CN107880592A - A kind of preparation method of composite conductive powder - Google Patents
A kind of preparation method of composite conductive powder Download PDFInfo
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- CN107880592A CN107880592A CN201711188804.9A CN201711188804A CN107880592A CN 107880592 A CN107880592 A CN 107880592A CN 201711188804 A CN201711188804 A CN 201711188804A CN 107880592 A CN107880592 A CN 107880592A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/36—Compounds of titanium
- C09C1/3607—Titanium dioxide
- C09C1/3653—Treatment with inorganic compounds
- C09C1/3661—Coating
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/06—Treatment with inorganic compounds
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/22—Rheological behaviour as dispersion, e.g. viscosity, sedimentation stability
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- C01P2006/40—Electric properties
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Abstract
A kind of preparation method of composite conductive powder, takes distilled water, and the pH value 5.0~10.0 of water is controlled using acid or alkali, the dispersing aid of wiring solution-forming is added, obtains dispersion liquid；Weigh titanium dioxide first product to be added in dispersion liquid, be well mixed, prepare titania slurry；Watersoluble modified graphene slurry and silicate solutions will be added in titania slurry in 1 hour~3 hours, meanwhile, using aluminum salt solution control system pH value 4.5~9.5, cure 1 hour~2 hours；Scrubbed, filtering, dry, crush, obtaining conductive powder body.Advantage is：Preparation technology is simple, low for equipment requirements, and cost is low, and the conductive powder material whiteness prepared is good, conductance high covering power is strong；And there is excellent chemical inertia, can be applied to coating, plastics, rubber, ink and the field for having antistatic requirement.
Description
Technical field
The present invention relates to a kind of preparation method of composite conductive powder.
Background technology
Conductive material can be divided into carbon system, metal system, metal oxide system and macromolecular according to the difference of chemical composition.
Wherein, carbon series conductive material mainly has conductive black, graphite, carbon fiber, carbon nanometer, grapheme tube, conductive good, coloring
The characteristics of power is strong, chemical stability is high, density is small, cheap；Its deficiency mainly have dispersion stabilization is poor, color depth.Metal
It is that conductive material mainly has silver-colored system, copper system, nickel system, there is good electric conductivity and ductility, color is relatively shallower；Its deficiency is main
There is price high, Ion transfer easily occurs, oxidation easily occurs, finally reduces electric conductivity.Metal oxide system conductive material master
There are antimony-doped stannic oxide, Al-Doped ZnO, indium doped tin oxide, there is the characteristics of fusing point is high, oxidation resistance is strong；Its deficiency is main
There is complex manufacturing, seriously polluted, and price is higher.Conducting polymer composite mainly has polyacetylene, polythiophene, poly- pyrrole
To cough up, polyaniline, polyhenylene etc., have the advantages that light, environmental stability is good, electrical conductivity is adjustable, its deficiency mainly has price,
In a small amount of synthesis phases in laboratory, do not industrialize.
Titanium dioxide is also known as titanium dioxide, nontoxic, harmless, whiteness is high, strong covering power, adhesive force are good, has good chemistry
Inertia, it is widely used in the numerous areas such as coating, plastics, papermaking, ink.But because usual titanium dioxide resistance value is higher, limit
Its application in antistatic field is made.Have both at home and abroad at present and much use coated by titanium dioxide antimony-doped stannic oxide, i.e. ATO.
But such product belongs to poisonous and harmful substance because of complex manufacturing using coating agent, thus predominantly stay in academic research and
It is sample aspect to prepare experiment, and industrialization and industrialization is also not implemented.
Graphene only absorbs 2.3% light, almost fully transparent, and thermal conductivity factor is up to 5300W/mK, resistance under normal temperature
Rate about 10-6Ω cm, lower than copper or silver, its own is a kind of very excellent conductive material.But because its color, an office
Use is limited in black or dark colour conduction application system.
The content of the invention
The composite conductive powder taken into account the technical problem to be solved in the present invention is to provide a kind of whiteness and electric conductivity index
Preparation method, conductive powder body cost prepared by this method is low, has splendid electric conductivity, dispersiveness, covering power, adhesive force, fits
Close application of the conductive-type product in light-coloured prods.
