KR100522922B1 - Resin composition for light conversion film - Google Patents

Resin composition for light conversion film Download PDF

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KR100522922B1
KR100522922B1 KR10-1998-0022602A KR19980022602A KR100522922B1 KR 100522922 B1 KR100522922 B1 KR 100522922B1 KR 19980022602 A KR19980022602 A KR 19980022602A KR 100522922 B1 KR100522922 B1 KR 100522922B1
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resin
light conversion
resin composition
light
film
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KR10-1998-0022602A
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KR20000002054A (en
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김용환
심광용
김경현
노성균
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삼성토탈 주식회사
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/18—Manufacture of films or sheets
    • 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
    • C08K3/30—Sulfur-, selenium- or tellurium-containing compounds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2300/00—Characterised by the use of unspecified polymers
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L101/00—Compositions of unspecified macromolecular compounds

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  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

본 발명은 고분자수지와 광전환 첨가제로서 하기 일반식의 무기형광제를 함유하는 광전환필름용 수지조성물에 관한 것이다.The present invention relates to a resin composition for a light conversion film containing a polymer resin and an inorganic fluorescent agent of the following general formula as a light conversion additive.

EumYnOkSl Eu m Y n O k S l

상기 식에서, m=0.01∼0.2, n=2∼3, k=2∼3, l=0∼1 이다.Wherein m = 0.01 to 0.2, n = 2 to 3, k = 2 to 3, and l = 0 to 1.

Description

광전환 필름용 수지조성물Resin composition for light conversion film

본 발명은 광전환필름용 수지 조성물에 관한 것으로, 보다 상세하게는 고분자 수지에 광을 전환할 수 있는 광전환 첨가제로서 무기형광제를 투입하여 제조되는 광전환 필름용 수지조성물에 관한 것이다.The present invention relates to a resin composition for a light conversion film, and more particularly to a resin composition for a light conversion film prepared by adding an inorganic fluorescent agent as a light conversion additive capable of converting light to a polymer resin.

일반적으로 광전환 필름은 광전환 첨가제가 첨가된 수지조성물로 제조되며, 이러한 필름에 빛이 통과할 때 불필요한 파장의 빛이 흡수되어 유용한 파장의 빛으로 전환된다. 통상 첨가되는 광전환 첨가제에 의해 흡수되는 빛의 파장과 다시 나오는 빛의 파장이 결정되며 사용하는 목적에 따른 다양한 용도의 광전환수지를 만들 수 있다.Generally, a light conversion film is made of a resin composition to which a light conversion additive is added, and when light passes through the film, light of an unnecessary wavelength is absorbed and converted into light of a useful wavelength. The wavelength of the light absorbed by the light conversion additive which is usually added and the wavelength of the light coming out again are determined, and the light conversion resin for various uses can be made according to the purpose of use.

