KR20060004158A - Aqueous conductive polymer composition with ptc of resistivity and preparation therof - Google Patents
Aqueous conductive polymer composition with ptc of resistivity and preparation therof Download PDFInfo
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- KR20060004158A KR20060004158A KR1020040053166A KR20040053166A KR20060004158A KR 20060004158 A KR20060004158 A KR 20060004158A KR 1020040053166 A KR1020040053166 A KR 1020040053166A KR 20040053166 A KR20040053166 A KR 20040053166A KR 20060004158 A KR20060004158 A KR 20060004158A
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- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/14—Conductive material dispersed in non-conductive inorganic material
- H01B1/18—Conductive material dispersed in non-conductive inorganic material the conductive material comprising carbon-silicon compounds, carbon or silicon
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/04—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of carbon-silicon compounds, carbon or silicon
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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Abstract
본 발명은 수용성 고분자 80 ~ 100중량부와, 알코올성 파라핀 왁스 80 ~ 100중량부, 그리고 입도가 0.02 ~ 0.06㎛인 카본블랙 분체 20 ~ 40 중량부 및 계면활성제 0.05 ~ 0.1 중량부로 이루어지는 것을 특징으로 하는 PTC 특성을 갖는 수성 도전성 중합체 조성물이다. 본 발명의 수성 도전성 중합체 조성물은 수용성 고분자 80 ~ 100 중량부와 알코올성 파라핀 왁스 80 ~ 100 중량부를 혼합하여 80 ~ 100℃ 의 온도로 가열하면서 용해시키고, 여기에 온수 80 ~ 800 중량부를 첨가하여 교반, 냉각 시킨 다음, 입도가 0.02 ~ 0.06㎛인 카본블랙 분체 20 ~ 40중량부와 계면활성제 0.05 ~ 0.1 중량부를 교반하에 차례로 첨가하여서 제조된다. The present invention comprises 80 to 100 parts by weight of water-soluble polymer, 80 to 100 parts by weight of alcoholic paraffin wax, and 20 to 40 parts by weight of carbon black powder having a particle size of 0.02 to 0.06 μm, and 0.05 to 0.1 parts by weight of surfactant. Aqueous conductive polymer composition having PTC properties. The aqueous conductive polymer composition of the present invention is dissolved by heating 80 to 100 parts by weight of the water-soluble polymer and 80 to 100 parts by weight of alcoholic paraffin wax, and heated to a temperature of 80 to 100 ℃, 80 to 800 parts by weight of hot water is added, stirring, After cooling, 20 to 40 parts by weight of carbon black powder having a particle size of 0.02 to 0.06 μm and 0.05 to 0.1 parts by weight of surfactant are sequentially added under stirring.
도전성 중합체, PTC, 면상 발열체Conductive Polymer, PTC, Planar Heating Element
Description
본 발명은 PTC 특성을 갖는 수성 도전성 중합체 조성물 및 그 제조방법에 관한 것으로서, 좀더 상세하게는 면상 발열체의 제조에 사용되며, 특히 자기 온도제어 특성이 있어서 초기 발열온도가 60 ~ 70℃까지 만 상승하고 더 이상은 발열이 되지 않는 PTC 특성을 가진 수성 도전성 중합체 조성물 및 그 제조방법에 관한 것이다.The present invention relates to an aqueous conductive polymer composition having a PTC characteristic and a method for manufacturing the same, and more particularly, used in the preparation of a planar heating element, and in particular, having an initial temperature control characteristic, the initial exothermic temperature rises only to 60 to 70 ° C. It further relates to an aqueous conductive polymer composition having a PTC characteristic that does not generate heat and a method for producing the same.
