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A kind of cyclic tio2(b) and its preparation method

A cyclic, ionic liquid technology, applied in the direction of titanium dioxide, titanium oxide/hydroxide, etc., can solve the problems of cumbersome preparation steps, low crystallinity, and low product purity

Inactive Publication Date: 2019-04-26
CAPITAL NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, TiO 2 (B) It is not a crystal form naturally occurring in nature, and it needs to be obtained through artificial synthesis, while TiO with high purity and high crystallinity is artificially prepared 2 (B) is also very difficult
Not only the preparation steps are cumbersome and the reaction time is too long, but also the obtained product has low purity and low crystallinity
For example, M.Fehse in France obtained TiO2 under the condition of concentrated alkali, hydrothermal for 3 days, ion exchange under acidic conditions, then drying and high temperature calcination. 2 (B) (J.Power Sources 2013,231:23–28), R.Grosjean from France, etc., shortened the water heating time to 3 hours by using microwave-assisted heating before water heating (J.Power Sources 2015,278 :1–8), but the preparation steps are still very cumbersome
However, cyclic TiO with high purity and high crystallinity was prepared by ionic liquid-assisted one-step hydrothermal method. 2 (B) Not yet reported

Method used

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  • A kind of cyclic tio2(b) and its preparation method
  • A kind of cyclic tio2(b) and its preparation method

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] (1) 10ml of tetra-n-butyl titanate is added to 3.4ml of trifluoroacetic acid solution with a mass concentration of 50% for hydrolysis, wherein the molar ratio of tetra-n-butyl titanate:trifluoroacetic acid is 1:0.5, and the room temperature is severe After stirring for 1 hour, the obtained yellow-brown solution was evaporated to dryness with a rotary evaporator to remove volatile by-products to obtain a soluble xerogel;

[0025] (2) 0.5g of the soluble xerogel obtained in step (1) was dissolved in 20mL of water, 1-butyl-3-methylimidazole tetrafluoroborate was added, and the addition amount was 1mL, and then the mixed solution was put into In a PTFE-lined stainless steel autoclave, the hydrothermal reaction was carried out at 180 °C for 24 hours. After the reaction is completed, the obtained precipitated product is filtered, washed and dried to obtain cyclic TiO 2 (B). The prepared cyclic TiO 2 (B) has a diameter of 450 nm and a pore size of 170 nm.

Embodiment 2

[0027] (1) 10ml of tetra-n-butyl titanate is added to 6.8ml of trifluoroacetic acid solution with a mass concentration of 50% for hydrolysis, wherein the molar ratio of tetra-n-butyl titanate:trifluoroacetic acid is 1:1, and the room temperature is violent After stirring for 1 hour, the obtained yellow-brown solution was evaporated to dryness with a rotary evaporator to remove volatile by-products to obtain a soluble xerogel;

[0028] (2) 0.5g of the soluble xerogel obtained in step (1) was dissolved in 20mL of water, 1-butyl-3-methylimidazolium hexafluorophosphate was added, and the addition amount was 0.5mL, and then the mixed solution was put into into a PTFE-lined stainless steel autoclave, and hydrothermally reacted at 230°C for 48 hours. After the reaction is completed, the obtained precipitated product is filtered, washed and dried to obtain cyclic TiO 2 (B). The prepared cyclic TiO 2 (B) has a diameter of 400 nm, a pore size of 100 nm, and a purity of 98%, as shown ...

Embodiment 3

[0030] (1) 10ml of tetra-n-butyl titanate is added to 13.6ml of trichloroacetic acid solution with a mass concentration of 75% and hydrolyzed, wherein the tetra-n-butyl titanate: the mol ratio of trichloroacetic acid is 1:3, and the room temperature is violent After stirring for 1 hour, the obtained yellow-brown solution was evaporated to dryness with a rotary evaporator to remove volatile by-products to obtain a soluble xerogel;

[0031] (2) Dissolve 0.8 g of the soluble xerogel obtained in step (1) in 20 mL of water, add N,N-diethyl-N-methyl-N-(2-methoxyethyl)ammonium tetrafluoroboron acid salt, the addition amount is 50 mL, and then the mixed solution is put into a stainless steel autoclave lined with PTFE, and hydrothermally reacted at 180° C. for 48 hours. After the reaction is completed, the obtained precipitated product is filtered, washed and dried to obtain cyclic TiO 2 (B). The prepared cyclic TiO 2 (B) has a diameter of 420 nm, a pore diameter of 160 nm, and a pu...

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Abstract

The invention relates to an annular TiO2(B) and a preparation method thereof. The preparation method comprises the following steps: hydrolyzing titanate in an aqueous solution of an organic acid, and drying the hydrolyzed titanate to obtain soluble xerogel; and dissolving the soluble xerogel in water, adding an ionic liquid, placing the obtained solution in a high pressure reaction kettle, and carrying out a hydrothermal reaction to obtain the high-purity and high-crystallinity annular TiO2(B). The preparation method has the advantages of simplicity in operation, and low cost. The prepared TiO2(B) has high purity and high crystallinity, and the preparation method is suitable for large-scale commercial production of the high-purity and high-crystallinity TiO2(B).

Description

technical field [0001] The invention belongs to the field of preparation of inorganic non-metallic materials, in particular to a cyclic TiO 2 (B) and its preparation method. Background technique [0002] Nano TiO 2 Due to its unique optical and electrical properties, it is widely used in photocatalytic degradation of organic pollutants, photocatalytic water production of H 2 It has important applications in the fields of solar cells and energy storage. Therefore, it has played an increasingly important role in alleviating the environmental and energy crisis. It is considered as one of the most promising materials because of its advantages of non-toxicity, low cost, abundant content and good chemical stability. [0003] TiO 2 There are 3 crystal forms in nature: anatase, rutile and brookite. There are also 5 crystal forms that need to be obtained by synthesis, namely TiO 2 (B), TiO 2 (R), TiO 2 (H), TiO 2 (II) and TiO 2 (III). Among them, TiO 2 (B) is TiO 2 It i...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G23/053
CPCC01G23/053C01P2002/72C01P2004/03C01P2004/62C01P2006/16C01P2006/80
Inventor 孟祥福吕立贞刘秀云王苗苗王丽丽闫文文李彤
Owner CAPITAL NORMAL UNIVERSITY