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Preparation method of ozone heterogeneous oxidation solid catalyst

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 low catalyst adsorption, poor toxicity resistance, Easy to lose catalytic activity and other problems, to achieve the effects of inhibiting smelting out, strong adsorption, and improving anti-toxicity and catalytic activity

Inactive Publication Date: 2017-08-04
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

Experimental program
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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: bis(acetylacetonate) beryllium weight ratio=1:1.2; add deionized water to wash to neutral, dry at 103°C to remove moisture, and then sieve 2.75g attapulgite of -200 mesh to +400 mesh standard sieve Weight (3 g) of soil, 3.75 g diopside, 4.75 g illite, 5.75 g sodium borite, 6.75 g aluminum hydroxide, 7.75 g lapis lazuli, lithium hypochlorite and bis(acetylacetonate)beryllium: porous material The weight (31.5g)=1:10.5, heat up to 36°C, continue to stir and react for 3.2h, filter, dry at 103°C and obtain 31g of pore-enlarging modified carrier; in a 500ml ultrasonic reactor, put pore-enlarging modified Carrier 31g, then add 3.25g trioctylmethyl ammonium chloride and dissolve in 100ml deionized water aqueous solutio...

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: bis(acetylacetonate) beryllium weight ratio=1:1.5; add deionized water to wash to neutral, dry at 103°C to remove moisture, and then sieve 1.45g attapulgite of -200 mesh to +400 mesh standard sieve Weight of soil, 1.65g diopside, 1.85g illite, 2.05g sodium borite, 2.25g aluminum hydroxide, 2.45g lapis lazuli, lithium hypochlorite and bis(acetylacetonate)beryllium (0.6g): Porous The weight of the material (11.7g)=1:19.5, heat up to 48°C, continue to stir and react for 5.8h, filter, and dry at 105°C to obtain a pore-expanding modified carrier of 11.5g; put it into a 100ml ultrasonic reactor Modified carrier 11.5g, then add 2.2g trioctylmethylammonium chloride and be dissolved in the aqueous solution of 26ml deioni...

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Abstract

The invention relates to a preparation method of an ozone heterogeneous oxidation solid catalyst, belonging to the technical field of environment-friendly and chemical catalysts. The preparation method comprises the following steps: by taking attapulgite, diopside, illite, ulexite, aluminum hydroxide and celestine porous materials as carriers, performing pore expansion and modification to the carriers through lithium hypochlorite and beryllium bis(acetylacetonate), adding a surfactant methyl trioctylammonium chloride and performing surface activation treatment under ultrasonic wave effect, then leading the ultrasonically surface-activated carriers to have hydrothermal reaction with a complex mineralizer, namely borax and potassium sulfate, catalytic activity assistant precursors, namely praseodymium(III) tris[3-(trifluoromethylhydroxymethylene)-D-camphorate], promethium tricyclopentadienide, tris(4,4,4-trifluoro-1-(2-thienyl)-1,3-butanediono) europium and lutetium carbonate hydrate rare earth metal organic compound, and catalytic active site component precursors, namely common transitional metal organic compound ferrous fumarate, nickel citrate and tungsten catechol ethylenediamine complex and precious metal compound potassium bis(thiocyanate) argentate (I) in a hydrothermal reactor under the action of an emulsifier dodecyl dimethyl (2-hydroxyl) ethylamine chloride, drying reactive products to remove moisture, and firing in a muffle furnace at certain temperature, to obtain the ozone heterogeneous oxidation solid catalyst.

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
CPCB01J20/04B01J20/045B01J20/06B01J20/08B01J20/10B01J20/12B01J20/20C02F1/281C02F1/725C02F1/78B01J23/8993B01J37/084B01J37/10C02F2101/30C02F2305/02B01J2220/4812B01J2220/42B01J2220/4806B01J35/60
Inventor 朱明刘阳宋佳柠
Owner SICHUAN NORMAL UNIVERSITY
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