CN1218065A - Thermal shock resistant polymer composite material with positive temperature coefficient and processing method therefor - Google Patents
Thermal shock resistant polymer composite material with positive temperature coefficient and processing method therefor Download PDFInfo
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- CN1218065A CN1218065A CN 97118882 CN97118882A CN1218065A CN 1218065 A CN1218065 A CN 1218065A CN 97118882 CN97118882 CN 97118882 CN 97118882 A CN97118882 A CN 97118882A CN 1218065 A CN1218065 A CN 1218065A
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Abstract
A polymer composition with the resistance against hot shock and positive temp coefficient for resistivity is prepared from polyolefine resin, pentaerythritol, 3-(3.5-ditert-butyl-hydroxyphenyl) octadecyl propionate, N, N'-2-beta-naphthyl p-benzodiamine, 2,2,4-trimethyl-1,2-dihydroquinoline polymer, vinyl tri(beta-methoxyethoxy) silane, acetylene black carbon and electrically conductive black carbon through mixing in a dual-roller mixer or mixing first in an internal mixer and then in the dual-roller mixer. Its advantages are simple process and low cost.
Description
The present invention relates to a kind of heat shock resistance type positive temperature coefficient of resistivity polymer composites and complete processing of using from the temperature control heating element thereof that can be used as.
Resistivity with polymer composites of positive temperature coefficient of resistivity has the dependency of height to temperature, and can change in the reversibility between Curie temperature generation conductor and the isolator.This material can be made into have two electrodes from the temperature control heating element; When two interpolars apply voltage V, there is electric current to pass through matrix material, produce thermal power V
2/ R (wherein R is two resistance between electrode of the heating element of the certain-length that extends along the electrode parallel direction).The heat that is produced raises the heating element self-temperature and dispels the heat to environment.When temperature was raised to the Curie-point temperature of material, resistivity sharply increased, and the resistance of heating element also increases, thermal power (V
2/ R) just descend.When the matrix material self-temperature reduces because of heat radiation, resistivity will reduce again, make thermal output (V
2/ R) rise again.So circulation just can reach the purpose of temperature automatically controlled heating with temperature maintenance in required scope (this temperature range is by the thermal parameter decision of the power and the heating object of heating element).Therefore, this is a kind of by automatically adjusting the localized heat output rating from the temperature control heating element, thereby is complementary with each local temperature of heating target, has the electric heating products of heat tracing and temperature automatically controlled function.It can be applied to the antifreeze paraffin removal of oil feed pipe, the temperature control insulation of chemical industry equipment, instrument, gardens gardening, multiple fields such as agriculture production and heating of house.Because it can be with the variation of envrionment temperature, heating power is automatically regulated in segmentation, and the homo(io)thermism that makes heating target is at a certain scope and uniform distribution.Thereby remedied the deficiency of steam jacket or various resistance heaters, have characteristics such as safe, energy-conservation, convenient.
In recent years, some developed countries had used this positive temperature coefficient of resistivity polymer materials to make from the temperature control heating element.As Japan 1991 the 49th phases of " industry on the radioactive rays " periodical, reported radiation crosslinking from application and the general principle of temperature control heating element at aspects such as gardens, pipelines.1997 the 18th the 4th phases of volume of the U.S. " Polymer Composites " periodical have announced on the P477-483 page or leaf through the rumbatron radiation crosslinking, have reached a kind of positive temperature coefficient of resistivity composite formulations of being made up of high density polyethylene(HDPE) (HDPE) and graphitized carbon black (CB) of gel resultant 80%.It consists of HDPE, and (density is 0.954g/cm
3, melting index 1.2g/10min, 118 ℃ of softening temperatures, degree of crystallinity 62%) and 100 parts, 15 parts of conductive acetylene carbon blacks, 1 part of triallyl isocyanate (TAIC), 1.2 parts in the mixture of a kind of hindered amine and hindered phenol.Through mixing, be extruded into heating element, again radiation crosslinking and make gel content reach 82% under electron beam with two electrodes.Though the heating element that this method is made has more stable ptc characteristics and conductivity at room temperature, can not accept thermal shocking more than the matrix melting temperature being higher than it.When the heating element of above composition was placed 20 minutes in 120 ℃ of warm airs after, room temperature resistivity rose to 10
1More than the Ω cm, can not conduct electricity, lose positive temperature coefficient of resistivity characteristic and use value.When voltage floats when too high, heating power surpasses heat radiation power at short notice, and material has little time to carry out the positive temperature coefficient response, makes the matrix local superheating and thermal runaway takes place.So repeatedly impact, its room temperature resistivity rises gradually, and positive temperature coefficient of resistivity descends, until the useful feature that loses as PTC material.In addition, take radiation crosslinking improve electric stability measure since cost of equipment very high, product cost is higher.
