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A kind of iodine supported catalyst, preparation method and a kind of preparation method of all-trans vitamin A acetate

A technology of supporting catalyst and acetate, applied in chemical instruments and methods, physical/chemical process catalysts, organic chemistry, etc., can solve problems such as harming environmental health, toxic iodine vapor, and inappropriate isomerization catalysis of vitamin A acetate

Active Publication Date: 2021-05-14
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Chemical isomerization can use organic acid or iodine as a catalyst, but under the catalysis of vitamin A acetate, in addition to the isomerization reaction, it is easy to undergo double bond displacement to generate reverse vitamin A acetate, which is not suitable for vitamin A acetate heterogeneous catalysis
Iodine has a good isomerization catalytic effect, and the isomerization reaction conditions are relatively mild, but in the post-treatment process of the reaction, it is necessary to use an aqueous solution of sodium thiosulfate to reduce iodine to sodium iodide, which will produce a large amount of iodine-containing wastewater. Industrial production will bring great wastewater treatment and environmental protection problems
At the same time, iodine may produce toxic iodine vapor during storage, endangering environmental health

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Iodine supported catalyst preparation:

[0037] Take 100g of natural fluoroapatite for mechanical crushing, take 100-200 mesh fluoroapatite through a sieve, and heat the fluoroapatite powder at 400°C for 5 hours to remove the adsorbed water. Weigh 62g of deionized water, 5g of iodine element, and 33g of KI solid and mix and dissolve to prepare a solution. The content of KI in this solution is 33wt%, and the content of iodine element is 5wt%. Weigh 5g of dehydrated apatite powder and pour it into the prepared solution, stir the mixture vigorously at 15°C and 800-1000rpm for 4h, filter, wash with deionized water, rinse with acetone, and dry at room temperature to obtain iodine Supported catalyst A 1 5.85g, the loading capacity of elemental iodine calculated by mass difference is 14.5%.

[0038] Preparation of all-trans vitamin A acetate:

[0039] Take by weighing 40gVA crude oil (13-cis vitamin A acetate content is 50wt% in crude oil, all-trans vitamin A acetate conte...

Embodiment 2

[0041] Catalyst preparation:

[0042]Take 100g of natural fluoroapatite for mechanical crushing, take 100-200 mesh fluoroapatite through a sieve, and heat the fluoroapatite powder at 250°C for 8 hours to remove the adsorbed water. Weigh 39.5g of deionized water, 1.5g of iodine element, and 9g of KI solid to mix and dissolve to prepare a solution. The content of KI in this solution is 18wt%, and the content of iodine element is 3wt%. Weigh 5g of dehydrated apatite powder and pour it into the prepared solution, stir the mixture vigorously at 10°C and 800-1000rpm for 5h, filter, wash with deionized water, rinse with acetone, and dry at room temperature to obtain iodine Supported catalyst A 2 5.45g, the loading capacity of elemental iodine calculated by mass difference is 8.3%;

[0043] Isomerization reaction:

[0044] Take by weighing 40gVA crude oil (13-cis vitamin A acetate content is 50wt% in crude oil, all-trans vitamin A acetate content is 35wt%, impurity content is 15wt...

Embodiment 3

[0046] Catalyst preparation:

[0047] Take 100g of natural fluoroapatite for mechanical crushing, take 100-200 mesh fluoroapatite through a sieve, and heat the fluoroapatite powder at 500°C for 2 hours to remove the adsorbed water. 32g of deionized water, 0.33g of iodine element, and 1g of KI solid were mixed and dissolved respectively to prepare a solution. The content of KI in the solution was 3wt%, and that of iodine was 1wt%. Weigh 5g of dehydrated apatite powder and pour it into the prepared solution, stir the mixture vigorously at 20°C, 800-1000rpm for 3h, filter, wash with deionized water, rinse with acetone, and dry at room temperature to obtain iodine Supported catalyst A 3 5.07g, the loading capacity of elemental iodine calculated by mass difference is 1.4%;

[0048] Isomerization reaction:

[0049] Take by weighing 40gVA crude oil (13-cis vitamin A acetate content is 50wt% in crude oil, all-trans vitamin A acetate content is 35wt%, impurity content is 15wt%) and...

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Abstract

The invention discloses an iodine-loaded catalyst, a preparation method and a preparation method of all-trans vitamin A acetate. Firstly, an iodine-supported catalyst supported by fluorapatite is prepared, and then the above-mentioned iodine-supported catalyst is used to efficiently isomerize 13-cis vitamin A acetate into all-trans vitamin A acetate. After the reaction is completed, the catalyst and the product can be completely separated by simple filtration and washing. This method can reduce the amount of iodine and avoid a large amount of iodine-containing waste water generated during the conventional treatment of simple iodine. It is suitable for large-scale Industrial production, but also conducive to environmental protection.

Description

technical field [0001] The invention belongs to the technical field of catalyst and compound preparation, and relates to an iodine-supported catalyst, a preparation method and a method for preparing all-trans vitamin A acetate catalyzed by the iodine-supported catalyst. Background technique [0002] Vitamin A acetate is an important class of medicines, used for the treatment of night blindness, dry eyes, corneal softening and dry skin; it can promote the growth and development of the human body, and can enhance the resistance to diseases; at the same time, vitamin A is also an important feed additives. Vitamin A acetate has a variety of cis and trans isomers, the common ones are 11-cis vitamin A acetate, 9-cis vitamin A acetate, 13-cis vitamin A acetate and all-trans vitamin A acetate . Among them, only all-trans vitamin A acetate has biological activity, so how to convert the cis isomer into the all-trans isomer is a very important reaction process. [0003] At present, ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/18C07C403/12
CPCB01J27/1806C07C403/12Y02P20/584
Inventor 张旭王明永黎源陈志刚王展胡展张涛吕英东
Owner WANHUA CHEM GRP CO LTD
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