KR100555962B1 - Hard foam rubber closed cellular ebonite - Google Patents

Hard foam rubber closed cellular ebonite Download PDF

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KR100555962B1
KR100555962B1 KR1020040078308A KR20040078308A KR100555962B1 KR 100555962 B1 KR100555962 B1 KR 100555962B1 KR 1020040078308 A KR1020040078308 A KR 1020040078308A KR 20040078308 A KR20040078308 A KR 20040078308A KR 100555962 B1 KR100555962 B1 KR 100555962B1
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nbr
float
foaming
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KR20060008199A (en
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만 영 차
진 숙 김
종 진 이
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만 영 차
종 진 이
진 숙 김
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L9/00Compositions of homopolymers or copolymers of conjugated diene hydrocarbons
    • C08L9/02Copolymers with acrylonitrile
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    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00Processes of treating or compounding macromolecular substances
    • C08J3/20Compounding polymers with additives, e.g. colouring
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C08J9/00Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
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    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
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    • C08L61/00Compositions of condensation polymers of aldehydes or ketones; Compositions of derivatives of such polymers
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    • C08L2205/02Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group

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Abstract

본 발명은 NBR계 합성고무를 주성분으로 각종 첨가제가 첨가되어 혼합생성된 고무생지를 발포시켜 형성되는 발포플로트의 혼합공정에서 각 첨가제의 조성비를 조절하고 카본블랙계 보강제를 첨가하여 내고압성 및 내가소홀성이 월등히 향상되는 발포플로트에 관한 것이다.The present invention is to control the composition ratio of each additive in the mixing process of the foamed float formed by foaming the rubber dough mixed with various additives added as the main component of the NBR-based synthetic rubber, and the carbon black-based reinforcing agent is added to It relates to a foamed float that greatly improves neglectability.

이를 실현하기 위한 본 발명은, 합성고무인 아크릴로 니트릴 부타디엔 라바(NBR)를 주성분으로 하여 각종 첨가제가 첨가되어 혼합되는 혼합공정, 상기 혼합공정에서 생성된 고무생지를 1차, 2차 가류성형 후 열처리하여 제조되는 발포플로트에 있어서, 상기 혼합공정은 NBR 100중량부에, 각종 첨가제와 그의 중량기준으로 내고압성을 향상시키는 보강제로서 SRF 또는 HAF 또는 MT 또는 Clay 중 어느 하나 이상이 50% 이하로 첨가되어 혼합되는 것을 특징으로 하는 내고압성 및 내가소홀이 향상되는 발포플로트를 제공하여 45kg/cm2이상에서도 파손되지 않는 내고압성 및 내가소홀성이 구비되어 LPG 연료 및 알콜계연료를 포함하여 거의 모든 액상연료의 연료탱크에 사용가능한 발명임.The present invention for realizing this is a mixing process in which various additives are added and mixed with acrylonitrile butadiene lava (NBR), which is a synthetic rubber, as a main component, and heat treatment after primary and secondary vulcanization molding of the rubber dough produced in the mixing process. In the foamed float produced in the above, the mixing step is added to the NBR 100 parts by weight, at least one of SRF, HAF, MT or Clay as a reinforcing agent to improve the high pressure resistance on the basis of various additives and its weight. It provides a high pressure resistance and foaming float that is improved, characterized in that the mixing is improved, the high pressure resistance and resistance to breakage is not broken even at 45kg / cm 2 or more, including LPG fuel and alcohol-based fuel The invention can be used for fuel tanks of all liquid fuels.

내고압성, 내가소홀성, MT, HAF, SRFHigh pressure resistance, neglect resistance, MT, HAF, SRF

Description

발포플로트{Hard foam rubber closed cellular ebonite}Foam float {Hard foam rubber closed cellular ebonite}

도 1은 본 발명에 따라 제조된 내고압성이 향상된 발포플로트의 50배 단면확대사진,1 is a 50 times cross-sectional enlarged photograph of a high-pressure-resistant foam float prepared according to the present invention,

도 2는 종래기술에 의한 발포플로트의 50배 단면확대사진,Figure 2 is a 50 times cross-sectional enlarged picture of the foam according to the prior art,

도 3a는 본 발명에 따라 제조된 내고압성이 향상된 발포플로트의 표면사진,Figure 3a is a photograph of the surface of the high pressure resistance foam foam improved according to the present invention,

도 3b는 본 발명에 따라 제조된 내가소홀성이 향상된 발포플로트의 표면사진,Figure 3b is a photograph of the surface of the expanded float prepared in accordance with the present invention,

도 4는 종래기술에 의한 발포플로트의 표면사진이다.4 is a photograph of the surface of the foamed float according to the prior art.

본 발명은 각종 액상연료가 저장되는 연료탱크 내에 설치되는 발포플로트에 관한 것으로, 더욱 상세하게는 NBR계 합성고무를 주성분으로 각종 첨가제가 첨가되어 혼합생성된 고무생지를 발포시켜 형성되는 발포플로트의 혼합공정에서 각 첨가제의 조성비를 조절하고 카본블랙계 보강제를 첨가하여 내고압성 및 내가소홀성이 월등히 향상되는 발포플로트에 관한 것이다.The present invention relates to a foamed float which is installed in a fuel tank in which various liquid fuels are stored. More specifically, a mixture of foamed floats formed by foaming a rubber produced by adding various additives as a main component of NBR-based synthetic rubber The present invention relates to a foam float in which the composition ratio of each additive in the process is adjusted and a carbon black-based reinforcing agent is added to improve the high pressure resistance and the resistance to resistance.

일반적으로 가솔린, 등유, 경유 또는 LPG(액화석유가스)를 연료로 사용하는 차량의 연료탱크내 연료의 액위를 감지하기 위하여 플로트(float) 및 게이지 등이 설치된다.In general, a float and a gauge are installed to detect the level of fuel in a fuel tank of a vehicle using gasoline, kerosene, diesel, or LPG (liquefied petroleum gas) as a fuel.

통상 가솔린 차량 등에 사용되는 플로트의 경우 5~10kg/cm2 의 압력에 견딜 수 있어야 하고, LPG 또는 산업용 차량 등에 사용되는 플로트의 경우 25~30kg/cm2의 압력에 견딜 수 있게 제작되어야 한다. Floats used in gasoline vehicles and the like must withstand a pressure of 5 to 10 kg / cm 2 , and floats used in LPG or industrial vehicles should be made to withstand a pressure of 25 to 30 kg / cm 2 .