The present invention technical solution be：
A kind of preparation method of composite conductive powder, it is comprised the following steps that：
1) distilled water is taken, the pH value range 5.0~10.0 of water is controlled using inorganic acid or aqueous slkali, adds the scattered of wiring solution-forming
Auxiliary agent, the dispersing aid are silicate, acrylates, polycarboxylate, citric acid, at least one of dodecyl sodium sulfate,
It is scattered 10 minutes~30 minutes, obtain dispersion liquid；
2) weigh titanium dioxide first product to be added in the dispersion liquid of step 1) preparation, be well mixed, it is dense to prepare titanium dioxide quality
Spend the slurry for 10%~50%；
3) slurry of step 2) is warming up to 60 DEG C~80 DEG C, and this temperature is maintained in whole coating process；
4) watersoluble modified graphene slurry and silicate solutions are added in the slurry of step 2) in 1 hour~3 hours, together
When, using aluminum salt solution control system pH value 4.5~9.5, cure 1 hour~2 hours；
5) step 4) washing, filtering, dry, crushing are obtained into conductive powder body.
Further, the watersoluble modified graphene slurry is carboxylated graphene or amination graphene, described water-based
Modified graphene stock quality concentration is 5%~10%；Watersoluble modified graphene slurry addition is starched with watersoluble modified graphene
C accounts for TiO in material2Weight is calculated as 5%~12%.
Further, silicate described in step 1) is sodium metasilicate or potassium silicate, and silicate addition is with silicate
SiO2Account for TiO2Weight is calculated as 0.1%~0.4%.
Further, the acrylates is ammonium acrylate or PAA, and the polycarboxylate is polycarboxylic acids ammonium or gathered
Carboxylic acid sodium.
Further, when the dispersant of addition is organic dispersing agent, dispersant addition accounts for TiO2The 0.2% of weight~
1.0%.
Further, when doing dispersant using silicate, the pH value of water is adjusted 9.5~10.0 using inorganic base；Use
When polyacrylate, polycarboxylate, dodecyl sodium sulfate are as dispersant, the pH value of water is adjusted using inorganic acid or aqueous slkali
6.5~7.5；During using citric acid as dispersant, the pH value of water is adjusted 5.0~6.0 using inorganic acid.
Further, in step 1) and step 4), silicate solutions are at least one in sodium silicate solution, potassium silicate solution
Kind, the silicate solution concentration is with SiO2It is calculated as 100g/L~200g/L；Silicate solutions addition is with silicic acid in step 4)
SiO in salting liquid2Account for TiO2Weight is calculated as 3%~5%.
Further, in step 4), the aluminium salt is aluminum sulfate, aluminium chloride, at least one of aluminum nitrate solution, solution
Concentration is with Al2O3It is calculated as 80g/L~100g/L.
When further, using silicate as dispersant, slurry pH controls are 4.5~9.5 during coating；Using poly-
When acrylates, polycarboxylate, sodium dodecyl sulfate solution are as dispersant, during coating slurry pH controls 6.5~
7.5；When using citric acid as dispersant, slurry pH controls are 5.5~6.5 during coating.
Further, titanium dioxide first product is produced using sulfuric acid process or chloridising in step 2).
The conductive powder body of the present invention, using rutile titanium dioxide first product, ordinary titanium powder production equipment can be achieved
Production, low for equipment requirements, preparation technology is simple, and cost is low, and the conductive powder material whiteness prepared is good, the high covering of conductance
Power is strong；And there is excellent chemical inertia, can apply to coating, plastics, rubber, ink and the neck for having antistatic requirement
In domain, market application foreground is extensive.
Embodiment
Embodiment 1
1st, a certain amount of distilled water is weighed, uses aqueous slkali hydrochloric acid to adjust distilled water pH as 4.5, adds sodium silicate solution thereto,
The addition of sodium silicate solution is with SiO in sodium metasilicate2Account for TiO2Weight is calculated as 0.1%, and sodium silicate solution concentration presses SiO2It is calculated as
200g/L, disperse 10 minutes, obtain dispersion liquid；
2nd, the rutile titanium dioxide by chloridising production adds above-mentioned dispersion liquid, prepares titanium dioxide mass concentration as 10%
Slurry；
3rd, 2 to 60 DEG C of heating step, and maintain this temperature in whole coating process；
4th, 5.0% is added in 3 hours (with SiO2Account for TiO2Weight meter) sodium silicate solution, sodium silicate solution concentration presses SiO2It is calculated as
200g/L, while it is 10% carboxylated graphene water slurry, the wherein mass ratio of carboxylated graphene and titanium dioxide to add concentration
By C/TiO212% is calculated as, and concentration is that 100g/L aluminum sulfate solutions control slurry pH value that it is small to cure 2 between 4.5-5.5
When；
5 and then slurry is washed, filtered, dried, vapour powder, both finished product.
