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Preparation method of 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 poor anti-toxicity, low catalyst adsorption, It is easy to lose catalytic activity and other problems, and achieve the effects 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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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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  • Preparation method of ozone heterogeneous oxidation solid catalyst
  • Preparation method of ozone heterogeneous oxidation solid catalyst

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 wheat rice of -200 mesh to +400 mesh standard sieve Stone, 3.75g wollastonite, 4.75g light shale ceramsite, 5.75g pyrophyllite, 6.75g sodium saltpetre, 7.75g dolomite, lithium hypochlorite and bis(acetylacetonate)beryllium weight (3g): Porous material The weight (31.5g)=1:10.5, heat up to 36°C, continue to stir and react for 3.2h, filter, dry at 103°C and obtain 31g of pore-enlarging modified carrier; in a 500ml ultrasonic reactor, put pore-enlarging modified Carrier 31g, add the aqueous solution that 3.25g cetyltrimethylammonium bromide is dissolved in 100ml deioniz...

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 Stone, 1.65g wollastonite, 1.85g light shale ceramsite, 2.05g pyrophyllite, 2.25g sodium saltpeter, 2.45g dolomite, lithium hypochlorite and bis(acetylacetonate) beryllium weight (0.6g): Porous The weight of the material (11.7g)=1:19.5, heat up to 48°C, continue to stir and react for 5.8h, filter, and dry at 105°C to obtain a pore-expanding modified carrier of 11.5g; put it into a 100ml ultrasonic reactor Modified carrier 11.5g, add the aqueous solution that 2.2g cetyltrimethylammonium bromide is dissolved in 26ml d...

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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-friendly and chemical engineering catalysts. The preparation method comprises the following steps: by taking medical stones, wollastonite, light shale ceramisite, pyrophyllite, nitratine and dolomite as carriers, after chambering and modifying the carriers through lithium hypochlorite and di(acetylacetone) beryllium, adding a surfactant, octadecyl trimethyl ammonium chloride, for surface activating treatment under the action of ultrasonic waves; then causing the carriers to generate hydrothermal reaction with borax and potassium sulfate which serve as compound mineralizers, isoproscandium oxide (III), 1,1,1-trifluoroacetyl acetone neodymium, tri(2,2,6,6-tetramethyl-3,5- heptylic diketone acid) gadolinium and holmium oxalate decahydrate which serve as catalytic active auxiliary agent precursors, and a titanocene ring substituted salicylic acid complex, nickel citrate, molybdenum L-aspartate and gold potassium tetrachloride which serve as catalytic active central compound precursors in a hydrothermal reaction kettle under the action of an emulsifier, N-octadecyl dimethyl-N'-propyl ammonium dichloride, drying a reaction product to remove 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): B01J23/89B01J32/00B01J20/20B01J20/30C02F1/28C02F1/78C02F101/30
CPCB01J20/04B01J20/043B01J20/06B01J20/10B01J20/12B01J20/16B01J20/20C02F1/281C02F1/725C02F1/78B01J23/8993B01J37/084B01J37/10C02F2305/02C02F2101/30B01J2220/42B01J2220/4806B01J2220/4812B01J35/617B01J35/60B01J35/635B01J35/647
Inventor 朱明秦丹苏智
Owner SICHUAN NORMAL UNIVERSITY
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