CN105754015A - Method for extracting chitin from oyster shell - Google Patents
Method for extracting chitin from oyster shell Download PDFInfo
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- CN105754015A CN105754015A CN201610110383.7A CN201610110383A CN105754015A CN 105754015 A CN105754015 A CN 105754015A CN 201610110383 A CN201610110383 A CN 201610110383A CN 105754015 A CN105754015 A CN 105754015A
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- oyster shell
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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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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Molecular Biology (AREA)
- Engineering & Computer Science (AREA)
- Biochemistry (AREA)
- Materials Engineering (AREA)
- General Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Sustainable Development (AREA)
- Meat, Egg Or Seafood Products (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
- Preparation Of Compounds By Using Micro-Organisms (AREA)
Abstract
The invention provides a method for extracting chitin from oyster shell. The method comprises the following steps: fetching oyster shell, cleaning with water and grinding to obtain oyster shell powder; adding the oyster shell powder into a complex enzyme-containing dilute hydrochloric acid solution and soaking; filtering; washing the filter residue with water to obtain demineralized oyster shell powder; adding the demineralized oyster shell powder into a NaOH solution and soaking; adjusting the pH of the extract liquid to 7.5-8.5 by using diluted sulfuric acid; adding trypsin for enzymolysis to obtain enzymatic hydrolysate; performing enzyme deactivation; filtering with an ultrafiltration membrane to obtain ultrafiltration permeate liquid; filtering with a nanofiltration membrane to obtain concentrate; finally, performing spray drying of the obtained concentrate to obtain powder; and conveying the powder into an extraction kettle and performing CO2 supercritical extraction to obtain chitin powder. The chitin extraction technology provided by the invention is simple to operate, and the obtained chitin has high yield and good purity.
Description
Technical field
The invention belongs to natural product technical field, be specifically related to a kind of method of chitin extraction from oyster shell.
Background technology
Chitin is quantitatively to be only second to cellulosic second largest living resources at nature, estimate that annual biosynthetic chitin is up to 10,000,000,000 tons, it it is one of Organic substance the abundantest on the earth, it is the inexhaustible living resources of the mankind, also being one of natural resources of not being fully utilized 21 century, wherein marine organisms growing amount reaches 1,000,000,000 tons.Because the cellulosic structure being widely present in the chemical constitution of chitin and plant is closely similar, therefore it is also called tunicin, chitin is widely present in the carapace of Crustaceans shrimp, Eriocheir sinensis, the carapace of insecticide, the cell wall of fungus (yeast, mycete) and in the cell wall of plant (such as mushroom).Owing to the yield of shrimp, Carapax Eriocheir sinensis is higher, the content of chitin higher (general chitin content more than 20～30%, have up to 60～85%), preparation method are relatively simple, therefore prepare chitin at present mainly by shrimp, Carapax Eriocheir sinensis.But utilizing shrimp, Carapax Eriocheir sinensis to prepare chitin and there is also some problems that can not be ignored, one is in addition to outside the marine products processing enterprise that some are large-scale, shrimp, Carapax Eriocheir sinensis are difficult to all be taken as rubbish after concentric acquisition, general eating at home or hotel eat and abandon and be difficult to reclaim；Two is that shrimp, Carapax Eriocheir sinensis are contained within the Symbionts such as substantial amounts of protein and fat, and pretreatment is cumbersome, processes not only or be not completely dried, very easily rises mould rotten during preservation.Just because of so some reasons, shrimp, making full use of of Carapax Eriocheir sinensis is made to be greatly limited.
Summary of the invention
It is an object of the invention to overcome the deficiencies in the prior art to provide a kind of method of chitin extraction from oyster shell, the method technological operation is simple, and gained chitin yield is high, good product purity.
A kind of method of chitin extraction from oyster shell, comprises the following steps:
Step 1, takes oyster shell, washes, and pulverizes, obtains oyster shell powder end；
Step 2, with parts by weight, by soaking in 10 parts of end of the step 1 gained oyster shell powder dilute hydrochloric acid solution added to containing 1～4wt% compound enzyme 30～50 parts, filters, and filtering residue obtains demineralization oyster shell powder through washing；
Step 3, with parts by weight, adds to step 2 gained demineralization oyster shell powder 10 parts in NaOH solution 20～30 parts and soaks, regulate the pH to 7.5～8.5 of lixiviating solution with dilute sulfuric acid, be subsequently adding trypsin 3～8 parts, enzymolysis, obtain enzymolysis solution；
Step 4, after step 3 gained enzymolysis solution enzyme denaturing, is filtered with ultrafilter membrane, obtains ultrafiltration permeate, then be filtered by NF membrane, obtain concentrated solution；
Step 5, is undertaken being spray dried to powder by step 5 gained concentrated solution, is sent into by powder in extraction kettle, through CO2Supercritical extraction, obtains chitin powder.
