Method for preparing nanometer titanium dioxide fiber composite material

By combining nano-titanium dioxide onto fibers using a low-temperature preparation method, the problems of particle agglomeration, easy detachment, and low photocatalytic activity in existing technologies are solved. This achieves a strong bond and excellent performance between nano-titanium dioxide and fibers, making it suitable for applications such as self-cleaning, sun protection, and deodorization.

CN117071282BActive Publication Date: 2026-03-27NINGBO NANOJP NEW MATERIAL TECH CO LTD
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2023-10-01
Publication Date
2026-03-27

AI Technical Summary

Technical Problem

Existing methods for loading nano-titanium dioxide suffer from problems such as particle agglomeration, easy detachment, reduced photocatalytic activity, limited substrate materials, and high cost, making it difficult to apply on a large scale to various materials.

Method used

A low-temperature preparation method is used to prepare peroxytitanic acid solution by mixing hydrated titanic acid with hydrogen peroxide. This solution is then added to the fiber and heat-treated under sealed conditions to obtain crystalline nano-titanium dioxide particles with a particle size of less than 10 nanometers, which are firmly bonded to the fiber.

Benefits of technology

It achieves a strong bond between nano-titanium dioxide and fibers at low temperatures, maintaining the fiber structure and color without shedding. It exhibits excellent photocatalytic activity and self-cleaning ability, making it suitable for a variety of fiber materials.

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Abstract

The application discloses a preparation method of a nano-titanium dioxide fiber composite material for improving the effect and performance of nano-titanium dioxide loaded fiber, and comprises the following steps: preparing hydrated titanic acid; mixing and stirring the prepared hydrated titanic acid with a hydrogen peroxide aqueous solution to form a peroxotitanic acid aqueous solution; adding the obtained peroxotitanic acid solution into fiber to form a peroxotitanic acid fiber composite material; partially drying the obtained peroxotitanic acid fiber composite material to obtain a peroxotitanic acid fiber composite material with a water content of 30-80%; and heat-treating the peroxotitanic acid fiber composite material with a water content of 30-80% under a sealed condition to obtain a nano-titanium dioxide fiber composite material.
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Description

TECHNICAL FIELD

[0001] The present application relates to a preparation method of a nanometer titanium dioxide fiber composite material. BACKGROUND

[0002] Nanometer titanium dioxide refers to titanium dioxide with a particle size of less than 100 nanometers, which has small particle size, high specific surface area, excellent photocatalytic activity, stable chemical and thermal properties, super-hydrophilicity and other special effects, and has irreplaceable application advantages in air treatment, sterilization and disinfection, self-cleaning materials, sunscreen and skin care products, etc. Loading nanometer titanium dioxide on the surface of different substrate materials is the premise of realizing the application of nanometer titanium dioxide in photocatalytic decomposition of pollutants, self-cleaning, and anti-ultraviolet fields. After loading nanometer titanium dioxide, the use efficiency of nanometer titanium dioxide can be improved, the shedding can be reduced, and the recycling can be increased.

[0003] Currently, there are mainly two ways to load nanometer titanium dioxide: (1) direct spraying method: this method is relatively simple to operate, mainly by spraying a nanometer titanium dioxide water solution on the surface of the substrate material and drying to obtain, in order to make the loading firm, a binder is usually added during the preparation of the nanometer titanium dioxide water solution; (2) spraying and sintering method: this method is to spray nanometer titanium dioxide or nanometer titanium dioxide precursor on the surface of the substrate material, dry and then sinter at high temperature to obtain.

