CN105885767A - Mdi基聚氨酯电子灌封胶与其制备方法和应用方法 - Google Patents

Mdi基聚氨酯电子灌封胶与其制备方法和应用方法 Download PDF

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CN105885767A
CN105885767A CN201610481675.1A CN201610481675A CN105885767A CN 105885767 A CN105885767 A CN 105885767A CN 201610481675 A CN201610481675 A CN 201610481675A CN 105885767 A CN105885767 A CN 105885767A
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黄金
陆南平
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MIANYANG WELLS ELECTRONIC MATERIAL CO Ltd
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Abstract

本发明公开了一种MDI基聚氨酯电子灌封胶及其制备方法和应用方法，该电子灌封胶由A、B两种组分组成；其中，A组分由按重量份计的50～60份的异氰酸酯、15～20份的低聚物多元醇和9～30份的反应型液体阻燃剂制成；B组分由低聚物多元醇、交联扩链剂、催化剂、填料、消泡剂和抗氧剂按一定比例制成。A、B组分按一定比例混合、固化，即制得该灌封胶。本发明通过半预聚法制备MDI基聚氨酯灌封胶，避免了NCO挥发所带来的毒性，以无卤反应型液体阻燃剂与填料协同阻燃，避免了添加型液体阻燃剂对聚氨酯灌封胶稳定性及性能的影响。所制得的聚氨酯弹性体适用于中小型电子元件的灌封。

