KR20240053415A - Fluoro rubber composition for eco-friendly o-ring with excellent low compression set at high temperature - Google Patents
Fluoro rubber composition for eco-friendly o-ring with excellent low compression set at high temperature Download PDFInfo
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- 229920001973 fluoroelastomer Polymers 0.000 title claims abstract description 37
- 230000006835 compression Effects 0.000 title claims abstract description 26
- 238000007906 compression Methods 0.000 title claims abstract description 26
- 239000000203 mixture Substances 0.000 title claims abstract description 21
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 40
- 239000002245 particle Substances 0.000 claims abstract description 40
- 239000006229 carbon black Substances 0.000 claims abstract description 31
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 19
- 241000872198 Serjania polyphylla Species 0.000 claims abstract description 14
- 239000000843 powder Substances 0.000 claims description 20
- 239000000654 additive Substances 0.000 claims description 11
- 239000003431 cross linking reagent Substances 0.000 claims description 11
- 229920001971 elastomer Polymers 0.000 claims description 11
- 238000002156 mixing Methods 0.000 claims description 11
- 239000005060 rubber Substances 0.000 claims description 11
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 10
- 230000000996 additive effect Effects 0.000 claims description 7
- 239000006057 Non-nutritive feed additive Substances 0.000 claims description 6
- 235000013869 carnauba wax Nutrition 0.000 claims description 5
- 239000004203 carnauba wax Substances 0.000 claims description 5
- FBBATURSCRIBHN-UHFFFAOYSA-N triethoxy-[3-(3-triethoxysilylpropyldisulfanyl)propyl]silane Chemical compound CCO[Si](OCC)(OCC)CCCSSCCC[Si](OCC)(OCC)OCC FBBATURSCRIBHN-UHFFFAOYSA-N 0.000 claims description 4
- VTHOKNTVYKTUPI-UHFFFAOYSA-N triethoxy-[3-(3-triethoxysilylpropyltetrasulfanyl)propyl]silane Chemical compound CCO[Si](OCC)(OCC)CCCSSSSCCC[Si](OCC)(OCC)OCC VTHOKNTVYKTUPI-UHFFFAOYSA-N 0.000 claims description 4
- 230000000704 physical effect Effects 0.000 abstract description 8
- 238000004064 recycling Methods 0.000 abstract description 8
- 238000003912 environmental pollution Methods 0.000 abstract description 6
- 230000003014 reinforcing effect Effects 0.000 abstract description 6
- 150000001875 compounds Chemical class 0.000 description 11
- 239000000463 material Substances 0.000 description 7
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 6
- 229910052731 fluorine Inorganic materials 0.000 description 6
- 239000011737 fluorine Substances 0.000 description 6
- BQCIDUSAKPWEOX-UHFFFAOYSA-N 1,1-Difluoroethene Chemical compound FC(F)=C BQCIDUSAKPWEOX-UHFFFAOYSA-N 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- HCDGVLDPFQMKDK-UHFFFAOYSA-N hexafluoropropylene Chemical compound FC(F)=C(F)C(F)(F)F HCDGVLDPFQMKDK-UHFFFAOYSA-N 0.000 description 5
- 230000006872 improvement Effects 0.000 description 5
- 241000237519 Bivalvia Species 0.000 description 4
- 229920002449 FKM Polymers 0.000 description 4
- 235000020639 clam Nutrition 0.000 description 4
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical compound FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 4
- KOMNUTZXSVSERR-UHFFFAOYSA-N 1,3,5-tris(prop-2-enyl)-1,3,5-triazinane-2,4,6-trione Chemical compound C=CCN1C(=O)N(CC=C)C(=O)N(CC=C)C1=O KOMNUTZXSVSERR-UHFFFAOYSA-N 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- 240000000254 Agrostemma githago Species 0.000 description 2
- 235000009899 Agrostemma githago Nutrition 0.000 description 2
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- 241000237536 Mytilus edulis Species 0.000 description 2
- 241000237502 Ostreidae Species 0.000 description 2
- 241000237503 Pectinidae Species 0.000 description 2
- 241001339782 Scapharca broughtonii Species 0.000 description 2
- 238000010304 firing Methods 0.000 description 2
- 238000004898 kneading Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 235000020638 mussel Nutrition 0.000 description 2
- 235000020636 oyster Nutrition 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 235000020637 scallop Nutrition 0.000 description 2
- 239000002689 soil Substances 0.000 description 2
- ODBCKCWTWALFKM-UHFFFAOYSA-N 2,5-bis(tert-butylperoxy)-2,5-dimethylhex-3-yne Chemical compound CC(C)(C)OOC(C)(C)C#CC(C)(C)OOC(C)(C)C ODBCKCWTWALFKM-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000007334 copolymerization reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- ZFSLODLOARCGLH-UHFFFAOYSA-N isocyanuric acid Chemical compound OC1=NC(O)=NC(O)=N1 ZFSLODLOARCGLH-UHFFFAOYSA-N 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 230000008447 perception Effects 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L15/00—Compositions of rubber derivatives