[0004] The above-mentioned main loading methods and loaded substrate materials all have problems, mainly as follows: (1) the primary particle size of nanometer titanium dioxide particles obtained by direct spraying method is usually greater than 50 nanometers, which is a micron-sized particle agglomerate, and is easy to fall off after spraying; (2) a binder needs to be added, after adding the binder, the photocatalytic activity of nanometer titanium dioxide is greatly reduced, and the substrate material is yellow, which affects the use and appearance; (3) the spraying and sintering method needs to go through a high-temperature sintering process, which can only be operated on the surface of materials such as metals and ceramics that can withstand high temperatures, the surface area of these materials is not large, so the loading content of titanium dioxide is not high, and the particle size of nanometer titanium dioxide after high-temperature sintering becomes larger, further reducing the application performance; (4) nickel mesh, aluminum mesh and other main loading materials cannot form a small pore structure, resulting in low contact efficiency of air and the surface of the filter mesh, in addition, the cost of these substrate materials is also relatively high, which is difficult to promote on a large scale.

[0005] In order to overcome the above-mentioned deficiencies, it is urgent to develop new preparation methods and technologies to improve the effect and performance of nanometer titanium dioxide loaded fiber. SUMMARY

[0006] In view of at least one of the above problems, the application innovatively develops a preparation technology of nano-titanium dioxide fiber composite material, which can realize crystallization of nano-titanium dioxide at low temperature, obtain nano-titanium dioxide particles with a particle size of less than 10 nanometers, and improve the catalytic activity of nano-titanium dioxide. Meanwhile, the application is carried out under the condition of containing a small amount of water vapor and at a relatively low temperature, so that the fiber structure and morphology will not change.

[0007] The application adopts the following technical scheme:

[0008] A preparation method of a nano-titanium dioxide fiber composite material, comprising the following steps:

[0009] A first step of preparing hydrated titanic acid;

[0010] A second step of mixing and stirring the prepared hydrated titanic acid with a hydrogen peroxide aqueous solution to form a peroxotitanic acid aqueous solution;

[0011] A third step of adding the obtained peroxotitanic acid solution to fibers to form a peroxotitanic acid fiber composite material;

[0012] A fourth step of partially drying the obtained peroxotitanic acid fiber composite material to obtain a peroxotitanic acid fiber composite material with a water content of 30% to 80%;

[0013] A fifth step of heat-treating the peroxotitanic acid fiber composite material with a water content of 30% to 80% under a sealed condition to obtain a nano-titanium dioxide fiber composite material.

[0014] As a preferred aspect, the primary particle size of the nano-titanium dioxide particles in the nano-titanium dioxide fiber composite material is less than 10 nanometers.

[0015] As a preferred aspect, the primary particle size of the nano-titanium dioxide particles in the nano-titanium dioxide fiber composite material is less than 5 nanometers.

[0016] As a preferred aspect, the nano-titanium dioxide in the nano-titanium dioxide fiber composite material is a crystalline nanoparticle; and the crystal phase of the crystalline nanoparticle is one of anatase phase and rutile phase or a combination thereof.

[0017] As a preferred aspect, the hydrated titanic acid is obtained through a hydrolysis, separation and purification process of a titanium source; and the titanium source is selected from one or a combination of the following: titanium sulfate, titanyl sulfate, titanium tetrachloride, titanium isopropoxide and tetrabutyl titanate.

[0018] As a preferred aspect, the mass fraction of peroxotitanic acid in the peroxotitanic acid aqueous solution is 0.001% to 5%.

[0019] As a preferred aspect, the mass fraction of peroxotitanium acid in the aqueous peroxotitanium acid solution is 0.005% to 2%.

[0020] As a preferred aspect, the method further comprises the step of adding a small amount of metal ions to the formed aqueous peroxotitanium acid solution.

[0021] The metal ions are selected from one or a combination of copper ions, silver ions, and zinc ions; and the molar ratio of the small amount of metal ions to the peroxotitanium acid in the aqueous solution is 1:1000 to 1:50.

[0022] As a preferred aspect, the obtained peroxotitanium acid fiber composite is partially dried to obtain a peroxotitanium acid fiber composite with a water content of 35% to 50%.

[0023] As a preferred aspect, in the process of adding the obtained peroxotitanium acid solution to the fibers to form a peroxotitanium acid fiber composite, the mass ratio of the peroxotitanium acid solution to the fibers is 1:1 to 10:1.