Description

MDI基聚氨酯电子灌封胶与其制备方法和应用方法
技术领域
本发明的实施方式涉及电子器件灌封胶，属于化学领域，更具体地，本发明的实施方式涉及用于小型电子元器件封装的MDI基无卤环保聚氨酯灌封胶与其制备方法和应用方法。
背景技术
灌封胶主要有环氧灌封胶、有机硅灌封胶、聚氨酯灌封胶等。环氧灌封胶粘接性能优良、绝缘性能好，但固化后较脆、弹性差、抗冲击性能差；有机硅灌封胶绝缘性能、耐高低温抗冲击性能优异，但其耐油性及黏附力较差。聚氨酯灌封胶绝缘性能、耐水耐油性能好，同时其机械性能可调范围大、成本较低，对电器元件无腐蚀，可应用于变压器、抗流圈、转换器、电容器、电感器、变阻器、电路板、LED驱动电源等的灌封。
传统聚氨酯灌封胶的制备方法主要有一步法、预聚法和半预聚法三种。其中采用一步法制得的聚氨酯灌封胶分子结构不规整，力学性能不如预聚体法好；而采用预聚法和半预聚法制得的聚氨酯灌封胶分子链段排列比较规整，制品具有较好的力学性能，重复性也较好。
聚氨酯灌封胶应用最早的是以TDI为固化剂建立起来的聚氨酯体系，该体系多采用预聚法制备，可以保证产品具有较高的工艺性和稳定性，但由于TDI易挥发、毒性大，这就为TDI的生产、运输、应用埋下了较大的安全隐患，同时TDI体系聚氨酯灌封胶预聚体中游离NCO也会为下游行业带来环保难题。MDI体系聚氨酯灌封胶可以很大程度上规避以上难题，而以MDI代替TDI制备聚氨酯灌封胶的趋势也越来越明显。但与TDI相比，MDI的活性高、制得的预聚体粘度大，所以MDI体系聚氨酯灌封胶多以一步法制备，这就使得产品的性能及稳定性很难保证。
发明内容
为解决上述问题，同时出于聚氨酯制备工艺及环保方面的考虑，本发明提出了一种适用于小型电子元器件封装的聚氨酯灌封胶及其制备方法，尤其涉及一种MDI基无卤环保聚氨酯灌封胶及其制备方法。本发明采取的技术方案如下：
一种MDI基聚氨酯电子灌封胶，该电子灌封胶由A、B两种组分组成；其中，A组分由按重量份计的50～60份的异氰酸酯、15～20份的低聚物多元醇和9～30份的反应型液体阻燃剂制成；B组分由按重量份计的55～100份低聚物多元醇、1.0～3.5份交联扩链剂、0.01～0.1份催化剂、105～140份填料、0.5～1份消泡剂和0.5～1份抗氧剂制成。
上述MDI基聚氨酯电子灌封胶中的异氰酸酯为MDI、碳化二亚胺改性MDI、PAPI中的一种或任意几种的混合物。
上述MDI基聚氨酯电子灌封胶的A、B组分中的低聚物多元醇为羟基官能度≥2、分子量为600～5000的端羟基聚丁二烯、聚环氧丙烯多元醇、蓖麻油多元醇中的一种或任意几种的混合物。
上述MDI基聚氨酯电子灌封胶中的反应型液体阻燃剂是羟基官能度为1～2的磷酸酯类阻燃剂；填料为氧化铝、氢氧化铝或硅微粉，填料的平均粒径在1～50um的范围内。
进一步的技术方案是，上述MDI基聚氨酯电子灌封胶中的反应型液体阻燃剂为三(一缩二丙二醇)亚磷酸酯、N,N-二(2-羟基乙基)氨甲基膦酸二乙酯、N,N-二(2-羟乙基)氨甲基膦酸二甲酯、端羟基聚磷酸酯。
上述MDI基聚氨酯电子灌封胶中的交联扩链剂为丙二醇、1,4-丁二醇或三羟甲基丙烷。
上述MDI基聚氨酯电子灌封胶中的催化剂为三乙胺、三亚乙基二胺、二月桂酸二丁基锡、辛酸亚锡、异辛酸锌或异辛酸铅。
上述MDI基聚氨酯电子灌封胶中的消泡剂为改性硅氧烷、丙烯酸酯共聚物或非硅酮高分子聚合物；抗氧剂为2,6-二叔丁基-4-甲基苯酚、亚磷酸三(壬基苯酯)或酚噻嗪。
本发明还提供了上述MDI基聚氨酯电子灌封胶的制备方法，它采用半预聚法，包括以下步骤：
A组分的制备
按比例称取A组分原料，将低聚物多元醇和反应型液体阻燃剂于110～120℃下真空脱水2～3h，再降温至60～70℃，加入异氰酸酯并在30min内逐渐升温至75～85℃反应，反应过程中通氮气保护，并测试NCO％值，在NCO％值达到设定值时，停止反应即得A组分；所述设定值在10％～15％范围内；
B组分的制备
按比例称取B组分原料，将低聚物多元醇、交联扩链剂、填料加入反应釜中并于110～120℃下真空搅拌2h，再降温至50～80℃，加入消泡剂、催化剂和抗氧剂，搅拌均匀即得B组分。
上述MDI基聚氨酯电子灌封胶的应用方法是：所述A组分和B组分按照质量比20～25:100混合后搅拌、脱泡，浇注于经干燥处理过的电子器件中，再于25℃固化7天或者于60℃固化24h，即完成电子器件的灌封。
与现有技术相比，本发明的有益效果之一是：本发明通过半预聚法制备MDI基聚氨酯灌封胶，既避免了TDI基聚氨酯灌封胶预聚体中游离NCO挥发所带来的毒性，又改善了MDI基聚氨酯灌封胶的制备工艺；同时该体系以无卤反应型液体阻燃剂与填料协同阻燃，由于阻燃剂分子结合到聚氨酯分子结构中，耐迁移、具有低成雾性及持久的阻燃性能，规避了阻燃剂对灌封胶稳定性及性能的影响。该体系所用原材料安全无毒、成本低廉，配方设计科学合理，操作简单易行。所制得的聚氨酯弹性体适用于中小型电子元件的灌封，且其固化速度可调，可室温或加温固化，储存稳定，具有良好的附着力、耐水性、阻燃性、导热性及电气性能。
