CN109762303A - A kind of fiber/copolymer composite conducting material and preparation method thereof - Google Patents
A kind of fiber/copolymer composite conducting material and preparation method thereof Download PDFInfo
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- CN109762303A CN109762303A CN201811572669.2A CN201811572669A CN109762303A CN 109762303 A CN109762303 A CN 109762303A CN 201811572669 A CN201811572669 A CN 201811572669A CN 109762303 A CN109762303 A CN 109762303A
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Abstract
The present invention provides a kind of fiber/copolymer composite conducting materials and preparation method thereof, are related to Material Field.The preparation method of material the following steps are included: take 32-46 parts of polybutylene terephthalate-polycaprolactone co-polymers, 14-18 parts of conductive fibers, 6-10 parts of tea polyphenols, 20-26 parts of acetone, 11-15 parts of epoxy resin, 2-5 parts of ethylenediamines, 14-16 parts of polyvinyl alcohol, 3-8 parts of compatilizers, 2-4 parts of curing agent to be placed in torque rheometer and be blended by weight, it is molded again with hydraulic forming machine, pressure maintaining cooling obtains fiber/copolymer composite conducting material.The fiber that the present invention is prepared/copolymer composite conducting material processing technology is simple, high production efficiency, with reliable practical value, the fiber/copolymer composite conducting material tensile strength being prepared is in 49.24-53.45MPa range, and impact strength is in 56.39-62.32KJm‑2Range, volume resistivity 1.69 × 102‑9.41×105Ω cm range.
Description
Technical field
The present invention relates to Material Fields, more particularly to a kind of fiber/copolymer composite conducting material and preparation method thereof.
Background technique
Develop as science and technology is continuous and perfect, impetus is also played for the development of material.In material supply section
Field, more and more performance function materials are applied in industrial production.The electric conductivity object critically important as material
Rationality can be mentioned more and more, and conductive material is also widely used in Electronics and Information Engineering, machining manufacture, aviation boat
The technical fields such as it.The volume resistivity of high molecular material is generally 1010-1020It is good insulating materials between Ω cm,
As the application range of high molecular material constantly expands, requirement is also increasingly improved, in recent decades, conductive polymer material
Research and development be constantly subjected to the most attentions of countries in the world, the demand to conductive polymer material is more more and more urgent.Therefore,
The present invention provides a kind of fiber/copolymer composite conducting materials, and processing technology is simple, high production efficiency, have reliable real
With value.
Summary of the invention
Technical problems to be solved:
It is an object of the present invention to solve the deficiency of the existing technology and provide a kind of fiber/copolymer composite conducting materials
And preparation method thereof.
Technical solution:
The present invention provides a kind of fiber/copolymer composite conducting material preparation methods, including following preparation step:
32-46 parts of polybutylene terephthalate-polycaprolactone co-polymers, 14-18 parts of conductive fibers, 6- are taken by weight
10 parts of tea polyphenols, 20-26 parts of acetone, 11-15 parts of epoxy resin, 2-5 parts of ethylenediamines, 14-16 parts of polyvinyl alcohol, 3-8 parts it is compatible
Agent, 2-4 parts of curing agent are placed in torque rheometer and are blended, then are molded with hydraulic forming machine, and pressure maintaining cooling obtains fibre
Dimension/copolymer composite conducting material.
Preferably, the blending temperature is 200-240 DEG C, and the blending time is 5min.
Preferably, the temperature of the molding is 260-280 DEG C, pressure 5-9MPa, time 5min.
Preferably, the polybutylene terephthalate-polycaprolactone co-polymer the preparation method comprises the following steps:
Polybutylene terephthalate and polycaprolactone are uniformly mixed according to weight ratio 3:1, it is sub- that octoate catalyst is added
Tin keeps nitrogen atmosphere, 4-6h is stirred to react at 55-75 DEG C, is cooled to room temperature after reaction, and 80 DEG C of vacuum drying are for 24 hours
It is spare to obtain polybutylene terephthalate-polycaprolactone co-polymer.
It is further preferred that catalyst in the preparation method of the polybutylene terephthalate-polycaprolactone co-polymer
Dosage be polycaprolactone quality 1%.
Preferably, the conductive fiber preparation method the following steps are included:
Step 1: shearing aramid fiber to 2mm, it is placed in sodium hydroxide solution, 50 DEG C of heating 20min, takes out and clean,
Acetone soln is added, 20min is cleaned by ultrasonic, cleans, is dried for standby;
Step 2: taking the aramid fiber handled well in reactor, copper-bath is added, dodecyl sulphur is then added
Sour sodium and polysorbas20,100r/min are stirred evenly, and keep revolving speed, and ortho phosphorous acid sodium solution is then added dropwise, filters after reaction,
Washing, 80 DEG C of vacuum drying 12h are up to conductive fiber.
