CN116218461B - 一种密封防水的单组份硅胶及其制备方法 - Google Patents
一种密封防水的单组份硅胶及其制备方法 Download PDFInfo
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Abstract
本发明涉及一种密封防水的单组份硅胶,包括以下质量份的原料:40‑60份α,ω‑二羟基聚二甲基硅氧烷,10‑15份端羟基含氟聚硅氧烷,5‑10份增粘树脂,5‑10份甲基硅油,1‑2份长链氟硅氧烷,10‑20份纳米碳酸钙,1‑5份着色剂,1‑5份气相二氧化硅,3‑5份交联剂,4‑6份偶联剂,0.1‑0.5份有机锡催化剂,0.1‑0.5份流平剂;所述交联剂为酮肟硅烷交联剂和聚乙二醇改性交联剂按照质量比4‑7:1的混合物。本发明制备得到的单组份硅胶具有适中的表干时间,固化程度深,粘接强度高,能够经受2次以上的回流焊测试,并且具有很好的防水耐高温性能,经受双85测试500h后,仍保持了很好的粘接强度。
Description
技术领域
本发明属于密封胶技术领域,具体涉及一种密封防水的单组份硅胶及其制备方法。
背景技术
随着科技水平的迅猛发展,国民经济的提升,手机成为了人们常用的生活、工作工具。手机成为了人们不可或缺的工具。目前,由于手机使用越来越普遍,人们对手机防水的要求越来越高,比如Type-C等作为手机充电的接口,对防水要求格外重要。
现有技术中对于Type-C接口的密封胶黏剂多为环氧类,比如CN113913139A公开了一种用于用于Type-C接口的防水耐高温单组分环氧胶粘剂,包括耐高温树脂,改性环氧树脂,改性固化剂,改性胺促进剂等。CN115141588A公开了一种Type C密封的环氧树脂胶粘剂,包括10-20份环氧树脂,5-20份脂环组环氧树脂,5-20份增韧树脂,30-60填料,0.1-5份触变剂,0.1-1份偶联剂,0.1-5份热引发剂。但是环氧树脂固化存在收缩率不一致的情况,是密封胶固化后具有较大的内应力,容易造成产品内部的缺陷损伤导致强度不足,或者外观的缺陷,而且环氧树脂类密封胶黏剂韧性不足,不能起到对电子元器件类精细结构的保护。
有机硅胶作为密封材料,目前的缺陷主要是现有的硅胶对基材粘接不佳,容易剥离;无法耐受两次以上的高温260℃回流焊,而且防水性能不足。目前硅胶应用市场很大,应用范围很广,但是主要的用量在于建筑和工业,应用于电子行业的硅胶较少。特别对于应用于Type-C接口密封防水的单组份硅胶要求很高,不仅要拥有很好的性能,还要满足现在各种环保要求,导致国内此类应用产品很少。现在市面上此类产品主要来源于美国道康宁和日本信越,他们在有机硅方面发展历史较长,拥有领先的硅胶技术,是硅胶行业的领导者。但是此类产品全靠进口,成本较高,而且受全球疫情影响,现在很容易导致断货。影响手机企业的生产。本发明提供了一种密封防水的单组份硅胶,具体是一种脱酮肟型有机硅胶黏剂及其制备方法,用于Type-C等接口密封防水粘接,能够替代进口产品,而且符合环保要求。本专利发明了一种单组分脱酮肟型有机硅胶黏剂及其制备方法,用于手机等电子元器件的密封防水粘接,比如Type-C接口。
发明内容
为了解决现有技术中有机硅胶固化时间长,固化后机械强度不足,不能耐受两次以上高温回流焊,防水性能不足的缺陷,本发明提出了一种密封防水的单组份硅胶,通过含有柔软聚醚段的交联剂,实现了表干时间适中,粘接强度高。
本发明通过以下技术方案实现上述目的:
一种密封防水的单组份硅胶,包括以下质量份的原料:40-60份α,ω-二羟基聚二甲基硅氧烷,10-15份端羟基含氟聚硅氧烷,5-10份增粘树脂,5-10份甲基硅油,1-2份长链氟硅氧烷,10-20份纳米碳酸钙,1-5份着色剂,1-5份气相二氧化硅,3-5份交联剂,4-6份偶联剂,0.1-0.5份有机锡催化剂,0.1-0.5份流平剂;所述交联剂为酮肟硅烷交联剂和聚乙二醇改性交联剂按照质量比4-7:1的混合物;
所述聚乙二醇改性交联剂通过包括以下步骤的制备方法得到:
(S1)乙烯基三氯硅烷和二巯基聚乙二醇(SH-PEG-SH)反应,得到中间产物I;
(S2)中间产物I和酮肟化试剂反应,得到聚乙二醇改性交联剂,所述酮肟化试剂为R1R2C=NOH,R1、R2独立选自苯基、C1-6的烷基。
本发明的聚乙二醇改性交联剂合成路线如下:
其中,表示聚乙二醇链段(PEG)。
进一步地,步骤(S1)中,二巯基聚乙二醇和乙烯基三氯硅烷的摩尔比为1.05-1.1:2,巯基相比于烯基稍过量;反应条件是在氮气或者惰性气氛,在催化剂或引发剂存在下,室温反应3-5h。所述催化剂为有机胺,具体选自三乙胺,吡啶中的至少一种,有机胺用量为乙烯基三氯硅烷质量的3-5wt%;引发剂选自AIBN,安息香双甲醚中至少一种,引发剂用量为乙烯基三氯硅烷质量的1-2wt%。步骤(S1)是典型的烯基-巯基点击化学反应,只需要少量的弱碱性催化剂,一般为有机胺存在下,室温即可反应。也可以在引发剂存在下反应,比如AIBN,安息香双甲醚。反应溶剂为无水甲醇、无水乙醇中的至少一种。
进一步地,步骤(S1)中,二巯基聚乙二醇的数均分子量为200-400g/mol,其中聚乙二醇链段具有一定的柔性,显著增加了有机硅胶固化后的韧性,但是聚乙二醇链段不能太长,否则降低交联密度,对材料的力学强度和粘接强度有一定不利影响。
进一步地,步骤(S2)中,所述酮肟化试剂选自丙酮肟、丁酮肟、戊酮肟、甲基异丁基酮肟中的至少一种;酮肟化试剂物质的量是中间产物I物质的量的15-20倍,在步骤(S2)中,酮肟化试剂作为反应原料和中间产物I进行反应,同时还作为反应的缚酸剂,因此酮肟化试剂需要过量,一般为中间产物I物质的量的15倍以上,但是不要超过20倍,否则造成原料的浪费,反应的效率和收率并不会进一步增加。
进一步地,步骤(S2)的反应条件是氮气或者惰性气氛下,室温下反应,反应时间4-6h,反应溶剂为正己烷,甲苯,二氯乙烷,醋酸乙酯中的至少一种。反应结束后,静置分层,分出下层粘稠液体(产生的酮肟盐酸盐),中和,过滤,滤液减压蒸馏,得到产物,即为聚乙二醇改性交联剂。
进一步地,所述酮肟硅烷交联剂选自甲基三丙酮肟基硅烷、甲基三丁酮肟基硅烷、苯基三丁酮肟基硅烷、四丁酮肟基硅烷、甲基三(甲基异丁酮肟基)硅烷、四(甲基异丁酮肟基)硅烷中的至少一种。本发明以自制的带有聚乙二醇链段改性的酮肟基硅烷交联剂和常规的小分子酮肟基硅烷交联剂一起复配使用,深层固化程度明显提高,显著提高对ABS和不锈钢基材的粘接强度,密封胶固化后的韧性好,粘接强度高,过三次回流焊不开裂;并且表干时间适中,粘度和触变较低,容易点胶。
进一步地,所述α,ω-二羟基聚二甲基硅氧烷的粘度为2000-20000mPa·s,优选为粘度为5000-7000mPa·s的α,ω-二羟基聚二甲基硅氧烷和粘度为10000-15000mPa·s的α,ω-二羟基聚二甲基硅氧烷按照质量比5-7:1的混合物。本发明一个优选技术方案中,选择低粘度和高粘度的α,ω-二羟基聚二甲基硅氧烷复配,表干时间适中,所得有机硅密封胶固化后的硬度,固化深度都较好,达到最优的粘接效果。
