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Method for synthesizing cosmetic-grade 1,3-butanediol

A cosmetic grade, butanediol technology, applied in chemical instruments and methods, preparation of organic compounds, condensation preparation of carbonyl compounds, etc., can solve the problem of high impurity content of 1,3-butanediol, difficulty in meeting cosmetic quality requirements, odor Major problems, to achieve the effect of stable product quality control, easy product quality, and no odor

Active Publication Date: 2016-05-18
LIAONING KELONG FINE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The liquid-phase condensation of acetaldehyde is a violent exothermic reaction. If the conditions are not properly controlled, acetaldehyde is prone to deep condensation, and the product 3-hydroxybutyraldehyde is also easily dehydrated to produce crotonaldehyde with a strong pungent smell, resulting in the product 1,3-butanedi The content of alcohol impurities is high, the color is large, and the smell is strong, which is difficult to meet the quality requirements of the cosmetics industry

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Example 1: A method for synthesizing cosmetic grade 1,3-butanediol,

[0035] 1) Mix the acetaldehyde water evenly according to the mass ratio of 7:1 and pour it into the reaction kettle, add 5% dilute sodium hydroxide solution dropwise until the pH of the reaction system is 10, keep the reaction temperature at 8°C, and keep the reaction for 15-90 minutes. Add dilute acetic acid dropwise to neutralize the reaction system to neutrality;

[0036] 2) flashing the reaction product in step (1) at 100°C, recovering the acetaldehyde obtained by distillation, and the distillation residue is 3-hydroxybutyraldehyde;

[0037] 3) Mix the 3-hydroxybutyraldehyde obtained in step (2) with the skeleton nickel evenly, inject it into the autoclave, keep the hydrogen pressure at 8mPa, and react for 30min;

[0038] 4) The product obtained in step (3) is centrifuged to obtain a catalyst for recycling, the feed liquid is flashed at 120°C to produce water, by-product ethanol and crotonaldehyd...

Embodiment 2

[0042] 1) Mix the acetaldehyde water evenly according to the mass ratio of 8:1 and pour it into the reaction kettle, add 5% dilute sodium hydroxide solution dropwise until the pH of the reaction system is 12, keep the reaction temperature at 8°C, and keep the reaction for 15-90 minutes. Add dilute acetic acid dropwise to neutralize the reaction system to neutrality;

[0043] 2) flashing the reaction product in step (1) at 90°C, recovering the acetaldehyde obtained by distillation, and the distillation residue is 3-hydroxybutyraldehyde;

[0044] 3) Mix the 3-hydroxybutyraldehyde obtained in step (2) with the skeleton nickel evenly, inject it into the autoclave, keep the hydrogen pressure at 10mPa, the reaction temperature is 100°C, and the reaction time is 60min;

[0045] 4) The product obtained in step (3) is centrifuged to obtain a catalyst for recycling, the feed liquid is flashed at 120°C to produce water, by-product ethanol and crotonaldehyde, and the crude 1,3-butanediol ...

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Abstract

The invention relates to a method for synthesizing cosmetic-grade 1,3-butanediol. The method includes the steps that acetaldehyde and water are mixed evenly and then injected into a reaction kettle, and dilute acetic acid is dripped under the alkaline condition so that the reaction system can be neutralized to be neutral; flashing is carried out, acetaldehyde obtained in distillation is recycled, and distillation residual liquid is 3-hydroxybutanal; obtained 3-hydroxybutanal and a catalyst are mixed evenly, hydrogen pressure is kept, centrifugal separation is carried out on the obtained product to obtain the catalyst for recycling, flashing is carried out on the liquor at 120 DEG C to obtain water and the byproducts ethyl alcohol and crotonaldehyde, and reduced pressure distillation is carried out to obtain coarse 1,3-butanediol; purification is carried out. The process of synthesizing 1,3-butanediol through condensation and hydrogenation reduction of an acetaldehyde liquid phase is improved through the steps, and thus the product 1,3-butanediol meets the quality requirement of the cosmetic industry.

Description

technical field [0001] The invention relates to a method for synthesizing cosmetic grade 1,3-butanediol, which belongs to the technical field of chemical synthesis. Background technique [0002] Cosmetic grade 1,3-butanediol is a colorless, transparent, viscous, extremely low impurity content, odorless liquid with good hygroscopicity and water solubility, and has good antibacterial effect. It can be used as a cosmetic moisturizer. In lotion, lotion, ointment, toothpaste and other products. [0003] There are multiple methods for the synthesis of 1,3-butanediol in patents and other public reports: (1) laser irradiation containing hydrogen peroxide and ethanol saturated with nitrogen to directly synthesize 1,3-butanediol; (2) Using epoxy compound and synthesis gas as raw materials, it is produced by carbonyl synthesis under the conditions of rhodium and phosphine catalysts; (3) acrolein reacts with 2,2-dimethyl-1,3-propanediol, and the product is carbonylated Hydrolysis and ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C31/20C07C29/80C07C29/141
CPCC07C29/141C07C29/80C07C45/45C07C31/207C07C47/19Y02P20/584
Inventor 周全凯黄动昊姜艳王炳帅秦丽翠
Owner LIAONING KELONG FINE CHEM
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