KR102519042B1 - Manufacturing method of high-viscosity adhesive with improved dispersion stability - Google Patents
Manufacturing method of high-viscosity adhesive with improved dispersion stability Download PDFInfo
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- 239000000853 adhesive Substances 0.000 title claims abstract description 65
- 230000001070 adhesive effect Effects 0.000 title claims abstract description 65
- 239000006185 dispersion Substances 0.000 title claims abstract description 31
- 238000004519 manufacturing process Methods 0.000 title claims description 14
- 238000003756 stirring Methods 0.000 claims abstract description 74
- 239000000203 mixture Substances 0.000 claims abstract description 69
- 238000002156 mixing Methods 0.000 claims abstract description 62
- 239000003822 epoxy resin Substances 0.000 claims abstract description 34
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 34
- 239000000945 filler Substances 0.000 claims abstract description 31
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 21
- 125000002091 cationic group Chemical group 0.000 claims abstract description 18
- 239000000654 additive Substances 0.000 claims abstract description 16
- 239000012952 cationic photoinitiator Substances 0.000 claims abstract description 16
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 16
- 230000000996 additive effect Effects 0.000 claims abstract description 15
- 239000002994 raw material Substances 0.000 claims abstract description 14
- 239000003085 diluting agent Substances 0.000 claims abstract description 13
- 238000010298 pulverizing process Methods 0.000 claims abstract description 13
- 239000002562 thickening agent Substances 0.000 claims abstract description 13
- 239000003112 inhibitor Substances 0.000 claims abstract description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 50
- 229910021485 fumed silica Inorganic materials 0.000 claims description 21
- -1 glycerin (triphosphate) triacrylate Chemical compound 0.000 claims description 12
- 239000002518 antifoaming agent Substances 0.000 claims description 9
- GUCYFKSBFREPBC-UHFFFAOYSA-N [phenyl-(2,4,6-trimethylbenzoyl)phosphoryl]-(2,4,6-trimethylphenyl)methanone Chemical compound CC1=CC(C)=CC(C)=C1C(=O)P(=O)(C=1C=CC=CC=1)C(=O)C1=C(C)C=C(C)C=C1C GUCYFKSBFREPBC-UHFFFAOYSA-N 0.000 claims description 6
- URQQDYIVGXOEDA-UHFFFAOYSA-N 2-(2-ethenoxyethoxy)ethyl prop-2-enoate Chemical compound C=COCCOCCOC(=O)C=C URQQDYIVGXOEDA-UHFFFAOYSA-N 0.000 claims description 5
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 5
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 5
- 239000000454 talc Substances 0.000 claims description 4
- 229910052623 talc Inorganic materials 0.000 claims description 4
- 239000010425 asbestos Substances 0.000 claims description 3
- 229910052895 riebeckite Inorganic materials 0.000 claims description 3
- 239000004850 liquid epoxy resins (LERs) Substances 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 26
- 230000000704 physical effect Effects 0.000 abstract description 20
- 238000001556 precipitation Methods 0.000 abstract description 6
- 238000000926 separation method Methods 0.000 abstract description 5
- 239000000463 material Substances 0.000 abstract 3
- 239000013530 defoamer Substances 0.000 abstract 1
- 239000002245 particle Substances 0.000 description 14
- 230000000694 effects Effects 0.000 description 10
- 230000002209 hydrophobic effect Effects 0.000 description 9
- 239000000377 silicon dioxide Substances 0.000 description 7
- 229910002029 synthetic silica gel Inorganic materials 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 239000007788 liquid Substances 0.000 description 5
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 4
- 230000001747 exhibiting effect Effects 0.000 description 4
- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 description 4
- 238000013019 agitation Methods 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000009775 high-speed stirring Methods 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 238000003801 milling Methods 0.000 description 3
- 239000004593 Epoxy Substances 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 2
- PXKLMJQFEQBVLD-UHFFFAOYSA-N bisphenol F Chemical compound C1=CC(O)=CC=C1CC1=CC=C(O)C=C1 PXKLMJQFEQBVLD-UHFFFAOYSA-N 0.000 description 2
- LIKFHECYJZWXFJ-UHFFFAOYSA-N dimethyldichlorosilane Chemical compound C[Si](C)(Cl)Cl LIKFHECYJZWXFJ-UHFFFAOYSA-N 0.000 description 2
- 238000010891 electric arc Methods 0.000 description 2
- 235000011187 glycerol Nutrition 0.000 description 2
- 239000005022 packaging material Substances 0.000 description 2
- 238000000197 pyrolysis Methods 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229910002027 silica gel Inorganic materials 0.000 description 2
- 239000000741 silica gel Substances 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 239000004332 silver Substances 0.000 description 2
- 238000005476 soldering Methods 0.000 description 2
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 description 1
- XVZXOLOFWKSDSR-UHFFFAOYSA-N Cc1cc(C)c([C]=O)c(C)c1 Chemical group Cc1cc(C)c([C]=O)c(C)c1 XVZXOLOFWKSDSR-UHFFFAOYSA-N 0.000 description 1
- 239000005909 Kieselgur Substances 0.000 description 1
- 239000004820 Pressure-sensitive adhesive Substances 0.000 description 1
- 239000006004 Quartz sand Substances 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 239000012790 adhesive layer Substances 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910001092 metal group alloy Inorganic materials 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 229920002120 photoresistant polymer Polymers 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000005049 silicon tetrachloride Substances 0.000 description 1
- 239000012258 stirred mixture Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
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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
- C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
- B01F27/60—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a horizontal or inclined axis
- B01F27/75—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a horizontal or inclined axis with stirrers having planetary motion, i.e. rotating about their own axis and about a sun axis
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F33/00—Other mixers; Mixing plants; Combinations of mixers
- B01F33/70—Mixers specially adapted for working at sub- or super-atmospheric pressure, e.g. combined with de-foaming
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F33/00—Other mixers; Mixing plants; Combinations of mixers
- B01F33/80—Mixing plants; Combinations of mixers
- B01F33/836—Mixing plants; Combinations of mixers combining mixing with other treatments
- B01F33/8361—Mixing plants; Combinations of mixers combining mixing with other treatments with disintegrating
- B01F33/83612—Mixing plants; Combinations of mixers combining mixing with other treatments with disintegrating by crushing or breaking
-
- 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
-
- 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
-
- 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
-
- 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
- C09J11/08—Macromolecular additives
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F2101/00—Mixing characterised by the nature of the mixed materials or by the application field
- B01F2101/36—Mixing of ingredients for adhesives or glues; Mixing adhesives and gas
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
Description
본 발명은 분산 안정성이 향상된 고점도 접착제의 제조방법에 관한 것으로, 더욱 상세하게는 고점도를 나타내면서도 접착제의 표면과 내부에 물성차이가 없고, 침전이나 분리현상이 발생되지 않을 뿐만 아니라, 기포제거 공정이 진행되어 우수한 분산안정성을 나타내는 분산 안정성이 향상된 고점도 접착제의 제조방법에 관한 것이다.The present invention relates to a method for producing a high-viscosity adhesive with improved dispersion stability, and more particularly, while exhibiting high viscosity, there is no difference in physical properties between the surface and the inside of the adhesive, no precipitation or separation occurs, and a bubble removal process It relates to a method for producing a high-viscosity adhesive having improved dispersion stability that progresses and exhibits excellent dispersion stability.
접착제는 다양한 산업분야에 적용되며, 서로 다른 부품들을 상호 결합시켜 사용하는데 활용되고 있는데, 볼트와 너트를 이용한 조립이나 납땜을 이용한 접합에 비해 공정이 간단하고, 경량화와 환경 안전 측면에서 유리하기 때문에, 그 사용량은 점차 증가하고 있다.Adhesives are applied in various industrial fields and are used to connect different parts to each other. Compared to assembly using bolts and nuts or joining using soldering, the process is simple, and it is advantageous in terms of light weight and environmental safety. Its usage is gradually increasing.