또한, LPG 또는 프로판가스가 저장되는 용기의 경우에도 과충전을 방지해 주는 안전장치로써 OPD(Overfill protection device)밸브 등이 채용되어 내부공간의 약 80% 정도가 충전되면 자동으로 가스유입을 차단하는데 여기에도 플로트가 설치된다.In addition, in the case of LPG or propane gas storage, an overfill protection device (OPD) valve is adopted as a safety device to prevent overcharging, and the gas inlet is automatically blocked when about 80% of the internal space is filled. Float is installed.

이처럼 플로트는 액상연료와 직접 접촉하는 부품인 만큼 비중이 낮아야 하고, 내유성 및 내수성 등의 내화학성이 강해야 하며, 고압용기 내에서 사용되므로 내고압성이 우수한 아크릴로 니트릴 부타디엔 라바(NBR; Acrylo nitrile-butadiene rubber)계 재질의 발포플로트가 주류를 이룬다.As the float is a part that is in direct contact with liquid fuel, the specific gravity should be low, and the chemical resistance such as oil resistance and water resistance should be strong, and the acrylonitrile butadiene lava (NBR; Butadiene rubber-based foam float is the mainstream.

발포플로트는 상기한 바와 같은 요건을 만족하기 위해 합성고무인 NBR에 여러가지 첨가제가 첨가되어 혼합생성된 고무생지를 발포 성형하는 방식으로 제조되며, 통상적으로 1차 가류성형하는 발포공정과 2차 가류성형하는 발포공정을 거쳐 제조된다.In order to satisfy the requirements as described above, the foamed float is manufactured by foam molding a rubber product mixed with various additives to NBR, which is a synthetic rubber, and is commonly used for the first vulcanization and the second vulcanization. It is manufactured through a foaming process.

이러한 발포플로트에 관한 종래기술로서 대한민국 등록특허공보 제307396호 에서는 NBR과 페놀수지를 주 원료로 하는 원료 혼합공정, 혼합공정 후 생성된 생지를 1차적으로 금형판에 주입하여 적당한 크기로 재단하는 공정, 재단된 생지를 1차 가류시키는 공정, 1차 가류 후 다시 200℃정도에서 가류하고 경화하는 성형공정과 성형물을 냉각 건조시키는 공정으로 제조되는 내가소홀성 발포플로트에 있어서, 상기 발포플로트가 메틸에틸케톤이 0.02∼0.1중량비율로 혼합된 에폭시수지혼합물로 코팅되는 것을 특징으로 하는 내가소홀성 발포플로트를 제시하고 있다.As a prior art for such a foam float, the Republic of Korea Patent Publication No. 307396 is a raw material mixing step of NBR and phenolic resin as the main raw material, the raw material produced after the mixing step is first injected into the mold plate and cut to a suitable size In the refractory foam float produced by the first step of vulcanized dough, the first step of vulcanization and curing at about 200 ℃ after the first cure and the step of cooling and drying the molded product, the foam float is methyl ethyl A ketone is proposed for a non-permeable foam float characterized in that it is coated with an epoxy resin mixture mixed at a weight ratio of 0.02 to 0.1.

그러나 종래기술에 의한 발포플로트는 그 사용압력이 약 20kg/cm2~30kg/cm2 정도의 내압성을 구비하고 있는바, 최근 들어 그 수요가 급증하고 있는 LPG를 연료로 사용하는 차량의 연료탱크 내에 설치되기에는 안정성에 있어 부족하다 할 것이다.However, the foamed float according to the prior art has a pressure resistance of about 20 kg / cm 2 to 30 kg / cm 2 , and thus, in a fuel tank of a vehicle using LPG as a fuel, the demand is increasing rapidly in recent years. It will be insufficient in stability to be installed.

또한, 일반적인 가솔린 자동차의 연료탱크의 경우에도 연료탱크 내에서 순간적으로 고압이 발생되는 경우나 발포플로트와 연료 간에 화학작용 등이 발생되는 경우에 발포플로트의 셀(cell; 기포, 기공)조직이 파손되고 결국 발포플로트에 연료가 침투하여 제 기능을 발휘하지 못한다는 문제점이 있다. In addition, even in the case of a fuel tank of a general gasoline automobile, the cell structure of the foamed float is damaged when a high pressure is generated in the fuel tank or when a chemical reaction between the foamed float and the fuel occurs. As a result, fuel penetrates into the foam float and does not exhibit proper function.

한편, 최근들어 우리나라 차량이 많이 수출되고 있는 중남미 등의 국가에서는 무연휘발유 80~90%와 절대에탄올 및 메탄올을 10~20%를 섞어서 만든 알콜계 자동차 연료인 가소홀(Gasohol)을 많이 사용하고 있는 바 이러한 국가에 자동차를 수출하는 우리나라의 실정을 감안하면 가소홀에도 내성이 우수한 발포플로트가 제시되어야 할 필요성이 있다.In recent years, countries such as Central and South America, where Korean vehicles are widely exported, use gasohol, an alcohol-based automobile fuel made of 80 to 90% unleaded gasoline and 10 to 20% of absolute ethanol and methanol. Considering Korea's situation of exporting automobiles to these countries, it is necessary to present foamed floats with excellent resistance to plastic holes.

그러나 상기 종래기술의 내가소홀성 발포플로트는 1차 가류공정과 2차 가류공정을 마친 후에 에폭시수지혼합물로 코팅하는 별도의 공정을 거쳐야 되는 바 제조공정이 추가되어 제조과정이 복잡해지므로써 제조단가를 상승시키고 발포플로트 자체에 내가소홀성이 구비되는 것이 아니라 그 외면에 내가소홀성 혼합물을 코팅하는 구조이므로 안정성이 떨어진다는 문제점이 있다.However, the non-resistant foam of the prior art has to go through a separate process of coating with epoxy resin mixture after the first vulcanization process and the second vulcanization process, the manufacturing process is added to the manufacturing process is complicated to increase the manufacturing cost There is a problem that the stability is lowered because the structure is coated with the non-hole-resistant mixture on the outer surface of the foam float itself is not provided.

