CN106478996A - A kind of method and its application for preparing calcium carbonate chitin composite granule with crab shell as raw material - Google Patents
A kind of method and its application for preparing calcium carbonate chitin composite granule with crab shell as raw material Download PDFInfo
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- CN106478996A CN106478996A CN201610820630.2A CN201610820630A CN106478996A CN 106478996 A CN106478996 A CN 106478996A CN 201610820630 A CN201610820630 A CN 201610820630A CN 106478996 A CN106478996 A CN 106478996A
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- 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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- 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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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
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Abstract
The invention discloses a kind of method and its application for preparing calcium carbonate chitin composite granule with crab shell as raw material.Preparation method is as follows：1) the remaining meat in crab shell, roller drying, crushing are removed；2) protein and the fat in powder is removed with 1%～10% alkali lye；3) powder is made to decolourize with the oxidizing agent solution that mass concentration is 0.1%～5%；4) wet grinding, press filtration, roller drying, crush, obtain calcium carbonate chitin composite granule.Raw material sources of the present invention are extensive, process is simple, operating condition is gentle, obtained powder remains the natural composite construction of calcium carbonate chitin in crab shell, combine calcium carbonate and the respective advantage of chitin, size distribution is homogeneous, and whiteness is high, can be used as the filler of plastics and rubber, adsorbent, flocculant, antiseptic, catalyst or tissue engineering material.
Description
Technical field
The present invention relates to crab shell recycling field, more particularly to one kind prepare calcium carbonate-crust with crab shell as raw material
The method of plain composite granule and its application.
Background technology
The main component of crab shell is calcium carbonate, chitin, protein, and the material such as a small amount of pigment and aliphatic acid.Wherein,
Calcium carbonate content is about 50%, protein about 30%, chitin about 20%.Chitin is intermeshed in threadiness in the housing
Random network structure；Protein is combined into proteoglycans with chitin fiber as skeleton with chitin；Calcium carbonate is in cellular
The crystalline texture of porous, is filled in the space between layers that chitin is constituted with protein.
At present, the extraction to the utilization mostly chitin of crab shell, such as patent " technique of chitin extraction from shrimp and crab shells ",
Number of patent application：200910182733；" a kind of preparation method of chitin ", number of patent application：201510978060；" a kind of
The preparation method of shitosan ", number of patent application：201010536585.Such technique fails utilization and accounts for the larger carbon of crab shell proportion
Sour calcium, and substantial amounts of calcic water is produced, increased environmental burden.For the process of calcic water, have plus sodium carbonate or logical dioxy
Change carbon and generate calcium carbonate, such as patent " handling process that a kind of crab and shrimp shell is recycled ", number of patent application：200510029843,
Also calcium citrate, such as patent " a kind of method that produce chitin, calcium citrate and albumen powder ", number of patent application are changed into：
200810159615；" a kind of method that recovery prepares calcium citrate from the calcic process water of production chitin ", patent application
Number：201410035984.Such method can preferably realize the comprehensive utilization of crab shell resource, but operating procedure is complex.
Patent " a kind of biological calcium carbonate chitin and its preparation method and application " number of patent application：201210562471,
The natural composite construction of calcium carbonate-chitin in crab shell is remained, for biological calcium carbonate chitin is prepared, the patent is by repeatedly
The pigment in centrifugation removing crab shell powder and aliphatic acid is boiled, and is removed by multiple sodium hydroxide solution hydrolysis and high speed centrifugation
Protein, obtains biological calcium carbonate chitin through air-flow crushing.
Content of the invention
The purpose of the present invention is shortcoming and the deficiency for overcoming prior art, provides one kind and prepares carbonic acid with crab shell as raw material
The method of calcium-chitin composite granule.
In the method that crab shell prepares calcium carbonate-chitin composite granule as raw material, comprise the following steps：
1) the remaining meat in crab shell, roller drying, crushing are removed；
2) the crab shell powder for obtaining the coarse crushing of 1 mass parts and the mass concentration of 1～10 mass parts are 1%～10%
Alkali lye mixes, and stirs 0.5h～24h in room temperature under conditions of 100 DEG C, removes protein and fat, press filtration, is washed to neutrality；
3) mass concentration for adding 1～10 mass parts toward in powder is 0.1%～5% oxidizing agent solution, in room temperature extremely
0.5h～24h is stirred under conditions of 100 DEG C, so that powder is decolourized, press filtration, it is in colourless to be washed to filtrate, and the high-speed stirred that adds water is obtained
Slip；
4) wet grinding, press filtration, roller drying, crush, obtain calcium carbonate-chitin composite granule.
Technique scheme can also provide some following preferred embodiments：
Step 2) described in alkali be NaOH, potassium hydroxide or calcium hydroxide.
Step 2) in filtrate containing alkali can be repeated for deproteinization and fat 2～3 times.