具体实施方式
为了使本发明的目的、技术方案及优点更加清楚明白，以下结合实施例，对本发明进行进一步详细说明。应当理解，此处所描述的具体实施例仅仅用以解释本发明，并不用于限定本发明。
实施例1
(1)A组分的制备：将20kg聚丙二醇(MN＝2000)、30kg端羟基聚磷酸酯(羟值为170mgKOH/g)加入到反应器中并于110℃下真空脱水3h，再降温至65℃，加入20kg4,4-二苯基甲烷二异氰酸酯、30kg多亚甲基多苯基多异氰酸酯，并在30min内逐渐升温至80℃反应，反应过程中通氮气保护，并测试NCO％值，在NCO％值达到11％时停止反应，即制得A组分。
(2)B组分的制备：将75kg聚丙二醇(MN＝3000)、22kg蓖麻油(羟值为170mgKOH/g)、3kg1,4-丁二醇、119kg氧化铝加入反应釜中并于115℃下真空搅拌2h，再降温至75℃，加入0.5kg消泡剂、0.01kg催化剂、0.5kg抗氧剂搅拌均匀即制得B组分。
(3)将A、B组分按重量比为20：100的比例称量、搅拌、脱泡后，浇筑于经干燥处理过的电子器件中，再于25℃固化7天。
实施例2
(1)A组分的制备：将20kg聚丙二醇(MN＝2000)、9kg三(一缩二丙二醇)亚磷酸酯(羟值为395mgKOH/g)加入到反应器中并于115℃下真空脱水2h，再降温至70℃，加入50kg液化4,4-二苯基甲烷二异氰酸酯，并在在30min内逐渐升温至85℃反应，反应过程中通氮气保护，并测试NCO％值，在NCO％值达到15％时停止反应，即制得A组分。
(2)B组分的制备：将72kg聚丙二醇(MN＝2000)、17kg蓖麻油(羟值为170mgKOH/g)、1kg丙二醇、50kg氧化铝、59kg氢氧化铝加入反应釜中并于120℃下真空搅拌2h，再降温至80℃，加入0.5kg消泡剂、0.01kg催化剂、0.5kg抗氧剂搅拌均匀即制得B组分。
(3)将A、B组分按重量比为20：100的比例称量、搅拌、脱泡后，浇筑于经干燥处理过的电子器件中，再于60℃固化24h。
实施例3
(1)A组分的制备：将15g聚丙二醇(MN＝2000)、12.5gN,N-二(2-羟乙基)氨甲基膦酸二乙酯(羟值为450mgKOH/g)加入到反应器中并于120℃下真空脱水2h，再降温至60℃，加入35g4,4-二苯基甲烷二异氰酸酯、15g多亚甲基多苯基多异氰酸酯并在30min内逐渐升温至75℃反应，反应过程中通氮气保护，并测试NCO％值，在NCO％值达到15％时停止反应，即制得A组分。
(2)B组分的制备：将39kg端羟基聚丁二烯(羟值为60mgKOH/g)、29kg蓖麻油(羟值为170mgKOH/g)、2kg1,4-丁二醇和129kg氢氧化铝加入反应釜中并于110℃下真空搅拌2h，再降温至60℃，加入0.5kg消泡剂、0.01kg催化剂、0.5kg抗氧剂搅拌均匀即制得B组分。
(3)将A、B组分按重量比为25：100的比例称量、搅拌、脱泡后，浇筑于经干燥处理过的电子器件中，再于25℃固化7天或于60℃固化24h。
实施例4
(1)A组分的制备：将15g聚丙二醇(MN＝2000)、10.5gN,N-二(2-羟乙基)氨甲基膦酸二甲酯(羟值为480mgKOH/g)加入到反应器中并于120℃下真空脱水2h，再降温至65℃，加入40g4,4-二苯基甲烷二异氰酸酯、10g多亚甲基多苯基多异氰酸酯并在30min内逐渐升温至75℃反应，反应过程中通氮气保护，并测试NCO％值，在NCO％值达到14％时停止反应，即制得A组分。
(2)B组分的制备：将17.2kg端羟基聚丁二烯(羟值为60mgKOH/g)、39.7kg聚丙二醇(MN＝2000)、3.1kg三羟甲基丙烷和139kg硅微粉加入反应釜中并于110℃下真空搅拌2h，再降温至50℃，加入0.5kg消泡剂、0.01kg催化剂、0.5kg抗氧剂搅拌均匀即制得B组分。
(3)将A、B组分按重量比为20：100的比例称量、搅拌、脱泡后，浇筑于经干燥处理过的电子器件中，再于25℃固化7天或于60℃固化24h。
上述实施例1～4所得产品的性能如表1所示。
表1各实施例性能对比
从上表可以看出，实施例1～4所制得的聚氨酯弹性体都具有较高的力学性能和导热性能，同时由于本发明无外加增塑剂和非反应型液体阻燃剂，这就使得该发明制备的聚氨酯灌封胶具有较高的阻燃性能和电性能。
尽管这里参照本发明的解释性实施例对本发明进行了描述，但是，应该理解，本领域技术人员可以设计出很多其他的修改和实施方式，这些修改和实施方式将落在本申请公开的原则范围和精神之内。更具体地说，在本申请公开的范围内，可以对主题组合布局的组成部件和/或布局进行多种变型和改进。除了对组成部件和/或布局进行的变型和改进外，对于本领域技术人员来说，其他的用途也将是明显的。