Embodiment 2
1st, a certain amount of water is weighed, uses sodium hydroxide solution to adjust distilled water pH as 7.5, it is molten to add Sodium Polyacrylate thereto
Liquid, sodium polyacrylate solution account for TiO with Sodium Polyacrylate2Weight meter 1.0%, disperse 20 minutes, obtain dispersion liquid；
2nd, the rutile titanium dioxide of Production By Sulfuric Acid Process is added into above-mentioned dispersion liquid, obtain preparing titanium dioxide mass concentration be
50% slurry；
3rd, the slurry of heating step 2 maintains this temperature to 70 DEG C, and in whole coating process.
4th, 3.0% is added in 1 hour (with SiO2Account for TiO2Weight meter) sodium silicate solution, sodium silicate solution concentration presses SiO2
100g/L is calculated as, while it is 5% carboxylated graphene water slurry, the wherein quality of carboxylated graphene and titanium dioxide to add concentration
Than by C/TiO25% is calculated as, and concentration is that 100g/L liquor alumini chloridis control slurry pH value between 6.5-7.5, curing 1
Hour；
5 and then slurry is washed, filtered, dried, vapour powder, both finished product.
Embodiment 3
1st, a certain amount of distilled water is weighed, uses hydrochloric acid to adjust distilled water pH as 6.5, adds polycarboxylic acids ammonium salt solution, poly- carboxylic thereto
The addition of acid ammonium solution accounts for TiO with polycarboxylic acids ammonium2Weight is calculated as 0.2%, disperses 15 minutes, obtains dispersion liquid；
2nd, the rutile titanium dioxide by chloridising production adds above-mentioned dispersion liquid, prepares titanium dioxide mass concentration as 20%
Slurry；
3rd, the slurry of heating step 2 maintains this temperature to 80 DEG C, and in whole coating process；
4th, 4.0% is added in 2 hours (with SiO2Account for TiO2Weight meter) potassium silicate solution, potassium silicate solution concentration presses SiO2It is calculated as
100g/L, while it is 5% amination graphene water slurry to add concentration, the mass ratio of wherein amination graphene and titanium dioxide is pressed
C/TiO28% is calculated as, and concentration is that 80g/L aluminum nitrate solutions control slurry pH value that it is small to cure 1.5 between 6.5-7.5
When；
5 and then slurry is washed, filtered, dried, vapour powder, both finished product.
Embodiment 4
1st, a certain amount of distilled water is weighed, uses watery hydrochloric acid to adjust distilled water pH as 6.5, adds citric acid solution, lemon thereto
The addition of acid solution accounts for TiO with citric acid2Weight is calculated as 0.5%, disperses 10 minutes, obtains dispersion liquid；
2nd, the rutile titanium dioxide of Production By Sulfuric Acid Process is added into above-mentioned dispersion liquid, obtain preparing titanium dioxide mass concentration be
30% slurry；
3rd, the slurry of heating step 2 maintains this temperature to 70 DEG C, and in whole coating process；
4th, 4.0% is added in 2 hours (with SiO2Account for TiO2Weight meter) sodium silicate solution, sodium silicate solution concentration presses SiO2It is calculated as
150g/L, while it is 10% amination graphene water slurry, the wherein mass ratio of amination graphene and titanium dioxide to add concentration
By C/TiO28% is calculated as, and concentration is that 80g/L aluminum sulfate solutions control slurry pH value that it is small to cure 1.5 between 5.5-6.5
When；
5 and then slurry is washed, filtered, dried, vapour powder, both finished product.
