KR19980065758A - Rubber composition with improved ozone resistance and aging resistance - Google Patents
Rubber composition with improved ozone resistance and aging resistance Download PDFInfo
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- KR19980065758A KR19980065758A KR1019970000871A KR19970000871A KR19980065758A KR 19980065758 A KR19980065758 A KR 19980065758A KR 1019970000871 A KR1019970000871 A KR 1019970000871A KR 19970000871 A KR19970000871 A KR 19970000871A KR 19980065758 A KR19980065758 A KR 19980065758A
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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
- C08L7/00—Compositions of natural rubber
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B60—VEHICLES IN GENERAL
- B60C—VEHICLE TYRES; TYRE INFLATION; TYRE CHANGING; CONNECTING VALVES TO INFLATABLE ELASTIC BODIES IN GENERAL; DEVICES OR ARRANGEMENTS RELATED TO TYRES
- B60C1/00—Tyres characterised by the chemical composition or the physical arrangement or mixture of the composition
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
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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
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/04—Homopolymers or copolymers of ethene
- C08L23/08—Copolymers of ethene
- C08L23/0807—Copolymers of ethene with unsaturated hydrocarbons only containing four or more carbon atoms
- C08L23/0838—Copolymers of ethene with unsaturated hydrocarbons only containing four or more carbon atoms with monomers including an aromatic carbocyclic ring
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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
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/16—Ethene-propene or ethene-propene-diene copolymers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/18—Homopolymers or copolymers of hydrocarbons having four or more carbon atoms
- C08L23/20—Homopolymers or copolymers of hydrocarbons having four or more carbon atoms having four to nine carbon atoms
- C08L23/22—Copolymers of isobutene; Butyl rubber; Homopolymers or copolymers of other iso-olefins
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- C—CHEMISTRY; METALLURGY
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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Abstract
본 발명의 타이어 고무조성물은 천연고무 60∼40중량부와 EPDM고무 40∼60중량부로 이루어진 혼합고무 100중량부에 대하여 점착제로서 폴리이소부틸렌 1∼3중량부와 부틸페놀-p-t-아세틸렌수지 2∼6중량부를 포함하는 것을 특징으로 한다.The tire rubber composition of the present invention is 1 to 3 parts by weight of polyisobutylene and butylphenol-pt-acetylene resin 2 as a pressure-sensitive adhesive based on 100 parts by weight of mixed rubber consisting of 60 to 40 parts by weight of natural rubber and 40 to 60 parts by weight of EPDM rubber. It is characterized by including-6 parts by weight.
본 발명의 고무조성물은 혼합공정중에 천연고무와 카본블랙 전체 배합량의 1/2을 먼저 혼합하는 프리블렌딩 공정을 적용하여 제조되는 것을 특징으로 한다.The rubber composition of the present invention is characterized by being prepared by applying a preblending process of first mixing half of the total amount of natural rubber and carbon black in the mixing process.
Description
본 발명은 TBR 또는 PCR 승용차 타이어에 있어서 사이드월 부위의 오존이나 내열에 의한 크랙을 개선하며 노방제의 적용시 외부로의 노방제 이동(Migration)에 의한 사이드월 부위의 변색을 감소시키므로써 타이어의 외관품질을 향상시키는 고무조성물에 관한 것이다.The present invention improves the cracks of ozone or heat resistance in the sidewall area of a TBR or PCR passenger car tire and reduces the discoloration of the sidewall area due to migration of the road agent to the outside when the road agent is applied. It relates to a rubber composition to improve the appearance quality.
오늘날 타이어의 요구성능은 매우 다양하여 소비자들의 기호에 맞게끔 타이어를 제조하여 공급하는 것이 타이어 제조회사의 궁극적인 목표가 될 수 있다.The demands of today's tires are so diverse that manufacturing and supplying tires to the tastes of consumers can be the ultimate goal of tire manufacturers.
