Method for preparing titanium polyacetylacetonate precursor sol spinning solution, titanium oxide continuous fiber and titanium oxide nanofiber

A technology of sol spinning solution and titanium precursor, which is applied in the direction of spinning solution preparation, dry spinning method, fiber treatment, etc., can solve the problem of difficult preparation of high-quality titanium oxide fiber, limit the popularization and application of titanium oxide powder, and make sol spinnable It has the advantages of easy separation and collection, good spinnability and low cost.

Active Publication Date: 2018-11-30
SHANDONG UNIV
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  • Application Information

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Problems solved by technology

Chinese patent document CN101314482A proposes a method for preparing anatase titanium oxide powder. The photocatalytic activity of anatase powder is relatively high, but due to the limitation of powder form, it is difficult to recycle and easy to cause secondary pollution. problems, and if the fixed technology will affect the photocatalytic activity, these problems limit the popularization and application of titanium oxide powder
The hydrolysis and polycondensation process of this method is still difficult to control, and the impurity Cl is inevitably introduced with titanium tetrachloride as the titanium source. - , affecting the quality of TiO fibers in subsequent sintering
CN100581648A has prepared titanium oxide fiber membrane by electrospinning, and its spinning liquid is that tetrabutyl titanate is dissolved in absolute ethanol, and absolute alcohol plays the role of suppressing hydrolysis, controls the pH value of solution by hydrochloric acid to control solution The hydrolysis polycondensation process of this method, the hydrolysis process control of this method is unstable, the preparation process is relatively complicated, and the sol spinnability and stability are not good
At present, the preparation of titanium oxide fibers mainly has the following two problems: one is that the price is high and the preparation process is complicated, the stability of the sol is poor, and it is difficult to prepare high-quality titanium oxide fibers; the other is that impurities will be introduced during the preparation process, which will affect the fiber quality.

Method used

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  • Method for preparing titanium polyacetylacetonate precursor sol spinning solution, titanium oxide continuous fiber and titanium oxide nanofiber
  • Method for preparing titanium polyacetylacetonate precursor sol spinning solution, titanium oxide continuous fiber and titanium oxide nanofiber
  • Method for preparing titanium polyacetylacetonate precursor sol spinning solution, titanium oxide continuous fiber and titanium oxide nanofiber

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Experimental program
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Embodiment 1

[0067] A preparation method of polyacetylacetonate titanium precursor sol spinning solution, comprising the following steps:

[0068] (1) Preparation of polyacetylacetonate titanium precursor

[0069] According to the molar ratio of tetrabutyl titanate: glacial acetic acid: water = 1:3:1, weigh 100g tetrabutyl titanate, 52.94g glacial acetic acid and 5.29g water, fully stir and react for 3h to obtain a golden yellow solution. It was placed in a flask and concentrated under reduced pressure at a temperature of 65°C for 6h until a dry solid product was obtained, which was dissolved in 200g of anhydrous methanol; the molar ratio of tetrabutyl titanate: acetylacetone: water = 1: 1:0.5 Add 29.41g of acetylacetone and 2.65g of water, stir and react for 3 hours to obtain a golden-red solution, that is, titanium polyacetylacetonate solution, put the golden-red solution in a flask, and concentrate under reduced pressure at a temperature of 65°C for 6 hours until A dry solid product, n...

Embodiment 2

[0078] A preparation method of titanium oxide nanofibers, comprising the following steps:

[0079] (i) Preparation of polyacetylacetonate titanium precursor sol spinning solution

[0080] Adopt the method in embodiment 1 to prepare polyacetylacetonate titanium alloy precursor sol spinning liquid, be used for electrospinning;

[0081] (ii) Electrospinning

[0082] The polyacetylacetonate titanium precursor sol spinning solution obtained in step (i) is placed in the syringe with a stainless steel needle in the spinning device, at a temperature of 25 ° C, a relative humidity of 55%, an applied voltage of 15 kV, and a stainless steel needle Model 5#, the feeding speed of the syringe is 2.5mL / h, and the distance between the stainless steel needle and the drum of the fiber collection device is 20cm, electrospinning is carried out, and the precursor of titanium polyacetylacetonate is obtained by drawing and collecting through the drum body fibers.

[0083] (iii) heat treatment

[0...

Embodiment 3

[0086] A kind of preparation method of titanium oxide continuous fiber, comprises steps as follows:

[0087] (a) The method in Example 1 is adopted to prepare the polyacetylacetonate titanium precursor sol-spinning solution, and then concentrate to obtain a sol-spinning solution with a viscosity of 75Pa·s (measured at 20° C.) by evaporating the solvent under reduced pressure. in dry spinning;

[0088] (b) Dry spinning

[0089] Place the sol spinning solution prepared in step (a) in the spinneret of the spinning device, vacuum defoaming at a temperature of 30°C for 10min, at a temperature of 30°C and a relative humidity of 40%, use a cylinder of nitrogen The method is to apply a pressure of 1.8MPa to the spinning solution, extrude it in a 0.04mm niobium-tantalum alloy spinneret, and obtain continuous fibers of polyacetylacetonate-titanium precursor after drawing and collecting;

[0090] (c) Preprocessing

[0091] The precursor continuous fiber obtained in step (b) is placed ...

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Abstract

The invention relates to a method for preparing a titanium polyacetylacetonate precursor sol spinning solution, a titanium oxide continuous fiber and a titanium oxide nanofiber. According to the method, tetrabutyl titanate is used as a titanium source for synthesis of a titanium polyacetylacetonate precursor, and the precursor, an auxiliary agent and a solvent are mixed uniformly to obtain the solspinning solution; the sol spinning solution is subjected to electrospinning and dry spinning so as to obtain a precursor nanofiber and a continuous fiber respectively; and then heat treatment is carried out so as to obtain the titanium oxide nanofiber and the titanium oxide continuous fiber. The prepared titanium oxide nanofiber has a diameter of 400 to 1200 nm and a length of 2 to 6 cm; and theprepared titanium oxide continuous fiber has a diameter of 20 to 100 [mu]m, a length of more than meters and a strength of 100 MPa to 1.0 GPa. The method of the invention has the advantages of simpleprocess, low cost and capacity of avoiding the existence of impurity ions; the prepared precursor sol has good spinnability and is stable and not prone to gelation; and the prepared fibers have highstrength and good catalytic performance.

Description

technical field [0001] The invention relates to a preparation method of polyacetylacetonate-titanium precursor sol spinning solution, titanium oxide continuous fiber and nanofiber, and belongs to the technical field of functional fiber materials. Background technique [0002] Due to the rapid development of industry, exhaust gas pollution, waste pollution and waste water pollution have become serious problems facing the world. Water resources are an indispensable material basis for human life and economic development. At present, due to industrial wastewater and domestic wastewater, water pollution is becoming more and more serious, aggravating the shortage of water resources, seriously affecting human survival and restricting human development. Therefore, people urgently need to find a kind of effective method of sewage treatment. Photocatalysis has attracted great attention since Fujishima and Honda reported that titanium oxide can be used to catalyze water splitting. P...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01F9/10D01D1/02D01D5/00D01D5/04
CPCD01D1/02D01D5/003D01D5/04D01F9/10
Inventor 王新强汪林朱陆益靳晓彤张光辉许东
Owner SHANDONG UNIV
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