CN112795001A - 低模量硅烷改性聚醚及其制备方法与应用 - Google Patents
低模量硅烷改性聚醚及其制备方法与应用 Download PDFInfo
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- CN112795001A CN112795001A CN202011603803.8A CN202011603803A CN112795001A CN 112795001 A CN112795001 A CN 112795001A CN 202011603803 A CN202011603803 A CN 202011603803A CN 112795001 A CN112795001 A CN 112795001A
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- polyether
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- modified polyether
- silane
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- 239000004526 silane-modified polyether Substances 0.000 title claims abstract description 74
- 238000002360 preparation method Methods 0.000 title claims description 25
- 239000004721 Polyphenylene oxide Substances 0.000 claims abstract description 71
- 229920000570 polyether Polymers 0.000 claims abstract description 71
- 239000003054 catalyst Substances 0.000 claims abstract description 21
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000003063 flame retardant Substances 0.000 claims abstract description 20
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910000077 silane Inorganic materials 0.000 claims abstract description 16
- 239000003999 initiator Substances 0.000 claims abstract description 10
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 claims abstract description 9
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical compound CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 claims abstract description 9
- 230000001588 bifunctional effect Effects 0.000 claims abstract description 9
- 238000000034 method Methods 0.000 claims abstract description 6
- 238000011033 desalting Methods 0.000 claims abstract description 5
- 238000004519 manufacturing process Methods 0.000 claims abstract description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000001257 hydrogen Substances 0.000 claims abstract description 4
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 4
- 238000006459 hydrosilylation reaction Methods 0.000 claims abstract description 4
- 239000000565 sealant Substances 0.000 claims description 57
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 28
- 238000006243 chemical reaction Methods 0.000 claims description 28
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 20
- 239000000945 filler Substances 0.000 claims description 15
- 239000003963 antioxidant agent Substances 0.000 claims description 14
