CN110028810A - A kind of preparation method and applications of composite modified nano yttrium oxide - Google Patents

A kind of preparation method and applications of composite modified nano yttrium oxide Download PDF

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CN110028810A
CN110028810A CN201910400378.3A CN201910400378A CN110028810A CN 110028810 A CN110028810 A CN 110028810A CN 201910400378 A CN201910400378 A CN 201910400378A CN 110028810 A CN110028810 A CN 110028810A
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yttrium oxide
added
nano yttrium
modified nano
composite modified
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龚晔
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CHANGZHOU GEOQUIN NANO NEW MATERIALS Co Ltd
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CHANGZHOU GEOQUIN NANO NEW MATERIALS Co Ltd
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    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
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    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
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    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/04—Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
    • C09C3/041—Grinding
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    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/06—Treatment with inorganic compounds
    • C09C3/063—Coating
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/12—Treatment with organosilicon compounds
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M125/00—Lubricating compositions characterised by the additive being an inorganic material
    • C10M125/10—Metal oxides, hydroxides, carbonates or bicarbonates
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/06—Metal compounds
    • C10M2201/062—Oxides; Hydroxides; Carbonates or bicarbonates
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/14—Inorganic compounds or elements as ingredients in lubricant compositions inorganic compounds surface treated with organic compounds
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/04—Detergent property or dispersant property

Abstract

The present invention provides a kind of preparation method and applications of composite modified nano yttrium oxide, belong to lube oil additive preparation field.YCl is added in dispersant solution3It is sufficiently stirred in solution, sodium carbonate liquor is then added, adjusting pH is 6~7；Polyether silane is added into the mixed liquor for adjusting pH value, is aged after being stirred, washes, calcining obtains nano yttrium oxide powder；Calcined nano yttrium oxide powder and deionized water are added in sand mill, additive grinding is added, slurry freeze-drying after grinding, sieving, obtain composite modified nano yttrium oxide particle, it can be used as lube oil additive application, the present invention coats one layer in nano rare earth mineral surfaces with composite modifying method, it obtains oil-soluble rare earth inorganic-organic nanocomposite and has both nano material, refer to application aspect as extreme pressure, Antiwear additive are resonable and have good development prospect.

Description

A kind of preparation method and applications of composite modified nano yttrium oxide
Technical field
The present invention relates to a kind of preparation method of composite modified nano yttrium oxide and its as the application of lube oil additive, Belong to lube oil additive preparation field.
Technical background
With the fast development of modern mechanical industry, lubricating oil has become its indispensable pith, and multi-functional, Efficiently, green lube oil additive determines the quality of modern lubricating oil.It is to reduce friction mill using the purpose of lubricating oil Damage reduces unnecessary material friction consumption.
Since nano material has the characteristics such as large specific surface area, high diffusibility, as lube oil additive, with traditional profit Lubricating oil, which is compared, has huge advantages for development, and conventional lubrication oil contains the environmentally harmful element such as S, P, and has to friction surface Have certain corrosion, and nano material be for environment it is environmentally protective, nano material when being used for lube oil additive, for Frictional abrasion surface has self-repair function, to protect friction surface, reduces friction.
Nanoscale yttrium has many new capabilities, but the partial size of nano yttrium oxide particle is small, large specific surface area, surface Active high, easy reunion, makes the application of nano yttrium oxide receive certain limitation, answering especially in terms of non-polar system With because nano yttrium oxide surface exhibits are polarity, summarizing dispersion that cannot be stable in non-polar system, and being easy to reunite cannot Embody the superiority of nano material, it is therefore necessary to carry out surface and be modified, so as to improve the limitation of its application, expand application Field.
