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Ozone heterogeneous oxidation solid catalyst preparation method

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

Method used

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  • Ozone heterogeneous oxidation solid catalyst preparation method

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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 -200 mesh to +400 mesh standard sieve 2.75g γ-oxidized Aluminum, 3.75g barite, 4.75g activated carbon, 5.75g carnallite, 6.75g dolomite, 7.75g calcite, weight of lithium hypochlorite and bis(acetylacetonate)beryllium (3g): weight of porous material (31.5 g)=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, and then Add 3.25g ditetradecyl dimethyl ammonium chloride and be dissolved in the aqueous solution of 100ml deionized wa...

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 -200 mesh to +400 mesh standard sieve 1.45g gamma-oxidized Aluminum, 1.65g barite, 1.85g activated carbon, 2.05g carnallite, 2.25g dolomite, 2.45g calcite, 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 11.5g of pore-enlarging modified carrier g, then add 2.2g of ditetradecyldimethylammonium chloride dissolved in 26ml deionized water aqueous solution, th...

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Abstract

The invention relates to an ozone heterogeneous oxidation solid catalyst preparation method, belonging to the technical field of environmental protection and chemical catalysts. The ozone heterogeneous oxidation solid catalyst preparation method comprises the following steps: carrying out pore-expanded modification on porous materials such as gamma-aluminum oxide, barite, activated carbon, carnallite, dolomite and calcite which serve as carriers by using lithium hypochlorite and bis(acetylacetone) beryllium, then adding ditetradecyl dimethyl ammonium chloride serving as a surface active agent to carry out surface activating treatment under the action of ultrasonic waves, and causing ultrasound surface activated carriers to generate hydrothermal reaction with borax and potassium sulfate which serve as composite mineralizers, rare earth organo metallic compounds such as cerium(IV)-2,2,6,6-tetramethylheptanedionate, tris(3-trifluoroacetyl-D-camphor)praseodymium(III), thulium(III) trifluoromethanesulfonate, and tris(trifluoromethane sulfimide) ytterbium which serve as catalytic activity assistant precursors, common transition organometallic compounds such as manganese lysine and cupric glutamate and precious metal compounds such as dithiocyanide potassium silver (I) and hexanitroso rhodium trisodium which serve as catalytic activity center components under the action of 2, 6-bis(diethylamino methyl)-4-nonylphenol-epichlorohydrin quaternary ammonium salt serving as an emulsifying agent in a hydrothermal reaction kettle, drying a reaction product to remove moisture, and firing in a muffle furnace at a 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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IPC IPC(8): B01J23/89B01J32/00B01J20/20B01J20/30C02F1/28C02F1/78C02F101/30
CPCB01J20/043B01J20/045B01J20/046B01J20/06B01J20/08B01J20/20C02F1/281C02F1/725C02F1/78B01J23/8986B01J37/084B01J37/10C02F2305/02C02F2101/30B01J2220/42B01J2220/4806B01J2220/4812B01J35/617B01J35/60B01J35/635B01J35/647
Inventor 朱明周小澜刘阳
Owner SICHUAN NORMAL UNIVERSITY
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