KR20150014614A - producing method of nanocomposite resin composition with fluoro rubber - Google Patents
producing method of nanocomposite resin composition with fluoro rubber Download PDFInfo
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Abstract
Description
본발명은 불소고무 나노복합재 수지조성물 제조방법에 관한 것으로, 보다 상세하게는 불소고무 나노복합재 수지조성물에 관한 것으로, 보다 상세하게는 마스터배치와, 카본블랙, 산화마그네슘, 가교제로 비스페놀 A ,수산화칼슘, 왁스, DOP 를 혼합하여 제조된 불소고무 나노복합재 수지조성물 제조방법에 관한 것이다.More particularly, the present invention relates to a fluororubber-based nanocomposite resin composition, and more particularly, to a fluororubber-based nanocomposite resin composition comprising a masterbatch, carbon black, magnesium oxide and a crosslinking agent such as bisphenol A, Wax, and DOP to prepare a fluororubber-based nanocomposite resin composition.
일반적으로 최근 불소고무 나노복합재 조성물이 개발되어 왔고, 일례로서 등록특허공보 등록번호 10-0501991호에는 요약서에 요오드함유 불소고무와 같은 유기과산화물, 다관능성 불포화 화합물 및 디쿠밀 퍼옥시드와 같은 가황온도하 에탄올 및 t-부탄올의 합계량의 2 몰/몰, 바람직하게는 0 몰/몰 이하를 함유하는 분해산물을 형성시키는 유기 과산화물로 가황될 수 있는 불소고무를 함유하는 가황 불소고무용 조성물. 단지 일차 가황으로 수득되는 성형물이 실질적으로 충분한 특성, 특히 내열성을 갖기 때문에 이차 가황은 이 조성물에서 불필요한 불소고무 가황용 조성물 및 불소고무 성형품이 공개되어 있다. In general, recently, fluorine rubber nanocomposite compositions have been developed. As an example, Patent Document Registration No. 10-0501991 discloses a fluorine rubber nano composite material composition having a vulcanization temperature such as an organic peroxide such as iodine-containing fluorine rubber, a polyfunctional unsaturated compound and dicumyl peroxide A fluorine rubber which can be vulcanized with an organic peroxide to form a decomposition product containing 2 mol / mol, preferably 0 mol / mol or less of the total amount of ethanol and t-butanol. Since the molded article obtained by only the primary vulcanization has substantially sufficient properties, particularly heat resistance, secondary vulcanization is disclosed in a composition for vulcanizing a fluororubber and a fluororubber molded article unnecessary in this composition.
또한, 등록특허공보 등록번호 10-0473549호에는 (a) 비닐리덴 플루오라이드 및 (b) 디요오도메탄, 1,2-디요오도-1,1-디플루오로에탄, 1-요오도-2-브로모-1,1-디플루오로에탄, 1-브로모-2-요오도-1,1-디플루오로에탄 및 1,2-디브로모-1,1-디플루오로에탄으로 구성된 군으로부터 선택된 하나 이상의 화합물의 중합체를 포함하며, 상기 중합체의 말단 기의 80 % 이상은 화학식 -CH2-X (식 중, X는 Br 또는 I이다)을 갖고, 요오드, 브롬 또는 이들 둘 다를 중합체의 1 내지 5 중량 %의 양으로 함유하고, 100 ℃ 및 ω=6.3 s-1에서 0.01 내지 30 kPa.s의 복합 점도를 갖고, 40 ℃ 및 100 ℃에서 점도의 지수로서 계산한 온도 지수 3 내지 250을 갖는 것인 불소 고무가 공개되어 있다.In addition, Patent Registration No. 10-0473549 discloses a process for the preparation of (a) vinylidene fluoride and (b) diiodomethane, 1,2-diiodo-1,1-difluoroethane, 1-difluoroethane, 1-bromo-2-iodo-1,1-difluoroethane and 1,2-dibromo-1,1-difluoroethane these include polymers of one or more compounds from the group consisting of, and not less than 80% of the end groups of the polymer has a (wherein a, X is Br or I) formula -CH 2 -X, iodine, bromine, or both of these Having a complex viscosity in the range of from 1 to 5% by weight of the polymer and having a viscosity of from 0.01 to 30 kPa.s at 100 DEG C and? = 6.3 s-1 and having a temperature index 3 calculated as an index of viscosity at 40 DEG C and 100 DEG C To 250. < / RTI >
그러나 상기 종래기술들은 저경도이면서 고강도, 고내열성이 요구되는 수지조성물 제조가 곤란하며, 고무용 혼련설비를 이용하여 나노입자의 미세분말을 균일하게 분산시키는 것은 용이하지 않았다.
