CN111153433A - Preparation method of composite light-colored conductive titanium dioxide powder - Google Patents
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Abstract
本发明属于化工技术领域，公开了一种复合型浅色导电二氧化钛粉体的制备方法，包括以下步骤：将锡盐、锑盐添加到双氧水溶液中，并通过滴加盐酸溶液使各组分充分溶解，得混合溶液A；其中，混合溶液A中锑盐和锡盐的摩尔比为1：50～100；将二氧化钛粉体分散于浓硫酸和过氧化氢的混合溶液中在常温下进行羟基化处理并抽滤洗涤。本发明通过对二氧化钛进行羟基化处理，增加了其表面活性，提高了与导电层的结合；另外通过添加双氧水，进一步提高了二者的结合能力，且提高了锑元素的掺杂价态，有利于提高导电层的导电性能；因此产物的包覆及导电效果较好且适用于各种形貌二氧化钛的导电包覆。
The invention belongs to the technical field of chemical industry, and discloses a preparation method of composite light-colored conductive titanium dioxide powder, comprising the following steps: adding tin salt and antimony salt into a hydrogen peroxide solution, and adding hydrochloric acid solution dropwise to make each component fully Dissolving to obtain mixed solution A; wherein, the molar ratio of antimony salt and tin salt in mixed solution A is 1:50-100; the titanium dioxide powder is dispersed in a mixed solution of concentrated sulfuric acid and hydrogen peroxide to carry out hydroxylation at room temperature Work up and wash with suction. In the present invention, the surface activity of titanium dioxide is increased by hydroxylation treatment, and the combination with the conductive layer is improved; in addition, the combination ability of the two is further improved by adding hydrogen peroxide, and the doping valence state of antimony element is improved. It is beneficial to improve the conductive performance of the conductive layer; therefore, the product has better coating and conductive effects and is suitable for conductive coating of titanium dioxide with various shapes.
Description
Technical Field
The invention belongs to the technical field of chemical industry, and particularly relates to a preparation method of composite light-colored conductive titanium dioxide powder.
Background
Commonly used conductive powders can be divided into several categories: metals, metal oxides, carbon-based, intrinsically conductive polymers. However, some of the conductive fillers in many reports present dark black, and some of the conductive fillers have complex preparation process and expensive production cost, and cannot simultaneously meet the requirements of light color, good conductivity and low production cost. As the conductive filler with a single component cannot meet the requirements of light color and high conductivity at the same time, the composite light-colored conductive filler with a core-shell structure is produced. Therefore, the production cost can be greatly reduced, and the light color of the core layer and the shell layer are conductive, so that the method has good industrial application value.
Antimony doped tin dioxide (ATO) is an n-type doped semiconductor, has good conductivity, weather resistance, chemical stability and thermal stability, is low in production cost, is not limited by weather and external environment when being used, has more advantages compared with other conductive materials, and is therefore widely used for industrial production of conductive and antistatic materials. The antimony element has two doping valence states of pentavalent and trivalent, and a compensation effect can occur when the antimony element is doped together with the trivalent element, so that the conductivity of the material is reduced, and therefore, the higher the doping proportion of the pentavalent element is, the better the conductivity is.
TiO2Is an extinction material with excellent performance, and also has the characteristics of no toxicity, good covering property and stable physicochemical property. Due to TiO2The size of the particles is generally smaller than the wavelength of the incident light, so that when light is transmitted to the TiO in the form of electromagnetic waves2During the process, the electrons in the particles will vibrate along with the propagation frequency of the light quantum to become a secondary propagation source, thereby continuously scattering light rays to all the surrounding directions to present a white appearance, and the method is the selection of the best inner core for preparing the composite light-colored conductive powder. Generally speaking, TiO2The surface has more active groups, but the active groups are gradually converted into stable lattice oxygen under high temperature. This change weakens the TiO2Surface-active to TiO of2The surface deposition of (2) is very disadvantageous.
