CN102838477B - Method for preparing high-purity calcium lactate by taking oyster shell as raw material - Google Patents
Method for preparing high-purity calcium lactate by taking oyster shell as raw material Download PDFInfo
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- CN102838477B CN102838477B CN 201210363045 CN201210363045A CN102838477B CN 102838477 B CN102838477 B CN 102838477B CN 201210363045 CN201210363045 CN 201210363045 CN 201210363045 A CN201210363045 A CN 201210363045A CN 102838477 B CN102838477 B CN 102838477B
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Abstract
The invention discloses a method for preparing high-purity calcium lactate by taking oyster shell as raw material. The method comprises the following steps: treating oyster shells through a water-refining method, converting the oyster shell with lactic acid, adding precipitator, flocculant and a decolorizing agent, and crystallizing to obtain high-purity calcium lactate. The obtained calcium lactate has high content, and is white in color, low in heavy metal residue and high in product yield.
Description
Technical field
The present invention relates to a kind of preparation method of calcium lactate, particularly a kind of is the method for feedstock production high-pure lactic acid calcium with the oyster shells.
Background technology
Crassostrea rivularis has another name called big oyster, is one of Qiezhou, Guangxi four big famous and precious marine products, and meat can be eaten raw, also can be processed into dried oyster, oyster sauce.Big oyster oyster meat is the fishery products with very high nutrition and health care function of high protein, lower fat, delicious flavour, and oyster meat protein content surpasses 40%, and is nutritious, and delicious flavour have the title of " marine milk ", also can be used as medicine simultaneously.Big oyster meat is rich in taurine, can promote the human brain development.
In recent years, oyster has become the important marine products economic shellfish output of China and has constantly increased, and is discarded in the refuse tip mostly or fills out the sea as solid waste and account for the oyster shells of its gross weight more than 80%, has become environment one big public hazards.The Chinese medicine oyster is the shell of Ostreidae animal Crassostrea rivularis, long oyster, Dalian Bay Concha Ostreae etc., because wherein the content of calcium carbonate is feedstock production biological calcium paid more and more attention up to about 90% with the oyster shell.But, according to bibliographical information, because how in the form of sheets or the strip form agent structure of shell, internal void is bigger, the connectedness in hole is better, and fluid is easy to be diffused into along the passage of bar shaped the surface of laminated structure, thereby coating interior is led in infiltration, thereby shell possessed the essential characteristic of sorbent material, and the heavy metal in the seawater is had absorption property.Therefore, bivalve (especially mussel and oyster) has very strong accumulation ability to heavy metal, can be used as the biological indicator species of pollution of the sea, and there is positive correlation in its heavy metal of body concentration (especially Pb) with marine environment.At present, the production technique of shell biological calcium is to be raw material with the oyster shell mostly, calcining or do not calcine and directly extract conversion after washing, and the Pb massfraction is up to 3x10 in its product
-5-10x10
-5, be higher than far away that the Pb massfraction is lower than 1.5x10 in the medicinal organism calcium that Bureau of Drugs Supervision promulgates
-5Requirement.And because oyster shell place of production difference, its heavy metal content differs greatly, and causes quality product to can not get good guarantee.Particularly in recent years, because offshore pollution, it is a ubiquitous problem that the biological calcium product lead that is obtained by the oyster shell roasting exceeds standard.
Along with going from strength to strength of oyster culture industry, the oyster shells resource becomes increasingly abundant, and the oyster deep processing is the only way which must be passed that industry enlarges development.At present, the supplementary calcium food of clinical application and calcic type of preparation are a lot, and the shell in the main source Yu Haiyang and bright bone mainly comprise organic calciums such as calcium lactate, calglucon, citrate of lime.Wherein, characteristics such as solubleness height, bioavailability height, mouthfeel are good because calcium lactate has, calcium contents height, Creta Preparata, glue crosslinking agent, solidifying agent be can be widely used in and crisp dose and toothpaste, cigarette quality modifying agent increased, especially as medicine and protective foods, more need highly purified calcium lactate.
