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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: 2017-09-15
SICHUAN NORMAL UNIVERSITY
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  • Claims
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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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  • Preparation method of ozone heterogeneous oxidation solid catalyst
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Examples

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Embodiment 1

[0007] Example 1: 1.35g lithium hypochlorite, 1.65g 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 2.1%. The weight ratio of lithium chlorate: bis(acetylacetone) beryllium=1:1.2; 2.75g wheat rice which is washed with deionized water until it is neutral, dried at 103°C to remove water, and then sieved through -200 mesh to +400 mesh standard sieve The weight of stone, 3.75g wollastonite, 4.75g dolomite, 5.75g calcite, 6.75g hydrotalcite, 7.75g magnesia, lithium hypochlorite and bis(acetylacetone) beryllium weight (3g): weight of porous material (31.5g)=1:10.5, heat up to 36°C, continue to stir and react for 3.2h, filter, dry at 103°C to obtain 31g of expanded modified carrier; put 31g of expanded modified carrier in a 500ml ultrasonic reactor , Then add 3.25g tetradecyltributylammonium chloride in 100ml deionized water solution, the weight concentratio...

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 wheat rice which 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 Weight of stone, 1.65g wollastonite, 1.85g dolomite, 2.05g calcite, 2.25g hydrotalcite, 2.45g magnesia, 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 tetradecyltributylammonium chloride in 26ml deionized water solution, the weight c...

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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, hydrotalcite and blodite, 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, tri[N,N-bis(trimethylsilane)amine] erbium and thulium trifluoromethane sulfonate which serve as catalytic active auxiliary precursors and a dicyclopentadienyl titanium cyclo-replaced salicylic acid complex, zinc lactate, a catechol ethanediamine tungsten complex and terpyridyl ruthenium chloride hexahydrate which serve as catalytic active center precursors under the action of N-dodecyl dimethyl-N'-trimethyl-2-hydroxypropyl ammonia dichloride 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, 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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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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