CN107501932A - A kind of preparation method of lightweight polypyrrole material - Google Patents
A kind of preparation method of lightweight polypyrrole material Download PDFInfo
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- CN107501932A CN107501932A CN201710783642.7A CN201710783642A CN107501932A CN 107501932 A CN107501932 A CN 107501932A CN 201710783642 A CN201710783642 A CN 201710783642A CN 107501932 A CN107501932 A CN 107501932A
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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
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/06—Pretreated ingredients and ingredients covered by the main groups C08K3/00 - C08K7/00
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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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
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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
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/09—Carboxylic acids; Metal salts thereof; Anhydrides thereof
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
Abstract
The invention discloses a kind of preparation method of lightweight polypyrrole material, using metallic compound as catalyst, so that the C=O bond of carbon-carbon double bond present in acrylic acid and siloxane dispersion could be formed with the conjugation of effect, effectively improve dispersiveness of the calcium carbonate in polypyrrole, the stability_intensity and mechanical property of finished product are improved, material of the invention has good electric conductivity, and light, stability is good, and combination property is superior.
Description
Technical field
The invention belongs to Material Field, and in particular to a kind of preparation method of lightweight polypyrrole material.
Background technology
Polypyrrole is the proper noun in chemistry, is common black, insoluble, molten, conductive polymer, polypyrrole be not usual
Obtained by pyrrole monomer oxidation polymerization, electrochemical anodic oxidation pyrroles is also the effective means for preparing polypyrrole；Polypyrrole can
For the modified electrode of biology, ion detection, electrochemical capacitance and antistatic material and photoelectrochemical cell, the electrode material of battery
Material.Further, it is also possible to as electromagnetic shielding material and gas separation membrane material, for electrochemical capacitor, electro-catalysis, conducting polymer
Composite etc., is of wide application, and the concern of people has been constantly subjected to since being found；
But the stability and poor mechanical property of electric polypyrrole material, in order to improve the performance of polypyrrole, great Liang Yan
The person of studying carefully by sight concentrate on polypyrrole and other materials it is compound on, in recent years with the compound exhibition extensively of the carbon material such as CNT
Open, result of study shows the compound performance that can significantly improve ultracapacitor with CNT, but CNT
There are the shortcomings such as cost is high, specific capacitance is low, therefore the present invention seeks to study a kind of compound polypyrrole material of brand-new inorganic filler,
The stability_intensity of polypyrrole and mechanical property are improved with this.
The content of the invention
It is an object of the invention to asking for the stability_intensity for polypyrrole material in the prior art and poor mechanical property
A kind of topic, there is provided preparation method of lightweight polypyrrole material.
To achieve the above object, the present invention uses following technical scheme：
A kind of preparation method of lightweight polypyrrole material, comprises the following steps：
（1）The 2- mercapto benzimidazoles of 0.3-0.7 parts by weight are taken, are added in the absolute ethyl alcohol of 10-19 times of its weight, are stirred
Uniformly, the melamine of 1-2 parts by weight is added, rise temperature is 60-70 DEG C, insulated and stirred 1-2 hours, obtains alkanolamine solution；
（2）Pyrroles's mixing of the acrylic acid, 30-40 parts by weight of 5-7 parts by weight is taken, is added to going for 20-30 times of compound weight
In ionized water, stir, add the ammonium persulfate of 0.6-0.7 parts by weight, be sent in reactor, be passed through nitrogen, rise temperature
Spend for 70-75 DEG C, insulated and stirred 3-4 hours, discharging cooling, obtain acid doping polypyrrole solution；
（3）The octylisothiazolinone of 0.1-0.3 parts by weight is taken, is added in the dimethylformamide of 20-30 times of its weight, stirs
The barium stearate for uniformly adding 0.8-1 parts by weight is mixed, rise temperature is 80-90 DEG C, adds the lightweight carbonic acid of 10-14 parts by weight
Calcium, insulated and stirred 40-50 minutes, obtain calcium carbonate dispersion liquid；
（4）The Arlacel-80 of 1.7-2 parts by weight is taken, is added in the deionized water of 30-40 times of its weight, stirs, obtain moisture
Dispersion liquid；
（5）The ZPT of 1-2 parts by weight is taken, is added in the absolute ethyl alcohol of 13-20 times of its weight, stirs, is added
The aminomethyl phenyl cyclotrisiloxane of 4-5 parts by weight, rise temperature is 60-70 DEG C, insulated and stirred 1-2 hours, adds above-mentioned moisture
Dispersion liquid, ultrasonic 4-5 minutes, ethanol is distilled off, obtains siloxane dispersion；
（6）Above-mentioned calcium carbonate dispersion liquid, siloxane dispersion mixing are taken, stirs, above-mentioned alkanolamine solution is added, in 35-40
Insulated and stirred 3-4 hours at DEG C, obtain alkylation alkanolamine solution；
（7）Above-mentioned acid doping polypyrrole solution, alkylation alkanolamine solution mixing are taken, stirs, adds 0.1-0.2 parts by weight
Catalyst, nitrogen is passed through, the insulation reaction 10-15 hours at 40-50 DEG C, discharging cooling, obtains crosslinked polymer solution；
（8）The calcium ricinoleate of 2-3 parts by weight is taken, is added in above-mentioned crosslinked polymer solution, ultrasonic 3-5 minutes, filtering will be heavy
Form sediment and wash, 2-3 hours are dried at 50-60 DEG C of vacuum, normal temperature is cooled to, produces the lightweight polypyrrole material.
