KR20030031368A - Silica rubber compound containing polyethylene glycol - Google Patents
Silica rubber compound containing polyethylene glycol Download PDFInfo
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- KR20030031368A KR20030031368A KR1020010063462A KR20010063462A KR20030031368A KR 20030031368 A KR20030031368 A KR 20030031368A KR 1020010063462 A KR1020010063462 A KR 1020010063462A KR 20010063462 A KR20010063462 A KR 20010063462A KR 20030031368 A KR20030031368 A KR 20030031368A
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- C—CHEMISTRY; METALLURGY
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L7/00—Compositions of natural rubber
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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
- C08K3/34—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
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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
- C08L71/00—Compositions of polyethers obtained by reactions forming an ether link in the main chain; Compositions of derivatives of such polymers
- C08L71/02—Polyalkylene oxides
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- C08L2207/00—Properties characterising the ingredient of the composition
- C08L2207/32—Properties characterising the ingredient of the composition containing low molecular weight liquid component
- C08L2207/324—Liquid component is low molecular weight polymer
Abstract
Description
본 발명은 폴리에틸렌글리콜을 함유하는 실리카 고무조성물로서, 보다 상세하게는 실리카를 보강재로 사용하는 고무조성물의 가공성 및 물성을 향상시키기 위하여 폴리에틸렌글리콜(polyethylene glycol)를 사용하는 실리카 고무조성물에 관한 것이다.The present invention relates to a silica rubber composition containing polyethylene glycol, and more particularly, to a silica rubber composition using polyethylene glycol in order to improve processability and physical properties of a rubber composition using silica as a reinforcing material.
실리카(silica)는 카본블랙(carbon black)에 비하여 다공성(porosity)이고 표면의 강한 극성 및 친수성에 기인한 촉진제의 흡착으로 촉진제의 손실을 야기시키고, 비극성계인 고무와 친화성이 떨어지며 상호작용이 감소하고 실리카간의 응집성이 강해지는 등과 같은 특성 때문에, 분산성이 나빠지고 점도의 증가 및 가교속도의 저하에 의해 가공성이 떨어지게 된다.Silica is more porous than carbon black, and due to adsorption of accelerator due to the strong polarity and hydrophilicity of the surface, it causes loss of accelerator, incompatibility with nonpolar rubber and reduced interaction. Due to such properties as the cohesiveness between silicas becomes stronger, dispersibility becomes poor, and workability is inferior due to an increase in viscosity and a decrease in crosslinking rate.
또한, 실리카는 가황촉진제의 효율이 떨어짐에 따라 과량의 촉진제가 필요하게 되며, 물성에도 영향을 미치게 되는데, 이러한 현상을 방지하기 위하여 실리카와 고무간의 결합력 강화 및 고무 매트릭스내 실리카의 분산성을 향상시킴과 동시에 표면으로 가황촉진제가 조기흡착되는 것을 억제시키는 것이 중요하다.In addition, as silica is less efficient in vulcanization accelerators, an excessive amount of accelerator is required, which affects physical properties. In order to prevent this phenomenon, the silica enhances the bonding strength between silica and rubber and improves the dispersibility of silica in the rubber matrix. At the same time, it is important to suppress premature adsorption of the vulcanization accelerator to the surface.
가황촉진제의 조기흡착 억제방법으로 실리카 표면의 개질 및 친수성을 갖는 첨가제를 사용하는 방법이 있는데, 오일(oil), 아연(Zn), 마그네슘(Mg)계 조성물 (compound), 트레타놀아민(trethanolamine) 또는 폴리에틸렌글리콜(PEG)과 같은 친수성을 갖는 첨가제를 사용함에 따라 고무배합물의 가공성 및 물성이 향상된다고 알려져 있다.As a method of inhibiting premature adsorption of the vulcanization accelerator, there is a method of using an additive having a surface modification and hydrophilicity of silica, and an oil, zinc (Zn), magnesium (Mg) -based composition (compound), and tretanolamine It is known that the processability and physical properties of the rubber compound are improved by using an additive having hydrophilicity such as polyethylene glycol (PEG).
