CN107151577A - A kind of preparation method of the vegetable oil based lubricating oil containing nano modified material - Google Patents
A kind of preparation method of the vegetable oil based lubricating oil containing nano modified material Download PDFInfo
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- CN107151577A CN107151577A CN201710299755.XA CN201710299755A CN107151577A CN 107151577 A CN107151577 A CN 107151577A CN 201710299755 A CN201710299755 A CN 201710299755A CN 107151577 A CN107151577 A CN 107151577A
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- oil
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- thorium
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- zine oxide
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- 239000000463 material Substances 0.000 title claims abstract description 24
- 235000015112 vegetable and seed oil Nutrition 0.000 title claims abstract description 22
- 239000008158 vegetable oil Substances 0.000 title claims abstract description 22
- 239000010687 lubricating oil Substances 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- ZSLUVFAKFWKJRC-IGMARMGPSA-N 232Th Chemical compound [232Th] ZSLUVFAKFWKJRC-IGMARMGPSA-N 0.000 claims abstract description 44
- 229910052776 Thorium Inorganic materials 0.000 claims abstract description 44
- 239000002994 raw material Substances 0.000 claims abstract description 27
- 238000013019 agitation Methods 0.000 claims abstract description 24
- 239000004359 castor oil Substances 0.000 claims abstract description 8
- 235000019438 castor oil Nutrition 0.000 claims abstract description 8
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 claims abstract description 8
- 239000004094 surface-active agent Substances 0.000 claims abstract description 8
- 238000011282 treatment Methods 0.000 claims abstract description 7
- 239000003456 ion exchange resin Substances 0.000 claims abstract description 6
- 229920003303 ion-exchange polymer Polymers 0.000 claims abstract description 6
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000000034 method Methods 0.000 claims abstract description 5
- 230000008878 coupling Effects 0.000 claims abstract description 4
- 238000010168 coupling process Methods 0.000 claims abstract description 4
- 238000005859 coupling reaction Methods 0.000 claims abstract description 4
- VGBPIHVLVSGJGR-UHFFFAOYSA-N thorium(4+);tetranitrate Chemical compound [Th+4].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VGBPIHVLVSGJGR-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000010306 acid treatment Methods 0.000 claims abstract 2
- NWZBFJYXRGSRGD-UHFFFAOYSA-M sodium;octadecyl sulfate Chemical compound [Na+].CCCCCCCCCCCCCCCCCCOS([O-])(=O)=O NWZBFJYXRGSRGD-UHFFFAOYSA-M 0.000 claims abstract 2
- 239000003921 oil Substances 0.000 claims description 48
- 235000019198 oils Nutrition 0.000 claims description 48
- ZCUFMDLYAMJYST-UHFFFAOYSA-N thorium dioxide Chemical compound O=[Th]=O ZCUFMDLYAMJYST-UHFFFAOYSA-N 0.000 claims description 29
- 229910003452 thorium oxide Inorganic materials 0.000 claims description 29
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 22
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 18
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 16
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 14
- 238000012986 modification Methods 0.000 claims description 12
- 230000004048 modification Effects 0.000 claims description 12
- 239000000377 silicon dioxide Substances 0.000 claims description 11
- 239000012071 phase Substances 0.000 claims description 10
- 239000004593 Epoxy Substances 0.000 claims description 9
- 239000002199 base oil Substances 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 239000008346 aqueous phase Substances 0.000 claims description 8
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 8
- 239000011734 sodium Substances 0.000 claims description 8
- 229910052708 sodium Inorganic materials 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 238000010792 warming Methods 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 7
- 239000001569 carbon dioxide Substances 0.000 claims description 7
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 7
- DMBHHRLKUKUOEG-UHFFFAOYSA-N diphenylamine Chemical class C=1C=CC=CC=1NC1=CC=CC=C1 DMBHHRLKUKUOEG-UHFFFAOYSA-N 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- 238000012545 processing Methods 0.000 claims description 7
- -1 sodium alkyl benzene Chemical class 0.000 claims description 7
- 229940077388 benzenesulfonate Drugs 0.000 claims description 6
- 239000007822 coupling agent Substances 0.000 claims description 6
- 230000009514 concussion Effects 0.000 claims description 5
- 239000007789 gas Substances 0.000 claims description 5
- 238000013517 stratification Methods 0.000 claims description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- 235000013312 flour Nutrition 0.000 claims description 4
