KR101591565B1 - Acrylic lubricant, method for preparing latex powder, and vinyl based resin composition - Google Patents
Acrylic lubricant, method for preparing latex powder, and vinyl based resin composition Download PDFInfo
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- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
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Abstract
본 발명은 아크릴계 활제, 라텍스 분체의 제조방법 및 염화비닐계 수지 조성물에 관한 것으로, 본 발명에 따르면 저분자량 아크릴계 코어에 점착 보강 화합물을 포함하고, 고분자량 아크릴계 쉘에 분체 흐름 보강 화합물을 각각 포함함으로써 이를 비닐계 수지에 첨가할 경우 용융 지연 및 금속 점착성을 향상시키고, 고온분체 흐름성 또한 개선시킬 수 있어 가공조제를 따로 첨가해야 하는 시간 및 수고를 줄일 수 있는 아크릴계 활제와 라텍스 분체의 제조방법, 및 압출 성형, 캘린더 성형, 블로우 성형, 주입 성형 시 장기 작업성을 제공 가능한 염화비닐계 수지 조성물을 제공하는 효과를 갖는다. The present invention relates to an acrylic lubricant, a method for producing a latex powder, and a vinyl chloride resin composition. According to the present invention, a low molecular weight acrylic core contains an adhesive reinforcing compound and a high molecular weight acrylic shell contains a powder flow reinforcing compound A method of producing an acrylic lubricant and a latex powder which can reduce the time and labor required to separately add a processing aid because it improves melting delay and metal tackiness and improves high temperature powder flowability when added to a vinyl resin, It is possible to provide a vinyl chloride resin composition capable of providing long-term workability during extrusion molding, calender molding, blow molding and injection molding.
Description
본 발명은 아크릴계 활제, 라텍스 분체의 제조방법 및 염화비닐계 수지 조성물에 관한 것으로, 보다 상세하게는 저분자량 아크릴계 코어에 점착 보강 화합물을 포함하고, 고분자량 아크릴계 쉘에 분체 흐름 보강 화합물을 각각 포함함으로써 이를 비닐계 수지에 첨가할 경우 용융 지연 및 금속 점착성을 향상시키고, 고온분체 흐름성 또한 개선된 아크릴계 활제, 라텍스 분체의 제조방법 및 염화비닐계 수지 조성물에 관한 것이다.
The present invention relates to an acrylic lubricant, a method for producing a latex powder and a vinyl chloride resin composition, and more particularly to a low molecular weight acrylic core containing an adhesive reinforcing compound and a powder flow reinforcing compound in a high molecular weight acrylic shell A method for producing latex powder, and a vinyl chloride resin composition, which are improved in melt delay and metal tackiness when added to a vinyl resin and improved in high temperature powder flowability.
일반적으로 염화비닐 수지는 물리적 성질 및 화학적 성질이 우수한 성형체를 제공하므로 여러 분야에 폭넓게 사용한다. 그러나 가공온도가 열분해 온도에 가까우므로 성형 가능한 온도 영역이 좁고, 용융점도가 높고, 유동성이 낮을 뿐 아니라 고온 가공에서는 가공기기의 금속 표면에 점착되는 경향이 있어 탄화물 생성이 빈번하고 이로 인하여 최종 제품의 품질을 저하시키는 등 다양한 가공상의 문제가 발생하고 있다.
Generally, vinyl chloride resins provide molded articles having excellent physical properties and chemical properties, and thus are widely used in various fields. However, since the processing temperature is close to the pyrolysis temperature, the temperature range for forming is narrow, the melt viscosity is high and the fluidity is low. In addition, since the high temperature processing tends to adhere to the metal surface of the processing machine, carbide production is frequent, There are various processing problems such as deteriorating the quality.
이에 별도의 활제 혹은 가공조제를 제조하여 용융 지연 및 금속 점착성을 개선시키는 다양한 연구가 진행 중에 있다. 일 관련 기술로서, 한국 공개특허 제10-2006-0127730호에는 실리콘 라텍스를 추가하여 금속과의 점착성이 개선된 다층 구조의 고분자 활제 및 그의 제조 방법, 을 개시하고 있다. Various studies are underway to manufacture a lubricant or a processing aid to improve the melting delay and the metallic stickiness. As a related art, Korean Patent Laid-Open No. 10-2006-0127730 discloses a polymeric lubricant having a multi-layer structure in which silicone latex is added to improve adhesion to metals and a method for producing the same.
그러나, 상기 기술에서는 고가의 실리콘계 라텍스를 별도의 중합으로 첨가하여야 할 뿐 아니라 가공 도중 실리콘 고분자가 이행하여 가공 불량을 초래하는 단점이 있다.
However, in the above technology, not only expensive silicon-based latex is added as a separate polymerization but also silicon polymers are migrated during processing, resulting in defective processing.
또한, 염화비닐 수지의 성형가공시 겔화를 촉진하거나, 성형체의 표면품질 및 기계적 물성을 향상시키기 위하여 가공조제를 투입할 필요가 있다. 관련 기술로서, 한국 공개특허 10-2004-0047510호에서는 고온에서 흐름성이 우수하여 고온 건조가 가능하여 대량 생산 가능한 가공보조제 공중합체 조성물을 제공하지만, 가공 도중 금속과의 내 점착성이 충분하지 못한 단점이 있다.
In addition, it is necessary to add a processing aid to accelerate the gelation of the vinyl chloride resin during molding or to improve the surface quality and mechanical properties of the molded article. As a related art, Korean Patent Laid-Open No. 10-2004-0047510 discloses a processing aid copolymer composition which is excellent in flowability at a high temperature and can be dried at a high temperature so as to be mass-produced, but has a disadvantage .
또한 상기 활제와 가공조제를 별도로 하여 투입하게 되면 제조공정상의 상당한 불편함이 따르는바, 최근 들어 활제와 가공조제의 기능을 동시에 가지는 첨가제가 요구되고 있는 실정이다.
In addition, when the lubricant and the processing aid are added separately, considerable inconvenience is incurred in the manufacturing process. In recent years, there has been a demand for an additive having both a lubricant and a processing aid.
본 발명자들은 상기 문제점들을 해결하고자 연구를 계속하던 중, 저분자량 아크릴계 코어에 점착 보강 화합물을 포함하고, 고분자량 아크릴계 쉘에 분체 흐름 보강 화합물을 각각 포함하고, 이를 비닐계 수지에 첨가할 경우 용융 지연 및 금속 점착성을 향상시키고, 고온분체 흐름성 또한 개선됨을 확인하고, 이를 토대로 본 발명을 완성하게 되었다.
The inventors of the present invention, while continuing the research to solve the above problems, have found that when a low molecular weight acrylic core contains an adhesive reinforcing compound and a high molecular weight acrylic shell contains a powder flow reinforcing compound, And metallic stickiness, and the high-temperature powder flowability is also improved, and the present invention has been accomplished on the basis thereof.
즉, 본 발명의 일 목적은 상기 문제점들을 해결하고자, 염화비닐 수지의 금속 점착성과 고온분체 흐름성을 동시에 향상시킬 수 있는 아크릴계 활제를 제공하는 데 있다.That is, one object of the present invention is to provide an acrylic-based lubricant capable of simultaneously improving the metallic cohesion and the high-temperature powder flowability of a vinyl chloride resin in order to solve the above problems.
본 발명의 다른 목적은 상기 아크릴계 활제를 라텍스 분체 타입으로 제조하는 방법 및 이를 포함하는 염화비닐계 수지 조성물을 제공하는 데 있다.
Another object of the present invention is to provide a method for producing the acrylic lubricant as a latex powder type and a vinyl chloride resin composition containing the same.