- 230000003078 antioxidant effect Effects 0.000 claims description 14
- 239000004611 light stabiliser Substances 0.000 claims description 14
- 229910052757 nitrogen Inorganic materials 0.000 claims description 14
- 239000004014 plasticizer Substances 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 12
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 12
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 12
- 239000013008 thixotropic agent Substances 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 239000002250 absorbent Substances 0.000 claims description 11
- 230000002745 absorbent Effects 0.000 claims description 11
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 10
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 8
- 239000002253 acid Substances 0.000 claims description 8
- OSDWBNJEKMUWAV-UHFFFAOYSA-N Allyl chloride Chemical compound ClCC=C OSDWBNJEKMUWAV-UHFFFAOYSA-N 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 7
- 238000009489 vacuum treatment Methods 0.000 claims description 7
- KEAYESYHFKHZAL-UHFFFAOYSA-N Sodium Chemical compound [Na] KEAYESYHFKHZAL-UHFFFAOYSA-N 0.000 claims description 6
- 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 6
- LJCFOYOSGPHIOO-UHFFFAOYSA-N antimony pentoxide Chemical compound O=[Sb](=O)O[Sb](=O)=O LJCFOYOSGPHIOO-UHFFFAOYSA-N 0.000 claims description 6
- 239000012975 dibutyltin dilaurate Substances 0.000 claims description 6
- PKTOVQRKCNPVKY-UHFFFAOYSA-N dimethoxy(methyl)silicon Chemical compound CO[Si](C)OC PKTOVQRKCNPVKY-UHFFFAOYSA-N 0.000 claims description 6
- 239000012312 sodium hydride Substances 0.000 claims description 6
- 229910000104 sodium hydride Inorganic materials 0.000 claims description 6
- 239000004952 Polyamide Substances 0.000 claims description 5
- 239000003153 chemical reaction reagent Substances 0.000 claims description 5
- 229920002647 polyamide Polymers 0.000 claims description 5
- 229920001451 polypropylene glycol Polymers 0.000 claims description 5
- YSMRWXYRXBRSND-UHFFFAOYSA-N TOTP Chemical compound CC1=CC=CC=C1OP(=O)(OC=1C(=CC=CC=1)C)OC1=CC=CC=C1C YSMRWXYRXBRSND-UHFFFAOYSA-N 0.000 claims description 4
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 4
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 4
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims description 4
- 239000000347 magnesium hydroxide Substances 0.000 claims description 4
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims description 4