[0024] As a preferred aspect, the fibers are selected from one or a combination of artificial fibers and plant fibers.

[0025] The artificial fibers are selected from one or a combination of polyester fibers, polyamide fibers, polyacrylonitrile fibers, polyolefin fibers, polyvinyl acetal fibers, polyvinyl chloride fibers, and carbon fibers.

[0026] The plant fibers are selected from one or a combination of cotton fibers, wood fibers, flax fibers, silk, and wool.

[0027] As a preferred aspect, the sealing condition is to place the peroxotitanium acid fiber composite with a water content of 30% to 80% in a fixed-volume container and seal it; the fixed-volume container does not change in volume under heating.

[0028] As a preferred aspect, the heat treatment is selected from one of microwave heating, electric heating, and water vapor heating; the temperature of the heat treatment is 100°C to 200°C; and the time of the heat treatment is 2 hours to 24 hours.

[0029] The present application provides a method for preparing a nanometer titanium dioxide fiber composite, which has the following technical and application advantages.

[0030] (1) Low-temperature preparation: This technical method is suitable for different fiber materials such as natural fibers and synthetic fibers, without damaging the fiber structure and changing the color of the fibers.

[0031] (2) Nanometer scale: the titanium dioxide particles obtained by the technical method are of nanometer scale, the particle size is less than 10 nanometers, the crystallinity is good, and the titanium dioxide has excellent photocatalytic activity, self-cleaning ability and ultraviolet absorption ability.

[0032] (3) Firm combination: in the titanium dioxide fiber composite material obtained by the technical method, the nanometer titanium dioxide particles are firmly combined with the fibers, and no nanometer titanium dioxide particles are found to fall off after various treatments such as soaking, immersion in water, ultrasonic treatment, scraping and washing.

[0033] (5) Excellent performance and broad application prospect: the nanometer titanium dioxide fiber composite material has excellent photocatalytic self-cleaning effect and can be woven into various self-cleaning, sunscreen, deodorizing and antibacterial filter screens, clothing and household products, etc. BRIEF DESCRIPTION OF DRAWINGS

[0034] In order to more clearly illustrate the technical solutions in the embodiments of the present application or the prior art, the drawings needed in the embodiment or prior art description will be briefly introduced below. Obviously, the drawings in the following description are only some embodiments of the present application, and other drawings can be obtained by those skilled in the art without creative labor on the basis of these drawings.

[0035] Figure 1 The product obtained in Example 1 is adhered to the sample stage of the scanning electron microscope with conductive glue, and the scanning electron microscope graph obtained by observing at low magnification is obtained;

[0036] Figure 2 The product obtained in Example 1 is adhered to the sample stage of the scanning electron microscope with conductive glue, and the scanning electron microscope graph obtained by observing at medium magnification is obtained;

[0037] Figure 3 The product obtained in Example 1 is adhered to the sample stage of the scanning electron microscope with conductive glue, and the scanning electron microscope graph obtained by observing at high magnification is obtained;

[0038] Figure 4 The product obtained in Example 1 is adhered to the sample stage of the scanning electron microscope with conductive glue, and the distribution graph of titanium element in the fiber obtained by EDS energy spectrum test is obtained.From the graph, it can be seen that the nanometer titanium dioxide in the present embodiment is uniformly combined with the fiber. Figure 4 DETAILED DESCRIPTION

[0039] To enable those skilled in the art to better understand the technical solutions of this invention, the technical solutions of the embodiments of this invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of this invention, and not all embodiments. Based on the embodiments of this invention, all other embodiments obtained by those skilled in the art without creative effort should fall within the scope of protection of this invention.

[0040] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention pertains. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. The term "and / or" as used herein includes any and all combinations of one or more of the associated listed items.

