KR20010084405A - Ultraviolet Control Film - Google Patents
Ultraviolet Control Film Download PDFInfo
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- KR20010084405A KR20010084405A KR1020000009424A KR20000009424A KR20010084405A KR 20010084405 A KR20010084405 A KR 20010084405A KR 1020000009424 A KR1020000009424 A KR 1020000009424A KR 20000009424 A KR20000009424 A KR 20000009424A KR 20010084405 A KR20010084405 A KR 20010084405A
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- E—FIXED CONSTRUCTIONS
- E02—HYDRAULIC ENGINEERING; FOUNDATIONS; SOIL SHIFTING
- E02D—FOUNDATIONS; EXCAVATIONS; EMBANKMENTS; UNDERGROUND OR UNDERWATER STRUCTURES
- E02D3/00—Improving or preserving soil or rock, e.g. preserving permafrost soil
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- E—FIXED CONSTRUCTIONS
- E02—HYDRAULIC ENGINEERING; FOUNDATIONS; SOIL SHIFTING
- E02D—FOUNDATIONS; EXCAVATIONS; EMBANKMENTS; UNDERGROUND OR UNDERWATER STRUCTURES
- E02D2300/00—Materials
- E02D2300/0001—Rubbers
- E02D2300/0003—Car tires
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- Engineering & Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- Structural Engineering (AREA)
- Agronomy & Crop Science (AREA)
- Environmental & Geological Engineering (AREA)
- Soil Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Mining & Mineral Resources (AREA)
- Paleontology (AREA)
- Civil Engineering (AREA)
- General Engineering & Computer Science (AREA)
- Laminated Bodies (AREA)
Abstract
Description
본 발명은 광호변성 성형물의 제조방법에 관한 것으로, 특히 광호변성 화합물 안료를 수지에 흡수시킨 후 성형하는 것을 특징으로 하는 광호변성 성형물의 제조방법에 관한 것이다.The present invention relates to a method for producing a photochromic molding, and more particularly, to a method for producing a photochromic molding, wherein the photochromic compound pigment is absorbed into a resin and then molded.
자동차나 건물, 전시장 등의 유리등에 부착하여 태양광을 차단하고 외부로부터의 프라이버시를 보호하는 자외선 차단 필름은 한국 특허공개공보 제 1999-026350 호 및 제 1999-026349 호에 기재된 바와 같이, 염료, 자외선 흡수제 및 고분자 결합제 또는 아크릴계 점착제로 이루어지는 광선 선택 투과층이 플라스틱 지지체 필름상에 적층되어 있다. 또한, 한국 특허 공개 공보 제 1999-18538 호에는UV blocking films that attach to glass, such as automobiles, buildings, exhibition halls, etc. to block sunlight and protect privacy from the outside, are disclosed in Korean Patent Laid-Open Publication Nos. 1999-026350 and 1999-026349. The light selective transmission layer which consists of an absorbent, a polymeric binder, or an acrylic adhesive is laminated | stacked on the plastic support film. In addition, Korean Patent Publication No. 1999-18538
이스필름(3)에 이형박리층(1), 점착층(2) 및 하드코팅층(4)을 형성시켜 제조되는솔라컨트롤 필름에 있어서, 점착층(2)을 점착용 수지에 근적외선영역에 큰 흡수파장역을 갖는 유기계 화합물인 열선흡수제를 배합한 접착제를 도포해 형성시키고, 하드코팅층(4)은 자외선 경화용 수지에 염료를 배합한 것을 사용하여 형성시키는 것을 특징으로 하는 솔라컨트롤필름의 제조방법이 게시되어 있다.In a solar control film produced by forming a release peeling layer (1), an adhesive layer (2), and a hard coating layer (4) on an es film (3), the adhesive layer (2) is largely absorbed in the near infrared region by the adhesive resin. A method of manufacturing a solar control film, which is formed by applying an adhesive containing a heat ray absorbent, which is an organic compound having a wavelength range, and forming the hard coating layer 4 using a mixture of a dye and an ultraviolet curing resin. Posted.
그러나, 이러한 제품들은 모두 자외선 차단층이 베이스 필름 위에 코팅되어 있는 형태로 되어 있어 쉽게 탈색이 되고 기재 층과 코팅층을 따로 제조하여 적층해야 하는 등 공정이 복잡해지는 문제점이 있었다.However, all of these products have a problem that the UV blocking layer is coated on the base film so that it is easily discolored and the process is complicated, such as to prepare and laminate the substrate layer and the coating layer separately.
