KR940002035B1 - Process for producing a silicone coating film - Google Patents

Process for producing a silicone coating film Download PDF

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Publication number
KR940002035B1
KR940002035B1 KR1019910009466A KR910009466A KR940002035B1 KR 940002035 B1 KR940002035 B1 KR 940002035B1 KR 1019910009466 A KR1019910009466 A KR 1019910009466A KR 910009466 A KR910009466 A KR 910009466A KR 940002035 B1 KR940002035 B1 KR 940002035B1
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South Korea
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silicone
film
silicone coating
coating film
producing
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KR1019910009466A
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Korean (ko)
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KR930000572A (en
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홍영기
서춘식
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주식회사 에스.케이.씨
최준식
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Priority to KR1019910009466A priority Critical patent/KR940002035B1/en
Priority to CA002069134A priority patent/CA2069134A1/en
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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
    • C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
    • C08J7/04—Coating
    • C08J7/0427—Coating with only one layer of a composition containing a polymer binder
    • 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
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
    • C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
    • C08J2323/10—Homopolymers or copolymers of propene
    • C08J2323/12—Polypropene
    • 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
    • C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
    • C08J2367/02—Polyesters derived from dicarboxylic acids and dihydroxy 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
    • C08J2483/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers

Abstract

The silicone-coated film is produced by (a) adding a solvent soluble dyestuff of a mixed cpd. of azo, anthraquinone, thioindigoid, quinolone or indanthrene cpd., and metal salt into a silicone coating soln. mixed with 0.1-5.0 wt.% silicone resin, 0.1-1.0 wt.% silicone curing catalyst and residual solvent, and (b) coating a silicon soln. added with 0.01-0.5 wt.% dyestuff on a transparent film i.e. polyethyleneterephthalate (PET) or oriented polypropylene (OPP) film. The silicone-coated film is used in the field of building materials.

Description

실리콘 코팅 필름의 제조방법Manufacturing Method of Silicone Coating Film

본 발명은 실리콘 코팅 필름(Silicone coated Film)의 제조방법에 관한 것으로, 더욱 상세하게는 건축자재 분야에 널리 적용되는 실리콘 코팅 필름에 있어서 실리콘 코팅액을 투명필름상에 도포하므로써, 실리콘 코팅처리 후, 코팅처리된 부분이 색상을 나타내도록 하여 코팅처리되지 않은 기존의 투명필름과 쉽게 구별되도록 한 새로운 실리콘 코팅필름에 관한 것이다.The present invention relates to a method for producing a silicone coated film, and more particularly, in the silicone coating film widely applied in the field of building materials, by coating a silicone coating liquid on a transparent film, the coating after the silicone coating treatment The present invention relates to a new silicone coating film which allows the treated part to exhibit a color so that it can be easily distinguished from an existing uncoated transparent film.

일반적으로, 실리콘 코팅 필름은 건축자재(The Shingle of roofing) 분야에 널리 쓰이는 것으로서, PET(Polyethylene Terephthalate), OPP(Oriented Polypropylene)와 같은 통상의 투명필름상에 필름의 권취시 또는 적층시 필름 상호간이 서로 쉽게 분리되도록 하기 위하여 실리콘 수지와 경화제류 및 용제류로 혼합 구성된 실리콘 코팅액을 도포하여 투명필름은 내열성이 좋은 PET를 사용하고, 두께는 9μ∼50μ의 것을 사용한다.In general, the silicone coating film is widely used in the construction materials (The Shingle of roofing) field, when the film is rolled or laminated on a conventional transparent film such as polyethylene terephthalate (PET), Oriented Polypropylene (OPP) In order to easily separate from each other, a silicone coating liquid mixed with a silicone resin, a curing agent, and a solvent is applied, and the transparent film uses PET having good heat resistance, and a thickness of 9μ to 50μ is used.

그러나, 이와같이 투명필름상에 실리콘 코팅액을 도포함에 있어서, 종래에는 투명필름상에 실리콘 코팅액을 처리하기전 상태와 처리한 후의 상태가 모두 투명한 상태가 되기 때문에 코팅작업 중 작업자가 육안으로 실리콘 코팅여부를 정확히 판단할 수 없어서 혼동을 일으키기 쉽다는 문제가 있었다.However, in applying the silicone coating liquid on the transparent film as described above, since the state before and after the treatment of the silicone coating liquid on the transparent film is both transparent state, the operator visually checks whether the silicone coating is performed during the coating operation. There is a problem that it is easy to confuse because it can not be accurately judged.

