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Catalyst for preparing formate from CO2 and preparation method thereof

A catalyst and formate technology, which is applied in the preparation of carboxylic acid esters, chemical instruments and methods, and the preparation of organic compounds. It can solve the problems of expensive formic acid raw materials, difficult to recycle sulfuric acid, and serious pollution, and achieve high formate The effect of synthetic activity and thermal stability, good reproducibility, and simple operation method

Active Publication Date: 2015-04-01
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above method prepares butyl formate, the formic acid raw material is more expensive, the process is complicated, the sulfuric acid used as the catalyst is difficult to recycle, the pollution is serious and energy consumption

Method used

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  • Catalyst for preparing formate from CO2 and preparation method thereof
  • Catalyst for preparing formate from CO2 and preparation method thereof
  • Catalyst for preparing formate from CO2 and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Take 5g of organic silicon waste contacts, wash twice with 100mL of ether and ethanol, filter and dry in a vacuum oven at 100°C for 2 hours, put it in a 500mL beaker, add 100mL of dilute hydrochloric acid, at 40°C Heat the reaction for 6h, slowly add sodium carbonate solution, adjust the pH value to 9, heat the reaction at 65°C for 6h, wash, filter, vacuum dry at 100°C for 6h, and calcinate at 350°C for 2h.

[0042] The catalyst material prepared above was subjected to XRD test on the X'Pert PROMPD multifunctional X-ray diffractometer produced by Panalytical Company (Panalytical) in the Netherlands.

[0043] The catalyst material prepared above is carried out ICP test on U.S. Pekin-Elmer Inductively Coupled Plasma Atomic Emission Spectrometer, copper element content is 3.0% (weight ratio, the same below), zinc element content is 0.1% (weight ratio, the same below) .

[0044] figure 1 For the XRD pattern of the catalyst obtained in Example 1, wherein 2θ=28.6° is the ch...

Embodiment 2

[0046] Take 5g of organic silicon waste contacts, wash them twice with 100mL of toluene and tetrahydrofuran respectively, filter and dry in a vacuum oven at 100°C for 2 hours, cool to room temperature, put it in a 500mL beaker, add 2gZn(N0 3 ) 2 , add 100mL dilute nitric acid, heat reaction at 60°C for 4h, slowly add ammonia solution, adjust the pH value to 11, heat reaction at 70°C for 4h, wash, filter, vacuum dry at 100°C for 6h, and calcinate at 100°C for 10h. .ICP test results show that the copper element content is 3.3%, and the zinc element content is 4.3%.

[0047] figure 2 For the XRD pattern of the catalyst obtained in Example 2, wherein 2θ=28.6° is the characteristic peak of Si, the shoulder peak composed of 2θ=35.5° and 2θ=38.7° is the characteristic peak of CuO, and 2θ=36.3° is the characteristic peak of ZnO Peak, it can be seen that the catalyst obtained by this method is a silicon / copper oxide / zinc oxide catalyst.

Embodiment 3

[0049] Take 5g of silicone waste contacts, wash them twice with 100mL of chloroform and acetone respectively, filter and dry in a vacuum oven at 100°C for 2 hours, put them in a muffle furnace, bake at 600°C for 2h, and cool to room temperature . Put the above materials in a 500mL beaker, add 1gZn(NO 3 ) 2 , add 100mL dilute sulfuric acid, heat reaction at 80°C for 2h, slowly add sodium hydroxide solution, adjust pH to 10, heat reaction at 80°C for 2h, wash, filter, vacuum dry at 100°C, and calcinate at 300°C for 5h. ICP test results show that the copper element content is 2.3%, and the zinc element content is 3.9%.

[0050] image 3 For the XRD pattern of the catalyst obtained in Example 3, wherein 2θ=28.6° is the characteristic peak of Si, the shoulder peak composed of 2θ=35.5° and 2θ=38.7° is the characteristic peak of CuO, and 2θ=36.3° is the characteristic peak of ZnO Peak, 2θ=26.6 ° is the characteristic peak of C, thus it can be seen that the catalyst obtained by th...

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Abstract

The invention relates to the field of chemical industry production of formate from CO2, particularly a catalyst for preparing formate from CO2 and a preparation method thereof. The method for preparing the catalyst for preparing formate from CO2-containing synthetic gas, which is a spent contact mass generated in an organosilicon monomer methyl chlorosilane production process, comprises the following steps: washing the spent contact mass with an organic solvent, filtering, roasting, dissolving with acid, precipitating with alkali, filtering, drying and calcining. The invention solves the problem of high-value comprehensive utilization of solid residue spent contact mass in organosilicon synthesis industry. The prepared catalyst for preparing formate from CO2-containing synthetic gas has the advantages of low raw material cost and simple operational method, and can easily implement large-scale production; and the catalyst provided by the invention has higher formate synthesis activity, higher heat stability and better reproducibility, and is beneficial to controlling the product quality.

Description

technical field [0001] The invention relates to the field of formic acid ester chemical production from synthesis gas, in particular to a method of utilizing CO 2 Catalyst for producing formate and its preparation method. Background technique [0002] Coal-to-synthesis gas (CO, H 2 and CO 2 ) to prepare high value-added chemicals is an important development direction in the field of coal chemical industry. The production and application of synthesis gas plays an important role in the chemical industry, and a series of chemicals can be produced from synthesis gas. For example: synthesis gas to produce ammonia and methanol, Fischer-Tropsch synthesis to produce liquid fuels, carbonylation to produce higher fatty aldehydes and alcohols, etc. In addition, the direct synthesis of ethylene glycol, ethanol, acetic acid, 1,4-butanediol, etc. from syngas is under development. At the same time, CO 2 Emission reduction and high-value utilization are also a hot spot in scientific r...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/80B01J35/10C07C69/06C07C67/00
Inventor 苏发兵赵丽润车红卫王莹利古芳娜翟世辉
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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