KR20000034197A - Method for emulsifying styrene-butadiene-styrene block copolymer - Google Patents

Method for emulsifying styrene-butadiene-styrene block copolymer Download PDF

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KR20000034197A
KR20000034197A KR1019980051463A KR19980051463A KR20000034197A KR 20000034197 A KR20000034197 A KR 20000034197A KR 1019980051463 A KR1019980051463 A KR 1019980051463A KR 19980051463 A KR19980051463 A KR 19980051463A KR 20000034197 A KR20000034197 A KR 20000034197A
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styrene
butadiene
block copolymer
weight
parts
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Korean (ko)
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김영상
김홍곤
조교동
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박찬구
금호석유화학 주식회사
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00—Processes of treating or compounding macromolecular substances
    • C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
    • C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
    • C08J3/07—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media from polymer solutions
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2353/00—Characterised by the use of block copolymers containing at least one sequence of a polymer obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers
    • C08J2353/02—Characterised by the use of block copolymers containing at least one sequence of a polymer obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers of vinyl aromatic monomers and conjugated dienes
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L53/00—Compositions of block copolymers containing at least one sequence of a polymer obtained by reactions only involving carbon-to-carbon unsaturated bonds; Compositions of derivatives of such polymers
    • C08L53/02—Compositions of block copolymers containing at least one sequence of a polymer obtained by reactions only involving carbon-to-carbon unsaturated bonds; Compositions of derivatives of such polymers of vinyl-aromatic monomers and conjugated dienes

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  • Chemical & Material Sciences (AREA)
  • Dispersion Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

PURPOSE: A process for emulsifying a styrene-butadiene-styrene block copolymer is provided which is capable of changing to a plant mix type easily. CONSTITUTION: An emulsifying method of a styrene-butadiene-styrene block copolymer comprises dissolving a styrene-butadiene-styrene block copolymer in a non polar solvent, emulsifying by adding 5 to 10 parts by weight of a mixed emulsifying agent consisting to a rosin salt, a salt of fatty acid, and a salt of oleic acid and 80 to 100 parts by weight of water to 100 parts by weight of the solution, removing the non polar solvent through a vacuum apparatus and concentrating. The emulsion can be applied to a plant mix type with ease while improving a rate of deformation and stability when applied to asphalt.

Description

스티렌-부타디엔-스티렌 블럭 공중합체의 수용화 방법Solubility Method of Styrene-Butadiene-Styrene Block Copolymer

본 발명은 스티렌-부타디엔-스티렌 블럭 공중합체(SBS)의 수용화 방법에 관한 것으로서, 더욱 상세하게는 스티렌-부타디엔-스티렌 블럭 공중합체를 프랜트 믹스 타입의 아스팔트 개질제로 적용하기 위해 혼합 유화제를 사용하여 수용화하는 방법에 관한 것이다.The present invention relates to a solubilization method of styrene-butadiene-styrene block copolymer (SBS), and more particularly, using a mixed emulsifier to apply the styrene-butadiene-styrene block copolymer as a plant mix type asphalt modifier. It is about a method of receiving.

아스팔트 개질제는 그 첨가의 시점에 따라 프리믹스 타입(pre-mix type)과 프랜트 믹스 타입(plant-mix type)으로 구분 할 수 있다.Asphalt modifiers can be divided into pre-mix type and plant-mix type according to the time of addition.

프리믹스 타입은 아스팔트에 사용되는 개질제를 녹여 개질아스팔트 제품으로 생산하는 방법으로서, 대량의 개질 아스콘 생산시 적용이 용이하다. 그러나, 소량 및 일반 아스콘과 번갈아 생산하고자 할 경우에는 변환이 용이하지 못한 문제점이 있다.The premix type is a method of melting the modifier used in asphalt to produce modified asphalt products, and is easy to apply when producing a large amount of modified asphalt. However, there is a problem that the conversion is not easy if you want to produce alternately with a small amount and ordinary ascon.

반면에 프랜트 믹스 타입은 아스콘에 개질제를 직접 투입함으로써 개질제의 첨가 유무에 따라 아스콘 타입을 변화시키기 용이한 장점을 갖는다.On the other hand, the plant mix type has an advantage of easily changing the ascon type depending on the presence or absence of the modifier by directly adding the modifier to the ascon.

