Ethynylation catalyst for synthesizing 1, 4-butynediol

A technology of butynediol and catalyst, applied in the field of acetylenic catalyst, can solve the problems of high production cost of 1,4-butynediol, short service life of catalyst, high price of catalyst, etc., and achieves remarkable economic and technical performance, The effect of strong stability and a wide range of operating conditions

Active Publication Date: 2014-03-19
XIAN SUNWARD AEROSPACE MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

More importantly, the catalyst is severely worn during use, and the active components are lost, resulting in a shorter service life of the catalyst
[0005] At present, the synthesis of 1,4-butynediol by domestic alkynylation uses the DuPont process and catalyst, and the catalyst is expensive, resulting in high production costs of 1,4-butynediol

Method used

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  • Ethynylation catalyst for synthesizing 1, 4-butynediol

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Embodiment 1

[0016] Disperse 260g of silica sol evenly in 2L of distilled water to obtain an aqueous solution of silica sol; dissolve 500g of copper nitrate, 23g of bismuth nitrate and 160g of magnesium nitrate in 500mL of 10% nitric acid aqueous solution, and slowly add silicon dropwise under stirring. In the sol aqueous solution, the molar ratio of Si atoms to Cu atoms, Bi atoms, and Mg atoms is 1:0.98:0.022:0.3, and a 30% sodium carbonate aqueous solution is added to make the pH of the resulting suspension 6.5 ~ 7.0, continue to stir for 1 hour, let stand for 12 hours, the precipitated precipitate is filtered, washed with distilled water, and dried at 150°C, then placed in a muffle furnace at 500°C for 6 hours to prepare it for synthesis of 1,4- The catalyst for acetylation of butynediol. The particle size distribution of the obtained catalyst is obtained by physical sieving and weighing method: 9% of particles smaller than or equal to 0.710μm, 80% of particles smaller than or equal to 0....

Embodiment 2

[0018] Weigh 1000g of sodium silicate and dissolve it in 10L of water to obtain an aqueous solution of sodium silicate; dissolve 540g of copper chloride, 49g of bismuth nitrate, and 150g of magnesium nitrate in 1L of nitric acid with a mass fraction of 10%. The resulting mixture is stirred under stirring conditions. Drop into the sodium silicate aqueous solution, where the molar ratio of Si atoms to Cu atoms, Bi atoms, and Mg atoms is 1:0.90:0.048:0.28, and neutralize to the pH value with a 23% sodium hydroxide aqueous solution. 6.5 ~ 7.0, continue to stir for 1 hour, let stand for 12 hours, the precipitated precipitate is filtered, washed with distilled water, dried at 150°C, and then placed in a muffle furnace at 460°C for 6 hours to prepare it for synthesis of 1,4- Catalyst for acetylation of butynediol.

Embodiment 3

[0020] Weigh 1220g of sodium silicate and dissolve it in 15L of water to obtain an aqueous solution of sodium silicate; dissolve 180g of magnesium nitrate, 50g of bismuth nitrate, and 900g of copper nitrate in 1L of 10% aqueous nitric acid solution. The resulting mixture is slowly stirred under stirring conditions. Drop into the sodium silicate aqueous solution, where the molar ratio of Si atoms to Cu atoms, Bi atoms, and Mg atoms is 1:0.86:0.024:0.16, and then neutralize to pH value with 30% sodium carbonate in water 6.5 ~ 7.0, after stirring for 1 hour, let stand for 12 hours, the precipitated precipitate is filtered, washed with distilled water, dried at 150°C, and calcined in a muffle furnace at 350°C for 6 hours to prepare it for synthesis 1,4 -Butynediol acetylation catalyst.

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Abstract

The invention discloses an ethynylation catalyst for synthesizing 1, 4-butynediol. The ethynylation catalyst is composite oxide of Cu, Bi, Si and Mg, and has the particle size distribution that the particles with the particle sizes less than or equal to 0.710 mum account for 9%, the particles with the particle sizes of 0.711-1.589 mum account for 80%, and the particles with the particle sizes more than or equal to 1.590 mum account for 11%; the ethynylation catalyst is prepared by a coprecipitation method or an impregnation-precipitation method. The ethynylation catalyst is used for synthesizing the 1, 4-butynediol in an ethynylation reaction of formaldehyde and acetylene, and is high in catalytic activity; the conversion rate of the formaldehyde reaches up to more than 97.0%, the selectivity of the 1, 4-butynediol reaches up to more than 98.7%, and the yield of the 1, 4-butynediol reaches 96.2%; furthermore, the ethynylation catalyst is long in service life.

Description

Technical field [0001] The invention belongs to the technical field of synthesis of 1,4-butynediol, and specifically relates to an acetylation catalyst for synthesizing 1,4-butynediol through a three-phase reaction of formaldehyde and acetylene. Background technique [0002] The main catalysts used for the production of 1,4-butynediol by the acetylene aldehyde method are copper-bismuth catalysts. Copper-bismuth catalysts mainly include supported and unsupported catalysts. [0003] For CuO-Bi 2 O 3 / Supported catalyst research mainly focuses on the screening of supports, for example, US2232867, US4002694, US3920759, US3294849, etc. disclose respective supported copper-based catalysts. This type of catalyst can increase the dispersion of active components and the wear resistance of the catalyst due to the existence of the carrier. But because the carrier is SiO 2 , Al 2 O 3 Etc., there is a strong interaction between the active component Cu and the support, which makes it difficult ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/843C07C33/046C07C29/42
Inventor 彭东徐成华封超
Owner XIAN SUNWARD AEROSPACE MATERIAL CO LTD
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