Embodiment 5
1st, a certain amount of distilled water is weighed, uses alkali sodium hydroxide solution to adjust distilled water pH as 9.5, it is molten to add potassium silicate thereto
Liquid, the addition of potassium silicate solution is with SiO2Account for TiO2Weight is calculated as 0.4%, and potassium silicate solution concentration presses SiO2It is calculated as 200g/L,
It is scattered 10 minutes, obtain dispersion liquid；
2nd, the rutile titanium dioxide of Production By Sulfuric Acid Process is added into above-mentioned dispersion liquid, prepares titanium dioxide mass concentration as 30%
Slurry；
3rd, the slurry of heating step 2 maintains this temperature to 70 DEG C, and in whole coating process；
4th, 4.0% is added in 2 hours (with SiO2Account for TiO2Weight meter) potassium silicate solution, potassium silicate solution concentration presses SiO2It is calculated as
150g/L, while it is 10% amination graphene water slurry, the wherein mass ratio of ether graphite alkene and titanium dioxide to add concentration
By C/TiO28% is calculated as, and concentration is that 80g/L aluminum sulfate solutions control slurry pH value that it is small to cure 1.5 between 8.5-9.5
When；
5 and then slurry is washed, filtered, dried, vapour powder, both finished product.
Embodiment 6
1st, it is 7.0 to weigh a certain amount of distilled water pH, adds sodium dodecyl sulfate solution, sodium dodecyl sulfate solution thereto
Addition TiO is accounted for dodecyl sodium sulfate2Weight is calculated as 0.3%, disperses 10 minutes, obtains dispersion liquid；
2nd, the rutile titanium dioxide by chloridising production adds above-mentioned dispersion liquid, obtain preparing titanium dioxide mass concentration be
40% slurry；
3rd, the slurry of heating step 2 maintains this temperature to 60 DEG C, and in whole coating process；
4th, 4.0% is added in 2 hours (with SiO2Account for TiO2Weight meter) potassium silicate solution, potassium silicate solution concentration presses SiO2It is calculated as
100g/L, while it is 5% amination graphene water slurry to add concentration, the mass ratio of wherein amination graphene and titanium dioxide is pressed
C/TiO28% is calculated as, and concentration is that 80g/L aluminum nitrate solutions control slurry pH value that it is small to cure 1.5 between 6.5-7.5
When；
5 and then slurry is washed, filtered, dried, vapour powder, both finished product.
Comparative example 1
1st, weigh a certain amount of distilled water, use sodium hydroxide solution adjust distilled water pH for 10.0, thereto addition 0.1% (with
SiO2Account for TiO2Weight meter) sodium silicate solution, sodium silicate solution concentration presses SiO2200g/L is calculated as, obtains dispersion liquid；
2nd, the rutile titanium dioxide by chloridising production adds above-mentioned dispersion liquid, obtain preparing titanium dioxide mass concentration be
10% slurry；
3rd, the slurry of heating step 2 maintains this temperature to 60 DEG C, and in whole coating process；
4th, 5.0% is added in 3 hours (with SiO2Account for TiO2Weight meter) sodium silicate solution, sodium silicate solution concentration presses SiO2It is calculated as
200g/L, and concentration is that 100g/L aluminum sulfate solutions control slurry pH value to be cured 2 hours between 4.5-5.5；
5 and then slurry is washed, filtered, dried, vapour powder, both finished product.
Comparative example 2
1st, weigh a certain amount of distilled water, use sodium hydroxide solution adjust distilled water pH for 10.0, thereto addition 0.1% (with
SiO2Account for TiO2Weight meter) sodium silicate solution, sodium silicate solution concentration presses SiO2200g/L is calculated as, obtains dispersion liquid；
2nd, the rutile titanium dioxide by chloridising production adds above-mentioned dispersion liquid, obtain preparing titanium dioxide mass concentration be
10% slurry；
3rd, the slurry of heating step 2 maintains this temperature to 60 DEG C, and in whole coating process；
4th, it is 10% carboxylated graphene water slurry, the wherein quality of carboxylated graphene and titanium dioxide concentration to be added in 3 hours
Than by C/TiO212% is calculated as, is cured 2 hours；
5 and then slurry is washed, filtered, dried, vapour powder, both finished product.
Table 1 is for the index of correlation of product in embodiment and using index
As can be seen from Table 1：Graphene is the most key to powder electric impact, and with the increase of addition, electrical conductivity exists
Decline, while lightness l value is also declining；In addition graphene blends is coated on titanium dioxide surface in alumina silicate, to product resistance
Rate and whiteness, which improve, certain effect.
