CN116355543A - 一种橡胶型锂电池压敏胶粘带 - Google Patents
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Abstract
本发明公开了一种橡胶型锂电池压敏胶粘带,制备方法为:(1)制备交联剂A;(2)制备交联剂B;(3)将天然橡胶在开炼机中塑炼,塑炼后切碎溶解在甲苯中,然后加入所述交联剂A、交联剂B和防老剂,搅拌均匀,加入甲苯调节黏度后涂布在PET薄膜上,130℃烘烤,获得所述橡胶型锂电池压敏胶粘带。本发明所述方法以天然橡胶为主要弹性体,通过添加本发明自制的交联剂,制备的胶粘带具有较高的剥离强度和耐高温性。
Description
技术领域
本发明涉及压敏胶材料技术领域,特别涉及一种橡胶型锂电池压敏胶粘带。
背景技术
锂电池压敏胶粘带主要应用于锂电池生产过程中电池极耳绝缘保护、电芯外部的正负极引线及电路的绝缘保护及封装固定、电芯终止端的绝缘固定及防止电解液的渗漏等,因此需要胶粘带具有适宜的粘性以及能够在极端锂电池电解液环境中保持性能稳定。目前,国内锂电池压敏胶粘带市场仍以聚丙烯酸酯类胶粘带为主,但由于其性能无法满足锂电池对胶粘带日益提高的性能要求,还具有一定的短板。天然橡胶的高粘弹性和低极性的特点能够使压敏胶性能受到锂电池电解液影响较小,在电解液中保持优异的性能,因此橡胶型将是锂电池压敏胶应用研究的一大热点。
发明内容
为此,本发明提供了一种橡胶型锂电池压敏胶粘带,其制备方法为:
(1)将聚碳酸酯二醇和N-甲基吡咯烷酮混合形成混合物,搅拌所述混合物,在搅拌状态下向混合物中加入环氧氯丙烷,加料完成后水浴恒温至50±3℃,到温后向混合物中加入三氟化硼乙醚,加料后保温120~150min,保温结束后再向混合物中加入氢氧化钠溶液,继续50±3℃水浴保温120~150min,然后空冷至常温,加乙酸乙酯萃取,去除水相,然后旋蒸去除乙酸乙酯,获得交联剂A;
(2)将甲苯二异氰酸酯三聚体和丙酮混合形成混合液,向所述混合液中加入聚乙二醇单甲醚,加料完成后水浴恒温至60±3℃,保温冷凝回流2h以上,然后向混合液中加入甲基乙基酮肟,加料完成后继续60±3℃水浴恒温,搅拌保温冷凝回流3h以上,然后混合液空冷至常温,旋蒸去除丙酮;再向混合液中滴加3-氨丙基三乙氧基硅烷,加料完成后水浴恒温至50±3℃,保温40min以上,然后再向混合液中依次加入N,N-二甲基乙醇胺和1,3-丙烷磺酸内酯,加料完成后50±3℃温度范围内搅拌保温60min以上,然后再向混合物中加入对甲氧基苯酚,获得交联剂B;
(3)将天然橡胶在开炼机中塑炼,塑炼后切碎溶解在甲苯中,然后加入所述交联剂A、交联剂B和防老剂,搅拌均匀,加入甲苯调节黏度后涂布在PET薄膜上,130℃烘烤,获得所述橡胶型锂电池压敏胶粘带。
进一步地,所述聚碳酸酯二醇和N-甲基吡咯烷酮混合量比为聚碳酸酯二醇:N-甲基吡咯烷酮=4~6g/100mL;所述环氧氯丙烷、三氟化硼乙醚加入质量与所述聚碳酸酯二醇的质量比为环氧氯丙烷:三氟化硼乙醚:聚碳酸酯二醇=10~14g:0.05~0.06g:4~6g。
进一步地,所述氢氧化钠溶液的浓度为40~50g/L,溶剂为水;所述氢氧化钠溶液的加入量与所述聚碳酸酯二醇的质量比为氢氧化钠溶液:聚碳酸酯二醇=50mL:4~6g。
