CN115678111A - Preparation method of water-repellent organic silicon composition - Google Patents
Preparation method of water-repellent organic silicon composition Download PDFInfo
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- CN115678111A CN115678111A CN202211316202.8A CN202211316202A CN115678111A CN 115678111 A CN115678111 A CN 115678111A CN 202211316202 A CN202211316202 A CN 202211316202A CN 115678111 A CN115678111 A CN 115678111A
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- Prior art keywords
- polysiloxane
- water
- vinyl
- containing polysiloxane
- micro powder
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- 239000000203 mixture Substances 0.000 title claims abstract description 39
- 239000005871 repellent Substances 0.000 title claims abstract description 30
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 17
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 17
- 239000010703 silicon Substances 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 229920001296 polysiloxane Polymers 0.000 claims abstract description 134
- -1 polysiloxane Polymers 0.000 claims abstract description 120
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 56
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims abstract description 54
- 229920002554 vinyl polymer Polymers 0.000 claims abstract description 54
- 239000000843 powder Substances 0.000 claims abstract description 49
- 239000000839 emulsion Substances 0.000 claims abstract description 43
- 239000011248 coating agent Substances 0.000 claims abstract description 27
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 24
- 239000001257 hydrogen Substances 0.000 claims abstract description 24
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 24
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000004090 dissolution Methods 0.000 claims abstract description 16
- 238000001035 drying Methods 0.000 claims abstract description 14
- 239000000853 adhesive Substances 0.000 claims abstract description 13
- 230000001070 adhesive effect Effects 0.000 claims abstract description 13
- 238000001694 spray drying Methods 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims description 39
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 38
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 38
- 239000003054 catalyst Substances 0.000 claims description 20
- 229920002472 Starch Polymers 0.000 claims description 18
- 235000019698 starch Nutrition 0.000 claims description 16
- 239000002245 particle Substances 0.000 claims description 15
- 239000008107 starch Substances 0.000 claims description 15
- 229920002125 Sokalan® Polymers 0.000 claims description 11
- 239000004584 polyacrylic acid Substances 0.000 claims description 11
- 230000002940 repellent Effects 0.000 claims description 10
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 8
- 229920002678 cellulose Polymers 0.000 claims description 7
- 239000001913 cellulose Substances 0.000 claims description 7
- 239000001509 sodium citrate Substances 0.000 claims description 7
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 7
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 6
- MWKFXSUHUHTGQN-UHFFFAOYSA-N decan-1-ol Chemical compound CCCCCCCCCCO MWKFXSUHUHTGQN-UHFFFAOYSA-N 0.000 claims description 6
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 6
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 6
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 6
- HLZKNKRTKFSKGZ-UHFFFAOYSA-N tetradecan-1-ol Chemical compound CCCCCCCCCCCCCCO HLZKNKRTKFSKGZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 5
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 claims description 5
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 5
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 5
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 claims description 5
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 claims description 5
- KBPLFHHGFOOTCA-UHFFFAOYSA-N 1-Octanol Chemical compound CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 claims description 4
- XFRVVPUIAFSTFO-UHFFFAOYSA-N 1-Tridecanol Chemical compound CCCCCCCCCCCCCO XFRVVPUIAFSTFO-UHFFFAOYSA-N 0.000 claims description 4
- 239000004354 Hydroxyethyl cellulose Substances 0.000 claims description 4
- 229920000663 Hydroxyethyl cellulose Polymers 0.000 claims description 4
- 229920002153 Hydroxypropyl cellulose Polymers 0.000 claims description 4
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 4
- 125000004432 carbon atom Chemical group C* 0.000 claims description 4
- 239000000969 carrier Substances 0.000 claims description 4
- LQZZUXJYWNFBMV-UHFFFAOYSA-N dodecan-1-ol Chemical compound CCCCCCCCCCCCO LQZZUXJYWNFBMV-UHFFFAOYSA-N 0.000 claims description 4
- BXWNKGSJHAJOGX-UHFFFAOYSA-N hexadecan-1-ol Chemical compound CCCCCCCCCCCCCCCCO BXWNKGSJHAJOGX-UHFFFAOYSA-N 0.000 claims description 4
- 235000019447 hydroxyethyl cellulose Nutrition 0.000 claims description 4
- 229920003063 hydroxymethyl cellulose Polymers 0.000 claims description 4
- 229940031574 hydroxymethyl cellulose Drugs 0.000 claims description 4
- 239000001863 hydroxypropyl cellulose Substances 0.000 claims description 4
- 235000010977 hydroxypropyl cellulose Nutrition 0.000 claims description 4
- 229910052751 metal Inorganic materials 0.000 claims description 4
- 239000002184 metal Substances 0.000 claims description 4
- GLDOVTGHNKAZLK-UHFFFAOYSA-N octadecan-1-ol Chemical compound CCCCCCCCCCCCCCCCCCO GLDOVTGHNKAZLK-UHFFFAOYSA-N 0.000 claims description 4
- 229910052697 platinum Inorganic materials 0.000 claims description 4
- 238000006116 polymerization reaction Methods 0.000 claims description 4
- 239000011734 sodium Substances 0.000 claims description 4
- 229910052708 sodium Inorganic materials 0.000 claims description 4
- ALSTYHKOOCGGFT-KTKRTIGZSA-N (9Z)-octadecen-1-ol Chemical compound CCCCCCCC\C=C/CCCCCCCCO ALSTYHKOOCGGFT-KTKRTIGZSA-N 0.000 claims description 3
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 3
- JSYPRLVDJYQMAI-ODZAUARKSA-N (z)-but-2-enedioic acid;prop-2-enoic acid Chemical compound OC(=O)C=C.OC(=O)\C=C/C(O)=O JSYPRLVDJYQMAI-ODZAUARKSA-N 0.000 claims description 3
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 3
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 3
- 229920002126 Acrylic acid copolymer Polymers 0.000 claims description 3