접착제를 전자제품에 적용하는 경우에는 접착성능 외에 전기 전도성을 부여해야 하는 경우가 있으며, 납땜을 대신한 전기 전도성 접착제의 경우 접착성능을 구현하는 에폭시 수지에 플레이크 형태의 은 미립자를 첨가하여 전기 전도성을 부여하는 방법이 주로 이용되고 있다.When adhesives are applied to electronic products, there are cases where electrical conductivity needs to be imparted in addition to adhesive performance. In the case of electrically conductive adhesives instead of soldering, flake-shaped silver particles are added to epoxy resin that realizes adhesive performance to improve electrical conductivity. The method of giving is mainly used.
상기의 과정에서 접착제에 전도성을 부여하기 위해서는 투입된 은 미립자들이 서로 연결되거나 서로 접촉되어 전류를 통할 수 있을 정도로 다량이 투입되어야 한다.In order to impart conductivity to the adhesive in the above process, a large amount of the injected silver particles must be connected or contacted with each other to allow current to pass through.
또한, 전자 제품의 작동 중에는 필연적으로 열을 발생시키는 경우가 많고, 발생된 열을 외부로 방출시키는 기술이 요구되며, 최근에는 전자제품의 소형화 추세에 따라, 작동 중 발생하는 열을 효과적으로 확산시켜 제거하기 위해 접착제에 높은 열 전도성을 요구하고 있는데, 일 예로 전자제품 제조시 반도체 칩을 부착하는데 사용하는 접착제의 경우 높은 열전도성을 가지는 것이 바람직하여, 열전도성이 양호한 미립자 형상의 은, 카본 블랙, 또는 금속 합금을 첨가한 접착제를 개발하고 있다. 그러나, 유기 고분자에 분산된 무기 또는 금속 미립자들의 충전제들은 일반적으로 전자와 양전자의 이동이 수월하지 못하고 계면 저항이 높은 것으로 인식되고 있다.In addition, there are many cases where electronic products inevitably generate heat during operation, and a technology for releasing the generated heat to the outside is required. Recently, according to the trend of miniaturization of electronic products, the heat generated during operation is effectively diffused and removed. In order to do this, high thermal conductivity is required for adhesives. For example, in the case of adhesives used for attaching semiconductor chips in the manufacture of electronic products, it is preferable to have high thermal conductivity. We are developing adhesives with added metal alloys. However, fillers of inorganic or metal fine particles dispersed in organic polymers are generally recognized to have high interfacial resistance and poor electron and positron movement.
한편, 기존의 LED 패키징 소재용 접착제로는 실리콘계와 에폭시계 수지가 일반적이지만, 대부분 방열특성이 낮고, 이로 인해 제품의 수명이 길지 못한 문제점이 있었다.On the other hand, silicone-based and epoxy-based resins are common as conventional adhesives for LED packaging materials, but most of them have low heat dissipation characteristics, resulting in a problem in that product life is not long.
뿐만 아니라, 종래에 LED 패키징 소재용 접착제의 경우에는 접착제의 표면과 내부의 물성에서 차이점을 나타내어 균일한 전도성이나 전열성능을 나타내지 못하며, 침전이나 상분이 등이 발생하여 분산안정성이 낮은 문제점이 있었다.In addition, conventional adhesives for LED packaging materials show differences in physical properties between the surface and the inside of the adhesive, so they do not exhibit uniform conductivity or heat transfer performance, and there is a problem of low dispersion stability due to precipitation or phase powder.
본 발명의 목적은 고점도를 나타내면서도 접착제의 표면과 내부에 물성차이가 없고, 침전이나 분리현상이 발생되지 않을 뿐만 아니라, 기포제거 공정이 진행되어 우수한 분산안정성을 나타내는 분산 안정성이 향상된 고점도 접착제의 제조방법을 제공하는 것이다.An object of the present invention is to manufacture a high-viscosity adhesive with improved dispersion stability that exhibits high viscosity, no difference in physical properties between the surface and the inside of the adhesive, no precipitation or separation, and excellent dispersion stability through a bubble removal process. is to provide a way
본 발명의 목적은 에폭시 수지 혼합물, 희석제 및 소포제를 혼합하는 원료혼합단계, 상기 원료혼합단계를 통해 제조된 혼합물을 플레네터리 믹서로 저속교반하는 제1교반단계, 상기 제1교반단계를 통해 교반된 혼합물에 충전재를 혼합하는 충전재혼합단계, 상기 충전재혼합단계를 통해 제조된 혼합물을 플레네터리 믹서로 저속교반하는 제2교반단계, 상기 제2교반단계를 통해 교반된 혼합물에 광개시제, 양이온 광개시제, 양이온 경화제, 중합억제제 및 증점제를 혼합하는 첨가제혼합단계, 상기 첨가제혼합단계를 통해 제조된 혼합물을 플레네터리 믹서로 고속교반하여 내부 기포를 제거하는 제3교반단계, 상기 제3교반단계를 통해 기포가 제거된 혼합물을 3-롤-밀로 분쇄 및 분산하는 분쇄분산단계 및 상기 분쇄분산단계를 통해 분쇄 및 분산된 혼합물을 플레네터리 믹서로 진공교반하는 진공교반단계로 이루어지는 것을 특징으로 하는 분산 안정성이 향상된 고점도 접착제의 제조방법을 제공함에 의해 달성된다.An object of the present invention is a raw material mixing step of mixing an epoxy resin mixture, a diluent and an antifoaming agent, a first stirring step of stirring the mixture prepared through the raw material mixing step at low speed with a planetary mixer, and stirring through the first stirring step A filler mixing step of mixing a filler with the prepared mixture, a second stirring step of stirring the mixture prepared through the filler mixing step at low speed with a planetary mixer, a photoinitiator, a cationic photoinitiator, An additive mixing step of mixing a cationic curing agent, a polymerization inhibitor, and a thickener, a third stirring step of removing internal bubbles by stirring the mixture prepared through the additive mixing step at high speed with a planetary mixer, and bubbles through the third stirring step Dispersion stability, characterized in that it consists of a pulverization and dispersion step of pulverizing and dispersing the removed mixture with a 3-roll-mill and a vacuum stirring step of vacuum stirring the pulverized and dispersed mixture through the pulverization and dispersion step with a planetary mixer It is achieved by providing a method for producing an improved high-viscosity adhesive.
본 발명의 바람직한 특징에 따르면, 상기 원료혼합단계는 에폭시 수지 혼합물 100 중량부, 희석제 10 내지 30 중량부 및 소포제 0.2 내지 1 중량부로 이루어지는 것으로 한다.According to a preferred feature of the present invention, the raw material mixing step is to consist of 100 parts by weight of the epoxy resin mixture, 10 to 30 parts by weight of the diluent and 0.2 to 1 part by weight of the antifoaming agent.
본 발명의 더 바람직한 특징에 따르면, 상기 에폭시 수지 혼합물은 에폭시 수지와 액상형 에폭시 수지가 1:1의 비율로 혼합되어 이루어지는 것으로 한다.According to a more preferred feature of the present invention, the epoxy resin mixture is made by mixing an epoxy resin and a liquid type epoxy resin in a ratio of 1:1.
본 발명의 더욱 바람직한 특징에 따르면, 상기 희석제는 글리세린(3인산)트리아크릴레이트 100 중량부 및 2-(2-비닐옥시에톡시)에틸아크릴레이트 20 내지 50 중량부로 이루어지는 것으로 한다.According to a more preferred feature of the present invention, the diluent is made of 100 parts by weight of glycerin (triphosphate) triacrylate and 20 to 50 parts by weight of 2-(2-vinyloxyethoxy)ethyl acrylate.
