CN107337807A - A kind of preparation method of attapulgite mica based conductive composite material - Google Patents
A kind of preparation method of attapulgite mica based conductive composite material Download PDFInfo
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- CN107337807A CN107337807A CN201710578228.2A CN201710578228A CN107337807A CN 107337807 A CN107337807 A CN 107337807A CN 201710578228 A CN201710578228 A CN 201710578228A CN 107337807 A CN107337807 A CN 107337807A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/02—Polyamines
- C08G73/026—Wholly aromatic polyamines
- C08G73/0266—Polyanilines or derivatives thereof
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/10—Silicon-containing compounds
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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
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/24—Electrically-conducting paints
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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Abstract
The invention belongs to inorganic functional material technical field, is related to rod sheets of conductive composite material and preparation method thereof, more particularly to a kind of preparation method of attapulgite mica based conductive composite material.Natural attapulgite, flaky mica powder, aniline monomer are added in acid solution, and vacuumizes and keeps vacuum state, continues to pressurize after finally recovering system to standard atmospheric pressure；Oxidizing agent solution is added dropwise under stirring and carries out oxidative polymerization, rod sheet three-dimensional attapulgite mica/polyaniline composite material is made.
Description
Technical field
The invention belongs to inorganic functional material technical field, is related to rod-sheets of conductive composite material and preparation method thereof, especially relates to
A kind of and preparation method of attapulgite-mica based conductive composite material.
Background technology
At present, the application of engineering plastics component all uses serialization electrostatic painting process.But due to these engineering plastic materials and parts
For insulator, it is impossible to conduct electrostatic charge caused by electrostatic spraying in time, can not directly carry out serialization electrostatic spraying
Operation.Therefore, the effective ways for assigning plastic member electric conductivity are to be coated with one layer of conductive primer on plastic member surface to be formed
Conductive layer.Now, the conductive primer used is typically that conductive material is added in insulating polymer (film-forming resin), makes its solidification
The conductive energy of coating after film forming.
Conductive mica is a kind of typical two-dimensional sheet conductive material and is used in electrically-conducting paint, but its shortcoming is to add
Dosage is relatively large, so as to have impact on the mechanical property of priming paint.To find out its cause, mainly there are two aspects：1. for Conductive mica
Nucleome material mica splittings depolymerization is not complete enough；2. sheets of conductive mica in the coating fails to form three-dimensional crosslinking structure.
The inorganic light-colored conductive material of threadiness has the advantages that dosage is relatively fewer and reinforcing property is good and enjoys favor.So
And the nucleome of fibrous inorganic light-colored conductive material in the market is mostly artificial synthesized, as micron order acicular titanium dioxide,
Potassium titanate crystal whisker etc., its manufacturing process route is complicated, and production cost is higher.Therefore, how to reduce conductive filler dosage, reduce life
Cost is produced, while it is the key issue for being badly in need of solving to improve coating mechanical property.
Attapulgite is a kind of rich magnesium silicate clay pit species native crystal with bar-shaped or fibrous microscopic appearance
Nucleome material, but natural attapulgite rod crystalline substance exists with nest like or bavin pile shape aggregate form mostly, and it is concavo-convex to turn into restriction
Rod stone industry or even the key technology bottleneck of fibrous conductive material industry development；And with sheets of conductive mica powder compound tense,
Both are often mechanical mixture, it is impossible to effectively mutually support and form three-dimensional net structure, so as to can not effectively reduce filler phase
To dosage.
