CN105418407B - A kind of production technology of soluble calcium citrate trihydrate - Google Patents
A kind of production technology of soluble calcium citrate trihydrate Download PDFInfo
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- CN105418407B CN105418407B CN201511003767.0A CN201511003767A CN105418407B CN 105418407 B CN105418407 B CN 105418407B CN 201511003767 A CN201511003767 A CN 201511003767A CN 105418407 B CN105418407 B CN 105418407B
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- calcium
- calcium citrate
- citric acid
- citrate trihydrate
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/41—Preparation of salts of carboxylic acids
- C07C51/412—Preparation of salts of carboxylic acids by conversion of the acids, their salts, esters or anhydrides with the same carboxylic acid part
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- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention mainly relates to a kind of production technology of soluble calcium citrate trihydrate, main technique includes：Food-grade citric acid, calcium carbonate and purified water react to obtain soluble three citric acid monohydrate calcium under certain condition, then filter, wash, drying and packaging obtains soluble three citric acid monohydrate calcium finished products.The soluble calcium citrate trihydrate that the present invention is prepared at normal temperatures, reduces industrial energy consumption, practical.Calcium citrate trihydrate prepared by the present invention is more easy to by human body and animal absorption, and can be used as calcium citrate injection and calcium citrate oral liquid, and its application substantially exceeds the calcium citrate of indissoluble.
Description
Technical field
The invention belongs to producing for the citrate in biochemical industry medicine food field, and in particular to a kind of three water of solubility
The production technology of calcium citrate.
Background technology
Calcium is the fifth-largest element in human body, and it is all played a very important role to many physiology courses in human body.People
99% is calcium in the tooth and bone of class.Therefore, either the calcium deficiency of trophism or metabolic can all have pole to the health of human body
Wide negative effect.At present, in the market calcium supplementing product such as calcium chloride, calcium carbonate, calcium phosphate, calcium acetate, calcium gluconate, lactic acid
Calcium etc., a certain degree of disadvantage all be present.
Calcium is basic element needed by human, presently commercially available calcium citrate, although its dissolubility is higher than inorganic calcium
Some are also accordingly improved so as to absorption of the human body to calcium, but calcium citrate is still fallen within that solubility is small, organic calcium of indissoluble, human body
Absorption to calcium receives certain limitation.Therefore it is bigger to prepare solubility for research and development one kind, it is easier to the water of solubility three of absorption
Calcium citrate is the most important thing.
The content of the invention
The invention provides a kind of production technology of soluble calcium citrate trihydrate, it is intended to improves traditional calcium citrate dissolving
The shortcomings that spending small, difficult absorption, a kind of new production Technology is developed under normal temperature.
To achieve the above object, the technical solution used in the present invention is as follows：
A kind of production technology of soluble calcium citrate trihydrate, specifically producing its step is：
（1）Calcium carbonate is sized mixing with purified water；
（2）Food-grade citric acid is dissolved with purified water, obtains food-grade citric acid solution；
（3）Calcium carbonate after sizing mixing is continuously added into constant temperature in food-grade citric acid solution to stir, when pH value is 4.0-5.1
Reach reaction end, generate three citric acid monohydrate calcium；
（4）Reaction finishes, and carries out separation of solid and liquid, obtains calcium citrate trihydrate solid；
（5）The calcium citrate trihydrate isolated is dried to obtain soluble calcium citrate trihydrate finished product；
Wherein, step（1）Mass fraction is 60%-80% after described calcium carbonate is sized mixing；
Step（2）Content after described food-grade citric acid dissolving is 1.10-1.40g/ml water；
Step（3）Described in reaction temperature control at 25 DEG C, speed of agitator 40-60rpm, reaction time 40-60
Minute.