In the prior art, make the calcium lactate that meets the pharmacopeia requirement and pass through secondary crystal even repeatedly crystallization more, but loss is too big, every crystallization once loses 10%; With edible lactic acid and the reaction of medicinal calcium lactate, also can make qualified medicinal calcium lactate, but capital is too high.Therefore, develop a kind of method that can effectively reduce oyster shell biological calcium product P b content, the preparation method of technical maturity, simple high-pure lactic acid calcium is the practical problems that needs to be resolved hurrily at present.
Summary of the invention
What the invention provides that a kind of technology is simple, efficient is high is the production method of feedstock production high-pure lactic acid calcium with the oyster shells.
The present invention is achieved through the following technical solutions:
A kind of is the method for feedstock production high-pure lactic acid calcium with the oyster shells, comprises the steps:
A. oyster shells is scrubbed clean, dries, be crushed to granularity with ball mill and get the oyster shells meal at the 80-100 order;
B. with the above-mentioned oyster shells meal that obtains, put in the appropriate vessel, add proper amount of clear water, grind to form pasty state, the water that adds volume again stirs, incline immediately and suspension, carry out repeatedly so repeatedly, impurity that can not suspendible discards, and the suspension that treating repeatedly inclines leaves standstill, post precipitation, inclining top clear water, will drain throw out and be used for following steps;
C. constantly stir in 50-60 ℃ of heating in water bath, slowly add weight in the above-mentioned oyster shell powder that obtains and be the heavy 2.0-2.5 of coarse grist doubly and concentration is the lactic acid solution of 75-85%, total reaction time is 2-5 hour;
D. above-mentioned gained suspension is filtered, add precipitation agent sal epsom in filtrate, add-on is the 0.20-0.25% of filtrate quality, leaves standstill 2-3 hour;
E. will go up step gained suspension and filter, adjusting filtrate pH is 9-10, adding flocculation agent polyacrylamide in the filtrate, and add-on is the 0.0010-0.0015% of filtrate quality, temperature of reaction 80-90 ℃, kept 0.5-1 hour;
F. will go up step gained suspension and filter, add the discoloring agent 30% concentration H that is equivalent to filtrate quality 0.001-0.002%
2O
2, stir, leave standstill crystallization in 12-18 hour, filter;
G. with above-mentioned gained crystallization 95-100 ℃ of drying, namely get white calcium lactate.
The calcium lactate that adopts the inventive method to make, color and luster is pure white, and product purity reaches more than 99%, and heavy metal lead remains in below the 0.1ppm.
Compared with prior art, advantage of the present invention:
1, by to the impurity composition analysis, in technology, add efficient precipitation agent, flocculation agent and discoloring agent, impurity such as protein-based, lipid, starch fine particle are fully removed, guarantee that filtrate is as clear as crystal, primary crystallization just makes product reach the pharmacopeia requirement like this;
2, the present invention only adopts primary crystallization, compares twice or above recrystallization, and the yield of product improves more than 10%, and the whole process time also shortens greatly.
Embodiment
The invention will be further described with embodiment below, but the present invention is not limited to these embodiment.
Embodiment 1:
A kind of is the method for feedstock production high-pure lactic acid calcium with the oyster shells, comprises the steps:
A. oyster shells is scrubbed clean, dries, be crushed to granularity with ball mill and get the oyster shells meal at 80 orders;
B. with the above-mentioned oyster shells meal 1kg that obtains, put in the stainless steel cask, add proper amount of clear water, grind to form pasty state, the water that adds volume again stirs, incline immediately and suspension, carry out repeatedly so repeatedly, impurity that can not suspendible discards, and the suspension that treating repeatedly inclines leaves standstill, post precipitation, inclining top clear water, will drain throw out and be used for following steps;
C. constantly stir in 50 ℃ of heating in water bath, slowly add concentration in the above-mentioned oyster shell powder that obtains and be 75% lactic acid solution 2.5kg, total reaction time is 3 hours;
D. above-mentioned gained suspension is filtered, in filtrate, add precipitation agent sal epsom 6.5g, left standstill 3 hours;
E. will go up step gained suspension and filter, adjusting filtrate pH is 10, adding flocculation agent polyacrylamide 0.03g in the filtrate, temperature of reaction 80-90 ℃, kept 1 hour;
F. will go up step gained suspension and filter, add the discoloring agent 30% concentration H of 0.03g
2O
2, stir, leave standstill crystallization in 18 hours, filter;
G. with above-mentioned gained crystallization 100 ℃ of dryings, namely get purity 99.6%, lead content is the white calcium lactate 1.72kg of 0.05ppm.
