KR102467058B1 - Fluoro rubber composition for o-ring with excellent low compression set at high temperature - Google Patents
Fluoro rubber composition for o-ring with excellent low compression set at high temperature Download PDFInfo
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Abstract
본 발명은 고온 영구압축줄음율 특성이 우수한 오링용 불소고무 조성물에 관한 것으로, 보다 구체적으로는 3원계 불소고무에 보강성이 우수한 입자크기 100nm 이하의 카본블랙을 적용하여 고온에서의 영구압축줄음율 및 인장강도를 확보하되, 입자크기가 상대적으로 큰 무수 실리카를 혼용하여 적용함으로써 카본블랙의 분산성 및 불소고무의 가공성을 향상시킬 뿐만 아니라 이로 인해 고온에서의 영구압축줄음율 및 인장강도를 더욱 효율적으로 개선시킬 수 있도록 하는, 고온 영구압축줄음율 특성이 우수한 오링용 불소고무 조성물에 관한 것이다.The present invention relates to a fluororubber composition for O-rings having excellent high-temperature compression set characteristics, and more specifically, to a ternary fluororubber by applying carbon black having a particle size of 100 nm or less with excellent reinforcing properties at high temperature compression set. and tensile strength, but by applying a mixture of anhydrous silica having a relatively large particle size, the dispersibility of carbon black and the workability of fluoroelastomer are improved, as well as the compression set and tensile strength at high temperatures are more efficiently It relates to a fluororubber composition for an O-ring having excellent high-temperature compression set characteristics that can be improved.
Description
본 발명은 고온에서의 영구압축줄음율 및 인장강도 등을 향상시킬 수 있도록 하는 오링용 불소고무 조성물에 관한 것이다.The present invention relates to a fluororubber composition for an O-ring capable of improving compression set and tensile strength at high temperatures.
일반적으로 불소고무는 현존하는 고무 중 내열성과 내유성이 가장 우수한 소재중 하나로써, 자동차, 선박 및 항공 엔진계통에 주로 이용되고 있으며, 이런 엔진들이 에너지 효율을 높이기 위해 점차 고출력화 되어감으로 인해, 엔진의 내부 환경이 가혹해지면서 여기에 적용되는 오링, 가소켓 소재 등은 좀 더 높은 내열성이 요구되고 있다.In general, fluororubber is one of the most excellent materials in heat resistance and oil resistance among existing rubbers, and is mainly used in automobile, ship, and aircraft engine systems. As the internal environment of the device becomes harsh, higher heat resistance is required for O-rings and gas-socket materials that are applied here.
이를 위해 종래 오링의 경우 내열성 등을 향상시키기 위해 이원계(VDF(vinylidenefluoride)/HFP(hexafluoropropylene)) 불소고무 또는 삼원계(VDF/HFP/TFE(tetrafluoroethylene))를 적용한 배합고무에 카본블랙과 같은 충진재를 적용하고 있다.To this end, in the case of conventional O-rings, fillers such as carbon black are applied to compound rubber to which binary (VDF (vinylidenefluoride)/HFP (hexafluoropropylene)) fluororubber or ternary (VDF/HFP/TFE (tetrafluoroethylene)) is applied to improve heat resistance. are applying
관련 선행기술로써 특허문헌 1에서는 불소고무중합체에 보강성이 우수한 입자크기 25 ~ 80nm의 카본블랙을 적용한 기술을 제안하였다. 하지만 불소고무의 특성상 가공성이 좋지않아 카본블랙의 입자크기가 작을수록 분산이 어려우며, 이로 인해 특허문헌 1의 경우 오히려 내열성의 향상효율이 미비해지는 문제점이 있었다.As a related prior art, Patent Document 1 proposed a technique in which carbon black having a particle size of 25 to 80 nm with excellent reinforcing property was applied to a fluoroelastomer polymer. However, due to the nature of fluoroelastomer, processability is not good, and the smaller the particle size of carbon black, the more difficult it is to disperse. As a result, in the case of Patent Document 1, there is a problem that the heat resistance improvement efficiency is rather insufficient.