[0041] Example 1

[0042] First, 10 g of titanium tetrachloride liquid was slowly added dropwise to 50 mL of water, stirring to form a solution. The solution was diluted with water to 100 mL, and then 1.0 mol / L ammonia solution was slowly added dropwise while stirring until the final solution reached a neutral pH, yielding a hydrated titanic acid precipitate. The hydrated titanic acid precipitate was separated and washed three times to remove ammonium and chloride ions, and then dried to obtain hydrated titanic acid. Next, the hydrated titanic acid was dispersed in 450 mL of water, and 50 mL of 30% hydrogen peroxide was added while stirring. After stirring at room temperature for 1 hour, 0.1 g of copper chloride was added, and stirring continued for 0.5 hours to obtain a light yellow, transparent peroxytitanic acid aqueous solution. Third, 200 g of cotton fibers were added to the light yellow, transparent peroxytitanic acid aqueous solution, and squeezed to ensure uniform and thorough contact between the cotton and the solution. The cotton was then removed and placed in an oven to dry until the total weight of the cotton was 300 g. Finally, the cotton was placed in a reaction vessel and sealed, and then kept at a constant temperature of 150 degrees Celsius in an electric heating oven for 6 hours to obtain the nano-titanium dioxide fiber composite material product.

[0043] The nano-titanium dioxide fibers obtained in Example 1 are still white. A small amount of the nano-titanium dioxide fibers obtained in Example 1 are adhered to the sample stage of a scanning electron microscope using conductive adhesive for observing the morphology of the sample under the scanning electron microscope. Figure 1 As shown. From Figure 1 It can be seen that the morphology and structure of the fibers remain intact, without damage or alteration, and still possess textile flexibility. They can be woven into various self-cleaning, sun-protective, deodorizing, and antibacterial filters, clothing, and household goods. Further observation using a magnified scanning electron microscope, such as... Figure 2 As shown. From Figure 2It can be seen that the titanium dioxide fiber composite material obtained in this embodiment 1 has nano titanium dioxide material uniformly distributed on the surface of the fiber, and the nano titanium dioxide particles are firmly combined with the fiber and do not fall off; after various treatments such as soaking, immersion in water, ultrasonic treatment, scraping and washing, no nano titanium dioxide particles are found to fall off. Further observation of the magnification scanning electron microscope shows that the titanium dioxide particles on the surface of the titanium dioxide fiber composite material obtained in this embodiment 1 are of nanometer size, the particle size is less than 10 nanometers, and the average particle size is 5-8 nanometers. Figure 3 As shown in Figure 3 It can be seen that the titanium dioxide fiber composite material obtained in this embodiment 1 has nano titanium dioxide material uniformly distributed on the surface of the fiber, and the nano titanium dioxide particles are firmly combined with the fiber and do not fall off; after various treatments such as soaking, immersion in water, ultrasonic treatment, scraping and washing, no nano titanium dioxide particles are found to fall off. Further observation of the magnification scanning electron microscope shows that the titanium dioxide particles on the surface of the titanium dioxide fiber composite material obtained in this embodiment 1 are of nanometer size, the particle size is less than 10 nanometers, and the average particle size is 5-8 nanometers. Figure 4 As shown in Figure 4 It can be seen that the titanium dioxide fiber composite material obtained in this embodiment 1 has nano titanium dioxide material uniformly distributed on the surface of the fiber, and the nano titanium dioxide particles are firmly combined with the fiber and do not fall off; after various treatments such as soaking, immersion in water, ultrasonic treatment, scraping and washing, no nano titanium dioxide particles are found to fall off. Further observation of the magnification scanning electron microscope shows that the titanium dioxide particles on the surface of the titanium dioxide fiber composite material obtained in this embodiment 1 are of nanometer size, the particle size is less than 10 nanometers, and the average particle size is 5-8 nanometers.

