CN108559437A - 反应型聚氨酯热熔胶及其制备方法 - Google Patents
反应型聚氨酯热熔胶及其制备方法 Download PDFInfo
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- CN108559437A CN108559437A CN201810167988.9A CN201810167988A CN108559437A CN 108559437 A CN108559437 A CN 108559437A CN 201810167988 A CN201810167988 A CN 201810167988A CN 108559437 A CN108559437 A CN 108559437A
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- type polyurethane
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- polyurethane hot
- melt adhesive
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- 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
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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- C—CHEMISTRY; METALLURGY
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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- C—CHEMISTRY; METALLURGY
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- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
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- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
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Abstract
本发明涉及一种反应型聚氨酯热熔胶及其制备方法。所述的反应型聚氨酯热熔胶，以重量份计，包括如下原料组分：结晶聚酯多元醇30～50份，液体聚酯多元醇30～50份，含磷多元醇10～20份，异氰酸酯10～50份，热塑性树脂10～30份，粘合促进剂1～3份，催化剂0.1～0.5份，抗氧剂1～2份。本发明的反应型聚氨酯热熔胶，具有阻燃性和粘结性优异的优点，且还具有固化速度快、最终粘接强度高，耐环境抵抗性好、雾化值低等特点，特别适合于对阻燃要求较高的领域使用，具有良好的市场前景。另外，该反应型聚氨酯热熔胶为单组分湿气固化聚氨酯胶黏剂，属于无溶剂环保型胶黏剂行业，可用于塑料、玻璃、金属、纺织等基材的粘接。
Description
技术领域
本发明涉及热熔胶，特别是涉及反应型聚氨酯热熔胶及其制备方法。
背景技术
反应型聚氨酯热熔胶(PUR)因具有操作简单、性能优异、环境友好等特点，近年来在汽车、电子电器、木材加工、书籍装订及食品包装等行业得到了快速发展。但现有的PUR阻燃性能比较差，限制了它在某些特定领域的应用。
通常，阻燃聚合物通过外加阻燃剂的方式制备而成，阻燃剂分无机阻燃剂和有机阻燃剂，若要PUR达到较好的阻燃效果，无机阻燃剂的添加量一般较大，这会导致PUR熔融黏度显著提高，施工性变差；而添加有机阻燃剂，则可能存在阻燃剂与PUR体系相容性较差，阻燃剂容易析出，使得PUR的粘接性能变差、VOC含量增加。