이를 해결하기 위해 일반적으로 카본블랙 중 입자사이즈가 상대적으로 큰(250 ~ 350nm) 카본블랙이 많이 적용되고 있으나, 이는 입자크기가 작은(100nm 이하) 카본블랙을 적용하는 경우보다 보강성이 미비하여 영구압축줄음율 및 인장강도 등의 개선 효율이 미비한 문제점이 있었다.In order to solve this problem, carbon black with a relatively large particle size (250 ~ 350 nm) is generally applied, but it is less reinforcing than carbon black with a small particle size (less than 100 nm), so it is permanent. There was a problem that the improvement efficiency such as compression set and tensile strength was insufficient.
본 발명은 상기와 같은 문제점을 해결하기 위한 것으로, 3원계 불소고무에 보강성이 우수한 입자크기 100nm 이하의 카본블랙을 적용하여 고온에서의 영구압축줄음율 및 인장강도를 확보하되, 입자크기가 상대적으로 큰 무수 실리카를 혼용하여 적용함으로써 카본블랙의 분산성 및 불소고무의 가공성을 향상시킬 뿐만 아니라 이로 인해 고온에서의 영구압축줄음율 및 인장강도를 더욱 효율적으로 개선시킬 수 있도록 함을 과제로 한다.The present invention is to solve the above problems, and secures permanent compression set and tensile strength at high temperatures by applying carbon black having a particle size of 100 nm or less, which has excellent reinforcing properties, to ternary fluoroelastomer, but the particle size is relatively small. It is a task to improve the dispersibility of carbon black and processability of fluoroelastomer by applying a mixture of large anhydrous silica, as well as to improve the permanent compression set and tensile strength at high temperatures more efficiently.
본 발명은 오링용 고무 조성물에 있어서, 불소고무에, 입자크기 28 ~ 36nm의 카본블랙과 입자크기 6,000 ~ 12,000nm의 무수 실리카를 혼합하여 이루어지는 것을 특징으로 하는, 고온 영구압축줄음율 특성이 우수한 오링용 불소고무 조성물을 과제의 해결 수단으로 한다.The present invention is an O-ring rubber composition for an O-ring, which is characterized in that it is formed by mixing carbon black with a particle size of 28 to 36 nm and anhydrous silica with a particle size of 6,000 to 12,000 nm in fluororubber, and has excellent high-temperature compression set characteristics. A fluororubber composition for use as a solution to the problem.
보다 구체적으로 상기 오링용 불소고무 조성물은, 3원계 불소고무 100 중량부에 대하여, 입자크기 28 ~ 36nm의 카본블랙 20 ~ 30 중량부, 입자크기 6,000 ~ 12,000nm의 무수 실리카 10 ~ 20 중량부 및 오링용 첨가제를 혼합하여 이루어지는 것이 바람직하다.More specifically, the fluororubber composition for an O-ring includes 20 to 30 parts by weight of carbon black having a particle size of 28 to 36 nm, 10 to 20 parts by weight of anhydrous silica having a particle size of 6,000 to 12,000 nm, and It is preferably formed by mixing additives for O-rings.
한편, 상기 오링용 첨가제는 상기 3원계 불소고무 100 중량부에 대하여, 카르나우바 왁스 1 ~ 2 중량부, 가공조제 2 ~ 3 중량부, 가교제 4 ~ 5 중량부 및 공가교제 5 ~ 6 중량부로 이루어지는 것이 바람직하다.On the other hand, the O-ring additive is 1 to 2 parts by weight of carnauba wax, 2 to 3 parts by weight of a processing aid, 4 to 5 parts by weight of a crosslinking agent and 5 to 6 parts by weight of a co-crosslinking agent, based on 100 parts by weight of the ternary fluoroelastomer. It is desirable that
본 발명은 3원계 불소고무에 보강성이 우수한 입자크기 100nm 이하의 카본블랙을 적용하여 고온에서의 영구압축줄음율 및 인장강도를 확보하되, 입자크기가 상대적으로 큰 무수 실리카를 혼용하여 적용함으로써 카본블랙의 분산성 및 불소고무의 가공성을 향상시킬 뿐만 아니라 이로 인해 고온에서의 영구압축줄음율 및 인장강도를 더욱 효율적으로 개선시킬 수 있는 효과가 있다.The present invention secures permanent compression set and tensile strength at high temperatures by applying carbon black with a particle size of 100 nm or less, which is excellent in reinforcing property, to ternary fluoroelastomer, but by mixing and applying anhydrous silica having a relatively large particle size, carbon black It not only improves the dispersibility of black and the workability of fluoroelastomer, but also has the effect of improving the compression set and tensile strength at high temperatures more efficiently.
