CN102617755A - Simple and easy process for preparing chitosan by utilizing shrimp shells or processed residues of shrimp shells - Google Patents
Simple and easy process for preparing chitosan by utilizing shrimp shells or processed residues of shrimp shells Download PDFInfo
- Publication number
- CN102617755A CN102617755A CN2012101166522A CN201210116652A CN102617755A CN 102617755 A CN102617755 A CN 102617755A CN 2012101166522 A CN2012101166522 A CN 2012101166522A CN 201210116652 A CN201210116652 A CN 201210116652A CN 102617755 A CN102617755 A CN 102617755A
- Authority
- CN
- China
- Prior art keywords
- shrimp shell
- chitosan
- shrimp
- shrimp shells
- described method
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Polysaccharides And Polysaccharide Derivatives (AREA)
- Meat, Egg Or Seafood Products (AREA)
Abstract
The invention relates to a process for preparing chitosan. Shrimp shells or processed residues of the shrimp shells are adopted as raw materials. The process is simple, the total preparation time is short, the energy consumption is low, the sodium hydroxide wastewater is less compared with a traditional process, the cost is low, and a product can be applied to the fields such as food, medicine, biology, cosmetics.
Description
Technical field
The present invention relates to the preparation method of chitosan, is the technology of feedstock production high-quality chitosan with biological raw materials such as shrimp shell, shrimp shell process residues particularly.
Background technology
Chitin (Chitin) formal name used at school β-(1,4)-2-ethanamide-2-deoxy-D-glucose has another name called chitin, Regitex FA, crab shell chitosan etc., and it is the linear polymer that N-acetyl-D-glycamine couples together with β-1,4 glycosidic link.Molecular formula is [C
8H
13NO
5]
n, the acetamido deacetylate on chitosan (Chitosan) chitin forms, and molecular formula is [C
6H
11NO
4]
nChitin extensively is present in the lower animal, like shrimp shell, insect shell etc., is a kind of reproducible abundant natural resource, and the annual biosynthetic crust of nature is nearly 10,000,000,000 tons according to estimates, is one of organism the abundantest on the earth.Chitin, chitosan are owing to have good film-forming properties, biocompatibility and to the special performances such as chelating of heavy metal, be widely used in fields such as weaving, papermaking, food environmental protection, medicine, agricultural, forestry, light industry, biotechnology.
At present; Chitin on the market and chitosan product all derive from shrimp, crab shell basically; With shrimp, crab shell is that feedstock production chitosan technology is to heat with certain density caustic soda soln to remove protein, soaks with Hydrogen chloride to remove mineral substance, handles obtaining chitin again through decolouring.Chitin at high temperature reacts deacetylate with concentrated base, obtains being dissolved in the chitosan of diluted acid.The whole machining process process need be carried out a s.t. at least, twice alkaline purification, and the consumption that can consume a large amount of soda acids, particularly alkali is very big, and the industrial chemicals cost is high, has also increased the cost of wastewater treatment.
Summary of the invention
The purpose of this invention is to provide a kind of simple and easy technology of from shrimp shell, shrimp shell process residues, extracting the preparation chitosan, preparation time is short, and the consumption of chemical is few, and the chitosan mass that obtains simultaneously is high.For addressing this problem, adopt following technical scheme.
1. sample pretreatment.
The pretreatment mainly is that sample is cleaned and crush, and removes impurity, becomes the homogeneous sample, to help fully reacting completely of subsequent experimental, mainly comprises following several kinds of processing modes to different samples:
(1) new fresh shrimp shell: after the cleaning of shrimp shell, be crushed to the 50-150 order;
(2) dried shrimp shell: directly dried shrimp shell meal is broken to the 50-200 order;
(3) shrimp shell process residues: will prepare the sample behind the materials such as extracting shrimp essence, protein, calcium, astaxanthin, clear water washing back oven dry is for use, and not pulverize early stage, need be crushed to the 50-200 order after the oven dry.
2. the technology of shrimp shell and shrimp shell process residues mineral is removed in the salt s.t..
Hydrochloric acid can become soluble salt with mineral elements such as calcium, through removing by filter.In the shrimp shell meal after 1 part of above-mentioned processing (weight ratio), add heavy 2%-10% (weight percent concentration) hydrochloric acid soln of 10-50 part, stir; 40-80 ℃ of water-bath 30 ~ 120min, soaking at room temperature 12-48 hour, after immersion finishes; Suction filtration, filter residue clean to pH neutral.
3. alkaline purification removes Deproteinization, fat and deacetylated technology.
In the filter residue after 1 part of above-mentioned processing (weight ratio), add heavy 20%-60% (weight percent concentration) sodium hydroxide solution of 5-40 part, extraction temperature is from 40 ℃ to 100 ℃; Time 2-8 hour, during stir 5 ~ 10 times, then with the alkali lye elimination; Centrifugal, wash to pH neutral.Deposition is deacetylation more than 90% through 40 ℃ of-105 ℃ of oven dry, and ash oontent is lower than 0.5% high-quality chitosan.
