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Preparation method of ozone heterogeneous oxidation solid catalyst

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, catalyst adsorption It can improve the anti-toxicity and catalytic activity, inhibit the melting and precipitation, and have the effect of strong adsorption.

Inactive Publication Date: 2017-08-18
SICHUAN NORMAL UNIVERSITY
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  • 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
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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 wheat rice of -200 mesh to +400 mesh standard sieve Weight of limestone, 3.75g wollastonite, 4.75g bentonite, 5.75g polyhalite, 6.75g basalt, 7.75g langbeinite, 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 of octadecyltrimethylammonium chloride dissolved in 100ml of deionized water, 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 wheat rice of -200 mesh to +400 mesh standard sieve Weight of limestone, 1.65g wollastonite, 1.85g bentonite, 2.05g polyhalite, 2.25g basalt, 2.45g langbeinite, lithium hypochlorite and bis(acetylacetonate) beryllium (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, add the aqueous solution that 2.2g octadecyltrimethylammonium chloride is dissolved in 26ml deionized water again, ...

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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 environment protection and chemical catalysts. The preparation method includes: using medical stone, wollastonite, bentonite, polyhalite, basalt and blodite as the carriers, using lithium hypochlorite and bis(acetylacetone) beryllium to perform pore expansion on the carriers, adding chlorinated octadecyl trimethyl ammonium to activate the carriers under ultrasonic action, allowing the carriers to have hydrothermal reaction with compound mineralizer including borax and potassium sulfate, catalytic activity promoter precursors including scandium(III) isopropoxide, holmium oxalate decahydrate, tri[N, N-bis(trimethyl silane) amine] erbium and tri(trifluoromethane sulfonimide) ytterbium, and catalytic activity central component precursors including titanocene ring substituted salicylic acid complex, L-aspartic acid molybdenum, K[Ag(SCN)2] and tetraammine dichloropalladium(II) in a hydrothermal reaction kettle under the effect of di(octadecyl) lauryl methyl ammonium bromide, drying to remove moisture, and burning 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): B01J23/89B01J32/00C02F1/28C02F1/78C02F101/30
CPCC02F1/281C02F1/725C02F1/78B01J23/002B01J23/8993B01J2523/00C02F2101/30B01J35/50B01J35/40B01J2523/11B01J2523/21B01J2523/13B01J2523/35B01J2523/3768B01J2523/3775B01J2523/3787B01J2523/47B01J2523/68B01J2523/824
Inventor 朱明夏梦琦宋佳柠
Owner SICHUAN NORMAL UNIVERSITY
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