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Preparation method of 1, 3-butylene glycol

A technology of butanediol and acetaldehyde, which is applied in the chemical industry, can solve the problems of pungent odor, unsatisfactory yield and purity of 1,3-butanediol, etc., achieve high reaction conversion rate and yield, and overcome product Poor quality, avoid the effect of deep condensation

Inactive Publication Date: 2019-03-05
DONGYING HI TECH SPRING CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But the 1,3-butanediol yield and purity that above-mentioned method prepares are all unsatisfactory, and have pungent smell

Method used

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  • Preparation method of 1, 3-butylene glycol
  • Preparation method of 1, 3-butylene glycol

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Experimental program
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Embodiment 1

[0039] (1) After acetaldehyde and water are mixed evenly according to the mass ratio of about 8:1, transport them to the material pretreatment tank, keep the temperature at 15°C, and carry out under the protection of nitrogen;

[0040] (2) Constant temperature of alkaline ionic liquid catalyst hydroxide 1-butyl-3-methylimidazolium salt to 15°C;

[0041] (3) acetaldehyde solution and ionic liquid catalyst in step (1), (2) are sent in the microchannel reactor;

[0042] (4) In the microchannel reactor, the acetaldehyde aqueous solution undergoes an aldol condensation reaction under the catalysis of an ionic liquid catalyst. The process controls the reaction temperature to 15° C., the reaction system PH11, and the reaction residence time of 5 minutes to obtain a crude product, mainly including unreacted Acetaldehyde (about 10% to about 20%), 3-hydroxybutyraldehyde (about 70% to 80%), a small amount of crotonaldehyde (about 0.3% to 0.5%), other impurities and water;

[0043] (5) S...

Embodiment 2

[0050] (1) After acetaldehyde and water are mixed evenly according to the mass ratio of about 9:1, transport them to the material pretreatment tank, keep the temperature at 20°C, and carry out under the protection of nitrogen;

[0051] (2) Constant temperature of alkaline ionic liquid catalyst hydroxide 1-butyl-3-methylimidazolium salt to 20°C;

[0052] (3) acetaldehyde solution and ionic liquid catalyst in step (1), (2) are sent in the microchannel reactor;

[0053] (4) In the microchannel reactor, the acetaldehyde aqueous solution undergoes an aldol condensation reaction under the catalysis of an ionic liquid catalyst. The process controls the reaction temperature to 20° C., the reaction system pH to 11.4, and the reaction residence time to 10 minutes to obtain a crude product, mainly containing Reaction of acetaldehyde (about 10% to about 20%), 3-hydroxybutyraldehyde (about 70% to 80%), a small amount of crotonaldehyde (about 0.3% to 0.5%), other impurities and water;

[0...

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Abstract

The invention provides a preparation method of 1, 3-butylene glycol. The preparation method comprises following steps: A, acetaldehyde is introduced into a microchannel reactor, under the effect of abasic ionic liquid catalyst, aldol reaction is carried out so as to obtain 3-hydroxybutyraldehyde; and B, 3-hydroxybutyraldehyde is subjected to continuous hydrogenation reaction in a fixed bed reactor so as to obtain 1, 3-butylene glycol. According to the preparation method, the traditional kettle type reaction technology is improved; the microchannel reactor is adopted, at the same time, the basic ionic liquid catalyst is adopted to replace conventional liquid alkali (such as sodium hydroxide) catalysts, and in the step of hydrogenation reduction, a supported nickel hydrogenation catalyst isadopted, and hydrogenation reduction is carried out in the fixed bed reactor. The preparation method is capable of solving problems in the prior art product quality is poor, product yield is low, andtechnology process is complex; relatively high reaction conversion rate and yield are achieved; no neutralizing or desalting process is needed in reaction process; and great improvement of traditional 1, 3-butylene glycol preparation technology is realized. The prepared 1, 3-butylene glycol is colorless and smelless, is high in purity, and is capable of satisfying application requirements of highgrade industries such as cosmetic.

Description

technical field [0001] The invention relates to the technical field of chemical industry, in particular to a preparation method of 1,3-butanediol. Background technique [0002] 1,3-Butanediol (1,3-BDO) has the characteristics of good hygroscopicity, odorless, low toxicity, and good water solubility. Polyester resin can also be used as a moisturizer and softener for textiles, tobacco and paper, and an antibacterial agent for cheese or meat. In addition, it is also widely used in cosmetics as a moisturizer, such as lotion, cream, lotion, toothpaste and other products. [0003] Patents and documents have reported a variety of methods for preparing 1,3-butanediol: (1) British Patent 853266 discloses that acetaldehyde is used as a raw material to generate 3-hydroxybutyraldehyde through aldol condensation in alkaline solution, A method for generating 1,3-butanediol by hydrogenation reduction of 3-hydroxybutyraldehyde; (2) Chinese patent 103102229 discloses a method for preparing...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/72C07C47/19C07C29/141C07C31/20B01J19/00
CPCB01J19/0093C07C29/141C07C45/72C07C47/19C07C31/207Y02P20/584
Inventor 滕文彬王春梅刘博闻郝小军祝秀林
Owner DONGYING HI TECH SPRING CHEM IND
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