또, 이러한 단점을 제거하고자 본 발명자는 특허출원 1999-48421 호에서, 수지 그래뉼을 톨루엔/에틸아세테이트/알코올 혼합용매와 함께 용융시키는 방법을 시도하였으나, 용융과정에 용매의 증발로 인해 성형에 어려움이 많았다.In addition, in order to eliminate this disadvantage, the present inventors attempted to melt a resin granule together with a toluene / ethyl acetate / alcohol mixed solvent in Patent Application No. 1999-48421, but it is difficult to mold due to evaporation of the solvent during the melting process. Many.
따라서, 본 발명의 목적은 수지 내부에 염료를 흡수시켜 탈색 염려가 없는 광호변성 수지 성형물의 제조방법을 제공하는 것이다.Accordingly, it is an object of the present invention to provide a method for producing a photochromic resin molded article having no fear of discoloration by absorbing dye inside the resin.
본 발명의 다른 목적은 성형에 문제가 없는 광호변성 수지 성형물의 제조방법을 제공하는 것이다.Another object of the present invention is to provide a method for producing a photochromic resin molded article having no molding problem.
도 1은 본 발명의 염료 용액을 침투시킨 수지 그래뉼 표면의 전자현미경 사진(400배).Figure 1 is an electron micrograph (400 times) of the surface of the resin granules infiltrated with the dye solution of the present invention.
도 2는 본 발명의 염료 용액을 침투시킨 수지 그래뉼의 중심부를 절단한 단면의 전자현미경 사진(400배).Figure 2 is an electron micrograph (400 times) of the cross section cut the center of the resin granules infiltrated the dye solution of the present invention.
상기의 본 발명의 목적은 스피로피란계 광호변성 화합물을 톨루엔/알코올 혼합용매에 용해시킨 용액을 수지 그래뉼에 20-50℃에서 0.05-48시간동안 침투시킨 후, 160-300℃로 가열하여, 성형하는 것을 특징으로 한다.The object of the present invention is to penetrate the solution of the spiropyran-based photochromic compound in a toluene / alcohol mixed solvent in the resin granule at 0.05-50 hours, then heated to 160-300 ℃, forming Characterized in that.
본 발명에 사용되는 수지 그래뉼은 PE, PP, PC, PET, ABS, CA, 또는 SAN 수지 등의 그래뉼을 사용할 수 있다.The resin granules used in the present invention may use granules such as PE, PP, PC, PET, ABS, CA, or SAN resin.
스피로피란계 광호변성 화합물은 공지되어 있으며, 약 0.1-1.0중량%의 광호변성 화합물을 톨루엔/알코올 혼합용매에 용해시킨다.Spiropyran-based photochromic compounds are known and about 0.1-1.0% by weight of the photochromic compounds are dissolved in a toluene / alcohol mixed solvent.
바람직하게는 하기 화학식의 스피로피란계 화합물이 사용된다.Preferably, a spiropyrane compound of the following formula is used.
본 발명의 성형물을 필름 형태로 성형하여 자외선 차단 필름으로 제조하는 경우 자외선 흡수제를 사용할 수 있다. 자외선 흡수제의 종류에 제한은 없으나, 시바가이기사의 티누빈(TINUVIN) 등이 바람직하게 사용된다. 자외선 흡수제는 용액 전체를 기준으로 약 1-3 중량%의 양으로 용해된다.In the case of forming the molded article of the present invention in the form of a film to produce a UV blocking film, a UV absorber may be used. Although there is no restriction | limiting in the kind of ultraviolet absorber, Tinubain (TINUVIN) etc. of Shivagaigi are used preferably. The ultraviolet absorbent is dissolved in an amount of about 1-3% by weight based on the total solution.