所述端羟基含氟聚硅氧烷的粘度为1000-2000mPa·s;所述长链氟硅氧烷为F109。本发明通过加入含氟树脂,端羟基含氟聚硅氧烷和小分子的长链氟硅氧烷F109搭配使用,显著改善了材料固化后的疏水性,使得有机硅密封胶的防水性能进一步提高。
所述增粘树脂为江西海多化工有限公司的MC751,MC750中的至少一种。
所述甲基硅油为粘度为100-2000mPa·s,优选500-1000 100-2000mPa·s;比如选自浙江润禾有机硅新材料有限公司低环体甲基硅油RH-510-100,RH-510-500,RH-510-1000,RH-510-2000中的至少一种。
所述纳米碳酸钙为欧米亚公司纳米碳酸钙Omyacarb 1T–JI,Omyacarb 1T–CU中的至少一种。
所述着色剂为日本三菱炭黑MA100,卡博特M800特种炭黑,韩国欧励隆炭黑HIBLACK 50L中的至少一种。
所述的流平剂为德国毕克BYK-300,BYK-307,BYK-370中的至少一种。
所述偶联剂为氨基硅烷偶联剂和环氧基硅烷偶联剂按照质量比2.5-3.4:1的复配,所述氨基硅烷偶联剂选自γ-氨丙基三甲氧基硅烷(KH-540),γ-氨丙基三乙氧基硅烷(KH-550),N-2-氨乙基-3-氨丙基三甲氧基硅烷(KH-792)中的至少一种,所述环氧基硅烷偶联剂选自3-缩水甘油醚氧基丙基三甲氧基硅烷(KH-560),3-(2,3-环氧丙氧)丙基三乙氧基硅烷(KH-561),3-(2,3-环氧丙氧)丙基甲基二甲氧基硅烷(KH-562)中的至少一种。复配的硅烷偶联剂使得表干时间适中,增强粘结强度和耐高温性能。
所述催化剂为有机锡催化剂,比如二月桂酸二丁基锡、二月桂酸二辛基锡、二辛葵酸二甲基锡和二醋酸二丁基锡中的至少一种。
本发明还提供了所述密封防水的单组份硅胶的制备方法,包括以下步骤:
(T1)将α,ω-二羟基聚二甲基硅氧烷,端羟基含氟聚硅氧烷,长链氟硅氧烷,气相二氧化硅,纳米碳酸钙,着色剂加入搅拌釜中,室温下搅拌至分散均匀;升温至110-140℃,抽真空进行脱水;
(T2)物料冷却至室温后,加入增粘树脂,甲基硅油,继续搅拌至混合均匀;
(T3)加入交联剂,偶联剂,流平剂,催化剂,抽真空,搅拌脱泡,得到密封防水的单组份硅胶。
进一步地,步骤(T1)至(T3)中搅拌釜为双行星搅拌釜,公转25-40Hz。抽真空使体系压力为0.01-0.1MPa。
具体实施方式
为使本发明的目的、技术方案和优点更加清楚,下面将对本发明的技术方案进行详细的描述。以下的实施例便于更好地理解本发明,但并不限定本发明。下述实施例中的实验方法,如无特殊说明,均为常规方法。
本发明实施例中所述“份”若无特别说明,均为质量份,所述“%”若无特别说明,均为质量百分比。
α,ω-二羟基聚二甲基硅氧烷(107硅树脂)采购自浙江润禾有机硅新材料有限公司,粘度分别为2000mPa·s(RH-107-2000D),5000mPa·s(RH-107-5000D),7000mPa·s(RH-107-7000D),10000mPa·s(RH-107-10000D),15000mPa·s(RH-107-15000D),20000mPa·s(RH-107-20000D)。
二巯基聚乙二醇(SH-PEG-SH)采购自魅罗科技,数均分子量分别为200,400,600,分别称为SH-PEG200-SH,SH-PEG400-SH,SH-PEG600-SH。