따라서 본 발명은 액상연료가 저장되는 연료탱크 내에 설치되는 발포플로트가 충분한 내고압성과 내유성 및 내수성을 구비하여 LPG 연료 및 알콜계 연료를 사용하는 차량의 연료탱크를 포함하여 액상연료를 저장하는 대부분의 연료탱크 내에서 안정적으로 사용가능하도록 하는 내고압성 또는 내가소홀성이 구비되는 발포플로트를 제공하고자 함에 그 목적이 있다.
Therefore, the present invention is a foam float installed in the fuel tank in which the liquid fuel is stored is provided with a sufficient high pressure resistance, oil resistance and water resistance, including the fuel tank of the vehicle using LPG fuel and alcohol fuel to store most of the liquid fuel It is an object of the present invention to provide a foam float having high pressure resistance or neglect resistance to be stably usable in a fuel tank.

상기한 목적을 달성하기 위한 본 발명은, 합성고무인 아크릴로 니트릴 부타디엔 라바(NBR)를 주성분으로 하여 페놀수지와 가류제와 발포제와 보강제 및 촉진제 등이 혼합되는 혼합공정, 상기 혼합공정에서 생성된 고무생지를 발포제의 분해 온도보다 낮은 온도에서 완제품의 크기보다 작게 1차 가류성형하여 생성된 발포성형물을 발포제의 분해온도 보다 높은 온도에서 완제품의 크기로 2차 가류성형 후 열처리하여 제조되는 발포플로트에 있어서, 상기 혼합공정은 NBR 100중량부에, 그의 중량기준으로 페놀수지 35∼55%, 가류제로서 유황 30∼40%, 가류조제로서 산화아연(ZnO) 5%~5.5% 및 스테아르산 1∼1.5%, 발포제로서 DPT 5∼7%, 발포조제로서 DPT조제 3∼4.5%, 촉진제로서 CZ 1.8∼2.1%, 보강제로서 SRF 또는 HAF 또는 MT 또는 Clay 중 어느 하나 이상이 50% 이하로 첨가되어 혼합되므로서 내고압성이 향상되는 것을 특징으로 한다.In order to achieve the above object, the present invention, a synthetic rubber, a phenol resin, a vulcanizing agent, a blowing agent, a reinforcing agent and an accelerator, etc. are mixed with the main component of acrylonitrile butadiene rubber (NBR), a rubber produced in the mixing process In the foam float produced by heat treatment after the second vulcanization molding to the size of the finished product at a temperature higher than the decomposition temperature of the blowing agent to the size of the final product at the temperature lower than the decomposition temperature of the blowing agent. The mixing step is based on the weight of NBR 100 parts by weight, 35 to 55% phenol resin, 30 to 40% sulfur as vulcanizing agent, 5% to 5.5% zinc oxide (ZnO) as vulcanizing aid and 1 to 1.5 stearic acid. %, 5-7% DPT as blowing agent, 3-4.5% DPT aid as foaming aid, 1.8-2.1% CZ as accelerator, 50% or less of any one of SRF or HAF or MT or Clay as reinforcing agent Since my books are mixed characterized in that the high-pressure castle improved.

본 발명의 다른 사상으로는, 합성고무인 아크릴로 니트릴 부타디엔 라바(NBR)를 주성분으로 하여 페놀수지와 가류제와 발포제와 보강제 및 촉진제 등이 혼합되는 혼합공정, 상기 혼합공정에서 생성된 고무생지를 발포제의 분해온도보다 낮은 온도에서 완제품의 크기보다 작게 1차 가류성형하여 생성된 발포성형물을 발포제의 분해온도 보다 높은 온도에서 완제품의 크기로 2차 가류성형 후 열처리하여 제조되는 발포플로트에 있어서, 상기 혼합공정은 NBR 100중량부에, 그의 중량기준으로 페놀수지 50∼60%, 가류제로서 유황 45∼55%, 가류조제로서 산화아연(ZnO) 5%~5.5% 및 스테아르산 1∼1.5%, 발포제로서 DPT 6∼7.5%, 발포조제로서 DPT조제 3∼4.5%, 촉진제로서 CZ 1.8∼2.1%, 보강제로서 MT 40~50% 및 Clay 3~5% 가 첨가되어 혼합되므로서 내가소홀성이 향상되는 것을 특징으로 한다.According to another aspect of the present invention, a synthetic process in which a phenol resin, a vulcanizing agent, a blowing agent, a reinforcing agent, an accelerator, and the like are mixed with acrylonitrile butadiene laba (NBR), which is a synthetic rubber, as a main component, and the rubber dough produced in the mixing step is a blowing agent. In the foam float produced by heat treatment after secondary vulcanization to the size of the finished product at the temperature higher than the decomposition temperature of the blowing agent to the foamed product produced by primary vulcanization molding at a temperature lower than the decomposition temperature of the foaming agent, the mixing The process is based on 100 parts by weight of NBR, 50 to 60% of phenol resin, 45 to 55% of sulfur as vulcanizing agent, 5% to 5.5% of zinc oxide (ZnO) as vulcanizing aid, and 1 to 1.5% of stearic acid, blowing agent. DPT 6 ~ 7.5% as a foaming aid, 3 ~ 4.5% as a foaming aid, CZ 1.8 ~ 2.1% as a promoter, MT 40-50% and Clay 3 ~ 5% as a reinforcing agent are added and mixed to improve the resistance that It characterized.

본 발명의 내고압성을 향상시키기 위한 발포플로트는 합성고무인 NBR을 주성분으로 하여 페놀수지, 가류제, 가류조제. 발포제, 발포조제, 보강제 및 촉진제가 첨가되어 고무생지를 혼합생성하는 혼합공정, 상기 고무생지를 적당히 재단하고 발포제의 분해온도보다 낮은 온도에서 완제품의 크기보다 작게 1차 가류성형하는 1차 발포공정, 상기 1차 발포공정에서 가류성형된 발포성형물을 발포제의 분해온도 보다 높은 온도에서 완제품의 크기로 2차 가류성형하는 2차 발포공정 및 열처리 공정 등을 포함하여 제조된다.The foamed float for improving the high pressure resistance of the present invention is a phenol resin, a vulcanizing agent, a vulcanizing aid mainly comprising NBR which is a synthetic rubber. Mixing process for mixing and producing rubber dough by adding foaming agent, foaming aid, reinforcing agent and accelerator, primary foaming process for primary vulcanization molding the rubber dough appropriately and smaller than the size of finished product at temperature lower than decomposition temperature of foaming agent, The foamed molded product vulcanized in the primary foaming process is prepared, including secondary foaming process and heat treatment process for secondary vulcanization to the size of the finished product at a temperature higher than the decomposition temperature of the blowing agent.