Claims (10)

1.一种MDI基聚氨酯电子灌封胶，其特征在于该电子灌封胶由A、B两种组分组成；其中，A组分由按重量份计的50～60份的异氰酸酯、15～20份的低聚物多元醇和9～30份的反应型液体阻燃剂制成；B组分由按重量份计的55～100份低聚物多元醇、1.0～3.5份交联扩链剂、0.01～0.1份催化剂、105～140份填料、0.5～1份消泡剂和0.5～1份抗氧剂制成。
2.根据权利要求1所述的MDI基聚氨酯电子灌封胶，其特征在于所述异氰酸酯为MDI、碳化二亚胺改性MDI、PAPI中的一种或任意几种的混合物。
3.根据权利要求1所述的MDI基聚氨酯电子灌封胶，其特征在于A、B组分中所述低聚物多元醇为羟基官能度≥2、分子量为600～5000的端羟基聚丁二烯、聚环氧丙烯多元醇、蓖麻油多元醇中的一种或任意几种的混合物。
4.根据权利要求1所述的MDI基聚氨酯电子灌封胶，其特征在于所述反应型液体阻燃剂是羟基官能度为1～2的磷酸酯类阻燃剂；所述填料为氧化铝、氢氧化铝或硅微粉，填料的平均粒径在1～50um的范围内。
5.根据权利要求4所述的MDI基聚氨酯电子灌封胶，其特征在于所述反应型液体阻燃剂为三(一缩二丙二醇)亚磷酸酯、N,N-二(2-羟基乙基)氨甲基膦酸二乙酯、N,N-二(2-羟乙基)氨甲基膦酸二甲酯、端羟基聚磷酸酯。
6.根据权利要求1所述的MDI基聚氨酯电子灌封胶，其特征在于所述交联扩链剂为丙二醇、1,4-丁二醇或三羟甲基丙烷。
7.根据权利要求1所述的MDI基聚氨酯电子灌封胶，其特征在于所述催化剂为三乙胺、三亚乙基二胺、二月桂酸二丁基锡、辛酸亚锡、异辛酸锌或异辛酸铅。
8.根据权利要求1所述的MDI基聚氨酯电子灌封胶，其特征在于所述消泡剂为改性硅氧烷、丙烯酸酯共聚物或非硅酮高分子聚合物；所述抗氧剂为2,6-二叔丁基-4-甲基苯酚、亚磷酸三(壬基苯酯)或酚噻嗪。
9.如权利要求1～8任意一项所述的MDI基聚氨酯电子灌封胶的制备方法，其特征在于它采用半预聚法，包括以下步骤：
A组分的制备
按比例称取A组分原料，将低聚物多元醇和反应型液体阻燃剂于110～120℃下真空脱水2～3h，再降温至60～70℃，加入异氰酸酯并在30min内逐渐升温至75～85℃反应，反应过程中通氮气保护，并测试NCO％值，在NCO％值达到设定值时，停止反应即得A组分；所述设定值在10％～15％范围内；
B组分的制备
按比例称取B组分原料，将低聚物多元醇、交联扩链剂、填料加入反应釜中并于110～120℃下真空搅拌2h，再降温至50～80℃，加入消泡剂、催化剂和抗氧剂，搅拌均匀即得B组分。
10.如权利要求1～8任意一项所述的MDI基聚氨酯电子灌封胶的应用方法，其特征在于所述A组分和B组分按照质量比20～25:100混合后搅拌、脱泡，浇注于经干燥处理过的电子器件中，再于25℃固化7天或者于60℃固化24h，即完成电子器件的灌封。
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CN114686154B (zh) * 2022-03-01 2023-09-26 深圳镝普材料科技有限公司 一种热至相变阻尼灌封胶粘剂及其制备方法
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CN115521752A (zh) * 2022-11-09 2022-12-27 江苏博韵低维材料科技有限公司 一种高导热灌封胶及其制备方法
CN116554825A (zh) * 2023-07-12 2023-08-08 山东理工大学 耐候丙烯酸酯聚氨酯灌封胶及其制备方法
CN116554825B (zh) * 2023-07-12 2023-10-20 山东理工大学 耐候丙烯酸酯聚氨酯灌封胶及其制备方法

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