进一步地,所述甲苯二异氰酸酯三聚体和丙酮混合质量比为甲苯二异氰酸酯三聚体:丙酮=8~10:150;所述聚乙二醇单甲醚、甲基乙基酮肟加入质量与所述甲苯二异氰酸酯三聚体的质量比为聚乙二醇单甲醚:甲基乙基酮肟:甲苯二异氰酸酯三聚体=4~6:0.8~1.2:8~10。
进一步地,向混合液中滴加3-氨丙基三乙氧基硅烷的质量比为3-氨丙基三乙氧基硅烷:混合液=6~9:50;所述N,N-二甲基乙醇胺、1,3-丙烷磺酸内酯和对甲氧基苯酚加入质量与所述3-氨丙基三乙氧基硅烷的质量比为N,N-二甲基乙醇胺:1,3-丙烷磺酸内酯:对甲氧基苯酚:3-氨丙基三乙氧基硅烷=0.15~0.25:0.3~0.4:0.03~0.06:6~9。
进一步地,涂布液中,所述塑炼后切碎的橡胶、交联剂A、交联剂B和防老剂按重量份数计为橡胶100份,交联剂A1~2份,交联剂B 0.2~0.4份,防老剂3~5份。
本发明的有益效果在于:本发明所述方法以天然橡胶为主要弹性体,通过添加本发明自制的交联剂,制备的胶粘带具有较高的剥离强度和耐高温性,优化了橡胶型锂电池压敏胶粘带的综合性能。
具体实施方式
下面结合实施例对本发明做进一步的说明。
实施例1
一种橡胶型锂电池压敏胶粘带,其制备方法为:
(1)将聚碳酸酯二醇和N-甲基吡咯烷酮混合形成混合物,所述聚碳酸酯二醇和N-甲基吡咯烷酮混合量比为聚碳酸酯二醇:N-甲基吡咯烷酮=4g/100mL;搅拌所述混合物,在搅拌状态下向混合物中加入环氧氯丙烷,加料完成后水浴恒温至50±3℃,到温后向混合物中加入三氟化硼乙醚,加料后保温120min,保温结束后再向混合物中加入氢氧化钠溶液,所述氢氧化钠溶液的浓度为40g/L,溶剂为水;所述氢氧化钠溶液的加入量与所述聚碳酸酯二醇的质量比为氢氧化钠溶液:聚碳酸酯二醇=50mL:4g;继续50±3℃水浴保温120min,然后空冷至常温,加乙酸乙酯萃取,去除水相,然后旋蒸去除乙酸乙酯,获得交联剂A;其中所述环氧氯丙烷、三氟化硼乙醚加入质量与所述聚碳酸酯二醇的质量比为环氧氯丙烷:三氟化硼乙醚:聚碳酸酯二醇=10g:0.05g:4g;
(2)将甲苯二异氰酸酯三聚体和丙酮混合形成混合液,混合液中所述甲苯二异氰酸酯三聚体和丙酮混合质量比为甲苯二异氰酸酯三聚体:丙酮=8:150;向所述混合液中加入聚乙二醇单甲醚,加料完成后水浴恒温至60±3℃,保温冷凝回流2h,然后向混合液中加入甲基乙基酮肟,其中所述聚乙二醇单甲醚、甲基乙基酮肟加入质量与所述甲苯二异氰酸酯三聚体的质量比为聚乙二醇单甲醚:甲基乙基酮肟:甲苯二异氰酸酯三聚体=4:0.8:8;加料完成后继续60±3℃水浴恒温,搅拌保温冷凝回流3h,然后混合液空冷至常温,旋蒸去除丙酮;再向混合液中滴加3-氨丙基三乙氧基硅烷,向混合液中滴加3-氨丙基三乙氧基硅烷的质量比为3-氨丙基三乙氧基硅烷:混合液=6:50;加料完成后水浴恒温至50±3℃,保温40min,然后再向混合液中依次加入N,N-二甲基乙醇胺和1,3-丙烷磺酸内酯,加料完成后50±3℃温度范围内搅拌保温60min,然后再向混合物中加入对甲氧基苯酚,获得交联剂B;其中所述N,N-二甲基乙醇胺、1,3-丙烷磺酸内酯和对甲氧基苯酚加入质量与所述3-氨丙基三乙氧基硅烷的质量比为N,N-二甲基乙醇胺:1,3-丙烷磺酸内酯:对甲氧基苯酚:3-氨丙基三乙氧基硅烷=0.15:0.3:0.03:6;
