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Preparation method of ozone heterogeneous oxidation solid catalyst

A heterogeneous oxidation, solid catalyst technology, applied in catalyst activation/preparation, physical/chemical process catalysts, metal/metal oxide/metal hydroxide catalysts, etc., can solve the problem of easy loss of catalytic activity and low catalyst adsorption , Poor anti-toxicity and other problems, to achieve the effects of improving anti-toxicity and catalytic activity, inhibiting melting and precipitation, and strong adsorption

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] Embodiment 1:1.4g lithium hypochlorite, 1.7g two (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 2.2%, 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 2.8g erionite of -200 mesh to +400 mesh standard sieve , 3.8g garnet, 4.7g pure diatom, 5.8g kyanite, 6.7g sodium saltpetre, 7.8g dolomite, weight of lithium hypochlorite and bis(acetylacetonate) beryllium (3.1g): weight of porous material (31.6g)=1:10.2, heat up to 36°C, continue stirring for 3.2h, filter, dry at 103°C and obtain 30g of pore-enlarging modified carrier; put 30g of pore-enlarging modified carrier into a 500ml ultrasonic reactor , then add 3.3g dodecyltrimethylammonium chloride dissolved in 100ml deionized water aqueous solution, the weight concentration...

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 erionite of -200 mesh to +400 mesh standard sieve , 1.65g garnet, 1.85g pure diatom, 2.05g kyanite, 2.25g sodium saltpeter, 2.45g dolomite, weight of lithium hypochlorite and bis(acetylacetonate) beryllium (0.6g): weight of porous material (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 the pore-enlarging modified carrier 11.5g, then add 2.2g dodecyltrimethylammonium chloride and be dissolved in the aqueous solution of 26ml deionized water, th...

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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, diatom pure, kyanite, nitratine and dolomite 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, 1,1,1-trifluoroacetyl acetone neodymium and tri[N,N-bis(trimethyl silyl)amide erbium; and performing a hydrothermal reaction with catalytic active central compound precursors a titanocene ring substituted salicylic acid complex, vanadium isonicotinoyl hydrazone pyruvate, zinc lactate and iridic tetrachloride dihydrate under the action of an emulsifier (2-(methacryloyloxy)ethyl) trimethyl 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, 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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IPC IPC(8): B01J23/648B01J32/00B01J20/20B01J20/30C02F1/28C02F1/78C02F101/30
CPCB01J20/04B01J20/043B01J20/06B01J20/103B01J20/14B01J20/16B01J20/165B01J20/20C02F1/281C02F1/725C02F1/78B01J23/6482B01J37/084B01J37/10C02F2101/30C02F2305/02B01J2220/4812B01J2220/4806B01J2220/42B01J35/617B01J35/60B01J35/635B01J35/647
Inventor 朱明丁瑶江燕妮
Owner SICHUAN NORMAL UNIVERSITY
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