CN101775080A - Chitosan preparation method - Google Patents
Chitosan preparation method Download PDFInfo
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- CN101775080A CN101775080A CN200910155132A CN200910155132A CN101775080A CN 101775080 A CN101775080 A CN 101775080A CN 200910155132 A CN200910155132 A CN 200910155132A CN 200910155132 A CN200910155132 A CN 200910155132A CN 101775080 A CN101775080 A CN 101775080A
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Abstract
The invention relates to a chitosan preparation method, which is characterized in that the method comprises the following steps: 1) gas explosion swelling: loading chitin raw materials into a gas explosion swelling tank, injecting a gas explosion swelling medium which adopts one kind of materials of water vapor, water, ammonia water and ethanol, instantaneously releasing pressure in the gas explosion swelling tank, and spraying the chitin raw materials into a normal pressure container to obtain fine chitin materials; 2) hydrolysis; 3) filtration; 4) soaking and water washing; 5) filtration; and 6) drying. Compared with the prior art, the invention has the characteristics that the chitin pretreated by a gas explosion swelling method is adopted as raw materials, the raw materials have high chemical activity, and low reaction temperature and short reaction time can be adopted in the hydrolysis process, so the generation of the secondary reaction is inhabited, and the decomposition of the chitosan is avoided. Thereby, the invention has the following advantages: 1) the consumption of alkali and energy sources is little;2) the reaction time is short; 3) the yield is high; 4) the production cost is low; 5) the pollutant discharge is little; and 6) the product quality is stable.
Description
Technical field
The present invention relates to a kind of preparation method of chitosan, particularly relate to the method for a kind of chitin of handling through the expanded method of gas explosion as the feedstock production chitosan.
Background technology
Chitosan, English name chitosan, another name soluble chitin, chitosan, chitosan.Chemical structural formula: B-(1 → 4)-2-deoxidation-D-dextran, molecular formula is: (C
6H
110
4N)
nChitosan is the chitin deacetylase product, and is water insoluble, can be dissolved in diluted acid.Its chemical structure is for being with cationic polymer alkalescence polysaccharide polymer, and has unique physicochemical property and bioactivation function.It is a kind of natural cationic polysaccharide that chitin obtains through deacetylation; have degradability, good film-forming properties, excellent biological compatibility and certain excellent properties such as antibiotic and antitumor, be widely used in industries such as medicine, food, chemical industry, environmental protection.
The preparation method of traditional chitosan technology adopts the method for separating deacetylate with strong lye from the chitin of shrimp, the extraction of crab shell mostly, and its technical process is: chitin-pulverizing-hydrolysis deacetylation-washing-drying-chitosan.The main quality index of chitosan product is deacetylation and viscosity.Because the chitin that extracts from shrimp, crab shell has fine and close crystalline structure, usually adopt breaking method to carry out pre-treatment, such pretreatment process, be difficult to change its fine and close crystalline structure, also be difficult to make it to carry out chemical modification, therefore, hydrolysis reaction has to adopt the alkali of higher concentration, higher temperature of reaction and long reaction times, and produce following shortcoming thus: 1) consumption of the alkali and the energy is big; 2) long reaction time; 3) yield is low; 4) production cost height; 5) pollutant emission is serious; 6) unstable product quality; " chitin chemistry " (Science Press as the Wang Aiqin chief editor, in January, 2008 first version) in pointed, the high alkali liquid method, this is the preparation method of at present the most frequently used chitosan, serves as the principal element that influences chitosan performance (viscosity and deacetylation) with concentration of lye, its alkali purification temp and time three factors.Experimentize by orthogonal experiment method, the result shows: with ground chitin (40 order) with mass ratio be 1: 10 be that 45%～50% NaOH solution mixes with mass percentage concentration, under 90 ℃ of temperature, react 8～10h then.And for example publication number is the Chinese patent " a kind of chitin preparation method and utilize chitin to prepare the method for chitosan " of CN101289518, chitin is 1: 20～25 to be that 40%～45% NaOH solution mixes with mass percentage concentration with mass ratio, 70～80 ℃ of temperature of reaction, per sampling half an hour is once to dissolving fully behind the reaction 8h, wash then, dry, again with obtaining finished product behind 20～25 times the NaOH solution washing.
Summary of the invention
The present invention proposes to adopt a kind of novel process for preparing chitosan, particularly proposes the method for a kind of chitin of handling through the expanded method of gas explosion as the feedstock production chitosan.