또한, 제조과정 중이나 제조 후의 가공작업시 실리콘 코팅처리된 필름에 실리콘 코팅처리되지 않은 필름이 섞여진 상태로 출하됨에 따라 필름의 권취나 적층시 필름 상호간의 분리가 쉽게 이루어지지 않는 등 제품에 대한 신뢰도가 저하된다는 문제가 있고, 또한 여러종류의 필름을 취급하는 점포에서도 일반 투명필름과 실리콘 코팅 필름을 혼동한 우려가 많아 판매자나 사용자 모두에게 매우 불편하다는 문제가 있었다.In addition, since the uncoated film is mixed with the silicon-coated film during the manufacturing process or during the manufacturing process, the film is not easily separated from each other when the film is wound or laminated. There is a problem that is lowered, and there is a concern that the store handling several kinds of films confuse the general transparent film and the silicone coating film, which is very uncomfortable for both the seller and the user.

본 발명은 이와같은 종래의 제반 문제점을 해결하기 위한 것으로, 미량의 염료가 첨가된 새로운 조성의 실리콘 코팅액을 기존의 투명필름상에 코팅하므로써, 코팅처리된 부분이 색상을 나타내도록 하여 실리콘 코팅 작업시 작업자가 실리콘 코팅 여부의 판별을 쉽게 할 수 있도록 하고, 실리콘 코팅되지 않은 필름이 실리콘 코팅처리된 필름속에 섞여 들어가는 것을 미연에 방지하며, 최종 공정인 슬릿팅(Slitting) 작업 후 육안검사 만으로도 코팅되지 않은 부분이 코팅된 부분속에 혼입되었는지의 여부를 손쉽게 판별할 수 있도록 한 새로운 실리콘 코팅 필름을 제공하는데 그 목적이 있다.The present invention is to solve such a conventional problem, by coating a silicone coating liquid of a new composition with a small amount of dye is added to the existing transparent film, so that the coated portion shows a color when the silicone coating operation It makes it easy for the operator to determine whether the silicon coating is applied, and it prevents the uncoated film from being mixed into the silicon coated film, and it is not coated by visual inspection after the slitting work. It is an object of the present invention to provide a new silicone coating film which makes it easy to determine whether a part has been incorporated into a coated part.

이하, 본 발명을 상세히 설명하면 다음과 같다.Hereinafter, the present invention will be described in detail.

본 발명은 실리콘 코팅처리된 필름에 있어서, 실리콘 수지와 경화제류 및 용제류로 혼합 구성된 기존의 실리콘 코팅액 조성에 용제 용해성(Solvent Soluble) 염료가 0.01∼0.5 중량% 첨가된 실리콘 코팅액이 도포되어 있는 실리콘 코팅 필름을 그 특징으로 한다.The present invention is a silicone coating film, the silicone coating liquid is added to the silicone coating solution of 0.01 to 0.5% by weight of solvent soluble (Solvent Soluble) dye to the existing silicone coating liquid composition consisting of a silicone resin, a curing agent and a solvent The coating film is characterized by that.

이하, 본 발명을 상세히 설명하면 다음과 같다.Hereinafter, the present invention will be described in detail.

본 발명은 통상의 투명필름으로서 특히 PET 또는 OPP 필름으로서 그 두께가 9∼50㎛인 것에 적용하는바, 이러한 투명필름이 권취시나 적층시 상호 접착되어 쉽게 분리되지 않은 현상을 방지하게 위하여 실리콘 코팅액으로 코팅 처리한 실리콘 코팅 필름을 제조하는 것이다.The present invention is applied to a conventional transparent film, especially PET or OPP film having a thickness of 9 ~ 50㎛, such a transparent film is bonded to each other during winding or lamination to prevent the phenomenon that is not easily separated by a silicone coating liquid It is to prepare a coated silicone coating film.

