CN104877043A - Method of extracting chitin in crab shell powder - Google Patents
Method of extracting chitin in crab shell powder Download PDFInfo
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- CN104877043A CN104877043A CN201510321183.1A CN201510321183A CN104877043A CN 104877043 A CN104877043 A CN 104877043A CN 201510321183 A CN201510321183 A CN 201510321183A CN 104877043 A CN104877043 A CN 104877043A
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Abstract
The invention discloses a method of extracting chitin in crab shell powder. The method comprises the steps of processing the crab shell powder with acetic acid, desorbing parts of ash contents which are easily removed, processing filter residues with hydrochloric acid, removing the rest of inorganic matter ash contents, and finally desorbing proteins with sodium hydroxide. Under the technical condition, the inorganic salt and the protein can be desorbed to obtain either the chitin or chitosan with higher purity. According to the method of extracting chitin in crab shell powder provided by the invention, the reaction time can be reduced, and the production efficiency can be improved; furthermore, the solubility and filterability of raw materials can be greatly improved.
Description
Technical field
The present invention relates to a kind of method of chitin extraction, be specifically related to a kind of novel process of chitin extraction from crab shell powder.
Background technology
Chitin is the straight-chain polysaccharide connect by β-(Isosorbide-5-Nitrae) glycosidic link by N-ethanoyl-D-glucosamine, is insoluble to rare acid, alkali, if boiled altogether with acid, hydrolysis produces acetic acid and D-Glucose amine.Chitin easily obtains, renewable, chitin is extensively present in the shell of crustacean, the cell wallss etc. of fungi such as lower plant mushroom, shrimp, crab, insect, be second the abundantest, be only second to cellulosic natural polymer, torpescence on chitin chemistry, do not change with body fluid, to can not organizing foreign body reaction, nontoxic, there is antithrombotic, the feature such as high temperature-resistant disinfected, but because of the hydrogen bond action that its intramolecule is very strong, solvability is very low, and range of application is restricted.At present, chitin mainly still extracts from the shrimp, crab shell of industrial waste.The chitin in crust, protein and inorganic substance are separated, and finally decolour again, obtain pure chitin, if remove ethanoyl through concentrated base process namely obtain chitosan.Its technical process is: shrimp and crab shells-washing-acidleach (6%HCl)-soda boiling (10%NaOH)-decolouring (KMnO
4)-drying-chitin finished product.The preparation process of chitin forms primarily of simple acid-alkali treatment technique, technical difficulty is little, but it is not high to there is solubleness with the chitin that this traditional technique is obtained, and solution filterableness is poor, the consumption of hydrochloric acid and sodium hydroxide is large, the shortcomings such as long reaction time.
Summary of the invention
It is not high that the chitin obtained to solve traditional technique also exists solubleness, and solution filterableness is poor, and the consumption of hydrochloric acid and sodium hydroxide is large, and the shortcomings such as long reaction time, propose a kind of method of chitin extraction from crab shell powder.
The present invention adopts following technical scheme as follows:
A method for chitin extraction from crab shell powder, described method comprises the steps:
(1) acetic acid acidolysis: get crab shell powder and put into container, and add acetum, solid-liquid ratio is 1: 1 ~ 1: 10, puts into water-bath and reacts 1-10h, obtain solution after mixing;
(2) once filter: the solution after acetic acid acidolysis in step (1) is filtered, and with distilled water cleaning, obtain filter residue;
(3) hydrochloric acidolysis: obtain adding in hydrochloric acid soln in filter residue by step (2), solid-liquid ratio is 1: 1 ~ 1: 10, puts into water-bath and reacts 1-10h, obtain solution after mixing;
(4) secondary filtration: the solution after hydrochloric acidolysis in step (3) is carried out secondary filtration, and with distilled water cleaning, obtain filter residue;
(5) sodium hydroxide deproteinated: put in container by obtaining filter residue in step (4), add sodium hydroxide solution, solid-liquid ratio is 1: 1 ~ 1: 10, puts into pressure kettle compressive reaction 1-10h, obtain solution after mixing;
(6) final filtration: the solution be obtained by reacting in step (5) is filtered, and with distilled water cleaning, obtain filter residue;
(7) dry, finished product: the filter residue after filtration in step (6) is put into loft drier and carries out drying, obtain chitin.