A kind of preparation method of chitosan is characterized in that adopting following steps:
1) gas explosion is expanded: chitin raw material is packed in the gas explosion Bulking tank, inject the expanded medium of gas explosion, the expanded medium of gas explosion adopts a kind of in water vapour, water, ammoniacal liquor, the ethanol; When the expanded medium of gas explosion was water vapour, charged pressure was that 0.3～0.5MPa, temperature are 130～150 ℃ water vapour, keeps 5～15min; When the expanded medium of gas explosion was water, the add-on of water was 10%～50% of a chitin raw material weight, was heated to 130～150 ℃, made jar interior corresponding pressure rise to 0.3～0.5MPa, kept 5～15min; When the expanded medium of gas explosion was ammoniacal liquor, the add-on of ammoniacal liquor was 10%～50% of a chitin raw material weight, was heated to 100～150 ℃, made jar interior corresponding pressure rise to 0.3～0.8MPa, kept 5～15min; When the expanded medium of gas explosion was ethanol, amount of alcohol added was 10%～50% of a chitin raw material weight, was heated to 100～150 ℃, made a jar interior relevant pressure rise to 0.3～0.8MPa, kept 5～15min;
Pressure in the moment venting gas explosion Bulking tank, and chitin raw material spurted in the non-pressure vessel, the chitin fine fodder obtained;
2) hydrolysis: the NaOH solution of concentration expressed in percentage by weight 40%～45% is inserted the vacuum reaction still, add the chitin fine fodder, 4～8h is hydrolyzed under 60～70 ℃ of temperature; Concentration expressed in percentage by weight is that the add-on of 40%～45% NaOH solution is 6～10 times of chitin weight;
3) filter: said hydrolyzed liquid is filtered, obtain the chitosan crude product;
4) soak, wash: the chitosan crude product is put into soaks 0.5～1.5h in the water, being washed to the pH value again is 7.2～7.4;
5) filter: the feed liquid after will washing is filtered;
6) drying: above-mentioned filter thing is carried out vacuum-drying, obtain the chitosan finished product.
2. the method for a Preparation of Chitosan is characterized in that adopting following steps:
1) gas explosion is expanded: chitin raw material is packed in the gas explosion Bulking tank, inject the expanded medium of gas explosion, the expanded medium of gas explosion adopts a kind of in water vapour, water, ammoniacal liquor, the ethanol; When the expanded medium of gas explosion was water vapour, charged pressure was that 0.3～0.5MPa, temperature are 130～150 ℃ water vapour, keeps 5～15min; When the expanded medium of gas explosion was water, the add-on of water was 10%～50% of a chitin raw material weight, was heated to 130～150 ℃, made jar interior corresponding pressure rise to 0.3～0.5MPa, kept 5～15min; When the expanded medium of gas explosion was ammoniacal liquor, the add-on of ammoniacal liquor was 10%～50% of a chitin raw material weight, was heated to 100～150 ℃, made jar interior corresponding pressure rise to 0.3～0.8MPa, kept 5～15min; When the expanded medium of gas explosion was ethanol, amount of alcohol added was 10%～50% of a chitin raw material weight, was heated to 100～150 ℃, made a jar interior relevant pressure rise to 0.3～0.8MPa, kept 5～15min;
Charge into N
2Perhaps CO
2Make pressure rise to 1.0～2.5MPa, keep 5～10min;
Pressure in the moment venting gas explosion Bulking tank, and chitin raw material spurted in the non-pressure vessel, the chitin fine fodder obtained;
2) hydrolysis: the NaOH solution of concentration expressed in percentage by weight 40%～45% is inserted the vacuum reaction still, add the chitin fine fodder, 4～8h is hydrolyzed under 60～70 ℃ of temperature; Concentration expressed in percentage by weight is that the add-on of 40%～45% NaOH solution is 6～10 times of chitin weight;
3) filter: said hydrolyzed liquid is filtered, obtain the chitosan crude product;
4) soak, wash: the chitosan crude product is put into soaks 0.5～1.5h in the water, being washed to the pH value again is 7.2～7.4;
5) filter: the feed liquid after will washing is filtered;
6) drying: above-mentioned filter thing is carried out vacuum-drying, obtain the chitosan finished product.
Compared with the prior art, the present invention has adopted through the pretreated chitin of the expanded method of gas explosion as raw material, raw material has higher chemically reactive, the reaction times of in hydrolytic process, can adopt lower temperature of reaction, lacking, thereby suppressed the generation of side reaction, avoided the decomposition of chitosan, so the present invention has following having a few: 1) consumption of the alkali and the energy is few; 2) reaction times is short; 3) yield height; 4) production cost is low; 5) pollutant emission is few; 6) constant product quality.
Embodiment 1:
A kind of preparation method of chitosan is characterized in that adopting following steps:
1) gas explosion is expanded: chitin raw material is packed in the gas explosion Bulking tank, inject the expanded medium of gas explosion, the expanded medium of gas explosion adopts water vapour; Charged pressure is that 0.5MPa, temperature are 150 ℃, keeps 5min; Pressure in the moment venting gas explosion Bulking tank, and chitin raw material spurted in the non-pressure vessel, the chitin fine fodder obtained;
2) hydrolysis: in the chitin weight ratio be 6: 1 ratio, the NaOH solution of concentration expressed in percentage by weight 45% is inserted the vacuum reaction still, add the chitin fine fodder, 4h is hydrolyzed under 70 ℃ of temperature;
3) filter: said hydrolyzed liquid is filtered, obtain the chitosan crude product;
4) soak, wash: the chitosan crude product is put into soaks 1.5h in the water, being washed to the pH value again is 7.2;
5) filter: the feed liquid after will washing is filtered;
6) drying: above-mentioned filter thing is carried out vacuum-drying, obtain the chitosan finished product.