본 발명자들은 상기와 같은 종래 실리카 고무조성물이 지니는 문제에 대한 해결방안을 연구하여 오던 중에 적절한 분자량을 갖는 폴리에틸렌글리콜의 함량을 조절함으로써 이와 같은 문제를 해결할 수 있음을 알아내고 본 발명을 완성하였다.The present inventors have completed the present invention by studying a solution to the problems of the conventional silica rubber composition as described above, by adjusting the content of polyethylene glycol having an appropriate molecular weight.
따라서 본 발명의 목적은 폴리에틸렌글리콜을 함유하여 고무조성물의 가공성 및 물성이 향상된 실리카 고무조성물을 제공함에 있다.Accordingly, an object of the present invention is to provide a silica rubber composition containing polyethylene glycol improved processability and physical properties of the rubber composition.
본 발명은 공지의 첨가제를 포함하는 실리카 고무조성물에 있어서, 천연고무 100 중량부에 대하여 폴리에틸렌글리콜 2-3 중량부를 포함하는 폴리에틸렌글리콜을 함유하는 실리카 고무조성물임을 특징으로 한다.The present invention is a silica rubber composition comprising a known additive, characterized in that the silica rubber composition containing polyethylene glycol containing 2-3 parts by weight of polyethylene glycol with respect to 100 parts by weight of natural rubber.
폴리에틸렌글리콜의 분자량에 따른 물성의 변화는 고무조성물내 폴리에틸렌글리콜 사슬의 유동성 및 말단에 존재하는 수산화기(-OH)에 의해 발생하는데, 본발명에 사용되는 폴리에틸렌글리콜은 분자량이 4,500-9,000인 것이 바람직하다.The change in physical properties according to the molecular weight of polyethylene glycol is caused by the flowability of the polyethylene glycol chain in the rubber composition and the hydroxyl group (-OH) present at the terminal. The polyethylene glycol used in the present invention preferably has a molecular weight of 4,500-9,000. .
폴리에틸렌글리콜은 실리카의 표면에 존재하는 실라놀기(silanol group)와 비극성인 고무와의 친화성을 증가시키며, 촉진제의 흡착을 방지하여 배합물의 가교시간, 점도, 압축율(compression set) 등을 감소시키고, 열적 특성(heat buildup)을 좋게 하며 각종 물성을 향상시키는 기능을 한다.Polyethyleneglycol increases the affinity of silanol groups on the surface of silica with nonpolar rubbers and prevents adsorption of accelerators, reducing crosslinking time, viscosity, compression set, etc. of the formulation, It improves heat buildup and improves various physical properties.
본 발명에 사용되는 폴리에틸렌글리콜은 천연고무 100 중량부에 대하여 2-3 중량부를 포함하는 것이 바람직한데, 그 이유는 2 중량부 이하를 포함하는 경우 가황촉진제의 흡착억제가 부족하고, 3중량부 이상을 포함하는 경우 고무화합물의 노화물성이 하락하기 때문이다.The polyethylene glycol used in the present invention preferably contains 2-3 parts by weight with respect to 100 parts by weight of natural rubber, because when it contains 2 parts by weight or less, the adsorption inhibition of the vulcanization accelerator is insufficient, 3 parts by weight or more It is because the sinterability of the rubber compound is reduced if it contains.
본 발명에 의한 실리카 고무조성물은 보강재로 실리카 70-90 중량부, 실란 커플링제 6-7 중량부를 포함하며, 기타 성분 예를 들면, 산화아연, 스테아린산, 왁스, 노화방지제, 유황, 가황촉진제 등은 공지의 실리카 고무조성물의 첨가제들로서 이들 각각은 이미 알려진 첨가량의 범위에 따라 적의 선택하여 실시하는 것으로 충분하므로 이들에 관한 상세한 설명은 생략한다.The silica rubber composition according to the present invention contains 70-90 parts by weight of silica and 6-7 parts by weight of a silane coupling agent as reinforcing materials, and other components such as zinc oxide, stearic acid, wax, antioxidant, sulfur, vulcanization accelerator, etc. As the additives of known silica rubber compositions, each of them is sufficient to be appropriately carried out according to a known range of addition amount, so detailed description thereof is omitted.
