KR100251466B1 - A manufacturing method for incombustible pressure sensitive adhesive - Google Patents

A manufacturing method for incombustible pressure sensitive adhesive Download PDF

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KR100251466B1
KR100251466B1 KR1019980013238A KR19980013238A KR100251466B1 KR 100251466 B1 KR100251466 B1 KR 100251466B1 KR 1019980013238 A KR1019980013238 A KR 1019980013238A KR 19980013238 A KR19980013238 A KR 19980013238A KR 100251466 B1 KR100251466 B1 KR 100251466B1
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sensitive adhesive
pressure
resin
adhesive
weight
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KR1019980013238A
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KR19990080175A (en
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백윤현
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백윤현
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02—Non-macromolecular additives
    • C09J11/06—Non-macromolecular additives organic
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J121/00—Adhesives based on unspecified rubbers
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J133/00—Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
    • C09J133/04—Homopolymers or copolymers of esters
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J4/00—Adhesives based on organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond ; adhesives, based on monomers of macromolecular compounds of groups C09J183/00 - C09J183/16
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J9/00—Adhesives characterised by their physical nature or the effects produced, e.g. glue sticks

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Adhesives Or Adhesive Processes (AREA)

Abstract

PURPOSE: A fire-resistant adhesive is provided to manufacture fire-resistant adhesive tapes that have an excellent fire resistance and transparency without deteriorating adhesiveness of the tape by adding fire retardant. CONSTITUTION: A method for manufacturing a fire-resistant adhesive for an adhesive tape which is mainly composed of resin, comprises polymerizing one of monomers, tris monobenzyl acrylate pentabromo benzyl acrylate, or tris bromo phenyl maleimide by 1-15 wt.% of solids, to supply fire resistance characteristic to the adhesive tapes. The resin monomers are acryl resin group monomers or rubber resin group monomers.

Description

난연성 점착제의 제조방법Manufacturing method of flame retardant adhesive

본 발명은 난연성(難燃性) 점착테이프 제조용 난연성 점착제의 제조방법에 관한 것이다.The present invention relates to a method for producing a flame-retardant pressure-sensitive adhesive for producing a flame-retardant pressure-sensitive adhesive tape.

최근 전기기기, 가정용 전자제품을 비롯하여 차량재료 등에 있어서 화재에 대한 안전성 유지가 중요하다는 인식이 확산되면서 이들에 대한 안전기준이 점차 엄격해 지고 있다.Recently, as safety awareness of fire safety is important in electric devices, household electronics, and vehicle materials, safety standards for them are becoming stricter.

특히, 미국의 텔레비젼, 오디오, 통신기계 분야에서는 UL마크(Underwriters Laboratories Mark)를 비롯하여 엄격한 규격에 합격하는 것을 필수 조건으로 하고 있다.In particular, in the US television, audio, and telecommunications machinery, passing stringent standards, including the Underwriters Laboratories Mark, is a requirement.

미국에서는 그 동안 자소성(自消性) 규격이 엄격한 "LU-94-V" 규격을 적용하여 오다가 최근에는 UL-94-Vo 규격으로 규격조건을 더욱 강화한 바 있다.In the United States, the "LU-94-V" standard, which has a strict self-extinguishing standard, has been applied. Recently, the UL-94-Vo standard has been further strengthened.

우리 나라에서도 "전기용품 안전관리법"을 비롯하여 소방법, 건축법 등에서도 사용 제품의 난연성(難燃性)을 규제하고 있으며 그 규격 수준도 점차 강화되는 추세에 있다.In Korea, flame retardancy of used products is regulated under the "Safety Control Act of Electric Appliances", Fire Protection Act, Building Law, etc., and the standard level is gradually increasing.

UL마크는 미국 보험업자협회가 관장하고 있는 세계 최대의 전기, 전자분야 공업규격으로서 이 마크를 획득하지 않고서 미국시장에 진출한다는 것은 거의 불가능한 실정이다.The UL Mark is the world's largest industrial standard for electrical and electronics, managed by the American Underwriters Association, and it is almost impossible to enter the US market without acquiring this mark.

본 발명은 UL-94-Vo 규격에 적합한 점착테이프 제조용 점착제의 제조방법에 관한 것이다.The present invention relates to a method for producing a pressure-sensitive adhesive for producing a pressure-sensitive adhesive tape conforming to the UL-94-Vo standard.

일반적으로 점착테이프 제조용 점착제는 주로 가연성의 고무 또는 합성수지계 물질들을 주원료로 사용하므로 점착제 조성물에 난연제(Fire retardant)를 첨가하여 난연성을 부여하고 있다.In general, the pressure-sensitive adhesive for preparing the adhesive tape mainly uses flammable rubber or synthetic resins as a main raw material, thereby adding flame retardant to the pressure-sensitive adhesive composition to impart flame retardancy.