본 발명은 고온 영구압축줄음율 특성이 우수한 오링용 불소고무 조성물에 관한 것으로써, 본 발명의 기술적 구성을 이해하는데 필요한 부분만이 설명되며 그 이외 부분의 설명은 본 발명의 요지를 흩트리지 않도록 생략될 것이라는 것을 유의하여야 한다.The present invention relates to a fluororubber composition for O-rings having excellent high-temperature compression set characteristics, and only parts necessary for understanding the technical configuration of the present invention are described, and descriptions of other parts are omitted so as not to distract from the gist of the present invention. It should be noted that there will be
본 발명에 따른 고온 영구압축줄음율 특성이 우수한 오링용 불소고무 조성물을 설명하면 다음과 같다.A fluororubber composition for an O-ring having excellent high-temperature compression set characteristics according to the present invention will be described as follows.
본 발명에 따른 고온 영구압축줄음율 특성이 우수한 오링용 불소고무 조성물은 불소고무에, 입자크기 28 ~ 36nm의 카본블랙과 입자크기 6,000 ~ 12,000nm의 무수 실리카를 혼합하여 이루어지는 것을 특징으로 하며, 보다 구체적으로는 3원계 불소고무 100 중량부에 대하여, 입자크기 28 ~ 36nm의 카본블랙 20 ~ 30 중량부, 입자크기 6,000 ~ 12,000nm의 무수 실리카 10 ~ 20 중량부 및 오링용 첨가제를 혼합하여 이루어진다.The fluororubber composition for O-rings having excellent high-temperature compression set characteristics according to the present invention is characterized in that it is formed by mixing fluororubber with carbon black having a particle size of 28 to 36 nm and anhydrous silica having a particle size of 6,000 to 12,000 nm. Specifically, it is made by mixing 20 to 30 parts by weight of carbon black with a particle size of 28 to 36 nm, 10 to 20 parts by weight of anhydrous silica with a particle size of 6,000 to 12,000 nm, and an additive for an O-ring with respect to 100 parts by weight of ternary fluoroelastomer.
상기 불소고무는 오링용 고무 조성물에 널리 사용되는 공지된 기재로써 내열성과 내유성이 가장 우수한 소재중 하나이며 자동차, 선박 및 항공 엔진계통에 주로 사용되고 있다. 한편 본 발명에서는 특정 불소고무에 한정하지 않고, 이미 공지된 다양한 종류의 불소고무를 적용할 수 있다.The fluororubber is a known substrate widely used in rubber compositions for O-rings, and is one of the materials having the best heat resistance and oil resistance, and is mainly used in automobile, ship, and aircraft engine systems. Meanwhile, in the present invention, it is not limited to a specific fluororubber, and various types of fluororubber that are already known can be applied.
한편, 본 발명에서는 일 예로 3원계 불소고무를 적용하며 3원계 불소고무는 VDF(vinylidenefluoride), HFP(hexafluoropropylene) 및 TFE(tetrafluoroethylene)의 공중합으로 이루어지는 불소고무로써 이미 공지된 물질이다.On the other hand, in the present invention, for example, ternary fluoroelastomer is applied, and the tertiary fluoroelastomer is a fluoroelastomer formed by copolymerization of vinylidenefluoride (VDF), hexafluoropropylene (HFP), and tetrafluoroethylene (TFE), and is a known material.
상기 카본블랙(carbon black)은 오링의 영구압축줄음율 및 인장강도 등을 보강하기 위해 첨가되는 것으로, 입자크기 28 ~ 36nm의 카본블랙을 사용한다.The carbon black is added to reinforce the permanent compression set and tensile strength of the O-ring, and carbon black having a particle size of 28 to 36 nm is used.
