KR100415162B1 - Silica-filler rubber composition dispersion improved - Google Patents

Silica-filler rubber composition dispersion improved Download PDF

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KR100415162B1
KR100415162B1 KR10-2001-0019049A KR20010019049A KR100415162B1 KR 100415162 B1 KR100415162 B1 KR 100415162B1 KR 20010019049 A KR20010019049 A KR 20010019049A KR 100415162 B1 KR100415162 B1 KR 100415162B1
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rubber
silica
phr
rubber composition
present
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KR10-2001-0019049A
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KR20020080021A (en
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이현화
한승철
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금호타이어 주식회사
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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
    • C08K5/04—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
    • 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
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L21/00—Compositions of unspecified rubbers
    • 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
    • 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
    • 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
    • C08L9/06—Copolymers with styrene

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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)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

본 발명은 실리카 고무조성물에 관한 것이다.The present invention relates to a silica rubber composition.

본 발명의 실리카 고무조성물은 공지의 실리카 고무조성물에 있어서, 원료고무로 천연고무, 스티렌 부타디엔 고무, 부타디엔 고무를 각각 사용하거나 또는 이들이 서로 혼합된 혼합고무인 원료고무 100 phr에 대하여 실리카의 분산성을 증가시켜 고무의 점도 개선 및 물성을 향상시키기 위해 분산제를 3∼12 phr 포함하는 것을 특징으로 한다.In the silica rubber composition of the present invention, in the known silica rubber composition, natural rubber, styrene butadiene rubber, butadiene rubber are used as raw material rubbers, or the dispersibility of silica is increased with respect to 100 phr of raw rubber which is a mixed rubber mixed with each other. It characterized in that it comprises 3 to 12 phr dispersant to improve the viscosity and physical properties of the rubber.

본 발명은 실리카 고무조성물에 있어서, 분산제로서 고가의 분산조제나 사용량의 많은 공정오일 대신 폐식용유를 원료로 제조한 재생비누를 사용하여 고무내에서 실리카의 분산성을 향상시켜 점도 개선 및 물성을 향상시키는 실리카 고무조성물의 제공을 목적으로 한다.The present invention is to improve the dispersibility of silica in rubber by improving the dispersibility of silica in rubber by using recycled soap made from waste cooking oil as a raw material instead of expensive dispersing aid or a large amount of process oil in the silica rubber composition. It is an object of the present invention to provide a silica rubber composition.

또한 폐식용유로부터 제조한 재생비누를 사용함으로써 폐식용유의 재활용을 촉진하여 폐식용유에 의한 환경오염의 방지를 본 발명의 다른 목적으로 한다.Another object of the present invention is to promote the recycling of waste cooking oil by using recycled soap prepared from waste cooking oil and to prevent environmental pollution by waste cooking oil.

Description

분산성이 향상된 실리카 고무조성물{Silica-filler rubber composition dispersion improved}Silica-filler rubber composition dispersion improved

본 발명은 실리카 고무조성물에 관한 것으로서 보다 상세하게는 실리카의 분산성을 향상시키기 위해 분산제로서 폐식용유로 제조된 재생비누를 첨가하는 것을 특징으로 하는 실리카 고무조성물에 관한 것이다.The present invention relates to a silica rubber composition, and more particularly, to a silica rubber composition comprising adding recycled soap made of waste cooking oil as a dispersant to improve the dispersibility of silica.

최근 타이어에 사용하는 고무에 있어서 보강충진제로 실리카를 적용하는 고무조성물이 증가하고 있다. 그러나 실리카는 고무조성물에 사용시 분산 불량에 의한 점도 상승 및 고무물성이 하락을 방지하기 위해서 분산조제 또는 공정오일을 사용하여 고무조성물에 있어서 실리카의 분산성을 향상시키고 있다.In recent years, rubber compositions that use silica as a reinforcing filler in rubber for tires have been increasing. However, silica is used to improve the dispersibility of silica in the rubber composition by using a dispersing aid or process oil in order to prevent the viscosity increase and the rubber property decrease due to poor dispersion when used in the rubber composition.

