CN108714420A - The preparation method of optomagnetic response hollow microsphere - Google Patents
The preparation method of optomagnetic response hollow microsphere Download PDFInfo
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- CN108714420A CN108714420A CN201810432761.2A CN201810432761A CN108714420A CN 108714420 A CN108714420 A CN 108714420A CN 201810432761 A CN201810432761 A CN 201810432761A CN 108714420 A CN108714420 A CN 108714420A
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- milliliter
- ethyl alcohol
- optomagnetic
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- 239000004005 microsphere Substances 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 44
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000002071 nanotube Substances 0.000 claims abstract description 18
- HPTYUNKZVDYXLP-UHFFFAOYSA-N aluminum;trihydroxy(trihydroxysilyloxy)silane;hydrate Chemical compound O.[Al].[Al].O[Si](O)(O)O[Si](O)(O)O HPTYUNKZVDYXLP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 235000019441 ethanol Nutrition 0.000 claims abstract description 17
- 229910052621 halloysite Inorganic materials 0.000 claims abstract description 17
- 239000004094 surface-active agent Substances 0.000 claims abstract description 17
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims abstract description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 11
- 229920001214 Polysorbate 60 Polymers 0.000 claims abstract description 9
- 239000002105 nanoparticle Substances 0.000 claims abstract description 9
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 9
- PRXRUNOAOLTIEF-ADSICKODSA-N Sorbitan trioleate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OC[C@@H](OC(=O)CCCCCCC\C=C/CCCCCCCC)[C@H]1OC[C@H](O)[C@H]1OC(=O)CCCCCCC\C=C/CCCCCCCC PRXRUNOAOLTIEF-ADSICKODSA-N 0.000 claims abstract description 8
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims abstract description 8
- 235000019394 potassium persulphate Nutrition 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 7
- 230000005855 radiation Effects 0.000 claims abstract description 7
- QQZMWMKOWKGPQY-UHFFFAOYSA-N cerium(3+);trinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O QQZMWMKOWKGPQY-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000006392 deoxygenation reaction Methods 0.000 claims abstract description 6
- 239000006210 lotion Substances 0.000 claims abstract description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 6
- 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 claims abstract description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 18
- 239000004408 titanium dioxide Substances 0.000 claims description 9
- 229910052684 Cerium Inorganic materials 0.000 claims description 8
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 238000005119 centrifugation Methods 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- 238000002604 ultrasonography Methods 0.000 claims description 5
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- 239000007764 o/w emulsion Substances 0.000 claims description 3
- CERQOIWHTDAKMF-UHFFFAOYSA-M Methacrylate Chemical compound CC(=C)C([O-])=O CERQOIWHTDAKMF-UHFFFAOYSA-M 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims 1
- 150000001336 alkenes Chemical class 0.000 claims 1
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 claims 1
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 abstract description 5
- 238000000034 method Methods 0.000 abstract description 3
- 239000002245 particle Substances 0.000 description 10
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 9
- 230000001699 photocatalysis Effects 0.000 description 9
- 238000007146 photocatalysis Methods 0.000 description 6
- 150000001875 compounds Chemical class 0.000 description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 239000003292 glue Substances 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- VIKNJXKGJWUCNN-XGXHKTLJSA-N norethisterone Chemical compound O=C1CC[C@@H]2[C@H]3CC[C@](C)([C@](CC4)(O)C#C)[C@@H]4[C@@H]3CCC2=C1 VIKNJXKGJWUCNN-XGXHKTLJSA-N 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 1
- 239000003999 initiator Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- ZWYDDDAMNQQZHD-UHFFFAOYSA-L titanium(ii) chloride Chemical compound [Cl-].[Cl-].[Ti+2] ZWYDDDAMNQQZHD-UHFFFAOYSA-L 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/10—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of rare earths
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
- B01J35/51—Spheres
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Cosmetics (AREA)
- Manufacturing Of Micro-Capsules (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
A kind of preparation method of optomagnetic response hollow microsphere, it is characterised in that include the following steps:1. tetrabutyl titanate, cerium nitrate hexahydrate and ethyl alcohol are mixed to form vitreosol;2. by clear solution, ethyl alcohol and halloysite nanotubes ultrasonic mixing, acetic acid is added dropwise and stirs evenly, is roasted 5 hours at 550 DEG C after being centrifuged with ethyl alcohol;3. surfactant Tween-60 is mixed with the nanotube after roasting, centrifuged after vacuumizing;4. 3. product and toluene that ferriferrous oxide nano-particle, step are obtained are mixed, surfactant Span85 is added, continue stirring and forms lotion, be added dropwise again N ' N- dimethacrylamide, methacrylic acid and potassium peroxydisulfate mixed liquor, after being passed through nitrogen deoxygenation, polymerization occurs through microwave irradiation and obtains hollow complex microsphere.Compared with the prior art, the advantages of the present invention are as follows:The lotion and microwave radiation stablized using the nano-particle with optomagnetic response are caused polymerization and obtain hollow microsphere, simple for process efficient, are had a wide range of application.
