JP2824529B2 - Emulsion adhesive for vinyl chloride resin - Google Patents
Emulsion adhesive for vinyl chloride resinInfo
- Publication number
- JP2824529B2 JP2824529B2 JP16177789A JP16177789A JP2824529B2 JP 2824529 B2 JP2824529 B2 JP 2824529B2 JP 16177789 A JP16177789 A JP 16177789A JP 16177789 A JP16177789 A JP 16177789A JP 2824529 B2 JP2824529 B2 JP 2824529B2
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- Prior art keywords
- chloride resin
- vinyl chloride
- adhesive
- weight
- emulsion
- 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.)
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Description
【発明の詳細な説明】 産業上の利用分野 本発明は、塩化ビニル樹脂用接着剤に関し、詳しく
は、例えば、塩化ビニル樹脂床材の接着に好適に用いる
ことができる接着剤に関する。Description: BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an adhesive for vinyl chloride resin, and more particularly, to an adhesive which can be suitably used for bonding vinyl chloride resin flooring, for example.
従来の技術 一般に、塩化ビニル樹脂床材用接着剤には、酢酸ビニ
ル、エポキシ樹脂系等の溶剤系接着剤とエマルジヨン系
等の水性接着剤とが用いられている。溶剤系接着剤は、
その接着力は比較的大きいものの、その施用時に有機溶
剤が揮散し、悪臭を生じるのみならず、引火や作業環
境、大気等の汚染を引き起こすおそれがあり、しかも、
施用後も、残存溶剤に起因して、床材に反りやふくれを
生じることもある。2. Description of the Related Art In general, as a vinyl chloride resin flooring adhesive, a solvent-based adhesive such as vinyl acetate or epoxy resin and a water-based adhesive such as emulsion-based are used. Solvent-based adhesives
Although its adhesive strength is relatively large, the organic solvent is volatilized at the time of application, and not only generates a bad smell, but also there is a risk of causing ignition, work environment, pollution of the atmosphere and the like.
Even after application, flooring may warp or bulge due to residual solvent.
これに対して、水性接着剤は、上記のような問題はな
いが、一般に、接着力、特に、剥離接着力が低く、接着
後に床材が剥離することがあるうえに、粘着性に乏しい
ので、多くは、粘着力等の初期性能を向上させるため
に、天然ゴム等のゴム物質が多量に配合されている。し
かし、このようにゴム物質を多量に配合することは、接
着剤の製造費用を高める。On the other hand, the water-based adhesive does not have the above-mentioned problems, but generally has a low adhesive strength, particularly, a peeling adhesive strength, and the floor material may be peeled off after bonding, and furthermore, it has poor tackiness. In many cases, a large amount of a rubber substance such as natural rubber is blended in order to improve initial performance such as adhesive strength. However, incorporation of such a large amount of rubber substance increases the production cost of the adhesive.
既に、アクリロニトリル及びブタジエンを主成分と
し、或いはアクリロニトリル、ブタジエン、スチレン及
びアクリル酸エステルを主成分とし、場合によつては、
アクリル酸、メタクリル酸等の不飽和酸成分を含む共重
合体のエマルジヨンや、このようなエマルジヨンの接着
剤への応用は、例えば、特公昭55−27567号公報、特開
昭56−145909号公報、特公昭62−19764号公報等に記載
されているように、知られている。また、特公昭62−84
43号公報には、アクリロニトリル、ブタジエン、スチレ
ン等の単量体成分からなる共重合体エマルジヨンを塗工
紙やカーペツト裏張りに用いることが記載されている。Already, acrylonitrile and butadiene as main components, or acrylonitrile, butadiene, styrene and acrylate as main components, and in some cases,
The application of copolymers containing unsaturated acid components such as acrylic acid and methacrylic acid to emulsions and the application of such emulsions to adhesives are described, for example, in JP-B-55-27567 and JP-A-56-145909. As described in JP-B-62-19764 and the like, it is known. In addition, Japanese Patent Publication No. 62-84
No. 43 describes that a copolymer emulsion comprising a monomer component such as acrylonitrile, butadiene, and styrene is used for a coated paper or a carpet backing.
しかしながら、従来、塩化ビニル樹脂、特に、塩化ビ
ニル樹脂床材に用いて、接着力にすぐれるエマルジヨン
系接着剤は知られておらず、かかる塩化ビニル樹脂床材
用エマルジヨン系接着剤が強く要望されている。However, conventionally, an emulsion adhesive having excellent adhesive strength, which is used for a vinyl chloride resin, particularly, a vinyl chloride resin floor material, has not been known. Such an emulsion adhesive for a vinyl chloride resin floor material has been strongly demanded. ing.
発明が解決しようとする課題 本発明は、かかる要望に応えるためになされたもので
あつて、多量のゴム物質の配合を必要とせずして、接着
力にすぐれるのみならず、粘着力のような初期性能や耐
油性等にもすぐれるエマルジヨン系塩化ビニル樹脂用接
着剤を提供することを目的とする。SUMMARY OF THE INVENTION The present invention has been made in order to meet such a demand, and does not require the compounding of a large amount of a rubber substance. It is an object of the present invention to provide an emulsion adhesive based vinyl chloride resin adhesive having excellent initial performance and excellent oil resistance.
課題を解決するための手段 本発明による塩化ビニル樹脂用エマルジヨン接着剤
は、メタクリロニトリル成分10〜75重量％、共役ジエン
成分90〜25重量％及びビニル芳香族化合物成分10〜35重
量％を含む共重合体のエマルジヨンを含有することを特
徴とする。The emulsion adhesive for vinyl chloride resin according to the present invention comprises 10 to 75% by weight of a methacrylonitrile component, 90 to 25% by weight of a conjugated diene component and 10 to 35% by weight of a vinyl aromatic compound component. It is characterized by containing a copolymer emulsion.
本発明において用いる共重合体エマルジヨンは、メタ
クリロニトリル成分10〜75重量％、共役ジエン成分90〜
25重量％及びビニル芳香族化合物成分10〜35重量％を含
み、好ましくは、メタクリロニトリル成分15〜45重量
％、共役ジエン成分85〜55重量％及びビニル芳香族化合
物成分10〜35重量％を含む。The copolymer emulsion used in the present invention contains 10 to 75% by weight of a methacrylonitrile component and 90 to 90% of a conjugated diene component.
25% by weight and 10-35% by weight of a vinyl aromatic compound component, preferably 15-45% by weight of a methacrylonitrile component, 85-55% by weight of a conjugated diene component and 10-35% by weight of a vinyl aromatic compound component. Including.
共重合体エマルジヨンにおいて、単量体成分中、メタ
クリロニトリル成分が５重量％よりも少ないときは、得
られる接着剤が塩化ビニル樹脂、特に、塩化ビニル樹脂
性床材に対する接着力において劣り、他方、75重量％を
越えるときは、得られる接着剤が塩化ビニル樹脂、特
に、塩化ビニル樹脂性床材に対する接着力において劣る
のみならず、エマルジヨンのゴム弾性が失なわれるの
で、得られる接着剤は、粘着力に乏しく、初期性能に劣
る。In the copolymer emulsion, when the methacrylonitrile component in the monomer component is less than 5% by weight, the obtained adhesive is inferior in adhesion to a vinyl chloride resin, particularly, a vinyl chloride resin floor material. If the amount exceeds 75% by weight, the obtained adhesive not only has poor adhesive strength to vinyl chloride resin, particularly to vinyl chloride resin flooring, but also loses the rubber elasticity of the emulsion. Poor adhesion and poor initial performance.
共役ジエン成分としては、ブタジエン、イソプレン、
クロロプレン等が用いられ、特に、ブタジエン又はイソ
プレンが好ましく用いられる。共重合体エマルジヨンに
おいて、共役ジエン成分が90重量％を越えるときは、得
られる接着剤が塩化ビニル樹脂、特に、塩化ビニル樹脂
性床材に対する接着力において劣り、25重量％よりも少
ないときは、得られる接着剤が初期性能に劣る。As the conjugated diene component, butadiene, isoprene,
Chloroprene or the like is used, and butadiene or isoprene is particularly preferably used. In the copolymer emulsion, when the conjugated diene component exceeds 90% by weight, the obtained adhesive is inferior in adhesive strength to vinyl chloride resin, particularly, vinyl chloride resin flooring, and when the adhesive is less than 25% by weight, The resulting adhesive has poor initial performance.
本発明においては、共重合体エマルジヨンは、前記メ
タクリロニトリル成分及び共役ジエン成分に加えて、ビ
ニル芳香族化合物成分を10〜35重量％の範囲で含有す
る。ここに、ビニル芳香族化合物としては、スチレン、
メチルスチレン、ビニルトルエン等を挙げることができ
るが、特に、スチレンが好ましく用いられる。In the present invention, the copolymer emulsion contains a vinyl aromatic compound component in a range of 10 to 35% by weight in addition to the methacrylonitrile component and the conjugated diene component. Here, as the vinyl aromatic compound, styrene,
Methylstyrene, vinyltoluene and the like can be mentioned, but styrene is particularly preferably used.
更に、本発明においては、機械的安定性、耐油性等を
向上させるために、α，β−不飽和カルボン酸や不飽和
アミド等の変性単量体を添加することができる。かかる
α，β−不飽和カルボン酸としては、例えば、アクリル
酸、メタクリル酸、イタコン酸等のほか、例えば、２−
ヒドロキシエチルアクリル酸、２−ヒドロキシプロピル
メタクリル酸等の水酸基を有するものを挙げることがで
きる。不飽和アミドとしては、例えば、Ｎ−ヒドロキシ
メチルアクリルアミド、アクリルアミド、メタクリルア
ミド等を挙げることができる。これらは、いずれも単量
体全体に対して、10重量％以下の範囲で用いることがで
きる。Further, in the present invention, a modified monomer such as α, β-unsaturated carboxylic acid or unsaturated amide can be added to improve mechanical stability, oil resistance and the like. Examples of the α, β-unsaturated carboxylic acid include, for example, acrylic acid, methacrylic acid, itaconic acid, etc .;
Examples having a hydroxyl group such as hydroxyethylacrylic acid and 2-hydroxypropylmethacrylic acid can be given. Examples of the unsaturated amide include N-hydroxymethylacrylamide, acrylamide, methacrylamide and the like. Any of these can be used in a range of 10% by weight or less based on the whole monomer.
また、本発明においては、得られる接着剤の耐油性を
高めるために、共重合体は、アクリロニトリルを５〜20
重量％の範囲にて含有することができる。特に、メタク
リロニトリル10〜20重量％及びアクリロニトリル10〜20
重量％の範囲で用いることが好ましい。In the present invention, in order to increase the oil resistance of the obtained adhesive, the copolymer is acrylonitrile 5-20.
It can be contained in the range of weight%. In particular, methacrylonitrile 10-20% by weight and acrylonitrile 10-20%
It is preferable to use it in the range of weight%.
本発明において用いる共重合体エマルジヨンは、通
常、乳化重合によつて得ることができる。乳化重合は、
常法に従つて、乳化剤としてロジン酸アルカリ金属塩、
ドデシルベンゼンスルホン酸ナトリウム等、重合開始剤
として過硫酸カリウム等の過硫酸塩やラジカル重合開始
剤又はレドツクス触媒系ラジカル重合開始剤等、分子量
調整剤としてｔ−ドデシルメルカプタンのようなアルキ
ルメルカプタンを用い、通常、０〜100℃の温度にて前
記単量体成分を水性媒体中にて乳化重合させればよい。
重合は、通常、単量体転化率が95〜98％に達するまで行
なわれる。The copolymer emulsion used in the present invention can be usually obtained by emulsion polymerization. Emulsion polymerization is
According to a conventional method, an alkali metal rosinate is used as an emulsifier,
Such as sodium dodecylbenzenesulfonate, a polymerization initiator such as persulfate such as potassium persulfate or a radical polymerization initiator or a redox catalyst-based radical polymerization initiator, and an alkyl mercaptan such as t-dodecyl mercaptan as a molecular weight regulator, Usually, the monomer component may be emulsion-polymerized in an aqueous medium at a temperature of 0 to 100 ° C.
The polymerization is usually carried out until the monomer conversion reaches 95-98%.
上記乳化重合は、得られるエマルジヨンの粒子径を均
一にするために、少量の芳香族ビニル化合物、例えば、
スチレンを予め乳化重合させて、シードとするシード重
合法を行なつてもよい。また、単量体成分を一括して重
合系に加える一括仕込み法のほか、単量体成分を分割し
て重合系に加える分割重合法を用いることもできる。The emulsion polymerization, in order to make the particle size of the resulting emulsion uniform, a small amount of an aromatic vinyl compound, for example,
A seed polymerization method in which styrene is preliminarily emulsion-polymerized and used as a seed may be performed. In addition to the batch charging method in which the monomer components are collectively added to the polymerization system, a split polymerization method in which the monomer components are divided and added to the polymerization system can also be used.
発明の効果 本発明による接着剤は、以上のように、メタクリロニ
トリル成分と共役ジエン成分とビニル芳香族化合物成分
とを含む共重合体エマルジヨンを含有する水性接着剤で
あつて、多量のゴム物質を配合せずして、塩化ビニル樹
脂、特に、塩化ビニル樹脂床材に対してすぐれた接着力
を有し、更に、初期性能や耐油性にもすぐれる。Effect of the Invention As described above, the adhesive according to the present invention is an aqueous adhesive containing a copolymer emulsion containing a methacrylonitrile component, a conjugated diene component and a vinyl aromatic compound component. By not blending, it has excellent adhesion to vinyl chloride resin, especially vinyl chloride resin flooring, and also has excellent initial performance and oil resistance.
実施例 以下に実施例を挙げて本発明を説明するが、本発明は
これら実施例により何ら限定されるものではない。以下
において部は重量部を示す。EXAMPLES Hereinafter, the present invention will be described with reference to examples, but the present invention is not limited to these examples. In the following, "part" indicates "part by weight".
実施例１及び比較例１ 温度計及び撹拌機を備えた1L容量オートクレーブにド
デシルベンゼンスルホン酸ナトリウム６部を脱イオン水
240部と共に仕込み、撹拌下に溶解させ、これに第１表
に示すように、ブタジエン50部、スチレン35部、メタク
リロニトリル10部、メタクリル酸５部、ｔ−ドデシルメ
ルカプタン0.5部及びクレジルハイドロパーオキサイド
0.4部と共に、ロンガリツト、硫酸鉄及びEDTAの混合物
の水溶液（ロンガリツト／硫酸鉄/EDTAの４ナトリウム
塩重量比10/0.01/1、50％水溶液）0.8部を加え、40℃に
て反応させて、共重合体エマルジヨンを得た。Example 1 and Comparative Example 1 In a 1 L autoclave equipped with a thermometer and a stirrer, 6 parts of sodium dodecylbenzenesulfonate was deionized water.
Charged together with 240 parts and dissolved under stirring, and as shown in Table 1, 50 parts of butadiene, 35 parts of styrene, 10 parts of methacrylonitrile, 5 parts of methacrylic acid, 0.5 part of t-dodecylmercaptan and 0.5 part of cresyl hydro Peroxide
Along with 0.4 parts, 0.8 parts of an aqueous solution of a mixture of Rongalite, iron sulfate and EDTA (10 / 0.01 / 1 weight ratio of tetrasodium salt of Rongalite / iron sulfate / EDTA, 50% aqueous solution) was added and reacted at 40 ° C. A copolymer emulsion was obtained.
同様にして、比較例１として、第１表に示すように、
スチレン35部とメタクリロニトリル10部に代えて、スチ
レン45部を用いた以外は、上記と同様にして、共重合体
エマルジヨンを得た。Similarly, as Comparative Example 1, as shown in Table 1,
A copolymer emulsion was obtained in the same manner as described above, except that 45 parts of styrene was used instead of 35 parts of styrene and 10 parts of methacrylonitrile.
得られた共重合体エマルジヨンにおいて、単量体の重
合率、全固形分及び粒子径を第１表に示す。Table 1 shows the polymerization rate of the monomer, the total solid content, and the particle size of the obtained copolymer emulsion.
実施例２〜５ 第１表に示す割合にてそれぞれの単量体を用いた以外
は、実施例１と同様にして、共重合体エマルジヨンを得
た。得られた共重合体エマルジヨンにおいて、単量体の
重合率、全固形分及び粒子径を第１表に示す。Examples 2 to 5 Copolymer emulsions were obtained in the same manner as in Example 1 except that the respective monomers were used in the proportions shown in Table 1. Table 1 shows the polymerization rate of the monomer, the total solid content, and the particle size of the obtained copolymer emulsion.
（試験例１） 次に、このようにして得られた共重合体エマルジヨン
を下記した重量部数割合にて充填剤、粘着付与剤、増粘
剤等と均一に混合して、接着剤を調製した。 (Test Example 1) Next, the copolymer emulsion thus obtained was uniformly mixed with a filler, a tackifier, a thickener and the like in the following parts by weight ratio to prepare an adhesive. .
エマルジヨン（固形分） 100 消泡剤a) 0.3 炭酸カルシウム 180 非イオン性界面活性剤b) 3 粘着付着剤c) 74 増粘剤d) 1.3 （注）ａ）シリコンKM−71（信越化学工業（株）） ｂ）エマルゲン930（花王（株）） ｃ）ハイレジンN060（日本石油化学工業（株））
の70％トルエン溶液 ｄ）アロンA7100（アロン化成工業（株）） このようにして得られた接着剤について、オープンタ
イム10分とし、市販の塩化ビニル樹脂製床材を接着し、
７日間養生した後、引張速度200mm/分にて90゜剥離強度
を測定した。結果を第２表に示す。Emulsion (solid content) 100 Defoamer a) 0.3 Calcium carbonate 180 Nonionic surfactant b) 3 Adhesive c) 74 Thickener d) 1.3 (Note) a) Silicon KM-71 (Shin-Etsu Chemical Co., Ltd.) B) Emulgen 930 (Kao Corporation) c) High Resin N060 (Nippon Petrochemical Industry Co., Ltd.)
D) Aron A7100 (Aron Kasei Kogyo Co., Ltd.) The adhesive thus obtained was set to an open time of 10 minutes, and a floor material made of a commercially available vinyl chloride resin was bonded.
After curing for 7 days, the 90 ° peel strength was measured at a tensile speed of 200 mm / min. The results are shown in Table 2.
実施例６ 温度計及び撹拌機を備えた1L容量オートクレーブにド
デシルベンゼンスルホン酸ナトリウム４部と過硫酸ナト
リウム0.8部を脱イオン水240部と共に仕込み、撹拌下に
溶解させ、これにメタクリロニトリル28部、スチレン28
部、ブタジエン136部、メタクリル酸８部及びｔ−ドデ
シルメルカプタン２部を加え、60℃に昇温し、反応させ
て、共重合体エマルジヨンを得た。 Example 6 Into a 1 L autoclave equipped with a thermometer and a stirrer, 4 parts of sodium dodecylbenzenesulfonate and 0.8 parts of sodium persulfate were charged together with 240 parts of deionized water, dissolved under stirring, and 28 parts of methacrylonitrile was added thereto. , Styrene 28
Parts, butadiene 136 parts, methacrylic acid 8 parts and t-dodecyl mercaptan 2 parts were added, and the mixture was heated to 60 ° C. and reacted to obtain a copolymer emulsion.
（試験例２） 次に、このようにして得られた共重合体エマルジヨン
を下記した重量部数割合にて充填剤、粘着付与剤、増粘
剤等と均一に混合して、接着剤を調製した。(Test Example 2) Next, the copolymer emulsion thus obtained was uniformly mixed with a filler, a tackifier, a thickener and the like in the following parts by weight ratio to prepare an adhesive. .
エマルジヨン（固形分） 100 トリポリリン酸ナトリウム 0.5 炭酸カルシウム 180 粘着付与剤a) 80 増粘剤b) 4 （注）ａ）ハイレジンN060（日本石油化学工業（株））
の70％トルエン溶液 ｂ）アロンA7100（アロン化成工業（株）） 接着試験 このようにして得られた接着剤をスレート板（JIS A
5403）に櫛ごてを用いて、幅75mmに塗布し、オープンタ
イム５分後、塩化ビニル樹脂シート（2.5×10cm）をそ
の上に載置し、ローラにて３往復の圧締（線圧2kg/cm）
を行ない、その７日後に引張速度200mm/分にて90゜剥離
強度を測定したところ、3.02kg/20mmであった。Emulsion (solid content) 100 Sodium tripolyphosphate 0.5 Calcium carbonate 180 Tackifier a) 80 Thickener b) 4 (Note) a) High Resin N060 (Nippon Petrochemical Industries, Ltd.)
B) Aron A7100 (Aron Kasei Kogyo Co., Ltd.) Adhesion test Adhesive obtained in this manner is applied to a slate plate (JIS A
5403) using a comb to apply a width of 75 mm, and after 5 minutes of open time, place a vinyl chloride resin sheet (2.5 × 10 cm) on it and press it back and forth with a roller (linear pressure). 2kg / cm)
After 7 days, the 90 ° peel strength was measured at a pulling speed of 200 mm / min and found to be 3.02 kg / 20 mm.
Claims (6)
役ジエン成分90〜25重量％及びビニル芳香族化合物成分
10〜35重量％を含む共重合体のエマルジヨンを含有する
ことを特徴とする塩化ビニル樹脂用エマルジヨン接着
剤。1. A methacrylonitrile component of 10 to 75% by weight, a conjugated diene component of 90 to 25% by weight and a vinyl aromatic compound component
An emulsion adhesive for a vinyl chloride resin, comprising a copolymer emulsion containing 10 to 35% by weight.
とする請求項第１項に記載の塩化ビニル樹脂用エマルジ
ヨン接着剤。2. The emulsion adhesive for a vinyl chloride resin according to claim 1, wherein the conjugated diene is butadiene.
を特徴とする請求項第１項に記載の塩化ビニル樹脂用エ
マルジヨン接着剤。3. The emulsion adhesive for vinyl chloride resin according to claim 1, wherein the vinyl aromatic compound is styrene.
を10重量％以下の範囲にて含有することを特徴とする請
求項第１項記載の塩化ビニル樹脂用エマルジヨン接着
剤。4. The emulsion adhesive for a vinyl chloride resin according to claim 1, wherein the copolymer contains an α, β-unsaturated carboxylic acid component in an amount of 10% by weight or less.
はメタクリル酸であることを特徴とする請求項第４項記
載の塩化ビニル樹脂用エマルジヨン接着剤。5. The emulsion adhesive for a vinyl chloride resin according to claim 4, wherein the α, β-unsaturated carboxylic acid is acrylic acid or methacrylic acid.
重量％含有することを特徴とする請求項第１項記載の塩
化ビニル樹脂用エマルジヨン接着剤。6. The copolymer according to claim 5, wherein the acrylonitrile component is 5 to 20%.
The emulsion adhesive for a vinyl chloride resin according to claim 1, wherein the adhesive is contained by weight.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP16177789A JP2824529B2 (en) | 1989-06-23 | 1989-06-23 | Emulsion adhesive for vinyl chloride resin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP16177789A JP2824529B2 (en) | 1989-06-23 | 1989-06-23 | Emulsion adhesive for vinyl chloride resin |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0326775A JPH0326775A (en) | 1991-02-05 |
| JP2824529B2 true JP2824529B2 (en) | 1998-11-11 |
Family
ID=15741709
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP16177789A Expired - Fee Related JP2824529B2 (en) | 1989-06-23 | 1989-06-23 | Emulsion adhesive for vinyl chloride resin |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2824529B2 (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE4404411A1 (en) * | 1994-02-11 | 1995-08-17 | Basf Ag | Dispersion floor adhesive |
| JP3675975B2 (en) * | 1996-07-29 | 2005-07-27 | 日本ゼオン株式会社 | Adhesive for vinyl chloride resin |
| ES2706479T3 (en) * | 2013-03-19 | 2019-03-29 | Nippon A&L Inc | Latex copolymer for adhesive and adhesive composition |
-
1989
- 1989-06-23 JP JP16177789A patent/JP2824529B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0326775A (en) | 1991-02-05 |
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