Described catalyst is one kind in tin ash, alchlor.
Advantages of the present invention：
The present invention is blended by acrylic acid using pyrroles as monomer, using ammonium persulfate as initiator, obtains acid doping polypyrrole solution,
Then using the formamide dispersion liquid processing precipitated calcium carbonate of barium stearate, then using the processing of aminomethyl phenyl cyclotrisiloxane, obtain
To alkylation alkanolamine solution, the polypyrrole solution of itself and acid doping is blended, using metallic compound as catalyst so that acrylic acid
Present in the C=O bond of carbon-carbon double bond and siloxane dispersion could be formed with the conjugation of effect, effectively improve calcium carbonate
Dispersiveness in polypyrrole, improves the stability_intensity and mechanical property of finished product, and material of the invention has good lead
Electrically, and light, stability is good, and combination property is superior.
Embodiment
Embodiment 1
A kind of preparation method of lightweight polypyrrole material, comprises the following steps：
（1）The 2- mercapto benzimidazoles of 0.7 parts by weight are taken, is added in the absolute ethyl alcohol of 19 times of its weight, is stirred, add
Enter the melamine of 2 parts by weight, rise temperature is 70 DEG C, insulated and stirred 12 hours, obtains alkanolamine solution；
（2）Pyrroles's mixing of the acrylic acid, 40 parts by weight of 7 parts by weight is taken, is added in the deionized water of 30 times of compound weight,
Stir, add the ammonium persulfate of 0.7 parts by weight, be sent in reactor, be passed through nitrogen, rise temperature is 75 DEG C, insulation
Stir 3-4 hours, discharging cooling, obtain acid doping polypyrrole solution；
（3）The octylisothiazolinone of 0.3 parts by weight is taken, is added in the dimethylformamide of 30 times of its weight, stirs,
The barium stearate of 1 parts by weight is added, rise temperature is 90 DEG C, the precipitated calcium carbonate of 14 parts by weight of addition, insulated and stirred 50 minutes,
Obtain calcium carbonate dispersion liquid；
（4）The Arlacel-80 of 2 parts by weight is taken, is added in the deionized water of 40 times of its weight, is stirred, obtain aqueous dispersions；
（5）The ZPT of 2 parts by weight is taken, is added in the absolute ethyl alcohol of 20 times of its weight, stirs, adds 5 weight
The aminomethyl phenyl cyclotrisiloxane of part, rise temperature are 70 DEG C, insulated and stirred 2 hours, add above-mentioned aqueous dispersions, 5 points of ultrasound
Clock, ethanol is distilled off, obtains siloxane dispersion；
（6）Above-mentioned calcium carbonate dispersion liquid, siloxane dispersion mixing are taken, stirs, adds above-mentioned alkanolamine solution, at 40 DEG C
Insulated and stirred 4 hours, obtains alkylation alkanolamine solution；
（7）Above-mentioned acid doping polypyrrole solution, alkylation alkanolamine solution mixing are taken, stirs, adds the catalysis of 0.2 parts by weight
Agent, nitrogen is passed through, insulation reaction 15 hours at 50 DEG C, discharging cooling, obtains crosslinked polymer solution；
（8）The calcium ricinoleate of 3 parts by weight is taken, is added in above-mentioned crosslinked polymer solution, ultrasound 5 minutes, filtering, water will be precipitated
Wash, dried 3 hours at 60 DEG C of vacuum, be cooled to normal temperature, produce the lightweight polypyrrole material.
Described catalyst is alchlor.