- 239000003513 alkali Substances 0.000 claims description 3
- 238000009833 condensation Methods 0.000 claims description 3
- 230000005494 condensation Effects 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 238000004821 distillation Methods 0.000 claims description 3
- 239000003729 cation exchange resin Substances 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 240000007594 Oryza sativa Species 0.000 claims 1
- 235000007164 Oryza sativa Nutrition 0.000 claims 1
- 235000009566 rice Nutrition 0.000 claims 1
- 239000000314 lubricant Substances 0.000 abstract description 8
- 239000012530 fluid Substances 0.000 abstract description 7
- 238000011017 operating method Methods 0.000 description 25
- 229910000831 Steel Inorganic materials 0.000 description 11
- 239000010959 steel Substances 0.000 description 11
- 230000000694 effects Effects 0.000 description 10
- 238000002474 experimental method Methods 0.000 description 8
- 229920002367 Polyisobutene Polymers 0.000 description 7
- 238000005259 measurement Methods 0.000 description 7
- VQTUBCCKSQIDNK-UHFFFAOYSA-N Isobutene Chemical compound CC(C)=C VQTUBCCKSQIDNK-UHFFFAOYSA-N 0.000 description 6
- 231100000241 scar Toxicity 0.000 description 6
- 238000012360 testing method Methods 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 239000002480 mineral oil Substances 0.000 description 3
- 235000010446 mineral oil Nutrition 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 2
- 241000790917 Dioxys <bee> Species 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- 229910003978 SiClx Inorganic materials 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 229910001882 dioxygen Inorganic materials 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000005461 lubrication Methods 0.000 description 2
- 238000005498 polishing Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 235000006708 antioxidants Nutrition 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000012208 gear oil Substances 0.000 description 1
- 239000010720 hydraulic oil Substances 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000010705 motor oil Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000010773 plant oil Substances 0.000 description 1
- 230000001172 regenerating effect Effects 0.000 description 1
- 230000001235 sensitizing effect Effects 0.000 description 1
- 238000010186 staining Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000002525 ultrasonication Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- 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
- C10M169/00—Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
- C10M169/04—Mixtures of base-materials and additives
- C10M169/048—Mixtures of base-materials and additives the additives being a mixture of compounds of unknown or incompletely defined constitution, non-macromolecular and macromolecular 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
- 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
- C10M2205/00—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions
- C10M2205/02—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers
- C10M2205/026—Butene
-
- 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
- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/10—Carboxylix acids; Neutral salts thereof
- C10M2207/24—Epoxidised acids; Ester derivatives thereof
- C10M2207/243—Epoxidised acids; Ester derivatives thereof used as base material
-
- 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
- C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant Compositions
- C10M2215/02—Amines, e.g. polyalkylene polyamines; Quaternary amines
- C10M2215/06—Amines, e.g. polyalkylene polyamines; Quaternary amines having amino groups bound to carbon atoms of six-membered aromatic rings
- C10M2215/064—Di- and triaryl amines
-
- 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
- C10M2219/00—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
- C10M2219/04—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions containing sulfur-to-oxygen bonds, i.e. sulfones, sulfoxides
- C10M2219/044—Sulfonic acids, Derivatives thereof, e.g. neutral salts
-
- 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
- C10N2030/06—Oiliness; Film-strength; Anti-wear; Resistance to extreme pressure
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Chemistry (AREA)
- Lubricants (AREA)
Abstract
The invention discloses a kind of preparation method of the vegetable oil based lubricating oil containing nano modified material, difference castor oil, nano oxidized thorium, nano zine oxide, surfactant sodium stearyl sulfate, the raw material such as ion exchange resin passes through acid treatment, coupling, magnetic agitation, the modified method such as microwave treatment is prepared and uses vegetable oil synthetic lubricant fluid containing nanometer thorium nitrate etc. is material modified.