본 발명에 따르면, According to the present invention,
점착 보강 화합물 함유 저분자량 아크릴계 코어 50 내지 80 중량%, 및 상기 코어를 감싸고, 분체 흐름 보강 화합물 함유 고분자량 아크릴계 쉘 50 내지 20 중량%,를 포함하는 아크릴계 활제를 제공한다.
50 to 80% by weight of a low molecular weight acrylic based core containing an adhesive reinforcing compound, and 50 to 20% by weight of a high molecular weight acrylic based shell containing the core and containing the powder flow reinforcing compound.
또한, 본 발명에 따르면, Further, according to the present invention,
비닐계 단량체 40 내지 80 중량%, 알킬 (메트)아크릴레이트계 단량체 10 내지 50 중량% 및 점착 보강 화합물 0.05 내지 10 중량%로 구성되고 중량평균 분자량 5000 내지 50만 g/mol인 아크릴계 코어를 제조하는 단계; Acrylic core composed of 40 to 80% by weight of a vinyl monomer, 10 to 50% by weight of an alkyl (meth) acrylate monomer and 0.05 to 10% by weight of an adhesive reinforcing compound and having a weight average molecular weight of 5,000 to 500,000 g / mol step;
상기 코어 50 내지 80 중량부에, 알킬 (메트)아크릴레이트계 단량체 70 내지 99.9 중량%, 비닐계 단량체 0.05 내지 20 중량% 및 분체 흐름 보강 화합물 0.05 내지 10 중량%를 50 내지 20 중량부로 투입하고 그라프트 중합하여 중량평균 분자량이 10만 내지 100만 g/mol인 고분자량 아크릴계 쉘 구조의 라텍스를 제조하는 단계: 및 50 to 20 parts by weight of an alkyl (meth) acrylate monomer, 0.05 to 20 parts by weight of a vinyl monomer and 0.05 to 10 parts by weight of a powder flow reinforcing compound are added to 50 to 80 parts by weight of the core, To prepare a latex of a high molecular weight acrylic shell structure having a weight average molecular weight of 100,000 to 1,000,000 g / mol; and
상기 라텍스를 응고하는 단계;를 포함하는 라텍스 분체의 제조방법을 제공한다.
And solidifying the latex. The present invention also provides a method for producing a latex powder comprising:
나아가, 본 발명에 따르면, Further, according to the present invention,
염화비닐 수지 100 중량부에 대하여, 상기 방법에 의해 제조된 라텍스 분체를 가공조제 겸용 활제로서 1 내지 10 중량부를 포함하는 염화비닐계 수지 조성물을 제공한다.
A vinyl chloride resin composition comprising 1 to 10 parts by weight of a latex powder prepared by the above method as a processing aid auxiliary lubricant, based on 100 parts by weight of a vinyl chloride resin.
이하, 본 발명에 대하여 보다 상세하게 설명한다. Hereinafter, the present invention will be described in more detail.
본 발명에서는 점착 보강 화합물 함유 저분자량 아크릴계 코어, 및 상기 코어를 감싸고, 분체 흐름 보강 화합물 함유 고분자량 아크릴계 쉘,을 포함하는 아크릴계 활제를 제공하는데 기술적 특징을 갖는다.
The present invention has a technical feature to provide an acryl-based lubricant comprising a low molecular weight acrylic-based core containing an adhesive-reinforcing compound and a high molecular weight acrylic-based shell containing the core and containing a powder flow reinforcing compound.
참고로, 본 발명에서 사용하는 용어 “점착 보강 화합물”은 달리 특정되지 않는 한, 폴리염화비닐 수지에 포함될 경우 수지의 고유 물성에 영향을 주지 않으면서 가공 시 가공기기 표면으로부터 점착성을 최소화할 수 있는 역할을 수행하는 화합물을 지칭한다. As used herein, unless otherwise specified, the term " adhesive reinforcing compound " used in the present invention refers to a compound capable of minimizing stickiness from the surface of a processing machine during processing without affecting the inherent properties of the resin, Quot; refers to a compound that performs a role.
또한, 본 발명에서 사용하는 용어 “분체 흐름 보강 화합물”은 달리 특정되지 않는 한, 그라프트 중합 시 분자량이 다소 낮은 코어 부분을 캡슐화하여 고온 분체 특성을 개선시킬 수 있는 역할을 수행하는 화합물을 지칭한다. The term " powder flow reinforcing compound " used in the present invention refers to a compound which, when not otherwise specified, performs a role of encapsulating a core portion having a slightly lower molecular weight during graft polymerization to improve the high temperature powder characteristics .
나아가, 본 발명에서 사용하는 용어 “저분자량 아크릴계 코어” 및 “고분자량 아크릴계 쉘”은 달리 특정하지 않는 한, 각각 분자량 조절제의 함량 조절을 통해 분자량을 조절한 아크릴계 라텍스로서, 코어와 쉘 중에서 코어 측 분자량이 다소 낮고, 쉘 측 분자량이 다소 높은 것을 지칭한다.
Further, unless otherwise specified, the terms "low molecular weight acrylic core" and "high molecular weight acrylic shell" used in the present invention are acrylic latexes whose molecular weights are adjusted by controlling the content of each molecular weight modifier, The molecular weight is somewhat low and the molecular weight on the shell side is somewhat higher.
특히, 본 발명에서 사용하는 상기 점착 보강 화합물은 상기 코어의 라디칼 공중합 자리 말단에 아크릴레이트 그라프트된 구조를 갖는 것을 일 특징으로 한다.
In particular, the adhesive and reinforcing compound used in the present invention is characterized in that it has acrylate grafted at the terminal of the radical copolymerization site of the core.
구체적인 예로, 상기 점착 보강 화합물은 하기 화학식 1의 구조를 갖고 중량평균 분자량이 200 내지 10,000 g/mol, 혹은 500 내지 2,000 g/mol일 수 있다. As a specific example, the pressure-sensitive adhesive compound may have a structure represented by the following Formula 1 and have a weight average molecular weight of 200 to 10,000 g / mol, or 500 to 2,000 g / mol.
[화학식 1][Chemical Formula 1]
CH3-(Si(CH3)2-O)n-ACH3- (Si (CH3) 2-O) n-A
일례로, A는 아크릴레이트 또는 메타크릴레이트이고, n은 2 내지 120의 정수일 수 있으며, 구체적인 예로, 상기 A는 메타크릴레이트이고, n은 8 내지 12의 정수일 수 있으며, 또 다른 예로, 상기 A는 메타크릴레이트이고, n은 10의 정수일 수 있다.
As an example, A may be acrylate or methacrylate, and n may be an integer of 2 to 120. As specific examples, A may be methacrylate, n may be an integer of 8 to 12, Is methacrylate, and n may be an integer of 10.
상기 점착 보강 화합물은 코어를 구성하는 전체 단량체와 화합물 총100 중량% 중 0.05 내지 10 중량%, 0.05 내지 5 중량%, 2.5 내지 10 중량%, 혹은 2.5 내지 5 중량%일 수 있다.
The adhesive and reinforcing compound may be 0.05 to 10% by weight, 0.05 to 5% by weight, 2.5 to 10% by weight, or 2.5 to 5% by weight based on 100% by weight of the total monomers constituting the core.
상기 저분자량 코어는 구체적인 예로, 비닐계 단량체 40 내지 80 중량%, 알킬 (메트)아크릴레이트계 단량체 10 내지 50 중량% 및 점착 보강 화합물 0.05 내지 10 중량%로 구성되고 중량평균 분자량 5000 내지 50만 g/mol인 것일 수 있다. Specific examples of the low-molecular-weight core include 40 to 80% by weight of a vinyl monomer, 10 to 50% by weight of an alkyl (meth) acrylate monomer and 0.05 to 10% by weight of an adhesive reinforcing compound, / mol. < / RTI >
상기 중량평균 분자량 범위는 분자량 조절제의 함량 조절에 따라 조절할 수 있다. The weight average molecular weight range can be controlled by adjusting the content of the molecular weight modifier.