본 발명의 더욱 더 바람직한 특징에 따르면, 상기 제1교반단계 및 제2교반단계는 500 내지 1500rpm의 속도로 30 내지 120초 동안 이루어지는 것으로 한다.According to a more preferred feature of the present invention, the first stirring step and the second stirring step are made for 30 to 120 seconds at a speed of 500 to 1500 rpm.
본 발명의 더욱 더 바람직한 특징에 따르면, 상기 첨가제혼합단계는 상기 제2교반단계를 통해 교반된 혼합물에 함유된 에폭시 수지 100 중량부 대비 광개시제 0.02 내지 0.2 중량부, 양이온 광개시제 1 내지 6 중량부, 양이온 경화제 1 내지 6 중량부, 중합억제제 0.01 내지 0.2 중량부 및 증점제 0.1 내지 40 중량부를 혼합하여 이루어지는 것으로 한다.According to a more preferred feature of the present invention, in the additive mixing step, 0.02 to 0.2 parts by weight of a photoinitiator, 1 to 6 parts by weight of a cationic photoinitiator, cations, based on 100 parts by weight of the epoxy resin contained in the mixture stirred through the second stirring step. It is made by mixing 1 to 6 parts by weight of a curing agent, 0.01 to 0.2 parts by weight of a polymerization inhibitor and 0.1 to 40 parts by weight of a thickener.
본 발명의 더욱 더 바람직한 특징에 따르면, 상기 소수성 제제는 폴리디메틸실록산, 헥사메틸디실라잔 및 디메틸디클로로실란으로 이루어진 그룹에서 선택된 하나로 이루어지는 것으로 한다.According to a more preferred feature of the present invention, the hydrophobic agent is made of one selected from the group consisting of polydimethylsiloxane, hexamethyldisilazane and dimethyldichlorosilane.
본 발명의 더욱 더 바람직한 특징에 따르면, 상기 증점제는 소수성 제제로 처리된 흄드 실리카로 이루어지는 것으로 한다.According to a further preferred feature of the present invention, the thickener is made of fumed silica treated with a hydrophobic agent.
본 발명의 더욱 더 바람직한 특징에 따르면, 상기 제3교반단계는 3000 내지 10000rpm의 속도로 30 내지 120초 동안 이루어지는 것으로 한다.According to a more preferred feature of the present invention, the third stirring step is to be made for 30 to 120 seconds at a speed of 3000 to 10000rpm.
본 발명의 더욱 더 바람직한 특징에 따르면, 상기 진공교반단계는 진공상태에서 500 내지 1500rpm의 속도로 30 내지 60초 동안 이루어지는 것으로 한다.According to a more preferred feature of the present invention, the vacuum stirring step is to be made for 30 to 60 seconds at a speed of 500 to 1500rpm in a vacuum state.
본 발명에 따른 분산 안정성이 향상된 고점도 접착제의 제조방법은 고점도를 나타내면서도 접착제의 표면과 내부에 물성차이가 없고, 침전이나 분리현상이 발생되지 않을 뿐만 아니라, 기포제거 공정이 진행되어 우수한 분산안정성을 나타내는 접착제를 제공하는 탁월한 효과를 나타낸다.The manufacturing method of the high-viscosity adhesive with improved dispersion stability according to the present invention shows high viscosity, but there is no difference in physical properties between the surface and the inside of the adhesive, and no precipitation or separation occurs. It exhibits an excellent effect of providing an adhesive that exhibits
도 1은 본 발명에 따른 분산 안정성이 향상된 고점도 접착제의 제조방법을 나타낸 순서도이다.1 is a flow chart showing a method for producing a high-viscosity adhesive having improved dispersion stability according to the present invention.
이하에는, 본 발명의 바람직한 실시예와 각 성분의 물성을 상세하게 설명하되, 이는 본 발명이 속하는 기술분야에서 통상의 지식을 가진 자가 발명을 용이하게 실시할 수 있을 정도로 상세하게 설명하기 위한 것이지, 이로 인해 본 발명의 기술적인 사상 및 범주가 한정되는 것을 의미하지는 않는다.Hereinafter, a preferred embodiment of the present invention and the physical properties of each component will be described in detail, but this is to be explained in detail so that a person having ordinary knowledge in the art to which the present invention belongs can easily practice the invention, This is not meant to limit the technical spirit and scope of the present invention.
본 발명에 따른 분산 안정성이 향상된 고점도 접착제의 제조방법은 에폭시 수지 혼합물, 희석제 및 소포제를 혼합하는 원료혼합단계(S101), 상기 원료혼합단계(S101)를 통해 제조된 혼합물을 플레네터리 믹서로 저속교반하는 제1교반단계(S103), 상기 제1교반단계(S103)를 통해 교반된 혼합물에 충전재를 혼합하는 충전재혼합단계(S105), 상기 충전재혼합단계(S105)를 통해 제조된 혼합물을 플레네터리 믹서로 저속교반하는 제2교반단계(S107), 상기 제2교반단계(S107)를 통해 교반된 혼합물에 광개시제, 양이온 광개시제, 양이온 경화제, 중합억제제 및 증점제를 혼합하는 첨가제혼합단계(S109), 상기 첨가제혼합단계(S109)를 통해 제조된 혼합물을 플레네터리 믹서로 고속교반하여 내부 기포를 제거하는 제3교반단계(S111), 상기 제3교반단계(S111)를 통해 기포가 제거된 혼합물을 3-롤-밀로 분쇄 및 분산하는 분쇄분산단계(S113) 및 상기 분쇄분산단계(S113)를 통해 분쇄 및 분산된 혼합물을 플레네터리 믹서로 진공교반하는 진공교반단계(S115)로 이루어진다.The method for producing a high-viscosity adhesive having improved dispersion stability according to the present invention includes a raw material mixing step (S101) of mixing an epoxy resin mixture, a diluent and an antifoaming agent, and the mixture prepared through the raw material mixing step (S101) is mixed with a planetary mixer at low speed. A first stirring step (S103) of stirring, a filler mixing step (S105) of mixing a filler with the mixture stirred through the first stirring step (S103), and the mixture prepared through the filler mixing step (S105) Plane A second stirring step (S107) of low-speed stirring with a terry mixer, an additive mixing step (S109) of mixing a photoinitiator, a cationic photoinitiator, a cationic curing agent, a polymerization inhibitor, and a thickener with the mixture stirred through the second stirring step (S107), A third stirring step (S111) of removing internal bubbles by stirring the mixture prepared through the additive mixing step (S109) at high speed with a planetary mixer, and the mixture from which bubbles are removed through the third stirring step (S111) It consists of a pulverization and dispersion step (S113) of pulverization and dispersion with a 3-roll-mill and a vacuum agitation step (S115) of vacuum agitation of the mixture pulverized and dispersed through the pulverization and dispersion step (S113) with a planetary mixer.
상기 원료혼합단계(S101)는 에폭시 수지 혼합물, 희석제 및 소포제를 혼합하는 단계로, 에폭시 수지 혼합물 100 중량부, 희석제 10 내지 30 중량부 및 소포제 0.2 내지 1 중량부로 이루어지는 것이 바람직하다.The raw material mixing step (S101) is a step of mixing an epoxy resin mixture, a diluent and an antifoaming agent, preferably composed of 100 parts by weight of the epoxy resin mixture, 10 to 30 parts by weight of the diluent, and 0.2 to 1 part by weight of the antifoaming agent.