(3)将天然橡胶在开炼机中塑炼,塑炼后切碎溶解在甲苯中,然后加入所述交联剂A、交联剂B和防老剂,搅拌均匀,加入甲苯调节黏度后涂布在PET薄膜上,涂布液中所述塑炼后切碎的橡胶、交联剂A、交联剂B和防老剂按重量份数计为橡胶100份,交联剂A1份,交联剂B 0.4份,防老剂(KY-405)3份;涂布后130℃烘烤2min,获得所述橡胶型锂电池压敏胶粘带(干胶厚度10μm)。
实施例2
一种橡胶型锂电池压敏胶粘带,其制备方法为:
(1)将聚碳酸酯二醇和N-甲基吡咯烷酮混合形成混合物,所述聚碳酸酯二醇和N-甲基吡咯烷酮混合量比为聚碳酸酯二醇:N-甲基吡咯烷酮=5g/100mL;搅拌所述混合物,在搅拌状态下向混合物中加入环氧氯丙烷,加料完成后水浴恒温至50±3℃,到温后向混合物中加入三氟化硼乙醚,加料后保温120min,保温结束后再向混合物中加入氢氧化钠溶液,所述氢氧化钠溶液的浓度为40g/L,溶剂为水;所述氢氧化钠溶液的加入量与所述聚碳酸酯二醇的质量比为氢氧化钠溶液:聚碳酸酯二醇=50mL:5g;继续50±3℃水浴保温120min,然后空冷至常温,加乙酸乙酯萃取,去除水相,然后旋蒸去除乙酸乙酯,获得交联剂A;其中所述环氧氯丙烷、三氟化硼乙醚加入质量与所述聚碳酸酯二醇的质量比为环氧氯丙烷:三氟化硼乙醚:聚碳酸酯二醇=12g:0.05g:5g;
(2)将甲苯二异氰酸酯三聚体和丙酮混合形成混合液,混合液中所述甲苯二异氰酸酯三聚体和丙酮混合质量比为甲苯二异氰酸酯三聚体:丙酮=9:150;向所述混合液中加入聚乙二醇单甲醚,加料完成后水浴恒温至60±3℃,保温冷凝回流2h,然后向混合液中加入甲基乙基酮肟,其中所述聚乙二醇单甲醚、甲基乙基酮肟加入质量与所述甲苯二异氰酸酯三聚体的质量比为聚乙二醇单甲醚:甲基乙基酮肟:甲苯二异氰酸酯三聚体=5:1:9;加料完成后继续60±3℃水浴恒温,搅拌保温冷凝回流3h,然后混合液空冷至常温,旋蒸去除丙酮;再向混合液中滴加3-氨丙基三乙氧基硅烷,向混合液中滴加3-氨丙基三乙氧基硅烷的质量比为3-氨丙基三乙氧基硅烷:混合液=7:50;加料完成后水浴恒温至50±3℃,保温40min,然后再向混合液中依次加入N,N-二甲基乙醇胺和1,3-丙烷磺酸内酯,加料完成后50±3℃温度范围内搅拌保温60min,然后再向混合物中加入对甲氧基苯酚,获得交联剂B;其中所述N,N-二甲基乙醇胺、1,3-丙烷磺酸内酯和对甲氧基苯酚加入质量与所述3-氨丙基三乙氧基硅烷的质量比为N,N-二甲基乙醇胺:1,3-丙烷磺酸内酯:对甲氧基苯酚:3-氨丙基三乙氧基硅烷=0.2:0.3:0.04:7;
(3)将天然橡胶在开炼机中塑炼,塑炼后切碎溶解在甲苯中,然后加入所述交联剂A、交联剂B和防老剂,搅拌均匀,加入甲苯调节黏度后涂布在PET薄膜上,涂布液中所述塑炼后切碎的橡胶、交联剂A、交联剂B和防老剂按重量份数计为橡胶100份,交联剂A1份,交联剂B 0.3份,防老剂(KY-405)4份;涂布后130℃烘烤2min,获得所述橡胶型锂电池压敏胶粘带(干胶厚度10μm)。
实施例3
一种橡胶型锂电池压敏胶粘带,其制备方法为:
(1)将聚碳酸酯二醇和N-甲基吡咯烷酮混合形成混合物,所述聚碳酸酯二醇和N-甲基吡咯烷酮混合量比为聚碳酸酯二醇:N-甲基吡咯烷酮=5g/100mL;搅拌所述混合物,在搅拌状态下向混合物中加入环氧氯丙烷,加料完成后水浴恒温至50±3℃,到温后向混合物中加入三氟化硼乙醚,加料后保温120min,保温结束后再向混合物中加入氢氧化钠溶液,所述氢氧化钠溶液的浓度为40g/L,溶剂为水;所述氢氧化钠溶液的加入量与所述聚碳酸酯二醇的质量比为氢氧化钠溶液:聚碳酸酯二醇=50mL:5g;继续50±3℃水浴保温120min,然后空冷至常温,加乙酸乙酯萃取,去除水相,然后旋蒸去除乙酸乙酯,获得交联剂A;其中所述环氧氯丙烷、三氟化硼乙醚加入质量与所述聚碳酸酯二醇的质量比为环氧氯丙烷:三氟化硼乙醚:聚碳酸酯二醇=13g:0.06g:5g;
(2)将甲苯二异氰酸酯三聚体和丙酮混合形成混合液,混合液中所述甲苯二异氰酸酯三聚体和丙酮混合质量比为甲苯二异氰酸酯三聚体:丙酮=9:150;向所述混合液中加入聚乙二醇单甲醚,加料完成后水浴恒温至60±3℃,保温冷凝回流2h,然后向混合液中加入甲基乙基酮肟,其中所述聚乙二醇单甲醚、甲基乙基酮肟加入质量与所述甲苯二异氰酸酯三聚体的质量比为聚乙二醇单甲醚:甲基乙基酮肟:甲苯二异氰酸酯三聚体=5:1:9;加料完成后继续60±3℃水浴恒温,搅拌保温冷凝回流3h,然后混合液空冷至常温,旋蒸去除丙酮;再向混合液中滴加3-氨丙基三乙氧基硅烷,向混合液中滴加3-氨丙基三乙氧基硅烷的质量比为3-氨丙基三乙氧基硅烷:混合液=8:50;加料完成后水浴恒温至50±3℃,保温40min,然后再向混合液中依次加入N,N-二甲基乙醇胺和1,3-丙烷磺酸内酯,加料完成后50±3℃温度范围内搅拌保温60min,然后再向混合物中加入对甲氧基苯酚,获得交联剂B;其中所述N,N-二甲基乙醇胺、1,3-丙烷磺酸内酯和对甲氧基苯酚加入质量与所述3-氨丙基三乙氧基硅烷的质量比为N,N-二甲基乙醇胺:1,3-丙烷磺酸内酯:对甲氧基苯酚:3-氨丙基三乙氧基硅烷=0.2:0.4:0.05:8;
(3)将天然橡胶在开炼机中塑炼,塑炼后切碎溶解在甲苯中,然后加入所述交联剂A、交联剂B和防老剂,搅拌均匀,加入甲苯调节黏度后涂布在PET薄膜上,涂布液中所述塑炼后切碎的橡胶、交联剂A、交联剂B和防老剂按重量份数计为橡胶100份,交联剂A 2份,交联剂B 0.3份,防老剂(KY-405)4份;涂布后130℃烘烤2min,获得所述橡胶型锂电池压敏胶粘带(干胶厚度10μm)。
实施例4
一种橡胶型锂电池压敏胶粘带,其制备方法为:
(1)将聚碳酸酯二醇和N-甲基吡咯烷酮混合形成混合物,所述聚碳酸酯二醇和N-甲基吡咯烷酮混合量比为聚碳酸酯二醇:N-甲基吡咯烷酮=6g/100mL;搅拌所述混合物,在搅拌状态下向混合物中加入环氧氯丙烷,加料完成后水浴恒温至50±3℃,到温后向混合物中加入三氟化硼乙醚,加料后保温120min,保温结束后再向混合物中加入氢氧化钠溶液,所述氢氧化钠溶液的浓度为40g/L,溶剂为水;所述氢氧化钠溶液的加入量与所述聚碳酸酯二醇的质量比为氢氧化钠溶液:聚碳酸酯二醇=50mL:6g;继续50±3℃水浴保温120min,然后空冷至常温,加乙酸乙酯萃取,去除水相,然后旋蒸去除乙酸乙酯,获得交联剂A;其中所述环氧氯丙烷、三氟化硼乙醚加入质量与所述聚碳酸酯二醇的质量比为环氧氯丙烷:三氟化硼乙醚:聚碳酸酯二醇=14g:0.06g:6g;