종래에는 타이어 사이드월 부위의 내오존성을 개선하기 위하여 폴리머는 NR/SBR/BR 블렌드고무나, NR/BR 블렌드 고무에 노방제로서 6PPD(N-(1,3-디메틸부틸), N1PH-P-페닐디아민), TMDQ(2,2,4-트리메틸-1,2-디하이드로퀴놀린), SPN(스티렌화페놀), BLE-N(디페닐아민과 아세톤의 반응물)등을 사용하였고, 마이크로크리스탈린 왁스도 고무표면에 피막을 형성하여 정적인 상태에서 오존공격에 의한 크랙을 감소시키기 위하여 2∼5phr 정도 사용하였다. 그러나 이들 방법에 있어 가장 문제가 되는 것은 노방제가 주행중 열이나 오존이 존재하는 대기중에서 소멸되므로써 노방효과의 감소나 오존 크랙을 발생하여 타이어의 수명 단축이나 심한 경우에는 타이어 사고를 유발할 수 있다는 점이다.Conventionally, in order to improve the ozone resistance of tire sidewalls, the polymer is NR / SBR / BR blend rubber or 6PPD (N- (1,3-dimethylbutyl), N 1 PH- as a lubricant for NR / BR blend rubber). P-phenyldiamine), TMDQ (2,2,4-trimethyl-1,2-dihydroquinoline), SPN (styreneated phenol), BLE-N (reactant of diphenylamine and acetone), and the like Crystalline wax was also used to form a film on the rubber surface to reduce cracks due to ozone attack in a static state of about 2 ~ 5phr. However, the most troublesome thing about these methods is that they can be reduced in the atmosphere due to heat or ozone in the air while driving, which can reduce the effects of the roadwork or cause ozone cracks, which can lead to tire life and, in severe cases, tire accidents.
실험실에서의 평가에 의하면, 기존 NR/SBR 블렌드 고무나, NR/SBR/BR 블렌드 고무에 노방제로서 6PPD 또는 TMDQ를 1∼4phr 적용하고, 마이크로크리스탈린왁스를 1∼2phr 적용한 경우, 노방제는 105℃에서 6일간 방치시 소멸로 인하여 노방제 잔류양은 초기량의 2∼3%이었으며, 마이크로크리스탈린왁스는 C30∼C35의 카본분포에서는 이동(Migration)에 의한 소멸이 거의 없었지만, C25∼C27의 카본분포에서는 왁스의 잔류양이 초기량의 85%이었다.According to the laboratory evaluation, when 1 to 4 phr of 6PPD or TMDQ is applied to the existing NR / SBR blend rubber or NR / SBR / BR blend rubber and 1 to 2 phr of microcrystalline wax is used, due at 105 ℃ to 6 days when left extinction was no control residual amount 2-3% of the initial amount, microcrystalline wax is in the carbon distribution of C 30 ~C 35 is destroyed by the mobile (Migration) substantially eopeotjiman, C 25 In the carbon distribution of -C 27, the amount of wax remaining was 85% of the initial amount.
이로인해, 주행시 타이어의 내부는 120∼140℃, 외부는 55∼75℃ 정도의 열이 발생되므로 노방제의 소멸로 인한 오존에 의한 크랙 발생을 방지하기에는 거의 불가능한 실정이다. 특히, 여름철이나 오존이 많이 발생하는 지역에서는 매우 심각한 실정이다.As a result, since the tire generates heat of about 120 to 140 ° C. and about 55 to 75 ° C. on the outside of the tire, it is almost impossible to prevent cracks caused by ozone due to the disappearance of the road agent. In particular, the situation is very serious in the summer or ozone-producing areas.
