CN105199189B - A kind of temp auto-controlled electric tracing high polymer material and preparation method thereof - Google Patents
A kind of temp auto-controlled electric tracing high polymer material and preparation method thereof Download PDFInfo
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- CN105199189B CN105199189B CN201510550721.4A CN201510550721A CN105199189B CN 105199189 B CN105199189 B CN 105199189B CN 201510550721 A CN201510550721 A CN 201510550721A CN 105199189 B CN105199189 B CN 105199189B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/04—Homopolymers or copolymers of ethene
- C08L23/06—Polyethene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/004—Additives being defined by their length
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2207/00—Properties characterising the ingredient of the composition
- C08L2207/06—Properties of polyethylene
- C08L2207/062—HDPE
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Abstract
The present invention discloses a kind of temp auto-controlled electric tracing high polymer material and preparation method thereof, includes the raw material of following parts by weight proportioning：0.1 0.15 parts of 100 parts of high density polyethylene (HDPE), 40 parts of EVA10,10 20 parts of carbon black, 14 parts of carbon fiber, 0.05 0.15 parts of crosslinking agent, 0.1 0.3 parts of bulking agent, 0.2 0.4 parts of compound stabilizer and fire retardant；The temp auto-controlled electric tracing high polymer material has low percolation threshold, excellent PTC repeatability, excellent mechanical property, heating temp can maintain 100 DEG C, and there is relatively low preparation cost, it is low to overcome current electric tracing high polymer material PTC repeatability, the problems such as poor mechanical property, it is expected to transport in petroleum pipeline, family's heating etc. is applied.
Description
Technical field
The invention belongs to polymer processing field, and in particular to a kind of temp auto-controlled electric tracing high polymer material and its preparation side
Method.
Background technology
New material is guide and the basis of hi-tech development, develops the new high polymer material with special function also
It is the main direction of development of current polymer material science.Conductive polymeric composite with its cost it is low, can adjust on a large scale
Whole electricity and mechanical property, and it is widely used in the fields such as electronic apparatus, national defence, aviation, military affairs.As composite conductive high molecular
One important branch of material, temp auto-controlled electric tracing high polymer material（High molecular based PTC composite）It is that its research is led at present
One of focus of domain concern, and the important topic of countries nowadays field of polymer technology research and development.Macromolecule matrix is processed into
Type is simple, and cost is low, and PTC transition temperatures are low.But high molecular based PTC composite also has many shortcomings, as stability is inadequate,
Mechanical performance is low etc..To solve these problems, domestic and foreign scholars have done substantial amounts of research work.
Polymer has all been carried out largely for the ptc material of matrix in theoretical research and engineer applied technical elements abroad
Research work, the PTC heating element heaters with commercial use are developed, and formed tandem product, what it is such as Raychem companies is
Row product.Scholars are also proposing some novel ideas simultaneously.Soares proposes PS/PIP (polyisoprene) blending ratio
For 40/45 when can form two-arch tunnel, it is PP/PIP/CB three-component compound system Thermodynamic effects that CB, which is distributed at two-phase interface,
Result, and CB is distributed in interface greatly reduces exceeding for compound system and ooze threshold values.Tchoudakov is to high-impact polyphenyl
The research of ethene (HIPS)/SBS (SIS)/CB compound systems shows, finds CB
It is mainly distributed in the big HIPS phases of affinity interaction power；He sends out after also studying PP/ polyamide (PA)/CB compound systems
Existing, CB tends to be distributed in PP/PA interfaces or the big PA phases of affinity interaction power.When matrix formation two-arch tunnel is blended,
Due to it is dual exceed ooze effect, exceed all lower than PP/CB or PA/CB can be obtained and ooze threshold values.Calberg have studied carbon black in polyphenyl
Ethene (PS)/polymethyl methacrylate（PMMA）The distribution in matrix is blended, it is found that CB is mainly distributed at two-phase interface, with
PS/PMMA blending composition is unrelated, interaction force all very littles of this explanation CB and each polymer phase.Narkis have studied
PVDF/UHMWPE/CB, poly- 4- methyl 1- amylenes (TPX)/ultra-high molecular weight polyethylene (UHMWPE)/CB compound system systems
Conducting process, he thinks the high viscosity due to UHMWPE, causes most of CB to be distributed in its surface or TPX phases, so that
The percolation threshold of compound system is lower than unitary system.