분산조제는 주로 금속 지방산염으로 구성된 화합물로서 금속이온에 의한 친수성기와 지방산에 의한 소수성기를 동시에 가지고 있는 양친화성 물질로써, 금속이온은 실리카 표면의 실라놀 그룹(silanol group, Si-OH) 들과 반응하여 수소결합이나 쌍극자 결합에 의해 강하게 결합되어 있는 실리카 응집(agglomerate)에 대해서 분자간의 표면에너지를 감소시킴으로써 혼합공정 중 실리카의 탈응집화(de-agglomerating)를 유도하고, 지방산은 고무사슬과 상용성이 우수하여 고무사슬 끼리의 결합력을 희석(diluting)시켜 고무의 점도를 낮추는 역할을 한다.Dispersion aid is a compound composed mainly of metal fatty acid salts and has an affinity material which has both hydrophilic group by metal ion and hydrophobic group by fatty acid. Metal ion reacts with silanol groups (Si-OH) on silica surface. By reducing the surface energy between molecules against silica agglomerates that are strongly bound by hydrogen bonding or dipole bonding, de-agglomerating of the silica is induced during the mixing process, and fatty acids are compatible with rubber chains. This excellent dilution of the bonding force between the rubber chain (diluting) serves to lower the viscosity of the rubber.

공정오일은 탄화수소로 구성된 소수성의 물질로서 고무사슬의 결합(entanglement)을 희석(diluting)시켜 고무의 점도를 낮추는 역할을 한다.Process oil is a hydrophobic substance composed of hydrocarbons, which reduces the viscosity of rubber by diluting the entanglement of the rubber chain.

그러나 분산제로 사용하는 분산조제는 가격이 비싼 단점이 있고, 분산제로 공정오일을 사용시 분산조제와 동등한 점도 하락 효과를 얻기 위해서는 오일의 첨가량이 분산조제의 첨가량보다 3배 이상 요구 되기 때문에 고무조성물에 사용하는 첨가제와 반응하여 고무의 물성을 하락시킬 위험이 있다.However, the dispersing agent used as a dispersant has a disadvantage that the price is expensive, and in order to obtain a viscosity drop effect equivalent to that of the dispersing aid when using the process oil as a dispersant, it is used in rubber compositions because the amount of oil is required more than three times the amount of the dispersing agent. There is a risk of reducing the physical properties of the rubber by reacting with the additive.

본 발명은 실리카 고무조성물에 있어서, 분산제로서 고가의 분산조제나 사용량의 많은 공정오일 대신 폐식용유를 원료로 제조한 재생비누를 사용하여 고무내에서 실리카의 분산성을 향상시켜 점도 개선 및 물성을 향상시키는 실리카 고무조성물의 제공을 목적으로 한다.The present invention is to improve the dispersibility of silica in rubber by improving the dispersibility of silica in rubber by using recycled soap made from waste cooking oil as a raw material instead of expensive dispersing aid or a large amount of process oil in the silica rubber composition. It is an object of the present invention to provide a silica rubber composition.

또한 폐식용유로부터 제조한 재생비누를 사용함으로써 폐식용유의 재활용을 촉진하여 폐식용유에 의한 환경오염의 방지를 본 발명의 다른 목적으로 한다.Another object of the present invention is to promote the recycling of waste cooking oil by using recycled soap prepared from waste cooking oil and to prevent environmental pollution by waste cooking oil.

본 발명의 분산성이 향상된 실리카 고무조성물은 공지의 실리카 고무조성물에 있어서, 원료고무로 천연고무, 스티렌 부타디엔 고무, 부타디엔 고무를 각각 사용하거나 또는 이들이 서로 혼합된 혼합고무인 원료고무 100 phr에 대하여 실리카의 분산성을 증가시켜 고무의 점도 개선 및 물성을 향상시키기 위해 분산제를 3∼12 phr 포함하는 것을 특징으로 한다.The silica rubber composition having improved dispersibility according to the present invention is a silica rubber composition in which known silica rubber compositions use natural rubber, styrene butadiene rubber, butadiene rubber as raw material rubbers, or 100 rubbers of raw rubbers which are mixed rubbers mixed with each other. It is characterized in that it comprises 3 to 12 phr dispersant to increase the dispersibility to improve the viscosity and physical properties of the rubber.

본 발명에서 사용하는 분산제는 폐식용유를 원료로 하여 제조된 재생비누를 사용하는데 이러한 분산제를 원료고무 100 phr에 대하여 3 phr 미만 사용하면 분산제의 역할을 충분히 하지 못하는 문제가 있고, 12 phr 초과 사용하면 과량의 분산제의 첨가로 인하여 고무의 점도의 하락등으로 인한 마모성능에 문제를 야기하는데 특히 충진제로 실리카를 사용하여 타이어의 트레드에 적용하는 경우 마모성능이 중요하기 때문에 분산제의 사용량은 원료고무 100 phr에 대하여 3∼12 phr 유지하는 것이 좋다.The dispersant used in the present invention uses recycled soap prepared using waste cooking oil as a raw material. If the dispersant is used in an amount of less than 3 phr with respect to 100 phr of raw rubber, the dispersant does not have a sufficient role as a dispersant. The addition of excess dispersant causes problems in wear performance due to the decrease in the viscosity of the rubber. Especially, when the silica is used as a filler and applied to tire treads, the amount of dispersant used is 100 phr. 3 to 12 phr is recommended.

