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WO2018196033A1 - 一种白乳胶黏合剂及其制备方法 - Google Patents

一种白乳胶黏合剂及其制备方法 Download PDF

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Publication number
WO2018196033A1
WO2018196033A1 PCT/CN2017/083430 CN2017083430W WO2018196033A1 WO 2018196033 A1 WO2018196033 A1 WO 2018196033A1 CN 2017083430 W CN2017083430 W CN 2017083430W WO 2018196033 A1 WO2018196033 A1 WO 2018196033A1
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parts
white latex
latex adhesive
filler
adhesive
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French (fr)
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龚彩萍
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J131/00—Adhesives 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 an acyloxy radical of a saturated carboxylic acid, of carbonic acid, or of a haloformic acid; Adhesives based on derivatives of such polymers
    • C09J131/02—Homopolymers or copolymers of esters of monocarboxylic acids
    • C09J131/04—Homopolymers or copolymers of vinyl acetate
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02—Non-macromolecular additives
    • C09J11/04—Non-macromolecular additives inorganic
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02—Non-macromolecular additives
    • C09J11/06—Non-macromolecular additives organic
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J129/00—Adhesives 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 an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Adhesives based on hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Adhesives based on derivatives of such polymers
    • C09J129/02—Homopolymers or copolymers of unsaturated alcohols
    • C09J129/04—Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K2003/2237—Oxides; Hydroxides of metals of titanium
    • C08K2003/2241—Titanium dioxide
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/30—Sulfur-, selenium- or tellurium-containing compounds
    • C08K2003/3009—Sulfides
    • C08K2003/3036—Sulfides of zinc
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/30—Sulfur-, selenium- or tellurium-containing compounds
    • C08K2003/3045—Sulfates
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00—Properties
    • C08L2201/08—Stabilised against heat, light or radiation or oxydation