종래 광전환 필름의 실제적 적용의 한 예로는 농업용 필름에 광전환 첨가제를 사용하여 식물성장에 유익한 빛의 양을 증가시켜 수확시기등을 앞당기는 것이다. 이러한 필름으로는 기존의 농업용 보광성필름이 있으며, 기본적인 원리는 특수첨가제가 태양광선중의 무익한 자외선(UV) 영역의 빛을 흡수하여 그중 일부를 615nm 근처의 적색광으로 변화를 시켜 식물성장을 촉진시키는 것으로 식물의 엽록소는 적과 청의 빛을 흡수하여 가장 효율적으로 광합성을 수행하는 것으로 알려져 있다. 이때 첨가되는 광전환 첨가제에 의해서 광의 흡수파장, 전환파장, 전환효율등이 달라지며, 식물성장에 미치는 효능도 달라지게 된다. 이러한 광전환 첨가제로는 일반적으로 형광제가 많이 쓰이며 사용가능한 물질이 비교적 다양하다. 예를들면, TiO2, 에어로실(aerosil), 및 유로피움니트레이트(europium nitrate)와 1,10-페난트롤린(1,10-phenanthroline) 또는 4,4-디프리딜(4,4-diphridill)로 된 유로피움 착화물(europium complex)(대한민국 공개특허 제96-17748호 참조) 등이 있다. 이중에서 맨 나중의 유로피움 착화물이 비교적 가장 좋은 효율을 보이나, 무기 형광제의 단점이라고 할 수 있는 비교적 큰 입자 크기 때문에 필름에 사용하였을 때 필름의 투명성 저하 및 필름내 분산의 어려움등의 문제점이 있고, 또한 제조과정이 비교적 복잡하고 고가인 문제점 등이 있다.One practical application of conventional light conversion films is to use light conversion additives in agricultural films to increase the amount of light beneficial to plant growth to speed up harvest times. These films include conventional agricultural light-transmitting films, and the basic principle is that special additives absorb light in the unsuitable ultraviolet (UV) region of the sun and change some of it into red light near 615 nm to promote plant growth. Chlorophyll is known to absorb red and blue light and perform photosynthesis most efficiently. At this time, the absorption wavelength, conversion wavelength, conversion efficiency, etc. of light are changed by the light conversion additive added, and the effect on plant growth is also changed. As such a light conversion additive, a fluorescent agent is generally used and a variety of materials can be used. For example, TiO 2 , aerosil, and europium nitrate and 1,10-phenanthroline or 4,4-dipridil (4,4- or europium complexes (see Korean Patent Application Laid-Open No. 96-17748). Of these, the last europium complex shows the best efficiency, but due to the relatively large particle size, which is a disadvantage of inorganic fluorescent agents, problems such as deterioration of film transparency and difficulty in dispersing in the film are found. In addition, there is a problem that the manufacturing process is relatively complicated and expensive.

따라서, 본 발명의 목적은 상기한 바와 같은 종래의 유로피움 착화물 무기형광제를 이용한 광전환 필름용 수지조성물의 문제점을 해결하기 위해서, 필름내에서의 분산이 비교적 용이할 뿐 아니라 제조공정이 간단하고, 비용이 저렴하며, 또한 기존의 유로피움 착화물 보다 광전환 효율이 더욱 우수한 무기형광제를 사용해 필름의 투명성과 광전환효율을 증가시킬 수 있는 광전환수지를 제공하는데 있다.Accordingly, an object of the present invention is to solve the problem of the resin composition for the light conversion film using the conventional europium complex inorganic fluorescent agent as described above, the dispersion in the film is relatively easy and the manufacturing process is simple. In addition, the present invention provides an optical conversion resin capable of increasing transparency and light conversion efficiency of a film by using an inorganic fluorescent agent which is inexpensive and inexpensive and has a light conversion efficiency that is higher than that of a conventional europium complex.

이하 본 발명을 구체적으로 설명한다.Hereinafter, the present invention will be described in detail.

본 발명은 보광성 필름제조에 사용되는 기존의 광전환수지에 있어서, 광전환 첨가제로서 하기 일반식의 무기 형광제를 사용하는 것을 특징으로 한다.The present invention is characterized in that an inorganic fluorescent agent of the following general formula is used as the light conversion additive in the existing light conversion resin used for manufacturing the light-transmissive film.

EumYnOkSl Eu m Y n O k S l

상기 식에서, m=0.01∼0.2, n=2∼3, k=2∼3, l=0∼1 이다.Wherein m = 0.01 to 0.2, n = 2 to 3, k = 2 to 3, and l = 0 to 1.

본 발명의 광전환필름용 수지조성물은 고분자수지와 광전환첨가제로 이루어지며, 그외 무적제, 슬립제, 안티블록킹제 등의 첨가제를 1종 이상을 함유할 수 있다.The resin composition for an optical conversion film of the present invention is composed of a polymer resin and an optical conversion additive, and may contain one or more additives such as a non-dropping agent, a slip agent, and an antiblocking agent.

고분자수지로는 폴리올레핀계 수지, 에틸렌/비닐아세테이트 공중합체, 폴리스티렌, ABS(acrylonitrile-butadiene-styrene) 수지, 염화폴리비닐, 염화폴리비닐리덴, 염화비닐/아세트산비닐 공중합체, 폴리카보네이트, 아크릴산수지, 에폭시수지, 폴리에스테르, 폴리아미드, 폴리우레탄, 니트로셀룰로우스 및 이들의 공중합체를 구성하는 단량체로 이루어진 공중합체와 같은 열가소성 수지 및 열경화성 수지가 사용될 수 있다.As the polymer resin, polyolefin resin, ethylene / vinyl acetate copolymer, polystyrene, ABS (acrylonitrile-butadiene-styrene) resin, polyvinyl chloride, polyvinylidene chloride, vinyl chloride / vinyl acetate copolymer, polycarbonate, acrylic acid resin, Thermoplastic resins and thermosetting resins such as copolymers composed of epoxy resins, polyesters, polyamides, polyurethanes, nitrocellulose and monomers constituting their copolymers can be used.

