CN102633627A - Solid-phase synthesis method for calcium citrate - Google Patents

Solid-phase synthesis method for calcium citrate Download PDF

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Publication number
CN102633627A
CN102633627A CN2012100947591A CN201210094759A CN102633627A CN 102633627 A CN102633627 A CN 102633627A CN 2012100947591 A CN2012100947591 A CN 2012100947591A CN 201210094759 A CN201210094759 A CN 201210094759A CN 102633627 A CN102633627 A CN 102633627A
Authority
CN
China
Prior art keywords
phase synthesis
lime
citrate
solid
citric acid
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
Application number
CN2012100947591A
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Chinese (zh)
Inventor
李永富
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Nantong Feiyu Fine Chemical Co Ltd
Jiangnan University
Original Assignee
Nantong Feiyu Fine Chemical Co Ltd
Jiangnan University
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Nantong Feiyu Fine Chemical Co Ltd, Jiangnan University filed Critical Nantong Feiyu Fine Chemical Co Ltd
Priority to CN2012100947591A priority Critical patent/CN102633627A/en
Publication of CN102633627A publication Critical patent/CN102633627A/en
Pending legal-status Critical Current

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Abstract

The invention discloses a solid-phase synthesis method for calcium citrate, comprising the following steps of: weighing the following components in parts by weight: 50-60% of citric acid and 40-50% of calcium carbonate; adding the weighed citric acid and calcium carbonate into a grinding tank of a high energy-activated planet grinder, controlling the rotating speed of the high energy-activated planet grinder at 1000-1500 revolutions/min, and mechanically grinding for 15-50minutes; and after grinding, pouring the obtained product into a container, dissolving by pouring hot water with the temperature of 90-100 DEG C, and naturally cooling to be crystallized, so that the calcium citrate can be obtained. The method adopts a mechano-chemical method, so that the activation energy of reaction can be reduced, the reactivity of reactant can be increased, the solid-phase synthesis of the calcium citrate can be realized, temperature control in a heating way does not need in the process of reaction, the pH does not need adjusting, and the solid-phase synthesis method is short in reaction time and low in energy consumption, thereby being a cleaning production technology.

Description

The method of solid phase synthesis citrate of lime
Technical field
The present invention relates to citrate of lime method of manufacture technical field, be specifically related to a kind of method of solid phase synthesis citrate of lime.
Background technology
Citrate of lime is mineral element supplement commonly used in the food and medicine field, is used for nutrient fortified food nutrition, replenishes the deficiency of calcium.Citrate of lime is an organic calcium, and it is compared with inorganic calcium has stable in properties, and the absorption rate advantages of higher is used more and more wider in food, medicine and field of fodder.
Existing synthesizing citric acid calcium is to adopt the acid-base neutralisation method, through control reaction temperature, regulates pH and realizes chemical reaction, and reaction needs is carried out in liquid phase, complex manufacturing, and power consumption is high, and production cost is higher.
Summary of the invention
Goal of the invention: the objective of the invention is provides the method for the solid phase synthesis citrate of lime that a kind of technology is simple, facility investment is few, production cost is low in order to remedy the deficiency of prior art.
The technical scheme that the present invention adopts: a kind of method of solid phase synthesis citrate of lime, it comprises the steps:
(1) takes by weighing following component by weight: Hydrocerol A: 50-60%, lime carbonate: 40-50%;
Said Hydrocerol A that (2) will take by weighing and lime carbonate join in the grinding pot of high energy activation planetary mills, and the rotating speed of said high energy activation planetary mills is controlled at 1000-1500 rev/min, mechanical mill 15-50 minute;
(3) grind to finish after, products therefrom is poured in the container, and is poured into 90-100 ℃ of hot water and dissolve, naturally cool to crystallization then and obtain citrate of lime.
Said Hydrocerol A is Citric Acid, usp, Anhydrous Powder or Citric acid monohydrate Food grade.
The addition of said hot water is 0.6-1.2 a times that said Hydrocerol A and lime carbonate grind back products therefrom weight.
Beneficial effect: the present invention adopts the method for mechanochemistry, reduces reaction activity, and the accretion qualitative response is active; Realize the solid phase synthesis citrate of lime, need not heat temperature control in the reaction process, need not regulate pH; Reaction times is short, and it is low to consume energy, and is a kind of process for cleanly preparing.
Embodiment
Below in conjunction with specific embodiment the present invention is described further:
Embodiment 1:
Take by weighing Citric Acid, usp, Anhydrous Powder 300g, lime carbonate 300g; Join in the grinding pot of high energy activation planetary mills, under 1000 rev/mins rotating speed, mechanical activation 15 minutes; The reaction product of gained naturally cools to crystallization and obtains citrate of lime with the hot water dissolving of 90 ℃ of 360 grams.
Embodiment 2:
Take by weighing Citric Acid, usp, Anhydrous Powder 366.6g, lime carbonate 300g; Join in the grinding pot of high energy activation planetary mills, under 1250 rev/mins rotating speed, mechanical activation 32 minutes; The reaction product of gained naturally cools to crystallization and obtains citrate of lime with the hot water dissolving of 95 ℃ of 599.9 grams.
Embodiment 3:
Take by weighing Citric Acid, usp, Anhydrous Powder 450g, lime carbonate 300g; Join in the grinding pot of high energy activation planetary mills, under 1500 rev/mins rotating speed, mechanical activation 50 minutes; The reaction product of gained naturally cools to crystallization and obtains citrate of lime with the hot water dissolving of 100 ℃ of 900 grams.
Embodiment 4:
Take by weighing Citric acid monohydrate Food grade 400g, lime carbonate 400g; Join in the grinding pot of high energy activation planetary mills, under 1500 rev/mins rotating speed, mechanical activation 50 minutes; The reaction product of gained naturally cools to crystallization and obtains citrate of lime with the hot water dissolving of 100 ℃ of 960 grams.
Embodiment 5:
Take by weighing Citric acid monohydrate Food grade 400g, lime carbonate 327.2g; Join in the grinding pot of high energy activation planetary mills, under 1250 rev/mins rotating speed, mechanical activation 32 minutes; The reaction product of gained naturally cools to crystallization and obtains citrate of lime with the hot water dissolving of 95 ℃ of 654.4 grams.
Embodiment 6:
Take by weighing Citric acid monohydrate Food grade 400g, lime carbonate 266.6g; Join in the grinding pot of high energy activation planetary mills, under 1000 rev/mins rotating speed, mechanical activation 15 minutes; The reaction product of gained naturally cools to crystallization and obtains citrate of lime with the hot water dissolving of 90 ℃ of 399.9 grams.