Embodiment 2:
A kind of preparation method of chitosan is characterized in that adopting following steps:
1) gas explosion is expanded: chitin raw material is packed in the gas explosion Bulking tank, inject the expanded medium of gas explosion, the expanded medium of gas explosion adopts water vapour; Charged pressure is that 0.4MPa, temperature are 140 ℃, keeps 10min; Pressure in the moment venting gas explosion Bulking tank, and chitin raw material spurted in the non-pressure vessel, the chitin fine fodder obtained;
2) hydrolysis: in the chitin weight ratio be 8: 1 ratio, the NaOH solution of concentration expressed in percentage by weight 42% is inserted the vacuum reaction still, add the chitin fine fodder, 6h is hydrolyzed under 65 ℃ of temperature;
3) filter: said hydrolyzed liquid is filtered, obtain the chitosan crude product;
4) soak, wash: the chitosan crude product is put into soaks 1.0h in the water, being washed to the pH value again is 7.3;
5) filter: the feed liquid after will washing is filtered;
6) drying: above-mentioned filter thing is carried out vacuum-drying, obtain the chitosan finished product.
Embodiment 3:
A kind of preparation method of chitosan is characterized in that adopting following steps:
1) gas explosion is expanded: chitin raw material is packed in the gas explosion Bulking tank, inject the expanded medium of gas explosion, the expanded medium of gas explosion adopts water vapour; Charged pressure is that 0.3MPa, temperature are 130 ℃, keeps 15min; Pressure in the moment venting gas explosion Bulking tank, and chitin raw material spurted in the non-pressure vessel, the chitin fine fodder obtained;
2) hydrolysis: in the chitin weight ratio be 10: 1 ratio, the NaOH solution of concentration expressed in percentage by weight 40% is inserted the vacuum reaction still, add the chitin fine fodder, 8h is hydrolyzed under 60 ℃ of temperature;
3) filter: said hydrolyzed liquid is filtered, obtain the chitosan crude product;
4) soak, wash: the chitosan crude product is put into soaks 0.5h in the water, being washed to the pH value again is 7.4;
5) filter: the feed liquid after will washing is filtered;
6) drying: above-mentioned filter thing is carried out vacuum-drying, obtain the chitosan finished product.
Embodiment 4:
A kind of preparation method of chitosan is characterized in that adopting following steps:
1) gas explosion is expanded: chitin raw material is packed in the gas explosion Bulking tank, inject the expanded medium of gas explosion, the expanded medium of gas explosion adopts water, and the add-on of water is 50% of a chitin raw material weight, is heated to 150 ℃, and corresponding pressure rises to 0.5MPa in making jar, keeps 5min; Pressure in the moment venting gas explosion Bulking tank, and chitin raw material spurted in the non-pressure vessel, the chitin fine fodder obtained;
2) hydrolysis: in the chitin weight ratio be 6: 1 ratio, the NaOH solution of concentration expressed in percentage by weight 45% is inserted the vacuum reaction still, add the chitin fine fodder, 4h is hydrolyzed under 70 ℃ of temperature;
3) filter: said hydrolyzed liquid is filtered, obtain the chitosan crude product;
4) soak, wash: the chitosan crude product is put into soaks 1.5h in the water, being washed to the pH value again is 7.2;
5) filter: the feed liquid after will washing is filtered;
6) drying: above-mentioned filter thing is carried out vacuum-drying, obtain the chitosan finished product.
Embodiment 5:
A kind of preparation method of chitosan is characterized in that adopting following steps:
1) gas explosion is expanded: chitin raw material is packed in the gas explosion Bulking tank, inject the expanded medium of gas explosion, the expanded medium of gas explosion adopts water, the add-on of water is 30% of a chitin raw material weight, be heated to 140 ℃, make jar interior corresponding pressure rise to 0.4MPa, keep 10min; Pressure in the moment venting gas explosion Bulking tank, and chitin raw material spurted in the non-pressure vessel, the chitin fine fodder obtained;
2) hydrolysis: in the chitin weight ratio be 8: 1 ratio, the NaOH solution of concentration expressed in percentage by weight 42% is inserted the vacuum reaction still, add the chitin fine fodder, 6h is hydrolyzed under 65 ℃ of temperature;
3) filter: said hydrolyzed liquid is filtered, obtain the chitosan crude product;
4) soak, wash: the chitosan crude product is put into soaks 1.0h in the water, being washed to the pH value again is 7.3;
5) filter: the feed liquid after will washing is filtered;
6) drying: above-mentioned filter thing is carried out vacuum-drying, obtain the chitosan finished product.
Embodiment 6:
A kind of preparation method of chitosan is characterized in that adopting following steps:
1) gas explosion is expanded: chitin raw material is packed in the gas explosion Bulking tank, inject the expanded medium of gas explosion, the expanded medium of gas explosion adopts water, the add-on of water is 10% of a chitin raw material weight, be heated to 130 ℃, make jar interior corresponding pressure rise to 0.3MPa, keep 15min; Pressure in the moment venting gas explosion Bulking tank, and chitin raw material spurted in the non-pressure vessel, the chitin fine fodder obtained;
2) hydrolysis: in the chitin weight ratio be 10: 1 ratio, the NaOH solution of concentration expressed in percentage by weight 40% is inserted the vacuum reaction still, add the chitin fine fodder, 8h is hydrolyzed under 60 ℃ of temperature;
3) filter: said hydrolyzed liquid is filtered, obtain the chitosan crude product;
4) soak, wash: the chitosan crude product is put into soaks 0.5h in the water, being washed to the pH value again is 7.4;
5) filter: the feed liquid after will washing is filtered;
6) drying: above-mentioned filter thing is carried out vacuum-drying, obtain the chitosan finished product.