Based on the status studied at present, high perofmrnace lubricating oils additive is obtained, it is necessary to nanoparticle be overcome easily to reunite The shortcomings that with non-oil-soluble, therefore the rare earth based additive for developing organic-inorganic nanocomposite just has great importance.With Composite modifying method coats one layer in nano rare earth mineral surfaces, obtains oil-soluble rare earth organic-inorganic nanocomposite material Material the advantages of having both nano material, rare earth material and organic material, as extreme pressure, Antiwear additive is resonable refers to Application aspect has good development prospect.
Summary of the invention
The present invention provides a kind of preparation methods of composite modified nano yttrium oxide, and its purpose is to nano yttrium oxide Coating modification is carried out, is mainly used for lube oil additive, it is desirable that modified powder can be in for a long time in dehydrated alcohol Suspended state has excellent dispersion stabilization.
In order to solve the above-mentioned technical problem, using following technical scheme:
(1) YCl of 01~0.4mol/L is prepared respectively first3Solution, 0.2-0.4mol/L sodium carbonate liquor and dispersing agent Solution；
(2) YCl is added in dispersant solution3It is sufficiently stirred in solution, then contains the addition of sodium carbonate liquor diaphragm pump There is the YCl of dispersing agent3In solution, addition speed is 7~8L/min, and it is 6~7 that pH is adjusted after addition, obtains mixed liquor；Diaphragm pump The stability of flow can more preferably be controlled；
(3) polyether silane is added into mixed liquor, is stirred 1~3h, is aged 3-5 hours after stirring；
(4) to be aged to be washed after the completion with 60~70 DEG C of deionized waters, the yttrium oxide presoma after washing is calcined, Obtain nano yttrium oxide powder；Nano yttrium oxide granular size is 20-50nm, and BET detects 20-30；
Primary and foremost purpose with 60~70 DEG C of hot water is the impurity of the ionic cleaned in yttrium oxide presoma, less than 60 DEG C Water difficult impurity for washing ionic if cleaning, needs the time longer, and can be improved after 60~70 DEG C of hot water are washed The BET of powder after calcination.
(5) calcined nano yttrium oxide powder and deionized water are added in sand mill, start to grind after additive is added Slurry after grinding will be freeze-dried, is sieved, obtains composite modified nano yttrium oxide particle, add for lubricating oil by mill Agent, granular size are 20-50nm, and BET detects 40-50.
Further, the dispersing agent is PEG 20000 or neopelex；Dispersing agent adding proportion is (adding proportion is by YCl to 2%-5%3Solution is converted into the 2%-5% of yttrium oxide weight)
Further, the polyether silane is Degussa4144；Polyether silane adding proportion is 1%-3% It (is according to YCl3Solution is converted into the 1%-3% of yttrium oxide weight)
Further, 750~850 DEG C of calcination temperature, calcination time are 2~5 hours；
Further, the additive is made of KH550, KH570, KH560, and the mixing of 1:2:1~1:3:1 in mass ratio adds Agent additional amount is added to account for by YCl3Solution is converted into the 2% of yttrium oxide powder quality.
Compared with prior art, the present invention what is obtained has the beneficial effect that
Product is deposited on powder surface using chemical reaction by the modified method of the precipitation reaction that the present invention uses,！In particle Surface forms tunic shape precipitating, forms one or more modified layers, keeps particle not easy to reunite during the growth process.
The present invention first be tentatively modified using polyether silane before nano yttrium oxide particle is formed, through preliminary modified Adsorptivity, wetability, lipophilicity can be improved in the property and structure for obtaining particle, and the cladding of early period can make the property and structure of particle It finalizes the design almost, powder retains the wetability of particle, lipophilicity substantially after calcination, is not only obviously improved effect to being coated with for later period Fruit, and modified technique and the time in later period are greatly simplified, cost process is reduced, it is suitable for mass production.
Detailed description of the invention
Fig. 1 is composite modified nano yttrium oxide electron-microscope scanning figure made of embodiment 1.
Fig. 2 is modified Nano yttrium oxide electron-microscope scanning figure made of comparative example 1.
