CN106751468A - A kind of composite with high-temperature dielectric and preparation method thereof - Google Patents
A kind of composite with high-temperature dielectric and preparation method thereof Download PDFInfo
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- CN106751468A CN106751468A CN201611034100.1A CN201611034100A CN106751468A CN 106751468 A CN106751468 A CN 106751468A CN 201611034100 A CN201611034100 A CN 201611034100A CN 106751468 A CN106751468 A CN 106751468A
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- 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
- C08J3/24—Crosslinking, e.g. vulcanising, of macromolecules
- C08J3/246—Intercrosslinking of at least two polymers
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L27/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers
- C08L27/02—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L27/12—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
- C08L27/18—Homopolymers or copolymers or tetrafluoroethene
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2363/00—Characterised by the use of epoxy resins; Derivatives of epoxy resins
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- 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
- C08J2427/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers
- C08J2427/02—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
- C08J2427/12—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
- C08J2427/18—Homopolymers or copolymers of tetrafluoroethylene
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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
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/24—Crystallisation aids
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08L2312/00—Crosslinking
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Abstract
It is prepared from the invention discloses a kind of composite with high-temperature dielectric and preparation method thereof, including following weight portion raw material：10 20 parts of epoxy resin, 10 20 parts of polytetrafluoroethylene (PTFE), 5 15 parts of propyl acetate, 5 15 parts of policapram, 25 parts of polypyrrole, 5 10 parts of silicon tetrachloride, 0.1 0.5 parts of nano barium phthalate, 15 parts of crosslinking agent；Composite of the present invention has dielectric constant big, and operating temperature advantage high promotes the application on the electronic device that polymer dielectric material for electrical works in hot environment.
Description
Technical field
The present invention relates to field of compound material, and in particular to a kind of with the composite of high-temperature dielectric and its preparation side
Method.
Background technology
With the fast development of hyundai electronicses science and technology, dielectric properties and electronics unit of the increasing application to electronic material
The miniaturization of part proposes requirement higher, and people are in the urgent need to high-k, low-loss, while having higher force
The dielectric material of performance and processability, the importance that this allows for high dielectric constant material is increasingly notable.Polymer matrix is answered
Dielectric material is closed due to receiving the concern of scientific research personnel with preferable mechanical performance, processing characteristics and insulating properties.
Capacitor is one of a large amount of electronic components for using in electronic equipment, as market demands are improved constantly, electronics
The working environment of information products equipment application is increasingly harsher (high temperature, low temperature etc.), such as field such as Aero-Space, oil drilling
Operating temperature range is already higher than 150 DEG C, or even the operating ambient temperature having is far above normal operating temperatures, such as manned aviation boat
My god, rocket satellite etc., these require that dielectric material has dielectric constant and low Rong Wenbian high within the scope of temperature wide
Rate.
Although however, having one on chemical property by the polymer matrix composite dielectric material for simply mixing
Fixed raising, also overcomes segmental defect, but still is difficult to meet electron trade to the higher and higher performance requirement of electronic material,
Therefore, deeply the polymer matrix composite dielectric material of research and development higher performance is still the direction of electronic material development from now on.
The content of the invention
It is an object of the invention to the low defect of the operating temperature for overcoming existing macromolecule composite dielectric material to exist, there is provided
A kind of composite with high-temperature dielectric and preparation method thereof；The present invention is using the analysis of high molecular polymerization, crosslinking and crystal
Go out principle, make it have dielectric constant greatly, operating temperature advantage high promotes polymer dielectric material for electrical work in hot environment
Application on the electronic device of work.
In order to realize foregoing invention purpose, the invention provides a kind of composite with high-temperature dielectric, including with
Lower weight portion raw material are prepared from：10-20 parts of epoxy resin, 10-20 parts of polytetrafluoroethylene (PTFE), 5-15 parts of poly-vinegar acid third
Ester, 5-15 parts of policapram, 2-5 parts of polypyrrole, 5-10 parts of silicon tetrachloride, 0.1-0.5 parts of nano barium phthalate, 1-5
The crosslinking agent of part.
A kind of composite with high-temperature dielectric, using mutual polymerization, crosslinking between gas chromatography, forms knot
Structure stabilization, high temperature-resistant polymer three-dimensional net structure, while poly- containing what is formed using nucleator in three-dimensional net structure
Compound is crystallized, the Interaction enhanced of the polymer crystallization and electric field, dielectric constant increase；Meanwhile, three-dimensional net structure makes to gather
Compound fusing point increases, and its operating temperature is higher；The composite dielectric material is bigger using scope, is conducive to the development of electron trade.
Preferably, wherein described molecular weight of epoxy resin is 1000-20000.
Preferably, wherein the described poly-vinegar propyl propionate degree of polymerization is 100-200.