The content of the invention
It is brilliant in attapulgite rod the invention provides a kind of preparation method of attapulgite-mica based conductive composite material
While beam and mica splittings aggregate disintegration, rod-sheet three-dimensional conductive composite is made in a step, and concrete operations are：
(1) natural attapulgite and flaky mica powder are added in acid solution, after fully dispersed, into gained dispersion liquid
Aniline monomer is added, the composite suspension liquid containing aniline salt is obtained, then gained suspension is vacuumized and keeps vacuum state,
Continue to pressurize after finally recovering system to standard atmospheric pressure,
Wherein, natural attapulgite and flaky mica powder mass ratio are 0.5~2:1, natural attapulgite, sheet mica
The gross mass of powder is 0.02~0.1 with acid solution mass ratio:1, aniline weight and natural attapulgite, flaky mica powder it is total
Mass ratio is 0.3~1:1,
Acid solution is hydrochloric acid solution or sulfuric acid solution, and molar concentration is 2.0~5.0 mol/Ls,
Vacuum is evacuated to as -0.1~-0.05MPa and is kept for 30~60 minutes；
After recovery system to standard atmospheric pressure, continue to be forced into system pressure as 45~90 points of 0.1~0.5MPa and holding
Clock；
(2) under stirring, oxidizing agent solution progress oxidative polymerization is added dropwise into the system obtained by step (1),
Continue to stir 6-24 hours after being added dropwise, filtering, washing filter cake, drying, crushing, i.e., obtained rod-sheet three-dimensional attapulgite-
Mica/polyaniline composite material,
Wherein, oxidant is persulfate, bichromate, iodate, perchlorate, hydrogen peroxide or ferric trichloride,
Molar concentration in oxidizing agent solution is 1.0~4.0 mol/Ls,
Oxidant is 1.0~2.0 with aniline mol ratio:1.
The beneficial effects of the present invention are：
The present invention using decompression (vacuumizing) repressurization afterwards method, in synthetic rod-sheet three-dimensional attapulgite-mica-based
While conducing composite material, the soft chemical depolymerization (dissociation) of attapulgite rod crystalline substance beam and mica splittings aggregate is realized,
During vacuumizing, the air remained between attapulgite rod crystalline substance interfascicular and mica splittings can be discharged；Recover in system to marking
After quasi- atmospheric pressure again in pressurization, due to the effect of pressure difference inside and outside presence, the solution containing aniline salt can quickly penetrate into recessed
Between convex rod stone rod crystalline substance interfascicular and mica splittings, finally in the presence of oxidant, between attapulgite rod crystalline substance interfascicular and mica splittings
Aniline salt monomer oxidative polymerization occurs, a kind of flexible active force can be produced during this simultaneously by attapulgite rod crystalline substance beam
Attapulgite monocrystalline and mica monolithic layer are slowly disintegrated into mica splittings, not only realizes attapulgite rod crystalline substance beam and mica sheet
The lossless depolymerization of layer aggregate, and effectively can mutually overlap, support and form three-dimensional net structure；Meanwhile polymerisation shape
Into conductive film layer can uniformly be wrapped in attapulgite monocrystalline and mica monolithic layer surface, it is three-dimensional concavo-convex so as to which rod-sheet be made
Rod stone-mica based conductive composite material.
Brief description of the drawings
Fig. 1 is the scanning of rod-sheet three-dimensional attapulgite-mica/polyaniline composite material obtained by embodiment 4
Electromicroscopic photograph.
Embodiment
Embodiment 1
(1) by 1.0 kilograms of natural attapulgite powders and 2.0 kilograms of flaky mica powders be added to 150.0 kilograms moles it is dense
Spend in the hydrochloric acid solution for 2.0 mol/Ls, after fully dispersed, 0.9 kilogram of aniline monomer is added into gained dispersion liquid, is obtained
Composite suspension liquid containing aniline salt, vacuum is then evacuated to gained suspension as -0.05MPa and keeps the vacuum shape
State 50 minutes, system pressure is further added by 0.1MPa after finally recovering system to standard atmospheric pressure, and kept for 90 minutes；
(2) under stirring, 19.3 liters of molar concentrations are added dropwise into the system obtained by step (1) as 1.0 mol/Ls
Ammonium persulfate solution carries out oxidative polymerization, continues stirring 6 hours after being added dropwise, filtering, washs filter cake, drying, crushing,
Rod-sheet three-dimensional attapulgite-mica/polyaniline composite material is made.
