CN107245164A - A kind of preparation method of three-dimensional attapulgite mica based conductive composite material - Google Patents
A kind of preparation method of three-dimensional attapulgite mica based conductive composite material Download PDFInfo
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Abstract
The invention belongs to inorganic functional material technical field, it is related to rod sheets of conductive composite material and preparation method thereof, more particularly to a kind of preparation method of three-dimensional attapulgite mica based conductive composite material.Rapidly fully infiltrated between the brilliant beam of attapulgite rod and mica splittings aggregation under certain temperature, condition of high voltage using supercritical carbon dioxide；Then void effect and shock effect are formed in cooling and rapid release simultaneously by the brilliant beam of attapulgite rod and mica splittings fater disintegration into attapulgite monocrystalline and mica monolithic layer, again using the brilliant and two-dimentional mica monolithic of the single rod of the attapulgite after dissociation as the standby rod sheets of conductive composite of nuclear regime, three-dimensional staggered spacial framework is formed in the coating, assigns the more excellent electric conductivity of coating and mechanical property.
Description
Technical field
The invention belongs to inorganic functional material technical field, it is related to rod-sheets of conductive composite material and preparation method thereof, especially relates to
And a kind of preparation method of three-dimensional attapulgite-mica based conductive composite material.
Background technology
High polymer material generally existing accumulation of static electricity phenomenon, the accident such as fire hazardous, blast.At present, mainly by
Conductive powder body is added in high polymer material to solve this problem.The conventional conductive powder body of in the market is mostly spherical, with addition
Amount is big, easily causes precipitation, influence matrix resin mechanical property etc., therefore, fibrous (one-dimensional) or sheet (two dimension) structure of exploitation
Conductive material turn into its development trend.
Attapulgite and mica are the natural minerals with a peacekeeping two-dimensional structure respectively, can be used for synthesis conductive
The nucleome material of material, for other artificial synthesized nucleome materials, has the advantages that rich reserves, cheap.
Exist mostly with nest like or bavin pile shape aggregate form however, natural attapulgite rod is brilliant, as restriction attapulgite industry
Or even the key technology bottleneck of fibrous conductive material industry development；Natural mica piece then exists in the form of lamella aggregation.
For that purpose it is necessary to carry out abundant depolymerization to obtain attapulgite list to the brilliant beam of attapulgite rod and mica splittings aggregation
Root rod crystalline substance and mica monolithic layer, just with actual application value.It is general using to roller, the mechanical treatment mode such as mill to concave convex rod
Stone rod crystalline substance beam and mica splittings aggregation carry out depolymerization, however, Mechanical Method can only be dissociated partly, while can also damage attapulgite
Rod crystalline substance and mica sheet crystal, cause its crystalline size not of uniform size, so as to greatly affected attapulgite and mica as core
The application performance of body material；And attapulgite and mica sheet compound tense, both are often mechanical mixture, it is impossible to effectively mutually support
And form three-dimensional net structure.