다른 일례로, 비닐계 단량체 40 내지 60 중량%, 알킬 (메트)아크릴레이트계 단량체 35 내지 50 중량% 및 점착 보강 화합물 0.05 내지 5 중량%로 구성되고 중량평균 분자량 10만 내지 50만 g/mol인 것일 수 있다.As another example, it is possible to provide a pressure-sensitive adhesive composition comprising 40 to 60% by weight of a vinyl monomer, 35 to 50% by weight of an alkyl (meth) acrylate monomer and 0.05 to 5% by weight of an adhesive reinforcing compound and having a weight average molecular weight of 100,000 to 500,000 g / Lt; / RTI >
또 다른 일례로, 비닐계 단량체 50 내지 60 중량%, 알킬 (메트)아크릴레이트계 단량체 35 내지 45 중량% 및 점착 보강 화합물 2.5 내지 10 중량%로 구성되고 중량평균 분자량 10만 내지 25만 g/mol인 것일 수 있다.
As another example, it is preferable that it comprises 50 to 60% by weight of a vinyl monomer, 35 to 45% by weight of an alkyl (meth) acrylate monomer and 2.5 to 10% by weight of an adhesive reinforcing compound and has a weight average molecular weight of 100 to 250,000 g / mol Lt; / RTI >
이같이 하여 수득된 저분자량 아크릴계 코어는 NICOMP 광산란측정기로 측정한 평균 입자경이 50 내지 200nm 범위 내일 수 있다.
The low molecular weight acrylic core thus obtained may have an average particle size of 50 to 200 nm as measured by a NICOMP light scattering meter.
또한 상기 분체 흐름 보강 화합물은 상기 저분자량 코어를 캡슐화하는 구조를 갖는 것을 특징으로 한다.The powder flow reinforcing compound is characterized by having a structure for encapsulating the low molecular weight core.
구체적인 예로, 상기 분체 흐름 보강 화합물은 하기 화학식 2의 구조를 갖고 중량평균 분자량이 200 내지 10,000 g/mol, 혹은 200 내지 2,000 g/mol일 수 있다. As a specific example, the powder flow reinforcing compound may have a structure represented by the following formula (2) and have a weight average molecular weight of 200 to 10,000 g / mol, or 200 to 2,000 g / mol.
[화학식 2](2)
H-(CH2-CH2-O)n-AH- (CH2-CH2-O) n-A
일례로, A는 아크릴레이트 또는 메타크릴레이트이고, n은 2 내지 200의 정수일 수 있으며, 구체적인 예로, 상기 A는 메타크릴레이트이고, n은 3 내지 10의 정수일 수 있으며, 또 다른 예로, 상기 A는 메타크릴레이트이고, n은 6의 정수일 수 있다.
For example, A may be an acrylate or methacrylate, and n may be an integer of 2 to 200. In a specific example, A may be methacrylate, n may be an integer of 3 to 10, Is methacrylate, and n may be an integer of 6.
상기 분체 흐름 보강 화합물은 쉘을 구성하는 전체 단량체와 화합물 총100 중량% 중 0.05 내지 10 중량%, 0.05 내지 5 중량%, 2.5 내지 10 중량%, 혹은 2.5 내지 5 중량%일 수 있다.
The powder flow reinforcing compound may be 0.05 to 10% by weight, 0.05 to 5% by weight, 2.5 to 10% by weight, or 2.5 to 5% by weight based on 100% by weight of the total monomers constituting the shell.
상기 고분자량 쉘은 구체적인 예로, 알킬 (메트)아크릴레이트계 단량체 70 내지 99.9 중량%, 비닐계 단량체 0.05 내지 20 중량% 및 분체 흐름 보강 화합물 0.05 내지 10 중량%로 구성되고 중량평균 분자량 10만 내지 100만 g/mol인 것일 수 있다. The high molecular weight shell is, for example, composed of 70 to 99.9% by weight of an alkyl (meth) acrylate monomer, 0.05 to 20% by weight of a vinyl monomer and 0.05 to 10% by weight of a powder flow reinforcing compound, G / mol. ≪ / RTI >
상기 중량평균 분자량 범위는 상술한 바와 같이, 분자량 조절제의 함량 조절에 따라 조절할 수 있다. The weight average molecular weight range can be controlled by adjusting the content of the molecular weight modifier as described above.
다른 일례로, 알킬 (메트)아크릴레이트계 단량체 80 내지 99.9 중량%, 비닐계 단량체 0.1 내지 10 중량%, 및 분체 흐름 보강 화합물 0.05 내지 5 중량%로 구성되고 중량평균 분자량 50만 내지 100만 g/mol인 것일 수 있다.As another example, it is possible to use a composition comprising 80 to 99.9% by weight of an alkyl (meth) acrylate monomer, 0.1 to 10% by weight of a vinyl monomer, and 0.05 to 5% by weight of a powder flow reinforcing compound and having a weight average molecular weight of 500,000 to 1,000,000 g / mol. < / RTI >
또 다른 일례로, 알킬 (메트)아크릴레이트계 단량체 87 내지 94.9 중량%, 비닐계 단량체 5 내지 7.5 중량% 및 분체 흐름 보강 화합물 2.5 내지 5 중량%로 구성되고 중량평균 분자량 75만 내지 90만 g/mol인 것일 수 있다.
As another example, it is possible to provide an ink composition comprising 87 to 94.9% by weight of an alkyl (meth) acrylate monomer, 5 to 7.5% by weight of a vinyl monomer, and 2.5 to 5% by weight of a powder flow reinforcing compound and having a weight average molecular weight of 750,000 to 900,000 g / mol. < / RTI >
또한 수득된 고분자량 아크릴계 쉘은 NICOMP 광산란측정기로 측정한 평균 입자경이 80 내지 250 nm 범위 내일 수 있다.
The obtained high molecular weight acrylic shell may have an average particle size of 80 to 250 nm measured by a NICOMP light scattering meter.
상기 아크릴계 활제는 구체적인 예로, 코어 50 내지 80 중량%, 60 내지 80 중량% 혹은 70 내지 80 중량%로 구성되고, 쉘 50 내지 20 중량%, 40 내지 20 중량%, 혹은 30 내지 20 중량%로 구성된 것일 수 있다.
The acrylic lubricant is, for example, composed of 50 to 80% by weight, 60 to 80% by weight or 70 to 80% by weight of a core, 50 to 20% by weight, 40 to 20% by weight, or 30 to 20% Lt; / RTI >
상기 저분자량 아크릴계 코어 및 고분자량 아크릴계 쉘을 구성하는, 상기 알킬 (메트)아크릴레이트계 단량체는 일례로, 메틸 아크릴레이트, 메틸 메타크릴레이트, 에틸 아크릴레이트, 에틸 메타크릴레이트, 부틸 아크릴레이트, 부틸 메타크릴레이트, 프로필 아크릴레이트, 프로필 메타크릴레이트, 2-에틸헥실 아크릴레이트 및 2-에틸헥실 메타크릴레이트 중에서 선택된 1종 이상일 수 있다.Examples of the alkyl (meth) acrylate-based monomer constituting the low-molecular-weight acrylic core and the high molecular weight acrylic shell include methyl acrylate, methyl methacrylate, ethyl acrylate, ethyl methacrylate, butyl acrylate, butyl Acrylate, methacrylate, propyl acrylate, propyl methacrylate, 2-ethylhexyl acrylate and 2-ethylhexyl methacrylate.
구체적인 예로, 상기 알킬 (메트)아크릴레이트계 단량체는 저분자량 아크릴계 코어에 대해서는 에틸 아크릴레이트와 메틸메타크릴레이트의 혼합물일 수 있고, 고분자량 아크릴계 쉘에 대해서는 메틸메타크릴레이트일 수 있다.