종래 고무계 또는 아크릴수지계 점착제를 난연성으로 하여 주기 위하여 클로로프렌고무, 염소고무, 염소화수지 등의 난연성 원료를 사용하거나 난연제를 첨가하여 사용하여 왔다.Conventionally, in order to make a rubber-based or acrylic resin-based adhesive a flame retardant, flame retardant raw materials such as chloroprene rubber, chlorine rubber and chlorinated resin have been used or flame retardant is added.

일반적으로 난연제는 할로겐(Halogen)계 난연제, 인(燐)계 난연제, 무기계 난연제로 대별되는데 점착제에 난연성을 부여하기 위하여 사용되는 할로겐계 난연제로서는 "데카부로모페닐옥사이드"(Decabromodiphenyl Oxide : 이하 DBDPO라 한다) 인계 난연제로서는 "트리스디클로로푸로필포스페이트"(Trisdichloropropyl phosphate : 이하 CRP라 한다)가 많이 사용되고 있다.In general, flame retardants are generally classified into halogen flame retardants, phosphorus flame retardants, and inorganic flame retardants. Halogen flame retardants used to impart flame retardancy to an adhesive are "decabromodiphenyl oxide" (hereinafter referred to as DBDPO). As the phosphorus flame retardant, "trisdichloropropyl phosphate" (hereinafter referred to as CRP) is often used.

DBDPO는 브롬함량이 높아(Br함량 83%) 난연성은 좋으나 이는 분말인 관계로 아크릴계 수지와 상용성(相溶性)이 나쁘고 일정량 이상을 첨가하게 되면 접착력을 저하시키는 단점이 있다.DBDPO has a high bromine content (Br content of 83%) and has good flame retardancy, but since it is a powder, it has a disadvantage in that compatibility with acrylic resin is poor, and when more than a predetermined amount is added, the adhesive strength is lowered.

본 발명의 목적은 우수한 난연성과 접착력을 가지면서 투명성을 갖는 난연성 점착제의 제조방법을 제공하는데 있다.It is an object of the present invention to provide a method for producing a flame retardant pressure-sensitive adhesive having transparency while having excellent flame retardancy and adhesion.

일반적으로 고무계 또는 아크릴수지계 첨착제는 천연고무 또는 합성 고무를 원료로 하거나 아크릴계 모노머를 중합하여 제조하는데 본 발명은 수지계 점착제 제조시 반응성 브롬화합물을 첨가, 중합 반응시켜 중합체내에 브롬이 부가되도록 하여 접착력의 저하 없이 난연성과 투명성을 함께 부여하는 방법에 관한 것이다.Generally, rubber or acrylic resin additives are prepared by using natural rubber or synthetic rubber as a raw material or by polymerizing acrylic monomers. In the present invention, when a resin adhesive is prepared, a bromine is added to a polymer by adding and polymerizing a reactive bromine compound, thereby improving adhesion. The present invention relates to a method of providing flame retardancy and transparency without deterioration.

본 발명자는 트리스모노벤질아크릴레이트(Tris monobenzyl acrylate), 펜타브로모벤질아크릴레이트(Penta bromo benzyl acrylate), 트리스브로모페닐말레이미드(Tris bromo phenyl maleimide) 중에서 선택된 것을 중합반응시 또는 합성반응시 고형분 중량의 1∼15중부 첨가하여 점착제를 제조하게 되면 접착력의 저하없이 난연성과 투명성을 함께 유지하는 점착제를 얻을 수 있음을 확인하고 본 발명을 완성하게 되었다.The inventors have selected solids from tris monobenzyl acrylate, penta bromo benzyl acrylate, tris bromo phenyl maleimide during polymerization or synthesis. When the pressure-sensitive adhesive was prepared by adding 1 to 15 parts by weight, it was confirmed that the pressure-sensitive adhesive maintaining flame retardancy and transparency without a decrease in adhesive strength was completed.

이하 실시예를 들어 본 발명을 구체적으로 설명한다.The present invention will be described in detail with reference to the following Examples.

실시예 1. (아크릴계 점착제)Example 1. (acrylic adhesive)

<사용원료><Raw material>

① 2-에틸헥실아크릴레이트(모노머) : 50중량부① 2-ethylhexyl acrylate (monomer): 50 parts by weight

② 부틸아크릴레이트(모노머) : 20중량부② Butyl acrylate (monomer): 20 parts by weight

③ 에틸아크릴레이트(모노머) : 14중량부③ ethyl acrylate (monomer): 14 parts by weight

④ 아크릴아마이드(모노머) : 3중량부④ Acrylamide (monomer): 3 parts by weight

⑤ 비닐아세테이트(모노머) : 13중량부⑤ Vinyl acetate (monomer): 13 parts by weight

⑥ 벤조일퍼옥사이드(중합개시제) : 0.3중량부⑥ Benzoyl peroxide (polymerization initiator): 0.3 parts by weight