그런데, 스티렌-부타디엔-스티렌 블럭 공중합체를 상기와 같은 장점을 갖는 프랜트 믹스 타입의 아스팔트 개질제로 사용하기 위해서는 아스콘에 개질제를 직접 투입하여야 하므로 수용화하여야 한다.However, in order to use the styrene-butadiene-styrene block copolymer as a plant mix type asphalt modifier having the above-described advantages, the modifier must be directly added to ascon, so that it must be solubilized.

본 발명의 목적은 아스팔트 개질제로 사용되는 스티렌-부타디엔-스티렌 블럭 공중합체를 효과적으로 수용화하여 프랜트 믹스 타입으로 적용할 수 있도록 하는 방법을 제공하는 데 있다.It is an object of the present invention to provide a method for effectively accepting styrene-butadiene-styrene block copolymers used as asphalt modifiers so that they can be applied as a plant mix type.

이와 같은 목적을 달성하기 위한 본 발명의 스티렌-부타디엔-스티렌 블럭 공중합체를 수용화시키는 방법은 스티렌-부타디엔-스티렌 블럭 공중합체를 비극성 용매에 10∼15% 되도록 용해시키는 단계, 상기 용액 100중량부를 혼합 유화제 5∼10중량부 및 물 80∼100 중량부로 이루어진 유화액을 사용하여 유화시키는 단계, 및 진공장치를 이용하여 비극성 용매를 제거·농축하여 에멀젼으로 제조하는 단계를 포함한다.In order to achieve the above object, the styrene-butadiene-styrene block copolymer of the present invention has a method of solubilizing the styrene-butadiene-styrene block copolymer in a nonpolar solvent so that 10 to 15%, by mixing 100 parts by weight of the solution Emulsifying using an emulsion comprising 5 to 10 parts by weight of an emulsifier and 80 to 100 parts by weight of water, and removing and concentrating the nonpolar solvent using a vacuum apparatus to prepare an emulsion.

이와같은 발명을 더욱 상세하게 설명하면 다음과 같다.The invention is described in more detail as follows.

본 발명에서 사용되는 스티렌-부타디엔-스티렌 블럭 공중합체는 당사에서 생산되는 제품으로, 그 형태는 펠렛 또는 파우더이며, 스티렌 함량 31%이고, 용액점도 15000cps, 비중 0.94g/㎤, 인장강도 160kgf/㎠, 300% 인장응력 28kgf/㎠이고, 신장율은 680%인 것을 사용한다.Styrene-butadiene-styrene block copolymer used in the present invention is a product produced by the company, the form is pellet or powder, styrene content 31%, solution viscosity 15000cps, specific gravity 0.94g / cm 3, tensile strength 160kgf / ㎠ , 300% tensile stress is 28kgf / ㎠, elongation is used 680%.

이같은 스티렌-부타디엔-스티렌 블럭 공중합체를 프랜트 믹스 타입의 아스팔트 개질제로 적용하기 위해서 우선 이를 비극성 용매에 용해시킨다. 이때 10∼15% 농도가 되도록 용해시키는 것이 바람직하다.To apply this styrene-butadiene-styrene block copolymer as a plant mix type asphalt modifier, it is first dissolved in a nonpolar solvent. At this time, it is preferable to dissolve so that it may become 10 to 15% concentration.

여기서, 비극성 용매로는 n-헥산, 사이클로헥산, 헵탄 및 옥탄 중에서 선택된 것을 사용할 수 있으며, 이중 가장 바람직하기로는 n-헥산을 사용하는 것이다.Here, as the nonpolar solvent, one selected from n-hexane, cyclohexane, heptane and octane may be used, and most preferably n-hexane is used.

만일, 비극성 용매에 공중합체를 10% 농도 미만되도록 용해시키면 비극성 용매 제거시 과다한 시간이 필요하게 되고 이에 따라 제조비용이 상승되는 문제가 발생될 수 있고, 15% 농도보다 진하게 용해시키는 경우에는 점도가 높아 유화하기 어려운 문제가 발생될 수 있다.If the copolymer is dissolved in a nonpolar solvent so that the concentration is less than 10%, excessive time is required when removing the nonpolar solvent, which may cause a problem that the manufacturing cost is increased. Problems that are difficult to emulsify may occur.

