CN115572573B - 一种用于智能穿戴的聚氨酯热熔胶及其制备方法 - Google Patents
一种用于智能穿戴的聚氨酯热熔胶及其制备方法 Download PDFInfo
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- CN115572573B CN115572573B CN202211397839.4A CN202211397839A CN115572573B CN 115572573 B CN115572573 B CN 115572573B CN 202211397839 A CN202211397839 A CN 202211397839A CN 115572573 B CN115572573 B CN 115572573B
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- diisocyanate
- polyurethane
- hot melt
- melt adhesive
- crystalline
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- 239000011737 fluorine Substances 0.000 claims abstract description 48
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- 238000003756 stirring Methods 0.000 claims description 22
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- 125000005442 diisocyanate group Chemical group 0.000 claims description 14
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- NIMLQBUJDJZYEJ-UHFFFAOYSA-N isophorone diisocyanate Chemical compound CC1(C)CC(N=C=O)CC(C)(CN=C=O)C1 NIMLQBUJDJZYEJ-UHFFFAOYSA-N 0.000 claims description 12
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- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 claims description 7
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- FKTHNVSLHLHISI-UHFFFAOYSA-N 1,2-bis(isocyanatomethyl)benzene Chemical compound O=C=NCC1=CC=CC=C1CN=C=O FKTHNVSLHLHISI-UHFFFAOYSA-N 0.000 claims description 4
- UPMLOUAZCHDJJD-UHFFFAOYSA-N 4,4'-Diphenylmethane Diisocyanate Chemical compound C1=CC(N=C=O)=CC=C1CC1=CC=C(N=C=O)C=C1 UPMLOUAZCHDJJD-UHFFFAOYSA-N 0.000 claims description 4
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- 239000011261 inert gas Substances 0.000 claims description 4
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- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 2
- IQGYVZCUVJNLLO-UHFFFAOYSA-N 1,1,2,2,3,3,4,4,5,5,6,6,7,7,8,8,9,9-octadecafluorononane-1,9-diol Chemical compound OC(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(O)(F)F IQGYVZCUVJNLLO-UHFFFAOYSA-N 0.000 claims description 2
- NNOZGCICXAYKLW-UHFFFAOYSA-N 1,2-bis(2-isocyanatopropan-2-yl)benzene Chemical compound O=C=NC(C)(C)C1=CC=CC=C1C(C)(C)N=C=O NNOZGCICXAYKLW-UHFFFAOYSA-N 0.000 claims description 2