Embodiment 2
A kind of preparation method of lightweight polypyrrole material, comprises the following steps：
（1）The 2- mercapto benzimidazoles of 0.3 parts by weight are taken, is added in the absolute ethyl alcohol of 10 times of its weight, is stirred, add
Enter the melamine of 1 parts by weight, rise temperature is 60 DEG C, insulated and stirred 1 hour, obtains alkanolamine solution；
（2）Pyrroles's mixing of the acrylic acid, 30 parts by weight of 5 parts by weight is taken, is added in the deionized water of 20 times of compound weight,
Stir, add the ammonium persulfate of 0.6 parts by weight, be sent in reactor, be passed through nitrogen, rise temperature is 70 DEG C, insulation
Stirring 3 hours, discharging cooling, obtains acid doping polypyrrole solution；
（3）The octylisothiazolinone of 0.1 parts by weight is taken, is added in the dimethylformamide of 20 times of its weight, stirs,
The barium stearate of 0.8 parts by weight is added, rise temperature is 80 DEG C, adds the precipitated calcium carbonate of 10 parts by weight, and insulated and stirred 40 is divided
Clock, obtain calcium carbonate dispersion liquid；
（4）The Arlacel-80 of 1.7 parts by weight is taken, is added in the deionized water of 30 times of its weight, is stirred, obtain aqueous dispersions；
（5）The ZPT of 1 parts by weight is taken, is added in the absolute ethyl alcohol of 13 times of its weight, stirs, adds 4 weight
The aminomethyl phenyl cyclotrisiloxane of part, rise temperature are 60 DEG C, insulated and stirred 1 hour, add above-mentioned aqueous dispersions, 4 points of ultrasound
Clock, ethanol is distilled off, obtains siloxane dispersion；
（6）Above-mentioned calcium carbonate dispersion liquid, siloxane dispersion mixing are taken, stirs, above-mentioned alkanolamine solution is added, in 35-40
Insulated and stirred 3 hours at DEG C, obtain alkylation alkanolamine solution；
（7）Above-mentioned acid doping polypyrrole solution, alkylation alkanolamine solution mixing are taken, stirs, adds the catalysis of 0.1 parts by weight
Agent, nitrogen is passed through, insulation reaction 10 hours at 40 DEG C, discharging cooling, obtains crosslinked polymer solution；
（8）The calcium ricinoleate of 2 parts by weight is taken, is added in above-mentioned crosslinked polymer solution, ultrasound 3 minutes, filtering, water will be precipitated
Wash, dried 2 hours at 50 DEG C of vacuum, be cooled to normal temperature, produce the lightweight polypyrrole material.
Described catalyst is tin ash.
Performance test：
The lightweight polypyrrole material of the embodiment of the present invention 1：
Charge-discharge test is carried out, the specific capacitance under the conditions of 0.2A/g discharge and recharges is 225F/g；Tensile strength is 107.6MPa；
The lightweight polypyrrole material of the embodiment of the present invention 2：
Charge-discharge test is carried out, the specific capacitance under the conditions of 0.2A/g discharge and recharges is 211F/g；Tensile strength 115.2MPa；
Commercially available pure polypyrrole：
Charge-discharge test is carried out, the specific capacitance under the conditions of 0.2A/g discharge and recharges is 114F/g；Tensile strength is 90.3MPa；Can
To find out, composite of the invention has more preferable conductive stability and a mechanical property, and combination property is superior.