However, it is difficult to produce a resin composition requiring low hardness, high strength and high heat resistance, and it is not easy to uniformly disperse fine particles of nanoparticles using a rubber kneading apparatus.
그러나 상기 종래기술들은 저경도이면서 고강도, 고내열성이 요구되는 수지조성물 제조가 곤란하며, 고무용 혼련설비를 이용하여 나노입자의 미세분말을 균일하게 분산시키는 것은 용이하지 않았다.However, it is difficult to produce a resin composition requiring low hardness, high strength and high heat resistance, and it is not easy to uniformly disperse fine particles of nanoparticles using a rubber kneading apparatus.
따라서 본 발명은 상기와 같은 문제점을 해결하고자 안출된 것으로서, 본발명의 불소고무 나노복합재 수지조성물에 의해 제조되는 제품은 저경도, 고강도, 고내열성을 가지며 우수한 가공성도 가지게 되는 불소고무 나노복합 수지조성물의 제조방법을 제공하고자 한다.SUMMARY OF THE INVENTION Accordingly, it is an object of the present invention to provide a fluororubber-based nanocomposite resin composition which has low hardness, And a method for producing the same.
본발명은 불소고무 나노복합재 수지조성물 제조방법에 관한 것으로, 불소고무인 헥사플루오르프로필렌(hexafluorpropylene)과 비니리덴플루오라이드(vinylidene fluoride)의 디폴리머(dipolymer), 실리카, 분산제를 포함하는 마스터배치를 제조하는 단계; 상기 제조된 마스터배치와 카본블랙, 산화마그네슘, 가교제로 비스페놀 A ,수산화칼슘, 왁스, DOP 를 혼합하여 불소고무 나노복합재 수지 조성물을 제조하는 단계;를 포함하는 것을 특징으로 한다.The present invention relates to a process for producing a fluororubber-based nanocomposite resin composition, which comprises preparing a master batch containing a fluorocarbon rubber, a hexafluoropropylene, a dipolymer of vinylidene fluoride, silica, step; Mixing the prepared master batch with bisphenol A, calcium hydroxide, wax and DOP with carbon black, magnesium oxide and a cross-linking agent to prepare a fluororubber-nano composite resin composition.
본 발명의 불소고무 나노복합재 수지조성물 제조방법에 의해 제조되는 제품은 저경도, 고강도, 고내열성을 가지며 우수한 가공성도 가지는 현저한 효과가 있다.The product produced by the process for producing a fluororubber-based nanocomposite resin composition of the present invention has remarkable effect of having low hardness, high strength, high heat resistance and excellent processability.
본 발명은 나노입자 분말 충진제가 균일하게 분산된 불소고무 나노복합재 수지 조성물 제조방법에 관한 것으로, 먼저 fumed silica의 한 종류인 hydrophobic silica를 관용의 쌍축 압축성형기(twin-screw extruder)를 이용하여 분산제를 투입하여 나노입자인 silica를 균일하게 분산시켜 나노입자 분말 충진제 MB(master batch)를 제조한다.
The present invention relates to a method for preparing a fluororubber-based nanocomposite resin composition in which a nanoparticle powder filler is uniformly dispersed. First, a hydrophobic silica, which is one kind of fumed silica, is dispersed by using a twin-screw extruder To prepare a master batch of nanoparticle powder filler by uniformly dispersing the nanoparticle silica.
