CN111704726A - 一种聚硅氧烷乳液的制备方法 - Google Patents
一种聚硅氧烷乳液的制备方法 Download PDFInfo
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- CN111704726A CN111704726A CN202010637516.2A CN202010637516A CN111704726A CN 111704726 A CN111704726 A CN 111704726A CN 202010637516 A CN202010637516 A CN 202010637516A CN 111704726 A CN111704726 A CN 111704726A
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- Prior art keywords
- polysiloxane
- emulsion
- polyoxyethylene
- water
- catalyst
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- -1 polysiloxane Polymers 0.000 title claims abstract description 133
- 229920001296 polysiloxane Polymers 0.000 title claims abstract description 121
- 239000000839 emulsion Substances 0.000 title claims abstract description 73
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 57
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 27
- 239000003054 catalyst Substances 0.000 claims abstract description 22
- 239000004721 Polyphenylene oxide Substances 0.000 claims abstract description 21
- 229920000570 polyether Polymers 0.000 claims abstract description 21
- 239000004094 surface-active agent Substances 0.000 claims abstract description 11
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 20
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 20
- 239000000203 mixture Substances 0.000 claims description 15
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 14
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- 125000004432 carbon atom Chemical group C* 0.000 claims description 11
- 125000001183 hydrocarbyl group Chemical group 0.000 claims description 10
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 9
- 239000001257 hydrogen Substances 0.000 claims description 9
- 229910052739 hydrogen Inorganic materials 0.000 claims description 9
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 8
- 125000000217 alkyl group Chemical group 0.000 claims description 8
- 125000001424 substituent group Chemical group 0.000 claims description 8
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- 229920001214 Polysorbate 60 Polymers 0.000 claims description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 6
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 6
- 229910052710 silicon Inorganic materials 0.000 claims description 6
- 239000010703 silicon Substances 0.000 claims description 6
- WBIQQQGBSDOWNP-UHFFFAOYSA-N 2-dodecylbenzenesulfonic acid Chemical compound CCCCCCCCCCCCC1=CC=CC=C1S(O)(=O)=O WBIQQQGBSDOWNP-UHFFFAOYSA-N 0.000 claims description 5
- 229920001213 Polysorbate 20 Polymers 0.000 claims description 5
- 229940060296 dodecylbenzenesulfonic acid Drugs 0.000 claims description 5
- 239000000256 polyoxyethylene sorbitan monolaurate Substances 0.000 claims description 5