Definitions

  • the invention relates to a binder, in particular to a white latex adhesive and a preparation method thereof.
  • White latex is one of the most widely used and most widely used adhesives. It is obtained by emulsion polymerization of water as a dispersion medium, and is an aqueous environmentally friendly glue. Mainly used in wood processing, furniture assembly, cigarette mouthpieces, architectural decoration, fabric bonding, product processing, printing and binding, handicraft manufacturing and leather processing, label fixing, tile bonding, etc., is an environmentally friendly adhesive. .
  • the white latex is a polyvinyl acetate emulsion. Because of the complicated preparation process, large equipment investment, and high vinyl acetate monomer price, the production cost of white latex is relatively high. Its obvious disadvantages are poor water resistance and moisture resistance, easy to absorb moisture in humid air, creeping at high temperature, which makes the bonding strength drop, and it is easy to freeze under -5 °C, so that the emulsion is damaged.
  • a white latex adhesive comprising 300-400 parts of polyvinyl alcohol, 5-8 parts of hydrochloric acid, 30-50 parts of sodium tripolyphosphate, 7-9 parts of liquid base, and emulsified by weight. 12-16 parts, 10-20 parts of dibutyl phthalate, 450-500 parts of polyvinyl acetate, 200-300 parts of filler, 2-4 parts of triethanolamine oleate.
  • the emulsifier is OP-10 or TX-10.
  • the filler is talc, titanium dioxide or zinc antimony white.
  • the invention also provides a preparation method of the above white latex adhesive, comprising the following steps:
  • Step 1 Dissolve the polyvinyl alcohol in water at 90-95 ° C, adjust the pH to 2-3 with hydrochloric acid, keep the temperature at 85-95 ° C, add sodium tripolyphosphate under stirring, and react 0.5-1 h. Cool down to below 50 ° C, add liquid alkali to adjust the pH to 6-8;
  • Step 2 while stirring, keep the temperature at 50 ° C, add emulsifier, dibutyl phthalate, heat at 40-50 ° C for 1 h and stir, then cool to room temperature, stir, add polyvinyl acetate, continue to stir 0.5h or more;
  • Step 3 adding the filler and oleic acid triethanolamine to the material obtained in the second step, and stirring for 1.5 hours to obtain the finished product.
  • the adhesive of the invention has low cold junction temperature, good antifreeze property, high tensile and shear strength, waterproof performance, no degumming, good heat resistance, high temperature resistance above 100 ° C, low cost and reaction Production can be carried out in a kettle or without a reaction kettle.
  • White latex adhesive including 400 parts of polyvinyl alcohol, 8 parts of hydrochloric acid, 50 parts of sodium tripolyphosphate, 9 parts of liquid base, 13 parts of emulsifier, 15 parts of dibutyl phthalate, and polyvinyl acetate 460 by weight. Parts, 250 parts of filler, 3.5 parts of triethanolamine oleate.
  • the emulsifier is OP-10 or TX-10; the filler is talc, titanium dioxide or zinc antimony white.
  • the preparation method of the white latex adhesive of the invention comprises the following steps:
  • Step 1 Dissolve polyvinyl alcohol in water at 90 ° C, adjust the pH to 2.5 with hydrochloric acid, keep the temperature at 90 ° C, add sodium tripolyphosphate under stirring, react for 1 h, cool down to below 50 ° C, add liquid The base adjusts the pH to 7;
  • Step 2 while stirring, keep the temperature at 50 ° C, add emulsifier, dibutyl phthalate, heat at 45 ° C for 1 h and stir, then cool to room temperature, stir, add polyvinyl acetate, continue to stir for 0.5 h the above;
  • Step 3 adding the filler and oleic acid triethanolamine to the material obtained in the second step, and stirring for 1.5 hours to obtain the finished product.
  • the zigzag file is used to comb the full and uninterrupted zigzag stripes on the base surface, which can effectively ensure the uniform application of the adhesive on the base surface.
  • the adhesive stripe convex portion is pressed. It enters the groove and is in full contact with wood, floor, etc. under the action of external pressure, effectively avoiding the phenomenon that wood, floor, etc. are empty due to inability to contact the adhesive well.
  • White latex adhesive including 330 parts of polyvinyl alcohol, 7 parts of hydrochloric acid, 45 parts of sodium tripolyphosphate, 7.5 parts of liquid alkali, 13 parts of emulsifier, 14 parts of dibutyl phthalate, and polyvinyl acetate 500 by weight. Parts, 300 parts of filler, 2 parts of triethanolamine oleate.
  • the emulsifier is OP-10 or TX-10; the filler is talc, titanium dioxide or zinc antimony white.
  • the preparation method of the white latex adhesive of the invention comprises the following steps:
  • Step 1 Dissolve polyvinyl alcohol in water at 95 ° C, adjust the pH to 2 with hydrochloric acid, keep the temperature at 95 ° C, add sodium tripolyphosphate under stirring, react for 1 h, cool down to below 50 ° C, add liquid The base adjusts the pH to 7.2;
  • Step 2 Under stirring, keep the temperature at 40 ° C, add emulsifier, dibutyl phthalate The ester was kept at 40 ° C for 1 h and stirred, then cooled to normal temperature, stirred, and added with polyvinyl acetate, and stirring was continued for more than 1 h;
  • Step 3 adding the filler and oleic acid triethanolamine to the material obtained in the second step, and stirring for 1.5 hours to obtain the finished product.
  • the zigzag file is used to comb the full and uninterrupted zigzag stripes on the base surface, which can effectively ensure the uniform application of the adhesive on the base surface.
  • the adhesive stripe convex portion is pressed. It enters the groove and is in full contact with wood, floor, etc. under the action of external pressure, effectively avoiding the phenomenon that wood, floor, etc. are empty due to inability to contact the adhesive well.
  • White latex adhesive including 380 parts of polyvinyl alcohol, 7 parts of hydrochloric acid, 35 parts of sodium tripolyphosphate, 8.5 parts of liquid alkali, 14 parts of emulsifier, 17 parts of dibutyl phthalate, and polyvinyl acetate 490 by weight. Parts, 280 parts of filler, 3 parts of triethanolamine oleate.
  • the emulsifier is OP-10 or TX-10; the filler is talc, titanium dioxide or zinc antimony white.
  • the preparation method of the white latex adhesive of the invention comprises the following steps:
  • Step 1 Dissolve polyvinyl alcohol in water at 92 ° C, adjust the pH to 2-3 with hydrochloric acid, keep the temperature at 92 ° C, add sodium tripolyphosphate under stirring, react for 1 h, and cool down to below 50 ° C. Add liquid base to adjust the pH to 6.5;
  • Step 2 while stirring, keep the temperature at 45 ° C, add emulsifier, dibutyl phthalate, heat at 45 ° C for 1 h and stir, then cool to room temperature, stir, add polyvinyl acetate, continue to stir for 0.5 h the above;
  • Step 3 adding the filler and oleic acid triethanolamine to the material obtained in the second step, and stirring for 2 hours to obtain the finished product.
  • the zigzag file is used to comb the full and uninterrupted zigzag stripes on the base surface, which can effectively ensure the uniform application of the adhesive on the base surface.
  • the adhesive stripe convex portion is pressed. It enters the groove and is in full contact with wood, floor, etc. under the action of external pressure, effectively avoiding the phenomenon that wood, floor, etc. are empty due to inability to contact the adhesive well.
  • this product has strong adhesion to wood, paper, cotton, leather, ceramics, etc., can be cured at room temperature, and the curing speed is fast, and the film after curing has certain Resilience, resistance to dilute alkali, dilute acid, and oil resistance, water resistance is also very good.
  • the adhesive of the invention has low cold junction temperature, good freeze resistance, high tensile and shear strength, waterproof performance, no degumming, good heat resistance, and high temperature resistance above 100 ° C; Low, production can be carried out in the presence or absence of a reaction kettle.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Adhesives Or Adhesive Processes (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)
  • Detergent Compositions (AREA)

