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KR100222912B1 - Mixed rubber compositions - Google Patents

Mixed rubber compositions Download PDF

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Publication number
KR100222912B1
KR100222912B1 KR1019970025893A KR19970025893A KR100222912B1 KR 100222912 B1 KR100222912 B1 KR 100222912B1 KR 1019970025893 A KR1019970025893 A KR 1019970025893A KR 19970025893 A KR19970025893 A KR 19970025893A KR 100222912 B1 KR100222912 B1 KR 100222912B1
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South Korea
Prior art keywords
rubber
phr
rubber composition
physical properties
present
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KR1019970025893A
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Korean (ko)
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KR19990002319A (en
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이화우
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신형인
금호산업주식회사
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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
    • 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
    • B60C1/0016—Compositions of the tread
    • 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
    • C08K5/04—Oxygen-containing compounds
    • C08K5/09—Carboxylic acids; Metal salts thereof; Anhydrides thereof
    • C08K5/098—Metal salts of carboxylic acids
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L9/00—Compositions of homopolymers or copolymers of conjugated diene hydrocarbons

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Tires In General (AREA)

Abstract

본 발명은 가공성을 향상시킨 고무조성물에 관한 것으로, 좀더 상세하게는 액상의 이소프렌 고무(Liquid Isoprene Rubber)을 변성시켜 기능성기를 도입한 기능성 액상고무를 사용하여 공정성을 개선시키면서도 물성이 향상된 고무조성물에 관한 것이다.The present invention relates to a rubber composition having improved processability, and more particularly, to a rubber composition having improved physical properties while improving processability by using a functional liquid rubber having a functional group introduced by modifying liquid isoprene rubber. will be.

본 발명의 목적은 액상의 이소프렌 고무를 변성시켜 기능성기를 도입한 기능성 액상고무를 사용하여 가동성 및 물성을 향상시킨 고무조성물을 제공함에 있다.SUMMARY OF THE INVENTION An object of the present invention is to provide a rubber composition having improved mobility and physical properties by using a functional liquid rubber in which a functional group is introduced by modifying a liquid isoprene rubber.

따라서, 본 발명은 에폭시기의 함량이 10

Figure kpo00001
60몰
Figure kpo00002
(mol
Figure kpo00003
)인 에폭시화 천연고무 60
Figure kpo00004
98phr과 액상의 이소프렌 고무에 카르복실기를 도입한 카르복실화 액상 이소프렌 고무 2
Figure kpo00005
40phr를 혼합한 100phr의 혼합고무를 함유하는 배합고무 조성물임을 특징으로 한다.Therefore, the present invention has an epoxy group content of 10
Figure kpo00001
60 moles
Figure kpo00002
(mol
Figure kpo00003
Epoxidized Natural Rubber 60
Figure kpo00004
Carboxylated liquid isoprene rubber incorporating carboxyl groups in 98 phr and liquid isoprene rubber 2
Figure kpo00005
Characterized in that it is a blended rubber composition containing 100phr mixed rubber mixed with 40phr.

본 발명에 의한 배합 고무조성물은 타이어의 트레드용 고무 조성물로 유용하게 사용될 수 있다.The compounded rubber composition according to the present invention can be usefully used as a rubber composition for tread of a tire.

Description

배합고무 조성물Compound Rubber Composition

본 발명은 가공성을 향상시킨 고무조성물에 관한 것으로, 좀 더 상세하게는 액상의 이소프렌 고무(Liquid Isoprene Rubber; 이하 "LIR")을 변성시켜 기능성기를 도입한 기능성 액상고무를 사용하여 공정성을 개선시키면서도 물성이 향상된 고무조성물에 관한 것이다.The present invention relates to a rubber composition with improved processability, and more particularly, to improve the processability by using a functional liquid rubber in which a functional group is introduced by modifying a liquid isoprene rubber (hereinafter referred to as "LIR"). This improved rubber composition.

자동차용 타이어의 요구성능은 사용용도 및 위치에 따라서 크게 다르다. 특히 노면과 접촉하는 트레드고무는 내마모성, 젖은 노면에서의 제동력, 크랙저항성 등의 많은 요구 특성이 있다. 이중 특히 안전성과 관계가 있는 타이어의 제동성능은 차량의 제동에 밀접한 관계가 있으므로 대단히 중요한 요구 특성중의 하나이다.The required performance of automobile tires varies greatly depending on the intended use and location. In particular, the tread rubber in contact with the road surface has many required characteristics such as wear resistance, braking force on wet road surfaces, and crack resistance. Of these, the braking performance of tires, which is particularly related to safety, is one of the very important requirements because it is closely related to the braking of the vehicle.