端羟基含氟聚硅氧烷采购自东莞晟邦,粘度1000mPa·s。
制备例1
(S1);氮气气氛下,1.1摩尔份的SH-PEG200-SH加入到4质量倍的无水甲醇中,加入2摩尔份的乙烯基三氯硅烷和引发剂安息香双甲醚(加入量是乙烯基三氯硅烷的2wt%),室温下搅拌反应4h,旋蒸除去溶剂,真空干燥得到黄色粘稠液体,为中间产物I;
(S2);氮气气氛下,取1摩尔份中间产物I,加入到正己烷溶剂中,加入15摩尔份的丁酮肟,室温下反应6h,转移至分液漏斗,静置分层,分出下层粘稠液体(为产生的酮肟盐酸盐),用三乙胺中和至中性,抽滤,滤液经过减压蒸馏回收未反应的丁酮肟和溶剂,得到粘稠状液体,为产物聚乙二醇改性交联剂。
制备例2
其他条件和制备例1相同,区别在于步骤(S1)中,SH-PEG200-SH替换为等摩尔量的SH-PEG400-SH。
制备例3
其他条件和制备例1相同,区别在于步骤(S1)中,SH-PEG200-SH替换为等摩尔量的SH-PEG600-SH。
实施例1
(T1)将50份RH-107-5000D,10份RH-107-15000D,15份端羟基含氟聚硅氧烷,2份长链氟硅氧烷F109,4.5份气相二氧化硅LM150,15份纳米碳酸钙Omyacarb 1T–CU,2份着色剂炭黑M800加入搅拌釜中,室温下搅拌至分散均匀;升温至120℃,抽真空进行脱水;
(T2)物料冷却至室温后,加入6份增粘树脂MC751,8份甲基硅油RH-510-500,继续搅拌至混合均匀;
(T3)加入4份甲基三丁酮肟基硅烷,1份制备例1制得的聚乙二醇改性交联剂,5份偶联剂(KH-540和KH-560按照质量比3:1的复配),0.3份流平剂BYK-370,0.25份催化剂二月桂酸二丁基锡,抽真空至0.01Mpa,搅拌脱泡,得到密封防水的单组份硅胶。
实施例2
(T1)将35份RH-107-5000D,5份RH-107-10000D,15份端羟基含氟聚硅氧烷,1份长链氟硅氧烷F109,3.7份气相二氧化硅R8200,10份纳米碳酸钙Omyacarb 1T–CU,2份着色剂炭黑MA800加入搅拌釜中,室温下搅拌至分散均匀;升温至130℃,抽真空进行脱水;
(T2)物料冷却至室温后,加入5份增粘树脂MC750,8.5份甲基硅油RH-510-1000,继续搅拌至混合均匀;
(T3)加入2.4份甲基三丙酮肟基硅烷,0.6份制备例1制得的聚乙二醇改性交联剂,4份偶联剂(KH-550和KH-561按照质量比2.5:1的复配),0.3份流平剂BYK-370,0.2份催化剂二月桂酸二丁基锡,抽真空至0.01Mpa,搅拌脱泡,得到密封防水的单组份硅胶。
实施例3
(T1)将52.5份RH-107-7000D,7.5份RH-107-15000D,12份端羟基含氟聚硅氧烷,1份长链氟硅氧烷F109,5份气相二氧化硅LM150,20份纳米碳酸钙Omyacarb 1T–CU,3份着色剂炭黑MA800加入搅拌釜中,室温下搅拌至分散均匀;升温至130℃,抽真空进行脱水;
(T2)物料冷却至室温后,加入10份增粘树脂MC750,10份甲基硅油RH-510-1000,继续搅拌至混合均匀;
(T3)加入4.375份甲基三丁酮肟基硅烷,0.625份制备例1制得的聚乙二醇改性交联剂,6份偶联剂(KH-550和KH-561按照质量比3.4:1的复配),0.3份流平剂BYK-370,0.3份催化剂二月桂酸二丁基锡,抽真空至0.01Mpa,搅拌脱泡,得到密封防水的单组份硅胶。
实施例4