본 발명에 따른 실리콘 코팅 필름은 실리콘 수지 0.1∼5.0 중량%와 실리콘 경화촉매 0.1∼1 중량% 및 잔여량의 용제가 혼합되어 이루어지는 통상의 실리콘 코팅액에 아조계, 안드라 퀴논계, 티오인디고이드(thioindigoid)계, 퀴놀론계 또는 인단트렌(Indanthrene)계 유기화합물에 금속염이 결합된 화합물 중에서 선택된 하나 또는 2이상의 용제 용해성 염료를 코팅액 전체조성의 0.01∼0.5 중량%로 첨가한 다음, 상기의 연료가 첨가된 실리콘 용액을 투명 필름상에 코팅처리 하게 되면 종래의 기존 실리콘 코팅액을 처리한 경우와는 달리 색상이 나타나게 되며, 이 색상은 용도에 맞도록 염료나 안료를 선택하여 다양하게 처리하며 색상의 농염도 또한 다양하게 선택할 수 있다.The silicone coating film according to the present invention is azo-based, andhra-quinone-based, and thioindigoid in a conventional silicone coating liquid in which 0.1-5.0 wt% of a silicone resin, 0.1-1 wt% of a silicone curing catalyst, and a residual amount of solvent are mixed. One or two or more solvent-soluble dyes selected from compounds in which metal salts are bonded to the organic, quinolone-based or indanthrene-based organic compounds are added at 0.01 to 0.5% by weight of the total coating liquid, and then the silicon to which the fuel is added When the solution is coated on a transparent film, a color appears unlike the conventional silicone coating solution, and this color is variously treated by selecting dyes or pigments to suit the purpose. You can choose to.

이때, 상기한 용제 용해성 염료가 0.01 중량% 보다 적은량으로 첨가되면 색상 발색효과가 너무 적어 첨가효과를 기대할 수 없고, 0.5 중량% 보다 많은량으로 첨가되면 발색효과는 좋으나 색상이 너무 진하고 발리력(peeling force)과 같은 물성이 저하되어 제품상의 문제가 발생하며, 바람직한 첨가량은 0.02∼0.1 중량%이다.In this case, when the solvent-soluble dye is added in an amount less than 0.01% by weight, the color development effect is too small to add the effect, and when added in an amount of more than 0.5% by weight, the color development effect is good but the color is too dark and peeling Physical properties such as force) are lowered to cause product problems, and the preferred amount is 0.02 to 0.1 wt%.

상기 사용되는 실리콘 수지로는 축합 또는 부가반응된 무용제형의 수지를 선택하여 사용하는데, 예를들면 다양한 실록산 화합물(≡SiOH 또는 ≡SiCH =CH2)과 가교제(HSi≡, ROSi≡, HOSi≡) 성분에 열강화가 가능한 촉매를 선택하여 제조하며, 이때 사용되는 촉매는 축합반응일 경우 주석(Sn) 계 촉매를 사용하며, 부가반응일 경우는 백금촉매를 사용하여 열경화된 실리콘 수지피막을 형성시킨다. 부가반응을 선택할 경우 염료에 의한 촉매피독 발생이 우려되므로 선택사용시 신중을 기하여야 한다.As the silicone resin used, a solvent of a condensation or addition reaction type is selected and used, for example, various siloxane compounds (화합물 SiOH or? SiCH = CH 2 ) and a crosslinking agent (HSiHS, ROSi≡, HOSi≡). A catalyst capable of thermally strengthening the component is selected, and the catalyst used is a tin (Sn) catalyst in the case of condensation reaction and a platinum catalyst in the case of the addition reaction to form a thermosetting silicone resin film. . When the addition reaction is selected, the poisoning of the catalyst may cause the poisoning of the dye.

또한, 용제는 통상적으로 n-헵탄과 메틸에틸케톤 및 톨루엔이 약 5 : 3 : 1로 혼합된 용액이 사용된다.In addition, a solvent is usually a solution in which n-heptane, methyl ethyl ketone, and toluene are mixed at about 5: 3: 1.

본 발명에서의 코팅처리는 공지의 방법을 이용하는 바, 예컨대 바이코팅(Bar Coating) 이나 리버스(Reverse) 또는 그라비아 코팅(Gravure Coating)후, 열풍 또는 복사열로 건조하는 방법을 이용한다.The coating treatment in the present invention uses a known method, such as bar coating, reverse or gravure coating, and then drying by hot air or radiant heat.

특히, 온도에 대해서는 통상적으로 필름이 변형되지 않는 조건에서 가능한 한 높은 온도를 유지시켜서 체류시간(건조시간)은 길수록 좋은 경화효과를 얻을 수 있지만 필름의 변형과 생산성을 고려하여 선택해야 한다.In particular, the temperature is generally maintained at the highest possible temperature under the condition that the film does not deform, so that the longer the residence time (drying time) can obtain a good curing effect, but should be selected in consideration of the deformation and productivity of the film.

