CN105355320A - Production technology of nanoscale conductive titanium dioxide - Google Patents
Production technology of nanoscale conductive titanium dioxide Download PDFInfo
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- CN105355320A CN105355320A CN201510700462.9A CN201510700462A CN105355320A CN 105355320 A CN105355320 A CN 105355320A CN 201510700462 A CN201510700462 A CN 201510700462A CN 105355320 A CN105355320 A CN 105355320A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
Abstract
The invention relates to a production technology of a nanoscale conductive titanium dioxide and belongs to the technical field of titanium dioxide production. The production technology comprises the following steps: reducing oxidized graphene into graphene, mixing the graphene with titanium dioxide, and finally forming a titanium dioxide-graphene composite material; oxidizing graphite powder with concentrated sulfuric acid and potassium permanganate, and forming the oxidized graphene after centrifugal precipitation; drying and grinding the oxidized graphene into powder, respectively putting the oxidized graphene and titanium dioxide powder into absolute ethyl alcohol, dripping an absolute ethyl alcohol dispersion liquid of the oxidized graphene into the absolute ethyl alcohol dispersion liquid of the titanium dioxide, and adding hydrochloric acid and distilled water to obtain a gel product; and carrying out ageing and ultrasonic cleaning, roasting and grinding the gel product, reducing the oxidized graphene into the graphene, and combining with the titanium dioxide to form conductive titanium dioxide. The nanoscale conductive titanium dioxide is applicable to low-temperature preparation of conductive and antistatic equipment, is also applicable to preparation of a variable-temperature sintered powder material of which the high temperature can reach 1600 DEG C and is applicable to popularization and application in related fields.
Description
Technical field
The present invention relates to titanium white production technical field, be specifically related to a kind of production technology of nano-level conducting titanium dioxide.
Background technology
Conductive titanium dioxide is, in the production process of nanometer titanium dioxide, Manufactured nanometer titanium dioxide is carried out surface treatment, semiconductor doping process, makes its stromal surface form conductivity oxide layer, thus obtained class novel electron conducting functional Semiconductor pigments or a filler, the absorption of conductive titanium dioxide to light is few, and scattering power is large, gloss, whiteness, reducing power, the optical properties such as covering power are good, can be made into the permanent conductive of near-white and other light color, antistatic product, requires higher conduction in whiteness, particularly applicable in antistatic product and environment, conductive titanium dioxide is nonpoisonous and tasteless, acidproof, alkaline-resisting, salt tolerant, organic solvent-resistant, fast light, stable below 800 DEG C, be not oxidized, do not fire, and there is fire retardation, be almost applicable to any requirement conduction, the environment of antistatic and occasion, made an addition to coating, plastics, rubber, adhesive, ink, cement, fiber, in pottery, coordinate with other pigment, be easily modulated into the permanent conductive of the shades of colours such as near-white, antistatic product, can be widely used in the conduction of each industrial department and people's daily life, antistatic field.
Titanium dioxide and graphite oxide is mainly adopted to carry out physical mixed to carry out in the production technology of existing conductive titanium dioxide, the conductive titanium dioxide photocatalytic activity produced is limited, good optical property can not be reached in actual use, degradation rate is higher, can not reach the requirement of permanent conductive, antistatic product well.
Traditional conduction method of production of titanium dioxide cardinal principle is metal-doped modification, such as, ceramic material research department of technical research institutes, Nagoya of Japanese industry technology institute develops the ceramic temperature sensor of titanium white series, thermistor and PTC pottery, its method is adulterate in titanium dioxide under certain conditions niobium, antimony and prepare conductive titanium dioxide, its conductive titanium dioxide photocatalytic activity prepared is limited, good optical property can not be reached in actual use, degradation rate is higher, can not reach the requirement of permanent conductive, antistatic well.
Summary of the invention
The invention provides a kind of production technology of nano-level conducting titanium dioxide, this technique can promote the photocatalytic activity of conductive titanium dioxide, optical property is in actual use better, and degradation rate has obvious reduction, can reach the service behaviour of permanent conductive, antistatic product better.