Although theoretical research is started late at home, in recent years country support energetically under, and scientist and
Under the joint efforts of enterprise, PTC products and research also emerge in large numbers as emerging rapidly in large numbersBamboo shoots after a spring rain.Typical research has, Hong Kong University of Science and Thchnology
Chan seminars be prepared for two kinds of composites of PVDF/HDPE/CB and ETFE/PVDF/CB, research finds CB selectively
Be dispersed in HDPE phases, and HDPE/CB with disperse phase in ETFE continuous phases, due to HDPE/CB phases and PVDF（ETFE）
Chain lock construction is mutually formd, limits moving freely for CB particles, so both compound systems are all postponed to some extent
The appearance of NTC phenomenons.Zhejiang University etc. be prepared for PA6/PS/CB and PA6/FAN/CB conducing composite materials, result of study
It is dispersed in it was found that carbon black particle is all selective in PA6 phases.This causes system conductive capability to be largely increased.It is prepared by Liang Peiliang
Two kinds are not mixed conductive material PP/PS/CB, NBR/EPDMCB mutually, have studied system process conditions, raw material proportioning, matrix grafting,
It is crosslinked to CB distributions and the influence of electrical property.As a result show not mix characteristic mutually due to matrix, can not only use cheap increasing
Strong CB replaces expensive conductive CB, and can improve the electric conductivity and mechanical property of composite.And by being grafted and handing over
Connection acts on the NTC effects that can substantially eliminate PP/PS/CB systems.The Pei Zhiqiang of Beijing University of Chemical Technology, the Liu Zhi of Zhejiang University
Just, the Hu Hao of Chengdu University of Technology is prepared for HDPE/EVA/CB composites by using EVA parts instead of HDPE, and they study
It was found that a small amount of EVA addition helps to improve processing characteristics, electric conductivity and the mechanical property of body system.Zhou Liyong LLDPE and
EMA's does not mix characteristic mutually, successfully develops the LV series low temperature macromolecule PTC switching device materials suitable for commercial Application.
PTC transition temperatures point is 85 DEG C, old by electricity less than 100 DEG C of the PTC temperature transitions value of China's like product, product far away
The property changed test, is entirely capable of the requirement for meeting commercial Application.The Wu seminars of East China University of Science are by adjusting EVA/LDPE, POE/
LDPE two-phase co-mixing system matrix ratios, mechanical property, electric property, the difference of CB distributions of compound system are have studied, is proposed
LDPE and POE compatibilities are preferably poor with EVA compatibilities.
Although the different degrees of NTC effects for reducing material of the research of above domestic and foreign scholars, also cause simultaneously
PTC intensity or stability of material or the mechanical property of materials sustain damage, so by the method using Double substrate micro insufficient for PTC
Material property obtains General Promotion.
The content of the invention
The technical problem to be solved in the present invention is to provide one kind to have low percolation threshold, and excellent PTC is repeated, excellent
Mechanical property, heating temp can maintain 100 DEG C, and have relatively low preparation cost, overcome current electric tracing macromolecule material
Expect that PTC repeatability is low, the problems such as poor mechanical property, be expected to transport in petroleum pipeline, family's heating etc. be applied from
Temperature control electric tracing high polymer material and preparation method thereof.
To solve the above problems, the present invention adopts the following technical scheme that：
A kind of temp auto-controlled electric tracing high polymer material, include the raw material of following parts by weight proportioning：High density polyethylene (HDPE) 100
It is part, EVA10-40 parts, carbon black 10-20 parts, carbon fiber 1-4 parts, crosslinking agent 0.05-0.15 parts, bulking agent 0.1-0.3 parts, compound
Stabilizer 0.2-0.4 parts and fire retardant 0.1-0.15 parts.