The specific embodiment of the present invention is these are only, is not intended to limit the invention, for those skilled in the art
For member, the present invention can have various modifications and variations.Any modification within the spirit and principles of the invention, being made,
Equivalent substitution, improvement etc., should be included in the scope of the protection.
Claims (10)
1. a kind of preparation method of composite conductive powder, it is characterized in that：
1) distilled water is taken, the pH value range 5.0~10.0 of water is controlled using inorganic acid or aqueous slkali, adds the scattered of wiring solution-forming
Auxiliary agent, the dispersing aid are silicate, acrylates, polycarboxylate, citric acid, at least one of dodecyl sodium sulfate,
It is scattered 10 minutes~30 minutes, obtain dispersion liquid；
2) weigh titanium dioxide first product to be added in the dispersion liquid of step 1) preparation, be well mixed, it is dense to prepare titanium dioxide quality
Spend the slurry for 10%~50%；
3) slurry of step 2) is warming up to 60 DEG C~80 DEG C, and this temperature is maintained in whole coating process；
4) watersoluble modified graphene slurry and silicate solutions are added in the slurry of step 2) in 1 hour~3 hours, together
When, using aluminum salt solution control system pH value 4.5~9.5, cure 1 hour~2 hours；
5) step 4) washing, filtering, dry, crushing are obtained into conductive powder body.
2. the preparation method of composite conductive powder according to claim 1, it is characterized in that：The watersoluble modified graphene slurry
Expect that for carboxylated graphene or amination graphene, the watersoluble modified graphene stock quality concentration be 5%~10%；It is water-based
Modified graphene slurry addition accounts for TiO with C in watersoluble modified graphene slurry2Weight is calculated as 5%~12%.
3. the preparation method of composite conductive powder according to claim 1, it is characterized in that：Silicate is described in step 1)
Sodium metasilicate or potassium silicate, silicate addition is with SiO in silicate2Account for TiO2Weight is calculated as 0.1%~0.4%.
4. the preparation method of composite conductive powder according to claim 1, it is characterized in that：The acrylates is acrylic acid
Ammonium or PAA, the polycarboxylate are polycarboxylic acids ammonium or polycarboxylic acids sodium.
5. the preparation method of composite conductive powder according to claim 1, it is characterized in that：The dispersant of addition is organic point
During powder, dispersant addition accounts for TiO2The 0.2%~1.0% of weight.
6. the preparation method of composite conductive powder according to claim 1, it is characterized in that：Dispersant is done using silicate
When, the pH value of water is adjusted 9.5~10.0 using inorganic base；Made using polyacrylate, polycarboxylate, dodecyl sodium sulfate
For dispersant when, the pH value of water is adjusted 6.5~7.5 using inorganic acid or aqueous slkali；During using citric acid as dispersant, adopt
With the pH value of inorganic acid regulation water 5.0~6.0.
7. the preparation method of composite conductive powder according to claim 1, it is characterized in that：In step 1) and step 4), silicon
Hydrochlorate is at least one of sodium silicate solution, potassium silicate solution, and the silicate solution concentration is with SiO2Be calculated as 100g/L~
200g/L；Silicate solutions addition is with SiO in silicate solutions in step 4)2Account for TiO2Weight is calculated as 3%~5%.
8. the preparation method of composite conductive powder according to claim 1, it is characterized in that：In step 4), the aluminium salt is
At least one of aluminum sulfate, aluminium chloride, aluminum nitrate solution, solution concentration is with Al2O3It is calculated as 80g/L~100g/L.
9. the preparation method of composite conductive powder according to claim 1, it is characterized in that：Dispersant is used as using silicate
When, slurry pH controls are 4.5~9.5 during coating；Use polyacrylate, polycarboxylate, sodium dodecyl sulfate solution
During as dispersant, slurry pH controls are 6.5~7.5 during coating；When using citric acid as dispersant, coating process
Middle slurry pH controls are 5.5~6.5.
10. the preparation method of composite conductive powder according to claim 1, it is characterized in that：In step 2) at the beginning of titanium dioxide
Product are produced using sulfuric acid process or chloridising.
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| CN109266048A (en) * | 2018-11-22 | 2019-01-25 | 中信钛业股份有限公司 | A kind of low viscosity, the preparation process of highly dispersible titanium dioxide slurry |
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