- GJZFGDYLJLCGHT-UHFFFAOYSA-N 1,2-diethylthioxanthen-9-one Chemical compound C1=CC=C2C(=O)C3=C(CC)C(CC)=CC=C3SC2=C1 GJZFGDYLJLCGHT-UHFFFAOYSA-N 0.000 claims description 2
- MSAHTMIQULFMRG-UHFFFAOYSA-N 1,2-diphenyl-2-propan-2-yloxyethanone Chemical compound C=1C=CC=CC=1C(OC(C)C)C(=O)C1=CC=CC=C1 MSAHTMIQULFMRG-UHFFFAOYSA-N 0.000 claims description 2
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- ALQLPWJFHRMHIU-UHFFFAOYSA-N 1,4-diisocyanatobenzene Chemical compound O=C=NC1=CC=C(N=C=O)C=C1 ALQLPWJFHRMHIU-UHFFFAOYSA-N 0.000 claims description 2
- JQYSLXZRCMVWSR-UHFFFAOYSA-N 1,6-dioxacyclododecane-7,12-dione;terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1.O=C1CCCCC(=O)OCCCCO1 JQYSLXZRCMVWSR-UHFFFAOYSA-N 0.000 claims description 2
- VPNRJIKJACGVJW-UHFFFAOYSA-N 1,8-dioxacycloicosane-9,20-dione Chemical compound O=C1CCCCCCCCCCC(=O)OCCCCCCO1 VPNRJIKJACGVJW-UHFFFAOYSA-N 0.000 claims description 2
- 239000012956 1-hydroxycyclohexylphenyl-ketone Substances 0.000 claims description 2
- PAUHLEIGHAUFAK-UHFFFAOYSA-N 1-isocyanato-1-[(1-isocyanatocyclohexyl)methyl]cyclohexane Chemical compound C1CCCCC1(N=C=O)CC1(N=C=O)CCCCC1 PAUHLEIGHAUFAK-UHFFFAOYSA-N 0.000 claims description 2
- MTEZSDOQASFMDI-UHFFFAOYSA-N 1-trimethoxysilylpropan-1-ol Chemical compound CCC(O)[Si](OC)(OC)OC MTEZSDOQASFMDI-UHFFFAOYSA-N 0.000 claims description 2
- LNBMZFHIYRDKNS-UHFFFAOYSA-N 2,2-dimethoxy-1-phenylethanone Chemical compound COC(OC)C(=O)C1=CC=CC=C1 LNBMZFHIYRDKNS-UHFFFAOYSA-N 0.000 claims description 2
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- DZJUUOUBBLVXSV-UHFFFAOYSA-N 2-chloro-10h-anthracen-9-one Chemical compound C1=CC=C2C(=O)C3=CC(Cl)=CC=C3CC2=C1 DZJUUOUBBLVXSV-UHFFFAOYSA-N 0.000 claims description 2
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- CKKQLOUBFINSIB-UHFFFAOYSA-N 2-hydroxy-1,2,2-triphenylethanone Chemical compound C=1C=CC=CC=1C(C=1C=CC=CC=1)(O)C(=O)C1=CC=CC=C1 CKKQLOUBFINSIB-UHFFFAOYSA-N 0.000 claims description 2
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- UUEWCQRISZBELL-UHFFFAOYSA-N 3-trimethoxysilylpropane-1-thiol Chemical compound CO[Si](OC)(OC)CCCS UUEWCQRISZBELL-UHFFFAOYSA-N 0.000 claims description 2
