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Method for preparing ozone heterogeneous oxidation solid catalyst

A heterogeneous oxidation, solid catalyst technology, applied in catalyst activation/preparation, physical/chemical process catalyst, metal/metal oxide/metal hydroxide catalyst, etc., can solve the problem of low catalyst adsorption, poor toxicity resistance, It is easy to lose catalytic activity and other problems, and achieve the effects of inhibiting precipitation, strong adsorption, and improving anti-toxicity and catalytic activity.

Inactive Publication Date: 2017-09-05
SICHUAN NORMAL UNIVERSITY
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  • Claims
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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

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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 of perlite with -200 mesh to +400 mesh standard sieve , 3.75g albite, 4.75g aluminum metahydroxide, 5.75g phosphorite, 6.75g magnesium spinel, 7.75g peridotite, weight of lithium hypochlorite and bis(acetylacetonate) beryllium (3g): Porous The weight of the material (31.5g) = 1:10.5, raised the temperature to 36°C, continued to stir and react for 3.2h, filtered, and dried at 103°C to obtain a pore-expanding modified carrier of 31g; in a 500ml ultrasonic reactor, put the pore-expanding modified 31g of carrier, then add 3.25g of nonylphenolic bisquaternary ammonium salt ...

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: the weight ratio of bis(acetylacetonate) beryllium=1:1.5; add deionized water to wash to neutral, dry at 103°C to remove moisture, and then sieve 1.45g perlite of -200 mesh to +400 mesh standard sieve , 1.65g albite, 1.85g aluminum metahydroxide, 2.05g phosphorite, 2.25g magnesium spinel, 2.45g peridotite, weight of lithium hypochlorite and bis(acetylacetonate) beryllium (0.6g): The weight of the porous material (11.7g) = 1:19.5, heated up to 48°C, continued to stir for 5.8h, filtered, and dried at 105°C to obtain a pore-expanding modified carrier of 11.5g; in a 100ml ultrasonic reactor, put the expanded Pore ​​modified carrier 11.5g, then add 2.2g nonylphenol base biquaternary ammonium salt and be dissolved in...

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Abstract

The invention relates to a method for preparing an ozone heterogeneous oxidation solid catalyst and belongs to the technical field of environmental protection and chemical catalysts. The preparation method comprises the following steps: taking perlite, albite, aluminum hydroxide, phosphorite, magnesia spinel and olivinite porous materials as a carrier, performing pore-enlarging modification on the carrier through lithium hypochlorite and bis(acetylacetonato) beryllium, and adding a surfactant nonyl phenol based biquaternary ammonium salt for performing surface activation treatment under the ultrasonic action; and enabling the ultrasonic surface activation carrier to be subjected to a hydrothermal reaction with compound mineralizers such as borax and potassium sulfate, catalytic active aid precursor neodymium 1,1,1-trifluoroacetylacetone, tris(2,2,6,6-tetramethyl-3,5-heptanedionato) gadolinium, thulium trifluoromethane sulfonate (III) and lutetium carbonate hydrate (III) rare-earth metal organic compounds, catalytic active center component precursor ordinary transition metal organic compounds such as cobalt gluconate, nickel citrate and L-aspartic acid molybdenum as well as a precious metal chemical complex dipotassium hexachloroosmate Pt in a hydrothermal reactor in the presence of an emulsifier diethyl maleate based bis(dodecyl dimethyl ammonium chloride), drying the reaction product to remove the moisture, firing in a muffle furnace, thereby obtaining 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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IPC IPC(8): B01J23/89B01J32/00B01J20/20B01J20/30C02F1/28C02F1/78C02F101/30
CPCB01J20/048B01J20/06B01J20/08B01J20/103B01J20/106B01J20/16B01J20/20C02F1/28C02F1/725C02F1/78B01J23/8993B01J37/084B01J37/10C02F2101/30C02F2305/02B01J2220/4806B01J2220/42B01J2220/4812B01J35/60B01J35/617B01J35/635B01J35/647
Inventor 朱明石小阳周小澜
Owner SICHUAN NORMAL UNIVERSITY
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