CN118006384A - Antistatic hydraulic oil - Google Patents
Antistatic hydraulic oil Download PDFInfo
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- CN118006384A CN118006384A CN202410410804.2A CN202410410804A CN118006384A CN 118006384 A CN118006384 A CN 118006384A CN 202410410804 A CN202410410804 A CN 202410410804A CN 118006384 A CN118006384 A CN 118006384A
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- Prior art keywords
- antistatic
- hydraulic oil
- oleic acid
- trimethylolpropane
- stirring
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- 239000010720 hydraulic oil Substances 0.000 title claims abstract description 58
- 239000000654 additive Substances 0.000 claims abstract description 54
- 230000000996 additive effect Effects 0.000 claims abstract description 54
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims abstract description 44
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims abstract description 44
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims abstract description 44
- 239000005642 Oleic acid Substances 0.000 claims abstract description 44
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims abstract description 44
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims abstract description 44
- 239000004721 Polyphenylene oxide Substances 0.000 claims abstract description 43
- 229920000570 polyether Polymers 0.000 claims abstract description 43
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims abstract description 42
- 239000002199 base oil Substances 0.000 claims abstract description 38
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 34
- FMNZBNCPTJEVDS-KVVVOXFISA-N 2-ethyl-2-(hydroxymethyl)propane-1,3-diol;(z)-octadec-9-enoic acid Chemical compound CCC(CO)(CO)CO.CCCCCCCC\C=C/CCCCCCCC(O)=O FMNZBNCPTJEVDS-KVVVOXFISA-N 0.000 claims abstract description 30
- 239000002131 composite material Substances 0.000 claims abstract description 29
- 229910019142 PO4 Inorganic materials 0.000 claims abstract description 26
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims abstract description 26
- 239000010452 phosphate Substances 0.000 claims abstract description 26
- DLYUQMMRRRQYAE-UHFFFAOYSA-N tetraphosphorus decaoxide Chemical compound O1P(O2)(=O)OP3(=O)OP1(=O)OP2(=O)O3 DLYUQMMRRRQYAE-UHFFFAOYSA-N 0.000 claims abstract description 24
- ZJCCRDAZUWHFQH-UHFFFAOYSA-N Trimethylolpropane Chemical compound CCC(CO)(CO)CO ZJCCRDAZUWHFQH-UHFFFAOYSA-N 0.000 claims abstract description 17
- RVGRUAULSDPKGF-UHFFFAOYSA-N Poloxamer Chemical compound C1CO1.CC1CO1 RVGRUAULSDPKGF-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 12
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 12
- 239000013556 antirust agent Substances 0.000 claims abstract description 12
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 12
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 12
- 239000006078 metal deactivator Substances 0.000 claims abstract description 12
- QGLWBTPVKHMVHM-KTKRTIGZSA-N (z)-octadec-9-en-1-amine Chemical compound CCCCCCCC\C=C/CCCCCCCCN QGLWBTPVKHMVHM-KTKRTIGZSA-N 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims description 45
- 238000002360 preparation method Methods 0.000 claims description 33
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 30
- 238000009210 therapy by ultrasound Methods 0.000 claims description 30
- 238000010438 heat treatment Methods 0.000 claims description 25
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 24
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 20
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 15
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 238000006243 chemical reaction Methods 0.000 claims description 15
- 239000000203 mixture Substances 0.000 claims description 15
- 239000003921 oil Substances 0.000 claims description 14
- -1 alkyl diphenylamine Chemical compound 0.000 claims description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 claims description 10
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 claims description 10
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical compound CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 claims description 10
- 239000003054 catalyst Substances 0.000 claims description 10
- 239000003112 inhibitor Substances 0.000 claims description 10
- 238000000199 molecular distillation Methods 0.000 claims description 10
- 239000003208 petroleum Substances 0.000 claims description 10
- 238000007670 refining Methods 0.000 claims description 10
- 238000005303 weighing Methods 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 6
- UGUHFDPGDQDVGX-UHFFFAOYSA-N 1,2,3-thiadiazole Chemical group C1=CSN=N1 UGUHFDPGDQDVGX-UHFFFAOYSA-N 0.000 claims description 5
- QIGBRXMKCJKVMJ-UHFFFAOYSA-N 1,4-Benzenediol Natural products OC1=CC=C(O)C=C1 QIGBRXMKCJKVMJ-UHFFFAOYSA-N 0.000 claims description 5
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 239000012295 chemical reaction liquid Substances 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 150000002148 esters Chemical class 0.000 claims description 5
- 239000000706 filtrate Substances 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- 125000000687 hydroquinonyl group Chemical group C1(O)=C(C=C(O)C=C1)* 0.000 claims description 5
- 229910052740 iodine Inorganic materials 0.000 claims description 5
- 239000011630 iodine Substances 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims description 5
- 239000012528 membrane Substances 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- IYDGMDWEHDFVQI-UHFFFAOYSA-N phosphoric acid;trioxotungsten Chemical group O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.OP(O)(O)=O IYDGMDWEHDFVQI-UHFFFAOYSA-N 0.000 claims description 5
- 238000004321 preservation Methods 0.000 claims description 5