The research of the literature finds that Chinese patent No. CN104630898A, which is named as a preparation method of conductive titanium dioxide whiskers, prepares the light-colored conductive titanium dioxide whiskers with excellent performance and uniform appearance by using the traditional liquid phase codeposition method. The patent number CN 102583524A is named as a preparation method of conductive titanium dioxide powder, and the method prepares conductive titanium dioxide by synthesizing titanium dioxide with different morphologies by a hydrothermal method and then utilizing a traditional liquid-phase codeposition method. The preparation method is simple and easy to operate, so that the production cost is low. However, the extensive production method often cannot regulate and control the conductivity of the conductive component, thereby being not beneficial to improving the conductivity of the product. Patent No. CN 07903664A, entitled a method for preparing inorganic light-colored conductive titanium dioxide powder, which prepares a coating agent with different charges and a titanium dioxide carrier to combine the coating agent and the titanium dioxide carrier in an electrostatic attraction manner, thus obtaining conductive titanium dioxide with low resistivity and light color. However, these methods do not consider the surface properties of the titania carrier and the doping valence of antimony in the ATO, so the conductivity of the material needs to be improved. Patent No. CN105271389A, entitled a method for preparing conductive titanium dioxide powder, which forms a transition layer on the surface of a titanium dioxide carrier by adding a zirconium salt solution, enhances the binding capacity of a coating agent and the carrier, but does not regulate and control the doping valence state of antimony. The patent number CN106564936A, entitled titanium dioxide conductive powder preparation method, the method uses the movement of medium ball to replace the titration method to add cladding agent, uses niobium element to replace part of antimony element to complete doping, and adds reducing agent to reduce compensation effect. However, the method has too many influencing factors in each step, and the prepared conductive titanium dioxide has poor performance stability.
Disclosure of Invention
The invention aims to provide a preparation method of composite light-colored conductive titanium dioxide powder, which has the advantages of excellent whiteness and conductivity, simple preparation process and low cost, can improve the gloss of a base material, is used for preparing light-colored conductive materials, and has wide application prospects in the fields of fibers, coatings, papermaking and other functional composite materials.
The technique and method adopted by the present invention to solve the above problems are as follows:
a preparation method of composite light-colored conductive titanium dioxide powder comprises the following steps:
s1, adding tin salt and antimony salt into the hydrogen peroxide solution, and dropwise adding a hydrochloric acid solution to fully dissolve the components to obtain a mixed solution A; wherein the molar ratio of the antimony salt to the tin salt in the mixed solution A is 1: 50-100 parts;
s2, dispersing titanium dioxide powder in a mixed solution of concentrated sulfuric acid and hydrogen peroxide to carry out hydroxylation treatment at normal temperature, and carrying out suction filtration and washing; wherein the volume ratio of the concentrated sulfuric acid to the 30% hydrogen peroxide is 7: 3; the hydroxylation treatment time is 1-5 min;
s3, pulping the titanium dioxide subjected to hydroxylation treatment in water, performing ultrasonic treatment to fully disperse the titanium dioxide, then dropping the mixed solution A obtained in the step S1 into a titanium dioxide suspension, controlling the pH value by using an alkali liquor with the concentration of 1-5 mol/L in the titration process, keeping the pH value constant at 1-4, controlling the temperature at 40-80 ℃, and controlling the titration time at 40-80 min to obtain a milky suspension; wherein the solid content of the suspension is 5-25%, and the molar ratio of the tin salt to the titanium dioxide is 1: 50-100 parts;
and S4, filtering, washing and drying the suspension, grinding the suspension into fine particles, and calcining the fine particles at high temperature to obtain the composite light-colored conductive titanium dioxide powder.
Further, in the step S1, the tin salt is at least one selected from tin sulfate, tin chloride, stannous chloride and tin nitrate; the antimony salt is at least one selected from antimony sulfate, antimony chloride, antimony nitrate and antimony acetate.
Further, the concentration of hydrochloric acid in the step S1 is 10% to 20%.
Further, the concentration of hydrogen peroxide in the step S1 is 30%; the hydrogen peroxide improves the conductivity of the product and generates a large amount of hydrogen peroxide free radical ions so as to form stronger bonding force with the titanium dioxide carrier; secondly, antimony element participating in doping in the solution is oxidized, so that the lattice distortion is reduced while the aim of effective doping is fulfilled.
Further, in the step S2, the titanium dioxide has at least one of a spherical shape, a rod shape, a tubular shape and an irregular shape; the hydroxylation treatment increases the number of hydroxyl groups on the surface of the titanium dioxide carrier, so that the reaction activity and the wettability of the titanium dioxide carrier are improved, and the coating of the conducting layer is more uniform and complete.
Further, the alkaline solution in step S3 is at least one selected from aqueous solutions of ammonia, urea, sodium carbonate, potassium carbonate, sodium hydroxide, and potassium hydroxide; the ultrasonic treatment time is 10-60 min.
Further, in the step S4, the drying temperature is 50-80 ℃, and the drying time is 8-16 h; the calcination temperature is 400-800 ℃, and the calcination time is 2-5 h.
