CN101348431B - Method for producing low lead light density granular calcium citrate - Google Patents
Method for producing low lead light density granular calcium citrate Download PDFInfo
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- CN101348431B CN101348431B CN 200710044067 CN200710044067A CN101348431B CN 101348431 B CN101348431 B CN 101348431B CN 200710044067 CN200710044067 CN 200710044067 CN 200710044067 A CN200710044067 A CN 200710044067A CN 101348431 B CN101348431 B CN 101348431B
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Abstract
The invention relates to a method for manufacturing low-lead low-density granular calcium citrate. The process is characterized in that after a heavy calcium carbonate raw material is converted into soluble calcium chloride, insoluble impurities in calcium carbonate are filtered out completely; because the commonly used quicklime method can not separate the insoluble impurities, and the impurities are brought in a final product, the method adopts a step during which dilute acetic acid solution is added to effectively control the content of lead; moreover, the obtained calcium citrate has higher purity; and a final step prevents the generation of dust during production, and ensures that stacking density of particles is less than 0.6g/cc. Moreover, the quality of the calcium citrate productprepared by the process reaches and exceeds the standards in United States Pharmacopeia USP29-NF24 and U.S. food additive FCC5.
Description
Technical field
The present invention relates to a kind of method of producing low lead light density granular calcium citrate.
Background technology
At present, the method for the production citrate of lime of related documents data introduction has two operational paths at home: 1, utilize ordinary student lime and edible citric acid to produce; 2, utilize the electrode method to produce active citrate of lime.The patent disclosure of China Patent Publication No.: CN1066443 a kind of method with ordinary student lime and the medicinal citrate of lime of edible citric acid high-purity, because medicinal and edible citrate of lime has special specification requirement, lead content＜0.25ppm, tap density＜0.6g/cc, need to carry out granulation to it for the manufacture of calcium tablet, the citrate of lime dry product does not possess viscosity, lead content＜the 1ppm that can only control in order to upper method, tap density＜0.65g/cc can not well reach the granulation effect.
Summary of the invention
The present invention is directed to above production shortcoming, a kind of processing method of new production citrate of lime is provided, it utilizes calcite in powder and technical hydrochloric acid reaction to generate calcium chloride, after making highly purified calcium carbonate by the reaction of calcium chloride and bicarbonate of ammonia, produce citrate of lime with edible citric acid again, its reaction principle is:
CaCO
3+HCl→CaCl
2+CO
2↑+H
2O，
CaCl
2+NH
3HCO
3→CaCO
3+NH
4Cl，
CaCO
3+C
6H
8O
7→Ca
3(C
6H
5O
7)
2+CO
2↑+H
2O。
In the citrate of lime of producing, add dilute acetic acid solution, the control lead amount, it utilizes reaction principle to be:
pb
2++C
2H
5COO→Pb(C
2H
5COO)
2，
pb
4++C
2H
5COO→pb(C
2H
5COO)
4。
Again with the heating deionized water to citrate of lime crystallization wash
The W-Gum of last adding 2% in the crystallization of 100Kg citrate of lime stirs, and reaches needed granularity and density by tablets press.
The characteristics of this technique are after the water-ground limestone raw material is become the calcium chloride of solubility, completely that impurity filter insoluble in the calcium carbonate is cleaner, can not separate insoluble impurity with common unslaked lime method, and impurity is brought in the final product, add the dilute acetic acid solution step and can effectively control lead amount, the citrate of lime purity that obtains is higher, and final step produces dust in having prevented from producing, and has solved packing density of particle＜0.6g/cc.The citrate of lime quality product that this technique is produced meets and exceeds the standard of American Pharmacopeia USP29-NF24 and U.S. food additive FCC5.
Embodiment
The technical characterictic that the present invention produces the method technique of low lead light density granular calcium citrate is:
A, produce calcium chloride solution, cross and filter out impurity, namely by following weight ratio:
Calcium carbonate (heavy): 30% hydrochloric acid: water=1:(2～3): 8 make calcium chloride solution after fully reacting, and filter clarification.