Abstract

一种白乳胶黏合剂及其制备方法，按重量份包括聚乙烯醇300-400份、盐酸5-8份、三聚磷酸钠30-50份、液碱7-9份、乳化剂12-16份、邻苯二甲酸二丁酯10-20份、聚醋酸乙烯450-500份、填料200-300份、油酸三乙醇胺2-4份。由此，黏合剂冷结温度低、防冻性好、抗拉及抗剪切强度高；具有防水性能、不脱胶；耐热性好，可抗100℃以上的高温；成本较低，在有反应釜或没有反应釜的条件下均可进行生产。

Description

一种白乳胶黏合剂及其制备方法 技术领域
本发明涉及黏合剂，尤其涉及一种白乳胶黏合剂及其制备方法。
背景技术
白乳胶是目前用途最广、用量最大的粘合剂品种之一。它是以水为分散介质进行乳液聚合而得，是一种水性环保胶。主要被用在木材加工、家具组装、卷烟接嘴、建筑装潢、织物粘结、制品加工、印刷装订、工艺品制造以及皮革加工、标签固定、瓷砖黏贴等，是一种环保型的胶黏剂。
一般所称的白乳胶即聚醋酸乙烯乳液，由于制备操作工艺较复杂，设备投资大，而且醋酸乙烯单体价格也较高，所以白乳胶的生产成本较高。它的较为明显的缺点是耐水性和耐湿性差，易在潮湿空气中吸湿，在高温下使用会产生蠕变现象，使胶接强度下降，在-5℃以下储存易冻结，使乳液受到破坏。
发明内容
本发明的目的提供一种白乳胶黏合剂及其制备方法，解决上述现有技术问题中的一个或者多个。
根据本发明的一个方面，提供一种白乳胶黏合剂，按重量份包括聚乙烯醇300-400份、盐酸5-8份、三聚磷酸钠30-50份、液碱7-9份、乳化剂12-16份、邻苯二甲酸二丁酯10-20份、聚醋酸乙烯450-500份、填料200-300份、油酸三乙醇胺2-4份。
在一些实施方式中：乳化剂为OP-10或TX-10。
在一些实施方式中：填料为滑石粉、钛白粉或锌钡白。
本发明还提供了上述的一种白乳胶黏合剂的制备方法，包括以下步骤：
步骤一：在90-95℃下，将聚乙烯醇溶解于水中，用盐酸调节pH值至2-3，保持温度在85-95℃，在搅拌下加入三聚磷酸钠，反应0.5-1h，降温至50℃以下，加入液碱调节pH值至6-8；
步骤二：在搅拌下，保持温度为50℃，加入乳化剂、领苯二甲酸二丁酯，在40-50℃下保温1h并搅拌，然后冷却至常温，搅拌，加入聚醋酸乙烯，继续搅拌0.5h以上；
步骤三：向步骤二所得物料中加入填料及油酸三乙醇胺，并搅拌1.5h，即可得成品。
本发明的黏合剂冷结温度低、防冻性好、抗拉及抗剪切强度高；具有防水性能、不脱胶；耐热性好，可抗100℃以上的高温；成本较低，在有反应釜或没有反应釜的条件下均可进行生产。
具体实施方式
下面通过实施例对本发明作进一步详细说明。
实施例1：
白乳胶黏合剂，按重量份包括聚乙烯醇400份、盐酸8份、三聚磷酸钠50份、液碱9份、乳化剂13份、邻苯二甲酸二丁酯15份、聚醋酸乙烯460份、填料250份、油酸三乙醇胺3.5份。
其中，乳化剂为OP-10或TX-10；填料为滑石粉、钛白粉或锌钡白。
本发明白乳胶黏合剂的制备方法：包括以下步骤：
步骤一：在90℃下，将聚乙烯醇溶解于水中，用盐酸调节pH值至2.5，保持温度在90℃，在搅拌下加入三聚磷酸钠，反应1h，降温至50℃以下，加入液碱调节pH值至7；
步骤二：在搅拌下，保持温度为50℃，加入乳化剂、领苯二甲酸二丁酯，在45℃下保温1h并搅拌，然后冷却至常温，搅拌，加入聚醋酸乙烯，继续搅拌0.5h以上；
步骤三：向步骤二所得物料中加入填料及油酸三乙醇胺，并搅拌1.5h，即可得成品。