According to the invention, titanium dioxide is subjected to hydroxylation treatment, so that the surface activity of the titanium dioxide is increased, and the combination with a conductive layer is improved; in addition, the hydrogen peroxide is added, so that the bonding capacity of the two is further improved, the doping valence state of the antimony element is improved, and the conductive performance of the conductive layer is improved; therefore, the product has good coating and conductive effects and is suitable for conductive coating of titanium dioxide with various shapes.
The method has simple preparation process and simple and convenient operation, is beneficial to mass production and has larger application prospect; the volume resistivity of the composite light-colored conductive titanium dioxide powder prepared by the method can reach 2.5 omega cm at the lowest, and the whiteness index can reach 91 percent at the highest.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts;
FIG. 1 is an SEM photograph of composite light-colored conductive titanium dioxide particles of example 1 of the present invention;
FIG. 2 is an SEM image of composite light-colored conductive titanium dioxide whiskers of example 2 of the invention;
FIG. 3 is a TEM image of composite light-colored conductive titanium dioxide whiskers of example 3 of the present invention;
FIG. 4 is an EDS diagram of composite light-colored conductive titanium dioxide whiskers of example 3 of the invention.
Detailed Description
The following detailed description of the preferred embodiments of the present invention, taken in conjunction with the accompanying drawings, will make the advantages and features of the invention easier to understand by those skilled in the art, and thus will make the scope of the invention more clearly and unequivocally defined;
example 1
As shown in fig. 1, in the preparation method of the composite light-colored conductive titanium dioxide powder in the technical scheme of the invention, titanium dioxide particles are subjected to hydroxylation treatment at normal temperature by using a mixed solution of concentrated sulfuric acid and hydrogen peroxide, wherein the treatment time is 2 min; then adding 10g of pretreated titanium dioxide into 100ml of water, uniformly pulping and ultrasonically treating, dripping a mixed solution containing 5.46g of crystallized tin tetrachloride, 0.51g of antimony trichloride and 30% and 10% of hydrogen peroxide and hydrochloric acid into a titanium dioxide suspension, controlling the reaction temperature to be 60 ℃, controlling the reaction pH by using a sodium hydroxide solution with the concentration of 2mol/L to ensure that the end pH is 1, continuously curing for 1h after the dripping is finished, washing, filtering, drying a filter cake in vacuum for 8h at 80 ℃, fully drying, grinding to fine particles, and then treating at 600 ℃ for 2h to obtain the composite light-colored conductive titanium dioxide particle powder. The volume resistivity of the test powder was 5.6. omega. cm, and the whiteness index was 89%.
Example 2
As shown in fig. 2, in the preparation method of the composite light-colored conductive titanium dioxide powder in the technical scheme of the invention, the titanium dioxide whiskers are subjected to hydroxylation treatment at normal temperature by using a mixed solution of concentrated sulfuric acid and hydrogen peroxide, wherein the treatment time is 2 min; and then adding 12g of pretreated titanium dioxide whisker into 100ml of water, uniformly pulping and ultrasonically treating, dripping a mixed solution containing 5.46g of crystalline stannic chloride, 0.51g of antimony trichloride, 30% and 15% of hydrogen peroxide and hydrochloric acid into a titanium dioxide suspension, controlling the reaction temperature to be 60 ℃, controlling the reaction pH by using a sodium hydroxide solution with the concentration of 2mol/L to ensure that the end pH is 4, continuously curing for 2h after the dripping is finished, washing, filtering, drying a filter cake in vacuum for 8h at 80 ℃, fully drying, grinding to fine particles, and then treating at 800 ℃ for 2h to obtain the composite light-colored conductive titanium dioxide whisker powder. The volume resistivity of the test powder was 24.8. omega. cm, and the whiteness index was 86%.
Example 3
As shown in fig. 3-4, in the preparation method of the composite light-colored conductive titanium dioxide powder in the technical scheme of the invention, the titanium dioxide whiskers are subjected to hydroxylation treatment at normal temperature by using a mixed solution of concentrated sulfuric acid and hydrogen peroxide, wherein the treatment time is 5 min; then adding 20g of pretreated titanium dioxide whisker into 100ml of water, uniformly pulping and ultrasonically treating, dripping a mixed solution containing 10g of crystallized tin tetrachloride, 1g of antimony trichloride and 30% and 10% of hydrogen peroxide and hydrochloric acid into a titanium dioxide suspension, controlling the reaction temperature to be 60 ℃, controlling the reaction pH by using a 2mol/L sodium hydroxide solution to control the reaction pH to be 2, continuing to cure for 1h after the dripping is finished, washing and filtering, then drying a filter cake in vacuum for 8h at 80 ℃, fully drying and grinding the filter cake to fine particles, and then carrying out high-temperature treatment for 2h at 500 ℃ to obtain the composite light-colored conductive titanium dioxide whisker powder. The volume resistivity of the test powder was 7.8. omega. cm, and the whiteness index was 83%.