Preferably, wherein the described polytetrafluoroethylene (PTFE) degree of polymerization is 200-500.
Preferably, wherein the described policapram degree of polymerization is 100-200.
Preferably, wherein the described polypyrrole degree of polymerization is 100-200, the degree of polymerization is too big, poor dielectric performance；The degree of polymerization
Too small, electric conductivity is high, uncomfortable cooperation dielectric material.
Preferably, wherein the particle diameter of described nano barium phthalate is 5-20 nanometers, particle diameter is too big, is unfavorable for macromolecular material
Crystallization nucleation；Particle diameter is too small, difficulties in dispersion, easily reunites.
Preferably, a kind of composite with high-temperature dielectric, including following weight portion raw material is prepared from：
10-20 parts of epoxy resin, 10-20 parts of polytetrafluoroethylene (PTFE), 5-10 parts of propyl acetate, 10-15 parts of policapram, 2-3
The polypyrrole of part, 5-8 parts of silicon tetrachloride, 0.1-0.3 parts of nano barium phthalate, 2-3 parts of crosslinking agent.
In order to realize foregoing invention purpose, further, the invention provides a kind of composite wood with high-temperature dielectric
The preparation method of material, comprises the following steps：
（1）Propyl acetate glycerine is dissolved to form solution, nano barium titanate calcium is added in the solution, crystallized after being uniformly dispersed
Separate out, obtain propyl acetate crystalline material；
（2）It is propyl acetate crystalline material that step 1 is obtained and epoxy resin, polytetrafluoroethylene (PTFE), silicon tetrachloride, polypyrrole, poly-
Cross-linking reaction is carried out after acetamide, crosslinking agent mixing, the composite with high-temperature dielectric is obtained.
A kind of preparation method of the composite with high-temperature dielectric, propyl acetate first dissolved to form solution, then profit
Nucleator is done with nano barium titanate calcium, propyl acetate is crystallized and is separated out the crystalline material as can be stronger with the interaction of electric field,
So that the dielectric constant increase of polymeric material；Finally with the crosslinking of other macromolecular materials, form with three-dimensional network
The composite with high-temperature dielectric of structure, increases melting point polymer, and its operating temperature is higher；There should be high-temperature dielectric
Property composite preparation method is simple, stabilization, reliable, be adapted to extensive, the work of the composite with high-temperature dielectric
Industry metaplasia is produced.
Preferably, the cross-linking reaction temperature is 240-280 DEG C, and crosslinking temperature is too high, is crosslinked transition, the three dimensional network of formation
Network irregular structure, properties of product reduction, crosslinking temperature is too low, and the reaction time is oversize, and the production cycle is long.
Preferably, the time of the cross-linking reaction is 1-3h, and the reaction time is long, and the production cycle is long, and efficiency is low, during reaction
Between it is too short, reaction is incomplete, properties of product reduction.
Compared with prior art, beneficial effects of the present invention：
1st, composite of the present invention with high-temperature dielectric contains the propyl acetate crystalline material separated out using nucleator crystallization,
With the characteristic stronger with the interaction of electric field, with dielectric constant higher.
2nd, the preparation method of composite of the present invention with high-temperature dielectric first passes through recrystallization, recycles crosslinking, will
Crystalline material is dispersed in three-dimensional net structure system, so as to increased the fusing point and dielectric constant of composite.
3rd, the preparation method of composite of the present invention with high-temperature dielectric is simple, stable, reliable, is adapted to have high temperature
Extensive, the industrialized production of the composite of dielectricity.
Specific embodiment
With reference to test example and specific embodiment, the present invention is described in further detail.But this should not be understood
For the scope of above-mentioned theme of the invention is only limitted to following embodiment, all technologies realized based on present invention belong to this
The scope of invention.
Embodiment 1
（1）The poly-vinegar propyl propionate glycerine that 10 weight parts of polymer degree are 150 is dissolved to form solution, 0.3 weight is added in the solution
Amount part nano barium titanate calcium, crystallization precipitation is carried out after being uniformly dispersed, and obtains poly-vinegar propyl propionate crystalline material；
（2）The poly-vinegar propyl propionate crystalline material and the molecular weight of 15 weight portions that step 1 is obtained are 5000 epoxy resin, 15 weights
The degree of polymerization for measuring part is 300 polytetrafluoroethylene (PTFE), the silicon tetrachloride of 8 weight portions, polypyrrole, 10 that 3 weight parts of polymer degree are 150
After the degree of polymerization of weight portion is the 150 crosslinking agent mixing of policapram, 3 weight portions, carry out being crosslinked at a temperature of 260 DEG C anti-
3h is answered, the composite with high-temperature dielectric is obtained.