Description
Technical field
The present invention relates to a kind of preparation method of the vegetable oil based lubricating oil containing nano modified material, belong to lubricating oil skill
Art field.
Background technology
At present, the lubricating oil overwhelming majority is oily based on mineral oil.Mineral oil is extract from oil, and it is led
Want the hydrocarbon molecules mixture that composition is two kinds of element compositions of carbon and hydrogen.Cheap due to it, performance can be met mostly
The lubrication of number machinery equipment needs, in occupation of leading market status.But in some Special use occasions, such as hydraulic oil, chain saw oil,
The open system such as outboard two stroke engine oil and open gear oil or the disposable circulatory system, due to transporting, revealing, splashing
Penetrate, naturally change etc. reason, lubricating oil inevitably will be directly discharged in environment, in forest, water source, farmland, mine etc.
Sensitizing range is especially true.And mineral based lubricating oil biodegradable poor ability in natural environment, gather in the environment simultaneously
Ecological environment is polluted, a series of environmental problems is produced.Increasingly cause people in environmental protection and sustainable development
Today for paying attention to, the problem of environmental pollution that lubricating oil is brought obtained some national great attentions, and makes laws and protected
Shield.At the same time, increasingly serious energy problem is also required to regenerative resource to replace current oil product.Therefore, study
It is imperative with developing a kind of " green " lubricating oil biodegradable, that conventional mineral oil can be substituted.I have invented a kind of profit
It is used as base oil with vegetable oil, some material modified synthesis such as nanometer thorium nitrate are a kind of new to contain nanometer thorium nitrate adding
Vegetable oil synthetic lubricant fluid is used etc. material modified, has good effect at wear-resistant aspect.
The content of the invention
In view of the above-mentioned problems of the prior art, the present invention provides a kind of plant oil base profit containing nano modified material
The preparation method of lubricating oil.
To achieve these goals, the technical solution adopted by the present invention is：A kind of vegetable oil containing nano modified material
The preparation method of based lubricating oil.Comprise the following steps：
Step 1, addition castor oil and acetic acid, cationic ion-exchange resin in 1000mL three-necked flasks, oil bath heat up and opened
Beginning magnetic agitation stirs (separately weighing hydrogen peroxide in separatory funnel).It is double that slowly dropwise addition is warming up in 80 DEG C of constant temperature, temperature-rise period
Oxygen water, control rate of addition is allowed to 3h or so and added, reaction 7h or so, separates aqueous phase after stopping magnetic agitation, stratification, obtains
To epoxy oil phase；
Step 2, the Epoxy oil obtained by reaction is warming up to 80 DEG C or so, adds 80 DEG C of temperature, the hydrogen-oxygen of mass fraction 5%
Change sodium solution, low speed magnetic agitation, while examining pH value, stop adding alkali lye during close to neutrality.Continue magnetic agitation 60min,
Aqueous phase is separated after stratification, 80 DEG C or so distillations is then added and washes 5-8 times, stand, separate aqueous phase；
Step 3, obtained oil phase handle 2h under ultrasonic wave, are then added thereto reactive silica silica flour, and then 100
DEG C oil bath, magnetic agitation 3h；
Step 4 and then it is transferred to above-mentioned with the epoxy oil phase of reactive silica Si modification in 1000mL ground flasks,
80~120min is dehydrated under the conditions of 120kPa vacuums, 100 DEG C of oil bath heatings, sample is taken out, obtains the base being made of vegetable oil
Plinth oil；
Step 5 and then will be added thereto to diphenylamines is modified, and microwave treatment 2h is carried out under nitrogen atmosphere, then
In 100 DEG C of oil baths, magnetic agitation 3h；
Step 6, by nano oxidized thorium carry out coupling processing modification, DL171 type coupling agents are added in nano oxidized thorium,
Magnetic agitation 2h；
Step 7, the nano oxidized thorium being modified added in the base oil after modification, then in hot 180 DEG C of HCl gas
2h is handled under body, then neutrality is being washed to deionized water；
Step 8, nano zine oxide is added in the base oil of above-mentioned modification, then carries out reciprocating concussion processing
2h, is then being transferred in reactor, by 15kpa/min, 10 DEG C/min, and program mode is warming up to 150kpa, 100 DEG C,
3:Under 7 carbon dioxide and nitrogen atmosphere, 2h is then reacted；
Step 9, reacted product poured into beaker, then add sodium alkyl benzene sulfonate (LAS) surfactant, gather
Isobutene (PIB) VI improver, the then oil bath heating at 100 DEG C, magnetic agitation 2h；
Step 10, reaction are handled after terminating with condensing tube condensation, are cooled to room temperature, are finally given containing nano oxidized thorium etc.
