CN107236127A - A kind of preparation method of compound monomer denatured conductive material - Google Patents
A kind of preparation method of compound monomer denatured conductive material Download PDFInfo
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- CN107236127A CN107236127A CN201710600161.8A CN201710600161A CN107236127A CN 107236127 A CN107236127 A CN 107236127A CN 201710600161 A CN201710600161 A CN 201710600161A CN 107236127 A CN107236127 A CN 107236127A
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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
- 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
- C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
- C08G73/0605—Polycondensates containing five-membered rings, not condensed with other rings, with nitrogen atoms as the only ring hetero atoms
- C08G73/0611—Polycondensates containing five-membered rings, not condensed with other rings, with nitrogen atoms as the only ring hetero atoms with only one nitrogen atom in the ring, e.g. polypyrroles
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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
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
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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
- C08K9/04—Ingredients treated with organic substances
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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
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
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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
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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Abstract
The invention discloses a kind of preparation method of compound monomer denatured conductive material, pyrroles is handled by paratoluensulfonyl chloride, obtain sulphonylpyrroles, then using parahydroxyben-zaldehyde as raw material, pass through bromo-reaction, obtained modified monomer is mixed with sulphonylpyrroles, using ferric trichloride as catalyst, chloroform is reaction dissolvent, the CNT that oleic acid is modified is added in the course of the polymerization process, the inorganic fillers such as CNT are effectively dispersed in polymer, strengthen the compatibility between inorganic filler and polymer, the agglomeration of inorganic filler can effectively be improved, improve the stability_intensity of finished-product material.
Description
Technical field
The invention belongs to Material Field, and in particular to a kind of preparation method of compound monomer denatured conductive material.
Background technology
Conducting polymer composite is with conducting function（Including semiconduction, metallic conductivity and superconductivity）, conductance
Polymeric material of the rate in more than 10S/m.Macromolecule conducting material have small density, easy processing, it is corrosion-resistant, can large area into
Film and electrical conductivity can be used as various metals material and nothing the features such as being adjusted in the range of more than ten orders of magnitude
The substitute of machine conductive material, and turned into the indispensable class material of many advanced industrial departments and sophisticated technology field
Material, by worldwide for many years widely studied, application of the conducting polymer in terms of new energy materialses has obtained very big
Development, but also have a certain distance from actual large-scale application.It is bad not high with stability that this is primarily due to its processability
Cause, seriously hinder the application of conductive polymer material industrially.Application especially in electric elements is, it is necessary to conduction material
Material has good intensity, stability, otherwise, can not also be applied even if other performance is good again；
Application number：201610885928.1 disclose the electrically-conducting paint of a kind of, including 45-55 parts of polyaniline, polypyrrole 18-20
Part, 25-40 parts of carbon fiber, 7-12 parts of petroleum coke, 8-16 parts of carborundum, 20-25 parts of graphite, 6-9 parts of silver powder, 7-11 parts of nickel powder,
20-22 parts of single-walled carbon nanotube, 36-40 parts of tin oxide, 23-25 parts of zinc oxide, 22-24 parts of sodium pyrophosphate, triethyl group hexyl phosphorus
Sour 4-8 parts, 16-20 parts of calgon, 7-9 parts of sodium carboxymethylcellulose, 11-15 parts of OPE, polyvinyl chloride tree
3-5 parts of fat, 12-16 parts of BMI, 20-25 parts of ethyl acrylate, 6-10 parts of NC Nitroncellulose and terpinol 13-16
Part, it is to be pre-mixed polypyrrole, single-walled carbon nanotube, then passes through point of calgon, sodium carboxymethylcellulose etc.
It is scattered to act on improving compatibility of the inorganic fillers such as single-walled carbon nanotube between polymer；But this inorganic scattered mode is very
Hardly possible improves the agglomeration of inorganic filler, is easily reduced the stability of finished product.
The content of the invention
In view of the defects and deficiencies of the prior art, the present invention intends to provide a kind of compound monomer denatured conductive material
Preparation method.