상기 혼합공정에 사용되는 NBR은 부타디엔(Butadiene)과 아크릴로니트릴(Acrylonitrile)의 공중합으로 제조되며, 내유성을 갖게하는 니트릴(Nitrile) 함량이 35.5%~45%인 제품을 사용한다.NBR used in the mixing process is manufactured by copolymerization of butadiene and acrylonitrile, and a product having a nitrile content of 35.5% to 45% having oil resistance is used.

이러한 NBR에 열경화성 페놀수지, 가류제로서 유황(Sulfur), 가류보조제로서 산화아연(ZnO)과 스테아르산(stearic acid), 발포제로서 DPT, 발포조제로서 DPT조제, 촉진제로서 CZ, 보강제로서 SRF 또는 HAF 또는 MT 또는 Clay 중 어느 하나 이상이 첨가되어 혼합공정을 수행한다.The thermosetting phenolic resin, sulfur as a vulcanizing agent, zinc oxide (ZnO) and stearic acid as a vulcanizing aid, DPT as a blowing agent, DPT as a foaming aid, CZ as a promoter, SRF or HAF as an adjuvant Or one or more of MT or Clay is added to perform the mixing process.

상기한 보강제로서 언급된 SRF, HAF, MT는 고무용 카본블랙(carbon black)계 보강제이다.SRF, HAF and MT mentioned as the above reinforcing agents are carbon black based reinforcing agents for rubber.

카본블랙이란 흑색의 미세한 탄소분말을 일컫는 것이며, 이른바 그을음에 상당하는 것으로 탄소입자의 크기는 1∼500mℓ이며 흑연과 비슷하다.Carbon black refers to black fine carbon powder, which corresponds to so-called soot, and the size of carbon particles is 1 to 500 ml and similar to graphite.

공업적으로는 천연가스, 타르 등을 불완전연소시켜 생긴 그을음을 모으거나, 그것들을 열분해하여 제조하고 있다.Industrially, soot produced by incomplete combustion of natural gas, tar, and the like is collected or pyrolyzed to produce them.

현재 소비량의 85 %가 고무용이고, 11% 정도가 인쇄잉크를 비롯하여 흑색안료로 사용된다. Currently 85% of the consumption is for rubber, and 11% is used for black pigments, including printing inks.

고무용에는 입자가 미세한 사슬 모양의 결합이 없는 것이 적합하며, 증강제나 내유성, 내열성 등의 성질을 주기 위해 사용된다.For rubber, it is suitable that the particles do not have fine chain-shaped bonds, and are used to give properties such as enhancer, oil resistance, heat resistance, and the like.

SRF(Semi reinforcing furnace)는 고무에 혼합이 잘 되고 다량배합해도 작업성이나 물성이 저하되지 않으며 중보강성 및 내노화성이 우수할 뿐만 아니라 가류중(성형중)에 변형이 적다.SRF (Semi reinforcing furnace) is well mixed with rubber and does not degrade workability or physical properties even if it is mixed in large quantities. It is not only excellent in medium reinforcement and aging resistance, but also has little deformation during vulcanization (in molding).

HAF(High abrasion furnace)는 보강성이 양호하고 내마모성, 인장강도, 신장율, 굴곡저항이 우수하여 타이어 등의 제조시에 사용되거나 강도를 요구하는 제품에 많이 사용된다. High abrasion furnace (HAF) has good reinforcement, good abrasion resistance, tensile strength, elongation rate and bending resistance, so it is used in the manufacture of tires or other products that require strength.

MT(Medium thermal)는 고탄성용으로 신장시 인열저항이 적고 다량 충진이 가능하며 특히 내수성이 양호해서 내알콜성이 있는 제품에 사용하면 미세한 조직을 얻을 수 있다.MT (Medium thermal) is a high elasticity, it has low tear resistance at the time of elongation and can be filled in large quantities. Especially, since it has good water resistance, it can obtain fine structure when used in alcohol-resistant products.

또한 상기에서 보강재로 언급된 Clay는 통상의 SiO2(규사)에 Al2O3(산화알미늄) 및 소량의 CaO(석회)가 혼합되어 생성되거나, CaO(석회)에 소량의 SiO2(규사)가 혼합되어 생성되는 경탄 등이 사용될 수 있다.In addition, the clay mentioned above as a reinforcing material is produced by mixing Al 2 O 3 (aluminum oxide) and a small amount of CaO (lime) with conventional SiO 2 (silica), or a small amount of SiO 2 (silica) with CaO (lime) Hard coal produced by mixing may be used.

하기의 표 1에서는 상기 혼합공정에 사용되는 카본블랙계 SRF, HAF, MT의 물 성치를 정리하였다.Table 1 below summarizes the physical properties of the carbon black SRF, HAF, and MT used in the mixing process.

Figure 112004044710341-pat00001
Figure 112004044710341-pat00001

한편 발포플로트에 형성되는 셀(cell; 기포, 기공)의 크기를 작게하고 동일면적에 셀 수량을 많이 형성하기 위하여 셀벽을 두껍게 형성하여야만 한다.On the other hand, in order to reduce the size of the cells (bubbles, pores) formed in the foam float and to form a large number of cells in the same area, the cell walls should be formed thick.

이에 상기 혼합공정에서 셀벽을 두껍게 형성하기 위하여 각 보강제(SRF, HAF, MT, Clay)의 비율을 조절하는 것이 대단히 중요하다.Therefore, it is very important to control the ratio of each reinforcing agent (SRF, HAF, MT, Clay) in order to form a thick cell wall in the mixing process.

