CN1102152C - Process for preparing water-soluble shitosan - Google Patents
Process for preparing water-soluble shitosan Download PDFInfo
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- CN1102152C CN1102152C CN00113649A CN00113649A CN1102152C CN 1102152 C CN1102152 C CN 1102152C CN 00113649 A CN00113649 A CN 00113649A CN 00113649 A CN00113649 A CN 00113649A CN 1102152 C CN1102152 C CN 1102152C
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Abstract
The present invention discloses a preparation method of water soluble chitosan, which comprises: chitosan is deacetylated by the treatment of 2 to 4 times of 55 to 70% of concentrated sodium hydroxide for 10 to 20 hours at the temperature of 75 to 95DEG C so as to obtain a crude product of the chitosan; then, the crude product of the chitosan stands still for hydrolyzing and purifying at the temperature of 5 to 25DEG C so as to obtain a fine product of water soluble chitosan. The chitosan prepared by the method of the present invention can be dissolved in water and can be absorbed by human bodies. The chitosan prepared by the method has good inhibiting effect of tumors. The chitosan can be prepared into various soluble medicine health products.
Description
The present invention relates to the preparation method of water-soluble chitosan.
Degradation product-the chitosan of chitin has very big value aspect health care, it not only can activating human body cells, enhancing body immunization but also can reduce cholesterol in the blood, for tumour certain prevention and restraining effect are arranged, this point has obtained studies confirm that.The chitosan molecule amount that the preparation method of existing chitosan makes is big, is insoluble in water, and difficulty is absorbed by the body, and there are some researches show, and the chitosan molecule amount has stronger inhibition tumour ability, and is dissolvable in water water 3000 following persons, is easy to be absorbed by human body.
The object of the present invention is to provide the preparation method of soluble chitosan.
Preparation method of the present invention may further comprise the steps:
(1), raw material handles: will remove tortoise, soft-shelled turtle or shrimp or crab housing after the meat, the clear water rinsing is standby;
(2), diluted acid handles: with the salt acid soak of case weight 2～4 times 6～10% (volume percent) 1～2 day, use the clear water rinsing again;
(3), soda boiling removes the albumen degreasing: the sodium hydroxide with 10～15% (weight percents) of 2～4 times of above-mentioned case weights boiled 2～4 hours, used the clear water rinsing;
(4), decalcification is handled again: to remove lime carbonate and calcium phosphate, use the clear water rinsing again with the salt acid soak of 10～15% (volume percent) of 2～4 times of the case weights after the above-mentioned degreasing;
(5), decolouring is handled: regulate pH value with the clear water of 2～4 times of the case weights after the above-mentioned decalcification and constantly stirring the KMnO that adds 1% (weight percent) about 5, under acidic conditions
4Till not taking off to red-purple,, use the clear water rinsing again to remove the organic pigment of housing;
(6), MnO is removed in reduction
2: the housing after will decolouring is soaked in the NaHSO of 1～3% (weight percent)
3In the solution, to remove MnO
2, use the oxalic acid bleaching of 1～4% (weight percent) to obtain fair and clear chitin again;
(7), deacetylation: the concentrated sodium hydroxide with above-mentioned chitin weight 2～4 times 55～70% (weight percent) was handled 10～20 hours at 75～95 ℃, obtained the chitosan crude product;
(8), purifies and separates: crude product is dissolved in 8～10 times of 3～6% (volume percent) dilute acetic acid of its weight, slowly add concentrated base about 10% (weight percent) to mucus occurring, be cooled to 5～25 ℃, left standstill hydrolysis 2～4 hours, be neutralized to pH value 8～9 with dilute hydrochloric acid, and generation floss, constantly stir, no longer produce to floss, filter, sodium-chlor is removed in washing, obtains the soluble chitosan elaboration.
The chitosan of method preparation of the present invention can be water-soluble, and absorption of human body is good, and is effective to the inhibition of tumour, can make the medicines and health protection product of multiple solubility again; And these raw material sources are many, good economy performance, even can utilization of waste material, have significant beneficial effect.