The above description is only for the specific embodiment of the present invention, but the protection scope of the present invention is not limited thereto, and any changes or substitutions that are not thought of by the inventive labor should be covered within the protection scope of the present invention, and therefore, the protection scope of the present invention should be subject to the protection scope defined by the claims.
Claims (7)
1. A preparation method of composite light-colored conductive titanium dioxide powder is characterized by comprising the following steps:
s1, adding tin salt and antimony salt into the hydrogen peroxide solution, and dropwise adding a hydrochloric acid solution to fully dissolve the components to obtain a mixed solution A; wherein the molar ratio of the antimony salt to the tin salt in the mixed solution A is 1: 50-100 parts;
s2, dispersing titanium dioxide powder in a mixed solution of concentrated sulfuric acid and hydrogen peroxide to carry out hydroxylation treatment at normal temperature, and carrying out suction filtration and washing; wherein the volume ratio of the concentrated sulfuric acid to the 30% hydrogen peroxide is 7: 3; the hydroxylation treatment time is 1-5 min;
s3, pulping the titanium dioxide subjected to hydroxylation treatment in water, performing ultrasonic treatment to fully disperse the titanium dioxide, then dropping the mixed solution A obtained in the step S1 into a titanium dioxide suspension, controlling the pH value by using an alkali liquor with the concentration of 1-5 mol/L in the titration process, keeping the pH value constant at 1-4, controlling the temperature at 40-80 ℃, and controlling the titration time at 40-80 min to obtain a milky suspension; wherein the solid content of the suspension is 5-25%, and the molar ratio of the tin salt to the titanium dioxide is 1: 50-100 parts;
and S4, filtering, washing and drying the suspension, grinding the suspension into fine particles, and calcining the fine particles at high temperature to obtain the composite light-colored conductive titanium dioxide powder.
2. The method for preparing composite light-colored conductive titanium dioxide powder according to claim 1, wherein the method comprises the following steps: the tin salt in the step S1 is at least one selected from tin sulfate, tin chloride, stannous chloride and tin nitrate; the antimony salt is at least one selected from antimony sulfate, antimony chloride, antimony nitrate and antimony acetate.
3. The method for preparing composite light-colored conductive titanium dioxide powder according to claim 1, wherein the method comprises the following steps: the concentration of the hydrochloric acid in the step S1 is 10-20%.
4. The method for preparing composite light-colored conductive titanium dioxide powder according to claim 1, wherein the method comprises the following steps: the concentration of hydrogen peroxide in the step S1 is 30%; the hydrogen peroxide improves the conductivity of the product and generates a large amount of hydrogen peroxide free radical ions so as to form stronger bonding force with the titanium dioxide carrier; secondly, antimony element participating in doping in the solution is oxidized, so that the lattice distortion is reduced while the aim of effective doping is fulfilled.
5. The method for preparing composite light-colored conductive titanium dioxide powder according to claim 1, wherein the method comprises the following steps: in the step S2, the shape of the titanium dioxide is at least one of spherical, rod-like, tubular and irregular; the hydroxylation treatment increases the number of hydroxyl groups on the surface of the titanium dioxide carrier, so that the reaction activity and the wettability of the titanium dioxide carrier are improved, and the coating of the conducting layer is more uniform and complete.
6. The method for preparing composite light-colored conductive titanium dioxide powder according to claim 1, wherein the method comprises the following steps: in the step S3, the alkaline solution is at least one of aqueous solutions of ammonia, urea, sodium carbonate, potassium carbonate, sodium hydroxide and potassium hydroxide; the ultrasonic treatment time is 10-60 min.
7. The method for preparing composite light-colored conductive titanium dioxide powder according to claim 1, wherein the method comprises the following steps: in the step S4, the drying temperature is 50-80 ℃, and the drying time is 8-16 h; the calcination temperature is 400-800 ℃, and the calcination time is 2-5 h.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112852208A (en) * | 2021-01-08 | 2021-05-28 | 上海大学 | Light-colored titanium dioxide conductive filler and preparation method and application thereof |
| CN115520896A (en) * | 2022-10-09 | 2022-12-27 | 南通大学 | Preparation method of composite conductive powder based on photoelectric effect |
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| CN115520896A (en) * | 2022-10-09 | 2022-12-27 | 南通大学 | Preparation method of composite conductive powder based on photoelectric effect |
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Application publication date: 20200515 |