또한, 상기 혼합공정에서 첨가되는 보강재(SRF, HAF, MT, Clay)는, NBR 100중량부에, 그의 중량기준으로 SRF 또는 HAF 또는 MT 또는 Clay 중 어느 하나 이상이 50% 이하로 첨가되어야 한다.In addition, the reinforcing material (SRF, HAF, MT, Clay) added in the mixing process, at least one of SRF or HAF, MT or Clay by 50% by weight based on its weight NBR.

이는 보강제의 함유량이 50%를 초과하면 NBR의 고무로서의 역할이 현격히 저하되기 때문이다.This is because when the content of the reinforcing agent exceeds 50%, the role of NBR as rubber is significantly reduced.

이하 상기 혼합공정에 사용되는 각 성분들의 조성비를 조절하여 상기한 조건을 충족시키는 다양한 실시예를 기술한다.Hereinafter, various embodiments for satisfying the above conditions by adjusting the composition ratio of each component used in the mixing process will be described.

실시예 1Example 1

NBR 100중량부에, 그의 중량기준으로 페놀수지 35∼55%, 가류제로서 유황 30∼40%, 가류조제로서 산화아연(ZnO) 5%~5.5%와 스테아르산 1∼1.5%, 발포제로서 DPT 5∼7%, 발포조제로서 DPT조제 3∼4.5%, 촉진제로서 CZ 1.8∼2.1%, 보강제로서 SRF 5~15%, MT 20~30% 가 첨가되어 혼합되는 고무생지를 만든다.100 parts by weight of NBR, 35 to 55% phenolic resin, 30 to 40% sulfur as vulcanizing agent, 5% to 5.5% zinc oxide (ZnO) as vulcanizing aid, 1 to 1.5% stearic acid, DPT as blowing agent 5 to 7%, 3 to 4.5% of DPT aid as foaming aid, 1.8 to 2.1% of CZ as accelerator, 5 to 15% of SRF as a reinforcing agent, and 20 to 30% of MT are added to form a rubber dough.

실시예 2Example 2

NBR 100중량부에, 그의 중량기준으로 페놀수지 35∼55%, 가류제로서 유황 30∼40%, 가류조제로서 산화아연(ZnO) 5%~5.5%와 스테아르산 1∼1.5%, 발포제로서 DPT 5∼7%, 발포조제로서 DPT조제 3∼4.5%, 촉진제로서 CZ 1.8∼2.1%, 보강제로서 HAF 10~20%와 MT 20~30% 가 첨가되어 혼합되는 고무생지를 만든다.100 parts by weight of NBR, 35 to 55% phenolic resin, 30 to 40% sulfur as vulcanizing agent, 5% to 5.5% zinc oxide (ZnO) as vulcanizing aid, 1 to 1.5% stearic acid, DPT as blowing agent 5 to 7%, 3 to 4.5% of DPT aid as foaming aid, 1.8 to 2.1% of CZ as accelerator, and 10 to 20% of HAF and 20 to 30% of MT as reinforcing agent are added to make rubber dough.

실시예 3Example 3

NBR 100중량부에, 그의 중량기준으로 페놀수지 35∼55%, 가류제로서 유황 30∼40%, 가류조제로서 산화아연(ZnO) 5%~5.5%와 스테아르산 1∼1.5%, 발포제로서 DPT 5∼7%, 발포조제로서 DPT조제 3∼4.5%, 촉진제로서 CZ 1.8∼2.1%, 보강제로서 Clay 3~5%와 MT 30~45% 가 첨가되어 혼합되는 고무생지를 만든다.100 parts by weight of NBR, 35 to 55% phenolic resin, 30 to 40% sulfur as vulcanizing agent, 5% to 5.5% zinc oxide (ZnO) as vulcanizing aid, 1 to 1.5% stearic acid, DPT as blowing agent 5 to 7%, 3 to 4.5% of DPT preparation as foaming aid, 1.8 to 2.1% of CZ as accelerator, and 3 to 5% of clay and 30 to 45% of MT as reinforcing agent are added to make rubber dough.

상기한 실시예 1, 2, 3에서 처럼 보강제의 종류와 함량을 달리하여 혼합생성된 고무생지는 통상의 발포플로트 제조시 사용되는 트랜스퍼 방식의 금형에 충진되어 1차 및 2차 발포공정을 거친다.As in Examples 1, 2, and 3, the rubber dough mixed and produced by varying the type and content of the reinforcing agent is filled in a transfer mold used in the manufacture of a conventional foam float, and undergoes primary and secondary foaming processes.

상기 1차 발포공정에서의 가류성형조건은 발포제의 발포온도 160~180℃ 보다 낮은 125℃에서 1200초 정도 가류성형하는 것이 바람직하다.The vulcanization molding conditions in the primary foaming step is preferably vulcanized for about 1200 seconds at 125 ℃ lower than the foaming temperature of 160 ~ 180 ℃ foaming agent.

일례로 1차 발포공정에 사용되는 금형의 설계치수는 완제품의 5할에서 7할정도로 설정되므로, 부피가 20cc이고 비중이 0.2 일 경우 4cc가 충전되어야 한다.For example, the design dimensions of the molds used in the primary foaming process are set at about 50 to 70% of the finished product, so if the volume is 20cc and the specific gravity is 0.2, 4cc should be filled.

이러한 1차 발포공정 후에 형성되는 발포성형물은 탄성체이고 2차 발포공정의 금형에 대해 5할에서 7할정도의 크기를 갖추게 되며 발포제의 발포온도 보다 낮은 온도에서 가류성형 되므로 아직은 미가류상태로 기포가 제대로 형성되지 않고 경도가 떨어지는 경향이 있으므로 2차 발포공정을 수행하게 된다.The foamed molded product formed after the primary foaming process is an elastic body, and has a size of about 50 to 70% of the mold of the secondary foaming process, and it is vulcanized at a temperature lower than the foaming temperature of the foaming agent, and thus bubbles are still uncured. Since it is not formed and the hardness tends to fall, the secondary foaming process is performed.

2차 발포공정의 가류성형조건은 발포제의 온도보다 높은 195℃에서 3600초 정도가 바람직하고, 완제품의 치수로 설정된 금형에 충진되어 가류성형되어 에보나이트화된다.Vulcanization molding conditions of the secondary foaming process is preferably about 3600 seconds at 195 ℃ higher than the temperature of the foaming agent, filled in a mold set to the dimensions of the finished product, vulcanized and emulsified.

