CN106497496A - 一种蒙脱土改性聚氨酯胶黏剂的制备方法 - Google Patents

一种蒙脱土改性聚氨酯胶黏剂的制备方法 Download PDF

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CN106497496A
CN106497496A CN201611016039.8A CN201611016039A CN106497496A CN 106497496 A CN106497496 A CN 106497496A CN 201611016039 A CN201611016039 A CN 201611016039A CN 106497496 A CN106497496 A CN 106497496A
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modified polyurethane
polyurethane adhesive
montmorillonite
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李长英
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Shaanxi Yipinda Petrochemical Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/08—Processes
    • C08G18/10—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/40—High-molecular-weight compounds
    • C08G18/48—Polyethers
    • C08G18/4825—Polyethers containing two hydroxy groups
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
    • C08G18/72—Polyisocyanates or polyisothiocyanates
    • C08G18/74—Polyisocyanates or polyisothiocyanates cyclic
    • C08G18/76—Polyisocyanates or polyisothiocyanates cyclic aromatic
    • C08G18/7657—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings
    • C08G18/7664—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings containing alkylene polyphenyl groups
    • C08G18/7671—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings containing alkylene polyphenyl groups containing only one alkylene bisphenyl group
    • 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
    • C09J175/00—Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
    • C09J175/04—Polyurethanes
    • C09J175/08—Polyurethanes from polyethers

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  • Health & Medical Sciences (AREA)
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Abstract

本发明公开了一种蒙脱土改性聚氨酯胶黏剂的制备方法，通过聚醚二醇和二苯基甲烷二异氰酸酯反应先制备预聚体，再将正己烷、丙酮、异丙醇、二乙烯三胺和蒙脱土反应得到席夫碱，得到的预聚体和席夫碱反应后，与环氧树脂和乙酸乙酯反应得到蒙脱土改性聚氨酯胶黏剂。本发明采用原位聚合法，制得蒙脱土改性聚氨酯胶黏剂，力学性能优异，制成的胶黏剂剪切强度大，拉伸强度和断裂伸长率较好，拉伸强度科大307MPa，断裂伸长率可达639%。

Description

一种蒙脱土改性聚氨酯胶黏剂的制备方法
技术领域
本发明属于胶黏剂的制备领域，具体涉及一种蒙脱土改性聚氨酯胶黏剂的制备方法。
背景技术
聚氨酯（PU）是一种性能有很大可调性的材料，具有特殊的微相分离结构，它是由软、硬链段交替形成的嵌段共聚物，由于两种链段的热力学不相容而产生微相分离。硬段提供PU材料的硬度、强度和模量性能，软段提供PU材料的弹性、韧性及低温性能。这种特殊结构的聚氨酯胶黏剂赋予其许多优良的性能，如粘结范围广、粘结工艺简单、耐低温、可设计性强。蒙脱土是一种层状硅酸盐，每个晶胞由两个硅氧四面体中间夹有一个铝氧八面体构成，两种晶片靠共用氧原子连结，堆积紧密，有序度高。蒙脱土来源广泛，价格低廉，力学性能好，有吸附能力和离子交换能力。
然而聚氨酯基体热稳定性、表面性能、耐老化性较低等缺点，限制了进一步的应用，因此需要对其进行改性以改善其存在的缺陷。
发明内容
本发明提供一种蒙脱土改性聚氨酯胶黏剂的制备方法，制备的聚氨酯胶黏剂具有较好的力学性能。
一种蒙脱土改性聚氨酯胶黏剂的制备方法，包含以下步骤：
（1）先将分子量为1000的聚醚二醇真空脱水3 h，然后加入二苯基甲烷二异氰酸酯，恒温80℃反应2.5 h制得预聚体；
（2）把正己烷、丙酮、异丙醇、二乙烯三胺和蒙脱土加入三颈瓶中，25℃反应5 h得到席夫碱；
（3）将预聚体倒入席夫碱中，搅拌，45℃反应1h，升温至70℃蒸馏，无馏出物时，升温至120℃减压蒸馏15 min，真空度控制在-0.06 MPa，降温至70℃，加入无水乙醇，回流搅拌0.5h，降至室温；
（4）称取相同质量的环氧树脂和乙酸乙酯，混合搅拌；
（5）将步骤（3）和步骤（4）的产物按质量比10：1混合均匀，室温下抽真空4h，除去胶液中气泡，在涂有脱模剂的胶盘中进行固化，固化工艺为：在25℃下固化／8 h，然后在50℃固化5h，最后在80℃下固化6 h，自然冷却，即得到蒙脱土改性聚氨酯胶黏剂。
步骤（1）中，聚醚二醇和二苯基甲烷二异氰酸酯的摩尔比为1:1.5。
步骤（2）中，正己烷、丙酮、异丙醇、二乙烯三胺和蒙脱土的质量比为1:3:2.5:4:3。
步骤（3）中，预聚体与席夫碱的质量比为1.5:1。
本发明的优点：
本发明采用原位聚合法，制得蒙脱土改性聚氨酯胶黏剂，力学性能优异，制成的胶黏剂剪切强度大，拉伸强度和断裂伸长率较好，拉伸强度科大307MPa，断裂伸长率可达639%。
具体实施方式
实施例1
一种蒙脱土改性聚氨酯胶黏剂的制备方法，包含以下步骤：
（1）先将分子量为1000的聚醚二醇真空脱水3 h，然后加入二苯基甲烷二异氰酸酯，恒温80℃反应2.5 h制得预聚体；
（2）把正己烷、丙酮、异丙醇、二乙烯三胺和蒙脱土加入三颈瓶中，25℃反应5 h得到席夫碱；
（3）将预聚体倒入席夫碱中，搅拌，45℃反应1h，升温至70℃蒸馏，无馏出物时，升温至120℃减压蒸馏15 min，真空度控制在-0.06 MPa，降温至70℃，加入无水乙醇，回流搅拌0.5h，降至室温；
（4）称取相同质量的环氧树脂和乙酸乙酯，混合搅拌；
（5）将步骤（3）和步骤（4）的产物按质量比10：1混合均匀，室温下抽真空4h，除去胶液中气泡，在涂有脱模剂的胶盘中进行固化，固化工艺为：在25℃下固化／8 h，然后在50℃固化5h，最后在80℃下固化6 h，自然冷却，即得到蒙脱土改性聚氨酯胶黏剂。
步骤（1）中，聚醚二醇和二苯基甲烷二异氰酸酯的摩尔比为1:1.5。
步骤（2）中，正己烷、丙酮、异丙醇、二乙烯三胺和蒙脱土的质量比为1:3:2.5:4:3。
步骤（3）中，预聚体与席夫碱的质量比为1.5:1。