Embodiment 2
(1) 2.0 kilograms of natural attapulgite powders and 1.0 kilograms of flaky mica powders are added to 30.0 kilograms of molar concentrations
In sulfuric acid solution for 5.0 mol/Ls, after fully dispersed, 3.0 kilograms of aniline monomers are added into gained dispersion liquid, are contained
There is the composite suspension liquid of aniline salt, vacuum is then evacuated to gained suspension as -0.1MPa and keeps the vacuum state
30 minutes, system pressure is further added by 0.5MPa after finally recovering system to standard atmospheric pressure, and kept for 45 minutes；
(2) under stirring, 8.1 liters of molar concentrations are added dropwise into the system obtained by step (1) as 4.0 mol/Ls
Liquor ferri trichloridi carries out oxidative polymerization, continues stirring 24 hours, filtering, washing filter cake, drying, powder after being added dropwise
It is broken, that is, rod-sheet three-dimensional attapulgite-mica/polyaniline composite material is made.
Embodiment 3
(1) 1.5 kilograms of natural attapulgite powders and 1.5 kilograms of flaky mica powders are added to 50.0 kilograms of molar concentrations
In hydrochloric acid solution for 4.0 mol/Ls, after fully dispersed, 1.95 kilograms of aniline monomers are added into gained dispersion liquid, are contained
There is the composite suspension liquid of aniline salt, vacuum is then evacuated to gained suspension as -0.08MPa and keeps the vacuum state
45 minutes, system pressure is further added by 0.3MPa after finally recovering system to standard atmospheric pressure, and kept for 67 minutes；
(2) under stirring, 15.7 liters of molar concentrations are added dropwise into the system obtained by step (1) as 2.0 mol/Ls
Potassium bichromate solution carries out oxidative polymerization, continues stirring 15 hours, filtering, washing filter cake, drying, powder after being added dropwise
It is broken, that is, rod-sheet three-dimensional attapulgite-mica/polyaniline composite material is made.
Embodiment 4
(1) by 1.3 kilograms of natural attapulgite powders and 1.7 kilograms of flaky mica powders be added to 100.0 kilograms moles it is dense
Spend in the hydrochloric acid solution for 3.5 mol/Ls, after fully dispersed, 3.0 kilograms of aniline monomers are added into gained dispersion liquid, are obtained
Composite suspension liquid containing aniline salt, vacuum is then evacuated to gained suspension as -0.06MPa and keeps the vacuum shape
State 60 minutes, system pressure is further added by 0.4MPa after finally recovering system to standard atmospheric pressure, and kept for 60 minutes；
(2) under stirring, 14.0 liters of molar concentrations are added dropwise into the system obtained by step (1) as 3.0 mol/Ls
Ammonium persulfate solution carries out oxidative polymerization, continues stirring 12 hours, filtering, washing filter cake, drying, powder after being added dropwise
It is broken, that is, rod-sheet three-dimensional attapulgite-mica/polyaniline composite material is made.
Comparative example 1
Flaky mica powder is replaced with natural attapulgite powder, other operations are same as Example 4, and specific steps are such as
Under：
(1) by 3 kilograms of natural attapulgite powders be added to 100.0 kilograms of molar concentrations be 3.5 mol/Ls hydrochloric acid it is molten
In liquid, after fully dispersed, 3.0 kilograms of aniline monomers are added into gained dispersion liquid, obtain the composite suspension liquid containing aniline salt,
Then vacuum is evacuated to gained suspension as -0.06MPa and keeps the vacuum state 60 minutes, finally recovers system extremely
System pressure is further added by after standard atmospheric pressure to 0.4MPa, and is kept for 60 minutes；
(2) under stirring, 14.0 liters of molar concentrations are added dropwise into the system obtained by step (1) as 3.0 mol/Ls
Ammonium persulfate solution carries out oxidative polymerization, continues stirring 12 hours, filtering, washing filter cake, drying, powder after being added dropwise
It is broken, that is, bar-shaped attapulgite/polyaniline composite material is made.