Concrete technical scheme of the present invention is:
A kind of production technology of nano-level conducting titanium dioxide, key point is, described production technology comprises in graphene oxide and titanium dioxide mixed process and is reduced to Graphene, and the Graphene after reduction is combined with titanium dioxide, final generation titanium dioxide-graphene composite material, i.e. nano-level conducting titanium dioxide, on this basis, the concrete steps of nano-level conducting titanium white production technique are as described below:
A1, graphene oxide powder and absolute ethyl alcohol are mixed to get mixed liquid B, ultrasonic disperse are carried out to mixed liquid B, obtains the absolute ethyl alcohol dispersion liquid of graphene oxide;
A2, mixed liquor C titania powder and absolute ethyl alcohol are mixed to get, carry out ultrasonic disperse to mixed liquor C, obtains the absolute ethyl alcohol dispersion liquid of titanium dioxide;
A3, the absolute ethyl alcohol dispersion liquid that the absolute ethyl alcohol dispersion liquid of graphene oxide joins titanium dioxide is obtained mixed liquor D, HCL and distilled water is added after mixed liquor D stirs, then carry out stirring and obtain light/dark balance colloidal sol, static rear formation light/dark balance gel, ultrasonic disperse is carried out after the ageing of light/dark balance gel, product after ultrasonic disperse carries out vacuum baking successively, grinding, oxygen-containing functional group on graphene oxide is reduced, titanium dioxide nano-particle instead of original oxygen-containing functional group and is attached on Graphene, finally obtain titanium dioxide-graphene composite material.
The preparation process of described graphene oxide comprises the steps:
B1, add graphite powder and KMnO4 and carry out stirring reaction in concentrated sulfuric acid, then add distilled water and stir, stirring equipment used is constant temperature blender with magnetic force, finally adds H2O2 and forms mixed solution A;
B2, add in mixed solution A HCL, distilled water and absolute ethyl alcohol mixed solution A is carried out in and, then centrifugation is carried out to the mixed solution A after neutralization and obtain graphene oxide, centrifugal sediment is carried out vacuumize and form the dry thing of graphene oxide, being carried out grinding by dry for graphene oxide thing becomes graphene oxide powder;
In described step b1, the rotating speed of constant temperature blender with magnetic force is 1250-1300r/min.
In described step b1, the concentrated sulfuric acid first carries out cold bath and is cooled to 0 DEG C, then adds graphite powder and KMnO4 while stirring, graphite powder and KMnO
4mass ratio be 1:3, every 22ml concentrated sulfuric acid needs to add 1g graphite powder and 3gKMnO4, reaction temperature after graphite powder and KMnO4 add the concentrated sulfuric acid controls at 3-5 DEG C and stirring reaction 2 hours, the volume ratio of institute's adding distil water and the concentrated sulfuric acid is 5:1, reaction temperature after adding distilled water is 80-100 DEG C and stirring reaction 30 minutes, the concentration of H2O2 used is 5%, and the reaction temperature after adding H2O2 is 80-100 DEG C.
In described step b2, the concentration of HCL is 5%, and centrifugation equipment used is centrifugal precipitation mechanism, and centrifugal sediment carries out vacuumize 24 hours under 60 DEG C of conditions.
Stirring device therefor in described step a3 is constant temperature blender with magnetic force, and rotating speed is 800-1000r/min.
In described step a1, the time of ultrasonic disperse is 1 hour.
In described step a2, the time of ultrasonic disperse is 0.5 hour.
In described step a3, the absolute ethyl alcohol dispersion liquid of graphene oxide adds feed postition in the absolute ethyl alcohol dispersion liquid of titanium dioxide for dropwise to add, in described mixed liquor D, the ratio of the amount of substance of titanium dioxide, distilled water and HCL is 1:3:0.08, the time of ageing is 72 hours, and the roasting of light/dark balance gel is 350 DEG C and continues to carry out 2 hours.