종래에는 트레드고무의 제동성을 향상시키기 위하여 천연고무 대시에 스티렌-부타디엔 유화중합체(E-SBR)을 사용하여 제동성능을 향상시켰으나, E-SBR은 천연고무에 비해서 탄성이 적고 발열이 커서 타이어에 적용하여 주행서 트레드 및 벨트부위의 쎄퍼레이숀을 유발할 가능성이 높아서 제동성능을 개선시킬 목적으로의 E-SBR 사용이 억제되어 왔다. 따라서 최근에 개발된 에폭시화 천연고무를 사용하면 젖은 노면에서의 제동력도 향상되면서 천연고무의 성능을 유지하기 때문에 인장에 의해 결정성이 이루어지므로 강성도 강해지고 다른 고무와의 점착성도 양호하다. 그러나 에폭시화 천연고무는 분자량이 높아서 보강성을 증대시키기 위해서 다량의 카본블랙을 사용하면 가공성이 불량하기 때문에 액상의 이소프렌 고무를 첨가하여 가공성을 개선시킨다. 그러나 이때 가공성은 개선되지만 물성이 저하된다는 단점이 있다.Conventionally, styrene-butadiene emulsion polymer (E-SBR) is used in the natural rubber dash to improve the braking property of the tread rubber. However, the E-SBR is less elastic and has a higher heat than the natural rubber. The use of E-SBR for the purpose of improving braking performance has been suppressed because it is highly likely to cause separation of the running tread and the belt part. Therefore, when the recently developed epoxidized natural rubber improves the braking force on the wet road surface and maintains the performance of the natural rubber, it is crystallized by tension, so that the rigidity is strong and the adhesion with other rubber is good. However, since epoxidized natural rubber has a high molecular weight and a large amount of carbon black is used to increase reinforcement, workability is poor. Therefore, liquid isoprene rubber is added to improve workability. However, at this time, the workability is improved, but the physical properties are deteriorated.

본 발명자는 상기의 문제점을 해결하고자 연구를 수행하던 중, 천연고무의 불포화기에 에폭시기를 도입한 에폭시화 천연고무(EPOXIDIZED NATURAL RUBBER; ENR)를 사용하는데 이때 내마모성능 등을 향상시키기 위해서 다량의 카본블랙을 사용하면 가공성이 불량하므로, 카르복실기가 도입된 액상의 이소프렌 고무를 사용하여 가공성을 개선시키면서도 탄성을 증가시킨 고무조성물을 제조할 수 있음을 알아내고 본 발명을 완성하였다.The present inventors use the epoxidized natural rubber (EPOXIDIZED NATURAL RUBBER; ENR) in which an epoxy group is introduced into an unsaturated group of natural rubber during the research to solve the above problems, in which a large amount of carbon black to improve the wear resistance, etc. Since the processability is poor, the present invention has been completed by finding that a rubber composition having increased elasticity can be manufactured while improving processability using a liquid isoprene rubber having a carboxyl group introduced therein.

따라서, 본 발명의 목적은 액상의 이소프렌 고무를 변성시켜 기능성기를 도입한 기능성 액상고무를 사용하여 가공성 및 물성을 향상시킨 고무조성물을 제공함에 있다.Accordingly, it is an object of the present invention to provide a rubber composition having improved processability and physical properties by using a functional liquid rubber in which a functional group is introduced by modifying a liquid isoprene rubber.

즉, 본 발명은 에폭시기의 함량이 10

Figure kpo00006
60몰
Figure kpo00007
(mol
Figure kpo00008
)인 에폭시화 천연고무 60
Figure kpo00009
98phr과 액상의 이소프렌 고무에 카르복실기를 도입한 카르복실화 액상 이소프렌 고무 2
Figure kpo00010
40phr를 혼합한 100phr의 혼합고무를 함유하는 배합고무 조성물임을 특징으로 한다.That is, the present invention has a content of 10 epoxy groups
Figure kpo00006
60 moles
Figure kpo00007
(mol
Figure kpo00008
Epoxidized Natural Rubber 60
Figure kpo00009
Carboxylated liquid isoprene rubber incorporating carboxyl groups in 98 phr and liquid isoprene rubber 2
Figure kpo00010
Characterized in that it is a blended rubber composition containing 100phr mixed rubber mixed with 40phr.