Further, the granularity at step 1 gained oyster shell powder end is at 20～40 orders.
Further, in step 2, compound enzyme is cellulase and protease mass ratio is the mixed enzyme of 2: 1.
Further, in step 2, soaking temperature is 50～70 DEG C, and the time is 20～40min.
Further, in step 3, the concentration of NaOH solution is 10～20wt%.
Further, in step 3, soaking temperature is 80～100 DEG C, and the time is 2～4h.
Further, in step 5, extraction temperature is 40～50 DEG C, and pressure is 20～30MPa, and flow is 15～30L/h.
The chitin extraction technology of the present invention is simple to operate, and gained chitin yield is high, good product purity.
Detailed description of the invention
Embodiment 1
A kind of method of chitin extraction from oyster shell, comprises the following steps:
Step 1, takes oyster shell, washes, and pulverizes, obtains oyster shell powder end；
Step 2, with parts by weight, by soaking in 10 parts of end of the step 1 gained oyster shell powder dilute hydrochloric acid solution added to containing 1wt% compound enzyme 30 parts, filters, and filtering residue obtains demineralization oyster shell powder through washing；
Step 3, with parts by weight, adds to step 2 gained demineralization oyster shell powder 10 parts in NaOH solution 20 parts and soaks, regulate the pH to 7.5 of lixiviating solution with dilute sulfuric acid, be subsequently adding trypsin 3 parts, enzymolysis, obtain enzymolysis solution；
Step 4, after step 3 gained enzymolysis solution enzyme denaturing, is filtered with ultrafilter membrane, obtains ultrafiltration permeate, then be filtered by NF membrane, obtain concentrated solution；
Step 5, is undertaken being spray dried to powder by step 5 gained concentrated solution, is sent into by powder in extraction kettle, through CO2Supercritical extraction, obtains chitin powder.
Wherein, the granularity at step 1 gained oyster shell powder end is at 20 orders；In step 2, compound enzyme is cellulase and protease mass ratio is the mixed enzyme of 2: 1, and soaking temperature is 50 DEG C, and the time is 20min；In step 3, the concentration of NaOH solution is 10wt%, and soaking temperature is 80 DEG C, and the time is 4h；In step 5, extraction temperature is 40 DEG C, and pressure is 30MPa, and flow is 15L/h.
Can preparing chitin 0.04kg in the oyster shell of every 1kg, purity is 93%.
Embodiment 2
A kind of method of chitin extraction from oyster shell, comprises the following steps:
Step 1, takes oyster shell, washes, and pulverizes, obtains oyster shell powder end；
Step 2, with parts by weight, by soaking in 10 parts of end of the step 1 gained oyster shell powder dilute hydrochloric acid solution added to containing 2wt% compound enzyme 35 parts, filters, and filtering residue obtains demineralization oyster shell powder through washing；
Step 3, with parts by weight, adds to step 2 gained demineralization oyster shell powder 10 parts in NaOH solution 23 parts and soaks, regulate the pH to 8.0 of lixiviating solution with dilute sulfuric acid, be subsequently adding trypsin 7 parts, enzymolysis, obtain enzymolysis solution；
Step 4, after step 3 gained enzymolysis solution enzyme denaturing, is filtered with ultrafilter membrane, obtains ultrafiltration permeate, then be filtered by NF membrane, obtain concentrated solution；
Step 5, is undertaken being spray dried to powder by step 5 gained concentrated solution, is sent into by powder in extraction kettle, through CO2Supercritical extraction, obtains chitin powder.
Wherein, the granularity at step 1 gained oyster shell powder end is at 30 orders；In step 2, compound enzyme is cellulase and protease mass ratio is the mixed enzyme of 2: 1, and soaking temperature is 60 DEG C, and the time is 30min；In step 3, the concentration of NaOH solution is 15wt%, and soaking temperature is 90 DEG C, and the time is 3h；In step 5, extraction temperature is 45 DEG C, and pressure is 25MPa, and flow is 20L/h.