Further, the weight of described step (1) crab shell powder is 3 ~ 15g, adds 3 ~ 150ml, concentration is the acetum of 1-10mol/L, and the temperature of water-bath is 25 ~ 80 DEG C.
Further, described step (3) adds 3 ~ 150ml, concentration is 0.1 ~ 1.0mol/L hydrochloric acid soln, and the temperature of water-bath is 25 ~ 80 DEG C.
Further, add 3 ~ 150ml in step (5), concentration is the sodium hydroxide solution of 0.1 ~ 1.0mol/L, pressure kettle temperature is 80 ~ 120 DEG C.
Further, described container is triangular flask.
Further, the drying temperature of step (7) is 80 ~ 120 DEG C.
The present invention has following beneficial effect:
Compared with prior art, advantage of the present invention is: compared with traditional technology, and consumption and the reaction times of hydrochloric acid and sodium hydroxide greatly reduce, and acidolysis is divided into two steps, first carry out acidolysis with acetic acid, the consumption of hydrochloric acid greatly reduces, waste liquid more easily processes, and economizes on resources.And the reaction times reduces, improve production efficiency.The solvability of raw material and filterableness have larger improvement.
Embodiment
Below in conjunction with embodiment, the present invention is described further:
A method for chitin extraction from crab shell powder, described method comprises the steps:
(1) acetic acid acidolysis: get crab shell powder and put into container, and add acetum, solid-liquid ratio is 1: 1 ~ 1: 10, puts into water-bath and reacts 1-10h, obtain solution after mixing;
(2) once filter: the solution after acetic acid acidolysis in step (1) is filtered, and with distilled water cleaning, obtain filter residue;
(3) hydrochloric acidolysis: obtain adding in hydrochloric acid soln in filter residue by step (2), solid-liquid ratio is 1: 1 ~ 1: 10, puts into water-bath and reacts 1-10h, obtain solution after mixing;
(4) secondary filtration: the solution after hydrochloric acidolysis in step (3) is carried out secondary filtration, and with distilled water cleaning, obtain filter residue;
(5) sodium hydroxide deproteinated: put in container by obtaining filter residue in step (4), add sodium hydroxide solution, solid-liquid ratio is 1: 1 ~ 1: 10, puts into pressure kettle compressive reaction 1-10h, obtain solution after mixing;
(6) final filtration: the solution be obtained by reacting in step (5) is filtered, and with distilled water cleaning, obtain filter residue;
(7) dry, finished product: the filter residue after filtration in step (6) is put into loft drier and carries out drying, obtain chitin.
The weight of described step (1) crab shell powder is 3 ~ 15g, adds 3 ~ 150ml, concentration is the acetum of 1-10mol/L, and the temperature of water-bath is 25 ~ 80 DEG C.
Described step (3) adds 3 ~ 150ml, concentration is 0.1 ~ 1.0mol/L hydrochloric acid soln, and the temperature of water-bath is 25 ~ 80 DEG C.
Add 3 ~ 150ml in step (5), concentration is the sodium hydroxide solution of 0.1 ~ 1.0mol/L, pressure kettle temperature is 80 ~ 120 DEG C.
Described container is triangular flask.
The drying temperature of step (7) is 80 ~ 120 DEG C.
Embodiment 1
(1) acetic acid acidolysis: first-selection gets the triangular flask that 3g crab shell powder puts into 150ml, and add 3ml, concentration is 1mol/L acetum, the water-bath putting into 25 DEG C after mixing reacts 1h, obtains solution;
(2) once filter: the solution after acetic acid acidolysis in step (1) is filtered, and with distilled water cleaning, obtain filter residue;
(3) hydrochloric acidolysis: will to obtain in step (2) in filter residue and add 3ml, concentration is in 0.1mol/L hydrochloric acid soln, the water-bath putting into 25 DEG C after mixing reacts 1h, obtains solution;
(4) secondary filtration: the solution after hydrochloric acidolysis in step (3) is carried out secondary filtration, and with distilled water cleaning, obtain filter residue;
(5) sodium hydroxide deproteinated: put in 150ml triangular flask by obtaining filter residue in step (4), add 3ml, concentration is the sodium hydroxide solution of 0.1mol/L, put into the pressure kettle compressive reaction 1h of 80 DEG C after mixing, obtain solution;
(6) final filtration: the solution be obtained by reacting in step (5) is filtered, and with distilled water cleaning, obtain filter residue;
(7) dry, finished product: the filter residue after filtration in step (6) is put into loft drier and carries out drying, temperature is 80 DEG C, obtains chitin.