그 다음, 비극성 용매에 스티렌-부타디엔-스티렌 블럭 공중합체가 용해된 액 100 중량부를 혼합 유화제 5∼10중량부와 물 80∼100중량부로 이루어진 유화액에 유화시키는 바, 이때 혼합 유화제로는 로진염, 페티염 및 올레인염의 혼합물을 사용한다.Next, 100 parts by weight of the styrene-butadiene-styrene block copolymer dissolved in a nonpolar solvent is emulsified in an emulsion composed of 5 to 10 parts by weight of a mixed emulsifier and 80 to 100 parts by weight of water. Mixtures of petti and oleine salts are used.

혼합 유화제 5∼10 중량부는 로진염 0.5∼5.0중량부, 페티염 0.1∼3.0중량부, 및 올레인염 0.1∼3.0 중량부로 이루어진다.5-10 weight part of mixed emulsifiers consists of 0.5-5.0 weight part of rosin salts, 0.1-3.0 weight part of petti salts, and 0.1-3.0 weight part of oleine salts.

여기서, 각각의 염의 혼합비가 상기 범위를 벗어나면 유화제 에멀젼의 안정성이 불량하여 저장안정성이 우수한 제품을 얻을 수 없다.Here, when the mixing ratio of each salt is out of the above range, the stability of the emulsifier emulsion is poor and a product having excellent storage stability cannot be obtained.

유화제는 KOH를 사용하여 검화시킨 것을 사용한다.An emulsifier uses what was saponified using KOH.

이같은 혼합유화제를 이용하여 비극성 용매에 용해된 공중합체를 유화시킨 다음, 진공장치를 이용하여 사용된 비극성 용매를 제거하고, 이를 농축하여 수용화된 스티렌-부타디엔-스티렌 블럭 공중합체를 얻을 수 있다.Such a mixed emulsifier can be used to emulsify the copolymer dissolved in the nonpolar solvent, and then use a vacuum apparatus to remove the used nonpolar solvent, and concentrate it to obtain a styrene-butadiene-styrene block copolymer.

이때, 진공장치는 교반장치가 부착된 것을 사용할 수 있으며 농축은 50∼53% 되도록 하는 것이 바람직하다.At this time, the vacuum device can be used that is attached to the stirring device, the concentration is preferably 50 to 53%.

얻어진 수용화된 스티렌-부타디엔-스티렌 블럭 공중합체는 종래의 스티렌-부타디엔-스티렌 블럭 공중합체가 프리믹스 타입으로 적용되던 것을 개선하여 프랜트 믹스 타입으로 적용할 수 있으므로 아스콘의 타입 변형이 용이한 효과를 얻을 수 있다.The obtained styrene-butadiene-styrene block copolymer obtained by improving the conventional styrene-butadiene-styrene block copolymer applied to the premix type can be applied as a plant mix type, so that the effect of the type conversion of ascone can be easily obtained. Can be.

상기와 같은 방법을 통해 수용화된 스티렌-부타디엔-스티렌 블럭 공중합체의 성상은 다음 표 1과 같다.The properties of the styrene-butadiene-styrene block copolymers solvated through the above method are shown in Table 1 below.

고형분 함량(%)Solid content (%) 50.250.2 pHpH 10.510.5 입자경(Å)Particle diameter 15201520 점도(cps)Viscosity (cps) 420420

이같은 수용화된 스티렌-부타디엔-스티렌 블럭 공중합체를 아스팔트 개질제로 혼합한 개질아스팔트와 첨가하지 않은 스트레이트 아스팔트의 성상을 비교하여 그 결과를 다음 표 2에 나타내었다. 여기서, 개질제의 첨가량은 고형분 기준으로 5%이다.The results of comparing the properties of the modified asphalt mixed with such styrene-butadiene-styrene block copolymers with the asphalt modifier and the non-added straight asphalt were shown in Table 2 below. Here, the amount of the modifier added is 5% based on the solid content.

스트레이트 아스팔트Straight asphalt 개질 아스팔트Modified asphalt 침입도(1/10mm)Breakthrough (1 / 10mm) 6969 5757 연화점(℃)Softening point (℃) 4848 5959 60℃ 점도(poise)60 ° C viscosity 13001300 74007400

상기 표 1과 같은 기본물성을 갖는 아스팔트 개질용 에멀젼으로 개질 아스콘을 제조하여 소성변형 발생을 측정하는 휠 트랙킹 시험을 실시하였으며, 그 결과는 다음 표 4에 나타내었다.A wheel tracking test was performed to prepare a modified ascon as an emulsion for modifying asphalt having basic properties as shown in Table 1, and to measure the occurrence of plastic deformation, and the results are shown in Table 4 below.