- C08L15/02—Rubber derivatives containing halogen
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K11/00—Use of ingredients of unknown constitution, e.g. undefined reaction products
- C08K11/005—Waste materials, e.g. treated or untreated sewage sludge
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/54—Silicon-containing compounds
- C08K5/548—Silicon-containing compounds containing sulfur
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L91/00—Compositions of oils, fats or waxes; Compositions of derivatives thereof
- C08L91/06—Waxes
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
- F16J—PISTONS; CYLINDERS; SEALINGS
- F16J15/00—Sealings
- F16J15/02—Sealings between relatively-stationary surfaces
- F16J15/06—Sealings between relatively-stationary surfaces with solid packing compressed between sealing surfaces
- F16J15/08—Sealings between relatively-stationary surfaces with solid packing compressed between sealing surfaces with exclusively metal packing
- F16J15/0818—Flat gaskets
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Abstract
본 발명은 고온 영구압축줄음율 특성이 우수한 친환경 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 할 뿐만 아니라 종래 폐기되던 패각을 첨가하여 재활용함으로써 오링의 물성을 더욱 향상시키면서도 종래 패각의 폐기에 따른 비용 발생 및 환경 오염문제를 해결할 수 있는 등 친환경적인 오링을 제공할 수 있도록 하는, 고온 영구압축줄음율 특성이 우수한 친환경 오링용 불소고무 조성물에 관한 것이다.The present invention relates to an eco-friendly fluororubber composition for O-rings with excellent high-temperature compression set properties. More specifically, it relates to a permanent compression set at high temperatures by applying carbon black with a particle size of 100 nm or less, which has excellent reinforcing properties, to ternary fluoroelastomer. While securing sound modulus and tensile strength, the dispersibility of carbon black and the processability of fluoroelastomer are improved by applying anhydrous silica with a relatively large particle size. This not only improves the permanent compression set and tensile strength at high temperatures. Not only can it be improved efficiently, but it can also improve the physical properties of O-rings by adding and recycling conventionally discarded shells, and provide eco-friendly O-rings by solving the cost and environmental pollution problems caused by disposal of conventional shells. It relates to an eco-friendly fluoroelastomer composition for O-rings with excellent high-temperature compression set properties.
Description
본 발명은 고온에서의 영구압축줄음율 및 인장강도 등을 향상시킬 수 있도록 할 뿐만 아니라 종래 폐기되던 패각을 재활용하여 패각의 폐기에 따른 비용 발생 및 환경 오염문제를 해결할 수 있도록 하는 오링용 불소고무 조성물에 관한 것이다.The present invention is a fluorine rubber composition for O-rings that not only improves permanent compression set and tensile strength at high temperatures, but also solves the cost and environmental pollution problems caused by shell disposal by recycling conventionally discarded shells. It's about.
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, fluoroelastomer is one of the materials with the best heat resistance and oil resistance among existing rubbers, and is mainly used in automobile, ship, and aviation engine systems. As these engines gradually become higher output to increase energy efficiency, the engine As the internal environment of the product becomes harsher, the O-ring and false socket materials used here are required to have higher heat resistance.
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, in order to improve heat resistance, etc., fillers such as carbon black are added to compound rubber using binary (VDF (vinylidenefluoride)/HFP (hexafluoropropylene)) fluoroelastomer or ternary (VDF/HFP/TFE (tetrafluoroethylene)) fluororubber. It is being applied.
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 technology that applied carbon black with a particle size of 25 to 80 nm, which has excellent reinforcing properties, to a fluoroelastomer polymer. However, due to the nature of fluorine rubber, processability is not good, so 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 was a problem in that the efficiency of improving heat resistance was 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.To solve this problem, carbon black with a relatively large particle size (250 ~ 350 nm) is generally used, but this has less reinforcing properties than when applying carbon black with a small particle size (100 nm or less), so it is not permanent. There was a problem of insufficient improvement efficiency in compression set rate and tensile strength.
