JP2645762B2 - Impact resistant paint - Google Patents
Impact resistant paintInfo
- Publication number
- JP2645762B2 JP2645762B2 JP3509891A JP50989191A JP2645762B2 JP 2645762 B2 JP2645762 B2 JP 2645762B2 JP 3509891 A JP3509891 A JP 3509891A JP 50989191 A JP50989191 A JP 50989191A JP 2645762 B2 JP2645762 B2 JP 2645762B2
- Authority
- JP
- Japan
- Prior art keywords
- weight
- plasticizer
- acetate copolymer
- paint
- pvc
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
- 239000003973 paint Substances 0.000 title claims description 18
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 16
- 229920003023 plastic Polymers 0.000 claims description 13
- 239000004033 plastic Substances 0.000 claims description 13
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 8
- 239000004014 plasticizer Substances 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 7
- 229920002689 polyvinyl acetate Polymers 0.000 claims description 7
- 239000011118 polyvinyl acetate Substances 0.000 claims description 7
- 239000000945 filler Substances 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 6
- 239000000654 additive Substances 0.000 claims description 5
- 238000000576 coating method Methods 0.000 claims description 5
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims description 4
- 239000003086 colorant Substances 0.000 claims description 4
- 229920001577 copolymer Polymers 0.000 claims description 4
- 239000003381 stabilizer Substances 0.000 claims description 4
- 239000000853 adhesive Substances 0.000 claims description 3
- 230000001070 adhesive effect Effects 0.000 claims description 3
- 238000009533 lab test Methods 0.000 claims description 3
- 239000012528 membrane Substances 0.000 claims description 3
- 239000004575 stone Substances 0.000 claims description 3
- 239000013008 thixotropic agent Substances 0.000 claims description 3
- 239000011248 coating agent Substances 0.000 claims description 2
- XNGIFLGASWRNHJ-UHFFFAOYSA-N o-dicarboxybenzene Natural products OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 claims 2
- -1 phthalic acid ester Chemical class 0.000 claims 2
- 230000000996 additive effect Effects 0.000 claims 1
- 239000000178 monomer Substances 0.000 description 4
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 description 2
- 239000002270 dispersing agent Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229920002554 vinyl polymer Polymers 0.000 description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 1
- MQIUGAXCHLFZKX-UHFFFAOYSA-N Di-n-octyl phthalate Natural products CCCCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCCC MQIUGAXCHLFZKX-UHFFFAOYSA-N 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- CERQOIWHTDAKMF-UHFFFAOYSA-M Methacrylate Chemical compound CC(=C)C([O-])=O CERQOIWHTDAKMF-UHFFFAOYSA-M 0.000 description 1
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical group C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- BJQHLKABXJIVAM-UHFFFAOYSA-N bis(2-ethylhexyl) phthalate Chemical compound CCCCC(CC)COC(=O)C1=CC=CC=C1C(=O)OCC(CC)CCCC BJQHLKABXJIVAM-UHFFFAOYSA-N 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D127/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers
- C09D127/02—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment
- C09D127/04—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
- C09D127/06—Homopolymers or copolymers of vinyl chloride
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Paints Or Removers (AREA)
Description
【発明の詳細な説明】 本発明は、可塑材と、プラスチック製の中空球体と炭
酸カルシウムから成る充填材とを加えた、PVCを主成分
とする衝撃応力に耐える塗料に関する。Description: TECHNICAL FIELD The present invention relates to a paint resistant to impact stress mainly composed of PVC, which comprises a plasticizer and a filler made of plastic hollow spheres and calcium carbonate.
この種の塗料は、飛石による衝撃から保護される、例
えば、防食床裏の様な自動車の外板部品に用いられる。This type of paint is used for automotive skin components, such as anticorrosive floors, which are protected from the impact of stepping stones.