본 발명에서 광전환 첨가제로 사용되는 일반식 EumYnOkSl의 무기 형광제는 Y2O2S와 Eu2O3를 혼합하여 200∼250℃에서 소성처리한 다음 세척한 후 볼밀(ball mill)로 분쇄하여 제조된다.Inorganic fluorescent agent of the general formula Eu m Y n O k S l used as the light conversion additive in the present invention is mixed with Y 2 O 2 S and Eu 2 O 3 and calcined at 200 ~ 250 ℃ and then ball mill It is prepared by grinding in a (ball mill).

광전환 첨가제의 입자 사이즈는 1∼30㎛가 적합하다. 1㎛ 이하에서는 제조공정이 추가되어 원가가 상승하고, 30㎛ 이상에서는 분산성이 떨어진다.As for the particle size of a light conversion additive, 1-30 micrometers is suitable. In 1 micrometer or less, a manufacturing process is added and a cost rises, and in 30 micrometers or more, dispersibility is inferior.

본 발명에서 광전환첨가제의 농도는 0.08∼0.25 중량%의 범위가 적당하나, 더욱 좋기로는 0.1∼0.2 중량% 정도가 좋다. 0.08중량% 이하일 경우에는 효능이 거의 미약하며, 0.25중량% 이상일 경우는 처방농도에 따른 비용에 비해 효율의 증가가 작다.In the present invention, the concentration of the optical conversion additive is suitably in the range of 0.08 to 0.25 wt%, more preferably about 0.1 to 0.2 wt%. When the amount is less than 0.08% by weight, the efficacy is almost insignificant, and when the amount is more than 0.25% by weight, the increase in efficiency is small compared to the cost according to the prescription concentration.

수지에 광전환제를 첨가하는 방법은 (1) 성형시 또는 공정중에 직접 첨가하거나, (2) 고농도의 마스터 배치를 만들고 공정시 이를 첨가하는 방법을 사용할 수 있다.The method of adding a photoconversion agent to the resin may be (1) added directly during molding or in the process, or (2) a high concentration master batch is added to the process.

본 발명에서는 안티블로킹제, 슬립제, 무적제 이외의 물질을 필요에 따라 수지조성물에 첨가할 수 있다.In the present invention, substances other than the antiblocking agent, slip agent, and invincible agent can be added to the resin composition as necessary.

하기의 실시예 및 비교예를 통해 본 발명을 더욱 상세히 설명한다.The present invention is explained in more detail through the following examples and comparative examples.

실시예 1∼6 및 비교예 1∼2Examples 1-6 and Comparative Examples 1-2

하기 표 1에 나타낸 조성대로 에틸렌비닐아세테이트수지(VA 12%)에 광전환첨가제, 안티블로킹제, 무적제를 투입하여 펠렛을 만든 후, 70㎜ 인플레이션 필름제조기를 이용하여 가공온도 140∼160℃에서 두께 60㎛ 필름을 제조하였다.Into the ethylene vinyl acetate resin (VA 12%) in the composition shown in Table 1, a light conversion additive, an antiblocking agent, a non-dropping agent was added to make a pellet, using a 70mm inflation film maker at a processing temperature 140 ~ 160 ℃ A 60 μm film was made.

제조된 필름을 발광/형광분석기(photoluminescence M/C)를 이용하여 상대적인 형광세기를 측정하였으며, 그 결과를 표 1에 나타내었다. 또한, 제조된 필름으로 시험용 비닐하우스(3m × 20m ×2m)를 설치하여 방울 토마토 및 딸기에 대한 작물시험을 하였고, 그 결과는 표 2 및 표 3에 나타내었다.Relative fluorescence intensity was measured for the prepared film using a luminescence / fluorescence analyzer (photoluminescence M / C), and the results are shown in Table 1. In addition, a test vinyl house (3m × 20m × 2m) was installed as a film for the crop test for cherry tomatoes and strawberries, the results are shown in Table 2 and Table 3.