- ZMSQJSMSLXVTKN-UHFFFAOYSA-N 4-[2-(2-morpholin-4-ylethoxy)ethyl]morpholine Chemical compound C1COCCN1CCOCCN1CCOCC1 ZMSQJSMSLXVTKN-UHFFFAOYSA-N 0.000 claims description 2
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- CHIHQLCVLOXUJW-UHFFFAOYSA-N benzoic anhydride Chemical compound C=1C=CC=CC=1C(=O)OC(=O)C1=CC=CC=C1 CHIHQLCVLOXUJW-UHFFFAOYSA-N 0.000 claims description 2
- 229960002130 benzoin Drugs 0.000 claims description 2
- RWCCWEUUXYIKHB-UHFFFAOYSA-N benzophenone Chemical compound C=1C=CC=CC=1C(=O)C1=CC=CC=C1 RWCCWEUUXYIKHB-UHFFFAOYSA-N 0.000 claims description 2
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- MQDJYUACMFCOFT-UHFFFAOYSA-N bis[2-(1-hydroxycyclohexyl)phenyl]methanone Chemical compound C=1C=CC=C(C(=O)C=2C(=CC=CC=2)C2(O)CCCCC2)C=1C1(O)CCCCC1 MQDJYUACMFCOFT-UHFFFAOYSA-N 0.000 claims description 2
- ZFVMWEVVKGLCIJ-UHFFFAOYSA-N bisphenol AF Chemical compound C1=CC(O)=CC=C1C(C(F)(F)F)(C(F)(F)F)C1=CC=C(O)C=C1 ZFVMWEVVKGLCIJ-UHFFFAOYSA-N 0.000 claims description 2
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- 229940106012 diethylene glycol adipate Drugs 0.000 claims description 2
- SBECZZGBLMCBLT-UHFFFAOYSA-N diphenylphosphoryl-(2,4,6-triphenylphenyl)methanone Chemical compound C=1C=CC=CC=1P(=O)(C=1C=CC=CC=1)C(=O)C1=C(C=2C=CC=CC=2)C=C(C=2C=CC=CC=2)C=C1C1=CC=CC=C1 SBECZZGBLMCBLT-UHFFFAOYSA-N 0.000 claims description 2
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- YRHRIQCWCFGUEQ-UHFFFAOYSA-N thioxanthen-9-one Chemical compound C1=CC=C2C(=O)C3=CC=CC=C3SC2=C1 YRHRIQCWCFGUEQ-UHFFFAOYSA-N 0.000 claims description 2
- KSBAEPSJVUENNK-UHFFFAOYSA-L tin(ii) 2-ethylhexanoate Chemical compound [Sn+2].CCCCC(CC)C([O-])=O.CCCCC(CC)C([O-])=O KSBAEPSJVUENNK-UHFFFAOYSA-L 0.000 claims description 2
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- GUCYFKSBFREPBC-UHFFFAOYSA-N [phenyl-(2,4,6-trimethylbenzoyl)phosphoryl]-(2,4,6-trimethylphenyl)methanone Chemical group CC1=CC(C)=CC(C)=C1C(=O)P(=O)(C=1C=CC=CC=1)C(=O)C1=C(C)C=C(C)C=C1C GUCYFKSBFREPBC-UHFFFAOYSA-N 0.000 description 1
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- SQMLHQFSNLRBFN-UHFFFAOYSA-N bis[2-(2-hydroxypropan-2-yl)phenyl]methanone Chemical compound CC(C)(O)C1=CC=CC=C1C(=O)C1=CC=CC=C1C(C)(C)O SQMLHQFSNLRBFN-UHFFFAOYSA-N 0.000 description 1
