CN101914012A - Preparation method of chromium citrate - Google Patents

Preparation method of chromium citrate Download PDF

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Publication number
CN101914012A
CN101914012A CN2010102653305A CN201010265330A CN101914012A CN 101914012 A CN101914012 A CN 101914012A CN 2010102653305 A CN2010102653305 A CN 2010102653305A CN 201010265330 A CN201010265330 A CN 201010265330A CN 101914012 A CN101914012 A CN 101914012A
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China
Prior art keywords
chromium
citrate
preparation
product
water
Prior art date
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Pending
Application number
CN2010102653305A
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Chinese (zh)
Inventor
张富强
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Tianjin Chemical Reagent Research Institute
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Tianjin Chemical Reagent Research Institute
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Priority to CN2010102653305A priority Critical patent/CN101914012A/en
Publication of CN101914012A publication Critical patent/CN101914012A/en
Pending legal-status Critical Current

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  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

The invention relates to a preparation method of chromium citrate, comprising the following steps of: (1) a chromic hydroxide preparing reaction step: throwing chromium sulfate and water into a reaction kettle, heating to the temperature of 70-80 DEG C for reacting while stirring, dropping ammonia, washing, draining and generating chromic hydroxide; (2) a salifying reaction step: suspending a separated granular chromic hydroxide product in a citrate aqueous solution, heating to 70-80 DEG C for reacting while stirring to obtain a purple solution, filtering and precipitating, and drying to obtain chromium citrate product. The invention uses the ammonia and the citrate as main raw materials in a production process, has the characteristics of simple realization and convenient operation, saves the investment of production devices and increases the production efficiency.

Description

A kind of preparation method of chromium citrate
Technical field
The invention belongs to the organic compound preparation field, especially a kind of preparation method of chromium citrate.
Background technology
In animal-feed humatite additive, chromium citrate more and more comes into one's own as a kind of organic chromium mineral additive, is with a wide range of applications.The common production method of chromium citrate is to utilize Trisodium Citrate and chromium sulphate reaction, and the product that obtains is thick thing, further handles comparatively difficulty, is difficult to sell.The problem thing that existing preparation method exists: 1, in further treatment step, product is clamminess, washing national calamity, foreign matter content height; Ventilation property is bad when 2, drying, and moisture evaporation is slow, is difficult for drying, needs to increase stir equipment automatically, and equipment is many, and complicated production cost height is difficult to reduce production costs; 3, be unfavorable for the development of enterprise and the raising of economic benefit.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, a kind of preparation method of chromium citrate is provided, the present invention can save facility investment, reduce cost, improves the quality of products, reduces foreign matter content.
It is to realize by the following technical solutions that the present invention solves its technical problem:
A kind of preparation method of chromium citrate may further comprise the steps:
(1) preparation chromium hydroxide reactions steps: chromium sulphate, water are dropped in the reactor, under agitation heat 70-80 ℃ of reaction simultaneously, dropping ammonia, washing is drained, and generates chromium hydroxide;
(2) salt-forming reaction step: the particulate state chromium hydroxide product with separation obtains, be suspended in the aqueous citric acid solution, under agitation heat 70-80 ℃ of reaction simultaneously, obtain purple solution, the suction filtration precipitation, oven dry obtains the chromium citrate product.
And the mol ratio of chromium sulphate, water and ammoniacal liquor is 1: 400 in the described step (1): 0.9-1.15.
And the mol ratio of the citric acid in the described step (2), water, chromium hydroxide is 1: 100: 0.9-1.2.
Advantage of the present invention and positively effect are:
1, this preparation method uses citric acid to replace Trisodium Citrate in feeding intake, and the product that obtains has only chromium citrate, and product is single, and the purity height is easy to drying after the separation.
2, the chromium citrate product that obtains of this preparation method is easy to drying, has saved facility investment, has reduced running cost.
3, the present invention uses ammoniacal liquor, citric acid to be main raw material in process of production, has to realize that simply convenience operation has been saved investment in production equipment, has improved production efficiency.
Embodiment
The invention will be further described below by specific embodiment, and following examples are descriptive, is not determinate, can not limit protection scope of the present invention with this.
Embodiment 1:
A kind of preparation method of chromium citrate may further comprise the steps:
(1) preparation chromium hydroxide reactions steps: have that heating unit, electricity stir, drop into 3 moles of chromium sulphates, 1200 moles in water successively in 50 milliliters of reactors of thermometer to one, under agitation heat 70-80 ℃ of reaction simultaneously, slowly add 3 moles of ammoniacal liquor, and under agitation reacted 1 hour, stop heating, reaction is finished.The suction filtration product, washing obtains the chromium hydroxide product, and this product not drying is directly used in following reaction.
(2) salt-forming reaction step: chromium hydroxide and 3 moles of citric acids, water that separation is obtained under agitation heat 70-80 ℃ of reaction for 300 moles simultaneously, obtain purple solution, after 5 hours, filter, the product solution that obtains concentrates and obtains finished product, and this chromium citrate product content is greater than 98%.
Embodiment 2:
A kind of preparation method of chromium citrate may further comprise the steps:
(1) preparation chromium hydroxide reactions steps: have that heating unit, electricity stir, drop into 3 moles of chromium sulphates, 1200 moles in water successively in 50 liters of reactors of thermometer to one, under agitation heat 70-80 ℃ of reaction simultaneously, slowly adding 3.3 moles of ammoniacal liquor under agitation reacted 1 hour, stop heating, reaction is finished.The suction filtration product, washing obtains the chromium hydroxide product, and this product not drying is directly used in following reaction.
(2) salt-forming reaction step: chromium hydroxide that separation is obtained and 3 moles of citric acids, 300 moles in water, under agitation heat 70-80 ℃ of reaction simultaneously, obtain purple solution, after 5 hours, filter the product solution that obtains, concentrate and obtain finished product, this chromium citrate product content is greater than 98%.
Embodiment 3:
A kind of preparation method of chromium citrate may further comprise the steps:
(1) preparation chromium hydroxide reactions steps: have that heating unit, electricity stir, drop into 3 moles of chromium sulphates, 1200 moles in water successively in 50 liters of reactors of thermometer to one, under agitation heat 70-80 ℃ of reaction simultaneously, slowly adding 2.7 moles of ammoniacal liquor under agitation reacted 1 hour, stop heating, reaction is finished.The suction filtration product, washing obtains the chromium hydroxide product, and this product not drying is directly used in following reaction.
(2) salt-forming reaction step: chromium hydroxide that separation is obtained and 3 moles of citric acids, 300 moles in water, under agitation heat 70-80 ℃ of reaction simultaneously, obtain purple solution, after 5 hours, filter the product solution that obtains, concentrate and obtain finished product, this chromium citrate product content is greater than 98%.