상기 에폭시 수지 혼합물은 본 발명을 통해 제조되는 분산 안정성이 향상된 고점도 접착제의 주재료가 되는 성분으로, 에폭시 수지와 액상형 에폭시 수지가 1:1의 비율로 혼합되어 이루어지는 것이 바람직하다.The epoxy resin mixture is a main component of the high-viscosity adhesive having improved dispersion stability prepared through the present invention, and is preferably made by mixing an epoxy resin and a liquid type epoxy resin in a ratio of 1:1.
상기 에폭시 수지는 비스페놀 A, F, 셀록사이드 계열의 에폭시 수지가 사용될 수 있다. 또한, 상기 액상형 에폭시 수지는 덕산 YDF-170이 사용될 수 있는데, 전열특성이 양호한 충전재를 혼합하여 에폭시수지의 매트릭스 내부에 포함하고 있을 경우, 상기 충전재가 에폭시수지의 매트릭스 내부의 안정된 액상에 의해 원래의 위치를 그대로 유지시켜줌으로써, 상기 충전재가 비중의 차이로 인해 에폭시수지에 혼합된 이후 시간이 경과하더라도 매트릭스 내부에서 분리되어 점차적으로 침전되는 현상을 방지해주는 현상을 억제하는 역할을 한다.As the epoxy resin, a bisphenol A, F, or celoxide-based epoxy resin may be used. In addition, Duksan YDF-170 can be used as the liquid type epoxy resin. When a filler having good heat transfer properties is mixed and included inside the matrix of the epoxy resin, the filler is a stable liquid phase inside the matrix of the epoxy resin to restore the original state. By maintaining the position as it is, it serves to suppress the phenomenon of preventing the phenomenon that the filler is separated from the inside of the matrix and gradually precipitated even after time elapses after being mixed with the epoxy resin due to the difference in specific gravity.
또한, 상기 희석제는 10 내지 30 중량부가 함유되며, 상기 에폭시 수지 혼합물을 희석시켜 점도를 납추면서도 접착성능은 크게 저하시키지 않도록 하는 역할을 하는데, 글리세린(3인산)트리아크릴레이트 100 중량부 및 2-(2-비닐옥시에톡시)에틸아크릴레이트 20 내지 50 중량부로 이루어지는 것이 바람직하다.In addition, the diluent contains 10 to 30 parts by weight, and serves to dilute the epoxy resin mixture to reduce the viscosity while not significantly reducing the adhesive performance, 100 parts by weight of glycerin (triphosphate) triacrylate and 2- It is preferably composed of 20 to 50 parts by weight of (2-vinyloxyethoxy)ethyl acrylate.
상기 희석제의 함량이 10 중량부 미만이면 접착제의 점도가 지나치게 높아 첨가제나 증점제 및 충진재 등이 고르게 혼합되지 못하기 때문에 균일한 물성을 나타내지 못하며, 상기 희석제의 함량이 30 중량부를 초과하게 되면 상대적으로 에폭시 수지 혼합물의 함량이 지나치게 낮아져 상기의 효과는 크게 향상되지 않으면서 점착제의 물성과 점도가 지나치게 저하될 수 있기 때문에 바람직하지 못하다.If the content of the diluent is less than 10 parts by weight, the viscosity of the adhesive is too high, so that additives, thickeners, fillers, etc. cannot be mixed evenly, so that uniform physical properties cannot be exhibited. It is undesirable because the content of the resin mixture is too low, and the physical properties and viscosity of the pressure-sensitive adhesive may be excessively reduced while the above effects are not greatly improved.
또한, 상기 소포제는 0.2 내지 1 중량부가 함유되는데, 본 발명을 통해 제조되는 접착제에 기포가 형성되는 것을 억제하여 분산성이 향상될 수 있도록 하는 역할을 하는데, BYK의 BYK-1790이 사용될 수 있다.In addition, the antifoaming agent is contained in an amount of 0.2 to 1 part by weight, and serves to improve dispersibility by suppressing the formation of bubbles in the adhesive prepared through the present invention, and BYK-1790 of BYK may be used.
상기 소포제의 함량이 0.2 중량부 미만이면 상기의 효과가 미미하며, 상기 소포제의 함량이 1 중량부를 초과하게 되면 상기의 효과는 크게 향상되지 않으면서 점착제의 물성이 저하될 수 있다.If the content of the antifoamer is less than 0.2 parts by weight, the above effect is insignificant, and if the content of the antifoamer exceeds 1 part by weight, the above effect may not be greatly improved and the physical properties of the adhesive may be deteriorated.
상기 제1교반단계(S103)는 상기 원료혼합단계(S101)를 통해 제조된 혼합물을 플레네터리 믹서(Planetary mixer)로 저속교반하는 단계로, 상기 원료혼합단계(S101)를 통해 제조된 혼합물을 플레네터리 믹서에 투입하고 500 내지 1500rpm의 속도로 30 내지 120초 동안 교반하는 과정으로 이루어지는 것이 바람직하다.The first stirring step (S103) is a step of stirring the mixture prepared through the raw material mixing step (S101) at low speed with a planetary mixer, and the mixture prepared through the raw material mixing step (S101) It is preferably composed of a process of adding to a planetary mixer and stirring for 30 to 120 seconds at a speed of 500 to 1500 rpm.
상기의 과정으로 이루어지는 제1교반단계(S103)를 거치면 상기 원료혼합단계(S101)를 통해 제조된 혼합물의 고르게 혼합되어 균일한 물성의 접착제를 제공할 수 있다.After the first stirring step (S103) consisting of the above process, the mixture prepared through the raw material mixing step (S101) is evenly mixed to provide an adhesive with uniform physical properties.
상기 충전재혼합단계(S105)는 상기 제1교반단계(S103)를 통해 교반된 혼합물에 충전재를 혼합하는 단계로, 상기 제1교반단계(S103)를 통해 교반된 혼합물에 함유된 에폭시 수지 혼합물 100 중량부 대비 충전재 0.1 내지 40 중량부를 혼합하여 이루어지는 것이 바람직한데, 상기와 같이 충전재가 함유되면 본 발명의 접착제로 이루어진 접착층의 내열성, 치수안정성, 및 굴곡 탄성률과 같은 물성이 향상될 수 있다.The filler mixing step (S105) is a step of mixing the filler with the mixture stirred through the first stirring step (S103), and 100 weight of the epoxy resin mixture contained in the mixture stirred through the first stirring step (S103). It is preferably made by mixing 0.1 to 40 parts by weight of the filler per part, and when the filler is contained as described above, physical properties such as heat resistance, dimensional stability, and flexural modulus of the adhesive layer made of the adhesive of the present invention can be improved.
이때, 상기 충전재는 비석면 타입의 활석으로 이루어지는 것이 바람직하며, KOCH의 KC3000이 사용될 수 있는데, 상기 충전재의 함량이 40 중량부를 초과하게 되면 상기의 효과는 크게 향상되지 않으면서 본 발명을 통해 제조되는 접착제의 접착력이 지나치게 저하될 수 있기 때문에 바람직하지 못하다.At this time, the filler is preferably made of non-asbestos type talc, and KOCH's KC3000 may be used. When the content of the filler exceeds 40 parts by weight, the effect is not greatly improved, and the present invention This is not preferable because the adhesive force of the adhesive may be excessively lowered.
상기 제2교반단계(S107)는 상기 충전재혼합단계(S105)를 통해 제조된 혼합물을 플레네터리 믹서로 저속교반하는 단계로, 상기 충전재혼합단계(S105)를 통해 제조된 혼합물을 플레네터리 믹서에 투입하고 500 내지 1500rpm의 속도로 30 내지 120초 동안 교반하는 과정으로 이루어지는 것이 바람직하다.The second stirring step (S107) is a step of stirring the mixture prepared through the filler mixing step (S105) at a low speed with a planetary mixer, and the mixture prepared through the filler mixing step (S105) is a planetary mixer It is preferably composed of a process of adding to and stirring for 30 to 120 seconds at a speed of 500 to 1500 rpm.