Description
Technical field
The present invention relates to catalysis materials, refer specifically to a kind of preparation method of optomagnetic response hollow microsphere.
Background technology
The environmental pollution of getting worse has severely impacted the life and development of the mankind.Photocatalysis technology is with its room
Temperature reaction and it can become a kind of ideal environmental pollution directly using solar energy as light source come drive response etc. special performances and control
Reason technology and clear energy sources production technology.Photocatalytic oxidation is the advanced water technology occurred in recent years, and semiconductor light is urged
Agent titanium dioxide causes the extensive concern of people due to the high and excellent photoelectric properties of nontoxic, inexpensive, stability.And such as
What improve titanium dioxide photocatalytic activity and load factor on carrier and good dispersibility be related to photocatalysis effect and
Using a kind of, the invention recyclable support type hollow microsphere of photocatalysis, i.e., by the doping cerium member with photocatalysis performance
Solid particles stabilization is collectively formed to halloysite nanotubes surface, with magnetic ferroferric oxide particle in the titanium dichloride load of element
Lotion, then hollow microsphere is formed by microwave radiation polymerization.The complex microsphere compared with similar products have high specific surface area,
Recuperability and high photocatalysis performance, have wide range of applications.
Invention content
The technical problem to be solved by the present invention is to the present situation to the prior art provide it is a kind of with photocatalytic activity can
The magnetic halloysite nanotube hollow microsphere of recycling.
Technical solution is used by the present invention solves above-mentioned technical problem:Optomagnetic response galapectite pipe hollow microsphere,
It is characterized in that preparation method is as follows:
1. tetrabutyl titanate, cerium nitrate hexahydrate and EtOH Sonicate are mixed 3 hours and form vitreosol;
2. after halloysite nanotubes are mixed ultrasound with ethyl alcohol, vitreosol and acetic acid is added dropwise, stirs 24 hours, use ethyl alcohol
It is roasted 5 hours at 550 DEG C after centrifugal drying;
3. the halloysite nanotubes ultrasonic mixing of the titanium dioxide of surfactant Tween-60 and doping cerium 30 minutes, takes out
Vacuum is kept for 24 hours, and surfactant is made to enter a nanometer tube cavity, dry after centrifugation;
4. 3. product, toluene and potassium peroxydisulfate that ferriferrous oxide nano-particle, step obtain is stirred, table is added
Face activating agent Span85 is stirred and is formed within 30 minutes the oil-in-water emulsion that solid particles is stablized, then N ' N- dimethyl allene acyls are added dropwise
The mixed liquor of amine, methacrylic acid is passed through nitrogen deoxygenation and stirs 20 minutes, through microwave radiation occur polymerization obtain it is hollow compound
Microballoon.
The tetrabutyl titanate (gram) and ethyl alcohol (milliliter) ratio are 0.5~2;
The ratio of the halloysite nanotubes (milligram), ethyl alcohol (milliliter) and vitreosol (milliliter) is 10:1:1~100:
10:1;Acetic acid is 0.5~2 milliliter;
The atomic ratio of the Ce elements and titanium elements is 1~40;
The quality of the surfactant Tween-60 is 0.5~3 gram;
The compound halloysite nanotubes of titanium dioxide containing cerium of the ferriferrous oxide nano-particle, loading Tween-60,
The mass ratio of potassium peroxydisulfate, toluene and Span85 is (0.01~1) gram:(0.01~1) gram:(0.1~1) gram:(2~5) milli
It rises:(0.1~0.5) milliliter;
N ' the N- dimethacrylamide volumes are 0.1~2 milliliter, and methacrylate volume is 0.1~2 milliliter;
The microwave power is 600W, 80 DEG C of reaction temperature, 30 minutes reaction time.
