CN108997561A - A kind of methylation conductive micro-balloons and preparation method thereof - Google Patents
A kind of methylation conductive micro-balloons and preparation method thereof Download PDFInfo
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- CN108997561A CN108997561A CN201810759893.6A CN201810759893A CN108997561A CN 108997561 A CN108997561 A CN 108997561A CN 201810759893 A CN201810759893 A CN 201810759893A CN 108997561 A CN108997561 A CN 108997561A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G61/00—Macromolecular compounds obtained by reactions forming a carbon-to-carbon link in the main chain of the macromolecule
- C08G61/12—Macromolecular compounds containing atoms other than carbon in the main chain of the macromolecule
- C08G61/122—Macromolecular compounds containing atoms other than carbon in the main chain of the macromolecule derived from five- or six-membered heterocyclic compounds, other than imides
- C08G61/123—Macromolecular compounds containing atoms other than carbon in the main chain of the macromolecule derived from five- or six-membered heterocyclic compounds, other than imides derived from five-membered heterocyclic compounds
- C08G61/126—Macromolecular compounds containing atoms other than carbon in the main chain of the macromolecule derived from five- or six-membered heterocyclic compounds, other than imides derived from five-membered heterocyclic compounds with a five-membered ring containing one sulfur atom in the ring
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/12—Powdering or granulating
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B5/00—Non-insulated conductors or conductive bodies characterised by their form
- H01B5/16—Non-insulated conductors or conductive bodies characterised by their form comprising conductive material in insulating or poorly conductive material, e.g. conductive rubber
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G2261/00—Macromolecular compounds obtained by reactions forming a carbon-to-carbon link in the main chain of the macromolecule
- C08G2261/10—Definition of the polymer structure
- C08G2261/11—Homopolymers
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G2261/00—Macromolecular compounds obtained by reactions forming a carbon-to-carbon link in the main chain of the macromolecule
- C08G2261/30—Monomer units or repeat units incorporating structural elements in the main chain
- C08G2261/32—Monomer units or repeat units incorporating structural elements in the main chain incorporating heteroaromatic structural elements in the main chain
- C08G2261/322—Monomer units or repeat units incorporating structural elements in the main chain incorporating heteroaromatic structural elements in the main chain non-condensed
- C08G2261/3223—Monomer units or repeat units incorporating structural elements in the main chain incorporating heteroaromatic structural elements in the main chain non-condensed containing one or more sulfur atoms as the only heteroatom, e.g. thiophene
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- C—CHEMISTRY; METALLURGY
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2365/00—Characterised by the use of macromolecular compounds obtained by reactions forming a carbon-to-carbon link in the main chain; Derivatives of such polymers
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Abstract
The invention discloses a kind of methylation conductive micro-balloons, it is composed of the following raw materials by weight: the formalin 20-30 of conductive colloidal sol 120-140, polysorbate 0.7-1, catalyst 0.1-0.3, zinc ricinate 1-2,10-13%, the present invention carries out methylation processing by formaldehyde, using triethylamine as catalyst, obtained conductive micro-balloons not only have good electric conductivity, and mechanical stability is strong, and comprehensive performance is superior.
Description
Technical field
The invention belongs to conductive material fields, and in particular to a kind of methylation conductive micro-balloons and preparation method thereof.
Background technique
Polythiophene can be used for organic solar batteries, chemical sensitisation, electroluminescent device etc..The derivative of polythiophene
PEDOT is important hole transport layer material in organic electroluminescence device preparation, polythiophene because its good optics, electricity and
Environmental stability, the attention by researcher；
Nano silica is a kind of inorganic chemical industry material, is commonly called as white carbon black, and due to being ultrafine nanometer, size range exists
1-100nm, therefore there are many unique properties, such as have to anti-ultraviolet optical property, it is anti-ageing other materials to be improved
Change, intensity and chemical-resistance.Purposes is very extensive.Nanometer grade silica is amorphous white powder, nontoxic, tasteless, nothing
Pollution, micro-structure is spherical shape, and in cotton-shaped and netted quasi- grain structure, molecular formula and structural formula are SiO2, not soluble in water；Nanometer
The purposes of silica point is very extensive, and for general weight of adding in 0.5-2%, individual product system can be to 10% or more.To production
The key that moral character can embody is: it is fully dispersed therefore, how to improve its surface-active in system, enhance point of its addition
Performance is dissipated, is the emphasis studied at present；
The object of the invention is to which nano silica is effectively compound with polythiophene, to assign composite material to lead
Electrical property, and guarantee that composite material has good surface strength and stability.