It is further preferred that the drop rate of ortho phosphorous acid sodium solution is in the preparation method step 2 of the conductive fiber
8mL/min。
The utility model has the advantages that
The fiber that the present invention is prepared/copolymer composite conducting material processing technology is simple, high production efficiency, and having can
The practical value leaned on, the fiber being prepared/copolymer composite conducting material tensile strength is in 49.24-53.45MPa range, punching
Hit intensity is in 56.39-62.32KJm-2Range, volume resistivity 1.69 × 102-9.41×105Ω cm range;
Polybutylene terephthalate and polycaprolactone co-polymer are prepared in the present invention, polybutylene terephthalate is
A kind of polyester, a kind of semicrystalline polymeric of polycaprolactone, the two are copolymerized the flexibility, processability and machinery that material can be improved
Performance;
Aramid fiber is subjected to roughing in surface oil removing pretreatment in the present invention, recycles copper sulphate and sodium hypophosphite anti-
It answers, the copper atom of generation can be attached on surface treated aramid fiber, make it have good electric conductivity.
Specific embodiment
The following examples can make those skilled in the art that the present invention be more fully understood, but not limit this in any way
Invention.
In embodiment 1-5 and comparative example 1 conductive fiber the preparation method comprises the following steps:
Step 1: shearing aramid fiber to 2mm, it is placed in the sodium hydroxide solution of 0.05wt%, 50 DEG C of heating
20min, taking-up are cleaned up with deionized water, add acetone soln, are cleaned by ultrasonic 20min, and taking-up is washed with deionized water,
60 DEG C are dried for standby;
Step 2: taking the aramid fiber 20g handled well in reactor, 100mL 20wt% copper-bath is added, so
0.4g lauryl sodium sulfate is added afterwards and 0.25g polysorbas20,100r/min are stirred evenly, keeps revolving speed, 80mL is then added dropwise
The ortho phosphorous acid sodium solution of 15wt%, drop rate 8mL/min are filtered after reaction, are washed with deionized, and 80 DEG C true
The dry 12h of sky is up to conductive fiber.
Embodiment 1
Take 32 parts of polybutylene terephthalate-polycaprolactone co-polymers, 18 parts of conductive fibers, 6 parts of tea more by weight
Phenol, 26 parts of acetone, 11 parts of E-44 bisphenol A type epoxy resins, 5 parts of ethylenediamines, 14 parts of polyvinyl alcohol, 8 parts of polypropylene grafted Malaysias
Acid anhydrides, 2 parts of curing agent F-52A are placed in torque rheometer, 240 DEG C of blending 5min, then with hydraulic forming machine in 260 DEG C, 9MPa
Under the conditions of be molded 5min, pressure maintaining cooling obtains fiber/copolymer composite conducting material;
Polybutylene terephthalate-the polycaprolactone co-polymer the preparation method comprises the following steps: by poly terephthalic acid fourth two
Ester and polycaprolactone are uniformly mixed according to weight ratio 2:1, and stannous octoate is added, and stannous octoate dosage is polycaprolactone quality
1%, nitrogen atmosphere is kept, 5h is stirred to react at 60 DEG C, is cooled to room temperature after reaction, 80 DEG C of vacuum drying obtain for 24 hours
Polybutylene terephthalate-polycaprolactone co-polymer is spare.
Embodiment 2
Take 46 parts of polybutylene terephthalate-polycaprolactone co-polymers, 14 parts of conductive fibers, 10 parts of tea more by weight
Phenol, 20 parts of acetone, 15 parts of E-44 bisphenol A type epoxy resins, 2 parts of ethylenediamines, 16 parts of polyvinyl alcohol, 3 parts of polypropylene grafted Malaysias
Acid anhydrides, 4 parts of curing agent F-52A are placed in torque rheometer, 200 DEG C of blending 5min, then with hydraulic forming machine in 280 DEG C, 5MPa
Under the conditions of be molded 5min, pressure maintaining cooling obtains fiber/copolymer composite conducting material;
Polybutylene terephthalate-the polycaprolactone co-polymer the preparation method comprises the following steps: by poly terephthalic acid fourth two
Ester and polycaprolactone are uniformly mixed according to weight ratio 2:1, and stannous octoate is added, and stannous octoate dosage is polycaprolactone quality
1%, nitrogen atmosphere is kept, 5h is stirred to react at 60 DEG C, is cooled to room temperature after reaction, 80 DEG C of vacuum drying obtain for 24 hours
Polybutylene terephthalate-polycaprolactone co-polymer is spare.