As a specific example, the alkyl (meth) acrylate monomer may be a mixture of ethyl acrylate and methyl methacrylate for a low molecular weight acrylic core and methyl methacrylate for a high molecular weight acrylic shell.
또한, 상기 저분자량 아크릴계 코어 및 고분자량 아크릴계 쉘을 구성하는, 상기 비닐계 단량체는 일례로 스티렌, α-메틸스티렌, ο-메틸스티렌, p-메틸스티렌 및 p-tert-부틸스티렌 중에서 선택된 1종 이상일 수 있고, 구체적인 예로는 스티렌일 수 있다.
The vinyl monomer constituting the low molecular weight acrylic core and the high molecular weight acrylic shell may be one kind selected from styrene,? -Methylstyrene,? -Methylstyrene, p-methylstyrene and p-tert- Or more, and a specific example may be styrene.
본 발명에 의한 상기 아크릴계 활제는 비닐계 수지용 가공조제 겸용 활제인 것을 일 특징으로 한다.
The acrylic-based lubricant according to the present invention is characterized by being a lubricant for both processing and auxiliary processing for vinyl-based resins.
상기 아크릴계 활제는 일례로 다음과 같은 방식으로 제조될 수 있다:The acrylic lubricant may be prepared, for example, in the following manner:
우선, 비닐계 단량체 40 내지 80 중량%, 알킬 (메트)아크릴레이트계 단량체 10 내지 50 중량% 및 점착 보강 화합물 0.05 내지 10 중량%로 구성되고 중량평균 분자량 5000 내지 50만 g/mol인 아크릴계 코어를 제조할 수 있다. First, an acrylic core composed of 40 to 80% by weight of a vinyl monomer, 10 to 50% by weight of an alkyl (meth) acrylate monomer and 0.05 to 10% by weight of an adhesive reinforcing compound and having a weight average molecular weight of 5,000 to 500,000 g / Can be manufactured.
그런 다음 상기 코어 50 내지 80 중량부에, 알킬 (메트)아크릴레이트계 단량체 70 내지 99.9 중량%, 비닐계 단량체 0.05 내지 20 중량% 및 분체 흐름 보강 화합물 0.05 내지 10 중량%를 50 내지 20 중량부로 투입하고 그라프트 중합하여 중량평균 분자량이 10만 내지 100만 g/mol인 고분자량 아크릴계 쉘 구조의 라텍스를 제조할 수 있다. Then, 50 to 80 parts by weight of the core is charged with 70 to 99.9% by weight of an alkyl (meth) acrylate monomer, 0.05 to 20% by weight of a vinyl monomer and 0.05 to 10% by weight of a powder flow reinforcing compound in an amount of 50 to 20 parts by weight And graft-polymerized to prepare a latex of a high molecular weight acrylic shell structure having a weight average molecular weight of 100,000 to 1,000,000 g / mol.
이어서 상기 라텍스를 응고, 나아가 세척 및 건조하여 라텍스 분체로 수득할 수 있다.
The latex can then be coagulated, washed and dried to obtain a latex powder.
구체적인 예로, 상기 아크릴계 코어는 유화 중합에 의해, 그리고 상기 아크릴계 쉘은 그라프트 유화 중합에 의해 제조될 수 있다. As a specific example, the acrylic core may be prepared by emulsion polymerization and the acrylic shell may be prepared by graft emulsion polymerization.
상기 중합 및 응고, 세척 및 건조에 소요되는 조건 및 중합 개시제, 유화제 또는 활성화 용액 등의 첨가제는 통상 사용되는 것을 적용할 수 있다. 일례로 중합 온도는 20 내지 80 ℃ 범위 내일 수 있다. The conditions for polymerization and coagulation, washing and drying, and additives such as a polymerization initiator, an emulsifying agent or an activating solution can be used in general use. For example, the polymerization temperature may be in the range of 20 to 80 占 폚.
상기 방법으로 수득된 라텍스 분체는 염화비닐 수지 100 중량부에 대하여, 라텍스 분체를 가공조제 겸용 활제로서 1 내지 10 중량부, 혹은 1 내지 5 중량부 범위 내로 포함하고 염화비닐계 수지 조성물을 제공할 수 있다. 또한 상기 그라프트 유화 중합시 중합온도를 달리하면서 수회 나누어 중합반응을 진행시킬 수 있다.
The latex powder obtained by the above method contains 1 to 10 parts by weight, or 1 to 5 parts by weight of latex powder as a processing aid auxiliary lubricant, based on 100 parts by weight of vinyl chloride resin, and can provide a vinyl chloride resin composition have. In addition, the polymerization reaction may be carried out by dividing the grafting emulsion polymerization several times while varying the polymerization temperature.
상기 염화비닐계 수지 조성물에 따르면, 압출 성형, 캘린더 성형, 블로우 성형, 주입 성형 시 장기 작업성을 제공할 수 있다.
According to the vinyl chloride resin composition, long-term workability can be provided during extrusion molding, calender molding, blow molding and injection molding.
본 발명에 따르면, 비닐계 수지에 첨가할 경우 용융 지연 및 금속 점착성을 향상시키고, 고온분체 흐름성 또한 개선시킬 수 있어 가공조제를 따로 첨가해야 하는 시간 및 수고를 줄일 수 있는 아크릴계 활제, 라텍스 분체의 제조방법 및 압출 성형, 캘린더 성형, 블로우 성형, 주입 성형 시 장기 작업성을 제공가능한 염화비닐계 수지 조성물을 제공할 수 있다.
INDUSTRIAL APPLICABILITY According to the present invention, it is possible to provide an acrylic lubricant which can be added to a vinyl-based resin to improve the melting delay and metal tackiness and to improve the flowability of high-temperature powder, It is possible to provide a vinyl chloride resin composition capable of providing a long-term workability during the production process, extrusion molding, calender molding, blow molding and injection molding.
이하, 본 발명의 이해를 돕기 위하여 실시예를 제시하나, 하기 실시예는 본 발명을 예시하는 것일 뿐 본 발명을 하기 실시예에 한정하는 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 the following examples.
실시예Example -1 -One
(저분자량 아크릴계 코어 제조)(Low molecular weight acrylic core)
교반기와 온도계, 질소 투입구와 순환 콘덴서를 장착한 4구 플라스크의 반응기를 준비하고 탈이온수(deionized water; DDI water) 50 중량부, 페로오스 설페이트(ferrous sulfate) 0.002 중량부, 디소듐 에틸렌디아민테트라아세테이트 0.04 중량부를 투입하고 질소 분위기 하에 반응기 내부 온도를 70 ℃로 유지시켰다. A reactor of a four-necked flask equipped with a stirrer, a thermometer, a nitrogen inlet and a circulating condenser was prepared, and 50 parts by weight of deionized water (DDI water), 0.002 part by weight of ferrous sulfate, 0.04 parts by weight were fed into the reactor, and the reactor internal temperature was maintained at 70 占 폚 under a nitrogen atmosphere.
반응 전 미리 단량체 프리에멀젼으로서, 상기 반응기에 이온수 60 중량부, 소디움 라우릴 설페이트 0.4 중량부, 스티렌 38.25 중량부, 에틸 아크릴레이트 25 중량부, 메틸메타크릴레이트 5 중량부, 폴리디메틸실록산 메타크릴레이트 오일(디메틸실록산의 단위수(화학식 1의 n에 해당): 10) 1.75 중량부, 분자량 조절제로서 t-도데실메르캅탄 0.7 중량부를 배합하였다. As the monomer pre-emulsion before the reaction, 60 parts by weight of ionized water, 0.4 parts by weight of sodium lauryl sulfate, 38.25 parts by weight of styrene, 25 parts by weight of ethyl acrylate, 5 parts by weight of methyl methacrylate, 5 parts by weight of polydimethylsiloxane methacrylate 1.75 parts by weight of an oil (the number of units of dimethylsiloxane (corresponding to n in Formula 1): 10) and 0.7 parts by weight of t-dodecylmercaptan as a molecular weight regulator were blended.