- 238000000967 suction filtration Methods 0.000 claims description 5
- 238000001291 vacuum drying Methods 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- DMBHHRLKUKUOEG-UHFFFAOYSA-N N-phenyl aniline Natural products C=1C=CC=CC=1NC1=CC=CC=C1 DMBHHRLKUKUOEG-UHFFFAOYSA-N 0.000 claims description 3
- QQVGEJLUEOSDBB-KTKRTIGZSA-N [3-hydroxy-2,2-bis(hydroxymethyl)propyl] (z)-octadec-9-enoate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OCC(CO)(CO)CO QQVGEJLUEOSDBB-KTKRTIGZSA-N 0.000 claims description 3
- 150000001336 alkenes Chemical class 0.000 claims description 3
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 claims description 3
- RYYWUUFWQRZTIU-UHFFFAOYSA-K thiophosphate Chemical compound [O-]P([O-])([O-])=S RYYWUUFWQRZTIU-UHFFFAOYSA-K 0.000 claims description 3
- IVTHSFJXIARUFL-UHFFFAOYSA-N triazanium;thiophosphate Chemical compound [NH4+].[NH4+].[NH4+].[O-]P([O-])([O-])=S IVTHSFJXIARUFL-UHFFFAOYSA-N 0.000 claims description 3
- MUHFRORXWCGZGE-KTKRTIGZSA-N 2-hydroxyethyl (z)-octadec-9-enoate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OCCO MUHFRORXWCGZGE-KTKRTIGZSA-N 0.000 claims 1
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 claims 1
- 229940095098 glycol oleate Drugs 0.000 claims 1
- 239000002994 raw material Substances 0.000 abstract description 4
- 230000003647 oxidation Effects 0.000 abstract description 3
- 238000007254 oxidation reaction Methods 0.000 abstract description 3
- 230000000052 comparative effect Effects 0.000 description 18
- 230000005611 electricity Effects 0.000 description 5
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 5
- 230000003068 static effect Effects 0.000 description 5
- 230000007547 defect Effects 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000009825 accumulation Methods 0.000 description 1
- 125000005037 alkyl phenyl group Chemical group 0.000 description 1
- 239000007866 anti-wear additive Substances 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 229910003002 lithium salt Inorganic materials 0.000 description 1
- 159000000002 lithium salts Chemical class 0.000 description 1
- 230000001050 lubricating effect Effects 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 150000004867 thiadiazoles Chemical class 0.000 description 1
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- Lubricants (AREA)
Abstract
The invention relates to the technical field of hydraulic oil development, in particular to antistatic hydraulic oil, wherein trimethylolpropane oleate prepared by taking trimethylolpropane and self-made oleic acid as raw materials is used as base oil of the hydraulic oil, so that the oxidation resistance of the hydraulic oil can be enhanced, and graphene modified by oleylamine is added to ensure that the prepared hydraulic oil has excellent wear resistance and extreme pressure resistance; secondly, the polyether phosphate antistatic component prepared by taking the prepared ethylene oxide propylene oxide block polyether and phosphorus pentoxide as raw materials has excellent antistatic performance, and the polyether phosphate antistatic component is taken as a main antistatic additive component to be added into base oil, so that the antistatic performance of the prepared hydraulic oil can be obviously improved; finally, the antiwear agent, the antioxidant, the antirust agent, the metal deactivator, the demulsifier and the trimethylolpropane oleate base oil are mixed to prepare the composite additive, and then the composite additive is added into the base oil, so that the performance of the prepared hydraulic oil can be improved.
Description
Technical Field
The invention relates to the technical field of hydraulic oil development, in particular to antistatic hydraulic oil.
Background
With the continuous development of industrial technology, the performance requirements of hydraulic oil serving as an important medium in industrial equipment are increasingly strict, particularly under certain special working environments such as high temperature, high pressure, high humidity and the like, the antistatic performance of the hydraulic oil is particularly important, and the accumulation of static electricity can not only lead to equipment failure, but also cause safety accidents such as fire and explosion, so that the development of the hydraulic oil with excellent antistatic performance is an urgent need in the current industrial field. Although the traditional hydraulic oil can meet the lubricating and sealing requirements of equipment to a certain extent, the traditional hydraulic oil has obvious defects in the aspect of antistatic performance, and in the process of static electricity generation, the traditional hydraulic oil often cannot effectively lead out or dissipate static electricity, so that the static electricity is accumulated in the equipment, and the risk of equipment failure is increased.
The low-setting antistatic anti-wear hydraulic oil disclosed in the patent application with the publication number of CN108441295A is prepared by compounding the first type oil and the second type oil according to a strict proportion, and adding the lithium salt anti-wear additive with good conductivity and more metal ions, so that the quality of the oil product is ensured, the conductivity of the oil product is improved, and the generation of static electricity is avoided. The invention only adds the existing additive with antistatic property into the base oil by mixing, and does not improve the property of the base oil, so that the invention needs to be improved on the basis.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention provides antistatic hydraulic oil, which can effectively solve the problems of poor antistatic performance, oxidation resistance and wear resistance of the hydraulic oil in the prior art.