Embodiment 7:
A kind of preparation method of chitosan is characterized in that adopting following steps:
1) gas explosion is expanded: chitin raw material is packed in the gas explosion Bulking tank, inject the expanded medium of gas explosion, the expanded medium of gas explosion adopts ammoniacal liquor, the add-on of ammoniacal liquor is 50% of a chitin raw material weight, be heated to 150 ℃, make jar interior corresponding pressure rise to 0.8MPa, keep 5min; Pressure in the moment venting gas explosion Bulking tank, and chitin raw material spurted in the non-pressure vessel, the chitin fine fodder obtained;
2) hydrolysis: in the chitin weight ratio be 6: 1 ratio, the NaOH solution of concentration expressed in percentage by weight 45% is inserted the vacuum reaction still, add the chitin fine fodder, 4h is hydrolyzed under 70 ℃ of temperature;
3) filter: said hydrolyzed liquid is filtered, obtain the chitosan crude product;
4) soak, wash: the chitosan crude product is put into soaks 1.5h in the water, being washed to the pH value again is 7.2;
5) filter: the feed liquid after will washing is filtered;
6) drying: above-mentioned filter thing is carried out vacuum-drying, obtain the chitosan finished product.
Embodiment 8:
A kind of preparation method of chitosan is characterized in that adopting following steps:
1) gas explosion is expanded: chitin raw material is packed in the gas explosion Bulking tank, inject the expanded medium of gas explosion, the expanded medium of gas explosion adopts ammoniacal liquor, the add-on of ammoniacal liquor is 30% of a chitin raw material weight, be heated to 130 ℃, make jar interior corresponding pressure rise to 0.5MPa, keep 10min; Pressure in the moment venting gas explosion Bulking tank, and chitin raw material spurted in the non-pressure vessel, the chitin fine fodder obtained;
2) hydrolysis: in the chitin weight ratio be 8: 1 ratio, the NaOH solution of concentration expressed in percentage by weight 42% is inserted the vacuum reaction still, add the chitin fine fodder, 6h is hydrolyzed under 65 ℃ of temperature;
3) filter: said hydrolyzed liquid is filtered, obtain the chitosan crude product;
4) soak, wash: the chitosan crude product is put into soaks 1.0h in the water, being washed to the pH value again is 7.3;
5) filter: the feed liquid after will washing is filtered;
6) drying: above-mentioned filter thing is carried out vacuum-drying, obtain the chitosan finished product.
Embodiment 9:
A kind of preparation method of chitosan is characterized in that adopting following steps:
1) gas explosion is expanded: chitin raw material is packed in the gas explosion Bulking tank, inject the expanded medium of gas explosion, the expanded medium of gas explosion adopts ammoniacal liquor, the add-on of ammoniacal liquor is 10% of a chitin raw material weight, be heated to 100 ℃, make jar interior corresponding pressure rise to 0.3MPa, keep 15min; Pressure in the moment venting gas explosion Bulking tank, and chitin raw material spurted in the non-pressure vessel, the chitin fine fodder obtained;
2) hydrolysis: in the chitin weight ratio be 10: 1 ratio, the NaOH solution of concentration expressed in percentage by weight 40% is inserted the vacuum reaction still, add the chitin fine fodder, 8h is hydrolyzed under 60 ℃ of temperature;
3) filter: said hydrolyzed liquid is filtered, obtain the chitosan crude product;
4) soak, wash: the chitosan crude product is put into soaks 0.5h in the water, being washed to the pH value again is 7.4;
5) filter: the feed liquid after will washing is filtered;
6) drying: above-mentioned filter thing is carried out vacuum-drying, obtain the chitosan finished product.
Embodiment 10:
A kind of preparation method of chitosan is characterized in that adopting following steps:
Change the expanded medium of the gas explosion among the embodiment 7 into ethanol by ammoniacal liquor, step and embodiment 7 are identical.
Embodiment 11:
A kind of preparation method of chitosan is characterized in that adopting following steps:
Change the expanded medium of the gas explosion among the embodiment 8 into ethanol by ammoniacal liquor, step and embodiment 8 are identical.
Embodiment 12:
A kind of preparation method of chitosan is characterized in that adopting following steps:
Change the expanded medium of the gas explosion among the embodiment 9 into ethanol by ammoniacal liquor, step and embodiment 9 are identical.
Embodiment 13:
A kind of preparation method of chitosan is characterized in that adopting following steps:
1) gas explosion is expanded: chitin raw material is packed in the gas explosion Bulking tank, inject the expanded medium of gas explosion, the expanded medium of gas explosion adopts water vapour, and charged pressure is that 0.5MPa, temperature are 150 ℃ water vapour, keeps 5min;
Charge into N
2Perhaps CO
2Make pressure rise to 1.0MPa, keep 10min;
Pressure in the moment venting gas explosion Bulking tank, and chitin raw material spurted in the non-pressure vessel, the chitin fine fodder obtained;
2) hydrolysis: in the chitin weight ratio be 6: 1 ratio, the NaOH solution of concentration expressed in percentage by weight 45% is inserted the vacuum reaction still, add the chitin fine fodder, 4h is hydrolyzed under 70 ℃ of temperature;
3) filter: said hydrolyzed liquid is filtered, obtain the chitosan crude product;
4) soak, wash: the chitosan crude product is put into soaks 1.5h in the water, being washed to the pH value again is 7.2;
5) filter: the feed liquid after will washing is filtered;
6) drying: above-mentioned filter thing is carried out vacuum-drying, obtain the chitosan finished product.
