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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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 ℃.
Priority Applications (1)
| 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 |
Applications Claiming Priority (1)
| 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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|---|---|
| CN1180079A true CN1180079A (en) | 1998-04-29 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 95106896 Pending 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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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 | Method for preparing Nano microparticles of monodisperse, oil soluble, surface modified iron oxide |
| 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 | Method for preparing Nano microparticles of monodisperse, oil soluble, surface modified iron oxide |
| 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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