(2)将甲苯二异氰酸酯三聚体和丙酮混合形成混合液,混合液中所述甲苯二异氰酸酯三聚体和丙酮混合质量比为甲苯二异氰酸酯三聚体:丙酮=10:150;向所述混合液中加入聚乙二醇单甲醚,加料完成后水浴恒温至60±3℃,保温冷凝回流2h,然后向混合液中加入甲基乙基酮肟,其中所述聚乙二醇单甲醚、甲基乙基酮肟加入质量与所述甲苯二异氰酸酯三聚体的质量比为聚乙二醇单甲醚:甲基乙基酮肟:甲苯二异氰酸酯三聚体=6:1.2:10;加料完成后继续60±3℃水浴恒温,搅拌保温冷凝回流3h,然后混合液空冷至常温,旋蒸去除丙酮;再向混合液中滴加3-氨丙基三乙氧基硅烷,向混合液中滴加3-氨丙基三乙氧基硅烷的质量比为3-氨丙基三乙氧基硅烷:混合液=9:50;加料完成后水浴恒温至50±3℃,保温40min,然后再向混合液中依次加入N,N-二甲基乙醇胺和1,3-丙烷磺酸内酯,加料完成后50±3℃温度范围内搅拌保温60min,然后再向混合物中加入对甲氧基苯酚,获得交联剂B;其中所述N,N-二甲基乙醇胺、1,3-丙烷磺酸内酯和对甲氧基苯酚加入质量与所述3-氨丙基三乙氧基硅烷的质量比为N,N-二甲基乙醇胺:1,3-丙烷磺酸内酯:对甲氧基苯酚:3-氨丙基三乙氧基硅烷=0.25:0.4:0.06:9;
(3)将天然橡胶在开炼机中塑炼,塑炼后切碎溶解在甲苯中,然后加入所述交联剂A、交联剂B和防老剂,搅拌均匀,加入甲苯调节黏度后涂布在PET薄膜上,涂布液中所述塑炼后切碎的橡胶、交联剂A、交联剂B和防老剂按重量份数计为橡胶100份,交联剂A2份,交联剂B 0.2份,防老剂(KY-405)5份;涂布后130℃烘烤2min,获得所述橡胶型锂电池压敏胶粘带(干胶厚度10μm)。
对比例1
一种作为对比的橡胶型锂电池压敏胶粘带,其制备方法为:
(1)将聚碳酸酯二醇和N-甲基吡咯烷酮混合形成混合物,所述聚碳酸酯二醇和N-甲基吡咯烷酮混合量比为聚碳酸酯二醇:N-甲基吡咯烷酮=5g/100mL;搅拌所述混合物,在搅拌状态下向混合物中加入环氧氯丙烷,加料完成后水浴恒温至50±3℃,到温后向混合物中加入三氟化硼乙醚,加料后保温120min,保温结束后再向混合物中加入氢氧化钠溶液,所述氢氧化钠溶液的浓度为40g/L,溶剂为水;所述氢氧化钠溶液的加入量与所述聚碳酸酯二醇的质量比为氢氧化钠溶液:聚碳酸酯二醇=50mL:5g;继续50±3℃水浴保温120min,然后空冷至常温,加乙酸乙酯萃取,去除水相,然后旋蒸去除乙酸乙酯,获得交联剂A;其中所述环氧氯丙烷、三氟化硼乙醚加入质量与所述聚碳酸酯二醇的质量比为环氧氯丙烷:三氟化硼乙醚:聚碳酸酯二醇=12g:0.05g:5g;
(2)将天然橡胶在开炼机中塑炼,塑炼后切碎溶解在甲苯中,然后加入所述交联剂A和防老剂,搅拌均匀,加入甲苯调节黏度后涂布在PET薄膜上,涂布液中所述塑炼后切碎的橡胶、交联剂A和防老剂按重量份数计为橡胶100份,交联剂A1.3份,防老剂(KY-405)4份;涂布后130℃烘烤2min,获得本对比例所述橡胶型锂电池压敏胶粘带(干胶厚度10μm)。