密度を減少するため、そして、従って、エネルギー節
約をするために、この様な塗料中にプラスチック製の中
空球体を使用することは公知である。（欧州特許公開公
報第26388号と、日本国特許公告公報平１−16870号参
照）この様な中空のプラスチック球体は通常の充填材の
一部に置き換えられると共に、当該先行技術中では、大
きな割合で少なくとも0.5ないし５重量％の範囲内で使
用されているが、但し、これより遥かに大きな割合でも
使用される。It is known to use plastic hollow spheres in such coatings in order to reduce the density and thus save energy. (See European Patent Publication No. 26388 and Japanese Patent Publication No. 1-16870.) Such hollow plastic spheres can be replaced by a part of ordinary fillers and have a large proportion in the prior art. At least in the range of 0.5 to 5% by weight, but much higher proportions are used.
しかしながら、経済性が改善されるには、密度減少ば
かりではなく、とりわけ膜の強さが高いこと、貯蔵安定
性に優れることが要求される。However, in order to improve the economic efficiency, it is required not only that the density is reduced, but also that the strength of the membrane be high and that the storage stability be excellent.
塗料が車両の初期の装備に使用される場合には貯蔵安
定性に優れていることが絶対的に必要である。When the paint is used for the initial equipment of a vehicle, it is absolutely necessary that the paint has excellent storage stability.
当該先行技術はこれらの条件に合致するような塗料を
提供することができなかった。The prior art has failed to provide a coating that meets these requirements.
とりわけ、PVC共重合体と組み合わせてジオクチルフ
タレートを使用すると、非常に短い貯蔵安定性になるこ
とがある。In particular, the use of dioctyl phthalate in combination with a PVC copolymer can result in very short storage stability.
これは、25ないし30℃において顕著な膨潤が予想され
るからであり、このため20℃で３ケ月の貯蔵期間であ
る。今日では普通に要求される貯蔵条件に合致すること
はできなくなる。（この貯蔵可能性、即ち貯蔵安定性
は、35℃で65時間に亘る実験室での耐久試験法を用いて
決定される。） 特に炭酸カルシウムである充填材の40％以上の比較的
に大量の添加は、膜の強さの低下につながる。This is because a significant swelling is expected at 25-30 ° C, and thus a storage period of 3 months at 20 ° C. Today it is no longer possible to meet the storage requirements that are normally required. (This storability, i.e., storage stability, is determined using a laboratory endurance test method at 65 ° C for 65 hours.) Relatively large amounts of more than 40% of the filler, especially calcium carbonate Addition leads to a decrease in the strength of the film.
全く一般的に充填材の添加は、ある種の状況下では相
当に膜の強さを減少することがある。Quite generally, the addition of fillers can, under certain circumstances, significantly reduce film strength.
密度を減少するために用いられたプラスチック製の中
空球体の体積は120℃以上で非常に早く０に向かって降
下する。The volume of plastic hollow spheres used to reduce the density drops very quickly to zero above 120 ° C.
塗料は保護すべき金属板表面に塗布された後で、一般
に130ないし170℃の温度負荷が加えられ、その結果とし
てプラスチック製中空球体がまず溶ける。上記温度にお
いてこのゲル工程を通して塗料は、中空球体の空洞をつ
ぶさない程充分に強固となる。公知の方法では、全般に
約30％の密度減少を得ることが可能である。After the paint has been applied to the surface of the metal sheet to be protected, a temperature load of generally 130 to 170 ° C. is applied, so that the plastic hollow spheres first melt. At this temperature, through this gel process, the paint is sufficiently strong not to collapse the cavities of the hollow sphere. With the known method, it is possible to obtain a density reduction of generally about 30%.
しかしながら、この方法は非常にコスト高である。更
に機械的強度、特に膜の強さが低下する。However, this method is very expensive. Furthermore, the mechanical strength, especially the strength of the film, is reduced.
従って、先行技術の塗料から出発して、その密度減少
にもかかわらず膜の強さが高いことと、優れた貯蔵安定
性を有する塗料を提供することが本発明の目的である。It is therefore an object of the present invention to provide, starting from prior art paints, a paint having a high film strength despite its reduced density and having excellent storage stability.
この目的は、以下の請求の範囲第１項の特徴部により
達成される。This object is achieved by the features of claim 1 below.
