CN108424731A - 一种压敏胶的制备方法 - Google Patents

一种压敏胶的制备方法 Download PDF

Info

Publication number
CN108424731A
CN108424731A CN201810306550.4A CN201810306550A CN108424731A CN 108424731 A CN108424731 A CN 108424731A CN 201810306550 A CN201810306550 A CN 201810306550A CN 108424731 A CN108424731 A CN 108424731A
Authority
CN
China
Prior art keywords
parts
sensitive adhesive
added
pressure sensitive
stirring
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.)
Withdrawn
Application number
CN201810306550.4A
Other languages
English (en)
Inventor
俞小峰
徐扣华
杨颖�
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Individual
Original Assignee
Individual
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Individual filed Critical Individual
Priority to CN201810306550.4A priority Critical patent/CN108424731A/zh
Publication of CN108424731A publication Critical patent/CN108424731A/zh
Withdrawn legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J7/00Adhesives in the form of films or foils
    • C09J7/30Adhesives in the form of films or foils characterised by the adhesive composition
    • C09J7/38Pressure-sensitive adhesives [PSA]
    • C09J7/381Pressure-sensitive adhesives [PSA] based on macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
    • C09J7/385Acrylic polymers
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F220/00Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
    • C08F220/02Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
    • C08F220/10Esters
    • C08F220/12Esters of monohydric alcohols or phenols
    • C08F220/14Methyl esters, e.g. methyl (meth)acrylate
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00Polymeric products of isocyanates or isothiocyanates
    • C08G18/06Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/30Low-molecular-weight compounds
    • C08G18/32Polyhydroxy compounds; Polyamines; Hydroxyamines
    • C08G18/3225Polyamines
    • C08G18/3228Polyamines acyclic
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00Polymeric products of isocyanates or isothiocyanates
    • C08G18/06Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/30Low-molecular-weight compounds
    • C08G18/34Carboxylic acids; Esters thereof with monohydroxyl compounds
    • C08G18/348Hydroxycarboxylic acids
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00Polymeric products of isocyanates or isothiocyanates
    • C08G18/06Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/40High-molecular-weight compounds
    • C08G18/48Polyethers
    • C08G18/4804Two or more polyethers of different physical or chemical nature
    • C08G18/4812Mixtures of polyetherdiols with polyetherpolyols having at least three hydroxy groups
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00Polymeric products of isocyanates or isothiocyanates
    • C08G18/06Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/67Unsaturated compounds having active hydrogen
    • C08G18/671Unsaturated compounds having only one group containing active hydrogen
    • C08G18/672Esters of acrylic or alkyl acrylic acid having only one group containing active hydrogen
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00Polymeric products of isocyanates or isothiocyanates
    • C08G18/06Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/70Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
    • C08G18/72Polyisocyanates or polyisothiocyanates
    • C08G18/74Polyisocyanates or polyisothiocyanates cyclic
    • C08G18/76Polyisocyanates or polyisothiocyanates cyclic aromatic
    • C08G18/7614Polyisocyanates or polyisothiocyanates cyclic aromatic containing only one aromatic ring
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/08Macromolecular additives
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J133/00Adhesives 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 only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
    • C09J133/04Homopolymers or copolymers of esters
    • C09J133/06Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
    • C09J133/10Homopolymers or copolymers of methacrylic acid esters
    • C09J133/12Homopolymers or copolymers of methyl methacrylate
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/08Stabilised against heat, light or radiation or oxydation
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/03Polymer mixtures characterised by other features containing three or more polymers in a blend
    • C08L2205/035Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J2301/00Additional features of adhesives in the form of films or foils
    • C09J2301/10Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet
    • C09J2301/12Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet by the arrangement of layers
    • C09J2301/122Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet by the arrangement of layers the adhesive layer being present only on one side of the carrier, e.g. single-sided adhesive tape
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J2301/00Additional features of adhesives in the form of films or foils
    • C09J2301/30Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier
    • C09J2301/302Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier the adhesive being pressure-sensitive, i.e. tacky at temperatures inferior to 30°C
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J2433/00Presence of (meth)acrylic polymer
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J2467/00Presence of polyester
    • C09J2467/006Presence of polyester in the substrate

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Adhesives Or Adhesive Processes (AREA)

