CN107349949A - A kind of production technology of conductive titanium dioxide - Google Patents
A kind of production technology of conductive titanium dioxide Download PDFInfo
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- CN107349949A CN107349949A CN201710471912.0A CN201710471912A CN107349949A CN 107349949 A CN107349949 A CN 107349949A CN 201710471912 A CN201710471912 A CN 201710471912A CN 107349949 A CN107349949 A CN 107349949A
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- titanium dioxide
- boron
- ethyl alcohol
- absolute ethyl
- oxidation nitridation
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 131
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 57
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 25
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims abstract description 45
- 230000003647 oxidation Effects 0.000 claims abstract description 44
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 44
- 229910052796 boron Inorganic materials 0.000 claims abstract description 37
- 229910052582 BN Inorganic materials 0.000 claims abstract description 31
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000007788 liquid Substances 0.000 claims abstract description 26
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims abstract description 25
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000012153 distilled water Substances 0.000 claims abstract description 18
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000006185 dispersion Substances 0.000 claims abstract description 17
- 239000012286 potassium permanganate Substances 0.000 claims abstract description 13
- 239000000843 powder Substances 0.000 claims abstract description 13
- 238000005119 centrifugation Methods 0.000 claims abstract description 10
- 238000002360 preparation method Methods 0.000 claims abstract description 10
- 239000002131 composite material Substances 0.000 claims abstract description 8
- SLFWTPQAQWXPBE-UHFFFAOYSA-N [O-2].[O-2].[Ti+4].[B+3] Chemical compound [O-2].[O-2].[Ti+4].[B+3] SLFWTPQAQWXPBE-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000000227 grinding Methods 0.000 claims abstract description 3
- 238000006243 chemical reaction Methods 0.000 claims description 16
- 238000003756 stirring Methods 0.000 claims description 16
- 239000011259 mixed solution Substances 0.000 claims description 12
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 9
- 239000001301 oxygen Substances 0.000 claims description 9
- 229910052760 oxygen Inorganic materials 0.000 claims description 9
- 230000008859 change Effects 0.000 claims description 8
- 125000000524 functional group Chemical group 0.000 claims description 6
- 229910002804 graphite Inorganic materials 0.000 claims description 6
- 239000010439 graphite Substances 0.000 claims description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- 230000008569 process Effects 0.000 claims description 4
- 230000003068 static effect Effects 0.000 claims description 4
- 239000010936 titanium Substances 0.000 claims description 4
- 229910052719 titanium Inorganic materials 0.000 claims description 4
- 238000001291 vacuum drying Methods 0.000 claims description 4
- 241000790917 Dioxys <bee> Species 0.000 claims description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 3
- 230000032683 aging Effects 0.000 claims description 3
- 230000007246 mechanism Effects 0.000 claims description 3
- 239000002105 nanoparticle Substances 0.000 claims description 3
- 238000001556 precipitation Methods 0.000 claims description 3
- 239000013049 sediment Substances 0.000 claims description 3
- 238000006386 neutralization reaction Methods 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 2
- 238000003760 magnetic stirring Methods 0.000 claims 1
- 235000010215 titanium dioxide Nutrition 0.000 abstract description 54
- 239000000463 material Substances 0.000 abstract description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 abstract 2
- 239000000919 ceramic Substances 0.000 description 10
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 239000004020 conductor Substances 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
- 230000001699 photocatalysis Effects 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 229910010293 ceramic material Inorganic materials 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 229910021389 graphene Inorganic materials 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000000049 pigment Substances 0.000 description 2
- 239000004593 Epoxy Substances 0.000 description 1
- 229910003408 SrCeO3 Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052810 boron oxide Inorganic materials 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 239000004567 concrete Substances 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000000976 ink Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 239000010955 niobium Substances 0.000 description 1
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 230000009967 tasteless effect Effects 0.000 description 1
- 150000003608 titanium Chemical class 0.000 description 1
- 238000004506 ultrasonic cleaning Methods 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
-
- B01J35/33—
-
- B01J35/39—
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/46—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
- C04B35/583—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on boron nitride
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
Abstract
The present invention relates to a kind of production technology of nano-level conducting titanium white, belong to titanium white production technical field, boron nitride is reduced into including oxidation nitridation boron and is mixed with titanium dioxide, eventually form titanium dioxide boron nitride composite, graphite powder is aoxidized with the concentrated sulfuric acid and potassium permanganate, oxidation nitridation boron is formed after centrifugation, dry simultaneously grind into powder, oxidation nitridation boron powder and titania powder are respectively put into absolute ethyl alcohol, the absolute ethyl alcohol dispersion liquid of oxidation nitridation boron is instilled in the absolute ethyl alcohol dispersion liquid of titanium dioxide, add hydrochloric acid and distilled water obtains gelatinous product, and it is aged, it is cleaned by ultrasonic, then it is calcined, grinding, oxidation nitridation boron is reduced to boron nitride and combines to form conductive titanium dioxide with titanium dioxide.The conductive titanium dioxide had both adapted to the conduction for low temperature preparation, antistatic aids, preparation of the high temperature up to 1600 degree of alternating temperature sintered powder material was also suitable for, suitable in association area popularization and application.