其他条件与操作和实施例1相同,区别在于聚乙二醇改性交联剂替换为等质量的制备例2制得的聚乙二醇改性交联剂。
实施例5
其他条件与操作和实施例1相同,区别在于聚乙二醇改性交联剂替换为等质量的制备例3制得的聚乙二醇改性交联剂。
实施例6
其他条件与操作和实施例1相同,区别在于RH-107-5000D替换为等质量的RH-107-2000D,RH-107-15000D替换为等质量的RH-107-20000D。
实施例7
其他条件与操作和实施例1相同,区别在于α,ω-二羟基聚二甲基硅氧烷全部为60份RH-107-5000D,即不加入RH-107-15000D。
实施例8
其他条件与操作和实施例1相同,区别在于α,ω-二羟基聚二甲基硅氧烷全部为60份RH-107-15000D,即不加入RH-107-5000D。
实施例9
其他条件与操作和实施例1相同,区别在于偶联剂为5份KH-540。
实施例10
其他条件与操作和实施例1相同,区别在于偶联剂为5份KH-560
实施例11
其他条件与操作和实施例1相同,区别在于交联剂为2.5份甲基三丁酮肟基硅烷,2.5份制备例1制得的聚乙二醇改性交联剂
对比例1
其他条件与操作和实施例1相同,区别在于交联剂为5份甲基三丁酮肟基硅烷,即不加入聚乙二醇改性交联剂。
效果例
对上述实施例和对比例制得有机硅密封胶进行如下性能测试,结果如表1所示:
表干时间测试:温度25±1℃,湿度50±3%按照GB/T 13477.5-2002进行测定。
固化深度:按照JB/T10900—2008标准进行测试
剪切强度:美特斯工业系统(中国)有限公司微机控制电子万能试验按照GB 7124-86进行测定。测试基材为PA/SUS,PA为尼龙,SUS为不锈钢。
回流焊测试:宝迪自动化设备有限公司BT301N小型桌面式抽屉式回流焊炉按照IPC-TM-650 2.6.27标准进行测定,测试条件室温固化24h,260℃,10min,进行三次回流焊。括号次数是在第几次回流焊测试开裂,(-)表示3次都没有开裂,(3)表示第三次开裂,(2)表示第2次开裂,(1)表示第一次开裂
表1有机硅密封胶性能测试结果
注:CF为内聚破坏,AF为界面破坏
通过表1可知,本发明制备得到的单组份硅胶具有适中的表干时间,固化程度深,粘接强度高,能够经受2次以上的回流焊测试,并且具有很好的防水耐高温性能,经受双85测试500h后,仍保持了很好的粘接强度,是一种综合性能优异的单组份硅胶。
Claims (10)
1.一种密封防水的单组份硅胶,其特征在于,包括以下质量份的原料:40-60份α,ω-二羟基聚二甲基硅氧烷,10-15份端羟基含氟聚硅氧烷,5-10份增粘树脂,5-10份甲基硅油,1-2份长链氟硅氧烷F109,10-20份纳米碳酸钙,1-5份着色剂,1-5份气相二氧化硅,3-5份交联剂,4-6份偶联剂,0.1-0.5份有机锡催化剂,0.1-0.5份流平剂;所述交联剂为酮肟硅烷交联剂和聚乙二醇改性交联剂按照质量比4-7:1的混合物;所述α,ω-二羟基聚二甲基硅氧烷为粘度5000-7000mPa·s的α,ω-二羟基聚二甲基硅氧烷和粘度为10000-15000 mPa·s的α,ω-二羟基聚二甲基硅氧烷按照质量比5-7:1的混合物;所述偶联剂为氨基硅烷偶联剂和环氧基硅烷偶联剂按照质量比2.5-3.4:1的复配;
所述聚乙二醇改性交联剂通过包括以下步骤的制备方法得到:
(S1)乙烯基三氯硅烷和二巯基聚乙二醇反应,得到中间产物I;二巯基聚乙二醇和乙烯基三氯硅烷的摩尔比为1.05-1.1:2;二巯基聚乙二醇的数均分子量为200-400 g/mol;