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Classifications
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- 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
- C09J175/14—Polyurethanes having carbon-to-carbon unsaturated bonds
-
- 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
- C08G18/30—Low-molecular-weight compounds
- C08G18/38—Low-molecular-weight compounds having heteroatoms other than oxygen
- C08G18/3802—Low-molecular-weight compounds having heteroatoms other than oxygen having halogens
- C08G18/3804—Polyhydroxy compounds
- C08G18/3812—Polyhydroxy compounds having fluorine atoms
-
- 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
- C08G18/42—Polycondensates having carboxylic or carbonic ester groups in the main chain
- C08G18/4205—Polycondensates having carboxylic or carbonic ester groups in the main chain containing cyclic groups
- C08G18/4208—Polycondensates having carboxylic or carbonic ester groups in the main chain containing cyclic groups containing aromatic groups
- C08G18/4211—Polycondensates having carboxylic or carbonic ester groups in the main chain containing cyclic groups containing aromatic groups derived from aromatic dicarboxylic acids and dialcohols
- C08G18/4213—Polycondensates having carboxylic or carbonic ester groups in the main chain containing cyclic groups containing aromatic groups derived from aromatic dicarboxylic acids and dialcohols from terephthalic acid and dialcohols
-
- 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
- C08G18/42—Polycondensates having carboxylic or carbonic ester groups in the main chain
- C08G18/4236—Polycondensates having carboxylic or carbonic ester groups in the main chain containing only aliphatic groups
- C08G18/4238—Polycondensates having carboxylic or carbonic ester groups in the main chain containing only aliphatic groups derived from dicarboxylic acids and dialcohols
-
- C—CHEMISTRY; METALLURGY
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Abstract
本发明提供了一种用于智能穿戴的聚氨酯热熔胶及其制备方法和应用,所述聚氨酯热熔胶包括氟改性聚氨酯丙烯酸酯、结晶性聚氨酯、光引发剂和硅烷偶联剂。通过氟改性聚氨酯丙烯酸酯、结晶性聚氨酯的协同作用,使得聚氨酯热熔胶制得的试样具有优良的粘结强度和3m防水性能,可以用于智能穿戴领域。