한편 본 발명에서 분산제로 사용하는 재생비누는 폐식용유를 원료로 하여 제조한 것으로서 달리 일정한 제조방법에 의해 제조된 것이 아니라 공지의 방법을 이용하여 제조된 것이다.Meanwhile, the recycled soap used as a dispersant in the present invention is manufactured by using waste cooking oil as a raw material, and is manufactured by a known method rather than by a predetermined manufacturing method.

이하 본 발명을 다음의 비교예, 실시예 및 시험예에 의하여 설명하고자 한다. 그러나 이들이 본 발명을 기술적 범위를 한정하는 것은 아니다.Hereinafter, the present invention will be described by the following comparative examples, examples and test examples. However, these do not limit the technical scope of the present invention.

<비교예 1>Comparative Example 1

아래의 표 1과 같이 스티렌-부타디엔 고무 80 phr 및 부타디엔 고무 20 phr로 구성된 원료고무 100 phr에 대하여 공지의 실리카 고무조성물의 첨가제로 사용하는 실리카 70 phr, 커플링제 12 phr, 활성제 5 phr, 황 1.5 phr, 가류촉진제 3.0 phr 및 분산제로 사용하는 분산조제 3 phr을 반버리 믹서에 넣고 혼합하여 160℃에서 15분 동안 가류하여 고무시편을 제조하였다.70 phr of silica, 12 phr of coupling agent, 5 phr of activator, sulfur 1.5, as an additive of a known silica rubber composition for 100 phr of a raw rubber composed of 80 phr of styrene-butadiene rubber and 20 phr of butadiene rubber as shown in Table 1 below. phr, 3.0 phr of vulcanization accelerator, and 3 phr of a dispersing aid used as a dispersant were put in a Banbury mixer, mixed, and vulcanized at 160 ° C. for 15 minutes to prepare a rubber specimen.

<비교예 2>Comparative Example 2

상기에서 분산제로 공정오일 10 phr 사용하는 것을 제외하고는 상기 비교예 1과 같은 조성물, 조성비 및 방법을 이용하여 고무시편을 제조하였다.A rubber specimen was prepared using the same composition, composition ratio, and method as in Comparative Example 1, except that 10 phr of process oil was used as a dispersant.

<실시예 1><Example 1>

아래의 표 1과 같이 스티렌-부타디엔 고무 80 phr 및 부타디엔 고무 20 phr로 구성된 원료고무 100 phr에 대하여 공지의 실리카 고무조성물의 첨가제로 사용하는 실리카 70 phr, 커플링제 12 phr, 활성제 5 phr, 황 1.5 phr, 가류촉진제 3.0 phr 및 분산제로 폐식용유를 원료로 제조된 재생비누 3 phr을 반버리 믹서에 넣고 혼합하여 160℃에서 15분 동안 가류하여 고무시편을 제조하였다.70 phr of silica, 12 phr of coupling agent, 5 phr of activator, sulfur 1.5, as an additive of a known silica rubber composition for 100 phr of a raw rubber composed of 80 phr of styrene-butadiene rubber and 20 phr of butadiene rubber as shown in Table 1 below. phr, 3.0 phr of vulcanization accelerator, and 3 phr of recycled soap prepared as a raw material of waste cooking oil as a dispersant were added to a Banbury mixer, mixed, and vulcanized at 160 ° C. for 15 minutes to prepare a rubber specimen.

<실시예 2><Example 2>

분산제로 폐식유로 제조된 재생비누 6 phr 사용하는 것을 제외하고는 상기 실시예 1과 같은 조성물, 조성비 및 방법을 이용하여 고무시편을 제조하였다.A rubber specimen was prepared using the same composition, composition ratio, and method as in Example 1, except that 6 phr of recycled soap prepared from waste oil was used as a dispersant.

<실시예 3><Example 3>

분산제로 폐식유로 제조된 재생비누 9 phr 사용하는 것을 제외하고는 상기 실시예 1과 같은 조성물, 조성비 및 방법을 이용하여 고무시편을 제조하였다.A rubber specimen was prepared using the same composition, composition ratio, and method as in Example 1, except that 9 phr of recycled soap prepared from waste oil was used as a dispersant.