[0044] In summary, the advantages of the present application are as follows: (1) low temperature preparation: the technical method is suitable for different fiber materials such as natural fibers and synthetic fibers, without damaging the fiber structure and changing the color of the fiber. (2) nanometer size: the titanium dioxide particles obtained by the technical method are of nanometer size, the particle size is less than 10 nanometers, the crystallinity is good, and the material has excellent photocatalytic activity, self-cleaning ability and ultraviolet absorption ability. (3) firm combination: the nano titanium dioxide particles in the titanium dioxide fiber composite material obtained by the technical method are firmly combined with the fiber, and no nano titanium dioxide particles are found to fall off after various treatments such as soaking, immersion in water, ultrasonic treatment, scraping and washing. (5) excellent performance and wide application prospect: the obtained nano titanium dioxide fiber composite material has excellent photocatalytic self-cleaning effect, and can be woven into various self-cleaning, sunscreen, deodorizing and antibacterial filtering nets, clothing and home supplies, etc.

[0045] Embodiment 2

[0046] First, 2 grams of isopropyl alcohol liquid is slowly added to 50 milliliters of water, and a hydrated titanic acid precipitate is obtained by hydrolysis under stirring; the hydrated titanic acid precipitate is separated, washed once, and dried to obtain hydrated titanic acid. Second, the hydrated titanic acid is dispersed in 490 milliliters of water, 10 milliliters of 30% hydrogen peroxide solution is added under stirring, and after stirring for 1 hour at room temperature, 0.01 grams of silver acetate is added, and stirring is continued for 0.5 hours to obtain a light yellow transparent peroxotitanic acid aqueous solution. Third, 150 grams of silk fibers are added to the light yellow transparent peroxotitanic acid aqueous solution, and the silk fibers are extruded to make them fully contact with the solution; then the silk fibers are taken out and placed in an oven for drying until the total weight of the silk fibers is 270 grams. Finally, the silk fibers are placed in a reaction kettle and sealed, and then treated at 105 degrees Celsius in an electric heating oven for 24 hours to obtain a nanometer titanium dioxide fiber composite product. The product of this example has basically the same performance as the product of Example 1.

[0047] Example 3

[0048] First, 20 grams of titanium sulfate liquid is slowly added to 100 milliliters of water to form a solution; the solution is diluted with water to 200 milliliters, and then 1.0 mole per liter of sodium hydroxide solution is slowly added under stirring until the pH value of the final solution is neutral to obtain a hydrated titanic acid precipitate; the hydrated titanic acid precipitate is separated, washed five times to remove sodium ions and sulfate ions, and then dried to obtain hydrated titanic acid. Second, the hydrated titanic acid is dispersed in 400 milliliters of water, and 100 milliliters of 30% hydrogen peroxide solution is added under stirring, and after stirring for 2 hours at room temperature, a light yellow transparent peroxotitanic acid aqueous solution is obtained. Third, 500 grams of polyester fibers are added to the light yellow transparent peroxotitanic acid aqueous solution, and the polyester fibers are extruded to make them fully contact with the solution; then the polyester fibers are taken out and placed in an oven for drying until the total weight of the polyester fibers is 650 grams. Finally, the polyester fibers are placed in a reaction kettle and sealed, and then treated at 200 degrees Celsius in an electric heating oven for 2 hours to obtain a nanometer titanium dioxide fiber composite product. The product of this example has basically the same performance as the product of Example 1.

[0049] Example 4

[0050] First, 20 grams of titanyl sulfate liquid was slowly added into 200 milliliters of water to form a solution; the solution was diluted to 400 milliliters with water, and 1.0 mole per liter of potassium hydroxide solution was slowly added dropwise under stirring until the pH of the final solution was neutral, to obtain a hydrated titanic acid precipitate; the hydrated titanic acid precipitate was separated, washed three times to remove potassium ions and sulfate ions, and then dried to obtain hydrated titanic acid. Second, the hydrated titanic acid was dispersed in 420 milliliters of water, and 80 milliliters of 30% hydrogen peroxide solution was added under stirring; after stirring at room temperature for 1.5 hours, a light yellow transparent peroxotitanic acid aqueous solution was obtained. Third, 200 grams of carbon fiber was added into the light yellow transparent peroxotitanic acid aqueous solution, and the carbon fiber was squeezed to make it fully contact with the solution; then the carbon fiber was taken out and dried in an oven until the total weight of the carbon fiber was 280 grams. Finally, the carbon fiber was sealed in a reaction kettle and subjected to microwave heating at 180 degrees Celsius for 4 hours to obtain a nanometer titanium dioxide fiber composite product. The product of this example has basically the same performance as the product of Example 1.

