CN108503830A - A kind of heat-resisting Polypyrrole Conducting Materials of phosphatization doping - Google Patents
A kind of heat-resisting Polypyrrole Conducting Materials of phosphatization doping Download PDFInfo
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- CN108503830A CN108503830A CN201810347897.3A CN201810347897A CN108503830A CN 108503830 A CN108503830 A CN 108503830A CN 201810347897 A CN201810347897 A CN 201810347897A CN 108503830 A CN108503830 A CN 108503830A
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- phosphatization
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/28—Nitrogen-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
- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/28—Nitrogen-containing compounds
- C08K2003/282—Binary compounds of nitrogen with aluminium
Abstract
The invention discloses a kind of phosphatizations to adulterate heat-resisting Polypyrrole Conducting Materials, it is made of the raw material of following weight parts：Double 12 parts of octyl methyl tertiary amines, modified 130 150 parts of phosphatization monomer, 0.4 1 parts of dibutyl tin laurate, 47 parts of cumyl peroxide, 0.01 0.03 parts of aphthenic acids lithium, 35 parts of trimethylolpropane, 0.01 0.02 parts of catalyst, 46 parts of aluminium nitride, 0.7 1 parts of 10 oleate of polyglycereol, the present invention handles aluminium nitride using trimethylolpropane, improve the surface-active of aluminium nitride, then the high temperature esterification with acid is realized under the catalytic action of p-methyl benzenesulfonic acid, to further improve the bond strength between aluminium nitride and polypyrrole, present invention adds a variety of heat-resisting stabilizing agents, temperature tolerance is good, conductive stability is strong.
Description
Technical field
The invention belongs to conductive material fields, and in particular to a kind of heat-resisting Polypyrrole Conducting Materials of phosphatization doping.
Background technology
Polypyrrole is a kind of typical silver type conducting polymer altogether, has good light, electricity, magnetic characteristic, and with opposite
The features such as being easy each system and preferable environmental stability, receives the extensive concern of researcher.Currently, the research of polypyrrole and answering
With very extensive, be directed not only to the fields such as sensor, capacitor, electroluminescent, electrochromism and electromagnetic shielding, and with life
Object, nanotechnology combine, and apply also for the intellectual materials neck such as controlled release of manufacture molecular wire, artificial-muscle and drug
Domain.
With the continuous development of composite material, more and more high-performance joint products come into being, however currently, polypyrrole
Because its temperature tolerance is not high, and limits application range, therefore, it is intended that a kind of new conductive material of research, to improve
The heat resistance of polypyrrole, to ensure the conductive stability of polypyrrole itself.
Invention content
Heat-resisting polypyrrole is adulterated in view of the defects and deficiencies of the prior art, the present invention intends to provide a kind of phosphatization to lead
Electric material.
To achieve the above object, the present invention uses following technical scheme：
A kind of heat-resisting Polypyrrole Conducting Materials of phosphatization doping, are made of the raw material of following weight parts：
Double octyl methyl tertiary amine 1-2, modified phosphatization monomer 130-150, dibutyl tin laurate 0.4-1, peroxidating two are different
Propyl benzene 4-7, aphthenic acids lithium 0.01-0.03, trimethylolpropane 3-5, catalyst 0.01-0.02, aluminium nitride 4-6, Natrulon H-10
Oleate 0.7-1.
What the modification phosphatization monomer was made of the raw material of following weight parts：
Phosphorus trichloride 10-14, pyrroles 100-120, calcium acetylacetonate 1-2, alkenyl succinic anhydride 3-4.
The modification phosphatization monomer, is made by following steps：
（1）Phosphorus trichloride is taken, is added in the chloroform of 5-7 times of its weight, stirs evenly, pyrroles is added, is sent to 50-55 DEG C
In water bath with thermostatic control, chloroform, phosphatization monomer is distilled off in insulated and stirred 30-40 minutes；
（2）Calcium acetylacetonate is taken, is added in the absolute ethyl alcohol of 10-15 times of its weight, stirs evenly, raising temperature is 60-65
DEG C, alkenyl succinic anhydride is added, above-mentioned phosphatization monomer is added in insulated and stirred 1-2 hours, and stirring to room temperature filters, by filter cake water
It washes, air drying is to get the modified phosphatization monomer.