Embodiment:
(1), raw material handles: will remove tortoise, soft-shelled turtle or shrimp or crab housing 1kg after the meat, the clear water rinsing is standby;
(2), diluted acid is handled: the hydrochloric acid with 3kg8% (volume percent) soaks above-mentioned housing 1.5 days, uses the clear water rinsing again;
(3), soda boiling removes the albumen degreasing: with 3kg12% (weight percent) sodium hydroxide housing was boiled 3 hours, use the clear water rinsing;
(4), decalcification is handled again: to remove lime carbonate and calcium phosphate, use the clear water rinsing with 3kg12% (volume percent) salt acid soak housing again;
(5), decolouring is handled: above-mentioned housing is put into the 3kg clear water, and transfer pH value at the KMnO that adds 1% (weight percent) about 5, under acidic conditions
4Till not taking off to red-purple,, use the clear water rinsing again to remove the organic pigment of housing;
(6), MnO is removed in reduction
2: the housing after will decolouring is soaked in the NaHSO of 2% (weight percent)
3In the solution, remove MnO
2, use the oxalic acid bleaching of 2.5% (weight percent) to obtain fair and clear chitin 16 grams again;
(7), deacetylation: the concentrated sodium hydroxide with 32 grams 65% (weight percent) is handled above-mentioned gained chitin 15 hours down at 85 ℃, obtains chitosan crude product 12 grams;
(8), purifies and separates: crude product is dissolved in 100 gram 5% (volume percent) dilute acetic acid, slowly add concentrated base about 10% (weight percent) to mucus occurring, be cooled to 15 ℃, left standstill hydrolysis 3 hours, be neutralized to pH value 8.5 and produce floss with 2N hydrochloric acid, constantly stir, no longer produce to floss, filter, washing is removed sodium-chlor and is obtained soluble chitosan elaboration 10 grams.
Claims (1)
1, the preparation method of water-soluble chitosan is characterized in that may further comprise the steps:
(1), raw material handles: will remove tortoise, soft-shelled turtle or shrimp or crab housing after the meat, the clear water rinsing is standby;
(2), diluted acid handles: with the salt acid soak of case weight 2～4 times 6～10% (volume percent) 1～2 day, use the clear water rinsing again;
(3), soda boiling removes the albumen degreasing: the sodium hydroxide with 10～15% (weight percents) of 2～4 times of above-mentioned case weights boiled 2～4 hours, used the clear water rinsing;
(4), decalcification is handled again: to remove lime carbonate and calcium phosphate, use the clear water rinsing again with the salt acid soak of 10～15% (volume percent) of 2～4 times of the case weights after the above-mentioned degreasing;
(5), decolouring is handled: regulate pH value with the clear water of 2～4 times of the case weights after the above-mentioned decalcification and constantly stirring the KMnO that adds 1% (weight percent) about 5, under acidic conditions
4Till not taking off to red-purple,, use the clear water rinsing again to remove the organic pigment of housing;
(6), MnO is removed in reduction
2: the housing after will decolouring is soaked in the NaHSO of 1～3% (weight percent)
3In the solution, to remove MnO
2, use the oxalic acid bleaching of 1～4% (weight percent) to obtain fair and clear chitin again;
(7), deacetylation: the concentrated sodium hydroxide with above-mentioned chitin weight 2～4 times 55～70% (weight percent) was handled 10～20 hours at 75～95 ℃, obtained the chitosan crude product;
(8), purifies and separates: crude product is dissolved in 8～10 times of 3～6% (volume percent) dilute acetic acid of its weight, slowly add concentrated base about 10% (weight percent) to mucus occurring, be cooled to 5～25 ℃, left standstill hydrolysis 2～4 hours, be neutralized to pH value 8～9 with dilute hydrochloric acid, and generation floss, constantly stir, no longer produce to floss, filter, sodium-chlor is removed in washing, obtains the soluble chitosan elaboration.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN00113649A CN1102152C (en) | 2000-08-28 | 2000-08-28 | Process for preparing water-soluble shitosan |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN00113649A CN1102152C (en) | 2000-08-28 | 2000-08-28 | Process for preparing water-soluble shitosan |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1283634A CN1283634A (en) | 2001-02-14 |
