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Supported catalyst for use in production of 1, 4-butynediol by Reppe method, preparation method thereof and application thereof

A butynediol and catalyst technology, applied in 1 field, can solve the problems of high cost, complex preparation process of molecular sieve and magnesium silicate carrier, short service life, etc.

Active Publication Date: 2011-07-20
HAISO TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this type of catalyst has the following disadvantages: (1) It is not easy to regenerate and recycle, and its life is short; (2) The preparation process of molecular sieve and magnesium silicate carrier is relatively complicated and relatively expensive

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Preparation of Catalyst Support

[0026] Take industrial-grade kaolin and wash it with sulfuric acid with a mass concentration of 10% to 25% for no less than 12 hours, then filter, and wash the filter cake with deionized water or distilled water until no SO can be detected in the soluble barium salt solution. 4 2- After drying, add ammonium sulfate to grind, the amount of ammonium sulfate added is 10% to 30% of the mass of the carrier, roast at 300°C to 800°C for more than 2.5 hours, and then wash with deionized water or distilled water until the soluble barium salt solution is detected Less than SO 4 2- After drying, the treated kaolin carrier is obtained. Used in the following examples.

Embodiment 2

[0028] a. Weigh 38gCu(NO 3 ) 2 ·3H 2 O is made into 300ml solution;

[0029] b. Weigh 1.5gBi(NO 3 ) 3 ·5H 2 O was dissolved in 3ml of 1:1 nitric acid solution;

[0030] c. take by weighing anhydrous sodium carbonate 18g and be made into 300ml solution;

[0031] d. take by weighing processed kaolin 30g in embodiment 1;

[0032] e. Put d in a stirred flask;

[0033] f. Mix a and b and add to e and stir for 1 hour;

[0034] g. Slowly add c to f under stirring conditions, so that the final pH of the reaction is 6.5-7.0, stop stirring, let the precipitated mixture stand for 3 hours, pour off the mother liquor, wash the precipitated with distilled water until the soluble barium salt solution is no longer detected to SO 4 2- , and then the filter cake was dried at 80°C for 3 hours, then at 120°C for 3 hours, and then roasted at 300°C to 800°C for no less than 3 hours to obtain a supported catalyst for the production of 1,4-butynediol by the Reppe method .

[0035] Take 2...

Embodiment 3

[0037] a. Weigh 50g Cu(NO3)2·3H2O to make 300ml solution;

[0038] b. Weigh 1.7gBi(NO3)3·5H2O and dissolve in 4ml of 1:1 nitric acid solution;

[0039] c. take by weighing anhydrous sodium carbonate 23g and be made into 450ml solution;

[0040] d. take by weighing processed kaolin 14g in embodiment 1;

[0041] e. Put d in a stirred flask;

[0042] f. Mix a and b and add to e and stir for 1 hour;

[0043] g. Slowly add c to f under stirring conditions, so that the final pH of the reaction is 6.5-7.0. Stop stirring, let the precipitation mixture stand for 3 hours, pour off the mother liquor, and wash the precipitation with distilled water until the soluble barium salt solution does not detect SO 4 2- , and then the filter cake was dried at 80°C for 3 hours, then at 120°C for 3 hours, and then roasted at 400°C to 700°C for no less than 3 hours to obtain a supported catalyst for the production of 1,4-butynediol by the Reppe method .

[0044] Take 25g of the catalyst prepared ...

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Abstract

The invention relates to a supported catalyst for use in the production of 1, 4-butynediol by a Reppe method, a preparation method thereof and application thereof, in particular to a method for preparing a catalyst for use in the synthesis of1, 4-butynediol by formaldehyde and acetylene in a slurry bed and application. The method is characterized by comprising the steps of: taking 40 to 60 mass percent of treated kaolin as a carrier, and depositing soluble copper salt and soluble bismuth salt on the carrier by a method for depositing sediments, so that the catalyst contains 57 to 37 mass percent of copper oxide. The catalyst prepared by the method has high activity and selectivity, and compared with similar catalysts without the carrier, the catalyst is wear-resistance and saves copper resources.

Description

technical field [0001] The invention relates to a carrier-containing catalyst for producing 1,4-butynediol, more precisely to the preparation and application of a 1,4-butynediol catalyst with kaolin as a carrier. Background technique [0002] 1,4-butanediol is hydrogenated to obtain 1,4-butanediol, and 1,4-butanediol is an important basic organic chemical and fine chemical raw material, mainly consumed in polyurethane (PU), poly Butylene terephthalate (PBT), γ-butyrolactone (GBL) and tetrahydrofuran (THF) and other fields. In recent years, my country's demand for 1,4-butanediol has continued to grow. [0003] In the 1940s, Reppe invented the process of synthesizing 1,4-butynediol from formaldehyde and acetylene. The process uses a copper acetylene catalyst, which increases the operational risk of acetylene and copper acetylene under reaction pressure. After the 1970s, a new catalyst for the synthesis of 1,4-butynediol was developed, which improved the Reppe process. The ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/843C07C33/046C07C29/42
Inventor 罗平武文豹李耀会张雄斌吕小婉李小定
Owner HAISO TECH
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