[0051] Example 5

[0052] First, 15 grams of isopropyl alcohol liquid was slowly added into 200 milliliters of water to form a solution; the solution was diluted to 400 milliliters with water, and 1.0 mole per liter of potassium hydroxide solution was slowly added dropwise under stirring until the pH of the final solution was neutral, to obtain a hydrated titanic acid precipitate; the hydrated titanic acid precipitate was separated, washed two times, and then dried to obtain hydrated titanic acid. Second, the hydrated titanic acid was dispersed in 400 milliliters of water, and 100 milliliters of 30% hydrogen peroxide solution was added under stirring; after stirring at room temperature for 1 hour, 0.2 grams of zinc acetate was added, and then the stirring was continued for 1 hour to obtain a light yellow transparent peroxotitanic acid aqueous solution. Third, 400 grams of polyamide fiber was added into the light yellow transparent peroxotitanic acid aqueous solution, and the polyamide fiber was squeezed to make it fully contact with the solution; then the polyamide fiber was taken out and dried in an oven until the total weight of the polyamide fiber was 650 grams. Finally, the polyamide fiber was sealed in a reaction kettle and subjected to constant temperature treatment in an electric heating oven at 130 degrees Celsius for 16 hours to obtain a nanometer titanium dioxide fiber composite product. The product of this example has basically the same performance as the product of Example 1.

[0053] Example 6

[0054] First, 15 grams of titanium tetrachloride liquid was slowly added to 70 milliliters of water, and stirred to form a solution; the above solution was diluted with water to 200 milliliters, and then 1.0 mole per liter of ammonia solution was slowly added dropwise under stirring until the final solution had a neutral pH value, to obtain a hydrated titanic acid precipitate; the above hydrated titanic acid precipitate was separated, washed three times to remove ammonium ions and chloride ions, and then dried to obtain hydrated titanic acid. Second, the above hydrated titanic acid was dispersed in 420 milliliters of water, and 80 milliliters of 30% mass fraction hydrogen peroxide was added under stirring, and stirred at room temperature for 3 hours to obtain a light yellow transparent peroxotitanic acid aqueous solution. Third, 50 grams of cotton fibers were added to the above light yellow transparent peroxotitanic acid aqueous solution, and squeezed to make the cotton fibers fully contact with the solution; then the cotton fibers were taken out and placed in an oven for drying until the total weight of the cotton fibers was 90 grams. Finally, the above cotton fibers were placed in a reaction kettle and sealed, and then treated in a 160-degree Celsius electric heating oven for 5 hours to obtain a nanometer titanium dioxide fiber composite material product.

[0055] Comparative Example 1

[0056] First, 10 grams of titanium tetrachloride liquid was slowly added to 50 milliliters of water, and stirred to form a solution, and then the above solution was diluted with water to 500 milliliters. Second, 200 grams of cotton fibers were added to the above aqueous solution, and squeezed to make the cotton fibers fully contact with the solution; then the cotton fibers were taken out and placed in an oven for drying until the total weight of the cotton fibers was 300 grams. Finally, the above cotton fibers were placed in a reaction kettle and sealed, and then treated in a 150-degree Celsius electric heating oven for 6 hours to obtain a comparative product. In this comparative example, the system was extremely acidic, the color of the fibers turned yellow, and the fibers were severely damaged; the nanometer titanium dioxide particles in the product were large in size, and did not firmly contact with the fibers, and were easily detached; the nanometer titanium dioxide was in an anatase phase, and had extremely low photocatalytic activity.