Claims (4)

1.一种蒙脱土改性聚氨酯胶黏剂的制备方法，其特征在于：包含以下步骤：
（1）先将分子量为1000的聚醚二醇真空脱水3 h，然后加入二苯基甲烷二异氰酸酯，恒温80℃反应2.5 h制得预聚体；
（2）把正己烷、丙酮、异丙醇、二乙烯三胺和蒙脱土加入三颈瓶中，25℃反应5 h得到席夫碱；
（3）将预聚体倒入席夫碱中，搅拌，45℃反应1h，升温至70℃蒸馏，无馏出物时，升温至120℃减压蒸馏15 min，真空度控制在-0.06 MPa，降温至70℃，加入无水乙醇，回流搅拌0.5h，降至室温；
（4）称取相同质量的环氧树脂和乙酸乙酯，混合搅拌；
（5）将步骤（3）和步骤（4）的产物按质量比10：1混合均匀，室温下抽真空4h，除去胶液中气泡，在涂有脱模剂的胶盘中进行固化，固化工艺为：在25℃下固化／8 h，然后在50℃固化5h，最后在80℃下固化6 h，自然冷却，即得到蒙脱土改性聚氨酯胶黏剂。
2.根据权利要求1所述的一种蒙脱土改性聚氨酯胶黏剂的制备方法，其特征在于：步骤（1）中，聚醚二醇和二苯基甲烷二异氰酸酯的摩尔比为1:1.5。
3.根据权利要求1所述的一种蒙脱土改性聚氨酯胶黏剂的制备方法，其特征在于：步骤（2）中，正己烷、丙酮、异丙醇、二乙烯三胺和蒙脱土的质量比为1:3:2.5:4:3。
4.根据权利要求1所述的一种蒙脱土改性聚氨酯胶黏剂的制备方法，其特征在于：步骤（3）中，预聚体与席夫碱的质量比为1.5:1。
CN201611016039.8A 2016-11-18 2016-11-18 一种蒙脱土改性聚氨酯胶黏剂的制备方法 Pending CN106497496A (zh)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111720646A (zh) * 2020-06-28 2020-09-29 浙江波士特机械有限公司 一种商用车气制动系统用快插连接头
TWI719307B (zh) * 2017-05-12 2021-02-21 日商可樂麗股份有限公司 硏磨層與其改質方法、硏磨墊及硏磨方法

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
TWI719307B (zh) * 2017-05-12 2021-02-21 日商可樂麗股份有限公司 硏磨層與其改質方法、硏磨墊及硏磨方法
US11053339B2 (en) 2017-05-12 2021-07-06 Kuraray Co., Ltd. Polyurethane for polishing layer, polishing layer including polyurethane and modification method of the polishing layer, polishing pad, and polishing method
US11787894B2 (en) 2017-05-12 2023-10-17 Kuraray Co., Ltd. Polyurethane for polishing layer, polishing layer including polyurethane and modification method of the polishing layer, polishing pad, and polishing method
CN111720646A (zh) * 2020-06-28 2020-09-29 浙江波士特机械有限公司 一种商用车气制动系统用快插连接头

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Application publication date: 20170315