상기 반응기 내부 온도 70 ℃에 도달할 때, 중합 개시제로서 t-부틸 하이드로퍼옥사이드 0.3 중량부와 소디움 포름알데히드 술폭시레이트 0.3 중량부를 상기 단량체 프리에멀젼과 함께 3 시간동안 동시 투입하여 반응을 진행시켰다.When the internal temperature of the reactor reached 70 DEG C, 0.3 part by weight of t-butyl hydroperoxide and 0.3 part by weight of sodium formaldehyde sulfoxylate were simultaneously added to the monomer pre-emulsion for 3 hours to proceed the reaction.
상기 단량체 프리에멀젼 투입 완료 30분 후 추가로 t-부틸 하이드로퍼옥사이드 0.01 중량부와 소디움 포름알데히드 술폭시레이트 0.01 중량부를 투입하고 1시간 동안 숙성시켰다. After 30 minutes of the monomer-free pre-emulsion addition, 0.01 part by weight of t-butyl hydroperoxide and 0.01 part by weight of sodium formaldehyde sulfoxylate were added and aged for 1 hour.
이때 NICOMP 광산란측정기로 측정한 라텍스 입자경은 100 nm이었다.
At this time, the latex particle size measured by NICOMP light scattering meter was 100 nm.
(고분자량 아크릴계 쉘 제조)(Manufactured by high molecular weight acrylic shell)
상기 저분자량 아크릴계 코어 70 중량부가 포함된 반응기의 내부 온도를 70℃로 유지하였다. The internal temperature of the reactor containing 70 parts by weight of the low molecular weight acrylic core was maintained at 70 캜.
또한 반응 전 미리 이온교환수 30 중량부, 소디움 포름알데히드 술폭시레이트 0.2 중량부, 메틸메타크릴레이트 27.75 중량부, 스티렌 1.5 중량부, 폴리에틸렌 글리콜 메타크릴레이트(에틸렌 옥사이드의 단위수(화학식 2의 n에 해당): 6) 0.75 중량부, 분자량 조절제로서 t-도데실메르캅탄 0.15 중량부를 배합하였다. Before the reaction, 30 parts by weight of ion-exchanged water, 0.2 part by weight of sodium formaldehyde sulfoxylate, 27.75 parts by weight of methyl methacrylate, 1.5 parts by weight of styrene, polyethylene glycol methacrylate (number of units of ethylene oxide : 6) and 0.15 part by weight of t-dodecyl mercaptan as a molecular weight regulator were mixed.
상기 단량체 프리 에멀젼과 개시제로서 t-부틸 하이드로퍼옥사이드 0.05 중량부, 소디움 포름알데히드 술폭시레이트 0.05 중량부를 1시간 동안 반응기에 투입하여 반응을 진행시켰다. 0.05 part by weight of t-butyl hydroperoxide and 0.05 part by weight of sodium formaldehyde sulfoxylate as an initiator were added to the reactor for 1 hour to conduct the reaction.
단량체 프리에멀젼 투입 완료 30분 후 개시제 t-부틸 하이드로퍼옥사이드 0.01 중량부 및 소디움 포름알데히드 술폭시레이트 0.01 중량부를 추가 투입하고 1시간 동안 숙성시켰다. After 30 minutes of the completion of the monomer pre-emulsion addition, 0.01 part by weight of initiator t-butyl hydroperoxide and 0.01 part by weight of sodium formaldehyde sulfoxylate were added thereto and aged for 1 hour.
제조된 라텍스의 총 고형분 함량(TSC)은 약 40중량%이었고, NICOMP 광산란측정기로 측정한 라텍스 입자경은 120 nm이었다.
The total solids content (TSC) of the prepared latex was about 40 wt%, and the latex particle size measured by NICOMP light scattering meter was 120 nm.
(라텍스 응고)(Latex coagulation)
수득된 중합체 라텍스 중 고형분에 대하여 4 중량부의 염화칼슘 용액(농도 10 중량%)을 일시 투입하여 응집하고 얻어진 슬러리를 이온쇼환수로 2-3회 세척하여 부산물을 씻어내었다. 여과(filtration)을 통해 다량 세척수를 제거한 후 실험실 용도로 사용되는 소형 유동층 건조기(Fluidized-bed dryer)를 사용하여 70 ℃에서 3시간 동안 건조시켜 분체 시료를 수득하였다.
4 parts by weight of a calcium chloride solution (concentration 10% by weight) was added to the polymer latex so that the solid was stirred and the resulting slurry was washed with ion shaking water 2-3 times to wash the by-products. After removing a large amount of washing water through filtration, a powdered sample was obtained by drying at 70 ° C for 3 hours using a fluidized-bed dryer used for laboratory use.
실시예Example -2-2
상기 실시예 1에서 (저분자량 아크릴계 코어 제조)단계에서 스티렌 36.5 중량부, 폴리디메틸실록산 메타크릴레이트 오일을 3.5 중량부 투입하고, (고분자량 아크릴계 쉘 제조)단계에서 메틸메타크릴레이트 27 중량부, 폴리에틸렌글리콜 메타크릴레이트 1.5 중량부를 사용한 것을 제외하고는 실시예 1과 동일한 공정을 반복하였다. 36.5 parts by weight of styrene and 3.5 parts by weight of polydimethylsiloxane methacrylate oil were charged in the step of preparing the low molecular weight acrylic core in Example 1, and 27 parts by weight of methyl methacrylate in the step of (high molecular weight acrylic shell) The same processes as in Example 1 were repeated except that 1.5 parts by weight of polyethylene glycol methacrylate was used .
이같이 하여 수득된 아크릴계 코어는 NICOMP 광산란측정기로 측정한 라텍스 입자경은 100 nm이었으며, 아크릴계 쉘의 총 고형분 함량(TSC)은 약 40중량%이었고, NICOMP 광산란측정기로 측정한 라텍스 입자경은 130 nm이었다.
The acrylic core thus obtained had a latex particle size of 100 nm as measured by a NICOMP light scattering meter, a total solid content (TSC) of the acrylic shell of about 40% by weight, and a latex particle size of 130 nm as measured by a NICOMP light scattering meter.
실시예Example -3-3
상기 실시예 2에서 (저분자량 아크릴계 코어 제조)단계에서 에틸 아크릴레이트를 30 중량부로 투입하면서 메틸메타크릴레이트를 미투입한 것을 제외하고는 실시예 2와 동일한 공정을 반복하였다. The same procedure as in Example 2 was repeated, except that methyl methacrylate was not added while 30 parts by weight of ethyl acrylate was added in the step of preparing the low molecular weight acrylic core (Example 2) .
이같이 하여 수득된 아크릴계 코어는 NICOMP 광산란측정기로 측정한 라텍스 입자경은 110 nm이었으며, 아크릴계 쉘의 총 고형분 함량(TSC)은 약 39중량%이었고, NICOMP 광산란측정기로 측정한 라텍스 입자경은 135 nm이었다.
The acrylic core thus obtained had a latex particle size of 110 nm as measured by a NICOMP light scattering meter, a total solid content (TSC) of about 39% by weight of the acrylic shell, and a latex particle size of 135 nm as measured by a NICOMP light scattering meter.
실시예Example -4-4
상기 실시예 1에서 (저분자량 아크릴계 코어 제조)단계에서 스티렌 35 중량부, 에틸 아크릴레이트 22 중량부, 폴리디메틸실록산 메타크릴레이트 오일 3 중량부 투입하고, (고분자량 아크릴계 쉘 제조)단계에서 메틸메타크릴레이트 35 중량부, 스티렌 3 중량부, 폴리에틸렌글리콜 메타크릴레이트 3 중량부를 사용한 것을 제외하고는 실시예 1과 동일한 공정을 반복하였다. 이같이 하여 수득된 아크릴계 코어는 NICOMP 광산란측정기로 측정한 라텍스 입자경은 85 nm이었으며, 아크릴계 쉘의 총 고형분 함량(TSC)은 약 39중량%이었고, NICOMP 광산란측정기로 측정한 라텍스 입자경은 125 nm이었다.