The catalyst is p-methyl benzenesulfonic acid.
The phosphatization of the present invention adulterates heat-resisting Polypyrrole Conducting Materials, is made by following steps：
（1）Aphthenic acids lithium is taken, is added in the absolute ethyl alcohol of 10-20 times of its weight, stirs evenly, trimethylolpropane is added,
It is 55-60 DEG C to increase temperature, and aluminium nitride is added, and insulated and stirred 1-2 hours obtains alkyl based solution；
（2）Cumyl peroxide is taken, is added in the isopropanol of 30-40 times of its weight, stirs evenly, obtain initiator solution；
（3）Double octyl methyl tertiary amines, modified phosphatization monomer mixing are taken, the deionized water of 20-30 times of mixture weight is added to
In, it stirs evenly, obtains phosphatization monomer solution；
（4）Above-mentioned phosphatization monomer solution is taken, is sent in reaction kettle, nitrogen is passed through, it is 60-70 DEG C to adjust temperature of reaction kettle, is added
Enter above-mentioned initiator solution, insulated and stirred 3-4 hours is added dibutyl tin laurate, stirs evenly, and discharging cooling obtains phosphorus
Change modified polypyrrole solution；
（5）Above-mentioned phosphatization modified polypyrrole solution is taken, mixes, stirs evenly with alkyl based solution, catalyst is added, increasing temperature is
90-95 DEG C, Natrulon H-10 oleate, stirring to room temperature is added in insulated and stirred 100-130 minutes, and filtering washes precipitation, very
Insulated and stirred 20-50 minutes at empty 57-60 DEG C, it is cooled to room temperature and adulterates heat-resisting Polypyrrole Conducting Materials to get the phosphatization.
Advantages of the present invention：
The present invention using phosphorus trichloride handle pyrroles, pyrroles surface introduce phosphonium ion, later with calcium acetylacetonate blending and modifying,
It can be effectively promoted the heat-resistant stability of pyrrole monomer, polymerize under initiator effect with the monomer later, with tin dilaurate
Dibutyl tin is stabilizer, obtains heat stabilized polymer, and the present invention handles aluminium nitride using trimethylolpropane, improves nitrogen
Change the surface-active of aluminium, the high temperature esterification with acid is then realized under the catalytic action of p-methyl benzenesulfonic acid, to further carry
High bond strength between aluminium nitride and polypyrrole, present invention adds a variety of heat-resisting stabilizing agents, and temperature tolerance is good, conductive stability
By force.
Specific implementation mode
The present invention is further described with reference to embodiment.
Embodiment 1
Each raw material is weighed by weight：Double 2 parts of octyl methyl tertiary amines, modified 150 parts of phosphatization monomer, dibutyl tin laurate
1 part, 7 parts of cumyl peroxide, 0.03 part of aphthenic acids lithium, 5 parts of trimethylolpropane, 0.02 part of p-methyl benzenesulfonic acid, nitridation
6 parts of aluminium, 1 part of Natrulon H-10 oleate.
The modification phosphatization monomer is made by following steps：
（1）It counts in parts by weight, weighs 14 parts of phosphorus trichloride, be added in the chloroform of 7 times of its weight, stir evenly, pyrrole is added
120 parts are coughed up, is sent in 55 DEG C of water bath with thermostatic control, chloroform, phosphatization monomer is distilled off in insulated and stirred 40 minutes；
（2）2 parts of calcium acetylacetonate is taken, is added in the absolute ethyl alcohol of 15 times of its weight, stirs evenly, it is 65 DEG C to increase temperature,
4 parts of alkenyl succinic anhydride is added, above-mentioned phosphatization monomer is added in insulated and stirred 2 hours, and stirring to room temperature filters, by filter cake water
It washes, air drying is to get the modified phosphatization monomer.
