CN1180079A - Fatty acid modifying metallic oxide or hydroxide nanometre powder and its preparing method - Google Patents
Fatty acid modifying metallic oxide or hydroxide nanometre powder and its preparing method Download PDFInfo
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- CN1180079A CN1180079A CN 95106896 CN95106896A CN1180079A CN 1180079 A CN1180079 A CN 1180079A CN 95106896 CN95106896 CN 95106896 CN 95106896 A CN95106896 A CN 95106896A CN 1180079 A CN1180079 A CN 1180079A
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- salt
- lipid acid
- fatty acid
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- 229910044991 metal oxide Inorganic materials 0.000 title claims abstract description 20
- 235000014113 dietary fatty acids Nutrition 0.000 title claims abstract description 18
- 239000000194 fatty acid Substances 0.000 title claims abstract description 18
- 229930195729 fatty acid Natural products 0.000 title claims abstract description 18
- 150000004665 fatty acids Chemical class 0.000 title claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 title claims abstract description 10
- 239000000843 powder Substances 0.000 title abstract description 6
- 238000000034 method Methods 0.000 title description 7
- 238000002360 preparation method Methods 0.000 claims abstract description 13
- 150000004706 metal oxides Chemical class 0.000 claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 25
- 239000002253 acid Substances 0.000 claims description 24
- 238000002156 mixing Methods 0.000 claims description 21
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 19
- 150000002632 lipids Chemical class 0.000 claims description 15
- 239000011858 nanopowder Substances 0.000 claims description 14
- 239000002105 nanoparticle Substances 0.000 claims description 13
- 229910052751 metal Inorganic materials 0.000 claims description 10
- 150000003839 salts Chemical class 0.000 claims description 9
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 8
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 8
- 239000012429 reaction media Substances 0.000 claims description 7
- 229910052693 Europium Inorganic materials 0.000 claims description 5
- 125000000217 alkyl group Chemical group 0.000 claims description 5
- 229910052742 iron Inorganic materials 0.000 claims description 5
- 229910052746 lanthanum Inorganic materials 0.000 claims description 5
- 229910052745 lead Inorganic materials 0.000 claims description 5
- 239000003595 mist Substances 0.000 claims description 5
- 229910052759 nickel Inorganic materials 0.000 claims description 5
- 229910052718 tin Inorganic materials 0.000 claims description 5
- 229910052719 titanium Inorganic materials 0.000 claims description 5
- 229910052727 yttrium Inorganic materials 0.000 claims description 5
- 229910052725 zinc Inorganic materials 0.000 claims description 5
- 229910052726 zirconium Inorganic materials 0.000 claims description 5
- 150000001875 compounds Chemical class 0.000 claims description 4
- 229910021518 metal oxyhydroxide Inorganic materials 0.000 claims description 4
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 4
- 230000007704 transition Effects 0.000 claims description 4
- 239000002184 metal Substances 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- AVXURJPOCDRRFD-UHFFFAOYSA-N Hydroxylamine Chemical compound ON AVXURJPOCDRRFD-UHFFFAOYSA-N 0.000 claims 1
- -1 fatty acid hydrocarbon Chemical class 0.000 abstract description 5
- 239000006185 dispersion Substances 0.000 abstract description 3
- 239000000654 additive Substances 0.000 abstract description 2
- 230000000996 additive effect Effects 0.000 abstract description 2
- 239000003973 paint Substances 0.000 abstract description 2
- 239000004033 plastic Substances 0.000 abstract description 2
- 229920003023 plastic Polymers 0.000 abstract description 2
- SDGKUVSVPIIUCF-UHFFFAOYSA-N 2,6-dimethylpiperidine Chemical compound CC1CCCC(C)N1 SDGKUVSVPIIUCF-UHFFFAOYSA-N 0.000 abstract 2
- 239000004215 Carbon black (E152) Substances 0.000 abstract 1
- 239000005069 Extreme pressure additive Substances 0.000 abstract 1
- 239000007866 anti-wear additive Substances 0.000 abstract 1
- 229910010293 ceramic material Inorganic materials 0.000 abstract 1
