CN1513590A - Nano-level iron oxide dispersion liquid and its preparation method - Google Patents
Nano-level iron oxide dispersion liquid and its preparation method Download PDFInfo
- Publication number
- CN1513590A CN1513590A CNA031335276A CN03133527A CN1513590A CN 1513590 A CN1513590 A CN 1513590A CN A031335276 A CNA031335276 A CN A031335276A CN 03133527 A CN03133527 A CN 03133527A CN 1513590 A CN1513590 A CN 1513590A
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- Prior art keywords
- nano
- level iron
- ether
- oxidate
- dispersion solution
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- 238000002360 preparation method Methods 0.000 title claims description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims description 3
- 239000007788 liquid Substances 0.000 title abstract description 24
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims abstract description 77
- 239000003381 stabilizer Substances 0.000 claims abstract description 15
- -1 disperser Substances 0.000 claims abstract description 13
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 92
- 239000006185 dispersion Substances 0.000 claims description 53
- 229910052742 iron Inorganic materials 0.000 claims description 46
- 239000002270 dispersing agent Substances 0.000 claims description 34
- 239000000843 powder Substances 0.000 claims description 34
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 22
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 18
- 229920000642 polymer Polymers 0.000 claims description 18
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 15
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 15
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 15
- 239000011248 coating agent Substances 0.000 claims description 14
- 238000000576 coating method Methods 0.000 claims description 14
- 229910002588 FeOOH Inorganic materials 0.000 claims description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 239000007822 coupling agent Substances 0.000 claims description 10
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 9
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 9
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 claims description 9
- 239000002131 composite material Substances 0.000 claims description 9
- 239000012530 fluid Substances 0.000 claims description 9
- 229930195733 hydrocarbon Natural products 0.000 claims description 9
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- JOLQKTGDSGKSKJ-UHFFFAOYSA-N 1-ethoxypropan-2-ol Chemical compound CCOCC(C)O JOLQKTGDSGKSKJ-UHFFFAOYSA-N 0.000 claims description 6
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- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 6
- BTANRVKWQNVYAZ-UHFFFAOYSA-N butan-2-ol Chemical compound CCC(C)O BTANRVKWQNVYAZ-UHFFFAOYSA-N 0.000 claims description 6
- DKPFZGUDAPQIHT-UHFFFAOYSA-N butyl acetate Chemical compound CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 claims description 6
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- ZXEKIIBDNHEJCQ-UHFFFAOYSA-N isobutanol Chemical compound CC(C)CO ZXEKIIBDNHEJCQ-UHFFFAOYSA-N 0.000 claims description 6
- HJOVHMDZYOCNQW-UHFFFAOYSA-N isophorone Chemical compound CC1=CC(=O)CC(C)(C)C1 HJOVHMDZYOCNQW-UHFFFAOYSA-N 0.000 claims description 6
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 6
- ULWHHBHJGPPBCO-UHFFFAOYSA-N propane-1,1-diol Chemical class CCC(O)O ULWHHBHJGPPBCO-UHFFFAOYSA-N 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 229910002012 Aerosil® Inorganic materials 0.000 claims description 5
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- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 4
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- HGCIXCUEYOPUTN-UHFFFAOYSA-N cyclohexene Chemical compound C1CCC=CC1 HGCIXCUEYOPUTN-UHFFFAOYSA-N 0.000 claims description 4
- XMGQYMWWDOXHJM-UHFFFAOYSA-N limonene Chemical compound CC(=C)C1CCC(C)=CC1 XMGQYMWWDOXHJM-UHFFFAOYSA-N 0.000 claims description 4
- 239000000314 lubricant Substances 0.000 claims description 4
- XNLICIUVMPYHGG-UHFFFAOYSA-N pentan-2-one Chemical compound CCCC(C)=O XNLICIUVMPYHGG-UHFFFAOYSA-N 0.000 claims description 4
- ODLMAHJVESYWTB-UHFFFAOYSA-N propylbenzene Chemical compound CCCC1=CC=CC=C1 ODLMAHJVESYWTB-UHFFFAOYSA-N 0.000 claims description 4
- UOCLXMDMGBRAIB-UHFFFAOYSA-N 1,1,1-trichloroethane Chemical class CC(Cl)(Cl)Cl UOCLXMDMGBRAIB-UHFFFAOYSA-N 0.000 claims description 3
- DURPTKYDGMDSBL-UHFFFAOYSA-N 1-butoxybutane Chemical compound CCCCOCCCC DURPTKYDGMDSBL-UHFFFAOYSA-N 0.000 claims description 3
- OAYXUHPQHDHDDZ-UHFFFAOYSA-N 2-(2-butoxyethoxy)ethanol Chemical compound CCCCOCCOCCO OAYXUHPQHDHDDZ-UHFFFAOYSA-N 0.000 claims description 3
- VXQBJTKSVGFQOL-UHFFFAOYSA-N 2-(2-butoxyethoxy)ethyl acetate Chemical compound CCCCOCCOCCOC(C)=O VXQBJTKSVGFQOL-UHFFFAOYSA-N 0.000 claims description 3
- CUDYYMUUJHLCGZ-UHFFFAOYSA-N 2-(2-methoxypropoxy)propan-1-ol Chemical compound COC(C)COC(C)CO CUDYYMUUJHLCGZ-UHFFFAOYSA-N 0.000 claims description 3
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims description 3
- POAOYUHQDCAZBD-UHFFFAOYSA-N 2-butoxyethanol Chemical compound CCCCOCCO POAOYUHQDCAZBD-UHFFFAOYSA-N 0.000 claims description 3
- NQBXSWAWVZHKBZ-UHFFFAOYSA-N 2-butoxyethyl acetate Chemical compound CCCCOCCOC(C)=O NQBXSWAWVZHKBZ-UHFFFAOYSA-N 0.000 claims description 3
- ZNQVEEAIQZEUHB-UHFFFAOYSA-N 2-ethoxyethanol Chemical compound CCOCCO ZNQVEEAIQZEUHB-UHFFFAOYSA-N 0.000 claims description 3
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 3
- NTIZESTWPVYFNL-UHFFFAOYSA-N Methyl isobutyl ketone Chemical compound CC(C)CC(C)=O NTIZESTWPVYFNL-UHFFFAOYSA-N 0.000 claims description 3
- UIHCLUNTQKBZGK-UHFFFAOYSA-N Methyl isobutyl ketone Natural products CCC(C)C(C)=O UIHCLUNTQKBZGK-UHFFFAOYSA-N 0.000 claims description 3
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 claims description 3
- 150000001298 alcohols Chemical class 0.000 claims description 3
- 239000004411 aluminium Substances 0.000 claims description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 3
- 229910052782 aluminium Inorganic materials 0.000 claims description 3
- 150000004945 aromatic hydrocarbons Chemical class 0.000 claims description 3
- 125000004855 decalinyl group Chemical group C1(CCCC2CCCCC12)* 0.000 claims description 3
- GJRQTCIYDGXPES-UHFFFAOYSA-N iso-butyl acetate Natural products CC(C)COC(C)=O GJRQTCIYDGXPES-UHFFFAOYSA-N 0.000 claims description 3
- FGKJLKRYENPLQH-UHFFFAOYSA-M isocaproate Chemical compound CC(C)CCC([O-])=O FGKJLKRYENPLQH-UHFFFAOYSA-M 0.000 claims description 3
- OQAGVSWESNCJJT-UHFFFAOYSA-N isovaleric acid methyl ester Natural products COC(=O)CC(C)C OQAGVSWESNCJJT-UHFFFAOYSA-N 0.000 claims description 3
- 239000003350 kerosene Substances 0.000 claims description 3
- 150000002576 ketones Chemical class 0.000 claims description 3
- 229940043265 methyl isobutyl ketone Drugs 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 239000003921 oil Substances 0.000 claims description 3
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 3
- FIABMSNMLZUWQH-UHFFFAOYSA-N propyl 2-methoxyacetate Chemical compound CCCOC(=O)COC FIABMSNMLZUWQH-UHFFFAOYSA-N 0.000 claims description 3
- LLHKCFNBLRBOGN-UHFFFAOYSA-N propylene glycol methyl ether acetate Chemical compound COCC(C)OC(C)=O LLHKCFNBLRBOGN-UHFFFAOYSA-N 0.000 claims description 3
- 150000003505 terpenes Chemical class 0.000 claims description 3
- 235000007586 terpenes Nutrition 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 2
- FGLBSLMDCBOPQK-UHFFFAOYSA-N 2-nitropropane Chemical compound CC(C)[N+]([O-])=O FGLBSLMDCBOPQK-UHFFFAOYSA-N 0.000 claims description 2
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 2
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 2
- MRABAEUHTLLEML-UHFFFAOYSA-N Butyl lactate Chemical compound CCCCOC(=O)C(C)O MRABAEUHTLLEML-UHFFFAOYSA-N 0.000 claims description 2
- 239000001293 FEMA 3089 Substances 0.000 claims description 2
- NHTMVDHEPJAVLT-UHFFFAOYSA-N Isooctane Chemical compound CC(C)CC(C)(C)C NHTMVDHEPJAVLT-UHFFFAOYSA-N 0.000 claims description 2
- 239000005642 Oleic acid Substances 0.000 claims description 2
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 2
- 235000021355 Stearic acid Nutrition 0.000 claims description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 2
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 2
- NUPSHWCALHZGOV-UHFFFAOYSA-N acetic acid n-decyl ester Natural products CCCCCCCCCCOC(C)=O NUPSHWCALHZGOV-UHFFFAOYSA-N 0.000 claims description 2
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- 239000001191 butyl (2R)-2-hydroxypropanoate Substances 0.000 claims description 2
- 150000001732 carboxylic acid derivatives Chemical class 0.000 claims description 2
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- 229940008099 dimethicone Drugs 0.000 claims description 2
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 2
- 235000013870 dimethyl polysiloxane Nutrition 0.000 claims description 2
- JVSWJIKNEAIKJW-UHFFFAOYSA-N dimethyl-hexane Natural products CCCCCC(C)C JVSWJIKNEAIKJW-UHFFFAOYSA-N 0.000 claims description 2
- POULHZVOKOAJMA-UHFFFAOYSA-M dodecanoate Chemical compound CCCCCCCCCCCC([O-])=O POULHZVOKOAJMA-UHFFFAOYSA-M 0.000 claims description 2
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- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 2
- 229940070765 laurate Drugs 0.000 claims description 2
- 229920005615 natural polymer Polymers 0.000 claims description 2
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 2
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 2
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 claims description 2
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 2
- RGSFGYAAUTVSQA-UHFFFAOYSA-N pentamethylene Natural products C1CCCC1 RGSFGYAAUTVSQA-UHFFFAOYSA-N 0.000 claims description 2
- 125000004817 pentamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 claims description 2
- FDPIMTJIUBPUKL-UHFFFAOYSA-N pentan-3-one Chemical compound CCC(=O)CC FDPIMTJIUBPUKL-UHFFFAOYSA-N 0.000 claims description 2
- 239000011297 pine tar Substances 0.000 claims description 2
- 229940068124 pine tar Drugs 0.000 claims description 2
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 2
- 239000011164 primary particle Substances 0.000 claims description 2
- XCRZAIPPBHIKOR-UHFFFAOYSA-N prop-2-enyl 4-amino-3-fluorobenzoate Chemical compound NC1=CC=C(C(=O)OCC=C)C=C1F XCRZAIPPBHIKOR-UHFFFAOYSA-N 0.000 claims description 2
- 150000003839 salts Chemical class 0.000 claims description 2
- 229910052710 silicon Inorganic materials 0.000 claims description 2
- 239000010703 silicon Substances 0.000 claims description 2
- 239000000377 silicon dioxide Substances 0.000 claims description 2
- 239000002689 soil Substances 0.000 claims description 2
- 239000008117 stearic acid Substances 0.000 claims description 2
- 230000008961 swelling Effects 0.000 claims description 2
- 239000010936 titanium Substances 0.000 claims description 2
- 229910052719 titanium Inorganic materials 0.000 claims description 2
- 239000011787 zinc oxide Substances 0.000 claims description 2
- 229910052726 zirconium Inorganic materials 0.000 claims description 2
- 238000000227 grinding Methods 0.000 abstract description 5
- 239000002245 particle Substances 0.000 abstract description 5
- 239000007787 solid Substances 0.000 abstract description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N ferric oxide Chemical compound O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 23
- 229960005191 ferric oxide Drugs 0.000 description 22
- 230000000052 comparative effect Effects 0.000 description 13
- 229920002521 macromolecule Polymers 0.000 description 12
- 238000000034 method Methods 0.000 description 10
- 238000005303 weighing Methods 0.000 description 8
- DQMUQFUTDWISTM-UHFFFAOYSA-N O.[O-2].[Fe+2].[Fe+2].[O-2] Chemical compound O.[O-2].[Fe+2].[Fe+2].[O-2] DQMUQFUTDWISTM-UHFFFAOYSA-N 0.000 description 6
- 239000004576 sand Substances 0.000 description 5
- XREXPQGDOPQPAH-QKUPJAQQSA-K trisodium;[(z)-18-[1,3-bis[[(z)-12-sulfonatooxyoctadec-9-enoyl]oxy]propan-2-yloxy]-18-oxooctadec-9-en-7-yl] sulfate Chemical compound [Na+].[Na+].[Na+].CCCCCCC(OS([O-])(=O)=O)C\C=C/CCCCCCCC(=O)OCC(OC(=O)CCCCCCC\C=C/CC(CCCCCC)OS([O-])(=O)=O)COC(=O)CCCCCCC\C=C/CC(CCCCCC)OS([O-])(=O)=O XREXPQGDOPQPAH-QKUPJAQQSA-K 0.000 description 5
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- MKYBYDHXWVHEJW-UHFFFAOYSA-N N-[1-oxo-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propan-2-yl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(C(C)NC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 MKYBYDHXWVHEJW-UHFFFAOYSA-N 0.000 description 1
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Landscapes
- Emulsifying, Dispersing, Foam-Producing Or Wetting Agents (AREA)
Abstract
A nano-clas iron oxide dispersed liquid is prepared from nano-class iron oxide particles, disperser, stabilizer and dispersing medium through sequentially and proportionally mixing, mechanically dispersing for 10-70 min, and grinding for 15 min-25 hr. Its advantages are high content of solid, low viscosity and high dispersity and stability.
Description
Technical field
The present invention relates to nanometer technology, be specially a kind of nano-level iron oxidate dispersion solution and preparation method thereof.
Background technology
The nano-level iron oxide is a kind of broad-spectrum nano material.It has semiconductor property, can improve the electrostatic screen performance of organic coating, and ultraviolet ray is had strong absorption.Nano ferriferrous oxide still prepares one of important materials of magnetic fluid.International monopoly WO98.58673 has reported the oxidation iron core nano-scale particle with two-layer at least involucrum, its shell in abutting connection with core is a coating, contain cationic group, its shell (multilayer) is by having neutrality and/or anionic group is formed, the nano-level iron oxide particle of involucrum can be fully distributed in the soma like this, can treat tumour.Chinese patent CN1334295 has reported that product purity reaches 99.9% with homogenized fluid process for preparing level ferric oxide red powder, and the product pellet average diameter is between 50～200nm.Chinese patent CN1312224 has reported the iron oxide red production method of a kind of liquid phase synthesis nano, can make the iron oxide red of spheric granules in various degree such as about 20-50nm, 50-100nm by the method.
The patent of magnetic fluid aspect also has report.U.S. Pat P6,068,785 discloses a kind of oil base magnetofluid making method, and this magnetic fluid is made up of di-iron trioxide, oily carrier, surfactant, uses to stir to grind the magnetic particle slurries that forming surfactants coats.But the content of magnetic particle is low in the slurries, is 8% as the shared volume ratio of magnetic particle in the typical slurries.
Summary of the invention
The object of the present invention is to provide a kind of have fine dispersion stability, highly filled nano-level iron oxidate dispersion solution and preparation method thereof, wherein the weight ratio of nano-level iron oxide can reach 65%, and this nano-level iron oxidate dispersion solution can be widely used in fields such as coating, printing ink, weaving, cosmetics.
Technical scheme of the present invention is by weight, and said composition is made up of the decentralized medium of nano-level iron oxide powder 5-65%, dispersant 0.5-20% below 150nm of the average grain diameter of primary particle, stabilizing agent 0.1-5%, surplus.
In the above-mentioned nano-level iron oxidate dispersion solution, weight ratio is nano-level iron oxide powder 25-55% preferably, dispersant 2-15%, and stabilizing agent 1-5%, surplus is a decentralized medium.
The nano-level iron oxide of indication is FeO, Fe among the present invention
2O
3, Fe
3O
4, FeOOH one or more are composite.
Described dispersant is meant one or two or more kinds composite of natural polymer subclass, synthetic high polymer class, polyvalent carboxylic acid's class, block macromolecular class dispersant.Disperbyk103 as German Bi Ke (BYK) chemical company, Disperbyk106, Disperbyk107, Disperbyk110, Disperbyk111, Disperbyk115, Disperbyk130, Disperbyk160, Disperbyk162, Disperbyk163, Disperbyk164, Disperbyk180, Disperbyk182, Disperbyk184, Disperbyk190, Disperbyk191, Disperbyk192, Disperbyk2000, Anti-Terra-P, Anti-Terra-202, Anti-Terra-204, Anti-Terra-206, Anti-Terra-207, Anti-Terra-P, Byk-P104S; The Solsperse3000 of Avecia company, Solsperse13940, Solsperse17000, Solsperse20000, Solsperse24000, Solsperse27000, Solsperse28000, Solsperse32000, Solsperse32500, Solsperse34750, Solsperse41090; The TEXAPHOR of Henkel (Henkel) company
963, TEXAPHOR
963 S, TEXAPHOR
3061, TEXAPHOR
3073, TEXAPHOR
3112, TEXAPHOR
3241, TEXAPHOR
3250, TEXAPHOR
3287, Hydropalat
1080, Hydropalat
3204, Hydropalat
3275; The Homogenol L-18 of Japanese Kao company, Homogenol L-95, Homogenol L-1820, Homogenol L-100; The EFKA-44 of Holland EFKA auxiliary agent company (EFKA), EFKA-46, EFKA-47, EFKA-48, EFKA-49, EFKA-54, EFKA-63, EFKA-64, EFKA-65, EFKA-66, EFKA-71, EFKA-701, EFKA-745, EFKA-764, EFKA-766, EFKA-4008, EFKA-4009, EFKA-4540, EFKA-4550, EFKA-5244, EFKA-POLYMER 400, EFKA-POLYMER 401, EFKA-POLYMER402, EFKA-POLYMER 403, EFKA-POLYMER 45 0, EFKA-POLYMER 451, EFKA-POLYMER 452, EFKA-POLYMER 453, EFKA-POLYMER 4010, EFKA-LP 4010, EFKA-LP 4050, EFKA-LP 4055; Dispers610, Dispers610S, Dispers630S, Dispers700, the Dispers710 of enlightening height (Tego) chemical company; Hypersol L4707, Hypersol L 4708, Hypersol L4742, HyPersol L4744, Hypersol P4963, Aquasol 4602, Aquasol 4604, the Aquasol5601 of Denmark KVK (Kemisk Vaerk Koege) company; Contain the fertile SER-AD FA of (SERVO) company 601, SER-AD FA 192, SER-AD FA 196, SER-AD FX 9080, SER-AD FX 9085, NUOSPERSE 657.
Dispersant is the Disperbyk103 of German Bi Ke chemical company preferably, Disperbyk106, Disperbyk107, Disperbyk110, Disperbyk111, Disperbyk115, Disperbyk130, Disperbyk160, Disperbyk162, Disperbyk163, Disperbyk164, Disperbyk180, Disperbyk182, Disperbyk184, Disperbyk190, Disperbyk191, Disperbyk192, Disperbyk2000, Anti-Terra-P, Anti-Terra-202, Anti-Terra-204, Anti-Terra-206, Anti-Terra-207, Anti-Terra-P, Byk-P104S; The Solsperse3000 of Avecia company, Solsperse13940, Solsperse17000, Solsperse20000, Solsperse24000, Solsperse27000, Solsperse28000, Solsperse32000, Solsperse32500, Solsperse34750, Solsperse41090; The EFKA-44 of Holland EFKA auxiliary agent company, EFKA-46, EFKA-47, EFKA-48, EFKA-49, EFKA-54, EFKA-63, EFKA-64, EFKA-65, EFKA-66, EFKA-701, EFKA-745, EFKA-764, EFKA-766, EFKA-4008, EFKA-4009, EFKA-4540, EFKA-4550, EFKA-5244, EFKA-POLYMER 400, EFKA-POLYMER 401, EFKA-POLYMER402, EFKA-POLYMER 403, EFKA-POLYMER 450, EFKA-POLYMER 451, EFKA-POLYMER 452, EFKA-POLYMER 453, EFKA-POLYMER 4010, EFKA-LP 4010, EFKA-LP 4050, EFKA-LP 4055; The HypersolL4707 of Denmark KVK company, Hypersol L 4708, Hypersol L 4742, Hypersol L4744, Hypersol P4963, Aquasol 4602, Aquasol 4604, Aquasol 560 1; Contain the fertile SER-AD FA of (SERVO) company 601, SER-AD FA 192, SER-AD FA 196, SER-AD FX 9080, SER-AD FX 9085, NUOSPERSE 657.
It is composite that described stabilizing agent is selected from one or more of aerosil, swelling great soil group, castor oil derivative or Ployethylene Wax.Change 7500DP, 2000T, 1000T, the SO-Thick 30 of Industrial Co., Ltd. as 201P, 202P, VISCOGELB4, VISCOGEL ED, the Taiwan three of the modest Trading Co., Ltd of Taiwan moral; The A-C 316 of Allied Signal company, A-C 316A, A-C 325, A-C 330, A-C 392, A-C 395, A-C 540, A-C 626, A-C 629A, A-C 655, A-C 656, A-C680; The AEROSIL 130,150,200,300,380 of Di Gaosha Co., Ltd, OX50, TT600, R972, AEROSIL MOX80, MOX170, COK 84 etc.
Described decentralized medium is fat hydrocarbon, alicyclic hydrocarbon type, arene, alcohols, ketone, ester class, terpene, alcohol ether and ether-ether class, replace hydro carbons, one or two or more kinds mixture of water, kerosene, synthetic lubricant fluid, synthetic hydraulic fluid.Wherein the fat hydrocarbon decentralized medium refer to benzinum, No. 200 solvent naphthas, raffinate oil, n-hexane, isohexane, normal heptane, isoheptane, normal octane, isooctane; The alicyclic hydrocarbon type decentralized medium refers to pentamethylene, cyclohexane, cyclohexene, decahydronaphthalenes; The arene decentralized medium refers to benzene,toluene,xylene, trimethylbenzene, Solvesso100, Solvesso150, Solvesso200, solvent naphtha, ethylbenzene, propyl benzene, isopropylbenzene; The alcohols decentralized medium refers to methyl alcohol, ethanol, normal propyl alcohol, isopropyl alcohol, sec-butyl alcohol, n-butanol, isobutanol, the tert-butyl alcohol, ethylene glycol, propane diols; The ketone decentralized medium refers to acetone, MEK, methylisobutylketone, cyclohexanone, isophorone, DAA, metacetone, methyl propyl ketone; Ester class decentralized medium refers to the just own ester of ethyl acetate, n-butyl acetate, isobutyl acetate, acetic acid, acetic acid dissident ester, the positive heptyl ester of acetic acid, acetic acid isocyanate, n-Decyl Acetate, acetic acid isodecyl ester, butyl lactate; The terpene decentralized medium refers to turpentine oil, pine tar, dipentene; Alcohol ether and ether-ether class decentralized medium refer to ethylene glycol ethyl ether, butyl glycol ether, ethylene glycol ether acetate, 2-Butoxyethyl acetate, diethylene glycol ether, diethylene glycol butyl ether, diethylene glycol ether acetate, diethylene glycol monobutyl ether acetate, propylene-glycol ethyl ether, propane diols butyl ether, 1-Methoxy-2-propyl acetate, propylene-glycol ethyl ether acetate, propane diols monobutyl ether acetate, dipropylene glycol methyl ether, DPG ether, methoxyacetic acid propyl ester; Replace the hydro carbons decentralized medium and refer to trichloroethanes, 2-nitropropane.
Decentralized medium is No. 200 solvent naphthas preferably, n-hexane, isohexane, normal heptane, isoheptane, cyclohexane, decahydronaphthalenes, toluene, dimethylbenzene, trimethylbenzene, Solvesso100, Solvesso150, Solvesso200, solvent naphtha, methyl alcohol, ethanol, normal propyl alcohol, isopropyl alcohol, n-butanol, isobutanol, sec-butyl alcohol, the tert-butyl alcohol, ethylene glycol, propane diols, MEK, methylisobutylketone, cyclohexanone, isophorone, ethyl acetate, n-butyl acetate, isobutyl acetate, the methoxyacetic acid propyl ester, ethylene glycol ethyl ether, butyl glycol ether, ethylene glycol ether acetate, 2-Butoxyethyl acetate, diethylene glycol ether, the diethylene glycol butyl ether, the diethylene glycol ether acetate, the diethylene glycol monobutyl ether acetate, propylene-glycol ethyl ether, the propane diols butyl ether, 1-Methoxy-2-propyl acetate, the propylene-glycol ethyl ether acetate, the propane diols monobutyl ether acetate, dipropylene glycol methyl ether, the DPG ether, trichloroethanes, water, kerosene, synthetic lubricant fluid, synthetic hydraulic fluid.
Nano-level iron oxidate dispersion solution of the present invention prepares through following method: dispersant is added in the decentralized medium, add nano-level iron oxide powder and stabilizing agent again, disperseed 10-70 minute with high speed dispersor 400-3200rpm, the nano-level iron oxidate dispersion solution of gained ground in ball mill, sand mill or ball mill 15 minutes-25 hours, made nano-level iron oxidate dispersion solution finished product.The surface of nano-level iron oxide powder can be handle through coating or not coating handle, the coating processing is meant in nano-level iron oxidate powder surface carries out inorganic processing, as carries out one or more coating processing of silica, alundum (Al, zinc oxide; Or carry out organic process in nano-level iron oxidate powder surface, as to carry out stearic acid, laurate, oleic acid or their metallic salt, titanium be that coupling agent, aluminium are that coupling agent, silicon are that coupling agent, tin are that coupling agent, zirconium are that one or more of coupling agent, dimethicone coat and handle; Or carry out inorganic and organic composite coated processing in nano-level iron oxidate powder surface.
Advantage of the present invention is as follows:
1. nano-level iron oxidate dispersion solution of the present invention is a kind of high solids content, low viscosity dispersion liquid, and its monodispersity is good, has high stability, can be widely used in fields such as coating, printing ink, weaving, cosmetics, magnetic fluid and magnetic recording material.
2. good stability.Nano-level iron oxidate dispersion solution viscosity of the present invention is low, is easy to use, and has high stability, can keep usually not precipitating half a year, not stratified, and best can be more than a year and a half.
The specific embodiment
Except that specializing, the ratio that relates to is weight ratio among the present invention.The performance test methods of nano-level iron oxidate dispersion solution is as follows in embodiment and the comparative example:
The granularity of nano-level iron oxidate dispersion solution is tested with day SA-CP3 centrifugal sedimentation Particle Size Analyzer of island proper Tianjin company, characterizes the granule size of nano-level iron oxide in the nano-level iron oxidate dispersion solution with average grain diameter.
The bin stability of nano-level iron oxidate dispersion solution is measured: by given embodiment and comparative example method preparation 300g dispersion liquid, the container of the sealing of packing in 50 ± 2 ℃ of storages 1 month, carries out the bin stability evaluation respectively.Bin stability is divided into 10 ranks successively.Wherein 0 grade the poorest, 10 grades are best.
Embodiment 1
In the 300ml beaker, take by weighing toluene 50g, add 7g dispersant SER-AD FA 192,7g dispersant EFKA-701, add 60nm nanoscale ferrous oxide 96.3g and 0.2g stabilizing agent 201P again, after disperseing 25 minutes with high speed dispersor 1500rpm, with ball mill grinding 7 hours, make nano-level iron oxide powder weight ratio and be 60% nanoscale ferrous oxide dispersion liquid.The total amount of dispersant is about 8.7% in this nanoscale ferrous oxide dispersion liquid.
Embodiment 2
Nanoscale ferrous oxide dispersion liquid method for making is with embodiment 1, adjust the addition of macromolecule dispersing agent SER-AD FA 192, macromolecule dispersing agent EFKA-701 and nanoscale ferrous oxide powder, the total amount that makes macromolecule dispersing agent is 0.6%, wherein macromolecule dispersing agent SER-AD FA 192 is identical with embodiment 1 with EFKA-701 weight ratio between the two, makes nanoscale ferrous oxide powder body weight than the nanoscale ferrous oxide dispersion liquid that is 60%.
Embodiment 3
Nanoscale ferrous oxide dispersion liquid method for making is with embodiment 1, adjust the addition of macromolecule dispersing agent SER-AD FA192, macromolecule dispersing agent EFKA-701 and nanoscale ferrous oxide powder, the total amount that makes macromolecule dispersing agent is 17%, wherein macromolecule dispersing agent SER-AD FA 192 is identical with embodiment 1 with EFKA-701 weight ratio between the two, makes nanoscale ferrous oxide powder body weight than the nanoscale ferrous oxide dispersion liquid that is 60%.
Embodiment 4
In the 300ml beaker, take by weighing MEK 50g, add 4g dispersant TEXAPHOR
963, add 30nm nanoscale tri-iron tetroxide 45g and 1g stabilizing agent A-C 540 that the sodium laurate coating is handled again, after disperseing 30 minutes with high speed dispersor 1200rpm, with ball mill grinding 14 hours, make nano-level iron oxide powder weight ratio and be 45% nanoscale tri-iron tetroxide dispersion liquid.Dispersant TEXAPHOR in this nanoscale tri-iron tetroxide dispersion liquid
963 weight ratio is 4%.
Embodiment 5
Nanoscale tri-iron tetroxide dispersion liquid method for making is adjusted macromolecule dispersing agent TEXAPHOR with embodiment 4
963 and the addition of nanoscale tri-iron tetroxide powder, making the total amount of macromolecule dispersing agent is 1.2%, makes nanoscale ferrous oxide powder body weight than the nanoscale tri-iron tetroxide dispersion liquid that is 45%.
Embodiment 6
Nanoscale tri-iron tetroxide dispersion liquid method for making is adjusted macromolecule dispersing agent TEXAPHOR with embodiment 4
963 and the addition of nanoscale tri-iron tetroxide powder, making the total amount of macromolecule dispersing agent is 18%, makes nanoscale ferrous oxide powder body weight than the nanoscale tri-iron tetroxide dispersion liquid that is 45%.
Embodiment 7
In the 300ml beaker, take by weighing 12# hydraulic oil 100g, add 4.92g dispersant Solsperse34750, add 100nm nanoscale di-iron trioxide 45.18g and AEROSIL R972 stabilizing agent 0.5g again, after disperseing 15 minutes with high speed dispersor 800rpm, ground 6 hours with sand mill, make nanoscale ferric oxide powder weight ratio and be 30% nanoscale di-iron trioxide dispersion liquid.The weight ratio of dispersant Solsperse34750 is about 3.3% in this nanoscale di-iron trioxide dispersion liquid.
Embodiment 8
In the 300ml beaker, take by weighing water 100g, add 5.14g dispersant Disperbyk184, add 15nm nanoscale FeOOH powder 11.85g and AEROSIL 300 stabilizing agent 1.5g again, after disperseing 20 minutes with high speed dispersor 500rpm, ground 50 minutes with sand mill, make nanoscale FeOOH powder weight ratio and be about 10% nanoscale FeOOH dispersion liquid.The weight ratio of dispersant Disperbyk184 is about 4.3% in this nanoscale FeOOH dispersion liquid.
Comparative example 1
In the 300ml beaker, take by weighing toluene 64.2g, add 60nm nanoscale ferrous oxide 96.3g, after disperseing 25 minutes with high speed dispersor 1500rpm,, obtain nano-level iron oxide powder weight ratio and be 60% nanoscale ferrous oxide dispersion liquid with ball mill grinding 7 hours.
Comparative example 2
In the 300ml beaker, take by weighing MEK 55g, add the 30nm nanoscale tri-iron tetroxide 45g that the sodium laurate coating is handled, after disperseing 30 minutes with high speed dispersor 1200rpm, with ball mill grinding 14 hours, obtain nano-level iron oxide powder weight ratio and be 45% nanoscale tri-iron tetroxide dispersion liquid.
Comparative example 3
In the 300ml beaker, take by weighing 12# hydraulic oil 105.42g, add 100nm nanoscale di-iron trioxide 45.18g, after disperseing 15 minutes with high speed dispersor 800rpm, ground 6 hours, obtain nanoscale ferric oxide powder weight ratio and be 30% nanoscale di-iron trioxide dispersion liquid with sand mill.
Comparative example 4
In the 300ml beaker, take by weighing water 106.64g, add 15nm nanoscale FeOOH powder 11.85g,, ground 50 minutes after 20 minutes with high speed dispersor 500rpm dispersion, obtain nanoscale FeOOH powder weight ratio and be about 10% nanoscale FeOOH dispersion liquid with sand mill.
Embodiment and comparative example explanation: table 1 is the performance data of the comparative example and the embodiment of nano-level iron oxidate dispersion solution.As can be seen from Table 1, the nano-level iron oxidate dispersion solution of identical nano-level iron oxide powder weight ratio is compared with corresponding comparative example 1-4, has bin stability preferably, less particle mean size.Also as can be seen, when the weight ratio of dispersant at 2-15%, in the weight ratio 0.1-5% scope of stabilizing agent, the bin stability of nano-level iron oxidate dispersion solution is better, particle mean size is littler.
Table 1
| The type of nano-sized iron oxide | The average grain diameter of nano-level iron oxide (nm) | The weight ratio of nano-level iron oxide (%) | The weight ratio of dispersant (%) | The weight ratio of stabilizing agent (%) | Nano oxidized aluminium paste average grain diameter (nm) | Bin stability, level | |
| Comparative example 1 | ??FeO | ????60 | ????60 | ????0 | ????0 | ????435 | ????- |
| Embodiment 1 | ??FeO | ????60 | ????60 | ????8.7 | ????0.1 | ????180 | ????8 |
| Embodiment 2 | ??FeO | ????60 | ????60 | ????0.6 | ????0.1 | ????237 | ????7 |
| Embodiment 3 | ??FeO | ????60 | ????60 | ????17 | ????0.1 | ????253 | ????5 |
| Comparative example 2 | ??Fe 3O 4 | ????30 | ????45 | ????0 | ????0 | ????397 | ????- |
| Embodiment 4 | ??Fe 3O 4 | ????30 | ????45 | ????4 | ????1 | ????154 | ????10 |
| Embodiment 5 | ??Fe 3O 4 | ????30 | ????45 | ????1.2 | ????1 | ????179 | ????8 |
| Embodiment 6 | ??Fe 3O 4 | ????30 | ????45 | ????18 | ????1 | ????201 | ????8 |
| Comparative example 3 | ??Fe 2O 3 | ????100 | ????30 | ????0 | ????0 | ????385 | ????2 |
| Embodiment 7 | ??Fe 2O 3 | ????100 | ????30 | ????3.3 | ????0.3 | ????221 | ????7 |
| Comparative example 4 | ??FeOOH | ????15 | ????10 | ????0 | ????0 | ????209 | ????1 |
| Embodiment 8 | ??FeOOH | ????15 | ????10 | ????4.3 | ????1.3 | ????128 | ????8 |
Annotate: "-" expression is because viscosity is big, and conglomeration can't be investigated bin stability.
Claims (10)
1, a kind of nano-level iron oxidate dispersion solution, it is characterized in that: by weight, said composition is made up of the decentralized medium of nano-level iron oxide powder 5-65%, dispersant 0.5-20% below 150nm of the average grain diameter of primary particle, stabilizing agent 0.1-5%, surplus.
2, according to the described nano-level iron oxidate dispersion solution of claim 1, it is characterized in that: the shared weight ratio of nano-level iron oxide powder is 25-55%, the shared weight ratio of dispersant is 2-15%, and the shared weight ratio of stabilizing agent is that 1-5%, surplus are decentralized medium.
3, according to the described nano-level iron oxidate dispersion solution of claim 1, it is characterized in that: it is composite that described dispersant is selected from one or more of natural polymer subclass, synthetic high polymer class, polyvalent carboxylic acid's class, block macromolecular class dispersant.
4, according to the described nano-level iron oxidate dispersion solution of claim 1, it is characterized in that: it is composite that described stabilizing agent is selected from one or more of aerosil, swelling great soil group, castor oil derivative or Ployethylene Wax.
5, according to the described nano-level iron oxidate dispersion solution of claim 1, it is characterized in that: described decentralized medium is selected from fat hydrocarbon, alicyclic hydrocarbon type, arene, alcohols, ketone, ester class, terpene, alcohol ether and ether-ether class, replaces hydro carbons, water, synthetic lubricant fluid, synthetic hydraulic fluid one or more are composite.
6, according to the described nano-level iron oxidate dispersion solution of claim 5, it is characterized in that: described decentralized medium is a benzinum, No. 200 solvent naphthas, raffinate oil, n-hexane, isohexane, normal heptane, isoheptane, normal octane, isooctane, pentamethylene, cyclohexane, cyclohexene, decahydronaphthalenes, benzene, toluene, dimethylbenzene, trimethylbenzene, Solvesso100, Solvesso150, Solvesso200, solvent naphtha, ethylbenzene, propyl benzene, isopropylbenzene, methyl alcohol, ethanol, normal propyl alcohol, isopropyl alcohol, sec-butyl alcohol, n-butanol, isobutanol, the tert-butyl alcohol, ethylene glycol, propane diols, acetone, MEK, methylisobutylketone, cyclohexanone, isophorone, DAA, metacetone, methyl propyl ketone, ethyl acetate, n-butyl acetate, isobutyl acetate, the just own ester of acetic acid, acetic acid dissident ester, the positive heptyl ester of acetic acid, the acetic acid isocyanate, n-Decyl Acetate, acetic acid isodecyl ester, butyl lactate, turpentine oil, pine tar, dipentene, ethylene glycol ethyl ether, butyl glycol ether, ethylene glycol ether acetate, 2-Butoxyethyl acetate, diethylene glycol ether, the diethylene glycol butyl ether, the diethylene glycol ether acetate, the diethylene glycol monobutyl ether acetate, propylene-glycol ethyl ether, the propane diols butyl ether, 1-Methoxy-2-propyl acetate, the propylene-glycol ethyl ether acetate, the propane diols monobutyl ether acetate, dipropylene glycol methyl ether, the DPG ether, the methoxyacetic acid propyl ester, trichloroethanes, the 2-nitropropane, water, kerosene, synthetic lubricant fluid, one or more of synthetic hydraulic fluid are composite.
7, according to the described nano-level iron oxidate dispersion solution of claim 1, it is characterized in that: described nano-level iron oxide is meant FeO, Fe
2O
3, Fe
3O
4, FeOOH one or more are composite.
8, a kind of preparation method according to described nano-level iron oxidate dispersion solution one of in the claim 1～7, it is characterized in that: dispersant is added in the decentralized medium, add nano-level iron oxide powder and stabilizing agent again, disperseed 10-70 minute with 400-3200rpm, the nano-level iron oxidate dispersion solution of gained ground 15 minutes-25 hours, made nano-level iron oxidate dispersion solution finished product.
9, according to the described nano-level iron oxidate dispersion solution of claim 8, it is characterized in that: handle through coating on the surface of described nano-level iron oxide powder.
10, according to the described nano-level iron oxidate dispersion solution of claim 9, it is characterized in that: described coating is handled and is meant one or more coating processing of carrying out silica, alundum (Al, zinc oxide in nano-level iron oxidate powder surface; Or carry out stearic acid, laurate, oleic acid or their metallic salt, titanium in nano-level iron oxidate powder surface be that coupling agent, aluminium are that coupling agent, silicon are that coupling agent, tin are that coupling agent, zirconium are that one or more of coupling agent, dimethicone coat and handle; Or the Combined Processing of carrying out above-mentioned coating processing in nano-level iron oxidate powder surface.
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