The phosphatization of the present embodiment adulterates heat-resisting Polypyrrole Conducting Materials, is made by following steps：
（1）Aphthenic acids lithium is taken, is added in the absolute ethyl alcohol of 20 times of its weight, stirs evenly, trimethylolpropane is added, is increased
Temperature is 60 DEG C, and aluminium nitride is added, and insulated and stirred 1-2 hours obtains alkyl based solution；
（2）Cumyl peroxide is taken, is added in the isopropanol of 40 times of its weight, is stirred evenly, obtain initiator solution；
（3）Double octyl methyl tertiary amines, modified phosphatization monomer mixing are taken, the deionized water of 20-30 times of mixture weight is added to
In, it stirs evenly, obtains phosphatization monomer solution；
（4）Above-mentioned phosphatization monomer solution is taken, is sent in reaction kettle, nitrogen is passed through, it is 70 DEG C to adjust temperature of reaction kettle, in addition
Initiator solution is stated, insulated and stirred 4 hours is added dibutyl tin laurate, stirs evenly, and discharging cooling obtains phosphatization modification
Polypyrrole solution；
（5）Above-mentioned phosphatization modified polypyrrole solution is taken, mixes, stirs evenly with alkyl based solution, catalyst is added, increasing temperature is
95 DEG C, Natrulon H-10 oleate, stirring to room temperature is added in insulated and stirred 130 minutes, and filtering washes precipitation, 60 DEG C of vacuum
Lower insulated and stirred 50 minutes is cooled to room temperature and adulterates heat-resisting Polypyrrole Conducting Materials to get the phosphatization.
Embodiment 2
Each raw material is weighed by weight：Double 1 part of octyl methyl tertiary amines, modified 130 parts of phosphatization monomer, dibutyl tin laurate
0.4 part, 4 parts of cumyl peroxide, 0.01 part of aphthenic acids lithium, 3 parts of trimethylolpropane, 0.01 part of p-methyl benzenesulfonic acid, nitrogen
Change 4 parts of aluminium, 0.7 part of Natrulon H-10 oleate.
The modification phosphatization monomer is made by following steps：
Phosphorus trichloride, pyrroles, calcium acetylacetonate, alkenyl succinic anhydride.
The preparation method of the modification phosphatization monomer, includes the following steps：
（1）10 parts of phosphorus trichloride is taken, is added in the chloroform of 5 times of its weight, stirs evenly, 100 parts of pyrroles is added, is sent to 50
DEG C water bath with thermostatic control in, chloroform, phosphatization monomer is distilled off in insulated and stirred 30 minutes；
（2）1 part of calcium acetylacetonate is taken, is added in the absolute ethyl alcohol of 10 times of its weight, stirs evenly, it is 60 DEG C to increase temperature,
3 parts of alkenyl succinic anhydride is added, above-mentioned phosphatization monomer is added in insulated and stirred 1 hour, and stirring to room temperature filters, by filter cake water
It washes, air drying is to get the modified phosphatization monomer.