Description
Technical field
The present invention relates to titanium white production technical field, and in particular to a kind of production technology of conductive titanium dioxide.
Background technology
Conductive titanium dioxide be Manufactured nanometer titanium dioxide is surface-treated in the production process of nanometer titanium dioxide,
Semiconductor doping processing, makes its stromal surface form electric conductivity oxide layer, so as to which a kind of novel electron conducting functional half be made
Conductor pigment or filler, absorption of the conductive titanium dioxide to light are lacked, and scattering power is big, the light such as gloss, whiteness, reducing power, covering power
Learn functional, can be made into near-white and other light permanent conductives, antistatic product, requiring higher in whiteness leads
Especially suitable in electricity, antistatic product and environment, conductive titanium dioxide is nonpoisonous and tasteless, acidproof, alkaline-resisting, salt tolerant, organic solvent-resistant, resistance to
Light, it is stable below 800 DEG C, do not aoxidize, be non-ignitable, and there is fire retardation, it is conductive, antistatic to be suitable for almost any requirement
Environment and occasion, made an addition in coating, plastics, rubber, adhesive, ink, cement, fiber, ceramics, matched somebody with somebody with other pigment
Close, be easily modulated into the permanent conductive, antistatic product of a variety of colors such as near-white, can be widely applied to each industrial department and
The conduction of people's daily life, antistatic field.
In the production technology of existing conductive titanium dioxide mainly using titanium dioxide and graphite oxide progress physical mixed come
Carry out, the conductive titanium dioxide photocatalytic activity produced is limited, can not reach good optical property in actual use, degraded
Rate is higher, it is impossible to is properly arrived at the requirement of permanent conductive, antistatic product.
Traditional conductive method of production of titanium dioxide cardinal principle is metal-doped modification, for example, Japan Industrial Technology Institute name is ancient
Ceramic material research department of room technical research institutes develops ceramic temperature sensor, thermistor and the PTC-ceramic of titanium white series,
Its method be under certain conditions in titanium dioxide adulterate niobium, antimony and prepare conductive titanium dioxide, its prepare conductive titanium white
Powder photocatalytic activity is limited, can not reach good optical property in actual use, and degradation rate is higher, it is impossible to is properly arrived at
The requirement of permanent conductive, antistatic.
The content of the invention
The invention provides a kind of production technology of conductive titanium dioxide, the photocatalysis that the technique can lift conductive titanium dioxide is lived
Property, optical property in actual use is preferable, and degradation rate has obvious reduction, can preferably reach permanent conductive, anti-quiet
The service behaviour of electrical article.
The present invention concrete technical scheme be：
A kind of production technology of conductive titanium dioxide, key point are that described production technology includes oxidation nitridation boron and dioxy
Change in titanium mixed process and be reduced to boron nitride, and the boron nitride after reducing is combined with titanium dioxide, ultimately generate titanium dioxide-
Boron nitride composite, i.e. conductive titanium dioxide, on this basis, comprising the following steps that for conductive titanium dioxide production technology are described：
A1, oxidation nitridation boron powder and absolute ethyl alcohol be mixed to get mixed liquid B, ultrasonic disperse is carried out to mixed liquid B, obtained
To the absolute ethyl alcohol dispersion liquid of oxidation nitridation boron；
A2, the mixed liquor C for being mixed to get titania powder and absolute ethyl alcohol, ultrasonic disperse is carried out to mixed liquor C, obtained
To the absolute ethyl alcohol dispersion liquid of titanium dioxide；
A3, the absolute ethyl alcohol dispersion liquid that the absolute ethyl alcohol dispersion liquid of oxidation nitridation boron is added to titanium dioxide are mixed
Liquid D, mixed liquor D are stirring evenly and then adding into HCL and distilled water, are then stirred to obtain light/dark balance colloidal sol, are formed after static shallow
Black gel, ultrasonic disperse being carried out after the ageing of light/dark balance gel, the product after ultrasonic disperse carries out vacuum baking, grinding successively,
It is reduced the oxygen-containing functional group on oxidation nitridation boron, titanium dioxide nano-particle instead of original oxygen-containing functional group and adhere to
On boron nitride, titanium dioxide-boron nitride composite is finally given.