휠 트랙킹 시험에 사용한 아스팔트는 표 3에 나타낸 바와 같은 품질을 갖는 AP-3를 사용하였으며, 아스콘 제조에 사용되는 골재 크기의 비는 다음 표 3과 같다.Asphalt used for the wheel tracking test was used AP-3 having the quality as shown in Table 3, the ratio of the aggregate size used in the manufacture of ascone is shown in Table 3.

또한, 소성변형을 억제하는 개질아스콘을 제조하는데 사용되는 아스팔트(AP-3), 혼합골재 및 개질제의 사용량은 다음 표 3과 같다.In addition, the amount of asphalt (AP-3), mixed aggregate, and modifier used to prepare modified ascon to suppress plastic deformation is shown in Table 3 below.

휠 트랙킹 시험은 영국 도로 및 교통연구소(Transporation Road Research Laboratory : TRRL)에서 고안한 대규모의 실규격 포장 시험 장치를 사용하였으며, 시험시 시편 표면에 접지압 7.0Kg/cm2을 가하여 실시하며, 단위시간 동안 바퀴 자국에 의한 패임깊이를 측정하여 결정하는 것으로 소성변형을 간접 평가 할 수 있는 가장 우수한 시험 방법으로 KS M 2250에 준하여 실시하였다.The wheel tracking test was carried out using a large scale pavement test apparatus devised by the UK's Transporation Road Research Laboratory (TRRL) .The test was performed by applying a ground pressure of 7.0Kg / cm2 to the specimen surface. The best test method for indirect evaluation of plastic deformation by measuring and determining the depth of cut due to the marks was carried out in accordance with KS M 2250.

변형량의 산출방법은 최초의 중심부를 통과할 때의 라이얼 게이지의 눈금을 원점으로 하며, 이 때 변형량은 시험륜의 주행범위 중앙에서 측정하였다.The method of calculating the deformation amount is the origin of the scale of the radial gauge when passing through the initial center, and the deformation amount was measured at the center of the driving range of the test wheel.

휠 트랙킹 시험 결과는 변형량(침하량)-시간 관계 곡선에서 변형량 증가율이 거의 일정하게 되는 45분에서 60분까지의 15분간 주행의 변형량을 취하여 이것을 변형율(RD, Rate of Deformation, mm/min.)로 나타낸다.The result of the wheel tracking test is to take the deformation amount of 15 minutes running from 45 minutes to 60 minutes when the deformation increase rate becomes almost constant in the deformation (settling) -time relationship curve, and this is referred to as the rate of deformation (mm / min.) Indicates.

시험시편 제작방법은 혼합 골재 100중량부를 200℃까지 가열한 다음 150℃로 가열된 아스팔트 5.79중량부를 혼합 골재에 부어 넣고 균일하게 혼합한 다음 개질제(고형분 기준)를 0.21중량부 첨가하여 균일하게 혼합하였다.The test specimen manufacturing method was heated 100 parts by weight of mixed aggregate to 200 ℃, and then poured into the mixing aggregate 5.79 parts by weight of asphalt heated to 150 ℃ was mixed uniformly and then mixed uniformly by adding 0.21 parts by weight of modifier (based on solids). .

이 혼합물(개질 아스콘)을 300mm 정사각형에 두께 50mm몰드에 부어 넣은 후 로울러 콤팩터로 다진다. 이때 다짐 하중은 900Kg으로 한다.The mixture (modified ascon) is poured into a 300 mm square into a 50 mm thick mold and compacted with a roller compactor. At this time, the compaction load is 900Kg.

아스팔트 품질Asphalt quality 비중(25℃)연화점(℃)침입도(25℃, 100g, 5초, 1/10mm)인화점(℃)신도(25℃, 5cm/min, cm)점도(60℃, POISE)박막가열 후 침입도비(%)박막가열 후 신도(25℃, 5cm/min, cm)트리클로로에탄 가용분(%)Specific gravity (25 ℃) Softening point (℃) Penetration degree (25 ℃, 100g, 5 seconds, 1 / 10mm) Flash point (℃) Elongation (25 ℃, 5cm / min, cm) Viscosity (60 ℃, POISE) After thin film heating Elongation (25 ℃, 5cm / min, cm) Trichloroethane soluble content after thin film heating (%) 1.03244.095338100 이상54068.475 이상99.721.03244.095338 100 or more54068.475 or more99.72 골재크기의 비(%)% Of aggregate size 19∼13mm13∼5mm5∼0mm모래석분19 to 13 mm 13 to 5 mm 5 to 0 mm sand powder 3024366430243664 아스팔트, 혼합골재 및 개질제의 사용량(중량부)Asphalt, Mixed Aggregate and Modifier Usage (parts by weight) 혼합골재아스팔트(AP-3)개질제Mixed Aggregate Asphalt (AP-3) Modifier 945.790.21945.790.21

