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Continuous extracting and purifying method of vitamin A intermediate

A purification method and intermediate technology, applied in the field of substance purification, can solve the problems of large amount of solvent, high concentration of inorganic salt, long process steps, etc., and achieve the effect of less solvent consumption, high product purity and simple operation

Active Publication Date: 2012-07-04
SHANGYU NHU BIOCHEM IND +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The process steps are long, using press filter or centrifuge, and the equipment is large and complicated. When forming salt, strong alkali materials such as sodium hydroxide and potassium hydroxide aqueous solution are used. When reducing, strong acids such as hydrochloric acid and sulfuric acid are used, which seriously corrodes the equipment; solvents during washing Large amount, high energy consumption for subsequent solvent recovery, high concentration of inorganic salts in the water layer, dissolved organic matter, and difficult wastewater treatment

Method used

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  • Continuous extracting and purifying method of vitamin A intermediate
  • Continuous extracting and purifying method of vitamin A intermediate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] 1000g of the crude condensate product (content 90%) is dissolved in 3000mL of 75% methanol aqueous solution by volume, and the formed material 1 enters the extraction tower from the upper inlet of the extraction tower 2, and the extraction agent 3 is toluene, which is fed from the lower inlet of the extraction tower. Enter the extraction tower, the extraction tower is first filled with toluene, the volume ratio of the alcohol aqueous solution to toluene is controlled at 1.2:1, the temperature of the extraction tower is 35°C, after the extraction is completed, all the methanol aqueous solution 4 containing the condensate is recovered under reduced pressure methanol and water to obtain condensate 914g, content 96.5%, molar yield 98.0%. The extractant tower tops out the extractant and most of the sundries 5.

Embodiment 2

[0020] 1000g of crude condensate (content 90%) was dissolved in 3000mL of 82% methanol aqueous solution by volume, the volume ratio of alcohol aqueous solution to toluene was controlled at 1.1:1, and the temperature of the extraction tower was 35°C. After the extraction was completed, the methanol containing condensate The aqueous solution recovers methanol and water under reduced pressure to obtain 917 g of condensate with a content of 96.8% and a molar yield of 98.6%.

Embodiment 3

[0022] The ratio of materials used for extraction is the same as in Example 1, the temperature of the extraction tower is 22°C, after the extraction is completed, methanol and water are recovered under reduced pressure from the aqueous methanol solution containing the condensate, and 912g of the condensate is obtained, with a content of 96.2% and a molar yield of 97.5%. .

[0023]

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PUM

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Abstract

The invention discloses a continuous extracting and purifying method of a vitamin A intermediate. The purifying method provided by the invention is a crystallization purifying method; a crude product is dissolved in a nonpolar solvent and is refrigerated and crystallized; an impurity in the crude product has strong dissolubility for crystallization; the crystallization rate is low; the energy consumption of low-temperature crystallization is large; and a product is easy to be oxidized to go bad after the crystallization. The purifying method provided by the invention comprises the following steps of: dissolving the crude product of the vitamin A intermediate in a lower alcohol aqueous solution with a volume ratio of 20-90% to form an alcohol-water material, and subsequently, enabling the alcohol-water material to enter an extracting tower continuously, wherein the operating conditions of the extracting tower are that: the extracting temperature is 10-50 DEG C, and the volume ratio of the alcohol-water material to low-polarity extracting agent for extraction is 1: 5 to 5: 1, after 5-20 stages of countercurrent extraction, most impurities are extracted by the extracting agent, and the micro vitamin A intermediate is brought out; and obtaining the purified vitamin A intermediate after the lower alcohol aqueous solution is recovered from the alcohol-water material obtained at the bottom of the extracting tower. The purity of the product obtained by the continuous extracting and purifying method is high, and a subsequent hydrogenation reaction is beneficial.

Description

[0001] technical field [0002] The invention relates to a method for purifying substances, in particular to a vitamin A intermediate 3,7-dimethyl-9-(2',6',6'-trimethyl-1-cyclohexenyl)-2 , Continuous extraction and purification method of 7-diene-4-yne-1,6-diol. Background technique [0003] Vitamin A intermediate 3,7-dimethyl-9-(2',6',6'-trimethyl-1-cyclohexenyl)-2,7-dien-4-yne-1,6 -diol, hereinafter referred to as condensate, molecular formula is as follows: [0004] [0005] The product is obtained by addition reaction of tetradecanal with hexacarbonyl alcohol and bromomagnesium ethane under the condition of ether as solvent, hydrolysis with hydrochloric acid or sulfuric acid aqueous solution, neutralization with sodium carbonate aqueous solution, and recovery of solvent from the oil layer. Because there are impurities in the raw materials tetradecanal and hexa-alkynyl alcohol, the crude condensate produced by the reaction has low purity, and the next step of selectiv...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C403/08
Inventor 王国富李军陈梦桥管敏虾袁娜娜沈丹
Owner SHANGYU NHU BIOCHEM IND