CN114249979B - Polyamide composition with NTC effect and preparation method thereof - Google Patents
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- C08L77/06—Polyamides derived from polyamines and polycarboxylic acids
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- G01K—MEASURING TEMPERATURE; MEASURING QUANTITY OF HEAT; THERMALLY-SENSITIVE ELEMENTS NOT OTHERWISE PROVIDED FOR
- G01K7/00—Measuring temperature based on the use of electric or magnetic elements directly sensitive to heat ; Power supply therefor, e.g. using thermoelectric elements
- G01K7/16—Measuring temperature based on the use of electric or magnetic elements directly sensitive to heat ; Power supply therefor, e.g. using thermoelectric elements using resistive elements
- G01K7/22—Measuring temperature based on the use of electric or magnetic elements directly sensitive to heat ; Power supply therefor, e.g. using thermoelectric elements using resistive elements the element being a non-linear resistance, e.g. thermistor
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Abstract
The invention discloses a polyamide composition with NTC effect and a preparation method thereof, wherein the polyamide composition with NTC effect comprises the following components in parts by weight: 100 parts of polyamide resin; 0.05-3 parts of metal iodide; 0.1-5 parts of a fluorosulfonic acid compound; 0-15 parts of a plasticizer; 0.1-1.5 parts of carbon black; 0-1 part of other auxiliary agents. The polyamide composition with the NTC effect prepared by the invention is a good polymer-based thermistor material (NTC material), has high elongation at break under low temperature, high electrifying stability and high thermal stability, and can be used in the fields of electric blankets, electric cushion cushions, warm air cushions, electric plate heaters, electric fireplaces, saddle heaters and other electric heaters.
Description
Technical Field
The invention belongs to the field of high molecular polymers, and particularly relates to a polyamide composition with an NTC effect and a preparation method thereof.
Background
NTC (negative Temperature coefficient) is a negative (sub-zero) Temperature coefficient. NTC materials refer to thermistor phenomena and materials having a negative temperature coefficient that decrease exponentially with temperature rise. In 1834, scientists first discovered that silver sulfide has a negative temperature coefficient of behavior. In 1930 scientists discovered that cuprous oxide-cupric oxide also has negative temperature coefficient properties and successfully utilized it in the temperature compensation circuit of aeronautical instruments. Subsequently, due to the continuous development of transistor technology, the research of thermistors has made a great progress.
In recent years, a polymer-based Negative Temperature coefficient Temperature-sensitive resistance material (NTC) is disclosed, which is a multiphase composite system formed by adding conductive fillers such as carbon black, metal powder and metal oxide into a polymer material serving as a matrix and performing post-treatment such as dispersion and compounding, wherein the resistivity of the multiphase composite system is reduced along with the increase of Temperature, and the NTC Temperature-sensitive resistance is mainly used for measurement and Temperature compensation of an electronic circuit.
In the prior art, the polyvinylidene fluoride-based temperature-sensitive resistance material is prepared by taking sodium styrene sulfonate grafted graphene or nano silver loaded graphene as a conductive filler, but the problems of high conductive phase filling, large room-temperature resistivity, low sensitivity and the like exist.
In the prior art, in order to improve the NTC effect of nylon products, a high content of iodine-containing compounds such as zinc iodide and the like are generally filled in nylon, and although the system has good heat-sensitive conductivity, the use of metal iodide and metal oxide with a high proportion reduces the toughness, the processability and the mechanical properties of nylon materials.
In the field, the problems of poor forming performance, difficult processing and the like of the polymer-based thermistor material (NTC) exist for a long time.
Disclosure of Invention
The invention aims to promote the dispersion of metal iodide to form a better ion channel through the perfluorosulfonate, so that a polyamide composition with an NTC effect, namely a good polymer-based thermistor material (NTC material) is formed, the fracture growth rate is high under a low-temperature condition, the electrification stability is high, and the thermal stability of the composition is high.
Further, the invention also provides a preparation method of the polyamide composition with the NTC effect.
A polyamide composition with NTC effect comprises the following components:
100 parts of polyamide resin;
0.05-3 parts of metal iodide;
0.1-5 parts of fluorosulfonic acid compound;
0-15 parts of a plasticizer;
0.1-1.5 parts of carbon black;
0-1 part of other auxiliary agents.