Claims (3)

1. the preparation method of a chromium citrate is characterized in that: may further comprise the steps:
(1) preparation chromium hydroxide reactions steps: chromium sulphate, water are dropped in the reactor, under agitation heat 70-80 ℃ of reaction simultaneously, dropping ammonia, washing is drained, and generates chromium hydroxide;
(2) salt-forming reaction step: the particulate state chromium hydroxide product with separation obtains, be suspended in the aqueous citric acid solution, under agitation heat 70-80 ℃ of reaction simultaneously, obtain purple solution, the suction filtration precipitation, oven dry obtains the chromium citrate product.
2. the preparation method of chromium citrate according to claim 1 is characterized in that: the mol ratio of chromium sulphate, water and ammoniacal liquor is 1: 400 in the described step (1): 0.9-1.15.
3. the preparation method of chromium citrate according to claim 1, it is characterized in that: the mol ratio of the citric acid in the described step (2), water, chromium hydroxide is 1: 100: 0.9-1.2.
CN2010102653305A 2010-08-28 2010-08-28 Preparation method of chromium citrate Pending CN101914012A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN2010102653305A CN101914012A (en) 2010-08-28 2010-08-28 Preparation method of chromium citrate

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN2010102653305A CN101914012A (en) 2010-08-28 2010-08-28 Preparation method of chromium citrate

Publications (1)

Publication Number Publication Date
CN101914012A true CN101914012A (en) 2010-12-15

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Family Applications (1)

Application Number Title Priority Date Filing Date
CN2010102653305A Pending CN101914012A (en) 2010-08-28 2010-08-28 Preparation method of chromium citrate

Country Status (1)

Country Link
CN (1) CN101914012A (en)

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
赵书清等: "柠檬酸铬合成方法的研究", 《黑龙江大学自然科学学报》 *

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Application publication date: 20101215