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Method of preparation of solid catalyst by ozone heterogeneous oxidation

A heterogeneous oxidation, solid catalyst technology, applied in the direction of catalyst activation/preparation, physical/chemical process catalyst, metal/metal oxide/metal hydroxide catalyst, etc., can solve the problem of poor toxicity resistance, easy loss of catalytic activity, Solve the problems of low catalyst adsorption, achieve strong adsorption, improve anti-toxicity and catalytic activity, and inhibit melting and precipitation

Inactive Publication Date: 2017-08-25
SICHUAN NORMAL UNIVERSITY
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Problems solved by technology

[0004] In view of the problems of low catalyst adsorption, poor anti-toxicity and easy loss of catalytic activity in the current preparation method of ozone heterogeneous oxidation solid catalyst, a multi-component porous carrier was developed to enhance the adsorption of the catalyst through pore expansion and surface activation. Rare earth metal organic compounds as precursors of catalytic active additives, common transition metal organic compounds and noble metal compounds as precursors of catalytic active centers and multi-component porous carriers through hydrothermal reaction and high temperature calcination to prepare ozone heterogeneous oxidation containing multiple metals The preparation method of solid catalyst to improve the anti-toxicity and catalytic activity of the catalyst is characterized in that component A and deionized water are added into a sealable reactor and stirred to prepare an aqueous solution, and the weight concentration of component A is controlled to be 2% to 6%. After the preparation is completed, add component B under stirring, raise the temperature to 35°C-50°C, continue to stir for 3h-6h, filter, and dry the reaction product at 102°C-106°C to obtain a modified carrier for pore expansion; pore expansion Put the modified carrier into the ultrasonic reactor, add the aqueous solution prepared by C component and deionized water, the weight concentration of C component is 3%~8%, stir and mix evenly, control the ultrasonic power density to 0.3~0.8W / m 3 , frequency 20kHz ~ 30kHz, 40 ℃ ~ 55 ℃, ultrasonic vibration 2h ~ 5h, the ultrasonic surface activation carrier mixture is obtained; the ultrasonic surface activation carrier mixture is transferred to the hydrothermal reaction kettle, and then add D component and deionized water to prepare The aqueous solution, the weight concentration of D component is 40% ~ 55%, by weight, the weight ratio of D component deionized aqueous solution: ultrasonic surface activation carrier mixture = 1: (1.5 ~ 2), control temperature 120 ℃ ~ 180°C, the hydrothermal reaction time is 8h~16h, and then dried to obtain fine particles; the fine particles are burned in a muffle furnace at 600°C~950°C for 3h~8h to obtain a solid catalyst for ozone heterogeneous oxidation

Method used

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Examples

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Effect test

Embodiment 1

[0007] Embodiment 1:1.35g lithium hypochlorite, 1.65g bis(acetylacetonate) beryllium, 140ml deionized water, join volume and be that in the sealable reactor of 500ml, stir and mix evenly, the weight concentration of this aqueous solution is 2.1%, times Lithium chlorate: the weight ratio of bis(acetylacetonate) beryllium=1:1.2; add deionized water to wash to neutral, dry at 103°C to remove moisture, and then sieve 2.75g diatoms of -200 mesh to +400 mesh standard sieve Weight of pure, 3.75g kyanite, 4.75g fluorite, 5.75g glauberite, 6.75g fly ash, 7.75g coal gangue, lithium hypochlorite and bis(acetylacetonate)beryllium (3g): weight of porous material (31.5g)=1:10.5, heat up to 36°C, continue to stir for 3.2h, filter, dry at 103°C and obtain 31g of pore-enlarging modified carrier; put 31g of pore-enlarging modified carrier into a 500ml ultrasonic reactor , then add 3.25g monoalkyl ether trimethyl ammonium chloride dissolved in 100ml deionized water aqueous solution, the weight c...