The content of the invention
The problem of in the presence of background technology, the invention provides a kind of three-dimensional attapulgite-mica-based conduction is multiple
The preparation method of condensation material, concrete operations are：
(1) dissociation (depolymerization) of the brilliant beam of attapulgite rod and mica splittings aggregation
In closed container, supercritical carbon dioxide is injected into the mixing of natural attapulgite powder and flaky mica powder
In powder, regulation enclosed system pressure is that 8.0~15.0MPa, temperature are 35~60 DEG C and kept, and rapid exhaust is interior at 1-2 second
It is decompressed to after normal pressure, that is, the attapulgite single rod crystalline substance and mica monolithic mixture of dissociation is made, acid solution is added thereto, is stirred
Fully obtained brilliant and mica monolithic the acid dispersion of attapulgite single rod is mixed, to the acidic dispersion of gained under stirring
In liquid add soluble silicate solution to system pH be 2~4 after, filtering, washing filter cake simultaneously calcine, that is, be made concave convex rod
Stone-mica/silica composite,
Wherein, natural attapulgite powder and flaky mica powder mass ratio are 0.5~2.0:1, supercritical carbon dioxide
The ratio between weight and mixed powder gross mass are 0.3:1~1.0:1,
It is 30~60 minutes to adjust the retention time after enclosed system pressure, temperature,
The mass percentage concentration of solute acid is 5%~15% in acid solution,
Brilliant and mica monolithic mixture and acid solution the mass ratio of the attapulgite single rod of dissociation is 0.05~0.20：
1,
In the solution of soluble silicate, silicate mass percentage concentration is 10%~20%,
Filter cake is washed after filtering to the μ S/cm of electrical conductivity≤100 of cleaning solution,
After washing, filter cake is calcined 2~6 hours under the conditions of 300~550 DEG C；
(2) preparation of tin antimonic salt acidic mixed solution
Stannic chloride pentahydrate (SnCl is added in hydrochloric acid solution4·5H2O), trichloride antimony (SbCl3), stir complete to solid
Portion dissolves, and tin antimonic salt acidic mixed solution is made；
Wherein, the molar concentration of hydrochloric acid solution is 1.0~4.0mol/L,
In mixed solution, pink salt concentration is 0.2~0.8g/mL (with SnCl4·5H2O is counted), the mass ratio of pink salt and antimonic salt
For 3~8:1；
(3) preparation of attapulgite-mica base conductive material
Attapulgite-mica/the silica composite obtained in step (1) is scattered in deionized water, heating state
It is lower to stir while being added dropwise after the tin antimonic salt acidic mixed solution and alkaline solution obtained in step (2), completion of dropping, continuation
Insulation reaction, filtering, Washing of Filter Cake, drying, calcining obtain attapulgite-mica based conductive composite material,
Heating-up temperature is 50~80 DEG C, and alkaline solution is ammoniacal liquor, sodium hydroxide solution or potassium hydroxide solution, molar concentration
For 1.0~4.0 mol/Ls,
When tin antimonic salt acidic mixed solution and alkaline solution is added dropwise, it is 0.5~5.0 to keep system pH,
SnCl4·5H2O is 0.3~1.0 with attapulgite-mica/silica composite mass ratio:1,
The insulation reaction time is 0.5~1 hour,
Washing of Filter Cake to the μ S/cm of cleaning solution electrical conductivity≤100,
After washing, filter cake is dried 6~12 hours at 60~90 DEG C,
Calcination operation is to be calcined 1~3 hour under conditions of 450~650 DEG C.
The beneficial effects of the present invention are：
The present invention is using supercritical carbon dioxide under certain temperature, condition of high voltage, and supercritical carbon dioxide can be quick
Ground is fully infiltrated between the brilliant beam of attapulgite rod and mica splittings aggregation；Then in rapid release, attapulgite rod crystalline substance beam
Supercritical carbon dioxide meeting rapid expansion between mica splittings, the void effect and shock effect formed during being somebody's turn to do can be simultaneously
By the brilliant beam of attapulgite rod with mica splittings fater disintegration into attapulgite monocrystalline and mica monolithic layer, so as to effectively realize two
The lossless dissociation of natural clay is planted, the technique has the advantages that dissociation efficiency is high, easy to operate, recyclable, nontoxic and with low cost；
The present invention is brilliant to attapulgite single rod and mica monolithic carries out the surface treatment of bag inorganic silicon and high-temperature heat treatment, and this has
Beneficial to conductive layer is improved in attapulgite and the adhesive force and filming performance of mica core surface, so as to greatly improve concave convex rod
The electric conductivity of stone-mica based composites；
The present invention is compound using the brilliant and two-dimentional mica monolithic of the single rod of one-dimensional attapulgite as the standby rod-sheets of conductive of nuclear regime
Material, effectively can mutually overlap, support and form three-dimensional staggered spacial framework in the coating, have one-dimensional electric concurrently concavo-convex
The advantage of rod stone and two-dimentional Conductive mica, compared with single conductive filler, can be greatly decreased conductive filler consumption, and can
Collaboration conduction and enhancing-toughening effect are played, the more excellent electric conductivity of coating and mechanical property is assigned.
Brief description of the drawings
Fig. 1 is electric for the scanning of three-dimensional attapulgite-mica based conductive composite material obtained by the embodiment 4 in the present invention
Mirror photo.
