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Nickel silicate catalyst as well as preparation method and application thereof

A catalyst, nickel-silicon technology, applied in the direction of catalyst activation/preparation, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of easy aggregation and growth, low catalytic activity, etc., to improve catalytic activity, improve low-temperature processing Hydrogen activity, the effect of overcoming poor stability

Inactive Publication Date: 2019-03-29
SHANXI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The present invention uses mineral salt (silicate) as a precursor to prepare a phylloid nickel silicate catalyst, abbreviated as Ni-PS. The precursor of succinic anhydride nickel-based catalyst is prepared by hydrogenation of anhydride. Through the confinement of its layered structure, the dispersion and stability of the active metal can be effectively regulated in the precursor, thereby improving its catalytic activity and overcoming the traditional impregnation of the prior art. Catalysts prepared by this method have poor stability of metal active sites, easy aggregation and growth, and low catalytic activity.

Method used

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  • Nickel silicate catalyst as well as preparation method and application thereof
  • Nickel silicate catalyst as well as preparation method and application thereof
  • Nickel silicate catalyst as well as preparation method and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0028] The preparation method of Ni-PS catalyst comprises the steps:

[0029] 1) At room temperature, 32 gNi(NO 3 ) 2 ·6H 2 Dissolve O in 300 ml distilled water, add 25% concentrated ammonia water (wt) dropwise to pH=11~12, and stir to make an ammonia complex solution;

[0030] 2) Add 25g of alkaline silica sol dropwise to the ammonium complex solution obtained in step 1) while stirring, continue to stir for 6 h after the dropwise addition, raise the temperature to 50 °C, and conduct uniform precipitation until the solution pH=7. The precipitate was centrifuged, washed with distilled water three times, then dried overnight at 90 °C, and then calcined at 5 °C / min to 450 °C for 4 h to make a catalyst. The mass ratio of the active metal Ni to the support was 2:3;

[0031] 3) Catalyst at 25V%H with a gas flow rate of 40 ml / min 2 -75V%N 2 In a mixed gas atmosphere, the temperature was raised to 400°C at 5°C / min and reduced for 2 h to obtain Catalyst A for maleic anhydride hydr...

Embodiment 2

[0033] 1) At room temperature, 20 gNi(NO 3 ) 2 ·6H 2 Dissolve O in a mixed solution of 250 ml of water and ethanol, add 25% concentrated ammonia water (wt) dropwise to pH=11~12, and stir to make an ammonia complex solution;

[0034] 2) Add 30 g of alkaline silica sol dropwise to the ammonium complex solution obtained in step 1) while stirring, continue to stir for 6 h after the dropwise addition, and raise the temperature to 60 °C for uniform precipitation until the solution pH=7 . The precipitate was centrifuged, washed with distilled water three times, then dried overnight at 100 °C, and then calcined at 550 °C for 5 h at 5 °C / min to make a catalyst. The mass ratio of the active metal Ni to the support was 1:3;

[0035] 3) Catalyst in H with a gas flow rate of 40 ml / min 2 -N 2 In a mixed gas atmosphere, the temperature was raised to 500 °C at 5 °C / min and reduced for 2 h to obtain catalyst B for maleic anhydride hydrogenation evaluation. The catalyst was added to a bat...

Embodiment 3

[0037] 1) At room temperature, 28 g Ni(NO 3 ) 2 ·6H 2 Dissolve O in 250 ml of water, add 25% concentrated ammonia water (wt) dropwise to pH=11~12, and stir to make ammonia complex solution;

[0038] 2) Add 25 g of alkaline silica sol dropwise to the ammonium complex solution obtained in step 1) while stirring, continue to stir for 10 h after the dropwise addition, and raise the temperature to 80 °C for uniform precipitation until the pH of the solution is 7 . The precipitate was centrifuged, washed with distilled water three times, then dried overnight at 80 °C, and then calcined at 5 °C / min to 600 °C for 4 h to make a catalyst. The mass ratio of the active metal Ni to the support was 1:1.78;

[0039] 3) Catalyst in H with a gas flow rate of 40 ml / min 2 -N 2 In a mixed gas atmosphere, the temperature was raised to 550 °C at 5 °C / min and reduced for 2 h to obtain catalyst C for maleic anhydride hydrogenation evaluation. The catalyst was added to a batch reactor to investi...

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Abstract

The invention discloses a nickel silicate catalyst as well as a preparation method and application thereof. A nickel phyllosilicate catalyst is prepared by using mineral salt silicate as a precursor;the obtained catalyst is the nickel phyllosilicate catalyst with a sandwich structure (2:1 type laminated structure) which is formed by silica tetrahedron and nickel-oxygen octahedron. That is, a layer of Ni is clamped between two layers of SiO2; the catalyst is abbreviated as a Ni-PS catalyst by using symbol of elements. Mineral salt nickel phyllosilicate with the sandwich structure is prepared by an ammonia distilling method and is used as a precursor for preparing a succinic anhydride nickel-based catalyst through catalysis of maleic anhydride hydrogenation; through the region limiting effect of the laminated structure of the mineral salt nickel phyllosilicate, the dispersion and the stability of active metal can be effectively regulated and controlled at the precursor; further, the catalytic activity is improved; the problems of poor metal active site stability, liability to aggregate and grow up and low catalytic activity of a traditional impregnation method in the prior art in the catalyst preparation are solved.

Description

technical field [0001] The invention relates to a nickel-silicon catalyst and its preparation method and application, in particular to a nickel-silicon catalyst for catalyzing the hydrogenation of maleic anhydride to prepare succinic anhydride at low temperature and its preparation method. The invention belongs to the technical field of chemical catalysts. Background technique [0002] Succinic anhydride, also known as succinic anhydride, has the molecular formula C 4 h 4 o 3 , is an important organic synthesis intermediate and fine chemical raw material, widely used in industrial fields such as polyester, paint, plastics, medicine, agriculture, food, surfactants, dyes, etc. The annual domestic demand is increasing year by year, but domestic production There is a large gap in the production capacity of polyester grade succinic anhydride, and the dependence on foreign countries is relatively high. [0003] At present, the methods for producing succinic anhydride mainly in...

Claims

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Application Information

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IPC IPC(8): B01J23/755B01J35/02C07D307/60
CPCC07D307/60B01J23/755B01J37/0018B01J35/00B01J35/30
Inventor 谭静静赵永祥张因崔静磊夏晓丽
Owner SHANXI UNIV
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