用锯齿形镘刀在基面上梳理出饱满无间断的锯齿状条纹，能有效保证胶粘剂均匀的涂抹在基面上，当将木材、地板等按压到胶粘剂上时，胶粘剂条纹凸出部分被压入凹槽内，并在外界压力的作用下与木材、地板等充分接触，有效避免了木材、地板等因无法与胶粘剂很好接触而出现空鼓的现象。
实施例2：
白乳胶黏合剂，按重量份包括聚乙烯醇330份、盐酸7份、三聚磷酸钠45份、液碱7.5份、乳化剂13份、邻苯二甲酸二丁酯14份、聚醋酸乙烯500份、填料300份、油酸三乙醇胺2份。
其中，乳化剂为OP-10或TX-10；填料为滑石粉、钛白粉或锌钡白。
本发明白乳胶黏合剂的制备方法：包括以下步骤：
步骤一：在95℃下，将聚乙烯醇溶解于水中，用盐酸调节pH值至2，保持温度在95℃，在搅拌下加入三聚磷酸钠，反应1h，降温至50℃以下，加入液碱调节pH值至7.2；
步骤二：在搅拌下，保持温度为40℃，加入乳化剂、领苯二甲酸二丁 酯，在40℃下保温1h并搅拌，然后冷却至常温，搅拌，加入聚醋酸乙烯，继续搅拌1h以上；
步骤三：向步骤二所得物料中加入填料及油酸三乙醇胺，并搅拌1.5h，即可得成品。
用锯齿形镘刀在基面上梳理出饱满无间断的锯齿状条纹，能有效保证胶粘剂均匀的涂抹在基面上，当将木材、地板等按压到胶粘剂上时，胶粘剂条纹凸出部分被压入凹槽内，并在外界压力的作用下与木材、地板等充分接触，有效避免了木材、地板等因无法与胶粘剂很好接触而出现空鼓的现象。
实施例3：
白乳胶黏合剂，按重量份包括聚乙烯醇380份、盐酸7份、三聚磷酸钠35份、液碱8.5份、乳化剂14份、邻苯二甲酸二丁酯17份、聚醋酸乙烯490份、填料280份、油酸三乙醇胺3份。
其中，乳化剂为OP-10或TX-10；填料为滑石粉、钛白粉或锌钡白。
本发明白乳胶黏合剂的制备方法：包括以下步骤：
步骤一：在92℃下，将聚乙烯醇溶解于水中，用盐酸调节pH值至2-3，保持温度在92℃，在搅拌下加入三聚磷酸钠，反应1h，降温至50℃以下，加入液碱调节pH值至6.5；
步骤二：在搅拌下，保持温度为45℃，加入乳化剂、领苯二甲酸二丁酯，在45℃下保温1h并搅拌，然后冷却至常温，搅拌，加入聚醋酸乙烯，继续搅拌0.5h以上；
步骤三：向步骤二所得物料中加入填料及油酸三乙醇胺，并搅拌2h，即可得成品。
用锯齿形镘刀在基面上梳理出饱满无间断的锯齿状条纹，能有效保证胶粘剂均匀的涂抹在基面上，当将木材、地板等按压到胶粘剂上时，胶粘剂条纹凸出部分被压入凹槽内，并在外界压力的作用下与木材、地板等充分接触，有效避免了木材、地板等因无法与胶粘剂很好接触而出现空鼓的现象。
上述实施例的产品与常规黏合剂对于使用后各项效果试验如下：
Figure PCTCN2017083430-appb-000001
Figure PCTCN2017083430-appb-000002
其中，发明人通过大量的实验得出，本品对如木材、纸张、棉布、皮革、陶瓷等有很强的粘结力，能够室温固化，且固化速度快，同时固化后的胶膜有一定的韧性，耐稀碱，稀酸，且耐油性、防水性也很好。
综上所述，本发明的黏合剂冷结温度低、防冻性好、抗拉及抗剪切强度高；具有防水性能、不脱胶；耐热性好，可抗100℃以上的高温；成本较低，在有反应釜或没有反应釜的条件下均可进行生产。
以上所述仅是本发明的一种实施方式，应当指出，对于本领域普通技术人员来说，在不脱离本发明创造构思的前提下，还可以做出若干相似的变形和改进，这些也应视为本发明的保护范围之内。