⑦ 에틸아세테이트(용제) : 50중량부⑦ Ethyl acetate (solvent): 50 parts by weight

⑧ 톨루엔(용제) : 100중량부⑧ Toluene (solvent): 100 parts by weight

⑨ 펜타브로모벤질아크릴레이트 : 5중량부⑨ Pentabromobenzyl acrylate: 5 parts by weight

이 실시예에서 ①∼⑤ 모노머의 합은 100중량부이고 ⑦∼⑧ 용제의 합은 150중량부이다.In this embodiment, the sum of the monomers 1 to 5 is 100 parts by weight and the sum of the solvents 7 to 8.9 is 150 parts by weight.

상기 모노머 ①∼⑤를 용제(⑦,⑧)에 용해시키고 여기에 반응성 브롬화합물인 펜타브로모벤질아크릴레이트를 첨가하고 약 70℃로 가열하면서 중합개시제를 첨가한다.The monomers (1) to (5) are dissolved in a solvent (7, 8), and pentabromobenzyl acrylate, which is a reactive bromine compound, is added thereto and a polymerization initiator is added while heating to about 70 ° C.

환류 냉각 반응기내에서 70∼80℃ 온도로 반응시키고 중합진행에 따른 점도상승에 맞추어 용제를 주입하면서 10시간 정도 중합반응시켜서 다음 [표 1]에 기재한 성능을 갖는 점착제를 얻었다.In the reflux cooling reactor, the reaction was carried out at a temperature of 70 to 80 ° C. and polymerization was carried out for about 10 hours while injecting a solvent in accordance with the viscosity increase according to the progress of polymerization to obtain a pressure-sensitive adhesive having the performance shown in the following [Table 1].

점착제의 성능비교Performance comparison of adhesive 구분division 점착제 AAdhesive A 점착제 BAdhesive B 점착제 CAdhesive C 점도(CPS)Viscosity (CPS) 4,0004,000 3,8003,800 400400 색상color 투명Transparency 투명Transparency 불투명(백색)Opaque (White) 접착력(g)Adhesive strength (g) 1,5001,500 1,5001,500 500500 난연성Flame retardant UL-94-VoUL-94-Vo 난연성을 갖지 않음Not flame retardant UL-94-VoUL-94-Vo ※ - 점착제 A : 실시예 1의 점착제- 점착제 B : 실시예 1에서 펜타브로모벤질아크릴레이트만 제외시켜 만든 점착제- 점착제 C : 실시예 1에서 펜타브로모벤질아크릴레이트 대신에 DBDPO 6중량부와 Sb2O33중량부를 첨가하여 만든 점착제- 난연성 시험 :UL-94 시험방법에 따름※-pressure-sensitive adhesive A: pressure-sensitive adhesive of Example 1-pressure-sensitive adhesive B: pressure-sensitive adhesive made by excluding the pentabromobenzyl acrylate in Example 1-pressure-sensitive adhesive C: DBDPO 6 parts by weight instead of pentabromobenzyl acrylate in Example 1 Adhesive made by adding 3 parts by weight of Sb 2 O 3 -Flame retardancy test: According to UL-94 test method

실시예 2. (고무계 점착제)Example 2 (rubber-based adhesive)

<사용원료><Raw material>

① 부틸아크릴레이트(모노머) : 10중량부① Butyl acrylate (monomer): 10 parts by weight

② 천연고무 : 10중량부② Natural rubber: 10 parts by weight

③ 톨루엔(용제) : 50중량부③ Toluene (solvent): 50 parts by weight

④ 펜타브로모벤질아크릴레이트 : 5중량부④ pentabromobenzyl acrylate: 5 parts by weight

⑤ 벤조일퍼옥사이드(중합개시제) : 0.2중량부⑤ Benzoyl peroxide (polymerization initiator): 0.2 parts by weight

⑥ 천연고무 : 40중량부⑥ Natural rubber: 40 parts by weight

⑦ 로진변성에스텔 : 40중량부⑦ rosin modified ester: 40 parts by weight

⑧ DOP(디옥틸푸탈레이트) : 3중량부⑧ DOP (dioctylphthalate): 3 parts by weight

⑨ 톨루엔 : 250중량부⑨ Toluene: 250 parts by weight

상기의 ② 천연고무를 ③ 톨루엔에 용해시킨 후 여기에 ① 부틸아크릴레이트모노머 ④ 펜타브로모벤질아크릴레이트 및 ⑤ 벤조일퍼옥사이드를 넣고 환류 반응기 중에서 약 7시간 동안 그라프트 중합시킨다. 이를 냉각시킨 것(이를 반응물 A라 한다), 별도로 ⑥ 천연고무와 ⑦ 로진변성에스텔 ⑧ DOP를 ⑨ 톨루엔에 용해시킨다.(이를 반응물 B라 한다)After dissolving ② natural rubber in ③ toluene, ① butyl acrylate monomer ④ pentabromobenzyl acrylate and ⑤ benzoyl peroxide are added thereto and graft polymerization is performed in a reflux reactor for about 7 hours. This is cooled (referred to as Reactant A), and separately ⑥ natural rubber and ⑦ rosin modified ester ⑧ DOP are dissolved in ⑨ toluene (referred to as Reactant B).

