastal a large amount of prawns, shrimp crab (being commonly called as shrimp basketry, skin skin shrimp) and swimming crab is arranged.Utilize local shrimp shell and shrimp and crab shells to extract not only aboundresources of chitosan, and to the protection environment, it is very favourable that minimizing is polluted.But, utilize prior art, this country is produced abundant shrimp shell and shrimp and crab shells handle to extract poly-grape amine candy, good effect and high extraction yield can not be arranged all the time.
The objective of the invention is to utilize national resource abundant shrimp shell and shrimp and crab shells, a preparation method who is particularly suitable for extracting chitosan from national shrimp shell and shrimp and crab shells is provided.
Purpose of the present invention can be achieved through the following technical solutions:
Chitosan of the present invention (chemical name: preparation method poly-grape amine candy):
1) shrimp, shrimp crab are decaptitated, takes off meat, continue to employ its shell;
2) with the clear water rinsing of shrimp, shrimp and crab shells;
3) with the shrimp after the clear water rinsing, shrimp and crab shells, carry out deproteinated and handle, in this operation, working concentration is about 2-6wt%NaOH (caustic soda) will handle back shrimp, shrimp and crab shells immersion, immersion is carried out under 85-102 ℃ of condition, and the treatment time is about 8～12 hours;
4) material after will soaking with the clear water rinsing to neutral;
5) take off inorganic salt then, in this operation:
The HCl (hydrochloric acid) that working concentration is about 10～20wt% handled 8～12 hours under 45～80 ℃ of conditions, was the inorganic salts of main component with calcium to the greatest extent until taking off fully.
6) will take off material rinsing behind the inorganic salt to neutral, the working concentration Glacial acetic acid that is about 2wt% soaked 2～4 hours then, and the material decolouring is handled to pure white;
7) material after will decolouring carries out deacetylation and handles, and carries out polymerization when handling, in this operation:
Working concentration is about the caustic soda of 25～35wt%, handles 4～6 hours under 80～100 ℃ of conditions;
8) material after deacetylation, the polymerization is extremely neutral with the clear water rinsing;
9) rinsing to neutral material is carried out drying;
10) then with exsiccant material pulverize or the aqueous finished product of sour melt into;
The present invention is described in further detail below by embodiment:
| Operation | Embodiment 1 | Embodiment 2 | Embodiment 3 |
| Raw material | The shrimp shell | Shrimp and crab shells | Shrimp/shrimp and crab shells compound |
| Rinsing | Clear water | Clear water | Clear water |
| Deproteinated treatment agent title consumption time hr temperature ℃ | 2wt% caustic soda excessive 12 102 | 6wt% caustic soda excessive 8 85 | 4wt% caustic soda excessive 10 95 |
| Rinsing | Clear water | Clear water | Clear water |
| Take off inorganic salt treatment agent title consumption time hr temperature ℃ | 10wt% salt excessive acid 12 65 | 20wt% salt excessive acid 8 45 | 15wt% salt excessive acid 10 80 |
| Rinsing | Clear water | Clear water | Clear water |
| Decolorizing treatment agent title consumption time hr | 2wt% Glacial acetic acid excessive 2 | 2wt% Glacial acetic acid excessive 4 | 2wt% Glacial acetic acid excessive 3 |
| Temperature ℃ | Normal temperature | Normal temperature | Normal temperature |
| Rinsing | Clear water | Clear water | Clear water |
| Deacetylation/aggregation processing agent title consumption time hr temperature ℃ | 25wt% caustic soda excessive 5～7 100 | 30wt% caustic soda excessive 6～8 90 | 15wt% caustic soda excessive 4～6 80 |
| Rinsing | Clear water | Clear water | Clear water |
| Dry | Prior art | Prior art | Prior art |
| Finished product | Acid is molten | Abrasive dust | Abrasive dust |
Processing condition of the present invention and operation can be adjusted in above-mentioned scope and different orderings, for example, can decolour after deacetylate, polymerization if desired; When adopting treatment agent to handle, also can adopt increases concentration method gradually, for example, initial concentration is fixed on lower bound, in the part of treatment time scope, makes it to be increased to a higher value and keeps the regular hour.
According to technology of the present invention, starting material-shrimp shell, the shrimp/shrimp and crab shells-processing of China can be purified, after polymerization, can reach following index:
Insolubles＜1wt%
Ash content＜3wt%
Molten back viscosity 1000/500c.p.s
Exploitation of the present invention is to carry out utilizing on the national resource basis, can not handle the raw material that originates in the Chinese place of production owing to directly adopt existing processes, or the requirement that does not reach use maybe can not reach above-mentioned index, therefore, technology of the present invention has solved this problem, simultaneously, also solve the raw material problem and be not subjected to the control of foreign country raw material.Chitosan price in the international market is 7800～10000 dollars one ton, of the present inventionly successfully earns foreign exchange for country can save foreign exchange.Because chitosan has function to the human body beneficial: anti-ageing, as to strengthen self immunizing power etc. thereby can be widely used in health care and medical aspect.
