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Catalyst Activation Method for Hydrogenation of Oxalate to Glycolate

A technology of glycolate ester and activation method, which is applied in the direction of carboxylate ester preparation, molecular sieve catalyst, chemical instrument and method, etc., and can solve the problems of low glycolate ester selectivity and large grain size of active components, etc.

Active Publication Date: 2018-02-13
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The technical problem to be solved by the present invention is that there are technical problems in the prior art that the active component of the catalyst for hydrogenation of oxalate to glycolate has a large grain size and low selectivity of glycolate. A new oxalate is provided Catalyst activation method for hydrogenation of methyl glycolate

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Take 800g of silica and alumina mixed carrier, which contains 90% of silica. According to the composition of the catalyst, 10 parts of silver, 2 parts of copper and 88 parts of carrier were prepared to impregnate equal volumes of impregnation solution on the carrier, left to age for 10 hours, and dried at 80° C. to obtain a catalyst precursor. Take 25g of the catalyst precursor and put it into the tubular activation furnace. Under the atmosphere condition of a mixture of oxygen and nitrogen, wherein the oxygen volume content is 8%, the temperature is raised to 150°C at a controlled temperature of 1.5°C / min for 50 minutes, and then the temperature is increased at 1°C / min. The temperature was programmed to rise to 350°C in minutes and kept at a constant temperature for 200 minutes. After the heat treatment, the catalyst is naturally cooled to room temperature, and the reactor is replaced with hydrogen, and then the hydrogen volume space velocity is 3000 hours. -1 Under t...

Embodiment 2

[0032] Take 25g of the catalyst precursor prepared in Example 1) and put it into a tubular activation furnace, change the atmosphere of the staged heat treatment to air, and control the temperature at 1.5°C / min to 150°C for 50 minutes at a constant temperature, and then program at 1°C / min Raise the temperature to 350°C and keep the temperature constant for 200 minutes. After the heat treatment is over, take 20g of the catalyst and put it into the reactor after the catalyst is naturally lowered to room temperature. When the hydrogen volume space velocity is 3000 hours -1 Under the conditions, the temperature is controlled to rise to 180° C. at 1° C. / min, and the temperature is kept constant for 240 minutes. After activation, a catalyst for synthesizing methyl glycolate is obtained. The catalyst was taken as a scanning electron microscope to test the average particle size of the silver grains, and the test results are shown in Table 1. And take 10g of catalyst and put it into t...

Embodiment 3

[0034]Get 25g of the catalyst precursor prepared in Example 1) and put it into a tube-type activation furnace. Under the atmosphere condition of oxygen and argon mixture, wherein the oxygen volume content is 1%, the temperature is raised to 150°C at a constant temperature of 50°C by controlling 1.5°C / min. Minutes, then the temperature was programmed to rise to 500°C at 1°C / min, and kept at a constant temperature for 200 minutes. After the heat treatment is over, take 20g of the catalyst and put it into the reactor after the catalyst is naturally lowered to room temperature. When the hydrogen volume space velocity is 3000 hours -1 Under the conditions, the temperature is controlled to rise to 180° C. at 1° C. / min, and the temperature is kept constant for 240 minutes. After activation, a catalyst for synthesizing methyl glycolate is obtained. The catalyst was taken as a scanning electron microscope to test the average particle size of the silver grains, and the test results are ...

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Abstract

The invention relates to an activation method of a catalyst for hydrogenating oxalate to glycolate, which mainly solves the problems of large noble metal particles on the surface of a catalyst carrier and low selectivity of methyl glycolate in the prior art. The present invention adopts the technical scheme of heat-treating the impregnated and dried catalyst precursor containing silver and silicon dioxide in stages under an atmosphere of oxygen-containing gas, and then performing temperature-programmed reduction with hydrogen or hydrogen-containing inert gas, preferably The problem is solved, and the method can be used in the industrial production of the catalyst for hydrogenating oxalate to methyl glycolate.

Description

technical field [0001] The invention relates to an activation method for a catalyst for hydrogenating oxalate to glycolate, in particular to an activation method for a catalyst for hydrogenating oxalate to produce methyl glycolate. Background technique [0002] Due to its unique molecular structure and the chemical properties of both alcohols and esters, methyl glycolate can undergo carbonylation reactions, hydrolysis reactions, oxidation reactions, etc., and has become an important chemical raw material. It can be widely used in many fields such as chemical industry, medicine, pesticide, feed, spices and fuel. [0003] Due to the wide application and high market demand of methyl glycolate, there are many researches on its synthesis process at home and abroad, mainly including one-step synthesis method of glyoxal and methanol, formaldehyde carbonylation monoester synthesis method, ester methylal and formic acid Method, coupling method, chloroacetic acid method, formaldehyde...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/89B01J29/00C07C69/675C07C67/31
Inventor 龚海燕宋海峰
Owner CHINA PETROLEUM & CHEM CORP