Embodiment 2
(1) acetic acid acidolysis: first-selection gets the triangular flask that 9g crab shell powder puts into 150ml, and add 76ml, concentration is 5.5mol/L acetum, the water-bath putting into 52.5 DEG C after mixing reacts 5.5h, obtains solution;
(2) once filter: the solution after acetic acid acidolysis in step (1) is filtered, and with distilled water cleaning, obtain filter residue;
(3) hydrochloric acidolysis: will to obtain in step (2) in filter residue and add 76ml, concentration is in 0.55mol/L hydrochloric acid soln, the water-bath putting into 52.5 DEG C after mixing reacts 5.5h, obtains solution;
(4) secondary filtration: the solution after hydrochloric acidolysis in step (3) is carried out secondary filtration, and with distilled water cleaning, obtain filter residue;
(5) sodium hydroxide deproteinated: put in 150ml triangular flask by obtaining filter residue in step (4), add 76ml, concentration is the sodium hydroxide solution of 0.55mol/L, put into the pressure kettle compressive reaction 5.5h of 100 DEG C after mixing, obtain solution;
(6) final filtration: the solution be obtained by reacting in step (5) is filtered, and with distilled water cleaning, obtain filter residue;
(7) dry, finished product: the filter residue after filtration in step (6) is put into loft drier and carries out drying, temperature is 100 DEG C, obtains chitin.
Embodiment 3
(1) acetic acid acidolysis: first-selection gets the triangular flask that 15g crab shell powder puts into 150ml, and add 150ml, concentration is 10mol/L acetum, the water-bath putting into 80 DEG C after mixing reacts 10h, obtains solution;
(2) once filter: the solution after acetic acid acidolysis in step (1) is filtered, and with distilled water cleaning, obtain filter residue;
(3) hydrochloric acidolysis: will to obtain in step (2) in filter residue and add 150ml, concentration is in 1.0mol/L hydrochloric acid soln, the water-bath putting into 80 DEG C after mixing reacts 10h, obtains solution;
(4) secondary filtration: the solution after hydrochloric acidolysis in step (3) is carried out secondary filtration, and with distilled water cleaning, obtain filter residue;
(5) sodium hydroxide deproteinated: put in 150ml triangular flask by obtaining filter residue in step (4), add 76ml, concentration is the sodium hydroxide solution of 1.0mol/L, put into the pressure kettle compressive reaction 10h of 120 DEG C after mixing, obtain solution;
(6) final filtration: the solution be obtained by reacting in step (5) is filtered, and with distilled water cleaning, obtain filter residue;
(7) dry, finished product: the filter residue after filtration in step (6) is put into loft drier and carries out drying, temperature is 120 DEG C, obtains chitin.
The above; be only the specific embodiment of the present invention, but protection scope of the present invention is not limited thereto, is anyly familiar with those skilled in the art in the technical scope that the present invention discloses; change can be expected easily or replace, all should be encompassed within protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection domain of described claim.
Claims (6)
1. the method for chitin extraction from crab shell powder, is characterized in that: described method comprises the steps:
(1) acetic acid acidolysis: get crab shell powder and put into container, and add acetum, solid-liquid ratio is 1: 1 ~ 1: 10, puts into water-bath and reacts 1-10h, obtain solution after mixing;
(2) once filter: the solution after acetic acid acidolysis in step (1) is filtered, and with distilled water cleaning, obtain filter residue;
(3) hydrochloric acidolysis: obtain adding in hydrochloric acid soln in filter residue by step (2), solid-liquid ratio is 1: 1 ~ 1: 10, puts into water-bath and reacts 1-10h, obtain solution after mixing;
(4) secondary filtration: the solution after hydrochloric acidolysis in step (3) is carried out secondary filtration, and with distilled water cleaning, obtain filter residue;
(5) sodium hydroxide deproteinated: put in container by obtaining filter residue in step (4), add sodium hydroxide solution, solid-liquid ratio is 1: 1 ~ 1: 10, puts into pressure kettle compressive reaction 1-10h, obtain solution after mixing;
(6) final filtration: the solution be obtained by reacting in step (5) is filtered, and with distilled water cleaning, obtain filter residue;
(7) dry, finished product: the filter residue after filtration in step (6) is put into loft drier and carries out drying, obtain chitin.