The objective of the invention is for provide a kind of in the raw material of matrix material, added the third phase material can postpone effectively material voltage float or environment short period of time overheat condition under local superheating takes place time, prevent irreversible thermal runaway; And interpolation expanding material, can improve the avidity of material, matrix material is had have the same good electric stability of analogous products and switch character with crosslinked mistake, can increase substantially the heat shock resistance type positive temperature coefficient of resistivity polymer composites of material thermal shock resistance without radiation crosslinking.
Another object of the present invention is to improve a kind of complete processing that does not need radiation crosslinking processing can reduce the heat shock resistance type positive temperature coefficient of resistivity polymer composites of product cost.
Purpose of the present invention can realize by following measure:
A kind of heat shock resistance type positive temperature coefficient of resistivity polymer composites is to be base-material with the polyolefin resin, adds various additives therein and forms; This matrix material is to be made by the raw material of following weight parts: 100 parts of polyolefin resines, Shawinigan black 13-20 part, graphitized carbon black 3-10 part, tetramethylolmethane 40-60 part, 3-(3,5-di-t-butyl-hydroxy phenyl) propionic acid octadecyl ester 1-2 part, N, N '-2-betanaphthyl Ursol D 0.1-1 part, 2,2,4-trimethylammonium-1,2-dihyaroquinoline polymer 0.5-1.5 part, vinyl three (beta-methoxy-oxyethyl group) silane 1.5-3 part.It is 30-100 μ m that described Shawinigan black can be selected median size for use, specific mass volume m3/kg, the Shawinigan black of resistivity≤0.5K Ω cm; It is 40-50nm that graphitized carbon black can be selected median size for use, specific surface area 200-300m
2/ g, the graphitized carbon black of DBP absorption value 150-200ml/g.
A kind of complete processing of heat shock resistance type positive temperature coefficient of resistivity polymer composites is earlier polyolefin resin to be added two roller mills and mill fluxing, add 3-(3 again, the 5-di-tert-butyl-hydroxy phenyl) propionic acid octadecyl ester, N, N '-2-betanaphthyl Ursol D, 2,2,4-trimethylammonium-1,2-dihyaroquinoline polymer, vinyl three (beta-methoxy-oxyethyl group) silane, mixing even; Add tetramethylolmethane then, mixing evenly, add again that graphitized carbon black and Shawinigan black are mixing evenly promptly to can be made into.
A kind of complete processing of heat shock resistance type positive temperature coefficient of resistivity polymer composites is each material in the raw material to be added in the lump mixingly in the Banbury mixer form a plasticity blend to powder and resin, takes out the back and opens refining evenly promptly can be made in mill.
Purpose of the present invention also can realize by following measure:
Polyolefin resin in the raw material of described heat shock resistance type positive temperature coefficient of resistivity polymer composites can be one or both mixtures in linear low density polyethylene, the high density polyethylene(HDPE), and adds one or both the blend in terpolymer EP rubber and ethene one vinyl acetate copolymer in above-mentioned polyethylene; Its parts by weight of raw materials is constant.