- 229920002545 silicone oil Polymers 0.000 claims description 4
- 239000004408 titanium dioxide Substances 0.000 claims description 4
- YUYCVXFAYWRXLS-UHFFFAOYSA-N trimethoxysilane Chemical compound CO[SiH](OC)OC YUYCVXFAYWRXLS-UHFFFAOYSA-N 0.000 claims description 4
- XZZNDPSIHUTMOC-UHFFFAOYSA-N triphenyl phosphate Chemical compound C=1C=CC=CC=1OP(OC=1C=CC=CC=1)(=O)OC1=CC=CC=C1 XZZNDPSIHUTMOC-UHFFFAOYSA-N 0.000 claims description 4
- BIKXLKXABVUSMH-UHFFFAOYSA-N trizinc;diborate Chemical compound [Zn+2].[Zn+2].[Zn+2].[O-]B([O-])[O-].[O-]B([O-])[O-] BIKXLKXABVUSMH-UHFFFAOYSA-N 0.000 claims description 4
- JVUAOHHLYDUVMM-UHFFFAOYSA-N C(CCCCCCC)OC(CCCCCCCCC)=O.[Bi] Chemical compound C(CCCCCCC)OC(CCCCCCCCC)=O.[Bi] JVUAOHHLYDUVMM-UHFFFAOYSA-N 0.000 claims description 3
- MQIUGAXCHLFZKX-UHFFFAOYSA-N Di-n-octyl phthalate Natural products CCCCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCCC MQIUGAXCHLFZKX-UHFFFAOYSA-N 0.000 claims description 3
- ZVFDTKUVRCTHQE-UHFFFAOYSA-N Diisodecyl phthalate Chemical compound CC(C)CCCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCCC(C)C ZVFDTKUVRCTHQE-UHFFFAOYSA-N 0.000 claims description 3
- BJQHLKABXJIVAM-UHFFFAOYSA-N bis(2-ethylhexyl) phthalate Chemical compound CCCCC(CC)COC(=O)C1=CC=CC=C1C(=O)OCC(CC)CCCC BJQHLKABXJIVAM-UHFFFAOYSA-N 0.000 claims description 3
- HBGGXOJOCNVPFY-UHFFFAOYSA-N diisononyl phthalate Chemical compound CC(C)CCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCC(C)C HBGGXOJOCNVPFY-UHFFFAOYSA-N 0.000 claims description 3
- UQEAIHBTYFGYIE-UHFFFAOYSA-N hexamethyldisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)C UQEAIHBTYFGYIE-UHFFFAOYSA-N 0.000 claims description 3
- UEZVMMHDMIWARA-UHFFFAOYSA-M phosphonate Chemical compound [O-]P(=O)=O UEZVMMHDMIWARA-UHFFFAOYSA-M 0.000 claims description 3
- BDAWXSQJJCIFIK-UHFFFAOYSA-N potassium methoxide Chemical compound [K+].[O-]C BDAWXSQJJCIFIK-UHFFFAOYSA-N 0.000 claims description 3
- 239000007858 starting material Substances 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- ADJMNWKZSCQHPS-UHFFFAOYSA-L zinc;6-methylheptanoate Chemical compound [Zn+2].CC(C)CCCCC([O-])=O.CC(C)CCCCC([O-])=O ADJMNWKZSCQHPS-UHFFFAOYSA-L 0.000 claims description 3
- 239000000440 bentonite Substances 0.000 claims description 2
- 229910000278 bentonite Inorganic materials 0.000 claims description 2
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims description 2