Description
技术领域
本发明属于热熔胶技术领域,尤其涉及一种智能穿戴用聚氨酯热熔胶及其制备方法。
背景技术
聚氨酯(PUR)热熔胶不含有水和溶剂,固含量为100%,是一种高性能环保型胶黏剂。它兼有普通热熔胶无溶剂、初粘性高、装配时定位迅速等特性,又具有反应型液态胶黏剂粘接强度高的优点,施胶温度却又低于普通热熔胶,近些年已被广泛应用于家电、消费电子等领域。
目前我国智能穿戴设备市场呈现高速、稳定发展态势,聚氨酯热熔胶本身无溶剂,安全环保无毒,满足智能穿戴要求。但由于智能穿戴电子产品需要长期与人体皮肤接触,对胶黏剂的防水性提出了更高的要求。
因此,针对上述问题,亟待寻求一种具有良好粘结强度和防水性能的聚氨酯热熔胶,以适应智能穿戴领域长期接触皮肤的需求。
发明内容
针对上述现有技术存在的缺陷,本发明的一个目的是,提供一种用于智能穿戴的聚氨酯热熔胶及其制备方法,旨在解决智能穿戴领域热熔胶粘结强度和防水的技术问题。
为实现上述目的,本发明采用的技术方案如下:
一种用于智能穿戴的聚氨酯热熔胶,包括如下组分及其质量百分含量:
氟改性聚氨酯丙烯酸酯30-60%;
结晶性聚氨酯30-60%;
光引发剂0.5-5%;
硅烷偶联剂0.5-5%;
所述氟改性聚氨酯丙烯酸酯是由含氟二醇、二异氰酸酯和(甲基)丙烯酸羟基酯在催化剂的存在下制备得到。
所述结晶性聚氨酯是由结晶性聚酯多元醇、二异氰酸酯在催化剂的存在下制备得到。
所述含氟二醇选自以下物质中的一种或多种:2,2,3,3-四氟-1,4-丁二醇、2,2,3,3,4,4-六氟-1,5-戊烷二醇、2,2,3,3,4,4,5,5-八氟-1,6-己二醇、十二氟-1,8-辛二醇、全氟-1,9-壬烷二醇、全氟-1,10-癸二醇、六氟双酚A、全氟聚醚二醇。
所述二异氰酸酯选自以下物质中的一种或多种:异佛尔酮二异氰酸酯(IPDI)、萘1,5-二异氰酸酯(NDI)、亚甲基双环己基异氰酸酯、亚甲基二苯基二异氰酸酯(MDI)、甲苯二异氰酸酯(TDI)、六亚甲基二异氰酸酯(HDI)、亚二甲苯基二异氰酸酯、氢化亚二甲苯基二异氰酸酯、四甲基亚二甲苯基二异氰酸酯、对亚苯基二异氰酸酯、3,3'-二甲基二苯基-4,4'-二异氰酸酯(DDDI)、2,2,4-三甲基六亚甲基二异氰酸酯(TMDI)、降冰片烷二异氰酸酯(NDI)、4,4'-二苄基二异氰酸酯(DBDI)。
所述(甲基)丙烯酸羟基酯选自以下物质中的一种或多种:(甲基)丙烯酸羟甲酯、(甲基)丙烯酸羟乙酯、(甲基)丙烯酸羟丙酯、(甲基)丙烯酸羟丁酯。
所述结晶性聚酯多元醇选自以下物质中的一种或多种:聚己二酸己二醇酯、聚对苯二甲酸己二醇酯、聚十二烷二酸己二醇酯、聚己二酸-对苯二甲酸-丁二醇酯、聚己二酸一缩二乙二醇酯、聚己内酯二元醇。
所述催化剂选自以下物质中的一种或多种:二月桂酸二丁基锡、辛酸亚锡、乙酸二丁烯、三乙烯二胺、双吗啉基二乙基醚。
基于二异氰酸酯的量,催化剂优选以0.005至3.5重量%的量存在。
所述含氟二醇、二异氰酸酯和(甲基)丙烯酸羟基酯的摩尔比为1:2:2。
所述结晶性聚酯多元醇、二异氰酸酯的摩尔比为1:1。
所述硅烷偶联剂选自以下物质中的一种或多种:氨丙基三乙氧基硅烷、γ-巯丙基三甲氧基硅烷、缩水甘油醚氧丙基三甲氧基硅烷。
所述光引发剂选自以下物质中的一种或多种:苄基缩酮、羟基酮、胺酮和酰基氧化膦诸如2-羟基-2-甲基-1-苯基-1-丙酮、二苯基(2,4,6-三苯基苯甲酰基)-氧化膦、2-苄基-二甲基氨基-1-(4-吗啉基苯基)-丁-1-酮、苯偶姻二甲基缩酮二甲氧基苯乙酮、α-羟基苄基苯基酮、1-羟基-1-甲基乙基苯基酮、寡-2-羟基-2-甲基-1-(4-(1-甲基乙烯基)苯基)丙酮、二苯甲酮;邻苄基苯甲酸甲酯;苯甲酰甲酸甲酯、2-二乙氧基苯乙酮、2,2-二仲丁氧基苯乙酮、对苯基二苯甲酮、2-异丙基噻吨酮、2-甲基蒽酮、2-乙基蒽酮、2-氯蒽酮、1,2-苯并蒽酮、苯甲酰醚、苯偶姻醚、苯偶姻甲基醚;苯偶姻异丙基醚、α-苯基苯偶姻、噻吨酮、二乙基噻吨酮、1,5-萘乙酮、1-羟基环己基苯基酮、对二甲基氨基苯甲酸乙酯。这些光引发剂可以单独使用或彼此组合使用。
在一个优选的实施方案中,光引发剂是双(2,4,6-三甲基苯甲酰基)-苯基氧化膦或Irgacure 819。
进一步地,所述氟改性聚氨酯丙烯酸酯具体通过如下步骤制得:
在惰性气体保护下的容器中,加入含氟二醇,在100-110℃真空脱水后,温度降为70-90℃,再加入二异氰酸酯和催化剂,70-90℃反应2-6h;再加入(甲基)丙烯酸羟基酯,降温至80-85℃下反应2-5h,得到氟改性聚氨酯丙烯酸酯。
进一步地,所述结晶性聚氨酯具体通过如下步骤制得:
在惰性气体保护下的容器中,加入结晶性聚酯多元醇,在100-130℃真空脱水后,温度降至70-80℃;再加入将异氰酸酯和催化剂,升温至120-160℃反应2-5小时,得到结晶性聚氨酯。
本发明的第二个目的是提供一种用于智能穿戴的聚氨酯热熔胶的制备方法,包括如下步骤:
S1、按配方称取各组分原料;
