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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 catalyst, metal/metal oxide/metal hydroxide catalyst, etc., can solve the problem of poor toxicity resistance, easy loss of catalytic activity, Solve the problems of low catalyst adsorption, achieve strong adsorption, improve anti-toxicity and catalytic activity, and inhibit melting and precipitation

Inactive Publication Date: 2017-08-11
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 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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Examples

Experimental program
Comparison scheme
Effect test

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 sodium saltpeter, 5.75g dolomite, 6.75g amazonite, 7.75g laponite, weight of lithium hypochlorite and bis(acetylacetonate)beryllium (3g): weight of porous material (31.5g)=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 , then add 3.25g dimethyl dioctadecyl ammonium chloride and be dissolved in the aqueous solution of 100ml deionized water,...

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 sodium saltpeter, 2.05g dolomite, 2.25g amazonite, 2.45g laponite, lithium hypochlorite and bis(acetylacetonate)beryllium weight (0.6g): Porous material Weight (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 pore-enlarging modified Carrier 11.5g, then add 2.2g dimethyl dioctadecyl ammonium chloride and dissolve in 26ml deionized water aqueous 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 environmental protection and chemical catalysts. The preparation method includes the steps: taking gamma-aluminum oxide, barite, nitratine, dolomite, amazonite and kunzite as carriers; chambering the carriers by lithium hypochlorite and bis(acetylacetonato) beryllium; adding dimethyl double octadecyl ammonium serving as a surface active agent for activation treatment under the action of ultrasonic waves; performing hydrothermal reaction on the carriers with compound mineralizing agents including borax and potassium sulfate, catalytic active auxiliary precursors including tetra(2,2,6,6-tetramethyl-3,5-hydrochelidonic acid) cerium (IV), tri(4,4,4-trifluoro-1-(2-thiophene)-1,3-butanedione) europium, terbium acetate hydrate and tri(fluoroform sulfimide) ytterbium and catalytic active central precursors including copper amino acid chelate, zirconium ammonium carbonate, trisodium hexanitrorhodate and iridium dihydrate tetrachloride in a hydrothermal reactor under the action of trimethylamine stearate ammonium chloride glycolate serving as an emulsifier; drying a reaction product, removing water and firing the reaction product in a muffle furnace 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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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/656B01J32/00B01J20/20B01J20/30C02F1/28C02F1/78C02F101/30
CPCB01J20/04B01J20/041B01J20/043B01J20/045B01J20/06B01J20/08B01J20/16B01J20/20C02F1/281C02F1/725C02F1/78B01J23/6562B01J37/084B01J37/10C02F2101/30C02F2305/02B01J2220/4806B01J2220/42B01J2220/4812B01J35/60
Inventor 朱明范耀月周小澜
Owner SICHUAN NORMAL UNIVERSITY
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