상기 나노입자 분말 충진제 MB(master batch)를 보다 상세하게 설명하면, 불소고무(Fluore Rubber)인 헥사플루오르프로필렌(hexafluorpropylene)과 비니리덴플루오라이드(vinylidene fluoride)의 디폴리머(dipolymer) {일례로서 다이킨사의 G763} 100 중량부에 대하여, 나노입자 충진제인 건식실리카(fumed silica)의 한 종류인 소수성 실리카(hydrophobic silica) 2~10 중량부, 분산제인 지방산 유도체(fatty acid) 1~3 중량부를 혼합하여 혼련기인 쌍축 압축성형기(twin extrude) 내에서 100℃에서 5분정도 성형하여 우유빛의 고체판재 형상으로 성형한 것이다.More specifically, the master batch of the nanoparticle powder filler may be a dipole polymer of hexafluoropropylene and vinylidene fluoride which is a fluoro rubber (for example, 2 to 10 parts by weight of a hydrophobic silica which is one kind of fumed silica which is a nanoparticle filler and 1 to 3 parts by weight of a fatty acid derivative as a dispersant are mixed with 100 parts by weight of G763 Molded in a twin extruder, which is a kneader, at 100 DEG C for about 5 minutes, and molded into a milky solid plate.
불소고무 100중량부에 대하여 소수성 실리카(hydrophobic silica)가 2중량부 미만이면, 제조가격이 상승되며 10중량부를 초과하면, 고강도, 고내열성, 작업성이 저하된다. 지방산 유도체(fatty acid)가 1중량부 미만이면, 제조가격이 상승되며 3중량부를 초과하면, 고강도, 고내열성, 작업성이 저하된다. 한편, 실리카 대신 클레이를 사용할 수 있다.
If the amount of the hydrophobic silica is less than 2 parts by weight based on 100 parts by weight of the fluorine rubber, the production cost is increased. If the amount is more than 10 parts by weight, high strength, high heat resistance and workability are deteriorated. If the amount of the fatty acid is less than 1 part by weight, the production cost is increased. If the amount is more than 3 parts by weight, high strength, high heat resistance and workability are deteriorated. On the other hand, clay can be used instead of silica.
제조된 마스터 배치(master batch)를 일반적으로 널리 알려져 사용되는 니이더, 반바리믹서, 인터믹서 등의 고무용 혼련설비를 이용하여 보강제, 수산제, 가공조제, 가소제, 활성제, 가교제 등을 순서대로 첨가하여 혼합하므로서 불소고무의 나노입자 분말수지 조성물이 제조된다.
The prepared master batch is mixed with a reinforcing agent, a fish oil agent, a processing aid, a plasticizer, an activator, a crosslinking agent, and the like in order by using a universal kneader, a Banbury mixer, an intermixer, And the mixture is mixed to produce a nanoparticle powdery resin composition of fluororubber.
상기 제조된 마스터배치 103~113 중량부에 대하여, 보강제로 카본블랙(carbon black) 5~20 중량부, 활성제인 고활성 산화마그네슘(high activity MgO) 1~5 중량부, 가교제로 비스페놀 A 2~5 중량부, 수산제로 수산화칼슘(calcium hydroxide) 2~8 중량부, 가공조제로 카나우바 왁스(carnauba wax) 1~ 3중량부, 가소제로 DOP (dioctyl phthalate di-2-ethylhexyl phthalate) 1~5 중량부를 혼합하여 우유빛의 고체판재인 불소고무 나노복합재 수지조성물을 제조한다.
5 to 20 parts by weight of carbon black as a reinforcing agent, 1 to 5 parts by weight of high activity MgO as an activator, and 1 to 5 parts by weight of high activity MgO as a reinforcing agent were added to 103 to 113 parts by weight of the prepared masterbatch, 2 to 8 parts by weight of calcium hydroxide as a hydroxylic acid, 1 to 3 parts by weight of carnauba wax as a processing aid, 1 to 5 parts by weight of dioctyl phthalate di-2-ethylhexyl phthalate (DOP) as a plasticizer Were mixed to prepare a fluoro rubber nanocomposite resin composition which is a solid plate of milky light.