톨루엔/알코올 혼합용매의 알코올 혼합은 부피비로 1 : 1-2 의 비율, 바람직하게는 1; 1.5의 비율로 이루어진다. 알코올 용매는 메틸알코올, 에틸 알코올, 프로필 알코올, 이소프로필 알코올, 부틸 알코올, 및 이소부틸 알코올로 구성된 그룹으로부터 선택된 하나 이상의 알코올이고 바람직하게는 이소프로필 알코올과 부틸 알콜을 동일한 비율로 혼합한 알코올이 사용된다. 스피로피란계 광호변성 화합물을 톨루엔/알코올 혼합용매에 용해시킨 용액에 폴리에틸렌, 폴리프로필렌, 폴리(에틸렌테레프탈레이트), 폴리카아보네이트, 셀룰로즈 아세테이트 수지, 스티렌/아크릴로니트린 공중합체 수지 또는 아크릴로니트릴/부타디엔/스티렌 공중합체 수지의 그래뉼을 2-24시간 침지시켜 광호변성 화합물이 침투되도록 한다. 화합물의 침투가 끝나면 그래뉼을 분리하여 용매를 건조시킨 다음 160-300℃로 가열하여 용융시켜, 압출 성형, 캘린더링 등의 일반 성형에 이용되는 성형방법을 이용하여 필름, 섬유, 판 등 다양한 모양으로 성형하면 된다.The alcohol mixing of the toluene / alcohol mixed solvent is in a volume ratio of 1: 1-2, preferably 1; It is made at the rate of 1.5. The alcohol solvent is at least one alcohol selected from the group consisting of methyl alcohol, ethyl alcohol, propyl alcohol, isopropyl alcohol, butyl alcohol, and isobutyl alcohol, and preferably used is an alcohol obtained by mixing isopropyl alcohol and butyl alcohol in the same ratio. do. Polyethylene, polypropylene, poly (ethylene terephthalate), polycarbonate, cellulose acetate resin, styrene / acrylonitrile copolymer resin or acrylonitrile in a solution in which a spiropyrane photochromic compound is dissolved in a toluene / alcohol mixed solvent The granule of / butadiene / styrene copolymer resin is immersed for 2 to 24 hours to allow the photochromic compound to penetrate. After the penetration of the compound, the granules are separated, the solvent is dried, heated to 160-300 ° C. and melted to form a variety of shapes such as films, fibers, and plates using a molding method used for general molding such as extrusion molding and calendering. It is good to shape.
수지를 용융시키는 과정에서 염료 용액을 함께 부가하는 경우 염료 수지 성형과정에서 용매가 다량 휘발하므로 수지의 성형이 어려웠으나, 본 발명에서는 광호변성 화합물과 자외선 흡수제를 직접 수지에 침투시킴으로써 이러한 부작용이 없어지게 되었다.When the dye solution is added together in the process of melting the resin, since the solvent is volatilized in the dye resin molding process, the molding of the resin was difficult, but in the present invention, such side effects are eliminated by directly infiltrating the photochromic compound and the ultraviolet absorbent into the resin. It became.
이하 본 발명을 실시예를 통해 보다 상세하게 설명한다.Hereinafter, the present invention will be described in more detail with reference to Examples.
실시예 1Example 1
하기 화학식의 스피로피란계 광호변성 화합물(영국 KROMA Corp. 제품) 2g, TINUVIN-P(시바가이기사 제품) 10g을 톨루엔 160㎖/이소프로필알콜 120㎖ + 부틸알콜 120㎖ 혼합용매에 용해시켜 선형 저밀도 폴리에틸렌(LLDPE) 그래뉼(SK 화학제품 모델명 FU149M) 500g을 상기 용액에 25-30℃에서 12시간 침지시켜 용액을 흡수시켰다.2 g of a spiropyrane photochromic compound (manufactured by KROMA Corp., UK) and 10 g of TINUVIN-P (manufactured by Ciba-Geigy Co., Ltd.) were dissolved in a mixed solvent of 160 ml of toluene and 120 ml of isopropyl alcohol and 120 ml of butyl alcohol. 500 g of polyethylene (LLDPE) granule (SK Chemical Model FU149M) was immersed in the solution at 25-30 ° C. for 12 hours to absorb the solution.
용매를 증발, 건조시킨 다음 표면의 전자현미경 사진을 촬영하였다. 그래뉼의 중심부를 잘라 그 단면을 역시 전자 현미경으로 촬영하였다. 그 결과를 도 1 및 도 2에 도시하였다. 염료가 그래뮬의 중심부까지 흡수되었음을 확인할 수 있었다.The solvent was evaporated and dried and an electron micrograph of the surface was taken. The center of the granule was cut and its cross section was also taken with an electron microscope. The results are shown in FIGS. 1 and 2. It was confirmed that the dye was absorbed to the center of the gramul.