Embodiment 2
（1）The poly-vinegar propyl propionate glycerine that 15 weight parts of polymer degree are 100 is dissolved to form solution, 0.1 weight is added in the solution
Amount part nano barium titanate calcium, crystallization precipitation is carried out after being uniformly dispersed, and obtains poly-vinegar propyl propionate crystalline material；
（2）The poly-vinegar propyl propionate crystalline material and the molecular weight of 10 weight portions that step 1 is obtained are 1000 epoxy resin, 20 weights
Measure part the degree of polymerization be 500 polytetrafluoroethylene (PTFE), the silicon tetrachloride of 10 weight portions, the polypyrrole that 5 weight parts of polymer degree are 200,
The degree of polymerization of 15 weight portions be 100 policapram, 5 weight portions crosslinking agent mixing after, be crosslinked at a temperature of 280 DEG C
Reaction 1h, obtains the composite with high-temperature dielectric.
Embodiment 3
（1）The poly-vinegar propyl propionate glycerine that 5 weight parts of polymer degree are 200 is dissolved to form solution, 0.5 weight is added in the solution
Part nano barium titanate calcium, crystallization precipitation is carried out after being uniformly dispersed, and obtains poly-vinegar propyl propionate crystalline material；
（2）Poly-vinegar propyl propionate crystalline material and the molecular weight of 20 weight portions that step 1 is obtained are 20000 epoxy resin, 10
The degree of polymerization of weight portion be 200 polytetrafluoroethylene (PTFE), the silicon tetrachloride of 5 weight portions, the polypyrrole that 1 weight parts of polymer degree is 100,
The degree of polymerization of 5 weight portions be 200 policapram, 2 weight portions crosslinking agent mixing after, be crosslinked at a temperature of 240 DEG C
Reaction 3h, obtains the composite with high-temperature dielectric.
Embodiment 4
（1）The poly-vinegar propyl propionate glycerine that 10 weight parts of polymer degree are 200 is dissolved to form solution, 0.2 weight is added in the solution
Amount part nano barium titanate calcium, crystallization precipitation is carried out after being uniformly dispersed, and obtains poly-vinegar propyl propionate crystalline material；
（2）Poly-vinegar propyl propionate crystalline material and the molecular weight of 10 weight portions that step 1 is obtained are 20000 epoxy resin, 20
The degree of polymerization of weight portion be 200 polytetrafluoroethylene (PTFE), the silicon tetrachloride of 5 weight portions, the polypyrrole that 1 weight parts of polymer degree is 100,
The degree of polymerization of 15 weight portions be 200 policapram, 1 weight portion crosslinking agent mixing after, be crosslinked at a temperature of 270 DEG C
Reaction 1.5h, obtains the composite with high-temperature dielectric.
Comparative example 1
（1）The poly-vinegar propyl propionate glycerine that 10 weight parts of polymer degree are 150 is dissolved to form solution, crystallization precipitation is carried out, obtained
Poly-vinegar propyl propionate crystalline material；
（2）The poly-vinegar propyl propionate crystalline material and the molecular weight of 15 weight portions that step 1 is obtained are 5000 epoxy resin, 15 weights
The degree of polymerization for measuring part is 300 polytetrafluoroethylene (PTFE), the silicon tetrachloride of 8 weight portions, polypyrrole, 10 that 3 weight parts of polymer degree are 150
After the degree of polymerization of weight portion is the 150 crosslinking agent mixing of policapram, 3 weight portions, carry out being crosslinked at a temperature of 260 DEG C anti-
3h is answered, the composite with high-temperature dielectric is obtained.
Comparative example 2
（1）The poly-vinegar propyl propionate glycerine that 10 weight parts of polymer degree are 150 is dissolved to form solution, 0.3 weight is added in the solution
Amount part nano barium titanate calcium, crystallization precipitation is carried out after being uniformly dispersed, and obtains poly-vinegar propyl propionate crystalline material；
（2）The poly-vinegar propyl propionate crystalline material and the molecular weight of 15 weight portions that step 1 is obtained are 5000 epoxy resin, 15 weights
The degree of polymerization for measuring part is 300 polytetrafluoroethylene (PTFE), the silicon tetrachloride of 8 weight portions, the poly- acetyl that the degree of polymerization of 10 weight portions is 150
After amine, the crosslinking agent mixing of 3 weight portions, cross-linking reaction 3h is carried out at a temperature of 260 DEG C, obtain compound with high-temperature dielectric
Material.
Comparative example 3
By being polymerized for the nano barium phthalate of 0.3 weight portion and the epoxy resin, 15 weight portions that the molecular weight of 15 weight portions is 5000
Spend the polytetrafluoroethylene (PTFE) for 300, the silicon tetrachloride of 8 weight portions, the polypyrrole that 3 weight parts of polymer degree are 150,10 weight portions it is poly-
After the crosslinking agent mixing of the right policapram, 3 weight portions for being 150, cross-linking reaction 3h is carried out at a temperature of 260 DEG C, must had
There is the composite of high-temperature dielectric.