The material modified lubricating oil synthesized with vegetable oil.
Beneficial effect:A kind of preparation side containing the material modified use vegetable oil synthetic lubricant fluid such as nano oxidized thorium of the present invention
Method, introducing modified Nano thorium oxide has more excellent physical property to be squeezed lubricating oil in preparation process
When can disperse pressure to reduce pressure, frictional resistance is so as to improving anti-wear effect, then passes through and the processing such as be coupled
Various additives can be adsorbed onto together by enhancing suction-operated, and nano zine oxide can strengthen scattered by polarity active force
Active force can scatter so as to further reduce crushing strength to improve wear-resistant effect by effect when being squeezed, moreover it is possible to
Each material is uniformly distributed so as to which lubricant effect is improved, the work of additive can be given full play to when friction
With, then by adding to the modified method nitrogen such as diphenylamines and magnetic-ultrasonic, react further under the atmosphere such as carbon dioxide
Improve its anti-oxidant high temperature resistant antiwear ability.Wherein preparing nano thorium oxide, nano zine oxide 5:3 sample.It is nano oxidized
5 parts of thorium, 3 parts of nano zine oxide.100 parts of castor oil, acetic acid 20ml, 6 parts of ion exchange resin, hydrogen peroxide 30ml, active dioxy
5 parts of SiClx powder, to 1 part of diphenylamines, 0.4 part of DL171 types coupling agent, 0.3 part of sodium alkyl benzene sulfonate (LAS) surfactant gathers
0.2 part of isobutene (PIB) VI improver.And preparing nano thorium oxide, nano zine oxide 2:5 sample.It is nano oxidized
2 parts of thorium, 5 parts of nano zine oxide.100 parts of castor oil, acetic acid 20ml, 6 parts of ion exchange resin, hydrogen peroxide 30ml, active dioxy
5 parts of SiClx powder, to 1 part of diphenylamines, 0.4 part of DL171 types coupling agent, 0.3 part of sodium alkyl benzene sulfonate (LAS) surfactant gathers
0.2 part of isobutene (PIB) VI improver.It is obtained material modified with plant containing nano oxidized thorium etc. under both ratios
The wear-resistant effect of thing oil synthetic lubricant fluid is best.
Embodiment
The preparing nano thorium oxide of embodiment 1, nano zine oxide 5:3 sample.Nano oxidized 5 parts of thorium, 3 parts of nano zine oxide.
100 parts of castor oil, acetic acid 20ml, 6 parts of ion exchange resin, hydrogen peroxide 30ml, 5 parts of reactive silica silica flour, to diphenylamines 1
Part, 0.4 part of DL171 types coupling agent, 0.3 part of sodium alkyl benzene sulfonate (LAS) surfactant, polyisobutene (PIB) viscosity index (VI)
0.2 part of modifying agent.
