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High-stability vitamin A and preparation method thereof

A high stability, vitamin technology, applied in the field of vitamins, can solve problems such as easy agglomeration and yellowing of crystal color, and achieve the effects of improving light stability, solving yellowing of crystal color, and improving chemical stability.

Pending Publication Date: 2022-02-11
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In addition, it effectively solves the problem of yellowish crystal color and easy reunion after crystallization of vitamin A acetate

Method used

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  • High-stability vitamin A and preparation method thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] 52.74g of crude raw material C15 phosphine salt was dissolved in 50.11g of water, and the above aqueous solution was added to 50.11g of solvent b (n-hexane 99.5wt% and methanol 0.5wt%) at 30°C and a rotation speed of 200rpm, stirred for 15min and allowed to stand The phases were separated for 15 minutes, and the composition of the raffinate phase was sampled and analyzed (excluding solvent a water): the content of compound I was 540 ppm, the content of compound II was 860 ppm, and the content of C15 phosphine salt was 99.86%.

[0039] In the raffinate phase, add 14.2g five carbon aldehydes, after being warmed up to 45 ℃, dropwise add 69g mass fraction and be 20% K 2 CO 3 solution, reacted for 1 hour at a pressure of 50 kPaA and a stirring speed of 200 rpm to obtain vitamin A crude oil. After sampling and measuring the composition, it can be obtained that the conversion rate of C15 phosphine salt is 95.2%, the selectivity of vitamin A is 99.3%, and the content of vitami...

Embodiment 2

[0042] 52.74g of crude raw material C15 phosphine salt was dissolved in 100.22g of water, and the above aqueous solution was added to 100.22g of solvent b (n-hexane 99.5wt% and water 0.5wt%) at 40°C and a rotation speed of 300rpm, stirred for 30min and allowed to stand The phases were separated for 30 minutes, and the composition of the raffinate phase was sampled and analyzed (excluding solvent a water): the content of compound I was 420 ppm, the content of compound II was 780 ppm, and the content of C15 phosphine salt was 99.88%.

[0043] In the raffinate phase, add 14.2g five carbon aldehydes, after being warmed up to 55 ℃, dropwise add 92g mass fraction and be 30% K 2 CO 3 The solution was reacted for 2 hours at a pressure of 100 kPaA and a stirring speed of 300 rpm to obtain vitamin A crude oil. After sampling and measuring the composition, it can be obtained that the conversion rate of C15 phosphonium salt is 95.4%, the selectivity of vitamin A is 99.4%, and the content...

Embodiment 3

[0046] 52.74g of the crude raw material C15 phosphine salt was dissolved in 150.33g of water, and the above aqueous solution was added to 150.33g of solvent b (n-hexane 99wt% and methanol 1wt%) at 30°C and a rotation speed of 400rpm, stirred for 45min and allowed to stand for 45min Phase, sampling and analysis of raffinate phase composition (excluding solvent a water): the content of compound I is 1200ppm, the content of compound II is 2100ppm, and the content of C15 phosphine salt is 99.67%.

[0047] In the raffinate phase, add 7.1g five-carbon aldehyde, after being warmed up to 65 ℃, dropwise add 18g mass fraction and be 40% K 2 CO 3 The solution was reacted for 3 hours at a pressure of 150 kPaA and a stirring speed of 400 rpm to obtain vitamin A crude oil. After sampling and measuring the composition, it can be obtained that the conversion rate of C15 phosphine salt is 95.1%, the selectivity of vitamin A is 99.2%, and the content of vitamin A dimer is 0.08%.

[0048] The ...

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Abstract

The invention discloses a high-stability vitamin A and a preparation method thereof. The method comprises the following steps: carrying out wittig reaction on a C15 phosphine salt mixture and pentacaraldehyde under the action of alkali liquor to prepare vitamin A acetate crude oil, and recrystallizing to obtain vitamin A crystals. By controlling the contents of the compound I and the compound II in the C15 phosphine salt mixture to be 0.1 wt%-1wt%, the content of VA dimer in the vitamin A acetate crude oil is less than 0.1%, and the chemical stability of a vitamin A product can be remarkably improved. The chromatic value of the obtained VA crystal solution is smaller than 60 HAzen, the average size of the VA crystal is 100-200 microns, and the problems that the VA crystal is yellow in color, easy to agglomerate and large in particle size are effectively solved.

Description

technical field [0001] The invention relates to the field of vitamins, in particular to a vitamin A product and a preparation method thereof. [0002] technical background [0003] C15 phosphonate is an important intermediate in the synthesis of vitamin A, carotenoids, apolate, etc. by wittig reaction. As mentioned in the patent CN100455558C, a C15 phosphine salt is generated by reacting β-vinylionol with triphenylphosphine in the presence of sulfuric acid, and then reacted with 4-acetoxy-2-methyl-but-2-enal The method for producing vitamin A acetate by Wittig reaction has a yield of about 90%, and a cis-trans isomer ratio of 7:3. This process has the advantages of less industrial waste, simple process flow, and low operating cost. However, the wittig reaction synthesis vitamin A process has the following pain points: First, due to the complexity of raw materials and excessive side reactions during the reaction process, the conditions that are conducive to the formation of v...

Claims

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Application Information

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IPC IPC(8): C07C403/12
CPCC07C403/12
Inventor 潘晓艺罗朝辉冯兴磊赵一鸣孙媛媛杨蕊宋明焱
Owner WANHUA CHEM GRP CO LTD
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