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Preparation method for solid catalyst for ozone heterogeneous oxidization

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: 2017-08-04
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: the weight ratio of bis(acetylacetonate) beryllium=1:1.2; adding deionized water to wash to neutrality, drying at 103°C to remove moisture, and then sieving 2.75g activated carbon of -200 mesh to +400 mesh standard sieve, Weight of 3.75g carnallite, 4.75g aluminum metahydroxide, 5.75g phosphorite, 6.75g potassium feldspar, 7.75g boromagnesite, lithium hypochlorite and bis(acetylacetonate)beryllium (3g): 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 diethyl maleate base bis(dodecyl dimethyl ammonium chlori...

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 neutrality, dry at 103°C to remove moisture, and then sieve 1.45g of activated carbon of -200 mesh to +400 mesh standard sieve, Weight of 1.65g carnallite, 1.85g aluminum metahydroxide, 2.05g phosphorite, 2.25g potassium feldspar, 2.45g boronite, 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 diethyl maleate bis (dodecyl dimethyl ammonium chloride) dis...

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Abstract

The invention relates to a preparation method for a solid catalyst for ozone heterogeneous oxidization and belongs to the technical field of environmental protection and chemical engineering catalysis. The preparation method comprises the following steps: taking an activated carbon, carnallite, aluminum hydroxide, phosphorite, potash feldspar and szaibelyite porous material as a carrier; modifying the carrier by broaching with lithium hypochlorite and bis(acetylacetone) beryllium, and then adding surfactant diethyl maleate bi(dodecyl dimethyl hydroxyethyl ammonium chloride) and performing surface activating treatment under the effect of ultrasonic wave; performing hydrothermal reaction on an ultrasonic surface activated carrier, a compound mineralizer including borax and potassium sulphate, catalytic activated assistant precursors, including tricyclopentadiene promethium, terbium acetate hydrate, holmium oxalate hydrate and tri(fluoroform sulfimide) ytterbium rare-earth metal organic compound and catalytic active central component precursors, including common transition metal organic compound cobalt gluconate, zinc lactate, diphenol ethylene diamine compound and precious metal chemical complex iridium tetrachloride in a hydrothermal reaction kettle under the effect of octadecyl dimethyl hydroxyethyl perchlorate used as an emulsifier; drying and dewatering the reaction product; and burning in a muffle furnace under a certain temperature, thereby acquiring the solid catalyst for ozone heterogeneous oxidization.

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
CPCB01J20/04B01J20/046B01J20/048B01J20/06B01J20/08B01J20/16B01J20/20C02F1/281C02F1/725C02F1/78B01J23/8993B01J37/084B01J37/10C02F2305/02C02F2101/30B01J2220/4806B01J2220/42B01J2220/4812B01J35/617B01J35/60B01J35/635B01J35/647
Inventor 朱明吴雨婕范耀月
Owner SICHUAN NORMAL UNIVERSITY
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