Embodiment
Residue prepared chitosan after embodiment 1 usefulness shrimp shell prepared the smart spices of shrimp.Get oven dry back residue 100g, be crushed to 100 orders, add the 1mol/L hydrochloric acid of 10 times of weight, 70 ℃ of waters bath with thermostatic control 1 hour, soaking at room temperature is 48 hours then, shakes therebetween 10 times, and suction filtration, and washing then is to neutral; Again deposition is joined in 400ml 45% sodium hydroxide solution, 100 ℃ of water-baths 4 hours, centrifuge washing will precipitate oven dry to neutral repeatedly, obtain the 16.02g chitosan, the warp detection, the chitosan deacetylation reaches more than 94%, and ash content is 0.19%.
The dried shrimp shell of embodiment 2 usefulness prepares chitosan.Get oven dry back shrimp shell 100g, be crushed to 100 orders, add the 1mol/L hydrochloric acid of 10 times of weight, 80 ℃ of waters bath with thermostatic control 0.5 hour, soaking at room temperature is 24 hours then, shakes therebetween 5 times, and suction filtration, and washing then is to neutral; Again deposition is joined in 400ml 50% sodium hydroxide solution, 80 ℃ of water-baths 6 hours, centrifuge washing will precipitate oven dry to neutral repeatedly, obtain the 17.02g chitosan, the warp detection, the chitosan deacetylation is more than 93%, and ash content is 0.18%.
The new fresh shrimp shell of embodiment 3 usefulness prepares chitosan.Get clean new fresh shrimp shell 100g, be crushed to 50 orders, add the 1mol/L hydrochloric acid of 10 times of weight, 60 ℃ of water-baths 2 hours, soaking at room temperature is 24 hours then, shakes therebetween 5 times, and suction filtration, and washing then is to neutral; Again deposition is joined in 400ml 50% sodium hydroxide solution, 60 ℃ of water-baths 7 hours, centrifuge washing will precipitate oven dry to neutral repeatedly, obtain the 3.65g chitosan, the warp detection, chitosan deacetylation 91%, ash content are 0.21%.
Residue prepared chitosan after embodiment 4 usefulness shrimp heads prepared the high-calcium nutrient material.Get oven dry back residue 100g, be crushed to 100 orders, 45% sodium hydroxide that adds 10 times of weight mixed 80 ℃ of water-baths after 6 hours, and centrifuge washing will precipitate oven dry to neutral repeatedly, obtain the 20.38g chitosan, and through detecting, chitosan deacetylation 94%, ash content are 0.25%.
Claims (5)
1. simple and easy method for preparing chitosan is characterized in that: adopt sample pretreatment, salt s.t., three steps of sodium-hydroxide treatment can obtain deacetylation more than 90%, ash oontent is lower than 0.5% high-quality chitosan.
2. the described method of claim 1 is characterized in that: the raw material that is used to prepare chitosan is shrimp shell or shrimp shell process residues.
3. the described method of claim 1 is characterized in that, the sample pretreatment step refers to several kinds of processing modes below the different samples employing:
(1) new fresh shrimp shell: after the cleaning of shrimp shell, be crushed to the 50-150 order;
(2) dried shrimp shell: directly dried shrimp shell meal is broken to the 50-200 order;
(3) shrimp shell process residues: will extract the shrimp shell process residues behind shrimp essence, protein, calcium, the astaxanthin, clear water washing back oven dry is crushed to the 50-200 order.
4. the described method of claim 1 is characterized in that, the salt acid treatment step refers in the shrimp shell meal (weight ratio) after 1 part of above-mentioned processing; Add heavy 2%-10% (weight percent concentration) hydrochloric acid soln of 10-50 part, stir 40-80 ℃ of water-bath 30 ~ 120min; Soaking at room temperature 12-48 hour; After immersion finished, suction filtration, filter residue cleaned to pH neutral.