여기서, 카본블랙의 입자크기가 상기 범위를 벗어날 경우 분산성 향상 효율이 미비해질 우려가 있다. 아울러 상기 카본블랙의 함량이 20 중량부 미만일 경우 보강효과가 미비해질 우려가 있으며, 30 중량부를 초과할 경우 분산성 향상 효율이 미비해질 우려가 있다.Here, when the particle size of the carbon black is out of the above range, there is a concern that the dispersibility improving efficiency may be insufficient. In addition, if the content of the carbon black is less than 20 parts by weight, there is a concern that the reinforcing effect may be insufficient, and if it exceeds 30 parts by weight, there is a concern that the dispersibility improvement efficiency may be insufficient.
상기 무수 실리카(anhydrous silica)는 상기 카본블랙의 분산성을 향상시키기 위해 첨가되는 것으로, 상기 카본블랙 보다 입자크기가 상대적으로 큰 무수 실리카를 혼용하여 적용함으로써 카본블랙의 분산성 및 불소고무의 가공성을 향상시킬 뿐만 아니라 이로 인해 영구압축줄음율 및 인장강도를 더욱 효율적으로 개선시킨다.The anhydrous silica is added to improve the dispersibility of the carbon black, and the dispersibility of the carbon black and the processability of the fluoroelastomer are improved by mixing and applying anhydrous silica having a relatively larger particle size than the carbon black. As a result, the compression set and tensile strength are improved more efficiently.
이를 위해 상기 무수 실리카는 입자크기가 6,000 ~ 12,000nm인 것을 사용하며, 입자크기가 상기 범위를 벗어날 경우 분산성 향상 효율이 미비해질 우려가 있다. 아울러 상기 무수 실리카의 함량이 10 중량부 미만일 경우 분산성 향상 효율이 미비해질 우려가 있으며, 20 중량부를 초과할 경우 오히려 가공성이 저하될 우려가 있다.To this end, the anhydrous silica is used having a particle size of 6,000 to 12,000 nm, and when the particle size is out of the above range, there is a concern that the efficiency of improving dispersibility may be insufficient. In addition, when the content of the anhydrous silica is less than 10 parts by weight, there is a concern that the dispersibility improvement efficiency may be insufficient, and when it exceeds 20 parts by weight, there is a concern that processability may rather deteriorate.
상기 오링용 첨가제는 오링의 제조시 일반적으로 사용되는 공지된 첨가제로써 후술되어질 첨가제의 종류 및 함량에 한정되지 않고 이미 공지된 다양한 첨가제 및 함량의 적용이 가능하다.The additive for the O-ring is a known additive generally used in the manufacture of an O-ring, and is not limited to the type and content of additives to be described later, and various additives and contents known in the art can be applied.
상기 오링용 첨가제의 일 예로, 카르나우바 왁스(carnauba wax) 1 ~ 2 중량부, 가공조제 2 ~ 3 중량부, 가교제 4 ~ 5 중량부 및 공가교제 5 ~ 6 중량부를 적용할 수 있으며, 보다 구체적으로는 가공조제는 올가노실리콘(organosilicone) 등을 적용할 수 있고, 가교제는 DHBP(2,5-dimethyl-2,5-di(tert-butylperoxy)hexyne) 등을 적용할 수 있으며, 공가교제는 TAIC(trially isocyanurate) 등을 적용할 수 있으나, 이미 상술한 바와 같이 여기에 한정되는 것은 아니고 이미 공지된 다양한 오링용 첨가제의 사용이 가능하다.As an example of the O-ring additive, 1 to 2 parts by weight of carnauba wax, 2 to 3 parts by weight of a processing aid, 4 to 5 parts by weight of a crosslinking agent, and 5 to 6 parts by weight of a co-crosslinking agent may be applied. Specifically, organosilicone and the like can be applied as the processing aid, and DHBP (2,5-dimethyl-2,5-di (tert-butylperoxy) hexyne) and the like can be applied as the crosslinking agent, and the co-crosslinking agent TAIC (trially isocyanurate) or the like can be applied, but as described above, it is not limited thereto, and various additives for O-rings already known can be used.
