Catalyst for synthesizing methyl acetal and its preparation method and application

A catalyst, methylal technology, applied in the preparation of organic compounds, chemical instruments and methods, catalysts for physical/chemical processes, etc., can solve problems such as troublesome separation and purification, and achieve a simple preparation method, mild reaction conditions, and easy operation. Effect

Inactive Publication Date: 2009-12-09
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This will bring some troubles to the separation and purification of the product

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Add to 0.5mol / L Cu(NO 3 ) 2 Add 2.5 mol / L NaOH solution to the solution until the precipitation is complete, filter the solution, wash and dry the filter cake, and then calcinate at 300°C for 4 hours to obtain the carrier CuO. CuO powder was added to the 13.9% ammonium perrhenate solution for immersion for 15h. Then the catalyst was moved into an oven and dried at 90 °C for 30 h. Then the dried catalyst was pressed into tablets and ground, and granules of 20-40 mesh were taken and filled into a fixed-bed reactor. Under the protection of Ar, the temperature was raised to 300°C at a heating rate of 2°C / min, and after a constant temperature of 8 hours, When the temperature is lowered to 205°C, the reaction can be started by feeding the reaction gas. CH 3 OH%=4.0v%, GHSV=5.6×10 3 h -1 , The reactivity of the catalyst is shown in Table 2.

Embodiment 2

[0022] Add to 2.0mol / L Cu(NO 3 ) 2 Add 1.0 mol / L NaOH solution to the solution until the precipitation is complete, filter the solution, wash and dry the filter cake, and then calcinate at 360° C. for 3 h to obtain the carrier CuO. CuO powder was added to the 12.5% ​​ammonium perrhenate solution for immersion for 12h. Then the catalyst was moved into an oven and dried at 70 °C for 30 h. Then the dried catalyst was pressed into tablets and ground, and the particles of 20-40 mesh were taken and filled into a fixed-bed reactor. Under the protection of Ar, the temperature was raised to 400°C at a heating rate of 8°C / min, and after a constant temperature of 3 hours, When the temperature is lowered to 220°C, the reaction can be started by feeding the reaction gas. CH 3 OH%=5.0v%, GHSV=1.12×10 4 h -1 , The reactivity of the catalyst is shown in Table 2.

Embodiment 3

[0024] Add to 1.5mol / L Cu(NO 3 ) 2 Add 2.0 mol / L NaOH solution to the solution until the precipitation is complete, filter the solution, wash and dry the filter cake, and then calcinate at 400° C. for 2 h to obtain the carrier CuO. CuO powder was added to 15.2% ammonium perrhenate solution for immersion for 15h. Then the catalyst was moved into an oven and dried at 60 °C for 48 h. Then the dried catalyst was pressed into tablets and ground, and the particles of 20-40 mesh were taken and filled into a fixed-bed reactor. Under the protection of Ar, the temperature was raised to 360°C at a heating rate of 6°C / min. After constant temperature for 6 hours, down to 205°C, adjust methanol feed rate and Ar rate, CH 3 OH%=7.7v%, GHSV=1.68×10 4 h -1 , The reactivity of the catalyst is shown in Table 2.

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PUM

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Abstract

A catalyst for synthesizing methylal is composed of ReOx and CuO, wherein the mass percentage of Re element on the catalyst is 5.56-10.5%. Add NaOH solution to the Cu(NO3)2 solution under stirring until the precipitation is complete, filter, and the filter cake is washed, dried and roasted to obtain the carrier CuO; the ammonium perrhenate is made into a product with a mass concentration between 10.0 and 17.6%. The aqueous solution is used to immerse the CuO powder in an equal volume for 12-18 hours, dried, pressed into tablets, and ground, and the particles of 20-40 meshes are used as catalysts. The preparation method of the catalyst provided by the invention is simple and easy to operate. Realized the advantages of methanol dehydrogenation under anaerobic conditions to obtain methylal and mild reaction conditions.

Description

technical field [0001] The invention belongs to a solid catalyst for synthesizing methylal by direct dehydrogenation of methanol, a preparation method and an application. Background technique [0002] Compared with tert-butyl methyl ether, as an oil additive, methylal not only has a high oxygen content, is not limited by the production of isobutylene, and has no environmental problems; in addition, it is also a good choice in cosmetics, pharmaceuticals, paints and rubber industries. organic solvents; as a cleaning agent, methylal can replace chlorinated solvents and reduce the emission of volatile organic compounds; methylal can also be used to synthesize high-purity formaldehyde. [0003] The traditional industrial methylal synthesis process is mainly divided into two steps starting from methanol. First, methanol is oxidized to formaldehyde, and then methanol and formaldehyde are condensed to form methylal. The former step is catalyzed by silver (600-650°C) or iron-molybde...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/889C07C43/303C07C41/50
Inventor 孙予罕魏伟曹虎管莲秀赵宁
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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