Step 1,100 parts of castor oil of addition and 20ml acetic acid, 6 parts of cationic ion-exchange resins in 1000mL three-necked flasks,
Oil bath, which heats up and starts magnetic agitation, stirs (separately weighing 30ml hydrogen peroxide in separatory funnel).80 DEG C of constant temperature are warming up to, are heated up
During be slowly added dropwise hydrogen peroxide, control rate of addition is allowed to 3h or so and added, reaction 7h or so, stops magnetic agitation, stands
Aqueous phase is separated after layering, epoxy oil phase is obtained；
Step 2, the Epoxy oil obtained by reaction is warming up to 80 DEG C or so, adds 80 DEG C of temperature, the hydrogen-oxygen of mass fraction 5%
Change sodium solution, low speed magnetic agitation, while examining pH value, stop adding alkali lye during close to neutrality.Continue magnetic agitation 60min,
Aqueous phase is separated after stratification, 80 DEG C or so distillations is then added and washes 5-8 times, stand, separate aqueous phase；
Step 3, obtained oil phase handle 2h under ultrasonic wave, are then added thereto 5 parts of reactive silica silica flours, then
100 DEG C of oil baths, magnetic agitation 3h；
Step 4 and then the epoxy oil phase by above-mentioned use reactive silica Si modification, in 120kPa vacuums, 100 DEG C of oil baths
80~120min is dehydrated under heating condition, sample is taken out, obtains the base oil being made of vegetable oil；
Step 5 and then be added thereto 1 part to diphenylamines is modified, and microwave treatment 2h is carried out under nitrogen atmosphere, so
Afterwards in 100 DEG C of oil baths, magnetic agitation 3h；
Step 6,5 parts of nano oxidized thoriums are subjected to coupling processing modifications, 0.4 part of DL171 type coupling agent is added to nanometer
In thorium oxide, magnetic agitation 2h；
Step 7, the nano oxidized thorium being modified added in the base oil after modification, then in hot 180 DEG C of HCl gas
2h is handled under body, then neutrality is being washed to deionized water；
Step 8, nano zine oxide is added in the base oil of above-mentioned modification, then carries out reciprocating concussion processing
2h, is then being transferred in reactor, by 15kpa/min, 10 DEG C/min, and program mode is warming up to 150kpa, 100 DEG C,
3:Under 7 carbon dioxide and nitrogen atmosphere, 2h is then reacted；
Step 9, reacted product poured into beaker, then add 0.3 part of sodium alkyl benzene sulfonate (LAS) surface-active
Agent, 0.2 part of polyisobutene (PIB) VI improver, the then oil bath heating at 100 DEG C, magnetic agitation 2h；
Step 10, reaction are handled after terminating with condensing tube condensation, are cooled to room temperature, are finally given containing nano oxidized thorium etc.
The material modified lubricating oil synthesized with vegetable oil.
The preparing nano thorium oxide of embodiment 2, nano zine oxide 2:5 sample.Nano oxidized 2 parts of thorium, 5 parts of nano zine oxide.
Other raw material dosages, operating procedure is with embodiment 1.
The preparing nano thorium oxide of embodiment 3, nano zine oxide 1:1 sample.Nano oxidized 1 part of thorium, 1 part of nano zine oxide.
Other raw material dosages, operating procedure is with embodiment 1.
The preparing nano thorium oxide of embodiment 4, nano zine oxide 1:2 sample.Nano oxidized 1 part of thorium, 2 parts of nano zine oxide.
Other raw material dosages, operating procedure is with embodiment 1
The preparing nano thorium oxide of embodiment 5, nano zine oxide 1:3 sample.Nano oxidized 1 part of thorium, 3 parts of nano zine oxide.
Other raw material dosages, operating procedure is with embodiment 1
The preparing nano thorium oxide of embodiment 6, nano zine oxide 1:4 sample.Nano oxidized 1 part of thorium, 4 parts of nano zine oxide.
Other raw material dosages, operating procedure is with embodiment 1
The preparing nano thorium oxide of embodiment 7, nano zine oxide 1:5 sample.Nano oxidized 1 part of thorium, 5 parts of nano zine oxide.