이하, 본 발명을 실시예에 의거하여 더욱 구체적으로 설명하겠는 바, 본 발명이 다음 실시예에 의해 한정되는 것은 아니다.Hereinafter, the present invention will be described in more detail based on examples, but the present invention is not limited by the following examples.
1. 오링의 제조1. Manufacture of O-rings
(실시예 1)(Example 1)
3원계 불소고무(FKM, Viton GF600S) 100 중량부에 대하여, 입자크기 28nm의 카본블랙(carbon black, 코리아카본블랙 N330) 20 중량부, 입자크기 6,000nm의 무수 실리카(anhydrous silica, Celite N219) 10 중량부, 카르나우바 왁스(carnauba wax) 1 중량부, 가공조제(organosilicone, STRUKTOL WS280) 2 중량부, 가교제(DHBP) 4 중량부 및 공가교제(TAIC) 5 중량부를 컴파운드 혼련기인 니이더에서 110℃, 약 10분동안 혼련하여 컴파운드를 제조하였다. 니이더 작업을 끝난 컴파운드는 오픈 롤밀에서 균일하게 혼합시킨 후 2mm 쉬트상의 컴파운드를 제조한다. 이렇게 제조된 시트상의 컴파운드를 시험규격에 따라 제작된 금형에 투입한 후 180℃, 150kg/cm2의 프레스 조건에서 약 10분간 프레스 성형한 후, 220℃에서 12시간 열처리하여 오링을 제조하였다.Based on 100 parts by weight of ternary fluoroelastomer (FKM, Viton GF600S), 20 parts by weight of carbon black (Korea Carbon Black N330) with a particle size of 28 nm, anhydrous silica (Celite N219) with a particle size of 6,000 nm 10 Parts by weight, carnauba wax 1 part by weight, processing aid (organosilicone, STRUKTOL WS280) 2 parts by weight, crosslinking agent (DHBP) 4 parts by weight and co-crosslinking agent (TAIC) 5 parts by weight 110 in a kneader, a compound kneader ℃, and kneaded for about 10 minutes to prepare a compound. The kneaded compound is uniformly mixed in an open roll mill, and then a 2mm sheet compound is manufactured. After putting the prepared sheet compound into a mold manufactured according to the test standard, press molding at 180 ° C and 150 kg / cm 2 for about 10 minutes, and then heat treatment at 220 ° C for 12 hours to prepare an O-ring.
(실시예 2)(Example 2)
3원계 불소고무(FKM, Viton GF600S) 100 중량부에 대하여, 입자크기 36nm의 카본블랙(carbon black, 코리아카본블랙 N330) 30 중량부, 입자크기 12,000nm의 무수 실리카(anhydrous silica, Celite N219) 20 중량부, 카르나우바 왁스(carnauba wax) 2 중량부, 가공조제(organosilicone, STRUKTOL WS280) 3 중량부, 가교제(DHBP) 5 중량부 및 공가교제(TAIC) 6 중량부를 컴파운드 혼련기인 니이더에서 110℃, 약 10분동안 혼련하여 컴파운드를 제조하였다. 니이더 작업을 끝난 컴파운드는 오픈 롤밀에서 균일하게 혼합시킨 후 2mm 쉬트상의 컴파운드를 제조한다. 이렇게 제조된 시트상의 컴파운드를 시험규격에 따라 제작된 금형에 투입한 후 180℃, 150kg/cm2의 프레스 조건에서 약 10분간 프레스 성형한 후, 220℃에서 12시간 열처리하여 오링을 제조하였다.Based on 100 parts by weight of ternary fluoroelastomer (FKM, Viton GF600S), 30 parts by weight of carbon black (Korea Carbon Black N330) with a particle size of 36 nm, anhydrous silica (Celite N219) with a particle size of 12,000 nm 20 Parts by weight, carnauba wax 2 parts by weight, processing aid (organosilicone, STRUKTOL WS280) 3 parts by weight, crosslinking agent (DHBP) 5 parts by weight and co-crosslinking agent (TAIC) 6 parts by weight 110 in a kneader, a compound kneader ℃, and kneaded for about 10 minutes to prepare a compound. The kneaded compound is uniformly mixed in an open roll mill, and then a 2mm sheet compound is manufactured. After putting the prepared sheet compound into a mold manufactured according to the test standard, press molding at 180 ° C and 150 kg / cm 2 for about 10 minutes, and then heat treatment at 220 ° C for 12 hours to prepare an O-ring.