면상 발열체(Plane heater)란 섬유직물에 미세한 입자의 세라믹과 도전성 카본입자를 균일하게 도포하고 여기에 전기를 통하면 열이 발생하는 신소재로서, 일반 가정이나 사무실의 난방재료로는 물론, 도로 제설용, 농업용 난방, 차량 시트, 각종 매트리스, 난방 의류 등의 소재로 다양하게 사용되고 있다. 이러한 면상 발열체를 제조하기 위해서는 일반적으로 도전성 중합체가 사용되는데, 본 발명자는 본 발명에 앞서서 미국특허 제5,556,576호 및 제5,728,322호를 통해서 PTC 특성을 갖는 도전성 중합물 및 그의 코팅방법에 대하여 특허등록을 받은 바 있다. 여기서, PTC라 함은 온도가 상승함에 따라 저항이 증가하는 정온도 계수(Positive temperature coefficients)의 약자로서, PTC 특성은 스스로 온도를 제어하는 자기 온도제어 특성을 말한다. Planar heater is a new material that generates fine heat evenly by applying fine ceramics and conductive carbon particles to textile fabrics and applying electricity to them. It is widely used in materials such as heating for agriculture, vehicle seats, various mattresses and heating clothes. In order to manufacture such a planar heating element, a conductive polymer is generally used, and the present inventors have received a patent registration for a conductive polymer having PTC properties and a coating method thereof through US Patent Nos. 5,556,576 and 5,728,322 prior to the present invention. have. Here, PTC is an abbreviation of positive temperature coefficients in which the resistance increases as the temperature increases, and the PTC characteristic refers to a magnetic temperature control characteristic that controls the temperature by itself.
그런데, 상기 미국특허에 소개된 도전성 중합체는 낮은 전기 저항과 유연한 PTC 특성, 그리고 용이한 성형성 등 여러 가지 소재적 장점이 있음에도 불구하고, 강력한 휘발성이 있는 유기 희석제를 사용하기 때문에 제품의 취급 및 운반, 보관에 있어서 극히 제한적인 조건이 요구되며, 특히 폴리머 제조 및 면상 발열체의 생산과정에서 작업환경이 유해하여 작업자의 건강을 해칠 우려가 있을 뿐만 아니라, 항상 화재 위험성에 노출 되어 있어서 현실적으로 대량 생산이 곤란하다는 문제점이 있었다. By the way, the conductive polymer introduced in the US patent has a variety of material advantages, such as low electrical resistance, flexible PTC properties, and easy formability, but because of the use of a strong volatile organic diluent, handling and transporting the product However, extremely limited conditions are required for storage, especially in the manufacture of polymers and in the production of planar heating elements, the working environment is harmful, which may harm the health of workers, and it is always exposed to the risk of fire, making it difficult to mass produce in reality. There was a problem.
본 발명은 상기와 같은 종래기술의 문제점을 해결하기 위하여, 그 구성성분이 수성 폴리머로서 제품의 취급이나 운반 및 보관이 용이하고, 특히 폴리머의 제조 및 제품 생산과정이 매우 안전하며, 화재의 위험성이 매우 낮기 때문에 대량 생산이 가능한 수성 도전성 중합체 조성물 및 그 제조방법을 제공하는데 그 목적이 있다.
The present invention, in order to solve the problems of the prior art as described above, the component is an aqueous polymer, easy to handle, transport and store the product, in particular, the manufacturing process of the polymer and the product production process is very safe, the risk of fire It is an object of the present invention to provide an aqueous conductive polymer composition and a method for producing the same, which are very low and capable of mass production.
이하, 본 발명을 상세히 설명하면 다음과 같다.Hereinafter, the present invention will be described in detail.
본 발명은 수용성 고분자 80 ~ 100중량부와, 알코올성 파라핀 왁스 80 ~ 100중량부, 그리고 입도가 0.02 ~ 0.06㎛인 카본블랙 분체 20 ~ 40중량부 및 계면활성제 0.05 ~ 0.1중량부로 이루어지는 것을 특징으로 하는 PTC 특성을 갖는 수성 도전성 중합체 조성물이다.The present invention comprises 80 to 100 parts by weight of water-soluble polymer, 80 to 100 parts by weight of alcoholic paraffin wax, and 20 to 40 parts by weight of carbon black powder having a particle size of 0.02 to 0.06 μm, and 0.05 to 0.1 parts by weight of surfactant. Aqueous conductive polymer composition having PTC properties.
또한, 본 발명은 수용성 고분자 80 ~ 100중량부와 알코올성 파라핀 왁스 80 ~ 100중량부를 혼합하여 80 ~ 100℃ 의 온도로 가열하면서 용해시키고, 여기에 온수 80 ~ 800 중량부를 첨가하여 교반, 냉각 시킨 다음, 입도가 0.02 ~ 0.06㎛인 카본블랙 분체 20 ~ 40중량부와 계면활성제 0.05 ~ 0.1중량부를 교반 하에 차례로 첨가하여서 되는 것을 특징으로 하는 PTC 특성을 갖는 수성 도전성 중합체 조성물의 제조방법이다.In addition, the present invention is dissolved by heating 80 to 100 parts by weight of water-soluble polymer and 80 to 100 parts by weight of alcoholic paraffin wax and heated to a temperature of 80 ~ 100 ℃, stirring and cooling by adding 80 to 800 parts by weight of hot water And 20 to 40 parts by weight of carbon black powder having a particle size of 0.02 to 0.06 μm and 0.05 to 0.1 parts by weight of a surfactant are added sequentially under stirring, thereby producing an aqueous conductive polymer composition having a PTC characteristic.
