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Solid catalyst for dimethyl carbonate and oxamide co-production process and preparation method of solid catalyst

A technology of dimethyl carbonate and solid catalyst, which is applied in the direction of carbonate/haloformate preparation, carboxylic acid amide preparation, chemical instruments and methods, etc. It can solve the problem that the proportion of active components and the loading method cannot meet the co-production reaction Needs and other issues, to achieve the effect of adjusting acidity and alkalinity, rational distribution, and improving stability

Active Publication Date: 2017-05-17
FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Compared with the synthesis of dimethyl carbonate by urea alcoholysis method, due to the specificity of the co-production process in terms of raw material selection and reaction condition control, the catalyst that was originally suitable for urea alcoholysis reaction with ZnO as the main component, its active group The type, ratio and load mode of the points can no longer meet the needs of the co-production reaction

Method used

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  • Solid catalyst for dimethyl carbonate and oxamide co-production process and preparation method of solid catalyst
  • Solid catalyst for dimethyl carbonate and oxamide co-production process and preparation method of solid catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] A. Weigh 11.8g copper nitrate and dissolve it in 20ml deionized water to prepare Cu salt solution.

[0019] B. Weigh 1.5g of calcium nitrate, 8.8g of indium nitrate and 3.8g of cadmium nitrate and dissolve them in 20ml of deionized water to prepare a mixed salt solution.

[0020] C. After uniformly mixing the salt solution prepared in steps A and B, slowly drop 20ml of urea aqueous solution with a concentration of 5mol / L under continuous stirring at 50°C, and after the addition is completed, raise the temperature to 100°C and continue stirring for 12 hours. After cooling down, it was filtered to obtain a colloidal precipitate.

[0021] D. Mix the colloidal precipitate obtained in step C with methanol, and crystallize at 200° C. for 24 hours. After cooling down to room temperature, the precipitate was taken out and filtered, then dried in an oven at 120°C for 12 hours, then placed in a muffle furnace for 3 hours at 650°C, and cooled to room temperature to obtain the cat...

Embodiment 2

[0024] The same as the preparation method of Example 1, the difference lies in step B: 12g of calcium nitrate and 16.6g of cadmium nitrate were weighed and dissolved in 3.7ml of deionized water to prepare a mixed salt solution. The catalyst CuO / CaO-CdO is prepared, wherein CuO accounts for 50% of the total mass of the catalyst, CaO accounts for 40% of the total mass of the catalyst, and CdO accounts for 10% of the total mass of the catalyst.

[0025] With the catalyst evaluation method of Example 1, the product analysis results are shown in Table 1.

Embodiment 3

[0027] The same as the preparation method of Example 1, the difference lies in step B: 8.8g of indium nitrate and 3.7g of cadmium nitrate were weighed and dissolved in 23ml of deionized water to prepare a mixed salt solution. Prepared catalyst CuO / In 2 o 3 -CdO, where CuO accounts for 50% of the total mass of the catalyst, In 2 o 3 It accounts for 40% of the total mass of the catalyst, and CdO accounts for 10% of the total mass of the catalyst. With the catalyst evaluation method of Example 1, the product analysis results are shown in Table 1.

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Abstract

The invention discloses a solid catalyst for a process for co-producing dimethyl carbonate and oxamide by taking urea and dimethyl oxalate as raw materials. The catalyst is represented as CuO / MO, wherein CuO accounts for 50 to 95 percent of the total mass of the catalyst, and MO represents a doped oxide adjuvant and accounts for 5 to 50 percent of the total mass of the catalyst. The catalyst is prepared by using technologies such as a precipitation method and a hydrothermal method; and various oxide adjuvants are doped into a CuO bulk phase, and reasonable distribution of all the components in the catalyst is realized. The introduction of the oxide adjuvants is favorable for improving the stability of the catalyst, adjusting the surface acid-base property of the catalyst and improving the adsorption capacity of an active site for reactants. The catalyst has a good activation effect on the reaction raw materials, namely the urea and dimethyl oxalate; and during a reaction, by the application of the catalyst, the yield of oxamide can be up to 90 to 99.8 percent, and the yield of dimethyl carbonate can be up to 30 to 57.6 percent.

Description

technical field [0001] The invention includes a catalyst for driving a specific reaction and its preparation technology, in particular to a multi-component composite oxide catalyst with CuO as the main component and its preparation technology. The catalyst is used to drive urea and dimethyl oxalate to efficiently recombine carbonic acid Co-production process of dimethyl ester and oxamide. Background technique [0002] As an important green chemical intermediate, dimethyl carbonate has broad application prospects in the fields of medicine, biology and energy. It is known as the new cornerstone of organic synthesis in the 21st century. It is mainly used to synthesize bulk chemical raw materials such as polycarbonate, replacing Phosgene participates in the methylation and carbonylation process of organic synthesis, and can also be used as a gasoline additive to increase the octane number of gasoline to increase its antiknock performance. Utilizing the alcoholysis reaction of u...

Claims

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Application Information

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IPC IPC(8): B01J23/825B01J23/80B01J23/78B01J23/83B01J23/89C07C68/00C07C69/96C07C231/10C07C233/56
CPCB01J23/002B01J23/78B01J23/80B01J23/825B01J23/83B01J23/8926B01J2523/00C07C68/00C07C231/10C07C69/96C07C233/56B01J2523/17B01J2523/28B01J2523/305B01J2523/31B01J2523/22B01J2523/33B01J2523/12B01J2523/11B01J2523/23
Inventor 姚元根乔路阳周张锋
Owner FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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