35 parts by weight of styrene, 22 parts by weight of ethyl acrylate and 3 parts by weight of polydimethylsiloxane methacrylate oil were charged in the step of preparing the low molecular weight acrylic core in Example 1, The same processes as in Example 1 were repeated except that 35 parts by weight of acrylate, 3 parts by weight of styrene, and 3 parts by weight of polyethylene glycol methacrylate were used . The acrylic core thus obtained had a latex particle size of 85 nm as measured by a NICOMP light scattering meter, a total solid content (TSC) of about 39% by weight of the acrylic shell, and a latex particle size of 125 nm as measured by a NICOMP light scattering meter.
실시예Example -5-5
상기 실시예 1에서 (저분자량 아크릴계 코어 제조)단계에서 스티렌 45 중량부, 에틸 아크릴레이트 31 중량부, 폴리디메틸실록산 메타크릴레이트 오일 4 중량부 투입하고, (고분자량 아크릴계 쉘 제조)단계에서 메틸메타크릴레이트 18 중량부, 스티렌 1 중량부, 폴리에틸렌글리콜 메타크릴레이트 1 중량부를 사용한 것을 제외하고는 실시예 1과 동일한 공정을 반복하였다. 45 parts by weight of styrene, 31 parts by weight of ethyl acrylate and 4 parts by weight of polydimethylsiloxane methacrylate oil were put in the step of preparing the low molecular weight acrylic core in Example 1, 18 parts by weight of acrylate, 1 part by weight of styrene, and 1 part by weight of polyethylene glycol methacrylate were used .
이같이 하여 수득된 아크릴계 코어는 NICOMP 광산란측정기로 측정한 라텍스 입자경은 105 nm이었으며, 아크릴계 쉘의 총 고형분 함량(TSC)은 약 40중량%이었고, NICOMP 광산란측정기로 측정한 라텍스 입자경은 125 nm이었다.
The acrylic core thus obtained had a latex particle size of 105 nm as measured by a NICOMP light scattering meter, a total solid content (TSC) of the acrylic shell of about 40% by weight, and a latex particle size as measured by a NICOMP light scattering meter of 125 nm.
비교예Comparative Example -1-One
상기 실시예 1에서 (저분자량 아크릴계 코어 제조)단계에서 스티렌 40 중량부, 에틸 아크릴레이트 25 중량부, 메틸메타크릴레이트 5 중량부를 투입하고 폴리디메틸실록산 메타크릴레이트 오일은 미투입하며, (고분자량 아크릴계 쉘 제조)단계에서 메틸메타크릴레이트 28.5 중량부, 스티렌 1.5 중량부를 투입하고 폴리에틸렌글리콜 메타크릴레이트는 미투입한 것을 제외하고는 실시예 1과 동일한 공정을 반복하였다. 40 parts by weight of styrene, 25 parts by weight of ethyl acrylate and 5 parts by weight of methyl methacrylate were added in the step of preparing the low molecular weight acrylic core in Example 1, and polydimethylsiloxane methacrylate oil was not added, Acryl-based shell), 28.5 parts by weight of methyl methacrylate and 1.5 parts by weight of styrene were charged, and the same processes as in Example 1 were repeated except that polyethylene glycol methacrylate was not added .
이같이 하여 수득된 아크릴계 코어는 NICOMP 광산란측정기로 측정한 라텍스 입자경은 80nm이었으며, 아크릴계 쉘의 총 고형분 함량(TSC)은 약 40중량%이었고, NICOMP 광산란측정기로 측정한 라텍스 입자경은 130 nm이었다.
The acrylic core thus obtained had a latex particle size of 80 nm as measured by a NICOMP light scattering meter, a total solid content (TSC) of the acrylic shell of about 40 wt%, and a latex particle size as measured by a NICOMP light scattering meter of 130 nm.
비교예Comparative Example -2-2
상기 실시예 1에서 (저분자량 아크릴계 코어 제조)단계에서 스티렌 45.5 중량부, 에틸 아크릴레이트 30 중량부, 메틸메타크릴레이트 10 중량부를 투입하고, (고분자량 아크릴계 쉘 제조)단계에서 메틸메타크릴레이트 9 중량부, 스티렌 0.5 중량부, 폴리에틸렌글리콜 메타크릴레이트는 0.5 중량부를 투입한 것을 제외하고는 실시예 1과 동일한 공정을 반복하였다. 45.5 parts by weight of styrene, 30 parts by weight of ethyl acrylate and 10 parts by weight of methyl methacrylate were charged in the step of preparing the low-molecular-weight acrylic-based core in Example 1, and methyl methacrylate 9 , 0.5 parts by weight of styrene, and 0.5 parts by weight of polyethylene glycol methacrylate were added .
이같이 하여 수득된 아크릴계 코어는 NICOMP 광산란측정기로 측정한 라텍스 입자경은 75 nm이었으며, 아크릴계 쉘의 총 고형분 함량(TSC)은 약 40중량%이었고, NICOMP 광산란측정기로 측정한 라텍스 입자경은 127 nm이었다.
The acrylic core thus obtained had a latex particle size of 75 nm as measured by a NICOMP light scattering meter, a total solid content (TSC) of about 40 wt% of the acrylic shell, and a latex particle size of 127 nm as measured by a NICOMP light scattering meter.
비교예Comparative Example -3-3
상기 실시예 1에서 (저분자량 아크릴계 코어 제조)단계에서 스티렌 45.5 중량부, 에틸 아크릴레이트 30 중량부, 메틸메타크릴레이트 10 중량부를 투입하고, (고분자량 아크릴계 쉘 제조)단계에서 메틸메타크릴레이트 9 중량부, 스티렌 0.5 중량부, 폴리에틸렌글리콜 메타크릴레이트는 0.5 중량부를 투입한 것을 제외하고는 실시예 1과 동일한 공정을 반복하였다. 45.5 parts by weight of styrene, 30 parts by weight of ethyl acrylate and 10 parts by weight of methyl methacrylate were charged in the step of preparing the low-molecular-weight acrylic-based core in Example 1, and methyl methacrylate 9 , 0.5 parts by weight of styrene, and 0.5 parts by weight of polyethylene glycol methacrylate were added .
이같이 하여 수득된 아크릴계 코어는 NICOMP 광산란측정기로 측정한 라텍스 입자경은 115 nm이었으며, 아크릴계 쉘의 총 고형분 함량(TSC)은 약 39중량%이었고, NICOMP 광산란측정기로 측정한 라텍스 입자경은 125 nm이었다.
The acrylic core thus obtained had a latex particle size of 115 nm as measured by a NICOMP light scattering meter, a total solid content (TSC) of about 39% by weight of the acrylic shell, and a latex particle size of 125 nm as measured by a NICOMP light scattering meter.
비교예Comparative Example -4-4
상기 실시예 1에서 (저분자량 아크릴계 코어 제조)단계에서 스티렌 25 중량부, 에틸 아크릴레이트 13 중량부, 폴리디메틸실록산 메타크릴레이트 오일 2 중량부를 투입하고, (고분자량 아크릴계 쉘 제조)단계에서 메틸메타크릴레이트 52 중량부, 스티렌 5 중량부, 폴리에틸렌글리콜 메타크릴레이트는 3 중량부를 투입한 것을 제외하고는 실시예 1과 동일한 공정을 반복하였다. 25 parts by weight of styrene, 13 parts by weight of ethyl acrylate and 2 parts by weight of polydimethylsiloxane methacrylate oil were charged in the step of preparing the low molecular weight acrylic core in Example 1, 52 parts by weight of acrylate, 5 parts by weight of styrene, and 3 parts by weight of polyethylene glycol methacrylate were added .