Abstract

本发明公开了一种压敏胶的制备方法,属于胶黏剂领域。本发明还加入以三乙烯四胺、丙二醇甲醚为原料获得的一种新型固化剂,其具有独特的分子结构:含有与被乳化的液体环氧树脂极相似的疏水链段,同时含有亲水性的柔性聚醚链段,从而能够改善压敏胶固化后性能较脆的缺陷。本发明解决了目前压敏胶大多采用水性丙烯酸酯环保和耐候性佳,但耐水性、初粘性低的问题。

Description

一种压敏胶的制备方法
技术领域
本发明属于胶黏剂领域,具体涉及一种压敏胶的制备方法。
背景技术
压敏胶材料是一类应用广泛的材料,它是由压敏胶涂覆在基材如标签纸、薄膜之上制得的胶带、双面胶带、保护膜、标签等产品的总称,其中的压敏胶是压敏胶粘剂的简称,是一类对压力有敏感性的胶粘剂。压敏胶按照主体树脂成分可分为橡胶型和树脂型两类,橡胶型又可分为天然橡胶和合成橡胶类,树脂型又主要包括聚丙烯酸酯类、有机硅类以及聚氨酯类。按照分散介质的不同,分为水性和溶剂型压敏胶。水性压敏胶是以水作为反应的介质进行反应,涂布烘干后即得压敏胶制品。由于水性压敏胶采用水作为溶剂,所以其价格低廉,生产速率较快,但其胶粘剂性能不高。溶剂型压敏胶用甲苯,乙酸乙酯等有机溶剂作为反应的介质进行反应,在溶剂型压敏胶成品中,有机溶剂占总重量的60~75%,胶粘剂占总重的25~40%。
溶剂型压敏胶的技术成熟,具有优良的压敏性和粘结性,又由于耐老化性、耐光性、耐水性、耐油性等优点,所以几乎没有经时变化引起压敏性下降的问题,而且可剥离性能优良。目前,溶剂型压敏胶由于环保问题而造成使用范围的逐步缩小,其原因是:由于溶剂型压敏胶在涂布的过程中,需要将其中含有的大量有机溶剂蒸发掉,因此造成的问题主要有:一、压敏胶制品的加工时间长;二、蒸发的溶剂对操作工人造成身体伤害;三、蒸发的溶剂本身没有充分的利用也会造成浪费;在加热过程中对涂布的基材造成伤害。此外,目前用于溶剂型压敏胶粘剂交联固化的固化剂主要是多异氰酸酯类,此类固化剂可在室温下对胶粘剂进行交联固化,但普遍存在固化速度慢、存储性能差和成本偏高的问题,一般需在涂布之前加入,随着交联反应的进行,压敏胶溶液的粘度会迅速上升,且由于多异氰酸酯会吸收溶剂中的水分和空气中的潮气而使胶液浑浊,从而使固化剂失效,故需对水分严加控制。
总结来说,现如今市场上的压敏胶主要采用水性丙烯酸酯环保和耐候性佳,但耐水性、初粘性低,影响产品质量。因此,我们有必要重新的设计制备出一种新型的压敏胶材料,以此来解决现如今市场上的压敏胶所存在的缺陷,以此来更好的适应于社会与有关部门的需求。
发明内容
本发明所要解决的技术问题:针对目前压敏胶大多采用水性丙烯酸酯环保和耐候性佳,但耐水性、初粘性低的问题,提供一种压敏胶的制备方法。
为解决上述技术问题,本发明采用如下所述的技术方案是:
一种压敏胶的制备方法,其特征在于,该制备方法包括如下步骤:
(1)按质量比1:1:0.2~0.3,将二羟基聚醚、三羟基聚醚、二羟甲基丙酸放入容器中,在温度70~80℃下真空脱水,得脱水物;
(2)按重量份数计,取40~50份乙二胺水溶液、10~15份甲苯二异氰酸酯、7~8份丙烯酸羟乙酯、5~6份脱水物、1~2份丙酮,将甲苯二异氰酸酯、丙烯酸羟乙酯进行混合,通入氮气保护,升温至68~70℃,搅拌,加入脱水物,升温至80~85℃,静置,加入丙酮,待温度降低至38~40℃,在搅拌下加入乙二胺水溶液,搅拌均匀,得搅拌物;
(3)按重量份数计,取40~50份水、10~15份甲基丙烯酸甲酯、7~8份丙烯酸丁酯、5~6份丙烯酸、3~4份搅拌物、2~3份环氧树脂、2~3份松香、1~2份乳化剂,将搅拌物、环氧树脂、松香、甲基丙烯酸甲酯、丙烯酸丁酯、丙烯酸进行混合,搅拌,加入乳化剂,搅拌均匀,加入去离子水,用高剪切分散乳化机分散,得分散乳液;