Can preparing chitin 0.05kg in the oyster shell of every 1kg, purity is 94%.
Embodiment 3
A kind of method of chitin extraction from oyster shell, comprises the following steps:
Step 1, takes oyster shell, washes, and pulverizes, obtains oyster shell powder end；
Step 2, with parts by weight, by soaking in 10 parts of end of the step 1 gained oyster shell powder dilute hydrochloric acid solution added to containing 3wt% compound enzyme 45 parts, filters, and filtering residue obtains demineralization oyster shell powder through washing；
Step 3, with parts by weight, adds to step 2 gained demineralization oyster shell powder 10 parts in NaOH solution 30 parts and soaks, regulate the pH to 8.5 of lixiviating solution with dilute sulfuric acid, be subsequently adding trypsin 7 parts, enzymolysis, obtain enzymolysis solution；
Step 4, after step 3 gained enzymolysis solution enzyme denaturing, is filtered with ultrafilter membrane, obtains ultrafiltration permeate, then be filtered by NF membrane, obtain concentrated solution；
Step 5, is undertaken being spray dried to powder by step 5 gained concentrated solution, is sent into by powder in extraction kettle, through CO2Supercritical extraction, obtains chitin powder.
Wherein, the granularity at step 1 gained oyster shell powder end is at 40 orders；In step 2, compound enzyme is cellulase and protease mass ratio is the mixed enzyme of 2: 1, and soaking temperature is 60 DEG C, and the time is 40min；In step 3, the concentration of NaOH solution is 20wt%, and soaking temperature is 90 DEG C, and the time is 2h；In step 5, extraction temperature is 50 DEG C, and pressure is 20MPa, and flow is 30L/h.
Can preparing chitin 0.04kg in the oyster shell of every 1kg, purity is 96%.
Embodiment 4
A kind of method of chitin extraction from oyster shell, comprises the following steps:
Step 1, takes oyster shell, washes, and pulverizes, obtains oyster shell powder end；
Step 2, with parts by weight, by soaking in 10 parts of end of the step 1 gained oyster shell powder dilute hydrochloric acid solution added to containing 4wt% compound enzyme 50 parts, filters, and filtering residue obtains demineralization oyster shell powder through washing；
Step 3, with parts by weight, adds to step 2 gained demineralization oyster shell powder 10 parts in NaOH solution 30 parts and soaks, regulate the pH to 8.5 of lixiviating solution with dilute sulfuric acid, be subsequently adding trypsin 8 parts, enzymolysis, obtain enzymolysis solution；
Step 4, after step 3 gained enzymolysis solution enzyme denaturing, is filtered with ultrafilter membrane, obtains ultrafiltration permeate, then be filtered by NF membrane, obtain concentrated solution；
Step 5, is undertaken being spray dried to powder by step 5 gained concentrated solution, is sent into by powder in extraction kettle, through CO2Supercritical extraction, obtains chitin powder.
Wherein, the granularity at step 1 gained oyster shell powder end is at 40 orders；In step 2, compound enzyme is cellulase and protease mass ratio is the mixed enzyme of 2: 1, and soaking temperature is 70 DEG C, and the time is 40min；In step 3, the concentration of NaOH solution is 20wt%, and soaking temperature is 100 DEG C, and the time is 2h；In step 5, extraction temperature is 50 DEG C, and pressure is 20MPa, and flow is 30L/h.
Can preparing chitin 0.05kg in the oyster shell of every 1kg, purity is 96%.
Claims (7)
1. the method for chitin extraction from oyster shell, it is characterised in that: comprise the following steps:
Step 1, takes oyster shell, washes, and pulverizes, obtains oyster shell powder end；
Step 2, with parts by weight, by soaking in 10 parts of end of the step 1 gained oyster shell powder dilute hydrochloric acid solution added to containing 1～4wt% compound enzyme 30～50 parts, filters, and filtering residue obtains demineralization oyster shell powder through washing；
Step 3, with parts by weight, adds to step 2 gained demineralization oyster shell powder 10 parts in NaOH solution 20～30 parts and soaks, regulate the pH to 7.5～8.5 of lixiviating solution with dilute sulfuric acid, be subsequently adding trypsin 3～8 parts, enzymolysis, obtain enzymolysis solution；
Step 4, after step 3 gained enzymolysis solution enzyme denaturing, is filtered with ultrafilter membrane, obtains ultrafiltration permeate, then be filtered by NF membrane, obtain concentrated solution；
Step 5, is undertaken being spray dried to powder by step 5 gained concentrated solution, is sent into by powder in extraction kettle, through CO2Supercritical extraction, obtains chitin powder.