본 발명에 따른 수성 도전성 중합체 조성물은 바인더 및 유화제의 역할을 하는 기초 수지물질인 수용성 고분자와, PTC 특성을 부여하는 단분자형 결정성 물질인 알코올형 파라핀 왁스, 그리고 중합체에 도전성을 부여하는 카본블랙 분체, 마지막으로 이들 구성성분들을 수상 용매에 미 분산 시켜주는 계면활성제로 이루어진다. The aqueous conductive polymer composition according to the present invention is a water-soluble polymer that is a basic resin material serving as a binder and an emulsifier, an alcoholic paraffin wax that is a monomolecular crystalline material that imparts PTC properties, and carbon black that imparts conductivity to the polymer. Powder, and finally, a surfactant that disperses these components in an aqueous phase solvent.
먼저 기초 수지물질인 수용성 고분자로는 예컨대 폴리에틸렌글리콜이나, 폴리에틸렌옥사이드 또는 이들의 혼합물을 사용할 수 있는데, 이와 같은 수용성 고분 자는 중합물이 경화 한 후에 기계적 강도를 제공하는 기능을 한다. 즉, 가열에 의해 경화 된 후, 열 및 산소에 대하여 충분한 내재적 저항을 가지며, 특히 반복되는 가열 및 냉각에 대해서도 물리적 및 기계적 강도를 안정적으로 유지한다. 본 발명에서 수용성 고분자의 함량은 80 ~ 100중량부인데, 만일 수용성 고분자의 함량이 80중량부 이하이면, 경화된 중합물의 기계적 강도가 약해져서 좋지 않고, 반대로 100중량부 이상이면 다른 구성 성분의 특성에 불리한 영향을 주게 된다. First, a water-soluble polymer that is a basic resin material may be, for example, polyethylene glycol, polyethylene oxide, or a mixture thereof. Such water-soluble polymers provide a mechanical strength after the polymer is cured. That is, after hardening by heating, it has sufficient intrinsic resistance to heat and oxygen, and especially maintains physical and mechanical strength stably even with repeated heating and cooling. In the present invention, the content of the water-soluble polymer is 80 to 100 parts by weight. If the content of the water-soluble polymer is 80 parts by weight or less, the mechanical strength of the cured polymer may not be weakened. Adverse effects.
다음으로, PTC특성을 부여하기 위하여 첨가하는 물질은 융점에서 최대 볼륨(volumn)을 갖는 결정성 단분자 화합물을 사용하는 것이 좋은데, 바람직하기로는 알코올성 파라핀왁스를 사용한다. 불순물이 없는 파라핀은 경화된 중합체에서 보다 큰 저항치를 갖는다. 본 발명에서 파라핀 왁스의 함량은 상기 수용성 고분자의 함량과 같은 80 ~ 100 중량부이다. 만일, 파라핀 왁스의 함량이 80 중량부 이하이면, 원하는 PTC 특성을 얻을 수 없고, 반대로 100 중량부 이상이면, 함량 증가에 따른 효과 상승을 기대 하기 어렵다. PTC특성 부여 물질은 기초 수지물질과 서로 잘 어울리는 상용성(compatibility)를 가져야 하며, 기초 수지물질의 종류가 달라지면, 그 기초 수지물질이 갖는 물리적, 기계적 특성을 실현하기 위해서는 PTC 특성 부여물질의 종류도 달라져야 한다.Next, it is preferable to use a crystalline monomolecular compound having a maximum volume at the melting point as the material to be added to impart PTC properties, preferably alcoholic paraffin wax. Paraffins without impurities have greater resistance in cured polymers. The content of paraffin wax in the present invention is 80 to 100 parts by weight, such as the content of the water-soluble polymer. If the content of paraffin wax is 80 parts by weight or less, desired PTC properties cannot be obtained, and conversely, if the content of paraffin wax is 100 parts by weight or more, it is difficult to expect an effect increase due to the content increase. The PTC characterizing material should have compatibility with the basic resin material. If the type of the basic resin material is different, the type of the PTC characteristic material may be used to realize the physical and mechanical properties of the basic resin material. It must be different.