한편, 해양 폐기물인 패각(예를 들면, 굴, 석화, 전복, 피조개, 바지락, 가리비조개, 진주조개, 진주담치, 꼬막 등의 껍질)은 연간 30만톤 이상이 발생하고 있다.Meanwhile, more than 300,000 tons of marine waste shells (e.g., shells of oysters, petrified, abalone, blood clams, clams, scallops, pearl clams, mussels, cockles, etc.) are generated annually.
더욱이 패각의 경우 방치되거나 무단투기되는 경우가 대부분이며, 방치되거나 무단투기된 패각은 연안환경을 해치는 주요원인, 즉 참기 힘든 악취 및 각종 환경오염문제를 발생시켜 지역 주민들의 민원이 제기되는 등 해당 지역에서 해결이 어려운 환경 및 사회 문제로 대두되고 있다.Moreover, in most cases, shells are neglected or illegally dumped, and neglected or illegally dumped shells are the main cause of damage to the coastal environment, that is, they cause unbearable odor and various environmental pollution problems, leading to complaints from local residents. is emerging as an environmental and social problem that is difficult to solve.
일반적으로 패각은 94% 정도가 탄산칼슘으로 되어 있으며, 중금속과 유기물에 대한 높은 흡착성과 미생물이 쉽게 부착하여 성장할 수 있는 특성으로 일부에서는 이를 재활용 및 가공하고자 하는 시도가 있으며, 주로 특허문헌 1 및 2 등에서와 같이, 패각을 이용한 비료나 사료로 활용되거나 또는 각종 복토재, 토양개량제, 중화제 등에 적용되고 있다.In general, about 94% of the shell is made of calcium carbonate, and due to its high adsorption capacity for heavy metals and organic matter and the ability for microorganisms to easily attach and grow, some are attempting to recycle and process it, mainly Patent Documents 1 and 2. As in the above, shells are used as fertilizer or feed, or are applied to various soil cover materials, soil conditioners, neutralizers, etc.
하지만 상기와 같은 재활용에도 불구하고 그 효능과 방법에 대한 부정적 인식에 의해 적극적으로 활용되지 못하가 있을 뿐만 아니라, 해양투기방지법에 따라 여전히 약 10만톤 이상이 처리가 곤란한 상태이다.However, despite recycling as described above, not only is it not actively utilized due to negative perceptions about its efficacy and method, but more than 100,000 tons are still difficult to dispose of due to the Marine Dumping Prevention Act.
즉, 현재 패각은 재활용율이 매우 미비하며, 재활용되지 못한 패각은 환경오염의 주범이 되고 있다. 따라서, 해양 폐기물로 분류되어 있는 패각을 재활용할 방안이 시급한 실정이다.In other words, the recycling rate of shells is currently very low, and shells that are not recycled are the main culprit of environmental pollution. Therefore, there is an urgent need for a plan to recycle shells classified as marine waste.
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 할 뿐만 아니라 종래 폐기되던 패각을 첨가하여 재활용함으로써 오링의 물성을 더욱 향상시키면서도 종래 패각의 폐기에 따른 비용 발생 및 환경 오염문제를 해결할 수 있는 등 친환경적인 오링을 제공할 수 있도록 함을 과제로 한다.The present invention is intended to solve the above problems, by applying carbon black with a particle size of 100 nm or less, which has excellent reinforcing properties, to ternary fluoroelastomer to secure permanent compression set and tensile strength at high temperatures, but the particle size is relative. By mixing large anhydrous silica, it not only improves the dispersibility of carbon black and the processability of fluoroelastomer, but also improves the permanent compression set and tensile strength at high temperatures more efficiently, as well as using previously discarded silica. The goal is to provide an eco-friendly O-ring that further improves the physical properties of the O-ring by adding and recycling the shell, while solving the cost and environmental pollution problems caused by disposal of the conventional shell.