Preferably, the polyamide composition with NTC effect comprises the following components in parts by weight:
preferably, the polyamide composition with NTC effect comprises the following components in parts by weight:
more preferably, the polyamide composition with NTC effect comprises the following components in parts by weight:
preferably, the polyamide resin is at least one selected from aliphatic polyamide, semi-aromatic polyamide and polylactam.
Preferably, the weight ratio of the metal iodide and the fluorosulfonic acid compound is 0.4 to 10, more preferably, the weight ratio of the metal iodide and the fluorosulfonic acid compound is 2 to 7.5, and more preferably, the weight ratio of the metal iodide and the fluorosulfonic acid compound is 2.5 to 7.5.
The polyamide may be chosen from polyamides obtained by polycondensation of at least one aliphatic dicarboxylic acid with at least one aliphatic or cyclic diamine, such as PA6, PA66, PA610, PA612, PA56, PA46, MXD6, PA510, PA11, PA12, PA1010, PA1012, PA 1212; or polyamides obtained by polycondensation of at least one aromatic dicarboxylic acid with at least one aliphatic diamine, such as polyterephthalamides, polyisophthalamides, polyaramides, in particular PA9T, PA 10T; or polyamides obtained by polycondensation of at least one amino acid or lactam with itself, such as PA6, PA7, PA11, PA 12; or mixtures or copolyamides thereof.
More preferably, the polyamide resin is preferably a nylon material with a melting point of 150 ℃ to 230 ℃, such as PA11, PA12, PA1012 and PA 1212. The nylon material, 0.5g nylon in 100ml solution, measured relative viscosity between 2.0-2.5.
Preferably, the metal iodide is at least one compound selected from the group consisting of zinc iodide, tin iodide, antimony iodide, copper iodide, nickel iodide, manganese iodide, cobalt iodide, iron iodide, lead iodide, cadmium iodide, titanium iodide, sodium iodide, potassium iodide, and hydrates thereof.
Preferably, the fluorosulfonic acid compound is selected from one or more of perfluorooctanesulfonic acid amine, perfluorooctanesulfonic acid potassium salt, perfluorooctanesulfonic acid tetraethyl amine, and perfluorooctanesulfonamidoglutamic acid potassium salt.
Wherein the carbon black has a BET specific surface area of 2 to 200m 2 Preferably, the carbon black has a BET specific surface area of 65 to 110m 2 The specific surface area is measured by GB/T19587-2017 determination of the specific surface area of solid substances by a gas adsorption BET method, the absorption of the carbon black oil absorption value (DBP) is 50-300ml/100g, the carbon black with the DBP being more than 120ml/100g is selected to be favorable for electrostatic dissipation, and the carbon black oil absorption value is detected according to the standard GB/T3780.2-2017.
Wherein the plasticizer is selected from the group consisting of N-butylbenzenesulfonamide (BBSA), p-toluenesulfonamide (PTSA), O-p-toluenesulfonamide (O/PTSA), p-toluenesulfonyl chloride (PTSC), N- (2-hydroxypropyl) benzenesulfonamide (HPBSA), N-ethyl-O-p-toluenesulfonamide (N-E-O/PTSA), N-ethyl-p-toluenesulfonamide (N-E-PTSA), toluenesulfonamide formaldehyde resin (MH/MS), toluenesulfonamide formaldehyde resin butyl acetate solution (MS-80), N-cyclohexyl-p-toluenesulfonamide (CTSA), N-diethyl-p-toluenesulfonamide (DETSA), N-Ethylbenzenesulfonamide (EBSA), N-Isopropylbenzenesulfonamide (IBSA), N-alkyl-p-toluenesulfonamide (TTSA), N- (2-hydroxyethyl) benzenesulfonamide, One or more of N, N-bis (2-hydroxyethyl) p-toluenesulfonamide, N- (2-hydroxyethyl) p-toluenesulfonamide, Benzenesulfonamide (BSA).
The other auxiliary agent comprises at least one of an antioxidant and a lubricant.
The antioxidant is selected from hindered phenol and phosphite antioxidant, such as antioxidant 1010, antioxidant 1098, antioxidant 1079, antioxidant 245 and antioxidant 168, antioxidant MD-1024, antioxidant PEP-36, antioxidant P-EPQ, antioxidant 626, antioxidant 627AV, etc.
The lubricant is selected from lubricant EBS or lubricant zinc stearate.