Claims (3)

1. the method for a solid phase synthesis citrate of lime, it is characterized in that: it comprises the steps:
(1) takes by weighing following component by weight: Hydrocerol A: 50-60%, lime carbonate: 40-50%;
Said Hydrocerol A that (2) will take by weighing and lime carbonate join in the grinding pot of high energy activation planetary mills, and the rotating speed of said high energy activation planetary mills is controlled at 1000-1500 rev/min, mechanical mill 15-50 minute;
(3) grind to finish after, products therefrom is poured in the container, and is poured into 90-100 ℃ of hot water and dissolve, naturally cool to crystallization then and obtain citrate of lime.
2. the method for solid phase synthesis citrate of lime according to claim 1 is characterized in that: said Hydrocerol A is Citric Acid, usp, Anhydrous Powder or Citric acid monohydrate Food grade.
3. the method for solid phase synthesis citrate of lime according to claim 1 is characterized in that: the addition of said hot water is 0.6-1.2 a times that said Hydrocerol A and lime carbonate grind back products therefrom weight.
CN2012100947591A 2012-04-01 2012-04-01 Solid-phase synthesis method for calcium citrate Pending CN102633627A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN2012100947591A CN102633627A (en) 2012-04-01 2012-04-01 Solid-phase synthesis method for calcium citrate

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN2012100947591A CN102633627A (en) 2012-04-01 2012-04-01 Solid-phase synthesis method for calcium citrate

Publications (1)

Publication Number Publication Date
CN102633627A true CN102633627A (en) 2012-08-15

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CN2012100947591A Pending CN102633627A (en) 2012-04-01 2012-04-01 Solid-phase synthesis method for calcium citrate

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CN (1) CN102633627A (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN106854153A (en) * 2015-12-08 2017-06-16 中粮生物化学(安徽)股份有限公司 A kind of preparation of calcium salt of citric acid and preparation method thereof and the calcium salt containing the citric acid

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4851221A (en) * 1985-02-19 1989-07-25 Mission Pharmacal Company Liquid calcium supplementation from readily soluble mixtures of calcium compound and citric acid
WO2003087028A1 (en) * 2002-04-12 2003-10-23 Technical And Commercial Services International Limited A method of making salt
CN1680258A (en) * 2004-02-18 2005-10-12 卡夫食品集团公司 Amorphous water-soluble calcium citrate salts and method of making and using same
CN101607890A (en) * 2008-06-17 2009-12-23 安徽丰原发酵技术工程研究有限公司 A kind of citric acid continuously in and extracting method

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4851221A (en) * 1985-02-19 1989-07-25 Mission Pharmacal Company Liquid calcium supplementation from readily soluble mixtures of calcium compound and citric acid
WO2003087028A1 (en) * 2002-04-12 2003-10-23 Technical And Commercial Services International Limited A method of making salt
CN1680258A (en) * 2004-02-18 2005-10-12 卡夫食品集团公司 Amorphous water-soluble calcium citrate salts and method of making and using same
CN101607890A (en) * 2008-06-17 2009-12-23 安徽丰原发酵技术工程研究有限公司 A kind of citric acid continuously in and extracting method

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN106854153A (en) * 2015-12-08 2017-06-16 中粮生物化学(安徽)股份有限公司 A kind of preparation of calcium salt of citric acid and preparation method thereof and the calcium salt containing the citric acid

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Application publication date: 20120815