To achieve the above object, the present invention uses following technical scheme：
A kind of preparation method of compound monomer denatured conductive material, comprises the following steps：
（1）Pyrroles is taken, in the tetrahydrofuran for being added to 30-44 times of its weight, is stirred, 60-70 DEG C of thermostatted water is sent to
In bath, metallic potassium is added, insulated and stirred 30-40 minutes, discharging cooling adds paratoluensulfonyl chloride, magnetic agitation 20-24 is small
When, product is added in deionized water, stirred, 10-15 hours are stood, filtering washes precipitation, 60-70 DEG C of vacuum
Lower dry 1-2 hours, obtain sulphonylpyrroles；
（2）Bromination of n-butane is taken, in the absolute ethyl alcohol for being added to 4-6 times of its weight, is stirred, bromhydrin dispersion liquid is obtained；
（3）Parahydroxyben-zaldehyde is taken, in the absolute ethyl alcohol for being added to 10-13 times of its weight, is stirred, metallic sodium is added, led to
Enter nitrogen, insulation reaction 30-40 minutes at 80-90 DEG C, above-mentioned bromhydrin dispersion liquid is added dropwise, the follow-up continuation of insurance temperature of completion of dropping is anti-
Answer 16-20 hours, ethanol is distilled off, modified monomer is obtained；
（4）Prodan is taken, in the deionized water for being added to 45-60 times of its weight, is stirred, is added at oleic acid, 80-90 DEG C
Precipitation is washed in insulated and stirred 1-2 hours, filtering, obtains the sour sodium of oleic acid modified fluoro-silicone；
（5）The sour sodium mixing of CNT, oleic acid modified fluoro-silicone is taken, 40-50 times of compound weight, 96-98% sulfuric acid is added to
In solution, insulated and stirred 1-2 hours at 50-60 DEG C, filtering washes precipitation, air drying, obtains oleic acid modification composite carbon and receives
Mitron；
（6）Ferric trichloride is taken, in the chloroform for being added to 100-130 times of its weight, magnetic agitation 5-10 minutes is added above-mentioned
Sulphonylpyrroles, modified monomer, are sent in reactor, are passed through nitrogen, and regulation temperature of reaction kettle is 4-6 DEG C, adds above-mentioned oil
The modified composite carbon nanometer tube of acid, insulation reaction 4-5 hours is discharged, and precipitation is washed in filtering, and 20- is dried at 70-75 DEG C of vacuum
23 hours, normal temperature is cooled to, the compound monomer denatured conductive material is produced；
Described pyrroles, metallic potassium, paratoluensulfonyl chloride, bromination of n-butane, parahydroxyben-zaldehyde, metallic sodium, prodan, oil
Acid, CNT, the weight ratio of ferric trichloride are 100-110:2-3:3-4:1-2:6-7:0.3-1:16-20:2-3:20-30:
1-3。
Advantages of the present invention：
The present invention handles pyrroles by paratoluensulfonyl chloride, obtains sulphonylpyrroles, then using parahydroxyben-zaldehyde as raw material,
By bromo-reaction, obtained modified monomer is mixed with sulphonylpyrroles, using ferric trichloride as catalyst, chloroform is anti-
Solvent is answered, the CNT that oleic acid is modified is added in the course of the polymerization process so that the inorganic filler such as CNT can effectively divide
Dissipate in the polymer, the compatibility between enhancing inorganic filler and polymer can effectively improve the agglomeration of inorganic filler,
Improve the stability_intensity of finished-product material.
Embodiment
Embodiment 1
A kind of preparation method of compound monomer denatured conductive material, comprises the following steps：
（1）Pyrroles is taken, in the tetrahydrofuran for being added to 44 times of its weight, is stirred, in the water bath with thermostatic control for being sent to 70 DEG C, plus
Enter metallic potassium, insulated and stirred 40 minutes, discharging cooling adds paratoluensulfonyl chloride, product is added to by magnetic agitation 20 hours
In deionized water, stir, stand 10 hours, precipitation is washed in filtering, is dried 1 hour at 70 DEG C of vacuum, is obtained sulfonyl pyrrole
Cough up；
（2）Bromination of n-butane is taken, in the absolute ethyl alcohol for being added to 6 times of its weight, stirs, obtains bromhydrin dispersion liquid；
（3）Parahydroxyben-zaldehyde is taken, in the absolute ethyl alcohol for being added to 13 times of its weight, is stirred, metallic sodium is added, is passed through nitrogen
Gas, insulation reaction 40 minutes at 90 DEG C, the above-mentioned bromhydrin dispersion liquid of dropwise addition, the follow-up continuous insulation reaction of completion of dropping 20 hours,
Ethanol is distilled off, modified monomer is obtained；
（4）Prodan is taken, in the deionized water for being added to 60 times of its weight, is stirred, adds to be incubated at oleic acid, 80 DEG C and stirs
Mix 1 hour, filter, precipitation is washed, obtain the sour sodium of oleic acid modified fluoro-silicone；
（5）The sour sodium mixing of CNT, oleic acid modified fluoro-silicone is taken, 50 times of compound weight, 96% sulfuric acid solution is added to
In, insulated and stirred 1 hour at 60 DEG C, filtering washes precipitation, air drying, obtains oleic acid and is modified composite carbon nanometer tube；
（6）Ferric trichloride is taken, in the chloroform for being added to 100 times of its weight, magnetic agitation 10 minutes adds above-mentioned sulfonyl
Pyrroles, modified monomer, are sent in reactor, are passed through nitrogen, and regulation temperature of reaction kettle is 4 DEG C, adds above-mentioned oleic acid and is modified again
Compound/carbon nano pipe, insulation reaction 5 hours is discharged, and precipitation is washed in filtering, is dried 23 hours at 70 DEG C of vacuum, is cooled to often
Temperature, produces the compound monomer denatured conductive material；
Described pyrroles, metallic potassium, paratoluensulfonyl chloride, bromination of n-butane, parahydroxyben-zaldehyde, metallic sodium, prodan, oil
Acid, CNT, the weight ratio of ferric trichloride are 100:2:3:1:6:0.3:20:3:20:1.
