Sulfonated coal loaded TiO2 photocatalyst and preparation method thereof

A technology of photocatalyst and sulfonated coal, which is applied in the direction of physical/chemical process catalyst, organic compound/hydride/coordination complex catalyst, chemical instrument and method, etc. It can solve the problem of reducing specific surface area, fine particle specific gravity, and not easy to settle and other problems, to achieve the effect of strong photocatalytic performance, simple equipment requirements, and good adsorption performance

Inactive Publication Date: 2014-01-22
TIANJIN UNIV
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Problems solved by technology

[0003] Nano TiO 2 Most of the preparation methods are high-temperature calcinations in muffle furnaces, and high-temperature calcinations have the following two disadvantages: First, high-temperature calcinations can promote nano-TiO 2 Crystal transformation [ 1 ] and strengthen the crystallinity, but it is also easy to cause serious crystal agglomeration and make nano-TiO 2 The size of the grains becomes larger, so that the specific surface area decreases
High crystallinity is beneficial to avoid the recombination of electron-hole pairs, and high specific surface area is conducive to the adsorption of degraded substances, both of which can improve the nano-TiO 2 photocatalytic efficiency [2] , but high temperature calcination increases the crystallinity but reduces the specific surface area
Second, high-temperature calcination not only consumes a lot of energy, but also increases the 2 The production cost limits large-scale investment and application, and also limits the use of some low thermal resistance materials (such as plastics, wood, PET and other organic polymers) as load base materials [3]
However, the current commercial titanium dioxide particles are small and have a small specific gravity, making it difficult to separate, recycle and recycle the photocatalyst by traditional separation methods such as filtration, precipitation, flocculation, and centrifugation. 2 Particles are easy to aggregate and not easy to settle in aqueous solution, the catalyst is difficult to recover, the loss of catalyst active components is large, and the suspended TiO 2 The absorption and blocking of light by particles will affect the irradiation depth of the light source and other reasons. At present, the suspended TiO 2 Photocatalytic systems are mainly used in laboratory research, and it is difficult to carry out large-scale industrial applications, which is not conducive to the recycling and reuse of catalysts [8]
At present, many research works tend to immobilize photocatalysts, which can not only solve the problem of difficult separation and recovery of catalysts, but also overcome the shortcomings of poor stability and easy poisoning of suspended phase catalysts. [9] , and improve the process on this basis, in order to improve the photocatalytic efficiency [10-14]

Method used

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  • Sulfonated coal loaded TiO2 photocatalyst and preparation method thereof
  • Sulfonated coal loaded TiO2 photocatalyst and preparation method thereof
  • Sulfonated coal loaded TiO2 photocatalyst and preparation method thereof

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Embodiment 1

[0032] Such as figure 1 As shown, semi-coke sulfonated coal loaded TiO 2 The photocatalyst preparation process mainly includes: one microwave, constant temperature water bath, centrifugal separation, multiple suction filtration and washing, two microwaves, ultrasonic washing, three microwaves.

[0033] Experimental procedure: add 12g of washed semi-coke sulfonated coal (mass ratio of semi-coke sulfonated coal to solution solute is 1:2.5) 0.15mm-0.3mm semi-coke sulfonated coal into pH=2 sulfuric acid solution dissolved with 30g titanium sulfate (solution concentration 0.1g / mL), stir well, add concentrated ammonia water dropwise until the pH of the mixture is 5-6, after stirring evenly, place the reaction kettle in a modified microwave experimental furnace with a reflux and stirring device, at power P =530W under the condition of microwave irradiation for 1h for the first time, then put the reaction kettle in a constant temperature water bath at 90°C for 11h, centrifuge, wash wi...

Embodiment 2

[0036] Add 3g of washed semi-coke sulfonated coal (mass ratio of semi-coke sulfonated coal to solution solute is 1:10) 0.15mm ~ 0.3mm semi-coke sulfonated coal into pH=2 sulfuric acid solution dissolved with 30g titanium sulfate (solution concentration is 0.2g / L), stir fully, add concentrated ammonia water dropwise until the pH of the mixture is 5-6, and after stirring evenly, place the reaction kettle in a modified microwave experimental furnace with a reflux and stirring device, in a power P=690W Under the conditions of microwave radiation for 75 minutes for the first time, then the reaction kettle was placed in a constant temperature water bath at 95°C for 10 hours, centrifuged, washed with deionized water and absolute ethanol and suction filtered, and the obtained filter cake was put into a microwave experimental furnace. Dry under the same conditions for 45 minutes. After the sample is microwaved again, use an ultrasonic cleaner to vibrate and wash for 20 minutes at 100 H...

Embodiment 3

[0039] Add 12g of washed semi-coke sulfonated coal (mass ratio of semi-coke sulfonated coal to solution solute is 1:2.5) 0.15mm ~ 0.3mm semi-coke sulfonated coal into pH=2 sulfuric acid solution dissolved with 30g titanium sulfate (solution concentration is 0.1g / mL), stir well, add concentrated ammonia water dropwise until the pH of the mixture is 5-6, after stirring evenly, place the reaction kettle in a modified microwave experimental furnace with a reflux and stirring device, under a power P=530W Under the conditions of microwave radiation for 1 hour for the first time, the reaction kettle was then placed in a constant temperature water bath at 90°C for 10 hours, centrifuged, washed with deionized water and absolute ethanol and suction filtered, and the obtained filter cake was put into a microwave experimental furnace. Dry under the same conditions for 45 minutes. After the sample is microwaved again, it is washed with an ultrasonic cleaner at 100 Hz for 30 minutes, filter...

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Abstract

The invention relates to a sulfonated coal loaded TiO2 photocatalyst and a preparation method thereof. A supported nanocrystal TiO2 photocatalyst taking semicoke sulfonated coal as a substrate is prepared through a microwave-liquid phase deposition method by taking high-polymer semi-organic matter sulfonated coal as a carrier and titanium sulfate as a titanium source, wherein the semicoke sulfonated coal as the carrier has the particle size of 0.15-0.3mm. The process comprises primary microwave radiation, centrifugal separation, multiple washing and suction filtration, secondary microwave radiation, ultrasonic wave washing and tertiary microwave radiation. The sulfonated coal loaded TiO2 photocatalyst prepared by the invention is better in adsorption property, high in photocatalytic performance, convenient to recycle, free of loss, incapable of weakening the photocatalytic performance, and suitable for wastewater treatment. The preparation method is simple in process, easy to operate, free of pollution and the like so as to be suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of semiconductor photocatalysts, and relates to a sulfonated coal loaded TiO 2 Photocatalyst and its preparation method. Background technique [0002] Photocatalytic technology is a new environmental treatment technology. In wastewater degradation, it has the advantages of low energy consumption, simple operation, mild reaction conditions, reduced secondary pollution and continuous operation. It has attracted much attention. TiO 2 Photocatalytic materials are currently the most promising photocatalysts. TiO 2 As durable photocatalysts, they have been applied to address various environmental issues. However, nanocrystalline TiO 2 It has not been used on a large scale, mainly because of its high cost, complicated preparation process and possible secondary pollution. [0003] Nano TiO 2 Most of the preparation methods are high-temperature calcinations in muffle furnaces, and high-temperature calcinations...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/38C02F1/30
Inventor 冯炜翟友存
Owner TIANJIN UNIV
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