2. the method for chitin extraction from oyster shell according to claim 1, it is characterised in that: the granularity at step 1 gained oyster shell powder end is at 20～40 orders.
3. the method for chitin extraction from oyster shell according to claim 1, it is characterised in that: in step 2, compound enzyme is cellulase and protease mass ratio is the mixed enzyme of 2: 1.
4. the method for chitin extraction from oyster shell according to claim 1, it is characterised in that: in step 2, soaking temperature is 50～70 DEG C, and the time is 20～40min.
5. the method for chitin extraction from oyster shell according to claim 1, it is characterised in that: in step 3, the concentration of NaOH solution is 10～20wt%.
6. the method for chitin extraction from oyster shell according to claim 1, it is characterised in that: in step 3, soaking temperature is 80～100 DEG C, and the time is 2～4h.
7. the method for chitin extraction from oyster shell according to claim 1, it is characterised in that: in step 5, extraction temperature is 40～50 DEG C, and pressure is 20～30MPa, and flow is 15～30L/h.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610110383.7A CN105754015A (en) | 2016-02-29 | 2016-02-29 | Method for extracting chitin from oyster shell |
| PCT/CN2016/107190 WO2017148186A1 (en) | 2016-02-29 | 2016-11-25 | Method for extracting chitin from oyster shells |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610110383.7A CN105754015A (en) | 2016-02-29 | 2016-02-29 | Method for extracting chitin from oyster shell |
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| CN105754015A true CN105754015A (en) | 2016-07-13 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201610110383.7A Pending CN105754015A (en) | 2016-02-29 | 2016-02-29 | Method for extracting chitin from oyster shell |
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| CN (1) | CN105754015A (en) |
| WO (1) | WO2017148186A1 (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106749739A (en) * | 2016-12-29 | 2017-05-31 | 广西还珠海洋生物科技有限公司 | A kind of method that shitosan is extracted from oyster shell |
| WO2017148186A1 (en) * | 2016-02-29 | 2017-09-08 | 苏州市贝克生物科技有限公司 | Method for extracting chitin from oyster shells |
| CN108164620A (en) * | 2018-02-07 | 2018-06-15 | 潢川创伟水产养殖有限公司 | The method of Subcritical water chromotagraphy chitin |
| CN110194811A (en) * | 2019-06-10 | 2019-09-03 | 水恣意(厦门)科技有限公司 | A method of chitin is prepared based on subcritical hydrolysis method |
| CN113073398A (en) * | 2021-04-21 | 2021-07-06 | 爱可比(苏州)新材料有限公司 | Superfine oyster-based fiber and preparation process thereof |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107984844A (en) * | 2017-12-11 | 2018-05-04 | 杭州科能新材料科技有限公司 | A kind of sealed membrane for being applicable in packaging for foodstuff and preparation method thereof |
| CN115232228A (en) * | 2022-08-04 | 2022-10-25 | 中国科学院海洋研究所 | Method for extracting chitin from sea cockroach |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2017148186A1 (en) * | 2016-02-29 | 2017-09-08 | 苏州市贝克生物科技有限公司 | Method for extracting chitin from oyster shells |
| CN106749739A (en) * | 2016-12-29 | 2017-05-31 | 广西还珠海洋生物科技有限公司 | A kind of method that shitosan is extracted from oyster shell |
| CN108164620A (en) * | 2018-02-07 | 2018-06-15 | 潢川创伟水产养殖有限公司 | The method of Subcritical water chromotagraphy chitin |
| CN110194811A (en) * | 2019-06-10 | 2019-09-03 | 水恣意(厦门)科技有限公司 | A method of chitin is prepared based on subcritical hydrolysis method |
| CN113073398A (en) * | 2021-04-21 | 2021-07-06 | 爱可比(苏州)新材料有限公司 | Superfine oyster-based fiber and preparation process thereof |
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| WO2017148186A1 (en) | 2017-09-08 |
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