Preparation method of 1, 3-butylene glycol

A technology of butanediol and hydroxybutyraldehyde, applied in the chemical industry, can solve the problems of pungent odor, unsatisfactory yield and purity of 1,3-butanediol, and reduce side reactions, avoid deep condensation and dehydration The effect of high reaction and yield

Active 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

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] (1) Mix acetaldehyde and water evenly at a mass ratio of 7:1 and transport to the material pretreatment tank, keep the temperature at 15°C, and carry out under nitrogen protection;

[0035] (2) packing the loaded solid basic catalyst in a fixed bed, wherein the carrier is an ion exchange resin, the active component is tetrabutylammonium bromide, and the temperature is constant to 15° C.;

[0036] (3) the acetaldehyde solution in the step (1) is pumped into the fixed-bed reactor;

[0037] (4) In the fixed-bed reactor, the acetaldehyde aqueous solution undergoes an aldol condensation reaction under the catalysis of a supported solid basic catalyst. During this process, the reaction temperature is controlled at 15°C to 20°C, the pH value is kept at 13, and the reaction residence time is 4min. The crude product mainly contains unreacted acetaldehyde (15%-20%), 3-hydroxybutyraldehyde (70%-80%), a small amount of crotonaldehyde (0.5%-1%), other impurities and water;

[0038]...

Embodiment 2

[0045] (1) Mix the acetaldehyde and water evenly according to the mass ratio of 8:1, then transport to the material pretreatment tank, keep the temperature at 20°C, and carry out under the protection of nitrogen;

[0046] (2) Packing the loaded solid basic catalyst in a fixed bed, wherein the carrier is activated carbon, the active components are potassium and cerium (mass ratio 20:1), and the temperature is constant to 15° C.;

[0047] (3) the acetaldehyde solution in the step (1) is pumped into the fixed-bed reactor;

[0048] (4) In the fixed-bed reactor, the acetaldehyde aqueous solution undergoes an aldol condensation reaction under the catalysis of a supported solid basic catalyst. During this process, the reaction temperature is controlled at 20°C to 25°C, the pH value is kept at 12, and the reaction residence time is 5min. The crude product mainly contains unreacted acetaldehyde (15%-20%), 3-hydroxybutyraldehyde (70%-80%), a small amount of crotonaldehyde (0.5%-1%), oth...

Embodiment 3

[0056] (1) Mix acetaldehyde and water evenly at a mass ratio of 9:1 and transport to the material pretreatment tank, keep the temperature at 25°C, and carry out under nitrogen protection;

[0057] (2) packing the loaded solid basic catalyst in a fixed bed, wherein the carrier is aluminum oxide, the active components are potassium and cesium (mass ratio 20:1), and the temperature is constant to 25°C;

[0058] (3) the acetaldehyde solution in the step (1) is pumped into the fixed-bed reactor;

[0059] (4) In a fixed-bed reactor, an aldol condensation reaction occurs in an aqueous solution of acetaldehyde under the catalysis of a loaded solid basic catalyst. The process controls the reaction temperature at 25° C., maintains a pH value of 11, and has a residence time of 6 minutes to obtain a crude product. It mainly contains unreacted acetaldehyde (15%-20%), 3-hydroxybutyraldehyde (70%-80%), a small amount of crotonaldehyde (0.5%-1%), other impurities and water;

[0060] (5) The ...

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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 fixed bed reactor, under the effect of a supported type solid basic catalyst, aldol condensation reaction is carried out so as to obtain 3-hydroxybutyraldehyde; and B, 3-hydroxybutyraldehyde is subjected to continuous hydrogenation reaction inthe fixed bed reactor so as to obtain 1, 3-butylene glycol. According to the preparation method, the fixed bed reactor is adopted, at the same time, the supported type solid basic catalyst is adoptedto replace a conventional liquid alkali (such as sodium hydroxide) catalysts, and in the step of hydrogenation reduction, a supported nickel hydrogenation catalyst is adopted. The preparation method is capable of solving problems in the prior art product quality is poor, product yield is low, technology process is complex, and a large amount of waste water and waste residue is generated; aldol condensation quenching step is avoided; side reactions are reduced; 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.

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, and is widely used in cosmetics, such as lotion, facial mask, cream, lotion, toothpaste Waiting for cleaning products. In addition, 1,3-butanediol can also be used in the production of plasticizers, unsaturated polyester resins, or as moisturizers and softeners for textiles, tobacco and paper, antibacterial agents for cheese or meat, etc. [0003] At present, patents and documents have reported a variety of methods for preparing 1,3-butanediol: (1) British Patent 853266 discloses a method that uses acetaldehyde as a raw material to generate 3-hydroxybutanediol through aldol condensation in alkaline solution Aldehyde, 3-hydroxybutyraldehyde hydrogenation reduction method to gene...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C31/20C07C29/141C07C29/80C07C47/19C07C45/72
CPCC07C29/141C07C29/80C07C45/72C07C47/19C07C31/207
Inventor 滕文彬王春梅杜桂强刘博闻祝秀林郝小军高腾
Owner DONGYING HI TECH SPRING CHEM IND
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