Embodiment 2

[0008] Embodiment 2:0.24g lithium hypochlorite, 0.36g bis(acetylacetonate) beryllium, 10ml deionized water, join volume and be that in the sealable reactor of 100ml, stir and mix evenly, the weight concentration of this aqueous solution is 5.7%, times Lithium chlorate: the weight ratio of bis(acetylacetonate) beryllium=1:1.5; add deionized water to wash to neutral, dry at 103°C to remove moisture, and then sieve 1.45g diatoms of -200 mesh to +400 mesh standard sieve Weight of pure, 1.65g kyanite, 1.85g fluorite, 2.05g glauberite, 2.25g fly ash, 2.45g coal gangue, lithium hypochlorite and bis(acetylacetonate) beryllium (0.6g): Porous material Weight (11.7g) = 1:19.5, heat up to 48°C, continue to stir for 5.8h, filter, dry at 105°C and obtain 11.5g of pore-enlarging modified carrier; in a 100ml ultrasonic reactor, put pore-enlarging modified Carrier 11.5g, then add 2.2g monoalkyl ether trimethyl ammonium chloride and dissolve in 26ml deionized water aqueous solution, the weight ...

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Abstract

The invention relates to a method of preparation of solid catalyst by ozone heterogeneous oxidation, belongs to the technical field of environmental protection and chemical engineering catalysts. Diatom pure, kyanite, fluorite, glauberite, pulverized coal ash and coal gangue are adopted as carriers after subjecting to bore-reaming by lithium hypochlorite and di-(acetylacetone) beryllium, activating treatment is conducted by the subjoining of surfactant mono alkyl ether trimethyl ammonium chloride under the action of ultrasonic waves, then the carriers are subject to hydrothermal reaction in a hydrothermal reaction kettle with a composite mineralizer borax and potassium sulfate, precursors of catalytic coagent tri-(acetylacetonate hexafluoride) yttrium (III) dihydrate, tricyclic cyclopentadienyl promethium, tri-(2, 2, 6, 6-tetramethyl-3, 5-pimelic keto acid) gadolinium, tri-(trifluoro methane sulfonyl imine) ytterbium, catalytic active core precursor of pyruvic acid isonicotinoyl hydrazone vanadium, cobalt gluconate, and tetra-chlorine potassium, hexa-nitroso rhodium tri-sodium under the action of emulsifying agent stearic acid trimethylamine ethanol ammonium chloride, after stoving, the moisture content is removed, and a solid catalyst by ozone heterogeneous oxidation is obtained by firing in a muffle furnace.

Description

technical field [0001] The invention relates to a preparation method of a solid catalyst for ozone heterogeneous oxidation, which belongs to the technical fields of environmental protection and chemical catalysts. Background technique [0002] Ozone oxidation technology utilizes the strong oxidation ability of ozone, which can oxidize and decompose many organic pollutants, and is widely used in wastewater treatment. Ozone catalytic oxidation technology is divided into ozone homogeneous catalytic oxidation and ozone heterogeneous catalytic oxidation. Ozone homogeneous catalytic oxidation has catalysts that are difficult to separate, recycle and reuse, and the low utilization rate of ozone leads to high water treatment operation costs. Ozone heterogeneous catalytic oxidation technology has the advantages of easy separation and recovery of catalysts and reusable use, high ozone utilization rate, and high removal rate of organic pollutants, which reduces water treatment. The ad...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/89B01J32/00B01J20/20B01J20/30C02F1/28C02F1/78C02F101/30
CPCB01J20/041B01J20/045B01J20/046B01J20/06B01J20/08B01J20/103B01J20/14B01J20/20C02F1/281C02F1/725C02F1/78B01J23/898B01J37/084B01J37/10C02F2101/30C02F2305/02B01J2220/4812B01J2220/42B01J2220/4806B01J35/60
Inventor 朱明刘阳魏玉君
Owner SICHUAN NORMAL UNIVERSITY
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