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Preparation method of Ru/C catalyst and glycerine hydrogenolysis method

A catalyst, glycerol technology, applied in the preparation of organic compounds, physical/chemical process catalysts, chemical instruments and methods, etc., can solve the problems of limited service life of catalysts, poor catalyst stability, complicated production operations, etc., and achieve outstanding activity stability. , good stability, the effect of reducing production costs

Active Publication Date: 2015-04-15
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Ru / C is more suitable for reacting in an aqueous solution, but because the aqueous solution of the reaction raw material contains a certain amount of alkali, the pH value is generally 9-11, and the Ru / C catalyst prepared by the existing method has poor stability in such a medium. The conversion rate will decrease with time, so the service life of the catalyst is limited. In order to maintain a certain catalytic activity, the catalyst needs to be replaced frequently, which makes the production operation complicated and the cost increases
Experiments have shown that the higher the alkali content in the reaction raw materials, the worse the stability of the catalyst

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0015] The preparation method of the glycerin hydrogenolysis catalyst of the present invention adopts ruthenium as the active component, activated carbon as the carrier, completes the loading of the active component by the exchange method, and then reduces it with a chemical reagent (formaldehyde or hydrazine hydrate), which is comparable to other preparation methods. Compared with this Ru / C catalyst, it can maintain better activity stability in alkaline raw materials. Compared with the copper catalyst, it is more suitable for dilute glycerol with higher water content as raw material, and can obtain better hydrogenolysis effect in the gas-liquid-solid three-phase reaction with relatively mild conditions. The active component ruthenium used is generally RuCl 3 ·xH 2 O, the carrier activated carbon is coconut shell activated carbon, etc. In order to better disperse the active components on the surface of the carrier, the carrier can be ground into a fine powder of 40-80 mesh. ...

Embodiment 1

[0018] Weigh 0.99gRuCl 3. wxya 2 O (containing Ru37.5-40%), after adding deionized water to dissolve, adjust the pH to 1 with hydrochloric acid, add 8g of activated carbon, and let it stand for 12 hours. Heat in a water bath at about 45°C, and at the same time adjust the pH to 9 with 4% NaOH aqueous solution, add 15ml of formaldehyde solution, heat to 80°C, and stir and reflux for 4 hours. After cooling to room temperature, wash with deionized water until neutral and free of Cl - ion (with 0.1M AgNO 3Aqueous solution inspection), obtain Ru / C catalyst, Ru content is about 4.7%.

Embodiment 2

[0020] Weigh 0.49gRuCl 3. wxya 2 O (containing Ru37.5-40%), after adding deionized water to dissolve, adjust the pH to 2 with hydrochloric acid, add 8g of activated carbon, and let it stand for 2 hours. Heat in a water bath at about 60°C, and at the same time adjust the pH to 11 with 4% NaOH aqueous solution, add 10ml of formaldehyde solution, heat to 90°C, and stir and reflux for 2 hours. After cooling to room temperature, it was washed with deionized water until neutral to obtain a Ru / C catalyst with a Ru content of about 2.3%.

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Abstract

The invention discloses a preparation method of a Ru / C catalyst and a glycerine hydrogenolysis method. The Ru / C catalyst uses active carbon as a carrier and Ru as an active component. The preparation method comprises the steps of: with a RuCl3 water solution as an exchange solution, loading RuCl3 on the carrier by using an exchange method; and with formaldehyde or hydrazine hydrate as a reducing agent, completing the reduction reaction under the alkaline condition to obtain the Ru / C catalyst. When the Ru / C catalyst is used in the glycerine hydrogenolysis reaction, the transformation rate of glycerine is high, the selectivity of dihydric alcohol is good, and the stability of the catalyst in a reaction medium is good; and the Ru / C catalyst is especially suitable for the hydrogenolysis reaction of dilute glycerine with high water content.

Description

technical field [0001] The invention relates to a preparation method of a Ru / C catalyst and a method for preparing diols by hydrogenolysis of glycerin. Ru / C is selected as a catalyst to hydrogenolyze glycerol into low molecular weight diols such as propylene glycol and ethylene glycol. Background technique [0002] The traditional production method of chemical alcohol is based on petroleum as raw material, and is prepared through a series of chemical processes (the most important of which is oxidation reaction). For example, the production of ethylene glycol from ethylene oxide and the production of propylene glycol from propylene oxide consume a large amount of petroleum products every year. Due to the shortage of petroleum resources and the non-renewability of petroleum, it is the development direction of this field to replace petroleum with renewable resources to produce polyhydric alcohols. For example, glycerin can be hydrogenated under high temperature and high pressu...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/46C07C31/20C07C29/60C07C29/00
Inventor 苏杰陈明李风华
Owner CHINA PETROLEUM & CHEM CORP