Mass fraction after calcium carbonate is sized mixing directly affects the generation of soluble calcium citrate trihydrate, too high to cause to flow
Property is very poor, too low to influence step（3）The generation of middle soluble calcium citrate trihydrate, therefore the mass fraction of calcium carbonate is 60-
80%。
In the course of reaction for generating calcium citrate, the too high levels of food-grade citric acid, dissolution time is long, is consumed
Quantity of steam is big；Food-grade citric acid content is too low, water loss increase, yield reduction, cost increase, so food-grade should be controlled
Citric acid content is in 1.10-1.40g/ml water.
Reaction time is long, increases production cost；Reaction time is too short, and reaction is not thorough.
Speed of agitator is slow, and material mixing is uneven, and reaction is not thorough, and the reaction time extends；Speed of agitator is too high and can shape
Into tiny particle, increase difficulty in filtration, the impurity brought into also accordingly increases.
Endpoint pH is too high, and calcium carbonate embedding is serious, and finished product pH value and carbonate are unqualified；PH value is too low, and the three of generation
Water citric acid calcium is not easy saturated crystallization.
After completion of the reaction, separation of solid and liquid is carried out using continuous crystallisation centrifugal separation technology, the calcium salt isolated enters steam
Dryer is dried.
Beneficial effects of the present invention：The soluble calcium citrate trihydrate that the present invention is prepared at normal temperatures, reduces work
Industry energy consumption, it is practical.Calcium citrate trihydrate white crystalline powder prepared by the present invention, it is odorless, slightly hygroscopicity, dissolve in
Water, it is practically insoluble in ethanol.Molecular formula Ca3(C6H5O7)2·3H2O, molecular weight：552.52 content 98.0-100.5（With Ca3
(C6H5O7)2Meter, arsenic（As）0.0003%, fluoride≤0.003%, heavy metal（In terms of Pb）≤ 0.002%, loss on drying 8.0%-
12.0%, acid non-soluble substance≤0.2%, solubility is 8.2 times of prior art calcium citrate, and it contains readily soluble calcium, be more easy to by human body and
Animal absorbs, and can be used as calcium citrate injection and calcium citrate oral liquid, and its application substantially exceeds the citric acid of indissoluble
Calcium.
Embodiment：
Embodiment 1
A kind of production technology of soluble calcium citrate trihydrate, its step are：
（1）Calcium carbonate is sized mixing with purified water, it is 60% to size mixing to mass fraction；
（2）Food-grade citric acid is dissolved with purified water, the content of food-grade citric acid is 1.10g/ml in solution
Water；
（3）Calcium carbonate after sizing mixing is continuously added in excessive food-grade citric acid solution, be stirred at a constant temperature
Reaction, speed of agitator 40rpm, reaches reaction end, pH value 4.0 after 40 minutes reaction time；
（4）Separation of solid and liquid is carried out using continuous crystallisation centrifugal separation technology after completion of the reaction；
（5）The calcium citrate trihydrate isolated is subjected to drying by steam drying machine and obtains finished product, calcium citrate trihydrate
Content be 98.
Embodiment 2
A kind of production technology of soluble calcium citrate trihydrate, its step are：
（1）Calcium carbonate is sized mixing with purified water, it is 70% to size mixing to mass fraction；
（2）Food-grade citric acid is dissolved with purified water, the content of food-grade citric acid is 1.20g/ml in solution
Water；
（3）Calcium carbonate after sizing mixing is continuously added in excessive food-grade citric acid solution, be stirred at a constant temperature
Reaction, speed of agitator 50rpm, reaches reaction end, pH value 4.5 after 50 minutes reaction time；
（4）Separation of solid and liquid is carried out using continuous crystallisation centrifugal separation technology after completion of the reaction；
（5）The calcium citrate trihydrate isolated is subjected to drying by steam drying machine and obtains finished product, calcium citrate trihydrate
Content be 99.3.