Further, the carbon black is conductive black, and particle diameter 200-300nm, typical oil factor is 150-200cc/
100g。
Further, the carbon fiber is diameter 50-100nm, and length is 1-5mm chopped conductivity type carbon fiber.
Further, the compound stabilizer is antioxidant 3114 [1,3,5- tri-（The hydroxyl benzyl of 3,5- di-t-butyls -4
Base）Isocyanuric acid], solubilizer be ethylene bis stearamide, fire retardant be melamine phosphate.
Further, the crosslinking agent is cumyl peroxide.
Further, carbon black drying silane coupler KH570 processing after acetone treatment 24h, and carbon fiber passes through
Dried after acetone treatment 12h, 4min is handled at 85 DEG C with the 6% KMnO4 aqueous solution.
Another technical problem to be solved by the invention is a kind of preparation method of temp auto-controlled electric tracing high polymer material of offer.
By 100 parts of high density polyethylene (HDPE), EVA 10-40 parts, carbon black 10-20 parts, solubilizer EBS 0.1-0.3 parts through at a high speed
After mixer mixing, in 160 DEG C of mixing 10min of mill, through pulling-on piece, cooling, crush, after sieving, addition carbon fiber 1-4 parts,
Crosslinking agent cumyl peroxide 0.05-0.15 parts, compound stabilizer 0.2-0.4 parts, flame-retardants melamine phosphate 0.1-
0.15 part, after being mixed with high-speed mixer, conducing composite material is obtained using twin-screw extrusion, granulation, finally in compression molding
Tinned wird is pressed on machine, the temp auto-controlled electric tracing high polymer material that width is 1cm is made, this material is through 100 DEG C of post processing 2h
Obtain final temp auto-controlled electric tracing high polymer material.
The beneficial effects of the invention are as follows：Carbon fiber alternatively conductive filler is introduced, cooperates, makes with carbon black
Obtain material property and obtained comprehensive lifting, because carbon fiber forms chain lock construction in the base, so significantly reducing
The percolation threshold of material, while also the stability of material and mechanical performance are improved.
Brief description of the drawings
Fig. 1 is the preparation flow figure of temp auto-controlled electric tracing high polymer material in the present invention；
Fig. 2 is the typical resistance-temperature curve figure of temp auto-controlled electric tracing high polymer material in the present invention；
Fig. 3 is the power on/off loop test curve map of temp auto-controlled electric tracing high polymer material in the present invention.
Embodiment
With reference to embodiment to invention be specifically described, it is necessary to it is pointed out here that be the present embodiment be served only for this
Invention is further described, but the embodiment should not be construed as limiting the scope of the invention, and the technology in the field is ripe
Some nonessential modifications and adaptations can be made according to the content of the invention described above by practicing personnel.
Embodiment 1
A kind of temp auto-controlled electric tracing high polymer material, it is characterised in that the composite-material formula is by weight：High density
Polyethylene（HDPE, MFI=0.8g/10min, d=0.96g/cm3）100 parts, EVA（MFI=2g/10min, d=0.94g/cm3）10
Part, carbon black（CB, DBP oil factor 174cc/100g, particle diameter 30nm, through γ-（Methacryloxypropyl）Propyl trimethoxy silicane is even
Join agent processing）13 parts, carbon fiber（CF, 7 μm of diameter, length 2mm, 25 DEG C of specific insulations, 6 × 10-3, at potassium permanganate
Reason）2 parts, cumyl peroxide（Fusing point=42 DEG C, relative density 1.082g/cm3, decomposition temperature=125 DEG C）0.05 part, ethylene
Bis-stearamides（Fusing point=146 DEG C, density=0.98g/cm3）0.1 part, 1,3,5- tri-（The hydroxybenzyl of 3,5- di-t-butyls -4）It is different
Cyanuric acid（Fusing point=220 DEG C, density=1.03g/cm3）0.2 part, melamine phosphate（Decomposition temperature=300 DEG C）0.1 part.