5. the described method of claim 1 is characterized in that, the sodium-hydroxide treatment step refers in the filter residue (weight ratio) after 1 part of above-mentioned processing; Add heavy 20%-60% (weight percent concentration) sodium hydroxide solution of 5-40 part, extraction temperature is from 40 ℃ to 100 ℃, time 2-8 hour; Stir during this time 5 ~ 10 times; With the alkali lye elimination, centrifugal then, wash to pH neutral; Deposition is deacetylation more than 90% through 40 ℃ of-105 ℃ of oven dry, and ash oontent is lower than 0.5% high-quality chitosan.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012101166522A CN102617755A (en) | 2012-04-20 | 2012-04-20 | Simple and easy process for preparing chitosan by utilizing shrimp shells or processed residues of shrimp shells |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012101166522A CN102617755A (en) | 2012-04-20 | 2012-04-20 | Simple and easy process for preparing chitosan by utilizing shrimp shells or processed residues of shrimp shells |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102617755A true CN102617755A (en) | 2012-08-01 |
Family
ID=46557999
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2012101166522A Pending CN102617755A (en) | 2012-04-20 | 2012-04-20 | Simple and easy process for preparing chitosan by utilizing shrimp shells or processed residues of shrimp shells |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102617755A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105750298A (en) * | 2016-02-29 | 2016-07-13 | 武汉大学 | Preparation method of shrimp shell powder |
| CN105875820A (en) * | 2016-04-12 | 2016-08-24 | 鞍山禾瑞生物科技有限公司 | Liquid compound biological preservative and preparation method and application thereof |
| CN113085319A (en) * | 2021-03-16 | 2021-07-09 | 晋江市新迪新材料科技有限公司 | Full-biodegradable composite material for tableware and tableware using same |
| CN114437249A (en) * | 2022-02-21 | 2022-05-06 | 龙岩学院 | Method for extracting chitosan from shrimp and crab shells in one step |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1592756A (en) * | 2001-08-02 | 2005-03-09 | 先进生物高分子聚合物公司 | Chitosan preparation |
-
2012
- 2012-04-20 CN CN2012101166522A patent/CN102617755A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1592756A (en) * | 2001-08-02 | 2005-03-09 | 先进生物高分子聚合物公司 | Chitosan preparation |
Non-Patent Citations (1)
| Title |
|---|
| 钱丹等: "制备脱乙酰甲壳素的研究", 《福州大学学报（自然科学版）》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105750298A (en) * | 2016-02-29 | 2016-07-13 | 武汉大学 | Preparation method of shrimp shell powder |
| CN105875820A (en) * | 2016-04-12 | 2016-08-24 | 鞍山禾瑞生物科技有限公司 | Liquid compound biological preservative and preparation method and application thereof |
| CN113085319A (en) * | 2021-03-16 | 2021-07-09 | 晋江市新迪新材料科技有限公司 | Full-biodegradable composite material for tableware and tableware using same |
| CN114437249A (en) * | 2022-02-21 | 2022-05-06 | 龙岩学院 | Method for extracting chitosan from shrimp and crab shells in one step |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CA2313836C (en) | Chitosan and method of preparing chitosan | |
| Brück et al. | Chitin and chitosan from marine organisms | |
| CN101289518B (en) | Method for preparing chitin and process for preparing chitosan by using chitin | |
| CN104788584B (en) | Novel process for cleanly producing chitosan and carboxymethyl chitosan by using crustacean raw materials | |
| CN101851300B (en) | Process for extracting chondroitin sulfate | |
| JP2014522240A (en) | Extraction of chitin in a single process using enzymatic hydrolysis in acidic media | |
| CN109628525A (en) | A kind of technique that enzymatic hydrolysis chitin prepares N-acetylglucosamine | |
| WO2017148186A1 (en) | Method for extracting chitin from oyster shells | |
| CN102617755A (en) | Simple and easy process for preparing chitosan by utilizing shrimp shells or processed residues of shrimp shells | |
| CN106749764A (en) | The method that a kind of step of quaternary ammonium salt ionic liquid one prepares chitin in shrimp and crab shells | |
| CN102732592A (en) | Method for preparing freshwater fish bone gelatin by enzyme process | |
| CN108752499A (en) | A method of separating-purifying can obtain right polysaccharide from microbial fermentation solution | |
| CN102702384A (en) | Method for removing proteins in chitin material | |
| CN101538335B (en) | Method for extracting chitosan from waste erdin mycelium generated from itaconic acid prepared by fermentation method | |
| CN105463040A (en) | Method for raising yield of xylooligosaccharide | |
| CN103665187A (en) | Preparation method for chitosan | |
| CN104262507A (en) | Method for preparing lobster shell chitosan through cooperation of ultrasonic wave and CDA (Chitin Deacetylase) | |
| CN114014952A (en) | Method for preparing chitosan by catalyzing shrimp and crab shells through hydrothermal method | |
| CN110724211B (en) | High-value comprehensive utilization method of shrimp and crab shells based on reducing sugar catalytic oxidation and application thereof | |
| CN113150186A (en) | Method for utilizing complete components of shrimp and crab shells | |
| CN106832057A (en) | A kind of preparation method of low polymerization degree chitin | |
| CN104892795B (en) | A kind of chitosan and alga fertilizer combine production method | |
| CN108250461A (en) | A kind of preparation method for the chitosan microball for being used to adsorb saxitoxin | |
| CN101659711B (en) | Technology for extracting chitin from shrimp and crab shells | |
| KR101206855B1 (en) | Method For Obtaining Chitin And Chitosan |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20120801 |