CN1178800A - Method for preparing chitosan - Google Patents
Method for preparing chitosan Download PDFInfo
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- CN1178800A CN1178800A CN 96121759 CN96121759A CN1178800A CN 1178800 A CN1178800 A CN 1178800A CN 96121759 CN96121759 CN 96121759 CN 96121759 A CN96121759 A CN 96121759A CN 1178800 A CN1178800 A CN 1178800A
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- shell material
- described method
- naoh solution
- chitin
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Abstract
Chitosan preparation processes include crushing shells, HCl decalcification, removing protein and ester with NaOH, chitin preparation with decoloring potassium permanganate, and product preparation by adding NaOH into chitin under the conditions of heating and pressurizing. The said method produces chitosan from shell as waste, and the product chitosan is used in medicine, chemical and other industry and agriculture.
Description
The present invention relates to a kind of preparation method of chitosan.
There is wide shoreline in China, has every year millions of tons crust to go out of use, and has not only wasted resource, and causes new biological pollution.Some unit fully utilizes and develops crust, can only reach the chitin extraction stage at present, also fails to extract crust chitin quality (chitosan).Chitosan has the reinforced immunological function, and anti-cancer, the development of control cancer cell and anti-ageing in the adsorbent or the effect of external toxin, also have antiacid alkali, effect such as wear-resisting simultaneously, are widely used in aspects such as medicine, industry, chemical industry, military project, environmental protection.Chinese patent 931176.6 discloses a kind of preparation method of chitin, and it comprises the following steps: that raw material is cleaned and pulverizing, and NaoH soaks, potassium permanganate liquid soaks, and uses the oxalic acid demanganization again, uses salt acid soak purifying etc. at last.Its weak point is: the chitin of being produced belongs to intermediate product, can't solve crust chitin quality and extract problem, and technology is complicated, and cost is higher.
It is the method for raw material preparing high purity chitosan with the crust that order of the present invention provides a kind of, and technology is simple, cost is low.
The object of the present invention is achieved like this:
The method for preparing chitosan comprises the following steps:
(1) at first the clean also powder of shell material is fragmentated, soaked 2～6 hours, remove the ore deposit and remove calcium, cross and filter to remove impurity, water washing shell material with an amount of dilute hydrochloric acid; (2) place the sodium hydroxide solution of middle and high concentration to soak 2～8 hours, take out the shell material and wash with water; (3) place potassium permanganate solution to carry out shank color and handle,, with oxalic acid washing shell material, remove manganese then so that the shades of colour of crust is removed; (4) again with in low-concentration ethanol dewater, soak with the sodium hydroxide solution of high density, heating, temperature is controlled at 60～90 ℃, 30～60 minutes time, reaction finishes the back and takes out that to clean intermediate product be chitin (chitin); (5) with low-concentration ethanol processed in the chitin usefulness, soak with high-concentration sodium hydroxide, under 2～4 normal atmosphere, heat 60～90 ℃, the time is 5～7 hours, and taking-up washes product with water and is chitosan.
Repeatedly test through the contriver, the result shows that step (1) mesochite material soaked 3～5 hours with 2～8%HCl, removes the ore deposit and removes calcium, and effect is better, and is best with 4.5 hours effects of 5%HCl immersion.
Step (2) shell material steeped 4～6 hours with 8～16%NaoH, and it is better to remove free protein and fat effect, and as steeping 5 hours with 12%NaoH, effect is best, and isolating protein and fat are complete.
The weight ratio 1～300 of step (3) mesochite material and potassium permanganate solution is carried out the shank color processing, then with 0.2% oxalic acid washing shell material.
Better with 50～60% dewatering of ethanol effects in step (4) and (5), it is best to carry out dehydrating effect with 55% alcohol.As with 70～80 ℃ of 20～23%Naoh heating, 40～50 minutes time, the reaction that is hydrolyzed, effect is best.
Step (5) adds 20～23%NaoH solution with chitin, under 2.5～3.5 normal atmosphere, heats 65～75 ℃, and 5.5～6.5 hours time effect is better, as uses 21.5%NaoH solution, under 2.5 normal atmosphere, heats 70 ℃, and effect was best in 6 hours.
The present invention has following advantage compared to existing technology:
1, make full use of the crust issuance of materials, extract chitosan, comprehensive utilization is turned waste into wealth, fully for industries such as medicine, chemical industry, military project, agricultural, environmental protection provide important source material.
2, waste liquid is few, and recyclable utilization
3, technology is simple, production cost is low, and product purity is up to 97.5%, and application prospect is good.