The phosphatization of the present embodiment adulterates heat-resisting Polypyrrole Conducting Materials, is made by following steps：
（1）Aphthenic acids lithium is taken, is added in the absolute ethyl alcohol of 10 times of its weight, stirs evenly, trimethylolpropane is added, is increased
Temperature is 55 DEG C, and aluminium nitride is added, and insulated and stirred 1 hour obtains alkyl based solution；
（2）Cumyl peroxide is taken, is added in the isopropanol of 30 times of its weight, is stirred evenly, obtain initiator solution；
（3）Double octyl methyl tertiary amines, modified phosphatization monomer mixing are taken, is added in the deionized water of 20 times of mixture weight,
It stirs evenly, obtains phosphatization monomer solution；
（4）Above-mentioned phosphatization monomer solution is taken, is sent in reaction kettle, nitrogen is passed through, it is 60 DEG C to adjust temperature of reaction kettle, in addition
Initiator solution is stated, insulated and stirred 3 hours is added dibutyl tin laurate, stirs evenly, and discharging cooling obtains phosphatization modification
Polypyrrole solution；
（5）Above-mentioned phosphatization modified polypyrrole solution is taken, mixes, stirs evenly with alkyl based solution, catalyst is added, increasing temperature is
90 DEG C, Natrulon H-10 oleate, stirring to room temperature is added in insulated and stirred 100 minutes, and filtering washes precipitation, 57 DEG C of vacuum
Lower insulated and stirred 20 minutes is cooled to room temperature and adulterates heat-resisting Polypyrrole Conducting Materials to get the phosphatization.
Performance test：
The phosphatization of the embodiment of the present invention 1 adulterates heat-resisting Polypyrrole Conducting Materials：
Charge-discharge test is carried out under room temperature, specific capacitance under the conditions of 0.2A/g charge and discharge is 184.60F/g；
1 hour is kept the temperature in 100 DEG C of boiling water bath, the specific capacitance after taking-up is cooling under the conditions of 0.2A/g charge and discharge is
184.0F/g；
The phosphatization of the embodiment of the present invention 2 adulterates heat-resisting Polypyrrole Conducting Materials：
Charge-discharge test is carried out under room temperature, specific capacitance under the conditions of 0.2A/g charge and discharge is 191.7F/g；
1 hour is kept the temperature in 100 DEG C of boiling water bath, the specific capacitance after taking-up is cooling under the conditions of 0.2A/g charge and discharge is
191.7F/g。
As can be seen that the materials conductive stability of the present invention, heat-resistant stability are good.
Claims (5)
1. a kind of phosphatization adulterates heat-resisting Polypyrrole Conducting Materials, it is characterised in that：The conductive material is the original by following weight parts
Material composition：
Double octyl methyl tertiary amine 1-2, modified phosphatization monomer 130-150, dibutyl tin laurate 0.4-1, peroxidating two are different
Propyl benzene 4-7, aphthenic acids lithium 0.01-0.03, trimethylolpropane 3-5, catalyst 0.01-0.02, aluminium nitride 4-6, Natrulon H-10
Oleate 0.7-1.
2. a kind of phosphatization according to claim 1 adulterates heat-resisting Polypyrrole Conducting Materials, it is characterised in that：The modification
Phosphatization monomer is made of the raw material of following weight parts：
Phosphorus trichloride 10-14, pyrroles 100-120, calcium acetylacetonate 1-2, alkenyl succinic anhydride 3-4.
3. a kind of phosphatization according to claim 2 adulterates heat-resisting Polypyrrole Conducting Materials, it is characterised in that：The modification
Phosphatization monomer is made by following steps：
（1）Phosphorus trichloride is taken, is added in the chloroform of 5-7 times of its weight, stirs evenly, pyrroles is added, is sent to 50-55 DEG C
In water bath with thermostatic control, chloroform, phosphatization monomer is distilled off in insulated and stirred 30-40 minutes；
（2）Calcium acetylacetonate is taken, is added in the absolute ethyl alcohol of 10-15 times of its weight, stirs evenly, raising temperature is 60-65
DEG C, alkenyl succinic anhydride is added, above-mentioned phosphatization monomer is added in insulated and stirred 1-2 hours, and stirring to room temperature filters, by filter cake water
It washes, air drying is to get the modified phosphatization monomer.
4. a kind of phosphatization according to claim 1 adulterates heat-resisting Polypyrrole Conducting Materials, it is characterised in that：The catalysis
Agent is p-methyl benzenesulfonic acid.