상기의 과정으로 이루어지는 제2교반단계(S107)를 거치면 상기 충전재혼합단계(S105)를 통해 제조된 혼합물에 함유된 충전재 성분의 분산성이 향상되어 균일한 물성의 접착제를 제공할 수 있다.After passing through the second stirring step (S107) consisting of the above process, the dispersibility of the filler component contained in the mixture prepared through the filler mixing step (S105) is improved to provide an adhesive with uniform physical properties.
상기 첨가제혼합단계(S109)는 상기 제2교반단계(S107)를 통해 교반된 혼합물에 광개시제, 양이온 광개시제, 양이온 경화제, 중합억제제 및 증점제를 혼합하는 단계로. 상기 제2교반단계(S107)를 통해 교반된 혼합물에 함유된 에폭시 수지 100 중량부 대비 광개시제 0.02 내지 0.2 중량부, 양이온 광개시제 1 내지 6 중량부, 양이온 경화제 1 내지 6 중량부, 중합억제제 0.01 내지 0.2 중량부 및 증점제 0.1 내지 40 중량부를 혼합하여 이루어지는 것이 바람직하다.The additive mixing step (S109) is a step of mixing a photoinitiator, a cationic photoinitiator, a cationic curing agent, a polymerization inhibitor, and a thickener with the mixture stirred through the second stirring step (S107). 0.02 to 0.2 parts by weight of a photoinitiator, 1 to 6 parts by weight of a cationic photoinitiator, 1 to 6 parts by weight of a cationic curing agent, 0.01 to 0.2 parts by weight of a polymerization inhibitor, based on 100 parts by weight of the epoxy resin contained in the mixture stirred through the second stirring step (S107) It is preferably formed by mixing parts by weight and 0.1 to 40 parts by weight of a thickener.
상기의 과정으로 이루어지는 첨가제혼합단계(S109)는 열과 빛에 민감한 광개시제, 양이온 광개시제, 양이온 경화제 등의 성분을 상기 제1교반단계(S103) 및 제2교반단계(S107) 이후에 혼합하기 때문에, 교반과정에서 광개시제, 양이온 광개시제, 양이온 경화제 등에 에너지가 전달되어 중합이 진행되는 현상을 개선할 수 있다.In the additive mixing step (S109) consisting of the above process, since components such as a photoinitiator, a cationic photoinitiator, and a cationic curing agent that are sensitive to heat and light are mixed after the first stirring step (S103) and the second stirring step (S107), stirring In the process, energy is transferred to a photoinitiator, a cationic photoinitiator, a cationic curing agent, etc., thereby improving a phenomenon in which polymerization proceeds.
상기 광개시제는 0.02 내지 0.2 중량부가 함유되며, 비스(2,4,6-트리메틸벤조일)-페닐포스핀옥사이드{Bis(2,4,6-trimethylbenzoyl)-phenylphosphineoxide}로 이루어지는 것이 바람직한데, 본 발명을 통해 제조되는 접착제가 광의 조사에 의해 경화될 수 있도록 하는 역할을 한다.The photoinitiator is contained in an amount of 0.02 to 0.2 parts by weight, and is preferably composed of bis(2,4,6-trimethylbenzoyl)-phenylphosphineoxide {Bis(2,4,6-trimethylbenzoyl)-phenylphosphineoxide}, the present invention It serves to allow the adhesive produced through the curing by irradiation of light.
상기 광개시제의 함량이 0.02 중량부 미만이면 광의 조사시 접착제의 경화가 지나치게 더디게 진행되며, 상기 광개시제의 함량이 0.2 중량부를 초과하게 되면 상기의 효과는 크게 향상되지 않으면서 접착제의 물성을 저하시킬 수 있다.If the content of the photoinitiator is less than 0.02 parts by weight, the curing of the adhesive proceeds too slowly when irradiated with light, and if the content of the photoinitiator exceeds 0.2 parts by weight, the above effect is not greatly improved, and the physical properties of the adhesive can be reduced. .
또한, 상기 양이온 광개시제 1 내지 6 중량부가 함유되며, 본 발명을 통해 제조되는 접착제에 양이온 경화 반응성능을 부여하는 역할을 하는데, 상온에서 높은 양이온 경화 반응성을 나타내며 안티몬이 함유되어 있지 않아 친환경적인 것을 사용하는 것이 바람직하며, CIBA의 Irgacure 290을 사용할 수 있다.In addition, 1 to 6 parts by weight of the cationic photoinitiator is contained, and serves to impart cationic curing reaction performance to the adhesive prepared through the present invention. It shows high cationic curing reactivity at room temperature and does not contain antimony. It is preferable, and CIBA's Irgacure 290 can be used.
상기 양이온 광개시제의 함량이 1 중량부 미만이면 양이온 경화 반응성능이 지나치게 낮고, 상기 양이온 광개시제의 함량이 6 중량부를 초과하게 되면 상기의 효과는 크게 향상되지 않으면서 접착제의 물성을 저하시킬 수 있기 때문에 바람직하지 못하다.If the content of the cationic photoinitiator is less than 1 part by weight, the cationic curing reaction performance is too low, and if the content of the cationic photoinitiator exceeds 6 parts by weight, the above effect is not greatly improved and the physical properties of the adhesive can be reduced. can't
또한, 상기 양이온 경화제는 1 내지 6 중량부가 함유되며, 양이온성 에폭시와 같은 열경화형 접착제, 포토레지스트, 패키징, 이방성 도전성 접착제에 양이온 경화성능을 부여하는 역할을 하는데, SAN의 AID SI-360을 사용하는 것이 바람직하다.In addition, the cationic curing agent is contained in an amount of 1 to 6 parts by weight, and serves to impart cationic curing performance to thermosetting adhesives such as cationic epoxy, photoresist, packaging, and anisotropic conductive adhesives, using SAN's AID SI-360 It is desirable to do
상기 양이온 경화제의 함량이 1 중량부 미만이면 상기의 효과가 미미하며, 상기 양이온 경화제의 함량이 6 중량부를 초과하게 되면 상기의 효과는 크게 향상되지 않으면서 접착제의 물성을 저하시킬 수 있다.If the content of the cationic curing agent is less than 1 part by weight, the above effect is insignificant, and if the content of the cationic curing agent exceeds 6 parts by weight, the above effect is not greatly improved and the physical properties of the adhesive may be reduced.
또한, 상기 중합억제제는 0.01 내지 0.2 중량부가 함유되며, 본 발명에 따른 접착제에서 광개시제나 양이온광개시제로 인해 중합반응이 지나치게 진행되어 점도가 지나치게 향상되지 않도록 중합반응을 조절하는 역할을 하는데, 상기 중합억제제의 함량이 0.01 중량부 미만이면 상기의 효과가 미미하며, 상기 중합억제제의 함량이 0.2 중량부를 초과하게 되면 광개시제나 양이온광개시제로 인한 중합개시 효과가 지나치게 저하될 수 있기 때문에 바람직하지 못하다.In addition, the polymerization inhibitor is contained in an amount of 0.01 to 0.2 parts by weight, and in the adhesive according to the present invention, the polymerization reaction proceeds excessively due to the photoinitiator or cationic photoinitiator and serves to control the polymerization reaction so that the viscosity is not excessively improved. If the content of is less than 0.01 parts by weight, the above effect is insignificant, and if the content of the polymerization inhibitor exceeds 0.2 parts by weight, the polymerization initiating effect due to the photoinitiator or cationic photoinitiator may be excessively reduced, which is not preferable.
이때, 상기 중합억제제는 SAN의 AID SI-S로 이루어질 수 있다.At this time, the polymerization inhibitor may be made of AID SI-S of SAN.