이하 본 발명의 내용을 실시예를 통해 구체적으로 설명하도록 한다. 그러나 다음의 실시예는 본 발명을 보다 상세하게 설명하기 위한 것으로, 본 발명의 권리 범위를 이에 한정하고자 하는 것은 아니다.Hereinafter, the contents of the present invention will be described in detail through examples. However, the following examples are intended to illustrate the present invention in more detail, and are not intended to limit the scope of the invention.
<실시예 1><Example 1>
하기 표 1에 개시된 배합비와 같이 원료고무로 천연고무(SMR CV60) 100 중량부에 대하여 분자량이 4,660 이고 수평균 분자량(number average molecular mass, Mn)이 1,350인 폴리에틸렌글리콜(PEG B) 2 중량부, 실리카(Z-175) 80 중량부, 커플링제(Si-69) 6.4 중량부, 산화아연 5 중량부, 스테아린산 3 중량부, 왁스 2 중량부, 노화방지제(6PPD) 2 중량부, 유황 2.5 중량부, 가황촉진제(BBS) 0.8 중량부, 디페닐구아니딘(DPG) 1중량부를 첨가하여 밴버리믹서에 배합하고 125℃의 온도에서 방출시켜 실리카 고무조성물을 제조하였다.2 parts by weight of polyethylene glycol (PEG B) having a molecular weight of 4,660 and a number average molecular mass (Mn) of 1,350, based on 100 parts by weight of natural rubber (SMR CV60) as a blending ratio disclosed in Table 1, 80 parts by weight of silica (Z-175), 6.4 parts by weight of coupling agent (Si-69), 5 parts by weight of zinc oxide, 3 parts by weight of stearic acid, 2 parts by weight of wax, 2 parts by weight of antioxidant (6PPD), 2.5 parts by weight of sulfur , 0.8 parts by weight of a vulcanization accelerator (BBS), 1 part by weight of diphenylguanidine (DPG) was added to the Banbury mixer, and released at a temperature of 125 ° C. to prepare a silica rubber composition.
<실시예 2><Example 2>
분자량이 9,470 이고 수평균 분자량이 8,600 인 폴리에틸렌글리콜(PEG C)을 2 중량부로 구성하는 하는 것 이외에는 실시예 1과 동일하게 실시하여 실리카 고무조성물을 제조하였다.A silica rubber composition was prepared in the same manner as in Example 1 except that polyethylene glycol (PEG C) having a molecular weight of 9,470 and a number average molecular weight of 8,600 was composed of 2 parts by weight.
<실시예 3><Example 3>
PEG B를 3 중량부로 구성하는 하는 것 이외에는 실시예 1과 동일하게 실시하여 실리카 고무조성물을 제조하였다.A silica rubber composition was prepared in the same manner as in Example 1 except that PEG B was composed of 3 parts by weight.
<실시예 4><Example 4>
PEG B를 1 중량부로 구성하는 하는 것 이외에는 실시예 1과 동일하게 실시하여 실리카 고무조성물을 제조하였다.A silica rubber composition was prepared in the same manner as in Example 1 except that PEG B was included in 1 part by weight.
<비교예 1>Comparative Example 1
분자량이 1,410 이고 수평균 분자량이 1,350인 폴리에틸렌글리콜(PEG A)을 2 중량부로 구성하는 하는 것 이외에는 실시예 1과 동일하게 실시하여 실리카 고무조성물을 제조하였다.A silica rubber composition was prepared in the same manner as in Example 1 except that polyethylene glycol (PEG A) having a molecular weight of 1,410 and a number average molecular weight of 1,350 was included in 2 parts by weight.
<비교예 2>Comparative Example 2
분자량이 13,800 이고 수평균 분자량이 11,400인 폴리에틸렌글리콜(PEG D)을 2 중량부로 구성하는 하는 것 이외에는 실시예 1과 동일하게 실시하여 실리카 고무조성물을 제조하였다.A silica rubber composition was prepared in the same manner as in Example 1 except that polyethylene glycol (PEG D) having a molecular weight of 13,800 and a number average molecular weight of 11,400 was included in 2 parts by weight.