(S2)中间产物I和酮肟化试剂反应,得到聚乙二醇改性交联剂,所述酮肟化试剂为R1R2C=NOH,R1、R2独立选自苯基、C1-6的烷基;酮肟化试剂选自丙酮肟、丁酮肟、戊酮肟、甲基异丁基酮肟中的至少一种,酮肟化试剂物质的量是中间产物I物质的量的15-20倍。
2.根据权利要求1所述的密封防水的单组份硅胶,其特征在于,步骤(S1)中,反应条件是在氮气或者惰性气氛,在催化剂或引发剂存在下,室温反应3-5h,步骤(S1)中所述催化剂为有机胺,有机胺用量为乙烯基三氯硅烷质量的3-5 wt%;引发剂选自AIBN,安息香双甲醚中至少一种,引发剂用量为乙烯基三氯硅烷质量的1-2 wt%。
3.根据权利要求2所述的密封防水的单组份硅胶,其特征在于,所述有机胺选自三乙胺,吡啶中的至少一种。
4.根据权利要求1所述的密封防水的单组份硅胶,其特征在于,步骤(S2)中,反应条件是氮气或者惰性气氛下,室温下反应,反应时间4-6h,反应溶剂为正己烷,甲苯,二氯乙烷,醋酸乙酯中的至少一种,反应结束后,静置分层,分出下层粘稠液体,中和,过滤,滤液减压蒸馏,得到产物,即为聚乙二醇改性交联剂。
5.根据权利要求1所述的密封防水的单组份硅胶,其特征在于,所述酮肟硅烷交联剂选自甲基三丙酮肟基硅烷、甲基三丁酮肟基硅烷、苯基三丁酮肟基硅烷、四丁酮肟基硅烷、甲基三(甲基异丁酮肟基)硅烷、四(甲基异丁酮肟基)硅烷中的至少一种。
6.根据权利要求1所述的密封防水的单组份硅胶,其特征在于,所述端羟基含氟聚硅氧烷的粘度为1000-2000 mPa·s。
7.根据权利要求1所述的密封防水的单组份硅胶,其特征在于,所述增粘树脂为江西海多化工有限公司的MC751,MC750中的至少一种;和/或
所述甲基硅油的粘度为100-2000 mPa·s;和/或
所述纳米碳酸钙为欧米亚公司的纳米碳酸钙Omyacarb 1T – JI,Omyacarb 1T – CU中的至少一种;和/或
所述着色剂为日本三菱炭黑MA100,卡博特M800特种炭黑,韩国欧励隆炭黑HIBLACK50L中的至少一种;和/或
所述的流平剂为德国毕克BYK-300,BYK-307,BYK-370中的至少一种;和/或
所述有机锡催化剂为二月桂酸二丁基锡、二月桂酸二辛基锡、二辛癸酸二甲基锡和二醋酸二丁基锡中的至少一种。
8.根据权利要求7所述的密封防水的单组份硅胶,其特征在于,所述甲基硅油的粘度500-1000 mPa·s。
9.根据权利要求1所述的密封防水的单组份硅胶,其特征在于,所述氨基硅烷偶联剂选自γ-氨丙基三甲氧基硅烷,γ-氨丙基三乙氧基硅烷,N-2-氨乙基-3-氨丙基三甲氧基硅烷中的至少一种,所述环氧基硅烷偶联剂选自3-缩水甘油醚氧基丙基三甲氧基硅烷,3-(2,3-环氧丙氧)丙基三乙氧基硅烷,3-(2,3-环氧丙氧)丙基甲基二甲氧基硅烷中的至少一种。
10.权利要求1-9任一项所述密封防水的单组份硅胶的制备方法,其特征在于,包括以下步骤:
(T1)将α,ω-二羟基聚二甲基硅氧烷,端羟基含氟聚硅氧烷,长链氟硅氧烷,气相二氧化硅,纳米碳酸钙,着色剂加入搅拌釜中,室温下搅拌至分散均匀;升温至110-140℃,抽真空进行脱水;
(T2)物料冷却至室温后,加入增粘树脂,甲基硅油,继续搅拌至混合均匀;
(T3)加入交联剂,偶联剂,流平剂,有机锡催化剂,抽真空,搅拌脱泡,得到密封防水的单组份硅胶。
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