또한, 실험실에서 NR/BR 블렌드고무나 NR/SBR/BR 블렌드고무에 노방제나 왁스를 적용하여 이에 대한 오존시험을 한 결과, 40℃, 50pphm 오존농도하의 정적 조건에서 24시간 정도만 방치해도 오존크랙이 발생하였다. 또한, 노방제의 소멸양이 많아 이를 보충키 위하여 노방제의 양을 많이 적용할 지라도 이에 대한 효과는 그리크지 않으며 이로인한 노방제의 이동에 의한 외관 품질에도 악영향을 미치게 된다.In addition, the ozone test was carried out by applying a preservative or wax to NR / BR blend rubber or NR / SBR / BR blend rubber in the laboratory. As a result, ozone cracks are maintained even if left alone for about 24 hours at 40 ° C and 50 ppm ozone concentration. Occurred. In addition, even if the amount of extinction agent is a lot of extinction agent to supplement this, even if the amount of the excreta agent is applied a lot, the effect is not so great and thereby adversely affects the appearance quality by the movement of the agent.
따라서 본 발명의 목적은 상기한 종래의 문제점을 해결하기 위하여 타이어에 첨가되는 고무와 첨가제들을 달리함으로써 타이어의 오존크랙을 감소시키는 고무조성물을 제공하고자 하는 것이다.Accordingly, an object of the present invention is to provide a rubber composition that reduces ozone cracks in a tire by varying rubber and additives added to a tire in order to solve the above-mentioned problems.
상기와 같은 목적을 달성하기 위한 본 발명에 따른 고무조성물은 기존에 사용된 고무인 NR, BR, SBR 고무는 이중결합이 많아 오존이 고무의 이중결합을 공격하여 고무분자쇄 절단을 가져오므로 이를 방지하기 위하여 이중결합이 적고 타고무와 공가류가 용이하며 공정가공성이 양호한 ENB(Oil extended) 타입의 EPDM 고무를 천연고무와 블렌드하여 적용하고, 노방제 및 마이크로크리스탈린왁스의 적용없이 점착제로서 폴리이소부틸렌(Poly Iso Butylene with different molecular weight)과 부틸페놀-p-t-아세틸렌수지(Butyl phenol-p-t-acetylene resin)를 적용하여 이루어진다.The rubber composition according to the present invention for achieving the above object is a rubber used in the existing NR, BR, SBR rubber has a large number of double bonds and ozone attacks the rubber double bonds, thereby preventing the rubber molecular chain cutting In order to reduce the number of double bonds, facilitate the application of rubber and co-vegetability, and processability, ENB (Oil extended) type EPDM rubber is applied by blending with natural rubber and polyisobutyl as an adhesive without the application of preservatives and microcrystalline waxes. It is made by applying ethylene (Poly Iso Butylene with different molecular weight) and butyl phenol-pt-acetylene resin.
즉, 본 발명의 고무조성물은 천연고무 60∼40중량부와 EPDM고무 40∼60중량부로 이루어진 혼합고무 100중량부에 대하여 점착제로서 폴리이소부틸렌 1∼3중량부와 부틸페놀-p-t-아세틸렌수지 2∼6 중량부를 포함하는 것을 특징으로 한다.That is, the rubber composition of the present invention is 1 to 3 parts by weight of polyisobutylene and butylphenol-pt-acetylene resin as an adhesive based on 100 parts by weight of a mixed rubber composed of 60 to 40 parts by weight of natural rubber and 40 to 60 parts by weight of EPDM rubber. It is characterized by including 2 to 6 parts by weight.
본 발명에서는 점착제를 상기 범위이상으로 사용할 경우 비용증가로 인해 제조원가가 상승되므로 바람직하지 않고, 상기 범위 이하로 사용할 경우 만족할 만한 효과를 얻지 못하므로 바람직하지 않다.In the present invention, when the pressure-sensitive adhesive is used in the above range, the manufacturing cost is increased due to the increase in cost, and when the pressure-sensitive adhesive is used in the range below, the satisfactory effect is not obtained.