또한, 상기 증점제는 0.1 내지 40 중량부가 함유되며, 본 발명을 통해 제조되는 접착제가 일정한 점도를 나타내어 접착성능이 유지될 수 있도록 하는 역할을 하는데, 소수성 제제로 처리된 흄드 실리카로 이루어지는 것이 바람직하다.In addition, the thickener is contained in an amount of 0.1 to 40 parts by weight, and serves to maintain adhesive performance by exhibiting a constant viscosity of the adhesive prepared through the present invention, preferably made of fumed silica treated with a hydrophobic agent.
이때, 상기 소수성 제제는 폴리디메틸실록산, 헥사메틸디실라잔 및 디메틸디클로로실란으로 이루어진 그룹에서 선택된 하나로 이루어지는 것이 바람직하다.At this time, the hydrophobic agent is preferably made of one selected from the group consisting of polydimethylsiloxane, hexamethyldisilazane and dimethyldichlorosilane.
일반적으로, 흄드 실리카는 합성 비정질 실리카의 일종으로, 합성 비정질 실리카(SAS)는 의도적으로 제조된 이산화규소(SiO2)의 한 형태로 자연 발생 비정질 실리카, 예를 들어, 규조토와 구별하게 한다. 인공 제품으로서 SAS는 거의 100% 순수한 비정질 실리카인 반면 자연 발생 비정질 실리카는 또한 결정질 형태의 실리카를 함유한다. SAS는 (1) 습식 공정 실리카(침강 실리카 및 실리카 겔 포함) 및 (2) 열 공정 실리카(흄드 실리카라고도 알려진 발열성 실리카 포함)의 두 가지 별개의 제조 관행을 특징으로 하는 두 가지 형태로 제조될 수 있다. 따라서, 흄드 실리카는 습식 공정과 반대로 열 공정에 의해 형성된 SAS다.In general, fumed silica is a type of synthetic amorphous silica, where synthetic amorphous silica (SAS) is an intentionally manufactured form of silicon dioxide (SiO 2 ), distinguishing it from naturally occurring amorphous silica, such as diatomaceous earth. As a man-made product, SAS is almost 100% pure amorphous silica, whereas naturally occurring amorphous silica also contains silica in crystalline form. SAS will be manufactured in two forms characterized by two distinct manufacturing practices: (1) wet process silica (including precipitated silica and silica gel) and (2) thermal process silica (including pyrogenic silica, also known as fumed silica). can Thus, fumed silica is SAS formed by a thermal process as opposed to a wet process.
흄드 실리카를 제조하기 위한 열 공정은 화염 열분해를 사용한다. 구체적으로, 흄드 실리카는 사염화규소의 화염 열분해 또는 3000℃ 전기 아크(arc)에서 기화된 석영 모래로 제조된다. 전기 아크에 비정질 실리카의 미세한 액적을 노출시키면 액적이 분지된 사슬형의 3차원 입자로 융합된 다음 3차 입자로 더 덩어리지게 된다. 그 결과, 흄드 실리카 입자는 실리카겔과 같은 습식 공정 실리카 입자보다 낮은 벌크 밀도 및 높은 표면적을 가지며, 침강 실리카에 비해 더 높은 순도를 갖는다. 흄드 실리카 입자는 또한 비다공성인 반면 습식 공정 실리카 입자는 다공성이다. 흄드 실리카 입자를 만드는 데 사용되는 열 공정의 결과로 흄드 실리카 입자는 특별히 처리되지 않는 한 본질적으로 친수성이다. 소수성 흄드 실리카 입자를 형성하기 위해, 흄드 실리카 입자(친수성)는 소수성 제제로 화학적 후처리를 거친다. 알콕시실란, 실라잔 또는 실록산과 같은 소수성 제제는 흄드 실리카 입자 상의 이산화규소 분자의 산화물기와 공유 결합하여 흄드 실리카 입자를 소수성으로 만든다. 본 발명에서 사용되는 소수성 처리된 흄드 실리카는 하나 이상의 산소 공유 결합을 통해 입자 표면에 결합된 소수성 제제를 갖는 입자 형태의 비다공성 흄드 실리카다.Thermal processes for producing fumed silica use flame pyrolysis. Specifically, fumed silica is produced from flame pyrolysis of silicon tetrachloride or quartz sand vaporized in an electric arc at 3000°C. When fine droplets of amorphous silica are exposed to an electric arc, the droplets fuse into branched, chain-like three-dimensional particles and then agglomerate further into three-dimensional particles. As a result, fumed silica particles have a lower bulk density and higher surface area than wet processed silica particles such as silica gel, and a higher purity than precipitated silica. Fumed silica particles are also non-porous whereas wet processed silica particles are porous. As a result of the thermal process used to make fumed silica particles, fumed silica particles are inherently hydrophilic unless specially treated. To form hydrophobic fumed silica particles, the fumed silica particles (hydrophilic) undergo a chemical post-treatment with a hydrophobic agent. A hydrophobic agent such as an alkoxysilane, silazane or siloxane makes the fumed silica particles hydrophobic by covalently bonding with oxide groups of silicon dioxide molecules on the fumed silica particles. The hydrophobically treated fumed silica used in the present invention is non-porous fumed silica in the form of particles having a hydrophobic agent bonded to the surface of the particle through one or more covalent oxygen bonds.
상기 제3교반단계(S111)는 상기 첨가제혼합단계(S109)를 통해 제조된 혼합물을 플레네터리 믹서로 고속교반하여 내부 기포를 제거하는 단계로, 상기 첨가제혼합단계(S109)를 통해 제조된 혼합물을 플레네터리 믹서에 투입하고 3000 내지 10000rpm의 속도로 30 내지 120초 동안 고속교반하여 이루어지는 것이 바람직하다.The third stirring step (S111) is a step of stirring the mixture prepared through the additive mixing step (S109) at high speed with a planetary mixer to remove internal bubbles, the mixture prepared through the additive mixing step (S109) It is preferably formed by introducing into a planetary mixer and stirring at a high speed of 3000 to 10000 rpm for 30 to 120 seconds.
상기의 과정을 통해 상기 첨가제혼합단계(S109)를 통해 제조된 혼합물이 고르게 혼합될 뿐만 아니라, 혼합물에 잔존하는 기포가 제거되어 균일한 물성을 나타내는 접착제가 제공될 수 있다.Through the above process, the mixture prepared through the additive mixing step (S109) is evenly mixed, and air bubbles remaining in the mixture are removed, thereby providing an adhesive exhibiting uniform physical properties.
상기 분쇄분산단계(S113)는 상기 제3교반단계(S111)를 통해 기포가 제거된 혼합물을 3-롤-밀로 분쇄 및 분산하는 단계로, 상기 제3교반단계(S111)를 통해 기포가 제거된 혼합물을 3-롤-밀(3-ROLL-MILL)로 1 내지 3회에 걸쳐 밀링하여 혼합물을 분쇄 및 분산하는 과정으로 이루어지는 것이 바람직한데, 상기와 같이 3-롤-밀로 분쇄 및 분산된 혼합물은 분산성이 개선된다.The grinding and dispersing step (S113) is a step of grinding and dispersing the mixture from which bubbles are removed through the third stirring step (S111) with a 3-roll-mill. It is preferable to mill the mixture 1 to 3 times with a 3-roll-mill to grind and disperse the mixture. As described above, the mixture ground and dispersed with the 3-roll-mill Dispersibility is improved.