Specific embodiment
Embodiment 1
1, the YCl of 1.72mol/L is taken3Solution 258L adds deionized water 1960L, is configured to 0.2mol/L；(equivalent oxidation Yttrium is 50kg)
2,75kg sodium carbonate is taken, deionized water 1769L is added, dissolution is sufficiently stirred, be configured to 0.4mol/L；
3,20000 1000g of taking polyethylene glycol is added a small amount of deionized water and sufficiently dissolves；
4, PEG 20000 solution is added to the YCl of 0.2mol/L3It is sufficiently stirred in solution；
5, the sodium carbonate liquor of 0.4mol/L is added to the YCl of step 4 with diaphragm pump3In solution, speed 7-8L/ is added Min adjusts PH6-7 after dropwise addition；
6,500g polyether silane (Degussa is added4144) it, stirs 1 hour；
7, room temperature is aged 3 hours；
8, with (60-70 DEG C) of deionized water washing after being aged；
9, the yttrium oxide presoma after washing is calcined, calcination temperature is 850 degrees Celsius, keeps the temperature 2 hours；
It 10, is 30-50nm, BET detection 30 with TEM, SEM characterization nano yttrium oxide granular size；
11, calcined nano yttrium oxide powder 50kg and deionized water 100kg is taken, is put into sand mill, addition is added Agent 1000g (additive is made of KH550, KH570, KH560 1:3:1 in mass ratio), starts to grind, and grinds revolving speed 2000r/ Min, milling time 60 minutes.
12, the slurry after grinding is dried, drying mode is freeze-drying；
13, the powder after drying is sieved, obtains composite modified nano yttrium oxide.
14, the powder detection being sieved is 30-50nm, BET detection 48 with TEM, SEM characterization nano yttrium oxide granular size；
Composite modified nano yttrium oxide powder is put into after being stirred in dehydrated alcohol and stands 72 hours and be not obviously layered.
Embodiment 2
1, the YCl of 1.72mol/L is taken3Solution 258L adds deionized water 4180L, is configured to 0.1mol/L；
2,75kg sodium carbonate is taken, deionized water 3538L is added, dissolution is sufficiently stirred, be configured to 0.2mol/L；
3,20000 2500g of taking polyethylene glycol is added a small amount of deionized water and sufficiently dissolves, obtains PEG 20000 solution；
4, PEG 20000 solution is added to the YCl of 0.1mol/L3It is sufficiently stirred in solution；
5, the sodium carbonate liquor of 0.2mol/L is added to the YCl of step 4 with diaphragm pump3In solution, speed 7-8L/ is added Min, PH:6-7 after dropwise addition；
6,1000g polyether silane (Degussa is added4144) it, stirs 2 hours；
7, it is aged 5 hours；
8, it is washed with (60-70 DEG C) of deionized water；
9, the yttrium oxide presoma after washing is calcined, 750 degrees Celsius of temperature, keeps the temperature 5 hours；
It 10, is 20-50nm, BET detection 28 with TEM, SEM characterization nano yttrium oxide granular size；
11, calcined nano yttrium oxide powder 50kg and deionized water 100kg is taken, is respectively put into sand mill, is added Additive 1000g (additive is made of KH550, KH570, KH560, ratio 1:2:1), starts to grind, and grinds revolving speed 2000r/ Min, milling time 30 minutes.
12, the slurry after grinding is dried, drying mode is freeze-drying；
13, the powder after drying is sieved, obtains composite modified nano yttrium oxide.
14, the powder detection being sieved is 20-50nm, BET detection 44 with TEM, SEM characterization nano yttrium oxide granular size；
Composite modified nano yttrium oxide powder is put into after being stirred in ethanol solution and stands 72 hours and obviously do not divide Layer.