Embodiment
Embodiment 1
(1) in closed container, 0.45 kilogram of supercritical carbon dioxide is injected into 0.5 kilogram of natural attapulgite powder
In the mixed powder of 1.0 kilograms of flaky mica powders, regulation enclosed system pressure is that 15.0MPa, temperature are 35 DEG C and keep 30
After minute, rapid exhaust is decompressed to the normal pressure used time 1 second, that is, the attapulgite single rod crystalline substance and mica monolithic mixture of dissociation is made,
The hydrochloric acid solution that 7.5 kilogram-mass percentage concentrations are 5%, the fully obtained attapulgite single rod crystalline substance of stirring and mica are added thereto
The acid dispersion of monolithic, is added dropwise the silicon that mass percentage concentration is 10% under stirring into the acid dispersion of gained
Acid sodium solution to system pH is filtering after 4, and the electrical conductivity of washing filter cake to cleaning solution is 100 μ S/cm and in 300 DEG C of conditions
Lower calcining 6 hours, that is, be made attapulgite-mica/silica composite；
(2) 0.4 kilogram of stannic chloride pentahydrate is added in 2.0 liters of molar concentrations is the hydrochloric acid solutions of 1.0 mol/Ls
(SnCl4·5H2O), 0.08 kilogram of trichloride antimony (SbCl3), stirring to solid is all dissolved, and tin antimonic salt acidic mixed is made molten
Liquid；
(3) by the attapulgite-mica/silica composite obtained in 1.0 kilograms of steps (1) be scattered in 5 kilograms go from
In sub- water, be heated to 50 DEG C stir while be added dropwise the tin antimonic salt acidic mixed solution that is obtained in 1.5 liters of steps (2) and mole
Concentration is the ammonia spirit of 4.0 mol/Ls and keeps system pH to be 5.0, after completion of dropping, continues insulation reaction 1 hour, mistake
Filter, the electrical conductivity of washing filter cake to cleaning solution is calcined for 100 μ S/cm and after 60 DEG C are dried 12 hours under the conditions of 650 DEG C
1 hour, obtain three-dimensional attapulgite-mica based conductive composite material.
Embodiment 2
(1) in closed container, 1.5 kilograms of supercritical carbon dioxides are injected into 1.0 kilograms of natural attapulgite powders
In the mixed powder of 0.5 kilogram of flaky mica powder, regulation enclosed system pressure is that 8.0MPa, temperature are 55 DEG C and are kept for 60 points
Zhong Hou, rapid exhaust, is decompressed to the normal pressure used time 2 seconds, that is, the attapulgite single rod crystalline substance and mica monolithic mixture of dissociation is made, to
Wherein add the salpeter solution that 30 kilogram-mass percentage concentrations are 15%, the fully obtained attapulgite single rod crystalline substance of stirring and mica list
The acid dispersion of piece, is added dropwise the silicic acid that mass percentage concentration is 20% under stirring into the acid dispersion of gained
Sodium solution to system pH is filtering after 2, and the electrical conductivity of washing filter cake to cleaning solution is 90 μ S/cm and forges under the conditions of 550 DEG C
Burn 2 hours, that is, attapulgite-mica/silica composite is made；
(2) 1.2 kilograms of stannic chloride pentahydrates are added in 1.5 liters of molar concentrations is the hydrochloric acid solutions of 4.0 mol/Ls
(SnCl4·5H2O), 0.06 kilogram of trichloride antimony (SbCl3), stirring to solid is all dissolved, and tin antimonic salt acidic mixed is made molten
Liquid；
(3) by the attapulgite-mica/silica composite obtained in 1.0 kilograms of steps (1) be scattered in 20 kilograms go from
In sub- water, it is heated to 80 DEG C and stirs while the tin antimonic salt acidic mixed solution obtained in 1.25 liters of steps (2) is added dropwise and rubs
You are the potassium hydroxide solution of 1.0 mol/Ls and keep system pH to be 0.5 concentration, after completion of dropping, continue insulation reaction
0.5 hour, filtering, the electrical conductivity of washing filter cake to cleaning solution is for 90 μ S/cm and after 90 DEG C are dried 6 hours, then at 450 DEG C of bars
Calcined 3 hours under part, obtain three-dimensional attapulgite-mica based conductive composite material.