Embodiment 14:
A kind of preparation method of chitosan is characterized in that adopting following steps:
1) gas explosion is expanded: chitin raw material is packed in the gas explosion Bulking tank, inject the expanded medium of gas explosion, the expanded medium of gas explosion adopts water vapour, and charged pressure is that 0.4MPa, temperature are 140 ℃ water vapour, keeps 10min;
Charge into N
2Perhaps CO
2Make pressure rise to 1.5MPa, keep 5min;
Pressure in the moment venting gas explosion Bulking tank, and chitin raw material spurted in the non-pressure vessel, the chitin fine fodder obtained;
2) hydrolysis: in the chitin weight ratio be 8: 1 ratio, the NaOH solution of concentration expressed in percentage by weight 42% is inserted the vacuum reaction still, add the chitin fine fodder, 6h is hydrolyzed under 65 ℃ of temperature;
3) filter: said hydrolyzed liquid is filtered, obtain the chitosan crude product;
4) soak, wash: the chitosan crude product is put into soaks 1.0h in the water, being washed to the pH value again is 7.3;
5) filter: the feed liquid after will washing is filtered;
6) drying: above-mentioned filter thing is carried out vacuum-drying, obtain the chitosan finished product.
Embodiment 15:
A kind of preparation method of chitosan is characterized in that adopting following steps:
1) gas explosion is expanded: chitin raw material is packed in the gas explosion Bulking tank, inject the expanded medium of gas explosion, the expanded medium of gas explosion adopts water vapour, and charged pressure is that 0.3MPa, temperature are 130 ℃ water vapour, keeps 15min;
Charge into N
2Perhaps CO
2Make pressure rise to 2.5MPa, keep 5min;
Pressure in the moment venting gas explosion Bulking tank, and chitin raw material spurted in the non-pressure vessel, the chitin fine fodder obtained;
2) hydrolysis: in the chitin weight ratio be 10: 1 ratio, the NaOH solution of concentration expressed in percentage by weight 40% is inserted the vacuum reaction still, add the chitin fine fodder, 8h is hydrolyzed under 60 ℃ of temperature;
3) filter: said hydrolyzed liquid is filtered, obtain the chitosan crude product;
4) soak, wash: the chitosan crude product is put into soaks 0.5h in the water, being washed to the pH value again is 7.4;
5) filter: the feed liquid after will washing is filtered;
6) drying: above-mentioned filter thing is carried out vacuum-drying, obtain the chitosan finished product.
Embodiment 16:
A kind of preparation method of chitosan is characterized in that adopting following steps:
1) gas explosion is expanded: chitin raw material is packed in the gas explosion Bulking tank, inject the expanded medium of gas explosion, the expanded medium of gas explosion adopts water, and the add-on of water is 50% of a chitin raw material weight, is heated to 150 ℃, and corresponding pressure rises to 0.5MPa in making jar, keeps 5min;
Charge into N
2Perhaps CO
2Make pressure rise to 1.0MPa, keep 10min;
Pressure in the moment venting gas explosion Bulking tank, and chitin raw material spurted in the non-pressure vessel, the chitin fine fodder obtained;
2) hydrolysis: in the chitin weight ratio be 6: 1 ratio, the NaOH solution of concentration expressed in percentage by weight 45% is inserted the vacuum reaction still, add the chitin fine fodder, 4h is hydrolyzed under 70 ℃ of temperature;
3) filter: said hydrolyzed liquid is filtered, obtain the chitosan crude product;
4) soak, wash: the chitosan crude product is put into soaks 1.5h in the water, being washed to the pH value again is 7.2;
5) filter: the feed liquid after will washing is filtered;
6) drying: above-mentioned filter thing is carried out vacuum-drying, obtain the chitosan finished product.
Embodiment 17:
A kind of preparation method of chitosan is characterized in that adopting following steps:
1) gas explosion is expanded: chitin raw material is packed in the gas explosion Bulking tank, inject the expanded medium of gas explosion, the expanded medium of gas explosion adopts water, the add-on of water is 30% of a chitin raw material weight, be heated to 140 ℃, make jar interior corresponding pressure rise to 0.4MPa, keep 10min;
Charge into N
2Perhaps CO
2Make pressure rise to 1.5MPa, keep 5min;
Pressure in the moment venting gas explosion Bulking tank, and chitin raw material spurted in the non-pressure vessel, the chitin fine fodder obtained;
2) hydrolysis: in the chitin weight ratio be 8: 1 ratio, the NaOH solution of concentration expressed in percentage by weight 42% is inserted the vacuum reaction still, add the chitin fine fodder, 6h is hydrolyzed under 65 ℃ of temperature;
3) filter: said hydrolyzed liquid is filtered, obtain the chitosan crude product;
4) soak, wash: the chitosan crude product is put into soaks 1.0h in the water, being washed to the pH value again is 7.3;
5) filter: the feed liquid after will washing is filtered;
6) drying: above-mentioned filter thing is carried out vacuum-drying, obtain the chitosan finished product.