Summary of the invention
In view of the defects and deficiencies of the prior art, the present invention intends to provide a kind of methylation conductive micro-balloons and its systems
Preparation Method.
To achieve the above object, the invention adopts the following technical scheme:
A kind of methylation conductive micro-balloons, it is composed of the following raw materials by weight:
The first of conductive colloidal sol 120-140, polysorbate 0.7-1, catalyst 0.1-0.3, zinc ricinate 1-2,10-13%
Aldehyde aqueous solution 20-30.
The catalyst is triethylamine.
What the conductive colloidal sol was made of the raw material of following weight parts:
Ethyl orthosilicate 27-30, thiophene 110-130, ferric trichloride 3-4, ammonium polyphosphate 2-3, alkanolamide 1-2, tetrahydro
Furfuryl alcohol 0.7-1；
Preparation method, comprising the following steps:
(1) ammonium polyphosphate is taken, is added in the deionized water of 25-30 times of its weight, stirs evenly, alkanolamide is added,
Insulated and stirred 3-10 minutes at 50-60 DEG C, amide dispersion liquid is obtained；
(2) ferric trichloride is taken, is added in the deionized water of 17-20 times of its weight, stirs evenly；
(3) thiophene is taken, is added in above-mentioned amide dispersion liquid, stirs evenly, be sent in reaction kettle, be passed through nitrogen, is adjusted
10-15 DEG C of temperature of reaction kettle of section, is added above-mentioned ferric chloride aqueous solutions, is stirred to react 10-12 hours, discharges, positive silicic acid is added
Ethyl ester stirs 3-4 hours, filters, filter cake is washed, air drying, obtain conductive colloidal sol.
A kind of preparation method for the conductive micro-balloons that methylate, comprising the following steps:
(1) zinc ricinate is taken, is added in the dehydrated alcohol of 13-20 times of its weight, stirs evenly, increasing temperature is
60-70 DEG C, polysorbate is added, insulated and stirred 5-10 minutes, obtains ester dispersion liquid；
(2) conductive colloidal sol is taken, is added in the deionized water of 30-40 times of its weight, stirs evenly, above-mentioned 10- is added dropwise
13% formalin is sent in 90-95 DEG C of water bath with thermostatic control, and catalyst is added, insulation reaction 10-13 hours, discharges,
It is blended with above-mentioned ester dispersion liquid, stirring to room temperature filters, filter cake is washed, and 1-2 hours are dried at 50-55 DEG C of vacuum to get institute
State methylation conductive micro-balloons.
Advantages of the present invention:
The present invention polymerize under ferric trichloride effect using thiophene as monomer, hydrolysis is blended with ethyl orthosilicate later, obtains
Then conductive colloidal sol carries out methylation processing by formaldehyde, using triethylamine as catalyst, obtained conductive micro-balloons not only have very
Good electric conductivity, and mechanical stability is strong, and comprehensive performance is superior.
Specific embodiment
Embodiment 1
A kind of methylation conductive micro-balloons, it is composed of the following raw materials by weight:
Conductive colloidal sol 120, polysorbate 0.7, catalyst 0.1, zinc ricinate 1,10% formalin 20.
The catalyst is triethylamine.