Embodiment 3
(1) in closed container, 1.5 kilograms of supercritical carbon dioxides are injected into 1.5 kilograms of natural attapulgite powders
In the mixed powder of 1.0 kilograms of flaky mica powders, regulation enclosed system pressure is that 11.5MPa, temperature are 47.5 DEG C and kept
After 45 minutes, rapid exhaust is decompressed to the normal pressure used time 1.5 seconds, that is, the attapulgite single rod crystalline substance and mica monolithic that dissociation is made are mixed
Compound, adds the sulfuric acid solution that 20 kilogram-mass percentage concentrations are 10% thereto, and the fully obtained attapulgite single rod of stirring is brilliant
With the acid dispersion of mica monolithic, into the acid dispersion of gained, dropwise addition mass percentage concentration is under stirring
15% sodium silicate solution to system pH is filtering after 3, and the electrical conductivity of washing filter cake to cleaning solution is 95 μ S/cm and in 425
Calcined under the conditions of DEG C 4 hours, that is, attapulgite-mica/silica composite is made；
(2) 1.0 kilograms of stannic chloride pentahydrates are added in 2.0 liters of molar concentrations is the hydrochloric acid solutions of 2.0 mol/Ls
(SnCl4·5H2O), 0.08 kilogram of trichloride antimony (SbCl3), stirring to solid is all dissolved, and tin antimonic salt acidic mixed is made molten
Liquid；
(3) by the attapulgite-mica/silica composite obtained in 1.0 kilograms of steps (1) be scattered in 10 kilograms go from
In sub- water, be heated to 65 DEG C stir while be added dropwise the tin antimonic salt acidic mixed solution that is obtained in 1.4 liters of steps (2) and mole
Concentration is the sodium hydroxide solution of 3.0 mol/Ls and keeps system pH to be 2.7, after completion of dropping, continues insulation reaction 0.7
Hour, filtering, the electrical conductivity of washing filter cake to cleaning solution is for 95 μ S/cm and after 70 DEG C are dried 9 hours, then at 500 DEG C of conditions
Lower calcining 2.5 hours, obtains three-dimensional attapulgite-mica based conductive composite material.
Embodiment 4
(1) in closed container, 1.6 kilograms of supercritical carbon dioxides are injected into 1.0 kilograms of natural attapulgite powders
In the mixed powder of 1.0 kilograms of flaky mica powders, regulation enclosed system pressure is that 13MPa, temperature are 55 DEG C and are kept for 60 points
Zhong Hou, rapid exhaust, is decompressed to the normal pressure used time 1 second, that is, the attapulgite single rod crystalline substance and mica monolithic mixture of dissociation is made, to
Wherein add the hydrochloric acid solution that 20 kilogram-mass percentage concentrations are 12%, the fully obtained attapulgite single rod crystalline substance of stirring and mica list
The acid dispersion of piece, is added dropwise the silicic acid that mass percentage concentration is 15% under stirring into the acid dispersion of gained
Sodium solution to system pH is filtering after 4, and the electrical conductivity of washing filter cake to cleaning solution is 98 μ S/cm and forges under the conditions of 500 DEG C
Burn 3 hours, that is, attapulgite-mica/silica composite is made；
(2) 0.9 kilogram of stannic chloride pentahydrate is added in 1.5 liters of molar concentrations is the hydrochloric acid solutions of 3.0 mol/Ls
(SnCl4·5H2O), 0.06 kilogram of trichloride antimony (SbCl3), stirring to solid is all dissolved, and tin antimonic salt acidic mixed is made molten
Liquid；
(3) by the attapulgite-mica/silica composite obtained in 1.0 kilograms of steps (1) be scattered in 8 kilograms go from
In sub- water, be heated to 75 DEG C stir while be added dropwise the tin antimonic salt acidic mixed solution that is obtained in 1.1 liters of steps (2) and mole
Concentration is the sodium hydroxide solution of 2.0 mol/Ls and keeps system pH to be 3.0, after completion of dropping, continues insulation reaction 0.8
Hour, filtering, the electrical conductivity of washing filter cake to cleaning solution is for 98 μ S/cm and after 85 DEG C are dried 8 hours, then at 550 DEG C of conditions
Lower calcining 2 hours, obtains three-dimensional attapulgite-mica based conductive composite material.