The preparation process of described oxidation nitridation boron comprises the following steps：
B1, graphite powder and KMnO4 are added in concentrated sulfuric acid and carries out stirring reaction, then add distilled water and be stirred,
Stirring equipment used is constant temperature blender with magnetic force, is eventually adding H2O2 and forms mixed solution A；
B2, add HCL in mixed solution A, during distilled water and absolute ethyl alcohol are carried out to mixed solution A and, then centering
Mixed solution A with after carries out centrifugation and obtains oxidation nitridation boron, and centrifugal sediment is carried out into vacuum drying forms nitrogen oxide
Change boron dried object, oxidation nitridation boron dried object is ground and is crushed into oxidation nitridation boron powder；
The rotating speed of constant temperature blender with magnetic force is 1250-1300r/min in described step b1.
In described step b1, the concentrated sulfuric acid first carries out cold bath and is cooled to 0 DEG C, then while stirring add graphite powder and
KMnO4, graphite powder and KMnO4 mass ratio are 1:3, need to add 1g graphite powders and 3gKMnO4, graphite powder per the 22ml concentrated sulfuric acids
The reaction temperature control added with KMnO4 after the concentrated sulfuric acid is in 3-5 DEG C and stirring reaction 2 hours, added distilled water and the concentrated sulfuric acid
Volume ratio be 5:1, the reaction temperature added after distilled water is 80-100 DEG C and stirring reaction 30 minutes, and H2O2's used is dense
Spend for 5%, the reaction temperature added after H2O2 is 80-100 DEG C.
In described step b2, HCL concentration is 5%, and the equipment used in centrifugation is centrifugal precipitation mechanism, centrifugation
Thing carries out vacuum drying 24 hours under the conditions of 60 DEG C.
It is constant temperature blender with magnetic force that device therefor is stirred in described step a3, rotating speed 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 oxidation nitridation boron adds the absolute ethyl alcohol dispersion liquid of titanium dioxide
In feed postition to be added dropwise, the ratio of the amount of the material of titanium dioxide, distilled water and HCL is in described mixed liquor D
1：3:0.08, the time of ageing is 72 hours, and light/dark balance gel is roasted to 350 DEG C and continues to carry out 2 hours.
The beneficial effects of the invention are as follows：The method that the present invention is mixed using boron nitride with Nano titanium dioxide prepares conductive
Titanium dioxide, boron nitride being first subjected to centrifugation stripping and forms oxidation nitridation boron, surface of graphene oxide has substantial amounts of oxygen-containing functional group,
Such as carboxyl, hydroxyl, epoxy radicals, graphene oxide is carried out into reduction by roasting turns into boron nitride, and titanium dioxide replaces oxygen-containing official
It can roll into a ball and be combined with boron nitride, oxidation nitridation boron is evenly distributed in titanium dioxide by the peptizaiton of absolute ethyl alcohol dispersion liquid, and two
The combination of titanium oxide and boron nitride can be highly uniform, and the boron nitride after reduction is very stable, has fabulous conductive and mechanical properties, most
The conductive titanium dioxide prepared eventually had both had the nano ZnO of nanometer titanium dioxide, had the conduction and static electricity resistance of boron nitride again
Can, its each particle is an independent semiconductor, so powder structure is not easy to be destroyed when scattered, coating is made
Resistance value it is relatively stable, antistatic coating smooth surface, the color that it is made are homogeneous, and the ultrahigh hardness due to boron nitride and
Overstable property so that meet material and possess high temperature resistant, corrosion resistant feature, nano-level conducting titanium dioxide production prepared by the present invention
Product had both adapted to the conduction for low temperature preparation, antistatic aids, were also suitable for high temperature up to 1600 degree of alternating temperature sintered powder material
Preparation, application widens significantly.