What the conductive colloidal sol was made of the raw material of following weight parts:
Ethyl orthosilicate 27, thiophene 110-, ferric trichloride 3, ammonium polyphosphate 2, alkanolamide 1, tetrahydrofurfuryl alcohol 0.7；
Preparation method, comprising the following steps:
(1) ammonium polyphosphate is taken, is added in the deionized water of 25 times of its weight, stirs evenly, alkanolamide is added, 50
Insulated and stirred 3 minutes at DEG C, obtain amide dispersion liquid；
(2) ferric trichloride is taken, is added in the deionized water of 17 times of its weight, stirs evenly；
(3) thiophene is taken, is added in above-mentioned amide dispersion liquid, stirs evenly, be sent in reaction kettle, be passed through nitrogen, is adjusted
10 DEG C of temperature of reaction kettle of section, is added above-mentioned ferric chloride aqueous solutions, is stirred to react 10 hours, discharges, and ethyl orthosilicate is added, stirs
It mixes 3 hours, filters, filter cake is washed, air drying, obtain conductive colloidal sol.
A kind of preparation method for the conductive micro-balloons that methylate, comprising the following steps:
(1) zinc ricinate is taken, is added in the dehydrated alcohol of 13 times of its weight, stirs evenly, increasing temperature is 60 DEG C,
Polysorbate is added, insulated and stirred 5 minutes, obtains ester dispersion liquid；
(2) conductive colloidal sol is taken, is added in the deionized water of 30 times of its weight, stirs evenly, above-mentioned 10% first is added dropwise
Aldehyde aqueous solution is sent in 90 DEG C of water bath with thermostatic control, and catalyst is added, insulation reaction 10 hours, discharges, with above-mentioned ester dispersion liquid
It is blended, stirring to room temperature filters, filter cake is washed, and 1 hour is dried at 50 DEG C of vacuum to get the methylation conductive micro-balloons.
Embodiment 2
A kind of methylation conductive micro-balloons, it is composed of the following raw materials by weight:
Conductive colloidal sol 140, polysorbate 1, catalyst 0.3, zinc ricinate 2,13% formalin 30.
The catalyst is triethylamine.
What the conductive colloidal sol was made of the raw material of following weight parts:
Ethyl orthosilicate 27, thiophene 110, ferric trichloride 3, ammonium polyphosphate 2, alkanolamide 1, tetrahydrofurfuryl alcohol 0.7；
Preparation method, comprising the following steps:
(1) ammonium polyphosphate is taken, is added in the deionized water of 25 times of its weight, stirs evenly, alkanolamide is added, 50
Insulated and stirred 3 minutes at DEG C, obtain amide dispersion liquid；
(2) ferric trichloride is taken, is added in the deionized water of 17 times of its weight, stirs evenly；
(3) thiophene is taken, is added in above-mentioned amide dispersion liquid, stirs evenly, be sent in reaction kettle, be passed through nitrogen, is adjusted
10 DEG C of temperature of reaction kettle of section, is added above-mentioned ferric chloride aqueous solutions, is stirred to react 10 hours, discharges, and ethyl orthosilicate is added, stirs
It mixes 3 hours, filters, filter cake is washed, air drying, obtain conductive colloidal sol.
A kind of preparation method for the conductive micro-balloons that methylate, comprising the following steps:
(1) zinc ricinate is taken, is added in the dehydrated alcohol of 13 times of its weight, stirs evenly, increasing temperature is 60 DEG C,
Polysorbate is added, insulated and stirred 5 minutes, obtains ester dispersion liquid；
(2) conductive colloidal sol is taken, is added in the deionized water of 30 times of its weight, stirs evenly, above-mentioned 10% first is added dropwise
Aldehyde aqueous solution is sent in 90 DEG C of water bath with thermostatic control, and catalyst is added, insulation reaction 10 hours, discharges, with above-mentioned ester dispersion liquid
It is blended, stirring to room temperature filters, filter cake is washed, and 1 hour is dried at 50 DEG C of vacuum to get the methylation conductive micro-balloons.
Performance test:
The present invention methylate conductive micro-balloons conductivity be 0.18-0.23S/cm, tensile strength 27.0-33.3Mpa.
Claims (4)
1. a kind of methylation conductive micro-balloons, which is characterized in that it is composed of the following raw materials by weight:
The formalin of conductive colloidal sol 120-140, polysorbate 0.7-1, catalyst 0.1-0.3, zinc ricinate 1-2,10-13%
Solution 20-30.
2. a kind of methylation conductive micro-balloons according to claim 1, which is characterized in that the catalyst is triethylamine.