Embodiment 3
Take 44 parts of polybutylene terephthalate-polycaprolactone co-polymers, 15 parts of conductive fibers, 9 parts of tea more by weight
Phenol, 22 parts of acetone, 14 parts of E-44 bisphenol A type epoxy resins, 2.5 parts of ethylenediamines, 15.5 parts of polyvinyl alcohol, 4 parts it is polypropylene grafted
Maleic anhydride, 3.5 parts of curing agent F-52A are placed in torque rheometer, 210 DEG C of blending 5min, then with hydraulic forming machine in 275
DEG C, 5min is molded under the conditions of 6MPa, pressure maintaining cooling obtains fiber/copolymer composite conducting material;
Polybutylene terephthalate-the polycaprolactone co-polymer the preparation method comprises the following steps: by poly terephthalic acid fourth two
Ester and polycaprolactone are uniformly mixed according to weight ratio 2:1, and stannous octoate is added, and stannous octoate dosage is polycaprolactone quality
1%, nitrogen atmosphere is kept, 5h is stirred to react at 60 DEG C, is cooled to room temperature after reaction, 80 DEG C of vacuum drying obtain for 24 hours
Polybutylene terephthalate-polycaprolactone co-polymer is spare.
Embodiment 4
Take 36 parts of polybutylene terephthalate-polycaprolactone co-polymers, 17 parts of conductive fibers, 7 parts of tea more by weight
Phenol, 24 parts of acetone, 12 parts of E-44 bisphenol A type epoxy resins, 4.5 parts of ethylenediamines, 14.5 parts of polyvinyl alcohol, 7 parts it is polypropylene grafted
Maleic anhydride, 2.5 parts of curing agent F-52A are placed in torque rheometer, 230 DEG C of blending 5min, then with hydraulic forming machine in 265
DEG C, 5min is molded under the conditions of 8MPa, pressure maintaining cooling obtains fiber/copolymer composite conducting material;
Polybutylene terephthalate-the polycaprolactone co-polymer the preparation method comprises the following steps: by poly terephthalic acid fourth two
Ester and polycaprolactone are uniformly mixed according to weight ratio 2:1, and stannous octoate is added, and stannous octoate dosage is polycaprolactone quality
1%, nitrogen atmosphere is kept, 5h is stirred to react at 60 DEG C, is cooled to room temperature after reaction, 80 DEG C of vacuum drying obtain for 24 hours
Polybutylene terephthalate-polycaprolactone co-polymer is spare.
Embodiment 5
Take 40 parts of polybutylene terephthalate-polycaprolactone co-polymers, 16 parts of conductive fibers, 8 parts of tea more by weight
Phenol, 23 parts of acetone, 13 parts of E-44 bisphenol A type epoxy resins, 3 parts of ethylenediamines, 14 parts of polyvinyl alcohol, 5.5 parts of polypropylene grafted horses
Carry out acid anhydrides, 3 parts of curing agent F-52A are placed in torque rheometer, 220 DEG C of blending 5min, then with hydraulic forming machine in 270 DEG C,
5min is molded under the conditions of 7MPa, pressure maintaining cooling obtains fiber/copolymer composite conducting material;
Polybutylene terephthalate-the polycaprolactone co-polymer the preparation method comprises the following steps: by poly terephthalic acid fourth two
Ester and polycaprolactone are uniformly mixed according to weight ratio 2:1, and stannous octoate is added, and stannous octoate dosage is polycaprolactone quality
1%, nitrogen atmosphere is kept, 5h is stirred to react at 60 DEG C, is cooled to room temperature after reaction, 80 DEG C of vacuum drying obtain for 24 hours
Polybutylene terephthalate-polycaprolactone co-polymer is spare.