본 발명은 오링용 고무 조성물에 있어서, 불소고무에, 입자크기 28 ~ 36nm의 카본블랙과 입자크기 6,000 ~ 12,000nm의 무수 실리카 및 패각 분말을 혼합하여 이루어지는 것을 특징으로 하는, 고온 영구압축줄음율 특성이 우수한 친환경 오링용 불소고무 조성물을 과제의 해결 수단으로 한다.The present invention relates to a rubber composition for O-rings, which is characterized by mixing fluoroelastomer with carbon black with a particle size of 28 to 36 nm, anhydrous silica and shell powder with a particle size of 6,000 to 12,000 nm, and high temperature compression set properties. This excellent eco-friendly fluoroelastomer composition for O-rings is used as a means of solving the problem.
보다 구체적으로 상기 친환경 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, 패각 분말 1 ~ 30 중량부 및 오링용 첨가제를 혼합하여 이루어지는 것이 바람직하다.More specifically, the eco-friendly fluororubber composition for O-rings contains 20 to 30 parts by weight of carbon black with a particle size of 28 to 36 nm and 10 to 20 parts by weight of anhydrous silica with a particle size of 6,000 to 12,000 nm, based on 100 parts by weight of ternary fluororubber. , it is preferably made by mixing 1 to 30 parts by weight of shell powder and an additive for O-ring.
그리고, 상기 패각 분말은 패각을 800 ~ 1000℃에서 3 ~ 5시간 소성한 후, 입자크기 300 ~ 500 mesh로 분쇄한 후 표면개질하되, 패각 분말 100 중량부에 대하여, 실란커플링제 5 ~ 15 중량부를 혼합하여 표면개질하며, 상기 실란커플링제는 비스(트리에톡시 실릴 프로필)테트라설파이드 또는 비스(트리에톡시 실릴 프로필)디설파이드를 사용하는 것이 바람직하다.In addition, the shell powder is surface-modified after firing the shell at 800-1000°C for 3-5 hours, pulverizing it to a particle size of 300-500 mesh, and adding 5-15 weight of silane coupling agent per 100 parts by weight of shell powder. The surface is modified by mixing the parts, and it is preferable to use bis(triethoxy silyl propyl)tetrasulfide or bis(triethoxy silyl propyl)disulfide as the silane coupling agent.
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.Meanwhile, the additive for O-ring is 1 to 2 parts by weight of carnauba wax, 2 to 3 parts by weight of processing aid, 4 to 5 parts by weight of crosslinking agent, and 5 to 6 parts by weight of co-crosslinking agent, based on 100 parts by weight of the ternary fluoroelastomer. It is desirable to make it happen.
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 있도록 할 뿐만 아니라 종래 폐기되던 패각을 첨가하여 재활용함으로써 오링의 물성을 더욱 향상시키면서도 종래 패각의 폐기에 따른 비용 발생 및 환경 오염문제를 해결할 수 있는 등 친환경적인 오링을 제공할 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 has excellent reinforcing properties, to ternary fluoroelastomer, and uses a mixture of anhydrous silica with a relatively large particle size to create carbon. Not only does it improve the dispersibility of black and the processability of fluorine rubber, but it also allows for more efficient improvement of permanent compression set and tensile strength at high temperatures, as well as improving the physical properties of O-rings by adding and recycling previously discarded shells. While further improving, it has the effect of providing an eco-friendly O-ring, such as solving the cost and environmental pollution problems caused by the disposal of conventional shells.
본 발명은 고온 영구압축줄음율 특성이 우수한 친환경 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 an eco-friendly fluoroelastomer composition for O-rings with excellent high-temperature compression set properties. Only the parts necessary to understand the technical structure of the present invention are described, and the description of other parts is provided so as not to distract from the gist of the present invention. Please note that this will be omitted.
본 발명에 따른 고온 영구압축줄음율 특성이 우수한 친환경 오링용 불소고무 조성물을 설명하면 다음과 같다.The eco-friendly fluoroelastomer composition for O-rings with excellent high-temperature compression set properties 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 실리카 및 패각 분말을 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, 패각 분말 1 ~ 30 중량부 및 오링용 첨가제를 혼합하여 이루어진다.The fluororubber composition for O-rings with excellent high-temperature compression set properties according to the present invention is characterized by mixing fluororubber with carbon black with a particle size of 28 to 36 nm, anhydrous silica and shell powder with a particle size of 6,000 to 12,000 nm. More specifically, for 100 parts by weight of ternary fluoroelastomer, 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 1 to 30 parts by weight of shell powder. It is made by mixing parts by weight and additives for O-rings.