B, the calcium chloride solution (calcium chloride content accounts for 40%) that makes and bicarbonate of ammonia are reacted, bicarbonate of ammonia dissolves first before the reaction, then carry out replacement(metathesis)reaction according to following weight ratio, calcium chloride: bicarbonate of ammonia=1:(1～2), obtained calcium carbonate (having the part Calcium hydrogen carbonate to generate) is through dehydration, washing, drying, cooling, sub-sieve makes material A.
C, with above-mentioned material A and edible citric acid and water according to following weight ratio, material A: edible citric acid: water=1:(1～2): 8, be mixed with solution and carry out chemical reaction, temperature of reaction is controlled between 70～100 ℃, reaction soln pH value 〉=7.
D, control lead amount:
In calcium carbonate and citric acid and finish, reheat and stirred 15 minutes, add the dilute acetic acid solution of configuration 20% in reactor, the dilute acetic acid solution that adds 30ml by every 100Kg output, stirred 15～20 minutes, and then with the deionized water of heating to citrate of lime crystallization wash to without acetic acid smell.
The making of e, light density particle
Because citrate of lime does not possess viscosity; we adopt W-Gum as tackiness agent; add 2% W-Gum adds according to the citrate of lime of every 100Kg dry product; with warm water W-Gum is made pasty state first; stir evenly with stirrer again; by granulator granulation, reach needed granularity and density.
Embodiment:
1, produce calcium chloride solution, cross and filter out impurity, namely by following weight ratio:
Calcium carbonate (heavy): 30% hydrochloric acid: water=1:2.45:8 makes calcium chloride solution after fully reacting, and filters clarification.
2, the calcium chloride solution (calcium chloride content accounts for 40%) that makes is reacted with ammonium hydrogencarbonate, ammonium hydrogencarbonate dissolves first before the reaction, then carry out replacement(metathesis)reaction according to following weight ratio, calcium chloride: ammonium hydrogencarbonate=1:1.55, obtained calcium carbonate (having the part Calcium hydrogen carbonate to generate) is through dehydration, washing, drying, cooling, sub-sieve makes material A.
3, with above-mentioned material A and edible citric acid and water according to following weight ratio, material A: edible citric acid: water=1:1.3:8 is mixed with solution and carries out chemical reaction, temperature of reaction is controlled between 70～100 ℃, reaction soln pH value 〉=7.
4, control lead amount:
In calcium carbonate and citric acid and finish, reheat and stirred 15 minutes, add the dilute acetic acid solution of configuration 20% in reactor, the dilute acetic acid solution that adds 30ml by every 100Kg output, stirred 15～20 minutes, and then with the deionized water of heating to citrate of lime crystallization wash to without acetic acid smell.
5, the making of light density particle
Because citrate of lime does not possess viscosity; we adopt W-Gum as tackiness agent; add 2% W-Gum adds according to the citrate of lime of every 100Kg dry product; with warm water W-Gum is made pasty state first; stir evenly with stirrer again; by granulator granulation, reach needed granularity and density.
The products obtained therefrom quality index is:
Citrate of lime content: 97.5～100.5%,
Heavy metal:＜0.001%,
Plumbous:＜0.000025%,
Hydrochloric acid insoluble substance content:＜0.01%,
Arsenic content:＜0.0002%,
Fluorochemical:＜0.0030%,
Granularity: (arbitrarily 10-80 purpose range),
Tap density: 0.45～0.55g/cc.