The invention has the beneficial effects as follows: the method that the present invention adopts Graphene to mix with Nano titanium dioxide prepares conductive titanium dioxide, first Graphene is carried out centrifugal stripping and form graphene oxide, surface of graphene oxide has a large amount of oxygen-containing functional groups, as carboxyl, hydroxyl, epoxy radicals, by roasting, graphene oxide is carried out reduction and become Graphene, titanium dioxide replaces oxygen-containing functional group to be combined with Graphene, graphene oxide is evenly distributed in titanium dioxide by the peptizaiton of absolute ethyl alcohol dispersion liquid, the combination of titanium dioxide and Graphene can be very even, Graphene after reduction is very stable, there is fabulous conductive and mechanical properties, the conductive titanium dioxide of final preparation had both had the nano ZnO of nanometer titanium dioxide, there is again conduction and the antistatic performance of Graphene, its each particle is an independently semiconductor, so powder structure is not easy to be destroyed when disperseing, the resistance value making coating is more stable, its antistatic coating surface smoothing made, color is homogeneous, and due to the ultrahigh hardness of Graphene and overstable character, making to meet material possesses high temperature resistant, corrosion resistant feature, nano-level conducting titanium dioxide product prepared by the present invention had both adapted to the conduction for low-temperature growth, antistatic aids, also the preparation that high temperature reaches the alternating temperature sintered powder material of 1600 degree is suitable for, range of application is widened greatly.
Accompanying drawing explanation
Fig. 1 is the schematic flow sheet of production technology in the present invention.
Embodiment
The present invention relates to a kind of production technology of nano-level conducting titanium dioxide, described production technology comprises in graphene oxide and titanium dioxide mixed process and is reduced to Graphene, and the Graphene after reduction is combined with titanium dioxide, final generation titanium dioxide-graphene composite material, i.e. nano-level conducting titanium dioxide.
Specific embodiment, the production technology concrete steps of nano-level conducting titanium dioxide are as described below:
First, need to prepare graphene oxide, the concrete steps of preparation are as described below:
B1, the concentrated sulfuric acid is injected constant temperature blender with magnetic force, use this blender can control temperature well, make mixed liquor have better stability, the concentrated sulfuric acid first carries out cold bath and is cooled to 0 DEG C, then adds graphite powder and KMnO4 while stirring, the concentrated sulfuric acid, KMnO
4it is oxidant, graphite oxidation can be become graphite oxide, the mass ratio of graphite powder and KMnO4 is 1:3, every 22ml concentrated sulfuric acid needs to add 1g graphite powder and 3gKMnO4, reaction temperature after graphite powder and KMnO4 add the concentrated sulfuric acid controls at 3-5 DEG C and stirring reaction 2 hours, the speed of agitator of constant temperature blender with magnetic force is 1275r/min, then add distilled water to stir, the volume ratio of institute's adding distil water and the concentrated sulfuric acid is 5:1, reaction temperature after adding distilled water is 80-100 DEG C and stirring reaction 30 minutes, add H2O2 subsequently, the concentration of H2O2 used is 5%, reaction temperature after adding H2O2 is 80-100 DEG C, finally form mixed solution A,
B2, add in mixed solution A HCL, distilled water and absolute ethyl alcohol mixed solution A is carried out in and, the concentration of HCL is 5%, then centrifugation is carried out to the mixed solution A after neutralization and obtain graphene oxide, namely adopt the method for centrifugal stripping that graphite oxide is peeled off into graphene oxide, centrifugation equipment used is centrifugal precipitation mechanism, graphene oxide carries out vacuumize and within 24 hours, forms the dry thing of graphene oxide under 60 DEG C of conditions, and being carried out grinding by dry for graphene oxide thing becomes graphene oxide powder;
After graphene oxide powder preparation completes, graphene oxide and titanium dioxide are mixed, mixed process is as described below:
A1, graphene oxide powder and absolute ethyl alcohol are mixed to get mixed liquid B, carry out ultrasonic disperse to mixed liquid B, the time of ultrasonic disperse is 1 hour, obtains the absolute ethyl alcohol dispersion liquid of graphene oxide;
A2, mixed liquor C titania powder and absolute ethyl alcohol are mixed to get, carry out ultrasonic disperse to mixed liquor C, and the time of ultrasonic disperse is 0.5 hour, obtains the absolute ethyl alcohol dispersion liquid of titanium dioxide;
A3, the absolute ethyl alcohol dispersion liquid that the absolute ethyl alcohol dispersion liquid of graphene oxide dropwise joins titanium dioxide is obtained mixed liquor D, dropwise add is to allow graphene oxide more be evenly distributed, titanium dioxide in mixed liquor D, the ratio of the amount of substance of distilled water and HCL is 1:3:0.08, mixing apparatus used is constant temperature blender with magnetic force, rotating speed is 900r/min, HCL and distilled water is added after mixed liquor D stirs, then carry out stirring and obtain light/dark balance colloidal sol, static rear formation light/dark balance gel, light/dark balance gel ageing 72 hours, carry out ultrasonic cleaning subsequently, product after ultrasonic cleaning carries out roasting successively, grinding, the roasting of light/dark balance gel is 350 DEG C and continues to carry out 2 hours, roasting oxidation Graphene can make graphene oxide be reduced into as Graphene, titanium dioxide replaces the oxygen-containing functional group in graphene oxide and is combined with Graphene, titanium dioxide nano-particle mainly tends to be attached to the edge of Graphene or the place of fold, Graphene-composite titania material is obtained after baking end.
