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A kind of nanometer tungstic acid catalyst and its preparation method and application

A technology of acid catalyst and nano-tungsten, applied in chemical instruments and methods, physical/chemical process catalysts, nanotechnology, etc., can solve the problems of complex preparation methods, high cost, and low selectivity of sulfide extraction, and achieve simple preparation methods , save the cost of use, the effect of mild conditions

Inactive Publication Date: 2018-12-21
SOUTH CHINA NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Such as acetic anhydride, it is difficult to realize the separation of catalyst and oil, and another example is ionic liquid (such as publication number CN104673370A), which has low selectivity for sulfide extraction by ionic liquid, and both have the disadvantage that the catalyst cannot be reused
Compared with homogeneous catalysis, heterogeneous catalysis is easy to realize the separation and reuse of reaction system and catalyst, but common heterogeneous catalysts, such as macroporous polystyrene resin, are modified with fluorine and loaded with phosphotungstic acid (such as publication number CN104357080A ), etc., most of them have complex preparation methods, high cost, and low catalyst stability.

Method used

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  • A kind of nanometer tungstic acid catalyst and its preparation method and application
  • A kind of nanometer tungstic acid catalyst and its preparation method and application
  • A kind of nanometer tungstic acid catalyst and its preparation method and application

Examples

Experimental program
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Effect test

Embodiment 1

[0026] Add 6.60g of calcium chloride to 20mL of distilled water, fully stir and dissolve to obtain solution A, add 1.11g of sodium tungstate to 20mL of distilled water, fully stir and dissolve to obtain solution B, add 0.10g to solutions A and B respectively Polyvinylpyrrolidone, fully stirred to dissolve, then drip solution B into solution A drop by drop, stir while dripping, stir until the white suspension precursor no longer increases, and obtain a suspension containing the white suspension precursor; The solution was transferred to a 150mL round bottom flask, and 10mL of hydrochloric acid with a substance concentration of 5mol / L was added, and the H in the solution + The concentration is about 1mol / L, and fully reacted in an oil bath at 120°C for 1 hour; after the reaction solution is cooled to room temperature, the reaction solution is centrifuged and washed, and the precipitate is first washed with deionized water for 3 times, and then washed with ethanol for 3 times. Ob...

Embodiment 2

[0030] Add 6.56g of calcium nitrate into 25mL of distilled water, fully stir and dissolve to obtain solution A, add 2.5g of potassium tungstate to 25mL of distilled water, fully stir and dissolve to obtain solution B, add 0.05g of poly Vinylpyrrolidone, fully stirred to dissolve, drop solution B into solution A drop by drop, stir while adding, stir for 30min, to obtain a suspension containing white suspension precursor; transfer the suspension to a 150mL round bottom flask, add 22mL of hydrochloric acid with a molar concentration of 2mol / L, the H in the solution + The concentration is about 0.61mol / L, fully react for 10h under the condition of 50°C oil bath; after the reaction is cooled to room temperature, centrifuge the reaction solution and separate the precipitate, wash the precipitate with deionized water 3 times, and then wash with ethanol 3 times to obtain a yellow solid, put the yellow solid in an oven, and bake it at 70°C for 10 hours; then fully grind the dried yello...

Embodiment 3

[0033] Add 7.90g of calcium acetate into 25mL of distilled water, fully stir and dissolve to obtain solution A, add 2.20g of sodium tungstate to 25mL of distilled water, fully stir and dissolve to obtain solution B, add 0.25g of polyethylene to solutions A and B respectively Pyrrolidone, fully stirred to dissolve, drop solution B into solution A drop by drop, and stir while adding dropwise, to obtain precursor suspension containing white suspended matter; transfer the suspension to a 150mL round-bottomed flask, add 4mL substance concentration is 12mol / L hydrochloric acid, the H in the solution + The concentration is about 0.89mol / L, fully react for 3.5h under the condition of 65℃ oil bath; after the reaction is cooled to room temperature, let the reactant stand for 20h, separate the precipitate, wash the precipitate with deionized water 3 times, and then After washing with ethanol for 3 times, a yellow solid was obtained, which was placed in an oven and baked at 65°C for 14 ho...

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Abstract

The invention discloses a nanometer tungstic acid catalyst, its preparation method and application. Dissolve calcium salt and tungstate in water respectively to obtain solution A and solution B, respectively add surfactant to solution A and solution B to disperse, stir to dissolve, then mix solution A and solution B, then add hydrochloric acid to make the pH of the solution ≤1, the reaction produces a precipitate, and after cooling, the precipitate is taken out, washed, dried and crushed to obtain a nano-tungstic acid catalyst. The preparation method of the nano-tungstic acid catalyst of the present invention is simple, the conditions are mild, and the cost is low. The prepared tungstic acid is in the form of flakes, which is suitable for heterogeneous catalytic diesel oxidation desulfurization. It does not need to be compounded with a carrier or other auxiliary reagents, and the tungstic acid catalyst is stable. High performance and easy to separate and recover. After the recovered tungstic acid catalyst is recycled for many times, the desulfurization activity of the tungstic acid catalyst will not be significantly reduced, which can save the cost of the catalyst. The nano tungstic acid catalyst of the present invention has high efficiency in catalyzing diesel oxidation desulfurization, and the desulfurization rate is greater than 94% under optimal conditions.

Description

technical field [0001] The invention belongs to the field of catalysts, and in particular relates to a nano-tungstic acid catalyst and its preparation method and application. Background technique: [0002] Fuel contains a large amount of thiophene sulfides (such as DBT, BT, DMDBT) and their derivatives. The exhaust gas generated by the combustion of these sulfides will cause environmental problems such as acid rain and smog, and will cause harm to human body and organisms. [0003] At present, desulfurization methods mainly include two categories, namely hydrodesulfurization and non-hydrodesulfurization. Hydrodesulfurization technology refers to the H adsorption on the catalyst under high temperature and pressure 2 Catalytic reaction with sulfur in sulfide to generate H 2 S to remove sulfur. The traditional hydrodesulfurization method is very effective for mercaptans and sulfides, but it is difficult to remove thiophene sulfides, and the process conditions are harsh and t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/30B82Y30/00B82Y40/00C10G27/12
CPCC10G27/12B82Y30/00B82Y40/00B01J23/30C10G2300/70B01J35/50B01J35/40
Inventor 肖信钟欢南俊民左晓希
Owner SOUTH CHINA NORMAL UNIVERSITY