Further, a method for preparing the polyamide composition having NTC effect as described above, comprising mixing the polyamide resin, the metal iodide, the fluorosulfonic acid compound, the plasticizer, the carbon black and other additives uniformly in proportion, and extruding and granulating the mixture through a twin-screw extruder to obtain the polyamide composition having NTC effect.
Compared with the prior art, the polyamide composition with the NTC effect has the temperature response characteristic, the polyamide resin is added with the metal sulfonate, the fluorosulfonic acid compound, the carbon black and the plasticizer, and the polyamide composition with the NTC effect can be prepared by adding the metal iodide in a low proportion under the combined action of the specific metal iodide, the specific fluorosulfonic acid compound and the carbon black and the plasticizer, is a good polymer-based thermistor material (NTC material), and can be widely applied to the fields of electric blankets, electric heating cushions, warm air cushions, electric heating plate heaters, electric fireplaces, saddle heaters and other electric heaters.
Drawings
FIG. 1 is a schematic diagram of a resistance line for performance testing.
Detailed Description
In order that those skilled in the art will better understand the disclosure, the present invention will be further described in detail with reference to the following specific examples.
PA 1212: tin-free invar nylon, ltd, melting point 183 ℃;
PA 66: 50BWFS, ASCED technologies, Inc., melting point 265 ℃;
zinc iodide, potassium iodide: analytically pure, Shanghai Aladdin Biotechnology GmbH;
carbon black 1: ENSACO, E250G, specific surface area 65m 2 (iv)/g, DBP value of 190ml/100g, Yirui stone China Co., Ltd.;
carbon black 2: ENSACO, E350G, specific surface area 770m 2 (iv)/g, DBP value of 220ml/100g, Yiruishi China Limited;
carbon black 3: HIBLACK 50L with a specific surface area of 110m 2 (iv)/g, DBP value 40ml/100 g: deguss chemical industry;
plasticizer: n-butylbenzenesulfonamide (BBSA), N-Ethylbenzenesulfonamide (EBSA), Kagaku, Neze, Inc.;
potassium perfluorooctane sulfonate PFBS-A: FC-98, WuhansaiVol chemical Co., Ltd;
antioxidant: riandong, RIANOX MD-1024;
the rest of the raw materials are commercially available.
Examples 1 to 14
Preparing materials according to the weight parts shown in table 1, uniformly mixing polyamide, metal iodide, fluorosulfonic acid compound, plasticizer, carbon black and antioxidant, and extruding and granulating by a double-screw extruder with a screw nominal diameter of 40mm to obtain the polyamide composition.
Comparative example 1
The polyamide composition is prepared by preparing the materials according to the weight parts shown in Table 1, uniformly mixing the polyamide, the metal iodide, the plasticizer, the carbon black and the antioxidant, and extruding and granulating the mixture by a double-screw extruder with a screw nominal diameter of 40 mm.
Comparative example 2
The polyamide composition is prepared by preparing the materials according to the weight parts shown in Table 1, uniformly mixing the polyamide, the fluorosulfonic acid compound, the plasticizer, the carbon black and the antioxidant, and performing extrusion granulation by using a double-screw extruder with a screw nominal diameter of 40 mm.
Comparative examples 3 to 5
The polyamide composition is prepared by preparing the materials according to the weight parts shown in Table 1, uniformly mixing the polyamide, the metal iodide, the fluorosulfonic acid compound, the plasticizer, the carbon black and the antioxidant, and performing extrusion granulation by a double-screw extruder with a screw nominal diameter of 40 mm.
Comparative example 6
The polyamide composition is prepared by preparing the materials according to the weight parts shown in Table 1, uniformly mixing the polyamide, the metal iodide, the fluorosulfonic acid compound, the plasticizer and the antioxidant, and performing extrusion granulation by using a double-screw extruder with a screw nominal diameter of 40 mm.
Performance testing
The polyamide compositions obtained in the examples and comparative examples were extruded to obtain a cable having a thickness of 0.8mm using a schematic diagram of a resistance wire as shown in FIG. 1, 1 being a polyester core wire (diameter 1.2mm, core wire based on PET having a relative viscosity of 1.0), 2 being a copper alloy electrode wire (thickness 0.3mm, copper-nickel content 98:2), 3 being a nylon heat-sensitive layer (0.8mm), 4 being a copper alloy electrode wire (thickness 0.3mm, copper-nickel content 98:2), 5. a heat-resistant PVC outer layer (0.8mm, PVC cable having a heat resistance rating of 105 ℃, provided by Annett Cable Co., Ltd., Changzhou). The extruded multilayer cable was folded in half at-30 ℃, and then the outer layer of the cable was peeled off, and the state of the nylon layer at the folded position was observed.