이같이 하여 수득된 아크릴계 코어는 NICOMP 광산란측정기로 측정한 라텍스 입자경은 70 nm이었으며, 아크릴계 쉘의 총 고형분 함량(TSC)은 약 39중량%이었고, NICOMP 광산란측정기로 측정한 라텍스 입자경은 132nm이었다.
The acrylic core thus obtained had a latex particle size of 70 nm as measured by a NICOMP light scattering meter, a total solid content (TSC) of about 39% by weight of the acrylic shell, and a latex particle size of 132 nm as measured by a NICOMP light scattering meter.
상기 실시예 1 내지 5 및 비교예 1 내지 4의 각 시료에 대하여 중량평균 분자량, 점착성 평가, 용융시간, 및 고온 분체 흐름성을 다음과 같은 방식으로 측정하고 결과를 하기 표 1에 나타내었다.The weight average molecular weight, the tackiness evaluation, the melting time, and the high temperature powder flowability of each of the samples of Examples 1 to 5 and Comparative Examples 1 to 4 were measured in the following manner, and the results are shown in Table 1 below.
*중량평균 분자량(g/* Weight average molecular weight (g / molmol ): ):
각 시료를 테트라하이드로퓨란에 녹인 다음 용해된 부분에 대해 겔 침투 크로마토그래피(GPC)를 사용하여 측정하였다. 검량선은 폴리스티렌 기준 시료를 이용하였다.Each sample was dissolved in tetrahydrofuran and then the dissolved portion was measured using gel permeation chromatography (GPC). Polystyrene standards were used for the calibration curve.
*점착성 평가: * Tackiness evaluation:
폴리염화비닐 수지(중합도 800, 엘지화학 제품 LS-080) 100 중량부, 틴계 열안정제(BT-107) 3 중량부, 칼슘-스테아레이트(Ca-St) 0.9 중량부를 상온에서 혼련기(Henshel mixer)에 투입한 다음 1,000 rpm으로 115 ℃까지 승온시키면서 믹싱하고 40 ℃까지 냉각시켜 마스터배치를 제조하였다. 100 parts by weight of a polyvinyl chloride resin (polymerization degree 800, LS-080 from LG Chemical Co.), 3 parts by weight of a thermosetting agent (BT-107) and 0.9 parts by weight of calcium-stearate (Ca-St) were kneaded in a kneader ), Followed by mixing at 1,000 rpm while raising the temperature to 115 DEG C and cooling to 40 DEG C to prepare a master batch.
상기 마스터배치에 각 시료를 각각 3 중량부씩 첨가한 다음 상온에서 다시 혼련하고 6인치 2-롤밀을 사용하여 분체 혼합물 100 중량부를 롤 혼련하고 200 ℃, 롤 회전 수 14x15 rpm, 롤 간격 0.3 mm 조건하에 4분간 밀링한 다음 롤 표면에서의 점착성을 이하 5점법에 따라 평가하였다. Three parts by weight of each sample was added to the masterbatch, and the mixture was further kneaded at room temperature, and 100 parts by weight of the powder mixture was kneaded by using a 6-inch 2-roll mill and kneaded under the conditions of 200 캜, roll revolution of 14 x 15 rpm, After 4 minutes of milling, the adhesion on the roll surface was evaluated according to the following five-point method.
5: 박리되면서 늘어남이 전혀 없음. 4: 박리되면서 늘어남 거의 없음. 3: 박리되면서 약간 늘어남. 2: 박리되나 많이 늘어남. 1: 박리되지 않음. 5: No peeling and no stretching. 4: Almost no increase in peeling. 3: slightly peeled off. 2: It is peeled, but it increases a lot. 1: Not peeled off.
*용융시간 평가:* Melting time evaluation:
상기 점착성 평가에서 사용한 폴리염화비닐 수지 조성물 60 중량부를 180 ℃, 30 rpm 하에 하케 레오미터(Haake Rheometer)를 사용하여 가공 후 최소 부하부터 최대 부하까지 걸리는 시간을 측정하였다. 60 parts by weight of the polyvinyl chloride resin composition used in the tackiness evaluation was processed at 180 캜 under 30 rpm using a Haake rheometer and the time taken from the minimum load to the maximum load was measured.
*고온 *High temperature 분체흐름성Powder flowability 평가: evaluation:
각 시료를 실험실 용도로 사용되는 소형 유동층 건조기(Fluidized-bed dryer)를 사용하여 75 ℃에서 30분간 운전시킨 다음 분체의 뭉침 정도를 이하 5점법에 따라 평가하였다. Each sample was run at 75 ° C for 30 minutes using a fluidized-bed dryer, which was used for laboratory use, and then the degree of aggregation of the powder was evaluated according to the following five-point method.
5: 시료 분체의 뭉침 현상이 전혀 없음, 4: 시료 분체의 뭉침 현상이 거의 없음, 3: 시료 분체의 1/4 정도 뭉침 현상이 발생함, 2: 시료 분체의 1/2 정도 뭉침 현상이 발생함, 1: 시료 분체의 3/4 이상 뭉침 현상이 발생함. 5: No aggregation of sample powder, 4: Almost no aggregation of sample powder, 3: Around 1/4 of sample powder aggregation occurred, 2: A half of sample powder aggregation occurred 1, 3 or more of the sample powder is aggregated.
(g/mol)Core Mw
(g / mol)
(g/mol)Shell Mw
(g / mol)
시간
(sec)Melting
time
(sec)
상기 표 1에서 보듯이, 실시예 1 내지 5의 경우에 점착성과 고온 분체 흐름성이 모두 개선된 결과를 확인할 수 있었다. As shown in Table 1, in Examples 1 to 5, both the adhesiveness and the high-temperature powder flowability were improved.
한편, 실시예 1 내지 5 대비, 코어 내 점착 보강용 화합물과 쉘 내 분체 흐름 보강용 화합물을 각각 미투입한 비교예 1, 저분자량 코어와 고분자량 쉘의 분자량 범위를 벗어난 비교예 2의 경우에는 각각 점착성과 고온 분체 흐름성이 불량한 것을 확인할 수 있었다. On the other hand, in the case of Comparative Example 1 in which the intracornerally adhesive reinforcing compound and the powder flow reinforcing compound in the shell were not respectively inserted in Examples 1 to 5 and Comparative Example 2 in which the molecular weight of the low molecular weight core and the high molecular weight shell were out of the range, It was confirmed that the adhesiveness and the high-temperature powder flowability were poor.
또한, 코어 함량이 80 중량% 초과한 비교예 3의 경우에는 고온 분체 흐름성이 저하되었고, 코어 함량이 50 중량% 이하인 비교예 4의 경우에는 점착성이 저하된 것을 확인할 수 있었다. In addition, in Comparative Example 3 in which the core content exceeded 80 wt%, the flowability of the hot powder decreased, and in Comparative Example 4 in which the core content was 50 wt% or less, it was confirmed that the adhesiveness was deteriorated.
Claims (17)
상기 점착 보강 화합물은 상기 코어의 라디칼 공중합 자리 말단에 아크릴레이트 그라프트된 구조를 갖는 것으로, 하기 화학식 1의 구조를 갖고 중량평균 분자량이 200 내지 10,000 g/mol이고,
[화학식 1]
CH3-(Si(CH3)2-O)n-A
(A는 아크릴레이트 또는 메타크릴레이트이고, n은 2 내지 120의 정수이다)
상기 저분자량 아크릴계 코어의 중량평균 분자량은 5000 내지 50만 g/mol이고,
상기 분체 흐름 보강 화합물은 상기 저분자량 코어를 캡슐화하는 구조를 갖는 것으로, 하기 화학식 2의 구조를 갖고 중량평균 분자량이 200 내지 10,000 g/mol이고,
[화학식 2]
H-(CH2-CH2-O)n-A
(A는 아크릴레이트 또는 메타크릴레이트이고, n은 2 내지 200의 정수이다)
상기 고분자량 아크릴계 쉘의 중량평균 분자량은 10만 내지 100만 g/mol인 아크릴계 활제.
