A kind of synthetic dibutyl carbonate catalyst and its preparation method and application

A technology of dibutyl carbonate and catalyst, which is applied in the field of synthesis of dibutyl carbonate catalyst and preparation, can solve the problems of complex process, high butanol, high butanol, urea molar ratio, etc., and achieve simple preparation method and high mechanical strength , the effect of large specific surface area

Active Publication Date: 2020-07-10
CHINA PETROLEUM & CHEM CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the applicant has found that the existing urea alcoholysis method needs a higher butanol and urea molar ratio.
[0004] CN102093221A discloses a method for synthesizing dibutyl carbonate, using butyl carbamate and n-butanol as raw materials, using MgO as a catalyst, CO2 as a reaction accelerator and ammonia absorbent, and the conversion rate of butyl carbamate reaches 99% , but there is a problem that the price of the raw material butyl carbamate is higher than that of the product dimethyl carbonate
Deng Youquan et al. (CN102557948A, CN102464588A) adopted a reaction separation system consisting of a tank reactor and a gas storage-condensation-carbamate amine trap, and adopted a two-stage heating method to control the reaction temperature to obtain a higher yield of dibutyl carbonate. But still there is complex technology and need higher butanol, the problem of urea mol ratio, generate 1mol dibutyl carbonate needs 2mol n-butanol and 1mol urea according to stoichiometric coefficient reaction, actual n-butanol is far excessive, the excess n-butanol Adding to increase the energy consumption of the system will also increase the load of the separation system

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Embodiment 1~9 is a kind of synthetic dibutyl carbonate catalyst of the present invention and the specific embodiment of preparation method thereof, wherein embodiment 1 is best embodiment.

[0030] Example 1

[0031] 1) Preparation of filter cake: Weigh 3654.7g, 311.5g, and 21.1g of nickel nitrate, zinc nitrate, and calcium nitrate, respectively, and make 1mol / L aqueous solutions, mix well and place them in a mixed salt solution storage tank; prepare a mass of 3100g Ammonia water with a concentration of 15% is placed in the precipitant storage tank. Two pumps are used to pump the mixed salt solution and precipitant ammonia water into the sedimentation tank with continuous stirring. =9. After precipitation, let it stand for 12 h, wash the slurry in the sedimentation tank repeatedly with distilled water until pH=8, and then filter to obtain a filter cake;

[0032] 2) Preparation of catalyst slurry: Weigh 24.9g of potassium carbonate to make a 1mol / L solution, add it to...

Embodiment 2

[0037] 1) Preparation of filter cake: Weigh 3654.7g, 389.4g, and 63.3g of nickel nitrate, zinc nitrate, and calcium nitrate, respectively, and make 1mol / L aqueous solutions, mix well and place them in a mixed salt solution storage tank; prepare a mass of 4723g Ammonia water with a concentration of 10% is placed in the precipitant storage tank. Two pumps are used to pump the mixed salt solution and precipitant ammonia water into the sedimentation tank with continuous stirring. =9.8. After precipitation, let it stand for 15 h, wash the slurry in the sedimentation tank repeatedly with distilled water until pH=8, and then filter to obtain a filter cake;

[0038] 2) Preparation of catalyst slurry: Weigh 44.1g of potassium carbonate to make a 0.8mol / L solution, add it to 500g of silica sol solution with a mass concentration of 20% to obtain a mixed solution of alkali metal and carrier, and filter cake obtained in the previous step Add it into the mixed solution of alkali metal and ...

Embodiment 3

[0043] 1) Preparation of filter cake: Weigh 3654.7g, 739.8g, and 210.8g of nickel nitrate, zinc nitrate, and calcium nitrate, respectively, and make 0.8mol / L aqueous solutions, mix well and place them in a mixed salt solution storage tank; prepare 4111g Ammonia water with a mass concentration of 13% is placed in the precipitant storage tank. Two pumps are used to pump the mixed salt solution and precipitant ammonia water into the sedimentation tank with continuous stirring. pH=9.5. After precipitation, let it stand for 24 hours, wash the slurry in the sedimentation tank repeatedly with distilled water until pH=8, and then filter to obtain a filter cake;

[0044] 2) Preparation of catalyst slurry: Weigh 58.8g of potassium carbonate to make a 0.9mol / L solution, add it to 666.7g of silica sol solution with a mass concentration of 30%, to obtain a mixed solution of alkali metal and carrier, filter the obtained solution in the previous step Add the cake to the mixed solution of al...

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Abstract

The invention provides a synthetic dibutyl carbonate catalyst, and a preparation method and an application thereof, belonging to the technical field of catalyst preparation. The synthetic dibutyl carbonate catalyst comprises components of ZnO, NiO, alkaline earth metal oxide, alkali metal oxide and a carrier with a weight ratio of 100: (3-60): (0.1-40): (0.1-10): (2-50). The preparation method for the synthetic dibutyl carbonate catalyst comprises the following steps: 1) filter cake preparation; 2) catalyst slurry preparation; and 3) catalyst molding. The synthetic dibutyl carbonate catalyst provided by the invention has high catalytic activity, long service life and high mechanical strength; the preparation method for the synthetic dibutyl carbonate catalyst is simple, convenient and practicable, and is applicable to large-scale industrial production; and the synthetic dibutyl carbonate catalyst is applicable to a reaction of n-butyl alcohol and urea for preparation of dibutyl carbonate.

Description

technical field [0001] The invention relates to a catalyst for synthesizing dibutyl carbonate, a preparation method and an application thereof, and belongs to the technical field of catalyst preparation. Background technique [0002] Dibutyl carbonate is a long carbon chain organic synthesis intermediate, which can be used to synthesize diphenyl carbonate, and then synthesize polycarbonate. It can also be used as a matrix material for lubricating oil, used in metal degreasing, leather treatment and other industries , a lot of uses. The synthesis methods of dibutyl carbonate mainly include phosgene method, urea alcoholysis method, oxidative carbonylation method and transesterification method. The phosgene method has disadvantages such as highly toxic raw materials, long operation period, and serious equipment corrosion by by-products, and is being phased out gradually. The oxidative carbonylation method generally uses palladium and other noble metals and their compounds as ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/80B01J35/10B01J35/02C07C68/00C07C69/96
CPCB01J23/002B01J23/80B01J35/023B01J35/1019B01J2523/00C07C68/00B01J2523/847B01J2523/27B01J2523/23B01J2523/13B01J2523/41C07C69/96
Inventor 贾庆龙菅秀君王申军马瑞杰孟宪谭孙丛丛
Owner CHINA PETROLEUM & CHEM CORP
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