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 fluoroelastomer is a known base material widely used in rubber compositions for O-rings, and is one of the materials with the best heat resistance and oil resistance, and is mainly used in automobile, ship, and aviation engine systems. Meanwhile, the present invention is not limited to a specific fluorine rubber, and various types of already known fluorine rubber 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.Meanwhile, in the present invention, ternary fluororubber is applied as an example, and ternary fluororubber is a fluororubber made of copolymerization of VDF (vinylidenefluoride), HFP (hexafluoropropylene), and TFE (tetrafluoroethylene), which 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 with 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, if the particle size of carbon black is outside the above range, there is a risk that the efficiency of improving dispersibility may be insufficient. In addition, if the content of carbon black is less than 20 parts by weight, the reinforcing effect may be insufficient, and if it exceeds 30 parts by weight, 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. By mixing anhydrous silica with a relatively larger particle size than the carbon black, the dispersibility of the carbon black and the processability of the fluorine rubber are improved. Not only does it improve, but it also improves permanent compression set and tensile strength 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.For this purpose, the anhydrous silica is used with a particle size of 6,000 to 12,000 nm. If the particle size is outside the above range, there is a risk that the efficiency of improving dispersibility may be insufficient. In addition, if the content of anhydrous silica is less than 10 parts by weight, there is a risk that the dispersibility improvement efficiency may be insufficient, and if it exceeds 20 parts by weight, there is a risk that processability may be reduced.
상기 패각 분말은 종래 폐기되던 패각을 재활용하는 것과 더불어 물성을 더욱 향상시키기 위해 첨가되는 것으로, 그 함량이 1 중량부 미만일 경우 물성 향상 효율이 미비해질 우려가 있으며, 30 중량부를 초과할 경우 분산성이 취약해질 우려가 있다.The shell powder is added to further improve physical properties in addition to recycling previously discarded shells. If the content is less than 1 part by weight, the efficiency of improving physical properties may be insufficient, and if it exceeds 30 parts by weight, dispersibility may be reduced. There is a risk of becoming vulnerable.
한편, 상기 패각 분말은 해양 폐자원으로 시중에서 흔히 구할 수 있는 패각(예를 들면, 굴, 석화, 전복, 피조개, 바지락, 가리비조개, 진주조개, 진주담치, 꼬막 등)의 껍질을 사용하며, 불필요한 이물질이 제거된 상태로 깨끗이 세척하여 사용한다.On the other hand, the shell powder uses the shells of shells (e.g., oysters, petrified abalone, blood clams, clams, scallops, pearl clams, pearl mussels, cockles, etc.) that are commonly available on the market as marine waste resources, Wash thoroughly to remove unnecessary foreign substances before use.
아울러, 상기 패각 분말은 물성 향상 효율 및 분산성을 더욱 향상시키기 위해 패각을 800 ~ 1000℃에서 3 ~ 5시간 소성한 후, 입자크기 300 ~ 500 mesh로 분쇄하여 사용하되, 패각 분말 100 중량부에 대하여 실란커플링제 5 ~ 15 중량부를 혼합하여 표면개질하여 사용한다.In addition, the shell powder is used by calcining the shell at 800 to 1000°C for 3 to 5 hours to further improve physical property improvement efficiency and dispersibility, and then grinding it to a particle size of 300 to 500 mesh. 100 parts by weight of the shell powder For this, mix 5 to 15 parts by weight of silane coupling agent and use it for surface modification.
여기서, 상기 실란커플링제는 비스(트리에톡시 실릴 프로필)테트라설파이드 또는 비스(트리에톡시 실릴 프로필)디설파이드 등의 사용이 가능하나 반드시 여기에 한정되는 것은 아니고 이미 공지된 다양한 실란커플링제의 사용이 가능하다.Here, the silane coupling agent can be used as bis(triethoxy silyl propyl)tetrasulfide or bis(triethoxy silyl propyl)disulfide, but is not necessarily limited thereto, and various known silane coupling agents can be used. possible.
한편, 상기 소성 온도 및 시간과 입자크기, 그리고 실란커플링제의 함량이 상기 범위를 벗어날 경우 물성 향상 효율이 미비하거나 또는 분산성이 미비해질 우려가 있다.On the other hand, if the firing temperature and time, particle size, and content of the silane coupling agent are outside the above range, there is a risk that the efficiency of improving physical properties may be insufficient or the dispersibility may be insufficient.
