CN105669967B - Nano inorganic material of polyether high molecular brush hydridization and preparation method thereof - Google Patents
Nano inorganic material of polyether high molecular brush hydridization and preparation method thereof Download PDFInfo
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- CN105669967B CN105669967B CN201610248301.5A CN201610248301A CN105669967B CN 105669967 B CN105669967 B CN 105669967B CN 201610248301 A CN201610248301 A CN 201610248301A CN 105669967 B CN105669967 B CN 105669967B
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- inorganic material
- hydridization
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- molecular brush
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- 229910010272 inorganic material Inorganic materials 0.000 title claims abstract description 44
- 239000011147 inorganic material Substances 0.000 title claims abstract description 44
- 229920000570 polyether Polymers 0.000 title claims abstract description 41
- 239000004721 Polyphenylene oxide Substances 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000003756 stirring Methods 0.000 claims abstract description 15
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 12
- 230000004044 response Effects 0.000 claims abstract description 11
- 230000002459 sustained effect Effects 0.000 claims abstract description 11
- 239000000243 solution Substances 0.000 claims description 19
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 15
- 238000005406 washing Methods 0.000 claims description 13
- 238000001035 drying Methods 0.000 claims description 10
- 239000002041 carbon nanotube Substances 0.000 claims description 8
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 8
- SMZOGRDCAXLAAR-UHFFFAOYSA-N aluminium isopropoxide Chemical compound [Al+3].CC(C)[O-].CC(C)[O-].CC(C)[O-] SMZOGRDCAXLAAR-UHFFFAOYSA-N 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 7
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical compound CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 claims description 5
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 239000011259 mixed solution Substances 0.000 claims description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 3
- 239000008096 xylene Substances 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 14
- 239000004593 Epoxy Substances 0.000 abstract description 9
- 239000000178 monomer Substances 0.000 abstract description 9
- 229920005862 polyol Polymers 0.000 abstract description 7
- 150000003077 polyols Chemical class 0.000 abstract description 7
- 239000006087 Silane Coupling Agent Substances 0.000 abstract description 5
- 239000003054 catalyst Substances 0.000 abstract description 4
- 229920002635 polyurethane Polymers 0.000 abstract description 4
- 239000004814 polyurethane Substances 0.000 abstract description 4
- 238000011065 in-situ storage Methods 0.000 abstract description 2
- 238000007151 ring opening polymerisation reaction Methods 0.000 abstract description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 30
- 229920000642 polymer Polymers 0.000 description 24
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 18
- 239000000463 material Substances 0.000 description 18
- 238000012986 modification Methods 0.000 description 10
- 230000004048 modification Effects 0.000 description 9
- 239000003921 oil Substances 0.000 description 9
- 239000002245 particle Substances 0.000 description 9
- 239000000377 silicon dioxide Substances 0.000 description 8
- 238000012360 testing method Methods 0.000 description 8
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 6
- 229910021389 graphene Inorganic materials 0.000 description 6
- 239000005543 nano-size silicon particle Substances 0.000 description 6
- 238000006116 polymerization reaction Methods 0.000 description 6
- 235000012239 silicon dioxide Nutrition 0.000 description 6
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 description 5
- UHOVQNZJYSORNB-UHFFFAOYSA-N monobenzene Natural products C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 5
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 4
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 4
- 229920005830 Polyurethane Foam Polymers 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 239000006229 carbon black Substances 0.000 description 3
- -1 glycol ester Chemical class 0.000 description 3
