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Method for preparing ozone heterogeneous oxidation solid catalysts

A heterogeneous oxidation, solid catalyst technology, applied in heterogeneous catalyst chemical elements, physical/chemical process catalysts, metal/metal oxide/metal hydroxide catalysts, etc., can solve the problem of easy loss of catalytic activity and anti-toxicity. It can improve the anti-toxicity and catalytic activity, strong adsorption, and inhibit the effect of melting and precipitation.

Inactive Publication Date: 2017-08-18
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 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

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 2.75g attapulgite of -200 mesh to +400 mesh standard sieve Weight of soil, 3.75g diopside, 4.75g fluorite, 5.75g glauberite, 6.75g magnesium spinel, 7.75g peridotite, lithium hypochlorite and bis(acetylacetonate)beryllium (3g): Porous material Weight (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; in a 500ml ultrasonic reactor, put the pore-enlarging modified carrier 31g, then add 3.25g trilauryl ammonium chloride dissolved in 100ml deionized water aqueous solution, the weight concentratio...

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 attapulgite of -200 mesh to +400 mesh standard sieve Weight of soil, 1.65g diopside, 1.85g fluorite, 2.05g glauberite, 2.25g magnesium spinel, 2.45g peridotite, lithium hypochlorite and bis(acetylacetonate)beryllium (0.6g): porous material The weight (11.7g)=1:19.5, heat up to 48°C, continue to stir and react for 5.8h, filter, dry at 105°C and obtain 11.5g of pore-enlarging modified carrier; in a 100ml ultrasonic reactor, put the pore-enlarging modified Carrier 11.5g, add 2.2g trilauryl ammonium chloride and be dissolved in the aqueous solution of 26ml deionized water ...

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Abstract

The invention relates to a method for preparing ozone heterogeneous oxidation solid catalysts, and belongs to the technical field of environmental protection and chemical catalysts. The method includes carrying out pore expansion and modification on carriers which are attapulgite, diopside, fluorite, glauberite, magnesia spinel and peridotite porous materials by the aid of lithium hypochlorite and bis (acetylacetone) beryllium; adding tri-lauryl ammonium chloride into the carriers and carrying surface activation treatment on the carriers under the effects of ultrasonic waves; carrying out hydrothermal reaction on the carriers which are subjected to ultrasonic surface activation, borax, potassium sulfate, tri (3-trifluoroacetyl-D-camphor) praseodymium (III), promethium tricyclic pentadiene, tri-(6, 6, 7, 7, 8, 8, 8-heptafluoro-2, 2-dimethyl-3, 5-octene diketone) dysprosium (III), thulium trifluoromethanesulfonate (III) rare earth metal organic compounds, ferrous fumarate, nickel citrate, gold potassium chloride and hexa-nitroso rhodium trisodium in hydrothermal reaction kettles under the effect of N-dimethyl dodecyl-N'-dodecyl-dimethyl-2-hydroxypropyl ammonium dichloride which is an emulsifier; drying reaction products to remove moisture; burning the reaction products in muffle furnaces at the certain temperatures to obtain the ozone heterogeneous oxidation solid catalysts. The tri-lauryl ammonium chloride is used as a surfactant. The borax and the potassium sulfate are used as composite mineralizers, the tri (3-trifluoroacetyl-D-camphor) praseodymium (III), the promethium tricyclic pentadiene, the tri-(6, 6, 7, 7, 8, 8, 8-heptafluoro-2, 2-dimethyl-3, 5-octene diketone) dysprosium (III) and the thulium trifluoromethanesulfonate (III) rare earth metal organic compounds are used as catalytic active auxiliary precursors, the ferrous fumarate, the nickel citrate, the gold potassium chloride and the hexa-nitroso rhodium trisodium are used as catalytic active central components, the ferrous fumarate is a common transition metal organic compound, and the gold potassium chloride and the hexa-nitroso rhodium trisodium are precious metal compounds.

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): B01J23/89B01J32/00C02F1/28C02F1/78
CPCC02F1/281C02F1/725C02F1/78B01J23/002B01J23/8946C02F2101/30B01J2523/00B01J35/50B01J35/40B01J2523/13B01J2523/3718B01J2523/3731B01J2523/3762B01J2523/3781B01J2523/842B01J2523/847B01J2523/12B01J2523/11B01J2523/21
Inventor 朱明刘阳宋佳柠
Owner SICHUAN NORMAL UNIVERSITY
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