Compared with prior art, hollow microsphere provided by the present invention loads surface-active using Microwave Emulsifier-Free Polymerization method
The compound galapectite and modified magnetic iron particle of agent form stable emulsion in oil meter face, add polymer monomer and initiator,
Caused by microwave and polymerize, compound galapectite pipe magnetism iron particle is made to form the shell being coated on oil droplet in oil droplets,
Then by later stage centrifugation, washing, drying, the optomagnetic response Hollow Microspheres with micro-nano hole structure are obtained;Not only carry significantly
High specific surface area, and there is good photocatalysis performance and recuperability, the compound galapectite Hollow Microspheres preparation condition temperature
With simple for process, the prices of raw materials are cheap and easily-available, are easy to be extended and applied.
Specific implementation mode
Present invention is further described in detail for following embodiment.
1 preparation method of embodiment is as follows:
1. it is transparent molten that 2 grams of tetrabutyl titanates, 0.01 gram of cerium nitrate hexahydrate and 2 milliliters of EtOH Sonicates are mixed formation in 2 hours
Glue;
2. after 50 milligrams of halloysite nanotubes are mixed ultrasound with 0.5 milliliter of ethyl alcohol, be added dropwise 0.5 milliliter vitreosol and
0.5 milliliter of acetic acid stirs 24 hours, is roasted 5 hours with ethyl alcohol centrifuge washing, then with 550 degree after water centrifuge washing times;
3. the titanium dioxide halloysite nanotubes ultrasonic mixing of 1 gram of surfactant Tween-60 and doping cerium 20 minutes,
Holding 24 hours is vacuumized, surfactant is made to enter a nanometer tube cavity, it is dry after centrifugation;
4. 3. product that 0.15 gram of ferriferrous oxide nano-particle, step are obtained, 0.1 gram of potassium peroxydisulfate and 2 milliliters of first
Benzene is stirred, and 0.1 milliliter of surfactant Span85 is added, and is stirred 30 minutes and is formed oil-in-water emulsion, then 0.1 milli is added dropwise
The mixed liquor for rising N ' N- dimethacrylamide and 0.1 milliliter of methacrylic acid is passed through nitrogen deoxygenation and stirs 20 minutes, through microwave
Radiation, radiated time are 30 minutes, and 80 DEG C of reaction temperature occurs polymerization and obtains hollow complex microsphere.
It is detected through particle size analyzer, microsphere particle size is distributed between 3~20 microns.
The preparation method of embodiment 2 is as follows:
1. it is transparent molten that 3 grams of tetrabutyl titanates, 0.02 gram of cerium nitrate hexahydrate and 5 milliliters of EtOH Sonicates are mixed formation in 2 hours
Glue;
2. after 70 milligrams of halloysite nanotubes are mixed ultrasound with 1 milliliter of ethyl alcohol, be added dropwise 0.6 milliliter vitreosol and
0.5 milliliter of acetic acid is stirred 24 hours, is roasted 5 hours at 550 DEG C after ethyl alcohol centrifugal drying;
3. the titanium dioxide halloysite nanotubes ultrasonic mixing of 2 grams of surfactant Tween-60 and doping cerium 20 minutes,
Holding 24 hours is vacuumized, surfactant is made to enter a nanometer tube cavity, it is dry after centrifugation;
4. 3. product that 0.2 gram of ferriferrous oxide nano-particle, step are obtained, 0.15 gram of potassium peroxydisulfate and 3 milliliters of first
Benzene is stirred, and 0.3 milliliter of surfactant Span85 is added, and is stirred and is formed within 30 minutes the lotion that solid particle is stablized, then drips
The mixed liquor for adding 0.3 milliliter of N ' N- dimethacrylamide and 0.3 milliliter of methacrylic acid is passed through nitrogen deoxygenation and stirs 20 points
Clock, through microwave radiation, radiated time is 30 minutes, 80 DEG C of reaction temperature, and polymerization occurs and obtains hollow complex microsphere.
It is detected through particle size analyzer, microsphere particle size is distributed between 3~20 microns.