Embodiment 3
1, the YCl of 1.72mol/L is taken3Solution 258L adds deionized water 851L, is configured to 0.4mol/L；
2,75kg sodium carbonate is taken, deionized water 2358L is added, dissolution is sufficiently stirred, be configured to 0.3mol/L；
3, neopelex 1500g is taken, a small amount of deionized water is added and sufficiently dissolves；
4, neopelex solution is added to the YCl of 0.4mol/L3It is sufficiently stirred in solution；
5, the sodium carbonate liquor of 0.3mol/L is added to the YCl of step 4 with diaphragm pump3In solution, speed 7-8L/ is added Min, PH:6-7 after dropwise addition；
6,1500g polyether silane (Degussa is added4144) it, stirs 2 hours；
7, it is aged 4 hours；
8, it is washed with (60-70 DEG C) of deionized water；
9, the yttrium oxide presoma after washing is calcined, 800 degrees Celsius of temperature, keeps the temperature 3 hours；
It 10, is 20-50nm, BET detection 25 with TEM, SEM characterization nano yttrium oxide granular size；
11, calcined nano yttrium oxide powder 50kg and deionized water 100kg is taken, is respectively put into sand mill, is added Additive 1000g (additive is made of KH550, KH570, KH560, ratio 1:2.5:1), starts to grind, and grinds revolving speed 2000r/min, milling time 50 minutes.
12, the slurry after grinding is dried, drying mode is freeze-drying；
13, the powder after drying is sieved, obtains composite modified nano yttrium oxide.
14, the powder detection being sieved is 20-50nm, BET detection 41 with TEM, SEM characterization nano yttrium oxide granular size；
Composite modified nano yttrium oxide powder is put into after being stirred in ethanol solution and stands 72 hours and obviously do not divide Layer.
Comparative example 1
1, the YCl of 1.72mol/L is taken3Solution 258L adds deionized water 1960L, is configured to 0.2mol/L；
2,75kg sodium carbonate is taken, deionized water 1769L is added, dissolution is sufficiently stirred, be configured to 0.4mol/L；
3,20000 1000g of taking polyethylene glycol is added a small amount of deionized water and sufficiently dissolves；
4, PEG 20000 solution is added to the YCl of 0.2mol/L3It is sufficiently stirred in solution；
5, the sodium carbonate liquor of 0.4mol/L is added to the YCl of step 4 with diaphragm pump3In solution, speed 7-8L/ is added Min, PH:6-7 after dropwise addition；
6, it is aged 3 hours；
7, it is washed with (60-70 DEG C) of deionized water；
8, the yttrium oxide presoma after washing is calcined, 850 degrees Celsius of temperature, keeps the temperature 2 hours；
It 9, is 30-50nm, BET detection 20 with TEM, SEM characterization nano yttrium oxide granular size；
10, calcined nano yttrium oxide powder 50kg and deionized water 100kg is taken, is respectively put into sand mill, is added Additive 1000g (additive is made of KH550, KH570, KH560, ratio 1:3:1), starts to grind, and grinds revolving speed 2000r/ Min, milling time 4 hours.
11, the slurry after grinding is dried, drying mode is freeze-drying；
12, the powder after drying is sieved.
13, the powder detection being sieved is 50-100nm, BET detection 30 with TEM, SEM characterization nano yttrium oxide granular size； Nano yttrium oxide powder is put into after standing 24 hours after stirring in ethanol solution and begins with obvious layering；
Fig. 2 is modified Nano yttrium oxide electron-microscope scanning figure made of 1 step 12 of comparative example.It can be seen that with after Fig. 1 comparison Embodiment 1 can make the property of particle and structure finalize the design almost by the cladding of early period, and powder retains the profit of particle substantially after calcination It is moist, lipophilic.
