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Method for preparing 1,4-butanediol-coproduced tetrahydro furan and gamma-butyrolactone

A technology of tetrahydrofuran and butanediol, applied in 1 field, can solve problems such as poor reaction stability, and achieve the effects of easy separation, less by-products, and improved selectivity

Active Publication Date: 2010-01-06
SHANGHAI HUAYI ENERGY CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0014] The technical problem to be solved by this invention is to provide a kind of with dimethyl maleate as raw material, make use of non-precious metal catalyst, carry out a gas-phase catalytic hydrogenation reaction to prepare 1, the method for 4-butanediol, to overcome existing The technology cannot obtain a high yield of 1,4-butanediol co-production of tetrahydrofuran and γ-butyrolactone under the condition of large raw material liquid volume feed space velocity, and the defect of poor reaction stability

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] 40 g of Cu(NO 3 ) 2 ·3H 2 O, 43.0 g Cr(NO 3 ) 3 9H 2 O was dissolved in 600 milliliters of deionized water, and after stirring evenly, ammonia water (concentration 23-25wt%) was dripped into the mixed salt solution with a peristaltic pump until the pH was 5.5 ± 0.2, filtered and washed, and the precipitate was collected and dried overnight at 100°C. Calcined at 500°C for 10 hours, and then molded to obtain a catalyst precursor. The obtained catalyst A: CuCr 0.65 o 29 .

Embodiment 2

[0035] 20 g of Cu(NO 3 ) 2 ·3H 2 O, 16.55 g Cr(NO 3 ) 3 9H 2 O was dissolved in 600 ml of deionized water, stirred evenly, stirred at 60°C, added Na 2 CO 3 solution until the pH is 5.8±0.2, filter and wash, collect the precipitate, dry at 100°C overnight, calcinate at 500°C for 10 hours, and then shape the catalyst precursor. The obtained catalyst B: Cu 2 CrO 3.5 .

Embodiment 3

[0037] 40 g of Cu(NO 3 ) 2 ·3H 2 O, 19.82 g Cr(NO 3 ) 3 9H 2 O, 28.4 grams of urea, dissolved in 500 ml of deionized water, stirred evenly, stirred at 90 ° C, aged for 24 hours until the pH was 6.5 ± 0.2, filtered and washed, collected precipitates, dried overnight at 100 ° C, and roasted at 500 ° C 10 hours, and then molded to obtain a catalyst precursor. The obtained catalyst C: CuCr 0.6 o 1.9 .

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PUM

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Abstract

The invention relates to a method for preparing 1,4-butanediol-coproduced tetrahydro furan and gamma-butyrolactone from maleic acid dimethyl ester through hydrogenization, which comprises the following steps that: after being gasified, under the condition of 170 to 190 DEG C and 4.0 to 6.0MPa, maleic acid dimethyl ester is prepared into the 1,4-butanediol-coproduced tetrahydro furan and the gamma-butyrolactone in the presence of a pre-reduced catalyst formed by the general formula of CuCr(a)O(x) by hydrogenization; and in the catalyst, a is equal to 0.5 to 0.65, and x is the oxygen atom number satisfying the valency of various metal elements. The method ensures that the raw material of the maleic acid dimethyl ester is completely converted, the mole selectivity of 1,4-butanediol reaches 70 percent to 85 percent, the mole selectivity of tetrahydro furan reaches 5 percent to 10 percent, and the mole selectivity of gamma-butyrolactone reaches 10 percent to 15 percent under the condition at higher liquid hourly space velocity.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and in particular relates to a preparation method of 1,4-butanediol. Background technique [0002] 1,4-Butanediol is an important organic chemical raw material, mainly used in the production of polybutylene terephthalate (PBT), polyurethane, γ-butyrolactone and tetrahydrofuran. Usually, 1,4-butanediol is synthesized from acetylene and formaldehyde under high pressure, and can also be prepared by hydrolysis of γ-butyrolactone or tetrahydrofuran. [0003] With the development of butane oxidation to prepare maleic anhydride technology, since the 1960s, the process of catalytic hydrogenation of maleic anhydride and its esters to 1,4-butanediol has fewer reaction steps, low investment, and The characteristics of the resulting product can be adjusted and attract attention. Early maleic anhydride vapor phase hydrogenation method adopts Zn-Cu-Cr catalyst (patent publication 44-32567) and CuO-...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C31/20C07C29/149C07D307/36C07D307/33B01J23/86
Inventor 杨菊群张旭红刘文艳赵正康何明康
Owner SHANGHAI HUAYI ENERGY CHEM