Embodiment 2
A kind of temp auto-controlled electric tracing high polymer material, it is characterised in that the composite-material formula is by weight：High density
Polyethylene（HDPE, MFI=0.8g/10min, d=0.96g/cm3）100 parts, EVA（MFI=2g/10min, d=0.94g/cm3）20
Part, carbon black（CB, DBP oil factor 174cc/100g, particle diameter 30nm, through γ-（Methacryloxypropyl）Propyl trimethoxy silicane is even
Join agent processing）12 parts, carbon fiber（CF, 7 μm of diameter, length 2mm, 25 DEG C of specific insulations, 6 × 10-3, handled through potassium permanganate）
3 parts, cumyl peroxide（Fusing point=42 DEG C, relative density 1.082g/cm3, decomposition temperature=125 DEG C）0.1 part, ethylene it is double hard
Acyl amine（Fusing point=146 DEG C, density=0.98g/cm3）0.2 part, 1,3,5- tri-（The hydroxybenzyl of 3,5- di-t-butyls -4）Isocyanide is urinated
Acid（Fusing point=220 DEG C, density=1.03g/cm3）0.3 part, melamine phosphate（Decomposition temperature=300 DEG C）0.12 part.
Embodiment 3
A kind of temp auto-controlled electric tracing high polymer material, it is characterised in that the composite-material formula is by weight：High density
Polyethylene（HDPE, MFI=0.8g/10min, d=0.96g/cm3）100 parts, EVA（MFI=2g/10min, d=0.94g/cm3）30
Part, carbon black（CB, DBP oil factor 174cc/100g, particle diameter 30nm, through γ-（Methacryloxypropyl）Propyl trimethoxy silicane is even
Join agent processing）14 parts, carbon fiber（CF, 7 μm of diameter, length 2mm, 25 DEG C of specific insulations, 6 × 10-3, handled through potassium permanganate）
1 part, cumyl peroxide（Fusing point=42 DEG C, relative density 1.082g/cm3, decomposition temperature=125 DEG C）0.15 part, ethylene pair
Stearmide（Fusing point=146 DEG C, density=0.98g/cm3）0.3 part, 1,3,5- tri-（The hydroxybenzyl of 3,5- di-t-butyls -4）Isocyanide
Uric acid（Fusing point=220 DEG C, density=1.03g/cm3）0.4 part, melamine phosphate（Decomposition temperature=300 DEG C）0.15 part.
Embodiment effect is as shown in the table
Preparation method：
As shown in fig.1, first by CB, CF acetone soak 48h, filtering, the drying under the conditions of 80 DEG C is until constant weight, so
Afterwards by CB 2% KH570 alcohol solution dipping 6h, filtering, 80 DEG C of dryings to constant weight.CF is with the 6% KMnO4 aqueous solution at 85 DEG C
4min is handled, filtering, 80 DEG C are dried under vacuum to constant weight.
By HDPE, EVA and modified CB mill 10min at 160 DEG C, after pulling-on piece, cooling, broken, sieving, oxidation is added
Carbon fiber, cumyl peroxide, compound stabilizer, flame-retardants melamine phosphate, after being mixed with high-speed mixer, use
Twin-screw extrusion, granulation obtain conducing composite material, and extrusion condition is as shown in the table：
As shown in fig.2, the room temperature from this material of temp auto-controlled electric tracing high polymer material resistance-temperature curve it can be seen from the figure that
Resistivity is 1 × 103, positive temperature coefficient（PTC intensity）For 3, there is not negative temperature effect（NTC）, it is shown that preferable PTC
Effect.
As shown in fig.3, prepared temp auto-controlled electric tracing high polymer material, after 100 power on/off circulation experiments, room
Warm change in resistance rate is 0.005%, and heating power rate of change is 0.01%, it is shown that preferable cyclical stability.
The beneficial effects of the invention are as follows：Carbon fiber alternatively conductive filler is introduced, cooperates, makes with carbon black
Obtain material property and obtained comprehensive lifting, because carbon fiber forms chain lock construction in the base, so significantly reducing
The percolation threshold of material, while also the stability of material and mechanical performance are improved.
The foregoing is only a specific embodiment of the invention, but protection scope of the present invention is not limited thereto, any
The change or replacement expected without creative work, it should all cover within the scope of the present invention.
Claims (5)
- A kind of 1. temp auto-controlled electric tracing high polymer material, it is characterised in that：Include the raw material of following parts by weight proportioning：High density 100 parts of polyethylene, EVA10-40 parts, carbon black 10-20 parts, carbon fiber 1-4 parts, crosslinking agent 0.05-0.15 parts, bulking agent 0.1- 0.3 part, compound stabilizer 0.2-0.4 parts and fire retardant 0.1-0.15 parts；The carbon black is conductive black, and particle diameter 200-300nm, typical oil factor is 150-200cc/100g；The carbon fiber is diameter 50-100nm, and length is 1-5mm chopped conductivity type carbon fiber.
- 2. temp auto-controlled electric tracing high polymer material as claimed in claim 1, it is characterised in that the compound stabilizer is anti-oxidant [the 1,3,5- tri- of agent 3114（The hydroxybenzyl of 3,5- di-t-butyls -4）Isocyanuric acid], solubilizer be ethylene bis stearamide, fire-retardant Agent is melamine phosphate.
- 3. temp auto-controlled electric tracing high polymer material as claimed in claim 1, it is characterised in that the crosslinking agent is that peroxidating two is different Propyl benzene.
- 4. temp auto-controlled electric tracing high polymer material as claimed in claim 1, it is characterised in that the carbon black is through acetone treatment 24h Silane coupler KH570 processing is used in drying afterwards, and carbon fiber is dried after acetone treatment 12h, with the 6% KMnO4 aqueous solution 85 DEG C processing 4min.
- A kind of 5. preparation method of temp auto-controlled electric tracing high polymer material as claimed in claim 1, it is characterised in that：By high density 100 parts of polyethylene, EVA10-40 parts, carbon black 10-20 parts, solubilizer EBS0.1-0.3 parts are after high-speed mixer mixes, Yu Kai 160 DEG C of mixing 10min of mill, after pulling-on piece, cooling, broken, sieving, add carbon fiber 1-4 parts, crosslinking agent peroxidating diisopropyl Benzene 0.05-0.15 parts, compound stabilizer 0.2-0.4 parts, flame-retardants melamine phosphate 0.1-0.15 parts, use high-speed mixer After mixing, conducing composite material is obtained using twin-screw extrusion, granulation, tinned wird is finally pressed on vulcanizing press, is made The temp auto-controlled electric tracing high polymer material that width is 1cm is obtained, this material obtains final temp auto-controlled electricity companion through 100 DEG C of post processing 2h Hot high polymer material.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1343560A (en) * | 2000-09-18 | 2002-04-10 | 扬州芬尔机械配件有限公司 | Process for preparing high molecular based PTC material |
| CN1844232A (en) * | 2005-04-06 | 2006-10-11 | 富致科技股份有限公司 | Positive temperature coefficient polymer composition and circuit protection device made therefrom |
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2015
- 2015-09-01 CN CN201510550721.4A patent/CN105199189B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1343560A (en) * | 2000-09-18 | 2002-04-10 | 扬州芬尔机械配件有限公司 | Process for preparing high molecular based PTC material |
| CN1844232A (en) * | 2005-04-06 | 2006-10-11 | 富致科技股份有限公司 | Positive temperature coefficient polymer composition and circuit protection device made therefrom |
Non-Patent Citations (2)
| Title |
|---|
| EVA 对HDPE /EVA/CB 导电复合材料性能的影响;李晓林 等;《塑料》;20070430;第36卷(第2期);第5-8页 * |
| 聚乙烯/炭黑/碳纤维复合材料阻温特性;沈烈 等;《复合材料学报》;20010831;第18卷(第3期);第18-21页 * |
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