Embodiment 18:
A kind of preparation method of chitosan is characterized in that adopting following steps:
1) gas explosion is expanded: chitin raw material is packed in the gas explosion Bulking tank, inject the expanded medium of gas explosion, the expanded medium of gas explosion adopts water, the add-on of water is 10% of a chitin raw material weight, be heated to 130 ℃, make jar interior corresponding pressure rise to 0.3MPa, keep 15min;
Charge into N
2Perhaps CO
2Make pressure rise to 2.5MPa, keep 5min;
Pressure in the moment venting gas explosion Bulking tank, and chitin raw material spurted in the non-pressure vessel, the chitin fine fodder obtained;
2) hydrolysis: in the chitin weight ratio be 10: 1 ratio, the NaOH solution of concentration expressed in percentage by weight 40% is inserted the vacuum reaction still, add the chitin fine fodder, 8h is hydrolyzed under 60 ℃ of temperature;
3) filter: said hydrolyzed liquid is filtered, obtain the chitosan crude product;
4) soak, wash: the chitosan crude product is put into soaks 0.5h in the water, being washed to the pH value again is 7.4;
5) filter: the feed liquid after will washing is filtered;
6) drying: above-mentioned filter thing is carried out vacuum-drying, obtain the chitosan finished product.
Embodiment 19:
A kind of preparation method of chitosan is characterized in that adopting following steps:
1) gas explosion is expanded: chitin raw material is packed in the gas explosion Bulking tank, inject the expanded medium of gas explosion, the expanded medium of gas explosion adopts ammoniacal liquor, the add-on of ammoniacal liquor is 50% of a chitin raw material weight, be heated to 150 ℃, make jar interior corresponding pressure rise to 0.8MPa, keep 5min;
Charge into N
2Perhaps CO
2Make pressure rise to 1.0MPa, keep 10min;
Pressure in the moment venting gas explosion Bulking tank, and chitin raw material spurted in the non-pressure vessel, the chitin fine fodder obtained;
2) hydrolysis: in the chitin weight ratio be 6: 1 ratio, the NaOH solution of concentration expressed in percentage by weight 45% is inserted the vacuum reaction still, add the chitin fine fodder, 4h is hydrolyzed under 70 ℃ of temperature;
3) filter: said hydrolyzed liquid is filtered, obtain the chitosan crude product;
4) soak, wash: the chitosan crude product is put into soaks 1.5h in the water, being washed to the pH value again is 7.2;
5) filter: the feed liquid after will washing is filtered;
6) drying: above-mentioned filter thing is carried out vacuum-drying, obtain the chitosan finished product.
Embodiment 20:
A kind of preparation method of chitosan is characterized in that adopting following steps:
1) gas explosion is expanded: chitin raw material is packed in the gas explosion Bulking tank, inject the expanded medium of gas explosion, the expanded medium of gas explosion adopts ammoniacal liquor, the add-on of ammoniacal liquor is 30% of a chitin raw material weight, be heated to 130 ℃, make jar interior corresponding pressure rise to 0.5MPa, keep 10min;
Charge into N
2Perhaps CO
2Make pressure rise to 1.5MPa, keep 5min;
Pressure in the moment venting gas explosion Bulking tank, and chitin raw material spurted in the non-pressure vessel, the chitin fine fodder obtained;
2) hydrolysis: in the chitin weight ratio be 8: 1 ratio, the NaOH solution of concentration expressed in percentage by weight 42% is inserted the vacuum reaction still, add the chitin fine fodder, 6h is hydrolyzed under 65 ℃ of temperature;
3) filter: said hydrolyzed liquid is filtered, obtain the chitosan crude product;
4) soak, wash: the chitosan crude product is put into soaks 1.0h in the water, being washed to the pH value again is 7.3;
5) filter: the feed liquid after will washing is filtered;
6) drying: above-mentioned filter thing is carried out vacuum-drying, obtain the chitosan finished product.
Embodiment 21:
A kind of preparation method of chitosan is characterized in that adopting following steps:
1) gas explosion is expanded: chitin raw material is packed in the gas explosion Bulking tank, inject the expanded medium of gas explosion, the expanded medium of gas explosion adopts ammoniacal liquor, the add-on of ammoniacal liquor is 10% of a chitin raw material weight, be heated to 100 ℃, make jar interior corresponding pressure rise to 0.3MPa, keep 15min;
Charge into N
2Perhaps CO
2Make pressure rise to 2.5MPa, keep 5min;
Pressure in the moment venting gas explosion Bulking tank, and chitin raw material spurted in the non-pressure vessel, the chitin fine fodder obtained;
2) hydrolysis: in the chitin weight ratio be 10: 1 ratio, the NaOH solution of concentration expressed in percentage by weight 40% is inserted the vacuum reaction still, add the chitin fine fodder, 8h is hydrolyzed under 60 ℃ of temperature;
3) filter: said hydrolyzed liquid is filtered, obtain the chitosan crude product;
4) soak, wash: the chitosan crude product is put into soaks 0.5h in the water, being washed to the pH value again is 7.4;
5) filter: the feed liquid after will washing is filtered;
6) drying: above-mentioned filter thing is carried out vacuum-drying, obtain the chitosan finished product.