2. the method for a kind of chitin extraction from crab shell powder according to claim 1, it is characterized in that: the weight of described step (1) crab shell powder is 3 ~ 15g, add 3 ~ 150ml, concentration is the acetum of 1-10mol/L, the temperature of water-bath is 25 ~ 80 DEG C.
3. the method for a kind of chitin extraction from crab shell powder according to claim 1, is characterized in that: described step (3) adds 3 ~ 150ml, concentration is 0.1 ~ 1.0mol/L hydrochloric acid soln, and the temperature of water-bath is 25 ~ 80 DEG C.
4. the method for a kind of chitin extraction from crab shell powder according to claim 1, is characterized in that: add 3 ~ 150ml in step (5), concentration is the sodium hydroxide solution of 0.1 ~ 1.0mol/L, pressure kettle temperature is 80 ~ 120 DEG C.
5. the method for a kind of chitin extraction from crab shell powder according to claim 1, is characterized in that: described container is triangular flask.
6. the method for a kind of chitin extraction from crab shell powder according to claim 1, is characterized in that: the drying temperature of step (7) is 80 ~ 120 DEG C.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108864323A (en) * | 2018-06-09 | 2018-11-23 | 浙江亿丰海洋生物制品有限公司 | The extraction process of chitin in a kind of shrimp shell slag |
| CN109053930A (en) * | 2018-09-06 | 2018-12-21 | 黄河三角洲京博化工研究院有限公司 | A kind of technique preparing chitin and coproduction organic calcium fertilizer |
| CN110944761A (en) * | 2017-05-30 | 2020-03-31 | 新加坡国立大学 | Method for treating crustal waste |
| CN112920291A (en) * | 2021-04-07 | 2021-06-08 | 上海海洋大学 | Squid sector bone beta-chitosan and preparation method and application thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS57139101A (en) * | 1981-02-24 | 1982-08-27 | Unitika Ltd | Chitin powder and its production |
| CN101289518A (en) * | 2008-06-06 | 2008-10-22 | 石勇 | Method for preparing chitin and process for preparing chitosan by using chitin |
| CN104558241A (en) * | 2013-10-17 | 2015-04-29 | 李文金 | Processing technology for producing chitin from crab shells |
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2015
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS57139101A (en) * | 1981-02-24 | 1982-08-27 | Unitika Ltd | Chitin powder and its production |
| CN101289518A (en) * | 2008-06-06 | 2008-10-22 | 石勇 | Method for preparing chitin and process for preparing chitosan by using chitin |
| CN104558241A (en) * | 2013-10-17 | 2015-04-29 | 李文金 | Processing technology for producing chitin from crab shells |
Non-Patent Citations (1)
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| 陈耀华主编: "《人类健康的金钥匙——壳寡糖（第1版）》", 31 August 2008, 中国医药科技出版社 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110944761A (en) * | 2017-05-30 | 2020-03-31 | 新加坡国立大学 | Method for treating crustal waste |
| CN108864323A (en) * | 2018-06-09 | 2018-11-23 | 浙江亿丰海洋生物制品有限公司 | The extraction process of chitin in a kind of shrimp shell slag |
| CN109053930A (en) * | 2018-09-06 | 2018-12-21 | 黄河三角洲京博化工研究院有限公司 | A kind of technique preparing chitin and coproduction organic calcium fertilizer |
| CN112920291A (en) * | 2021-04-07 | 2021-06-08 | 上海海洋大学 | Squid sector bone beta-chitosan and preparation method and application thereof |
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