Comparative example 1
By in the step of embodiment 4 (1) injection supercritical carbon dioxide process delete, other operation with the phase of embodiment 4
Together：
(1) in closed container, to 1.0 kilograms of natural attapulgite powders and the mixed powder of 1.0 kilograms of flaky mica powders
The hydrochloric acid solution that 20 kilogram-mass percentage concentrations are 12%, the fully obtained acid dispersion of stirring, then at stirring shape are added in body
It is mistake after 4 that sodium silicate solution to the system pH that mass percentage concentration is 15%, which is added dropwise, into the acid dispersion of gained under state
Filter, the electrical conductivity of washing filter cake to cleaning solution is calcined 3 hours for 98 μ S/cm and under the conditions of 500 DEG C, i.e., and obtained attapulgite-
Mica/silica composite；
(2) be the same as Example 4；
(3) be the same as Example 4.
Comparative example 2
By in the step of embodiment 4 (1) bag inorganic silicon surface treatment and high-temperature heat treatment process delete, other operation with
Embodiment 4 is identical：
(1) in closed container, 1.6 kilograms of supercritical carbon dioxides are injected into 1.0 kilograms of natural attapulgite powders
In the mixed powder of 1.0 kilograms of flaky mica powders, regulation enclosed system pressure is that 13MPa, temperature are 55 DEG C and are kept for 60 points
Zhong Hou, rapid exhaust, is decompressed to the normal pressure used time 1 second, that is, the attapulgite single rod crystalline substance and mica monolithic mixture of dissociation is made；
(2) be the same as Example 4；
(3) the attapulgite single rod crystalline substance and mica monolithic mixture of the dissociation obtained in 1.0 kilograms of steps (1) are scattered in
In 8 kilograms of deionized waters, it is heated to 75 DEG C and stirs while the tin antimonic salt acidic mixed obtained in 1.1 liters of steps (2) is added dropwise
Solution and molar concentration are the sodium hydroxide solution of 2.0 mol/Ls and keep system pH to be 3.0, after completion of dropping, continue to protect
Temperature reaction 0.8 hour, filtering, the electrical conductivity of washing filter cake to cleaning solution is 98 μ S/cm and after 85 DEG C are dried 8 hours, then at
Calcined 2 hours under the conditions of 550 DEG C, obtain attapulgite-mica based conductive composite material..
Comparative example 3
Remove mica nucleome material, using pure natural Concave-convex clay rod powder as nucleome, other operation with the phase of embodiment 4
Together：
(1) in closed container, 1.6 kilograms of supercritical carbon dioxides are injected into 2.0 kilograms of natural attapulgite powders
In, regulation enclosed system pressure is that 13MPa, temperature are 55 DEG C and after being kept for 60 minutes, and rapid exhaust is decompressed to the normal pressure used time 1
Second, that is, the attapulgite single rod that dissociation is made is brilliant, and the hydrochloric acid solution that 20 kilogram-mass percentage concentrations are 12% is added thereto, is stirred
The brilliant acid dispersion of fully obtained attapulgite single rod is mixed, matter is added dropwise into the acid dispersion of gained under stirring
Sodium silicate solution to the system pH that amount percentage concentration is 15% is filtering after 4, and the electrical conductivity of washing filter cake to cleaning solution is 98
μ S/cm are simultaneously calcined 3 hours under the conditions of 500 DEG C, that is, attapulgite/silica composite is made；
(2) be the same as Example 4；
(3) attapulgite/silica composite obtained in 1.0 kilograms of steps (1) is scattered in 8 kilograms of deionized waters
In, it is heated to 75 DEG C and stirs while the tin antimonic salt acidic mixed solution obtained in 1.1 liters of steps (2) and molar concentration is added dropwise
Sodium hydroxide solution for 2.0 mol/Ls simultaneously keeps system pH to be 3.0, after completion of dropping, continues insulation reaction 0.8 hour,
Filtering, the electrical conductivity of washing filter cake to cleaning solution is calcined for 98 μ S/cm and after 85 DEG C are dried 8 hours under the conditions of 550 DEG C
2 hours, obtain attapulgite based conductive composite material.