Comparative example 2
1, the YCl of 1.72mol/L is taken3Solution 258L adds deionized water 4180L, is configured to 0.1mol/L；
2,75kg sodium carbonate is taken, deionized water 3538L is added, dissolution is sufficiently stirred, be configured to 0.2mol/L；
3,20000 2500g of taking polyethylene glycol is added a small amount of deionized water and sufficiently dissolves；
4, PEG 20000 solution is added to the YCl of 0.1mol/L3It is sufficiently stirred in solution；
5, the sodium carbonate liquor of 0.2mol/L is added to the YCl of step 4 with diaphragm pump3In solution, speed 7-8L/ is added Min, PH:6-7 after dropwise addition；
6,1000g Silane coupling agent KH550 is added, stirs 2 hours；
7, it is aged 5 hours；
8, it is washed with (60-70 DEG C) of deionized water；
9, the yttrium oxide presoma after washing is calcined, 750 degrees Celsius of temperature, keeps the temperature 5 hours；
It 10, is 40-70nm, BET detection 21 with TEM, SEM characterization nano yttrium oxide granular size；
11, calcined nano yttrium oxide powder 50kg and deionized water 100kg is taken, is respectively put into sand mill, is added Additive 1000g (additive is made of KH550, KH570, KH560, ratio 1:2:1), starts to grind, and grinds revolving speed 2000r/ Min, milling time 30 minutes.
12, the slurry after grinding is dried, drying mode is freeze-drying；
13, the powder after drying is sieved.
14, the powder detection being sieved is 40-70nm, BET detection 33 with TEM, SEM characterization nano yttrium oxide granular size；
Final nano yttrium oxide powder obtained is put into after can standing 2 hours after stirring in ethanol solution and is started There is obvious layering；
Comparative example 3
1, the YCl of 1.72mol/L is taken3Solution 258L adds deionized water 851L, is configured to 0.4mol/L；
2,75kg sodium carbonate is taken, deionized water 2358L is added, dissolution is sufficiently stirred, be configured to 0.3mol/L；
3, neopelex 1500g is taken, a small amount of deionized water is added and sufficiently dissolves；
4, neopelex solution is added to the YCl of 0.4mol/L3It is sufficiently stirred in solution；
5, the sodium carbonate liquor of 0.3mol/L is added to the YCl of step 4 with diaphragm pump3In solution, speed 7-8L/ is added Min, PH:6-7 after dropwise addition；
6,1500g polyether silane (Degussa is added4144) it, stirs 2 hours；
7, it is aged 4 hours；
8, it is washed with (60-70 DEG C) of deionized water；
9, the yttrium oxide presoma after washing is calcined, 800 degrees Celsius of temperature, keeps the temperature 3 hours；
It 10, is 20-50nm, BET detection 25 with TEM, SEM characterization nano yttrium oxide granular size；
11, nano yttrium oxide powder 50kg and deionized water 100kg after, are respectively put into sand mill, and additive is added 600g (additive is made of KH550, KH570, KH560, ratio 1:1:1), starts to grind, and grinds revolving speed 2000r/min, grinding Time 50 minutes.
12, the slurry after grinding is dried, drying mode is freeze-drying；
13, the powder after drying is sieved.
14, the powder detection being sieved is 50-100nm, BET detection 31 with TEM, SEM characterization nano yttrium oxide granular size； Final nano yttrium oxide powder obtained is put into after standing 24 hours after stirring in ethanol solution and starts gradually to be layered.
Comparative example 4
1, the YCl of 1.72mol/L is taken3Solution 258L adds deionized water 851L, is configured to 0.4mol/L；
2,75kg sodium carbonate is taken, deionized water 2358L is added, dissolution is sufficiently stirred, be configured to 0.3mol/L；
3, neopelex 1500g is taken, a small amount of deionized water is added and sufficiently dissolves；
4, neopelex solution is added to the YCl of 0.4mol/L3It is sufficiently stirred in solution；
5, the sodium carbonate liquor of 0.3mol/L is added to the YCl of step 4 with diaphragm pump3In solution, speed 7-8L/ is added Min, PH:6-7 after dropwise addition；
6,1500g polyether silane is added, stirs 2 hours；
7, it is aged 4 hours；
8, it is washed with (60-70 DEG C) of deionized water；
9, the yttrium oxide presoma after washing is calcined, 800 degrees Celsius of temperature, keeps the temperature 3 hours；
It 10, is 20-50nm, BET detection 25 with TEM, SEM characterization nano yttrium oxide granular size；
11, nano yttrium oxide powder 50kg and deionized water 100kg after, are respectively put into sand mill, and additive is added (KH550) 600g starts to grind, grind revolving speed 2000r/min, milling time 50 minutes.