ENR은 천연고무의 주쇄에 에폭시기가 부가되므로서 유리전이온도(glass transition temperature; Tg)가 상승하므로 ENR을 타이어의 여러부위중 트레드 부위에 사용하면 젖은 노면에서의 제동력이 향상되고 인너라이너 부위에 사용하면 내공기 투과성이 증가하며 그외에 금속 및 섬유등과 접착력 향상을 목적으로 사용되어 지는 최근에 개발되 고무이다. 그러나 천연고무 중에 포함되어 있는 불포화 이중 결합에 에폭시기가 과도하게 도입되면 제동성능 및 내공기투과성은 향상되지만 유리전이온도가 너무 높아져서 내한성능이 하락하고 신장시 일어나는 결정성도 일어나지 않아서 다른 물성도 급격히 하락한다. 또한 에폭시기가 너무 적게 도입되면 제동선능 및 내공기투과성의 개선효과가 적다. 다음의 표 1과 같이 천연고무에 포함된 에폭시기가 10몰

Figure kpo00011
이하이면 개선 성능이 거의 없으며, 60몰
Figure kpo00012
이상이면 제동성능 및 내공기투과성은 개선되지만 다른 물성이 크게 하락한다. 그러나 ENR 또한 제동력은 크게 향상시키지만 보강선능을 향상시키기 위해서 카본블랙을 다량 첨가하면 가공성능이 저하되어 현실적으로 적용에 어려움이 있다. 이러한 고무의 가공성을 향상시키기 위해서 공정유를 다량사용하면 물성의 하락이 크고, 이러한 물성의 하락을 최소화시키면서도 공정성을 개선시킬 목적으로 LIR을 사용하면 공정성은 개선되고 물성의 저하를 어느정도 억제시키지만 LIR을 사용하지 않은 경우에 비해서 물성이 하락된다. 액상의 이소프렌 고무에 카르복실기를 도입한 카르복실화 LIR(carboxylated liquid isoprene; CLIR)을 ENR과 혼합하여 사용하면 공정성이 개선되면서도 카르복실기와 에폭시기가 서로 반응하여 세로운 결합을 형성하므로서 탄성이 증가하게 된다. 이때 분자량이 낮은 액상의 CLIR을 40phr(parts per hundred rubber) 이상 사용하면 고무의 혼련이 곤란하여 적용이 곤란하다. CLIR과 ENR의 반응은 다음의 그림 1과 같다.ENR increases the glass transition temperature (Tg) as epoxy groups are added to the main chain of natural rubber, so when ENR is used on the tread part of the tire, the braking force on wet roads is improved and the inner liner part is used. The lower air permeability is increased and the rubber is recently developed to be used for the purpose of improving adhesion with metals and fibers. However, excessive introduction of epoxy groups into unsaturated double bonds contained in natural rubber improves braking performance and air permeability, but the glass transition temperature is so high that cold resistance decreases and crystallinity does not occur due to elongation. . In addition, when too little epoxy group is introduced, the braking performance and the air permeability are less improved. As shown in Table 1, 10 moles of epoxy groups contained in natural rubber
Figure kpo00011
There is almost no improvement if it is less than 60 moles
Figure kpo00012
Above, the braking performance and air permeability are improved, but other physical properties are greatly reduced. However, ENR also greatly improves the braking force, but adding a large amount of carbon black to improve the reinforcement performance lowers the processing performance, which makes it difficult to apply it in reality. When using a large amount of process oil to improve the processability of such rubber, there is a large drop in physical properties, and the use of LIR for the purpose of improving processability while minimizing such a drop in physical properties improves fairness and suppresses the degradation of physical properties to some extent. Physical properties are lower than when not used. When the carboxylated liquid isoprene (CLIR) with carboxyl group introduced into the liquid isoprene rubber is mixed with ENR, the elasticity is increased because the carboxyl group and the epoxy group react with each other to form a new bond. At this time, if the low molecular weight liquid CLIR is used in more than 40phr (parts per hundred rubber), rubber kneading is difficult to apply. The reaction between CLIR and ENR is shown in Figure 1 below.