Other raw material dosages, operating procedure is with embodiment 1
The preparing nano thorium oxide of embodiment 8, nano zine oxide 1:6 sample.Nano oxidized 1 part of thorium, 6 parts of nano zine oxide.
Other raw material dosages, operating procedure is with embodiment 1
The preparing nano thorium oxide of embodiment 9, nano zine oxide 1:7 sample.Nano oxidized 1 part of thorium, 7 parts of nano zine oxide.
Other raw material dosages, operating procedure is with embodiment 1
The preparing nano thorium oxide of embodiment 10, nano zine oxide 1:8 sample.Nano oxidized 1 part of thorium, 8 parts of nano zine oxide.
Other raw material dosages, operating procedure is with embodiment 1
The preparing nano thorium oxide of embodiment 11, nano zine oxide 2:1 sample.Nano oxidized 2 parts of thorium, 1 part of nano zine oxide.
Other raw material dosages, operating procedure is with embodiment 1
The preparing nano thorium oxide of embodiment 12, nano zine oxide 3:1 sample.Nano oxidized 3 parts of thorium, 1 part of nano zine oxide.
Other raw material dosages, operating procedure is with embodiment 1
The preparing nano thorium oxide of embodiment 13, nano zine oxide 4:1 sample.Nano oxidized 4 parts of thorium, 1 part of nano zine oxide.
Other raw material dosages, operating procedure is with embodiment 1
The preparing nano thorium oxide of embodiment 14, nano zine oxide 5:1 sample.Nano oxidized 5 parts of thorium, 1 part of nano zine oxide.
Other raw material dosages, operating procedure is with embodiment 1
The preparing nano thorium oxide of embodiment 15, nano zine oxide 6:1 sample.Nano oxidized 6 parts of thorium, 1 part of nano zine oxide.
Other raw material dosages, operating procedure is with embodiment 1
The preparing nano thorium oxide of embodiment 16, nano zine oxide 7:1 sample.Nano oxidized 7 parts of thorium, 1 part of nano zine oxide.
Other raw material dosages, operating procedure is with embodiment 1
The preparing nano thorium oxide of embodiment 17, nano zine oxide 8:1 sample.Nano oxidized 8 parts of thorium, 1 part of nano zine oxide.
Other raw material dosages, operating procedure is with embodiment 1
The preparing nano thorium oxide of reference examples 1, nano zine oxide 5:3 sample.Nano oxidized 5 parts of thorium, 3 parts of nano zine oxide.
Without dioxygen water process, other raw material dosages, operating procedure is with embodiment 1.
The preparing nano thorium oxide of reference examples 2, nano zine oxide 5:3 sample.Nano oxidized 5 parts of thorium, 3 parts of nano zine oxide.
Without ultrasonication, other raw material dosages, operating procedure is with embodiment 1.
The preparing nano thorium oxide of reference examples 3, nano zine oxide 5:3 sample.Nano oxidized 5 parts of thorium, 3 parts of nano zine oxide.
Without magnetic agitation, but mechanical agitation, other raw material dosages, operating procedure is with embodiment 1.
The preparing nano thorium oxide of reference examples 4, nano zine oxide 5:3 sample.Nano oxidized 5 parts of thorium, 3 parts of nano zine oxide.
Handled without reciprocating concussion, other raw material dosages, operating procedure is with embodiment 1.
The preparing nano thorium oxide of reference examples 5, nano zine oxide 5:3 sample.Nano oxidized 5 parts of thorium, 3 parts of nano zine oxide.
Without hot HCl gas treatments, other raw material dosages, operating procedure is with embodiment 1.
The preparing nano thorium oxide of reference examples 6, nano zine oxide 5:3 sample.Nano oxidized 5 parts of thorium, 3 parts of nano zine oxide.
Not 3:Reacted under 7 carbon dioxide and nitrogen atmosphere, but under air, other raw material dosages, operating procedure is with embodiment 1
Equally.