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 O-ring is a known additive commonly used in the manufacture of O-ring, and is not limited to the type and content of the additive to be described later, and various already known additives and content 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 additive for the O-ring, 1 to 2 parts by weight of carnauba wax, 2 to 3 parts by weight of processing aid, 4 to 5 parts by weight of crosslinking agent, and 5 to 6 parts by weight of co-crosslinking agent can be applied. Specifically, the processing aid can be organosilicone, etc., and the crosslinking agent can be DHBP (2,5-dimethyl-2,5-di(tert-butylperoxy)hexyne). TAIC (trially isocyanurate), etc. can be applied, but as already described above, it is not limited to this, and various already known additives for O-rings 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 to the following examples.
1. 오링의 제조1. Manufacturing 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, 패각 분말(패각을 800℃에서 5시간 소성한 후, 입자크기 300 mesh로 분쇄하고, 패각 분말 100 중량부에 대하여 실란커플링제인 비스(트리에톡시 실릴 프로필)테트라설파이드(TESPT) 5 중량부를 혼합하여 표면개질) 1 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.For 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, 10 parts by weight of anhydrous silica (Celite N219) with a particle size of 6,000 nm. Parts by weight, shell powder (the shells were calcined at 800°C for 5 hours, then ground to a particle size of 300 mesh, and 5 parts by weight of bis(triethoxy silyl propyl)tetrasulfide (TESPT), a silane coupling agent, per 100 parts by weight of shell powder. Surface modification by mixing parts by weight) 1 part by weight, carnauba wax 1 part by weight, processing aid (organosilicone, STRUKTOL WS280) 2 parts by weight, cross-linking agent (DHBP) 4 parts by weight and co-crosslinking agent (TAIC) 5 parts by weight The compound was manufactured by kneading the part in a kneader, a compound kneader, at 110°C for about 10 minutes. After completing the kneader work, the compound is mixed uniformly in an open roll mill and then a 2mm sheet-like compound is manufactured. The sheet-shaped compound prepared in this way was put into a mold manufactured according to the test standard, press molded for about 10 minutes under press conditions of 180°C and 150 kg/cm 2 , and then heat treated at 220°C for 12 hours to produce 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, 패각 분말(패각을 1000℃에서 3시간 소성한 후, 입자크기 500 mesh로 분쇄하고, 패각 분말 100 중량부에 대하여 실란커플링제인 비스(트리에톡시 실릴 프로필)디설파이드(TESPD) 15 중량부를 혼합하여 표면개질) 30 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.For 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, 20 parts by weight of anhydrous silica (Celite N219) with a particle size of 12,000 nm Parts by weight, shell powder (the shells were calcined at 1000°C for 3 hours, then ground to a particle size of 500 mesh, and 15 parts by weight of bis(triethoxy silyl propyl)disulfide (TESPD), a silane coupling agent, per 100 parts by weight of shell powder. (surface modification by mixing parts) 30 parts by weight, carnauba wax 2 parts by weight, processing aid (organosilicone, STRUKTOL WS280) 3 parts by weight, cross-linking agent (DHBP) 5 parts by weight, and co-cross-linking agent (TAIC) 6 parts by weight A compound was prepared by kneading at 110°C for about 10 minutes in a compound kneader, a kneader. After completing the kneader work, the compound is mixed uniformly in an open roll mill and then a 2mm sheet-like compound is manufactured. The sheet-shaped compound prepared in this way was put into a mold manufactured according to the test standard, press molded for about 10 minutes under press conditions of 180°C and 150 kg/cm 2 , and then heat treated at 220°C for 12 hours to produce an O-ring.
(비교예 1)(Comparative Example 1)
실시예 1과 동일하게 제조하되, 무수 실리카를 사용하지 않았고, 패각 분말을 첨가하지 않았다.It was prepared in the same manner as in Example 1, but anhydrous silica was not used and shell powder was not added.
(비교예 2)(Comparative Example 2)
실시예 2와 동일하게 제조하되, 무수 실리카를 사용하지 않았고, 입자크기 250nm의 카본블랙(carbon black, 코리아카본블랙 N990)을 사용하였으며, 패각 분말을 첨가하지 않았다.It was prepared in the same manner as in Example 2, but anhydrous silica was not used, carbon black (Korea Carbon Black N990) with a particle size of 250 nm was used, and shell powder was not added.