Step 3) described in oxidant include hydrogen peroxide, potassium permanganate, sodium hypochlorite or calcium hypochlorite.
Step 4) described in wet grinding device include vertical grinding machine, horizontal sand mill, Ball-stirring mill, machine for cutting charge into pieces or ball
Grinding machine.
The crab class includes fresh water crab or sea crab, such as Eriocheir sinensis, Lithodes, Portunus trituberculatus Miers, P.sanguinolentus or remote
Extra large swimming crab etc..
Step 1) in using floatation remove crab shell on remaining meat.
The calcium carbonate that said method is prepared-chitin composite granule can be applicable to filler, the absorption of plastics and rubber
The aspects such as agent, flocculant, antiseptic, catalyst or tissue engineering material.
It is an advantage of the invention that raw material sources are extensively, process is simple, operating condition are gentle, and equipment investment and energy consumption are little, become
This is cheap；The calcium carbonate of preparation-chitin composite granule remains the natural composite construction of calcium carbonate-chitin in crab shell, table
Face functional group enriches, and good surface activity has a extensive future, with good economic and social benefit.
Description of the drawings
Fig. 1 is the X-ray diffractogram of calcium carbonate-chitin composite granule obtained in the embodiment of the present invention 1.
Fig. 2 is the X-ray diffractogram of calcium carbonate-chitin composite granule obtained in the embodiment of the present invention 2.
Fig. 3 is the size distribution curve of calcium carbonate-chitin composite granule obtained in the embodiment of the present invention 1.
Fig. 4 is the size distribution curve of calcium carbonate-chitin composite granule obtained in the embodiment of the present invention 2.
Fig. 5 is the size distribution curve of calcium carbonate-chitin composite granule obtained in the embodiment of the present invention 3.
Fig. 6 is the size distribution curve of calcium carbonate-chitin composite granule obtained in the embodiment of the present invention 4.
Fig. 7 is the appearance of calcium carbonate-chitin composite granule obtained in the embodiment of the present invention 1.
Fig. 8 is the appearance of calcium carbonate-chitin composite granule obtained in the embodiment of the present invention 2.
Fig. 9 is the appearance of calcium carbonate-chitin composite granule obtained in the embodiment of the present invention 3.
Figure 10 is the appearance of calcium carbonate-chitin composite granule obtained in the embodiment of the present invention 4.
Specific embodiment
Embodiment 1：
1) the remaining meat in Eriocheir sinensis crab shell, roller drying, crushing are removed with floatation；Then by powder successively
Carry out subsequent treatment；
2) the crab shell powder for obtaining the coarse crushing of 1 mass parts and the mass concentration of 1 mass parts are 10% NaOH
Solution mixes, and stirs 0.5h at 100 DEG C, removes protein and fat, press filtration, is washed to neutrality；
3) mass concentration for adding 1 mass parts toward in powder is 5% hydrogenperoxide steam generator, stirs 0.5h at 100 DEG C,
Powder is made to decolourize, press filtration, it is in colourless to be washed to filtrate, and the high-speed stirred that adds water is obtained slip；
4) wet grinding in vertical grinding machine is placed in, press filtration, roller drying, crush, obtain calcium carbonate-chitin composite powder
Body.
The diffraction maximum of calcium carbonate and chitin can be seen from the X-ray diffraction in figure of Fig. 1, the size distribution from Fig. 3 is bent
Line can be seen that about 18 μm of the average grain diameter of sample, and size distribution is homogeneous, and the whiteness of sample is higher as seen from Figure 7, decolourize
Effect is good.This method is successfully prepared calcium carbonate-chitin composite granule, and the powder combines the enhancing function of calcium carbonate and first
The toughening functions of shell element, and good with the compatibility of macromolecular material, can be used as the filler of plastics and rubber, improve the machine of material
Tool performance.
Embodiment 2：
1) the remaining meat in Lithodes crab shell, roller drying, crushing are removed with floatation；Then after powder being carried out successively
Continuous process；
2) the crab shell powder for obtaining the coarse crushing of 1 mass parts and the mass concentration of 10 mass parts are 1% potassium hydroxide
Solution mixes, and 24h is stirred at room temperature, and removes protein and fat, press filtration, is washed to neutrality；
3) mass concentration for adding 10 mass parts toward in powder is 0.1% liquor potassic permanganate, is stirred at room temperature
24h, makes powder decolourize, press filtration, and it is in colourless to be washed to filtrate, and the high-speed stirred that adds water is obtained slip；
4) wet grinding in horizontal sand mill is placed in, press filtration, roller drying, crush, obtain calcium carbonate-chitin composite powder
Body.