Reference examples 7 produce the sample for being added without nano oxidized thorium.Other raw material dosages, operating procedure is with embodiment 1.
Reference examples 8 produce the sample for being added without nano zine oxide.Other raw material dosages, operating procedure is with embodiment 1.
Reference examples 9, which are produced, is added without nano oxidized thorium, the sample of nano zine oxide.Other raw material dosages, operating procedure is with reality
As applying example 1.
Anti-wear performance is tested
Test method
Wear scar diameter is read by reading microscope.Type used in wear scar diameter is Jinan ensaying group production MR-H5A type machineries
The wearing resistance test machine when ball of formula four is long, experimental condition:Temperature is 75+2 DEG C, and speed is 1700+35r/mni, and load is 500N, when
Between be 60min, steel ball be Shanghai Steel Ball Plant produce four-ball tester special-purpose steel ball, material be part Cr4, by ANSI (steel ball association of the U.S.) mark
Quasi- steel No.E 1 is made, a diameter of φ 12.7mm, 64 1 66HRe, and grade is 25EP (ultraphotic).
Test procedure:
1. with washing gasoline or petrol ether carefully four experiment steel balls of cleaning, upper ball fixture, oil box and with experiment oil sample
The all parts of contact, are then dried up standby.Experiment steel ball after cleaning answers bright and clean without rust staining.
2. an experiment steel ball is attached in chuck, and chuck on main shaft.
3. three experiment steel balls are placed in oil box, and hold-down ring is placed on nut tightening above experiment steel ball, examination
Test oil sample to pour into oil box, it is submerged steel ball and more than top 3mm.
4. switch power supply, the adjustment speed of mainshaft to 1700+35r/min, dally 10 minutes or so, adjust timer.
5. oil box is placed on oil box seat, slowly imposed load is to 500N.
6. heat run oil sample is simultaneously adjusted to 75+2 DEG C.Under test temperature, the rotation of motor drive shaft is started.
7. test period reaches 60min, stop heating and turn off motor, remove load and take out oil box, experiment oil sample is fallen
Go out.
8. with the wear scar diameter being measured microscopically in oil box on three lower balls, measurement accuracy is 0.01mm, on each ball
Wear scar diameter is measured twice, once along oil box central ray direction, and another time vertical with first time.Reported in units of millimeter
The wear scar diameter arithmetic mean of instantaneous value of three steel balls, six measurements.Observation line during measurement should vertically grind spot surface.If mill spot is
One ellipse, then do one-shot measurement in polishing scratch direction, and another one-shot measurement is vertical with polishing scratch direction.
If 9. the average value measured twice of a lower ball is more than 0.04mm with six times all measurement average values, answered
The axle center centering situation of ball and oil box in the inspection.
Each oil product prepared is done into above-mentioned experiment respectively.
The wear scar diameter measurement result of table one
Test result indicates that：It can be found that embodiment 1,2 prepare use vegetable oil containing nano oxidized thorium etc. is material modified
Synthetic lubricant fluid anti-wear effect preferably, illustrates preparing nano thorium oxide, nano zine oxide 5:3,2:5 sample, internal each several part it
Between the best wear-resistant best results of synergy.It is obtained under other ratios to use plant containing nano oxidized thorium etc. is material modified
The oily wear-resistant effect of synthetic lubricant fluid is general.Comparative example 1, comparative example 1,2,3,4,5,6 is can be found that.Without dioxygen
Water, ultrasonic wave, magnetic agitation, reciprocating concussion, hot HCl gas treatments, not 3:It is anti-under 7 carbon dioxide and nitrogen atmosphere
Should, but wait operation is obtained to contain the material modified wear-resistant effects of use vegetable oil synthetic lubricant fluid such as nano oxidized thorium under air
It is really bad.Comparative example 1, comparative example 7,8,9 are it can be found that is added without nano oxidized thorium, nano zine oxide or both not
It is bad that the obtained lubrication oil antiwear of addition damages effect.