Brief description of the drawings
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 conductive titanium dioxide, described production technology includes oxidation nitridation boron and dioxy
Change in titanium mixed process and be reduced to boron nitride, and the boron nitride after reducing is combined with titanium dioxide, ultimately generate titanium dioxide-
Boron nitride composite, i.e. conductive titanium dioxide.
Specific embodiment, the production technology of conductive titanium dioxide comprise the following steps that described：
Firstly, it is necessary to prepare oxidation nitridation boron, comprising the following steps that for preparation is described：
B1, by the concentrated sulfuric acid inject constant temperature blender with magnetic force in, can control temperature well using the agitator, make mixing
Liquid has more preferable stability, and the concentrated sulfuric acid first carries out cold bath and is cooled to 0 DEG C, then adds graphite powder and KMnO4 while stirring, dense
Sulfuric acid, KMnO4 are oxidants, can be by graphite oxidation into graphite oxide, and graphite powder and KMnO4 mass ratio are 1:3, per 22ml
The concentrated sulfuric acid needs to add 1g graphite powders and 3gKMnO4, and the reaction temperature that graphite powder and KMnO4 are added after the concentrated sulfuric acid is controlled in 3-5
DEG C and stirring reaction 2 hours, the speed of agitator of constant temperature blender with magnetic force is 1275r/min, then adds distilled water and is stirred
Mix, the volume ratio of added distilled water and the concentrated sulfuric acid is 5:1, the reaction temperature added after distilled water is 80-100 DEG C and stirs anti-
Answer 30 minutes, then add H2O2, H2O2 used concentration is 5%, and the reaction temperature after addition H2O2 is 80-100 DEG C, most
After form mixed solution A；
B2, add HCL in mixed solution A, during distilled water and absolute ethyl alcohol are carried out to mixed solution A and, HCL concentration
For 5%, centrifugation is then carried out to the mixed solution A after neutralization and obtains oxidation nitridation boron, i.e., the method peeled off using centrifugation
Graphite oxide is peeled off into oxidation nitridation boron, the equipment used in centrifugation is centrifugal precipitation mechanism, and oxidation nitridation boron is in 60 DEG C of bars
Vacuum drying is carried out under part and forms oxidation nitridation boron dried object within 24 hours, oxidation nitridation boron dried object is ground and is crushed into
Graphene oxide powder；
After the completion of prepared by oxidation nitridation boron powder, oxidation nitridation boron and titanium dioxide are mixed, mixed process is as follows
It is described：
A1, oxidation nitridation boron powder and absolute ethyl alcohol be mixed to get mixed liquid B, ultrasonic disperse is carried out to mixed liquid B, surpassed
The sound scattered time is 1 hour, obtains the absolute ethyl alcohol dispersion liquid of oxidation nitridation boron；
A2, the mixed liquor C for being mixed to get titania powder and absolute ethyl alcohol, ultrasonic disperse is carried out to mixed liquor C, surpassed
The sound scattered time 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 oxidation nitridation boron is added dropwise to titanium dioxide obtain
Mixed liquor D, it is titanium dioxide, distilled water and HCL in mixed liquor D in order to allow oxidation nitridation boron to be more evenly distributed to be added dropwise
Material amount ratio be 1：3:0.08, mixing apparatus used is constant temperature blender with magnetic force, rotating speed 900r/min, is mixed
Liquid D is stirring evenly and then adding into HCL and distilled water, is then stirred to obtain light/dark balance colloidal sol, light/dark balance gel is formed after static,
Light/dark balance gel is aged 72 hours, is then cleaned by ultrasonic, the product after ultrasonic cleaning is calcined, ground successively, somber
Color gel is roasted to 350 DEG C and continues to carry out 2 hours, and roasting oxidation boron nitride can be such that oxidation nitridation boron is reduced into as nitrogen
Change boron, titanium dioxide replaces the oxygen-containing functional group in oxidation nitridation boron and combined with boron nitride, and titanium dioxide nano-particle is main
Tend to be attached to the edge of boron nitride or the place of fold, boron nitride-composite titania material is obtained after baking end.
