CN116355175A - Preparation method for in-situ synthesis of zinc oxide polyurethane emulsion - Google Patents
Preparation method for in-situ synthesis of zinc oxide polyurethane emulsion Download PDFInfo
- Publication number
- CN116355175A CN116355175A CN202310430353.4A CN202310430353A CN116355175A CN 116355175 A CN116355175 A CN 116355175A CN 202310430353 A CN202310430353 A CN 202310430353A CN 116355175 A CN116355175 A CN 116355175A
- Authority
- CN
- China
- Prior art keywords
- zinc oxide
- polyurethane emulsion
- situ synthesized
- mass
- preparing
- Prior art date
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- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 title claims abstract description 171
- 239000011787 zinc oxide Substances 0.000 title claims abstract description 85
- 239000000839 emulsion Substances 0.000 title claims abstract description 62
- 229920002635 polyurethane Polymers 0.000 title claims abstract description 43
- 239000004814 polyurethane Substances 0.000 title claims abstract description 43
- 238000011065 in-situ storage Methods 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 230000015572 biosynthetic process Effects 0.000 title description 6
- 238000003786 synthesis reaction Methods 0.000 title description 5
- 150000001875 compounds Chemical class 0.000 claims abstract description 29
- 239000002243 precursor Substances 0.000 claims abstract description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims abstract description 10
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims abstract description 6
- 150000003751 zinc Chemical class 0.000 claims abstract description 6
- 239000004246 zinc acetate Substances 0.000 claims abstract description 6
- 241000196324 Embryophyta Species 0.000 claims description 30
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 26
- 229920005862 polyol Polymers 0.000 claims description 20
- 238000000034 method Methods 0.000 claims description 19
- 150000003077 polyols Chemical class 0.000 claims description 19
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- 229920001730 Moisture cure polyurethane Polymers 0.000 claims description 16
- 229920000642 polymer Polymers 0.000 claims description 13
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 12
- 239000007787 solid Substances 0.000 claims description 11
- 239000004359 castor oil Substances 0.000 claims description 10
- 239000003054 catalyst Substances 0.000 claims description 10
- 239000003995 emulsifying agent Substances 0.000 claims description 10
- 239000011425 bamboo Substances 0.000 claims description 8
- 235000019438 castor oil Nutrition 0.000 claims description 8
- 238000004090 dissolution Methods 0.000 claims description 8
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- 235000017166 Bambusa arundinacea Nutrition 0.000 claims description 7
- 235000017491 Bambusa tulda Nutrition 0.000 claims description 7
- 241001330002 Bambuseae Species 0.000 claims description 7
- 235000015334 Phyllostachys viridis Nutrition 0.000 claims description 7
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 claims description 7
- 239000012948 isocyanate Substances 0.000 claims description 7
- 238000005303 weighing Methods 0.000 claims description 7
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 6
- 150000002513 isocyanates Chemical class 0.000 claims description 6
- 229920000909 polytetrahydrofuran Polymers 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 238000004945 emulsification Methods 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 238000010025 steaming Methods 0.000 claims description 5
- 239000005057 Hexamethylene diisocyanate Substances 0.000 claims description 4
- 239000005058 Isophorone diisocyanate Substances 0.000 claims description 4
- BCKXLBQYZLBQEK-KVVVOXFISA-M Sodium oleate Chemical compound [Na+].CCCCCCCC\C=C/CCCCCCCC([O-])=O BCKXLBQYZLBQEK-KVVVOXFISA-M 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 125000005442 diisocyanate group Chemical group 0.000 claims description 4
- CCIVGXIOQKPBKL-UHFFFAOYSA-M ethanesulfonate Chemical compound CCS([O-])(=O)=O CCIVGXIOQKPBKL-UHFFFAOYSA-M 0.000 claims description 4
- RRAMGCGOFNQTLD-UHFFFAOYSA-N hexamethylene diisocyanate Chemical compound O=C=NCCCCCCN=C=O RRAMGCGOFNQTLD-UHFFFAOYSA-N 0.000 claims description 4
- NIMLQBUJDJZYEJ-UHFFFAOYSA-N isophorone diisocyanate Chemical compound CC1(C)CC(N=C=O)CC(C)(CN=C=O)C1 NIMLQBUJDJZYEJ-UHFFFAOYSA-N 0.000 claims description 4
- 229920001451 polypropylene glycol Polymers 0.000 claims description 4
- DVKJHBMWWAPEIU-UHFFFAOYSA-N toluene 2,4-diisocyanate Chemical compound CC1=CC=C(N=C=O)C=C1N=C=O DVKJHBMWWAPEIU-UHFFFAOYSA-N 0.000 claims description 4
- 239000002699 waste material Substances 0.000 claims description 4
- 239000012975 dibutyltin dilaurate Substances 0.000 claims description 3
- KSBAEPSJVUENNK-UHFFFAOYSA-L tin(ii) 2-ethylhexanoate Chemical compound [Sn+2].CCCCC(CC)C([O-])=O.CCCCC(CC)C([O-])=O KSBAEPSJVUENNK-UHFFFAOYSA-L 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 2
- KCLIFOXATBWLMW-UHFFFAOYSA-M sodium;ethane-1,2-diamine;ethanesulfonate Chemical group [Na+].NCCN.CCS([O-])(=O)=O KCLIFOXATBWLMW-UHFFFAOYSA-M 0.000 claims description 2
- UPMLOUAZCHDJJD-UHFFFAOYSA-N 4,4'-Diphenylmethane Diisocyanate Chemical compound C1=CC(N=C=O)=CC=C1CC1=CC=C(N=C=O)C=C1 UPMLOUAZCHDJJD-UHFFFAOYSA-N 0.000 claims 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 5
- 239000000463 material Substances 0.000 abstract description 5
- 229910052760 oxygen Inorganic materials 0.000 abstract description 5
- 239000001301 oxygen Substances 0.000 abstract description 5
- 229930003935 flavonoid Natural products 0.000 abstract description 4
- 235000017173 flavonoids Nutrition 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 4
- 239000004480 active ingredient Substances 0.000 abstract description 3
- 235000014113 dietary fatty acids Nutrition 0.000 abstract description 3
- 239000000194 fatty acid Substances 0.000 abstract description 3
- 229930195729 fatty acid Natural products 0.000 abstract description 3
- 150000004665 fatty acids Chemical class 0.000 abstract description 3
- 150000002215 flavonoids Chemical class 0.000 abstract description 3
- 239000012266 salt solution Substances 0.000 abstract description 3
- 229930182490 saponin Natural products 0.000 abstract description 3
- 150000007949 saponins Chemical class 0.000 abstract description 3
- 235000017709 saponins Nutrition 0.000 abstract description 3
- 239000000243 solution Substances 0.000 description 18
- 238000005187 foaming Methods 0.000 description 9
- 239000000843 powder Substances 0.000 description 8
- 238000005189 flocculation Methods 0.000 description 6
- 230000016615 flocculation Effects 0.000 description 6
- 238000003860 storage Methods 0.000 description 6
- 230000002776 aggregation Effects 0.000 description 5
- -1 and meanwhile Substances 0.000 description 5
- 239000012535 impurity Substances 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 238000005054 agglomeration Methods 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 238000010790 dilution Methods 0.000 description 4
- 239000012895 dilution Substances 0.000 description 4
- 238000004321 preservation Methods 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000000945 filler Substances 0.000 description 3
- 239000004088 foaming agent Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 238000010257 thawing Methods 0.000 description 3
- 239000011701 zinc Substances 0.000 description 3
- WRMNZCZEMHIOCP-UHFFFAOYSA-N 2-phenylethanol Chemical compound OCCC1=CC=CC=C1 WRMNZCZEMHIOCP-UHFFFAOYSA-N 0.000 description 2
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 2
- 230000002159 abnormal effect Effects 0.000 description 2
- 230000005856 abnormality Effects 0.000 description 2
- 239000003638 chemical reducing agent Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 239000000178 monomer Substances 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- UOURRHZRLGCVDA-UHFFFAOYSA-D pentazinc;dicarbonate;hexahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Zn+2].[Zn+2].[Zn+2].[Zn+2].[Zn+2].[O-]C([O-])=O.[O-]C([O-])=O UOURRHZRLGCVDA-UHFFFAOYSA-D 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 206010063409 Acarodermatitis Diseases 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- 101100136092 Drosophila melanogaster peng gene Proteins 0.000 description 1
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 1
- 241000221017 Euphorbiaceae Species 0.000 description 1
- 229920002488 Hemicellulose Polymers 0.000 description 1
- 239000004642 Polyimide Substances 0.000 description 1
- 241000447727 Scabies Species 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- GAMYVSCDDLXAQW-AOIWZFSPSA-N Thermopsosid Natural products O(C)c1c(O)ccc(C=2Oc3c(c(O)cc(O[C@H]4[C@H](O)[C@@H](O)[C@H](O)[C@H](CO)O4)c3)C(=O)C=2)c1 GAMYVSCDDLXAQW-AOIWZFSPSA-N 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- PTFCDOFLOPIGGS-UHFFFAOYSA-N Zinc dication Chemical compound [Zn+2] PTFCDOFLOPIGGS-UHFFFAOYSA-N 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 238000007605 air drying Methods 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 235000006708 antioxidants Nutrition 0.000 description 1
- 239000007900 aqueous suspension Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 239000013522 chelant Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000006071 cream Substances 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 150000002009 diols Chemical class 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000001804 emulsifying effect Effects 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000010685 fatty oil Substances 0.000 description 1
- 229930003944 flavone Natural products 0.000 description 1
- 150000002212 flavone derivatives Chemical class 0.000 description 1
- 235000011949 flavones Nutrition 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 210000000497 foam cell Anatomy 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 150000004676 glycans Chemical class 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000010409 ironing Methods 0.000 description 1
- 150000002596 lactones Chemical class 0.000 description 1
- 229920005610 lignin Polymers 0.000 description 1
- 150000002632 lipids Chemical class 0.000 description 1
- 230000000873 masking effect Effects 0.000 description 1
- 238000010907 mechanical stirring Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000002715 modification method Methods 0.000 description 1
- 238000007034 nitrosation reaction Methods 0.000 description 1
- 238000000643 oven drying Methods 0.000 description 1
- 150000007965 phenolic acids Chemical class 0.000 description 1
- 235000017807 phytochemicals Nutrition 0.000 description 1
- 229930000223 plant secondary metabolite Natural products 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 208000005687 scabies Diseases 0.000 description 1
- 230000002000 scavenging effect Effects 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- KQFAFFYKLIBKDE-UHFFFAOYSA-M sodium;ethanesulfonate Chemical compound [Na+].CCS([O-])(=O)=O KQFAFFYKLIBKDE-UHFFFAOYSA-M 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- 239000011573 trace mineral Substances 0.000 description 1
- 235000013619 trace mineral Nutrition 0.000 description 1
- 238000011179 visual inspection Methods 0.000 description 1
- VHBFFQKBGNRLFZ-UHFFFAOYSA-N vitamin p Natural products O1C2=CC=CC=C2C(=O)C=C1C1=CC=CC=C1 VHBFFQKBGNRLFZ-UHFFFAOYSA-N 0.000 description 1
- RNWHGQJWIACOKP-UHFFFAOYSA-N zinc;oxygen(2-) Chemical compound [O-2].[Zn+2] RNWHGQJWIACOKP-UHFFFAOYSA-N 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
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
- C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
- C08G18/6666—Compounds of group C08G18/48 or C08G18/52
- C08G18/6696—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/36 or hydroxylated esters of higher fatty acids of C08G18/38
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/30—Low-molecular-weight compounds
- C08G18/36—Hydroxylated esters of higher fatty acids
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
- C08G18/4825—Polyethers containing two hydroxy groups
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
- C08G18/4854—Polyethers containing oxyalkylene groups having four carbon atoms in the alkylene group
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
- C08G18/72—Polyisocyanates or polyisothiocyanates
- C08G18/73—Polyisocyanates or polyisothiocyanates acyclic
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
- C08G18/72—Polyisocyanates or polyisothiocyanates
- C08G18/74—Polyisocyanates or polyisothiocyanates cyclic
- C08G18/75—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic
- C08G18/751—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring
- C08G18/752—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group
- C08G18/753—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group containing one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate group
- C08G18/755—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group containing one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate group and at least one isocyanate or isothiocyanate group linked to a secondary carbon atom of the cycloaliphatic ring, e.g. isophorone diisocyanate
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
- C08G18/72—Polyisocyanates or polyisothiocyanates
- C08G18/74—Polyisocyanates or polyisothiocyanates cyclic
- C08G18/76—Polyisocyanates or polyisothiocyanates cyclic aromatic
- C08G18/7614—Polyisocyanates or polyisothiocyanates cyclic aromatic containing only one aromatic ring
- C08G18/7621—Polyisocyanates or polyisothiocyanates cyclic aromatic containing only one aromatic ring being toluene diisocyanate including isomer mixtures
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Polyurethanes Or Polyureas (AREA)
Abstract
The invention belongs to the technical field of zinc oxide materials, in particular to a preparation method of in-situ synthesized zinc oxide polyurethane emulsion, which adopts zinc acetate or zinc nitrate inorganic divalent zinc salt solution with simple preparation method and wide raw material sources as a precursor of zinc oxide, utilizes plant polyhydroxy compounds to contain a large amount of plant active ingredients such as flavonoids, saponins, fatty acids and the like, and combines with dissolved oxygen in water to form nano zinc oxide.
Description
Technical Field
The invention belongs to the technical field of zinc oxide materials, and particularly relates to a preparation method for in-situ synthesis of zinc oxide polyurethane emulsion.
Background
Emulsion products containing zinc oxide find application in a variety of fields. For example, people have conventionally used zinc oxide emulsions to wipe on the nose and cheeks to prevent damage from sunlight. In the past, nano zinc oxide or zinc oxide powder is used in which solids are directly blended into an emulsion. However, zinc oxide and a matrix, namely the organic high polymer or resin, have different surface or interface properties, are poor in compatibility, are difficult to uniformly disperse in the matrix, and are easy to cause the defects of reduced mechanical properties, easy embrittlement and the like due to direct or excessive filling, so that the application effect is poor. The inventor starts the research of nano zinc oxide in 1998, the research results have filed a plurality of invention patents to China patent office, wherein CN113621164B utilizes in-situ synthesized zinc oxide emulsion foaming material to generate zinc oxide and plays a role of foaming agent, precursor basic zinc carbonate emulsion of emulsion foaming zinc oxide is uniformly dispersed, particle agglomeration caused by adding filling zinc oxide in the past is avoided, meanwhile, uniformly distributed zinc oxide is generated, gas escape is uniform, emulsion uniformly expands to form uniform-sized air holes, uniform foaming is better, zinc oxide is generated by decomposing basic zinc carbonate, but the method is only limited to emulsion foaming treatment of the surface of high-temperature resistant fiber fabric, and meanwhile, emulsion components are limited to high-temperature resistant polymer emulsion of polyimide emulsion and polytetrafluoroethylene emulsion, so that the method has certain limitation in use. In order to solve the above problems, a preparation method and application of in-situ synthesized zinc oxide polyurethane emulsion are needed to meet the existing market demand and performance requirement.
Disclosure of Invention
Aiming at the problems, the invention aims to provide a preparation method for in-situ synthesis of zinc oxide polyurethane emulsion.
The preparation method of the in-situ synthesized zinc oxide polyurethane emulsion comprises the following steps:
preparing polyurethane prepolymer by reacting polymer polyol, plant polyhydroxy compound and isocyanate, specifically, dehydrating the plant polyhydroxy compound and the polymer polyol in vacuum at 90-100 ℃ and 0.1MPa for 0.5-1 h, weighing 35-40 parts by mass of dehydrated polymer polyol, 7-8 parts by mass of plant polyhydroxy compound and 10-15 parts by mass of diisocyanate in a reaction kettle, mixing and stirring, heating to 75-80 ℃, adding 0.02-0.04 part by mass of catalyst, and reacting for 2-2.5 h by heat preservation and stirring to obtain polyurethane prepolymer;
under the catalysis, plant sources such as bamboo materials and the like can be liquefied into plant polyhydroxy compounds in a liquefying agent.
For example, castor oil is a fatty oil extracted from seeds of castor oil, a plant of the family Euphorbiaceae, and has been used in medicine to treat dry stool, sores, scabies, burns, etc.
For another example, the bamboo extract contains flavone, phenolic acid, lactone, polysaccharide, trace elements and other physiologically active substances, and has the effects of scavenging active oxygen free radicals, blocking nitrosation reaction, reducing blood lipid and the like.
b. Weighing inorganic bivalent water-soluble zinc salt, adding deionized water, and performing ultrasonic dissolution to obtain zinc oxide precursor solution;
c. and adding a mixture of 2-4 parts by mass of ethanol and 120-140 parts by mass of acetone into the polyurethane prepolymer, adding a zinc oxide precursor solution and an emulsifier, continuously stirring at 50-60 ℃ for 0.5-1 hour for emulsification, then steaming out the acetone at the normal pressure of 94 ℃ until no smell is detected, cooling to room temperature, and adding water to dilute the required concentration to obtain the in-situ synthesized zinc oxide polyurethane emulsion.
Further, the polymer is at least one of polytetrahydrofuran glycol and polypropylene glycol, and the molecular weight is 100-3000.
Further, the diisocyanate is at least one of isophorone diisocyanate, hexamethylene diisocyanate and toluene diisocyanate.
Further, the zinc oxide precursor solution is 0.25-0.5 mol/L.
Further, the solid content of the in-situ synthesized zinc oxide polyurethane emulsion in the step c is 25% -50%, and the emulsifier is sodium ethylenediamine ethanesulfonate or sodium oleate ethanesulfonate, and accounts for 0.5% -0.8% of the mass of the in-situ synthesized zinc oxide polyurethane emulsion.
Further, the plant polyhydroxy compound comprises one of bamboo waste liquefied polyhydroxy compound and castor oil polyol.
Further, the inorganic divalent water-soluble zinc salt in the step b is zinc nitrate or zinc acetate.
Further, the catalyst in the step a is one of dibutyl tin dilaurate and stannous octoate.
The mechanism of in-situ synthesis of nano zinc oxide by plant polyhydroxy compounds is as follows:
the invention has the beneficial effects that:
the inventors have tried to replace the conventional zinc oxide with nano zinc oxide in actual production, and the disadvantage of agglomeration has not been solved effectively yet. In the prior art, a large number of complex and complicated zinc oxide surface modification methods are adopted, but the steps are complicated, and the cost is high.
In the daily practice of zinc oxide polyurethane emulsion production, it has been found by accident that a batch of polyurethane emulsion is formed on a substrate with a thin coating thickness and a very flat surface effect. The present inventors have found that this is due to the fact that the aqueous suspension, which is to be added as nano zinc oxide, is due to operator error, and that the precursor salt solution, which is not zinc oxide, is added to the polyurethane emulsion during the preparation of the polyurethane emulsion, and because the plant polyol, which is used as the monomer component of the polyol, is present. Through multiple practices, the preparation process of the zinc oxide in-situ synthesized zinc oxide polyurethane emulsion is formed.
The invention uses compound polyol, plant polyhydroxy compound and isocyanate to react to prepare polyurethane prepolymer, and adopts zinc oxide precursor solution to emulsify, the plant polyhydroxy compound is used as reaction monomer to react with isocyanate to generate polyurethane, and also plays the role of reducing agent to generate zinc oxide in situ, the plant polyhydroxy compound contains a large amount of plant active ingredients such as flavonoids, saponins and fatty acids, and the like, and the compounds often serve as antioxidants to neutralize active oxygen, free radicals and chelate metals, in particular polyhydroxy flavonoid compounds can serve as masking agents and biological reducing agents to promote the formation of nano particles. Zn (II) interacts with phytochemical molecules in the extract and is reduced into Zn (0), and the aggregation of Zn (0) can be prevented due to the existence of active molecules, and finally, the Zn (0) and dissolved oxygen in water are combined to synthesize nano zinc oxide in situ and uniformly dispersed in polyurethane emulsion.
Compared with the prior art, the invention has the following advantages:
in a polyurethane emulsion formula system, in order to better improve various performances of emulsion and reduce cost, fine powder or superfine powder filler is often added, but because the specific surface area of the superfine powder filler is large, the superfine powder filler is easy to agglomerate and is extremely easy to adhere to each other to form agglomeration, the polyurethane emulsion is difficult to fluidize normally like common powder in the using process, a conveying pipeline is often blocked, the interaction force among fine powder particles is mainly Van der Waals force, and the existing superfine powder is almost universally ground in superfine mode, and the production cost is high and dust pollution exists. In the prior production practice, the preparation of the polyurethane emulsion containing zinc oxide also distributes zinc oxide into the polyurethane emulsion by means of additional addition and mechanical stirring, but the defect of agglomeration is still not solved.
The invention adopts zinc acetate or zinc nitrate inorganic divalent zinc salt solution with simple preparation method and wide raw material sources as a precursor of zinc oxide, utilizes plant polyhydroxy compounds to contain a large amount of plant active ingredients such as flavonoids, saponins, fatty acids and the like, and combines with dissolved oxygen in water to form nano zinc oxide. After the foaming agent is added, the method and the product of the invention can also be used for foaming treatment of the surfaces of cotton, polyester and other fibers which are not resistant to high temperature, and after drying and baking, the pattern is foamed and thickened to present a three-dimensional state, and meanwhile, the zinc oxide nano particles are generated in situ, the film layer formed by the emulsion, or the surface foaming layer has certain antibacterial and photosensitive degradation performance, thus realizing better and more beautiful coating appearance than common powder and reducing the production cost.
Description of the embodiments
The invention is illustrated, but not limited, by the following specific examples.
Examples
Preparing raw materials: castor oil polyol YC-CY-210, 1000 polypropylene glycol 200 parts, YC-CY-210 castor oil polyol 35 parts, catalyst Heng Guang T-12 dibutyl tin dilaurate, silver photochemical TDI-100 toluene diisocyanate 75 parts, ethanol 2 parts and acetone 120 parts.
Firstly, weighing zinc acetate, adding deionized water, performing ultrasonic dissolution to obtain a zinc oxide precursor solution, and performing ultrasonic dissolution to obtain a zinc oxide precursor solution, wherein the concentration of the zinc oxide precursor solution is 0.5mol/L;
secondly, reacting plant polyhydroxy compound-castor oil polyol with isocyanate to prepare polyurethane prepolymer, vacuum dehydrating the plant polyhydroxy compound and polymer polyol at 100 ℃ and 0.1MPa for 1h, heating to 60 ℃ to dissolve the plant polyhydroxy compound in the polypropylene glycol, heating to 80 ℃, adding 0.04 parts by mass of catalyst T-12, then slowly dropwise adding TDI-100 toluene diisocyanate, reacting for 2h under heat preservation and stirring to obtain polyurethane prepolymer;
and thirdly, adding a mixture of ethanol and acetone into the polyurethane prepolymer, adding a zinc oxide precursor solution and an emulsifier sodium oleate ethanesulfonate, continuously stirring at 7000rpm at 50 ℃ for 0.5 hour for emulsification, wherein the emulsifier accounts for 0.8% of the mass of the in-situ synthesized zinc oxide polyurethane emulsion, then steaming out the acetone at the normal pressure of 94 ℃ until no smell is detected, and cooling to room temperature to obtain the in-situ synthesized zinc oxide polyurethane emulsion with the solid content of 50%.
The product is as follows: the appearance was a milky emulsion of pH6 with 50% cream solids without mechanical impurities, no floc, 15% ash. The storage stability at 50 ℃ is free from abnormality, hard lump, floccule, obvious layering and skinning, the freezing and thawing stability for 3 times is free from hard lump and flocculation, the dilution stability is 1:12, the flocculation is free, uniform liquid can be formed, the mechanical stability is free from demulsification, and obvious floccule is free.
Comparative example 1
In this comparative example, in comparison with example 1, the zinc oxide precursor solution was not added in the third step, but water and zinc oxide JH-1 produced by Jinhua zinc oxide mill, wherein zinc oxide was 15% of the emulsion mass, and the remaining steps were the same as example 1.
The product is as follows: the emulsion of pH6 which has no mechanical impurities in appearance and a milky white solid content of 20% and has a small amount of floccules has a small amount of hard lumps, a small amount of floccules, a small amount of layering and skinning in storage at 50 ℃, has no hard lumps and no flocculation in 3 times of freeze thawing stability, has no dilution stability of 1:12, has no flocculation, can form uniform liquid, has no demulsification in mechanical stability, and has no obvious floccules.
Examples
Castor oil polyol YC-CY-210, PTG PTMEG-1000 polytetrahydrofuran glycol 200 parts, YC-CY-310 castor oil polyol 35 parts, kosmos 29 stannous octoate catalyst, isophorone diisocyanate 50 parts, ethanol 4 parts, and acetone 140 parts.
Firstly, weighing zinc acetate, adding deionized water, performing ultrasonic dissolution to obtain a zinc oxide precursor solution, and performing ultrasonic dissolution to obtain a zinc oxide precursor solution, wherein the concentration of the zinc oxide precursor solution is 0.25mol/L;
secondly, reacting polytetrahydrofuran glycol, plant polyhydroxy compound-castor oil polyol and isocyanate to prepare polyurethane prepolymer, vacuum dehydrating the plant polyhydroxy compound and the polymer polyol at 90 ℃ and 0.1MPa for 0.5h, heating to 60 ℃ to dissolve the plant polyhydroxy compound in the tetrahydrofuran glycol, heating to 75 ℃, adding 0.02 mass part of catalyst, then slowly dropwise adding isophorone diisocyanate, and reacting for 2.5h under heat preservation and stirring to obtain the polyurethane prepolymer;
and thirdly, adding a mixture of ethanol and acetone into the polyurethane prepolymer, adding zinc oxide precursor solution and emulsifier sodium oleate ethanesulfonate, continuously stirring at 8000rpm at 50 ℃ for 0.5 hour for emulsification, wherein the emulsifier accounts for 0.5% of the mass of the in-situ synthesized zinc oxide polyurethane emulsion, then steaming out acetone at normal pressure of 94 ℃ until no smell is detected, and cooling to room temperature to obtain the in-situ synthesized zinc oxide polyurethane emulsion with 25% of solid content.
The product is as follows: the emulsion with the pH of 6 and the milky white solid content of 25 percent and without mechanical impurities and floccules has no abnormality in storage stability at 50 ℃, no hard lump, no floccules, no obvious layering and skinning, no hard lump and no flocculation in 3 times of freeze thawing stability, no dilution stability of 1:12 and no flocculation, and can form uniform liquid; mechanical stability: does not break emulsion and has no obvious floccule.
Examples
Referring to (Liu Yuhuan, high Long Lan, peng Gong, zhou Houde, ruan Rongsheng. Study of liquefaction of bamboo waste to produce polyhydroxy compounds [ J ]. Modern chemical, 2008 (S2): 214-217.), a process for producing plant polyhydroxy compounds, wherein the bamboo material is a plant polyhydroxy compound comprising mountain forest head dragon table Mao Zhuliao, wherein water is 10.13%, ash is 1.60%, cellulose is 46.34%, hemicellulose is 18.76%, lignin 23.68%, phenethyl alcohol extract is 9.50%. The liquefying conditions are that the temperature is 160 ℃, the consumption of concentrated sulfuric acid is 3%, the adding amount of bamboo scraps is 30%, the reaction is carried out for 120min, the liquefying efficiency reaches 95%, the hydroxyl value of the polyhydroxy compound of the liquefied product is 205mg (KOH)/g, and the viscosity is 890 mPa.s.
Preparing raw materials: 175 parts of PTG company PTMEG-1000 polytetrahydrofuran glycol, 27.0 parts of liquefied product polyhydroxy compound, a T-12 dibutyl tin laurate catalyst, 50 parts of TPA-100 hexamethylene diisocyanate, 3 parts of ethanol and 130 parts of acetone.
Firstly, weighing zinc nitrate, adding deionized water, performing ultrasonic dissolution to obtain a zinc oxide precursor solution, and performing ultrasonic dissolution to obtain a zinc oxide precursor solution, wherein the concentration of the zinc oxide precursor solution is 0.25mol/L;
secondly, liquefying plant polyhydroxy compound-bamboo waste to prepare polyhydroxy compound isocyanate, reacting to prepare polyurethane prepolymer, dehydrating the plant polyhydroxy compound and polymer polyol under the conditions of 100 ℃ and 0.1MPa for 0.5h, heating to 60 ℃ to dissolve the plant polyhydroxy compound in polytetrahydrofuran diol, heating to 76 ℃, adding 0.04 parts by mass of catalyst, slowly dropwise adding hexamethylene diisocyanate, reacting for 2.2h under heat preservation and stirring to obtain polyurethane prepolymer;
thirdly, when the viscosity of the polyurethane prepolymer is measured to be about 84000CPS, adding a mixture of ethanol and acetone, adding zinc oxide precursor solution and emulsifier ethylenediamine-based sodium ethanesulfonate, continuously stirring at 6000rpm at 55 ℃ for 0.7 hour for emulsification, wherein the emulsifier accounts for 0.6% of the mass of the in-situ synthesized zinc oxide polyurethane emulsion, then steaming acetone at the normal pressure of 94 ℃ until no smell is detected, and cooling to the room temperature to obtain the in-situ synthesized zinc oxide polyurethane emulsion with the solid content of 25%.
The product is as follows: no mechanical impurities, opalescent emulsion of pH6 with 25% translucent solids without floc, ash 7.5%.
The storage stability at 50 ℃ is not abnormal, the film hardness is 45.8 Shore A, the film tensile strength is 8.9MPa, and the film elongation at break is 311.4%.
Comparative example 2
In this comparative example, as compared with example 3, 25% polyurethane emulsion was obtained by adding nano zinc oxide JH-1 of Jinhua zinc oxide factory in mountain county in the same mass content without adding zinc oxide precursor solution in example 3, and emulsifying in the same procedure.
The product is as follows: an emulsion of opalescent blue light semitransparent solid content of 20% at pH6 without mechanical impurities with a small amount of floc.
The storage stability at 50 ℃ is not abnormal, the film hardness is 46 Shore A, the film tensile strength is 8.2MPa, and the film elongation at break is 304.5%.
Wherein the tensile strength, elongation at break and hardness of the film are measured according to QB/T2415.
Examples
Preparing a foaming coating by utilizing in-situ synthesized zinc oxide polyurethane emulsion:
the in-situ synthesized zinc oxide polyurethane emulsion obtained in example 3 is added with a strong foamability polyurethane emulsion foaming agent AFCONA-7380 with the mass ratio of 4 percent to carry out polyurethane emulsion foaming, so that fine and uniform foam cells can be formed, and the height of the foam can be keptStability. Printing with manual platen screen with screen mesh size of 120 mesh, oven drying or air drying, and ironing with YP500 flat plate under 100kg/cm 2， The temperature was 120℃and the time was 4s.
The product has smooth and average surface after foaming and good fastness.
Note that: wherein the test conditions are as follows: the temperature in the laboratory was 23℃and the humidity was 50%, the condition was adjusted before the test of the sample, the time of the sample was 6 hours, the reagents for the test were analytically pure and three-stage water as specified in GB/T6682, and the samples were uniformly and thinly coated on a clean glass plate with a glass rod for appearance and examined by visual inspection. The mass fraction of the non-volatile matters is at the constant temperature of 150 ℃ and the drying time of 60min, and other methods are carried out according to the method specified by 5.2 in GB/T11175-2002; the pH value is carried out according to the method specified in GB/T8325; the freeze-thaw stability was performed as specified in GB/T11175-2002 at 5.5. The storage stability was carried out according to the method specified in GB/T11175-2002 at 5.6. Dilution stability was carried out according to the procedure specified in GB/T11175-2002 at 5.7. Mechanical stability is carried out in accordance with the procedure specified in GB/T11175-2002, 5.8.
Claims (8)
1. The preparation method of the in-situ synthesized zinc oxide polyurethane emulsion is characterized by comprising the following steps of:
a. preparing polyurethane prepolymer by reacting polymer polyol, plant polyhydroxy compound and isocyanate, specifically, dehydrating the plant polyhydroxy compound and the polymer polyol in vacuum at 90-100 ℃ and 0.1MPa for 0.5-1 h, weighing 35-40 parts by mass of dehydrated polymer polyol, 7-8 parts by mass of plant polyhydroxy compound and 10-15 parts by mass of diisocyanate in a reaction kettle, mixing and stirring, heating to 75-80 ℃, adding 0.02-0.04 part by mass of catalyst, preserving heat and stirring for 2-2.5 h to obtain polyurethane prepolymer;
b. weighing inorganic bivalent water-soluble zinc salt, adding deionized water, and performing ultrasonic dissolution to obtain zinc oxide precursor solution;
c. and adding a mixture of 2-4 parts by mass of ethanol and 120-140 parts by mass of acetone into the polyurethane prepolymer, adding a zinc oxide precursor solution and an emulsifier, continuously stirring at 50-60 ℃ for 0.5-1 hour for emulsification, then steaming out the acetone at the normal pressure of 94 ℃ until no smell is detected, cooling to room temperature, and adding water to dilute the required concentration to obtain the in-situ synthesized zinc oxide polyurethane emulsion.
2. The method for preparing the in-situ synthesized zinc oxide polyurethane emulsion according to claim 1, wherein the polymer is at least one of polytetrahydrofuran glycol and polypropylene glycol, and the molecular weight is 100-3000.
3. The method for preparing the in-situ synthesized zinc oxide polyurethane emulsion according to claim 1, wherein the diisocyanate is at least one of isophorone diisocyanate, hexamethylene diisocyanate, toluene diisocyanate and diphenylmethane diisocyanate.
4. The method for preparing the in-situ synthesized zinc oxide polyurethane emulsion according to claim 1, wherein the zinc oxide precursor solution contains 0.25-0.5 mol/L.
5. The method for preparing the in-situ synthesized zinc oxide polyurethane emulsion according to claim 1, wherein the solid content of the in-situ synthesized zinc oxide polyurethane emulsion in the step c is 25% -50%, and the emulsifier is sodium ethylenediamine ethanesulfonate or sodium oleate ethanesulfonate, and accounts for 0.5% -0.8% of the mass of the in-situ synthesized zinc oxide polyurethane emulsion.
6. The method for preparing an in-situ synthesized zinc oxide polyurethane emulsion according to claim 1, wherein the plant polyhydroxy compound comprises one of bamboo waste liquefied polyhydroxy compound and castor oil polyol.
7. The method for preparing an in-situ synthesized zinc oxide polyurethane emulsion according to claim 1, wherein the inorganic divalent water-soluble zinc salt in the step b is zinc nitrate or zinc acetate.
8. The method for preparing the in-situ synthesized zinc oxide polyurethane emulsion according to claim 1, wherein the catalyst in the step a is one of dibutyl tin dilaurate and stannous octoate.
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| CN111087061A (en) * | 2018-10-23 | 2020-05-01 | 南通安广美术图案设计有限公司 | Green preparation method of nano-iron |
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| US20080188605A1 (en) * | 2005-01-24 | 2008-08-07 | Lubrizol Advanced Materials, Inc. | Aqueous Dispersions Of Nanoparticle/Polyurethane Composites |
| CN111087061A (en) * | 2018-10-23 | 2020-05-01 | 南通安广美术图案设计有限公司 | Green preparation method of nano-iron |
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