3-(3 in the raw material of described heat shock resistance type positive temperature coefficient of resistivity polymer composites, 5-di-t-butyl-hydroxy phenyl) the propionic acid octadecyl ester can be used N, N '-2-betanaphthyl Ursol D, 1,1,3-three (2-methyl-4-hydroxyl-5-tert-butyl-phenyl) butane, Tyox B replace, and its parts by weight of raw materials is constant.
Tetramethylolmethane in the raw material of described heat shock resistance type positive temperature coefficient of resistivity polymer composites can be used on 80-300 ℃ the replacement of reversible heat absorption phase converting substances takes place; As indium, tin, bismuth/tin/zinc alloy, six hydration magnesium salts, Succinic anhydried, pyrocatechol, Resorcinol, chinol, its parts by weight of raw materials is constant.
Vinyl three (beta-methoxy-oxyethyl group) silane in the raw material of described heat shock resistance type positive temperature coefficient of resistivity polymer composites can replace with the mixture of other silicane material, metatitanic acid organic ester or itself and silane, and its parts by weight of raw materials is constant.
The present invention has following advantage compared to existing technology:
1, the mixture that adopts Shawinigan black and graphitized carbon black in the raw material of the present invention has not only been brought into play the good low-temperature electroconductibility of graphitized carbon black as conductive filler material, has utilized Shawinigan black to give material with bigger positive temperature coefficient of resistivity again.
2, the present invention adds tetramethylolmethane as the third phase material outside crystalline polymer and carbon black, and this third phase material can be more than the crystalline polymer fusing point first order phase transition, the heat absorption of tetragonal system to isometric system takes place 187 ℃ the time, and latent heat of phase change reaches 425J/cm
3, hot melt is changed to 3.18J/ ℃ of g; Under the thermal shocking situation, the heat of composite inner is accumulated and is made the third phase material take place to change mutually, absorbs most of unnecessary heat and stores with chemical potential energy form; When thermal shocking is removed, when temperature drops to below 187 ℃, reverse transformation mutually taking place again, discharges the heat that is absorbed gradually, can postpone effectively like this material voltage float or environment short period of time overheat condition under local superheating takes place time, prevent irreversible thermal runaway.
3, the present invention adds vinyl three (beta-methoxy-oxyethyl group) silicane series material as its mutual expanding material, to improve its avidity between crystalline polymer and carbon black; When the temperature of crystalline polymer is raised to its fusing point Tm when above, viscosity reduces rapidly.At this moment, carbon black particle spontaneously gathers together because of pedesis, has changed original homogeneously dispersed state.This is because the surface properties of carbon black and crystalline polymer differs greatly, and a little less than the avidity, does not exist Van der Waals force, hydrogen bond etc. to restrict the physical chemistry bonding force of carbon black particle and polymkeric substance.By adding expanding material, strengthened the two surperficial avidity, go and other particle accumulations even make carbon black particle under high temperature, low viscous condition, also can not leave original position; Thereby make the positive temperature coefficient of resistivity polymer composites of preparation have much better resistance to sudden heating without radiation crosslinking.Its 120 ℃ of thermal shocking times can extend near 10 times the room temperature resistivity of just having an appointment in 40 hours rises.
4, the present invention adopts 3-(3,5-di-t-butyl-hydroxy phenyl) propionic acid stearic acid Hinered phenols and N, 2 of N '-2-betanaphthyl Ursol D hindered amines material and aggretion type, 2,4-trimethylammonium-1, the 2-dihyaroquinoline can prevent high temperature oxidation as the collaborative antioxidant systems of polyolefin resin; Can use 30 years at the melting temperature of polyolefin resin and do not have the decline (extension at break variability≤15%) of obvious mechanical property.
5, complete processing of the present invention is simple, does not need to make product have the electric property identical with radiation crosslinking through radiation crosslinking, has reduced product cost.