3. a kind of methylation conductive micro-balloons according to claim 1, which is characterized in that the conductive colloidal sol is by following
The raw material composition of parts by weight:
Ethyl orthosilicate 27-30, thiophene 110-130, ferric trichloride 3-4, ammonium polyphosphate 2-3, alkanolamide 1-2, tetrahydrofurfuryl alcohol
0.7-1；
Preparation method, comprising the following steps:
(1) ammonium polyphosphate is taken, is added in the deionized water of 25-30 times of its weight, stirs evenly, alkanolamide is added, in 50-
Insulated and stirred 3-10 minutes at 60 DEG C, amide dispersion liquid is obtained；
(2) ferric trichloride is taken, is added in the deionized water of 17-20 times of its weight, stirs evenly；
(3) thiophene is taken, is added in above-mentioned amide dispersion liquid, is stirred evenly, be sent in reaction kettle, nitrogen is passed through, is adjusted anti-
10-15 DEG C of kettle temperature degree is answered, above-mentioned ferric chloride aqueous solutions are added, is stirred to react 10-12 hours, is discharged, ethyl orthosilicate is added,
Stirring 3-4 hours filters, filter cake is washed, air drying, obtain conductive colloidal sol.
4. a kind of preparation method of the conductive micro-balloons of methylation as described in claim 1, which comprises the following steps:
(1) zinc ricinate is taken, is added in the dehydrated alcohol of 13-20 times of its weight, stirs evenly, raising temperature is 60-70
DEG C, polysorbate is added, insulated and stirred 5-10 minutes, obtains ester dispersion liquid；
(2) conductive colloidal sol is taken, is added in the deionized water of 30-40 times of its weight, stirs evenly, is added dropwise above-mentioned 10-13%'s
Formalin is sent in 90-95 DEG C of water bath with thermostatic control, and catalyst is added, insulation reaction 10-13 hour, discharges, and above-mentioned
Ester dispersion liquid is blended, and stirring to room temperature filters, filter cake is washed, and 1-2 hours are dried at 50-55 DEG C of vacuum to get the methyl
Change conductive micro-balloons.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110676445A (en) * | 2019-09-19 | 2020-01-10 | 安徽清泉新能源科技集团有限责任公司 | Sol-coated lithium battery material and preparation method thereof |
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| CN102344650A (en) * | 2010-08-02 | 2012-02-08 | 中国科学院理化技术研究所 | Preparation method of Fe3O4-poly (3, 4-ethylenedioxythiophene) core-shell structured composite microspheres |
| CN102766250A (en) * | 2012-07-31 | 2012-11-07 | 中国科学院宁波材料技术与工程研究所 | Polythiophene microballs and preparation method thereof |
| CN106810991A (en) * | 2016-12-20 | 2017-06-09 | 铜陵市经纬流体科技有限公司 | A kind of anti-oxidant hybrid microspheres grafting silicon composite coating and preparation method thereof |
-
2018
- 2018-07-11 CN CN201810759893.6A patent/CN108997561A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101585907A (en) * | 2008-05-21 | 2009-11-25 | 中国科学院理化技术研究所 | The preparation method of conductive polymer poly (3,4 dioxoethyl) thiophene tiny balloon |
| CN102344650A (en) * | 2010-08-02 | 2012-02-08 | 中国科学院理化技术研究所 | Preparation method of Fe3O4-poly (3, 4-ethylenedioxythiophene) core-shell structured composite microspheres |
| CN102766250A (en) * | 2012-07-31 | 2012-11-07 | 中国科学院宁波材料技术与工程研究所 | Polythiophene microballs and preparation method thereof |
| CN106810991A (en) * | 2016-12-20 | 2017-06-09 | 铜陵市经纬流体科技有限公司 | A kind of anti-oxidant hybrid microspheres grafting silicon composite coating and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110676445A (en) * | 2019-09-19 | 2020-01-10 | 安徽清泉新能源科技集团有限责任公司 | Sol-coated lithium battery material and preparation method thereof |
| CN110676445B (en) * | 2019-09-19 | 2022-11-08 | 安徽清泉新能源科技集团有限责任公司 | Lithium battery material and preparation method thereof |
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