- 235000010486 polyoxyethylene sorbitan monolaurate Nutrition 0.000 claims description 5
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 claims description 5
- 229920000053 polysorbate 80 Polymers 0.000 claims description 5
- 239000003755 preservative agent Substances 0.000 claims description 5
- 239000002562 thickening agent Substances 0.000 claims description 5
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 4
- HVUMOYIDDBPOLL-XWVZOOPGSA-N Sorbitan monostearate Chemical compound CCCCCCCCCCCCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O HVUMOYIDDBPOLL-XWVZOOPGSA-N 0.000 claims description 4
- 239000004147 Sorbitan trioleate Substances 0.000 claims description 4
- PRXRUNOAOLTIEF-ADSICKODSA-N Sorbitan trioleate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OC[C@@H](OC(=O)CCCCCCC\C=C/CCCCCCCC)[C@H]1OC[C@H](O)[C@H]1OC(=O)CCCCCCC\C=C/CCCCCCCC PRXRUNOAOLTIEF-ADSICKODSA-N 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- 239000001818 polyoxyethylene sorbitan monostearate Substances 0.000 claims description 4
- 235000010989 polyoxyethylene sorbitan monostearate Nutrition 0.000 claims description 4
- 239000001816 polyoxyethylene sorbitan tristearate Substances 0.000 claims description 4
- 235000010988 polyoxyethylene sorbitan tristearate Nutrition 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- 235000019337 sorbitan trioleate Nutrition 0.000 claims description 4
- 229960000391 sorbitan trioleate Drugs 0.000 claims description 4
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 claims description 4
- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 claims description 4
- 239000003377 acid catalyst Substances 0.000 claims description 3
- 150000001336 alkenes Chemical class 0.000 claims description 3
- 239000000945 filler Substances 0.000 claims description 3
- 239000000244 polyoxyethylene sorbitan monooleate Substances 0.000 claims description 3
- ZORQXIQZAOLNGE-UHFFFAOYSA-N 1,1-difluorocyclohexane Chemical compound FC1(F)CCCCC1 ZORQXIQZAOLNGE-UHFFFAOYSA-N 0.000 claims description 2
- MFGOFGRYDNHJTA-UHFFFAOYSA-N 2-amino-1-(2-fluorophenyl)ethanol Chemical compound NCC(O)C1=CC=CC=C1F MFGOFGRYDNHJTA-UHFFFAOYSA-N 0.000 claims description 2
- XZIIFPSPUDAGJM-UHFFFAOYSA-N 6-chloro-2-n,2-n-diethylpyrimidine-2,4-diamine Chemical compound CCN(CC)C1=NC(N)=CC(Cl)=N1 XZIIFPSPUDAGJM-UHFFFAOYSA-N 0.000 claims description 2
- BWDBEAQIHAEVLV-UHFFFAOYSA-N 6-methylheptan-1-ol Chemical compound CC(C)CCCCCO BWDBEAQIHAEVLV-UHFFFAOYSA-N 0.000 claims description 2
- AVXURJPOCDRRFD-UHFFFAOYSA-N Hydroxylamine Chemical compound ON AVXURJPOCDRRFD-UHFFFAOYSA-N 0.000 claims description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 2