Claims (4)

  1. 一种白乳胶黏合剂，其特征在于：按重量份包括聚乙烯醇300-400份、盐酸5-8份、三聚磷酸钠30-50份、液碱7-9份、乳化剂12-16份、邻苯二甲酸二丁酯10-20份、聚醋酸乙烯450-500份、填料200-300份、油酸三乙醇胺2-4份。
  2. 根据权利要求1所述的一种白乳胶黏合剂，其特征在于：所述乳化剂为OP-10或TX-10。
  3. 根据权利要求1所述的一种白乳胶黏合剂，其特征在于：所述填料为滑石粉、钛白粉或锌钡白。
  4. 一种制备权利要求1-3任一项所述白乳胶黏合剂的方法,其特征在于,包括以下步骤:
    步骤一：在90-95℃下，将聚乙烯醇溶解于水中，用盐酸调节pH值至2-3，保持温度在85-95℃，在搅拌下加入三聚磷酸钠，反应0.5-1h，降温至50℃以下，加入液碱调节pH值至6-8；
    步骤二：在搅拌下，保持温度为50℃，加入乳化剂、领苯二甲酸二丁酯，在40-50℃下保温1h并搅拌，然后冷却至常温，搅拌，加入聚醋酸乙烯，继续搅拌0.5h以上；
    步骤三：向步骤二所得物料中加入填料及油酸三乙醇胺，并搅拌1.5h，即可得成品。
PCT/CN2017/083430 2017-04-27 2017-05-08 一种白乳胶黏合剂及其制备方法 Ceased WO2018196033A1 (zh)

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