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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 catalysts, metal/metal oxide/metal hydroxide catalysts, etc., can solve the problems of poor toxicity resistance, low catalyst adsorption, It is easy to lose catalytic activity and other problems, and achieve the effects of strong adsorption, inhibition of melting and precipitation, and improvement of anti-toxicity and catalytic activity

Inactive Publication Date: 2017-09-15
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 organometallic compounds as catalyst precursors, common transition metal organic compounds and noble metal compounds as catalyst active center precursors, and multi-component porous supports are prepared by hydrothermal reaction and high-temperature calcination to prepare multi-metal-containing ozone heterogeneous oxidation 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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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 wheat rice of -200 mesh to +400 mesh standard sieve 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 tetradecyltributylammonium chloride and be dissolved in the aqueous solution of 100ml deionized water, the weight concentration of this aqueous solution is 3.1%, stir and mix well, tetradecyltribu...

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 wheat rice of -200 mesh to +400 mesh standard sieve 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, add 2.2g tetradecyltributylammonium chloride and be dissolved in the aqueous solution of 26ml deionized water, the weight concentration of this aqueous solution is 7.8%, stir and mix evenly, tetradecyltribut...

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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 environmentally-friendly and chemical catalysts. The preparation method comprises the following steps: by taking medical stone, wollastonite, dolomite, calcite, nitratine and dolomite as carriers, reaming the carriers with lithium hypochlorite and bis(acetylacetone) beryllium, then adding myristyl tributyl ammonia chloride serving as a surfactant for activation treatment under ultrasonic action, putting the carriers into a hydrothermal reaction kettle for hydrothermal reaction together with borax and potassium sulfate which serve as composite mineralizers, isopropyl scandium oxide (III), tri(4,4,4-trifluoro-1-(2-thiophene)-1,3-butanedione) europium, thulium trifluoromethane sulfonate (III) and lutetium carbonate hydrate which serve as catalytic active auxiliary precursors, a dicyclopentadienyl titanium cyclo-replaced salicylic acid complex, zinc lactate and a catechol ethanediamine tungsten complex which serve as catalytic active center precursors and iridium tetrachloride under the action of dimethyl hexadecyl ethyl sulfate serving as an emulsifier, drying a reaction product to remove water, and firing the reaction product in a muffle furnace, thus obtaining 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): B01J23/652B01J35/10B01J37/08B01J37/10B01J37/34B01J20/20B01J20/28B01J20/30
CPCB01J20/06B01J20/20B01J20/28054B01J23/6527B01J37/084B01J37/10B01J37/343B01J35/60
Inventor 朱明苏智岳馥莲
Owner SICHUAN NORMAL UNIVERSITY
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