Figure kpo00013
Figure kpo00013

또한 ENR고무를 사용할 때에 스코치타임이 짧아져서 공정성이 불량한 단점이 있으므로 칼슘스테아린산 또는 소디움카보네이트(Na2CO3) 등을 사용하여 공정성을 개선시키는데 이때 사용하는 적정량은 칼슘스테아린산 1-8phr 또는 소디움카보네이트(Na2CO3) 0.1-3.0phr을 사용하는 것이 바람직하며, 과량사용시에는 그 효과가 오히려 감소되는 경향을 나타낸다.In addition, when using ENR rubber, the scorch time is shortened, resulting in poor processability. Therefore, calcium stearic acid or sodium carbonate (Na 2 CO 3 ) is used to improve fairness. Na 2 CO 3 ) It is preferable to use 0.1-3.0 phr, and the effect tends to decrease rather than excessive use.

Figure kpo00014
Figure kpo00014

이하 실시예를 통하여 본 발명을 보다 상세히 설명한다. 그러나 본 발명이 이들 실시예에 국한되는 것은 아니다.Hereinafter, the present invention will be described in more detail with reference to the following examples. However, the present invention is not limited to these examples.

[실시예 1]Example 1

에폭시기의 함량이 25몰

Figure kpo00015
인 에폭시화 천연고무 100phr과 카본블랙 60phr, 산화아연 5phr, 스테아린산 2Phr, 노화방지제 2phr, 공정유 5phr, 황 2phr 및 가류촉진제 1phr을 배합하고 160℃의 온도에서 방출시켰다.25 moles of epoxy group
Figure kpo00015
100 phr of phosphorus epoxidized natural rubber, 60 phr of carbon black, 5 phr of zinc oxide, 2 Phr of stearic acid, 2 phr of antioxidant, 5 phr of process oil, 2 phr of sulfur, and 1 phr of vulcanization accelerator were combined and released at a temperature of 160 ° C.

생성된 중합체 조성물의 점도, 제동성능, 탄성, 스코치타임 등의 물리적 성질을 ASTM 표준방법에 의해 측정하였는바, 중합체 조성물의 배합비와 물리적 성질 측정결과를 다음의 표 2에 나타내었다.Physical properties such as viscosity, braking performance, elasticity, scorch time, etc. of the resulting polymer composition were measured by the ASTM standard method, and the blending ratio and physical property measurement results of the polymer composition are shown in Table 2 below.

이때, 지수값은 에폭시화 천연고무를 함유하지 않은 조성물(비교예 1)의 값을 100으로 환산한 값으로, 지수가 높을수록 양호함을 의미한다.At this time, the index value is a value obtained by converting the value of the composition (Comparative Example 1) containing no epoxidized natural rubber into 100, and the higher the index, the better.

[실시예 2]Example 2

에폭시화 천연고무를 85phr로 하고, 카르복실화 액상 이소프렌 고무를 15phr로 하는 것 이외에는 실시예 1과 동일하게 실시하여 물리적 성질을 측정하였는 바, 중합체 조성물의 배합비와 물리적 성질의 측정 결과를 표 2에 나타내었다.The physical properties were measured in the same manner as in Example 1 except that the epoxidized natural rubber was 85 phr and the carboxylated liquid isoprene rubber was 15 phr. The results of measurement of the blending ratio and physical properties of the polymer composition are shown in Table 2. Indicated.

[실시예 3]Example 3

소디움카보네이트 1phr을 추가로 첨가하는 것 이외에는 실시예 2와 동일하게 실시하여 물리적 성질을 측정하였는 바, 중합체 조성물의 배합비와 물리적 성질의 측정결과를 표 2에 나타내었다.Except for adding 1 phr of sodium carbonate, the physical properties were measured in the same manner as in Example 2, and the results of measurement of the blending ratio and physical properties of the polymer composition are shown in Table 2.