(4)按质量比10~15:1~2:0.4~0.8,将分散乳液、引发剂、碳酸氢钠放入容器中,在温度75~85℃下静置,待冷却至室温,过滤,调节pH值7~8,得乳液,备用;
(5)按质量比2~3:1:15~20,将三乙烯四胺、丙二醇甲醚、水进行混合,放入容器中,通入氮气保护,在温度70~80℃下搅拌,再以60 mL/h的速度滴加水质量20~30%的聚醚多元醇二缩水甘油醚,保温,得保温物;
(6)按质量比1:2,将保温物、乙醇进行混合,搅拌均匀,加入冷却物质量10~15倍的步骤(4)备用的乳液,搅拌均匀,得搅拌乳液,将搅拌乳液涂布在经电晕处理、厚度为36μm的聚对苯二甲酸乙二醇酯膜上,置于鼓风干燥箱中干燥固化,即得压敏胶。
所述步骤(3)中乳化剂是按质量比1:0.8:10~20,将聚氧乙烯辛基苯酚醚-10、吐温80、去离子水进行混合,搅拌均匀,即得乳化剂。
所述步骤(4)中引发剂是过硫酸钾、过硫酸铵其中的任意一种。
本发明与其他方法相比,有益技术效果是:
(1)本发明以丙烯酸酯乳液为原料,聚氨酯、环氧树脂、松香为改性物,其中聚氨酯加入前利用二羟基聚醚、三羟基聚醚进行改性,聚醚的增加,导致硬段含量升高,在体系中增加高内聚能密度的氨酯键和脉键,且此基团具有很强的极性,它能够与薄膜表面的极性基团形成氢键,产生较大的粘接强度,利用改性聚氨酯乳液、丙烯酸酯乳液复合,兼备聚氨酯和聚丙烯酸酯的特性,从而使压敏胶的粘结强度增强,同时环氧树脂能够直接参与共聚接入聚氨酯主链,由于聚氨酯和环氧-丙烯酸酯间发生交联聚合反应,使聚合物链变长,形成网状结构,物理机械缠结程度更高,增加了乳胶膜的致密性,使得聚合物内聚力变大,致使压敏胶的持粘力、耐高温性以及耐水性都明显提高,虽然交联有助于提高丙烯酸酯压敏胶的内聚强度、耐热性及抗蠕变性能,但是过度交联会导致压敏胶对基材的润湿性
差,剥离强度下降,从而通过向丙烯酸酯乳液中引入松香作为增黏树脂,能够提高其粘结性能,从而制备出优良的耐高温丙烯酸酯压敏胶。
(2)本发明还加入以三乙烯四胺、丙二醇甲醚为原料获得的一种新型固化剂,其具有独特的分子结构:含有与被乳化的液体环氧树脂极相似的疏水链段,同时含有亲水性的柔性聚醚链段,从而能够改善压敏胶固化后性能较脆的缺陷。
具体实施方式
乳化剂是按质量比1:0.8:10~20,将聚氧乙烯辛基苯酚醚-10、吐温80、去离子水进行混合,搅拌均匀,即得乳化剂。
引发剂是过硫酸钾、过硫酸铵其中的任意一种。
一种压敏胶的制备方法,该制备方法包括如下步骤:
(1)按质量比1:1:0.2~0.3,将二羟基聚醚、三羟基聚醚、二羟甲基丙酸放入容器中,在温度70~80℃下真空脱水1~2h,得脱水物;
(2)按重量份数计,取40~50份0.2mol/L乙二胺水溶液、10~15份甲苯二异氰酸酯、7~8份丙烯酸羟乙酯、5~6份脱水物、1~2份丙酮,将甲苯二异氰酸酯、丙烯酸羟乙酯进行混合,通入氮气保护,升温至68~70℃,搅拌1~2h,加入脱水物,升温至80~85℃,静置2~3h,加入丙酮,待温度降低至38~40℃,在800~900r/min搅拌下加入乙二胺水溶液,搅拌均匀,得搅拌物;
(3)按重量份数计,取40~50份水、10~15份甲基丙烯酸甲酯、7~8份丙烯酸丁酯、5~6份丙烯酸、3~4份搅拌物、2~3份环氧树脂、2~3份松香、1~2份乳化剂,将搅拌物、环氧树脂、松香、甲基丙烯酸甲酯、丙烯酸丁酯、丙烯酸进行混合,以500~600r/min搅拌0.5~1h,加入乳化剂,搅拌均匀,加入去离子水,用高剪切分散乳化机分散25~30min,得分散乳液;