일례로 상기한 1차 발포공정과 2차 발포공정에서 사용되는 금형은 최종완성되는 발포플로트에 연료게이지의 아암과 결합되기 위한 아암홀이 형성되도록 아암홀형성을 위한 핀 등이 부착될 수 있고, 발포공정에서 발생되는 질소가스의 배출을 위한 가스배출홀을 다수개 가공하는 것도 바람직하다.For example, the mold used in the primary foaming process and the secondary foaming process may be attached with a pin for forming an arm hole such that an arm hole for joining with an arm of a fuel gauge is formed in a foam float to be finally completed. It is also preferable to process a plurality of gas discharge holes for the discharge of nitrogen gas generated in the foaming process.

한편, 1차, 2차 발포공정을 거쳐 형성된 발포성형물은 최종적으로 80℃~100℃를 유지하는 오븐 등에서 24~36시간 정도 열처리되어 내고압성 발포플로트로 완성된다.Meanwhile, the foamed molded product formed through the primary and secondary foaming processes is finally heat treated for about 24 to 36 hours in an oven maintaining 80 ° C. to 100 ° C., thereby completing a high pressure resistant foam float.

다음은 본 발명에 따라 제조된 내고압성 발포플로트와 종래제품을 45kg/cm2이상의 수압에서 3분간 침적유지 후 측정한 중량변화율을 표 2에서 정리하였다.Next is summarized in Table 2 the weight change rate measured after maintaining the high pressure-resistant foam float and the conventional product prepared in accordance with the present invention for 3 minutes immersion at a water pressure of 45kg / cm 2 or more.

Figure 112004044710341-pat00002
Figure 112004044710341-pat00002

통상 중량변화율은 3% 내에서 변동이 없어야 되나 상기 실험에서와 같이 종래 기술에 의한 발포플로트는 중량변화율이 3%를 훨씬 상회하는 수치를 나타내었고 본 발명에 의한 발포플로트는 극히 미미한 중량변화율이 나타났다.In general, the weight change rate should be unchanged within 3%, but as in the above experiment, the foam float according to the prior art showed a value of more than 3% in weight change rate, and the foam float according to the present invention showed a very small weight change rate. .

본 발명의 다른사상에 의한 내가소홀성을 향상시키기 위한 발포플로트는 상기한 내고압성 발포플로트에서의 각 제조공정을 거쳐 제조되나 혼합공정에서 보강제로서 Clay와 MT가 첨가되는 상기 실시예 3의 조성비에서 페놀수지와 유황의 함량을 높인다는 것과 2차 발포공정에서 가류시간이 증가된다는 것에서 차이점이 있다.The foaming float for improving the resistance to resistance due to the other idea of the present invention is manufactured through each manufacturing process in the above-mentioned high pressure resistant foaming float, but the composition ratio of Example 3 in which clay and MT are added as a reinforcing agent in the mixing process There is a difference between increasing the content of phenolic resin and sulfur at and the increase in vulcanization time in the secondary foaming process.

한편, 알콜계 연료에 사용되는 발포플로트는 내알콜성을 갖추어야 하며 이러한 내알콜성 갖추기 위하여는 내유성(耐油性)과 내수성(耐水性)이 우수하여야 한다.On the other hand, the foamed float used in the alcohol-based fuel must have alcohol resistance and in order to have such alcohol resistance must be excellent in oil resistance (water resistance) and water resistance (耐水 性).

이하 상기 혼합공정에 사용되는 각 성분들의 조성비를 조절하여 상기한 조건을 충족시키는 실시예를 기술한다.Hereinafter, an embodiment of satisfying the above conditions by adjusting the composition ratio of each component used in the mixing process will be described.

실시예 4Example 4

NBR 100중량부에, 그의 중량기준으로 페놀수지 50%, 가류제로서 유황 30∼40%, 가류조제로서 산화아연(ZnO) 5%와 스테아르산 1%, 발포제로서 DPT 5%, 발포조제로서 DPT조제 3.5%, 촉진제로서 CZ 2%, 보강제로서 Clay 2%, MT 43% 가 첨가되어 혼합되는 고무생지를 만든다.100 parts by weight of NBR, 50% phenolic resin, 30-40% sulfur as vulcanizing agent, 5% zinc oxide (ZnO) and 1% stearic acid as vulcanizing agent, 5% DPT as blowing agent, DPT as foaming aid 3.5% of the preparation, 2% of CZ as an accelerator, 2% of clay as a reinforcing agent, and 43% of MT are added to form a rubber dough to be mixed.

상기한 실시예 4에 의해 혼합생성된 고무생지는 상기한 내고압성 발포플로트와 같이 트랜스퍼 방식의 금형에 충진되어 1차 및 2차 발포공정과 열처리 공정을 거친다.The rubber dough mixed and produced by Example 4 is filled in a transfer mold such as the high pressure resistant foam float, and undergoes primary and secondary foaming and heat treatment.

한편 2차 발포공정에서는 상기한 내고압성 발포플로트의 2차 발포공정에서와 같이 가류온도는 195℃ 로 동일하나 가류시간이 약 3600초 정도에서 약 4000초 정도로 길어진다.On the other hand, in the secondary foaming process, as in the secondary foaming process of the above-mentioned high pressure resistant foam float, the vulcanization temperature is the same as 195 ° C., but the vulcanization time is increased from about 3600 seconds to about 4000 seconds.

이와같이 페놀수지와 유황의 함량이 높아지므로서 내가소홀성이 향상되는 원리에 대한 물리적 설명은 어려우나 본 출원인이 수 년간 각고의 실험에 의하여 카본블랙계 보강제인 MT와 규사가 함유되는 Clay가 첨가되고 페놀수지와 유황성분의 조성비를 높이므로서 2차 가류시간이 길어져 내가소홀성이 향상되는 것으로 파악된다.As described above, it is difficult to explain the physical principle of the principle of improving the resistance to the increase of the phenol resin and the sulfur. However, the inventors have been experimenting for several years with the addition of clay containing the carbon black reinforcing agent MT and silica. By increasing the composition ratio of the resin and the sulfur component, the secondary vulcanization time is prolonged and the resistance to neglect is improved.