The diffraction maximum of calcium carbonate and chitin can be seen from the X-ray diffraction in figure of Fig. 2, the size distribution from Fig. 4 is bent
Line can be seen that about 17 μm of the average grain diameter of sample, and size distribution is homogeneous, and the whiteness of sample is higher as seen from Figure 8, decolourize
Effect is good.This method is successfully prepared calcium carbonate-chitin composite granule.Chitin has preferable absorption property, antibiotic property
Energy and histocompatbility, the presence of calcium carbonate increased the density of powder, improve settling property and the intensity of powder, the powder
Can be applicable to the aspects such as adsorbent, flocculant, antiseptic, catalyst and tissue engineering material.
Embodiment 3：
1) the remaining meat in Portunus trituberculatus Miers crab shell, roller drying, crushing are removed with floatation；Then by powder successively
Carry out subsequent treatment；
2) the crab shell powder for obtaining the coarse crushing of 1 mass parts is molten with calcium hydroxide that the mass concentration of 5 mass parts is 5%
Liquid mixes, and stirs 10h at 50 DEG C, removes protein and fat, press filtration, is washed to neutrality；
3) mass concentration for adding 5 mass parts toward in powder is 2% liquor natrii hypochloritis, stirs 10h, make at 50 DEG C
Powder decolourizes, press filtration, and it is in colourless to be washed to filtrate, and the high-speed stirred that adds water is obtained slip；
4) wet grinding in Ball-stirring mill is placed in, press filtration, roller drying, crush, obtain calcium carbonate-chitin composite granule.
About 12 μm of the average grain diameter of sample is can be seen that from the size distribution curve of Fig. 5, and size distribution is homogeneous, can from Fig. 9
To find out the good decolorizing effect of sample, whiteness is higher.This method is successfully prepared calcium carbonate-chitin composite granule, the powder
Combine calcium carbonate and the respective advantage of chitin, can be applicable to the filler of plastics and rubber, adsorbent, flocculant, antiseptic,
The aspect such as catalyst and tissue engineering material.
Embodiment 4：
1) the remaining meat in P.sanguinolentus crab shell, roller drying, crushing are removed with floatation；Then by powder successively
Carry out subsequent treatment；
2) the crab shell powder for obtaining the coarse crushing of 1 mass parts is molten with NaOH that the mass concentration of 2 mass parts is 8%
Liquid mixes, and stirs 8h at 60 DEG C, removes protein and fat, press filtration, is washed to neutrality.
3) mass concentration for adding 2 mass parts toward in powder is 3% calcium hypochlorite solution, stirs 10h, make at 40 DEG C
Powder decolourizes, press filtration, and it is in colourless to be washed to filtrate, and the high-speed stirred that adds water is obtained slip；
4) wet grinding in machine for cutting charge into pieces is placed in, press filtration, roller drying, crush, obtain calcium carbonate-chitin composite granule.
About 13 μm of the average grain diameter of sample is can be seen that from the size distribution curve of Fig. 6, and size distribution is homogeneous, can from Figure 10
To find out the good decolorizing effect of sample, whiteness is higher.This method is successfully prepared calcium carbonate-chitin composite granule, the powder
Combine calcium carbonate and the respective advantage of chitin, can be applicable to the filler of plastics and rubber, adsorbent, flocculant, antiseptic,
The aspect such as catalyst and tissue engineering material.
Embodiment 5：
1) the Portunus pelagicus crab shell washing that reclaims is removed remaining meat, dry, pulverize；Then powder is carried out successively
Subsequent treatment；
2) the crab shell powder for obtaining the coarse crushing of 1 mass parts is molten with NaOH that the mass concentration of 4 mass parts is 4%
Liquid mixes, and stirs 6h at 70 DEG C, removes protein and fat, press filtration, is washed to neutrality；
3) mass concentration for adding 3 mass parts toward in powder is 1% liquor natrii hypochloritis, stirs 6h, make at 60 DEG C
Powder decolourizes, press filtration, and it is in colourless to be washed to filtrate, and the high-speed stirred that adds water is obtained slip；
4) wet grinding in ball mill is placed in, press filtration, roller drying, crush, obtain calcium carbonate-chitin composite granule.
Embodiment described above is one kind preferably scheme of the present invention, and so it is not intended to limiting the invention.Have
The those of ordinary skill for closing technical field, without departing from the spirit and scope of the present invention, can also make various changes
Change and modification.Therefore the technical scheme obtained by all modes for taking equivalent or equivalent transformation, all falls within the guarantor of the present invention
In the range of shield.