<비교예 3>Comparative Example 3
PEG를 사용하지 않은 것을 제외하고는 실시예 1과 동일하게 실시하여 실리카 고무조성물을 제조하였다. 아래의 표 1중에 PEG의 함량 괄호안의 부호 A, B, C 및 D는 사용한 PEG의 종류를 의미한다.A silica rubber composition was prepared in the same manner as in Example 1 except that PEG was not used. In Table 1 below, the symbols A, B, C and D in the parentheses of the content of PEG refer to the type of PEG used.
<표 1> 고무배합비 (단위: 중량부)<Table 1> Rubber compounding ratio (unit: parts by weight)
<시험예 1><Test Example 1>
실시예 및 비교예에서 제조한 고무조성물에 첨가된 PEG의 분자량 및 함량의 변화가 가교특성에 미치는 영향을 알아보기 위하여 각 고무조성물의 가류시간 curing time)과 토크(torque)를 측정하였는 바, 그 결과를 표 2에 나타내었다.Curing time curing time and torque of each rubber composition were measured to determine the effect of changes in molecular weight and content of PEG added to the rubber compositions prepared in Examples and Comparative Examples. The results are shown in Table 2.
표 2에서 T2,T40및T90은 각각 2% 가류진행 시간, 40% 가류진행 시간 및 90% 가류진행 시간을 의미하며, MH,ML및MH-ML은 각각 최대토크, 최소토크 및 상대 가교밀도를 의미하는 것으로서, 온도를 가하면 고무의 가교가 진행됨에 따라 힘이 작용하게 되는데 이를 리오미터(rheometer)를 통하여 토크를 측정하는 수치이다.In Table 2, T 2, T 40 and T 90 represent 2% vulcanization time, 40% vulcanization time and 90% vulcanization time, respectively, M H, M L and M H -M L are the maximum torque, It means the minimum torque and the relative crosslinking density. When temperature is added, the force acts as the crosslinking of the rubber proceeds, which is a value for measuring the torque through a rheometer.
<표 2> 가교특성 영향측정 결과<Table 2> Measurement result of crosslinking characteristics
<시험예 2><Test Example 2>
상기 표 1의 배합비에 의해 첨가된 PEG 분자량의 변화에 따른 고무조성물의 점도, 모듈러스, 인장강도 등과 같은 각종 기계적 물성을 ASTM 표준규격에 따라 측정한 결과를 표 3에 나타내었는데, 첨가된 PEG의 함량은 2 중량부 이었다. 이때, 아래 표 3중 괄호 안의 수치는 노화후 (105℃, 24시간)의 물성을 측정한 결과를 나타낸 것이다.Table 3 shows the results of measuring various mechanical properties such as viscosity, modulus, tensile strength, etc. of the rubber composition according to the change in the molecular weight of PEG added by the mixing ratio of Table 1 according to ASTM standard. Was 2 parts by weight. In this case, the numerical values in parentheses in Table 3 below show the results of measuring physical properties after aging (105 ° C., 24 hours).
<표 3> PEG 분자량의 변화에 따른 기계적 물성 측정결과<Table 3> Measurement results of mechanical properties according to changes in PEG molecular weight
<시험예 3><Test Example 3>
상기 표 1의 배합비에 의해 첨가된 PEG의 함량변화에 따른 고무조성물의 점도, 모듈러스, 인장강도 등과 같은 각종 기계적 물성을 ASTM 표준규격에 따라 측정한 결과를 표 4에 나타내었는데, 사용된 폴리에틸렌글리콜은 PEG B이었다. 이때, 아래 표 4중 괄호 안의 수치는 노화후(105℃, 24시간)의 물성을 측정한 결과를 나타낸 것이다.Table 4 shows the results of measuring various mechanical properties such as viscosity, modulus, tensile strength, etc. of the rubber composition according to the content of PEG added by the mixing ratio of Table 1 according to the ASTM standard. PEG B. In this case, the numerical values in parentheses in Table 4 below show the results of measuring physical properties after aging (105 ° C., 24 hours).
