Method for synthesizing zinc citrate trihydrate

A technology of zinc trihydrate and synthesis method, which is applied in the separation/purification of carboxylic acid compounds, preparation of organic compounds, chemical instruments and methods, etc., and can solve the unseen synthesis process of zinc citrate trihydrate, zinc citrate There are few reports on the direct synthesis of trihydrate, etc., to achieve the effect of novel method, enhanced reaction contact, and product specificity

Active Publication Date: 2015-05-13
NANTONG FEIYU FINE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] Although there are multiple synthetic methods of zinc citrate in the prior art, these methods often involve the preparation process of dihydrate, but there are few reports on the direct synthesis of zinc citrate trihydrate
[0008] In addition, the existing zinc citrate trihydrate has no related synthesis process

Method used

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  • Method for synthesizing zinc citrate trihydrate
  • Method for synthesizing zinc citrate trihydrate
  • Method for synthesizing zinc citrate trihydrate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Add citric acid and deionized water into the reaction kettle, stir and heat up to 55°C, then add zinc carbonate to it, after the addition is complete, add catalyst 4-tert-butyl-calix[4]arene and additive 1-vinyl -3-Ethylimidazolium bromide, stir and heat up to 75°C, and stir and react at this temperature for 10 minutes. After the reaction is completed, centrifuge and filter, wash the obtained solid with water and absolute ethanol in sequence, and finally fully vacuum-dry. That is, zinc citrate trihydrate was obtained with a yield of 99.1% (based on citric acid).

[0029] Wherein, the mass ratio of citric acid and deionized water is 1:2, the mol ratio of citric acid and zinc carbonate is 1:3.5, and the molar dosage of 4-tert-butyl-calix[4]arene is 2% of the molar dosage of citric acid. %, the molar dosage of 1-vinyl-3-ethylimidazolium bromide is 5% of the molar dosage of citric acid. The mass spectrum data of gained zinc citrate is as follows:

[0030] MS m / z: 628.38 (...

Embodiment 2

[0032] Add citric acid and deionized water into the reactor, stir and heat up to 60°C, then add zinc nitrate into it, after the addition is complete, add catalyst 4-tert-butyl-calix[4]arene and additive 1-vinyl -3-Ethylimidazolium bromide, stirred and heated to 80°C, and stirred at this temperature for 8 minutes. After the reaction was completed, centrifuged and filtered, the obtained solid was washed with water and absolute ethanol in turn, and finally fully vacuum-dried. That is, zinc citrate trihydrate was obtained with a yield of 98.5% (calculated as citric acid).

[0033] Wherein, the mass ratio of citric acid to deionized water is 1:3.5, the molar ratio of citric acid to zinc nitrate is 1:3.7, and the molar dosage of 4-tert-butyl-calix[4]arene is 2.5% of the molar dosage of citric acid. %, the molar dosage of 1-vinyl-3-ethylimidazolium bromide is 6% of the molar dosage of citric acid. The mass spectrum data of gained zinc citrate is as follows:

[0034] MS m / z: 628.36 ...

Embodiment 3

[0036] Add citric acid and deionized water into the reactor, stir and heat up to 65°C, then add zinc carbonate to it, after the addition is complete, add catalyst 4-tert-butyl-calix[4]arene and additive 1-vinyl - 3-Ethylimidazolium Bromide, stir and heat up to 85°C, and stir and react at this temperature for 7 minutes. After the reaction is completed, centrifuge and filter, wash the obtained solid with water and absolute ethanol in sequence, and finally fully vacuum-dry. That is, zinc citrate trihydrate was obtained with a yield of 98.8% (calculated as citric acid).

[0037] Wherein, the mass ratio of citric acid and deionized water is 1:5, and the molar ratio of citric acid and zinc carbonate is 1:4, and the molar dosage of 4-tert-butyl-calix [4] arene is 3% of the molar dosage of citric acid. %, the molar dosage of 1-vinyl-3-ethylimidazolium bromide is 8% of the molar dosage of citric acid. The mass spectrum data of gained zinc citrate is as follows:

[0038] MS m / z: 628.3...

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Abstract

The invention relates to a method for synthesizing zinc citrate trihydrate. The method comprises the following steps: adding citric acid and deionized water into a reaction kettle, and stirring and heating to the temperature of 55-65 DEG C; adding a zinc compound, adding a catalyst and aids after the zinc compound is completely added, stirring, heating, and reacting; centrifuging and filtering after the reaction is ended, sequentially washing and performing absolute ethyl alcohol washing on the obtained solids; and finally, fully performing vacuum drying, thereby obtaining the zinc citrate trihydrate. According to the method, a complex reaction system with specific catalyst and aids is adopted, rapid and high-yield preparation of the target product is realized by virtue of dual effects of the micro-hole reaction environment and assistant catalysis, and the method has very obvious technical effects and achieves wide industrial application prospects and market potentials.

Description

technical field [0001] The invention relates to a method for synthesizing organic acid salt hydrate, more specifically to a method for catalytically synthesizing zinc citrate trihydrate, which belongs to the field of organic chemical synthesis. Background technique [0002] Zinc is one of the trace elements needed by the human body. Zinc deficiency in the human body can lead to serious problems such as growth retardation and poor wound healing. The existing zinc supplements mainly include zinc sulfate, zinc acetate, and zinc gluconate. In addition, zinc citrate is also a very commonly used organic zinc supplement, which has the advantages of less irritation to the stomach and high zinc content, and can effectively enhance the digestion and absorption function of the human body. Zinc citrate generally contains two crystal waters, and reports on the preparation process of dihydrate are common in the prior art. Since zinc citrate trihydrate [(C 6 h 5 o 7 ) 2 Zn 3 ·3H 2 O...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C59/265C07C51/41
CPCC07C51/412C07C51/42C07C59/265
Inventor 姚建飞朱碧君姚佼
Owner NANTONG FEIYU FINE CHEM
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