The present invention also will be described in further detail in conjunction with the embodiments:
Embodiment one:
A kind of heat shock resistance type positive temperature coefficient of resistivity polymer composites is to be made by the raw material of following weight parts: 100 parts of linear low density polyethylenes, 18 parts of Shawinigan blacks, 5 parts of graphitized carbon blacks, 45 parts of tetramethylolmethanes, 3-(3,5-di-t-butyl-hydroxy phenyl) 1 part of propionic acid octadecyl ester, N, 0.6 part of N '-2-betanaphthyl Ursol D, 2,2,4-trimethylammonium-1,1.5 parts of 2-dihyaroquinoline polymers, 1.5 parts in vinyl three (beta-methoxy-oxyethyl group) silane.
Its complete processing is earlier polyolefin resin to be added two roller mills, and mill fluxing, add 3-(3 again, the 5-di-tert-butyl-hydroxy phenyl) propionic acid octadecyl ester, N, N '-2-betanaphthyl Ursol D, 2,2,4-trimethylammonium-1,2-dihyaroquinoline polymer, vinyl three (beta-methoxy-oxyethyl group) silane are mixing evenly; It is mixing evenly to add tetramethylolmethane then, adds that graphitized carbon black and Shawinigan black are mixing evenly promptly to can be made into again.
Its complete processing also can add each material in the raw material in the lump mixingly in the Banbury mixer forms a plasticity blend to powder and resin, takes out the back and opens refining evenly promptly can be made in mill.
Embodiment two;
A kind of heat shock resistance type positive temperature coefficient of resistivity polymer composites is to be made by the raw material of following weight parts: 50 parts of 100 parts of high density polyethylene(HDPE)s, 13 parts of Shawinigan blacks, 10 parts of graphitized carbon blacks, indium, 1,1,2 parts of butane of 3-three (2-methyl-4-hydroxyl-5-tert-butyl-phenyl), N, 0.2 part of N '-2-betanaphthyl Ursol D, 2,2,4-trimethylammonium-1,0.5 part of 2-dihyaroquinoline polymer, 3 parts in vinyl three (beta-methoxy-oxyethyl group) silane.Its complete processing and example are together.
Embodiment three:
A kind of heat shock resistance type positive temperature coefficient of resistivity polymer composites is to be made by the raw material of following weight parts: 80 parts of linear low density polyethylenes, 20 parts of high density polyethylene(HDPE)s, 15 parts of Shawinigan blacks, 8 parts of graphitized carbon blacks, bismuth/tin/(56/40/4) 60 part on zinc, 1.2 parts of Tyox Bs, N; 0.9 part of N '-2-betanaphthyl Ursol D, 2; 2; 4-trimethylammonium-1,1 part of 2-dihyaroquinoline polymer, 2 parts of isopropyl triisostearoyl titanates.
Its complete processing and example are together.
Embodiment four:
A kind of heat shock resistance type positive temperature coefficient of resistivity polymer composites is to be made by the raw material of following weight parts: 70 parts of linear low density polyethylenes, 30 parts of terpolymer EP rubbers, 20 parts of Shawinigan blacks, 3 parts of graphitized carbon blacks, 55 parts of chinols, 1.8 parts of Tyox Bs, N; 0.4 part of N '-2-betanaphthyl Ursol D, 2; 2; 4-trimethylammonium-1,1.2 parts of 2-dihyaroquinoline polymers, 1 part in vinyl three (beta-methoxy-oxyethyl group) silane, 1.5 parts of isopropyl triisostearoyl titanates.
Its complete processing and example are together.
Embodiment five:
A kind of heat shock resistance type positive temperature coefficient of resistivity polymer composites is to be made by the raw material of following weight parts: 60 parts of linear low density polyethylenes, 40 parts of ethylene-vinyl acetate copolymers, 16 parts of Shawinigan blacks, 6 parts of graphitized carbon blacks, 40 parts of Magnesium dichloride hexahydrates, 3-(3,5-di-t-butyl-hydroxy phenyl) 1.6 parts of propionic acid octadecyl esters, N, 1 part of N '-2-betanaphthyl Ursol D, 2,2,4-trimethylammonium-1,0.8 part of 2-dihyaroquinoline polymer, 1.8 parts of vinyltriethoxysilanes.