이때, 상기 분쇄분산단계(S113)에서 3-롤-밀의 밀링 횟수는 제조된 혼합물의 점도를 고려하여 진행되는 것이 바람직한데, 상기 3-롤-밀의 밀링 횟수가 3회를 초과하게 되면 접착제의 분산성은 향상되지만 점도가 지나치게 낮아져 접착성능이 저하될 수 있기 때문에 바람직하지 못하다.At this time, it is preferable that the number of milling of the 3-roll-mill in the grinding and dispersing step (S113) is performed in consideration of the viscosity of the prepared mixture. When the number of milling of the 3-roll-mill exceeds 3 times, the adhesive is dispersed. Although the properties are improved, it is not preferable because the viscosity is too low and the adhesive performance may be deteriorated.
상기 진공교반단계(S115)는 상기 분쇄분산단계(S113)를 통해 분쇄 및 분산된 혼합물을 플레네터리 믹서로 진공교반하는 단계로, 상기 분쇄분산단계(S113)를 통해 분쇄 및 분산된 혼합물을 플레네터리 믹서에 투입하고 진공상태에서 500 내지 1500rpm의 속도로 30 내지 60초 동안 이루어지는 것이 바람직하다.The vacuum stirring step (S115) is a step of vacuum stirring the mixture pulverized and dispersed through the pulverization and dispersion step (S113) with a planetary mixer. It is preferably introduced into a netary mixer and made for 30 to 60 seconds at a speed of 500 to 1500 rpm in a vacuum state.
상기의 과정으로 이루어지는 진공교반단계(S115)를 통해 분쇄분산단계(S113)를 통해 분쇄 및 분산된 혼합물에 함유된 성분이 고르게 혼합되면서도 각 성분간의 반응이 억제되어 표면과 내부에 물성차이가 없고 분산 안정성이 향상된 고점도 접착제를 제공할 수 있다.Through the vacuum stirring step (S115) consisting of the above process, the components contained in the mixture pulverized and dispersed through the pulverization and dispersion step (S113) are evenly mixed, but the reaction between each component is suppressed so that there is no difference in physical properties between the surface and the inside, and there is no difference in physical properties and dispersion A high-viscosity adhesive with improved stability can be provided.
이하에서는, 본 발명에 따른 분산 안정성이 향상된 고점도 접착제의 제조방법 및 그 제조방법을 통해 제조된 고점도 접착제의 물성을 실시예를 들어 설명하기로 한다.Hereinafter, the manufacturing method of the high-viscosity adhesive with improved dispersion stability according to the present invention and the physical properties of the high-viscosity adhesive manufactured through the manufacturing method will be described with examples.
<실시예 1><Example 1>
에폭시 수지 혼합물(에폭시 수지와 액상형 에폭시 수지가 1:1의 비율로 혼합) 100 중량부, 희석제{글리세린(3인산)트리아크릴레이트 100 중량부 및 2-(2-비닐옥시에톡시)에틸아크릴레이트 35 중량부} 20 중량부 및 소포제(BYK의 BYK-1790) 0.5 중량부를 혼합하고 플레네터리 믹서에 투입하고 1000rpm의 속도로 75초 동안 저속교반하고, 저속교반된 혼합물 100 중량부에 충전재(비석면 타입의 활석, KC3000) 20 중량부를 혼합하고, 충전재가 혼합된 혼합물을 플레네터리 믹서에 투입하고 1000rpm의 속도로 75초 동안 저속교반하고, 저속교반된 혼합물에 함유된 에폭시 수지 100 중량부 대비 광개시제[비스(2,4,6-트리메틸벤조일)-페닐포스핀옥사이드{Bis(2,4,6-trimethylbenzoyl)-phenylphosphineoxide)}] 0.1 중량부, 양이온 광개시제(Irgacure 290) 3.5 중량부, 양이온 경화제(AID SI-360) 3.5 중량부, 중합억제제(AID SI-S) 0.1 중량부 및 증점제(폴리디메틸실록산으로 처리된 흄드실리카) 20 중량부를 혼합하고 플레네터리 믹서에 투입하여 7500rpm의 속도로 75초 동안 고속교반하여 기포를 제거하고, 고속교반되어 기포가 제거된 혼합물을 3-롤-밀(3-ROLL-MILL)로 2회에 걸쳐 밀링하여 혼합물을 분쇄 및 분산하고, 분쇄 및 분산된 혼합물을 플레네터리 믹서에 투입하고 진공상태에서 1000rpm의 속도로 45초 동안 진공교반하여 분산 안정성이 향상된 고점도 접착제를 제조하였다.Epoxy resin mixture (epoxy resin and liquid type epoxy resin mixed in a ratio of 1: 1) 100 parts by weight, diluent {glycerin (triphosphate) triacrylate 100 parts by weight and 2- (2-vinyloxyethoxy) ethyl acrylate 35 parts by weight} 20 parts by weight and 0.5 parts by weight of an antifoaming agent (BYK-1790 from BYK) were mixed and put into a planetary mixer and stirred at low speed for 75 seconds at a speed of 1000 rpm. 20 parts by weight of cotton-type talc, KC3000) was mixed, the mixture mixed with the filler was put into a planetary mixer and stirred at low speed for 75 seconds at a speed of 1000 rpm, compared to 100 parts by weight of the epoxy resin contained in the low-speed stirred mixture Photoinitiator [bis (2,4,6-trimethylbenzoyl) -phenylphosphine oxide {Bis (2,4,6-trimethylbenzoyl) -phenylphosphineoxide)] 0.1 parts by weight, cationic photoinitiator (Irgacure 290) 3.5 parts by weight, cationic curing agent (AID SI-360) 3.5 parts by weight, polymerization inhibitor (AID SI-S) 0.1 parts by weight and thickener (fumed silica treated with polydimethylsiloxane) 20 parts by weight were mixed and put into a planetary mixer at a speed of 7500 rpm Bubbles were removed by high-speed stirring for 75 seconds, and the mixture from which bubbles were removed by high-speed stirring was milled twice with a 3-ROLL-MILL to pulverize and disperse the mixture, and pulverize and disperse the mixture. The mixture was put into a planetary mixer and vacuum stirred at a speed of 1000 rpm for 45 seconds in a vacuum state to prepare a high-viscosity adhesive having improved dispersion stability.
<비교예 1><Comparative Example 1>
에폭시 수지 혼합물(에폭시 수지와 액상형 에폭시 수지가 1:1의 비율로 혼합) 100 중량부, 희석제{글리세린(3인산)트리아크릴레이트 100 중량부 및 2-(2-비닐옥시에톡시)에틸아크릴레이트 35 중량부} 20 중량부 및 소포제(BYK의 BYK-1790) 0.5 중량부, 충전재(비석면 타입의 활석, KC3000) 20 중량부, 광개시제[비스(2,4,6-트리메틸벤조일)-페닐포스핀옥사이드{Bis(2,4,6-trimethylbenzoyl)-phenylphosphineoxide)}] 0.1 중량부, 양이온 광개시제(Irgacure 290) 3.5 중량부, 양이온 경화제(AID SI-360) 3.5 중량부, 중합억제제(AID SI-S) 0.1 중량부 및 증점제(폴리디메틸실록산으로 처리된 흄드실리카) 20 중량부를 혼합하고 플레네터리 믹서에 투입하여 7500rpm의 속도로 75초 동안 고속교반하여 고점도 접착제를 제조하였다.Epoxy resin mixture (epoxy resin and liquid type epoxy resin mixed in a ratio of 1: 1) 100 parts by weight, diluent {glycerin (triphosphate) triacrylate 100 parts by weight and 2- (2-vinyloxyethoxy) ethyl acrylate 35 parts by weight} 20 parts by weight and antifoaming agent (BYK-1790 from BYK) 0.5 parts by weight, filler (non-asbestos type talc, KC3000) 20 parts by weight, photoinitiator [bis(2,4,6-trimethylbenzoyl)-phenylphos Pinoxide {Bis(2,4,6-trimethylbenzoyl)-phenylphosphineoxide)}] 0.1 parts by weight, cationic photoinitiator (Irgacure 290) 3.5 parts by weight, cationic curing agent (AID SI-360) 3.5 parts by weight, polymerization inhibitor (AID SI- S) 0.1 part by weight and 20 parts by weight of a thickener (fumed silica treated with polydimethylsiloxane) were mixed and put into a planetary mixer, followed by high-speed stirring at a speed of 7500 rpm for 75 seconds to prepare a high-viscosity adhesive.