Embodiment 22:
A kind of preparation method of chitosan is characterized in that adopting following steps:
1) gas explosion is expanded: chitin raw material is packed in the gas explosion Bulking tank, inject the expanded medium of gas explosion, the expanded medium of gas explosion adopts ethanol, and amount of alcohol added is 50% of a chitin raw material weight, is heated to 150 ℃, makes a jar interior relevant pressure rise to 0.8MPa, keeps 5min;
Charge into N
2Perhaps CO
2Make pressure rise to 1.0MPa, keep 10min;
Pressure in the moment venting gas explosion Bulking tank, and chitin raw material spurted in the non-pressure vessel, the chitin fine fodder obtained;
2) hydrolysis: in the chitin weight ratio be 6: 1 ratio, the NaOH solution of concentration expressed in percentage by weight 45% is inserted the vacuum reaction still, add the chitin fine fodder, 4h is hydrolyzed under 70 ℃ of temperature;
3) filter: said hydrolyzed liquid is filtered, obtain the chitosan crude product;
4) soak, wash: the chitosan crude product is put into soaks 1.5h in the water, being washed to the pH value again is 7.2;
5) filter: the feed liquid after will washing is filtered;
6) drying: above-mentioned filter thing is carried out vacuum-drying, obtain the chitosan finished product.
Embodiment 23:
A kind of preparation method of chitosan is characterized in that adopting following steps:
1) gas explosion is expanded: chitin raw material is packed in the gas explosion Bulking tank, inject the expanded medium of gas explosion, the expanded medium of gas explosion adopts ethanol, amount of alcohol added is 30% of a chitin raw material weight, be heated to 130 ℃, make a jar interior relevant pressure rise to 0.5MPa, keep 10min;
Charge into N
2Perhaps CO
2Make pressure rise to 1.5MPa, keep 5min;
Pressure in the moment venting gas explosion Bulking tank, and chitin raw material spurted in the non-pressure vessel, the chitin fine fodder obtained;
2) hydrolysis: in the chitin weight ratio be 8: 1 ratio, the NaOH solution of concentration expressed in percentage by weight 42% is inserted the vacuum reaction still, add the chitin fine fodder, 6h is hydrolyzed under 65 ℃ of temperature;
3) filter: said hydrolyzed liquid is filtered, obtain the chitosan crude product;
4) soak, wash: the chitosan crude product is put into soaks 1.0h in the water, being washed to the pH value again is 7.3;
5) filter: the feed liquid after will washing is filtered;
6) drying: above-mentioned filter thing is carried out vacuum-drying, obtain the chitosan finished product.
Embodiment 24:
A kind of preparation method of chitosan is characterized in that adopting following steps:
1) gas explosion is expanded: chitin raw material is packed in the gas explosion Bulking tank, inject the expanded medium of gas explosion, the expanded medium of gas explosion adopts ethanol, amount of alcohol added is 10% of a chitin raw material weight, be heated to 100 ℃, make a jar interior relevant pressure rise to 0.3MPa, keep 15min;
Charge into N
2Perhaps CO
2Make pressure rise to 2.5MPa, keep 5min;
Pressure in the moment venting gas explosion Bulking tank, and chitin raw material spurted in the non-pressure vessel, the chitin fine fodder obtained;
2) hydrolysis: in the chitin weight ratio be 10: 1 ratio, the NaOH solution of concentration expressed in percentage by weight 40% is inserted the vacuum reaction still, add the chitin fine fodder, 8h is hydrolyzed under 60 ℃ of temperature;
3) filter: said hydrolyzed liquid is filtered, obtain the chitosan crude product;
4) soak, wash: the chitosan crude product is put into soaks 0.5h in the water, being washed to the pH value again is 7.4;
5) filter: the feed liquid after will washing is filtered;
6) drying: above-mentioned filter thing is carried out vacuum-drying, obtain the chitosan finished product.
Claims (2)
1. the preparation method of a chitosan is characterized in that adopting following steps:
1) gas explosion is expanded: chitin raw material is packed in the gas explosion Bulking tank, inject the expanded medium of gas explosion, the expanded medium of gas explosion adopts a kind of in water vapour, water, ammoniacal liquor, the ethanol; When the expanded medium of gas explosion was water vapour, charged pressure was that 0.3～0.5MPa, temperature are 130～150 ℃ water vapour, keeps 5～15min; When the expanded medium of gas explosion was water, the add-on of water was 10%～50% of a chitin raw material weight, was heated to 130～150 ℃, made jar interior corresponding pressure rise to 0.3～0.5MPa, kept 5～15min; When the expanded medium of gas explosion was ammoniacal liquor, the add-on of ammoniacal liquor was 10%～50% of a chitin raw material weight, was heated to 100～150 ℃, made jar interior corresponding pressure rise to 0.3～0.8MPa, kept 5～15min; When the expanded medium of gas explosion was ethanol, amount of alcohol added was 10%～50% of a chitin raw material weight, was heated to 100～150 ℃, made a jar interior relevant pressure rise to 0.3～0.8MPa, kept 5～15min;
Pressure in the moment venting gas explosion Bulking tank, and chitin raw material spurted in the non-pressure vessel, the chitin fine fodder obtained;
2) hydrolysis: the NaOH solution of concentration expressed in percentage by weight 40%～45% is inserted the vacuum reaction still, add the chitin fine fodder, 4～8h is hydrolyzed under 60～70 ℃ of temperature; Concentration expressed in percentage by weight is that the add-on of 40%～45% NaOH solution is 6～10 times of chitin weight;
3) filter: said hydrolyzed liquid is filtered, obtain the chitosan crude product;
4) soak, wash: the chitosan crude product is put into soaks 0.5～1.5h in the water, being washed to the pH value again is 7.2～7.4;
5) filter: the feed liquid after will washing is filtered;
6) drying: above-mentioned filter thing is carried out vacuum-drying, obtain the chitosan finished product.