표 1. 비교예 및 실시예의 고무조성물(단위 : phr)Table 1. Rubber Compositions of Comparative Examples and Examples (Unit: phr)

항목Item 비교예 1Comparative Example 1 비교예 2Comparative Example 2 실시예 1Example 1 실시예 2Example 2 실시예 3Example 3 S-SBRS-SBR 110110 110110 110110 110110 110110 BRBR 2020 2020 2020 2020 2020 실리카Silica 7070 7070 7070 7070 7070 커플링제Coupling agent 1212 1212 1212 1212 1212 활성제Active agent 55 55 55 55 55 분산조제Dispersion Preparation 33 -- -- -- -- 공정오일Process oil -- 1010 -- -- -- 재생비누Recycled Soap -- -- 33 66 99 황sulfur 1.51.5 1.51.5 1.51.5 1.51.5 1.51.5 가류촉진제Vulcanization accelerator 3.03.0 3.03.0 3.03.0 3.03.0 3.03.0

<시험예><Test Example>

상기 비교예 및 실시예의 고무시편을 ASTM 관련규정에 의하여 레오미터, 인장물성, 무니점도, 동적특성 및 마모특성을 측정하여 그 결과를 아래의 표 2에 정리하여 나타내었다.The rubber specimens of Comparative Examples and Examples were measured by rheometer, tensile properties, Mooney viscosity, dynamic properties, and wear characteristics according to ASTM-related regulations, and the results are summarized in Table 2 below.

표 2. 비교예 및 실시예 시편의 물성측정 결과Table 2. Results of Measurement of Physical Properties of Comparative Examples and Examples

항목Item 비교예 1Comparative Example 1 비교예 2Comparative Example 2 실시예 1Example 1 실시예 2Example 2 실시예 3Example 3 레오미터Rheometer T40T40 8.38.3 7.97.9 8.58.5 8.28.2 7.67.6 T90T90 13.013.0 16.716.7 13.713.7 11.911.9 11.211.2 최대토크Torque 43.143.1 44.644.6 44.344.3 42.142.1 37.937.9 인장물성Tensile Properties 경도Hardness 7070 7070 7171 7070 6969 300%모듈러스300% modulus 125125 132132 123123 114114 100100 인장강도The tensile strength 183183 179179 173173 195195 186186 신장율Elongation 435435 420420 385385 508508 526526 무니점도Mooney viscosity 점도Viscosity 8080 8585 8282 7171 6363 스코치 시간Scotch time 41.941.9 35.935.9 41.641.6 42.242.2 39.439.4 동적특성Dynamic characteristics Tan δ(0℃)Tan δ (0 ℃) 0.2120.212 0.2210.221 0.2220.222 0.2210.221 0.2170.217 Tan δ(60℃)Tan δ (60 ° C) 0.1000.100 0.1110.111 0.1040.104 0.0990.099 0.0930.093

상기 시험예의 결과인 표 2에서처럼 실리카 고무조성물에 있어서 분산성을 향상시키기 위해 분산제로 폐식용유를 원료로 제조된 재생비누를 사용한 본 발명의 실리카 고무조성물인 실시예 고무시편은 종래의 고무조성물인 비교예 고무시편에 비해 점도의 개선 및 인장물성이 동등 또는 향상되었음을 알 수 있다.As shown in Table 2, which is the result of the test example, the silica rubber composition of the present invention using recycled soap prepared from waste vegetable oil as a dispersant to improve dispersibility in the silica rubber composition is compared with a conventional rubber composition. Example It can be seen that the viscosity and tensile properties are equal or improved compared to the rubber specimens.

한편 현재의 분산제는 고가이어서 폐식용유로 만든 재생비누를 분산제로 사용시 분산제의 비용을 절감할 수 있으며 또한 환경문제를 야기할 수 있는 폐식용유의 처리에도 효과적이다.On the other hand, the current dispersant is expensive and can reduce the cost of the dispersant when using recycled soap made of waste cooking oil as a dispersant and is also effective in the treatment of waste cooking oil that can cause environmental problems.

Claims (3)

공지의 실리카 고무조성물에 있어서,In known silica rubber compositions, 원료고무 100 phr에 대하여 분산제로서 폐식용유를 원료로 제조된 재생비누 3∼12 phr 포함하는 것을 특징으로 하는 분산성이 향상된 실리카 고무조성물.A silica rubber composition with improved dispersibility, comprising from 3 to 12 phr of recycled soap made from waste vegetable oil as a dispersant based on 100 phr of raw rubber. 제 1항에 있어서, 원료고무는 천연고무, 스티렌 부타디엔 고무, 부타디엔 고무를 각각 사용하거나 또는 이들이 서로 혼합된 혼합고무임을 특징으로 하는 분산성이 향상된 실리카 고무조성물The silica rubber composition according to claim 1, wherein the raw material rubber is natural rubber, styrene butadiene rubber, butadiene rubber or mixed rubber mixed with each other. 삭제delete
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