본 발명에서는 EPDM 고무와 천연고무가 잘 혼합되게 하기 위하여 천연고무와 카본블랙 전체 배합량의 1/2을 프리블렌딩(preblending)한 다음, 이를 EPDM 고무와 혼합하고 이어서 약품을 투입하여 배합을 한다. 또한, 본 발명에서는 EPDM 고무의 점착성이 타고무에 비해 떨어지므로 약품 투입시 점착제인 폴리이소부틸렌(Poly Iso Butylene with different molecular weight)을 적용하였다. 이때 EPDM 고무는 40phr 이상만 적용하면 오존에 의한 크랙은 전혀 발생하지 않는다.In the present invention, in order to mix the EPDM rubber and natural rubber well, half of the total blended amount of natural rubber and carbon black is preblended, and then mixed with EPDM rubber, followed by chemical injection. In addition, in the present invention, since the adhesiveness of EPDM rubber is inferior to that of the rubber, polyisobutylene (Poly Iso Butylene with different molecular weight) was applied during chemical injection. At this time, when only 40 phr of EPDM rubber is applied, no crack is generated by ozone.
또한, 본 발명에서는 노방제와 마이크로크리스탈린왁스를 적용하지 않으므로, 이들의 소멸로 인한 오존에 의한 크랙이 발생되지 않게 된다.In addition, in the present invention, since the preservative and the microcrystalline wax are not applied, cracks due to ozone due to their disappearance do not occur.
이하 실시예를 통하여 본 발명을 상세하게 설명한다.The present invention will be described in detail through the following examples.
[실시예]EXAMPLE
(1) 시험고무의 준비(1) Preparation of test rubber
하기 표1은 고무의 중량을 100으로 하여 무게를 나타냈으며 고무의 가공성과 화학적인 반응 특성을 고려하여 배합조성을 설정하였다. 배합 순서는 반바리믹서에서 고무의 분산개선에 의한 물성을 향상시키기 위하여 천연고무 40phr에 카본블랙의 전체 배합량의 1/2인 30phr을 먼저 블렌딩하는 1차 배합을 실시하고 2차 배합에서 EPDM 고무와 혼합하고 3차 배합에서 나머지 카본블랙 30phr과 활성제 점착제 노방제 등의 약품을 투입하여 배합하였다. 이때 EPDM 고무는 점착성이 타고무에 비해 떨어지므로 약품 투입시 EPDM에 점착성이 강한 점착제인 폴리이소부틸렌과 부틸페놀-p-t-아세틸렌수지를 적용하였다. 4차 배합에서는 반바리믹서에서 유황과 촉진제를 첨가하여 배합하였다.Table 1 shows the weight of the rubber as 100, and set the blending composition in consideration of the processability and chemical reaction characteristics of the rubber. In order to improve the physical properties of rubber in the semi-barrier mixer, the first blending process is to first blend 30 phr, which is 1/2 of the total amount of carbon black, to 40 phr of natural rubber, In the tertiary blending, the remaining carbon black 30 phr and the activator pressure-sensitive adhesive agent was added and blended. At this time, since EPDM rubber is inferior in adhesiveness to rubber, polyisobutylene and butylphenol-p-t-acetylene resin, which are strong adhesives in EPDM, were applied when chemicals were injected. In the fourth formulation, sulfur and an accelerator were added in a half-barrier mixer.