The preparation method of embodiment 3 is as follows:
1. 5 grams of tetrabutyl titanates and 0.04 gram of cerium nitrate hexahydrate, 8 milliliters of EtOH Sonicates mixing are formed for 2 hours transparent molten
Glue;
2. after 100 milligrams of halloysite nanotubes are mixed ultrasound with 2 milliliters of ethyl alcohol, 1 milliliter of vitreosol and 1 is added dropwise
The acetic acid of milliliter is stirred 24 hours, is roasted 5 hours at 550 DEG C after ethyl alcohol centrifugal drying;
3. the halloysite nanotubes ultrasonic mixing 20 of 4 grams of surfactant Tween-60 and the titanium dioxide of doping cerium are divided
Clock vacuumizes holding 24 hours, surfactant is made to enter a nanometer tube cavity, dry after centrifugation;
4. 3. product that 0.3 gram of ferriferrous oxide nano-particle, step are obtained, 0.2 milliliter of potassium peroxydisulfate and 4 milliliters of first
Benzene is stirred, and 0.5 milliliter of surfactant Span85 is added, and is stirred and is formed within 30 minutes the lotion that solids are stablized, then drips
The mixed liquor for adding 0.5 milliliter of N ' N- dimethacrylamide and 0.5 milliliter of methacrylic acid is passed through nitrogen deoxygenation and stirs 20 points
Clock, through microwave radiation, radiated time is 30 minutes, 80 DEG C of reaction temperature, and polymerization occurs and obtains hollow complex microsphere.
Claims (3)
1. a kind of hollow galapectite pipe microballoon of optomagnetic response, it is characterised in that preparation method is as follows:
1. tetrabutyl titanate, cerium nitrate hexahydrate and EtOH Sonicate are mixed 2 hours and form vitreosol, the tetrabutyl titanate
(gram) and ethyl alcohol (milliliter) ratio is 0.5~2;
2. after halloysite nanotubes are mixed ultrasound with ethyl alcohol, vitreosol and acetic acid is added dropwise, stirs 24 hours, centrifuged with ethyl alcohol
It is roasted 5 hours at 550 DEG C after drying;The halloysite nanotubes (milligram), ethyl alcohol (milliliter) and vitreosol (milliliter) ratio
Example is 10:1:1~100:10:1;Acetic acid is 0.5~2 milliliter;
3. by the halloysite nanotubes ultrasonic mixing 20 minutes of surfactant Tween-60 and the titanium dioxide of doping cerium, take out true
Sky is kept for 24 hours, and surfactant is made to enter a nanometer tube cavity, dry after centrifugation;The quality of the surfactant is 0.5-
3 grams;
4. 3. product, potassium peroxydisulfate and toluene that ferriferrous oxide nano-particle, step obtain is stirred, surface is added and lives
Property agent Span85, stir and form within 30 minutes the lotion that solids are stablized, then N ' N- dimethacrylamide and methyl-prop is added dropwise
The mixed liquor of olefin(e) acid is passed through nitrogen deoxygenation and stirs 20 minutes, forms oil-in-water emulsion, and through microwave radiation, radiated time is 30 points
Clock, 80 DEG C of reaction temperature occur polymerization and obtain hollow complex microsphere.
2. the preparation method of optomagnetic response hollow microsphere according to claim 1, it is characterised in that step 4. described in
Ferriferrous oxide nano-particle, load the titanium dioxide halloysite nanotubes containing cerium of Tween-60, potassium peroxydisulfate, toluene and
The ratio of Span85 is (0.01~1) gram:(0.01~1) gram:(0.1~1) gram:(2~5) milliliter:(0.1~0.5) milliliter;Institute
It is 0.1~2 milliliter to state N ' N- dimethacrylamide volumes;Methacrylate volume is 0.1~2 milliliter.
3. the preparation method of optomagnetic response hollow microsphere according to claim 1, it is characterised in that step 4. in microwave
Power 600W, 30 minutes reaction time, reaction temperature 80.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN114606041A (en) * | 2022-03-16 | 2022-06-10 | 四川大学 | Wear-resistant lubricant based on modified halloysite and preparation method thereof |
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2018
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN114606041A (en) * | 2022-03-16 | 2022-06-10 | 四川大学 | Wear-resistant lubricant based on modified halloysite and preparation method thereof |
CN114606041B (en) * | 2022-03-16 | 2023-01-24 | 四川大学 | Wear-resistant lubricant based on modified halloysite and preparation method thereof |
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