Comparative example 4
Remove attapulgite nucleome material, using pure mica powder as nucleome, other operations are same as Example 4：
(1) in closed container, 1.6 kilograms of supercritical carbon dioxides are injected into 2.0 kilograms of flaky mica powders, adjusted
Enclosed system pressure is that 13MPa, temperature are 55 DEG C and after being kept for 60 minutes, and rapid exhaust is decompressed to the normal pressure used time 1 second, that is, made
Mica monolithic is obtained, the hydrochloric acid solution that 20 kilogram-mass percentage concentrations are 12%, the fully obtained mica monolithic of stirring are added thereto
Acid dispersion, under stirring into the acid dispersion of gained be added dropwise mass percentage concentration be 15% sodium metasilicate
Solution to system pH be 4 after, filtering, washing filter cake to cleaning solution electrical conductivity for 98 μ S/cm and under the conditions of 500 DEG C calcine
3 hours, that is, mica/silica composite is made；
(2) 0.9 kilogram of stannic chloride pentahydrate is added in 1.5 liters of molar concentrations is the hydrochloric acid solutions of 3.0 mol/Ls
(SnCl4·5H2O), 0.06 kilogram of trichloride antimony (SbCl3), stirring to solid is all dissolved, and tin antimonic salt acidic mixed is made molten
Liquid；
(3) mica/silica composite obtained in 1.0 kilograms of steps (1) is scattered in 8 kilograms of deionized waters, plus
Heat is stirred to 75 DEG C while it is 2.0 that the tin antimonic salt acidic mixed solution obtained in 1.1 liters of steps (2) and molar concentration, which is added dropwise,
The sodium hydroxide solution of mol/L simultaneously keeps system pH to be 3.0, after completion of dropping, continues insulation reaction 0.8 hour, filtering,
Filter cake is washed to the electrical conductivity of cleaning solution for 98 μ S/cm and after 85 DEG C are dried 8 hours, calcining 2 is small under the conditions of 550 DEG C
When, obtain mica based conductive composite material.
Comparative example 5
Attapulgite based conductive composite material and 1.0 kilograms of contrasts obtained by taking in 1.0 kilograms of comparative examples 3 are implemented
Obtained mica based conductive composite material in example 4, both mechanical mixtures are uniform, that is, obtain attapulgite base and mica-based is mixed
Close conductive material.
The performance evaluation of conductive material in primers
The preparation of conductive coating：First, take various embodiments above and prepared by comparing embodiment conducing composite material (
On the premise of sheet resistance is equal, the mass percent that conducing composite material accounts for all components is as shown in table 1) be added to mixing it is molten
In agent (20 grams of butyl acetates and 20 grams of toluene Mixed Solvents), stirring, ultrasonic disperse 30 minutes；Then the dispersion liquid of gained is added
Enter into 30 grams of thermoplastic acrylic resins (trade mark HypomerAC-7435), add dispersant B YK-163 (0.5wt%), breast
Change and disperse 30 minutes, that is, be configured to conductive composite coating.
Each coating obtained above is evenly applied to after ABS plastic sheet material and polishing using bar spreader (80 mesh)
On tinplate, (solidification) 24 hours is dried at room temperature, that is, conductive composite paint film is made.Surveyed using the probe resistance rate of RTS-9 types four
Try the coating surface resistance on instrument measure ABS plastic sheet material；Paint film mechanic property test method on tinplate is as follows：Using
GB/T1732-1993《Paint film impact resistance assay method》Bioassay standard, weight quality is 1kg, not cause paint film destruction most
Highly represent greatly, unit is kgcm, determine the impact resistance of different paint films.Specific testing result is as shown in table 1.