Comparative example 2
Natural attapulgite powder is replaced with flaky mica powder, other operations are same as Example 4, and specific steps are such as
Under：
(1) 3 kilograms of flaky mica powders are added in the hydrochloric acid solution that 100.0 kilograms of molar concentrations are 3.5 mol/Ls,
After fully dispersed, 3.0 kilograms of aniline monomers are added into gained dispersion liquid, obtain the composite suspension liquid containing aniline salt, then
Vacuum is evacuated to gained suspension as -0.06MPa and keeps the vacuum state 60 minutes, finally recovers system to standard
System pressure is further added by after atmospheric pressure to 0.4MPa, and is kept for 60 minutes；
(2) under stirring, 14.0 liters of molar concentrations are added dropwise into the system obtained by step (1) as 3.0 mol/Ls
Ammonium persulfate solution carries out oxidative polymerization, continues stirring 12 hours, filtering, washing filter cake, drying, powder after being added dropwise
It is broken, that is, sheet mica/polyaniline composite material is made.
Comparative example 3
The process that vacuumizes in embodiment 4 is removed, other operations are same as Example 4, comprise the following steps that：
(1) by 1.3 kilograms of natural attapulgite powders and 1.7 kilograms of flaky mica powders be added to 100.0 kilograms moles it is dense
Spend in the hydrochloric acid solution for 3.5 mol/Ls, after fully dispersed, 3.0 kilograms of aniline monomers are added into gained dispersion liquid, are obtained
Composite suspension liquid containing aniline salt；
(2) under stirring, 14.0 liters of molar concentrations are added dropwise into the system obtained by step (1) as 3.0 mol/Ls
Ammonium persulfate solution carries out oxidative polymerization, continues stirring 12 hours, filtering, washing filter cake, drying, powder after being added dropwise
It is broken, that is, rod-sheet attapulgite-mica/polyaniline composite material is made.
Comparative example 4
Take bar-shaped attapulgite/polyaniline composite material and 1.7 thousand obtained in 1.3 kilograms of comparative examples 1
Obtained sheet mica/polyaniline composite material in gram comparative example 2, will both mechanical mixtures it is uniform, that is, obtain
Rod-sheet attapulgite/polyaniline and mica/polyaniline mixing 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.
After each coating obtained above is evenly applied into 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 1kg, not cause paint film to destroy most
Highly represent greatly, unit kgcm, determine the impact resistance of different paint films.Specific testing result is as shown in table 1.
Table 1
| Dosage/% | Coating surface resistance/M Ω | Impact strength/kgcm | |
| Embodiment 1 | 18 | 1 | 40 |
| Embodiment 2 | 16 | 1 | 43 |
| Embodiment 3 | 17 | 1 | 42 |
| Embodiment 4 | 15 | 1 | 45 |
| Comparative example 1 | 28 | 1 | 35 |
| Comparative example 2 | 30 | 1 | 25 |
| Comparative example 3 | 25 | 1 | 38 |
| Comparative example 4 | 23 | 1 | 40 |
Claims (8)
- A kind of 1. preparation method of attapulgite-mica based conductive composite material, it is characterised in that：Described method is,(1) natural attapulgite and flaky mica powder are added in acid solution, after fully dispersed, added into gained dispersion liquid Aniline monomer, the composite suspension liquid containing aniline salt is obtained, then gained suspension is vacuumized and keeps vacuum state, finally Continue to pressurize after recovery system to standard atmospheric pressure；(2) under stirring, oxidizing agent solution is added dropwise into the system obtained by step (1) and carries out oxidative polymerization, dropwise addition After continue stir 6-24 hours, filtering, washing filter cake, drying, crushing, that is, be made rod-sheet three-dimensional attapulgite-cloud Mother/polyaniline composite material.