Embodiment 3
A kind of production technology of soluble calcium citrate trihydrate, its step are：
（1）Calcium carbonate is sized mixing with purified water, it is 80% to size mixing to mass fraction；
（2）Food-grade citric acid is dissolved with purified water, the content of food-grade citric acid is 1.40g/ml in solution
Water；
（3）Calcium carbonate after sizing mixing is continuously added in excessive food-grade citric acid solution, be stirred at a constant temperature
Reaction, speed of agitator 60rpm, reaches reaction end, pH value 5.1 after 60 minutes reaction time；
（4）Separation of solid and liquid is carried out using continuous crystallisation centrifugal separation technology after completion of the reaction；
（5）The calcium citrate trihydrate isolated is subjected to drying by steam drying machine and obtains finished product, calcium citrate trihydrate
Content be 100.5.
Claims (1)
- A kind of 1. production technology of soluble calcium citrate trihydrate, it is characterised in that：Specifically producing its step is：(1) calcium carbonate is sized mixing with purified water；(2) food-grade citric acid is dissolved with purified water, obtains food-grade citric acid solution；(3) calcium carbonate after sizing mixing is continuously added into constant temperature in food-grade citric acid solution to stir, pH value reaches when being 4.0-5.1 Reaction end, generate three citric acid monohydrate calcium；(4) reaction finishes carry out separation of solid and liquid, obtains calcium citrate trihydrate solid；(5) calcium citrate trihydrate isolated is dried to obtain soluble calcium citrate trihydrate finished product；Wherein, mass fraction is 60%-80% after the calcium carbonate described in step (1) is sized mixing；The content after the dissolving of food-grade citric acid described in step (2) is 1.10-1.40g/ml water；Reaction temperature described in step (3) is controlled at 25 DEG C, speed of agitator 40-60rpm, and the reaction time is 40-60 minutes；Separation described in step (4) is using continuous crystallisation centrifugal separation technology.
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| CN201511003767.0A CN105418407B (en) | 2015-12-29 | 2015-12-29 | A kind of production technology of soluble calcium citrate trihydrate |
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| CN201511003767.0A CN105418407B (en) | 2015-12-29 | 2015-12-29 | A kind of production technology of soluble calcium citrate trihydrate |
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| CN105418407A CN105418407A (en) | 2016-03-23 |
| CN105418407B true CN105418407B (en) | 2018-01-30 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102225894A (en) * | 2011-04-18 | 2011-10-26 | 山东恒通生物科技有限公司 | Preparation method of soluble calcium citrate trihydrate |
| CN102491893A (en) * | 2011-12-07 | 2012-06-13 | 南通市飞宇精细化学品有限公司 | Zinc citrate trihydrate and preparation method thereof |
| CN103058853A (en) * | 2012-12-17 | 2013-04-24 | 日照金禾博源生化有限公司 | Method for producing calcium hydrogen citrate |
| CN104529754A (en) * | 2014-12-24 | 2015-04-22 | 日照金禾博源生化有限公司 | Production process of amorphous superfine calcium citrate |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7267832B2 (en) * | 2004-02-18 | 2007-09-11 | Kraft Foods Holdings, Inc. | Amorphous water-soluble calcium citrate salts and method of making and using same |
-
2015
- 2015-12-29 CN CN201511003767.0A patent/CN105418407B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102225894A (en) * | 2011-04-18 | 2011-10-26 | 山东恒通生物科技有限公司 | Preparation method of soluble calcium citrate trihydrate |
| CN102491893A (en) * | 2011-12-07 | 2012-06-13 | 南通市飞宇精细化学品有限公司 | Zinc citrate trihydrate and preparation method thereof |
| CN103058853A (en) * | 2012-12-17 | 2013-04-24 | 日照金禾博源生化有限公司 | Method for producing calcium hydrogen citrate |
| CN104529754A (en) * | 2014-12-24 | 2015-04-22 | 日照金禾博源生化有限公司 | Production process of amorphous superfine calcium citrate |
Non-Patent Citations (1)
| Title |
|---|
| 柠檬酸氢钙水合物的制备与表征;陈连蔚 等;《应用化工》;20150220;第44卷(第2期);199-202 * |
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