Prepn of photocatalytic titania fiber material

A functional material, titanium dioxide technology, applied in chemical instruments and methods, physical/chemical process catalysts, chemical/physical processes, etc., can solve the problems of low strength of titanium dioxide fiber, complicated spinning solution preparation process, and practical application limitations of fibers, etc. Achieve high strength, high porosity, easy operating conditions

Inactive Publication Date: 2006-05-17
SHANDONG UNIV
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  • Abstract
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

titanate dealkalization by molten M 2 O nTiO 2 , where M is Na, K, Rb, Cs, n=1-5, fibrous titanate crystals are obtained, and titanium dioxide fibers are obtained by acid elution and alkali removal. Although this method is simple in process, it can only obtain micron-scale lengths Titanium dioxide fiber, strictly speaking, should not be called titanium dioxide fiber, but fibrous titanium dioxide, so the actual application of the fiber is still limited
The preparation of titanium dioxide fiber by impregnation method is to obtain titanium dioxide fiber by immersing the organic silk in the titanium alkoxide solution, taking it out after absorbing enough, drying, calcining, and burning off the organic matter. Because the content of organic matter in the precursor fiber is too high, this method is adopted TiO2 fibers obtained have very low strength
The sol-gel method is used to prepare titanium dioxide fibers, using titanium alkoxide as raw material, through hydrolysis or acidolysis and polycondensation reaction, to obtain sol spinning solution, spinning and calcining to obtain titanium dioxide fibers, although this method has more advantages than previous technologies. Great progress has been made, but there are still problems such as complicated spinning solution preparation process, harsh reaction conditions, and long reaction time.

Method used

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  • Prepn of photocatalytic titania fiber material
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  • Prepn of photocatalytic titania fiber material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Embodiment 1: the preparation method of titanium dioxide short fiber adopts the following steps

[0038] 1. Synthesis of polyethylacetoacetate titanium precursor. According to the ratio of tetrabutyl titanate: distilled water: ethyl acetoacetate = 1mol: 1.5mol: 0.5mol, measure 34ml, 2.7ml, 6.4ml of the above three liquid reagents (analytical grade) respectively, and dilute them in two parts respectively. In isopropanol, dilute tetrabutyl titanate and ethyl acetoacetate in the same part of isopropanol, wherein the volume dilution factor of tetrabutyl titanate is 3 times, and at room temperature, dilute tetrabutyl titanate Mixed and stirred with ethyl acetoacetate diluent in isopropanol for 60 min to obtain mixed diluent A. Dilute the distilled water in another part of isopropanol, and the volume dilution factor is 20-30 times to obtain the mixed dilution B. Then, under the condition of stirring and 0℃~40℃, add the mixed diluent B or A dropwise into the mixed diluent A ...

Embodiment 2

[0043] Embodiment 2: the preparation method of titanium dioxide porous short fiber

[0044] As described in Example 1, the difference is that the heating program in step 4 is changed as follows: the heating rate at 25°C to 95°C is 100°C / h, and the temperature is kept at 95°C for 24 hours, and the heating rate at 95°C to 250°C is The heating rate is 200℃ / h, the heating rate is 50℃ / h at 250℃~350℃, the heating rate is 300℃ / h at 350℃~550℃, the heating rate is 50℃ / h at 550℃~650℃, and the heating rate is 50℃ / h at 650℃~700℃ The heating rate is 300°C / h, and the temperature is kept at 700°C for 1 hour, and the temperature is naturally lowered. Obtain a tensile strength of 100MPa~1.2Gpa, a diameter of 10μm~25μm, a continuous length of monofilament of 5cm~50cm, and a BET specific surface area of ​​250m 2 Titanium dioxide porous short fiber with / g, ​​pore diameter of 5nm-10nm, grain size of 10nm-30nm, crystal phase of anatase phase.

Embodiment 3

[0045] Embodiment 3: the preparation method of titanium dioxide continuous fiber

[0046] As described in Example 1, the difference is that the solution is concentrated by evaporating the solvent in step 2 so that the viscosity of the spinning solution reaches 75 Pa·s, and the spinning method in step 3 is changed to dry spinning. Move the spinning solution into the liquid material tank in the dry spinning device, vacuum defoam for 10 minutes, and apply a pressure of 2.0 MPa to the spinning solution under the condition of a temperature of 25°C and a relative humidity of 40%, so that it can be removed from a hole diameter of 0.15 The mm niobium-tantalum alloy spinning plate is sprayed out, and after drafting and drum collection, the length can be almost arbitrarily long, transparent and orderly continuous precursor long fibers. Such as figure 2 Photos shown. image 3 is its scanning electron microscope (SEM) picture.

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Abstract

The preparation process of photocatalytic titania fiber material includes the following steps: synthesizing polyacetyl ethyl acetate-titanium complex as the precursor; dissolving the synthesized polyacetyl ethyl acetate-titanium complex in tetrahydrofuran to compounding spinning liquid of viscosity 5-100 Pa.s, with the ratio between the synthesized polyacetyl ethyl acetate-titanium complex and tetrahydrofuran being 100 g to 400-800 ml; centrifugally spinning the spinning liquid of viscosity 5-100 Pa.s into short precursor fiber; dry spinning the spinning liquid of viscosity 50-100 Pa.s into continuous long precursor fiber; and final water steam activation of the precursor fiber and heat treatment and sintering. The preparation process has simple operation, easy control and low power consumption.

Description

(1) Technical field [0001] The invention relates to a preparation method of a titanium dioxide fiber which can be used as a photocatalyst or a catalyst carrier, and belongs to the field of functional fiber materials. (2) Background technology [0002] In 1972, Fujishima and Honda discovered TiO irradiated by light 2 The particles can make the redox reaction of water continue to produce hydrogen gas. Since then, many researchers have explored photocatalytic oxidation technology. After more than 30 years of research, it has occupied an important position as an advanced oxidation technology in the fields of chemical engineering and building materials. Among various semiconductor oxides used in photocatalysis, titanium dioxide has been proved to be one of the most effective photocatalysts. As a green and environment-friendly photocatalytic purifying agent, titanium dioxide has good chemical stability, wear resistance, low cost, safety and non-toxicity, etc., which makes it sho...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J21/06B01J35/06
Inventor 包南张锋张成禄孙剑马东
Owner SHANDONG UNIV
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