마스터배치가 103중량부 미만이면 본발명 불소고무 나노복합재 수지 조성물에 의해 제조되는 제품의 고강도, 고내열성, 작업성이 저하되며, 113중량부를 초과하면 제품가격이 상승된다. 보강제인 카본블랙(carbon black)이 5중량부 미만이면 제품이 물러지며 20 중량부를 초과하면 너무 딱딱해진다. 활성제인 고활성 산화마그네슘(high activity MgO)이 1중량부 미만이면 제품성형이 잘되지 않고 5 중량부를 초과하면 제품의 고강도, 고내열성, 작업성이 저하된다. 가교제인 비스페놀 A 2중량부 미만이면 제품성형이 잘되지 않고 5 중량부를 초과하면 제품의 고강도, 고내열성, 작업성이 저하된다. 수산화칼슘(calcium hydroxide)은 성형시간을 단축하는 것으로, 2중량부 미만이면 성형시간이 길어지며 8 중량부를 초과하면 제품 탄성이 떨어진다. 가공조제인 카나우바 왁스(carnauba wax) 가 1중량부 미만이면 제품 성형이 잘되지 않고 3중량부를 초과하면 제품의 고강도, 고내열성, 작업성이 저하된다. 가소제인 DOP (dioctyl phthalate di-2-ethylhexyl phthalate)가 1중량부 미만이면 제품 성형이 잘되지 않고 5중량부를 초과하면 제품의 고강도, 고내열성, 작업성이 저하된다.When the masterbatch is less than 103 parts by weight, the product produced by the fluororubber-based nanocomposite resin composition of the present invention has a high strength, high heat resistance and workability, and when it exceeds 113 parts by weight, the product price is increased. If the amount of the carbon black as the reinforcing agent is less than 5 parts by weight, the product is recycled. If the amount exceeds 20 parts by weight, the product becomes too hard. When the amount of the high activity MgO is less than 1 part by weight, the product is not easily molded. If the amount is more than 5 parts by weight, the product has a high strength, high heat resistance and workability. If the amount is less than 2 parts by weight of bisphenol A, which is a crosslinking agent, molding of the product is difficult. If the amount is more than 5 parts by weight, high strength, high heat resistance and workability of the product are deteriorated. Calcium hydroxide shortens the molding time. When the amount is less than 2 parts by weight, the molding time is prolonged. When the amount is more than 8 parts by weight, the elasticity of the product is inferior. When the amount of carnauba wax as the processing aid is less than 1 part by weight, the product is not easily molded. If the amount is more than 3 parts by weight, the product has high strength, high heat resistance and workability. If the amount of dioctyl phthalate di-2-ethylhexyl phthalate (DOP) is less than 1 part by weight, the product is not easily molded. If the amount is more than 5 parts by weight, the product has a high strength, high heat resistance and workability.
제조방법은 혼련기에서 혼련단계를 거치게 된다. 혼련은 혼련기에서 100℃에서 5분간 정도 혼련한다. The production method is subjected to a kneading step in a kneader. The kneading is carried out at 100 DEG C for about 5 minutes in a kneader.
실시예Example
상기 표 1에 나타난 바와 같이, 본 발명에 의한 방법으로 처리된 나노입자 분말 충진제를 2~10 pne로 첨가한 경우 우수한 인장강도를 나타냈다.
As shown in Table 1, when the nanoparticle powder filler treated by the method of the present invention was added at 2 to 10 pne, excellent tensile strength was exhibited.
#1 : dipolymer of hexafluorpropylene and vinylidene fluoride# 1: dipolymer of hexafluoropropylene and vinylidene fluoride
#2 : hydrophobic silica(reacting hydrophilic silica with organic silica) 10~20 nm(나노 미터)# 2: hydrophobic silica (reacting hydrophilic silica with organic silica) 10 to 20 nm (nanometer)
#3 : special fatty acid derivative and silicones on inorganic carrier
# 3: special fatty acid derivative and silicones on inorganic carrier
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