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Method for preparing TiO2-PS nucleocapsid structure nano powder by microwave assisted hydrothermal method

A core-shell structure, microwave hydrothermal technology, applied in the direction of microsphere preparation, microcapsule preparation, chemical instruments and methods, etc., can solve the problems of high energy consumption and long reaction time (several days or longer) The effects of fast nuclear growth, short reaction time, and low energy consumption

Inactive Publication Date: 2008-12-17
SHANDONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, the hydrothermal-solvothermal reaction method is a commonly used and effective method for preparing nanomaterials, but it has the disadvantages of long reaction time (several days or longer) and high energy consumption.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] (1) Preparation of PS polystyrene bead microemulsion: add 150g of deionized water, 90g of styrene and 0.48g of potassium persulfate into a three-necked flask under the protection of high-purity nitrogen to prepare a volume of about 240ml of styrene before polymerization The body was vigorously stirred by electromagnetic for 1 hour, and 50ml of deionized water dissolved with 2.15g of sodium laurate was slowly added dropwise into the reaction system within 1 hour. Heat the water bath to 65°C to start the reaction, react for 3 hours, stop heating, and obtain polystyrene PS bead microemulsion with a diameter of tens of nanometers and uniform size.

[0014] (2) Mix 5ml of PS microemulsion with 15ml of tetrabutyl titanate, and add 100ml of ionized water or alcohols or organic acids to hydrolyze, alcoholyze or acidolyze tetrabutyl titanate. Add 25ml of ammonia water to facilitate complete hydrolysis, alcoholysis or acidolysis of tetrabutyl titanate, and dilute the system to 25...

Embodiment 2

[0018] (1) Preparation of PS polystyrene bead microemulsion: add 200g of deionized water, 140g of styrene and 1.0g of potassium persulfate into a three-necked flask under the protection of high-purity nitrogen to prepare a volume of about 340ml of styrene before polymerization The body was vigorously stirred by electromagnetic for 2 hours, and 100ml of deionized water dissolved with 5g of sodium laurate was slowly added dropwise into the reaction system within 2 hours. The water bath is heated to 65° C. to start the reaction, and the heating is stopped after 5 hours of reaction to obtain a uniform polystyrene PS bead microemulsion with a diameter of tens of nanometers.

[0019] (2) Mix 10ml of PS bead microemulsion with 20ml of tetrabutyl titanate, and add 150ml of ionized water or alcohols or organic acids to hydrolyze, alcoholyze or acidolyze tetrabutyl titanate. Add 30ml of ammonia water to facilitate complete hydrolysis, alcoholysis or acidolysis of tetrabutyl titanate, an...

Embodiment 3

[0023] (1) Preparation of PS polystyrene bead microemulsion: Add 200 g of deionized water, 160 g of styrene and 0.8 g of potassium persulfate into a three-necked flask under the protection of high-purity nitrogen to prepare a volume of about 360 ml of styrene before polymerization. The body was vigorously stirred by electromagnetic for 3 hours, and 175ml of deionized water dissolved with 6.15g of sodium laurate was slowly added dropwise into the reaction system within 3 hours. The water bath was heated to 65° C. to start the reaction, and the heating was stopped after 4 hours of reaction to obtain a microemulsion of polystyrene PS beads with a diameter of tens of nanometers and a uniform size.

[0024](2) Mix 8ml of PS microemulsion with 18ml of tetrabutyl titanate, and add 120ml of ionized water or alcohols or organic acids to hydrolyze, alcoholyze or acidolyze tetrabutyl titanate. Add 28ml of ammonia water to facilitate complete hydrolysis, alcoholysis or acidolysis of tetra...

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Abstract

The invention provides a method for preparing nanometer beads of TiO2-PS core-shell structure by microwave hydrothermal which comprises the following steps: (1) a PS bead microemulsion is prepared or purchased with the diameter between 10nm and 999nm; (2) the PS bead micro-emulsion and tetrabutyl titanate are mixed according to certain ratio, ionic water or alcohol or organic acid is added to carry out hydrolysis, alcoholysis or acidolysis towards the tetrabutyl titanate; ammonia water is added during the hydrolysis process and deionized water is used for dilution; the microemulsion of TiO2-PS core-shell former body is obtained after 1 hour of ultrasonic vibration, heating, boiling and reflux; (3) the microemulsion of TiO2-PS core-shell former body prepared is transferred to a microwave hydrothermal reaction device to react, so as to obtain the nanometer microemulsion of TiO2-PS core-shell structure; (4) the nanometer microemulsion of TiO2-PS core-shell structure prepared is dried in an oven to obtain the nanometer beads of TiO2-PS core-shell structure. The method of the invention has the advantages of fast nucleation growth of the nano-crystalline, short reaction period, low energy consumption, etc.

Description

technical field [0001] The present invention relates to a kind of TiO 2 -Microwave hydrothermal rapid preparation method of PS (titanium dioxide-polystyrene) core-shell structure nanospheres, belonging to TiO 2 - PS nano powder preparation technical field. Background technique [0002] Titanium dioxide (TiO 2 ) is a wide bandgap semiconductor material, which generally has rutile phase, anatase phase and brookite phase. Brookite TiO 2 No photocatalytic activity, rutile TiO 2 The activity is also low. Experiments show that anatase TiO 2 Catalyzes the production of H 2 The rate is rutile TiO 2 7 times. This is because on the one hand the rutile TiO 2 The band gap is small (rutile TiO 2 The forbidden band width is 3.1eV, while that of anatase is 3.3eV), and its positive conduction band hinders the O 2 reduction reaction; on the other hand, rutile TiO 2 It is the most stable crystal structure form, with a relatively complete crystal structure, small defects, photoindu...

Claims

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Application Information

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IPC IPC(8): B01J13/02C30B7/10C01G23/047B01J21/06B01J35/08B01J37/02
Inventor 尉吉勇张晓阳秦晓燕黄柏标
Owner SHANDONG UNIV
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