Its complete processing and example are together.
Embodiment six:
A kind of heat shock resistance type positive temperature coefficient of resistivity polymer composites is to be made by the raw material of following weight parts: 70 parts of linear low density polyethylenes, 20 parts of terpolymer EP rubbers, 10 parts of ethylene-vinyl acetate copolymers, 14 parts of Shawinigan blacks, 9 parts of graphitized carbon blacks, 48 parts of Succinic anhydrieds, 3-(3,5-di-t-butyl-hydroxy phenyl) 1.1 parts of propionic acid octadecyl esters, N, 0.1 part of N '-2-betanaphthyl Ursol D, 2,2,4-trimethylammonium-1,0.6 part of 2-dihyaroquinoline polymer, 2.7 parts in vinyl three (beta-methoxy-oxyethyl group) silane.
Its complete processing and example are together.
Embodiment seven:
A kind of heat shock resistance type positive temperature coefficient of resistivity polymer composites is to be made by the raw material of following weight parts: 50 parts of high density polyethylene(HDPE)s, 30 parts of terpolymer EP rubbers, 20 parts of ethylene-vinyl acetate copolymers, 17 parts of Shawinigan blacks, 4 parts of graphitized carbon blacks, 53 parts of pyrocatechols, 3-(3,5-di-t-butyl-hydroxy phenyl) 1.5 parts of propionic acid octadecyl esters, N, 0.5 part of N '-2-betanaphthyl Ursol D, 2,2,4-trimethylammonium-1,1.4 parts of 2-dihyaroquinoline polymers, 1.6 parts in vinyl three (beta-methoxy-oxyethyl group) silane.
Its complete processing and example are together.
Claims (7)
1, a kind of heat shock resistance type positive temperature coefficient of resistivity polymer composites is to be base-material with the polyolefin resin, adds various additives therein and forms; It is characterized in that this matrix material is to be made by the raw material of following weight parts:
100 parts of polyolefin resines
Shawinigan black 13-20 part
Graphitized carbon black 3-10 part
Tetramethylolmethane 40-60 part
3-(3,5-di-t-butyl-hydroxy phenyl) propionic acid octadecyl ester 1-2 part
N, N '-2-betanaphthyl Ursol D 0.1-1 part
2,2,4-trimethylammonium-1,2-dihyaroquinoline polymer 0.5-1.5 part
Vinyl three (beta-methoxy-oxyethyl group) silane 1.5-3 part
2, heat shock resistance type positive temperature coefficient of resistivity polymer composites as claimed in claim 1, it is characterized in that polyolefin resin in the raw material can be one or both mixtures in linear low density polyethylene, the high density polyethylene(HDPE), and in above-mentioned polyethylene, add one or both the blend in terpolymer EP rubber and the ethylene-vinyl acetate copolymer; Its parts by weight of raw materials is constant.
3, heat shock resistance type positive temperature coefficient of resistivity polymer composites as claimed in claim 1, it is characterized in that the 3-(3 in the raw material, 5-di-t-butyl-hydroxy phenyl) the propionic acid octadecyl ester can be used N, N '-2-betanaphthyl Ursol D, 1,1,3-three (2-methyl-4-hydroxyl-5-tert-butyl-phenyl) butane, Tyox B replace, and its parts by weight of raw materials is constant.
4, heat shock resistance type positive temperature coefficient of resistivity polymer composites as claimed in claim 1 is characterized in that the tetramethylolmethane in the raw material can be used on the replacement of 80-300 ℃ of generation reversible heat absorption phase converting substances; As indium, tin, bismuth/tin/zinc alloy, six hydration magnesium salts, Succinic anhydried, pyrocatechol, chinol, its parts by weight of raw materials is constant.
5, heat shock resistance type positive temperature coefficient of resistivity polymer composites as claimed in claim 1, it is characterized in that vinyl three (beta-methoxy-oxyethyl group) silane in the raw material can replace with the mixture of other silicane material, metatitanic acid organic ester or itself and silane, its parts by weight of raw materials is constant.