- IYFATESGLOUGBX-YVNJGZBMSA-N Sorbitan monopalmitate Chemical compound CCCCCCCCCCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O IYFATESGLOUGBX-YVNJGZBMSA-N 0.000 claims description 2
- IJCWFDPJFXGQBN-RYNSOKOISA-N [(2R)-2-[(2R,3R,4S)-4-hydroxy-3-octadecanoyloxyoxolan-2-yl]-2-octadecanoyloxyethyl] octadecanoate Chemical compound CCCCCCCCCCCCCCCCCC(=O)OC[C@@H](OC(=O)CCCCCCCCCCCCCCCCC)[C@H]1OC[C@H](O)[C@H]1OC(=O)CCCCCCCCCCCCCCCCC IJCWFDPJFXGQBN-RYNSOKOISA-N 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims description 2
- HUCVOHYBFXVBRW-UHFFFAOYSA-M caesium hydroxide Inorganic materials [OH-].[Cs+] HUCVOHYBFXVBRW-UHFFFAOYSA-M 0.000 claims description 2
- 235000019438 castor oil Nutrition 0.000 claims description 2
- 239000004359 castor oil Substances 0.000 claims description 2
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 claims description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 2
- 239000002736 nonionic surfactant Substances 0.000 claims description 2
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 claims description 2
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 2
- 238000006116 polymerization reaction Methods 0.000 claims description 2
- 239000000249 polyoxyethylene sorbitan monopalmitate Substances 0.000 claims description 2
- 235000010483 polyoxyethylene sorbitan monopalmitate Nutrition 0.000 claims description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 2
- 230000002335 preservative effect Effects 0.000 claims description 2
- 239000011347 resin Substances 0.000 claims description 2
- 229920005989 resin Polymers 0.000 claims description 2
- 229940035044 sorbitan monolaurate Drugs 0.000 claims description 2
- 239000001593 sorbitan monooleate Substances 0.000 claims description 2
- 235000011069 sorbitan monooleate Nutrition 0.000 claims description 2
- 229940035049 sorbitan monooleate Drugs 0.000 claims description 2
- 239000001570 sorbitan monopalmitate Substances 0.000 claims description 2
- 235000011071 sorbitan monopalmitate Nutrition 0.000 claims description 2
- 229940031953 sorbitan monopalmitate Drugs 0.000 claims description 2
- 239000001587 sorbitan monostearate Substances 0.000 claims description 2
- 235000011076 sorbitan monostearate Nutrition 0.000 claims description 2
- 229940035048 sorbitan monostearate Drugs 0.000 claims description 2
- 239000001589 sorbitan tristearate Substances 0.000 claims description 2
- 235000011078 sorbitan tristearate Nutrition 0.000 claims description 2
- 229960004129 sorbitan tristearate Drugs 0.000 claims description 2
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims 3
