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Preparation method of ozone heterogeneous oxidation solid catalyst

A heterogeneous oxidation and solid catalyst technology, applied in the direction of heterogeneous catalyst chemical elements, physical/chemical process catalysts, metal/metal oxide/metal hydroxide catalysts, etc., can solve the problem of poor toxicity resistance and catalyst adsorption Low, easy to lose catalytic activity and other issues, to achieve strong adsorption, inhibit smelting out, improve 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

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  • Preparation method of ozone heterogeneous oxidation solid catalyst
  • Preparation method of ozone heterogeneous oxidation solid catalyst

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Embodiment 1

[0007] Example 1: 1.4g lithium hypochlorite, 1.7g bis(acetylacetone) beryllium, 140ml deionized water were added to a 500ml sealable reactor and stirred and mixed uniformly. The weight concentration of the aqueous solution was 2.2%. Lithium chlorate: bis(acetylacetone) beryllium weight ratio=1:1.2; add deionized water to wash to neutrality, dry at 103°C to remove moisture, sieving 2.8g erionite from -200 mesh to +400 mesh standard sieve , 3.8g garnet, 4.7g medical stone, 5.8g wollastonite, 6.7g perlite, 7.8g albite, lithium hypochlorite and bis(acetylacetonate) beryllium weight (3.1g): of porous material Weight (31.6g)=1:10.2, heat up to 36℃, continue to stir and react for 3.2h, filter and dry at 103℃ to obtain 30g of expanded modified carrier; put into the expanded modified carrier in a 500ml ultrasonic reactor 30g, then add 3.3g of dodecyltrimethylammonium chloride in 100ml of deionized water solution, the weight concentration of the aqueous solution is 3.2%, stir and mix eve...

Embodiment 2

[0008] Example 2: 0.24g lithium hypochlorite, 0.36g bis(acetylacetone) beryllium, 10ml deionized water were added to a 100ml sealable reactor and stirred and mixed uniformly. The weight concentration of the aqueous solution was 5.7%. The weight ratio of lithium chlorate: bis(acetylacetone) beryllium=1:1.5; 1.45g erionite that is washed with deionized water until it is neutral, dried at 103℃ to remove water, and then sieved through -200 mesh to +400 mesh standard sieve , 1.65g garnet, 1.85g medical stone, 2.05g wollastonite, 2.25g perlite, 2.45g albite, lithium hypochlorite and bis(acetylacetone) beryllium weight (0.6g): of porous material Weight (11.7g)=1:19.5, heat up to 48°C, continue to stir and react for 5.8h, filter, dry at 105°C to obtain 11.5g of expanded modified carrier; put into the expanded modified carrier in a 100ml ultrasonic reactor Carrier 11.5g, then add 2.2g of dodecyltrimethylammonium chloride in 26ml deionized water solution, the weight concentration of the ...

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Abstract

The invention relates to a preparation method of an ozone heterogeneous oxidation solid catalyst and belongs to the technical field of environmental-friendly and chemical engineering catalysts. The preparation method comprises the following steps: by taking erionite, garnet, medical stones, wollastonite, perlite and albite as a carrier, after chambering and modifying the carrier through lithium hypochlorite and di(acetylacetone) beryllium, adding a surfactant dodecyl trimethyl ammonium chloride for surface activating treatment under the action of ultrasonic waves; then performing a reaction on the ultrasonic surface activated carrier in a hydrothermal reaction kettle and a compound mineralizer borax and potassium sulfate and catalytic active auxiliary agent precursors isoproscandium oxide (III), a tri(hexafluoroacetyl acetone) yttrium (III) dihydrate, lanthanum stearate and tri(2,2,6,6-tetramethyl-3,5- heptylic diketone acid) gadolinium; and performing a hydrothermal reaction on catalytic active central compound precursors a titanocene ring substituted salicylic acid complex, vanadium isonicotinoyl hydrazone pyruvate, manganese lysine and iridic tetrachloride dehydrate under the action of an emulsifier myristyl tributyl ammonium chloride, drying a reaction product to remove water, and firing the reaction product in a muffle furnace 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, belonging to the technical field of environmental protection and chemical catalysts. Background technique [0002] Ozone oxidation technology takes advantage of the strong ability of ozone to oxidize and decompose many organic pollutants, and is widely used in wastewater treatment. Ozone catalytic oxidation technology is divided into homogeneous catalytic oxidation of ozone and heterogeneous catalytic oxidation of ozone. In homogeneous catalytic oxidation of ozone, the catalyst is difficult to separate and recycle and reuse, and the low utilization rate of ozone leads to higher water treatment operating costs and removal of organic pollutants. The low rate and easy to cause secondary pollution of water make its application limited; the ozone heterogeneous catalytic oxidation technology has catalysts that are easy to separate and recover and can be reused, hi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/656B01J32/00C02F1/28C02F1/78C02F101/30
CPCC02F1/281C02F1/725C02F1/78B01J23/002B01J23/6562C02F2101/30B01J2523/00B01J35/50B01J35/617B01J35/40B01J35/635B01J35/647B01J2523/35B01J2523/36B01J2523/3706B01J2523/375B01J2523/47B01J2523/72B01J2523/55B01J2523/827
Inventor 朱明宋佳柠廖乾邑
Owner SICHUAN NORMAL UNIVERSITY