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Method for preparing 1, 3-butanediol through catalytic hydrogenation

A technology for catalytic hydrogenation and butanediol, applied in chemical instruments and methods, preparation of hydroxyl compounds, preparation of organic compounds, etc., can solve the problems of reduced reaction selectivity, low hydrogenation activity of Raney nickel, low production efficiency, etc.

Inactive Publication Date: 2020-07-10
南京大学淮安高新技术研究院
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, 3-hydroxybutyraldehyde is mainly hydrogenated in a tank reactor using Raney nickel. Due to the low hydrogenation activity of Raney nickel, a higher reaction temperature is usually required, which will lead to the formation of 3-hydroxybutyraldehyde in the product. The content of crotonaldehyde generated by dehydration of butyraldehyde increases, which reduces the selectivity of the reaction, and the longer residence time in the reactor will also lead to a further increase of impurities
Although the noble metal catalyst supported by Pd / C has high hydrogenation activity and good product selectivity, the catalyst is relatively expensive, the production cost is high, and the separation operation of the reaction product and the catalyst is required, and the production efficiency is low.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] 29.72 g of Ni(NO 3 ) 2 ·6H 2 O, 25.64 g of Na 2 SiO3 9H 2 O was dissolved in 200 ml of distilled water to obtain solution A, and 23.57 g of anhydrous Na 2 CO 3 Dissolve in 200 ml of distilled water to obtain solution B. Under stirring conditions, solution A and solution B were added dropwise to 400 ml of distilled water at the same time to form a green precipitate, and the filter cake obtained by washing and dehydrating the precipitate was dispersed in 200 ml of n-butanol, and the solvent was evaporated at 353 K, and Continue drying at 393 K to obtain a supported metal nickel catalyst precursor. The obtained catalyst precursor is pressed into tablets, sieved, and 60-80 mesh catalyst precursor particles are collected by sieving.

Embodiment 2

[0020] Take 4 g of the pre-reduced metal nickel catalyst particles prepared in Example 2, pack them into a fixed-bed reaction tube, and reduce them in 40 ml / min flowing hydrogen at a temperature of 723 K for 2 h, and then drop the temperature to 333 K. The hydrogen pressure was raised to 3 MPa, and the DMF solution with a mass percentage of 50% of 3-hydroxybutyraldehyde was injected into the reactor with a metering pump, and a trickle bed catalytic hydrogenation reaction was carried out, and the flow rate of the reaction solution was 3 ml / h , the ratio of the amount of hydrogen to 3-hydroxybutyraldehyde is 20:1. The solution after the reaction was collected, and its composition was analyzed by chromatography. It was calculated that the conversion rate of 3-hydroxybutyraldehyde was 86%, and the selectivity of 1,3-butanediol was 88%.

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Abstract

The invention discloses a method for preparing 1, 3-butanediol through catalytic hydrogenation, and belongs to the technical field of catalytic hydrogenation. 3-hydroxybutyraldehyde is taken as a rawmaterial, and catalytic hydrogenation reaction is carried out in a trickle bed reactor in the presence of a supported metal nickel catalyst and an alkaline solvent under the hydrogen atmosphere of 293-3733K and 1.0-8.0MPa. Under optimized conditions, the hydrogenation conversion rate of 3-hydroxybutyraldehyde can reach 86%, and the selectivity of 1, 3-butanediol can reach 88%.

Description

technical field [0001] The invention relates to a method for preparing 1,3-butanediol through catalytic hydrogenation, belonging to the technical field of catalytic hydrogenation. Background technique [0002] 1,3-Butanediol can be used as humectant, antibacterial agent, widely used in the production of cosmetics, ointment and toothpaste. At the same time, 1,3-butanediol is also the raw material of polyester resin and alkyd resin. Its various monocarboxylic acid monoesters are excellent plasticizers for PVC resin. Monomers such as dianhydrides can be polymerized to obtain unsaturated resins. Due to its antibacterial and low toxicity properties, 1,3-butanediol is also used as an antibacterial agent in dairy products and meat. [0003] The synthesis of 1,3-butanediol mainly includes biological method and chemical synthesis method. The biological fermentation method has relatively mild conditions, high selectivity, and less discharge of three wastes, but the output is low and...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C29/141C07C31/20
CPCC07C29/141C07C31/207
Inventor 沈俭一徐铮
Owner 南京大学淮安高新技术研究院
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