Embodiment 1:
Get the clean shell 1.5 * 0.5cm of 250g
2Particle, putting into 2%HCl vacuole 2 hours removes the ore deposit and removes calcium, observe no gas discharge in the liquid, take out shell material, washing only, soak 2 hours to remove floating preteins and fat with 8%NaoH, adularescent feels that getting final product appears in the shallow lake thing in the observation solution, behind the separating and filtering, place the 25kg1% potassium permanganate liquid to carry out shank color,, take out the shell material variegated removing in the shell material, with eccysis demanganize in 0.2% oxalic acid, use 50% ethanol dehydration then,, react and took out the clean chitin (chitin) that is of product in 30 minutes again with 60 ℃ of 20%NaoH heating.With chitin 50% ethanol dehydration, under 2 normal atmosphere, heat 60 ℃ with 20%NaoH solution again, reacted 5 hours, take out and be chitosan 8.9g, purity 62.3%.
Embodiment 2:
Get the clean shell 2 * 3cm of 250g
2Particle, putting into 8%HCl vacuole 6 hours removes the ore deposit and removes calcium, soak 7 hours to remove albumen and fat with 16%NaoH, 1% potassium permanganate 8.3kg shank color is handled, variegated removing in the shell material, wash back 60% ethanol dehydration with 0.2% oxalic acid, again with 90 ℃ of 23%NaoH liquid heating, 60 minutes, the taking-up product was a chitin.With chitin 70% ethanol dehydration, under 4 normal atmosphere, heat 80 ℃ with 23%NaoH, reacted 7 hours, take out and be product chitosan 8.75g, purity 68.9%.
Embodiment 3:
Get the clean shell 6.5 * 0.5cm of 250g
2Fragment, putting into 5%HCl vacuole 4.5 hours removes the ore deposit and removes calcium, removed floating preteins and fat in 5 hours with the 12%NaoH bubble, 1% potassium permanganate 12.5kg leg shell the material variegated, with the washing of 0.2% oxalic acid, use 55% ethanol dehydration more then, add 75 ℃ of 21.5%NaoH heating again, 45 minutes, the taking-up product was a chitin.With chitin 55% ethanol dehydration, add 21.5%NaoH solution again, heating is 75 ℃ under 2.5 normal atmosphere, reacts 6 hours, takes out and is the product chitosan, weight 8.64 grams, purity 97.5%.
Claims (7)
1, a kind of is the method for feedstock production chitosan with the shell material, it is characterized in that: comprise the following steps (1) at first with the shell material with an amount of dilute hydrochloric acid bubble 2～6 hours, filter, washing; (2) place the NaoH solution of middle and high concentration to soak 2～8 hours, remove free protein and fat, take out the washing of shell material; (3) put into potassium permanganate solution and carry out the shank color processing, and wash the shell material with oxalic acid; (4) dewatering of ethanol of lower concentration in the usefulness is used the NaoH solution soaking of high density then, and is heated 60～90 ℃, 30～60 minutes, gets chitin; (5) with in the low-concentration ethanol processed, use the NaoH solution soaking of high density again, under 2～4 normal atmosphere, heat 60～80 ℃, 5～7 hours, taking-up water washing after product was a chitosan.
2,, it is characterized in that step (1) shell material steeped 3～5 hours with 2～8%HCl by the described method of claim 1.
3, by the described method of claim 1, it is characterized in that step (2) with 8～16%NaoH bubble 4～6 hours except that free protein and fat.
4,, it is characterized in that in step (4) and the step (5) with 50～60% dewatering of ethanol by the described method of claim 1.
5, by the described method of claim 1, it is characterized in that step (4) joins the shell material in 20～23%NaoH solution, heat 70～80 ℃, 40～50 minutes.
6, by the described method of claim 1, it is characterized in that in the step (5) the gained chitin being added in 20～23%NaoH solution, under 2.5～3.5 normal atmosphere, heat 65～75 ℃, 5.5～6.5 hours.
7, by the described method of claim 1, it is characterized in that the gained chitin is added 21.5%NaoH solution, under 2.5 normal atmosphere, heat 70 ℃, 6 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 96121759 CN1178800A (en) | 1996-10-03 | 1996-10-03 | Method for preparing chitosan |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 96121759 CN1178800A (en) | 1996-10-03 | 1996-10-03 | Method for preparing chitosan |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1178800A true CN1178800A (en) | 1998-04-15 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 96121759 Pending CN1178800A (en) | 1996-10-03 | 1996-10-03 | Method for preparing chitosan |
Country Status (1)
| Country | Link |
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| CN (1) | CN1178800A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102808239A (en) * | 2012-08-24 | 2012-12-05 | 东北林业大学 | Method for preparing chitin nano filaments |
-
1996
- 1996-10-03 CN CN 96121759 patent/CN1178800A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102808239A (en) * | 2012-08-24 | 2012-12-05 | 东北林业大学 | Method for preparing chitin nano filaments |
| CN102808239B (en) * | 2012-08-24 | 2014-04-02 | 东北林业大学 | Method for preparing chitin nano filaments |
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| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |