CN103073686A - High thermal stability polymer matrix conductive composite and method for preparing self-regulating heating cable by adopting high thermal stability polymer matrix conductive composite - Google Patents
High thermal stability polymer matrix conductive composite and method for preparing self-regulating heating cable by adopting high thermal stability polymer matrix conductive composite Download PDFInfo
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- CN103073686A CN103073686A CN2013100041331A CN201310004133A CN103073686A CN 103073686 A CN103073686 A CN 103073686A CN 2013100041331 A CN2013100041331 A CN 2013100041331A CN 201310004133 A CN201310004133 A CN 201310004133A CN 103073686 A CN103073686 A CN 103073686A
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Abstract
The invention discloses a high thermal stability polymer matrix conductive composite which is prepared from polymer, conductive filler, polymerizable polar monomer, inorganic filler and processing agent. The invention further discloses a method for preparing a self-regulating heating cable by adopting the high thermal stability polymer matrix conductive composite. The polymer matrix conductive composite is added with the polymerizable polar monomer to strengthen the stability of a conductive network in the composite and reduce the interface resistance between the conductive composite and an electrode after the heating cable is placed at a high temperature, therefore, the polymer matrix conductive composite has good resistance reproducibility and stability. The self-regulating heating cable is prepared by using an initiator to achieve stem grafting, so that the processing process is simple, and the cost is low.
Description
Technical field
The present invention is a kind of to relate to polymer-based conducing composite material, is specifically related to the polymer-based conducing composite material of a kind of high thermal stability, and Bian with this matrix material preparation from the method for limitting warm accompanying-heat cable.
Background technology
The resistivity of polymer-based conducing composite material has the characteristic that varies with temperature and change, when energising, and the circuit persistent fever, when high temperature phenomenon occured when, its resistance can be elevated to a high value state moment, makes cable be in trip condition, to reach the purpose of limit temperature.Therefore, conductive polymer composites can be prepared into the heat generating core band is applied in the cable.
Polymer-based conducing composite material generally is composited by polymer base material and conductive filler material, is uniformly distributed in the described polymer base material on the conductive filler material macroscopic view.Polymer is generally polyolefine and multipolymer thereof, such as polyethylene or ethylene-propylene copolymer etc., and conductive filler material the most frequently used be carbon black and electrically conductive graphite.Carbon black is made the polymer-based conducing composite material of conductive filler material, because special aggregate structure and its surface of carbon black has polar group, and the normally surperficial nonpolarity group of polyphosphazene polymer alkene presents inertia, thereby the cohesive force of carbon black and macromolecule matrix is relatively poor.When the accompanying-heat cable of preparation is limit temperature certainly in heating, because carbon black is from agglomeration, get back to normal temperature carbon black and polymer phase-splitting, form conductive chain by carbon black in the macromolecule matrix destroyed gradually along with using, the normal temperature state resistance rises gradually, heating power reduces or is deteriorated, has reduced work-ing life and the reliability of operation of accompanying-heat cable.
In addition, because conductive electrode is metal, its surface is polarity, and macromolecule surface is inertia, when jacketed electrode, cohesive force also relatively a little less than.When limit was warm, because the greatest differences of metal and macromolecular material coefficient of thermal expansion, when getting back to normal temperature, the interface resistance between electrode and the polymer-based conducing composite material also increased thereupon, has influence on equally the normal use of accompanying-heat cable in the accompanying-heat cable heating.
At present, though the cohesive force of adding between all kinds of coupling agents to improve polymers and the carbon black is arranged, coupling agent one terminal polar group group and carbon black reaction, the other end organic group and polymer form physics " entanglement ", thereby have slowed down the certainly reunion of carbon black in the macromolecule matrix; But, owing to be the organic group of short chain on the coupling agent, and the physics between the high molecular long chain molecule " entanglement " power is still lower.If the long period is under the environment of high-temperature, normal temperature resistance still can significantly raise, and affects the validity of its work-ing life and operation.In addition, coupling agent is also relatively complicated to the process of surface treatment of carbon black, and cost is also higher.
Summary of the invention
The present invention aims to provide that a kind of electrical specification is stable, the polymer-based conducing composite material of high thermal stability of long service life, and the present invention also provides Bian, and oneself limits the method for warm accompanying-heat cable with this matrix material preparation.
One of the present invention discloses the polymer-based conducing composite material of a kind of high thermal stability, and it comprises to be mixed with by polymer, conductive filler material, polymerisable polar monomer, mineral filler and processing aid and forms, and the volume percent of each component is as follows:
(1) concrete, the high molecular volume percent of the above crystallinity or hemicrystalline is preferably more than 25% greater than 15%, and more excellent is greater than 35%; The volume percent of conductive filler material is preferably greater than 30% greater than 25%, and more excellent is greater than 35%; The volume percent of polymerisable polar monomer is preferably greater than 1% greater than 0.5%, and more excellent is greater than 2%; The volume percent of mineral filler is less than 30%, and preferably less than 25%, more excellent is less than 20%; Initiator is preferred 1% in the processing aid, and preferably less than 0.8%, more excellent is 0.6%.
(2) on the basis of such scheme, crystallinity or hemicrystalline polymer are one or more in polypropylene, polyvinylidene difluoride (PVDF), polyolefin elastomer, polyethylene, ethylene-tetrafluoroethylene copolymer, polymethylmethacrylate, the ethylene-propylene copolymer.Wherein polyethylene is Low Density Polyethylene, linear low density polyethylene, medium-density polyethylene or high density polyethylene(HDPE), and poly melting index is elected 0.1 ~ 15.0 g/10min as, is preferably 0.3 ~ 10.0g/10min; Poly Vicat softening point selects 95 ℃, is preferably 100 ℃.
(3) on the basis of such scheme, polymerisable polar monomer is one or more in acid anhydrides, (methyl) vinylformic acid (fat), vinyl cyanide, acid amides, peptamine and the unsaturated amine.
(4) on the basis of such scheme, conductive filler material is that particle diameter is carbon black or graphite, and wherein the particle diameter of carbon black is 10nm～10 μ m, preferred 30nm ~ 1um, the iodine absorption value 40～300cc/kg of carbon black, BET nitrogen adsorption method specific surface area 30 ~ 80m
2/ g.
(5) on the basis of such scheme, mineral filler is one or more in enhancing carbon black, laminar nano polynite, nanometer or micro-calcium carbonate, magnesium oxide, aluminum oxide and the zinc oxide.Wherein, the enhancing particle size carbon black is 60 ~ 150nm, and its dibutyl phthalate absorption is 50 ~ 120cc/100g, and BET nitrogen specific absorption surface-area is less than 30m
2/ g; Other mineral fillers are laminar nano polynite, nanometer or micro-calcium carbonate, magnesium oxide, aluminum oxide or zinc oxide, and particle diameter is preferentially less than 1um.
(6) on the basis of such scheme, processing aid is one or more in initiator, oxidation inhibitor, lubricant, metal deactivator and the fire retardant.Wherein, initiator is one or more of organo-peroxide, azo-initiator and redox initiator, and described organic peroxide evocating agent is benzoyl peroxide and/or dicumyl peroxide; Described azo-initiator is Diisopropyl azodicarboxylate or 2,2'-Azobis(2,4-dimethylvaleronitrile); Described redox initiator is hydrogen peroxide/iron protochloride or isopropyl benzene hydroperoxide/tetrem alkene imines;
Above-mentioned oxidation inhibitor is primary antioxidant (phenols or aminated compounds are such as oxidation inhibitor ANOX20) and secondary oxidation inhibitor (ortho-phosphoric acid ester class or sulfide are such as AT168).
Above-mentioned lubricant is metal soap (such as stearate) or saturated hydrocarbons (such as polyethylene wax);
Above-mentioned metal deactivator is selected MD1024;
Above-mentioned fire retardant is magnesium hydroxide or aluminium hydroxide.
2, Bian limits the method for warm accompanying-heat cable as follows with the polymer-based conducing composite material preparation of the present invention certainly:
(1) polymer base material, conductive filler material, polymerisable polar monomer, mineral filler, initiator and auxiliary agent are dropped into mixing equipment by recipe ratio, under the temperature that is higher than more than the polymer melt temperature, carry out melting mixing.Mixing equipment can be torque rheometer, Banbury mixer, mill, single screw extrusion machine or twin screw extruder.The material that melting mixing is good can be pulverized or the cutting machine granulation by pulverizer, prepares the matrix material pellet.The room temperature of this conductive polymer composites (25 ℃) resistivity is 1 ~ 10K Ω cm.
(2) at two parallel metal cores that certain distance is arranged as electrode, will on electrode, lay continuously coating after the above-mentioned matrix material melting, can prepare from limitting the heat generating core band of warm accompanying-heat cable.
(3) coat one deck insulating coating as the protective sleeve of accompanying-heat cable at the skin of the above-mentioned heat generating core band for preparing again.