(4)按质量比10~15:1~2:0.4~0.8,将分散乳液、引发剂、碳酸氢钠放入容器中,在温度75~85℃下静置2~3h,待冷却至室温,过滤,调节pH值7~8,得乳液,备用;
(5)按质量比2~3:1:15~20,将三乙烯四胺、丙二醇甲醚、水进行混合,放入容器中,通入氮气保护,在温度70~80℃,500~600r/min条件搅拌1~2h,再以60 mL/h的速度滴加水质量20~30%的聚醚多元醇二缩水甘油醚,保温1~2h,得保温物;
(6)按质量比1:2,将保温物、乙醇进行混合,以200~300r/min搅拌均匀,加入冷却物质量10~15倍的步骤(4)备用的乳液,搅拌均匀,得搅拌乳液,将搅拌乳液涂布在经电晕处理、厚度为36μm的聚对苯二甲酸乙二醇酯膜上,置于鼓风干燥箱中干燥固化,即得压敏胶。
乳化剂是按质量比1:0.8:10,将聚氧乙烯辛基苯酚醚-10、吐温80、去离子水进行混合,搅拌均匀,即得乳化剂。
引发剂是过硫酸钾。
一种压敏胶的制备方法,该制备方法包括如下步骤:
(1)按质量比1:1:0.2,将二羟基聚醚、三羟基聚醚、二羟甲基丙酸放入容器中,在温度70℃下真空脱水1h,得脱水物;
(2)按重量份数计,取40份0.2mol/L乙二胺水溶液、105份甲苯二异氰酸酯、7份丙烯酸羟乙酯、5份脱水物、1份丙酮,将甲苯二异氰酸酯、丙烯酸羟乙酯进行混合,通入氮气保护,升温至68℃,搅拌1h,加入脱水物,升温至80℃,静置2h,加入丙酮,待温度降低至38℃,在800r/min搅拌下加入乙二胺水溶液,搅拌均匀,得搅拌物;
(3)按重量份数计,取40份水、10份甲基丙烯酸甲酯、7份丙烯酸丁酯、5份丙烯酸、3份搅拌物、2份环氧树脂、2份松香、1份乳化剂,将搅拌物、环氧树脂、松香、甲基丙烯酸甲酯、丙烯酸丁酯、丙烯酸进行混合,以500r/min搅拌0.5h,加入乳化剂,搅拌均匀,加入去离子水,用高剪切分散乳化机分散25min,得分散乳液;
(4)按质量比10:1:0.4,将分散乳液、引发剂、碳酸氢钠放入容器中,在温度75℃下静置2h,待冷却至室温,过滤,调节pH值7,得乳液,备用;
(5)按质量比2:1:15,将三乙烯四胺、丙二醇甲醚、水进行混合,放入容器中,通入氮气保护,在温度70℃,500r/min条件搅拌1h,再以60 mL/h的速度滴加水质量20%的聚醚多元醇二缩水甘油醚,保温1h,得保温物;
(6)按质量比1:2,将保温物、乙醇进行混合,以200r/min搅拌均匀,加入冷却物质量10倍的步骤(4)备用的乳液,搅拌均匀,得搅拌乳液,将搅拌乳液涂布在经电晕处理、厚度为36μm的聚对苯二甲酸乙二醇酯膜上,置于鼓风干燥箱中干燥固化,即得压敏胶。
乳化剂是按质量比1:0.8:20,将聚氧乙烯辛基苯酚醚-10、吐温80、去离子水进行混合,搅拌均匀,即得乳化剂。
引发剂是过硫酸铵其中的任意一种。
一种压敏胶的制备方法,该制备方法包括如下步骤:
(1)按质量比1:1:0.3,将二羟基聚醚、三羟基聚醚、二羟甲基丙酸放入容器中,在温度80℃下真空脱水2h,得脱水物;
(2)按重量份数计,取50份0.2mol/L乙二胺水溶液、15份甲苯二异氰酸酯、8份丙烯酸羟乙酯、6份脱水物、2份丙酮,将甲苯二异氰酸酯、丙烯酸羟乙酯进行混合,通入氮气保护,升温至70℃,搅拌2h,加入脱水物,升温至85℃,静置3h,加入丙酮,待温度降低至40℃,在900r/min搅拌下加入乙二胺水溶液,搅拌均匀,得搅拌物;