- 239000010954 inorganic particle Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 239000011496 polyurethane foam Substances 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- 241000209094 Oryza Species 0.000 description 2
- 235000007164 Oryza sativa Nutrition 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- 239000005864 Sulphur Substances 0.000 description 2
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 2
- 150000001336 alkenes Chemical class 0.000 description 2
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- WTEOIRVLGSZEPR-UHFFFAOYSA-N boron trifluoride Chemical compound FB(F)F WTEOIRVLGSZEPR-UHFFFAOYSA-N 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N diphenyl Chemical compound C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 2
- 238000009396 hybridization Methods 0.000 description 2
- 239000011256 inorganic filler Substances 0.000 description 2
- 229910003475 inorganic filler Inorganic materials 0.000 description 2
- 229920003225 polyurethane elastomer Polymers 0.000 description 2
- 238000010526 radical polymerization reaction Methods 0.000 description 2
- 235000009566 rice Nutrition 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 239000004332 silver Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- QQQSFSZALRVCSZ-UHFFFAOYSA-N triethoxysilane Chemical compound CCO[SiH](OCC)OCC QQQSFSZALRVCSZ-UHFFFAOYSA-N 0.000 description 2
- YUYCVXFAYWRXLS-UHFFFAOYSA-N trimethoxysilane Chemical compound CO[SiH](OC)OC YUYCVXFAYWRXLS-UHFFFAOYSA-N 0.000 description 2
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 description 1
- RBACIKXCRWGCBB-UHFFFAOYSA-N 1,2-Epoxybutane Chemical class CCC1CO1 RBACIKXCRWGCBB-UHFFFAOYSA-N 0.000 description 1
- FZIIBDOXPQOKBP-UHFFFAOYSA-N 2-methyloxetane Chemical compound CC1CCO1 FZIIBDOXPQOKBP-UHFFFAOYSA-N 0.000 description 1
- 229920000936 Agarose Polymers 0.000 description 1
- 229910015900 BF3 Inorganic materials 0.000 description 1
- 241000790917 Dioxys <bee> Species 0.000 description 1
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 229910003978 SiClx Inorganic materials 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 230000000845 anti-microbial effect Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000004305 biphenyl Substances 0.000 description 1
- 235000010290 biphenyl Nutrition 0.000 description 1
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 1
- 239000004327 boric acid Substances 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
- 150000001721 carbon Chemical class 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 description 1
- GAURFLBIDLSLQU-UHFFFAOYSA-N diethoxy(methyl)silicon Chemical compound CCO[Si](C)OCC GAURFLBIDLSLQU-UHFFFAOYSA-N 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- PKTOVQRKCNPVKY-UHFFFAOYSA-N dimethoxy(methyl)silicon Chemical compound CO[Si](C)OC PKTOVQRKCNPVKY-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 239000000806 elastomer Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- CWAFVXWRGIEBPL-UHFFFAOYSA-N ethoxysilane Chemical compound CCO[SiH3] CWAFVXWRGIEBPL-UHFFFAOYSA-N 0.000 description 1
- SBRXLTRZCJVAPH-UHFFFAOYSA-N ethyl(trimethoxy)silane Chemical compound CC[Si](OC)(OC)OC SBRXLTRZCJVAPH-UHFFFAOYSA-N 0.000 description 1
- LYCAIKOWRPUZTN-UHFFFAOYSA-N ethylene glycol Natural products OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 1
- 229940056319 ferrosoferric oxide Drugs 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 238000007306 functionalization reaction Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229920000578 graft copolymer Polymers 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 230000007773 growth pattern Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 239000003999 initiator Substances 0.000 description 1
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 description 1
- 239000002122 magnetic nanoparticle Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052901 montmorillonite Inorganic materials 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- HXITXNWTGFUOAU-UHFFFAOYSA-N phenylboronic acid Chemical compound OB(O)C1=CC=CC=C1 HXITXNWTGFUOAU-UHFFFAOYSA-N 0.000 description 1
- 229920000058 polyacrylate Polymers 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 150000005846 sugar alcohols Polymers 0.000 description 1
- 230000033772 system development Effects 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- DENFJSAFJTVPJR-UHFFFAOYSA-N triethoxy(ethyl)silane Chemical compound CCO[Si](CC)(OCC)OCC DENFJSAFJTVPJR-UHFFFAOYSA-N 0.000 description 1
- 230000004580 weight loss Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- 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
- C08G65/04—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 only
- C08G65/06—Cyclic ethers having no atoms other than carbon and hydrogen outside the ring
- C08G65/08—Saturated oxiranes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- 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
- C08G65/04—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 only
- C08G65/06—Cyclic ethers having no atoms other than carbon and hydrogen outside the ring
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- 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
- C08G65/04—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 only
- C08G65/06—Cyclic ethers having no atoms other than carbon and hydrogen outside the ring
- C08G65/16—Cyclic ethers having four or more ring atoms
- C08G65/18—Oxetanes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- 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
- C08G65/04—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 only
- C08G65/06—Cyclic ethers having no atoms other than carbon and hydrogen outside the ring
- C08G65/16—Cyclic ethers having four or more ring atoms
- C08G65/20—Tetrahydrofuran
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- 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
- C08G65/04—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 only
- C08G65/22—Cyclic ethers having at least one atom other than carbon and hydrogen outside the ring
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Polyethers (AREA)
- Silicon Compounds (AREA)
Abstract
The invention discloses a kind of nano inorganic material of polyether high molecular brush hydridization and preparation method thereof.First 1~4h will be reacted at 60~100 DEG C obtain functionalized nano inorganic material containing epoxy-terminated silane coupling agent and nano inorganic material; again epoxy monomer is added to the functionalized nano inorganic material; quick stirring and 5~100h of sustained response, obtain the nano inorganic material of polyether high molecular brush hydridization under the conditions of nitrogen protection, catalyst, 50~150 DEG C of oil baths.The present invention triggers the ring-opening polymerisation of epoxy monomer by " from surface grafting " method in nano inorganic material surface in situ, obtain the nano inorganic material of the polyether high molecular brush hydridization of high grafting density, the inorganic material of the polyether high molecular brush hydridization has extraordinary compatibility with polyether polyol, it can realize dispersed, further expand application of the nano inorganic material in polyurethane system.
Description
Technical field
It is special the present invention relates to a kind of polymeric material field and the organic/inorganic hybridization material of field of inorganic materials
It is not related to a kind of nano inorganic material of polyether high molecular brush hydridization and preparation method thereof.
Background technology
The development of nanosecond science and technology is more and more noticeable, and applications to nanostructures is obtained for extensive pass in every field
Note, especially in terms of polymer composite.Nano inorganic material can not only improve the mechanical performance of high molecular material, and
And the functional characteristics such as its many unique light, electricity, magnetic can be assigned so that people are growing day by day to the interest in this field.But
It is the particle diameter very little of nano-particle, high surface energy and specific surface area make it easily reunite, and form offspring, so as to cause point
Dissipate property be deteriorated, its nano effect can not be played, limit itself application and composite material development.Based on the above problem, lead to
Cross to surface modifying inorganic particle, avoid occurring to reunite and luming, realize that it is uniformly and stably dispersed into polymeric system
For the important research topic in the field.By surface grafting polymerization thing polymer brush can be very good improve inorganic filler with it is organic
The interface compatibility of polymer, achievees the purpose that to improve inorganic particulate dispersiveness.
In the growth pattern difference of particle surface and it can be classified as being grafted to surface according to polymeric brush
(Grafting onto) and it is grafted two methods of (Grafting from) polymer from particle surface." being grafted to surface " method
It is to be realized by the reaction of the active group of reactive functional groups on polymer and surface of inorganic particles, this method is simple but first
Steric hindrance can be produced by being grafted on the polymer of particle surface, cause grafting density very low." from surface grafting " method is by being connected to
The initiator of surface of inorganic particles triggers monomer polymerization, in surface grafting polymerization thing.Since small molecule monomer diffusion steric hindrance is small,
" from surface grafting " method can obtain the polymer brush decorative layer that grafting density is high, surface nature is homogeneous, thus as research
Hot spot.Such as：Liu et al. is using Transfer Radical Polymerization respectively via Grafting onto and Grafting from legal systems
For the modification carbon black particle of surface construction butyl polyacrylate polymer brush, the results showed that changed with Grafting from methods
Property carbon black particle surface be covered with dense crown, surface polymer grafting density is high；And use Grafting onto methods
Modified carbon black particle surface is without crown, surface polymer grafting density low (Langmuir, 2003,19 (16):6342-
6345).201510689514.7 inventions of Chinese patent CN are a kind of based on gathering in nano-Ag particles surface grafting methacrylic acid
The method that glycol ester (POEGMA) polymer brush prepares antimicrobial coating, the hybrid material of this polymer brush grafting
The shortcomings that material can overcome silver ion release too fast, and improve the antibacterial activity of elemental silver.Chinese patent CN
A kind of amides compound using the group containing phenyl boric acid of 201510228136.2 inventions is monomer, in magnetic nano-particle poly- third
Olefin(e) acid, silica gel and agarose surface polymerization, prepare the boric acid affinity separation polymer of polymer brush grafting, and this separation material has
Adsorption capacity is high, good, the fast advantage of mass transfer rate of selectivity.However, according to similar compatibility principle, these are in inorganic filler surface
The method of graft polymers polymer brush is not suitable for solving scattering problem of the nano inorganic material in polyether polyol system,
Limit application of the nano inorganic material in polyurethane system (such as polyurethane elastomer, polyurethane foam).
In conclusion the method for the polymeric brush modified Nano inorganic material that most of researchs obtain all is at present
Using radical polymerization, and it is poor with the compatibility of polyether polyol, polyether polyol system can not be applied to.Therefore, for
The organic/inorganic hybridization material that polyether polyol system development goes out polymer brush graft modification has highly important practical valency
Value.
The content of the invention
Of low cost, polyether high molecular brush hydridization suitable for industrialized production received it is an object of the invention to provide a kind of
Rice inorganic material and preparation method thereof, further improves scattering problem of the nano inorganic material in polyether polyol, and expansion is received
Application of the rice inorganic material in polyurethane system (such as polyurethane elastomer, polyurethane foam).
To solve above-mentioned technical problem, one embodiment of the present invention uses following technical scheme：
A kind of preparation method of the nano inorganic material of polyether high molecular brush hydridization, it comprises the following steps：
(1) first solution will be obtained containing epoxy-terminated silane coupling agent is soluble in water, it is then that nano inorganic material is uniform
Ground is scattered in above-mentioned solution, and 1~4h is then reacted under 60~100 DEG C of temperature conditionss, filtered after the completion of reaction, wash
Wash, is dry, obtaining functionalized nano inorganic material；The volume matter of the epoxy-terminated silane coupling agent and nano inorganic material
It is 25mL to measure ratio：0.5~20g；
(2) the functionalized nano inorganic material is scattered in solvent again, under nitrogen protection, sequentially adds epoxy
Class monomer and catalyst, stir evenly；The ratio of the functionalized nano inorganic material, epoxy monomer and catalyst is 1g:1
~20mL:1~5g；
(3) solution that step (2) obtains is put into 50~150 DEG C of oil baths, is quickly stirred with the speed of 200~800rpm
Mix, 5~100h of sustained response, filtered after the completion of reaction, washing, drying, obtain the nano inorganic of polyether high molecular brush hydridization
Material.
The preparation method of the nano inorganic material of above-mentioned polyether high molecular brush hydridization containing epoxy-terminated silane coupling agent
For 3- (2,3- epoxypropoxies) trimethoxy silane, 3- (2,3- epoxypropoxies) triethoxysilane, 3- (2,3- rings
The third oxygen propyl group of oxygen) methyl dimethoxysilane, 3- (2,3- epoxypropoxies) methyldiethoxysilane, 2- (3,4- epoxies
Hexamethylene) ethyl trimethoxy silane, any one in 2- (3,4- 7-oxa-bicyclo[4.1.0s) ethyl triethoxysilane.
Further technical solution is that the preparation method of the nano inorganic material of above-mentioned polyether high molecular brush hydridization contains ring
The silane coupling agent of oxygen end group is 3- (2,3- epoxypropoxies) trimethoxy silanes or 3- (2,3- epoxypropoxies) three
Ethoxysilane.
The nano inorganic material of the preparation method of the nano inorganic material of above-mentioned polyether high molecular brush hydridization is dioxy
Any one in SiClx, ferroso-ferric oxide, montmorillonite, carbon nanotubes, graphene, gold, silver.
Further technical solution is：The preparation method of the nano inorganic material of above-mentioned polyether high molecular brush hydridization uses two
The particle diameter of silica is 7~500nm.
The epoxy monomer of the preparation method of the nano inorganic material of above-mentioned polyether high molecular brush hydridization using ethylene oxide,
Any one or more in propylene oxide, 1,2- epoxy butanes, tetrahydrofuran, epoxy prapanol, methyloxetane.
The catalyst of the preparation method of the nano inorganic material of above-mentioned polyether high molecular brush hydridization is using aluminium isopropoxide, hydrogen-oxygen
Change one kind in potassium, sodium hydroxide, aluminium chloride, iron chloride, boron trifluoride.
In the preparation method of the nano inorganic material of above-mentioned polyether high molecular brush hydridization, step (2) described solvent is benzene, first
One kind in benzene, dimethylbenzene, biphenyl and dimethyl sulfoxide.
In the preparation method of the nano inorganic material of above-mentioned polyether high molecular brush hydridization, step (1) adds the nanometer nothing
It is 1~3 first to adjust the pH value of the solution with the concentrated sulfuric acid before machine material.
The nano inorganic material of the polyether high molecular brush hydridization obtained using above-mentioned preparation method is also that present invention request is protected
The content of shield.
Compared with existing polymer brush hybridized nanometer inorganic material preparation method, the polyether high molecular brush of the invention prepared
The nano inorganic material of hydridization has the characteristics that：1. the polymerization that the present invention uses passes through for ring-opening polymerisation method
Grafting from methods trigger epoxy monomer polymerization in nano inorganic material surface in situ, obtain the poly- of high grafting density
The nano inorganic material of ether polymer brush hydridization.2. due to the polyether high molecular brush decorative layer and polyethers on nano inorganic material surface
Polyalcohol has similar or identical molecular structure so that the inorganic material of the polyether high molecular brush hydridization has with polyether polyol
There is extraordinary compatibility, can realize dispersed, further expanded nano inorganic material in polyurethane system (such as poly- ammonia
Ester elastomer, polyurethane foam etc.) in application.
Brief description of the drawings
Fig. 1 is SiO before and after 1 polyethylene oxide polymer brush graft modification of embodiment2FT-IR spectrograms.
Fig. 2 is SiO before and after 1 polyethylene oxide polymer brush graft modification of embodiment2TGA figure.
Fig. 3 is SiO before and after 1 polyethylene oxide polymer brush graft modification of embodiment2TEM spectrograms.
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to the accompanying drawings and embodiments, it is right
The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.
Embodiment 1：
3- (2,3- epoxypropoxy) trimethoxy silane of 25mL is added in 250mL water, by the way that dense sulphur is added dropwise
Acid adjustment pH value of solution is 2 or so, then the addition 10g nano grade silica particles into above-mentioned mixed solution, ultrasonic disperse 10min,
Reaction temperature is controlled at 80 DEG C, reacts 3h, then, filtered, washing, drying, obtain functionalized nano silica.Weigh 1g
Functionalized nano silica is scattered in 50mL toluene solutions, under nitrogen protection, sequentially adds the ethylene oxide and 2g of 1mL
Aluminium isopropoxide, stir evenly, be put into 80 DEG C of oil baths, quickly stirred with the stir speed (S.S.) of 300rpm, sustained response 24h, warp
Filtering, washing, drying, obtain the nano silicon dioxide of powdered polyether high molecular brush hydridization.
SiO before and after polyethylene oxide polymer brush graft modification2FT-IR spectrograms, TGA figure and TEM spectrograms such as Fig. 1~3.
Its grafting amount is tested using thermal gravimetric analyzer (TGA) to prepared material, test condition is：Nitrogen is protected,
Heating rate：10 DEG C/min, temperature test scope is：40 DEG C~800 DEG C.The thermal weight loss of prepared material is 19.3wt%.
Embodiment 2：
The present embodiment the other the same as in Example 1, difference are：By 1g functionalized nano silica, 50mL is scattered in
In toluene solution, under nitrogen protection, the ethylene oxide of 3mL and the aluminium isopropoxide of 2g are sequentially added, is stirred evenly, be put into 80 DEG C
In oil bath, quickly stirred with the stir speed (S.S.) of 300rpm, sustained response 48h, filtered, washing, drying, it is high to obtain powdered polyethers
The nano silicon dioxide of molecular brush hydridization.Prepared material is used thermal gravimetric analyzer (TGA) test its grafting amount for
17.8wt%.
Embodiment 3：
The present embodiment the other the same as in Example 1, difference are：By 1g functionalized nano silica, 50mL is scattered in
In toluene solution, under nitrogen protection, the ethylene oxide of 5mL and the aluminium isopropoxide of 1g are sequentially added, is stirred evenly, be put into 80 DEG C
In oil bath, quickly stirred with the stir speed (S.S.) of 800rpm, sustained response 24h, filtered, washing, drying, it is high to obtain powdered polyethers
The nano silicon dioxide of molecular brush hydridization.Prepared material is used thermal gravimetric analyzer (TGA) test its grafting amount for
13.5wt%.
Embodiment 4：
The present embodiment the other the same as in Example 1, difference are：By 2g functionalized nano silica, 50mL is scattered in
In toluene solution, under nitrogen protection, the propylene oxide of 10mL and the aluminium isopropoxide of 2g are sequentially added, is stirred evenly, is put into 100
In DEG C oil bath, quickly stirred with the stir speed (S.S.) of 300rpm, sustained response 24h, it is filtered, washing, dry, obtain powdered polyethers
The nano silicon dioxide of polymer brush hydridization.Prepared material is used thermal gravimetric analyzer (TGA) test its grafting amount for
23.6wt%.
Embodiment 5：
The present embodiment the other the same as in Example 1, difference are：By 2g functionalized nano silica, 50mL is scattered in
In toluene solution, under nitrogen protection, the propylene oxide of 5mL and the potassium hydroxide of 2g are sequentially added, is stirred evenly, be put into 80 DEG C
In oil bath, quickly stirred with the stir speed (S.S.) of 500rpm, sustained response 24h, filtered, washing, drying, it is high to obtain powdered polyethers
The nano silicon dioxide of molecular brush hydridization.Prepared material is used thermal gravimetric analyzer (TGA) test its grafting amount for
6.5wt%.
Embodiment 6：
The present embodiment the other the same as in Example 1, difference are：By 2g functionalized nano silica, 50mL is scattered in
In toluene solution, under nitrogen protection, the epoxy prapanol of 10mL and the potassium hydroxide of 2g are sequentially added, is stirred evenly, is put into 130
In DEG C oil bath, quickly stirred with the stir speed (S.S.) of 300rpm, sustained response 24h, it is filtered, washing, dry, obtain powdered polyethers
The nano silicon dioxide of polymer brush hydridization.Prepared material is used thermal gravimetric analyzer (TGA) test its grafting amount for
15.4wt%.
Embodiment 7：
3- (2,3- epoxypropoxy) triethoxysilane of 25mL is added in 250mL water, by the way that dense sulphur is added dropwise
Acid adjustment pH value of solution is 2 or so, then the carbon nanotubes of 5g, ultrasonic disperse 30min, by reaction temperature are added into above-mentioned mixed solution
Degree control reacts 4h at 100 DEG C, and then, filtered, washing, drying, obtain functionalized carbon nano-tube.1g functionalized carbons are weighed to receive
Mitron, is scattered in 50mL xylene solutions, under nitrogen protection, sequentially adds the propylene oxide of 10mL and the isopropanol of 4g
Aluminium, stirs evenly, and is put into 80 DEG C of oil baths, is quickly stirred with the stir speed (S.S.) of 500rpm, sustained response 96h, filtered, wash
Wash, is dry, obtaining the carbon nanotubes of powdered polyether high molecular brush hydridization.Thermal gravimetric analyzer is used to prepared material
(TGA) it is 25.3wt% to test its grafting amount.
Embodiment 8：
3- (2,3- epoxypropoxies) triethoxysilane of 25mL is added to the oxidation that 500mL concentration is 1mg/ml
In graphene aqueous solution, it is 2 or so, ultrasonic disperse 30min by the way that the concentrated sulfuric acid is added dropwise to adjust pH value of solution, reaction temperature control is existed
100 DEG C, 4h is reacted, then, filtered, washing, drying, obtain functional graphene oxide.Weigh 0.5g functionalization graphite oxides
Alkene, is scattered in 50mL dimethyl sulfoxide solutions, under nitrogen protection, sequentially adds the ethylene oxide of 1mL and the aluminium isopropoxide of 1g,
Stir evenly, be put into 80 DEG C of oil baths, quickly stirred with the stir speed (S.S.) of 500rpm, sustained response 24h, filtered, washing, do
It is dry, the graphene oxide of powdered polyether high molecular brush hydridization is obtained, then above-mentioned graphene oxide is reduced by hydrazine hydrate,
Obtain the graphene of polyether high molecular brush hydridization.Its grafting amount is tested using thermal gravimetric analyzer (TGA) to prepared material
For 20.5wt%.
Although reference be made herein to invention has been described for explanatory embodiment of the invention, however, it is to be understood that ability
Field technique personnel can be designed that a lot of other modifications and embodiment, these modifications and embodiment will fall in the application public affairs
Within the spirit and spirit opened.More specifically, can be to the group of theme combination layout in the range of disclosure
A variety of variations and modifications are carried out into component and/or layout.In addition to the variations and modifications carried out to building block and/or layout,
To those skilled in the art, other purposes also will be apparent.
Claims (1)
1. a kind of preparation method of the nano inorganic material of polyether high molecular brush hydridization, it is characterised in that it comprises the following steps：
3- (2,3- epoxypropoxy) triethoxysilane of 25mL is added in 250mL water, by the way that concentrated sulfuric acid tune is added dropwise
Whole pH value of solution is 2, then the carbon nanotubes of 5g is added into above-mentioned mixed solution, and ultrasonic disperse 30min, reaction temperature control is existed
100 DEG C, 4h is reacted, then, filtered, washing, drying, obtain functionalized carbon nano-tube；1g functionalized carbon nano-tubes are weighed, are disperseed
In 50mL xylene solutions, under nitrogen protection, the propylene oxide of 10mL and the aluminium isopropoxide of 4g are sequentially added, stirring is equal
It is even, it is put into 80 DEG C of oil baths, is quickly stirred with the stir speed (S.S.) of 500rpm, sustained response 96h, filtered, washing, drying, obtains
The carbon nanotubes of powdered polyether high molecular brush hydridization.
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| CN106084750A (en) * | 2016-06-21 | 2016-11-09 | 秦廷廷 | A kind of anti-reflection organic silicon modified polyurethane glue being applied to LED plant growth lamp chip package |
| CN107328752A (en) * | 2017-06-23 | 2017-11-07 | 天津科技大学 | A kind of D S ERS substrates based on polymer brush/metallic nanoparticle composite membrane and preparation method thereof |
| CN108362890B (en) * | 2018-02-08 | 2021-04-23 | 南京大学 | Method for enriching, desalting and identifying glycopeptide based on boron-containing comb polymer patterned target plate |
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