[실시예 4]Example 4

소디움카보네이트의 함량에 따른 물성변화를 알아보기 위하여 소디움카보네이트를 3phr로 하는 것 이외에는 실시예 3과 동일하게 실시하여 물리적 서질을 측정하였는 바, 중합체 조성물의 배합비와 물리적 성질의 측정결과를 표 2에 나타내었다.In order to determine the change in physical properties according to the content of sodium carbonate was measured in the same manner as in Example 3 except that the sodium carbonate to 3phr, the measurement results of the blending ratio and physical properties of the polymer composition is shown in Table 2 It was.

[비교예][Comparative Example]

에폭시화 천연고무 대신에 천연고무를 100phr로 하는 것 이외에는 실시예 1과 동일하게 실시하여 물리적 성질을 측정하였는바, 중합체 조성물의 배합비와 물리적 성질의 측정결과를 표 2에 나타내었다.The physical properties of the polymers were measured in the same manner as in Example 1 except that 100 phr of natural rubber was used instead of epoxidized natural rubber. Table 2 shows the results of the mixing ratio and physical properties of the polymer composition.

Figure kpo00016
Figure kpo00016

본 발명에 의한 배합고무 조성물은 표 2에서 보는 바와 같이, 천연고무를 사용한 종래의 트레드 고무조성물에 비하여 안정성과 관계가 있는 타이어의 제동성능이 월등히 개선되고, 점도, 탄성 및 스코치 타임이 양호하여 가공성이 향상된 것으로 타이어의 트레드용 고무조성물로 유용하게 사용될 수 있다.As shown in Table 2, the compounded rubber composition according to the present invention is significantly improved in braking performance of tires related to stability, compared to conventional tread rubber compositions using natural rubber, and has excellent viscosity, elasticity and scorch time. This improvement can be usefully used as a rubber composition for tread of tires.

Claims (3)

고무원료, 가류활성제, 가류제, 가황촉진제, 공정오일, 노화방지제 및 공정개선제로 구성된 고무조성물에 있어서, 고무원료로 타이어의 제동력과 탄성을 부여하는 에폭시화 천연고무(ENR) 60-98phr과 고정성을 부여하며 물성하락을 방지하기 위해 카르복실화 액상 이소프렌 고무(CLIR) 2-40phr를 혼합한 100phr의 혼합고무를 함유하는 배합고무 조성물.Epoxylated natural rubber (ENR) 60-98 phr and rubber for rubber composition composed of rubber raw materials, vulcanizing agents, vulcanizing agents, vulcanization accelerators, process oils, anti-aging agents and process improving agents. A compounded rubber composition containing 100 phr of mixed rubber in which 2-40 phr of carboxylated liquid isoprene rubber (CLIR) is added to impart qualities and prevent physical property deterioration. 제1항에 있어서, 에폭시화 천연고무의 에폭시기 함량이 10-60몰
Figure kpo00017
(mol
Figure kpo00018
)임을 특징으로 하는 배합고무 조성물.The epoxy group content of the epoxidized natural rubber is 10-60 mol.
Figure kpo00017
(mol
Figure kpo00018
Compound rubber composition, characterized in that). 제1항에 있어서, 공정개선제로 1-8phr의 칼슘스테아린산 또는 0.1-3.0phr의 소디움카보네이트(Na2CO3)를 사용함을 특징으로 하는 배합고무 조성물.The compound rubber composition according to claim 1, wherein 1-8 phr of calcium stearic acid or 0.1-3.0 phr of sodium carbonate (Na 2 CO 3 ) is used as a process improving agent.
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Publication number Priority date Publication date Assignee Title
CN105131381A (en) * 2015-08-18 2015-12-09 合肥市再德高分子材料有限公司 Environmental-protection wear-resistant wet-skid resistant rubber material specially used for tyre treads

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* Cited by examiner, † Cited by third party
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KR100426067B1 (en) * 2001-10-12 2004-04-06 금호타이어 주식회사 Tread Rubber composition improved wet traction
KR100803319B1 (en) * 2007-02-23 2008-02-13 금호타이어 주식회사 Master batch comprising modified isoprene rubber, tertiary amine, silica, silan coupling agent and rubber composition for tire thereof
KR100871990B1 (en) * 2007-09-21 2008-12-05 금호타이어 주식회사 Tire tread rubber composition comprising carboxylated liquid isoprene rubber

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105131381A (en) * 2015-08-18 2015-12-09 合肥市再德高分子材料有限公司 Environmental-protection wear-resistant wet-skid resistant rubber material specially used for tyre treads

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