6, the complete processing of the described heat shock resistance type of a kind of claim 1 positive temperature coefficient of resistivity polymer composites, it is characterized in that this technology is earlier polyolefin resin to be added two roller mills, and mill fluxing, add 3-(3 again, the 5-di-tert-butyl-hydroxy phenyl) propionic acid octadecyl ester, N, N '-2-betanaphthyl Ursol D, 2,2,4-trimethylammonium-1,2-dihyaroquinoline polymer, vinyl three (beta-methoxy-oxyethyl group) silane are mixing evenly; It is mixing evenly to add tetramethylolmethane then, adds that graphitized carbon black and Shawinigan black are mixing evenly promptly to can be made into again.
7, the complete processing of the described heat shock resistance type of a kind of claim 1 positive temperature coefficient of resistivity polymer composites, it is characterized in that each material in the raw material added in the lump and mixingly in the Banbury mixer form a plasticity blend to powder and resin, take out the back and in mill, open refining and evenly promptly can be made into.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN 97118882 CN1218065A (en) | 1997-11-10 | 1997-11-10 | Thermal shock resistant polymer composite material with positive temperature coefficient and processing method therefor |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN 97118882 CN1218065A (en) | 1997-11-10 | 1997-11-10 | Thermal shock resistant polymer composite material with positive temperature coefficient and processing method therefor |
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| CN1218065A true CN1218065A (en) | 1999-06-02 |
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| CN 97118882 Pending CN1218065A (en) | 1997-11-10 | 1997-11-10 | Thermal shock resistant polymer composite material with positive temperature coefficient and processing method therefor |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102176361A (en) * | 2011-02-22 | 2011-09-07 | 深圳市长园维安电子有限公司 | Base materials of PTC (Positive Temperature Coefficient) thermistor, PTC thermistor and preparation method thereof |
| CN102176360A (en) * | 2011-02-22 | 2011-09-07 | 深圳市长园维安电子有限公司 | PTC thermistor and substrate applied therein and manufacturing method thereof |
| CN103205056A (en) * | 2012-01-17 | 2013-07-17 | 比亚迪股份有限公司 | Positive temperature coefficient composite material and thermistor |
| CN110483580A (en) * | 2019-09-06 | 2019-11-22 | 广东先导先进材料股份有限公司 | A kind of high-purity trialkyl antimony and the preparation method and application thereof |
-
1997
- 1997-11-10 CN CN 97118882 patent/CN1218065A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102176361A (en) * | 2011-02-22 | 2011-09-07 | 深圳市长园维安电子有限公司 | Base materials of PTC (Positive Temperature Coefficient) thermistor, PTC thermistor and preparation method thereof |
| CN102176360A (en) * | 2011-02-22 | 2011-09-07 | 深圳市长园维安电子有限公司 | PTC thermistor and substrate applied therein and manufacturing method thereof |
| CN102176360B (en) * | 2011-02-22 | 2012-10-10 | 深圳市长园维安电子有限公司 | PTC thermistor and substrate applied therein and manufacturing method thereof |
| CN102176361B (en) * | 2011-02-22 | 2012-10-10 | 深圳市长园维安电子有限公司 | Base materials of PTC (Positive Temperature Coefficient) thermistor, PTC thermistor and preparation method thereof |
| CN103205056A (en) * | 2012-01-17 | 2013-07-17 | 比亚迪股份有限公司 | Positive temperature coefficient composite material and thermistor |
| CN103205056B (en) * | 2012-01-17 | 2016-03-30 | 比亚迪股份有限公司 | A kind of Positive temperature coefficient composite material and a kind of thermistor |
| CN110483580A (en) * | 2019-09-06 | 2019-11-22 | 广东先导先进材料股份有限公司 | A kind of high-purity trialkyl antimony and the preparation method and application thereof |
| CN110483580B (en) * | 2019-09-06 | 2022-04-19 | 广东先导微电子科技有限公司 | High-purity trialkyl antimony, and preparation method and application thereof |
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