(4) in order further to improve the use properties of cable; usually also on the basis of (3); at accompanying-heat cable braiding multiple layer metal line screen layer with coat multilayer protective coating, wherein screen layer or protective sleeve can single multilayer coating structure also can intersect multilayer coating structure by metal wire weaving machine.
Of the present invention from limitting the employed polymer-based conducing composite material of warm accompanying-heat cable owing to having added polymerisable polar monomer, in the melting mixing process, polymerisable polar monomer under the promotion of initiator with polyethylene generation graft reaction, the stability of the conductive network in the matrix material that the polar monomer in the grafting can improve enhancing that the conductive filler material carbon black is combined with interface between the polyethylene; Simultaneously on the polar monomer with polar group and the good adhesion between the conductive electrode, reduced the interface resistance between the conducing composite material and electrode after accompanying-heat cable is placed through high temperature, therefore have good resistance reproducibility and stability.In addition, the present invention limits warm accompanying-heat cable by the initiator grafting in preparation certainly, and is therefore complete processing is simple, with low cost.
Description of drawings
Fig. 1 is that a kind of coventional type of the present invention is from the structural representation of limitting warm accompanying-heat cable;
Fig. 2 is that a kind of explosion-proof type of the present invention is from the structural representation of limitting warm accompanying-heat cable.
Embodiment
Preparation is from limitting the volume percent of the polymer-based conducing composite material of warm accompanying-heat cable to be:
(it is 0.925g/cm with density that melt temperature is 111 ℃ for crystallinity or hemicrystalline polymer
3Low Density Polyethylene), volume percent is 41%;
Polymerisable polar monomer is double bond containing maleic anhydride (MAH), and volume percent is 3%;
Conductive filler material is nano carbon black, and its volume percent is 48.4%;
Mineral filler is zinc oxide, and its volume percent is 7%;
Processing aid, selecting dicumyl peroxide (DCP) is initiator, its volume percent is for being 0.6%.
Preparation process from the warm accompanying-heat cable of limit is as follows:
Above-mentioned materials is added high-speed mixer together by proportioning fully mix, add then that twin screw extruder mixes, plastifies, extrudes, granulation, obtain polymer-based conducing composite material;
The extruding of special mouthful mould continuous uniform of the above-mentioned polymer-based conducing composite material 2 that makes by two single screw extrusion machines is coated on two parallel metal electrodes 1, can makes from the heat generating core band of limitting warm accompanying-heat cable; Wherein, the distance of two metal electrodes 1 is 10.0mm ± 2.0mm, and the coating thickness of polymer-based conducing composite material 2 is 2.0mm ± 0.6mm.At the outer one deck insulating sheath 3 that coats of core band, the coventional type that can make is as shown in Figure 1 limit warm accompanying-heat cable to the hot core band that will make again certainly by common process.
Again with the above-mentioned coventional type that makes from limit warm accompanying-heat cable by braiding machine at its outer braid layer of metal screen layer 4 and/or coat one deck insulating sheath 5, can make as shown in Figure 2 explosion-proof type from limitting warm accompanying-heat cable.
The present embodiment with coventional type shown in Figure 1 from limit warm accompanying-heat cable as electrical specification as shown in table 1.
The preparation method is same as embodiment 1.
Compare with embodiment 1, the Low Density Polyethylene volume fraction is reduced to 40% by 41%; The volume percent of polymerizable polar monomer MAH is increased to 4% by 3%, and the volume percent of all the other components is constant.
The present embodiment with coventional type shown in Figure 1 from limit warm accompanying-heat cable as electrical specification as shown in table 1.
The preparation method is same as embodiment 1.
Compare with embodiment 1, the Low Density Polyethylene volume fraction is reduced to 39% by 41%; The volume percent of polymerizable polar monomer MAH is increased to 5% by 3%, and the volume percent of all the other components is constant.
The present embodiment with shown in Figure 1 from limit warm accompanying-heat cable as electrical specification as shown in table 1.
Embodiment 4
The preparation method is same as embodiment 1.
Compare with embodiment 1, the polymerizable polar monomer is replaced with vinylformic acid (AA) by MAH, volume percent is 3%, and the volume percent of all the other components is constant.
The present embodiment with coventional type shown in Figure 1 from limit warm accompanying-heat cable as electrical specification as shown in table 1.
The preparation method is same as embodiment 1.
Compare with embodiment 1, the polymerizable polar monomer is replaced with vinylformic acid (AA) by MAH, volume percent is 3%; The volume percent of conductive filler material nano carbon black increases by 0.3%; The volume percent of initiator DCP reduces 0.3%, and the volume percent of all the other components is constant.