중합체에 도전성을 부여하기 위하여 첨가되는 카본블랙 분체는 입도가 0.02 ~ 0.06㎛인 것을 사용하는 것이 가장 좋고, 그 함량은 20 ~ 40 중량부인 것이 가장 좋다. 본 발명에서 도전성 카본블랙의 함량이 20 중량부 이하이면 도전성이 불량하게 되어 결국 원하는 발열효과를 얻을 수 없고, 반대로 40 중량부 이상이면 다른 구성 성분의 함량이 상대적으로 낮아져서 전체적인 물성에 나쁜 영향을 미친다.The carbon black powder added in order to impart conductivity to the polymer is best to use a particle size of 0.02 ~ 0.06㎛, the content is most preferably 20 to 40 parts by weight. In the present invention, when the content of the conductive carbon black is 20 parts by weight or less, the conductivity becomes poor, and thus, the desired heat generation effect cannot be obtained. On the contrary, when the content of the conductive carbon black is 40 parts by weight or more, the content of other components is relatively low, which adversely affects the overall physical properties. .
마지막으로 계면활성제로는 비이온성 분산균염제를 사용한다. 계면활성제는 상기와 같은 구성 성분들을 수상 용매에 미분산 시키는 기능을 하며, 그 함량은 0.05 ~ 0.1중량부인 것이 가장 효과적이다. Finally, nonionic dispersion bactericides are used as surfactants. The surfactant functions to disperse the above components in the aqueous phase solvent, and the content thereof is most effectively 0.05 to 0.1 parts by weight.
본 발명에 따른 도전성 중합체 조성물은 다음과 같은 방법으로 제조된다.The conductive polymer composition according to the present invention is prepared by the following method.
먼저 수용성 고분자 80 ~ 100중량부와 알코올성 파라핀왁스 80 ~ 100중량부를 충분히 혼합하고, 이 혼합물을 80 ~ 100℃ 의 온도로 가열하면서 용해시킨 다음, 상기 혼합물에 80 내지 800 중량부의 온수를 첨가하고, 충분히 교반하면서 상온까지 냉각 시킨다. 이어서 상기 혼합물에 입도가 0.02 ~ 0.06㎛인 카본블랙 분체 20 ~ 40중량부를 첨가하여 매끄러운 페이스트가 형성될 때 까지 교반 하고, 여기에 계면활성제 0.05 ~ 0.1중량부를 첨가하여 상기 카본블랙 분체가 실질적으로 균일한 분산체가 될 때 까지 충분히 교반한다. First, 80 to 100 parts by weight of the water-soluble polymer and 80 to 100 parts by weight of alcoholic paraffin wax are sufficiently mixed, the mixture is dissolved while heating to a temperature of 80 to 100 ° C., and then 80 to 800 parts by weight of hot water is added to the mixture, Cool to room temperature with sufficient stirring. Subsequently, 20 to 40 parts by weight of carbon black powder having a particle size of 0.02 to 0.06 μm was added to the mixture, followed by stirring until a smooth paste was formed, and 0.05 to 0.1 parts by weight of surfactant was added thereto to make the carbon black powder substantially uniform. Stir well until you get one dispersion.
이렇게 하여 제조된 도전성 중합체 조성물을 이용하여 면상 발열체를 제조하기 위해서는 먼저 상기 도전성 중합체를 함침 가능한 페이스트 형태로 제조하고, 이 페이스트에다 미리 준비된 섬유 기재를 함침 하므로써 본 발명에 따른 면상 발 열체를 제조할 수 있다. 이때, 제조된 면상 발열체의 표면에다 표면 방습제로서 바람직하기로는 스티렌-부타디엔 고무(SBR), 예컨대 LATEX를 처리할 수도 있다. In order to manufacture the planar heating element using the conductive polymer composition thus prepared, the planar heating element according to the present invention can be prepared by first preparing the conductive polymer in the form of a paste that can be impregnated, and impregnating the previously prepared fiber substrate. have. At this time, styrene-butadiene rubber (SBR) such as LATEX may be treated on the surface of the manufactured planar heating element, preferably as a surface desiccant.
이하, 본 발명에 대한 실시 예를 들어 보면 다음과 같다. 그러나 본 발명의 범위가 실시 예에 한정되는 것은 아니다.Hereinafter, an embodiment of the present invention will be described. However, the scope of the present invention is not limited to the embodiment.