압출성형기에 그래뉼을 넣고 200℃로 혼합하여 균일한 혼합물을 제조한 다음 필름 형상으로 압출성형하였다. 아크릴 점착제를 도포하고 실리콘 이형필름으로 라미네이트하여 자외선 차단 필름을 제조하였다.Granules were put in an extruder and mixed at 200 ° C. to produce a uniform mixture, and then extruded into a film shape. An acrylic pressure-sensitive adhesive was applied and laminated with a silicone release film to prepare a sunscreen film.
가시광선 투과율 및 자외선 차단율Visible light transmittance and UV blocking rate
제조된 필름을 상온에서 7일간 숙성한 후, 이형 필름을 벗겨내고 폭 3㎝, 길이 4.5㎝가 되게 하여 시료를 준비한 후, UV-VIS SPECTROPHOTOMETER를 이용하여 가시광선 투과율 및 자외선 차단율(370㎚에서)을 측정하였다. 자외선 차단율이 99%였다.After aging the prepared film at room temperature for 7 days, the release film was peeled off and the sample was prepared to have a width of 3 cm and a length of 4.5 cm, and then visible light transmittance and UV blocking rate (at 370 nm) using UV-VIS SPECTROPHOTOMETER. Was measured. UV blocking rate was 99%.
염료탈착평가Dye Desorption Evaluation
제조한 필름을 상온에서 7일간 에이징한 후, 이형필름을 벗겨내고 폭 30㎝, 길이 50㎝가 되게하여 시료를 준비한 후, 유리창의 시공시에 물기 제거시 나타나는 현상을 확인 함으로써 측정하였다. 탈리되는 염료는 0%였다.After the prepared film was aged at room temperature for 7 days, the release film was peeled off, and the sample was prepared to have a width of 30 cm and a length of 50 cm, and then measured by checking the phenomenon of water removal during the construction of the glass window. The dye released was 0%.
상기 실시예에서 확인되듯이 본 발명의 방법에 의해 자외선 차단필름을 제조하는 경우 자외선 흡수제와 광호변성 염료가 수지중에 흡수되어 염료가 탈리되는 현상이 완전히 제거되었으며, 제조공정이 간단하여 매우 경제적이다.As confirmed in the above embodiment, when the UV blocking film is manufactured by the method of the present invention, a phenomenon in which the UV absorber and the photochromic dye are absorbed in the resin and the dye is detached is completely removed, and the manufacturing process is simple and very economical.
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Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4367170A (en) * | 1975-01-24 | 1983-01-04 | American Optical Corporation | Stabilized photochromic materials |
JPS6231802A (en) * | 1985-08-01 | 1987-02-10 | Nippon Sheet Glass Co Ltd | Coated photochromic plastic optical parts |
KR920008620A (en) * | 1990-10-31 | 1992-05-28 | 다쯔노 히요시 | Communication control device between IC card and host device |
KR930008951A (en) * | 1991-10-02 | 1993-05-22 | 김광호 | Method of manufacturing lenticular mask |
KR940007355A (en) * | 1992-09-30 | 1994-04-27 | 와다 요시히로 | Valve shift timing controller of engine |
KR20010045215A (en) * | 1999-11-03 | 2001-06-05 | 이영신 | Ultraviolet Control Film |
-
2000
- 2000-02-25 KR KR1020000009424A patent/KR20010084405A/en not_active Application Discontinuation
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4367170A (en) * | 1975-01-24 | 1983-01-04 | American Optical Corporation | Stabilized photochromic materials |
JPS6231802A (en) * | 1985-08-01 | 1987-02-10 | Nippon Sheet Glass Co Ltd | Coated photochromic plastic optical parts |
KR920008620A (en) * | 1990-10-31 | 1992-05-28 | 다쯔노 히요시 | Communication control device between IC card and host device |
KR930008951A (en) * | 1991-10-02 | 1993-05-22 | 김광호 | Method of manufacturing lenticular mask |
KR940007355A (en) * | 1992-09-30 | 1994-04-27 | 와다 요시히로 | Valve shift timing controller of engine |
KR20010045215A (en) * | 1999-11-03 | 2001-06-05 | 이영신 | Ultraviolet Control Film |
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