50 to 80% by weight of a low molecular weight acrylic based core containing an adhesive reinforcing compound, and 50 to 20% by weight of a high molecular weight acrylic shell containing the powder flow reinforcing compound,
Wherein the pressure-sensitive adhesive compound has an acrylate grafted structure at the terminal of a radical copolymerization site of the core and has a structure represented by the following formula (1) and has a weight average molecular weight of 200 to 10,000 g / mol,
[Chemical Formula 1]
CH3- (Si (CH3) 2-O) nA
(A is acrylate or methacrylate, and n is an integer of 2 to 120)
The weight average molecular weight of the low molecular weight acrylic core is 5,000 to 500,000 g / mol,
The powder flow reinforcing compound has a structure to encapsulate the low molecular weight core, and has a structure of the following formula (2) and has a weight average molecular weight of 200 to 10,000 g / mol,
(2)
H- (CH2-CH2-O) nA
(A is acrylate or methacrylate, and n is an integer of 2 to 200)
Wherein the high molecular weight acrylic shell has a weight average molecular weight of 100,000 to 1,000,000 g / mol.
상기 점착 보강 화합물은 코어를 구성하는 전체 단량체와 화합물 총100 중량% 중 0.05 내지 10 중량%인 것을 특징으로 하는 아크릴계 활제.
The method according to claim 1,
Wherein the viscous reinforcing compound is 0.05 to 10% by weight based on 100% by weight of the total monomers constituting the core and the compound.
상기 저분자량 코어는 비닐계 단량체 40 내지 80 중량%, 알킬 (메트)아크릴레이트계 단량체 10 내지 50 중량% 및 점착 보강 화합물 0.05 내지 10 중량%로 구성되는 것을 특징으로 하는 아크릴계 활제.
The method according to claim 1,
Wherein the low molecular weight core is composed of 40 to 80% by weight of a vinyl monomer, 10 to 50% by weight of an alkyl (meth) acrylate monomer, and 0.05 to 10% by weight of an adhesive reinforcing compound.
상기 분체 흐름 보강 화합물은 쉘을 구성하는 전체 단량체와 화합물 총100 중량% 중 0.05 내지 10 중량%인 것을 특징으로 하는 아크릴계 활제.
The method according to claim 1,
Wherein the powder flow reinforcing compound is 0.05 to 10% by weight based on 100% by weight of the total monomer and compound constituting the shell.
상기 고분자량 쉘은 알킬 (메트)아크릴레이트계 단량체 70 내지 99.9 중량%, 비닐계 단량체 0.05 내지 20 중량% 및 분체 흐름 보강 화합물 0.05 내지 10 중량%로 구성되는 것을 특징으로 하는 아크릴계 활제.
The method according to claim 1,
Wherein the high molecular weight shell comprises 70 to 99.9% by weight of an alkyl (meth) acrylate monomer, 0.05 to 20% by weight of a vinyl monomer, and 0.05 to 10% by weight of a powder flow reinforcing compound.
상기 알킬 (메트)아크릴레이트계 단량체는 메틸 아크릴레이트, 메틸 메타크릴레이트, 에틸 아크릴레이트, 에틸 메타크릴레이트, 부틸 아크릴레이트, 부틸 메타크릴레이트, 프로필 아크릴레이트, 프로필 메타크릴레이트, 2-에틸헥실 아크릴레이트 및 2-에틸헥실 메타크릴레이트 중에서 선택된 1종 이상인 것을 특징으로 하는 아크릴계 활제.
10. The method according to claim 5 or 9,
The alkyl (meth) acrylate monomer may be selected from the group consisting of methyl acrylate, methyl methacrylate, ethyl acrylate, ethyl methacrylate, butyl acrylate, butyl methacrylate, propyl acrylate, propyl methacrylate, Acrylate, and 2-ethylhexyl methacrylate.
상기 비닐계 단량체는 스티렌, α-메틸스티렌, ο-메틸스티렌, p-메틸스티렌 및 p-tert-부틸스티렌 중에서 선택된 1종 이상인 것을 특징으로 하는 아크릴계 활제.
10. The method according to claim 5 or 9,
Wherein the vinyl-based monomer is at least one selected from the group consisting of styrene,? -Methylstyrene,? -Methylstyrene, p-methylstyrene and p-tert-butylstyrene.
[화학식 1]
CH3-(Si(CH3)2-O)n-A
(A는 아크릴레이트 또는 메타크릴레이트이고, n은 2 내지 120의 정수이다)의 구조를 갖고 중량평균 분자량이 200 내지 10,000 g/mol인 점착 보강 화합물 0.05 내지 10 중량%로 구성되고 중량평균 분자량 5000 내지 50만 g/mol인 아크릴계 코어를 제조하는 단계;
상기 코어 50 내지 80 중량부에, 알킬 (메트)아크릴레이트계 단량체 70 내지 99.9 중량%, 비닐계 단량체 0.05 내지 20 중량% 및 하기 화학식 2
[화학식 2]
H-(CH2-CH2-O)n-A
(A는 아크릴레이트 또는 메타크릴레이트이고, n은 2 내지 200의 정수이다)의 구조를 갖고 중량평균 분자량이 200 내지 10,000 g/mol인 분체 흐름 보강 화합물 0.05 내지 10 중량%를 50 내지 20 중량부로 투입하고 그라프트 중합하여 중량평균 분자량이 10만 내지 100만 g/mol인 고분자량 아크릴계 쉘 구조의 라텍스를 제조하는 단계: 및
상기 라텍스를 응고하는 단계;를 포함하는 라텍스 분체의 제조방법.
40 to 80% by weight of a vinyl monomer, 10 to 50% by weight of an alkyl (meth) acrylate monomer,
[Chemical Formula 1]
CH3- (Si (CH3) 2-O) nA
(A is acrylate or methacrylate, and n is an integer of 2 to 120) and 0.05 to 10% by weight of an adhesive reinforcing compound having a weight average molecular weight of 200 to 10,000 g / mol, and has a weight average molecular weight of 5000 To about 500,000 g / mol;
Wherein 70 to 99.9% by weight of an alkyl (meth) acrylate monomer, 0.05 to 20% by weight of a vinyl monomer,
(2)
H- (CH2-CH2-O) nA
From 0.05 to 10% by weight of a powder flow reinforcing compound having a structure represented by the following formula (A is acrylate or methacrylate and n is an integer of 2 to 200) and having a weight average molecular weight of 200 to 10,000 g / mol And graft polymerization to prepare a latex of a high molecular weight acrylic shell structure having a weight average molecular weight of 100,000 to 1,000,000 g / mol; and
And solidifying the latex.
A vinyl chloride resin composition comprising 1 to 10 parts by weight of a latex powder produced by the method of claim 13 as a processing aid auxiliary lubricant, based on 100 parts by weight of a vinyl chloride resin.
상기 염화비닐계 수지 조성물은 압출 성형, 캘린더 성형, 블로우 성형 또는 주입 성형 시 장기 작업성을 나타내는 것을 특징으로 하는 염화비닐계 수지 조성물.17. The method of claim 16,
Wherein the vinyl chloride resin composition exhibits long-term workability during extrusion molding, calender molding, blow molding or injection molding.
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| JP2000264936A (en) * | 1999-03-16 | 2000-09-26 | Sekisui Chem Co Ltd | Vinyl chloride-based resin and its production |
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