<표 4> PEG 함량의 변화에 따른 기계적 물성 측정결과<Table 4> Measurement results of mechanical properties according to changes in PEG content
상기 표 3과 표 4에서 보는 바와 같이, 본 발명에 의한 실리카 고무조성물은 폴리에틸렌글리콜의 분자량 증가에 따라 고무와 실리카의 결합력 감소현상을 볼 수 잇으며, 발열특성은 감소하는 경향을 보이고 있다.As shown in Table 3 and Table 4, the silica rubber composition according to the present invention can be seen to decrease the bonding strength of the rubber and silica as the molecular weight of polyethylene glycol increases, the exothermic characteristics are shown to decrease.
폴리에틸렌글리콜 함량 증가에 따른 영향은 폴리에틸렌글리콜에 의한 보강재표면 극성그룹의 반응성 억제 및 촉진제의 흡착방지에 의해 가교속도가 빨라지며, 점도감소, 기계적 물성 및 가공성이 향상었음을 알 수 있다.The effect of increasing the polyethylene glycol content is that the crosslinking speed is increased by suppressing the reactivity of the polar group of the reinforcing material surface by polyethylene glycol and preventing the adsorption of the accelerator, and it can be seen that the viscosity decrease, the mechanical properties and the processability are improved.
본 발명에 의한 실리카 고무조성물은 보강재로 실리카를 사용한 고무조성물의 가공성 및 기계적 물성을 향상시키기 위하여 폴리에틸렌글리콜의 분자량 및 함량을 달리함으로써 가교특성, 유변학적 특성, 동적 점탄성 특성 뿐만 아니라 기계적 특성 등이 향상되는 효과가 있다.The silica rubber composition according to the present invention improves the crosslinking, rheological and dynamic viscoelastic properties as well as mechanical properties by varying the molecular weight and content of polyethylene glycol in order to improve the processability and mechanical properties of the rubber composition using silica as a reinforcing material. It is effective.
Claims (3)
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Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
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US5703151A (en) * | 1995-04-17 | 1997-12-30 | Sumitomo Chemical Company, Limited | Rubber composition |
JPH11130908A (en) * | 1997-10-29 | 1999-05-18 | Sumitomo Rubber Ind Ltd | Rubber composition |
KR100228870B1 (en) * | 1997-07-09 | 1999-11-01 | 신형인 | Tread rubber composition |
JPH11343366A (en) * | 1998-06-01 | 1999-12-14 | Sumitomo Rubber Ind Ltd | Rubber composition for tire tread |
KR20010081360A (en) * | 2000-02-14 | 2001-08-29 | 신형인 | Rubber compositions containing silica master batch |
KR100321858B1 (en) * | 1999-07-07 | 2002-02-01 | 신형인 | Low Hardness Snow Tread Compound for Ice Road Enhanced Wear Resistant |
KR100388629B1 (en) * | 2000-08-24 | 2003-06-25 | 금호산업주식회사 | rubber composi tion filled silica and rubber compound method thereof |
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2001
- 2001-10-15 KR KR1020010063462A patent/KR20030031368A/en not_active Application Discontinuation
Patent Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5703151A (en) * | 1995-04-17 | 1997-12-30 | Sumitomo Chemical Company, Limited | Rubber composition |
KR100228870B1 (en) * | 1997-07-09 | 1999-11-01 | 신형인 | Tread rubber composition |
JPH11130908A (en) * | 1997-10-29 | 1999-05-18 | Sumitomo Rubber Ind Ltd | Rubber composition |
JPH11343366A (en) * | 1998-06-01 | 1999-12-14 | Sumitomo Rubber Ind Ltd | Rubber composition for tire tread |
KR100321858B1 (en) * | 1999-07-07 | 2002-02-01 | 신형인 | Low Hardness Snow Tread Compound for Ice Road Enhanced Wear Resistant |
KR20010081360A (en) * | 2000-02-14 | 2001-08-29 | 신형인 | Rubber compositions containing silica master batch |
KR100388629B1 (en) * | 2000-08-24 | 2003-06-25 | 금호산업주식회사 | rubber composi tion filled silica and rubber compound method thereof |
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