Claims (9)
1. a kind of method that calcium carbonate-chitin composite granule is prepared as raw material with crab shell, it is characterised in that including following step
Suddenly：
1) the remaining meat in crab shell, roller drying, crushing are removed；
2) the crab shell powder for obtaining the coarse crushing of 1 mass parts and the mass concentration of 1～10 mass parts are 1%～10% alkali lye
Mixing, stirs 0.5h～24h in room temperature under conditions of 100 DEG C, removes protein and fat, press filtration, is washed to neutrality；
3) mass concentration for adding 1～10 mass parts toward in powder is 0.1%～5% oxidizing agent solution, in room temperature to 100 DEG C
Under conditions of stir 0.5h～24h, so that powder is decolourized, press filtration, be washed to filtrate in colourless, the high-speed stirred that adds water is obtained slip；
4) wet grinding, press filtration, roller drying, crush, obtain calcium carbonate-chitin composite granule.
2. a kind of method that calcium carbonate-chitin composite granule is prepared as raw material with crab shell as claimed in claim 1, its feature
Be, step 2) described in alkali be NaOH, potassium hydroxide or calcium hydroxide.
3. a kind of method that calcium carbonate-chitin composite granule is prepared as raw material with crab shell as claimed in claim 1, its feature
Be, step 2) in filtrate containing alkali can be repeated for deproteinization and fat 2～3 times.
4. a kind of method that calcium carbonate-chitin composite granule is prepared as raw material with crab shell as claimed in claim 1, its feature
Be, step 3) described in oxidant include hydrogen peroxide, potassium permanganate, sodium hypochlorite or calcium hypochlorite.
5. a kind of method that calcium carbonate-chitin composite granule is prepared as raw material with crab shell as claimed in claim 1, its feature
Be, step 4) described in wet grinding device include vertical grinding machine, horizontal sand mill, Ball-stirring mill, machine for cutting charge into pieces or ball milling
Machine.
6. a kind of method that calcium carbonate-chitin composite granule is prepared as raw material with crab shell as claimed in claim 1, its feature
It is, the crab class includes fresh water crab or sea crab.
7. a kind of method that calcium carbonate-chitin composite granule is prepared as raw material with crab shell as claimed in claim 1, its feature
It is, the crab class is Eriocheir sinensis, Lithodes, Portunus trituberculatus Miers, P.sanguinolentus or Portunus pelagicus.
8. a kind of method that calcium carbonate-chitin composite granule is prepared as raw material with crab shell as claimed in claim 1, its feature
Be, step 1) in using floatation remove crab shell on remaining meat.
9. a kind of application of calcium carbonate-chitin composite granule that method as claimed in claim 1 is prepared, as plastics and
The filler of rubber, adsorbent, flocculant, antiseptic, catalyst or tissue engineering material.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107096508A (en) * | 2017-06-28 | 2017-08-29 | 江西省农业科学院土壤肥料与资源环境研究所 | A kind of modification biological crust heavy metal absorbent and preparation method and application |
| CN108083780A (en) * | 2017-12-28 | 2018-05-29 | 海南汉地阳光石油化工有限公司 | A kind of filler porcelain ball and preparation method thereof |
| CN109225156A (en) * | 2018-10-26 | 2019-01-18 | 浙江海洋大学 | A kind of preparation method of the new and effective adsorbent for silver ion recycling |
| CN109529105A (en) * | 2018-10-04 | 2019-03-29 | 南京航空航天大学溧水仿生产业研究院有限公司 | The preparation method of biomimetic artificial bone materials |
| CN109608309A (en) * | 2019-01-23 | 2019-04-12 | 湖北葛店人福药用辅料有限责任公司 | A kind of refining methd of glycerol |
| CN113088045A (en) * | 2021-03-16 | 2021-07-09 | 晋江市新迪新材料科技有限公司 | Shrimp shell-based powder modified fully-degradable composite material |
| 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 |
| CN113402734A (en) * | 2021-06-17 | 2021-09-17 | 东北农业大学 | Preparation method and application of hydrogel for indicating freshness of chilled meat |
| CN116554557A (en) * | 2022-01-30 | 2023-08-08 | 武汉大学 | Preparation method of chitin/chitosan material compounded with natural calcium carbonate |
| CN117945374A (en) * | 2024-01-26 | 2024-04-30 | 浙江大学台州研究院 | Preparation method of novel hydroxyapatite and application of novel hydroxyapatite in heavy metal polluted water restoration |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107096508B (en) * | 2017-06-28 | 2019-12-06 | 江西省农业科学院土壤肥料与资源环境研究所 | Modified biological crusta heavy metal adsorbent and preparation method and application thereof |
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| CN109608309A (en) * | 2019-01-23 | 2019-04-12 | 湖北葛店人福药用辅料有限责任公司 | A kind of refining methd of glycerol |
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| 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 |
| CN113088045B (en) * | 2021-03-16 | 2023-03-10 | 晋江市新迪新材料科技有限公司 | Shrimp shell-based powder modified fully-degradable composite material |
| CN113402734A (en) * | 2021-06-17 | 2021-09-17 | 东北农业大学 | Preparation method and application of hydrogel for indicating freshness of chilled meat |
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