스트레이트 아스팔트Straight asphalt 개질 아스팔트Modified asphalt 변형율(mm/분)Strain rate (mm / min) 0.11760.1176 0.02430.0243 동적안정도(회/mm)Dynamic Stability (times / mm) 372372 16701670

상기 표 4의 결과로부터 본 발명에 따른 아스팔트 개질제 에멀젼을 골재상에 도포된 아스팔트 위에 분사한 결과 아스팔트의 소성 변형율이 상당부분 줄어들고, 안정도도 향상됨을 알 수 있다.As a result of spraying the asphalt modifier emulsion according to the present invention on the asphalt coated on the aggregate from the results of Table 4, it can be seen that the plastic strain of the asphalt is substantially reduced, and the stability is also improved.

이상에서 상세히 설명한 바와 같이 , 본 발명에 따른 스티렌-부타디엔-스티렌 블럭 공중합체를 수용화하는 방법에 따라 얻어진 에멀젼을 아스팔트에 적용한 결과 변형율 및 안정도를 향상 시킬수 있을 뿐만 아니라 프랜트 믹스 타입으로 적용이 가능하므로 아스콘 프랜트에서 아스콘의 타입의 변형을 용이하게 할 수 있는 효과 등이 있다.As described in detail above, as a result of applying the emulsion obtained according to the method of solubilizing the styrene-butadiene-styrene block copolymer according to the present invention to asphalt, it is possible to improve strain and stability as well as to apply as a plant mix type. There is an effect that can facilitate the modification of the type of ascon in the ascon plant.

Claims (3)

스티렌-부타디엔-스티렌 블럭 공중합체를 비극성 용매에 10∼15% 되도록 용해시키는 단계,Dissolving styrene-butadiene-styrene block copolymer in 10% to 15% in a non-polar solvent, 상기 용액 100중량부를 혼합 유화제 5∼10중량부 및 물 80∼100 중량부로 이루어진 유화액을 사용하여 유화시키는 단계, 및Emulsifying 100 parts by weight of the solution using an emulsion comprising 5-10 parts by weight of a mixed emulsifier and 80-100 parts by weight of water, and 진공장치를 이용하여 비극성 용매를 제거·농축하여 에멀젼으로 제조하는 단계를 포함하는 스티렌-부타디엔-스티렌 블럭 공중합체의 수용화 방법.A method of solubilizing a styrene-butadiene-styrene block copolymer comprising the steps of removing and concentrating a nonpolar solvent using a vacuum apparatus to prepare an emulsion. 제 1 항에 있어서, 비극성 용매로는 n-헥산, 사이클로헥산, 헵탄 및 옥탄 중에서 선택하여 사용하는 것을 특징으로 하는 스티렌-부타디엔-스티렌 블럭 공중합체의 수용화 방법.The method of claim 1, wherein the non-polar solvent is selected from n-hexane, cyclohexane, heptane and octane to be used for the solubilization method of the styrene-butadiene-styrene block copolymer. 제 1 항에 있어서, 혼합유화제는 로진염 0.5∼5.0 중량부, 페티염 0.1∼3.0 중량부 및 올레인염 0.1∼3.0 중량부로 이루어진 것을 사용하는 것을 특징으로 하는 스티렌-부타디엔-스티렌 블럭 공중합체의 수용화 방법.The styrene-butadiene-styrene block copolymer according to claim 1, wherein the mixed emulsifier comprises 0.5 to 5.0 parts by weight of rosin salt, 0.1 to 3.0 parts by weight of petti salt and 0.1 to 3.0 parts by weight of oleine salt. Receptive method.
KR1019980051463A 1998-11-28 1998-11-28 Method for emulsifying styrene-butadiene-styrene block copolymer KR20000034197A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100348759B1 (en) * 2000-01-11 2002-08-13 금호석유화학 주식회사 Method of rubberized asphalt emulsion by using styrene-butadiene block copolymer

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100348759B1 (en) * 2000-01-11 2002-08-13 금호석유화학 주식회사 Method of rubberized asphalt emulsion by using styrene-butadiene block copolymer

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