다음은 본 발명에 따라 제조된 내가소홀성 발포플로트와 종래제품을 가소홀액(알코올혼합연료;가솔린,메탄올,에탄올의 혼합액)에 침전시키고 60℃에서 200시 간 유지시킨 후 측정한 중량변화율을 표 3에서 정리하였다.The following is the weight change rate measured after precipitating the non-porous foam float prepared in accordance with the present invention and the conventional product in a plastic hole solution (alcohol mixed fuel; gasoline, methanol, ethanol mixed solution) and maintained at 60 ℃ for 200 hours Summarized in 3.

Figure 112004044710341-pat00003
Figure 112004044710341-pat00003

이와같은 실험에서 중량변화율은 통상 10% 내에서 변동이 없어야 되나 상기 실험에서와 같이 종래 기술에 의한 발포플로트는 중량변화율이 10% 를 훨씬 상회하는 수치를 나타내었고 본 발명에 의한 발포플로트는 허용되는 범위내에서 중량변화율이 나타났다.In this experiment, the weight change rate should normally be unchanged within 10%. However, as in the above experiment, the foam float according to the prior art showed a value in which the weight change rate far exceeded 10%, and the foam float according to the present invention is acceptable. The rate of change of weight appeared within the range.

이상과 같이 본 발명에 따른 내고압성 발포플로트는 카본블랙계 보강제를 사용하여 종래의 발포플로트에 비해 단위면적당 셀수가 급격히 증가(도 1 및 도 2참조)한 것을 볼 수 있고, 이는 곧 발포플로트의 강도 및 경도를 높혀 종래 기술에 비해 훨씬 향상된 내고압성을 구비하게 되는 것이다.As described above, the high pressure resistant foam float according to the present invention can be seen that the number of cells per unit area is increased sharply (see FIGS. 1 and 2) compared to the conventional foam float using a carbon black reinforcement agent, which is a foam float. By increasing the strength and hardness of the will have a much improved high pressure resistance compared to the prior art.

한편, 본 발명의 다른사상에 따른 내가소홀성 발포플로트는 발포플로트 자체에 내가소홀성이 구비되는 것으로 상기 종래기술의 내가소홀성 발포플로트가 내가소홀성 혼합물을 코팅하던 것에 비하면 월등히 안정적이다.On the other hand, the non-resistant foam float according to another aspect of the present invention is to be resistant to the foam float itself is highly stable compared to the non-resistant foam float of the prior art coating the resistant mixture.

이처럼 본 발명에 따른 내고압성 발포플로트 및 내가소홀성 발포플로트는 완성품의 표면역시 종래 기술에 비해 크랙이 거의 없다시피 하고 매끈하여 미감이 우수(도 3a, 도 3b 및 도 4참조)하므로 더욱 경쟁력을 갖춘 상품으로 수출 등에도 훨 씬 유리하다 할 것이고, 그 형상은 상기한 도면에서 나타난 바와같이 원통형 또는 사각형 등으로 금형에 따라 다양한 형상으로 형성된다.As described above, the high pressure resistant foam float and the refractory foam float according to the present invention have almost no cracks compared to the prior art, and the smoothness is excellent and the aesthetics are excellent (see FIGS. 3a, 3b and 4). It will be much more advantageous to export goods, etc., the shape is formed in a variety of shapes depending on the mold, such as cylindrical or square, as shown in the above drawings.

상기한 바와같이 본 발명은 독립적인 셀(기포, 기공)이 형성된 경질발포체로서 45kg/cm2이상에서도 파손되지 않을 뿐만 아니라 내유성, 내수성, 내LPG성 및 내가소홀성 등이 탁월하여 LPG 연료탱크를 포함하여 알콜계 연료를 사용하는 거의 모든 액상연료의 연료탱크에 사용가능하다는 장점이 있다.As described above, the present invention is a rigid foam formed with an independent cell (bubble, pores), not only damaged at 45kg / cm 2 or more, but also excellent in oil resistance, water resistance, LPG resistance, and neglect resistance, and thus, LPG fuel tank. The advantage is that it can be used in fuel tanks of almost all liquid fuels using alcoholic fuels.

Claims (5)