Referring to GB/T666.3-2007 (direct heating negative temperature coefficient thermistor), the national standard adopts a Haake single screw extruder to extrude a sheet with the diameter of 1mm, cuts out a sheet with the diameter of 70mm multiplied by 1mm, connects a high resistance instrument with the model of PROSTAT @ PRC-801 at two ends of the sheet, and is matched with a constant temperature oven to test the change of the sheet resistance with the diameter of 70mm multiplied by 1mm at different temperatures. A voltage of 10V-100V was applied to both ends of the sheet, and both ends of the sheet were placed in an oven for 30min, and the oven temperatures were set to 30 ℃ and 70 ℃ respectively, and the change in the resistance of the insulating material was measured and is shown in Table 2.
Tensile strength and elongation at break were measured by injection moulding 0.75mm tensile specimens according to standard ISO 5251 BA, drawing at a speed of 50mm/min and are shown in tables 2 and 3, respectively.
TABLE 1 tables of formulations of examples and comparative examples
TABLE 2 Properties of Polyamide compositions test Table-1
TABLE 3 Properties of Polyamide compositions Table-2
| Comparative example 1 | Comparative example 2 | Comparative example 3 | Comparative example 4 | Comparative example 5 | Comparative example 6 | |
| Resistance 1/ohm (30 ℃ C.) | 93000 | 46000 | 9420 | 8730 | 6700 | 93000 |
| |
37000 | 10300 | 4930 | 3210 | 2300 | 7800 |
| Elongation at Break (%) | 73 | 68 | 40 | 35 | 90 | 70 |
| Bending at 180 degrees at-30 ℃, and observing the change of the nylon layer | Does not crack | Does not crack | Cracking of | Cracking of | Does not crack | Does not crack |
| NTC effect (resistance 1/resistance 2) | 2.5 | 4.4 | 1.9 | 2.7 | 2.9 | 12 |
Experimental results show that the elongation at break of the material at low temperature can be influenced by adding high-content inorganic matters, and the NTC effect value of the polyamide composition with the NTC effect is between 20 and 60; the elongation at break is high, and the cracking phenomenon is not easy to generate particularly under the low-temperature environment.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (11)
1. Polyamide composition having an NTC effect, characterized in that: comprises the following components in parts by weight:
2. polyamide composition with NTC effect according to claim 1, characterized in that: the composition comprises the following components in parts by weight:
3. polyamide composition with NTC effect according to claim 2, characterized in that:
the weight ratio of the metal iodide to the fluorosulfonic acid compound is 0.4 to 10.
4. Polyamide composition with NTC effect according to any of claims 1 to 3, characterized in that:
the polyamide resin is at least one selected from aliphatic polyamide, semi-aromatic polyamide and polylactam.
5. Polyamide composition with NTC effect according to any of claims 1 to 3, characterized in that:
the polyamide resin is selected from polyamides with a melting point of 150-230 ℃.
6. Polyamide composition with NTC effect according to any of claims 1 to 3, characterized in that:
the metal iodide is at least one compound selected from the group consisting of zinc iodide, tin iodide, antimony iodide, copper iodide, nickel iodide, manganese iodide, cobalt iodide, iron iodide, lead iodide, cadmium iodide, titanium iodide, sodium iodide, and potassium iodide, and hydrates thereof.
7. Polyamide composition with NTC effect according to any of claims 1 to 3, characterized in that:
the fluorosulfonic acid compound is selected from one or more of perfluorooctane sulfonate amine, perfluorooctane sulfonate potassium, perfluorooctane sulfonate tetraethyl amine, and perfluorooctane sulfonate amidoglutamate potassium.
8. Polyamide composition with NTC effect according to any of claims 1 to 3, characterized in that:
the carbon black has a BET specific surface area of 2 to 200m 2 (iv)/g, standard DBP absorption is 50-300ml/100 g.