(3)按重量份数计,取50份水、15份甲基丙烯酸甲酯、8份丙烯酸丁酯、6份丙烯酸、4份搅拌物、3份环氧树脂、3份松香、2份乳化剂,将搅拌物、环氧树脂、松香、甲基丙烯酸甲酯、丙烯酸丁酯、丙烯酸进行混合,以600r/min搅拌1h,加入乳化剂,搅拌均匀,加入去离子水,用高剪切分散乳化机分散30min,得分散乳液;
(4)按质量比15:2:0.8,将分散乳液、引发剂、碳酸氢钠放入容器中,在温度85℃下静置3h,待冷却至室温,过滤,调节pH值8,得乳液,备用;
(5)按质量比3:1:20,将三乙烯四胺、丙二醇甲醚、水进行混合,放入容器中,通入氮气保护,在温度80℃,600r/min条件搅拌2h,再以60 mL/h的速度滴加水质量30%的聚醚多元醇二缩水甘油醚,保温2h,得保温物;
(6)按质量比1:2,将保温物、乙醇进行混合,以300r/min搅拌均匀,加入冷却物质量15倍的步骤(4)备用的乳液,搅拌均匀,得搅拌乳液,将搅拌乳液涂布在经电晕处理、厚度为36μm的聚对苯二甲酸乙二醇酯膜上,置于鼓风干燥箱中干燥固化,即得压敏胶。
乳化剂是按质量比1:0.8:15,将聚氧乙烯辛基苯酚醚-10、吐温80、去离子水进行混合,搅拌均匀,即得乳化剂。
引发剂是过硫酸钾。
一种压敏胶的制备方法,该制备方法包括如下步骤:
(1)按质量比1:1:0.25,将二羟基聚醚、三羟基聚醚、二羟甲基丙酸放入容器中,在温度75℃下真空脱水1.5h,得脱水物;
(2)按重量份数计,取45份0.2mol/L乙二胺水溶液、12.5份甲苯二异氰酸酯、7.5份丙烯酸羟乙酯、5.5份脱水物、1.5份丙酮,将甲苯二异氰酸酯、丙烯酸羟乙酯进行混合,通入氮气保护,升温至69℃,搅拌1.5h,加入脱水物,升温至83℃,静置2.5h,加入丙酮,待温度降低至39℃,在850r/min搅拌下加入乙二胺水溶液,搅拌均匀,得搅拌物;
(3)按重量份数计,取45份水、12.5份甲基丙烯酸甲酯、7.5份丙烯酸丁酯、5.5份丙烯酸、3.5份搅拌物、2.5份环氧树脂、2.5份松香、1.5份乳化剂,将搅拌物、环氧树脂、松香、甲基丙烯酸甲酯、丙烯酸丁酯、丙烯酸进行混合,以550r/min搅拌0.75h,加入乳化剂,搅拌均匀,加入去离子水,用高剪切分散乳化机分散27.5min,得分散乳液;
(4)按质量比12.5:1.5:0.6,将分散乳液、引发剂、碳酸氢钠放入容器中,在温度80℃下静置2.5h,待冷却至室温,过滤,调节pH值7.5,得乳液,备用;
(5)按质量比2.5:1:17.5,将三乙烯四胺、丙二醇甲醚、水进行混合,放入容器中,通入氮气保护,在温度75℃,550r/min条件搅拌1.5h,再以60mL/h的速度滴加水质量25%的聚醚多元醇二缩水甘油醚,保温1.5h,得保温物;
(6)按质量比1:2,将保温物、乙醇进行混合,以250r/min搅拌均匀,加入冷却物质量12.5倍的步骤(4)备用的乳液,搅拌均匀,得搅拌乳液,将搅拌乳液涂布在经电晕处理、厚度为36μm的聚对苯二甲酸乙二醇酯膜上,置于鼓风干燥箱中干燥固化,即得压敏胶。
对比例:阜城县某公司生产的压敏胶。
将实施例以及对比例所制得的压敏胶分别进行粘接性能测试,再放入水中浸泡24小时之后拿到室外放置,观察开裂情况,测试结果见表1。
表1:
测试项目 实施例1 实施例2 实施例3 对比例
粘度MPa·s 8793 9017 9136 6011~6121
初粘时间min 28 31 27 12~14
开裂情况 无开裂 无开裂 轻微开裂 开裂严重
实验证明,本发明所制备的压敏胶具有更强的粘接性,在使用中所表示出来的综合性能更好,值得大力推广使用。