[표 1] TABLE 1
1) EPDM 고무 : 100% Oil extended ENB 타입1) EPDM Rubber: 100% Oil extended ENB Type
2) 노방제 : 6PPD(N-(1,3-디메틸부틸),N1PH-P-페닐디아민)2) Furnishing agent: 6PPD (N- (1,3-dimethylbutyl), N 1 PH-P-phenyldiamine)
TMDQ(2,2,4-트리메틸-1,2-디하이드로퀴놀린)TMDQ (2,2,4-trimethyl-1,2-dihydroquinoline)
3) 왁스 : 마이크로크리스탈린왁스(M.P : 63℃)3) Wax: Microcrystalline Wax (M.P: 63 ℃)
4) 점착제 : BPA(부틸페놀-P-t-아세틸렌수지)4) Adhesive: BPA (Butylphenol-P-t-acetylene resin)
PIB(Poly Iso Butylene with different molecular weight)Poly Iso Butylene with different molecular weight (PIB)
BPA : PIB = 2 : 3BPA: PIB = 2: 3
2. 가황특성 및 물성 측정2. Vulcanization Characteristics and Property Measurement
배합고무의 가황조건 및 시험은 ASTM 규격에 준하여 시험하였고 그 결과는 표2와 같다.Vulcanization conditions and tests of the compounded rubber were tested in accordance with ASTM standards and the results are shown in Table 2.
[표 2] TABLE 2
상기 표2에서 나타난 결과에서 알 수 있듯이, NR, BR, SBR 고무를 모두 사용한 경우(비교예)에는 노방제 6PPD, TMDQ와 마이크로크리스탈린 왁스를 적용해도 고무의 특성상 오존시험결과 정적오존시험에서도 24시간만에 오존 크랙이 발생하였으며, 동적시험에서는 4시간만에 오존크랙이 발생하였다.As can be seen from the results shown in Table 2, when all NR, BR, and SBR rubbers are used (comparative example), even in the case of using 6PPD, TMDQ and microcrystalline wax as a preservative, the ozone test results showed a static ozone test. Ozone crack occurred in time, and ozone crack occurred in 4 hours in dynamic test.
그러나 이중결합이 적은 EPDM 고무를 적용한 경우 (실시예 2∼3)에는 20중량부 적용한 경우에는 별효과를 나타내지 않았지만, 40중량부 적용한 경우에는 정적 오존시험에서, 60일간 방치해도 전혀 오존 크랙의 발생이 없었다. 또한 동적 오존시험에서도 30일 방치해도 오존 크랙의 발생이 나타나지 않았다.However, when 20 parts by weight of EPDM rubber with less double bonds was applied (Examples 2 to 3), no significant effect was observed. However, when 40 parts by weight were applied, ozone cracks were not generated at all in the static ozone test for 60 days. There was no. In addition, the ozone crack did not appear even after 30 days in the dynamic ozone test.
상기 표1에서 알 수 있듯이, EPDM 고무의 적용시 물성 조절(경도, 300% 모듈러스, 인장강도)을 기하기 위하여 카본블랙양을 기존보다 증가시켜 배합하였고, 점착성능을 개선하기 위하여 EPDM 고무에 점착성이 우수한 폴리이소부틸렌과 부틸페놀-p-t-아세틸렌수지를 적용하였다.As can be seen in Table 1, in order to control the physical properties (hardness, 300% modulus, tensile strength) when applying the EPDM rubber, the amount of carbon black was increased and blended to the conventional, and the adhesion to the EPDM rubber to improve the adhesive performance This excellent polyisobutylene and butylphenol-pt-acetylene resin were applied.
균일한 물성유지와 폴리머의 블렌딩 개선에 의한 내굴곡성을 개선하기 위하여 EPDM 고무와 천연고무가 잘 혼합하기 위하여 천연고무와 카본블랙 전체 배합량의 1/2을 프리블렌딩 실시하고 이어서 EPDM 고무와 혼합한 다음에 약품을 투입하여 배합을 하는 프리블렌딩 믹싱(Preblending Mixing)을 실시하면 우수한 물성유지와 내오존성에서는 획기적으로 우수한 고무 조성물을 얻을 수 있음을 알 수 있었다.In order to mix the EPDM rubber and natural rubber well in order to maintain uniform physical properties and to improve the bending resistance by improving the blending of the polymer, 1/2 of the total amount of natural rubber and carbon black is preblended and then mixed with the EPDM rubber. When preblending mixing was carried out by adding a chemical to the formulation, it was found that a rubber composition was obtained with excellent physical properties and ozone resistance.
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