Comparative example 1
This comparative example is the difference from embodiment 1 is that polybutylene terephthalate-polycaprolactone co-polymer amount is lower than
Claim limited range.Specifically:
Take 20 parts of polybutylene terephthalate-polycaprolactone co-polymers, 18 parts of conductive fibers, 6 parts of tea more by weight
Phenol, 26 parts of acetone, 11 parts of E-44 bisphenol A type epoxy resins, 5 parts of ethylenediamines, 14 parts of polyvinyl alcohol, 8 parts of polypropylene grafted Malaysias
Acid anhydrides, 2 parts of curing agent F-52A are placed in torque rheometer, 240 DEG C of blending 5min, then with hydraulic forming machine in 260 DEG C, 9MPa
Under the conditions of be molded 5min, pressure maintaining cooling obtains fiber/copolymer composite conducting material;
Polybutylene terephthalate-the polycaprolactone co-polymer the preparation method comprises the following steps: by poly terephthalic acid fourth two
Ester and polycaprolactone are uniformly mixed according to weight ratio 2:1, and stannous octoate is added, and stannous octoate dosage is polycaprolactone quality
1%, nitrogen atmosphere is kept, 5h is stirred to react at 60 DEG C, is cooled to room temperature after reaction, 80 DEG C of vacuum drying obtain for 24 hours
Polybutylene terephthalate-polycaprolactone co-polymer is spare.
Comparative example 2
This comparative example the difference from embodiment 1 is that in conductive fiber preparation process ortho phosphorous acid sodium solution drop rate
For 15mL/min.Specifically:
Take 32 parts of polybutylene terephthalate-polycaprolactone co-polymers, 18 parts of conductive fibers, 6 parts of tea more by weight
Phenol, 26 parts of acetone, 11 parts of E-44 bisphenol A type epoxy resins, 5 parts of ethylenediamines, 14 parts of polyvinyl alcohol, 8 parts of polypropylene grafted Malaysias
Acid anhydrides, 2 parts of curing agent F-52A are placed in torque rheometer, 240 DEG C of blending 5min, then with hydraulic forming machine in 260 DEG C, 9MPa
Under the conditions of be molded 5min, pressure maintaining cooling obtains fiber/copolymer composite conducting material;
Polybutylene terephthalate-the polycaprolactone co-polymer the preparation method comprises the following steps: by poly terephthalic acid fourth two
Ester and polycaprolactone are uniformly mixed according to weight ratio 2:1, and stannous octoate is added, and stannous octoate dosage is polycaprolactone quality
1%, nitrogen atmosphere is kept, 5h is stirred to react at 60 DEG C, is cooled to room temperature after reaction, 80 DEG C of vacuum drying obtain for 24 hours
Polybutylene terephthalate-polycaprolactone co-polymer is spare.
Conductive fiber the preparation method comprises the following steps:
Step 1: shearing aramid fiber to 2mm, it is placed in the sodium hydroxide solution of 0.05wt%, 50 DEG C of heating
20min, taking-up are cleaned up with deionized water, add acetone soln, are cleaned by ultrasonic 20min, and taking-up is washed with deionized water,
60 DEG C are dried for standby;
Step 2: taking the aramid fiber 20g handled well in reactor, 100mL 20wt% copper-bath is added, so
0.4g lauryl sodium sulfate is added afterwards and 0.25g polysorbas20,100r/min are stirred evenly, keeps revolving speed, 80mL is then added dropwise
The ortho phosphorous acid sodium solution of 15wt%, drop rate 15mL/min are filtered after reaction, are washed with deionized, and 80 DEG C
12h is dried in vacuo up to conductive fiber.
It is tested for the property fiber/copolymer composite conducting material is prepared in embodiment 1-5 and comparative example 1-2,
Mechanical property is carried out according to GB/T 1040-90, and electric property is carried out according to GB1410-89, and test result see the table below:
Tensile strength/MPa | Impact strength/KJm-2 | Volume resistivity/Ω cm | |
Embodiment 1 | 49.24 | 56.39 | 9.41×105 |
Embodiment 2 | 50.73 | 58.48 | 7.68×104 |
Embodiment 3 | 52.55 | 59.87 | 6.35×103 |
Embodiment 4 | 52.32 | 60.94 | 5.44×102 |
Embodiment 5 | 53.45 | 62.32 | 1.69×102 |
Comparative example 1 | 42.67 | 52.88 | 10.73×105 |
Comparative example 2 | 49.71 | 55.89 | 3.85×106 |
It is raw by test result it is found that fiber/copolymer composite conducting material processing technology for being prepared of the present invention is simple
Produce it is high-efficient, have reliable practical value.The fiber being prepared/copolymer composite conducting material tensile strength is in 49.24-
53.45MPa range, impact strength is in 56.39-62.32KJm-2Range, volume resistivity 1.69 × 102-9.41×105
Ω cm range, preparation method is optimised process in embodiment 5 in the present invention.
Polybutylene terephthalate and polycaprolactone co-polymer are prepared in the present invention, polybutylene terephthalate is
A kind of polyester, a kind of semicrystalline polymeric of polycaprolactone, the two are copolymerized the flexibility, processability and machinery that material can be improved
Performance.