표 1Table 1

구 분division 수 지(중량%)Resin (% by weight) 광전환첨가제Optical conversion additive 안티블로킹제(중량%)Anti blocking agent (% by weight) 무적제(중량%)Invincible (wt%) 형광세기(×1000)(photon counts/sec)Fluorescence intensity (× 1000) (photon counts / sec) 종류Kinds 양(중량%)Volume (% by weight) 실시예1Example 1 96.7096.70 A1) A 1) 0.100.10 1.51.5 1.71.7 190190 실시예2Example 2 96.6596.65 AA 0.150.15 1.51.5 1.71.7 351351 실시예3Example 3 96.6096.60 AA 0.200.20 1.51.5 1.71.7 542542 실시예4Example 4 96.7096.70 B2) B 2) 0.100.10 1.51.5 1.71.7 177177 실시예5Example 5 96.6596.65 BB 0.150.15 1.51.5 1.71.7 321321 실시예6Example 6 96.6096.60 BB 0.200.20 1.51.5 1.71.7 490490 비교예1Comparative Example 1 96.8096.80 -- -- 1.51.5 1.71.7 -- 비교예2Comparative Example 2 96.6096.60 C3) C 3) 0.100.10 1.51.5 1.71.7 145145

(주) 1) 광전환 첨가제 A : Eu0.09Y2O2S 1) Light conversion additive A: Eu 0.09 Y 2 O 2 S

2) 광전환 첨가제 B : Eu0.07Y2O2S3) 2) Light Conversion Additive B: Eu 0.07 Y 2 O 2 S 3)

광전환 첨가제 C : 630T(러시아 plastopolyoner 제품)Light conversion additive C: 630T (Russian plastopolyoner product)

표 2. 방울토마토의 수확량Table 2. Yields of Cherry Tomato

필름의 종류Type of film 수확량(g)2월 5일∼2월 15일Yield (g) February 5 to February 15 수확량(g)2월 5일∼2월 25일Yield (g) February 5-February 25 수확량(g)2월 5일∼3월 4일Yield (g) February 5-March 4 방울토마토의 수2월 5일∼3월 4일Cherry tomatoes: February 5-March 4 평균중량(g)Average weight (g) 실시예 1Example 1 1089.81089.8 1367.81367.8 1790.81790.8 121121 14.814.8 실시예 2Example 2 1185.81185.8 1518.21518.2 2008.32008.3 133133 15.115.1 실시예 3Example 3 1227.91227.9 1595.81595.8 2142.02142.0 140140 15.315.3 실시예 4Example 4 1064.21064.2 1341.71341.7 1752.01752.0 120120 14.614.6 실시예 5Example 5 1154.01154.0 1473.31473.3 1951.91951.9 131131 14.914.9 실시예 6Example 6 1214.81214.8 1579.01579.0 2128.02128.0 140140 15.215.2 비교예 1Comparative Example 1 1063.51063.5 1217.91217.9 1367.41367.4 106106 12.912.9 비교예 2Comparative Example 2 1066.71066.7 1233.11233.1 1607.41607.4 114114 14.114.1

상기 표 1과 표 2에서 알 수 있는 바와 같이, 본 발명의 무기형광제를 광전환 첨가제로 이용한 수지조성물로 제조된 필름은 동량의 기존 유로피움착화물 무기 형광제를 이용한 경우보다 광전환 효율이 우수하고, 그로 인해 작물 수확량 촉진 효과도 더욱 우수한 것으로 나타났다.As can be seen in Table 1 and Table 2, the film made of a resin composition using the inorganic fluorescent agent of the present invention as a light conversion additive has a light conversion efficiency than when using the same amount of the conventional europium complexed inorganic fluorescent agent It is excellent, and the crop yield promoting effect is also excellent.