이와같이 제조된 실리콘 코팅 필름은 180°분리시의 박리력이 0.5∼2.0g/㎝이며, 배면전사율이 30% 이내인 것으로서, 코팅처리 전과 코팅처리 후의 상태가 색상에 의해 뚜렷이 구분됨에 따라 실리콘 코팅처리되지 않은 필름이 실리콘 코팅처리된 필름에 혼힙되는 것이 방지되어 제품의 신뢰도가 제고되는 효과가 있으며, 특히 최종 공정인 슬릿팅 작업후, 육안검사 만으로도 실리콘 코팅되지 않은 필름의 혼입여부를 손쉽게 판별할 수 있으므로 작업성이 향상된다는 효과가 있다.The silicone coating film thus prepared has a peel force of 0.5 to 2.0 g / cm at 180 ° separation, and has a back transfer rate of less than 30%, and the silicone coating is clearly distinguished by color before and after the coating treatment. Since the untreated film is prevented from being mixed with the silicon-coated film, the reliability of the product is improved. In particular, after the slitting operation, which is the final process, it is easy to determine whether the uncoated film is mixed by visual inspection alone. As a result, workability is improved.

또한 본 발명에 의한 필름의 중요물성은 용도에 맞는 다양한 색상(7 color-무지개색)을 임의 선택사용할 수 있으며, 농염 또는 조절할 수 있다.In addition, the important physical properties of the film according to the present invention can be arbitrarily used in a variety of colors (7 color-rainbow color) to suit the purpose, can be concentrated or adjusted.

특히, 필름에 형성된 실리콘층의 접착력과 경화도가 매우 중요하며, 마모에 의한 내구성, 접착제로의 이행성, 도포층의 박리력 등을 잘 관리 보존하여야 한다.In particular, the adhesion and the degree of curing of the silicone layer formed on the film is very important, it should be well managed and preserved durability by wear, transferability to the adhesive, peeling force of the coating layer and the like.

[평가방법][Assessment Methods]

1. 박리력 : 1인치 스카치테이프를 실리콘 도포면에 5㎏ 힘으로 밀착한 후, 100㎜/분 속도로 180°로 분리시 걸리는 힘(g/인치)1. Peeling force: 1 inch Scotch tape is adhered to silicon coated surface with 5kg force, and the force applied when separating 180 ° at 100mm / min speed (g / inch)

2. 전사율 : 1인치 스카치테이프를 실리콘 도포면에 5㎏ 힘으로 밀착하고, 100℃/10분 방치후 100㎜/분 속도로 180°분리시 도포 전후힘을 비교하여 나눈것(%)2. Transfer rate: 1inch Scotch tape is adhered to silicon coated surface with 5kg force, and it is divided by comparing the force before and after applying 180 ° separation at 100mm / min after leaving 100 ℃ / 10 minutes (%).

3. 내구성 : 마른헝겊(거즈)를 20회 문지른 후(반복) 박리력 변화를 측정하는 것3. Durability: measuring the change of peeling force after rubbing (repeat) a dry cloth (gauze) 20 times

이와같은 본 발명을 실시예에 의거 상세히 설명하면 다음과 같다.The present invention will be described in detail with reference to Examples.

[실시예 1]Example 1

[축합반응][Condensation reaction]

실리콘 코팅액을 다음의 조성으로 하여 4.5g/㎡의 량으로 PET, OPP의 필름표면에 코팅처리한다.The silicone coating solution is coated on the film surface of PET and OPP in an amount of 4.5 g / m 2 with the following composition.

[실리콘 코팅액 조성][Silicone Coating Liquid Composition]

-실리콘 수지(일본 도오시바 제품 YC 6843) 3%3% silicone resin (YC 6843, manufactured by Toshiba, Japan)

-Sn계 실리콘 경화촉매제 Ⅰ(일본 도오시바 제품 YC 6831) 0.12%-Sn based silicone curing catalyst Ⅰ (YC 6831 manufactured by Toshiba, Japan) 0.12%

-Sn계 실리콘 경화촉매제 Ⅱ(일본 도오시바 제품 YC 6919) 0.06%-Sn based silicone curing catalyst Ⅱ (YC 6919 from Toshiba, Japan) 0.06%

-티오인디고이드계 유기염료(상품명 "오라졸") 0.02%-Thioindigoide organic dye (trade name "Orazole") 0.02%

-n-헵탄 50%-n-heptane 50%

-메틸에틸케톤 30%-Methyl ethyl ketone 30%

톨루엔 16.8%Toluene 16.8%

상기조성을 이용한 코팅처리는 실리콘 코팅액을 그라비아 방식으로 필름에 도포한 다음 180℃의 열품으로 건조하여 연한 회색을 띠는 실리콘 코팅 필름을 제조하였다.In the coating treatment using the composition, the silicone coating solution was applied to the film in a gravure manner, and then dried with a hot product at 180 ° C. to prepare a light gray silicone coating film.