The present embodiment with coventional type shown in Figure 1 from limit warm accompanying-heat cable as electrical specification as shown in table 1.
Embodiment 6
The preparation method is same as embodiment 1.
Compare with embodiment 1, with the volume percent reduction by 0.3% of polymerizable polar monomer by MAH; The volume percent of initiator DCP increases by 0.3%, and the volume percent of all the other components is constant.
The present embodiment with coventional type shown in Figure 1 from limit warm accompanying-heat cable as electrical specification as shown in table 1.
Comparative example
Prepare polymer-based conducing composite material and certainly limit the step of warm accompanying-heat cable identical with embodiment 1, but do not add polymerisable polar monomer and initiator, the volume percent of all the other components is constant.This comparative example with coventional type shown in Figure 1 from limit warm accompanying-heat cable as electrical specification as shown in table 1.
Table 1 is placed 1 hour test resistance data for certainly limitting warm accompanying-heat cable after constant temperature under 105 ℃ of conditions is placed for some time by the coventional type of polymer-based conducing composite material preparation of the present invention in 25 ℃ of environment, wherein accompanying-heat cable length is 120cm.
In the table 1, R
0From the hot initial resistance of limit temperature companion;
R
1From limitting warm accompanying-heat cable after placing 1h under 105 ℃ of conditions, to take out the normal temperature test resistance;
R
25From limitting warm accompanying-heat cable after placing 25h under 105 ℃ of conditions, to take out the normal temperature test resistance;
R
50From limitting warm accompanying-heat cable after placing 50h under 105 ℃ of conditions, to take out the normal temperature test resistance;
R
100From limitting warm accompanying-heat cable after placing 100h under 105 ℃ of conditions, to take out the normal temperature test resistance;
R
168From limitting warm accompanying-heat cable after placing 168h under 105 ℃ of conditions, to take out the normal temperature test resistance.
Table 1 coventional type from the electrical specification of limitting warm accompanying-heat cable relatively
| R 0?(Ω) | R 1?(Ω) | R 25?(Ω) | R 50?(Ω) | R 100?(Ω) | R 168?(Ω) | |
| |
783 | 785 | 802 | 826 | 847 | 868 |
| |
805 | 808 | 828 | 847 | 864 | 881 |
| |
789 | 894 | 811 | 832 | 849 | 871 |
| Embodiment 4 | 801 | 803 | 823 | 840 | 856 | 875 |
| |
792 | 796 | 814 | 837 | 856 | 875 |
| Embodiment 6 | 779 | 781 | 797 | 818 | 815 | 837 |
| Comparative example | 797 | 802 | 823 | 849 | 872 | 895 |
As can be seen from Table 1, all add a certain amount of polymerisable polar monomer and initiator among the embodiment 1～6, certainly limit the resistance value after warm accompanying-heat cable is placed through high temperature all little than the comparative example that does not add polymerisable polar monomer.And among the embodiment 1～6, in the situation that same polyethylene and conductive filler material volume fraction, the relative MAH content of initiator DCP is excessive, in preparation conducing composite material process, the crosslinking side reaction probability increases, and the MAH percentage of grafting is relatively low, and when preparation accompanying-heat cable core band, the current of electric of single screw extrusion machine is bigger than normal, difficult processing.Among embodiment 2 and the embodiment 4, the volume percent of initiator DCP and polymerisable polar monomer is suitable, and percentage of grafting is higher, therefore behind its high temperature test, certainly limit the resistance reproducibility of warm accompanying-heat cable best in an embodiment.
Claims (10)
1. polymer-based conducing composite material of high thermal stability, it is characterized in that this matrix material by the component of following volume percent through mixing, plastify, extrude, granulation step is prepared from:
Crystallinity or hemicrystalline polymer 15% ~ 50%
Conductive filler material 25% ~ 75%
Polymerisable polar monomer 0.5% ~ 10%
Mineral filler 5% ~ 30%
Processing aid 0.05% ~ 5%.
2. the polymer-based conducing composite material of a kind of high thermal stability according to claim 1 is characterized in that described crystallinity or hemicrystalline polymer are one or more in polypropylene, polyvinylidene difluoride (PVDF), polyolefin elastomer, polyethylene, ethylene-tetrafluoroethylene copolymer, polymethylmethacrylate, the ethylene-propylene copolymer.
3. the polymer-based conducing composite material of a kind of high thermal stability according to claim 1 is characterized in that described conductive filler material is that particle diameter is 10nm～10 μ m carbon black or graphite.