- LPNYRYFBWFDTMA-UHFFFAOYSA-N potassium tert-butoxide Chemical compound [K+].CC(C)(C)[O-] LPNYRYFBWFDTMA-UHFFFAOYSA-N 0.000 claims description 2
- 239000011787 zinc oxide Substances 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims 1
- 238000010276 construction Methods 0.000 claims 1
- 238000007789 sealing Methods 0.000 abstract description 10
- 239000000463 material Substances 0.000 abstract description 7
- 238000011084 recovery Methods 0.000 abstract description 5
- 230000008569 process Effects 0.000 abstract description 3
- 230000009471 action Effects 0.000 abstract description 2
- 230000032683 aging Effects 0.000 abstract description 2
- 238000010924 continuous production Methods 0.000 abstract description 2
- 238000003860 storage Methods 0.000 abstract description 2
- 238000005937 allylation reaction Methods 0.000 abstract 1
- 238000005265 energy consumption Methods 0.000 abstract 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 8
- 238000002156 mixing Methods 0.000 description 6
- MKPXGEVFQSIKGE-UHFFFAOYSA-N [Mg].[Si] Chemical compound [Mg].[Si] MKPXGEVFQSIKGE-UHFFFAOYSA-N 0.000 description 5
- 239000003463 adsorbent Substances 0.000 description 5
- 238000011049 filling Methods 0.000 description 5
- 238000001914 filtration Methods 0.000 description 5
- 238000001179 sorption measurement Methods 0.000 description 5
- 150000001335 aliphatic alkanes Chemical class 0.000 description 4
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 4
- 238000006073 displacement reaction Methods 0.000 description 4
- 230000003472 neutralizing effect Effects 0.000 description 4
- 238000011161 development Methods 0.000 description 3
- 230000018109 developmental process Effects 0.000 description 3
- 238000000576 coating method Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- KXDHJXZQYSOELW-UHFFFAOYSA-M Carbamate Chemical compound NC([O-])=O KXDHJXZQYSOELW-UHFFFAOYSA-M 0.000 description 1
- XFXPMWWXUTWYJX-UHFFFAOYSA-N Cyanide Chemical compound N#[C-] XFXPMWWXUTWYJX-UHFFFAOYSA-N 0.000 description 1
- 239000006096 absorbing agent Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 150000004703 alkoxides Chemical class 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 239000004588 polyurethane sealant Substances 0.000 description 1
- 239000002987 primer (paints) Substances 0.000 description 1
- 239000004590 silicone sealant Substances 0.000 description 1
- 230000035882 stress Effects 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
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- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/02—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
- C08G65/26—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds
- C08G65/2603—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing oxygen
- C08G65/2606—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing oxygen containing hydroxyl groups
- C08G65/2609—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing oxygen containing hydroxyl groups containing aliphatic hydroxyl groups
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- C08G65/32—Polymers modified by chemical after-treatment
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- C08G65/32—Polymers modified by chemical after-treatment
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- C08G65/32—Polymers modified by chemical after-treatment
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Abstract
本发明提供一种低模量硅烷改性聚醚,其包括以下结构式I和结构式II:其中,R为‑CH3,R1和R2为‑H或‑CH3,R3为C10‑C18烷烃,a为80~500,b为60~300,n为2或3。所述低模量硅烷改性聚醚首先由单官能度聚醚和双官能度聚醚为混合起始剂,在双金属络合催化剂作用下,与环氧丙烷反应获得特殊结构聚醚;然后通过烯丙基化反应,精致除盐获得烯丙基封端聚醚;再与含氢硅烷进行硅氢加成反应,制得低模量硅烷改性聚醚。本发明的低模量硅烷改性聚醚与现有技术比,具有更高弹性恢复率、更低模量,且具有优异密封及粘接性能、阻燃性能、耐老化性能和储存稳定性,采用连续化生产工艺,生产效率高、物耗能耗低、性能更稳定。
Description
技术领域
本发明涉及密封胶技术领域,尤其涉及一种低模量硅烷改性聚醚及其制备方法、以及应用所述硅烷改性聚醚的密封胶及其制备方法与应用。
背景技术
随着国家对装配式建筑的大力支持和推广,以及各地相关政策与标准的相继持续出台,我国装配式建筑逐步进步快速发展阶段,且正在逐渐变大。相比传统建筑模式,装配式建筑模式具有节能环保、生产效率高等优点。密封胶作为装配式建筑最主要的嵌缝密封材料,主要应用于各种构件之间,尤其是预制外墙板(PC墙板)间的连接和密封,随之也迎来快速发展期。
密封胶作为装配式建筑的密封及防水材料,其质量直接影响装配式建筑的品质,所以装配式建筑领域对密封胶提出系列要求:(1)粘接性和位移能力:混凝土表面疏松多孔,有效粘结面积减小,且拼接处要承受较大位移应力普通密封胶无法满足性能要求。此外,混凝土属于碱性材料,在多雨湿度较大地区,可能出现反碱现象,可能导致粘结界面破坏,所以装配式建筑用密封胶要有优异的粘接性能和抗位移能力。(2)耐候性:装配式建筑用密封胶直接暴露在户外环境下,长期受阳光照射和雨水冲刷,所以要求密封胶具有良好的耐候性能。(3)可涂装性:对于需要涂饰的预制墙面,密封胶还需要具备优良的可涂饰性,要求密封胶与涂料具有良好的相容性,可直接涂饰。
装配式建筑常用密封胶主要有硅酮(SR)建筑密封胶、聚氨酯(PU)建筑密封胶和硅烷改性聚醚(MS)建筑密封胶。硅酮密封胶具有良好的耐候性能和回弹性,但对混凝土的粘接性能和可涂饰性差;聚氨酯密封胶对混凝土的粘结效果和表面可涂饰性能优异,但耐候性能较差,易黄变开裂;硅烷改性聚醚密封胶具有较好的混凝土粘接性、表面可涂饰性和耐候性能等,是我国装配式密封胶的主流产品。但随着行业不断发展,装配式建筑对更低模量、更高回弹性能,以及密封胶的阻燃性、施工性等综合性能提出更高的要求。
鉴于此,迫切需要开发一种更低模量、更高弹性恢复率、综合性能优异的硅烷改性聚醚及其密封胶。
发明内容
基于以上现有技术的不足,本发明旨在于提供一种具有低模量以及高弹性恢复率的硅烷改性聚醚及其制备方法、以及应用所述硅烷改性聚醚的密封胶及其制备方法。
为实现上述目的,本发明一实施方式提供一种低模量硅烷改性聚醚,其包括以下结构式I和结构式II:
其中,R为-CH3,R1和R2为-H或-CH3,R3为C10-C18烷烃,a为80~500,b为60~300,n为2或3。
本发明一实施方式还提供上述低模量硅烷改性聚醚的一种制备方法,其包括以下步骤:
(1)特殊结构聚醚的制备:向反应釜中加入包括单官能度聚醚和双官能度聚醚的混合起始剂以及DMC催化剂,持续通入环氧丙烷反应得到特殊结构聚醚;
(2)烯丙基封端聚醚的制备:将所述特殊结构聚醚及醇盐化试剂在氮气保护下进行醇盐化反应,然后加入烯丙基氯混合反应,再进行精致除盐得到烯丙基封端聚醚;
