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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 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 effect of strong adsorption, inhibition of melting and precipitation, and improvement of anti-toxicity and catalytic activity

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

AI Technical Summary

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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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; add deionized water to wash to neutrality, dry at 103°C to remove water, sieving 2.75g perlite with -200 mesh ~ +400 mesh standard sieve , 3.75g albite, 4.75g montmorillonite, 5.75g potash, 6.75g brucite, 7.75g serpentinite, lithium hypochlorite and bis(acetylacetonate) beryllium weight (3g): porous material The weight (31.5g)=1:10.5, heat up to 36℃, continue to stir and react for 3.2h, filter, dry at 103℃ to obtain 31g of expanded modified carrier; put into the expanded modified carrier in a 500ml ultrasonic reactor Carrier 31g, then add 3.25g nonylphenol bisquaternary ammonium salt in 100ml deionized water solution, the weight concentration of the aqueous solution is 3.1...

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; add deionized water to wash to neutrality, dry at 103°C to remove the water, sieving 1.45g perlite with -200 mesh to +400 mesh standard sieve , 1.65g albite, 1.85g montmorillonite, 2.05g potash salt, 2.25g brucite, 2.45g serpentine, lithium hypochlorite and bis(acetylacetonate) beryllium weight (0.6g): porous The weight of the material (11.7g)=1:19.5, the temperature is raised to 48℃, and the reaction is continued for 5.8h, filtered, and dried at 105℃ to obtain 11.5g of expanded modified carrier; put into the expanded hole in a 100ml ultrasonic reactor 11.5g modified carrier, then add 2.2g nonylphenol bisquaternary ammonium salt dissolved in 26ml deionized water solution, t...

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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: taking a perlite, albite, montmorillonite, sylvine, brucite and serpentinite porous material as a carrier; modifying the carrier by broaching with lithium hypochlorite and bis(acetylacetone) beryllium, and then adding surfactant nonylphenol diquaternary ammonium salt and performing surface activating treatment under the effect of ultrasonic wave; performing hydrothermal reaction on an ultrasonic surface activated carrier, a compound mineralizer including borax and potassium sulphate, catalytic activated assistant precursors, including 1,1,1-trifluoroacetylacetone neodymium, terbium acetate hydrate, tri[N,N-bi(trimethyl silyl)amide] erbium and tri(fluoroform sulfimide) ytterbium rare-earth metal organic compound and catalytic active core component precursors, including common transition metal organic compound cobalt gluconate, nickel citrate, catechol ethylene diamine tungsten compound and precious metal chemical complex gold potassium chloride in a hydrothermal reaction kettle under the effect of oleamide propyl dimethyl hydroxyethyl ammonium chloride 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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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/89B01J20/20B01J20/30C02F1/78
CPCB01J20/041B01J20/046B01J20/06B01J20/10B01J20/106B01J20/12B01J20/16B01J20/20C02F1/725C02F1/78B01J23/8993B01J37/084B01J37/10C02F2305/02B01J2220/4806B01J2220/42B01J2220/4812B01J35/60
Inventor 朱明何汐然王麒麟
Owner SICHUAN NORMAL UNIVERSITY
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