- 108010010803 Gelatin Proteins 0.000 claims description 3
- 239000005642 Oleic acid Substances 0.000 claims description 3
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 3
- 235000021355 Stearic acid Nutrition 0.000 claims description 3
- 229920000159 gelatin Polymers 0.000 claims description 3
- 239000008273 gelatin Substances 0.000 claims description 3
- 235000019322 gelatine Nutrition 0.000 claims description 3
- 235000011852 gelatine desserts Nutrition 0.000 claims description 3
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 3
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 3
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 3
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 3
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 3
- 229940055577 oleyl alcohol Drugs 0.000 claims description 3
- XMLQWXUVTXCDDL-UHFFFAOYSA-N oleyl alcohol Natural products CCCCCCC=CCCCCCCCCCCO XMLQWXUVTXCDDL-UHFFFAOYSA-N 0.000 claims description 3
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 claims description 3
- 229920002401 polyacrylamide Polymers 0.000 claims description 3
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 claims description 3
- 239000008117 stearic acid Substances 0.000 claims description 3
- 229920000881 Modified starch Polymers 0.000 claims description 2
- 229910004283 SiO 4 Inorganic materials 0.000 claims description 2
- 125000000217 alkyl group Chemical group 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims description 2
- 229930182470 glycoside Natural products 0.000 claims description 2
- JEGUKCSWCFPDGT-UHFFFAOYSA-N h2o hydrate Chemical compound O.O JEGUKCSWCFPDGT-UHFFFAOYSA-N 0.000 claims description 2
- 125000001183 hydrocarbyl group Chemical group 0.000 claims description 2
- 235000019426 modified starch Nutrition 0.000 claims description 2
- 239000001508 potassium citrate Substances 0.000 claims description 2
- 229960002635 potassium citrate Drugs 0.000 claims description 2
- QEEAPRPFLLJWCF-UHFFFAOYSA-K potassium citrate (anhydrous) Chemical compound [K+].[K+].[K+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O QEEAPRPFLLJWCF-UHFFFAOYSA-K 0.000 claims description 2
- 235000011082 potassium citrates Nutrition 0.000 claims description 2
- 239000008213 purified water Substances 0.000 claims description 2
- 235000015424 sodium Nutrition 0.000 claims description 2
- 235000011083 sodium citrates Nutrition 0.000 claims description 2
- 125000001424 substituent group Chemical group 0.000 claims description 2
- 239000008399 tap water Substances 0.000 claims description 2
- 235000020679 tap water Nutrition 0.000 claims description 2
- 239000004368 Modified starch Substances 0.000 claims 1
- 125000003118 aryl group Chemical group 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 8
- 239000007787 solid Substances 0.000 abstract description 7
- 238000006243 chemical reaction Methods 0.000 abstract description 5
- 230000001681 protective effect Effects 0.000 abstract description 5
- 229920000642 polymer Polymers 0.000 abstract description 4
- 238000003860 storage Methods 0.000 abstract description 4
- 229940032147 starch Drugs 0.000 description 13
- 238000010521 absorption reaction Methods 0.000 description 8
- 125000002091 cationic group Chemical group 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 239000004570 mortar (masonry) Substances 0.000 description 5
- WMGXSRPANDQJNK-UHFFFAOYSA-N platinum;propan-2-ol Chemical compound [Pt].CC(C)O WMGXSRPANDQJNK-UHFFFAOYSA-N 0.000 description 5
- 239000000463 material Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 125000002057 carboxymethyl group Chemical group [H]OC(=O)C([H])([H])[*] 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 230000002401 inhibitory effect Effects 0.000 description 3
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 239000002518 antifoaming agent Substances 0.000 description 2
- 239000004568 cement Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000007822 coupling agent Substances 0.000 description 2
- 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
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 239000010440 gypsum Substances 0.000 description 2
- 229910052602 gypsum Inorganic materials 0.000 description 2
- 230000005764 inhibitory process Effects 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 241000894007 species Species 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000004078 waterproofing Methods 0.000 description 2
- 229940100445 wheat starch Drugs 0.000 description 2
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 1
- 229920002261 Corn starch Polymers 0.000 description 1
- 229920000858 Cyclodextrin Polymers 0.000 description 1
- SNRUBQQJIBEYMU-UHFFFAOYSA-N Dodecane Natural products CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 229920002774 Maltodextrin Polymers 0.000 description 1
- 239000005913 Maltodextrin Substances 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 229920002367 Polyisobutene Polymers 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 125000005055 alkyl alkoxy group Chemical group 0.000 description 1
- 125000001204 arachidyl group Chemical group [H]C([*])([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])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 150000005840 aryl radicals Chemical class 0.000 description 1
- 125000002511 behenyl group Chemical group [H]C([*])([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])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])[H] 0.000 description 1
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 235000010948 carboxy methyl cellulose Nutrition 0.000 description 1
- 239000008112 carboxymethyl-cellulose Substances 0.000 description 1
- 125000003901 ceryl group Chemical group [H]C([*])([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])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])C([H])([H])[H] 0.000 description 1
- 229960000541 cetyl alcohol Drugs 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000008120 corn starch Substances 0.000 description 1
- 125000002704 decyl 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])* 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 125000004051 hexyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 150000004754 hydrosilicons Chemical class 0.000 description 1