[실시예 2]Example 2

[부가반응][Additional reaction]

실리콘 코팅액을 다음의 조성으로 하여 3.0g/㎡의 량으로 PET, OPP의 필름표면에 코팅처리한다.The silicone coating solution is coated on the film surface of PET and OPP in an amount of 3.0 g / m 2 with the following composition.

[실리콘 코팅액 조성][Silicone Coating Liquid Composition]

-실리콘 수지(일본 신네츄 제품 KS-774) 2%2% silicone resin (KS-774 from Shin-Nechu, Japan)

-PE계 실리콘 경화촉매제(일본 신네츄 제품 PL-4) 0.04%-PE type silicone curing catalyst (PL-4, Shin-Nechu Japan) 0.04%

-n-헵탄 70.0%-n-heptane 70.0%

-MEK 20.0%-MEK 20.0%

-톨루엔 7.93%Toluene 7.93%

-티오인디고이드계 유기염료(상품명 네오자판) 0.03%-Thioindigoide organic dye (brand name Neozapan) 0.03%

상기 조성을 이용한 코팅처리는 실리콘 코팅액을 그라비아 방식으로 필름에 도포한 다음, 160℃의 열품으로 건조하여 연한 청색을 띠는 실리콘 필름을 제조하였다.In the coating treatment using the composition, the silicone coating solution was applied to the film in a gravure manner, and then dried with a hot product at 160 ° C. to produce a light blue silicone film.

Claims (5)

실리콘 코팅처리된 필름의 제조방법에 있어서, 실리콘 수지가교제, 경화촉진제 및 용제가 혼합 구성된 통상의 실리콘 코팅액 조성에 용제 용해성 염료를 0.01∼0.5 중량%로 첨가하여 도포함을 특징으로 하는 실리콘 코팅 필름의 제조방법.In the method for producing a silicone-coated film, the silicone coating film characterized in that the coating by adding a solvent soluble dye in 0.01 to 0.5% by weight to a conventional silicone coating liquid composition composed of a silicone resin crosslinking agent, a curing accelerator and a solvent Manufacturing method. 제1항에 있어서, 상기 용제 용해성 염료는 아조계, 안드라 퀴논계, 티오인디고이드(thioindigoid)계, 퀴놀린계 또는 인단트렌(Indanthrene)계 유기화합물에 금속염이 결합된 화합물 중에서 선택된 하나 또는 2이상의 혼합물인 것을 특징으로 하는 실리콘 코팅 필름의 제조방법.The method of claim 1, wherein the solvent soluble dye is one or a mixture of two or more selected from azo, andhra quinone, thioindigoid, quinoline or indanthrene-based compound of the metal salt Method for producing a silicone coating film, characterized in that. 제1항에 있어서, 상기 실리콘 수지는 축합 또는 부가반응된 무용제형의 수지를 선택하여 사용함을 특징으로 하는 실리콘 코팅 필름의 제조방법.According to claim 1, wherein the silicone resin is a method of producing a silicone coating film, characterized in that the condensation or addition-reaction of the non-solvent type resin selected. 제1항에 있어서, 상기 투명 필름은 PET 또는 OPP로서 그 두께가 9∼5㎛인 것을 사용함을 특징으로 하는 실리콘 코팅 필름의 제조방법.The method of claim 1, wherein the transparent film is PET or OPP, and has a thickness of 9 μm to 5 μm. 제1항에 있어서, 상기 실리콘 코팅 필름은 그 박리력이 180°분리시 0.5∼2.0g/㎝이며, 배면 전사율이 30% 이내인 것을 특징으로 하는 실리콘 코팅 필름의 제조방법.The method of claim 1, wherein the silicone coating film has a peel force of 0.5 to 2.0 g / cm at 180 ° separation and a back transfer ratio of 30% or less.
KR1019910009466A 1991-06-08 1991-06-08 Process for producing a silicone coating film KR940002035B1 (en)

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KR1019910009466A KR940002035B1 (en) 1991-06-08 1991-06-08 Process for producing a silicone coating film
CA002069134A CA2069134A1 (en) 1991-06-08 1992-05-21 Silicone coating composition for film

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
KR1019910009466A KR940002035B1 (en) 1991-06-08 1991-06-08 Process for producing a silicone coating film

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KR930000572A KR930000572A (en) 1993-01-15
KR940002035B1 true KR940002035B1 (en) 1994-03-14

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CA2069134A1 (en) 1992-12-09

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