Claims (4)
1. a kind of preparation method of the vegetable oil based lubricating oil containing nano modified material, it is characterised in that utilize castor oil, receive
Rice thorium oxide, nano zine oxide, surfactant sodium stearyl sulfate, the raw material such as ion exchange resin passes through acid treatment, even
Join, magnetic agitation, the modified method such as microwave treatment is prepared to be lubricated containing material modified synthesized with vegetable oil such as nanometer thorium nitrate
Oil.
2. a kind of preparation method of vegetable oil based lubricating oil containing nano modified material according to claim 1, it is special
Levy and be, preparation method is as follows：
Step 1, castor oil and acetic acid, cationic ion-exchange resin are being added, oil bath heat up and starts magnetic agitation and stir, separately weighs
Hydrogen peroxide is warming up in 80 DEG C of constant temperature, temperature-rise period after hydrogen peroxide reaction, stratification is slowly added dropwise and separated in separatory funnel
Aqueous phase, obtains epoxy oil phase；
Step 2, the Epoxy oil obtained by reaction is warming up to 80 DEG C or so, adds 80 DEG C of temperature, the sodium hydroxide of mass fraction 5%
Solution, stirring while examining pH value, stops adding alkali lye during close to neutrality, continues to separate water after stirring 60min, stratification
Phase, then adds 80 DEG C or so distillations and washes 5-8 times, stand, separate aqueous phase；
Step 3, obtained oil phase are handled under ultrasonic wave, are then added thereto reactive silica silica flour, then 100 DEG C of oil
Bath, stirring；
Step 4 and then the epoxy oil phase by above-mentioned use reactive silica Si modification, in 120kPa vacuums, 100 DEG C of oil bath heatings
Under the conditions of be dehydrated 80~120min, take out sample, obtain the base oil being made of vegetable oil；
Step 5 and then will be added thereto to diphenylamines is modified, and microwave treatment is carried out under nitrogen atmosphere, then at 100 DEG C
Oil bath, stirring；
Step 6, by nano oxidized thorium carry out coupling processing modification, DL171 type coupling agents are added in nano oxidized thorium, stirred
Mix；
Step 7, by the nano oxidized thorium being modified add modification after base oil in, then under HCl gases handle, so
Afterwards neutrality is being washed to deionized water；
Step 8, nano zine oxide is added in the base oil of above-mentioned modification, then carries out reciprocating concussion processing, so
It is being transferred in reactor, under carbon dioxide and nitrogen atmosphere, is then reacting afterwards；
Step 9, reacted product poured into beaker, then add sodium alkyl benzene sulfonate (LAS) surfactant, poly- isobutyl
Alkene (PIB) VI improver, then oil bath heating, magnetic agitation；
Step 10, reaction are handled after terminating with condensing tube condensation, cool to room temperature, are finally given modified containing nano oxidized thorium etc.
The lubricating oil that material is synthesized with vegetable oil.
3. a kind of preparation method of vegetable oil based lubricating oil containing nano modified material according to claim 1, it is special
Levy and be, in described step 8, carbon dioxide and nitrogen ratios are 3:7.
4. a kind of preparation method of vegetable oil based lubricating oil containing nano modified material according to claim 1, it is special
Levy and be, the stirring in step 2,3,5,6 is magnetic agitation.
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| CN110776973A (en) * | 2019-10-29 | 2020-02-11 | 中国科学院兰州化学物理研究所 | Amine nano lubricating oil additive and application thereof |
| CN113583741A (en) * | 2021-07-20 | 2021-11-02 | 广东月福汽车用品有限公司 | Brake anti-occlusion lubricant and preparation method and application thereof |
| CN115651739A (en) * | 2022-10-08 | 2023-01-31 | 余洲芳 | Degradable long-acting lubricating oil and preparation method thereof |
| CN118650155A (en) * | 2024-07-08 | 2024-09-17 | 常州市知宇粉末冶金有限公司 | A powder metallurgy oil-containing bearing and a preparation method thereof |
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