Embodiment 2:
A kind of is the method for feedstock production high-pure lactic acid calcium with the oyster shells, comprises the steps:
A. oyster shells is scrubbed clean, dries, be crushed to granularity with ball mill and get the oyster shells meal at 100 orders;
B. with the above-mentioned oyster shells meal 1kg that obtains, put in the stainless steel cask, add proper amount of clear water, grind to form pasty state, the water that adds volume again stirs, incline immediately and suspension, carry out repeatedly so repeatedly, impurity that can not suspendible discards, and the suspension that treating repeatedly inclines leaves standstill, post precipitation, inclining top clear water, will drain throw out and be used for following steps;
C. constantly stir in 60 ℃ of heating in water bath, slowly add concentration in the above-mentioned oyster shell powder that obtains and be 75% lactic acid solution 2.0kg, total reaction time is 5 hours;
D. above-mentioned gained suspension is filtered, in filtrate, add precipitation agent sal epsom 8.25g, left standstill 2 hours;
E. will go up step gained suspension and filter, adjusting filtrate pH is 9, adding flocculation agent polyacrylamide 0.05g in the filtrate, temperature of reaction 80-90 ℃, kept 1 hour;
F. will go up step gained suspension and filter, add the discoloring agent 30% concentration H of 0.06g
2O
2, stir, leave standstill crystallization in 12 hours, filter;
G. with above-mentioned gained crystallization 100 ℃ of dryings, namely get purity 99.7%, lead content is the white calcium lactate 1.75kg of 0.06ppm.
Claims (1)
1. one kind is the method for feedstock production 99% above high-pure lactic acid calcium with the oyster shells, comprises the steps:
A. oyster shells is scrubbed clean, dries, be crushed to granularity with ball mill and get the oyster shells meal at the 80-100 order;
B. with the above-mentioned oyster shells meal that obtains, put in the appropriate vessel, add proper amount of clear water, grind to form pasty state, the water that adds volume again stirs, incline immediately and suspension, carry out repeatedly so repeatedly, impurity that can not suspendible discards, and the suspension that treating repeatedly inclines leaves standstill, post precipitation, inclining top clear water, will drain throw out and be used for following steps;
C. constantly stir in 50-60 ℃ of heating in water bath, slowly add weight in the above-mentioned oyster shell powder that obtains and be the heavy 2.0-2.5 of coarse grist doubly and concentration is the lactic acid solution of 75-85%, total reaction time is 2-5 hour;
D. above-mentioned gained suspension is filtered, add precipitation agent sal epsom in filtrate, add-on is the 0.20-0.25% of filtrate quality, leaves standstill 2-3 hour;
E. will go up step gained suspension and filter, adjusting filtrate pH is 9-10, adding flocculation agent polyacrylamide in the filtrate, and add-on is the 0.0010-0.0015% of filtrate quality, temperature of reaction 80-90 ℃, kept 0.5-1 hour;
F. will go up step gained suspension and filter, add the discoloring agent 30% concentration H that is equivalent to filtrate quality 0.001-0.002%
2O
2, stir, leave standstill crystallization in 12-18 hour, filter;
G. with above-mentioned gained crystallization 95-100 ℃ of drying, namely get white calcium lactate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201210363045 CN102838477B (en) | 2012-09-26 | 2012-09-26 | Method for preparing high-purity calcium lactate by taking oyster shell as raw material |
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|---|---|---|---|
| CN 201210363045 CN102838477B (en) | 2012-09-26 | 2012-09-26 | Method for preparing high-purity calcium lactate by taking oyster shell as raw material |
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| CN102838477A CN102838477A (en) | 2012-12-26 |
| CN102838477B true CN102838477B (en) | 2013-09-18 |
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