실시예 1Example 1
폴리에틸렌글리콜 95중량부와 파라핀왁스 95중량부를 혼합하여 교반용기에 넣고 약 90℃ 까지 가열하여 용해시킨 후, 여기에다 200중량부의 온수를 첨가 하면서 고형분이 미 분산 될 때까지 교반한 다음, 상온까지 냉각 처리한다. 이어서 입도가 0.02 ~ 0.06㎛인 카본블랙 30중량부를 투입하고 약 1500rpm 으로 3시간 정도 교반한 다음, 계면활성제[제품명; Disperol UDL-200, 제조사; 신영화성공업(주)] 0.08중량부를 첨가하고, 이 혼합물을 3개의 롤링밀에 통과 시켜서 최종적인 수성 도전성 중합체 조성물을 얻는다.95 parts by weight of polyethylene glycol and 95 parts by weight of paraffin wax are mixed and dissolved in a stirring container by heating to about 90 ° C., and then stirred until the solid content is undispersed while adding 200 parts by weight of hot water, followed by cooling to room temperature. do. Subsequently, 30 parts by weight of carbon black having a particle size of 0.02 to 0.06 µm was added thereto, stirred at about 1500 rpm for about 3 hours, and then a surfactant [product name; Disperol UDL-200, manufacturer; Shinyoung Kogyo Co., Ltd.] 0.08 parts by weight is added, and the mixture is passed through three rolling mills to obtain a final aqueous conductive polymer composition.
실시예 2Example 2
수용성 고분자로서 폴리에틸렌글리콜 대신에 폴리에틸렌옥사이드를 사용하는 것 이외에는 상기 실시예 1과 동일한 방법으로 수성 도전성 중합체 조성물을 제조한다.An aqueous conductive polymer composition was prepared in the same manner as in Example 1 except that polyethylene oxide was used instead of polyethylene glycol as a water-soluble polymer.
실시예 3Example 3
수용성 고분자로서 폴리에틸렌글리콜과 폴리에틸렌옥사이드의 등량 혼합물을 사용하는 것 이외에는 상기 실시예 1과 동일한 방법으로 수성 도전성 중합체 조성물을 제조한다.An aqueous conductive polymer composition was prepared in the same manner as in Example 1, except that an equivalent mixture of polyethylene glycol and polyethylene oxide was used as the water-soluble polymer.
상기 실시예 1 ~ 3에 따라 제조된 수성 도전성 중합체 조성물의 페이스트에다 섬유를 함침 시킨 후, 130℃에서 건조하고 경화하여 면상 발열체를 제조하고, 그 표면에 LATEX를 도포하여 방습 처리한다. 이와같이 하여 제조된 면상 발열체에 대하여 Rp/Rr값(Rp는 최대 저항값, Rr은 상온에서의 저항값)을 측정한 결과, 약 10 인 것으로 나타났으며, 각 실시예 별로 유의성있는 차이는 나타나지 않았다. After impregnating the fibers in the paste of the aqueous conductive polymer composition prepared according to Examples 1 to 3, and dried and cured at 130 ℃ to produce a planar heating element, the surface is coated with LATEX to be moisture-proof. As a result of measuring the Rp / Rr value (Rp is the maximum resistance value and Rr is the resistance value at room temperature) of the planar heating element thus manufactured, it was found to be about 10, and there was no significant difference in each example. .
본 발명에 따른 수성 도전성 중합체 조성물은 휘발성 유기 희석제를 사용하지 않기 때문에 무엇보다 작업 공정이 안전하고 화재의 염려가 없어서 대량생산이 가능하다는 효과가 있다. 또한, 본 발명의 수성 도전성 중합체 조성물은 초기 발열온도가 60 ~ 70℃까지만 상승하고 더 이상은 발열이 되지 않는 PTC 특성을 가지고 있어서 열 안정성이 매우 우수하고, 염색 처리가 가능한 면상 발열체를 대량으로 제조 할 수 있다.Since the aqueous conductive polymer composition according to the present invention does not use a volatile organic diluent, the working process is safe and there is no fear of fire. In addition, the aqueous conductive polymer composition of the present invention has a PTC characteristic that the initial exotherm temperature rises only to 60 ~ 70 ℃ and does not generate any more heat, so excellent in thermal stability, and a large amount of planar heating elements capable of dyeing treatment are produced. can do.
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