합성고무인 아크릴로 니트릴 부타디엔 라바(NBR)를 주성분으로 하여 페놀수지와 가류제와 발포제와 보강제 및 촉진제 등이 혼합되는 혼합공정, 상기 혼합공정에서 생성된 고무생지를 발포제의 분해온도보다 낮은 온도에서 완제품의 크기보다 작게 1차 가류성형하여 생성된 발포성형물을 발포제의 분해온도 보다 높은 온도에서 완제품의 크기로 2차 가류성형 후 열처리하여 제조되는 발포플로트에 있어서,Synthetic rubber based on acrylonitrile butadiene lava (NBR), a phenol resin, a vulcanizing agent, a blowing agent, a reinforcing agent, and an accelerator. In the foamed float produced by primary vulcanization molding to be smaller than the size of the foamed product produced by heat treatment after secondary vulcanization to the size of the finished product at a temperature higher than the decomposition temperature of the blowing agent, 상기 혼합공정은 NBR 100중량부에, 그의 중량기준으로 페놀수지 35∼55%, 가류제로서 유황 30∼40%, 가류조제로서 산화아연(ZnO) 5%~5.5% 및 스테아르산 1∼1.5%, 발포제로서 DPT 5∼7%, 발포조제로서 DPT조제 3∼4.5%, 촉진제로서 CZ 1.8∼2.1%, 보강제로서 SRF 5~15% 및 MT 20~30%가 첨가되어 혼합되므로서 내고압성이 향상되는 것을 특징으로 하는 발포플로트.The mixing step is based on the weight of NBR 100 parts by weight, 35 to 55% phenol resin, 30 to 40% sulfur as vulcanizing agent, 5% to 5.5% zinc oxide (ZnO) as vulcanizing aid and 1 to 1.5% stearic acid DPT 5-7% as foaming agent, DPT 3 ~ 4.5% as foaming aid, CZ 1.8-2.1% as promoter, SRF 5-15% and MT 20-30% as reinforcing agent are added and mixed Foam float, characterized in that improved. 합성고무인 아크릴로 니트릴 부타디엔 라바(NBR)를 주성분으로 하여 페놀수지와 가류제와 발포제와 보강제 및 촉진제 등이 혼합되는 혼합공정, 상기 혼합공정에서 생성된 고무생지를 발포제의 분해온도보다 낮은 온도에서 완제품의 크기보다 작게 1차 가류성형하여 생성된 발포성형물을 발포제의 분해온도 보다 높은 온도에서 완제품의 크기로 2차 가류성형 후 열처리하여 제조되는 발포플로트에 있어서,Synthetic rubber based on acrylonitrile butadiene lava (NBR), a phenol resin, a vulcanizing agent, a blowing agent, a reinforcing agent, and an accelerator, and the rubber dough produced in the mixing process at a lower temperature than the decomposition temperature of the blowing agent. In the foamed float produced by primary vulcanization molding to be smaller than the size of the foamed product produced by heat treatment after secondary vulcanization to the size of the finished product at a temperature higher than the decomposition temperature of the blowing agent, 상기 혼합공정은 NBR 100중량부에, 그의 중량기준으로 페놀수지 35∼55%, 가류제로서 유황 30∼40%, 가류조제로서 산화아연(ZnO) 5%~5.5% 및 스테아르산 1∼1.5%, 발포제로서 DPT 5∼7%, 발포조제로서 DPT조제 3∼4.5%, 촉진제로서 CZ 1.8∼2.1%, 보강제로서 HAF 10~20% 및 MT 20~30%가 첨가되어 혼합되므로서 내고압성이 향상되는 것을 특징으로 하는 발포플로트.The mixing step is based on the weight of NBR 100 parts by weight, 35 to 55% phenol resin, 30 to 40% sulfur as vulcanizing agent, 5% to 5.5% zinc oxide (ZnO) as vulcanizing aid and 1 to 1.5% stearic acid DPT 5-7% as foaming agent, DPT 3 ~ 4.5% as foaming aid, CZ 1.8-2.1% as promoter, HAF 10-20% and MT 20-30% as mixing agent are added and mixed Foam float, characterized in that improved. 합성고무인 아크릴로 니트릴 부타디엔 라바(NBR)를 주성분으로 하여 페놀수지와 가류제와 발포제와 보강제 및 촉진제 등이 혼합되는 혼합공정, 상기 혼합공정에서 생성된 고무생지를 발포제의 분해온도보다 낮은 온도에서 완제품의 크기보다 작게 1차 가류성형하여 생성된 발포성형물을 발포제의 분해온도 보다 높은 온도에서 완제품의 크기로 2차 가류성형 후 열처리하여 제조되는 발포플로트에 있어서,Synthetic rubber based on acrylonitrile butadiene lava (NBR), a phenol resin, a vulcanizing agent, a blowing agent, a reinforcing agent, and an accelerator, and the rubber dough produced in the mixing process at a lower temperature than the decomposition temperature of the blowing agent. In the foamed float produced by primary vulcanization molding to be smaller than the size of the foamed product produced by heat treatment after secondary vulcanization to the size of the finished product at a temperature higher than the decomposition temperature of the blowing agent, 상기 혼합공정은 NBR 100중량부에, 그의 중량기준으로 페놀수지 35∼55%, 가류제로서 유황 30∼40%, 가류조제로서 산화아연(ZnO) 5%~5.5% 및 스테아르산 1∼1.5%, 발포제로서 DPT 5∼7%, 발포조제로서 DPT조제 3∼4.5%, 촉진제로서 CZ 1.8∼2.1%, 보강제로서 Clay 3~5% 및 MT 30~45%가 첨가되어 혼합되므로서 내고압성이 향상되는 것을 특징으로 하는 발포플로트.The mixing step is based on the weight of NBR 100 parts by weight, 35 to 55% phenol resin, 30 to 40% sulfur as vulcanizing agent, 5% to 5.5% zinc oxide (ZnO) as vulcanizing aid and 1 to 1.5% stearic acid DPT 5-7% as foaming agent, DPT 3 ~ 4.5% as foaming aid, CZ 1.8-2.1% as accelerator, 3-5% Clay as reinforcing agent and 30-45% MT as mixing agent are added and mixed. Foam float, characterized in that improved. 합성고무인 아크릴로 니트릴 부타디엔 라바(NBR)를 주성분으로 하여 페놀수지와 가류제와 발포제와 보강제 및 촉진제 등이 혼합되는 혼합공정, 상기 혼합공정에서 생성된 고무생지를 발포제의 분해온도보다 낮은 온도에서 완제품의 크기보다 작게 1차 가류성형하여 생성된 발포성형물을 발포제의 분해온도 보다 높은 온도에서 완제품의 크기로 2차 가류성형 후 열처리하여 제조되는 발포플로트에 있어서,Synthetic rubber based on acrylonitrile butadiene lava (NBR), a phenol resin, a vulcanizing agent, a blowing agent, a reinforcing agent, and an accelerator, and the rubber dough produced in the mixing process at a lower temperature than the decomposition temperature of the blowing agent. In the foamed float produced by primary vulcanization molding to be smaller than the size of the foamed product produced by heat treatment after secondary vulcanization to the size of the finished product at a temperature higher than the decomposition temperature of the blowing agent, 상기 혼합공정은 NBR 100중량부에, 그의 중량기준으로 페놀수지 50∼60%, 가류제로서 유황 45∼55%, 가류조제로서 산화아연(ZnO) 5%~5.5% 및 스테아르산 1∼1.5%, 발포제로서 DPT 6∼7.5%, 발포조제로서 DPT조제 3∼4.5%, 촉진제로서 CZ 1.8∼2.1%, 보강제로서 MT 40~50% 및 Clay 3~5% 가 첨가되어 혼합되므로서 내가소홀성이 향상되는 것을 특징으로 하는 발포플로트.The mixing step is based on the weight of NBR 100 parts by weight, 50 to 60% phenol resin, 45 to 55% sulfur as vulcanizing agent, 5% to 5.5% zinc oxide (ZnO) as vulcanizing aid and 1 to 1.5% stearic acid. , DPT 6-7.5% as foaming agent, DPT 3 ~ 4.5% as foaming aid, CZ 1.8-2.1% as accelerator, MT 40-50% and Clay 3-5% as reinforcing agent are added and mixed Foam float, characterized in that improved. 삭제delete
KR1020040078308A 2004-07-21 2004-10-01 Hard foam rubber closed cellular ebonite KR100555962B1 (en)

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