Aramid fiber is subjected to roughing in surface oil removing pretreatment in the present invention, recycles copper sulphate and sodium hypophosphite anti-
It answers, the copper atom of generation can be attached on surface treated aramid fiber, make it have good electric conductivity, ortho phosphorous acid
If too fast will cause of the rate of addition of sodium reacts insufficient, causes the copper atom adhered on fiber less, reduce its electric conductivity
Energy.
Claims (7)
1. a kind of fiber/copolymer composite conducting material preparation method, which is characterized in that including following preparation step: by weight
Amount part take 32-46 parts of polybutylene terephthalate-polycaprolactone co-polymers, 14-18 parts of conductive fibers, 6-10 parts of tea polyphenols,
20-26 parts of acetone, 11-15 parts of epoxy resin, 2-5 parts of ethylenediamines, 14-16 parts of polyvinyl alcohol, 3-8 parts of compatilizers, 2-4 parts of solidifications
Agent is placed in torque rheometer and is blended, then is molded with hydraulic forming machine, and it is compound that pressure maintaining cooling obtains fiber/copolymer
Conductive material.
2. a kind of preparation method of fiber/copolymer composite conducting material according to claim 1, which is characterized in that institute
Stating blending temperature is 200-240 DEG C, and the blending time is 5min.
3. a kind of preparation method of fiber/copolymer composite conducting material according to claim 1, which is characterized in that institute
The temperature for stating molding is 260-280 DEG C, pressure 5-9MPa, time 5min.
4. a kind of preparation method of fiber/copolymer composite conducting material according to claim 1, which is characterized in that institute
State polybutylene terephthalate-polycaprolactone co-polymer the preparation method comprises the following steps:
Polybutylene terephthalate and polycaprolactone are uniformly mixed according to weight ratio 3:1, octoate catalyst stannous is added, is protected
Nitrogen atmosphere is held, 4-6h is stirred to react at 55-75 DEG C, is cooled to room temperature after reaction, 80 DEG C of vacuum drying are gathered for 24 hours
Butylene terephthalate-polycaprolactone co-polymer is spare.
5. a kind of preparation method of fiber/copolymer composite conducting material according to claim 4, which is characterized in that institute
The dosage for stating catalyst in polybutylene terephthalate-polycaprolactone co-polymer preparation method is polycaprolactone quality
1%.
6. a kind of preparation method of fiber/copolymer composite conducting material according to claim 1, which is characterized in that institute
State the preparation method of conductive fiber the following steps are included:
Step 1: shearing aramid fiber to 2mm, it is placed in sodium hydroxide solution, 50 DEG C of heating 20min, takes out and clean, then plus
Enter acetone soln, be cleaned by ultrasonic 20min, cleans, be dried for standby;
Step 2: taking the aramid fiber handled well in reactor, copper-bath is added, lauryl sodium sulfate is then added
And polysorbas20,100r/min are stirred evenly, and keep revolving speed, and ortho phosphorous acid sodium solution is then added dropwise, filters, washes after reaction
It washs, 80 DEG C of vacuum drying 12h are up to conductive fiber.
7. a kind of preparation method of fiber/copolymer composite conducting material according to claim 6, which is characterized in that institute
The drop rate for stating ortho phosphorous acid sodium solution in the preparation method step 2 of conductive fiber is 8mL/min.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN114451608A (en) * | 2022-03-25 | 2022-05-10 | 无锡市锡山人民医院 | Antibacterial degradable polylactic acid protective clothing |
CN115584132A (en) * | 2022-11-08 | 2023-01-10 | 福建省二轻工业研究所有限公司 | Low-temperature shaping material for manufacturing artificial limb mold and preparation method and application thereof |
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2018
- 2018-12-21 CN CN201811572669.2A patent/CN109762303A/en not_active Withdrawn
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
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CN114451608A (en) * | 2022-03-25 | 2022-05-10 | 无锡市锡山人民医院 | Antibacterial degradable polylactic acid protective clothing |
CN114451608B (en) * | 2022-03-25 | 2023-10-31 | 无锡市锡山人民医院 | Antibacterial degradable polylactic acid protective clothing |
CN115584132A (en) * | 2022-11-08 | 2023-01-10 | 福建省二轻工业研究所有限公司 | Low-temperature shaping material for manufacturing artificial limb mold and preparation method and application thereof |
CN115584132B (en) * | 2022-11-08 | 2024-03-22 | 福建省二轻工业研究所有限公司 | Low-temperature molding material for manufacturing artificial limb mold, and preparation method and application thereof |
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