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Preparation method of copper silicon catalyst for hydrogenation of dimethyl oxalate to ethylene glycol

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 that it is difficult to produce copper phyllosilicate species, achieve high conversion rate, high active effect

Active Publication Date: 2017-11-07
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, et al. Applied Catalysis a-General 2008,349(1-2):91-99.)

Method used

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  • Preparation method of copper silicon catalyst for hydrogenation of dimethyl oxalate to ethylene glycol
  • Preparation method of copper silicon catalyst for hydrogenation of dimethyl oxalate to ethylene glycol
  • Preparation method of copper silicon catalyst for hydrogenation of dimethyl oxalate to ethylene glycol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] (1) The silica sol is added to water to prepare a 1.5g / L silica sol solution, and the silica sol dispersion is obtained after 10-30 minutes of ultrasound.

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

[0037] (3) The silica sol dispersion obtained in step (1) is slowly added dropwise to the cupramide ion mixed solution obtained in step (2), and a mixed solution of silica sol and cupramide ion is obtained after stirring for 30 minutes.

[0038] (4) Transfer the mixed solution obtained in step (3) to a closed container, place it in a constant temperature environment of 150° C., and keep it for 96 hours.

[0039] (5) The blue precipitate obtained in step (4) is repeatedl...

Embodiment 2

[0044] (1) The silica sol is added to water to prepare a 1.5g / L silica sol solution, and the silica sol dispersion is obtained after 10-30 minutes of ultrasound.

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

[0046] (3) The silica sol dispersion obtained in step (1) is slowly added dropwise to the cupramide ion mixed solution obtained in step (2), and a mixed solution of silica sol and cupramide ion is obtained after stirring for 30 minutes.

[0047] (4) Transfer the mixed solution obtained in step (3) to a closed container, place it in a constant temperature environment of 170° C., and keep it for 72 hours.

[0048] (5) The blue precipitate obtained in step (4) is re...

Embodiment 3

[0053] (1) The silica sol is added to water to prepare a 1.5g / L silica sol solution, and the silica sol dispersion is obtained after 10-30 minutes of ultrasound.

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

[0055] (3) The silica sol dispersion obtained in step (1) is slowly added dropwise to the cupramide ion mixed solution obtained in step (2), and a mixed solution of silica sol and cupramide ion is obtained after stirring for 30 minutes.

[0056] (4) Transfer the mixed solution obtained in step (3) to a closed container, place it in a constant temperature environment at 190°C, and keep it for 48 hours.

[0057] (5) The blue precipitate obtained in step (4) is repeat...

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Abstract

The invention discloses a preparation method of a copper-silicon catalyst used for hydrogenation of dimethyl oxalate to ethylene glycol, relating to the copper-silicon catalyst. Add silica sol to water to obtain silica sol dispersion; dissolve copper salt in deionized water, add ammonia water to form copper ammonium ion solution, and then add ammonium chloride to obtain copper ammonium ion mixed solution; add silica sol dispersion to copper A mixed solution of ammonium ions to obtain a mixed solution of silica sol and copper ammonium ions, then transferred to a closed container, placed in a constant temperature environment, to obtain a blue precipitate, washed and dried to obtain a blue powder, and then dispersed in water, Obtain the dispersion of the mesoporous copper-silicon catalyst precursor after ultrasonication; then place it in a water bath, add L-arginine and cationic surfactant to the dispersion, and then add ethyl orthosilicate to obtain a light blue precipitate; After washing and drying, a light blue powder is obtained. After heat treatment, the cationic surfactant is removed from the light blue powder to obtain a copper-silicon catalyst for hydrogenation of dimethyl oxalate to ethylene glycol.

Description

Technical field [0001] The invention relates to a copper-silicon catalyst, in particular to a method for preparing a copper-silicon catalyst for hydrogenating dimethyl oxalate to prepare ethylene glycol. Background technique [0002] As a widely used chemical product, ethylene glycol has been applied in 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 number one consumer, 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 relatively insufficient production capacity has become increasingly fierce. According to incomplete statistics, my country's ethylene glycol demand in 2012 is expected to be around 9.5 million tons, but domestic production is abo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/72C07C29/149C07C31/20
CPCY02P20/52
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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