Method for preparing 1, 3-butylene glycol by adopting fixed bed continuous reaction

A fixed-bed reactor and butanediol technology, which is applied to the preparation of carbon-based compounds, chemical instruments and methods, and the preparation of hydroxyl compounds, can solve problems such as inability to recycle, difficult separation, and smaller particle size of Raney nickel. Achieve the effect of simple operation, good stability and low operating cost

Active Publication Date: 2021-02-23
QINGDAO INST OF BIOENERGY & BIOPROCESS TECH CHINESE ACADEMY OF SCI
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  • Abstract
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Problems solved by technology

[0004] NaOH is corrosive and cannot be recycled. After the first step of the acetaldehyde condensation reaction is completed, it needs to use acetic acid to quench the reaction, which will generate saline wastewater; although the Raney nickel catalyst is stable in the hydrogenation reaction, after filtration or After centrifugation, it can be recycled, but in the tank reactor, due to the continuous collision and wear with the stirring blade, the particle size of Raney nickel will become smaller, resulting in difficulty in separation, and it is necessary to add a catalyst during use.

Method used

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  • Method for preparing 1, 3-butylene glycol by adopting fixed bed continuous reaction
  • Method for preparing 1, 3-butylene glycol by adopting fixed bed continuous reaction

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preparation example Construction

[0054] The solid base catalyst used in the step 1) of the preparation method according to the present invention is packed in a fixed-bed reactor, and the catalyst is stable under reaction conditions, for example, the very important properties of the reaction process include stability to moisture and air , and the impact resistance of reactive materials are very stable. The catalyst can efficiently promote the condensation reaction of acetaldehyde, the reaction mainly generates 3-hydroxybutyraldehyde, and the by-product is crotonaldehyde (also known as crotonaldehyde). The total selectivity of the products 3-hydroxybutyraldehyde and crotonaldehyde of this step reaction is generally above 80%, and under preferred conditions, the total selectivity can exceed 90%, even exceed 95%. The by-product crotonaldehyde of this step reaction is generated by dehydration of 3-hydroxybutyraldehyde. Using the technology developed by the patent of the present invention, the ratio of 3-hydroxybut...

preparation Embodiment 1

[0058] 130g Mg(NO 3 ) 2 ·6H 2 0, 8g of silica gel, 1g of zinc oxide and 1g of activated carbon were mixed in a flask, added 150g of water, stirred at 80°C for 5 hours, evaporated to dryness, then roasted at a high temperature at 900°C in a nitrogen atmosphere, then crushed and sieved, 10 -20 mesh sieve to obtain gray black catalyst particles.

Embodiment 1 to 6

[0059] Embodiment 1 to 6: the condensation reaction of the acetaldehyde reaction raw material of different concentration in fixed-bed reactor

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Abstract

The invention discloses a method for preparing 1, 3-butylene glycol by adopting a fixed bed continuous reaction, and the preparation method comprises the following steps of: 1) feeding an acetaldehydeaqueous solution into a condensation reaction fixed bed reactor filled with a solid base catalyst by using carrier gas to obtain a condensation reaction product; 2) feeding the reaction material flowfrom which acetaldehyde is separated and a hydrogen flow into a hydrogenation reactor together, and carrying out hydrogenation reaction on 3-hydroxy butyraldehyde in the presence of a hydrogenation catalyst to generate 1, 3-butylene glycol; and 3) finally acquiring the 1, 3-butylene glycol product by separation and purification methods like vacuum rectification. According to the preparation method disclosed by the invention, a specific solid base catalyst is adopted, so that efficient condensation reaction of acetaldehyde is realized, and further the 1, 3-butylene glycol is prepared. The method is simple and efficient, particularly, the fixed bed reactor is combined with the specific catalyst, and the method is simple and convenient to operate, green, environment-friendly and few in industrial three wastes, and is a sustainable green synthesis route.

Description

technical field [0001] The invention relates to the field of chemical synthesis, in particular to a method for preparing 1,3-butanediol by using a fixed-bed continuous reaction. Background technique [0002] 1,3-Butanediol (1,3-Butylene Glycol, 1,3-BDO) is a widely used chemical product, such as: 1,3-Butanediol and phthalic anhydride, maleic anhydride and other monomers The unsaturated polyester resin has good water resistance, softness and impact resistance; the plasticizer made of 1,3-butanediol has the advantages of low volatility, migration resistance and oil resistance. 1,3-Butanediol also has the characteristics of good hygroscopicity, odorless, low toxicity, and good water solubility. It can be used as a moisturizer and softener for textiles, tobacco and paper, and an antibacterial agent for cheese or meat; It is mainly used as a moisturizing agent in cosmetics, and has a good antibacterial effect, and can be used in the production of various lotions, ointments and t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/72C07C47/19C07C29/141C07C31/20B01J23/80B01J23/06
CPCC07C45/72C07C29/141B01J23/80B01J23/06C07C47/19C07C31/207
Inventor 徐国强蒋士峰高鹍牟新东王喜成
Owner QINGDAO INST OF BIOENERGY & BIOPROCESS TECH CHINESE ACADEMY OF SCI
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