Claims (1)
1. method of producing low lead light density granular calcium citrate is characterized in that:
A, produce calcium chloride solution, cross and filter out impurity, namely by following weight ratio: water-ground limestone: 30% hydrochloric acid: water=1: (2～3): 8 make calcium chloride solution after fully reacting, and filter, and clarify;
B, calcium chloride solution and the bicarbonate of ammonia that makes is reacted, bicarbonate of ammonia dissolves first before the reaction, then carry out replacement(metathesis)reaction according to following weight ratio, calcium chloride: bicarbonate of ammonia=1: (1～2), obtained calcium carbonate is through dehydration, washing, drying, cooling, sub-sieve makes material A;
C, with above-mentioned material A and edible citric acid and water according to following weight ratio, material A: edible citric acid: water=1: (1～2): 8, be mixed with solution and carry out chemical reaction, temperature of reaction is controlled between 70～100 ℃, reacting solution pH value 〉=7;
D, control lead amount: in calcium carbonate and citric acid and the end, reheat and stirred 15 minutes, add the dilute acetic acid solution of configuration 20% in reactor, the dilute acetic acid solution that adds 30ml by every 100Kg output, stirred 15～20 minutes, and then with the deionized water of heating to citrate of lime crystallization wash to without acetic acid smell;
The making of e, light density particle: because citrate of lime does not possess viscosity; adopt W-Gum as tackiness agent; add 2% W-Gum adds according to the citrate of lime of every 100Kg dry product; with warm water W-Gum is made pasty state first; stir evenly the citrate of lime that adds W-Gum with stirrer again; by granulator granulation, reach needed granularity and density.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200710044067 CN101348431B (en) | 2007-07-20 | 2007-07-20 | Method for producing low lead light density granular calcium citrate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200710044067 CN101348431B (en) | 2007-07-20 | 2007-07-20 | Method for producing low lead light density granular calcium citrate |
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| Publication Number | Publication Date |
|---|---|
| CN101348431A CN101348431A (en) | 2009-01-21 |
| CN101348431B true CN101348431B (en) | 2013-03-27 |
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|---|---|---|---|
| CN 200710044067 Active CN101348431B (en) | 2007-07-20 | 2007-07-20 | Method for producing low lead light density granular calcium citrate |
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102181288B (en) * | 2011-03-08 | 2013-08-07 | 营口市荣兴达科技实业有限公司 | Method for preparing fluorescent powder from leftovers obtained by producing organosilicon |
| CN102351688A (en) * | 2011-08-16 | 2012-02-15 | 山东恒通生物科技有限公司 | Preparation method of high soluble crystal calcium citrate |
| CN102557920B (en) * | 2011-12-22 | 2014-08-20 | 日照金禾博源生化有限公司 | Process for producing calcium citrate |
| CN102895916A (en) * | 2012-11-07 | 2013-01-30 | 如皋市江北添加剂有限公司 | Production process for calcium citrate granules |
| CN102875363A (en) * | 2012-11-07 | 2013-01-16 | 如皋市江北添加剂有限公司 | Production technology of low-lead calcium citrate |
| CN104326902B (en) * | 2014-10-20 | 2016-08-17 | 南通市飞宇精细化学品有限公司 | A kind of production technology of manganese citrate granule |
| CN106146290A (en) * | 2015-04-02 | 2016-11-23 | 中粮生物化学（安徽）股份有限公司 | A kind of method producing calcium citrate salts |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB597936A (en) * | 1943-11-08 | 1948-02-06 | Miles Lab | Improvements in or relating to the manufacture of mono-calcium citrate dihydrate |
| CN1066443A (en) * | 1992-06-25 | 1992-11-25 | 上海川沙恒大商行 | Produce the method for high purity medical citrate of lime with ordinary student lime and edible citric acid |
-
2007
- 2007-07-20 CN CN 200710044067 patent/CN101348431B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB597936A (en) * | 1943-11-08 | 1948-02-06 | Miles Lab | Improvements in or relating to the manufacture of mono-calcium citrate dihydrate |
| CN1066443A (en) * | 1992-06-25 | 1992-11-25 | 上海川沙恒大商行 | Produce the method for high purity medical citrate of lime with ordinary student lime and edible citric acid |
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|---|---|
| CN101348431A (en) | 2009-01-21 |
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Address after: 226000 Zhao Dianju, Ping Chao Town, Tongzhou District, Nantong, Jiangsu Patentee after: Nantong Feiyu Food Technology Co., Ltd. Address before: 226300 Pingdian village, Pingdong Town, Tongzhou, Jiangsu Patentee before: Nantong Feiyu Fine Chemical Co., Ltd. |