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Preparing method of copper-silicon catalyst for preparing ethylene glycol by hydrogenating dimethyl oxalate

A technology of dimethyl oxalate and ethylene glycol, which is applied in the preparation of organic compounds, chemical instruments and methods, preparation of hydroxyl compounds, etc., can solve the problem of difficulty in producing copper phyllosilicate species, etc., and achieves good dispersibility and high Active, anti-agglomeration effect

Active Publication Date: 2016-06-22
厦门嘉氢科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the existing copper-silicon catalysts are difficult to produce copper phyllosilicate species and monovalent copper (Yin, A.Y., X.Y. Guo, etal. Applied Catalysis-General 2008, 349(1-2): 91-99.)

Method used

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  • Preparing method of copper-silicon catalyst for preparing ethylene glycol by hydrogenating dimethyl oxalate
  • Preparing method of copper-silicon catalyst for preparing ethylene glycol by hydrogenating dimethyl oxalate
  • Preparing method of copper-silicon catalyst for preparing ethylene glycol by hydrogenating dimethyl oxalate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] (1) Add silica sol to water to prepare a 1.5g / L silica sol solution, and obtain a dispersion of silica sol after ultrasonication for 10-30 minutes.

[0036] (2) Add ammonia water to the 0.08mol / L copper chloride aqueous solution, and control the concentration of ammonia water to 5mol / L to form a copper ammonium ion solution, stir for 10-30min, then add ammonium chloride, and control the chlorination The concentration of ammonium was 0.15mol / L to finally obtain a mixed solution of copper ammonium ions.

[0037] (3) Slowly add the silica sol dispersion obtained in step (1) dropwise to the copper ammine ion mixed solution obtained in step (2), and stir for 30 minutes to obtain a mixed solution of silica sol and copper ammonium ions.

[0038] (4) The mixed solution obtained in step (3) was transferred to a closed container, placed in a constant temperature environment of 150° C., and kept for 96 hours.

[0039] (5) Repeatedly wash the blue precipitate obtained in step (4) ...

Embodiment 2

[0044] (1) Add silica sol to water to prepare a 1.5g / L silica sol solution, and obtain a dispersion of silica sol after ultrasonication for 10-30 minutes.

[0045] (2) Add ammonia water to 0.04mol / L copper chloride aqueous solution, and control the concentration of ammonia water to 2.5mol / L to form a copper ammonium ion solution, stir for 10-30min, then add ammonium chloride, and control the concentration of chlorine The concentration of ammonium chloride is 0.15mol / L to finally obtain a mixed solution of copper ammonium complex ions.

[0046] (3) Slowly add the silica sol dispersion obtained in step (1) dropwise to the copper ammine ion mixed solution obtained in step (2), and stir for 30 minutes to obtain a mixed solution of silica sol and copper ammonium ions.

[0047] (4) The mixed solution obtained in step (3) was transferred to a closed container, placed in a constant temperature environment of 170° C., and kept for 72 hours.

[0048] (5) Repeatedly wash the blue precip...

Embodiment 3

[0053] (1) Add silica sol to water to prepare a 1.5g / L silica sol solution, and obtain a dispersion of silica sol after ultrasonication for 10-30 minutes.

[0054] (2) Add ammonia water to the 0.02mol / L copper chloride aqueous solution, and control the concentration of ammonia water to 10mol / L to form a copper ammonium ion solution, stir for 10-30min, then add ammonium chloride, and control the chlorination The concentration of ammonium was 0.15mol / L to finally obtain a mixed solution of copper ammonium ions.

[0055] (3) Slowly add the silica sol dispersion obtained in step (1) dropwise to the copper ammine ion mixed solution obtained in step (2), and stir for 30 minutes to obtain a mixed solution of silica sol and copper ammonium ions.

[0056] (4) The mixed solution obtained in step (3) was transferred to a closed container, placed in a constant temperature environment of 190° C., and kept for 48 hours.

[0057] (5) Repeatedly wash the blue precipitate obtained in step (4)...

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Abstract

The invention relates to copper-silicon catalysts, in particular to a preparing method of a copper-silicon catalyst for preparing ethylene glycol by hydrogenating dimethyl oxalate. The preparing method includes the steps that silica sol is added into water to obtain silica sol dispersion liquid; copper salt is dissolved in deionized water, ammonia water is added to form a copper-ammonia complex-ion solution, and then ammonia chloride is added to obtain a copper-ammonia complex-ion mixed solution; the silica sol dispersion liquid is added into the copper-ammonia complex-ion mixed solution to obtain a silica sol and copper-ammonia complex-ion mixed solution, the mixed solution is transferred into a closed container, the container is placed in a constant-temperature environment to obtain blue precipitate, blue powder is obtained through cleaning and then airing and dispersed into water again, and dispersion liquid of a mesoporous copper-silicon catalyst precursor is obtained after ultrasound treatment; the dispersion liquid is placed in a water bath, L-arginine and a cationic surface active agent are added into the dispersion liquid, and then tetraethoxysilane is added to obtain light blue precipitate; the light blue powder is obtained through cleaning, airing and heat treatment, and the cationic surface active agent is removed from the light blue powder to obtain the copper-silicon catalyst for preparing ethylene glycol by hydrogenating dimethyl oxalate.

Description

technical field [0001] The invention relates to a copper-silicon catalyst, in particular to a method for preparing a copper-silicon catalyst used for hydrogenation of dimethyl oxalate to ethylene glycol. Background technique [0002] As a widely used chemical product, ethylene glycol has been applied in the polyester industry, energy, fine chemicals, textiles, and automobile manufacturing. In recent years, with the development of my country's national economy, the market demand for ethylene glycol has grown rapidly. my country has become the world's largest consumer country, accounting for more than 30% of the world's total ethylene glycol consumption. At the same time, the contradiction between the rapid growth of my country's demand for ethylene glycol and the relative shortage of production capacity is becoming increasingly fierce. According to incomplete statistics, my country's demand for ethylene glycol in 2012 is expected to be about 9.5 million tons, but the domesti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/72C07C29/149C07C31/20
CPCY02P20/52B01J23/72B01J21/08C07C29/149C07C31/202
Inventor 郑南峰许潮发陈光需
Owner 厦门嘉氢科技有限公司
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