对比例2
一种作为对比的橡胶型锂电池压敏胶粘带,其制备方法为:
(1)将甲苯二异氰酸酯三聚体和丙酮混合形成混合液,混合液中所述甲苯二异氰酸酯三聚体和丙酮混合质量比为甲苯二异氰酸酯三聚体:丙酮=9:150;向所述混合液中加入聚乙二醇单甲醚,加料完成后水浴恒温至60±3℃,保温冷凝回流2h,然后向混合液中加入甲基乙基酮肟,其中所述聚乙二醇单甲醚、甲基乙基酮肟加入质量与所述甲苯二异氰酸酯三聚体的质量比为聚乙二醇单甲醚:甲基乙基酮肟:甲苯二异氰酸酯三聚体=5:1:9;加料完成后继续60±3℃水浴恒温,搅拌保温冷凝回流3h,然后混合液空冷至常温,旋蒸去除丙酮;再向混合液中滴加3-氨丙基三乙氧基硅烷,向混合液中滴加3-氨丙基三乙氧基硅烷的质量比为3-氨丙基三乙氧基硅烷:混合液=7:50;加料完成后水浴恒温至50±3℃,保温40min,然后再向混合液中依次加入N,N-二甲基乙醇胺和1,3-丙烷磺酸内酯,加料完成后50±3℃温度范围内搅拌保温60min,然后再向混合物中加入对甲氧基苯酚,获得本对比例所述交联剂B;其中所述N,N-二甲基乙醇胺、1,3-丙烷磺酸内酯和对甲氧基苯酚加入质量与所述3-氨丙基三乙氧基硅烷的质量比为N,N-二甲基乙醇胺:1,3-丙烷磺酸内酯:对甲氧基苯酚:3-氨丙基三乙氧基硅烷=0.2:0.3:0.04:7;
(2)将天然橡胶在开炼机中塑炼,塑炼后切碎溶解在甲苯中,然后加入所述交联剂B和防老剂,搅拌均匀,加入甲苯调节黏度后涂布在PET薄膜上,涂布液中所述塑炼后切碎的橡胶、交联剂B和防老剂按重量份数计为橡胶100份,交联剂B1.3份,防老剂(KY-405)4份;涂布后130℃烘烤2min,获得本对比例所述橡胶型锂电池压敏胶粘带(干胶厚度10μm)。
实施例5
按照标准GB/T2792-2014标准的要求分别测试上述各实施例和对比例制得的胶粘带的剥离强度,剥离速率均设定为300mm/min,被粘基材为不锈钢;测耐高温性能的测试:将上述各实施例和对比例制得的胶粘带粘贴在不锈钢钢板(表面粗糙度为RA0.8μm)上,在160℃的恒温烤箱中烘烤规定时间,再在烤箱中热剥剥开胶粘带,观察不锈钢钢板上有无残胶痕迹。结果如表1所示。
表1
试验组 | 剥离强度(N/25mm) | 耐温性能160℃ |
实施例1 | 8.776 | 4h不残胶,4.5h轻微残胶 |
实施例2 | 9.014 | 4h不残胶,4.5h轻微残胶 |
实施例3 | 8.957 | 4h不残胶,4.5h轻微残胶 |
实施例4 | 8.809 | 4h不残胶,4.5h轻微残胶 |
对比例1 | 5.244 | 2h不残胶,2.5h有残胶 |
对比例2 | 3.929 | 1.5h不残胶,2h有残胶 |
由表1可知,本发明所述方法制备的胶粘带具有较高的剥离强度和耐高温性能,这可能主要是由于本发明制备的交联剂A和交联剂B能够与天然橡胶中含有的活性基团发生交联,进而改变压敏胶的分子构造,使得分子间作用力更强,内聚强度更高,压敏胶的交联密度也相应升高,从而提高胶粘带的剥离强度和耐高温性能。
以上对本发明所提供的技术方案进行了详细介绍,对于本领域的一般技术人员,依据本发明实施例的思想,在具体实施方式及应用范围上均会有改变之处,综上所述,本说明书内容不应理解为对本发明的限制。