Table 1
| Consumption/% | Sheet resistance/M Ω | Impact strength/kgcm | |
| Embodiment 1 | 14 | 1 | 41 |
| Embodiment 2 | 12 | 1 | 44 |
| Embodiment 3 | 13 | 1 | 43 |
| Embodiment 4 | 11 | 1 | 46 |
| Comparative example 1 | 20 | 1 | 37 |
| Comparative example 2 | 24 | 1 | 40 |
| Comparative example 3 | 32 | 1 | 30 |
| Comparative example 4 | 30 | 1 | 25 |
| Comparative example 5 | 28 | 1 | 35 |
Claims (8)
1. a kind of preparation method of three-dimensional attapulgite-mica based conductive composite material, it is characterised in that：The preparation method
For,
(1) in closed container, supercritical carbon dioxide is injected into the mixing of natural attapulgite powder and flaky mica powder
In powder, regulation enclosed system pressure is that 8.0~15.0MPa, temperature are 35~60 DEG C and kept, rapid exhaust decompression to normal pressure
Afterwards, that is, the attapulgite single rod crystalline substance and mica monolithic mixture of dissociation is made, acid solution is added thereto, stirring is fully made
Brilliant and mica monolithic the acid dispersion of attapulgite single rod, being added under stirring into the acid dispersion of gained can
The solution of soluble silicate to system pH be 2~4 after, filtering, washing filter cake simultaneously calcine, that is, be made attapulgite-mica/oxygen
SiClx compound；
(2) preparation of tin antimonic salt acidic mixed solution
Stannic chloride pentahydrate, trichloride antimony are added in hydrochloric acid solution, stirring to solid is all dissolved, tin antimonic salt acidity is made mixed
Close solution；
(3) preparation of attapulgite-mica base conductive material
Attapulgite-mica/the silica composite obtained in step (1) is scattered in deionized water, heating state is next
Side is stirred while being added dropwise after the tin antimonic salt acidic mixed solution and alkaline solution obtained in step (2), completion of dropping, and continuation is incubated
Reaction, filtering, Washing of Filter Cake, drying, calcining obtain attapulgite-mica based conductive composite material.
2. the preparation method of conducing composite material as claimed in claim 1, it is characterised in that：In step (1), natural concave convex rod
Stone flour body and flaky mica powder mass ratio are 0.5~2.0:1, the ratio between supercritical carbon dioxide weight and mixed powder gross mass
For 0.3:1~1.0:1.
3. the preparation method of conducing composite material as claimed in claim 1, it is characterised in that：In step (1), obturator is adjusted
Be retention time after pressure, temperature be 30~60 minutes.
4. the preparation method of conducing composite material as claimed in claim 1, it is characterised in that：Mixed solution in step (2)
In, pink salt concentration is 0.2~0.8g/mL, and the mass ratio of pink salt and antimonic salt is 3~8:1.
5. the preparation method of conducing composite material as claimed in claim 1, it is characterised in that：In step (3), heating-up temperature is
50~80 DEG C.
6. the preparation method of conducing composite material as claimed in claim 1, it is characterised in that：In step (3), tin antimonic salt is added dropwise
During acidic mixed solution, it is 0.5~5.0 to keep system pH.
7. the preparation method of conducing composite material as claimed in claim 1, it is characterised in that：In step (3), five water four are controlled
Stannic chloride is 0.3~1.0 with attapulgite-mica/silica composite mass ratio:1.
8. the preparation method of conducing composite material as claimed in claim 1, it is characterised in that：In step (3), calcination operation
To be calcined 1~3 hour under conditions of 450~650 DEG C.
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| CN110655635A (en) * | 2019-09-09 | 2020-01-07 | 浙江凯色丽科技发展有限公司 | Polyurethane composite emulsion containing mica-based conductive material and preparation method thereof |
| CN113517089A (en) * | 2021-04-07 | 2021-10-19 | 浙江凯色丽科技发展有限公司 | Light-colored three-dimensional conductive powder for powder coating and preparation method thereof |
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| CN113517089A (en) * | 2021-04-07 | 2021-10-19 | 浙江凯色丽科技发展有限公司 | Light-colored three-dimensional conductive powder for powder coating and preparation method thereof |
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