(3)硅烷改性聚醚的制备:在氮气保护下,向所述烯丙基封端聚醚中加入氯铂酸溶液,然后加入含氢硅烷进行硅氢加成反应,然后减压脱除未反应的硅烷,制得所述硅烷改性聚醚;
其中,所述混合起始剂包括以下结构式III和结构式IV:
所述特殊结构聚醚包括以下结构式V和结构式VI:
所述烯丙基封端聚醚包括如下结构式VII和结构式VIII:
其中,c为6~12,d为10~18。
本发明一实施方式还提供一种低模量硅烷改性聚醚密封胶,其由以下重量份的物质组成:上述低模量硅烷改性聚醚25~40份、填料40~60份、增塑剂15~30份、触变剂2~5份、阻燃剂1~10份、吸水剂1~5份、硅烷偶联剂0.5~5份、光稳定剂0.5~2份、抗氧化剂0.5~2份、催化剂0.2~2份。
本发明一实施方式还提供一种上述低模量硅烷改性聚醚密封胶的制备方法,其包括以下步骤:按各组分的计量配比,先将所述硅烷改性聚醚、所述填料、所述增塑剂、所述触变剂、所述阻燃剂、所述光稳定剂和所述抗氧化剂于50-90℃下真空处理1~2h,再高速分散0.5~1h;然后降温至30~40℃加入吸水剂、硅烷偶联剂和催化剂,真空高速分散0.2~0.5h,制得所述硅烷改性聚醚密封胶。
本发明一实施方式还提供一种上述硅烷改性聚醚密封胶的应用,所述硅烷改性聚醚密封胶应用于装配式建筑、汽车和集装箱领域。
与现有技术相比,本发明的硅烷改性聚醚及其密封胶具有如下优点:
一、本发明的硅烷改性聚醚是单官能度和双官能度聚醚制备的复合型产品,单官能度结构的引入可有效降低模量、提升弹性。此外,分子量越高,弹性越好;分子量越低,强度越高;通过对硅烷改性聚醚的结构多方面设计,有效提升了产品的弹性恢复率、抗位移能力和粘接性能。另外,本发明的硅烷改性聚醚不含氨基甲酸酯,绿色环保。
二、本发明的硅烷改性聚醚密封胶,采用阻燃填料和阻燃剂协同作用,具有优异的阻燃性能,可达FV-0等级,适用于对阻燃性能有高要求的粘接和密封场合。同时,搭配抗氧化剂和光稳定剂使用,赋予密封胶优异的耐温性能和耐老化性能,应用范围更广泛。
三、本发明实现了硅烷改性聚醚及其密封胶连续化生产工艺,有效减少水分和湿气对产品品质的影响,生产效率更高、品质更稳定。密封胶制备过程中,填料无需预先热处理,采用与增塑剂、阻燃剂、光稳定剂和抗氧化剂等混合处理工艺,分散效果更佳,可有效提升密封胶的储存稳定性和深层固化性能,且无底涂工艺下具有优异粘接强度。
具体实施方式
下面结合实施例对本发明作进一步说明,但不以任何方式限制本发明。
本发明一实施方式提供一种低模量硅烷改性聚醚,所述低模量硅烷改性聚醚包括以下结构式I和结构式II:
式中,R为-CH3,R1和R2为-H或-CH3,R3为C10-C18烷烃,a为80~500,b为60~300,n为2或3。
本发明一实施方式还提供一种低模量硅烷改性聚醚的制备方法,其包括以下步骤:
(1)特殊结构聚醚的制备:向反应釜中加入包括单官能度聚醚和双官能度聚醚的混合起始剂和双金属氰化络合物(DMC)催化剂,持续通入环氧丙烷反应得到特殊结构聚醚;
(2)烯丙基封端聚醚的制备:将所述特殊结构聚醚及醇盐化试剂在氮气保护下进行醇盐化反应,然后加入烯丙基氯混合反应,在进行精致除盐得到烯丙基封端聚醚;
(3)硅烷改性聚醚的制备:在氮气保护下,向所述烯丙基封端聚醚中加入氯铂酸溶液,然后加入含氢硅烷进行硅氢加成反应,然后减压脱除未反应的硅烷,制得所述硅烷改性聚醚。
其中,所述混合起始剂包括以下结构式III和结构式IV:
所述特殊结构聚醚包括以下结构式V和结构式VI:
所述烯丙基封端聚醚包括如下结构式VII和结构式VIII:
式中,R1和R2为-H或-CH3,R3为C10-C18烷烃,c为6~12,d为10~18,a为80~500,b为60~300。
步骤(1)中,反应温度可为90~140℃,所述环氧丙烷在所述反应釜升温到反应温度后通入所述反应釜中,在所述DMC催化剂作用下,与所述混合起始剂进行反应。可选的,所述混合起始剂的分子量为400~1200g·mol-1。
步骤(2)中,步骤(1)得到的特殊结构聚醚输送至另一反应釜中与所述醇盐化试剂进行反应,其中,醇盐化反应的反应温度可控制在100~130℃,反应时间可控制在6~7h;混合反应时,所述反应釜中的压力控制在0.3~0.5MPa,反应温度控制在60~70℃,反应时间控制在5~7h。在一些实施方式中,所述醇盐化试剂包括叔丁醇钾、氢化钠、甲醇钾及氢氧化钾中的至少一种。
可选的,步骤(2)中的精致除盐包括:加入酸溶液进行中和至pH值为4~6,然后加入硅镁吸附剂进行吸附和过滤,从而得到所述烯丙基封端聚醚。
在一些实施方式中,所述含氢硅烷可以为但不限于甲基二甲氧基硅烷、三甲氧基硅烷中至少一种。
本发明一实施方式还提供一种低模量硅烷改性聚醚密封胶,其由以下重量份的物质组成:低模量硅烷改性聚醚25~40份、填料40~60份、增塑剂15~30份、触变剂2~5份、阻燃剂1~10份、吸水剂1~5份、硅烷偶联剂0.5~5份、光稳定剂0.5~2份、抗氧化剂0.5~2份、催化剂0.2~2份。所述硅烷改性密封胶应用于装配式建筑、汽车和集装箱领域。
在一些实施方式中,所述填料包括纳米碳酸钙、重质碳酸钙、钛白粉、氢氧化铝、氢氧化镁中至少两种。
在一些实施方式中,所述增塑剂包括邻苯二甲酸二辛酯、邻苯二甲酸二异壬酯、邻苯二甲酸二异癸酯、聚丙二醇中至少一种。
在一些实施方式中,所述触变剂包括聚酰胺蜡、有机膨润土、羟基硅油中至少一种。
在一些实施方式中,所述阻燃剂包括磷酸三苯酯、磷酸三甲苯酯、膦酸三丁酯、五氧化二锑、硼酸锌、氧化锌中至少两种。
在一些实施方式中,所述吸水剂包括KH171、KH151、KH-3112、HMDSO中至少一种。
在一些实施方式中,所述光稳定剂包括326、329、770、765中至少一种。
在一些实施方式中,所述抗氧化剂包括1010、1035、1076、245、168中至少一种。
在一些实施方式中,所述硅烷偶联剂包括KH 540、KH 550、KH 560、KH 792、1146中至少一种。
在一些实施方式中,所述催化剂包括二月桂酸二丁基锡、异辛酸锌、辛癸酸铋中至少一种。
本发明一实施方式还提供一种低模量硅烷改性聚醚密封胶的制备方法,其包括以下步骤:按各组分的计量配比,先将硅烷改性聚醚、填料、增塑剂、触变剂、阻燃剂、光稳定剂和抗氧化剂于50~90℃下真空处理1~2h,再高速分散0.5~1h;然后降温至30~40℃加入吸水剂、硅烷偶联剂和催化剂,真空高速分散0.2~0.5h,灌装密封储存,制得所述硅烷改性聚醚密封胶。
下面通过实施例对本发明的低模量硅烷改性聚醚及其密封胶的制备及其性能进行具体说明。
实施例1
(1)特殊结构聚醚的制备:向反应釜中加入包括22g单官能度C10烷烃聚醚和10g双官能度聚醚的混合起始剂(羟值约为178mgKOH/g)以及0.12gDMC催化剂,于90~140℃下通入968g环氧丙烷反应得到特殊结构聚醚(羟值约为5mgKOH/g);
(2)烯丙基封端聚醚的制备:将所得特殊结构聚醚及4.6g质量分数为60%的氢化钠,在氮气保护下于100~130℃进行醇盐化反应6~7h;然后加入8.75g烯丙基氯,在0.3~0.5MPa、60~70℃下混合反应5~7h,经磷酸中和至pH值4.0~6.0,再加入60g硅镁吸附剂进行吸附和过滤,得到所述烯丙基封端聚醚;
(3)硅烷改性聚醚的制备:在氮气保护下,向将所得烯丙基封端聚醚中加入0.035g氯铂酸溶液,然后加入11.8g甲基二甲氧基硅烷,于50~90℃反应1~5h,然后减压脱除未反应的硅烷,制得所述硅烷改性聚醚;
(4)硅烷改性密封胶的制备:按照如下组分配比进行备料,其中各组分的重量份为:25份硅烷改性聚醚、50份重质碳酸钙、2份钛白粉、3份氢氧化铝、25份邻苯二甲酸二异壬酯、2份羟基硅油、5份磷酸三苯酯、5份磷酸三甲苯酯、2份KH171、0.5份KH 792、0.3份KH560、0.3份326、0.2份765、0.8份1010、0.2份二月桂酸二丁基锡;将硅烷改性聚醚、填料、增塑剂、触变剂、阻燃剂、光稳定剂和抗氧化剂于50~90℃下真空处理1~2h,再高速分散0.5~1h;降温至30~40℃加入吸水剂、硅烷偶联剂和催化剂,真空高速分散0.2~0.5h,灌装密封储存,制得所述硅烷改性聚醚密封胶。
实施例2
(1)特殊结构聚醚的制备:向反应釜中加入包括28.6g单官能度C14烷烃聚醚和20g双官能度聚醚的混合起始剂(羟值约为134mgKOH/g)以及0.10gDMC催化剂,于90~140℃下通入951g环氧丙烷反应得到特殊结构聚醚(羟值约为5.3mgKOH/g);
(2)烯丙基封端聚醚的制备:将所得特殊结构聚醚、2.6g质量分数为60%的氢化钠和1.4g粉末状氢氧化钾,在氮气保护下于100~130℃进行醇盐化反应6~7h;然后加入9.3g烯丙基氯,在0.3~0.5MPa、60~70℃下混合反应5~7h,经磷酸中和至pH值4.0~6.0,再加入55g硅镁吸附剂进行吸附和过滤,得到所述烯丙基封端聚醚;
(3)硅烷改性聚醚的制备:在氮气保护下,向将所得烯丙基封端聚醚中加入0.04g氯铂酸溶液,然后加入12.37g甲基二甲氧基硅烷,于50~90℃反应1~5h,然后减压脱除未反应的硅烷,制得所述硅烷改性聚醚;
(4)硅烷改性密封胶的制备:按照如下组分配比进行备料,其中各组分的重量份为:25份硅烷改性聚醚、40份重质碳酸钙、2份轻质碳酸钙、3份氢氧化镁、25份聚丙二醇2000、2份聚酰胺蜡、3份羟基硅油、7份膦酸三丁酯、3份五氧化二锑、2份KH151、0.5份KH-3112、0.5份KH 792、0.2份1146、0.3份329、0.3份765、0.5份1076、0.5份168、0.15份二月桂酸二丁基锡、0.5份异辛酸锌;将硅烷改性聚醚、填料、增塑剂、触变剂、阻燃剂、光稳定剂和抗氧化剂于50~90℃下真空处理1~2h,再高速分散0.5~1h;降温至30~40℃加入吸水剂、硅烷偶联剂和催化剂,真空高速分散0.2~0.5h,灌装密封储存,制得所述硅烷改性聚醚密封胶。
实施例3
(1)特殊结构聚醚的制备:向反应釜中加入包括34.3g单官能度C16烷烃聚醚和10g双官能度聚醚的混合起始剂(羟值约为130mgKOH/g)以及0.08gDMC催化剂,于90~140℃下通入956g环氧丙烷反应得到特殊结构聚醚(羟值约为4.6mgKOH/g);
(2)烯丙基封端聚醚的制备:将所得特殊结构聚醚、2.78g质量分数为60%的氢化钠和2.1g甲醇钾,在氮气保护下于100~130℃进行醇盐化反应6~7h;然后加入7.87g烯丙基氯,在0.3~0.5MPa、60~70℃下混合反应5~7h,经磷酸中和至pH值4.0~6.0,再加入60g硅镁吸附剂进行吸附和过滤,得到所述烯丙基封端聚醚;
(3)硅烷改性聚醚的制备:在氮气保护下,向将所得烯丙基封端聚醚中加入0.032g氯铂酸溶液,然后加入5.3g甲基二甲氧基硅烷和6.2g三甲氧基硅烷,于50~90℃反应1~5h,然后减压脱除未反应的硅烷,制得所述硅烷改性聚醚;
(4)硅烷改性密封胶的制备:按照如下组分配比进行备料,其中各组分的重量份为:20份硅烷改性聚醚、40份重质碳酸钙、5份轻质碳酸钙、5份氢氧化铝、20份聚丙二醇3000、5份邻苯二甲酸二辛酯、2份聚酰胺蜡、2份有机膨润土、8份磷酸三苯酯、2份硼酸锌、1份KH171、1份HMDSO、0.5份KH 792、0.3份KH540、0.3份KH550、0.5份326、0.2份770、0.2份1035、0.2份245、0.2份二月桂酸二丁基锡;将硅烷改性聚醚、填料、增塑剂、触变剂、阻燃剂、光稳定剂和抗氧化剂于50~90℃下真空处理1~2h,再高速分散0.5~1h;降温至30~40℃加入吸水剂、硅烷偶联剂和催化剂,真空高速分散0.2~0.5h,灌装密封储存,制得所述硅烷改性聚醚密封胶。
实施例4
(1)特殊结构聚醚的制备:向反应釜中加入包括47.6g单官能度C16~18烷烃聚醚和11.6g双官能度聚醚的混合起始剂(羟值约为98mgKOH/g)以及0.06gDMC催化剂,于90~140℃下通入940g环氧丙烷反应得到特殊结构聚醚(羟值约为4.6mgKOH/g);
(2)烯丙基封端聚醚的制备:将所得特殊结构聚醚、3.45g质量分数为60%的氢化钠和1.1g粉末状氢氧化钾,在氮气保护下于100~130℃进行醇盐化反应6~7h;然后加入8.75g烯丙基氯,在0.3~0.5MPa、60~70℃下混合反应5~7h,经磷酸中和至pH值4.0~6.0,再加入70g硅镁吸附剂进行吸附和过滤,得到所述烯丙基封端聚醚;
(3)硅烷改性聚醚的制备:在氮气保护下,向将所得烯丙基封端聚醚中加入0.028g氯铂酸溶液,然后加入7.5g甲基二甲氧基硅烷和2.8g三甲氧基硅烷,于50~90℃反应1~5h,然后减压脱除未反应的硅烷,制得所述硅烷改性聚醚;
(4)硅烷改性密封胶的制备:按照如下组分配比进行备料,其中各组分的重量份为:硅烷改性聚醚30份、40份重质碳酸钙、2份钛白粉、3份氢氧化镁、15份聚丙二醇4000、10份邻苯二甲酸二异癸酯、2份聚酰胺蜡、6份磷酸三甲苯酯、4份硼酸锌、1.2份KH171、0.6份KH-3112、0.5份KH 792、0.5份1146、0.3份329、0.2份770、0.2份1010、0.4份1035、0.15份二月桂酸二丁基锡、0.1份辛癸酸铋;将硅烷改性聚醚、填料、增塑剂、触变剂、阻燃剂、光稳定剂和抗氧化剂于50~90℃下真空处理1~2h,再高速分散0.5~1h;降温至30~40℃加入吸水剂、硅烷偶联剂和催化剂,真空高速分散0.2~0.5h,灌装密封储存,制得所述硅烷改性聚醚密封胶。
将实施例1-4制得的硅烷改性聚醚以及硅烷改性聚醚密封胶进行性能测试,测试标准及测试结果如表1所示。
表1
从表1中可以看出各实施例的改性聚醚及其密封胶具有低粘度、易操作、施工性好,具有低模量、高弹性恢复率,且具有优异密封及粘接性能和阻燃性能,适用于对阻燃性能高要求的装配式建筑、汽车和集装箱等领域。
另外,本领域技术人员还可在本发明精神内做其它变化,当然,这些依据本发明精神所做的变化,都应包含在本发明所要求保护的范围内。
Claims (10)
2.如权利要求1所述的低模量硅烷改性聚醚的制备方法,其包括以下步骤:
(1)特殊结构聚醚的制备:向反应釜中加入包括单官能度聚醚和双官能度聚醚的混合起始剂以及DMC催化剂,持续通入环氧丙烷反应得到特殊结构聚醚;
(2)烯丙基封端聚醚的制备:将所述特殊结构聚醚及醇盐化试剂在氮气保护下进行醇盐化反应,然后加入烯丙基氯混合反应,再进行精致除盐得到烯丙基封端聚醚;
(3)硅烷改性聚醚的制备:在氮气保护下,向所述烯丙基封端聚醚中加入氯铂酸溶液,然后加入含氢硅烷进行硅氢加成反应,然后减压脱除未反应的硅烷,制得所述硅烷改性聚醚;
其中,所述混合起始剂包括以下结构式III和结构式IV:
所述特殊结构聚醚包括以下结构式V和结构式VI:
所述烯丙基封端聚醚包括如下结构式VII和结构式VIII:
其中,c为6~12,d为10~18。
3.如权利要求2所述的低模量硅烷改性聚醚的制备方法,其特征在于,所述醇盐化试剂为叔丁醇钾、氢化钠、甲醇钾及氢氧化钾中的至少一种。
4.如权利要求2所述的低模量硅烷改性聚醚的制备方法,其特征在于,所述含氢硅烷为甲基二甲氧基硅烷、三甲氧基硅烷中至少一种。
5.一种低模量硅烷改性聚醚密封胶,其由以下重量份的物质组成:如权利要求1所述的硅烷改性聚醚25~40份、填料40~60份、增塑剂15~30份、触变剂2~5份、阻燃剂1~10份、吸水剂1~5份、硅烷偶联剂0.5~5份、光稳定剂0.5~2份、抗氧化剂0.5~2份、催化剂0.2~2份。
6.如权利要求5所述的低模量硅烷改性聚醚密封胶,其特征在于,所述填料为纳米碳酸钙、重质碳酸钙、钛白粉、氢氧化铝、氢氧化镁中至少两种。
7.如权利要求5所述的低模量硅烷改性聚醚密封胶,其特征在于,所述阻燃剂为磷酸三苯酯、磷酸三甲苯酯、膦酸三丁酯、五氧化二锑、硼酸锌、氧化锌中至少两种。
8.如权利要求5所述的低模量硅烷改性聚醚密封胶,其特征在于,所述增塑剂为邻苯二甲酸二辛酯、邻苯二甲酸二异壬酯、邻苯二甲酸二异癸酯、聚丙二醇中至少一种;所述触变剂为聚酰胺蜡、有机膨润土、羟基硅油中至少一种;所述催化剂为二月桂酸二丁基锡、异辛酸锌、辛癸酸铋中至少一种;所述吸水剂为KH171、KH151、KH-3112、HMDSO中至少一种;所述光稳定剂为326、329、770、765中至少一种;所述抗氧化剂为1010、1035、1076、245、168中至少一种;所述硅烷偶联剂为KH 540、KH 550、KH 560、KH 792、1146中至少一种。
9.如权利要求5-8中任一种低模量硅烷改性聚醚密封胶的制备方法,其包括以下步骤:按各组分的计量配比,先将所述硅烷改性聚醚、所述填料、所述增塑剂、所述触变剂、所述阻燃剂、所述光稳定剂和所述抗氧化剂于50-90℃下真空处理1~2h,再高速分散0.5~1h;然后降温至30~40℃加入吸水剂、硅烷偶联剂和催化剂,真空高速分散0.2~0.5h,制得所述硅烷改性聚醚密封胶。
10.一种如权利要求5-8中任一项所述的低模量硅烷改性聚醚密封胶的应用,其特征在于,所述低模量硅烷改性密封胶应用于装配式建筑、汽车和集装箱领域。
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