Preparation of copper-bismuth-silicon dioxide catalyst

A silicon dioxide and catalyst technology, which is applied in the field of copper bismuth catalysts, can solve the problems of complex catalyst preparation process, unfavorable industrial development and use, unstable carrier magnesium silicate, etc., and achieve simple preparation process, uniform particle size, and improved stability Effect

Inactive Publication Date: 2016-11-16
XINJIANG UNIVERSITY
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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) the carrier magnesium silicate is unstable and will dissolve in the reaction system, and its life is short; (2) the interaction bet

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0010] Weigh 9.0 g cetyltrimethylammonium bromide (CTAB) and 28.5 g Na 2 SiO 3 10H 2 O was dissolved in 250 mL of water. Then weigh 7.2 g Cu(NO 3 ) 2 ·3H 2 O and 0.8 g Bi(NO 3 ) 3 ·5H 2 Dissolve O in 50 mL of water, add 5 mL of polyethylene glycol 400, quickly add 10 mL of concentrated ammonia water, and stir for 0.5 h. Add the mixed solution of copper and bismuth to the above solution containing CTAB and sodium silicate, stir for 0.5 h, then use 1 mol / LH 2 SO 4 Adjust the pH value of the solution to 9-10, stir at room temperature for 3-24 h, then centrifuge, wash with distilled water and absolute ethanol for several times, dry at room temperature, place in a high-temperature furnace and roast at 550°C for 5 h to obtain copper bismuth / silicon dioxide catalyst. The above-prepared catalyst was used for alkynylation reaction. After 7 hours of reaction, the conversion rate of formaldehyde was 66%, the selectivity of 1,4-butynediol was 91%, and the copper ion content in ...

Embodiment 2

[0012] Weigh 10.0 g of cetyltrimethylammonium bromide (CTAB) and 25.0 g of ethyl orthosilicate respectively and dissolve them in 100 mL of ethanol aqueous solution. Then weigh 7.2 g Cu(NO 3 ) 2 ·3H 2 O and 0.8 g Bi(NO 3 ) 3 ·5H 2 Dissolve O in 50 mL of water, add 5 mL of polyethylene glycol 400, quickly add 10 mL of concentrated ammonia water, and stir for 0.5 h. Add the copper-bismuth mixture to the above solution containing CTAB and ethyl orthosilicate, stir for 0.5 h, and then use 1 mol / LH 2 SO 4 Adjust the pH value to 9-10, stir at room temperature for 3-24 hours, then centrifuge, wash with distilled water and absolute ethanol several times, dry at room temperature, place in a high-temperature furnace and roast at 550°C for 5 hours to obtain a copper-bismuth / silica catalyst . The above-prepared catalyst was used for alkynylation reaction. After 7 hours of reaction, the conversion rate of formaldehyde was 67%, the selectivity of 1,4-butynediol was 90%, and the coppe...

Embodiment 3

[0014] Weigh 10.0 g of dodecylamine (DDA) and 25.0 g of tetraethylorthosilicate and dissolve them in 100 mL of ethanol solution. Then weigh 5.1 g CuCl 2 2H 2 O and 0.8 g Bi(NO 3 ) 3 ·5H 2 Dissolve O in 30 mL of water, add 5 mL of polyethylene glycol 400, quickly add 10 mL of concentrated ammonia water, and stir for 0.5 h. Add the copper-bismuth mixture to the above solution containing CTAB and ethyl orthosilicate, stir for 0.5 h, and then use 1 mol / LH 2 SO 4 Adjust the pH value to 9-10, stir at room temperature for 3-24 hours, then centrifuge, wash with distilled water and absolute ethanol several times, dry at room temperature, place in a high-temperature furnace and roast at 550°C for 5 hours to obtain a copper-bismuth / silica catalyst . The above-prepared catalyst was used for alkynylation reaction. After 7 hours of reaction, the conversion rate of formaldehyde was 60%, the selectivity of 1,4-butynediol was 94%, and the copper ion content in the filtrate after the rea...

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PUM

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Abstract

The invention relates to the preparation of a copper bismuth/silicon dioxide catalyst. It is characterized in that a copper-bismuth/silicon dioxide catalyst is prepared by a "one-pot method", the content of copper oxide is 10-40%, the content of bismuth is 1-10%, and the rest is silicon dioxide. Copper-bismuth species are highly dispersed on the inner and outer surfaces of silica, which improves the reaction center of the catalyst, enhances the wear resistance of the catalyst, and reduces the desolvation of copper ions. In the application of alkynylation reaction to synthesize 1,4-butynediol, the copper-bismuth catalyst has good activity, high selectivity, and low amount of copper species desolvation.

Description

technical field [0001] The invention relates to a copper-bismuth catalyst for producing 1,4-butynediol, which uses a "one-pot method" to prepare the copper-bismuth / silicon dioxide catalyst and its application in alkynylation. Background technique [0002] Copper-bismuth catalyst can catalyze acetylene and formaldehyde to generate 1,4-butynediol in the alkynylation reaction. 1,4-butynediol can be converted into 1,4-butanediol by hydrogenation reaction. 1,4-Butanediol is an important organic chemical raw material. A series of downstream chemical products can be prepared through reactions such as dehydrogenation and dehydration, such as polybutylene terephthalate (PBT), γ-butyrolactone (GBL ), polyurethane (PU), N-methylpyrrolidone (NMP), tetrahydrofuran (THF) and polytetramethylene glycol ether (PTMEG), etc. Due to the high industrial added value of 1,4-butanediol, its demand continues to grow. The industrial production process of 1,4-butynediol is mainly the improved alkyn...

Claims

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Application Information

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IPC IPC(8): B01J23/843C07C29/42C07C33/046
CPCB01J23/002B01J23/8437B01J2523/00C07C29/42
Inventor 杨桂花王吉德董长
Owner XINJIANG UNIVERSITY
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