Boron nitride initial oxidation is turned into oxidation nitridation boron by this patent, is restored as boron nitride and is combined to form with titanium dioxide
High temperature resistant, corrosion resistant conductive material, make the conductive material both have the function of nano material, have semiconductor conductive, anti-again
The function of electrostatic, the product had both adapted to the conduction for low temperature preparation, antistatic aids, were also suitable for high temperature up to 1600 degree of change
The preparation of warm sintered powder material, such as conductivity ceramics, the conductivity ceramics researched and developed at present are usually silicon carbide ceramics, silica
Ceramics, zirconia ceramics, aluminium oxide ceramics, but what is really had use value is SrCeO3 series type proton conducting ceramics temperatures, this
Titanium dioxide-the boron nitride composite being related in invention has high temperature resistant, corrosion resistant characteristic, can also be applied to conduction
The preparation of ceramic material.
Claims (5)
1. a kind of production technology of conductive titanium dioxide, it is characterised in that described production technology includes oxidation nitridation boron and dioxy
Change in titanium mixed process and be reduced to boron nitride, and the boron nitride after reducing is combined with titanium dioxide, ultimately generate titanium dioxide-
Boron nitride composite, i.e. conductive titanium dioxide, on this basis, comprising the following steps that for conductive titanium dioxide production technology are described：
A1, oxidation nitridation boron powder and absolute ethyl alcohol be mixed to get mixed liquid B, ultrasonic disperse is carried out to mixed liquid B, obtains oxygen
Change the absolute ethyl alcohol dispersion liquid of boron nitride；
A2, the mixed liquor C for being mixed to get titania powder and absolute ethyl alcohol, ultrasonic disperse is carried out to mixed liquor C, obtains two
The absolute ethyl alcohol dispersion liquid of titanium oxide；
A3, the absolute ethyl alcohol dispersion liquid that the absolute ethyl alcohol dispersion liquid of oxidation nitridation boron is added to titanium dioxide obtain mixed liquor D,
Mixed liquor D is stirring evenly and then adding into HCL and distilled water, is then stirred to obtain light/dark balance colloidal sol, light/dark balance is formed after static
Gel, ultrasonic disperse is carried out after the ageing of light/dark balance gel, the product after ultrasonic disperse carries out vacuum baking, grinding successively, makes oxygen
The oxygen-containing functional group changed on boron nitride is reduced, and titanium dioxide nano-particle instead of original oxygen-containing functional group and be attached to nitrogen
Change on boron, finally give titanium dioxide-boron nitride composite.
A kind of 2. production technology of conductive titanium dioxide according to claim 1, it is characterised in that：Described oxidation nitridation boron
Preparation process comprise the following steps：
B1, graphite powder and KMnO4 are added in concentrated sulfuric acid and carries out stirring reaction, then add distilled water and be stirred, stir
Equipment used is constant temperature blender with magnetic force, is eventually adding H2O2 and forms mixed solution A；
B2, add HCL in mixed solution A, during distilled water and absolute ethyl alcohol are carried out to mixed solution A and, then to neutralization after
Mixed solution A carry out centrifugation obtain oxidation nitridation boron, centrifugal sediment is carried out into vacuum drying forms oxidation nitridation boron
Dried object, oxidation nitridation boron dried object is ground and is crushed into oxidation nitridation boron powder.
A kind of 3. production technology of conductive titanium dioxide according to claim 2, it is characterised in that：It is permanent in described step b1
The rotating speed of warm magnetic stirring apparatus is 1250-1300r/min.
A kind of 4. production technology of conductive titanium dioxide according to claim 2, it is characterised in that：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, graphite powder and KMnO4 quality while stirring
Than for 1:3, need to add 1g graphite powders and 3gKMnO4, the reaction that graphite powder and KMnO4 are added after the concentrated sulfuric acid per the 22ml concentrated sulfuric acids
For temperature control in 3-5 DEG C and stirring reaction 2 hours, the volume ratio of added distilled water and the concentrated sulfuric acid is 5:1, add distilled water it
Reaction temperature afterwards is 80-100 DEG C of simultaneously stirring reaction 30 minutes, and H2O2 used concentration is 5%, the reaction added after H2O2
Temperature is 80-100 DEG C.
A kind of 5. production technology of conductive titanium dioxide according to claim 2, it is characterised in that：In described step b2,
HCL concentration is 5%, and the equipment used in centrifugation is centrifugal precipitation mechanism, and centrifugal sediment carries out vacuum under the conditions of 60 DEG C
Dry 24 hours.
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