The preparation-obtained composite with high-temperature dielectric in above-described embodiment 1-4 and comparative example 1-3 is carried out
Performance detection（25 DEG C, 10KHz）, experimental result is recorded, record data is as follows：
| Numbering | Dielectric constant | Maximum operation (service) temperature（℃） |
| Embodiment 1 | 32 | 220 |
| Embodiment 2 | 31 | 210 |
| Embodiment 3 | 29 | 215 |
| Embodiment 4 | 30 | 205 |
| Comparative example 1 | 20 | 210 |
| Comparative example 2 | 23 | 170 |
| Comparative example 3 | 19 | 165 |
Above-mentioned analysis of experimental data is understood, is situated between with high temperature using what technical solution of the present invention was prepared in embodiment 1-4
Big, the maximum temperature in use of electrical composite dielectric constant is high；Meanwhile, contrasting all embodiment 1-4 and comparative example 1-3 can
Know, nano barium phthalate does not use nano barium titanate to the dielectric constant of the main influence composite of composite in comparative example 1
Barium, it is impossible to form the crystalline material of barium titanate-poly-vinegar propyl propionate, the poly-vinegar propyl propionate for obtaining is weak to electric field interaction, its Jie
Electric constant is significantly reduced；Do not use the three-dimensional network configuration of polypyrrole, formation to there is fault of construction in comparative example 2, be crosslinked shape
Into its dielectric constant of polymer and maximum operation (service) temperature significantly reduce；In comparative example 3 directly by nano barium phthalate with it is poly-
Compound carries out cross-linked polymeric, does not exist, the crystalline material of barium titanate-poly-vinegar propyl propionate, and interact weak, dielectric constant to electric field
It is low, meanwhile, the three-dimensional network configuration being cross-linked to form also has certain defect, and the temperature in use of composite is significantly reduced.
Claims (10)
1. a kind of composite, it is characterised in that be prepared from including following weight portion raw material：10-20 parts of epoxy resin,
10-20 parts of polytetrafluoroethylene (PTFE), 5-15 parts of poly-vinegar propyl propionate, 5-15 parts of policapram, 2-5 parts of polypyrrole, 5-10 parts
Silicon tetrachloride, 0.1-0.5 parts of nano barium phthalate, 1-5 parts of crosslinking agent.
2. composite according to claim 1, it is characterised in that be prepared from including following weight portion raw material：10-
20 parts of epoxy resin, 10-20 parts of polytetrafluoroethylene (PTFE), 5-10 parts of propyl acetate, 10-15 parts of policapram, 2-3 parts
Polypyrrole, 5-8 parts of silicon tetrachloride, 0.1-0.3 parts of nano barium phthalate, 2-3 parts of crosslinking agent.
3. composite according to claim 1, it is characterised in that the molecular weight of epoxy resin is 1000-20000.
4. composite according to claim 1, it is characterised in that the polytetrafluoroethylene (PTFE) degree of polymerization is 200-500.
5. composite according to claim 1, it is characterised in that the policapram degree of polymerization is 100-200.
6. composite according to claim 1, it is characterised in that the polypyrrole degree of polymerization is 100-200.
7. composite according to claim 1, it is characterised in that the particle diameter of the nano barium phthalate is 1-20nm.
8. the preparation method of composite described in a kind of claim 1, it is characterised in that comprise the following steps：
（1）Propyl acetate glycerine is dissolved to form solution, nano barium titanate calcium is added in the solution, crystallized after being uniformly dispersed
Separate out, obtain propyl acetate crystalline material；
（2）It is propyl acetate crystalline material that step 1 is obtained and epoxy resin, polytetrafluoroethylene (PTFE), silicon tetrachloride, polypyrrole, poly-
Cross-linking reaction is carried out after acetamide, crosslinking agent mixing, the composite with high-temperature dielectric is obtained.
9. preparation method according to claim 8, it is characterised in that cross-linking reaction temperature is 240-280 DEG C in step 3.
10. preparation method according to claim 8, it is characterised in that cross-linking reaction time is 1-3h in step 3.
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| CN201611034100.1A CN106751468A (en) | 2016-11-23 | 2016-11-23 | A kind of composite with high-temperature dielectric and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107266867A (en) * | 2017-07-10 | 2017-10-20 | 合肥雄川机械销售有限公司 | A kind of preparation method of sower defertilizing box |
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2016
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107266867A (en) * | 2017-07-10 | 2017-10-20 | 合肥雄川机械销售有限公司 | A kind of preparation method of sower defertilizing box |
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Application publication date: 20170531 |