发明内容
基于此，有必要提供一种反应型聚氨酯热熔胶。该反应型聚氨酯热熔胶具有较佳的阻燃效果，且粘结性能优异，施工性好。
一种反应型聚氨酯热熔胶，以重量份计，包括如下原料组分：
其中，所述粘合促进剂的分子结构中包括至少一个异氰酸酯基和至少一个三甲氧基硅基。
在其中一个实施例中，所述的反应型聚氨酯热熔胶，以重量份计，包括如下原料组分：
在其中一个实施例中，所述的反应型聚氨酯热熔胶，以重量份计，包括如下原料组分：
在其中一个实施例中，所述粘合促进剂由三羟甲基丙烷、间苯二亚甲基异氰酸酯与二(3-三甲氧基甲硅烷基丙基)胺缩合而成。
在其中一个实施例中，所述粘合促进剂选自式(1)、式(2)化合物中的至少一种：
在其中一个实施例中，所述含磷多元醇的羟值在100～500mgKOH/g之间，含磷量在10～20％之间。
在其中一个实施例中，所述热塑性树脂为热塑性聚氨酯(TPU)、乙烯醋酸乙烯共聚物(EVA)、热塑性聚酯、丙烯酸树脂中的至少一种。
在其中一个实施例中，所述异氰酸酯为4,4’-二苯基甲烷二异氰酸酯(MDI)、碳化二亚胺改性MDI、MDI-50中的至少一种。
在其中一个实施例中，所述结晶聚酯多元醇的羟值在10～112mgKOH/g之间。优选羟值在10～40mgKOH/g之间。
在其中一个实施例中，所述结晶聚酯多元醇由下述醇和酸反应得到：酸为己二酸、癸二酸、对苯二甲酸、十二烷二酸中的至少一种；醇为乙二醇、1,4-丁二醇、1,6-己二醇中的至少一种。
在其中一个实施例中，所述液体聚酯多元醇的羟值在10～112mgKOH/g之间。优选羟值在18～40mgKOH/g之间。
在其中一个实施例中，所述液体聚酯多元醇由下述醇和酸反应得到：酸为己二酸、癸二酸、对苯二甲酸、邻苯二甲酸、间苯二甲酸中的至少一种；醇为乙二醇、1,4-丁二醇、异戊二醇、1,6-己二醇中的至少一种。
在其中一个实施例中，所述催化剂为二月桂酸二丁基锡(DBTDL)、三亚乙基二胺、二吗啉基二乙基醚(DMDEE)中的至少一种。
在其中一个实施例中，所述抗氧剂为2,6-二叔丁基对甲基苯酚、四[β-(3,5-二叔丁基-4-羟基苯基)丙酸]季戊四醇酯(抗氧剂1010)、β-(3,5-二叔丁基-4-羟基苯基)丙酸正十八碳醇酯、三(2.4-二叔丁基苯基)亚磷酸酯(抗氧剂168)、双(3,5-二叔丁基-4-羟基苯基)硫醚中的至少一种。
本发明还提供所述的反应型聚氨酯热熔胶制备方法，包括如下步骤：
(1)将所述结晶聚酯多元醇、液体聚酯多元醇、含磷多元醇、热塑性树脂投入反应釜中，加热至100～130℃，在搅拌下真空脱水1～3小时，真空度为-0.095～0.05MPa；
(2)降温至80～90℃，于所述反应釜中投入预热到55～65℃的所述异氰酸酯，在惰性气体保护下于75～85℃搅拌反应1～3小时；
(3)然后于所述反应釜中依次加入所述粘合促进剂、催化剂、抗氧化剂，在惰性气体保护下于75～85℃搅拌混合0.5～2小时，即得。
在其中一个实施例中，还包括步骤(4)：将步骤(3)所得反应物升温至100～130℃，抽真空至无气泡出现。以此去除所含的小分子或挥发性杂质。
与现有技术相比，本发明具有以下有益效果：
本发明在合理配置各原料组分的基础上，采用结晶聚酯多元醇和液体聚酯多元醇，配合适量包括至少一个异氰酸酯基和至少一个三甲氧基硅基的粘合促进剂，利用粘合促进剂附带的三甲氧基硅基与粘接基材表面形成氢键或发生化学反应，附带的异氰酸酯基可以参与热熔胶的湿固化反应，从而可以提高热熔胶对粘接基材的附着力及粘接后耐环境抵抗性；同时，在此基础上配伍以含磷多元醇，含磷多元醇能够参与预聚反应制备预聚体，使热熔胶具有较好的阻燃效果和较低的VOC排放，避免了阻燃剂析出的缺陷，粘结性和施工性能好。