Graphene initial oxidation is become graphene oxide by this patent, restore as Graphene and be combined with titanium dioxide formed high temperature resistant, corrosion resistant electric conducting material, this electric conducting material is made both to have had the function of nano material, there is again semiconductor conduction, the function of antistatic, this product had both adapted to the conduction for low-temperature growth, antistatic aids, also the preparation that high temperature reaches the alternating temperature sintered powder material of 1600 degree is suitable for, such as conductivity ceramics, the conductivity ceramics of current research and development is generally silicon carbide ceramics, SiO 2-ceramic, zirconia ceramics, aluminium oxide ceramics, but what really have use value is SrCeO3 series type proton conducting ceramics temperature, titanium dioxide-the graphene composite material related in the present invention has high temperature resistant, corrosion resistant characteristic, also the preparation of conducting ceramic material can be applicable to.
Claims (9)
1. the production technology of a nano-level conducting titanium dioxide, it is characterized in that, described production technology comprises in graphene oxide and titanium dioxide mixed process and is reduced to Graphene, and the Graphene after reduction is combined with titanium dioxide, final generation titanium dioxide-graphene composite material, i.e. nano-level conducting titanium dioxide, on this basis, the concrete steps of nano-level conducting titanium white production technique are as described below:
A1, graphene oxide powder and absolute ethyl alcohol are mixed to get mixed liquid B, ultrasonic disperse are carried out to mixed liquid B, obtains the absolute ethyl alcohol dispersion liquid of graphene oxide;
A2, mixed liquor C titania powder and absolute ethyl alcohol are mixed to get, carry out ultrasonic disperse to mixed liquor C, obtains the absolute ethyl alcohol dispersion liquid of titanium dioxide;
A3, the absolute ethyl alcohol dispersion liquid that the absolute ethyl alcohol dispersion liquid of graphene oxide joins titanium dioxide is obtained mixed liquor D, HCL and distilled water is added after mixed liquor D stirs, then carry out stirring and obtain light/dark balance colloidal sol, static rear formation light/dark balance gel, ultrasonic disperse is carried out after the ageing of light/dark balance gel, product after ultrasonic disperse carries out vacuum baking successively, grinding, oxygen-containing functional group on graphene oxide is reduced, titanium dioxide nano-particle instead of original oxygen-containing functional group and is attached on Graphene, finally obtain titanium dioxide-graphene composite material.
2. the production technology of a kind of nano-level conducting titanium dioxide according to claim 1, is characterized in that: the preparation process of described graphene oxide comprises the steps:
B1, add graphite powder and KMnO4 and carry out stirring reaction in concentrated sulfuric acid, then add distilled water and stir, stirring equipment used is constant temperature blender with magnetic force, finally adds H2O2 and forms mixed solution A;
B2, add in mixed solution A HCL, distilled water and absolute ethyl alcohol mixed solution A is carried out in and, then centrifugation is carried out to the mixed solution A after neutralization and obtain graphene oxide, centrifugal sediment is carried out vacuumize and form the dry thing of graphene oxide, being carried out grinding by dry for graphene oxide thing becomes graphene oxide powder.