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 125000002463 lignoceryl group Chemical group [H]C([*])([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])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])[H] 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 229940035034 maltodextrin Drugs 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 125000002819 montanyl group Chemical group [H]C([*])([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])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])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 125000001802 myricyl group Chemical group [H]C([*])([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])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])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 125000001421 myristyl group Chemical group [H]C([*])([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])C([H])([H])[H] 0.000 description 1
- 125000004123 n-propyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 125000002347 octyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- MSRJTTSHWYDFIU-UHFFFAOYSA-N octyltriethoxysilane Chemical compound CCCCCCCC[Si](OCC)(OCC)OCC MSRJTTSHWYDFIU-UHFFFAOYSA-N 0.000 description 1
- 229960003493 octyltriethoxysilane Drugs 0.000 description 1
- 125000000913 palmityl group Chemical group [H]C([*])([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])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 239000012188 paraffin wax Substances 0.000 description 1
- 125000001147 pentyl group Chemical group C(CCCC)* 0.000 description 1
- 125000000286 phenylethyl group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C([H])([H])C([H])([H])* 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 150000003242 quaternary ammonium salts Chemical class 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- HFHDHCJBZVLPGP-UHFFFAOYSA-N schardinger α-dextrin Chemical compound O1C(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(O)C2O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC2C(O)C(O)C1OC2CO HFHDHCJBZVLPGP-UHFFFAOYSA-N 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 229920002050 silicone resin Polymers 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 229940080313 sodium starch Drugs 0.000 description 1
- GBPOWOIWSYUZMH-UHFFFAOYSA-N sodium;trihydroxy(methyl)silane Chemical compound [Na+].C[Si](O)(O)O GBPOWOIWSYUZMH-UHFFFAOYSA-N 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 125000004079 stearyl group Chemical group [H]C([*])([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])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
Abstract
The invention relates to a preparation method of a water-repellent organic silicon composition, which consists of an organic carrier, an adhesive, hydrogen-containing polysiloxane micro powder and vinyl polysiloxane micro powder. The two kinds of polysiloxane micropowder are prepared by preparing emulsion from polysiloxane, emulsifier and water, adding coating agent, and spray drying. The preparation method of the water-repellent organosilicon composition reduces the contact of the polysiloxane and external influencing factors and ensures the stability of a molecular structure. When the polysiloxane protective film is used, the polysiloxane micro powder is added into a solid or powder application system, active molecules are slowly released through the dissolution of a high molecular polymer, and a primary polysiloxane protective film is formed through reaction in the drying process. The organosilicon product prepared by the method has stable performance in the storage period; can exert the effect for a long time in an application system.
Description
Technical Field
The patent relates to a preparation method of a water-repellent organic silicon composition, belonging to the technical field of fine chemical engineering.
Background
Polysiloxanes have received extensive research and attention since the 50 s of the 20 th century. Polysiloxane materials have been penetrated into various fields of national economy as a novel chemical material due to their low surface tension and hydrophobicity, which determine their particular use. The products formed by taking polysiloxane as a main material have a plurality of varieties, and particularly have subdivision functions of bonding, defoaming, leveling, wetting, demolding, water proofing and the like. The external forms of silicone materials application are mainly solvent-based, bulk, aqueous emulsion, and solid.
Water-based emulsion type products are inherently of great interest because of their "environmentally friendly" character. CN201410028888 introduces an emulsion composed of octyl triethoxysilane and a prepolymer of silicone resin, which is used for a waterproof emulsion and has a certain waterproof effect when used as an internal reference of concrete, but the cost is high; CN200810019295.1 adopts a method of compounding a high-viscosity emulsifier and a low-viscosity emulsifier to prepare an emulsion, and an attempt is made to disperse a high-viscosity organosilicon composition in water to obtain the emulsion; CN201010584419.8 is an emulsion prepared by means of intense shearing with various different equipment; US5241866A uses alkyl alkoxy coupling agent, quaternary ammonium salt-containing coupling agent, paraffin emulsion and polyisobutylene to prepare a waterproof agent; US7294195 describes organosilicon emulsions based on gypsum, hydroxycellulose or sodium methylsiliconate as waterproofing agents for gypsum. EP0210721 describes silicone compositions with fatty acid fatty alcohols as carriers;
however, the emulsion-type silicone additive is not an ideal choice for solid or powder-type application environments, because the polysiloxane containing active hydrosilicon is easy to generate polymer in water for a long time, the molecular structure is changed, and the use of the polysiloxane is greatly limited, for example, the end user does not like to apply the emulsion-type defoaming agent to washing powder, but hopes that the emulsion-type silicone additive is a solid-type product; the users of concrete do not want to use emulsion type water repellent, but prefer a powder type or solid type water repellent auxiliary. The user of powder coating can only add a powder type defoaming agent to control the foam generated during construction because solid-solid mixing is easier than solid-liquid mixing.