由此，本发明的反应型聚氨酯热熔胶，阻燃性和粘结性优异，且还具有固化速度快、最终粘接强度高，耐环境抵抗性好、雾化值低等特点，特别适合于对阻燃要求较高的领域使用，具有良好的市场前景。另外，该反应型聚氨酯热熔胶为单组分湿气固化聚氨酯胶黏剂，属于无溶剂环保型胶黏剂行业，可用于塑料、玻璃、金属、纺织等基材的粘接。
进一步地，选择添加一定的热塑性树脂，在热熔胶冷却时，可以加速热熔胶凝聚，有利于提高热熔胶的初粘力。
本发明的反应型聚氨酯热熔胶的制备方法工艺简单，容易操作，易于工业化。
具体实施方式
以下结合具体实施例对本发明的反应型聚氨酯热熔胶及其制备方法作进一步详细的说明。
本发明实施例中采用的结晶聚酯多元醇购自赢创公司的7300系列，具体如下：
7360，羟值为27～34mgKOH/g；
7361，羟值在10～16mgKOH/g；
7380，羟值在27～34mgKOH/g；
上述结晶聚酯多元醇由下述醇和酸反应得到：酸为己二酸、癸二酸、对苯二甲酸、十二烷二酸中的至少一种；醇为乙二醇、1,4-丁二醇、1,6-己二醇中的至少一种。
液体聚酯多元醇购自赢创公司的7200系列，具体如下：
7250，羟值在18～24mgKOH/g；
7230，羟值在27～34mgKOH/g；
上述液体聚酯多元醇由下述醇和酸反应得到：酸为己二酸、癸二酸、对苯二甲酸、邻苯二甲酸、间苯二甲酸中的至少一种；醇为乙二醇、1,4-丁二醇、异戊二醇、1,6-己二醇中的至少一种。
含磷多元醇购自科莱恩公司OP 550和OP560，其中，
OP 550羟值在130mgKOH/g，含磷量17％；
OP560羟值在429mgKOH/g，含磷量12％。
粘合促进剂的化学结构如下式：
该粘合促进剂可为市售产品，也可自制。自制方法如下：
在反应釜中加入经过除水处理的三羟甲基丙烷1摩尔份和间苯二亚甲基二异氰酸酯3摩尔份，再加入适量无水甲苯，在氮气保护下加热至80℃左右，搅拌反应3小时；
然后在持续搅拌的条件下通过滴加的方式，将2摩尔份的间苯二亚甲基的二(3-三甲氧基甲硅烷基丙基)胺加入反应釜，滴加完毕，继续在氮气保护下搅拌反应2小时；
最后，抽真空减压蒸馏，将反应釜内的甲苯和残留的低分子脱除，冷却、出料，制得粘合促进剂。
其余原料组分均为市售产品。
实施例1-3
本实施例三种反应型聚氨酯热熔胶，以重量份计，原料组分如下(表1)：
表1
上述反应型聚氨酯热熔胶的制备方法如下：
(1)、将结晶聚酯多元醇、液体聚酯多元醇、含磷多元醇、热塑性树脂投入反应釜中，加热至100～130℃，在搅拌下真空脱水2小时，真空度为-0.095～0.05MPa；
(2)、降温至80～90℃，投入预热到60℃的异氰酸酯，在N2保护下于75～85℃搅拌反应1.5小时；
(3)、依次加入粘合促进剂、催化剂、抗氧化剂，在N2保护下于75～85℃搅拌混合1小时；
(4)、升温至100～130℃，抽真空至无气泡出现，出料，即得。
对比例1-2
本对比例两种反应型聚氨酯热熔胶，其原料组分和制备方法类似实施例3，区别如下(表2)：
表2
效果测试：
取实施例1-3和对比例1-2制得的反应型聚氨酯热熔胶，按GB/T 7124-2008测试热熔胶的初粘强度(试样在25℃/50％RH的条件下进行固化3min后测试的拉伸剪切强度)、最终粘接强度(试样在25℃/50％RH的条件下进行固化7d后测试的拉伸剪切强度)和高温高湿后粘接强度(试样在25℃/50％RH的条件下进行固化7d后，在85℃/85％RH的条件下再放置7d后测试的拉伸剪切强度)；按UL94测试热熔胶的阻燃等级；按GB/T10707-2008测试热熔胶的氧指数；按HG/T 4909-2016测试热熔胶的雾化值；测试结果如表3所示。
表3
由表3中实施例3与对比例1的性能对比可以看出，添加粘合促进剂可以明显提高热熔胶对基材粘接强度和耐高温高湿性能；实施例3与对比例2的性能对比可以看出，添加相同份量含磷量差不多的含磷多元醇OP 550制得的热熔胶比添加液体含磷阻燃剂乙基磷酸二乙酯制得的热熔胶具有更好的阻燃性、粘接强度和耐高温高湿性能，且实施例3制得的热熔胶的雾化值显著低于由对比例2制得的热熔胶。