2. the method for a Preparation of Chitosan is characterized in that adopting following steps:
1) gas explosion is expanded: chitin raw material is packed in the gas explosion Bulking tank, inject the expanded medium of gas explosion, the expanded medium of gas explosion adopts a kind of in water vapour, water, ammoniacal liquor, the ethanol; When the expanded medium of gas explosion was water vapour, charged pressure was that 0.3～0.5MPa, temperature are 130～150 ℃ water vapour, keeps 5～15min; When the expanded medium of gas explosion was water, the add-on of water was 10%～50% of a chitin raw material weight, was heated to 130～150 ℃, made jar interior corresponding pressure rise to 0.3～0.5MPa, kept 5～15min; When the expanded medium of gas explosion was ammoniacal liquor, the add-on of ammoniacal liquor was 10%～50% of a chitin raw material weight, was heated to 100～150 ℃, made jar interior corresponding pressure rise to 0.3～0.8MPa, kept 5～15min; When the expanded medium of gas explosion was ethanol, amount of alcohol added was 10%～50% of a chitin raw material weight, was heated to 100～150 ℃, made a jar interior relevant pressure rise to 0.3～0.8MPa, kept 5～15min;
Charge into N
2Perhaps CO
2Make pressure rise to 1.0～2.5MPa, keep 5～10min;
Pressure in the moment venting gas explosion Bulking tank, and chitin raw material spurted in the non-pressure vessel, the chitin fine fodder obtained;
2) hydrolysis: the NaOH solution of concentration expressed in percentage by weight 40%～45% is inserted the vacuum reaction still, add the chitin fine fodder, 4～8h is hydrolyzed under 60～70 ℃ of temperature; Concentration expressed in percentage by weight is that the add-on of 40%～45% NaOH solution is 6～10 times of chitin weight;
3) filter: said hydrolyzed liquid is filtered, obtain the chitosan crude product;
4) soak, wash: the chitosan crude product is put into soaks 0.5～1.5h in the water, being washed to the pH value again is 7.2～7.4;
5) filter: the feed liquid after will washing is filtered;
6) drying: above-mentioned filter thing is carried out vacuum-drying, obtain the chitosan finished product.
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|---|---|---|---|
| CN200910155132A CN101775080A (en) | 2009-12-07 | 2009-12-07 | Chitosan preparation method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910155132A CN101775080A (en) | 2009-12-07 | 2009-12-07 | Chitosan preparation method |
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|---|---|
| CN101775080A true CN101775080A (en) | 2010-07-14 |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102816808A (en) * | 2012-07-17 | 2012-12-12 | 肖丽凤 | Method for preparing chitosan by using shrimp shells |
| CN102887964A (en) * | 2011-07-17 | 2013-01-23 | 高邮市明增生物制品厂 | Method for producing high-viscosity chitosan |
| CN102976802A (en) * | 2012-11-23 | 2013-03-20 | 山东嘉丰海洋生物科技有限公司 | Processing method of chitosan fluid fertilizer |
| TWI567089B (en) * | 2015-08-28 | 2017-01-21 | 蔡敏郎 | Method of pretreating crab or shrip shells and method of preparing α-chitin |
| CN107118287A (en) * | 2017-06-04 | 2017-09-01 | 陈泽勇 | A kind of high purity of shell glycan production method |
| CN110387331A (en) * | 2018-04-23 | 2019-10-29 | 广州莱孚高生物科技有限公司 | A kind of ethyl alcohol blasting method, ethyl alcohol demolition set and breaking trachytectum of glossy ganoderma equipment |
-
2009
- 2009-12-07 CN CN200910155132A patent/CN101775080A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102887964A (en) * | 2011-07-17 | 2013-01-23 | 高邮市明增生物制品厂 | Method for producing high-viscosity chitosan |
| CN102816808A (en) * | 2012-07-17 | 2012-12-12 | 肖丽凤 | Method for preparing chitosan by using shrimp shells |
| CN102816808B (en) * | 2012-07-17 | 2014-05-28 | 中山火炬职业技术学院 | Method for preparing chitosan by using shrimp shells |
| CN102976802A (en) * | 2012-11-23 | 2013-03-20 | 山东嘉丰海洋生物科技有限公司 | Processing method of chitosan fluid fertilizer |
| CN102976802B (en) * | 2012-11-23 | 2014-09-03 | 山东嘉丰海洋生物科技有限公司 | Processing method of chitosan fluid fertilizer |
| TWI567089B (en) * | 2015-08-28 | 2017-01-21 | 蔡敏郎 | Method of pretreating crab or shrip shells and method of preparing α-chitin |
| CN107118287A (en) * | 2017-06-04 | 2017-09-01 | 陈泽勇 | A kind of high purity of shell glycan production method |
| CN110387331A (en) * | 2018-04-23 | 2019-10-29 | 广州莱孚高生物科技有限公司 | A kind of ethyl alcohol blasting method, ethyl alcohol demolition set and breaking trachytectum of glossy ganoderma equipment |
| CN110387331B (en) * | 2018-04-23 | 2023-09-19 | 广州莱孚高生物科技有限公司 | Ethanol blasting method, ethanol blasting device and ganoderma lucidum spore wall breaking equipment |
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