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A kind of method for preparing 1,3-butanediol by using 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, smaller particle size of Raney nickel, and difficulty in separation. Achieve the effect of simple operation and less industrial waste

Active Publication Date: 2022-07-29
QINGDAO INST OF BIOENERGY & BIOPROCESS TECH CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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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  • A kind of method for preparing 1,3-butanediol by using fixed bed continuous reaction
  • A kind of method for preparing 1,3-butanediol by using fixed bed continuous reaction

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preparation example Construction

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

preparation Embodiment 1

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

Embodiment 1 to 6

[0059] Examples 1 to 6: Condensation of acetaldehyde reaction feedstocks with different concentrations in a fixed bed reactor

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Abstract

The invention discloses a method for preparing 1,3-butanediol by a fixed-bed continuous reaction. The preparation method includes the following steps: 1) using a carrier gas to send an aqueous acetaldehyde solution into a condensation reaction equipped with a solid base catalyst The fixed-bed reactor obtains the condensation reaction product; 2) the reactant stream and the hydrogen stream from which the acetaldehyde is separated are sent together into the hydrogenation reactor, and in the presence of a hydrogenation catalyst, 3-hydroxybutyraldehyde is subjected to a hydrogenation reaction to 1,3-butanediol is generated; 3) 1,3-butanediol product can be obtained by separation and purification methods such as vacuum rectification at last. According to the preparation method of the present invention, a specific solid base catalyst is used to realize an efficient condensation reaction from acetaldehyde, thereby preparing 1,3-butanediol. The method is simple and efficient, especially the fixed bed reactor is combined with a specific catalyst, the operation is simple, the environmental protection is green, and the three industrial wastes are less, and it 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-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 from 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, and can be used as a moisturizing agent and softening agent 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 ...

Claims

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Application Information

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Patent Type & Authority Patents(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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