표 3. 딸기 수확량Table 3. Strawberry Yield

필름의 종류Type of film 수확량(g)4월 4일∼4월 14일Yield (g) April 4 to April 14 수확량(g)4월 4일∼4월 24일Yield (g) April 4 to April 24 수확량(g)4월 4일∼5월 4일Yield (g) April 4-May 4 방울토마토의 수4월 4일∼5월 4일Cherry tomatoes: April 4-May 4 평균중량(g)Average weight (g) 실시예 1Example 1 826.4826.4 1037.31037.3 1358.01358.0 140140 9.79.7 실시예 2Example 2 850.2850.2 1088.61088.6 1440.01440.0 144144 10.010.0 실시예 3Example 3 853.7853.7 1109.51109.5 1489.21489.2 146146 10.210.2 실시예 4Example 4 804.7804.7 1014.61014.6 1324.81324.8 138138 9.69.6 실시예 5Example 5 822.7822.7 1050.41050.4 1391.61391.6 142142 9.89.8 실시예 6Example 6 836.0836.0 1086.71086.7 1464.51464.5 145145 10.110.1 비교예 1Comparative Example 1 879.2879.2 1006.91006.9 1130.51130.5 133133 8.58.5 비교예 2Comparative Example 2 801.6801.6 990.1990.1 1278.41278.4 136136 9.49.4

본 발명의 무기형광제가 함유된 수지조성물은 기존의 유로피움 착화물계 무기형광제에 비하여 제조공정이 간단하고 가격도 저렴하며, 또한 광전환 효율이 뛰어나 수확량 촉진효과가 우수한 장점을 갖는다.The resin composition containing the inorganic fluorescent agent of the present invention has the advantages of a simple manufacturing process, low cost, and excellent light conversion efficiency compared to the conventional europium complex-based inorganic fluorescent agent, and has an excellent yield promoting effect.

Claims (2)

고분자수지와 광전환첨가제로서 하기 일반식의 무기 형광제를 0.08∼0.25중량% 함유하는 것을 특징으로 하는 광전환 필름용 수지조성물.A resin composition for a light conversion film, comprising 0.08 to 0.25% by weight of an inorganic fluorescent agent of the following general formula as a polymer resin and a light conversion additive. EumYnOkSl Eu m Y n O k S l 상기 식에서, m=0.01∼0.2, n=2∼3, k=2∼3, l=0∼1 이다.Wherein m = 0.01 to 0.2, n = 2 to 3, k = 2 to 3, and l = 0 to 1. 제 1 항에 있어서, 고분자수지는 폴리올레핀계 수지, 에틸렌/비닐아세테이트 공중합체, 폴리스티렌, ABS 수지, 염화폴리비닐, 염화폴리비닐리덴, 염화비닐/아세트산비닐 공중합체, 폴리카보네이트, 아크릴산수지, 에폭시수지, 폴리에스테르, 폴리아미드, 폴리우레탄, 니트로셀룰로우스 및 이들의 공중합체를 구성하는 단량체로이루어진 공중합체와 같은 열가소성 수지 및 열경화성 수지로부터 선택되는 것을 특징으로 하는 광전환 필름용 수지조성물.The method of claim 1, wherein the polymer resin is a polyolefin resin, ethylene / vinyl acetate copolymer, polystyrene, ABS resin, polyvinyl chloride, polyvinylidene chloride, vinyl chloride / vinyl acetate copolymer, polycarbonate, acrylic resin, epoxy resin And a thermoplastic resin and a thermosetting resin such as polyester, polyamide, polyurethane, nitrocellulose, and a copolymer composed of monomers constituting a copolymer thereof.
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KR100404977B1 (en) * 1996-06-27 2004-03-19 삼성아토피나주식회사 Resin composition for light conversion film
KR19980068864A (en) * 1997-02-25 1998-10-26 장사인 Agricultural polymer film and its production method
WO1999027006A1 (en) * 1997-11-25 1999-06-03 Ljubov Robertovna Bratkova Light-converting material and composition for producing the same
KR102036217B1 (en) * 2012-07-30 2019-10-24 어플라이드 머티리얼즈 이스라엘 리미티드 System and method for temperature control of a semiconductor wafer
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KR100942691B1 (en) 2008-06-05 2010-02-16 (주)엔담 Ethylene vinyl acetate fluorescence color former stick instead of neon sign

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