4. the polymer-based conducing composite material of a kind of high thermal stability according to claim 3 is characterized in that described carbon black is Shawinigan black, furnace treated black or thermally oxidized black.
5. the polymer-based conducing composite material of a kind of high thermal stability according to claim 1 is characterized in that described polymerisable polar monomer is one or more in acid anhydrides, (methyl) vinylformic acid (fat), vinyl cyanide, acid amides, peptamine and the unsaturated amine.
6. the polymer-based conducing composite material of a kind of high thermal stability according to claim 1 is characterized in that described mineral filler is one or more in enhancing carbon black, laminar nano polynite, nanometer or micro-calcium carbonate, magnesium oxide, aluminum oxide and the zinc oxide.
7. the polymer-based conducing composite material of a kind of high thermal stability according to claim 1 is characterized in that described processing aid is one or more in initiator, oxidation inhibitor, lubricant, metal deactivator and the fire retardant.
8. the polymer-based conducing composite material of a kind of high thermal stability according to claim 7 is characterized in that described initiator is one or more in organo-peroxide, azo-initiator and the redox initiator.
9. the polymer-based conducing composite material of a kind of high thermal stability according to claim 8 is characterized in that described organic peroxide evocating agent is benzoyl peroxide and/or dicumyl peroxide; Described azo-initiator is Diisopropyl azodicarboxylate or 2,2'-Azobis(2,4-dimethylvaleronitrile); Described redox initiator is hydrogen peroxide/iron protochloride or isopropyl benzene hydroperoxide/tetrem alkene imines.
10. Bian, is characterized in that comprising the steps: from the method for limitting warm accompanying-heat cable with the described polymer-based conducing composite material preparation of one of claim 1 to 9
(1) gets two parallel plain conductors as electrode, coat one of claim 1 to 9 described polymer-based conducing composite material at electrode, make two electrodes form the loop by the form of the continuous parallel connection of polymer-based conducing composite material, polymer-based conducing composite material is limit the heat generating core band of warm accompanying-heat cable again as oneself with the form of heating element;
(2) at the outer coated insulation overcoat of the heat generating core band of step (1), described insulating coating is crosslinked polyolefin or fluoroplastics class cable sheath material, can form coventional type from limitting warm accompanying-heat cable;
(3) in outer braid metal screen layer and/or the coated insulation sheathcoat of the insulating coating of step (2), can form explosion-proof type from limitting warm accompanying-heat cable.
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Cited By (6)
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| CN103304873A (en) * | 2013-05-24 | 2013-09-18 | 安邦电气集团有限公司 | PTC (Positive Temperature Coefficient) macromolecular composite heating material based on iron and copper powder and preparation method thereof |
| CN104829937A (en) * | 2015-04-23 | 2015-08-12 | 苏州圣利线缆有限公司 | Sheath material for aerospace cables and manufacturing method thereof |
| CN105072721A (en) * | 2015-08-06 | 2015-11-18 | 浙江大铭新材料股份有限公司 | Novel positive temperature coefficient (PTC) heating plastic tube and fabrication method thereof |
| CN110382560A (en) * | 2017-03-03 | 2019-10-25 | 日本优必佳株式会社 | Electrical/electronic part crystallinity radical-polymerizable composition uses the electrical/electronic part formed body of the composition and the manufacturing method of the electrical/electronic part formed body |
| CN112111093A (en) * | 2020-09-23 | 2020-12-22 | 芜湖科阳新材料股份有限公司 | PTC conductive composite material for heat tracing band and preparation method thereof |
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| CN103304873A (en) * | 2013-05-24 | 2013-09-18 | 安邦电气集团有限公司 | PTC (Positive Temperature Coefficient) macromolecular composite heating material based on iron and copper powder and preparation method thereof |
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| CN105072721A (en) * | 2015-08-06 | 2015-11-18 | 浙江大铭新材料股份有限公司 | Novel positive temperature coefficient (PTC) heating plastic tube and fabrication method thereof |
| CN110382560A (en) * | 2017-03-03 | 2019-10-25 | 日本优必佳株式会社 | Electrical/electronic part crystallinity radical-polymerizable composition uses the electrical/electronic part formed body of the composition and the manufacturing method of the electrical/electronic part formed body |
| CN112111093A (en) * | 2020-09-23 | 2020-12-22 | 芜湖科阳新材料股份有限公司 | PTC conductive composite material for heat tracing band and preparation method thereof |
| CN114933757A (en) * | 2022-07-05 | 2022-08-23 | 无锡桑普电器科技发展有限公司 | Self-temperature-limiting electrothermal film and preparation method thereof |
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Application publication date: 20130501 |