<비교예 2><Comparative Example 2>
상기 실시예 1과 동일하게 진행하되, 3-롤-밀로 밀링하는 공정과 진공교반하는 과정을 생략하여 분산 안정성이 향상된 고점도 접착제를 제조하였다.In the same manner as in Example 1, a high-viscosity adhesive with improved dispersion stability was prepared by omitting the milling process with a 3-roll-mill and the process of vacuum stirring.
<비교예 3><Comparative Example 3>
상기 실시예 1과 동일하게 진행하되, 진공교반하는 과정을 생략하여 분산 안정성이 향상된 고점도 접착제를 제조하였다.Proceed in the same manner as in Example 1, but the process of vacuum stirring was omitted to prepare a high-viscosity adhesive with improved dispersion stability.
상기 실시예 1 및 비교예 1 내지 3을 통해 제조된 고점도 접착제의 분산안정성을 측정하여 아래 표 1에 나타내었다.The dispersion stability of the high-viscosity adhesives prepared in Example 1 and Comparative Examples 1 to 3 was measured and shown in Table 1 below.
<표 1><Table 1>
상기 표 1에 나타낸 것처럼, 본 발명의 실시예 1을 통해 제조된 고점도 접착제는 시간이 경과해도 성부와 하부의 점도차이가 크기 않아 우수한 분산성을 나타내는 것을 알 수 있다.As shown in Table 1, it can be seen that the high-viscosity adhesive prepared in Example 1 of the present invention exhibits excellent dispersibility because the difference in viscosity between the upper part and the lower part is not large over time.
반면, 비교예 1 내지 3을 통해 제조되는 72시간이 경과하면 하부에 경화현상이 발생하는 것을 알 수 있다.On the other hand, it can be seen that a curing phenomenon occurs in the lower part after 72 hours manufactured through Comparative Examples 1 to 3.
따라서, 본 발명에 따른 분산 안정성이 향상된 고점도 접착제의 제조방법은 고점도를 나타내면서도 접착제의 표면과 내부에 물성차이가 없고, 침전이나 분리현상이 발생되지 않을 뿐만 아니라, 기포제거 공정이 진행되어 우수한 분산안정성을 나타내는 접착제를 제공한다.Therefore, the manufacturing method of the high-viscosity adhesive with improved dispersion stability according to the present invention shows high viscosity, but there is no difference in physical properties between the surface and the inside of the adhesive, no precipitation or separation occurs, and excellent dispersion due to the bubble removal process. An adhesive exhibiting stability is provided.
S101 ; 원료혼합단계
S103 ; 제1교반단계
S105 ; 충전재혼합단계
S107 ; 제2교반단계
S109 ; 첨가제혼합단계
S111 ; 제3교반단계
S113 ; 분쇄분산단계
S115 ; 진공교반단계S101; Raw material mixing step
S103; 1st stirring step
S105; Filler mixing step
S107; 2nd stirring step
S109; Additive mixing step
S111; 3rd stirring step
S113; Grinding and dispersing step
S115; vacuum agitation step
Claims (10)
상기 원료혼합단계를 통해 제조된 혼합물을 플레네터리 믹서에 투입하고 1000rpm의 속도로 75초 동안 저속교반하는 제1교반단계;
상기 제1교반단계를 통해 교반된 혼합물 100 중량부에 충전재 20 중량부를 혼합하는 충전재혼합단계;
상기 충전재혼합단계를 통해 제조된 혼합물을 플레네터리 믹서로에 투입하고 1000rpm의 속도로 75초 동안 저속교반하는 제2교반단계;
상기 제2교반단계를 통해 교반된 혼합물에 함유된 에폭시 수지 100 중량부 대비 광개시제 0.1 중량부, 양이온 광개시제 3.5 중량부, 양이온 경화제 3.5 중량부, 중합억제제 0.1 중량부 및 증점제 20 중량부를 혼합하는 첨가제혼합단계;
상기 첨가제혼합단계를 통해 제조된 혼합물을 플레네터리 믹서에 투입하고 7500rpm의 속도로 75초 동안 고속교반하여 내부 기포를 제거하는 제3교반단계;
상기 제3교반단계를 통해 기포가 제거된 혼합물을 3-롤-밀로 2회에 걸쳐 분쇄 및 분산하는 분쇄분산단계; 및
상기 분쇄분산단계를 통해 분쇄 및 분산된 혼합물을 플레네터리 믹서에 투입하고 1000rpm의 속도로 45초 동안 진공교반하는 진공교반단계;로 이루어지며,
상기 에폭시 수지 혼합물은 에폭시 수지와 액상형 에폭시 수지가 1:1의 비율로 혼합되어 이루어지고,
상기 희석제는 글리세린(3인산)트리아크릴레이트 100 중량부 및 2-(2-비닐옥시에톡시)에틸아크릴레이트 35 중량부로 이루어지며,
상기 충전재는 비석면 타입의 활석으로 이루어지고,
상기 광개시제는 비스(2,4,6-트리메틸벤조일)-페닐포스핀옥사이드로 이루어지며,
상기 증점제는 폴리디메틸실록산으로 처리된 흄드실리카로 이루어지는 것을 특징으로 하는 분산 안정성이 향상된 고점도 접착제의 제조방법.A raw material mixing step of mixing 100 parts by weight of an epoxy resin mixture, 20 parts by weight of a diluent and 0.5 parts by weight of an antifoaming agent;
A first stirring step of introducing the mixture prepared through the raw material mixing step into a planetary mixer and stirring at a low speed of 1000 rpm for 75 seconds;
A filler mixing step of mixing 20 parts by weight of a filler with 100 parts by weight of the mixture stirred through the first stirring step;
A second stirring step of introducing the mixture prepared through the filler mixing step into a planetary mixer furnace and stirring at a speed of 1000 rpm for 75 seconds;
Additive mixing of 0.1 parts by weight of photoinitiator, 3.5 parts by weight of cationic photoinitiator, 3.5 parts by weight of cationic curing agent, 0.1 part by weight of polymerization inhibitor and 20 parts by weight of thickener with respect to 100 parts by weight of epoxy resin contained in the mixture stirred through the second stirring step. step;
A third stirring step of removing internal bubbles by introducing the mixture prepared through the additive mixing step into a planetary mixer and stirring at a high speed of 7500 rpm for 75 seconds;
A pulverization and dispersion step of pulverizing and dispersing the mixture from which bubbles are removed through the third stirring step twice with a 3-roll-mill; and
A vacuum stirring step of putting the mixture ground and dispersed through the grinding and dispersing step into a planetary mixer and vacuum stirring for 45 seconds at a speed of 1000 rpm;
The epoxy resin mixture is made by mixing an epoxy resin and a liquid epoxy resin in a ratio of 1: 1,
The diluent is composed of 100 parts by weight of glycerin (triphosphate) triacrylate and 35 parts by weight of 2-(2-vinyloxyethoxy)ethyl acrylate,
The filler is made of non-asbestos type talc,
The photoinitiator is composed of bis(2,4,6-trimethylbenzoyl)-phenylphosphine oxide,
The thickener is a method for producing a high viscosity adhesive having improved dispersion stability, characterized in that consisting of fumed silica treated with polydimethylsiloxane.
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