S2、将氟改性聚氨酯丙烯酸酯、结晶性聚氨酯以及硅烷偶联剂加入反应釜中,在真空条件下以100-200rpm的速度搅拌30-60分钟;
S3、在避光条件下,将光引发剂加入步骤S2的反应釜中,在真空条件下以100-200rpm的速度搅拌20-60分钟,在避光和氮气保护下快速出料并抽真空密封保存。
本发明的第三个目的是提供一种用于智能穿戴的聚氨酯热熔胶在智能穿戴领域中的应用,特别是在改善智能穿戴领域热熔胶粘结强度和防水性能方面的应用。
与现有技术相比,本发明具有如下优点:
(1)本发明创造性地引入氟改性聚氨酯丙烯酸酯,通过在聚氨酯链段中引入可光固化的双键丙烯酸酯和非极性地含氟链段,一方面丙烯酸酯固化在加快固化时间的基础上进一步增加体系的交联度,提高了聚氨酯热熔胶的粘结强度,另一方面,含氟链段带来了聚氨酯热熔胶耐汗和防水性能的提高。
(2)本发明人创造性地发现,氟改性聚氨酯丙烯酸酯和结晶性聚氨酯二者在聚氨酯热熔胶体系中产生了协同作用,带来聚氨酯热熔胶粘结强度和防水性能的改善。
具体实施方式
为更好地说明本发明的目的、技术方案和优点,下面将结合具体实施例对本发明作进一步说明。
制备例1
氟改性聚氨酯丙烯酸酯(F-1)的制备:
在配有搅拌器、温度计和通氮气装置的三口烧瓶中,加入0.1mol的2,2,3,3-四氟-1,4-丁二醇,在110℃真空脱水2h后,温度降为85℃,再加入0.2mol异佛尔酮二异氰酸酯和0.03wt%(基于异佛尔酮二异氰酸酯的质量分数)二月桂酸二丁基锡,85℃反应3h;再加入0.2mol甲基丙烯酸羟乙酯,降温至80℃下反应5h,得到氟改性聚氨酯丙烯酸酯F-1。
制备例2
氟改性聚氨酯丙烯酸酯(F-2)的制备:
在配有搅拌器、温度计和通氮气装置的三口烧瓶中,加入0.1mol的全氟-1,10-癸二醇,在110℃真空脱水2h后,温度降为85℃,再加入0.2mol异佛尔酮二异氰酸酯和0.03wt%(基于异佛尔酮二异氰酸酯的质量分数)二月桂酸二丁基锡,85℃反应3h;再加入0.2mol甲基丙烯酸羟乙酯,降温至80℃下反应5h,得到氟改性聚氨酯丙烯酸酯F-2。
制备例3
氟改性聚氨酯丙烯酸酯(F-3)的制备:
在配有搅拌器、温度计和通氮气装置的三口烧瓶中,加入0.1mol的全氟-1,10-癸二醇,在110℃真空脱水2h后,温度降为85℃,再加入0.2mol异佛尔酮二异氰酸酯和0.03wt%(基于异佛尔酮二异氰酸酯的质量分数)二月桂酸二丁基锡,85℃反应3h;再加入0.2mol甲基丙烯酸羟丁酯,降温至80℃下反应5h,得到氟改性聚氨酯丙烯酸酯F-3。
制备例4
结晶性聚氨酯(PU-1)的制备:
在配有搅拌器、温度计和通氮气装置的三口烧瓶中,加入0.1mol的聚己二酸己二醇酯(Mw=2000),在110℃真空脱水2h后,温度降为80℃,再加入0.1mol异佛尔酮二异氰酸酯和0.03wt%(基于异佛尔酮二异氰酸酯的质量分数)二月桂酸二丁基锡,120℃反应3h,得到结晶性聚氨酯PU-1。
制备例5
结晶性聚氨酯(PU-2)的制备:
在配有搅拌器、温度计和通氮气装置的三口烧瓶中,加入0.1mol的聚对苯二甲酸己二醇酯(Mw=2000),在110℃真空脱水2h后,温度降为80℃,再加入0.1mol异佛尔酮二异氰酸酯和0.03wt%(基于异佛尔酮二异氰酸酯的质量分数)二月桂酸二丁基锡,120℃反应3h,得到结晶性聚氨酯PU-2。
实施例1
用于智能穿戴的聚氨酯热熔胶的制备:
S1、按照以下质量百分比准备各原料:
氟改性聚氨酯丙烯酸酯F-1 50%;
结晶性聚氨酯PU-1 47%;
光引发剂2%;
硅烷偶联剂1%;
S2、将氟改性聚氨酯丙烯酸酯F-1、结晶性聚氨酯PU-1以及硅烷偶联剂KH550加入反应釜中,在真空条件下以200rpm的速度搅拌60分钟;
S3、在避光条件下,将光引发剂Irgacure 819加入步骤S2的反应釜中,在真空条件下以200rpm的速度搅拌30分钟,在避光和氮气保护下快速出料并抽真空至铝管中密封保存。
实施例2
用于智能穿戴的聚氨酯热熔胶的制备:
S1、按照以下质量百分比准备各原料:
氟改性聚氨酯丙烯酸酯F-2 50%;
结晶性聚氨酯PU-1 47%;
光引发剂2%;
硅烷偶联剂1%;
S2、将氟改性聚氨酯丙烯酸酯F-2、结晶性聚氨酯PU-1以及硅烷偶联剂KH550加入反应釜中,在真空条件下以200rpm的速度搅拌60分钟;
S3、在避光条件下,将光引发剂Irgacure 819加入步骤S2的反应釜中,在真空条件下以200rpm的速度搅拌30分钟,在避光和氮气保护下快速出料并抽真空至铝管中密封保存。
实施例3
用于智能穿戴的聚氨酯热熔胶的制备:
S1、按照以下质量百分比准备各原料:
氟改性聚氨酯丙烯酸酯F-3 50%;
结晶性聚氨酯PU-1 47%;
光引发剂2%;
硅烷偶联剂1%;
S2、将氟改性聚氨酯丙烯酸酯F-3、结晶性聚氨酯PU-1以及硅烷偶联剂KH550加入反应釜中,在真空条件下以200rpm的速度搅拌60分钟;
S3、在避光条件下,将光引发剂Irgacure 819加入步骤S2的反应釜中,在真空条件下以200rpm的速度搅拌30分钟,在避光和氮气保护下快速出料并抽真空至铝管中密封保存。
实施例4
用于智能穿戴的聚氨酯热熔胶的制备:
S1、按照以下质量百分比准备各原料:
氟改性聚氨酯丙烯酸酯F-2 40%;
结晶性聚氨酯PU-1 57%;
光引发剂2%;
硅烷偶联剂1%;
S2、将氟改性聚氨酯丙烯酸酯F-2、结晶性聚氨酯PU-1以及硅烷偶联剂KH550加入反应釜中,在真空条件下以200rpm的速度搅拌60分钟;
S3、在避光条件下,将光引发剂Irgacure 819加入步骤S2的反应釜中,在真空条件下以200rpm的速度搅拌30分钟,在避光和氮气保护下快速出料并抽真空至铝管中密封保存。
实施例5
用于智能穿戴的聚氨酯热熔胶的制备:
S1、按照以下质量百分比准备各原料:
氟改性聚氨酯丙烯酸酯F-2 60%;
结晶性聚氨酯PU-1 37%;
光引发剂2%;
硅烷偶联剂1%;
S2、将氟改性聚氨酯丙烯酸酯F-2、结晶性聚氨酯PU-1以及硅烷偶联剂KH550加入反应釜中,在真空条件下以200rpm的速度搅拌60分钟;
S3、在避光条件下,将光引发剂Irgacure 819加入步骤S2的反应釜中,在真空条件下以200rpm的速度搅拌30分钟,在避光和氮气保护下快速出料并抽真空至铝管中密封保存。
实施例6
用于智能穿戴的聚氨酯热熔胶的制备:
S1、按照以下质量百分比准备各原料:
氟改性聚氨酯丙烯酸酯F-2 50%;
结晶性聚氨酯PU-2 47%;
光引发剂2%;
硅烷偶联剂1%;
S2、将氟改性聚氨酯丙烯酸酯F-2、结晶性聚氨酯PU-2以及硅烷偶联剂KH550加入反应釜中,在真空条件下以200rpm的速度搅拌60分钟;
S3、在避光条件下,将光引发剂Irgacure 819加入步骤S2的反应釜中,在真空条件下以200rpm的速度搅拌30分钟,在避光和氮气保护下快速出料并抽真空至铝管中密封保存。
对比例1
用于智能穿戴的聚氨酯热熔胶的制备:
S1、按照以下质量百分比准备各原料:
结晶性聚氨酯PU-1 97%;
光引发剂2%;
硅烷偶联剂1%;
S2、将结晶性聚氨酯PU-1以及硅烷偶联剂KH550加入反应釜中,在真空条件下以200rpm的速度搅拌60分钟;
S3、在避光条件下,将光引发剂Irgacure 819加入步骤S2的反应釜中,在真空条件下以200rpm的速度搅拌30分钟,在避光和氮气保护下快速出料并抽真空至铝管中密封保存。
对比例2
用于智能穿戴的聚氨酯热熔胶的制备:
S1、按照以下质量百分比准备各原料:
氟改性聚氨酯丙烯酸酯F-2 97%;
光引发剂2%;
硅烷偶联剂1%;
S2、将氟改性聚氨酯丙烯酸酯F-2以及硅烷偶联剂KH550加入反应釜中,在真空条件下以200rpm的速度搅拌60分钟;
S3、在避光条件下,将光引发剂Irgacure 819加入步骤S2的反应釜中,在真空条件下以200rpm的速度搅拌30分钟,在避光和氮气保护下快速出料并抽真空至铝管中密封保存。
对比例3
用于智能穿戴的聚氨酯热熔胶的制备:
S1、按照以下质量百分比准备各原料:
氟改性聚氨酯丙烯酸酯F-2 20%;
结晶性聚氨酯PU-1 77%;
光引发剂2%;
硅烷偶联剂1%;
S2、将氟改性聚氨酯丙烯酸酯F-2、结晶性聚氨酯PU-1以及硅烷偶联剂KH550加入反应釜中,在真空条件下以200rpm的速度搅拌60分钟;
S3、在避光条件下,将光引发剂Irgacure 819加入步骤S2的反应釜中,在真空条件下以200rpm的速度搅拌30分钟,在避光和氮气保护下快速出料并抽真空至铝管中密封保存。
样品制备与性能测试:
拉伸剪切性能测试:将实施例1-6,对比例1-3的聚氨酯热熔胶通过针头加热130℃,胶管加热100℃,出胶压力0.4Mpa,点胶至透明PET上,每块PET的尺寸为100mm(长)/25mm(宽)/1.5mm(厚),每块被粘试片的整个宽度上涂胶,涂胶长度为12.5mm,涂胶典型厚度为0.2mm,PET试片两两粘接,确保两粘接试片精确对齐,尽可能使胶层厚度均匀一致。将试片在波长为350-400nm的紫外光光源下,曝光10s后,自然放置24h后参照GB/T 7124-2008测试剪切强度。
防水性能测试:将实施例1-6,对比例1-3的聚氨酯热熔胶通过针头加热130℃,胶管加热100℃,出胶压力0.4Mpa,点胶至梳型电路板(尺寸75mm×38mm×1mm)表面,涂胶典型厚度为0.2mm,尽可能使胶层厚度均匀一致。将上述试片在波长为350-400nm的紫外光光源下,曝光10s后,自然放置24h后待测得到相应试样。
将上述试样通过导线连接直流电源,额定电压为15V,再将连有导线的试样放入水深3m的透明圆柱管中,开始计时,当用万用表监测到电路电流突然增大时,停止计时,记录该时间。
剪切强度和防水性能具体见表1。
表1
对比表1中实施例1-6和对比例1-2可知,氟改性聚氨酯丙烯酸酯和结晶性聚氨酯具有协同作用,二者复配共同改善了聚氨酯热熔胶的粘结性能和防水性能,体现为拉伸剪切强度和防水时间的提高。
对比表1中实施例2,4-5以及对比例3可知,随着聚氨酯热熔胶中氟改性聚氨酯丙烯酸酯含量的增加,热熔胶的粘结性能和防水性能有上升的趋势,在氟改性聚氨酯丙烯酸酯含量为50%时最佳,说明热熔胶中引入光固化链段和含氟链段带来了粘结力和防水性能的提高。