- 2. the preparation method of attapulgite as claimed in claim 1-mica based conductive composite material, it is characterised in that：Step (1) in, natural attapulgite and flaky mica powder mass ratio are 0.5~2:1.
- 3. the preparation method of attapulgite as claimed in claim 1-mica based conductive composite material, it is characterised in that：Step (1) in, natural attapulgite, the gross mass of flaky mica powder and acid solution mass ratio are 0.02~0.1:1.
- 4. the preparation method of attapulgite as claimed in claim 1-mica based conductive composite material, it is characterised in that：Step (1) in, aniline weight and natural attapulgite, the ratio between the gross mass of flaky mica powder are 0.3~1:1.
- 5. the preparation method of attapulgite as claimed in claim 1-mica based conductive composite material, it is characterised in that：Step (1) in, acid solution is hydrochloric acid solution or sulfuric acid solution, and molar concentration is 2.0~5.0 mol/Ls.
- 6. the preparation method of attapulgite as claimed in claim 1-mica based conductive composite material, it is characterised in that：Step (1) in, vacuum is evacuated to as -0.1~-0.05MPa and is kept for 30~60 minutes；After recovery system to standard atmospheric pressure, Continue to be forced into system pressure as 0.1~0.5MPa and kept for 45~90 minutes.
- 7. the preparation method of attapulgite as claimed in claim 1-mica based conductive composite material, it is characterised in that：Step (2) in, oxidant is persulfate, bichromate, iodate, perchlorate, hydrogen peroxide or ferric trichloride, in the oxidation Molar concentration in agent solution is 1.0~4.0 mol/Ls.
- 8. the preparation method of attapulgite as claimed in claim 1-mica based conductive composite material, it is characterised in that：Step (2) in, oxidant is 1.0~2.0 with aniline mol ratio:1.
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Cited By (6)
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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 |
| CN110961072A (en) * | 2019-12-23 | 2020-04-07 | 常州纳欧新材料科技有限公司 | CeO (CeO)2Titanium oxide/conductive potassium titanate composite lead adsorption material and preparation method thereof |
| CN110975856A (en) * | 2019-12-18 | 2020-04-10 | 常州纳欧新材料科技有限公司 | Titanium oxide/conductive potassium titanate composite desulfurization photocatalytic material and preparation method thereof |
| CN112980276A (en) * | 2021-04-16 | 2021-06-18 | 浙江凯色丽科技发展有限公司 | Attapulgite-mica-based conductive anticorrosive paint and preparation method thereof |
| CN113135744A (en) * | 2021-04-02 | 2021-07-20 | 浙江凯色丽科技发展有限公司 | Attapulgite/mica/carbon composite 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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| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
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| CN110975856B (en) * | 2019-12-18 | 2023-01-03 | 常州纳欧新材料科技有限公司 | Titanium oxide/conductive potassium titanate composite desulfurization photocatalytic material and preparation method thereof |
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| CN110961072B (en) * | 2019-12-23 | 2022-04-05 | 常州纳欧新材料科技有限公司 | CeO (CeO)2Titanium oxide/conductive potassium titanate composite lead adsorption material and preparation method thereof |
| CN113135744A (en) * | 2021-04-02 | 2021-07-20 | 浙江凯色丽科技发展有限公司 | Attapulgite/mica/carbon composite material and preparation method thereof |
| CN113135744B (en) * | 2021-04-02 | 2022-04-01 | 浙江凯色丽科技发展有限公司 | Attapulgite/mica/carbon composite 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 |
| CN112980276A (en) * | 2021-04-16 | 2021-06-18 | 浙江凯色丽科技发展有限公司 | Attapulgite-mica-based conductive anticorrosive paint and preparation method thereof |
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