即ち、該塗料が PVCを 20ないし30重量％と、 ポリビニルアセテート共重合体を10ないし20重量％と、
炭酸カルシウムを 15ないし20重量％と、 プラスチック製中空球体を 0.3ないし0.4重量％と、 可塑剤を 30ないし40重量％と、 それらに、着色剤と添加剤（揺変剤と接着剤とシンナ
ーと安定剤）を加えて合計100重量％にした組成を有
し、少なくとも４ないし7N/mm2の膜の強さと、20℃で３
ヶ月間の貯蔵安定剤（または実験室での試験で35℃で65
時間の貯蔵安定性）と、多くても1200kg/m3の密度を有
し、更に、鎖の長さの値Ｋ＝60と、約14重量％のアセテ
ート含有量を有するアセテート共重合体が用いられる、
衝撃応力に耐える塗料により達成される。That is, the paint contains 20 to 30% by weight of PVC, 10 to 20% by weight of polyvinyl acetate copolymer,
15 to 20% by weight of calcium carbonate, 0.3 to 0.4% by weight of hollow plastic spheres, 30 to 40% by weight of plasticizer, and colorants and additives (thixotropic agent, adhesive, thinner, etc.) (Stabilizer) to a total of 100% by weight, a film strength of at least 4 to 7 N / mm 2 and a
Monthly storage stabilizer (or 65 at 35 ° C in laboratory tests)
Storage stability over time) and an acetate copolymer having a density of at most 1200 kg / m 3 and a chain length value K = 60 and an acetate content of about 14% by weight. Can be
Achieved by paints that withstand impact stress.
各従属請求項の特徴は、本発明の別の展開を提供する
ものである。これらにより請求の範囲第５項および第６
項に記載の用途が可能となる利点がある。The features of each dependent claim provide another development of the invention. According to these, claims 5 and 6
There is an advantage that the use described in the section is enabled.
本発明の塗料は、その上、経済的に興味深い。何故な
らば、膜の強さが高いことが用いられるべき充填材のコ
スト減少を可能にするからである。The coatings according to the invention are moreover economically interesting. This is because the high strength of the membrane allows a reduction in the cost of the filler to be used.
更に、その場合材料の組成は、通常工業的に使用され
ている方法により、飛石による損傷に対する抵抗が大変
良好となるように、即ち、最低でも８時間は良好となる
ように調整される。Furthermore, the composition of the materials is then adjusted by the methods commonly used in the industry so that the resistance to stepping stone damage is very good, ie at least 8 hours.
このような試験においては５ないし8mmのサイズの砂
利が合計で300g用いられる。In such a test, a total of 300 g of gravel having a size of 5 to 8 mm is used.
膜の強さが増すと同時に優れた貯蔵安定性が得られる
のは、恐らく、特に高いＫ値と、同時に高アセテート含
有量を有するポリビニル共重合体が用いられるという事
実に帰因する。The increased storage strength and at the same time the excellent storage stability obtained are probably due to the fact that particularly high K values and at the same time polyvinyl copolymers having a high acetate content are used.
更に、プラスチック製中空球体が従来使用されて来た
中空の無機物と比較して大変低い耐摩耗性しか有しない
ので、プラスチック製中空球体を少量たった0.3ないし
0.4重量％加えることは適切な密度減少となると共に、
摩損の改善となる。Furthermore, plastic hollow spheres have very low abrasion resistance as compared to conventionally used hollow inorganic materials, so that only a small amount of plastic hollow spheres of 0.3 to
Adding 0.4% by weight leads to a proper density reduction,
This leads to an improvement in wear.
別の重要な特徴は、分散剤の添加を必要としないこと
である。Another important feature is that no additional dispersant is required.
このことは、実質的なコスト削減に結びつく。分散剤
が別の技術的な不利益を有することがあるからである。This leads to substantial cost savings. This is because dispersants can have other technical disadvantages.
次いで、約200バールの圧力で公知の「エアレス」方
式を用いて本発明の組成物を噴射することもできるが、
それは、また、車両の初期装備用としての使用を容易に
する。The composition of the present invention can then be sprayed using a known `` airless '' method at a pressure of about 200 bar,
It also facilitates use for initial equipment of the vehicle.
本発明の塗料は次の組成を有する。 The paint of the present invention has the following composition.
即ち、 PVC 20〜30重量％ ポリビニルアセテート共重合体 10〜20重量％ 炭酸カルシウム 15〜20重量％ プラスチック製中空球体 0.3〜0.4重量％ 可塑剤 30〜40重量％ それに、着色剤と各種添加剤（揺変剤、接着剤、シン
ナー並びに安定剤）を加えて合計100重量％のものであ
る。That is, PVC 20-30% by weight Polyvinyl acetate copolymer 10-20% by weight Calcium carbonate 15-20% by weight Plastic hollow sphere 0.3-0.4% by weight Plasticizer 30-40% by weight In addition, colorant and various additives ( (A thixotropic agent, an adhesive, a thinner, and a stabilizer).
鎖の長さの価、即ちＫ値＝60と約14重量％のアセテー
ト含有量を有するアセテート共重合体を用いれば、適当
な選択により、少なくとも４ないし7N/mm2の膜の強さと
（35℃で65時間の実験室試験に対応する）20℃で３ケ月
の貯蔵期間、更に、多くても1200kg/m2好ましくは1100k
g/m2の密度を得ることができる。With an acetate copolymer having a chain length value, i.e. K value = 60, and an acetate content of about 14% by weight, with appropriate choice, a film strength of at least 4 to 7 N / mm @ 2 (35 (Corresponds to a laboratory test at 65 ° C. for 65 hours) 3 months storage period at 20 ° C., and at most 1200 kg / m 2, preferably 1100 k
A density of g / m 2 can be obtained.
次の特定材料組成物ＡとＢは、特別に優れたものであ
ることが判明した。The following specific material compositions A and B proved to be particularly excellent.
即ち、 である。That is, It is.
ここでのポリビニルアセテート共重合体は、ビニルア
セテートと、ビニルモノマー及び／又はスチレンモノマ
ー及び／又はアクリレートモノマー及び／又はメタアク
リレートモノマー及び／又はエチレンモノマー等のいわ
ゆる当業者にとって周知の単量体との共重合体である。The polyvinyl acetate copolymer here is a mixture of vinyl acetate and a monomer known to those skilled in the art, such as a vinyl monomer and / or a styrene monomer and / or an acrylate monomer and / or a methacrylate monomer and / or an ethylene monomer. It is a copolymer.
Claims (6)
酸カルシウムから成る充填材とを加えた、PVCを主成分
とする衝撃応力に耐える塗料において、 該塗料が PVCを 20ないし30重量％と、 ポリビニルアセテート共重合体を10ないし20重量％と、
炭酸カルシウムを 15ないし20重量％と、 プラスチック製中空球体を 0.3ないし0.4重量％と、 可塑剤を 30ないし40重量％と、 それらに、着色剤と添加剤（揺変剤と接着剤とシンナー
と安定剤）を加えて合計100重量％にした組成を有し、
少なくとも４ないし7N/mm2の膜の強さと、20℃で３ケ月
間の貯蔵安定性（または実験室での試験で35℃で65時間
の貯蔵安定性）と、多くても1200kg/m3の密度を有し、
更に、鎖の長さの値Ｋ＝60と、約14重量％のアセテート
含有量を有するアセテート共重合体が用いられる、衝撃
応力に耐える塗料。1. A paint which contains a plasticizer, a plastic hollow sphere and a filler made of calcium carbonate and which withstands an impact stress mainly composed of PVC, wherein the paint contains 20 to 30% by weight of PVC. 10 to 20% by weight of a polyvinyl acetate copolymer,
15 to 20% by weight of calcium carbonate, 0.3 to 0.4% by weight of hollow plastic spheres, 30 to 40% by weight of plasticizer, and colorants and additives (thixotropic agent, adhesive, thinner, etc.) Stabilizer) to a total of 100% by weight,
A membrane strength of at least 4 to 7 N / mm 2 , storage stability for 3 months at 20 ° C. (or storage stability at 35 ° C. for 65 hours in laboratory tests) and at most 1200 kg / m 3 Having a density of
In addition, impact-stress resistant coatings are used in which an acetate copolymer having a chain length value K = 60 and an acetate content of about 14% by weight is used.
ビニルアセテート共重合体とフタル酸エステルの比が１
対２である請求の範囲第１項に記載の塗料。2. The method according to claim 1, wherein the plasticizer is a phthalic acid ester and the ratio of the polyvinyl acetate copolymer to the phthalic acid ester is one.