- 239000004519 grease Substances 0.000 abstract 1
- 229930195733 hydrocarbon Natural products 0.000 abstract 1
- 230000002209 hydrophobic effect Effects 0.000 abstract 1
- 230000001050 lubricating effect Effects 0.000 abstract 1
- 229910000000 metal hydroxide Inorganic materials 0.000 abstract 1
- 239000002994 raw material Substances 0.000 abstract 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 19
- 239000000243 solution Substances 0.000 description 14
- 238000001556 precipitation Methods 0.000 description 13
- 238000001914 filtration Methods 0.000 description 12
- 229960000935 dehydrated alcohol Drugs 0.000 description 11
- 238000005406 washing Methods 0.000 description 11
- 229910021529 ammonia Inorganic materials 0.000 description 10
- 239000002244 precipitate Substances 0.000 description 10
- 238000001291 vacuum drying Methods 0.000 description 10
- GHVNFZFCNZKVNT-UHFFFAOYSA-N decanoic acid Chemical compound CCCCCCCCCC(O)=O GHVNFZFCNZKVNT-UHFFFAOYSA-N 0.000 description 8
- 230000001476 alcoholic effect Effects 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- 239000005632 Capric acid (CAS 334-48-5) Substances 0.000 description 4
- 235000021355 Stearic acid Nutrition 0.000 description 4
- OBETXYAYXDNJHR-UHFFFAOYSA-N alpha-ethylcaproic acid Natural products CCCCC(CC)C(O)=O OBETXYAYXDNJHR-UHFFFAOYSA-N 0.000 description 4
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 4
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 4
- WWZKQHOCKIZLMA-UHFFFAOYSA-N octanoic acid Chemical compound CCCCCCCC(O)=O WWZKQHOCKIZLMA-UHFFFAOYSA-N 0.000 description 4
- 239000008117 stearic acid Substances 0.000 description 4
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 3
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 3
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 3
- 239000005642 Oleic acid Substances 0.000 description 3
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- KQNPFQTWMSNSAP-UHFFFAOYSA-N isobutyric acid Chemical compound CC(C)C(O)=O KQNPFQTWMSNSAP-UHFFFAOYSA-N 0.000 description 3
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 3
- 239000012046 mixed solvent Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- OBETXYAYXDNJHR-SSDOTTSWSA-M (2r)-2-ethylhexanoate Chemical compound CCCC[C@@H](CC)C([O-])=O OBETXYAYXDNJHR-SSDOTTSWSA-M 0.000 description 2
- FERIUCNNQQJTOY-UHFFFAOYSA-N Butyric acid Chemical compound CCCC(O)=O FERIUCNNQQJTOY-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- QVQLCTNNEUAWMS-UHFFFAOYSA-N barium oxide Chemical compound [Ba]=O QVQLCTNNEUAWMS-UHFFFAOYSA-N 0.000 description 2
- 238000005352 clarification Methods 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- AEBZCFFCDTZXHP-UHFFFAOYSA-N europium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Eu+3].[Eu+3] AEBZCFFCDTZXHP-UHFFFAOYSA-N 0.000 description 2
- NNMXSTWQJRPBJZ-UHFFFAOYSA-K europium(iii) chloride Chemical compound Cl[Eu](Cl)Cl NNMXSTWQJRPBJZ-UHFFFAOYSA-K 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- VKOBVWXKNCXXDE-UHFFFAOYSA-N icosanoic acid Chemical compound CCCCCCCCCCCCCCCCCCCC(O)=O VKOBVWXKNCXXDE-UHFFFAOYSA-N 0.000 description 2
- 230000003993 interaction Effects 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 2
- YEXPOXQUZXUXJW-UHFFFAOYSA-N oxolead Chemical compound [Pb]=O YEXPOXQUZXUXJW-UHFFFAOYSA-N 0.000 description 2
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 2
- 239000011550 stock solution Substances 0.000 description 2
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 2
- NQPDZGIKBAWPEJ-UHFFFAOYSA-N valeric acid Chemical compound CCCCC(O)=O NQPDZGIKBAWPEJ-UHFFFAOYSA-N 0.000 description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 1
- AMQJEAYHLZJPGS-UHFFFAOYSA-N N-Pentanol Chemical compound CCCCCO AMQJEAYHLZJPGS-UHFFFAOYSA-N 0.000 description 1
- 229910021627 Tin(IV) chloride Inorganic materials 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- XFBXDGLHUSUNMG-UHFFFAOYSA-N alumane;hydrate Chemical compound O.[AlH3] XFBXDGLHUSUNMG-UHFFFAOYSA-N 0.000 description 1
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 1
- 239000000908 ammonium hydroxide Substances 0.000 description 1
- WDIHJSXYQDMJHN-UHFFFAOYSA-L barium chloride Chemical compound [Cl-].[Cl-].[Ba+2] WDIHJSXYQDMJHN-UHFFFAOYSA-L 0.000 description 1
- 229910001626 barium chloride Inorganic materials 0.000 description 1
- 229940045511 barium chloride Drugs 0.000 description 1
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 description 1
- 239000001110 calcium chloride Substances 0.000 description 1
- 229910001628 calcium chloride Inorganic materials 0.000 description 1
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 1
- 239000000920 calcium hydroxide Substances 0.000 description 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003995 emulsifying agent Substances 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 1
- 235000015110 jellies Nutrition 0.000 description 1
- 239000008274 jelly Substances 0.000 description 1
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 description 1
- ICAKDTKJOYSXGC-UHFFFAOYSA-K lanthanum(iii) chloride Chemical compound Cl[La](Cl)Cl ICAKDTKJOYSXGC-UHFFFAOYSA-K 0.000 description 1
- RLJMLMKIBZAXJO-UHFFFAOYSA-N lead nitrate Chemical compound [O-][N+](=O)O[Pb]O[N+]([O-])=O RLJMLMKIBZAXJO-UHFFFAOYSA-N 0.000 description 1
- 238000005461 lubrication Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000000593 microemulsion method Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 229910000476 molybdenum oxide Inorganic materials 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 1
- PQQKPALAQIIWST-UHFFFAOYSA-N oxomolybdenum Chemical compound [Mo]=O PQQKPALAQIIWST-UHFFFAOYSA-N 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 229910001961 silver nitrate Inorganic materials 0.000 description 1
- 229910000108 silver(I,III) oxide Inorganic materials 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 description 1
- 229940005605 valeric acid Drugs 0.000 description 1
- PCMOZDDGXKIOLL-UHFFFAOYSA-K yttrium chloride Chemical compound [Cl-].[Cl-].[Cl-].[Y+3] PCMOZDDGXKIOLL-UHFFFAOYSA-K 0.000 description 1
- DUNKXUFBGCUVQW-UHFFFAOYSA-J zirconium tetrachloride Chemical compound Cl[Zr](Cl)(Cl)Cl DUNKXUFBGCUVQW-UHFFFAOYSA-J 0.000 description 1
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- Oxygen, Ozone, And Oxides In General (AREA)
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
- Colloid Chemistry (AREA)
Abstract
The present invention provides a fatty acid modified metal oxide or hydroxide nano-fine powder and its preparation method. Due to the existence of fatty acid hydrocarbon hydrophobic chain, said invented nano-fine powder possesses good dispersion property in organic medium, so that it can be used as antiwear and extreme pressure additive for lubricating grease, and additive for paint and plastics, and also can be used for raw material preparation of ceramic material.
Description
The present invention relates to nano powder of a kind of fatty acid modifying metallic oxide or oxyhydroxide and preparation method thereof.
Nano material is because its special physics and chemical property make it be subjected to paying attention to widely, therefore nano powder and by the preparation of its compacting, the integral material that sinters in recent years, performance and applied research become multi-disciplinary crossing research field, and the bulk ceramics material that is prepared by nanoparticle has good intensity.Nanoparticle also is used as coating, and the additive of plastics, CN1041335 adopt the micro-emulsion method to prepare the ZrO of epigranular, good fluidity
2Powder is used for ZrO
2The preparation of pottery.CN10494485A has proposed the production method of the compound material of metal oxide and this powder of sintering and the stupalith that makes, but the resulting metal of these methods (hydrogen) oxide compound, because the hydrophilic interaction of its surperficial OH group, it is difficult at organic medium (as oil paint, good dispersiveness is arranged the lubrication base wet goods), and more serious agglomeration arranged, although adopt the method for emulsion to control to reunite and grain distribution of sizes, but the interaction that emulsifying agent and metal (hydrogen) oxide surface is weak also makes it be difficult to reach the purpose of stable dispersion in organic medium.Therefore its application is restricted.
The object of the present invention is to provide a kind of new surface that good dispersion arranged in organic medium is the metal oxide modified of lipid acid or hydroxide nano particulate and preparation method thereof.
The present invention realizes by following measure:
Fatty acid modifying metallic oxide of the present invention or hydroxide nano particulate are meant lipid acid
Be chemically bound in the nanoparticle of metal oxide or oxyhydroxide, wherein the chain length of R is C in the lipid acid
2-C
20Straight or branched alkane, metal oxide or oxyhydroxide comprise the oxide compound or the oxyhydroxide of transition group and second and third, four, five main group metal elements, and fatty acid hydrocarbon chain shared weight percent in the decorated nanometer particulate is 5%-80%.
Fatty acid modifying metallic oxide that the present invention preferentially selects for use or hydroxide nano grain are C
8-C
18The fatty acid chemistry of straight or branched alkyl be bonded to the metal oxide of Zr, Ti, Sn, Y, Pb, Zn, Fe, Co, Ni, La, Eu element or the nanoparticle of oxyhydroxide, and fatty acid hydrocarbon chain shared weight percent in the decorated nanometer particulate is preferably 15%-60%
The method for preparing the fatty acid modifying metallic oxide nanoparticle comprises:
A) lipid acid, ammonium hydroxide and the soluble metallic salt of use formula (I)
R is C in the formula (I)
2-C
20The straight or branched alkyl, soluble metallic salt comprises transition group and second and third, four, five main group metal elements;
B) in the presence of reaction medium;
C) normal temperature-120 ℃ following reaction is 2-48 hour
Prepare that reaction medium is a tetrahydrofuran (THF) in the method for fatty acid modifying metallic oxide or hydroxide nano particulate, C
1-C
4Lipid acid, acetone and these solvents alone or in combination with the blending agent of water;
Prepare in the method for fatty acid modifying metallic oxide or hydroxide nano particulate, the mol ratio of lipid acid and metal-salt is 1: 0.1-10;
Prepare in the method for fatty acid modifying metallic oxide or hydroxide nano particulate, the mol ratio of lipid acid and reaction medium is 1: 500-2000;
The optimum range of the lipid acid R chain length of above-mentioned reaction is C
8-C
18
The metallic element of the suitableeest soluble metallic salt is Zr, Ti, Sn, Y, Pb, Zn, Fe, Co, Ni, La, Eu.
Reaction medium is an optimum with 66% alcohol+34% water.
The temperature of reaction optimum value is 60-80 ℃
The mol ratio optimum value of dirty acid of fat and metal-salt is 1: 1-4.
Characteristics of the present invention be the finishing of carrying be meant modifier be chemically bound in receive the material particulate the surface, form stable chemically modified layer.Therefore, it is multiple in the surface of nanometer emblem grain that it both had been different from surfactant package, mixture that neither two kinds of compounds, the effect of this finishing, the not only generation of the size of may command nanometer and reunion the more important thing is that it can make nanoparticle be scattered in organic medium.
In order to understand the present invention better, describe by embodiment, but enforcement of the present invention is not limited to following examples.
Example 1:
The 50mmol isopropylformic acid is joined in the 50ml water and 100ml alcoholic acid mixed solution of constant temperature to 75 ℃, the aqueous solution of hydrogen that adds 5ml 25-28% again, reacted 30 minutes, to solution clarification, will be dissolved in advance then 15ml water (the 50mmol basic zirconium chloride under agitation dropwise adds reaction soln, there are a large amount of white jelly precipitations to occur immediately, continue isothermal reaction 6 hours, precipitation is washed after filtration, drying promptly obtains isopropylformic acid and modifies ZrO
2Nano powder.
Example 2:
Get the 50mmol tetrabutyl titanate and add in the 100ml dehydrated alcohol, stir and cushioning constant temperature to 50 ℃, add the 100mmol 2 ethyl hexanoic acid, behind the isothermal reaction 2h, dropwise add the 50mmol deionized water, reaction 4h obtains faint yellow transparent solution, after solvent is volatilized, obtain the white powder material.This is a 2 ethyl hexanoic acid modified titanic oxide nano powder.
Example 3:
The 100mmol n-caprylic acid is added in the mixing solutions of the 100ml water of 60 ℃ of constant temperature and 50ml acetone, the ammonia soln that adds 25ml 25-28% again, isothermal reaction 30 minutes, the 100mmol calcium chloride that will be dissolved in 100ml water then in advance dropwise adds reaction soln under strong mixing, there are a large amount of white gelatinous precipitates to generate immediately, continue isothermal reaction 2 hours, precipitate after filtration, wash, and dry under 80 ℃, promptly obtain size of particles and modify the calcium hydroxide nano powder at the n-caprylic acid of 2-5nm.
Example 4:
With 50ml 14molL
-1Ammoniacal liquor add in the mixing solutions of the 100ml acetate of 50 ℃ of constant temperature and 50ml water, react after 30 minutes, add 100mmol and be dissolved in alcoholic acid SnCl in advance
4, there is relatively large sour shape precipitation to generate immediately, add the 50mmol capric acid then, and be warmed up to 75-80 ℃, and under strong mixing isothermal reaction 10-20 hour, sedimentation and filtration, washing, and dry under 110 ℃, promptly obtain size of particles and modify the stannic oxide nanometer micro mist at the capric acid of 10-20nm.
Example 5:
50mmol oleic acid is added in the 80ml water and 70ml alcoholic acid mixing solutions of 60 ℃ of constant temperature, add 25ml 14mol.L again
-1Ammonia soln, react solution clarification in 30 minutes, then water-soluble in advance 100mmol Europium trichloride is dropwise added reaction soln under strong mixing, there are a large amount of white gelatinous precipitates to generate immediately, continue isothermal reaction 6-12 hour, precipitation after filtration, washing and dry, promptly obtain the europium sesquioxide nano powder of size of particles at 10-20nm.
Example 6:
The 20mmol capric acid is added in the 80ml water 50ml acetone and 20ml alcoholic acid mixing solutions of 75 ℃ of constant temperature, the ammonia soln that adds 10ml 25-28% again, react and clarified to solution in 30 minutes, the 50mmol bariumchloride that will be dissolved in 50ml water then in advance dropwise adds reaction soln under strong mixing, there have a large amount of white glues to be settled out immediately to be existing, continues isothermal reaction 5-10 hour, and precipitation is washing after filtration, and, promptly obtain capric acid and modify (hydrogen) barium oxide nano powder 110 ℃ of following vacuum-dryings 6 hours.
Example 7:
The 20mmol valeric acid is added in the 50ml water and 100ml alcoholic acid mixing solutions of 75 ℃ of constant temperature, the ammonia soln that adds 10ml 25-28% again, reacted 30 minutes, to be dissolved in 50ml alcoholic acid 100mmol yttrium trichloride then in advance, under strong mixing, dropwise add reaction soln, precipitation after filtration, washing, and 110 ℃ of following vacuum-dryings 6 hours, promptly obtain amylalcohol and modify the yttrium oxide nano powder.
Example 8:
The Sodium orthomolybdate of 50mmol is dissolved in 30ml deionized water and heated constant temperature to 50 ℃, adding dehydrated alcohol has microprecipitation to generate, and then the adding less water is just dissolved precipitation, constant temperature 30 minutes dropwise adds the butyro-alcohol-water of 500mmol (1: 2) mixing solutions to there being a large amount of white flockss to occur, and continues reaction 10 hours, precipitation after filtration, absolute ethanol washing, and 60 ℃ of following vacuum-dryings 6 hours, promptly obtain butyric acid and modify the molybdenum oxide nano powder.
Example 9:
The 100mmol 2 ethyl hexanoic acid is dissolved in the 100ml ethanolic soln, and the ammonia soln of heated constant temperature to 60 ℃ adding 25ml 25-28%, reacted 30 minutes, and under strong mixing, dropwise added the 50mmol iron trichloride that is dissolved in the 50ml dehydrated alcohol in advance then, have a large amount of reddish-brown gelatinous precipitates to generate, continue isothermal reaction 24 hours, cooling precipitates after filtration absolute ethanol washing, and, promptly obtain 2 ethyl hexanoic acid modified ferric oxide nano micro mist 110 ℃ of following vacuum-dryings 12 hours.
Example 10:
The sad 100ml ethanolic soln that is dissolved in of 100mmol, and heated constant temperature to 60 ℃ adding 120mmol is dissolved in the sodium hydroxide solution of 20ml water in advance, reacted 30 minutes, if precipitation is arranged, can add less water and make its dissolving, under strong mixing, dropwise add the 50mmol silver nitrate aqueous solution then, there are a large amount of white gelatinous precipitates to generate, continue reaction 10 hours, precipitation after filtration, wash for several times with 60 ℃ of warm water again behind the absolute ethanol washing, and, promptly obtain sad modification silver suboxide nano powder 60 ℃ of following vacuum-dryings 24 hours.
Example 11:
The aluminum trichloride (anhydrous) of 100mmol is dissolved in the 20ml dehydrated alcohol makes stock solution A, the isopropylformic acid of 200mmol is dissolved in 100ml dehydrated alcohol and heated constant temperature to 60 ℃, adds the ammonia soln of 25ml-30ml 25-28% again, reacts 30 minutes.Then stock solution A is dropwise added, and the generation of adularescent gelatinous precipitate, precipitate after filtration, wash, and, promptly obtain sad modification aluminium hydrate nano micro mist 60 ℃ of following vacuum-dryings 24 hours.
Example 12:
The 20mmol stearic acid is dissolved in the 100ml dehydrated alcohol, heated constant temperature to 60 ℃, add the ammonia soln of 15ml 25-28%, reacted 30 minutes, under strong mixing, dropwise add the 100mmol lead nitrate solution that is dissolved in advance in the 50ml water then, the adularescent gelatinous precipitate generates immediately, continue isothermal reaction 24 hours, filtered while hot, and use absolute ethanol washing, and, promptly obtain stearic acid and modify the plumbous oxide nano powder 110 ℃ of following vacuum-dryings 24 hours.
Example 13:
The 100mmol stearic acid is dissolved in the mixing solutions of 100ml dehydrated alcohol and 50ml water, heated constant temperature to 60 ℃, the ammonia soln that adds 30ml 25-28%, reacted 30 minutes, under strong mixing, dropwise add the 100mmol Lanthanum trichloride that is dissolved in advance in the 50ml dehydrated alcohol then, the adularescent gelatinous precipitate generates immediately, continue isothermal reaction 6 hours, filtered while hot, and with the washing of 1: 1 ethanol-water mixed solvent, and, promptly obtain stearic acid and modify the lanthanum trioxide nano powder 110 ℃ of vacuum-dryings 24 hours.
Example 14:
The ammonia soln that in the 50ml water of constant temperature to 80 ℃ and 100ml alcohol mixed solvent, adds 100mmol oleic acid and 20ml 25-28%, react and clarified to solution in 30 minutes, the tin tetrachloride that will be dissolved in the 150mmol of 20ml dehydrated alcohol then in advance dropwise adds reaction soln under strong mixing, there have a large amount of white colloids to be settled out immediately to be existing, continue isothermal reaction 10 hours, precipitation after filtration, washing, and, promptly obtain oleic acid modified stannic oxide nanometer particulate 110 ℃ of following vacuum-dryings 48 hours.
Example 15:
In the 30ml water of constant temperature to 80 ℃ and 100ml alcohol mixed solvent, add 20ml 25-28% ammonia soln, the 100mmol europium chloride that will be dissolved in the 20ml dehydrated alcohol then in advance dropwise adds reaction soln under strong mixing, adularescent colloidal precipitation generates, the 100mmol arachic acid that will be dissolved in the 50ml dehydrated alcohol then in advance adds reaction soln under strong mixing, isothermal reaction 24 hours, precipitation after filtration, washing, and 110 ℃ of following vacuum-dryings 48 hours.Promptly obtain arachic acid and modify the europium sesquioxide nanoparticle.
Claims (8)
1. fatty acid modifying metallic oxide or hydroxide nano micro mist is characterized in that it being lipid acid
Be chemically bound in the nanoparticle of metal oxide or oxyhydroxide, and fatty acid hydrocarbon chain shared weight percent in the decorated nanometer particulate is 5%-80%, wherein the chain length of lipid acid R is C
2-C
20The straight or branched alkyl, metal oxide or oxyhydroxide comprise the oxide compound or the oxyhydroxide of transition group and second and third, four, five main group metal elements.
2. nano powder as claimed in claim 1 is characterized in that being C
8-C
18The fatty acid chemistry of straight or branched alkyl be bonded to metal oxide or the oxyhydroxide of Zr, Ti, Sn, Pb, Zn, Fe, Y, Co, Ni, La, Eu.
3. fatty acid modifying metallic oxide or hydroxide nano micro mist preparation method is characterized in that A) use lipid acid
, oxyammonia and soluble metal salt, wherein the R chain length is C in the lipid acid
2-C
20The straight or branched alkyl, soluble metallic salt comprises transition group and second and third, four, five main group metal elements, the mol ratio of lipid acid and metal-salt is 1: 0.1-10 is tetrahydrofuran (THF), C at reaction medium B)
1-C
4Lipid acid, acetone and these solvents exist down with the blending agent of water alone or in combination, and the mol ratio of lipid acid and reaction medium is 1: 500-2000, C) normal temperature-120 ℃ reacted 2-48 hour down.
4. as the preparation method of nanoparticle as described in the claim 3, it is characterized in that the R chain length is C in the lipid acid
8-C
18
5. the preparation method of nanoparticle as claimed in claim 3 is characterized in that the salt of solubility comprises Zr, Ti, Sn, Pb, Fe, Zn, Y, Co, Ni, La, Eu metallic element salt.The salt of solubility comprises Zr, Ti, Sn, Pb, Fe, Zn, Y, Co, Ni, La, Eu metallic element salt.
6. the preparation method of nanoparticle as claimed in claim 3, the mol ratio that it is characterized in that lipid acid and metal-salt is 1: 1-4.
7. the preparation method of nanoparticle as claimed in claim 3 is characterized in that reaction medium is 66% alcohol+34% water.
8. the preparation method of nanoparticle as claimed in claim 3 is characterized in that temperature of reaction is 60-80 ℃.
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| CN 95106896 CN1180079A (en) | 1995-07-06 | 1995-07-06 | Fatty acid modifying metallic oxide or hydroxide nanometre powder and its preparing method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 95106896 CN1180079A (en) | 1995-07-06 | 1995-07-06 | Fatty acid modifying metallic oxide or hydroxide nanometre powder and its preparing method |
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ID=5076107
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1058984C (en) * | 1998-10-08 | 2000-11-29 | 中国科学院兰州化学物理研究所 | Nano size rare earth hydroxide lubricant oil additive |
| CN1058985C (en) * | 1998-10-08 | 2000-11-29 | 中国科学院兰州化学物理研究所 | Nano size rare earth fluoride lubricant oil additive |
| CN101003386B (en) * | 2006-10-19 | 2010-05-12 | 河南大学 | A method for preparing monodisperse, oil-soluble surface-modified iron oxide nanoparticles |
| CN103904332A (en) * | 2014-02-19 | 2014-07-02 | 上海璞泰来新材料技术有限公司 | Lithium titanate negative electrode material and preparation method thereof and lithium ion battery using material |
| EP3091065A1 (en) | 2015-04-20 | 2016-11-09 | China Petroleum&Chemical Corporation | Lubricant composition, and preparation method and use thereof |
-
1995
- 1995-07-06 CN CN 95106896 patent/CN1180079A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1058984C (en) * | 1998-10-08 | 2000-11-29 | 中国科学院兰州化学物理研究所 | Nano size rare earth hydroxide lubricant oil additive |
| CN1058985C (en) * | 1998-10-08 | 2000-11-29 | 中国科学院兰州化学物理研究所 | Nano size rare earth fluoride lubricant oil additive |
| CN101003386B (en) * | 2006-10-19 | 2010-05-12 | 河南大学 | A method for preparing monodisperse, oil-soluble surface-modified iron oxide nanoparticles |
| CN103904332A (en) * | 2014-02-19 | 2014-07-02 | 上海璞泰来新材料技术有限公司 | Lithium titanate negative electrode material and preparation method thereof and lithium ion battery using material |
| CN103904332B (en) * | 2014-02-19 | 2016-02-24 | 上海璞泰来新能源科技股份有限公司 | A kind of lithium titanate anode material and preparation method thereof and apply the lithium ion battery of this lithium titanate anode material |
| EP3091065A1 (en) | 2015-04-20 | 2016-11-09 | China Petroleum&Chemical Corporation | Lubricant composition, and preparation method and use thereof |
| US9944883B2 (en) | 2015-04-20 | 2018-04-17 | China Petroleum & Chemical Corporation | Lubricant composition, and preparation method and use thereof |
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