반응물 A와 반응물 B를 혼합하면 본 발명의 점착제가 되는 것이다.When reactant A and reactant B are mixed, it becomes the adhesive of this invention.

점착제의 성능비교Performance comparison of adhesive 구분division 점착제 DAdhesive D 점착제 EAdhesive E 점착제 FAdhesive F 점도(CPS)Viscosity (CPS) 5,0005,000 8,0008,000 7,0007,000 색상color 황색, 투명Yellow, transparent 백색, 불투명White, opaque 황색, 투명Yellow, transparent 접착력(g)Adhesive strength (g) 1,7001,700 700700 1,7001,700 난연성Flame retardant UL-94-VoUL-94-Vo UL-94-VoUL-94-Vo 나타내지 않음Not shown ※ - 점착제 D : 실시예 2의 점착제- 점착제 E : 실시예 2에서 펜타브로모벤질아크릴 대신에 DBDPO 6중량부와 Sb2O33중량부를 첨가하여서 만든 점착제- 점착제 F : 실시예 2에서 펜타브로모벤질아크릴레이트를 제외하고 만든 점착제- 난연성 시험 :UL-94-Vo 시험방법에 따름※-pressure-sensitive adhesive D: pressure-sensitive adhesive of Example 2-pressure-sensitive adhesive E: pressure-sensitive adhesive F made by adding 6 parts by weight of DBDPO and 3 parts by weight of Sb 2 O 3 instead of pentabromobenzyl acryl in Example 2-pressure-sensitive adhesive F: Penta in Example 2 Pressure-sensitive adhesive made of bromobenzyl acrylate except for flame retardancy test: According to UL-94-Vo test method

점착제에 난연성을 부여하기 위하여 DBDPO와 같은 난연제를 사용하게 되면 난연성은 부여되나 점착력이 낮아진다는 단점이 있었으나 본 발명의 방법으로 제조되는 점착제는 난연제를 첨가하지 않은 점착제와 동일성능의 점착력을 가지면서 우수한 난연성을 갖는다는 이점이 있다.If a flame retardant such as DBDPO is used to impart flame retardancy to the pressure-sensitive adhesive, the flame retardancy is imparted but has a disadvantage of low adhesive strength. However, the pressure-sensitive adhesive prepared by the method of the present invention has excellent adhesive strength with the same performance as the pressure-sensitive adhesive without the flame retardant It has the advantage of being flame retardant.

Claims (2)

수지(resin)류를 주성분으로 하는 난연성 점착테이프 제조용 난연성 점착제의 제조방법에 있어서, 수지 제조용 단량체 조성물에 트리스모노벤질아크릴레이트, 펜타브로모벤질아크릴레이트, 트리스브로모페닐말레이미드 중에서 선택된 어느하나를 중합반응시 고형분 중량의 1∼15중량부 첨가 중합반응시켜 난연성을 부여하는 수지계 점착제의 제조방법.In the method for producing a flame-retardant pressure-sensitive adhesive for producing a flame-retardant pressure-sensitive adhesive tape containing resins as the main component, any one selected from trismonobenzyl acrylate, pentabromobenzyl acrylate, and trisbromophenyl maleimide in the monomer composition for resin production A method for producing a resin-based pressure-sensitive adhesive which imparts flame retardancy by adding 1 to 15 parts by weight of a solid content weight during a polymerization reaction. 제1항에 있어서, 수지계 단량체가 아크릴수지계 단량체 이거나 또는 고무계 수지인 수지계 점착제의 제조방법.The method for producing a resin pressure sensitive adhesive according to claim 1, wherein the resin monomer is an acrylic resin monomer or a rubber resin.
KR1019980013238A 1998-04-14 1998-04-14 A manufacturing method for incombustible pressure sensitive adhesive KR100251466B1 (en)

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Publication number Priority date Publication date Assignee Title
KR20030059956A (en) * 2002-01-04 2003-07-12 (주)삼원 Flame retardancy chemistry adhesive manufacture method

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KR101027854B1 (en) 2008-08-20 2011-04-07 주식회사 엘지화학 Composition for acrylic pressure-sensitive adhesive and surface finishing material comprising the same

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20030059956A (en) * 2002-01-04 2003-07-12 (주)삼원 Flame retardancy chemistry adhesive manufacture method

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