[0057] Comparative Example 2

[0058] First, 10 grams of titanium tetrachloride liquid is slowly added into 50 milliliters of water, and stirred to form a solution; the above solution is diluted to 100 milliliters with water, and then 1.0 mole per liter of ammonia solution is slowly added dropwise under stirring until the final solution has a neutral pH value, to obtain a hydrated titanic acid precipitate; the above hydrated titanic acid precipitate is separated, washed three times to remove ammonium ions and chloride ions, and then dried to obtain hydrated titanic acid. Second, the above hydrated titanic acid is dispersed in 450 milliliters of water, and 50 milliliters of 30% mass fraction hydrogen peroxide is added under stirring, and stirred at room temperature for 1 hour, and then 0.1 grams of copper chloride is added, and then continues to stir for 0.5 hours to obtain a light yellow transparent peroxotitanic acid aqueous solution. Third, 200 grams of cotton fibers are added into the above light yellow transparent peroxotitanic acid aqueous solution, and squeezed to make the cotton fibers fully contact with the solution, and then placed in a reaction kettle and sealed, and then heated in a 150 degree Celsius electric heating oven for constant temperature treatment for 6 hours to obtain a comparative product. In the comparative example, the titanium dioxide cannot form a good composite material with the fibers, mainly because the nano-titanium dioxide particles are generated in the solution by "nucleation growth", and cannot be effectively combined with the fibers. In addition, the nano-titanium dioxide particles obtained by this method have a size greater than 20 nanometers, and have very low photocatalytic activity.

[0059] Any numerical values recited herein include all values from the lower value to the upper value in increments of one unit, unless the context clearly dictates otherwise. As an example, if a numerical value is recited as from 1 to 90, preferably from 20 to 80, and more preferably from 30 to 70, it is intended that values such as 15 to 85, 22 to 68, 43 to 51, and 30 to 32, etc. are expressly enumerated in this specification. For values which are less than one, one unit is considered to be 0.0001, 0.001, 0.01, 0.1, etc. These are only examples of what is specifically enumerated herein, and are intended to be continuous ranges merely for convenience. Any number obtained by adding or subtracting these amount from the upper threshold of these ranges is also intended to be within this application in a similar manner. Any numerical range recited herein constitutes both a numerical range and individual possibilities of the numbers within that range.

[0060] Unless otherwise stated, all ranges include both endpoints and all numbers between the endpoints. "Approximately" or "about" applied to a range of values should be construed to cover the range explicitly indicated and the individual possibilities of the numbers within that range. Thus, "about 20 to 30" is intended to cover "about 20 to about 30", including at least the endpoints.

[0061] It is to be understood that the above description is intended to be illustrative, and not restrictive. Many embodiments and many applications other than the examples provided would be apparent upon reading the above description. The scope of the teachings should, therefore, be determined not with reference to the above description, but should instead be determined with reference to the appended claims, along with the full scope of equivalents to which such claims are entitled. The disclosures of all articles and references, including patent applications and publications, are incorporated by reference for all purposes. The omission in the following claims of any aspect of subject matter that is disclosed herein is not a disclaimer of such subject matter, nor should it be regarded that the inventors did not consider such subject matter to be part of the disclosed inventive subject matter.

Claims

1. A method for preparing a nanometer titanium dioxide fiber composite material, characterized in that, The method comprises the following steps: preparing hydrated titanic acid; mixing the prepared hydrated titanic acid with aqueous hydrogen peroxide solution to form aqueous peroxotitanic acid solution; adding the obtained peroxotitanic acid solution to fibers to form peroxotitanic acid fiber composite material; partially drying the obtained peroxotitanic acid fiber composite material to obtain peroxotitanic acid fiber composite material with water content of 30% to 80%; heat-treating the peroxotitanic acid fiber composite material with water content of 30% to 80% under sealed condition to obtain nanometer titanium dioxide fiber composite material.