3. the production technology of a kind of nano-level conducting titanium dioxide according to claim 2, is characterized in that: in described step b1, the rotating speed of constant temperature blender with magnetic force is 1250-1300r/min.
4. the production technology of a kind of nano-level conducting titanium dioxide according to claim 2, it is characterized in that: in described step b1, the concentrated sulfuric acid first carries out cold bath and is cooled to 0 DEG C, then graphite powder and KMnO4 is added while stirring, the mass ratio of graphite powder and KMnO4 is 1:3, every 22ml concentrated sulfuric acid needs to add 1g graphite powder and 3gKMnO4, reaction temperature after graphite powder and KMnO4 add the concentrated sulfuric acid controls at 3-5 DEG C and stirring reaction 2 hours, the volume ratio of institute's adding distil water and the concentrated sulfuric acid is 5:1, reaction temperature after adding distilled water is 80-100 DEG C and stirring reaction 30 minutes, the concentration of H2O2 used is 5%, reaction temperature after adding H2O2 is 80-100 DEG C.
5. the production technology of a kind of nano-level conducting titanium dioxide according to claim 2, it is characterized in that: in described step b2, the concentration of HCL is 5%, and centrifugation equipment used is centrifugal precipitation mechanism, and centrifugal sediment carries out vacuumize 24 hours under 60 DEG C of conditions.
6. the production technology of a kind of nano-level conducting titanium dioxide according to claim 1, is characterized in that: stirring device therefor in described step a3 is constant temperature blender with magnetic force, and rotating speed is 800-1000r/min.
7. the production technology of a kind of nano-level conducting titanium dioxide according to claim 1, is characterized in that: in described step a1, and the time of ultrasonic disperse is 1 hour.
8. the production technology of a kind of nano-level conducting titanium dioxide according to claim 1, is characterized in that: in described step a2, and the time of ultrasonic disperse is 0.5 hour.
9. the production technology of a kind of nano-level conducting titanium dioxide according to claim 1, it is characterized in that: in described step a3, the absolute ethyl alcohol dispersion liquid of graphene oxide adds feed postition in the absolute ethyl alcohol dispersion liquid of titanium dioxide for dropwise to add, in described mixed liquor D, the ratio of the amount of substance of titanium dioxide, distilled water and HCL is 1:3:0.08, the time of ageing is 72 hours, and the roasting of light/dark balance gel is 350 DEG C and continues to carry out 2 hours.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106872063A (en) * | 2017-01-17 | 2017-06-20 | 中国电子科技集团公司第四十九研究所 | A kind of preparation method and application of tubulose tungsten oxide graphene composite material |
| CN107349949A (en) * | 2017-06-20 | 2017-11-17 | 江苏特丰新材料科技有限公司 | A kind of production technology of conductive titanium dioxide |
| CN107393622A (en) * | 2017-06-27 | 2017-11-24 | 宁波墨西科技有限公司 | A kind of graphene Asia titanium oxide combined conductive agent and preparation method thereof |
| CN107880592A (en) * | 2017-11-24 | 2018-04-06 | 锦州钛业股份有限公司 | A kind of preparation method of composite conductive powder |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106872063A (en) * | 2017-01-17 | 2017-06-20 | 中国电子科技集团公司第四十九研究所 | A kind of preparation method and application of tubulose tungsten oxide graphene composite material |
| CN107349949A (en) * | 2017-06-20 | 2017-11-17 | 江苏特丰新材料科技有限公司 | A kind of production technology of conductive titanium dioxide |
| CN107393622A (en) * | 2017-06-27 | 2017-11-24 | 宁波墨西科技有限公司 | A kind of graphene Asia titanium oxide combined conductive agent and preparation method thereof |
| CN107393622B (en) * | 2017-06-27 | 2020-01-21 | 宁波墨西科技有限公司 | Graphene-titanium suboxide composite conductive agent and preparation method thereof |
| CN107880592A (en) * | 2017-11-24 | 2018-04-06 | 锦州钛业股份有限公司 | A kind of preparation method of composite conductive powder |
| CN107880592B (en) * | 2017-11-24 | 2020-09-11 | 中信钛业股份有限公司 | Preparation method of composite conductive powder |
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