Claims (2)
1. the preparation method of a chitosan is characterized in that selecting for use shrimp shell, shrimp and crab shells:
1) shrimp, shrimp crab are decaptitated, takes off meat, continue to employ its shell;
2) with the clear water rinsing of shrimp, shrimp and crab shells;
3) with the shrimp after the clear water rinsing, shrimp and crab shells, carry out deproteinated and handle, in this operation, working concentration is that the NaOH of 2-6wt% will handle the back shrimp, shrimp and crab shells soaks, and immersion is carried out under 85-102 ℃ of condition, and the treatment time is 8～12 hours;
4) material after will soaking with the clear water rinsing to neutral;
5) take off inorganic salt then, in this operation:
Working concentration is the HCl of 10～20wt%, under 45～80 ℃ of conditions, handled 8～12 hours, and be the inorganic salts of main component with calcium to the greatest extent until taking off fully;
6) will take off material rinsing behind the inorganic salt to neutral, working concentration is that the Glacial acetic acid of 2wt% soaked 2～4 hours then, and the material decolouring is handled to pure white;
7) under 80～100 ℃ of conditions, working concentration is the caustic soda of 25～35wt%, the material after the decolouring is carried out deacetylation handled 4～6 hours;
8) material behind the deacetylation is extremely neutral with the clear water rinsing;
9) rinsing to neutral material is carried out drying;
10) then with exsiccant material pulverize or the aqueous finished product of sour melt into.
2. the preparation method of chitosan according to claim 1 is characterized in that the concentration of described treatment agent increases gradually.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN96101077A CN1056853C (en) | 1996-02-26 | 1996-02-26 | Method for prepn. of chitose |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN96101077A CN1056853C (en) | 1996-02-26 | 1996-02-26 | Method for prepn. of chitose |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1158335A CN1158335A (en) | 1997-09-03 |
| CN1056853C true CN1056853C (en) | 2000-09-27 |
Family
ID=5116913
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN96101077A Expired - Fee Related CN1056853C (en) | 1996-02-26 | 1996-02-26 | Method for prepn. of chitose |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1056853C (en) |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1113896C (en) * | 1998-01-04 | 2003-07-09 | 刘荣秀 | Preparation of epidermal growth factor with marine products and relevant discard |
| CN101200505B (en) * | 2007-11-29 | 2011-01-19 | 湖北东方天琪生物工程股份有限公司 | Method for preparing high deacetylate degree and high viscosity chitosan by using shrimp shell |
| CN101249275B (en) * | 2008-01-10 | 2011-06-29 | 中国人民解放军第二军医大学 | Wound dressing capable of insulating sea water and method of preparing the same |
| WO2009117499A1 (en) | 2008-03-19 | 2009-09-24 | Agratech International, Inc. | Chitosan manufacturing process |
| CN109021145B (en) * | 2018-06-19 | 2020-11-20 | 南京理工大学泰州科技学院 | Method for preparing chitosan by taking crude chitin as raw material |
| CN112294907A (en) * | 2020-10-27 | 2021-02-02 | 青岛翼科新程生物科技有限公司 | Chlorine dioxide nano-zinc disinfection and bacteriostasis wash-free gel |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6142547A (en) * | 1984-08-03 | 1986-03-01 | Unitika Ltd | Chitin molding |
| US5010181A (en) * | 1988-03-28 | 1991-04-23 | Coughlin Robert W | Partially treated shellfish waste for removal of heavy metals from aqueous solution |
| JPH05279401A (en) * | 1992-03-31 | 1993-10-26 | Nippon Kayaku Co Ltd | Production of powdery chitosan |
-
1996
- 1996-02-26 CN CN96101077A patent/CN1056853C/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6142547A (en) * | 1984-08-03 | 1986-03-01 | Unitika Ltd | Chitin molding |
| US5010181A (en) * | 1988-03-28 | 1991-04-23 | Coughlin Robert W | Partially treated shellfish waste for removal of heavy metals from aqueous solution |
| JPH05279401A (en) * | 1992-03-31 | 1993-10-26 | Nippon Kayaku Co Ltd | Production of powdery chitosan |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1158335A (en) | 1997-09-03 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| C53 | Correction of patent of invention or patent application | ||
| CB02 | Change of applicant information |
Applicant after: BEIJING SHENGMINGZHIGUANG SCIENCE & TECHNOLOGY DEVELOPMENT Co.,Ltd. Applicant before: Li Zhiqiu |
|
| CB03 | Change of inventor or designer information |
Inventor after: Li Zhiqiu Inventor after: Zhang Jiandong Inventor after: Zhang Zhendong Inventor before: Zhang Jiandong Inventor before: Li Zhiqiu Inventor before: Zhang Zhendong |
|
| COR | Change of bibliographic data |
Free format text: CORRECT: INVENTOR; FROM: ZHANG JIANDONG; LI ZHIQIU; ZHANG ZHENDONG TO: LI ZHIQIU; ZHANG JIANDONG; ZHANG ZHENDONG |
|
| SE01 | Entry into force of request for substantive examination | ||
| C57 | Notification of unclear or unknown address | ||
| DD01 | Delivery of document by public notice |
Addressee: BEIJING SHENGMINGZHIGUANG SCIENCE & TECHNOLOGY DEVELOPMENT Co.,Ltd. Document name: Notice of first review |
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| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C19 | Lapse of patent right due to non-payment of the annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |