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A kind of preparation method of synthetic dimethyl oxalate catalyst carrier

A technology for synthesizing dimethyl oxalate and dimethyl oxalate, which is applied in the direction of catalyst carrier, carbon monoxide or formate reaction preparation, chemical instruments and methods, etc., can solve the problem of smaller specific surface area and average pore size, which is not conducive to catalyst activity, It is unfavorable for the dispersion of active components and other problems, and achieves the effect of high crystallinity, high dispersion and good catalytic activity

Active Publication Date: 2018-03-09
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

It has been reported (104190414B, 104190415B, 102527377A, 102527377A, 105597743A, 105381799A, etc.) that the catalyst for synthesizing dimethyl oxalate is to use α-Al 2 o 3 As a carrier, due to α-Al 2 o 3 It needs to be calcined at 1300°C, which will make α-Al 2 o 3 Some pores of the carrier collapse during high-temperature calcination, resulting in a smaller specific surface area and average pore diameter
The specific surface area is too small, which is not conducive to the dispersion of active components, which is not conducive to the development of catalyst activity

Method used

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  • A kind of preparation method of synthetic dimethyl oxalate catalyst carrier
  • A kind of preparation method of synthetic dimethyl oxalate catalyst carrier
  • A kind of preparation method of synthetic dimethyl oxalate catalyst carrier

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Weigh 0.02mol tetra-ortho titanate and dissolve it in glacial acetic acid to form a 0.5mol / L solution. Weigh 0.02mol magnesium nitrate and dissolve it in deionized water to form a 0.4mol / L solution, add it to the prepared tetra-n-butyl titanate acetic acid solution under constant stirring, and add 0.02g cyclodextrin at the same time as porogen. The above mixed solution was placed in a water bath at 80° C. to obtain a transparent gel. The above gel was dried in an oven at 60°C for 12 hours, then raised to 100°C for 12 hours, then transferred to a corundum crucible and calcined at 600°C for 2 hours in a muffle furnace to obtain a blocky white powder. After ball milling the above white powder, add 5mL of 1mol / L polyvinyl alcohol aqueous solution as an adhesive, mix thoroughly and extrude into strips, and finally place it in a muffle furnace at 700°C for 2 hours to obtain MgTiO 3 carrier.

[0024] For the obtained MgTiO 3 For carrier characterization results, see Figu...

Embodiment 2

[0026] Weigh 0.04mol tetraisobutyl titanate and dissolve it in glacial acetic acid to form a 1mol / L solution. Weigh 0.04mol calcium nitrate and dissolve it in deionized water to form a 0.8mol / L solution, add it to the prepared tetraisobutyl titanate acetic acid solution under constant stirring, and add 0.04g cyclodextrin as porogen. The above mixed solution was placed in a water bath at 85° C. to obtain a transparent gel. The above gel was dried in an oven at 70°C for 12 hours, then raised to 110°C for 12 hours, then transferred to a corundum crucible and calcined at 500°C for 4 hours in a muffle furnace to obtain a blocky white powder. After ball milling the above white powder, add 5mL of 1.5mol / L polyvinyl alcohol aqueous solution as an adhesive, mix well and carry out extrusion molding, and finally place it in a muffle furnace at 700°C for 4 hours to obtain CaTiO 3 carrier.

Embodiment 3

[0028] Weigh 0.02mol tetra-n-propyl titanate and dissolve it in glacial acetic acid to form a 0.5mol / L solution. Weigh 0.02mol cobalt nitrate and dissolve it in deionized water to form a 0.4mol / L solution, add it to the acetic acid solution of tetra-n-propyl titanate prepared under constant stirring, and add 0.02g chitosan as porogen. The above mixed solution was placed in a water bath at 75° C. to obtain a transparent gel. The above gel was dried in an oven at 80°C for 12 hours, then raised to 120°C for 12 hours, then transferred to a corundum crucible and baked at 600°C in a muffle furnace for 6 hours to obtain a blocky black powder. After the above-mentioned black powder is ball-milled, 5 mL of 2mol / L polyvinyl alcohol aqueous solution is added as an adhesive, mixed thoroughly, extruded into strips, and finally placed in a muffle furnace at 700°C for 5 hours to obtain the CoTiO of the present invention. 3 carrier.

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Abstract

The invention discloses a preparation method of a carrier for synthesizing dimethyl oxalate catalyst. The preparation method adopted in the present invention is to add soluble M salt (M salt is nitrate, chloride, acetate of Zn, Mg, Ca and Co) into the glacial acetic acid solution of titanate, and then add large molecular weight The organic matter is used as a porogen, and is stirred continuously in a water bath at 60 to 90°C until a transparent gel is formed. The gel is dried, roasted, and extruded to prepare an MTiO3 carrier. The carrier prepared by this method has high crystallinity and has an irregular flaky structure. The surface of the carrier has alkaline sites of different strengths, but they are mainly weakly alkaline. The specific surface area of ​​the prepared carrier is 10-35m2 / g, and its average pore diameter is 8-25nm. The carrier prepared by this method is suitable for preparing a supported Pd-based catalyst to catalyze the oxidative coupling of carbon monoxide to synthesize dimethyl oxalate.

Description

technical field [0001] The invention relates to a method for preparing a carrier. The carrier is mainly used for preparing a supported Pd-based catalyst to catalyze the oxidative coupling of carbon monoxide to synthesize dimethyl oxalate, and belongs to the technical field of dimethyl oxalate preparation. Background technique [0002] Carrier is an important part of solid catalyst, and it is a substance used to support active components and additives. The role of the carrier in the catalytic reaction mainly includes: (1) increasing the active surface and providing a suitable pore structure; (2) improving the mechanical strength of the catalyst to ensure that it has a certain shape; (3) improving the thermal conductivity and Thermal stability to prevent sintering deactivation of the catalyst caused by local overheating; (4) disperse and support the main catalyst. [0003] The gas-phase catalytic coupling of carbon monoxide to synthesize dimethyl oxalate is a key step in the ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G23/00B01J23/58B01J23/60B01J23/89B01J32/00B01J35/10C07C67/36C07C69/36
CPCC01G23/003C01G23/006C07C67/36B01J23/58B01J23/60B01J23/8913B01J23/892B01J35/613B01J35/647C07C69/36
Inventor 姚元根张鑫潘鹏斌覃业燕黄园园王彦端陈建珊
Owner FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI