TW200300155A

TW200300155A - Polychloroprene latex composition, water-base primer and adhesive bonding process

Info

Publication number: TW200300155A
Application number: TW091132525A
Authority: TW
Inventors: Kenji Mochizoki; Kosuke Watanabe
Original assignee: Denki Kagaku Kogyo Kk
Priority date: 2001-11-02
Filing date: 2002-11-01
Publication date: 2003-05-16
Also published as: KR100880136B1; CN100339426C; KR20040062562A; CN1582315A; WO2003037980A1; TWI275610B

Abstract

The invention provides a water-base primer or adhesive capable of giving a bond strength equivalent to that of organic solvent type primers or adhesives of the prior art; specifically, a polychloroprene latex composition which comprises as the essential components polychloroprene and sodium orthosilicate in a state dispersed or dissolved in water and further contains polyethyleneimine and a tackifier resin; adhesive bonding is conducted by using a water-base primer containing the latex composition.

Description

200300155 A7 B7 五、發明説明（彳) 技術範圍 (請先閲讀背面之注意事項再填寫本頁) 本發明是對橡膠彈性體，合成樹脂等的被著體有良好的粘著強度的發現’用於此等被著體的粘著水系粘著劑或水系底漆的主成分來說是給與有用的聚氯丁二烯系乳膠組成物。技術背景歷來要粘著橡膠彈性體合成樹脂等的難粘著的被著體的方法來說，主要採用溶劑系的底漆或粘著劑，但是溶劑系的話則由於使用多量甲苯、乙酸乙酯、甲基乙基甲酮、對作業員的安全衛生面、環境面不好。因此粘著劑或底漆的水性化的要求年年增高，例如特開2 0 0 1 — 6 4 6 1 6或特開2 0 0 1 - 2 6 7 5 6等的幾個提案的形成。但是對實用化，還有粘著強度的不足則是現狀。本發明鑑於有關現狀，爲了匹敵於歷來使用過溶劑系的底漆或粘著劑給與粘著強度，水系底漆或水系粘著劑的主成分來說是供給合適的聚氯丁二烯系乳膠組成物爲目的經濟部智慧財產局員工消費合作社印製發明的揭示本發明人們是爲了達成上記的目的重覆精心總檢討的結果，以聚氯丁二烯與原矽酸鈉爲必須成分，彼等在水中分散、或被溶解的聚氯丁二烯系乳膠組成物對橡膠彈性體合成樹脂等的被著體，能看出賦與優異的粘著強度，以至本紙張尺度適用中國國家標準（CNS Γα4規格（210X 297公釐) c . 200300155 A7 B7 經濟部智慧財產局員工消費合作社印製五、發明説明（2 ) 於完成了本發明。亦即本發明是具有下列的要旨。 (1 )以聚氯丁二烯與原矽酸鈉爲必須成分彼等在水中或被溶解爲其特徵的聚氯丁二烯系乳膠組成物。 (2 )聚氯丁二烯系乳膠組成物中的固體成分濃度是 4 0〜7 0重量％，是在上記（1 )記載的聚氯丁二烯系乳膠組成物。 (3 )原矽酸鈉的含有量是聚氯丁二烯（固體成分） 100重量份的範圍，含有0 · 1〜30重量份在上記（ 1 )或（2 )記載的聚氯丁二烯系乳膠組成物。 (4)聚乙亞胺是聚氯丁二烯（固體成分）1 0 0重量份的範圍，含有0 · 1〜5重量份，在上記（1)〜（ 3 )任一記載的聚氯丁二烯系乳膠組成物。 (5 )粘著賦與樹脂是聚氯丁二烯（固體成分） 1 0 0重量份的範圍。含有1〜8 0重量份，在上記（1 )〜（4 )任一記載的聚氯丁二烯系乳膠組成物。 (6) 增粘劑是聚氯丁二烯（固體成分）100重量份的範圍，含有0 . 0 1〜1 0重量份在上記（1 )〜（ 5 )任一記載的聚氯丁二烯系乳膠組成物。 (7) 在上記（1)〜（6)任一記載的聚氯丁二烯系乳膠組成物。 (8 )在上記（7 )記載的用水系底漆將被著體粘著的粘著方法。爲了實施發明最好的形態 (請先閲讀背面之注意事項再填寫本頁} ·# 訂200300155 A7 B7 V. Description of the invention (彳) Technical scope (please read the precautions on the back before filling in this page) The present invention is a discovery of good adhesion strength for adherends such as rubber elastomers and synthetic resins. The main component of the water-based adhesive or water-based primer of these adherends is a useful polychloroprene-based latex composition. Technical background Conventionally, a method for adhering difficult-to-be-adhered adherends such as a rubber elastomer synthetic resin mainly uses a solvent-based primer or an adhesive. However, for a solvent-based method, a large amount of toluene and ethyl acetate are used , Methyl ethyl ketone, the safety and health aspects of the operator, the environment is not good. Therefore, the requirements for the hydration of the adhesive or the primer are increasing every year, for example, the formation of several proposals such as JP 2 0 1-6 4 6 1 6 or JP 2 0 1-2 6 7 5 6 and the like. However, for practical use, there is still a lack of adhesive strength. In view of the present situation, the present invention provides a suitable polychloroprene system for the main component of a water-based primer or a water-based adhesive in order to match the strength of a conventional solvent-based primer or a pressure-sensitive adhesive. The purpose of the latex composition is to print and invent the invention printed by the employee's consumer cooperative of the Intellectual Property Bureau of the Ministry of Economic Affairs. The inventor repeated the results of careful and comprehensive review in order to achieve the above-mentioned purpose. Polychloroprene and sodium orthosilicate are essential ingredients It can be seen that the polychloroprene-based latex composition dispersed or dissolved in water has excellent adhesion strength to adherends such as rubber elastomer synthetic resins, so that this paper scale applies Chinese national standards (CNS Γα4 specification (210X 297 mm) c. 200300155 A7 B7 Printed by the Consumer Cooperative of the Intellectual Property Bureau of the Ministry of Economic Affairs. 5. Description of the invention (2) The invention was completed. That is, the invention has the following gist. (1 ) Polychloroprene-based latex composition with polychloroprene and sodium orthosilicate as essential components, each of which is characterized by being dissolved in water or being dissolved. (2) Polychloroprene-based latex composition The solid content concentration is 40 to 70% by weight, and is a polychloroprene-based latex composition described in (1) above. (3) The content of sodium orthosilicate is polychloroprene (solid content ) 100 parts by weight, containing 0.1 to 30 parts by weight of the polychloroprene-based latex composition described in (1) or (2) above. (4) Polyethyleneimine is polychloroprene ( The solid content) is in a range of 100 parts by weight, and contains from 0.1 to 5 parts by weight. The polychloroprene-based latex composition described in any one of (1) to (3) above. (5) Adhesive administration The resin is in the range of 100 parts by weight of polychloroprene (solid content). The resin contains 1 to 80 parts by weight of the polychloroprene-based latex composition described in any one of (1) to (4) above. (6) The thickener is in a range of 100 parts by weight of polychloroprene (solid content), and contains 0.01 to 10 parts by weight of the polychloroprene described in any one of (1) to (5) above. (7) The polychloroprene-based latex composition described in any one of (1) to (6) above. (8) The water-based primer described in (7) above will adhere to the body Sticking method In order to implement the best form of the invention (Please read the precautions on the back before filling out this page} · # Order

本纸張尺度適用中國國家標準（CNS ) A4規格（210X297公釐） -6- 200300155 A7 B7 五、發明説明（3 ) 以下將本發明的內容詳細說明，本發明所云的聚氯丁二烯係2 —氯代一 1 ，3 丁二烯（以下稱爲氯丁二烯）的均聚體或係氯丁二烯與氯丁二烯經共聚合可能的單體與共聚合體。在此所示的共聚合體則是在聚氯丁二烯的存在下將其他的單體經過接枝聚合狀態也含有接枝共聚合體。上記的氯丁二烯與共聚合可能的理想單體來說，例如 2，3 二氯代一 1，3 丁二烯、1—氯代—1 ，3 丁二烯、丁二烯、異戊二烯、苯乙烯、丙烯腈、丙烯酸或其酯類、甲基丙烯酸或其酯類等是被推舉的，應於必要使用2種類以上又沒關係。爲了要得到聚氯丁二烯、氯丁二烯的聚合方法是沒有特別被限定，在依照乳化聚合方法係一般性又簡便。使適用於得到本發明的聚氯丁二烯乳膠則有必要將聚氯丁二烯在水中被分散，將聚氯丁二烯以乳化聚合法而得時則可將所得的聚氯丁二烯乳膠維持原狀來使用。在聚氯丁二烯系乳膠的乳化聚合法被使用的乳化劑及 /或分散劑並無特別限定，在通常氯丁二烯乳膠被使用的各種陰離子型、非離子型、陽離子型是可使用的。陰離子型的乳化劑來說是羧酸型、磺酸型、硫酸酯型等，例如可推舉玫瑰酸的鹼金屬鹽、碳素酸在8〜2 0個的烷基磺酸鹽、烷基芳基硫的鹽、萘磺酸鈉、甲醛與其縮合物等。非離子型的具體例來說可推舉聚乙烯醇或其共聚合體（例如丙烯醯胺與其共聚合體）、聚乙烯醚或其共聚本紙張尺度適用中國國家標準（CNS ) A4規格（210X297公釐） (請先閱讀背面之注意事項再填寫本頁) 訂This paper size applies the Chinese National Standard (CNS) A4 specification (210X297 mm) -6- 200300155 A7 B7 V. Description of the invention (3) The content of the present invention will be described in detail below. The polychloroprene used in the present invention System 2—Homopolymer of chloro-1,3 butadiene (hereinafter referred to as chloroprene) or monomer and copolymer that are possible by copolymerization of chloroprene and chloroprene. The copolymer shown here is a graft copolymer in which other monomers are subjected to graft polymerization in the presence of polychloroprene. For the chloroprene mentioned above and the ideal monomer for copolymerization, for example, 2,3 dichloro-1,3 butadiene, 1-chloro-1,3 butadiene, butadiene, isoprene Diene, styrene, acrylonitrile, acrylic acid or its esters, methacrylic acid or its esters are recommended, and two or more types should be used if necessary. The polymerization method for obtaining polychloroprene and chloroprene is not particularly limited, and it is general and simple according to the emulsion polymerization method. To make the polychloroprene latex suitable for use in the present invention, it is necessary to disperse the polychloroprene in water, and when the polychloroprene is obtained by emulsion polymerization, the obtained polychloroprene can be obtained. Use the latex as it is. The emulsifier and / or dispersant used in the emulsion polymerization method of polychloroprene-based latex is not particularly limited, and various anionic, non-ionic, and cationic types can be used in general chloroprene latex. of. Anionic emulsifiers are carboxylic acid type, sulfonic acid type, sulfuric acid ester type, and the like. For example, alkali metal salts of rose acid, alkyl sulfonates of 8 to 20 carbon acids, and alkyl aromatics can be recommended. Salts of sodium sulfide, sodium naphthalenesulfonate, formaldehyde and its condensates, and the like. Specific examples of non-ionic types include polyvinyl alcohol or its copolymers (such as acrylamide and its copolymers), polyvinyl ether or its copolymers. The paper size is applicable to the Chinese National Standard (CNS) A4 specification (210X297 mm). (Please read the notes on the back before filling this page)

經濟部智慧財產局員工消費合作社印製 200300155 A7 B7 經濟部智慧財產局員工消費合作社印製五、發明説明（4 ) 合體（例如馬來酸與其共聚合體）、聚乙烯吡咯烷酮或其共聚合體（例如乙烯基醋酸與其共聚合體）或者是將此等 (共）聚合體作化學修飾之物、或者是纖維系衍生物（經乙基纖維素）等，陽離子型的具體例來說可推舉脂肪族胺鹽、脂肪族4級銨鹽等。例如十八烷基三甲基銨氯化物、月桂基三甲基銨氯化物、二月桂基二甲基銨氯化物等。聚氯丁二烯系乳膠中的乳化劑及/或分散劑是在氯丁二烯的聚之際，將乳化劑及/或分散劑、氯丁二烯的初期下料單體的合計1 〇〇質量部理想是對〇 · 5〜2 0質量部依添加含有而含有，未滿5質量部時則乳化力不充足，如超過2 0質量部則有使耐水粘著力降低的欠點。關於本發明將聚氯丁二烯系乳膠依聚合而得時的聚合溫度並無特別限定。爲了將聚合反應圓滿的進行將聚合溫度設定在0〜5 0°C是理想。聚合的起始劑是過硫酸鉀等的過硫酸鹽。第3 - 丁基氫過氧化物等的有機過氧化物等可合適使用此等並無限定。氯丁二烯的聚合則是在應於必要可使用鏈轉移劑，其種類並無特別限定。通常在氯丁二烯的乳化聚合所使用之物是可使用的，例如正-十二烷硫醇、四-十二烷硫醇等的長鏈烷基硫醇類、二異丁黃原二硫化物或二乙黃原二硫化物等的二烷黃原二硫化物類、碘仿等的公知的鏈轉移劑是可使用的。聚氯丁二烯的聚合抑制劑（聚合禁止劑）m P (熔點）並無特別限定，例如2，6 -叔丁基一甲酚、吩噻嗪、羥基胺等是可使用的。 (請先閲讀背面之注意事項再填寫本頁) ▼衣.Printed by the Employees 'Cooperative of the Intellectual Property Bureau of the Ministry of Economic Affairs 200300155 A7 B7 Printed by the Employees' Cooperative of the Intellectual Property Bureau of the Ministry of Economic Affairs Vinyl acetic acid and its copolymers) or these (co) polymers are chemically modified, or fiber derivatives (via ethyl cellulose), etc., for specific examples of cationic types, aliphatic amines can be recommended Salt, aliphatic grade 4 ammonium salt, etc. For example, octadecyltrimethylammonium chloride, lauryltrimethylammonium chloride, dilauryldimethylammonium chloride, and the like. The emulsifier and / or dispersant in the polychloroprene-based latex is a total of 1 when the emulsifier and / or dispersant and the initial monomers of the chloroprene are cut off during the polymerization of chloroprene. 〇 The mass part is preferably contained in an amount of 0.5 to 20 mass parts. If the content is less than 5 mass parts, the emulsification power is insufficient. If the mass part exceeds 20 mass parts, there is a shortcoming that the water resistance is reduced. The polymerization temperature when the polychloroprene-based latex is polymerized in the present invention is not particularly limited. It is desirable to set the polymerization temperature to 0 to 50 ° C in order to successfully perform the polymerization reaction. The polymerization initiator is a persulfate such as potassium persulfate. Organic peroxides, such as the 3rd-butyl hydroperoxide, etc. These can be used suitably, It is not limited. In the polymerization of chloroprene, a chain transfer agent may be used as necessary, and the type thereof is not particularly limited. Usually used in the emulsion polymerization of chloroprene, such as n-dodecanethiol, tetra-dodecanethiol and other long-chain alkyl mercaptans, diisobutylxanthine Known chain transfer agents such as dioxane xanthan disulfides such as sulfide and diethylxanthane disulfide, and iodoform can be used. The polymerization inhibitor (polymerization inhibitor) m P (melting point) of the polychloroprene is not particularly limited, and for example, 2,6-tert-butylmonocresol, phenothiazine, hydroxylamine, and the like can be used. (Please read the precautions on the back before filling out this page) ▼ clothing.

本紙張尺度適用中國國家標準（CNS ) A4規格（210X297公釐） -8- 200300155 A7 B7 五、發明説明（5 ) (請先閲讀背面之注意事項再填寫本頁) 聚氯丁二烯的最終聚合率並無特別被限定，可任意作調節。未反應的單體是依據脫除單體的操作而被除去。其方法並無特別限定。本發明的聚氯丁二烯系乳膠係由於聚合而得，將聚氯丁二烯乳膠濃縮或是以水等的添加作稀釋，能將固體成分濃度控制在必要的濃度。濃縮的方法來說有減壓濃縮等，並無特別限定。關於本發明聚氯丁二烯系乳膠的性狀並無特別被限定，聚合溫度，聚合開始劑，鏈轉移劑，聚合抑制劑，最終聚合率，脫單體，濃縮條件等作恰當的選定，因要控制，有可能調整固體成分濃度，甲苯可溶部的分子量，甲苯不溶成分（凝膠含有量）等。經濟部智慧財產局員工消費合作社印製由初期粘著力與常態粘著力的平衡點，將聚氯丁二烯系乳膠中的氯丁二烯（共）聚合體的凝膠含有量，理想是調整到3〜6 0重量％爲理想，尙且凝膠含有量是如次的被要求。將聚氯丁二烯系乳膠試料作凍結乾燥，經精秤作成A。以甲苯溶解（在〇 · 6 %調製），使用遠心分離機 ’進一步用2 0 0網眼的金網將凝膠作分離，將凝膠成分風吹乾後在1 0 0 °C的空氣乾燥1小時，經精秤作成B將上記A，B使用依次式算出凝膠含有量。凝膠含有量（％)=B/Axl〇〇石夕酸鈉一*般式是以Na2〇· nS i 〇2 ·ιπΗ2〇表示，N a 2〇與S i〇2的莫耳比，亦即依係數η可分爲正位矽酸鈉、間佔矽酸鈉、矽酸鈉1號、矽酸鈉2號、矽酸本紙張尺度適用中國國家標準（CNS ) Α4規格（21〇Χ：297公釐） -9 - 200300155 A7 B7 經濟部智慧財產局員工消費合作社印製五、發明説明（6 ) 鈉3號、矽酸鈉4號等，在本發明特別是採用正位矽酸鈉、正位矽酸鈉的使用，如在後記實施例的指示與其他的砂酸鈉比較其粘著力的點得到優異的效果。在本發明聚氯丁二烯系乳膠中的正位矽酸鈉的含有量並無特別規定，但是從粘著強度的點，聚氯丁二烯1 0 0重量份（固體成分）的範圍，有0 . 1〜3 0重量份是理想，更理想是1〜 1 5重量份。本發明的聚氯丁二烯系乳膠組成物，就其原狀即可發現充分的粘著力，由於使之含有聚乙亞胺能更提高效果，聚乙亞胺的含有量是聚氯丁二烯系乳膠1 〇〇質量部（固體成分換算）對〇 · 1〜5重量份（固體成分換算）爲理想，特別理想是0 · 5〜3重量份是適當。在本發明所用的聚乙亞胺是持有下記的一般式的聚合物，合成方法並無特別限定，在一般上能依據乙抱亞胺的開環聚合來合成，以下記的一般式X、y聚合物的平均分子量是1 0 0 0以上爲理想，特別理想是選擇在成爲 1 0 0 0 0以上之樣態。 H2N-(CH2-CH2- y)x-(CH2-CH2- AT)y. CH2-CH2-N< 還有對於本發明的聚氯丁二烯系乳膠組成物。因添加粘著賦予樹脂，由於初期粘著力、耐水粘著力、粘著保持時間等的特性，能平衡於實用上之物。在水系粘著劑作配合的粘著賦予樹脂的種類是無特別受限定。爲了欲得十分的初期粘著力，軟化點溫度在5 〇本紙張尺度適用中國國家樣準（ CNS ) A4規格（210X297公潑) 二 - (請先閲讀背面之注意事項再填寫本頁) k· 訂This paper size applies Chinese National Standard (CNS) A4 specification (210X297 mm) -8- 200300155 A7 B7 V. Description of the invention (5) (Please read the precautions on the back before filling this page) The final polychloroprene The polymerization rate is not particularly limited and can be arbitrarily adjusted. Unreacted monomer is removed according to the operation of removing the monomer. The method is not particularly limited. The polychloroprene-based latex of the present invention is obtained by polymerization. By concentrating the polychloroprene-based latex or diluting it with the addition of water or the like, the concentration of the solid content can be controlled to a necessary concentration. The concentration method is not particularly limited as long as it is concentrated under reduced pressure. The properties of the polychloroprene-based latex of the present invention are not particularly limited, and the polymerization temperature, polymerization initiator, chain transfer agent, polymerization inhibitor, final polymerization rate, demonomerization, and concentration conditions are appropriately selected because To control, it is possible to adjust the solid content concentration, the molecular weight of the toluene-soluble portion, and the toluene-insoluble component (gel content). The Consumer Cooperative of the Intellectual Property Bureau of the Ministry of Economic Affairs prints the gel content of chloroprene (co) polymer in polychloroprene-based latex from the balance between initial adhesion and normal adhesion. It is ideal to be 3 to 60% by weight, and the gel content is as required. A polychloroprene-based latex sample was freeze-dried, and A was prepared by a fine scale. Dissolve in toluene (prepared at 0.6%), use a telecentric separator to further separate the gel with a 200 mesh gold mesh, and blow dry the gel components in air at 100 ° C for 1 hour. After the fine scale is made into B, the above-mentioned A and B are calculated using the sequential formula to calculate the gel content. Gel content (%) = B / Ax100 sodium oxalate * The general formula is expressed as Na2O · nS i 02 · ιπΗ2〇, and the molar ratio of Na 2 0 to S 10 2 is also That is, according to the coefficient η, it can be divided into ortho-sodium silicate, meta-sodium silicate, sodium silicate No. 1, sodium silicate No. 2, and silicate. 297 mm) -9-200300155 A7 B7 Printed by the Consumer Cooperative of the Intellectual Property Bureau of the Ministry of Economic Affairs. 5. Description of the invention (6) Sodium No. 3, Sodium Silicate No. 4, etc. In the present invention, in particular, ortho-sodium silicate, The use of ortho-sodium silicate, as indicated in the postscript examples, has an excellent effect on the point of adhesion compared to other sodium silicate. The content of ortho-sodium silicate in the polychloroprene-based latex of the present invention is not particularly specified, but from the point of adhesive strength, the range of 100 parts by weight (solid content) of polychloroprene, It is preferably 0.1 to 30 parts by weight, and more preferably 1 to 15 parts by weight. In the polychloroprene-based latex composition of the present invention, sufficient adhesion can be found in its original state. Since it contains polyethyleneimine, the effect can be further enhanced. The content of polyethyleneimine is polychloroprene The mass fraction of the latex 100 (solid content conversion) is preferably from 0.1 to 5 parts by weight (solid content conversion), and particularly preferably from 0.5 to 3 parts by weight. The polyethyleneimine used in the present invention is a polymer having the following general formula, and the synthesis method is not particularly limited. Generally, it can be synthesized by ring-opening polymerization of ethyleneimine. The general formula X, It is desirable that the average molecular weight of the y polymer is 1 000 or more, and it is particularly desirable to select a state in which the y polymer is 1 000 or more. H2N- (CH2-CH2-y) x- (CH2-CH2-AT) y. CH2-CH2-N < Also the polychloroprene-based latex composition of the present invention. The addition of the adhesion-imparting resin can balance the practical use due to characteristics such as initial adhesion, water-resistant adhesion, and adhesion holding time. The type of the adhesion-imparting resin compounded with the water-based adhesive is not particularly limited. In order to obtain a very good initial adhesion, the softening point temperature is 50. This paper size is applicable to the Chinese National Standard (CNS) A4 specification (210X297). Second-(Please read the precautions on the back before filling this page) k · Order

200300155 A7 B7 五、發明説明（7 ) (請先閲讀背面之注意事項再填寫本頁) 〜1 6 〇°C的樹脂爲理想，在具體上可推舉松香樹脂、聚合松香樹脂、α -蒎烯樹脂、/3 -蒎烯樹脂、萜烯苯酚樹脂、碳5餾分系石油樹脂、碳9餾分系石油樹脂、碳5 / 碳9餾分系石油樹脂、d C P D系石油樹脂、烷基苯酚樹脂、二甲苯樹脂、香豆酮樹脂、香豆酮茚樹脂等。其中還是松香樹脂爲理想。200300155 A7 B7 V. Description of the invention (7) (Please read the precautions on the back before filling in this page) ~ 16 ° C resin is ideal, and specifically, rosin resin, polymerized rosin resin, α-pinene can be recommended. Resin, / 3-pinene resin, terpene phenol resin, carbon 5 fraction petroleum resin, carbon 9 fraction petroleum resin, carbon 5 / carbon 9 fraction petroleum resin, d CPD petroleum resin, alkylphenol resin, Toluene resin, coumarone resin, coumarone indene resin, and the like. Among them, rosin resin is also preferable.

經濟部智慧財產局員工消費合作社印製粘著賦予樹脂的配合量是聚氯丁二烯系乳膠1 〇〇質量部（固體成分換算）對1〜8 0重量份（固體成分換算 )爲理想。特別理想是合適的5〜5 0重量份，粘著賦予樹脂的配合方法並無特別被限定，在乳膠中爲了將樹脂均勻的分散、添加水性乳膠爲理想。粘著賦予樹脂的水性乳膠的製法則是在甲苯等的有機溶劑，將被溶解之物用乳化劑在水中乳化/被分散後，將有機溶劑一面減壓一面加熱的消除方法則能在微粒子作粉碎，乳化/被分散方法等，由於微粒子的乳膠能製作前者爲理想。本發明的聚氯丁二烯系乳膠組成物的固體成分濃度是無特別被限定，爲了不使乳化系的安定性損失則是7 0重量％以下爲理想。還有將本發明的聚氯丁二烯系乳膠組成物。各自做爲水系粘著劑使用時則在4 0〜7 0重量％爲理想，做爲水系啓發劑使用時則在1 0〜4 0重量％爲理想，將固體成分濃度作調節而使用較合適。此狀的固體成分的調節能由純水稀釋或由除去水分濃縮依照任意去進行。尙且本發明的聚氯丁二烯系乳膠的固體成分濃度是可作如次的操作而求得。只秤量鋁皿得A，將乳膠試料2 ml放入鉛皿而秤量得 -11 - 本紙張尺度適用中國國家標準（CNS ) A4規格（210X297公釐） 200300155 A7 B7 經濟部智慧財產局員工消費合作社印製五、發明説明（8 ) B，將乳膠試料放入鉛皿在1 1 〇 °c的空氣下乾燥2小時後，秤量得C。固體成分濃度（重量％)是由下式算出。固體成分濃度（％) = [(C-A)/(B-A)]X 1〇〇關於本發明聚氯丁二烯系乳膠組成物作上述以外也要配合要求性能，則可任意添加增粘劑、金屬氧化物、充塡劑、造膜助劑、紫外線吸收劑、氧化防止劑、可塑劑、硫化劑、硫化促進劑、消泡劑等。本發明的聚氯丁二烯系乳膠組成物，因配合增粘劑在任意的粘度有調節的可能。具體上的增粘劑來^說可推舉聚乙烯醇（P V A )、聚丙烯酸鈉、水溶性聚氨酯、會合型聚氨酯系乳膠、鹼膨潤型丙烯系乳膠羧甲基纖維素（ CMC)、甲基纖維素（MC)、羥乙基纖維素（HEC )、羥丙基纖維素（HPC)、聚乙烯醇、合成蒙脫石等〇增粘劑的配合量是聚氯丁二烯系乳膠1 0 0質量部（固體成分換算）對0 · 1〜1 0質量部（固體成分換算）爲合適。以此範圍配合對粘著物性並無惡影響。有可能調節聚氯丁二烯系乳膠組成物的粘度。被本發明的聚氯丁二烯系乳膠組成物適用的橡膠、彈性體、合成樹脂等並無特別被限定，在具體上是丁二烯橡膠（BR)、氯丁二烯橡膠（CR)、天然橡膠（NR) 、異戊二烯橡膠（IR)、苯乙烯一丁二烯橡膠（SBR )、丁基橡膠（IIR)、原菠烯橡膠（NOR)、硝基橡膠（NBR)、氫化硝基橡膠（HNBR)、溴化丁基 (請先閱讀背面之注意事項再填寫本頁) 衣. 訂Printed by the Consumer Cooperative of the Intellectual Property Bureau of the Ministry of Economic Affairs The compounding amount of the adhesion-imparting resin is preferably a polychloroprene-based latex 100 mass portion (solid content conversion) to 1 to 80 parts by weight (solid content conversion). Particularly preferred is a suitable 5 to 50 parts by weight. The method of blending the tack-imparting resin is not particularly limited. In order to disperse the resin uniformly in the latex, it is desirable to add an aqueous latex. The method for preparing an adhesive resin-provided water-based latex is to remove organic matter such as toluene, emulsify / disperse the dissolved substance with an emulsifier in water, and remove the organic solvent by heating while reducing the pressure of the organic solvent. Crushing, emulsifying / dispersing methods, etc., are ideal because the former can be made from fine particle emulsions. The solid content concentration of the polychloroprene-based latex composition of the present invention is not particularly limited, and it is preferably 70% by weight or less so as not to lose the stability of the emulsion system. Furthermore, the polychloroprene-based latex composition of the present invention is used. When each is used as an aqueous adhesive, it is preferably 40 to 70% by weight, and when used as an aqueous heuristic, it is ideal to be 10 to 40% by weight. It is more appropriate to adjust the solid content concentration . The adjustment of such a solid content can be carried out optionally by diluting it with pure water or concentrating it by removing water. The solid content concentration of the polychloroprene-based latex of the present invention can be obtained by the following operations. Only weigh aluminum dish to get A, put 2 ml of latex sample into lead dish and weigh -11-This paper size applies Chinese National Standard (CNS) A4 specification (210X297 mm) 200300155 A7 B7 Employees ’Cooperative of Intellectual Property Bureau, Ministry of Economic Affairs 5. The description of the invention (8) B is printed. The latex sample is placed in a lead dish and dried under air at 110 ° C for 2 hours, and then measured to obtain C. The solid content concentration (% by weight) was calculated by the following formula. Solid content concentration (%) = [(CA) / (BA)] X 100. Regarding the polychloroprene-based latex composition of the present invention as well as the required performance in addition to the above, a tackifier, metal can be added arbitrarily. Oxides, fillers, film-forming aids, ultraviolet absorbers, oxidation inhibitors, plasticizers, vulcanizing agents, vulcanization accelerators, defoamers, etc. The polychloroprene-based latex composition of the present invention may be adjusted at an arbitrary viscosity by blending a thickener. Specific tackifiers can be mentioned as polyvinyl alcohol (PVA), sodium polyacrylate, water-soluble polyurethane, meeting polyurethane-based latex, alkali-swelling propylene-based latex carboxymethyl cellulose (CMC), methyl fiber (MC), hydroxyethyl cellulose (HEC), hydroxypropyl cellulose (HPC), polyvinyl alcohol, synthetic montmorillonite, etc. The blending amount of the tackifier is polychloroprene-based latex 1 0 0 The mass portion (solid content conversion) is suitable for 0 · 1 to 10 mass portion (solid content conversion). Mixing within this range has no adverse effect on the physical properties of the adhesive. It is possible to adjust the viscosity of the polychloroprene-based latex composition. The rubber, elastomer, synthetic resin, etc. to which the polychloroprene-based latex composition of the present invention is applied are not particularly limited, and specifically, butadiene rubber (BR), chloroprene rubber (CR), Natural rubber (NR), isoprene rubber (IR), styrene-butadiene rubber (SBR), butyl rubber (IIR), raw spinene rubber (NOR), nitro rubber (NBR), hydrogenated nitrate Rubber (HNBR), bromobutyl (please read the precautions on the back before filling this page). Order

本紙張尺度適用中國國家標準（CNS ) A4規格（210X 297公釐） -12- 200300155 A7 B7 經濟部智慧財產局員工消費合作社印製五、發明説明（9 ) 橡膠（BIIR)、氯化丁基橡膠（CIIR)、丙烯腈 —異戊二烯橡膠（NIR)、乙丙二烯橡膠（EPDM) 等的硫化橡膠苯乙烯-丁二烯-苯乙烯•塊共聚合體（ S B S )、聚酯系、尿烷系、烯系等的彈性體、氯化乙烯基樹脂（PVC)、乙基—乙酸乙烯酯共聚合體（EVA )、1，2 —聚丁二烯（RB)、聚烯樹脂、苯乙烯系樹月旨、丙烯腈一丁二烯一苯乙烯共聚合體（AB S )等是被例示的。還有此等材料的配合組成、交聯密度、形狀等並無特別限定，就是發泡體也有可能適用。關於用途也是運動用品的緊夾、靴底、建材用等，任何範圍也可適當的使用。實施例以下由實施例及比較例將本發明的效果詳細說明，此等的實施例並不限定於本發明，尙且於以下的說明並無中斷極限，部及％是以重量基準表示。〔合成例1〕用內容器3升的反應器在氮氣流下加入小1 0 0部，不均化玫塊酸5部、氫氧化鈉0 . 6部、氫氧化鉀0 . 7 部甲醛萘碼酸縮合物的鈉鹽0 . 3部、亞硫酸氫鈉0 . 3 部、溶解後、一面攪拌一面加入氯丁二烯單體1 〇〇部與正-十二烷硫醇〇 . 1 4部。用過硫酸鉀做開始劑。在氮氣下以1 0°C聚合，在聚合率達到9 0%時加入吩噻嗪的 (請先閲讀背面之注意事項再填寫本頁) ▼This paper size applies Chinese National Standard (CNS) A4 specification (210X 297 mm) -12- 200300155 A7 B7 Printed by the Consumer Cooperatives of the Intellectual Property Bureau of the Ministry of Economic Affairs 5. Description of the invention (9) Rubber (BIIR), chlorinated butyl Vulcanized rubber such as rubber (CIIR), acrylonitrile-isoprene rubber (NIR), ethylene propylene diene rubber (EPDM), styrene-butadiene-styrene • block copolymer (SBS), polyester, urine Ethane-based, olefin-based elastomers, chlorinated vinyl resin (PVC), ethyl-vinyl acetate copolymer (EVA), 1,2-polybutadiene (RB), polyolefin resin, styrene Shuyuezhi, acrylonitrile-butadiene-styrene copolymer (AB S), and the like are exemplified. In addition, the composition, cross-linking density, shape, and the like of these materials are not particularly limited, and even a foam may be applicable. Regarding the use, it is also used for sports products, such as clamps, boot soles, and building materials. It can be used in any range. EXAMPLES The effects of the present invention will be described in detail in the following examples and comparative examples. These examples are not limited to the present invention, and the following description does not have an interruption limit. Parts and% are expressed on a weight basis. [Synthesis Example 1] Using a 3 liter reactor, 100 small portions were added under nitrogen flow, 5 pieces of heterogeneous rose block acid, 0.6 portions of sodium hydroxide, and 0.7 portions of potassium hydroxide were formed. 0.3 parts of the sodium salt of the acid condensate, 0.3 parts of sodium bisulfite, and 100 parts of chloroprene monomer and n-dodecanethiol 0.1 part after being dissolved, while stirring. . Use potassium persulfate as a starter. Polymerize at 10 ° C under nitrogen, and add phenothiazine when the polymerization rate reaches 90% (please read the precautions on the back before filling this page) ▼

、1T, 1T

本紙張尺度適用中國國家標準（CNS ) Α4規格（21〇Χ29*7公釐） -13- 200300155 A7 B7 五、發明説明（10 ) 乳濁液並停止聚合，在減壓下除去未反應單體而得聚氯丁二烯乳膠。在更減壓下將水分蒸發進行濃縮，固體成分是調整成5 0質量％。〔實施例1〕使用在合成例1所得的聚氯丁二烯乳膠、聚氯丁二烯乳膠1 0 0部對粘著賦了樹脂所成固體成分濃度5 3 %的萜烯苯酚樹脂乳膠所成托碼E- 100/荒川化學工業公司製 )5 0部，固體成分3 0 %的原矽酸鈉溶液（旭電化工業公司製）3部添加後，進一步加純水並調整配合物合體的固體成分至2 0%作爲水系底漆。還有以合成例1所得聚氯丁二烯乳膠1 〇〇部對粘著賦予樹脂所成固體成分濃度5 3 %的萜烯苯酚樹脂乳膠托碼E- 100 /荒川化學工業公司製）5 0部，聚丙烯酸鈉水溶液系增粘劑（亞隆A- 2 0 L/東亞合成公司製） 2 · 0部，作爲充塡劑的氫氧化銘粉末（愛喜郎η - 4 2 Μ/昭和電工公司製）1 〇部，作爲氧化劑固體成分濃度 5 0 %的氧化亞鉛分散液2部，作爲硬化劑的水分散型異氰酸酯化合物（鐵格WD- 7 3 0/三井武田化學公司製） 2部加以配合後作爲水系粘著劑。粘著面以磨光加工（表面硏磨）後由於用丙酮洗淨而除去削減沈渣，用硫化苯乙烯丁二烯橡膠（硫化S B R、糊塗部分的尺寸是寬2Ommx長度70mm) 2片的各表面，以實施例1所得的水系底漆用紗布沾上輕輕擦拭，本紙張尺度適用中國國家標準（CNS ) A4規格（210X297公釐） (請先閱讀背面之注意事項再填寫本頁) 訂 ^%· 經濟部智慧財產局員工消費合作社印製 -14 - 200300155 Α7 Β7 五、發明説明（u ) 在6 0°C空氣下乾燥1 0分鐘在其上用水系粘著劑2 0 0 克（濕的）/ m 2用毛刷塗布在6 0 °C空氣下乾燥6分鐘後貼合用手動滾筒壓著後，就以此方法所得的試驗片而言，進行以下的評價。〔初期粘著力評價試驗〕從做壓著1 0分鐘後用拉伸試驗機以拉伸速度2 〇〇 m m/m i η，T型剝離強度測定之。〔常態粘著力評價試驗〕從做壓著1天後，用拉伸試驗機，以拉伸速度2 〇 (3 m m/m i η，Τ型剝離強度測定之。〔實施例2〕以實施例1所製作的底漆，在加純水之前’進〜步加聚乙亞胺（環氧Ρ — 1000 (固體成30%)/公司臼本觸媒社製）3 . 3部，其後用純水調整固體成分$ 2 〇 %以外，進行與實施例1同樣的試驗，做爲實施例2 ° 〔比較例1〕不使用水系底漆以外，實施與實施例1同樣的試驗做爲比較例1。〔比較例2〕 (請先閱讀背面之注意事項再填寫本頁) -、_叮This paper size applies Chinese National Standard (CNS) A4 specification (21〇 × 29 * 7mm) -13- 200300155 A7 B7 V. Description of the invention (10) Emulsion and stop polymerization, remove unreacted monomer under reduced pressure And polychloroprene latex was obtained. The water was evaporated and concentrated under reduced pressure, and the solid content was adjusted to 50% by mass. [Example 1] A terpene phenol resin latex using a polychloroprene latex and a polychloroprene latex obtained in Synthesis Example 1 having a solid content concentration of 53% by resin was added to 100 parts of the polychloroprene latex. E-100 (made by Arakawa Chemical Industry Co., Ltd.) 50 parts, 3 parts of sodium orthosilicate solution (manufactured by Asahi Denka Kogyo Co., Ltd.) with a solid content of 30% are added, and pure water is further added to adjust the complex composition. Solid content to 20% as a water-based primer. In addition, a terpene phenol resin latex pallet E-100 (made by Arakawa Chemical Industry Co., Ltd.) with a solid content concentration of 53% of 100 parts of the polychloroprene latex obtained in Synthesis Example 1 for adhesion to the resin (50) Part, sodium polyacrylate aqueous solution thickener (Yaron A-2 0 L / manufactured by Toa Kosei Co., Ltd.) 2. Part 0, hydration powder for powder (Akiro η-4 2 M / Showa Denko Corporation) (Production) 10 parts, 2 parts of a lead oxide dispersion with a solid content concentration of 50% as an oxidant, 2 parts of a water-dispersible isocyanate compound (iron grid WD-7 3 0 / manufactured by Mitsui Takeda Chemical Co., Ltd.) as a hardener After mixing, it acts as a water-based adhesive. After the adhesive surface is polished (surface honing), it is washed with acetone to remove the sediment, and the surface is made of vulcanized styrene butadiene rubber (vulcanized SBR, the size of the paste part is 20mm wide and 70mm long). The water-based primer obtained in Example 1 was gently wiped with gauze. The paper size applies the Chinese National Standard (CNS) A4 specification (210X297 mm) (Please read the precautions on the back before filling this page) Order ^ % · Printed by the Consumer Cooperative of the Intellectual Property Bureau of the Ministry of Economy -14-200300155 Α7 Β7 V. Description of the invention (u) Dry at 60 ° C for 10 minutes with water-based adhesive 2 0 g (wet) / M 2 was applied with a brush and dried under air at 60 ° C. for 6 minutes, followed by lamination with a manual roller, and the following evaluation was performed on the test piece obtained by this method. [Initial adhesion evaluation test] T-peel strength was measured from a tensile tester at a tensile speed of 2000 m m / m i η after 10 minutes of pressing. [Normal Adhesion Evaluation Test] One day after the pressing, a tensile tester was used to measure the peeling strength at a tensile speed of 20 (3 mm / min, T type.) [Example 2] Example 1 Prior to the addition of pure water, the prepared primer was added with 3.3 parts of polyethyleneimine (epoxy P-1000 (30% solids) / Made by Usmoto Catalysts Co., Ltd.), followed by pure Except for water-adjusted solid content of $ 20%, the same test as in Example 1 was performed as Example 2 ° [Comparative Example 1] The same test as in Example 1 was performed as Comparative Example 1 except that no water-based primer was used. 〔Comparative Example 2〕 (Please read the precautions on the back before filling in this page)-, _ Ding

經濟部智慧財產局員工消費合作社印製本紙張尺度適用中國國家標準（CNS ) Α4規格（210X297公釐） -15- ----^ 200300155 A7 B7 五、發明说明（12 ) 不使用原矽酸鈉以外’實施與實施例1同樣的試驗做爲比較例2。 (請先閱讀背面之注意事項再填寫本頁) 〔比較例3〜5〕使用他種的矽酸鈉來代替原矽酸鈉以外’實施與實施例1同樣的試驗，做爲比較例3〜5。〔比較例6〕用溶劑系底漆來代替水系底漆以外，實施與實施例1 同樣的試驗，做爲比較例6。尙且在此處的溶劑系底漆是已做如次的調製。用內容積3升的反應器在氮氣流下加入水1 2 0部，不均化玫瑰酸4部，氫氧化鈉0 · 8部，甲醛萘磺酸縮合物的鈉鹽0 _ 5部，亞硫酸氫鈉0 · 3部，溶解後一面攪拌一面加入氯丁二烯單體1 0 0部與正-十二烷硫醇經濟部智慧財產局員工消費合作社印製 0 · 2 5部。用過硫酸鉀做開始劑，在氮氣下以1 〇。(：聚合。在聚合率達到7 0 %時加入吩噻嗪的乳濁液並停止聚合，在減壓下除去未反應單體後，以常法的凍結凝固乾燥法而得聚氯丁二烯的晶片。以所得的聚氯丁二烯的晶片 1 0 0克，放入內容積1升的反應器，加甲苯6 0 0克一面攪拌一面溶解。溶解後加甲基丙烯酸酯5 0克，用過氧化苯醯作開始劑。在8 5 °C進行5小時接枝聚合。在添加 2，6 —二一 t 一丁基—4 一甲酚的甲苯溶液時停止聚合反應。更進一步用甲苯稀釋合乎固體成分濃度5%做成溶本紙張尺度適用中國國家標準（CNS ) A4規格（210X297公釐） 200300155 A7 B7 五、發明説明（13 劑型底漆經濟部智慧財產局員工消費合作社印製 (請先閲讀背面之注意事項再填寫本頁)Printed by the Consumers' Cooperative of the Intellectual Property Bureau of the Ministry of Economic Affairs, the paper size is applicable to the Chinese National Standard (CNS) A4 specification (210X297 mm) -15- ---- ^ 200300155 A7 B7 V. Description of the invention (12) Do not use orthosilicic acid Except for sodium, the same test as in Example 1 was performed as Comparative Example 2. (Please read the precautions on the back before filling in this page) [Comparative Examples 3 to 5] Use other types of sodium silicate instead of sodium orthosilicate 'to perform the same test as in Example 1 as Comparative Examples 3 to 5. [Comparative Example 6] The same test as in Example 1 was performed as a comparative example 6 except that the solvent-based primer was used instead of the water-based primer. The solvent-based primer here is the same as before. In a 3 liter reactor, add 120 parts of water under nitrogen flow, 4 parts of heterogeneous rose acid, 0. 8 parts of sodium hydroxide, 0-5 parts of sodium salt of formaldehyde naphthalenesulfonic acid condensate, sulfurous acid 0,3 parts of sodium hydrogen hydride, while stirring, add 100 parts of chloroprene monomer and n-dodecanethiol, Ministry of Economic Affairs, Intellectual Property Bureau, Employee Consumption Cooperative, and print 0.5 parts. Potassium persulfate was used as the starting agent, under 10 under nitrogen. (: Polymerization. When the polymerization rate reaches 70%, an emulsion of phenothiazine is added and the polymerization is stopped. After removing unreacted monomers under reduced pressure, polychloroprene is obtained by a conventional freeze-drying method. Take 100 g of the obtained polychloroprene wafer, put it into a 1-liter reactor, add 600 g of toluene and dissolve while stirring. Add 50 g of methacrylate after dissolving, Phenylhydrazine peroxide was used as the initiator. Graft polymerization was carried out at 85 ° C for 5 hours. The polymerization reaction was stopped when a toluene solution of 2,6-di-t-butyl-4-cresol was added. Further, toluene was used. Dilution meets the solid content concentration of 5% to make the dissolved paper. The size of the paper is applicable to the Chinese National Standard (CNS) A4 specification (210X297 mm) 200300155 A7 B7 V. Description of the invention (13 Dosage Primer Printed by the Consumer Cooperatives of the Intellectual Property Bureau of the Ministry of Economic Affairs (Please read the notes on the back before filling out this page)

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Claims

200300155 經濟部智慧財產局員工消費合作社印製 A8 B8 C8 D8六、申請專利範圍 1 1 . 一種聚氯丁二烯系乳膠組成物’其特徵係在於以聚氯丁二烯與原矽酸鈉爲必須成分，彼等在水中可分散或溶解。 2 .如申請專利範圍第1項記載之聚氯丁二烯系乳膠組成物，其中聚氯丁二烯系乳膠中的固體成分濃度係4 0 〜7 0重量％。 3 .如申請專利範圍第1項或第2項記載之聚氯丁二烯系乳膠組成物，其中原矽酸鈉之含量係對聚氯丁二烯（固體成分）100重量份爲〇 · 1〜30重量份。 4 ·如申請專利範圍第1〜3項中任一記載之聚氯丁二烯系乳膠組成物，其中聚乙烯亞胺對聚氯丁二烯（固體成分）100重量份係含有〇·1〜5重量份。 5 ·如申請專利範圍第1〜4項中任一記載之聚氯丁二烯系乳膠組成物，其中，粘著賦予樹脂對聚氯丁二烯（· 固體成分）1 0 0重量份係含有1〜8 0重量份。 6 .如申請專利範圍第1〜5項中任一記載之聚氯丁二烯系乳膠組成物，其中增粘劑對聚氯丁二烯（固體成分 )100重量份係含有0·01〜10重量份。 7 · —種水系底漆，其特徵爲如申請專利範圍第1〜 6項中任一記載之聚氯丁二烯系乳膠組成物使用爲主成分〇 8 · —種粘著方法，其特徵爲將如申請專利範圍第7 項記載之水系底漆粘著於被粘著層。 ^^裝-- (請先閱讀背面之注意事項再填寫本頁) 、11200300155 Printed by A8, B8, C8, D8, Consumer Cooperative of the Intellectual Property Bureau of the Ministry of Economic Affairs 6. Application for patent scope 1 1. A polychloroprene latex composition 'characterized by using polychloroprene and sodium orthosilicate as Essential ingredients, they can be dispersed or dissolved in water. 2. The polychloroprene-based latex composition according to item 1 of the scope of the patent application, wherein the solid content concentration in the polychloroprene-based latex is 40 to 70% by weight. 3. The polychloroprene-based latex composition as described in item 1 or 2 of the scope of patent application, wherein the content of sodium orthosilicate is 0.1 to 100 parts by weight of polychloroprene (solid content). ~ 30 parts by weight. 4. The polychloroprene-based latex composition according to any one of items 1 to 3 in the scope of the patent application, in which 100 parts by weight of polyethyleneimine to polychloroprene (solid content) contains 0.1 to 1 5 parts by weight. 5. The polychloroprene-based latex composition according to any one of claims 1 to 4 in the scope of the patent application, wherein the adhesion-imparting resin contains polychloroprene (solid content) in an amount of 100 parts by weight. 1 to 80 parts by weight. 6. The polychloroprene-based latex composition according to any one of items 1 to 5 in the scope of the patent application, wherein the tackifier contains 0.01 to 10 parts by weight of 100 parts by weight of the polychloroprene (solid content). Parts by weight. 7 · A water-based primer characterized by using a polychloroprene-based latex composition as described in any one of claims 1 to 6 in the application scope as a main component. 0 ·· An adhesion method characterized by The water-based primer described in item 7 of the scope of patent application is adhered to the adhered layer. ^^ Equipment-(Please read the precautions on the back before filling this page), 11

本紙張尺度適用中國國家標準（CNS ) A4規格（210X297公釐） -19 _ 200300155 陸、（一〇、本案指定代表圖爲：無 (二）、本代表圖之元件代表符號簡單說明：無柒、本案若有化學式時，請揭示最能顯示發明特徵的化學式：無This paper size applies the Chinese National Standard (CNS) A4 specification (210X297 mm) -19 _ 200300155 Lu, (10) The designated representative figure in this case is: None (two), the component representative symbol of this representative figure is simply explained: None 2. If there is a chemical formula in this case, please disclose the chemical formula that best shows the characteristics of the invention: None