Dimethyl oxalate hydrogenation catalyst as well as preparation method and application thereof

A technology of dimethyl oxalate and hydrogenation catalyst, which is applied in the direction of carboxylate preparation, metal/metal oxide/metal hydroxide catalyst, heterogeneous catalyst chemical elements, etc., which can solve the complicated process and complicated preparation method And other issues

Pending Publication Date: 2022-02-18
CHINA CATALYST HLDG CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The problem that these prior art exists is: preparation method is complicated, uses different catalysts when making ethylene glycol and making methyl glycolate, causes process complication

Method used

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  • Dimethyl oxalate hydrogenation catalyst as well as preparation method and application thereof
  • Dimethyl oxalate hydrogenation catalyst as well as preparation method and application thereof

Examples

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preparation example Construction

[0043] The present inventor also provides the preparation method of this catalyzer, adopts ammonia distillation method (supporting copper operation) and impregnation method (supporting M operation) to synthesize this catalyzer, specifically comprises the following steps:

[0044] 1), at 20-30°C, an aqueous solution made of soluble copper salt; after adding ammonia water, it becomes a copper-ammonia complex solution

[0045] 2), at 20-30°C, add silica sol and cuproammonia solution dropwise at the same time; after the dropwise addition is completed, heat up to deamination until the pH value of the slurry in the kettle is 6-7;

[0046] 3), filtering, washing the filter cake with water, drying, and roasting to obtain the roasted precursor CuO / SiO 2 ;and

[0047] 4) Configure a co-active component metal salt solution with a mass fraction of 0.1-5%, and quickly add the roasted precursor CuO / SiO 2 , impregnated at room temperature for 2-24h, dried, roasted, and reduced to obtain a ...

Embodiment 1

[0062] Precursor preparation: Weigh 60.74g of copper nitrate trihydrate and 265g of water to dissolve, add 205g of 20.88% ammonia water to form a copper-ammonia complex solution, weigh 533.3g of 15% silica sol solution, and co-feed at 10g / min The method is to drop the two materials of copper ammonia complex solution and silica sol solution into the kettle respectively. After the dropping is completed, the temperature is raised to deamination until the pH value of the slurry in the kettle is between 6-7, filtered, and dried at 120°C for 12h, 400°C After calcination at ℃ for 6h, the catalyst precursor 20.0% CuO / SiO was obtained 2 (Meaning: CuO mass content accounts for the precursor (CuO and SiO 2 ) percentage of the total mass, the following examples have the same meaning; in addition, the catalyst precursor here is also referred to as "calcined precursor" in this application).

[0063] Catalyst preparation: Weigh 0.51g of platinum chloride to prepare an aqueous solution with ...

Embodiment 2

[0066] Precursor preparation: Weigh 75.93g of copper nitrate trihydrate and 545g of water to dissolve, add 267g of 20.88% ammonia water to configure a copper-ammonia complex solution, weigh 883g of 8.5% silica sol solution, and feed it at 10g / min Add copper ammonia complex solution and silica sol solution dropwise. After the dropwise addition, raise the temperature to deamination until the pH value of the slurry in the kettle is between 6-7, filter, dry at 120°C for 12 hours, and roast at 400°C for 6 hours. Obtain catalyst precursor 25.0wt% CuO / SiO 2 .

[0067] Catalyst preparation: Dissolve 0.56g of palladium chloride in 100g of 1% hydrochloric acid aqueous solution, add 20g of precursor, and age at room temperature for 12h; dry at 120°C for 12h, and roast at 400°C for 4h to obtain a catalyst with an atomic ratio of Pd and Cu of 0.05. Catalyst 2: Contains 1.93 wt% PdO-25.0 wt% CuO.

[0068] Ethylene glycol synthesis: place the catalyst in a fixed-bed reactor, set the hydrog...

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Abstract

The invention provides a dimethyl oxalate hydrogenation catalyst as well as a preparation method and application thereof. The dimethyl oxalate hydrogenation catalyst contains a precursor and an auxiliary active component, wherein the precursor is Cu / SiO2, Cu is a main active component, SiO2 is a carrier, an auxiliary active component is M and / or M oxide, and the atomic ratio of the auxiliary active component M to the main active component Cu is 0.01-0.2 based on the atomic ratio of metal. The dimethyl oxalate hydrogenation catalyst is synthesized by adopting an ammonia distillation method and an impregnation method. The catalyst provided by the invention solves the problem that a byproduct 1,2-butanediol which is difficult to separate is generated in the process of synthesizing ethylene glycol by hydrogenation of dimethyl oxalate, and the service life of the catalyst is prolonged. More importantly, by adjusting the proportion of each component in the catalyst and the reaction conditions of dimethyl oxalate hydrogenation, the variety of products can be controlled, high-selectivity methyl glycolate or ethylene glycol can be independently obtained, and switching production of the above products is facilitated in industrial practical application.

Description

technical field [0001] The invention relates to a dimethyl oxalate hydrogenation catalyst, its preparation method and application, and relates to the technical field of coal chemical catalysts. Background technique [0002] Due to its unique molecular structure and the chemical properties of alcohol and ester, methyl glycolate can undergo carbonylation reaction, hydrolysis reaction, oxidation reaction, etc., and is an important chemical raw material. It can be widely used in many fields such as chemical industry, medicine, pesticide, feed, spices and fuel. In particular, methyl glycolate can be used as the raw material of degradable plastics. With the rapid development and application of degradable plastics, the market demand for methyl glycolate is growing rapidly. [0003] Ethylene glycol is a valuable industrial chemical. Ethylene glycol (EG) is an important basic organic raw material for petrochemicals, mainly used to produce polyester fibers, antifreeze agents, and uns...

Claims

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Application Information

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IPC IPC(8): B01J23/89C07C29/149C07C67/31C07C69/675C07C31/20
CPCB01J23/002B01J23/8926C07C29/149C07C67/31B01J2523/00B01J2523/17B01J2523/41B01J2523/828B01J2523/822B01J2523/18B01J2523/19B01J2523/821C07C31/202C07C69/675Y02P20/52
Inventor 王蕊王庆吉李进王炳春孙红影王贤彬
Owner CHINA CATALYST HLDG CO LTD
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