Single-step hydrothermal micro-emulsion method for preparing iron-doped nano titanium dioxide powder

A technology of nano-titanium dioxide and microemulsion method, which is applied in the preparation of iron-doped nano-titanium dioxide powder and the field of nano-titanium dioxide powder preparation, to achieve the effect of simple equipment, controllable size and high catalytic activity

Inactive Publication Date: 2015-06-17
ZHANJIANG NORMAL UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] The purpose of the present invention is to provide a one-step preparation method of iron-doped nano-titanium dioxide powder. The preparation method selects cheap butyl titanate as the titanium source, reacts in a low-temperature microemulsion hydrothermal environment, and can be prepared in one step. The iron-doped nano-titanium dioxide powder is obtained, which solves the problem of the influence of high temperature treatment on the shape and stability of the product, and has the advantages of simple preparation process, low cost, fast speed, energy saving and high efficiency. The iron prepared by this preparation method doped nano TiO 2 The size of the powder is controllable and uniform, with an average diameter of 10-25 nm, and it is expected to be widely used in the fields of photolysis of water to produce hydrogen and degradation of organic pollutants.

Method used

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  • Single-step hydrothermal micro-emulsion method for preparing iron-doped nano titanium dioxide powder
  • Single-step hydrothermal micro-emulsion method for preparing iron-doped nano titanium dioxide powder
  • Single-step hydrothermal micro-emulsion method for preparing iron-doped nano titanium dioxide powder

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Experimental program
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Effect test

Embodiment 1

[0034] Add 8 ml of alkylphenol polyoxyethylene ether (OP-10), 12 ml of n-butanol (C 4 H 9 OH), 40 ml cyclohexane (C 6 H 12 ), 4 ml butyl titanate (Ti(OC) 4 H 9 ) 4 and 4 ml of ferric chloride (1 M) in hydrochloric acid (0.1 M) in a volume ratio of butyl titanate: alkylphenol ethoxylate: n-butanol: cyclohexane 1:2:3:10 , stir evenly for 15 min, the ratio of oil to water in the above-mentioned water-in-oil W / O microemulsion is 10:1, then transferred to a 100 ml lined polytetrafluoroethylene hydrothermal reaction kettle, put into a constant temperature drying oven at 120 °C, The reaction was kept for 1 h under solvothermal conditions. After the reaction, it was naturally cooled to room temperature, and ultrasonically washed three times with distilled water and absolute ethanol for 50 min each time. The diameter of titanium dioxide powder prepared by this step is about 10-25 nm.

Embodiment 2

[0036] Add 8 ml of alkylphenol polyoxyethylene ether (OP-10), 12 ml of n-butanol (C 4 H 9 OH), 40 ml cyclohexane (C 6 H 12 ), 4 ml butyl titanate (Ti(OC) 4 H 9 ) 4 and 4 ml of ferric chloride (1 M) in hydrochloric acid (0.1 M) in a volume ratio of butyl titanate: alkylphenol ethoxylate: n-butanol: cyclohexane 1:2:3:10 , stir evenly for 15 min, the ratio of oil to water in the above-mentioned water-in-oil W / O microemulsion is 10:1, then transferred to a 100 ml lined polytetrafluoroethylene hydrothermal reaction kettle, put into a constant temperature drying oven at 140 °C, The reaction was kept for 1 h under solvothermal conditions. After the reaction, it was naturally cooled to room temperature, and ultrasonically cleaned with distilled water and absolute ethanol for three times each for 40 min. The product was dried in a drying oven at 60 °C for 24 h under vacuum. The diameter of titanium dioxide powder prepared by this step is about 10-25 nm.

Embodiment 3

[0038] Add 8 ml of alkylphenol polyoxyethylene ether (OP-10), 12 ml of n-butanol (C 4 H 9 OH), 40 ml cyclohexane (C 6 H 12 ), 4 ml butyl titanate (Ti(OC) 4 H 9 ) 4 and 4 ml of ferric chloride (1 M) in hydrochloric acid (0.1 M) in a volume ratio of butyl titanate: alkylphenol ethoxylate: n-butanol: cyclohexane 1:2:3:10 , stir evenly for 15 min, the ratio of oil to water in the above-mentioned water-in-oil W / O microemulsion is 10:1, then transferred to a 100 ml lined polytetrafluoroethylene hydrothermal reaction kettle, and put into a constant temperature drying oven at 160 °C, The reaction was kept for 1 h under solvothermal conditions. After the reaction, it was naturally cooled to room temperature, and ultrasonically cleaned with distilled water and absolute ethanol for three times each for 30 min. The product was dried in a drying oven at 60 °C for 24 h under vacuum. The diameter of titanium dioxide powder prepared by this step is about 10-25 nm.

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Abstract

The invention relates to a single-step hydrothermal micro-emulsion method for preparing iron-doped nano titanium dioxide powder. The single-step hydrothermal micro-emulsion method specifically comprises the following steps of constituting water-in-oil W / O type micro-emulsion by using alkylphenol ethoxylates (OP-10) as a surfactant, using n-butyl alcohol (C4H9OH) as a cosurfactant, using cyclohexane (C6H12) as an oil phase, using butyl titanate (Ti(OC4H9)4) as a titanium source and using hydrochloric acid (HCl) liquor of ferric chloride (FeCl3.6H2O) as a water phase; uniformly stirring, and transferring into a lined polytetrafluoroethylene reaction kettle for keeping heat for 1 hour-5 hours at a constant temperature of 120 DEG C-160 DEG C, naturally cooling to the room temperature; and washing, separating and drying to prepare the iron-doped nano titanium dioxide powder. According to the single-step hydrothermal micro-emulsion method disclosed by the invention, the iron-doped titanium dioxide is obtained by directly reacting in a low-temperature liquid phase, the preparation process is simple, and the prepared iron-doped nano TiO2 powder is controllable in dimension, uniform in size and provided with average diameter of 10 nm-25 nm; moreover, the iron-doped nano TiO2 powder is expected to be widely applied in the fields such as hydrogen production by photodecomposition of water, degradation of organic pollutants, and the like.

Description

technical field [0001] The invention relates to a preparation method of nano titanium dioxide powder, in particular to a preparation method of iron-doped nano titanium dioxide powder which can be completed by a hydrothermal microemulsion method in one step, and belongs to the technical field of inorganic material preparation. Background technique [0002] With the acceleration of the global industrialization process, the problem of environmental pollution is becoming more and more serious, and more and more attention has been paid to the treatment of the environment. In particular, wastewater treatment has become a common concern of all countries in the world. Therefore, the photochemical reaction is in the field of environmental pollution control. widely used. Studies have shown that the photocatalysis of semiconductors can effectively degrade and eliminate harmful pollutants, such as heavy metal ions, dyes, surfactants, organic halides, pesticides, grease, cyanide, harmful...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/745
Inventor 徐旭耀周小松马琳
Owner ZHANJIANG NORMAL UNIV
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