Claims (2)
1. a kind of preparation method of lightweight polypyrrole material, it is characterised in that comprise the following steps：
（1）The 2- mercapto benzimidazoles of 0.3-0.7 parts by weight are taken, are added in the absolute ethyl alcohol of 10-19 times of its weight, are stirred
Uniformly, the melamine of 1-2 parts by weight is added, rise temperature is 60-70 DEG C, insulated and stirred 1-2 hours, obtains alkanolamine solution；
（2）Pyrroles's mixing of the acrylic acid, 30-40 parts by weight of 5-7 parts by weight is taken, is added to going for 20-30 times of compound weight
In ionized water, stir, add the ammonium persulfate of 0.6-0.7 parts by weight, be sent in reactor, be passed through nitrogen, rise temperature
Spend for 70-75 DEG C, insulated and stirred 3-4 hours, discharging cooling, obtain acid doping polypyrrole solution；
（3）The octylisothiazolinone of 0.1-0.3 parts by weight is taken, is added in the dimethylformamide of 20-30 times of its weight, stirs
The barium stearate for uniformly adding 0.8-1 parts by weight is mixed, rise temperature is 80-90 DEG C, adds the lightweight carbonic acid of 10-14 parts by weight
Calcium, insulated and stirred 40-50 minutes, obtain calcium carbonate dispersion liquid；
（4）The Arlacel-80 of 1.7-2 parts by weight is taken, is added in the deionized water of 30-40 times of its weight, stirs, obtain moisture
Dispersion liquid；
（5）The ZPT of 1-2 parts by weight is taken, is added in the absolute ethyl alcohol of 13-20 times of its weight, stirs, is added
The aminomethyl phenyl cyclotrisiloxane of 4-5 parts by weight, rise temperature is 60-70 DEG C, insulated and stirred 1-2 hours, adds above-mentioned moisture
Dispersion liquid, ultrasonic 4-5 minutes, ethanol is distilled off, obtains siloxane dispersion；
（6）Above-mentioned calcium carbonate dispersion liquid, siloxane dispersion mixing are taken, stirs, above-mentioned alkanolamine solution is added, in 35-40
Insulated and stirred 3-4 hours at DEG C, obtain alkylation alkanolamine solution；
（7）Above-mentioned acid doping polypyrrole solution, alkylation alkanolamine solution mixing are taken, stirs, adds 0.1-0.2 parts by weight
Catalyst, nitrogen is passed through, the insulation reaction 10-15 hours at 40-50 DEG C, discharging cooling, obtains crosslinked polymer solution；
（8）The calcium ricinoleate of 2-3 parts by weight is taken, is added in above-mentioned crosslinked polymer solution, ultrasonic 3-5 minutes, filtering will be heavy
Form sediment and wash, 2-3 hours are dried at 50-60 DEG C of vacuum, normal temperature is cooled to, produces the lightweight polypyrrole material.
A kind of 2. preparation method of lightweight polypyrrole material according to claim 1, it is characterised in that described catalyst
For one kind in tin ash, alchlor.
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| CN201710783642.7A CN107501932A (en) | 2017-09-04 | 2017-09-04 | A kind of preparation method of lightweight polypyrrole material |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108182984A (en) * | 2018-01-22 | 2018-06-19 | 王旭 | A kind of ion liquid modified Polypyrrole Conducting Materials |
| CN108193314A (en) * | 2018-01-22 | 2018-06-22 | 王家浩 | A kind of polypyrrole conductive fiber |
| CN108250437A (en) * | 2018-01-23 | 2018-07-06 | 宿州市微腾知识产权运营有限公司 | A kind of preparation method of Polypyrrole Conducting Materials |
| CN108250559A (en) * | 2018-03-05 | 2018-07-06 | 象山杰尔德智能科技有限公司 | A kind of high-performance rotational moulding type urea box and preparation method thereof |
| CN108597646A (en) * | 2018-04-02 | 2018-09-28 | 张庆 | A kind of compound Polypyrrole Conducting Materials of carbon nanotube and preparation method thereof |
| CN109505021A (en) * | 2018-10-22 | 2019-03-22 | 董荣志 | A kind of conduction colloidal sol toughened fiber and preparation method thereof |
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| CN102532894A (en) * | 2012-01-06 | 2012-07-04 | 北京交通大学 | Preparation method of graphite oxide/polypyrrole composite material |
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2017
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| CN102532894A (en) * | 2012-01-06 | 2012-07-04 | 北京交通大学 | Preparation method of graphite oxide/polypyrrole composite material |
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| CN105038143A (en) * | 2015-07-21 | 2015-11-11 | 菏泽学院 | Film made of nano material and doped with polypyrrole and preparation method of film |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108182984A (en) * | 2018-01-22 | 2018-06-19 | 王旭 | A kind of ion liquid modified Polypyrrole Conducting Materials |
| CN108193314A (en) * | 2018-01-22 | 2018-06-22 | 王家浩 | A kind of polypyrrole conductive fiber |
| CN108250437A (en) * | 2018-01-23 | 2018-07-06 | 宿州市微腾知识产权运营有限公司 | A kind of preparation method of Polypyrrole Conducting Materials |
| CN108250559A (en) * | 2018-03-05 | 2018-07-06 | 象山杰尔德智能科技有限公司 | A kind of high-performance rotational moulding type urea box and preparation method thereof |
| CN108597646A (en) * | 2018-04-02 | 2018-09-28 | 张庆 | A kind of compound Polypyrrole Conducting Materials of carbon nanotube and preparation method thereof |
| CN109505021A (en) * | 2018-10-22 | 2019-03-22 | 董荣志 | A kind of conduction colloidal sol toughened fiber and preparation method thereof |
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