2. 오링의 평가2. Evaluation of O-ring
상기 실시예 및 비교예에 따른 오링에 대한 영구압축줄음율 및 인장강도를 평가하였고 그 결과는 아래 [표 1]에 나타내었다.The compression set rate 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 reduction rate (%)
(200℃, 24 hours)
(200℃, 72시간)Permanent compression reduction rate (%)
(200℃, 72 hours)
(kgf/cm2)tensile strength
(kgf/ cm2 )
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 개선하였을 뿐만 아니라 종래 폐기되던 패각을 첨가하여 재활용함으로써 오링의 물성을 더욱 향상시키면서도 친환경적인 오링을 제공할 수 있음을 알 수 있다.As shown in [Table 1] above, the O-ring according to the embodiment of the present invention uses a mixture of carbon black with a particle size of 100 nm or less and anhydrous silica with a relatively large particle size in ternary fluoroelastomer to improve the dispersibility of carbon black. It can be seen that not only has the permanent compression set rate and tensile strength been improved more efficiently, but also the physical properties of the O-ring can be further improved by adding and recycling shells that were previously discarded, while providing an eco-friendly O-ring.
상술한 바와 같이, 본 발명에 따른 고온 영구압축줄음율 특성이 우수한 친환경 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 eco-friendly fluororubber composition for O-rings with excellent high-temperature compression set characteristics according to the present invention has been explained through the above preferred embodiments and its excellence has been confirmed, but those skilled in the art will be able to understand the scope of the patent claims below. It will be understood that the present invention can be modified and changed in various ways without departing from the spirit and scope of the present invention described in.
Claims (4)
불소고무에, 입자크기 28 ~ 36nm의 카본블랙과 입자크기 6,000 ~ 12,000nm의 무수 실리카 및 패각 분말을 혼합하여 이루어지는 것을 특징으로 하는, 고온 영구압축줄음율 특성이 우수한 친환경 오링용 불소고무 조성물.
In the rubber composition for O-ring,
An eco-friendly fluororubber composition for O-rings with excellent high-temperature permanent compression set properties, characterized in that it is made by mixing carbon black with a particle size of 28 to 36 nm and anhydrous silica and shell powder with a particle size of 6,000 to 12,000 nm.
상기 친환경 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, 패각 분말 1 ~ 30 중량부 및 오링용 첨가제를 혼합하여 이루어지는 것을 특징으로 하는, 고온 영구압축줄음율 특성이 우수한 친환경 오링용 불소고무 조성물.
According to clause 1,
The eco-friendly fluoroelastomer composition for O-ring is,
For 100 parts by weight of ternary fluoroelastomer, 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, 1 to 30 parts by weight of shell powder, and additives for O-rings. An eco-friendly fluoroelastomer composition for O-rings with excellent high-temperature compression set properties, characterized in that it is made by mixing.
상기 패각 분말은,
패각을 800 ~ 1000℃에서 3 ~ 5시간 소성한 후, 입자크기 300 ~ 500 mesh로 분쇄한 후 표면개질하되,
패각 분말 100 중량부에 대하여, 실란커플링제 5 ~ 15 중량부를 혼합하여 표면개질하며, 상기 실란커플링제는 비스(트리에톡시 실릴 프로필)테트라설파이드 또는 비스(트리에톡시 실릴 프로필)디설파이드를 사용하는 것을 특징으로 하는, 고온 영구압축줄음율 특성이 우수한 친환경 오링용 불소고무 조성물.
According to clause 2,
The shell powder is,
The shell is fired at 800 ~ 1000℃ for 3 ~ 5 hours, then ground to a particle size of 300 ~ 500 mesh, and the surface is modified.
For 100 parts by weight of shell powder, 5 to 15 parts by weight of a silane coupling agent is mixed to modify the surface, and the silane coupling agent is one using bis(triethoxy silyl propyl)tetrasulfide or bis(triethoxy silyl propyl)disulfide. An eco-friendly fluoroelastomer composition for O-rings, characterized in that it has excellent high-temperature permanent compression set properties.
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 것을 특징으로 하는, 고온 영구압축줄음율 특성이 우수한 친환경 오링용 불소고무 조성물.According to clause 1,
The additive for the O-ring is,
High temperature, characterized in that it consists of 1 to 2 parts by weight of carnauba wax, 2 to 3 parts by weight of processing aid, 4 to 5 parts by weight of crosslinking agent, and 5 to 6 parts by weight of co-crosslinking agent, based on 100 parts by weight of the ternary fluoroelastomer. An eco-friendly fluoroelastomer composition for O-rings with excellent permanent compression set properties.
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