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Catalyst for use in preparation of 1,2-propanediol by low-temperature low-pressure hydrogenation of biological glycerol and preparation method thereof

A low-temperature, low-pressure, bio-glycerin technology, applied in the chemical industry, can solve the problems of difficult separation of acetol and catalysts, complex 1,2-propanediol process, etc., and achieve the effects of industrial application, good low-temperature activity, and high activity

Inactive Publication Date: 2012-03-28
HAO HUA CHENGDU TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The two-step method for preparing 1,2-propanediol is relatively complicated, especially in the first stage of the reaction, it is difficult to separate the intermediate product acetol from the catalyst
[0007] There are few domestic research reports on the process and catalyst of bioglycerol hydrogenation to 1,2-propanediol

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Weigh 25g Cu(NO 3 ) 2 and 1.5g Ni(NO 3 ) 2 Add deionized water to prepare 200mL mixed salt solution, heat and keep at 50°C. Under stirring conditions, add 41g of sodium silicate solution dropwise to control the pH value of the solution at the end of the reaction to 7.0; after the reaction is completed, the feed liquid is filtered while it is hot, and then washed with deionized water for three times and suction filtered; After drying for 12 hours at 380°C, it was calcined at 380°C for 6 hours to finally obtain a catalyst sample. Put 15ml of the catalyst sample of 20-40 mesh after molding and screening into the reaction tube, use pure hydrogen with a flow rate of 100mL / min, reduce it at 250°C for 6 hours, adjust to the reaction process conditions for hydrogenation reaction, and after 5 hours of hydrogenation reaction Sampling and analysis by gas chromatography showed that the conversion rate of glycerin reached 100%, and the selectivity of 1,2-propanediol was 98.2%. ...

Embodiment 2

[0030] Weigh 28g Cu(NO 3 ) 2 and 1.45g Mn(NO 3 ) 2 Add deionized water to prepare a mixed salt solution with a concentration of 0.2M, heat and keep at 70°C. Under stirring conditions, slowly drop 75.8g of silica sol into the salt solution until the pH value of the solution at the end of the reaction is 7.0; after the reaction is completed, the feed solution is filtered while it is hot, and then washed with deionized water for three times and suction filtered; the catalyst After drying at 90°C for 12 hours, it was calcined at 500°C for 6 hours to finally obtain a catalyst sample. Put 15ml of the catalyst sample of 20-40 mesh after molding and screening into the reaction tube, use pure hydrogen with a flow rate of 100mL / min, reduce it at 280°C for 6 hours, adjust to the reaction process conditions to carry out hydrogenation reaction, after hydrogenation reaction for 5 hours Sampling, the result of gas chromatographic analysis shows that the conversion rate of glycerin is 99....

Embodiment 3

[0032] Weigh 28g Cu(NO 3 ) 2 and 1.83g Mn(NO 3 ) 2Add deionized water to prepare a mixed salt solution with a concentration of 0.2M, heat and maintain at 80°C. Under stirring conditions, drop 73.4g tetraethyl orthosilicate into the salt solution until the pH value of the solution at the end of the reaction is 7; after the reaction is completed, filter the feed solution while it is hot, wash it with deionized water three times and then suction filter ; After the catalyst was dried at 120°C for 12 hours, it was calcined at 400°C for 6 hours to finally obtain a catalyst sample. Put 15ml of the catalyst sample of 20-40 mesh after molding and screening into the reaction tube, use pure hydrogen with a flow rate of 100mL / min, reduce it at 230°C for 10 hours, adjust to the reaction process conditions for hydrogenation reaction, after hydrogenation reaction for 5 hours Sampling, the result of gas chromatographic analysis shows that the conversion rate of glycerin is 97.4%, and the ...

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Abstract

The invention discloses a catalyst for use in the preparation of 1,2-propanediol by low-temperature low-pressure hydrogenation of biological glycerol and a preparation method thereof. The catalyst consists of an active main body, an assistant catalyst and a carrier, wherein the active main body is metal copper which is 15 to 35 mass percent; the carrier is silicon dioxide and is one or more than one of silicate, silica sol or silicate ester; and the assistant catalyst is one or more of transitional metal nickel, manganese and cobalt and is 1 to 5 mass percent. When the catalyst is used, aqueous solution of glycerol, which serves as a raw material, can react at a very mild reaction condition, the conversion rate of glycerol is up to 100 percent, and the selectivity for 1,2-propanediol reaches over 99 percent. The method has the advantages that: the reaction process is simple and convenient; the operation is easy; the controllability is high; the reaction temperature is low; the reaction pressure is low; the target product yield is high; and the like.

Description

[0001] technical field [0002] The invention relates to a catalyst used for low-temperature and low-pressure hydrogenation of biological glycerol to prepare 1,2-propanediol and a preparation method thereof, belonging to the technical field of chemical industry. [0003] Background technique [0004] [0005] 1,2-Propanediol is a colorless, odorless, slightly viscous, low-toxic, hygroscopic liquid that is widely used in the food and pharmaceutical industries. 1,2-propanediol can also be used as antifreeze and heat carrier, and at the same time, it is the raw material for making unsaturated polyester resin, plasticizer, surfactant and emulsifier, etc. Generally speaking, it is a bulk chemical product with a wide range of uses . The traditional production technology in our country is to use propylene oxide as the raw material through hydration, or to generate dimethyl carbonate by-product to obtain propylene glycol through transesterification of propylene carbonate. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/755B01J23/889C07C31/20C07C29/60
Inventor 朱小学刘芃叶秋云李南锌郑敏王华
Owner HAO HUA CHENGDU TECH
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