This patent wraps up on the surface of polysiloxane with water-soluble high molecular polymer, forms the polysiloxane miropowder through spray drying technique, has reduced the contact of polysiloxane with external influence factor, ensures molecular structure's stability. When the polysiloxane protective film is used, the polysiloxane micro powder is added into a solid application system, active molecules are slowly released through the dissolution of a high molecular polymer, and a primary polysiloxane protective film is formed through reaction in the drying process, so that the effects of release, water resistance and demoulding are achieved, and the technology can also be used for preparing other organic silicon products.
Disclosure of Invention
The invention provides a preparation method of a water-repellent organic silicon composition, and an organic silicon product prepared by the method has stable performance in a storage period; in an application system, the slow-release and chemical reaction can occur, and the effect can be exerted for a long time.
The water-repellent organic silicon composition consists of an organic carrier, an adhesive, hydrogen-containing polysiloxane micro powder and vinyl polysiloxane micro powder in percentage by mass as follows:
organic carrier: 30 to 90 percent;
adhesive: 2 to 10 percent;
hydrogen-containing polysiloxane micropowder: 1 to 10 percent;
vinyl polysiloxane micropowder: 5 to 50 percent;
1. organic carrier:
the organic carrier is a water-soluble organic carrier and comprises:
cellulose such as carboxymethyl cellulose, hydroxyethyl cellulose, hydroxypropyl cellulose;
natural starches, such as wheat starch, corn starch;
modified starches such as cyclodextrin, maltodextrin, phosphate starch, acid hydrolyzed starch, cationic starch, carboxymethyl starch, and the like;
these carriers are used singly or in combination.
2. Adhesive:
the adhesive is selected from one or more of water, polyacrylic acid, sodium polyacrylate, maleic acid-acrylic acid copolymer, sodium carboxymethyl cellulose, sodium citrate, potassium citrate, alkyl glycoside and polyvinylpyrrolidone.
3. Polysiloxane micropowder:
the hydrogen-containing polysiloxane micro powder is prepared by firstly preparing emulsion under certain process conditions and then performing spray drying technology on the emulsion, wherein the hydrogen-containing polysiloxane micro powder consists of hydrogen-containing polysiloxane, an emulsifier, water and a coating agent.
The vinyl-containing polysiloxane micropowder is obtained by preparing emulsion from vinyl-containing polysiloxane, an emulsifier, a coating agent, a catalyst and water and then performing spray drying technology.
The two kinds of the polysiloxane micropowder have certain similarity and difference in composition.
The two types of the polysiloxane micro powder comprise the following components:
A. polysiloxanes
The polysiloxane is hydrogen-containing polysiloxane and vinyl-containing polysiloxane, and is respectively used for preparing hydrogen-containing polysiloxane micro powder and vinyl-containing polysiloxane micro powder:
a1, hydrogen-containing polysiloxane
The general structural formula of the hydrogenpolysiloxane is as follows:
in the formula (I), subscripta、b、cSubscripts, for three linkscIs an integer of 1~2; r 1 And R 2 The same or different; r is 1 And R 2 Is a hydrocarbon group with 1 to 20 carbon atoms or a hydrogen atom;
the dynamic viscosity of the hydrogenpolysiloxane at 25 ℃ is 2 to 50mPa & s;
the dosage of the hydrogenous polysiloxane is 5 to 45 percent of the total feeding amount of the hydrogenous polysiloxane micro powder.
A2 vinyl-containing polysiloxane
The structural general formula of the vinyl-containing polysiloxane is as follows:
（R 3 Me 2 SiO 1/2 ) d (Me 2 SiO 2/2 ) e (R 4 MeSiO 2/2 ) f (MeViSiO 2/2 ) g (SiO 4/2 ) h
（Ⅱ）
in the formula (II), the compound is shown in the specification,Meis a methyl group, and the like,Viis a vinyl group;d，e，f，gandhthe polymerization degrees of the five chain links in the formula are respectively, the values of the polymerization degrees determine the viscosity of polysiloxane,gat least one of the group consisting of at least 1,hat least 1, and the viscosity is 100 to 20,000mPas.
R 3 And R 4 Are identical or different substituents selected from:
(1) Alkyl groups having 1 to 30 carbon atoms including methyl, ethyl, n-propyl, isopropyl, butyl, pentyl, hexyl, octyl, decyl, dodecyl, tetradecyl, hexadecyl, octadecyl, eicosyl, docosyl, tetracosyl, hexacosyl, octacosyl, triacontyl;
(2) Aryl radicals, includingα-methylphenylethyl and phenylethyl;
(3) A hydrogen atom.
The dosage of the vinyl-containing polysiloxane is 5 to 45 percent of the total dosage of the vinyl-containing polysiloxane micro powder.
B. Emulsifier
The emulsifier is selected from one or more of octanol polyoxyethylene ether, decanol polyoxyethylene ether, dodecanol polyoxyethylene ether, tetradecanol polyoxyethylene ether, C12-C14 alcohol polyoxyethylene ether, isomeric tridecanol polyoxyethylene ether, hexadecanol polyoxyethylene ether, octadecanol polyoxyethylene ether, oleyl alcohol polyoxyethylene ether, alkynol polyoxyethylene ether, oleic acid polyoxyethylene ether, stearic acid polyoxyethylene ether and alkylphenol polyoxyethylene ether.
The dosage of the emulsifier is 2 to 10 percent of the total dosage of the polysiloxane micro powder.
C. Coating agent
The coating agent refers to a water-soluble protective substance which can form a layer of solid on the surface of polysiloxane particles after emulsion spray drying, and comprises one or a mixture of more of sodium carboxymethylcellulose, hydroxymethyl cellulose, hydroxyethyl cellulose, hydroxypropyl cellulose, gelatin, sodium carboxymethyl starch, polyacrylamide, polyvinyl alcohol, polyacrylic acid and polyvinylpyrrolidone.
The dosage of the coating agent is 2 to 10 percent of the total dosage of the polysiloxane micro powder.
D. Catalyst and process for preparing same
The catalyst is mainly used for catalyzing chemical reaction between silicon hydrogen bond and unsaturated bond. The catalyst is a metal platinum catalyst selected from platinum-alcohol complex, platinum-olefin complex, platinum-alkoxide complex, platinum-ether complex and platinum-ketone complex.
The dosage of the catalyst is 5 to 20ppm (calculated by metal platinum) of the total feeding amount of the polysiloxane micro powder.
E. Water (W)
The water comprises tap water, process water and purified water, and the using amount of the water is 30-80% of the total feeding amount of the polysiloxane micro powder.
The preparation method of the polysiloxane micropowder comprises the following steps:
preparation of hydrogen-containing polysiloxane micropowder:
adding water and an emulsifier into a container, starting stirring, converting to 2000-6000rpm, controlling the temperature to be 50-80 ℃, and stirring for 10-30min to ensure complete dissolution; then, the hydrogenous polysiloxane is slowly added into the mixture for 10 to 60min to ensure that the particle size of the emulsion is 0.1 to 5 mu m, and then the coating agent is added into the emulsion and spray-dried to obtain powdery hydrogenous polysiloxane micro powder.
Preparation of vinyl-containing polysiloxane micropowder:
adding water and an emulsifier into a container, starting stirring and converting to 3000-10000 rpm, controlling the temperature to be 30-60 ℃, and stirring for 10-30min to ensure complete dissolution; then slowly adding vinyl-containing polysiloxane into the mixture, controlling the time to be 20 to 90min so that the particle size of the emulsion is 0.1 to 3 mu m, then adding a catalyst and a coating agent into the emulsion, and performing spray drying to obtain powdery vinyl-containing polysiloxane micropowder.
Preparation of the water repellent silicone composition:
adding an organic carrier into a mixer, starting stirring, adding hydrogen-containing polysiloxane micro powder and vinyl-containing polysiloxane micro powder according to a proportion, controlling the rotating speed to be 1000-3000 rpm, adding an adhesive, granulating and drying to obtain the water-repellent organic silicon composition.
The product has good fluidity and drying property, and no caking, and is easy for storage.
Detailed Description
The species of the hydrogenpolysiloxane A1 in the examples are shown in table 1:
example 1:
adding 35 parts of water and 10 parts of emulsifier decanol polyoxyethylene ether (7) into a container, starting stirring and converting to 2000rpm, controlling the temperature to be 80 ℃, and stirring for 20min to ensure complete dissolution; then, 45 parts of hydrogenpolysiloxane A1-2 was slowly added thereto over a period of 360min so that the particle diameter of the emulsion was D90 = 0.3. Mu.m, and then 10 parts of coating agent sodium carboxymethyl cellulose was added to the emulsion and spray-dried to obtain powdery hydrogenpolysiloxane micropowder PH-1.
Example 2:
adding 60 parts of water, 3 parts of oleyl alcohol polyoxyethylene ether (18) and 2 parts of cetyl alcohol polyoxyethylene ether (18) into a container, starting stirring, converting to 4000rpm, controlling the temperature to be 50 ℃, and stirring for 10min to ensure complete dissolution; then, 30 parts of hydrogenpolysiloxane A1-3 was slowly added thereto for 60min so that the particle diameter of the emulsion was D90 = 5 μm, and then 5 parts of coating agent polyvinylpyrrolidone was added to the emulsion and spray-dried to obtain powdery hydrogenpolysiloxane micropowder PH-2.
Example 3:
adding 80 parts of water and 2 parts of alkylphenol polyoxyethylene ether (18) serving as an emulsifier into a container, starting stirring at 6000rpm, controlling the temperature to be 60 ℃, and stirring for 30min to ensure complete dissolution; then, 16 parts of hydrogenpolysiloxane A1-1 was slowly added thereto for 10min so that the particle diameter of the emulsion was D90 = 0.8. Mu.m, and then 2 parts of coating agent polyvinyl alcohol was added to the emulsion and spray-dried to obtain powdery hydrogenpolysiloxane micropowder PH-3.
Example 4:
adding 78 parts of water and 5 parts of C12-14 polyoxyethylene ether (25) serving as an emulsifier into a container, starting stirring, converting to 3500rpm, controlling the temperature to 65 ℃, and stirring for 25min to ensure complete dissolution; then, 7 parts of hydrogenpolysiloxane A1-5 was slowly added thereto for 55min so that the particle diameter of the emulsion was D90 = 1.3 μm, and then 10 parts of coating agent gelatin was added to the emulsion and spray-dried to obtain powdery hydrogenpolysiloxane micropowder PH-4.
Example 5:
adding 65 parts of water and 5 parts of emulsifier stearic acid polyoxyethylene ether (21) into a container, starting stirring and converting to 4500rpm, controlling the temperature to be 55 ℃, and stirring for 18min to ensure complete dissolution; then, 25 parts of hydrogenpolysiloxane A1-4 was slowly added thereto for 30min so that the particle size of the emulsion was D90 = 4.0. Mu.m, and then 4 parts of coating agent carboxymethyl starch sodium and 1 part of polyvinyl alcohol 2488 were added to the emulsion and spray-dried to obtain powdery hydrogenpolysiloxane micropowder pH-5.
The species of the vinyl-containing polysiloxane A2 in the examples are shown in table 2:
example 6:
adding 40 parts of water and 5 parts of emulsifier lauryl polyoxyethylene ether into a container, starting stirring to convert to 3000rpm, controlling the temperature to be 60 ℃, and stirring for 30min to ensure complete dissolution; then, 45 parts of vinyl-containing polysiloxane A2-5 was slowly added thereto for 90min so that the particle diameter of the emulsion was D90 = 3 μm, and then 10ppm of a platinum-vinyl complex catalyst and 10 parts of polyacrylamide (molecular weight 300 ten thousand) as a coating agent were added to the emulsion and spray-dried to obtain powdery vinyl-containing polysiloxane micropowder PV-1.
Example 7:
adding 80 parts of water and 2 parts of emulsifier oleic acid polyoxyethylene ether (12) into a container, starting stirring to convert to 10000rpm, controlling the temperature to be 30 ℃, and stirring for 10min to ensure complete dissolution; then, 16 parts of vinyl-containing polysiloxane A2-3 was slowly added thereto for 20 minutes so that the particle diameter of the emulsion was D90 = 0.2. Mu.m, and then 5ppm of a catalyst platinum-ether complex and 2 parts of a coating agent polyacrylic acid were added to the emulsion and spray-dried to obtain powdery vinyl-containing polysiloxane micropowder PV-2.
Example 8:
adding 80 parts of water and 3 parts of emulsifier tetradecanol polyoxyethylene ether (25) into a container, starting stirring and converting to 5000rpm, controlling the temperature to be 45 ℃, and stirring for 20min to ensure complete dissolution; then 7 parts of vinyl-containing polysiloxane A2-1 was slowly added thereto for 60min so that the particle diameter of the emulsion was D90 = 1 μm, and then 8ppm of a platinum-isopropanol solution as a catalyst and 10 parts of a coating agent of hydroxypropyl cellulose were added to the emulsion and spray-dried to obtain powdery vinyl-containing polysiloxane micropowder PV-3.
Example 9:
adding 50 parts of water, 6 parts of alkynol polyoxyethylene ether (10) and 4 parts of isomeric tridecanol polyoxyethylene ether (5) into a container, starting stirring and converting to 6000rpm, controlling the temperature to be 35 ℃, and stirring for 25min to ensure complete dissolution; then, 35 parts of vinyl-containing polysiloxane A2-2 was slowly added thereto for 50min so that the particle diameter of the emulsion was D90 = 0.6 μm, and then 18ppm of a platinum-vinyl complex catalyst and 5 parts of hydroxyethyl cellulose as a coating agent were added to the emulsion and spray-dried to obtain powdery vinyl-containing polysiloxane micropowder PV-4.
Example 10:
adding 65 parts of water and 4 parts of emulsifier isomeric tridecanol polyoxyethylene ether (8) into a container, starting stirring and converting to 7500rpm, controlling the temperature to be 50 ℃, and stirring for 15min to ensure complete dissolution; then, 26 parts of vinyl-containing polysiloxane A2-4 was slowly added thereto for a controlled period of 85min so that the particle diameter of the emulsion was D90 = 2.5 μm, and then 9ppm of a platinum-ketone complex catalyst, 3 parts of a sodium polyacrylate as a coating agent, and 2 parts of polyvinyl alcohol 1799 as a coating agent were added to the emulsion and spray-dried to obtain powdery vinyl-containing polysiloxane micropowder PV-5.
Example 11:
adding 85 parts of organic carrier wheat starch into a mixer, starting stirring, adding 1 part of hydrogen-containing polysiloxane micro powder PH-2 and 9 parts of vinyl-containing polysiloxane micro powder PV-5 according to the proportion, controlling the rotating speed to be 1000rpm, adding 5 parts of adhesive polyacrylic acid, granulating and drying to obtain the water-repellent silicone composition SA-1.
Example 12:
adding 33 parts of organic carrier sodium carboxymethyl starch into a mixer, starting stirring, adding 9 parts of hydrogen-containing polysiloxane micro powder PH-4 and 48 parts of vinyl-containing polysiloxane micro powder PV-1 according to the proportion, controlling the rotating speed to be 2500rpm, adding 10 parts of adhesive water, granulating and drying to obtain the water-repellent organic silicon composition SA-2.
Example 13:
adding 60 parts of organic carrier hydroxymethyl cellulose into a mixer, starting stirring, adding 3 parts of hydrogen-containing polysiloxane micro powder PH-1 and 35 parts of vinyl-containing polysiloxane micro powder PV-4 according to the proportion, controlling the rotating speed to be 3000rpm, adding 2 parts of adhesive maleic acid-acrylic acid copolymer, granulating and drying to obtain the water repellent type organic silicon composition SA-3.
Example 14:
adding 62 parts of cationic starch and 15 parts of cellulose into an organic carrier, starting stirring, adding 8 parts of hydrogen-containing polysiloxane micro powder PH-3 and 5 parts of vinyl-containing polysiloxane micro powder PV-3 according to the proportion, controlling the rotating speed to be 1800rpm, adding 2 parts of sodium citrate and 8 parts of polyacrylic acid, granulating and drying to obtain the water-repellent organic silicon composition SA-4.
Comparative example 1:
adding 62 parts of cationic starch and 15 parts of cellulose into an organic carrier, starting stirring, adding 8 parts of hydrogenpolysiloxane A1-1, 5 parts of vinyl-containing polysiloxane A2-1 and 8ppm of catalyst platinum-isopropanol solution according to the proportion, controlling the rotating speed to be 1800rpm, adding 2 parts of sodium citrate and 8 parts of polyacrylic acid, granulating and drying to obtain the water-repellent organic silicon composition SA-4-1.
Comparative example 2:
adding 62 parts of cationic starch and 15 parts of cellulose into an organic carrier, starting stirring, adding 2 parts of hydrogenpolysiloxane A1-1, 11 parts of vinyl-containing polysiloxane A2-1 and 8ppm of catalyst platinum-isopropanol solution according to the proportion, controlling the rotating speed to be 1800rpm, adding 2 parts of sodium citrate and 8 parts of polyacrylic acid, granulating and drying to obtain the water-repellent organic silicon composition SA-4-2.
Comparative example 3:
adding 62 parts of cationic starch and 15 parts of cellulose into an organic carrier, starting stirring, adding 11 parts of hydrogenpolysiloxane A1-1, 2 parts of vinyl-containing polysiloxane A2-1 and 8ppm of catalyst platinum-isopropanol solution according to the proportion, controlling the rotating speed to be 1800rpm, adding 2 parts of sodium citrate and 8 parts of polyacrylic acid, granulating and drying to obtain the water-repellent organic silicon composition SA-4-3.
Comparative example 4:
adding 54 parts of cationic starch and 10 parts of cellulose serving as organic carriers into a mixer, starting stirring, adding 16 parts of hydrogen-containing polysiloxane A1-1, 10 parts of vinyl-containing polysiloxane A2-1 and 8ppm of catalyst platinum-isopropanol solution according to the proportion, controlling the rotating speed to be 1800rpm, adding 2 parts of sodium citrate and 8 parts of polyacrylic acid, granulating and drying to obtain the water-repellent organosilicon composition SA-4-4.
Example 15:
adding 44 parts of carboxymethyl starch sodium starch and 10 parts of hydroxymethyl cellulose into an organic carrier, starting stirring, adding 2 parts of hydrogenpolysiloxane micro powder PH-1, 4 parts of hydrogenpolysiloxane micro powder PH-5, 25 parts of vinyl-containing polysiloxane micro powder PV-2 and 8 parts of vinyl-containing polysiloxane micro powder PV-1 according to the proportion, controlling the rotating speed to be 2150rpm, adding 2 parts of polyvinylpyrrolidone and 5 parts of water, granulating and drying to obtain the water-repellent silicone composition SA-5.
Performance testing of Silicone compositions
In order to verify the effects of the silicone compositions obtained in the present invention, samples of SA1 to SA5, SA-4-1 to SA-4-4 were mixed with concrete, and changes in water absorption inhibition over time were examined.
Preparing a mortar test block: the weight ratio of water to cement is 0.8, the mass ratio of sand to cement is 3.0, the samples SA 1-SA 5, SA-4-1 to SA-4-4 in the examples are added into mortar according to the same addition, and then test blocks of 100mm multiplied by 100mm are prepared and standard maintenance is carried out for 28 days. The water absorption of each mortar test block after soaking in water for 24 hours and 7 days was tested according to the "technical Specification for lightweight aggregate concrete", and then a sample of the organosilicon composition was placed in an oven at 40 ℃ for 3 months and tested again for water absorption inhibition, with the results shown in Table 3.
As can be seen from the water absorption data in table 3, the water absorption inhibiting performance of the proprietary silicone composition samples is good, and the data after 3 months of aging is substantially changed, that is, the water absorption inhibiting performance is not changed; in comparison, comparative examples SA-4-1~4 had higher water absorption for 24h and 7 days and varied significantly; and the water absorption inhibiting property after 3 months of storage is further reduced, that is, the property of the product is degraded. For analytical reasons, it is mainly because the chemical reaction between the hydrogenpolysiloxane and the vinyl-containing polysiloxane is influenced by other factors, and a hydrophobic film covering the surface, even the inside, of the mortar block is not formed; the hydrogenpolysiloxane and the vinyl-containing polysiloxane are separately protected by the coating agent, so that the influence of the hydrogenpolysiloxane and the vinyl-containing polysiloxane on the outside is avoided, particularly the influence of the alkalinity of mortar is avoided, and the water repellent effect is ideal; as can be seen from the results of SA-4-4 of comparative example 4, the desired effect was not achieved even by doubling the amount of polysiloxane, which further illustrates the effect of the coating agent.
Claims (7)
1. The water-repellent organosilicon composition is characterized by comprising an organic carrier, an adhesive, hydrogen-containing polysiloxane micro powder and vinyl polysiloxane micro powder, wherein the mass percent of the hydrogen-containing polysiloxane micro powder and the vinyl polysiloxane micro powder is as follows:
organic carrier: 30 to 90 percent;
adhesive: 2 to 10 percent;
hydrogen-containing polysiloxane micropowder: 1 to 10 percent;
vinyl-containing polysiloxane micropowder: 5 to 50 percent;
the organic carrier is water-soluble organic carrier selected from cellulose, natural starch and modified starch; these carriers may be used alone or in admixture of two or more;
the adhesive is selected from one or more of water, polyacrylic acid, sodium polyacrylate, maleic acid-acrylic acid copolymer, sodium carboxymethyl cellulose, sodium citrate, potassium citrate, alkyl glycoside and polyvinylpyrrolidone;
the hydrogen-containing polysiloxane micro powder consists of hydrogen-containing polysiloxane, an emulsifier, water and a coating agent;
the vinyl-containing polysiloxane micro powder consists of vinyl-containing polysiloxane, an emulsifier, a coating agent, a catalyst and water;
preparation of hydrogen-containing polysiloxane micropowder:
adding water and an emulsifier into a container, starting stirring, converting to 2000-6000rpm, controlling the temperature to be 50-80 ℃, and stirring for 10-30min to ensure complete dissolution; then slowly adding hydrogenous polysiloxane into the mixture for 10 to 60min to ensure that the particle size of the emulsion is 0.1 to 5 mu m, then adding a coating agent into the emulsion, and performing spray drying to obtain powdery hydrogenous polysiloxane micro powder;
preparation of vinyl-containing polysiloxane micropowder:
adding water and an emulsifier into a container, starting stirring and converting to 3000-10000 rpm, controlling the temperature to be 30-60 ℃, and stirring for 10-30min to ensure complete dissolution; then slowly adding vinyl-containing polysiloxane into the mixture, controlling the time to be 20 to 90min, enabling the particle size of the emulsion to be 0.1 to 3 mu m, then adding a catalyst and a coating agent into the emulsion, and performing spray drying to obtain powdery vinyl-containing polysiloxane micropowder;
the preparation of the water-repellent organosilicon composition comprises the following steps:
adding an organic carrier into a mixer, starting stirring, adding hydrogen-containing polysiloxane micro powder and vinyl-containing polysiloxane micro powder according to a proportion, controlling the rotating speed to be 1000-3000 rpm, adding an adhesive, granulating and drying to obtain the water-repellent organic silicon composition.
2. The water repellent silicone composition according to claim 1, wherein said hydrogenpolysiloxane has the following general structural formula:
in the formula (I), subscripta、b、cSubscripts, being three-linkcIs an integer of 1~2; r 1 And R 2 The same or different; r 1 And R 2 Is a hydrocarbon group with 1 to 20 carbon atoms or a hydrogen atom;
the dynamic viscosity of the hydrogenous polysiloxane at 25 ℃ is 2 to 50mPa.s, and the dosage of the hydrogenous polysiloxane is 5 to 45 percent of the total dosage of the hydrogenous polysiloxane micro powder.
3. The water repellent silicone composition according to claim 1, wherein said vinyl-containing polysiloxane has the following general structural formula:
（R 3 Me 2 SiO 1/2 ) d (Me 2 SiO 2/2 ) e (R 4 MeSiO 2/2 ) f (MeViSiO 2/2 ) g (SiO 4/2 ) h
（Ⅱ）
in the formula (II), the compound is shown in the specification,Meis a methyl group, and the like,Viis a vinyl group;d，e，f，gandhthe polymerization degrees of the five chain links in the formula are respectively, the values of the polymerization degrees determine the viscosity of the vinyl-containing polysiloxane,gat least one of the group consisting of at least 1,hat least 1, the viscosity is 100 to 20,000mPa s;
R 3 and R 4 The same or different substituents are selected from alkyl with 1 to 30 carbon atoms, aryl and hydrogen atoms;
the dosage of the vinyl-containing polysiloxane is 5 to 45 percent of the total dosage of the vinyl-containing polysiloxane micro powder.
4. The water repellent silicone composition according to claim 1, wherein the emulsifier is one or more selected from octanol polyoxyethylene ether, decanol polyoxyethylene ether, dodecanol polyoxyethylene ether, tetradecanol polyoxyethylene ether, C12-C14 alcohol polyoxyethylene ether, isomeric tridecanol polyoxyethylene ether, hexadecanol polyoxyethylene ether, octadecanol polyoxyethylene ether, oleyl alcohol polyoxyethylene ether, alkynol polyoxyethylene ether, oleic acid polyoxyethylene ether, stearic acid polyoxyethylene ether and alkylphenol polyoxyethylene ether, and the amount of the emulsifier is 2 to 10% of the total amount of the polysiloxane micropowder.
5. The water repellent silicone composition according to claim 1, wherein the coating agent is selected from one or more of sodium carboxymethylcellulose, hydroxymethylcellulose, hydroxyethylcellulose, hydroxypropylcellulose, gelatin, sodium carboxymethyl starch, polyacrylamide, polyvinyl alcohol, polyacrylic acid, and polyvinylpyrrolidone, and is used in an amount of 2 to 10% of the total amount of the polysiloxane micropowder.
6. The water repellent silicone composition according to claim 1, wherein said catalyst is a metal platinum catalyst selected from the group consisting of platinum-alcohol complexes, platinum-olefin complexes, platinum-alkoxide complexes, platinum-ether complexes, platinum-ketone complexes; the dosage of the metal platinum is 5 to 20ppm of the total feeding amount of the polysiloxane micro powder.
7. The water-repellent silicone composition according to claim 1, wherein the water is tap water, process water or purified water, and the dosage of the water is 30 to 80 percent of the total dosage of the polysiloxane micropowder.
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