5. a kind of phosphatization according to claim 1 adulterates heat-resisting Polypyrrole Conducting Materials, it is characterised in that：By following steps
It is made：
（1）Aphthenic acids lithium is taken, is added in the absolute ethyl alcohol of 10-20 times of its weight, stirs evenly, trimethylolpropane is added,
It is 55-60 DEG C to increase temperature, and aluminium nitride is added, and insulated and stirred 1-2 hours obtains alkyl based solution；
（2）Cumyl peroxide is taken, is added in the isopropanol of 30-40 times of its weight, stirs evenly, obtain initiator solution；
（3）Double octyl methyl tertiary amines, modified phosphatization monomer mixing are taken, the deionized water of 20-30 times of mixture weight is added to
In, it stirs evenly, obtains phosphatization monomer solution；
（4）Above-mentioned phosphatization monomer solution is taken, is sent in reaction kettle, nitrogen is passed through, it is 60-70 DEG C to adjust temperature of reaction kettle, is added
Enter above-mentioned initiator solution, insulated and stirred 3-4 hours is added dibutyl tin laurate, stirs evenly, and discharging cooling obtains phosphorus
Change modified polypyrrole solution；
（5）Above-mentioned phosphatization modified polypyrrole solution is taken, mixes, stirs evenly with alkyl based solution, catalyst is added, increasing temperature is
90-95 DEG C, Natrulon H-10 oleate, stirring to room temperature is added in insulated and stirred 100-130 minutes, and filtering washes precipitation, very
Insulated and stirred 20-50 minutes at empty 57-60 DEG C, it is cooled to room temperature and adulterates heat-resisting Polypyrrole Conducting Materials to get the phosphatization.
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| CN201810347897.3A CN108503830A (en) | 2018-04-18 | 2018-04-18 | A kind of heat-resisting Polypyrrole Conducting Materials of phosphatization doping |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109401453A (en) * | 2018-12-13 | 2019-03-01 | 周弛逍 | A kind of heat-resisting phosphatization powdery paints 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 |
| CN109575411A (en) * | 2018-11-28 | 2019-04-05 | 安徽天大环保新材料股份有限公司 | A kind of nylon doping packaging bag and preparation method thereof |
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| JP2006247505A (en) * | 2005-03-10 | 2006-09-21 | Osaka Univ | Method for manufacturing metal nano cluster |
| CN102496481A (en) * | 2011-12-23 | 2012-06-13 | 北京航空航天大学 | Graphene/polypyrrole nanotube composite material, super capacitor with graphene/polypyrrole nanotube composite material as electrode, and methods for preparing graphene/polypyrrole nanotube composite material and super capacitor |
| CN106366621A (en) * | 2016-08-31 | 2017-02-01 | 安徽中润电缆集团股份有限公司 | Composite cable material with heat conductivity improved through polypyrrole coated composite filler |
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2018
- 2018-04-18 CN CN201810347897.3A patent/CN108503830A/en not_active Withdrawn
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006247505A (en) * | 2005-03-10 | 2006-09-21 | Osaka Univ | Method for manufacturing metal nano cluster |
| CN102496481A (en) * | 2011-12-23 | 2012-06-13 | 北京航空航天大学 | Graphene/polypyrrole nanotube composite material, super capacitor with graphene/polypyrrole nanotube composite material as electrode, and methods for preparing graphene/polypyrrole nanotube composite material and super capacitor |
| CN106366621A (en) * | 2016-08-31 | 2017-02-01 | 安徽中润电缆集团股份有限公司 | Composite cable material with heat conductivity improved through polypyrrole coated composite filler |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109505021A (en) * | 2018-10-22 | 2019-03-22 | 董荣志 | A kind of conduction colloidal sol toughened fiber and preparation method thereof |
| CN109575411A (en) * | 2018-11-28 | 2019-04-05 | 安徽天大环保新材料股份有限公司 | A kind of nylon doping packaging bag and preparation method thereof |
| CN109401453A (en) * | 2018-12-13 | 2019-03-01 | 周弛逍 | A kind of heat-resisting phosphatization powdery paints and preparation method thereof |
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