- PLFFHJWXOGYWPR-HEDMGYOXSA-N (4r)-4-[(3r,3as,5ar,5br,7as,11as,11br,13ar,13bs)-5a,5b,8,8,11a,13b-hexamethyl-1,2,3,3a,4,5,6,7,7a,9,10,11,11b,12,13,13a-hexadecahydrocyclopenta[a]chrysen-3-yl]pentan-1-ol Chemical compound C([C@]1(C)[C@H]2CC[C@H]34)CCC(C)(C)[C@@H]1CC[C@@]2(C)[C@]4(C)CC[C@@H]1[C@]3(C)CC[C@@H]1[C@@H](CCCO)C PLFFHJWXOGYWPR-HEDMGYOXSA-N 0.000 claims 1
- PLLBRTOLHQQAQQ-UHFFFAOYSA-N 8-methylnonan-1-ol Chemical compound CC(C)CCCCCCCO PLLBRTOLHQQAQQ-UHFFFAOYSA-N 0.000 claims 1
- 229920006197 POE laurate Polymers 0.000 claims 1
- HMDDXIMCDZRSNE-UHFFFAOYSA-N [C].[Si] Chemical group [C].[Si] HMDDXIMCDZRSNE-UHFFFAOYSA-N 0.000 claims 1
- 125000003118 aryl group Chemical group 0.000 claims 1
- 229940049964 oleate Drugs 0.000 claims 1
- 229920000259 polyoxyethylene lauryl ether Polymers 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 6
- 239000000463 material Substances 0.000 abstract description 6
- 238000006243 chemical reaction Methods 0.000 abstract description 4
- 239000011083 cement mortar Substances 0.000 abstract description 2
- 238000000034 method Methods 0.000 description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- WXMKPNITSTVMEF-UHFFFAOYSA-M sodium benzoate Chemical compound [Na+].[O-]C(=O)C1=CC=CC=C1 WXMKPNITSTVMEF-UHFFFAOYSA-M 0.000 description 6
- 239000004299 sodium benzoate Substances 0.000 description 6
- 235000010234 sodium benzoate Nutrition 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- FJKROLUGYXJWQN-UHFFFAOYSA-M 4-hydroxybenzoate Chemical compound OC1=CC=C(C([O-])=O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-M 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 229910000077 silane Inorganic materials 0.000 description 5
- XFRVVPUIAFSTFO-UHFFFAOYSA-N 1-Tridecanol Chemical compound CCCCCCCCCCCCCO XFRVVPUIAFSTFO-UHFFFAOYSA-N 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 4
- 239000004568 cement Substances 0.000 description 4
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 description 4
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 description 4
- ALVYUZIFSCKIFP-UHFFFAOYSA-N triethoxy(2-methylpropyl)silane Chemical compound CCO[Si](CC(C)C)(OCC)OCC ALVYUZIFSCKIFP-UHFFFAOYSA-N 0.000 description 4
- 229920002907 Guar gum Polymers 0.000 description 3
- IGFHQQFPSIBGKE-UHFFFAOYSA-N Nonylphenol Natural products CCCCCCCCCC1=CC=C(O)C=C1 IGFHQQFPSIBGKE-UHFFFAOYSA-N 0.000 description 3
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 3
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 3
- 239000000665 guar gum Substances 0.000 description 3
- 229960002154 guar gum Drugs 0.000 description 3
- 235000010417 guar gum Nutrition 0.000 description 3
- 239000004570 mortar (masonry) Substances 0.000 description 3
- SNQQPOLDUKLAAF-UHFFFAOYSA-N nonylphenol Chemical compound CCCCCCCCCC1=CC=CC=C1O SNQQPOLDUKLAAF-UHFFFAOYSA-N 0.000 description 3
- MSRJTTSHWYDFIU-UHFFFAOYSA-N octyltriethoxysilane Chemical compound CCCCCCCC[Si](OCC)(OCC)OCC MSRJTTSHWYDFIU-UHFFFAOYSA-N 0.000 description 3
- 230000002940 repellent Effects 0.000 description 3
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- KBPLFHHGFOOTCA-UHFFFAOYSA-N 1-Octanol Chemical compound CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 description 2
- SNRUBQQJIBEYMU-UHFFFAOYSA-N Dodecane Natural products CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 description 2
- NWGKJDSIEKMTRX-AAZCQSIUSA-N Sorbitan monooleate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O NWGKJDSIEKMTRX-AAZCQSIUSA-N 0.000 description 2
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
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- 125000003438 dodecyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 2
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 description 2
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 description 2
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 2
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- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 2
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- INJVFBCDVXYHGQ-UHFFFAOYSA-N n'-(3-triethoxysilylpropyl)ethane-1,2-diamine Chemical compound CCO[Si](OCC)(OCC)CCCNCCN INJVFBCDVXYHGQ-UHFFFAOYSA-N 0.000 description 2
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- CHHHXKFHOYLYRE-UHFFFAOYSA-M 2,4-Hexadienoic acid, potassium salt (1:1), (2E,4E)- Chemical compound [K+].CC=CC=CC([O-])=O CHHHXKFHOYLYRE-UHFFFAOYSA-M 0.000 description 1
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- DHNRXBZYEKSXIM-UHFFFAOYSA-N chloromethylisothiazolinone Chemical compound CN1SC(Cl)=CC1=O DHNRXBZYEKSXIM-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明涉及一种聚硅氧烷乳液的制备方法，该聚硅氧烷包括超支化的聚硅氧烷、线性聚硅氧烷、交联剂、聚醚改性聚硅氧烷、表面活性剂、催化剂和水。通过超支化结构聚硅氧烷、线性聚硅氧烷和交联剂反应，形成致密的结构，并通过活性基团与水泥砂浆等基材进一步反应，解决现有技术中防水效果不佳和不持久的问题。
Description
技术领域
本专利涉及一种聚硅氧烷乳液的制备方法，其具有提高防水效率和延长使用寿命的优点。
背景技术
混凝土作为质优价廉的材料在各种基础设施建设中发挥着重要的作用，其被大量应用在公路、桥梁、海港、隧道、机场等各种建筑的建设上。混凝土在被广泛使用的同时，其结构特征所引起的防水耐久性不足的缺点逐渐暴露出来，成为人们研究的热点。尤其我国地域广阔，气候温度条件跨度巨大，从而导致混凝土结构建筑，存在着被氯离子腐蚀、酸雨腐蚀、混凝土碳化、碱-骨料反应和冻融破坏的危险。
针对这些问题，已有不少研究学者和公司深入研究。US3772065采用异丁基三乙氧基硅烷单体或其用有机溶剂的稀释物作为防水剂。由于异丁基三乙氧基硅烷的沸点低、挥发性大等缺陷，防水效果不理想，且使用有机溶剂容易导致环境污染。CN105036602A采用复合乳化剂、三乙胺、正辛基三乙氧基硅烷等原料制备聚合物基料方法制备硅烷乳液，乳液稳定性提高，但是乳液制备过程工艺复杂，在实际生产过程中不易操作。CN99813908用一种烷氧基硅烷直接乳化制备防水乳液；CN0083430用烷氧基硅烷和含有烷氧基的有机硅氧烷制备水性乳液；CN201610473691用聚醚改性聚硅氧烷乳化烷氧基硅烷制备防水剂乳液；CN201410174448采用硅溶胶和硅烷乳液等混合在一定温度条件下反应制得，硅溶胶加入可提高防水层的致密性，但工艺复杂，使用过程容易在混凝土表面会有残留。CN201710364092提供一种混凝土防水剂的解决方案，通过改性三甲基封端的甲基含氢聚硅氧烷得到共聚物，用这个产物制备防水乳液，但是，含氢聚硅氧烷的含氢量和改性后的聚硅氧烷剩余活泼氢的含量是影响产品应用效果的关键因素，一旦做成乳液，乳液中含氢聚硅氧烷的稳定性也会逐步下降，这些因素导致不能大规模实施应用。作为用于混凝土中的防水剂，要使得它一次使用，终身发挥作用，防水剂务必要和混凝土中的组分发挥化学作用。而目前大量的技术资料都通过“吸附”的方法使得聚硅氧烷分子吸附在混凝土的表面，这种吸附仅限于物理作用，根本达不到长期防水的目的，严重威胁到大型工程的安全性，也别是长期在海水中浸泡的水泥固体。
本专利通过选择多种硅氧烷混合制备乳液，通过超支化的聚硅氧烷的介入，利用活性基团与水泥基体以及硅烷发生反应，建成“永久性”的“Si-O-Si”的化学键，也就形成了“永久性”的防水膜。
发明内容
本发明涉及一种聚硅氧烷乳液制备方法，其通过超支化结构聚硅氧烷、线性聚硅氧烷和交联剂反应，形成致密的结构，并通过活性基团与水泥砂浆等基材进一步反应，解决现有技术中防水效果不佳和不持久的问题。
所述的聚硅氧烷乳液包括超支化的聚硅氧烷、线性聚硅氧烷、交联剂、聚醚改性聚硅氧烷、表面活性剂、催化剂1、催化剂2和水等。
、超支化聚硅氧烷
所述的超支化聚硅氧烷结构式如下：
（Ⅰ）
式（Ⅰ）超支化聚硅氧烷分子中取代基R至少有一个活泼氢原子存在，且活泼氢原子的个数不超过取代基R总数量的5%，其余取代基R为烃基；
R为烃基时，它包括：
（1）碳原子数为1~30的烷基，如甲基、乙基、正丙基、异丙基、丁基、戊基、己基、辛基、癸基、十二烷基、十四烷基、十六烷基、十八烷基、二十烷基、二十二烷基、二十四烷基、二十六烷基、二十八烷基、三十烷基及其同分异构体；
（2）芳基，包括α-甲基苯乙基和苯乙基；
（3）烯烃，包括碳原子数为2~20的烯烃，如乙烯、丙烯、丁烯、己烯、癸烯及其同分异构体。
所述的超支化聚硅氧烷的用量为聚硅氧烷乳液总质量的0.1~10%。
、线性聚硅氧烷
所述的线性聚硅氧烷的结构通式如下：
（Ⅱ）
其中，下标a和b分别是链节-Me2SiO-和链节-MeR1SiO-的聚合度，a的值为5~100，b的值为0或1~50；R1 为羟基或者碳原子为1~20的烃基。所述线性聚硅氧烷粘度范围在10~1,000mPa·s。
所述的线性聚硅氧烷的用量为聚硅氧烷乳液总质量的0.5~20%。
、交联剂
所述的交联剂的结构通式如下：
（Ⅲ）
式中，下标c 为0、1、2、3；R2为碳原子数1~6的烃基，优选是碳原子1~4的烷基，特别优选的是甲基或乙基。R3是硅碳键键合的烃基，包括含有碳原子1~18的烃基和被氯原子、醚基、酯基、环氧烷基、巯基、氰基或氨基取代的碳原子数1~18的烃基。
所述的交联剂包括：甲基三甲氧基硅烷、甲基三乙氧基硅烷、异丁基三甲氧基硅烷、异丁基三乙氧基硅烷、正辛基三乙氧基硅烷、异辛基三乙氧基硅烷、乙烯基三甲氧基硅烷、乙烯基三乙氧基硅烷、苯基三甲氧基硅烷、苯基三乙氧基硅烷、四乙氧基硅烷、二丁基氨甲基三乙氧基硅烷、二丁基氨甲基三丁氧基硅烷、环己基氨甲基三甲氧基硅烷、环己基氨甲基三乙氧基硅烷、氨乙基氨丙基三乙氧基硅烷、氨乙基氨丙基三甲氧基硅烷、吗琳基甲基三异丙氧基硅烷、吗琳基甲基三乙氧基硅烷、3-二甲基氨丙基氨甲基三甲氧基硅烷、吗琳基甲基三烷氧基硅烷。
所述的交联剂优选甲基三甲氧基硅烷、甲基三乙氧基硅烷、异丁基三乙氧基硅烷、正辛基三乙氧基硅烷、乙烯基三甲氧基硅烷、乙烯基三乙氧基硅烷、四乙氧基硅烷、氨乙基氨丙基三乙氧基硅烷、氨乙基氨丙基三甲氧基硅烷。
所述的交联剂的用量为聚硅氧烷乳液总质量的5~60%。
、聚醚改性聚硅氧烷
所述的聚醚改性聚硅氧烷，其特征在于，具有以下结构：
（Ⅳ）
其中下标d 为5~100，下标e为5~100，下标m为10~40，下标n为1~20，取代基R4为1~4个碳原子的烷基或氢原子。
所述的含氢聚硅氧烷的含氢质量份数范围为0.05%~1.5%，粘度范围为10~600mPa·s。
所述聚醚改性聚硅氧烷的用量为聚硅氧烷乳液总质量的0.1~10%。
、表面活性剂
所述的表面活性剂为非离子表面活性剂，包括壬基酚聚氧乙烯醚、辛基酚聚氧乙烯醚、月桂酸聚氧乙烯醚、油酸聚氧乙烯醚、月桂醇聚氧乙烯醚、辛醇聚氧乙烯醚、异辛醇聚氧乙烯醚、异构癸醇聚氧乙烯醚、异构十三醇聚氧乙烯醚、十六醇聚氧乙烯醚、十八醇聚氧乙烯醚、失水山梨醇单月桂酸酯、失水山梨醇单棕榈酸酯、失水山梨醇单硬脂酸酯、失水山梨醇单油酸酯、失水山梨醇三硬脂酸酯、失水山梨醇三油酸酯、聚氧乙烯失水山梨醇单月桂酸酯、聚氧乙烯失水山梨醇单棕榈酸酯、聚氧乙烯失水山梨醇单硬脂酸酯、聚氧乙烯失水山梨醇单油酸酯、聚氧乙烯失水山梨醇三硬脂酸酯、聚氧乙烯失水山梨醇三油酸酯、蓖麻油聚氧乙烯醚、聚乙烯醇中的一种或多种的混合物，优选多种混合物。
所述的表面活性剂用量为聚硅氧烷乳液总质量的0.1~10%。
、催化剂1
所述的催化剂1为酸性催化剂，选自十二烷基苯磺酸、盐酸、硫酸、磷酸、对甲苯磺酸以及一些以固体载体的强酸催化剂。
催化剂1的用量为聚硅氧烷乳液总质量的0.01%~0.1%。
、催化剂2
所述的催化剂2为缩合催化剂，选自铂-醇络合物、铂-烯烃络合物、铂-醇盐络合物、铂-醚络合物、 铂-酮络合物、氯铂酸异丙醇溶液、铑-醇络合物、铑-醇盐络合物、氢氧化钠、氢氧化钾、氢氧化铯、四甲基氢氧化铵、羟胺、强碱性树脂。
催化剂2的用量为聚硅氧烷乳液总质量的0 .01% ~ 0 .1%。
、水
所述的水是乳液的连续相，选自自来水、去离子水、工艺水、湖水、江水、河水等干净的水，水的来源对于本发明影响不大。
所述的水分成两部分添加，第一部分水用量为乳液总质量的5%~20%；第二部分水用量为乳液总质量的5%~70%。
乳液中水的总用量为聚硅氧烷乳液总质量的10~90%。
依据本发明的乳液，可以进一步加入防腐剂，适合的防腐剂包括：5-氯-2甲基-4异噻唑啉-3 酮 和 2-甲基-4-异噻唑啉-3-酮（卡松）、苯并异噻唑啉酮、辛基异噻唑啉酮、2,2-二溴-3-次氮基丙酰胺、2-溴-2-硝基-1,3-丙二醇、山梨酸钾、对羟基苯甲酸酯、乳酸钠、苯甲酸钠。
依据本发明的乳液，可以进一步加入水溶性的增稠剂，包括聚丙烯酸、聚丙烯酸酯（盐）、纤维素醚、天然胶、聚氨酯，增稠剂的加量根据乳液的粘度调整。
依据本发明的乳液，可以进一步含有二氧化硅、二氧化钛或氧化铝作为填料，其BET表面积为20~1000m2/g，粒径优选小于10μm。任选的填料优选二氧化硅，具有BET表面积为50~500m2/g，包括沉淀法和气相法制备而成，例如Wacker公司的HDK H16、HDK H2100和Evonik公司的SIPERNAT D11。
上述各组分的用量总和为100%。
所述的聚硅氧烷乳液的制备方法如下：
将线性聚硅氧烷、交联剂和催化剂1加入到反应器中，温度控制在20~100℃，在转速为100~1000rpm，保温30~120min；然后向上述混合物中加入超支化聚硅氧烷和催化剂2，在转速100~1000rpm条件下控制温度为60~80℃，保温30~120min；然后再向反应器中加入聚醚改性聚硅氧烷和表面活性剂，选择转速500~3000rpm的条件下，向反应器中缓慢加入第一部分水，保温10~60min；然后提高转速为3000~10000rpm，在30~100min之间加入第二部分水，最后加入防腐剂、增稠剂即得到所需含量的有机硅乳液。
具体实施方式
、超支化聚硅氧烷的举例
本发明实施例超支化聚硅氧烷结构式Ⅰ中各个下标取值列举如下：
2、线性聚硅氧烷的举例
本发明实施例线性聚硅氧烷结构式Ⅱ中各个下标取值列举如下：
3、交联剂
本发明实施例线性聚硅氧烷结构式Ⅲ中各个下标取值列举如下：
4、聚醚改性聚硅氧烷
本发明聚醚改性聚硅氧烷结构式Ⅳ中各个下标取值列举如下：
实施例1：
将1份线性聚硅氧烷Ⅱ-1、59份交联剂Ⅲ-1和0.02份磷酸加入反应器中，温度控制在60℃，在转速为200rpm条件下，保温60min；然后然后向上述混合物中加入5份超支化聚硅氧烷Ⅰ-1和0.03份铂-醇络合物，在转速100rpm条件下，控制温度60℃，保温120min；然后向反应器中加入1份聚醚改性聚硅氧烷（Ⅳ-1）、2份司盘80和2.6份吐温80，选择转速为1000rpm，向反应器中缓慢加入6份水，加完后保温40min；然后提高转速为5000rpm，在30min之内加入49份水，最后加入0.2份苯甲酸钠和0.2份的瓜儿胶即得到含量56.21%的有机硅乳液E-1。
实施例2：
将5份线性聚硅氧烷Ⅱ-2、50份交联剂Ⅲ-2和0.03份十二烷基苯磺酸加入反应器中，温度控制在80℃，在转速为500rpm，保温40min；然后向上述混合物中加入9份超支化聚硅氧烷Ⅰ-2和0.1份铂-醇络合物加入到反应器中，在转速为1000rpm条件下，控制温度为40℃，保温40min；然后向反应器中加入9份聚醚改性聚硅氧烷（Ⅳ-2）、4份司盘60和5.5份吐温60，选择转速为500rpm向反应器中加入10份水，加完后保温12min；然后提高转速为3100mPa.s，在50min内加入40份水，最后加入0.2份苯甲酸钠和0.1份羧甲基纤维素醚，即得含量62.26%的有机硅乳液E-2。
实施例3：
将10份线性聚硅氧烷Ⅱ-3、30份交联剂Ⅲ-3和0.06份十二烷基苯磺酸加入反应器中，控制温度在50℃，在转速为950rpm条件下，保温100min；然后向上述混合物中加入2份超支化聚硅氧烷Ⅰ-3和0.05份铂-醇络合物加入到反应器中，在转速为600rpm条件下，并控制温度65℃，保温100min；然后再向反应器中加入8份聚醚改性聚硅氧烷（Ⅳ-3）和0.5份异构十三醇聚氧乙烯醚，选择转速为2850rpm，向反应器中加入15份水，保温20min；然后提高转速为9000rpm，在70min内加入65份水，最后加入0.2份苯甲酸钠和0.1份聚丙烯酸酯，即得含量38.70%的有机硅乳液E-3。
实施例4：
将18份线性聚硅氧烷Ⅱ-4、20份交联剂Ⅲ-4 和0.1份盐酸加入反应器中，在转速为700rpm，控制温度在80℃条件下，保温120min；然后向上述混合物中加入1份超支化聚硅氧烷Ⅰ-4和0.03份氢氧化钾加入到反应器中，在转速为100rpm条件下，并控制温度为75℃，保温60min；然后向反应器中加入4份聚醚改性聚硅氧烷（Ⅳ-4）和3份脂肪醇聚氧乙烯醚，在转速为1500rpm，向反应器中加入15份水，保温30min；然后提高转速为8000rpm，在90min内加入15份水，最后加入0.2份对羟基苯甲酸酯和0.3份瓜儿胶，即得含量60.53%的有机硅乳液E-4。
实施例5：
将15份线性聚硅氧烷Ⅱ-5、8份交联剂Ⅲ-5和0.08份磷酸加入反应器中，控制温度在90℃，在转速100rpm的条件下，保温40min；然后向上述混合物中加入0.5份超支化聚硅氧烷Ⅰ-5和0.01份氢氧化钠加入到反应器中，在转速为500rpm，控制温度在30℃，保温110min；然后向反应器中加入0.3份聚醚改性聚硅氧烷（Ⅳ-5）和1份壬基酚聚氧乙烯醚，在转速为2000rpm，向反应器中加入18份水，保温60min；提高转速为6500rpm，在95min加6份水，最后加入0.2份对羟基苯甲酸酯和0.2份聚丙烯酸钠，即得含量50.82%的有机硅乳液E-5。
实施例6：
将0.5份线性聚硅氧烷Ⅱ-5、40份交联剂Ⅲ-3和0.08份磷酸加入反应器中，在转速为500rpm，控制温度在20℃条件下，保温60min；然后向上述混合物中加入6份超支化聚硅氧烷Ⅰ-6和0.01份氢氧化钠加入到反应器中，在转速为500rpm条件下控制温度在40℃，保温120min；然后向反应器中加入1份聚醚改性聚硅氧烷（Ⅳ-4）、1份壬基酚聚氧乙烯醚和1份异构十醇聚氧乙烯醚，在转速为1500rpm，向反应器中加入18份水，保温50min；然后提高转速为6500rpm，在55min内加入50份水，最后加入0.2份对羟基苯甲酸酯和0.2份聚丙烯酸钠，即得含量42.16%的有机硅乳液E-6。
实施例7：
将4份 线性聚硅氧烷Ⅱ-3、44份交联剂Ⅲ-2和0.05份磷酸加入反应器中，在转速为600rpm，控制温度在70℃的条件下，保温30min；然后向上述混合物中加入5份超支化聚硅氧烷Ⅰ-7和0.01份铂-醇络合物加入到反应器中，在转速为500rpm的条件下控制温度为60℃保温110min；然后向反应器中加入3份聚醚改性聚硅氧烷（Ⅳ-3）和3份异构十三醇聚氧乙烯醚，在转速为1000rpm，向反应器中加入15份水，保温15min；然后提高转速为4500rpm，在45min内加入45份水，最后加入0.2份对羟基苯甲酸酯和0.2份聚丙烯酸钠，即得含量49.58%的有机硅乳液E-7。
对比例1：
将1份线性聚硅氧烷Ⅱ-1、59份交联剂Ⅲ-1和0.02份磷酸加入反应器中，在转速为200rpm，控制温度在60℃的条件下，保温60min；然后向上述混合物中加入1份聚醚改性聚硅氧烷（Ⅳ-1）、2份司盘80和2.6份吐温80，在转速为1000rpm，向反应器中加入10份水，保温40min；然后提高转速为5000rpm，在60min内向反应器中加入45份水，最后加入0.2份苯甲酸钠和0.2份的瓜儿胶即得到含量54.40%的有机硅乳液C-1。
对比例2：
将5份 线性聚硅氧烷Ⅱ-2、50份交联剂Ⅲ-2和0.03份十二烷基苯磺酸加入反应器中，在转速为500rpm，控制温度为80℃的条件下，保温40min；然后向上述混合物中加入9份超支化聚硅氧烷CⅠ-1和0.1份铂-醇络合物加入到反应器中，在转速为900rpm的条件下控制温度为40℃，保温40min；然后向反应器中加入9份聚醚改性聚硅氧烷（Ⅳ-2）、4份司盘60和5.5份吐温60，在转速为500rpm，向反应器中加入19份水，保温40min；然后提高转速为3100rpm，在50min内向反应器中加入31份水，最后加入0.2份苯甲酸钠和0.1份羧甲基纤维素醚，即得含量62.26%的有机硅乳液C-2。
对比例3：
将44份交联剂Ⅲ-2、5份超支化聚硅氧烷Ⅰ-1和0.01份铂-醇络合物加入到反应器中，在转速为500rpm条件下并控制温度为70℃，保温110min；然后向反应器中加入3份聚醚改性聚硅氧烷（Ⅳ-3）和3份异构十三醇聚氧乙烯醚，在转速为1500rpm，向反应器中加入20份水，保温20min；然后提高转速为4500rpm，在45min内向反应器中加入40份水，最后加入0.2份对羟基苯甲酸酯和0.2份聚丙烯酸钠，即得含量47.83%的有机硅乳液C-3。
乳液样品测试结果
为了验证专利发明所得到的乳液的效果，分别将上述E1~E5，C1~C3用水稀释成2%的固含量。
砂浆试块制备：水/水泥重量比=0.6，砂/水泥质量比=2.8，将实施例E1~E5和对比例C1~C3按同等加量加入砂浆中，然后制成（100×100×100）毫米试块，标养28天。按《轻集料混凝土技术规程》，测试各砂浆试块在水中浸泡24h和7d的吸水率。测试吸水率结果列于下表。
从上表可以看出掺入对比例C1~C3，浸泡24h的吸水率明显比实施例高。对比例C1~C3分析主要原因难以实现致密网状结构的防水层，和不能与基材形成牢固的结合，导致浸泡时间延长，防水效果下降；其余实施例，在线性聚硅氧烷、超支化聚硅氧烷以及交联剂三者作用下，结构紧密并和基材充分结合，从而吸水率低持久性好。
Claims (9)
1.一种聚硅氧烷乳液，其特征在于，它包括超支化的聚硅氧烷、线性聚硅氧烷、交联剂、聚醚改性聚硅氧烷、表面活性剂、催化剂1、催化剂2和水：
A、超支化聚硅氧烷：所述的超支化聚硅氧烷结构式如下：
（Ⅰ）
式（Ⅰ）中取代基R至少有一个活泼氢原子存在，且活泼氢原子的个数不超过取代基R总数量的5%，其余取代基R为烃基；R为烃基时，它包括：碳原子数为1~30的烷基、芳基、烯烃；所述的超支化聚硅氧烷的用量为聚硅氧烷乳液总质量的0.1~10%；
B、线性聚硅氧烷：所述的线性聚硅氧烷的用量为聚硅氧烷乳液总质量的0.5~20%；
C、交联剂：所述的交联剂的用量为聚硅氧烷乳液总质量的5~60%；
D、聚醚改性聚硅氧烷：所述聚醚改性聚硅氧烷的用量为聚硅氧烷乳液总质量的0.1~10%；
E、表面活性剂：所述的表面活性剂用量为聚硅氧烷乳液总质量的0.1~10%；
F、催化剂1：所述的催化剂1用量为聚硅氧烷乳液总质量的0.01%~0.1%；
G、催化剂2：所述的催化剂2用量为聚硅氧烷乳液总质量的0 .01% ~ 0 .1%；
H、水：所述的水是乳液的连续相，乳液中水的总用量为聚硅氧烷乳液总质量的10~90%；
所述的聚硅氧烷乳液的制备方法如下：
将线性聚硅氧烷、交联剂和催化剂1加入到反应器中，温度控制在20~100℃，在转速为100~1000rpm，保温30~120min；然后向上述混合物中加入超支化聚硅氧烷和催化剂2，在转速100~1000rpm条件下控制温度为60~80℃，保温30~120min；然后再向反应器中加入聚醚改性聚硅氧烷和表面活性剂，选择转速500~3000rpm的条件下，向反应器中缓慢加入第一部分水，保温10~60min；然后提高转速为3000~10000rpm，在30~100min之间加入第二部分水，最后加入防腐剂、增稠剂即得到所需含量的有机硅乳液。
2.根据权利要求1所述的一种聚硅氧烷乳液，其特征在于，所述的线性聚硅氧烷的结构通式如下：
（Ⅱ）
下标a和b分别是链节-Me2SiO-和链节-MeR1SiO-的聚合度，a的值为5~100，b的值为0或1~50；R1 为羟基或者碳原子为1~20的烃基，所述线性聚硅氧烷粘度范围在10~1,000mPa·s。
3.根据权利要求1所述的一种聚硅氧烷乳液，其特征在于，所述的交联剂的结构通式如下：
（Ⅲ）
下标c 为0、1、2、3；R2为碳原子数1~6的烃基；R3是硅碳键键合的烃基。
4.根据权利要求1所述的一种聚硅氧烷乳液，其特征在于，所述聚醚改性聚硅氧烷具有以下结构：
下标d 为5~100，下标e为5~100，下标m为10~40，下标n为1~20，取代基R4为1~4个碳原子的烷基或氢原子；所述的含氢聚硅氧烷的含氢质量份数范围为0.05%~1.5%，粘度范围为10~600mPa·s。
5.根据权利要求1所述的一种聚硅氧烷乳液，其特征在于，所述的表面活性剂为非离子表面活性剂，包括壬基酚聚氧乙烯醚、辛基酚聚氧乙烯醚、月桂酸聚氧乙烯醚、油酸聚氧乙烯醚、月桂醇聚氧乙烯醚、辛醇聚氧乙烯醚、异辛醇聚氧乙烯醚、异构癸醇聚氧乙烯醚、异构十三醇聚氧乙烯醚、十六醇聚氧乙烯醚、十八醇聚氧乙烯醚、失水山梨醇单月桂酸酯、失水山梨醇单棕榈酸酯、失水山梨醇单硬脂酸酯、失水山梨醇单油酸酯、失水山梨醇三硬脂酸酯、失水山梨醇三油酸酯、聚氧乙烯失水山梨醇单月桂酸酯、聚氧乙烯失水山梨醇单棕榈酸酯、聚氧乙烯失水山梨醇单硬脂酸酯、聚氧乙烯失水山梨醇单油酸酯、聚氧乙烯失水山梨醇三硬脂酸酯、聚氧乙烯失水山梨醇三油酸酯、蓖麻油聚氧乙烯醚、聚乙烯醇中的一种或多种的混合物。
6.根据权利要求1所述的一种聚硅氧烷乳液，其特征在于，所述的催化剂1选自十二烷基苯磺酸、盐酸、硫酸、磷酸、对甲苯磺酸以及一些以固体载体的强酸催化剂。
7.根据权利要求1所述的一种聚硅氧烷乳液，其特征在于，所述的催化剂2选自铂-醇络合物、铂-烯烃络合物、铂-醇盐络合物、铂-醚络合物、 铂-酮络合物、氯铂酸异丙醇溶液、铑-醇络合物、铑-醇盐络合物、氢氧化钠、氢氧化钾、氢氧化铯、四甲基氢氧化铵、羟胺、强碱性树脂。
8.根据权利要求1所述的一种聚硅氧烷乳液，其特征在于，所述的水分成两部分添加，第一部分水用量为乳液总质量的5%~20%；第二部分水用量为乳液总质量的5%~70%。
9.根据权利要求1所述的一种聚硅氧烷乳液，其特征在于，乳液还可以进一步加入防腐剂、增稠剂和填料。
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