Claims (1)
1. a kind of preparation method of compound monomer denatured conductive material, it is characterised in that comprise the following steps：
（1）Pyrroles is taken, in the tetrahydrofuran for being added to 30-44 times of its weight, is stirred, 60-70 DEG C of thermostatted water is sent to
In bath, metallic potassium is added, insulated and stirred 30-40 minutes, discharging cooling adds paratoluensulfonyl chloride, magnetic agitation 20-24 is small
When, product is added in deionized water, stirred, 10-15 hours are stood, filtering washes precipitation, 60-70 DEG C of vacuum
Lower dry 1-2 hours, obtain sulphonylpyrroles；
（2）Bromination of n-butane is taken, in the absolute ethyl alcohol for being added to 4-6 times of its weight, is stirred, bromhydrin dispersion liquid is obtained；
（3）Parahydroxyben-zaldehyde is taken, in the absolute ethyl alcohol for being added to 10-13 times of its weight, is stirred, metallic sodium is added, led to
Enter nitrogen, insulation reaction 30-40 minutes at 80-90 DEG C, above-mentioned bromhydrin dispersion liquid is added dropwise, the follow-up continuation of insurance temperature of completion of dropping is anti-
Answer 16-20 hours, ethanol is distilled off, modified monomer is obtained；
（4）Prodan is taken, in the deionized water for being added to 45-60 times of its weight, is stirred, is added at oleic acid, 80-90 DEG C
Precipitation is washed in insulated and stirred 1-2 hours, filtering, obtains the sour sodium of oleic acid modified fluoro-silicone；
（5）The sour sodium mixing of CNT, oleic acid modified fluoro-silicone is taken, 40-50 times of compound weight, 96-98% sulfuric acid is added to
In solution, insulated and stirred 1-2 hours at 50-60 DEG C, filtering washes precipitation, air drying, obtains oleic acid modification composite carbon and receives
Mitron；
（6）Ferric trichloride is taken, in the chloroform for being added to 100-130 times of its weight, magnetic agitation 5-10 minutes is added above-mentioned
Sulphonylpyrroles, modified monomer, are sent in reactor, are passed through nitrogen, and regulation temperature of reaction kettle is 4-6 DEG C, adds above-mentioned oil
The modified composite carbon nanometer tube of acid, insulation reaction 4-5 hours is discharged, and precipitation is washed in filtering, and 20- is dried at 70-75 DEG C of vacuum
23 hours, normal temperature is cooled to, the compound monomer denatured conductive material is produced；
Described pyrroles, metallic potassium, paratoluensulfonyl chloride, bromination of n-butane, parahydroxyben-zaldehyde, metallic sodium, prodan, oil
Acid, CNT, the weight ratio of ferric trichloride are 100-110:2-3:3-4:1-2:6-7:0.3-1:16-20:2-3:20-30:
1-3。
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710600161.8A CN107236127A (en) | 2017-07-21 | 2017-07-21 | A kind of preparation method of compound monomer denatured conductive material |
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| CN201710600161.8A CN107236127A (en) | 2017-07-21 | 2017-07-21 | A kind of preparation method of compound monomer denatured conductive material |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108193314A (en) * | 2018-01-22 | 2018-06-22 | 王家浩 | A kind of polypyrrole conductive fiber |
| CN114702177A (en) * | 2022-03-29 | 2022-07-05 | 宁波博汇化工科技股份有限公司 | Method for advanced oxidation treatment of sewage by BDD electrode |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104059432A (en) * | 2013-03-20 | 2014-09-24 | 北京阿格蕾雅科技发展有限公司 | Transparent carbon-nanotube high-molecular composite conductive ink and preparation method thereof |
| CN104211618A (en) * | 2009-02-25 | 2014-12-17 | 武田药品工业株式会社 | Process for producing pyrrole compound |
| CN106432721A (en) * | 2016-09-30 | 2017-02-22 | 同济大学 | Method for preparing carbon nano-tubes/polypyrrole nano-particles with performance of metamaterials |
-
2017
- 2017-07-21 CN CN201710600161.8A patent/CN107236127A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104211618A (en) * | 2009-02-25 | 2014-12-17 | 武田药品工业株式会社 | Process for producing pyrrole compound |
| CN104059432A (en) * | 2013-03-20 | 2014-09-24 | 北京阿格蕾雅科技发展有限公司 | Transparent carbon-nanotube high-molecular composite conductive ink and preparation method thereof |
| CN106432721A (en) * | 2016-09-30 | 2017-02-22 | 同济大学 | Method for preparing carbon nano-tubes/polypyrrole nano-particles with performance of metamaterials |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108193314A (en) * | 2018-01-22 | 2018-06-22 | 王家浩 | A kind of polypyrrole conductive fiber |
| CN114702177A (en) * | 2022-03-29 | 2022-07-05 | 宁波博汇化工科技股份有限公司 | Method for advanced oxidation treatment of sewage by BDD electrode |
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