Claims (6)
1.一种橡胶型锂电池压敏胶粘带,其特征在于,制备方法为:
(1)将聚碳酸酯二醇和N-甲基吡咯烷酮混合形成混合物,搅拌所述混合物,在搅拌状态下向混合物中加入环氧氯丙烷,加料完成后水浴恒温至50±3℃,到温后向混合物中加入三氟化硼乙醚,加料后保温120~150min,保温结束后再向混合物中加入氢氧化钠溶液,继续50±3℃水浴保温120~150min,然后空冷至常温,加乙酸乙酯萃取,去除水相,然后旋蒸去除乙酸乙酯,获得交联剂A;
(2)将甲苯二异氰酸酯三聚体和丙酮混合形成混合液,向所述混合液中加入聚乙二醇单甲醚,加料完成后水浴恒温至60±3℃,保温冷凝回流2h以上,然后向混合液中加入甲基乙基酮肟,加料完成后继续60±3℃水浴恒温,搅拌保温冷凝回流3h以上,然后混合液空冷至常温,旋蒸去除丙酮;再向混合液中滴加3-氨丙基三乙氧基硅烷,加料完成后水浴恒温至50±3℃,保温40min以上,然后再向混合液中依次加入N,N-二甲基乙醇胺和1,3-丙烷磺酸内酯,加料完成后50±3℃温度范围内搅拌保温60min以上,然后再向混合物中加入对甲氧基苯酚,获得交联剂B;
(3)将天然橡胶在开炼机中塑炼,塑炼后切碎溶解在甲苯中,然后加入所述交联剂A、交联剂B和防老剂,搅拌均匀,加入甲苯调节黏度后涂布在PET薄膜上,130℃烘烤,获得所述橡胶型锂电池压敏胶粘带。
2.根据权利要求1所述的一种橡胶型锂电池压敏胶粘带,其特征在于,所述聚碳酸酯二醇和N-甲基吡咯烷酮混合量比为聚碳酸酯二醇:N-甲基吡咯烷酮=4~6g/100mL;所述环氧氯丙烷、三氟化硼乙醚加入质量与所述聚碳酸酯二醇的质量比为环氧氯丙烷:三氟化硼乙醚:聚碳酸酯二醇=10~14g:0.05~0.06g:4~6g。
3.根据权利要求2所述的一种橡胶型锂电池压敏胶粘带,其特征在于,所述氢氧化钠溶液的浓度为40~50g/L,溶剂为水;所述氢氧化钠溶液的加入量与所述聚碳酸酯二醇的质量比为氢氧化钠溶液:聚碳酸酯二醇=50mL:4~6g。
4.根据权利要求1所述的一种橡胶型锂电池压敏胶粘带,其特征在于,所述甲苯二异氰酸酯三聚体和丙酮混合质量比为甲苯二异氰酸酯三聚体:丙酮=8~10:150;所述聚乙二醇单甲醚、甲基乙基酮肟加入质量与所述甲苯二异氰酸酯三聚体的质量比为聚乙二醇单甲醚:甲基乙基酮肟:甲苯二异氰酸酯三聚体=4~6:0.8~1.2:8~10。
5.根据权利要求4所述的一种橡胶型锂电池压敏胶粘带,其特征在于,向混合液中滴加3-氨丙基三乙氧基硅烷的质量比为3-氨丙基三乙氧基硅烷:混合液=6~9:50;所述N,N-二甲基乙醇胺、1,3-丙烷磺酸内酯和对甲氧基苯酚加入质量与所述3-氨丙基三乙氧基硅烷的质量比为N,N-二甲基乙醇胺:1,3-丙烷磺酸内酯:对甲氧基苯酚:3-氨丙基三乙氧基硅烷=0.15~0.25:0.3~0.4:0.03~0.06:6~9。
6.根据权利要求1所述的一种橡胶型锂电池压敏胶粘带,其特征在于,涂布液中,所述塑炼后切碎的橡胶、交联剂A、交联剂B和防老剂按重量份数计为橡胶100份,交联剂A1~2份,交联剂B 0.2~0.4份,防老剂3~5份。
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