9. Polyamide composition with NTC effect according to any of claims 1 to 3, characterized in that:
the plasticizer is selected from one or more of N-butyl benzene sulfonamide, p-toluene sulfonamide, o-p-toluene sulfonamide, p-toluene sulfonyl chloride, N- (2-hydroxypropyl) benzene sulfonamide, N-ethyl o-p-toluene sulfonamide, N-ethyl p-toluene sulfonamide, toluene sulfonamide formaldehyde resin butyl acetate solution, N-cyclohexyl p-toluene sulfonamide, N-diethyl p-toluene sulfonamide, N-ethyl benzene sulfonamide, N-isopropyl benzene sulfonamide, N-alkyl p-toluene sulfonamide, N- (2-hydroxyethyl) benzene sulfonamide, N-bis (2-hydroxyethyl) p-toluene sulfonamide, N- (2-hydroxyethyl) p-toluene sulfonamide and benzene sulfonamide.
10. Polyamide composition with NTC effect according to any of claims 1 to 3, characterized in that:
the other auxiliary agent comprises at least one of an antioxidant and a lubricant.
11. A process for the preparation of a polyamide composition having NTC effect according to any one of claims 1 to 10:
the polyamide resin, the metal iodide, the fluorosulfonic acid compound, the plasticizer, the carbon black and other additives are uniformly mixed in proportion, and are extruded and granulated through a double-screw extruder to prepare the polyamide composition with the NTC effect.
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| CN202010996708.2A CN114249979B (en) | 2020-09-21 | 2020-09-21 | Polyamide composition with NTC effect and preparation method thereof |
| PCT/CN2021/078174 WO2022057210A1 (en) | 2020-09-21 | 2021-02-26 | Polyamide composition having ntc effect and preparation method therefor |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS58215449A (en) * | 1982-06-08 | 1983-12-14 | Daicel Chem Ind Ltd | High-molecular temperature-sensing element |
| JPH08313364A (en) * | 1995-05-18 | 1996-11-29 | Matsushita Electric Ind Co Ltd | High polymer temperature sensing body and temperature sensing element using it and electric heater |
| CN104497394A (en) * | 2014-12-11 | 2015-04-08 | 郑州大学 | Polymer based temperature-sensitive resistance material with negative temperature coefficient (NTC) effect and preparation method thereof |
Family Cites Families (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| AT259946B (en) * | 1964-07-24 | 1968-02-12 | Sueddeutsche Kabelwerke | Temperature-independent resistance ignition cable with compensated semiconducting thermoplastic ground conductor, in whose longitudinal axis a tensile core is arranged |
| EP0782153B1 (en) * | 1994-07-13 | 2003-10-29 | Matsushita Electric Industrial Co., Ltd. | Temperature-sensing polymer body and temperature-sensing element made therefrom |
| JPH1017765A (en) * | 1996-07-02 | 1998-01-20 | Matsushita Electric Ind Co Ltd | Polymer temperature sensing element and temperature sensing element using the same |
| TW460429B (en) * | 1997-10-08 | 2001-10-21 | Murata Manufacturing Co | Semiconductive ceramic composition and semiconductive ceramic element using the same |
| CN1215120C (en) * | 2003-04-10 | 2005-08-17 | 广州金发科技股份有限公司 | Nylon(PA66) complex with low surface energy and its preparing method |
| US9175146B2 (en) * | 2006-08-08 | 2015-11-03 | Sabic Global Technologies B.V. | Thermal conductive polymeric PTC compositions |
| EP2438599A2 (en) * | 2009-06-04 | 2012-04-11 | Lydall, Inc. | Electrical insulation materials and methods of making and using same |
| KR101820099B1 (en) * | 2013-01-18 | 2018-01-18 | 에스프린팅솔루션 주식회사 | resistive heat generating material, heating member and fusing device adopting the same |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS58215449A (en) * | 1982-06-08 | 1983-12-14 | Daicel Chem Ind Ltd | High-molecular temperature-sensing element |
| JPH08313364A (en) * | 1995-05-18 | 1996-11-29 | Matsushita Electric Ind Co Ltd | High polymer temperature sensing body and temperature sensing element using it and electric heater |
| CN104497394A (en) * | 2014-12-11 | 2015-04-08 | 郑州大学 | Polymer based temperature-sensitive resistance material with negative temperature coefficient (NTC) effect and preparation method thereof |
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