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Preparation method for solid catalyst for ozone heterogeneous oxidization

A heterogeneous oxidation, solid catalyst technology, applied in the direction of catalyst activation/preparation, physical/chemical process catalyst, catalyst carrier, etc., can solve the problems of easy loss of catalytic activity, low catalyst adsorption, poor toxicity resistance, etc.

Inactive Publication Date: 2017-08-04
SICHUAN NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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 for solid catalyst for ozone heterogeneous oxidization
  • Preparation method for solid catalyst for ozone heterogeneous oxidization

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 basalt, 7.75g magnesia, lithium hypochlorite and bis(acetylacetone) beryllium weight (3g): weight of porous material ( 31.5g)=1:10.5, heat up to 36℃, continue to stir and react for 3.2h, filter and dry at 103℃ to obtain 31g of expanded modified carrier; put 31g of expanded modified carrier in a 500ml ultrasonic reactor, Then add 3.25g of tetradecyltributylammonium chloride in 100ml of deionized water, the weight concentration of the...

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 basalt, 2.45g magnesia, lithium hypochlorite and bis(acetylacetone) beryllium weight (0.6g): weight of porous material (11.7g)=1:19.5, heat up to 48℃, continue to stir and react for 5.8h, filter and dry at 105℃ to obtain 11.5g of expanded modified carrier; put the expanded modified carrier into a 100ml ultrasonic reactor 11.5g, then add 2.2g of tetradecyltributylammonium chloride in 26ml of deionized water solution, the weight concentrati...

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Abstract

The invention relates to a preparation method for a solid catalyst for ozone heterogeneous oxidization and belongs to the technical field of an environment-friendly and chemical catalyst. The preparation method comprises the following steps: by taking medical stone, wollastonite, dolomite, calcite, basalt and blodite as carriers, modifying the carriers by broaching with lithium hypochlorite and bis(acetylacetone) beryllium, and then adding a surfactant, tetradecyl tributyl ammonium chloride, and performing surface activating treatment under the effect of ultrasonic wave; performing hydrothermal reaction on the carriers, compound mineralizers including borax and potassium sulphate, catalytic activated assistant precursors including isopropoxy scandium (III), tri(4,4,4-trifluoro-1-(2-thiophene)-1,3-butanedione) europium, holmium oxalate hydrate and lutetium carbonate hydrate, and catalytic active core component precursors including dicyclopentadienyl titanium substituted salicylic acid complex, zinc lactate, diphenol ethylene diamine tungsten compound and gold potassium chloride in a hydrothermal reaction kettle under the effect of 2,6-bi(diethylamine)-4-nonyl phenol-epoxy chloropropane hyamine used as an emulsifier; drying and dewatering the reaction product; burning in a muffle furnace under a certain temperature, thereby acquiring the solid catalyst for ozone heterogeneous oxidization.

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. Low rate and easy to cause secondary pollution of water make its application limited; Ozone heterogeneous catalytic oxidation technology has catalysts that are easy to separate and recover and can be reused, high ozone...

Claims

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Application Information

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IPC IPC(8): B01J23/68B01J32/00B01J20/20B01J20/30C02F1/28C02F1/78C02F101/30
CPCB01J20/043B01J20/045B01J20/06B01J20/10B01J20/103B01J20/16B01J20/20C02F1/281C02F1/725C02F1/78B01J23/687B01J37/084B01J37/10C02F2305/02C02F2101/30B01J2220/4806B01J2220/42B01J2220/4812B01J35/617B01J35/60B01J35/635B01J35/647
Inventor 朱明苏智岳馥莲
Owner SICHUAN NORMAL UNIVERSITY
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