Claims (3)

1.一种压敏胶的制备方法,其特征在于,该制备方法包括如下步骤:
(1)按质量比1:1:0.2~0.3,将二羟基聚醚、三羟基聚醚、二羟甲基丙酸放入容器中,在温度70~80℃下真空脱水,得脱水物;
(2)按重量份数计,取40~50份乙二胺水溶液、10~15份甲苯二异氰酸酯、7~8份丙烯酸羟乙酯、5~6份脱水物、1~2份丙酮,将甲苯二异氰酸酯、丙烯酸羟乙酯进行混合,通入氮气保护,升温至68~70℃,搅拌,加入脱水物,升温至80~85℃,静置,加入丙酮,待温度降低至38~40℃,在搅拌下加入乙二胺水溶液,搅拌均匀,得搅拌物;
(3)按重量份数计,取40~50份水、10~15份甲基丙烯酸甲酯、7~8份丙烯酸丁酯、5~6份丙烯酸、3~4份搅拌物、2~3份环氧树脂、2~3份松香、1~2份乳化剂,将搅拌物、环氧树脂、松香、甲基丙烯酸甲酯、丙烯酸丁酯、丙烯酸进行混合,搅拌,加入乳化剂,搅拌均匀,加入去离子水,用高剪切分散乳化机分散,得分散乳液;
(4)按质量比10~15:1~2:0.4~0.8,将分散乳液、引发剂、碳酸氢钠放入容器中,在温度75~85℃下静置,待冷却至室温,过滤,调节pH值7~8,得乳液,备用;
(5)按质量比2~3:1:15~20,将三乙烯四胺、丙二醇甲醚、水进行混合,放入容器中,通入氮气保护,在温度70~80℃下搅拌,再以60 mL/h的速度滴加水质量20~30%的聚醚多元醇二缩水甘油醚,保温,得保温物;
(6)按质量比1:2,将保温物、乙醇进行混合,搅拌均匀,加入冷却物质量10~15倍的步骤(4)备用的乳液,搅拌均匀,得搅拌乳液,将搅拌乳液涂布在经电晕处理、厚度为36μm的聚对苯二甲酸乙二醇酯膜上,置于鼓风干燥箱中干燥固化,即得压敏胶。
2.根据权利要求1所述压敏胶的制备方法,其特征在于,所述步骤(3)中乳化剂是按质量比1:0.8:10~20,将聚氧乙烯辛基苯酚醚-10、吐温80、去离子水进行混合,搅拌均匀,即得乳化剂。
3.根据权利要求1所述压敏胶的制备方法,其特征在于,所述步骤(4)中引发剂是过硫酸钾、过硫酸铵其中的任意一种。
CN201810306550.4A 2018-04-08 2018-04-08 一种压敏胶的制备方法 Withdrawn CN108424731A (zh)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201810306550.4A CN108424731A (zh) 2018-04-08 2018-04-08 一种压敏胶的制备方法

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201810306550.4A CN108424731A (zh) 2018-04-08 2018-04-08 一种压敏胶的制备方法

Publications (1)

Publication Number Publication Date
CN108424731A true CN108424731A (zh) 2018-08-21

Family

ID=63160439

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201810306550.4A Withdrawn CN108424731A (zh) 2018-04-08 2018-04-08 一种压敏胶的制备方法

Country Status (1)