对比表1中实施例1-6可知,氟改性聚氨酯丙烯酸酯中柔性链段的长度增加增大了链段旋转能力,带来了热熔胶粘结强度的提高,结晶性聚氨酯中选择柔性链段较刚性链段对粘结强度的贡献更大。
最后需要说明的是,以上实施例仅用以说明本发明实施例的技术方案而非对其进行限制,尽管参照较佳实施例对本发明实施例进行了详细的说明,本领域的普通技术人员应当理解依然可以对本发明实施例的技术方案进行修改或者等同替换,而这些修改或者等同替换亦不能使修改后的技术方案脱离本发明实施例技术方案的范围。
Claims (6)
1.一种用于智能穿戴的聚氨酯热熔胶,其特征在于,由如下组分及其质量百分含量组成:
氟改性聚氨酯丙烯酸酯30-60%;
结晶性聚氨酯30-60%;
光引发剂0.5-5%;
硅烷偶联剂0.5-5%;
所述氟改性聚氨酯丙烯酸酯是由含氟二醇、二异氰酸酯和(甲基)丙烯酸羟基酯在催化剂的存在下制备得到;所述结晶性聚氨酯是由结晶性聚酯多元醇、二异氰酸酯在催化剂的存在下制备得到;
所述含氟二醇选自以下物质中的一种或多种:2,2,3,3-四氟-1,4-丁二醇、2,2,3,3,4,4-六氟-1,5-戊烷二醇、2,2,3,3,4,4,5,5-八氟-1,6-己二醇、十二氟-1,8-辛二醇、全氟-1,9-壬烷二醇、全氟-1,10-癸二醇、六氟双酚A、全氟聚醚二醇;
所述二异氰酸酯选自以下物质中的一种或多种:异佛尔酮二异氰酸酯(IPDI)、萘1,5-二异氰酸酯(NDI)、亚甲基双环己基异氰酸酯、亚甲基二苯基二异氰酸酯(MDI)、甲苯二异氰酸酯(TDI)、六亚甲基二异氰酸酯(HDI)、亚二甲苯基二异氰酸酯、氢化亚二甲苯基二异氰酸酯、四甲基亚二甲苯基二异氰酸酯、对亚苯基二异氰酸酯、3,3'-二甲基二苯基-4,4'-二异氰酸酯(DDDI)、2,2,4-三甲基六亚甲基二异氰酸酯(TMDI)、降冰片烷二异氰酸酯(NDI)、4,4'-二苄基二异氰酸酯(DBDI);
所述(甲基)丙烯酸羟基酯选自以下物质中的一种或多种:(甲基)丙烯酸羟甲酯、(甲基)丙烯酸羟乙酯、(甲基)丙烯酸羟丙酯、(甲基)丙烯酸羟丁酯;
所述结晶性聚酯多元醇选自以下物质中的一种或多种:聚己二酸己二醇酯、聚对苯二甲酸己二醇酯、聚十二烷二酸己二醇酯、聚己二酸-对苯二甲酸-丁二醇酯、聚己二酸一缩二乙二醇酯、聚己内酯二元醇;
所述催化剂选自以下物质中的一种或多种:二月桂酸二丁基锡、辛酸亚锡、乙酸二丁烯、三乙烯二胺、双吗啉基二乙基醚;
基于二异氰酸酯的量,催化剂以0.005至3.5重量%的量存在;所述含氟二醇、二异氰酸酯和(甲基)丙烯酸羟基酯的摩尔比为1:2:2;所述结晶性聚酯多元醇、二异氰酸酯的摩尔比为1:1。
2.根据权利要求1所述的聚氨酯热熔胶,其特征在于,所述硅烷偶联剂选自以下物质中的一种或多种:氨丙基三乙氧基硅烷、γ-巯丙基三甲氧基硅烷、缩水甘油醚氧丙基三甲氧基硅烷;
所述光引发剂选自以下物质中的一种或多种:2-羟基-2-甲基-1-苯基-1-丙酮、二苯基(2,4,6-三苯基苯甲酰基)-氧化膦、2-苄基-二甲基氨基-1-(4-吗啉基苯基)-丁-1-酮、苯偶姻二甲基缩酮二甲氧基苯乙酮、α-羟基苄基苯基酮、1-羟基-1-甲基乙基苯基酮、寡-2-羟基-2-甲基-1-(4-(1-甲基乙烯基)苯基)丙酮、二苯甲酮;邻苄基苯甲酸甲酯;苯甲酰甲酸甲酯、2-二乙氧基苯乙酮、2,2-二仲丁氧基苯乙酮、对苯基二苯甲酮、2-异丙基噻吨酮、2-甲基蒽酮、2-乙基蒽酮、2-氯蒽酮、1,2-苯并蒽酮、苯甲酰醚、苯偶姻醚、苯偶姻甲基醚;苯偶姻异丙基醚、α-苯基苯偶姻、噻吨酮、二乙基噻吨酮、1,5-萘乙酮、1-羟基环己基苯基酮、对二甲基氨基苯甲酸乙酯。
3.根据权利要求1所述的聚氨酯热熔胶,其特征在于,所述氟改性聚氨酯丙烯酸酯具体通过如下步骤制得:
在惰性气体保护下的容器中,加入含氟二醇,在100-110℃真空脱水后,温度降为70-90℃,再加入二异氰酸酯和催化剂,70-90℃反应2-6h;再加入(甲基)丙烯酸羟基酯,降温至80-85℃下反应2-5h,得到氟改性聚氨酯丙烯酸酯;
所述结晶性聚氨酯具体通过如下步骤制得:
在惰性气体保护下的容器中,加入结晶性聚酯多元醇,在100-130℃真空脱水后,温度降至70-80℃;再加入异氰酸酯和催化剂,升温至120-160℃反应2-5小时,得到结晶性聚氨酯。
4.一种权利要求1-3任一项所述用于智能穿戴的聚氨酯热熔胶的制备方法,包括如下步骤:
S1、按配方称取各组分原料;
S2、将氟改性聚氨酯丙烯酸酯、结晶性聚氨酯以及硅烷偶联剂加入反应釜中,在真空条件下以100-200rpm的速度搅拌30-60分钟;
S3、在避光条件下,将光引发剂加入步骤S2的反应釜中,在真空条件下以100-200rpm的速度搅拌20-60分钟,在避光和氮气保护下快速出料并抽真空密封保存,即得所述用于智能穿戴的聚氨酯热熔胶。
5.一种权利要求1-3任一项所述用于智能穿戴的聚氨酯热熔胶在智能穿戴领域中的应用。
6.一种权利要求1-3任一项所述用于智能穿戴的聚氨酯热熔胶在改善智能穿戴领域热熔胶粘结强度和防水性能方面的应用。
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