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A novel acetylenylation catalyst for synthesizing 1,4-butynediol and its preparation method

A technology of butynediol and catalyst, which is applied in the direction of catalyst activation/preparation, preparation of organic compounds, physical/chemical process catalysts, etc., which can solve the problems of easy formation of catalysts and loss of copper ions, etc., and inhibit the formation of surface polymers , low preparation cost, good wear resistance

Active Publication Date: 2020-07-14
XIAN SUNWARD AEROSPACE MATERIAL CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] In order to solve the shortcomings of existing catalysts used in the synthesis of 1,4-butynediol, which have the disadvantages of copper ion loss and easy formation of polymers on the surface of the catalyst, the present invention provides a novel acetylenization catalyst for synthesizing 1,4-butynediol and Its preparation method, the acetylenization catalyst has the characteristics of high activity, high selectivity, good wear resistance, less loss of copper ions, can inhibit the formation of catalytic reaction polymer, and easy separation of catalyst and product

Method used

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  • A novel acetylenylation catalyst for synthesizing 1,4-butynediol and its preparation method
  • A novel acetylenylation catalyst for synthesizing 1,4-butynediol and its preparation method

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Embodiment 1

[0034] 260g of silica sol was uniformly dispersed in 2L of distilled water to obtain an aqueous solution of silica sol; 500g of copper nitrate, 23g of bismuth nitrate and 160g of magnesium nitrate were dissolved in 500mL of 8% nitric acid aqueous solution; under stirring conditions, the salt solution and The aqueous solution of the silicon source material is added dropwise to water for reaction at the same time, and the pH value of the reaction is adjusted to 4-5 by using nitric acid and sodium hydroxide, wherein the molar ratio of Si atoms to Cu atoms, Bi atoms, and Mg atoms is 1:0.98:0.02: 0.6, add mass fraction again and be 30% sodium carbonate aqueous solution, make the pH value of the suspension that obtains be 7.0~8.0, continue to stir for 1 hour, leave standstill for 12 hours, the precipitate that separates out is filtered, washed with distilled water, and then The precipitate was re-pulped and placed in a hydrothermal kettle for hydrothermal treatment at 180°C for 50 ho...

Embodiment 2

[0037] 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 an aqueous nitric acid solution with a mass fraction of 8%, and mix the salt solution and silicon The aqueous solution of the source material is added dropwise to the water for reaction at the same time, and the pH value of the reaction is controlled at 4 to 5, wherein the molar ratio of Si atoms to Cu atoms, Bi atoms, and Mg atoms is 1:0.90:0.05:0.28, and the mass fraction is 23 % sodium hydroxide aqueous solution to neutralize to a pH value of 7.0 to 8.0, continue stirring for 1 hour, and let stand for 12 hours. After hydrothermal treatment at 180°C for 30 hours, the precipitate was filtered, dried at 150°C, and then calcined in a muffle furnace at 400°C for 10 hours to prepare an acetylation catalyst for the synthesis of 1,4-butynediol.

[0038] The obtained al...

Embodiment 3

[0040] Weigh 1220g ethyl orthosilicate and dissolve it in 15L water to obtain an aqueous solution of ethyl orthosilicate; dissolve 180g of magnesium nitrate, 50g of bismuth nitrate, and 900g of copper nitrate in 1L of 8% nitric acid aqueous solution, and dissolve the salt under stirring. The solution and the aqueous solution of the silicon source material are added dropwise to water for reaction at the same time, and the pH value of the reaction is controlled at 4 to 5, wherein the molar ratio of Si atoms to Cu atoms, Bi atoms, and Mg atoms is 1:0.86:0.024:0.10, and then used The mass fraction is 30% sodium carbonate solution and neutralized to pH value of 6.5-7.0, continue to stir for 1 hour, let it stand for 12 hours, the precipitate is filtered, washed with distilled water, and then the precipitate is re-pulped and placed in water Hydrothermal treatment at 150°C for 45 hours in a hot kettle, then filter the precipitate, dry it at 150°C, and bake it in a muffle furnace at 470...

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Abstract

The invention specifically relates to a new type of alkynylation catalyst for synthesizing 1,4-butynediol and its preparation method. The alkynylation catalyst is a homogeneous copper silicate structure and is doped with a trace amount of Bi. 2 O 3 and MgO, the particle size distribution is: 10% of particles less than or equal to 12 μm, 80% of particles of 12 to 35 μm, and 10% of particles of greater than or equal to 35 μm. The compacted bulk density of the alkynylation catalyst is 2.2 to 2.5 kg. / L. The preparation method of the catalyst mainly includes the following steps: under stirring conditions, soluble salt solutions of Cu, Bi, and Mg and an aqueous solution of silicon source materials are simultaneously dropped into a nitric acid aqueous solution for reaction, and the product is filtered and washed; The precipitate is re-pulped, and the obtained slurry is subjected to hydrothermal treatment, filtered, dried, and roasted to prepare the catalyst. The catalyst of the present invention has the characteristics of high activity, high selectivity, good wear resistance, low copper ion loss, can inhibit the formation of catalytic reaction polymers, easy separation of the catalyst and the product, and has a significantly increased service life.

Description

technical field [0001] The invention belongs to the technical field of synthesis of 1,4-butynediol, and in particular relates to a novel acetylenization catalyst for synthesizing 1,4-butynediol and a preparation method thereof. Background technique [0002] The catalysts used to produce 1,4-butynediol by the alkyne aldehyde method are mainly copper-bismuth catalysts, and copper-bismuth catalysts mainly include supported and unsupported catalysts. [0003] For CuO-Bi 2 o 3 The research on supported catalysts mainly focuses on the screening of supports. For example, US2232867, US4002694, US3920759, US3294849, etc. disclose their respective supported copper-based catalysts. Due to the existence of the carrier, this kind of catalyst can increase the dispersion degree of the active component and the wear resistance of the catalyst. But since the carrier is made of SiO 2 、Al 2 o 3 etc., there is a strong interaction between the active component Cu and the support, which make...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/843B01J35/02B01J37/10C07C29/42C07C33/046B01J35/00
CPCC07C29/42B01J23/002B01J23/8437B01J37/10B01J35/40C07C33/046
Inventor 封超彭东徐成华侯亚楠王国妮卫冰赵少丹
Owner XIAN SUNWARD AEROSPACE MATERIAL CO LTD
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