(비교예 1)(Comparative Example 1)
실시예 1과 동일하게 제조하되, 무수 실리카를 사용하지 않았다.It was prepared in the same manner as in Example 1, but anhydrous silica was not used.
(비교예 2)(Comparative Example 2)
실시예 2와 동일하게 제조하되, 무수 실리카를 사용하지 않았고, 입자크기 250nm의 카본블랙(carbon black, 코리아카본블랙 N990)을 사용하였다.It was prepared in the same manner as in Example 2, but anhydrous silica was not used, and carbon black (Korea Carbon Black N990) having a particle size of 250 nm was used.
2. 오링의 평가2. O-ring evaluation
상기 실시예 및 비교예에 따른 오링에 대한 영구압축줄음율 및 인장강도를 평가하였고 그 결과는 아래 [표 1]에 나타내었다.The permanent compression set and tensile strength of the O-rings according to the above Examples and Comparative Examples were evaluated, and the results are shown in [Table 1] below.
(200℃, 24시간)Permanent compression set (%)
(200℃, 24 hours)
(200℃, 72시간)Permanent compression set (%)
(200℃, 72 hours)
(kgf/cm2)The tensile strength
(kgf/cm 2 )
상기 [표 1]에서와 같이, 본 발명의 실시예에 따른 오링은 3원계 불소고무에 입자크기 100nm 이하의 카본블랙과 함께 입자크기가 상대적으로 큰 무수 실리카를 혼용하여 적용함으로써 카본블랙의 분산성을 향상시키고 이로 인해 영구압축줄음율 및 인장강도를 더욱 효율적으로 개선하였음을 알 수 있다.As shown in [Table 1], the O-ring according to the embodiment of the present invention is applied in combination with carbon black having a particle size of 100 nm or less and anhydrous silica having a relatively large particle size to the ternary fluoroelastomer, thereby improving the dispersibility of carbon black. It can be seen that the compression set and tensile strength were improved more efficiently.
상술한 바와 같이, 본 발명에 따른 고온 영구압축줄음율 특성이 우수한 오링용 불소고무 조성물을 상기의 바람직한 실시 예를 통해 설명하고, 그 우수성을 확인하였지만 해당 기술 분야의 당업자라면 하기의 특허청구범위에 기재된 본 발명의 사상 및 영역으로부터 벗어나지 않는 범위 내에서 본 발명을 다양하게 수정 및 변경시킬 수 있음을 이해할 수 있을 것이다.As described above, the fluororubber composition for O-rings having excellent high-temperature compression set characteristics according to the present invention has been described through the above preferred examples and its excellence has been confirmed, but those skilled in the art It will be understood that various modifications and changes may be made to the present invention without departing from the spirit and scope of the described invention.
Claims (3)
3원계 불소고무 100 중량부에 대하여, 입자크기 28 ~ 36nm의 카본블랙 20 ~ 30 중량부, 입자크기 6,000 ~ 12,000nm의 무수 실리카 10 ~ 20 중량부 및 오링용 첨가제를 혼합하여 이루어지되,
상기 오링용 첨가제는 카르나우바 왁스 1 ~ 2 중량부, 가공조제 2 ~ 3 중량부, 가교제 4 ~ 5 중량부 및 공가교제 5 ~ 6 중량부로 이루어지는 것을 특징으로 하는, 고온 영구압축줄음율 특성이 우수한 오링용 불소고무 조성물.In the rubber composition for O-rings,
Based on 100 parts by weight of ternary fluoroelastomer, 20 to 30 parts by weight of carbon black having a particle size of 28 to 36 nm, 10 to 20 parts by weight of anhydrous silica having a particle size of 6,000 to 12,000 nm, and an additive for an O-ring are mixed.
The additive for the O-ring is composed of 1 to 2 parts by weight of carnauba wax, 2 to 3 parts by weight of a processing aid, 4 to 5 parts by weight of a crosslinking agent and 5 to 6 parts by weight of a co-crosslinking agent. Excellent fluoroelastomer composition for O-rings.
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