由此可见，本发明实施例1-3制备的反应型聚氨酯热熔胶具有阻燃性好，初粘强度和最终粘接强度优良，耐高温高湿优异，雾化值低等特点，可应用于阻燃性能要求高的特定领域。其中，实施例3的反应型聚氨酯热熔胶的综合性能最为优异。
以上所述实施例的各技术特征可以进行任意的组合，为使描述简洁，未对上述实施例中的各个技术特征所有可能的组合都进行描述，然而，只要这些技术特征的组合不存在矛盾，都应当认为是本说明书记载的范围。
以上所述实施例仅表达了本发明的几种实施方式，其描述较为具体和详细，但并不能因此而理解为对发明专利范围的限制。应当指出的是，对于本领域的普通技术人员来说，在不脱离本发明构思的前提下，还可以做出若干变形和改进，这些都属于本发明的保护范围。因此，本发明专利的保护范围应以所附权利要求为准。
Claims (10)
1.一种反应型聚氨酯热熔胶，其特征在于，以重量份计，包括如下原料组分：
其中，所述粘合促进剂的分子结构中包括至少一个异氰酸酯基和至少一个三甲氧基硅基。
2.根据权利要求1所述的反应型聚氨酯热熔胶，其特征在于，以重量份计，包括如下原料组分：
3.根据权利要求1所述的反应型聚氨酯热熔胶，其特征在于，所述粘合促进剂由三羟甲基丙烷、间苯二亚甲基异氰酸酯与二(3-三甲氧基甲硅烷基丙基)胺缩合而成。
4.根据权利要求3所述的反应型聚氨酯热熔胶，其特征在于，所述粘合促进剂选自式(1)、式(2)化合物中的至少一种：
5.根据权利要求1所述的反应型聚氨酯热熔胶，其特征在于，所述含磷多元醇的羟值在100～500mgKOH/g之间，含磷量在10～20％之间。
6.根据权利要求1-5任一项所述的反应型聚氨酯热熔胶，其特征在于，所述热塑性树脂为热塑性聚氨酯、乙烯醋酸乙烯共聚物、热塑性聚酯、丙烯酸树脂中的至少一种。
7.根据权利要求1-5任一项所述的反应型聚氨酯热熔胶，其特征在于，所述异氰酸酯为4,4’-二苯基甲烷二异氰酸酯、碳化二亚胺改性MDI、MDI-50中的至少一种。
8.根据权利要求1-5任一项所述的反应型聚氨酯热熔胶，其特征在于，所述结晶聚酯多元醇的羟值在10～112mgKOH/g之间；所述液体聚酯多元醇的羟值在10～112mgKOH/g之间。
9.根据权利要求1-5任一项所述的反应型聚氨酯热熔胶，其特征在于，所述催化剂为二月桂酸二丁基锡、三亚乙基二胺、二吗啉基二乙基醚中的至少一种；所述抗氧剂为2,6-二叔丁基对甲基苯酚、四[β-(3,5-二叔丁基-4-羟基苯基)丙酸]季戊四醇酯、β-(3,5-二叔丁基-4-羟基苯基)丙酸正十八碳醇酯、三(2.4-二叔丁基苯基)亚磷酸酯、双(3,5-二叔丁基-4-羟基苯基)硫醚中的至少一种。
10.权利要求1-9任一项所述的反应型聚氨酯热熔胶制备方法，其特征在于，包括如下步骤：
(1)将所述结晶聚酯多元醇、液体聚酯多元醇、含磷多元醇、热塑性树脂投入反应釜中，加热至100～130℃，在搅拌下真空脱水1～3小时，真空度为-0.095～0.05MPa；
(2)降温至80～90℃，于所述反应釜中投入预热到55～65℃的所述异氰酸酯，在惰性气体保护下于75～85℃搅拌反应1～3小时；
(3)然后于所述反应釜中依次加入所述粘合促进剂、催化剂、抗氧化剂，在惰性气体保护下于75～85℃搅拌混合0.5～2小时，即得。
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| CN116144308A (zh) * | 2022-11-22 | 2023-05-23 | 广州集泰化工股份有限公司 | 一种阻燃硅烷改性聚醚密封胶及其制备方法和应用 |
| CN115838579A (zh) * | 2022-12-06 | 2023-03-24 | 康菲胶粘剂技术（广东）有限公司 | 一种厚板材用pur平贴产品及其制备方法 |
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