Country Link
CN (1) CN108424731A (zh)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109054664A (zh) * 2018-07-05 2018-12-21 胡果青 一种热熔胶的制备方法
CN110041847A (zh) * 2019-04-24 2019-07-23 厦门市豪尔新材料股份有限公司 一种温控性粘离胶及包含其的温控性粘离膜
CN115093819A (zh) * 2022-07-01 2022-09-23 张家港飞腾复合新材料股份有限公司 复合板连接用胶粘剂及其应用方法

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20100135568A (ko) * 2009-06-17 2010-12-27 공주대학교 산학협력단 아크릴계 다이싱용 점착제 조성물 및 그 테이프
CN103435760A (zh) * 2013-08-12 2013-12-11 华南理工大学 一种改性双组份水性聚氨酯耐高温压敏胶的制备方法

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20100135568A (ko) * 2009-06-17 2010-12-27 공주대학교 산학협력단 아크릴계 다이싱용 점착제 조성물 및 그 테이프
CN103435760A (zh) * 2013-08-12 2013-12-11 华南理工大学 一种改性双组份水性聚氨酯耐高温压敏胶的制备方法

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
周继亮 等: "非离子型自乳化水性环氧固化剂的合成与性能", 《高校化学工程学报》 *
王荣: "改性丙烯酸酯乳液压敏胶的研究", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 *
赖婉婷: "耐高温水性丙烯酸酯压敏胶的制备", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109054664A (zh) * 2018-07-05 2018-12-21 胡果青 一种热熔胶的制备方法
CN110041847A (zh) * 2019-04-24 2019-07-23 厦门市豪尔新材料股份有限公司 一种温控性粘离胶及包含其的温控性粘离膜
CN115093819A (zh) * 2022-07-01 2022-09-23 张家港飞腾复合新材料股份有限公司 复合板连接用胶粘剂及其应用方法
CN115093819B (zh) * 2022-07-01 2024-03-15 张家港飞腾复合新材料股份有限公司 复合板连接用胶粘剂及其应用方法

Similar Documents

Publication Publication Date Title
CN104788623B (zh) 互穿网络型水性聚氨酯‑丙烯酸酯复合乳液的制备方法
CN102516904B (zh) 一种蒸发式降温湿帘用单组分水性胶粘剂及其制备方法
CN108424731A (zh) 一种压敏胶的制备方法
CN105295781B (zh) 一种水性压敏胶及其制备方法和用途
CN102199254A (zh) 一种单组份耐溶剂保护膜胶的制备方法
CN104099047B (zh) 用于改进胶粘带对玻璃表面的粘合性的黑硅烷底胶
CN107974221A (zh) 一种多响应聚合物粘附胶材料及其应用
CN107057629A (zh) 环保高强度密封胶组合物及其制备方法
CN103805122A (zh) 一种水性聚氨酯贴布胶及其制备方法
CN106753081B (zh) 一种fpc用胶膜及其制备方法和fpc
CN114058313B (zh) 一种高粘接热固胶膜及其制备方法和应用
CN111334236A (zh) 一种双组份水性聚氨酯耐水煮胶粘剂的制备方法
CN107903353A (zh) 纺织品印花台板胶及其制备方法
CN107779156A (zh) 一种水性聚氨酯胶黏剂
CN107236477B (zh) 一种无残留型临时固定粘合剂及其制备方法
CN109735255A (zh) 一种耐热抗寒的户外用压敏胶及其压敏胶带
CN103509162A (zh) 一种环氧改性聚酯丙烯酸酯及其制备方法
CN106749841A (zh) 改性共聚树脂的制备方法
CN107459605B (zh) 一种高速涂布纸塑复合用高固含低粘度丙烯酸压敏胶粘剂制备方法
CN110003807A (zh) 一种水性乳胶异种接枝材料及其制备方法、以及其在软质pvc薄膜压敏胶带中的应用
WO2018187935A1 (en) Water borne dry lamination bonding agent with heat resistance improvement
CN106752355A (zh) 塑料油墨涂料的制备方法
CN115029085A (zh) 一种电子束固化丙烯酸酯压敏胶及其制备方法
CN106749844A (zh) 丙烯酸酯树脂组合物的制备方法
CN109385137B (zh) 一种反应性以及温敏性微凝胶改性的水性uv固化油墨及其制备方法

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
WW01 Invention patent application withdrawn after publication
WW01 Invention patent application withdrawn after publication

Application publication date: 20180821