2. The coating according to claim 1, wherein the ratio is two.
の範囲第１項または第２項に記載の塗料。 PVC 23.0 ポリビニルアセテート共重合体 17 炭酸カルシウム 15.1 プラスチック製中空球体 0.3 可塑剤 33.8 着色剤 0.3 添加剤 10.53. A paint according to claim 1 or claim 2 having the following composition (expressed in% by weight): PVC 23.0 Polyvinyl acetate copolymer 17 Calcium carbonate 15.1 Plastic hollow sphere 0.3 Plasticizer 33.8 Colorant 0.3 Additive 10.5
の範囲第１項に記載の塗料。 PVC 28.0 ポリビニルアセテート共重合体 10.0 炭酸カルシウム 18 プラスチック製中空球体 0.4 可塑剤 38.0 添加剤 5.64. A paint according to claim 1, having the following composition (expressed in% by weight): PVC 28.0 Polyvinyl acetate copolymer 10.0 Calcium carbonate 18 Plastic hollow spheres 0.4 Plasticizer 38.0 Additives 5.6
床裏用に用いられる請求の範囲第１項ないし第４項のう
ちいずれかに記載の塗料。5. The paint according to claim 1, which is used for an anticorrosive floor of a vehicle which is protected from damage caused by flying stones.
いられる請求の範囲第５項に記載の塗料。6. The paint according to claim 5, which is used for initial equipment of mass-produced vehicles.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE19904018022 DE4018022C1 (en) | 1990-06-05 | 1990-06-05 | |
| DE4018022.0 | 1990-06-05 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH05500685A JPH05500685A (en) | 1993-02-12 |
| JP2645762B2 true JP2645762B2 (en) | 1997-08-25 |
Family
ID=6407829
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP3509891A Expired - Fee Related JP2645762B2 (en) | 1990-06-05 | 1991-06-03 | Impact resistant paint |
Country Status (5)
| Country | Link |
|---|---|
| JP (1) | JP2645762B2 (en) |
| DE (1) | DE4018022C1 (en) |
| GB (1) | GB2251439B (en) |
| TR (1) | TR25019A (en) |
| WO (1) | WO1991018953A1 (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SE500077C2 (en) * | 1992-06-03 | 1994-04-11 | Casco Nobel Ab | Plastisol-based coating composition, method of spray coating a surface and use of the coating composition as coating composition on cars |
| SE510857C2 (en) * | 1994-11-14 | 1999-06-28 | Casco Products Ab | Coating composition based on polyvinyl chloride plastisol containing thermoplastic microspheres |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE2939141C2 (en) * | 1979-09-27 | 1982-07-08 | Basf Farben + Fasern Ag, 2000 Hamburg | Use of coating compounds |
| JPH0781100B2 (en) * | 1986-04-21 | 1995-08-30 | 日本特殊塗料株式会社 | Ultra lightweight chipping resistant paint for airless painting |
| US4889562A (en) * | 1987-06-16 | 1989-12-26 | Ciba-Geigy Corporation | Organic pigments coated with crosslinked ethyl cellulose |
| JPH0364347A (en) * | 1989-08-02 | 1991-03-19 | Cemedine Co Ltd | High physical property chipping resistant paint |
-
1990
- 1990-06-05 DE DE19904018022 patent/DE4018022C1/de not_active Expired - Fee Related
-
1991
- 1991-06-03 WO PCT/EP1991/001026 patent/WO1991018953A1/en not_active Ceased
- 1991-06-03 JP JP3509891A patent/JP2645762B2/en not_active Expired - Fee Related
- 1991-06-05 TR TR91/0569A patent/TR25019A/en unknown
-
1992
- 1992-02-05 GB GB9202417A patent/GB2251439B/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| GB2251439B (en) | 1993-08-25 |
| JPH05500685A (en) | 1993-02-12 |
| DE4018022C1 (en) | 1991-11-28 |
| GB9202417D0 (en) | 1992-03-18 |
| GB2251439A (en) | 1992-07-08 |
| TR25019A (en) | 1992-09-01 |
| WO1991018953A1 (en) | 1991-12-12 |
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