2. The method for preparing a nano-titanium dioxide fiber composite material as described in claim 1, characterized in that: The primary particle size of the nanometer titanium dioxide particles in the nanometer titanium dioxide fiber composite material is less than 10 nanometers.

3. The method for preparing a nano-titanium dioxide fiber composite material as described in claim 1, characterized in that: The primary particle size of the nanometer titanium dioxide particles in the nanometer titanium dioxide fiber composite material is less than 5 nanometers.

4. The method for preparing a nano-titanium dioxide fiber composite material as described in claim 1, characterized in that: The nanometer titanium dioxide in the nanometer titanium dioxide fiber composite material is crystalline nanoparticles; the crystal phase of the crystalline nanoparticles is one of anatase phase and rutile phase or a combination thereof.

5. The method for preparing a nano-titanium dioxide fiber composite material as described in claim 1, characterized in that: The hydrated titanic acid is obtained through hydrolysis, separation and purification of a titanium source; the titanium source is selected from one or a combination of titanium sulfate, titanyl sulfate, titanium tetrachloride, titanium isopropoxide and tetrabutyl titanate.

6. The method of claim 1, wherein the nanotitania fiber composite is prepared by the steps of: a) providing a nanotitania fiber; b) providing a polymer; c) mixing the nanotitania fiber and the polymer; and d) heating the mixture to form the nanotitania fiber composite. The mass fraction of peroxotitanic acid in the aqueous peroxotitanic acid solution is 0.001% to 5%.

7. The method for preparing a nano-titanium dioxide fiber composite material as described in claim 1, characterized in that: The mass fraction of peroxotitanic acid in the aqueous peroxotitanic acid solution is 0.005% to 2%.

8. The method for preparing a nano-titanium dioxide fiber composite material as described in claim 1, characterized in that, The method further comprises the step of adding a small amount of metal ions to the formed aqueous peroxotitanic acid solution; The metal ions are selected from one or a combination of copper ions, silver ions and zinc ions; the molar ratio of the small amount of metal ions to peroxotitanic acid in the aqueous solution is 1:1000 to 1:

50.

9. The method for preparing a nano-titanium dioxide fiber composite material as described in claim 1, characterized in that: The obtained peroxotitanic acid fiber composite material is partially dried to obtain peroxotitanic acid fiber composite material with water content of 35% to 50%; In the process of adding the obtained peroxotitanic acid solution to fibers to form peroxotitanic acid fiber composite material, the mass ratio of peroxotitanic acid solution to fibers is 1:1 to 10:

1.

10. The method for preparing a nano-titanium dioxide fiber composite material as described in claim 1, characterized in that: The fibers are selected from one or a combination of artificial fibers and plant fibers; The artificial fibers are selected from one or a combination of polyester fibers, polyamide fibers, polyacrylonitrile fibers, polyolefin fibers, polyvinyl acetal fibers, polyvinyl chloride fibers and carbon fibers; The plant fibers are selected from one or a combination of cotton fibers, wood fibers and flax fibers.

11. The method for preparing a nano-titanium dioxide fiber composite material as described in claim 1, characterized in that: The sealed condition is to place the peroxotitanic acid fiber composite material with water content of 30% to 80% into a fixed-volume container for sealing; the fixed-volume container does not change in volume under heating.

12. The method for preparing a nano-titanium dioxide fiber composite material as described in claim 1, characterized in that: The heat-treatment mode is selected from one of microwave heating, electric heating and water vapor heating; the heat-treatment temperature is 100°C to 200°C; the heat-treatment time is 2 hours to 24 hours.

Citation Information

Patent Citations

  • Method for preparing extrafine anatase titanium dioxide nano rods

    CN101559979A

  • Method for modifying nanometer titanium dioxide polyester fiber with high photocatalytic activity

    CN102912620A