| CN1102152C true CN1102152C (en) | 2003-02-26 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN00113649A Expired - Fee Related CN1102152C (en) | 2000-08-28 | 2000-08-28 | Process for preparing water-soluble shitosan |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1317967C (en) * | 2003-12-05 | 2007-05-30 | 李效时<Del/> | Chitin feed binder and its preparation method |
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|---|---|---|---|---|
| EP1247819A1 (en) * | 2001-04-04 | 2002-10-09 | Dainichiseika Color & Chemicals Mfg. Co. Ltd. | Purified chitins and production process thereof |
| CN1313500C (en) * | 2004-06-25 | 2007-05-02 | 中国科学院海洋研究所 | Preparation of chitin oligose compound |
| CN100491406C (en) * | 2006-11-24 | 2009-05-27 | 暨南大学 | Phosphoryl choline chitosan derivative synthesis method |
| CN102767078A (en) * | 2012-05-24 | 2012-11-07 | 青岛云宙生物科技有限公司 | Special process finished chitosan antibacterial and deodorant health care sock |
| CN103061109B (en) * | 2012-12-14 | 2016-03-02 | 青岛海蓝生物制品有限公司 | Water-insoluble chitin fiber modification becomes the method for water soluble chitosan fiber |
| CN103396263B (en) * | 2013-07-26 | 2015-07-08 | 青岛加中农业科技有限公司 | Biological culture medium using chitin as raw material and application thereof |
| CN103689073A (en) * | 2013-12-16 | 2014-04-02 | 苏州安特实业有限公司 | Preparation technology of fruit and vegetable fresh-keeping agent |
| CN103690956A (en) * | 2013-12-31 | 2014-04-02 | 深圳先进技术研究院 | Hemostatic powder and preparation method thereof |
| CN104788584B (en) * | 2014-01-17 | 2021-08-10 | 厦门大学 | Novel process for cleanly producing chitosan and carboxymethyl chitosan by using crustacean raw materials |
| CN106893005A (en) * | 2017-03-28 | 2017-06-27 | 周景天 | A kind of manufacture craft of soluble chitin |
| CN108641015B (en) * | 2018-05-11 | 2020-08-07 | 武汉轻工大学 | Chitin oxidative degradation method |
| CN110041447A (en) * | 2019-05-14 | 2019-07-23 | 深圳市仙迪化妆品有限公司 | Small molecule algae chitosan and the preparation method and application thereof |
Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN86106726A (en) * | 1986-09-27 | 1988-04-06 | 中国科学院广州化学研究所 | Production of chitin by stepwise acid process |
| US5010181A (en) * | 1988-03-28 | 1991-04-23 | Coughlin Robert W | Partially treated shellfish waste for removal of heavy metals from aqueous solution |
| JPH03127964A (en) * | 1989-10-09 | 1991-05-31 | Yoji Otonari | Animal meat paste product |
| JPH05279401A (en) * | 1992-03-31 | 1993-10-26 | Nippon Kayaku Co Ltd | Production of powdery chitosan |
| CN1085564A (en) * | 1993-08-20 | 1994-04-20 | 连云港开发区金祥贸易有限公司 | A kind of preparation method of chitin |
| CN1089620A (en) * | 1993-12-15 | 1994-07-20 | 屈步华 | Preparation method and product with natural structure chitin |
| CN1097012A (en) * | 1993-06-30 | 1995-01-04 | 上海科学技术大学 | The preparation method of N,O-CMC |
| CN1126048A (en) * | 1995-05-06 | 1996-07-10 | 陈松伟 | Textured vegetable protein containing chitin and its derivatives and prepn. method thereof |
| CN1138336A (en) * | 1994-12-02 | 1996-12-18 | 汉克尔股份两合公司 | Cationic biopolymers |
-
2000
- 2000-08-28 CN CN00113649A patent/CN1102152C/en not_active Expired - Fee Related
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN86106726A (en) * | 1986-09-27 | 1988-04-06 | 中国科学院广州化学研究所 | Production of chitin by stepwise acid process |
| US5010181A (en) * | 1988-03-28 | 1991-04-23 | Coughlin Robert W | Partially treated shellfish waste for removal of heavy metals from aqueous solution |
| JPH03127964A (en) * | 1989-10-09 | 1991-05-31 | Yoji Otonari | Animal meat paste product |
| JPH05279401A (en) * | 1992-03-31 | 1993-10-26 | Nippon Kayaku Co Ltd | Production of powdery chitosan |
| CN1097012A (en) * | 1993-06-30 | 1995-01-04 | 上海科学技术大学 | The preparation method of N,O-CMC |
| CN1085564A (en) * | 1993-08-20 | 1994-04-20 | 连云港开发区金祥贸易有限公司 | A kind of preparation method of chitin |
| CN1089620A (en) * | 1993-12-15 | 1994-07-20 | 屈步华 | Preparation method and product with natural structure chitin |
| CN1138336A (en) * | 1994-12-02 | 1996-12-18 | 汉克尔股份两合公司 | Cationic biopolymers |
| CN1126048A (en) * | 1995-05-06 | 1996-07-10 | 陈松伟 | Textured vegetable protein containing chitin and its derivatives and prepn. method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1317967C (en) * | 2003-12-05 | 2007-05-30 | 李效时<Del/> | Chitin feed binder and its preparation method |
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| CN1283634A (en) | 2001-02-14 |
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