12, the slurry after grinding is dried, drying mode is freeze-drying；
13, the powder after drying is sieved.
14, the powder detection being sieved is 50-100nm, BET detection 30 with TEM, SEM characterization nano yttrium oxide granular size； Final nano yttrium oxide powder obtained is put into after standing 12 hours after stirring in ethanol solution and starts gradually to be layered.

Claims (7)

1. a kind of preparation method of composite modified nano yttrium oxide, it is characterised in that: specifically preparation step is；
(1) YCl of 01~0.4mol/L is prepared respectively first3Solution, 0.2-0.4mol/L sodium carbonate liquor and dispersant solution；
(2) YCl is added in dispersant solution3It is sufficiently stirred in solution, then sodium carbonate liquor is added with diaphragm pump, speed is added Degree is 7~8L/min, and it is 6~7 that pH is adjusted after addition, obtains mixed liquor；
(3) polyether silane is added into mixed liquor, is stirred 1~3h, is aged after stirring；
(4) to be aged to be washed after the completion with 60~70 DEG C of deionized waters, the yttrium oxide presoma after washing is calcined, must be received Rice yttrium oxide powder；Nano yttrium oxide granular size is 20-50nm, and BET detects 20-30；
(5) calcined nano yttrium oxide powder and deionized water are added in sand mill, start to grind after additive is added, grinds Slurry after mill is freeze-dried, sieving, obtains composite modified nano yttrium oxide, and granular size is 20-50nm, and BET detects 40- 50。
2. the preparation method of composite modified nano yttrium oxide according to claim 1, it is characterised in that: the dispersing agent For PEG 20000 or neopelex.
3. the preparation method of composite modified nano yttrium oxide according to claim 1, it is characterised in that: the polyether silane For Degussa4144。
4. the preparation method of composite modified nano yttrium oxide according to claim 1, it is characterised in that: the digestion time It is 3-5 hours.
5. the preparation method of composite modified nano yttrium oxide according to claim 1, it is characterised in that: the calcination temperature It is 750~850 DEG C, calcination time is 2~5 hours.
6. the preparation method of composite modified nano yttrium oxide according to claim 1, it is characterised in that: the additive by KH550, KH570, KH560 1:2:1~1:3:1 in mass ratio are mixed to prepare, and additive additional amount accounts for nano yttrium oxide powder matter The 2% of amount.
7. the application of any one of -6 composite modified nano yttrium oxides according to claim 1, it is characterised in that: described compound Application of the modified Nano yttrium oxide as lube oil additive.
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CN112010338A (en) * 2020-07-27 2020-12-01 常州市卓群纳米新材料有限公司 Method for preparing low-sodium nanometer ytterbium oxide with good monodispersity by sodium salt precipitation
CN113547459A (en) * 2021-07-22 2021-10-26 广东新劲刚金刚石工具有限公司 Modified PA-66 composite resin diamond grinding tool and preparation method thereof

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CN111017976A (en) * 2019-12-27 2020-04-17 江西鑫泰功能材料科技有限公司 Preparation method of nano yttrium oxide for dielectric ceramic capacitor
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CN113547459A (en) * 2021-07-22 2021-10-26 广东新劲刚金刚石工具有限公司 Modified PA-66 composite resin diamond grinding tool and preparation method thereof

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