In order to achieve the above purpose, the invention is realized by the following technical scheme:
An antistatic hydraulic oil, the composition of which comprises: trimethylolpropane oleate base oil, modified graphene additive component, polyether phosphate antistatic component and composite additive;
the preparation method of the antistatic hydraulic oil comprises the following steps: 90 parts of trimethylolpropane oleate base oil, 0.01 part of modified graphene additive component, 0.5 part of polyether phosphate antistatic component and 0.7 part of composite additive are weighed according to parts by weight, added into a reaction kettle, and stirred for 4-5 hours at 58-65 ℃ at a stirring speed of 100r/min, thus obtaining the antistatic hydraulic oil.
Further, the preparation steps of the trimethylolpropane oleate base oil are as follows:
Step one, according to 1:3, weighing the calculated amount of trimethylolpropane and self-made oleic acid according to the molar ratio, pouring the calculated amount of trimethylolpropane and self-made oleic acid into a flask, adding a catalyst accounting for 4% of the total weight of the trimethylolpropane and the self-made oleic acid, an inhibitor accounting for 0.08% and an entrainer accounting for 40%, and marking the mixture as a mixed system;
Heating the oil bath of the mixed system to 80-82 ℃, then carrying out heat preservation reaction for 6-8h, filtering, separating and refining the crude ester by molecular distillation, and separating unreacted oleic acid to obtain the trimethylolpropane oleate base oil.
Further, in the first step, the preparation method of self-made oleic acid comprises the following steps: according to 3:1:1, weighing and mixing calculated amount of oleic acid, maleic anhydride and methyl acrylate according to the molar ratio, stirring for 5min at the stirring speed of 150r/min, adding elemental iodine with the weight of 2% of that of the oleic acid, heating to 200 ℃, reacting for 3h, naturally cooling, and separating and refining by molecular distillation to obtain self-made oleic acid.
Further, in the first step, the catalyst is phosphotungstic acid, the inhibitor is hydroquinone, and the entrainer is petroleum ether.
Further, the preparation steps of the modified graphene additive component are as follows:
step I, according to 1: dispersing graphene in N, N-dimethylformamide in a solid-liquid ratio of 500g/mL, adjusting the pH value to 8-10 after primary ultrasonic treatment, dripping oleylamine with a weight half that of the graphene, performing ultrasonic treatment again, and then reacting for 6 hours at the temperature of 80 ℃ under the protection of nitrogen;
and II, carrying out suction filtration on the reaction liquid in the step I, sequentially washing a filter membrane by using N, N-dimethylformamide, absolute ethyl alcohol and petroleum ether after removing filtrate, and carrying out vacuum drying at the temperature of 60 ℃ for 12 hours to obtain the modified graphene additive component.
Further, in the step I, the frequency of the primary ultrasonic treatment is 22-23kHz, the time of the primary ultrasonic treatment is 30min, the pH value is adjusted by using a sodium hydroxide solution with the concentration of 1.0mol/L, the frequency of the secondary ultrasonic treatment is 22-23kHz, and the time of the secondary ultrasonic treatment is 15min.
Further, the preparation steps of the polyether phosphate antistatic component are as follows:
step 1, pouring 2mL of ethylene glycol and 0.1g of potassium hydroxide into a flask, heating an oil bath to 100 ℃, sequentially dripping 20g of ethylene oxide and 22g of propylene oxide, and recording the mixture as ethylene oxide propylene oxide block polyether after the dripping is completed;
And 2, adding ethylene oxide and propylene oxide block polyether into the flask, heating to 45-48 ℃ under stirring, then adding phosphorus pentoxide in 3 times, stirring and reacting for 3 hours under constant temperature condition of 65-68 ℃, and obtaining the antistatic component of the polyether phosphate.
Further, in step 2, the feeding mole ratio of the ethylene oxide propylene oxide block polyether to the phosphorus pentoxide is 3:1, the stirring speeds are 200r/min.
Further, the preparation method of the composite additive comprises the following steps: adding 60% of antiwear agent, 20% of antioxidant, 6% of antirust agent, 3% of metal deactivator, 0.5% of demulsifier and 10.5% of trimethylolpropane oleate base oil into a reaction kettle according to weight percentage, stirring and heating to 50-70 ℃ at a stirring speed of 150r/min, and continuously stirring for 5-6h at a temperature of 50-70 ℃ to obtain the composite additive.
Further, in the preparation method of the composite additive, the antiwear agent is one of phosphorothioate, ammonium phosphorothioate and sulfurized olefin, the antioxidant is one of alkyl diphenylamine and alkyl phenylpropionate, the antirust agent is one of alkene butyl diacid, oleic acid glycol ester and pentaerythritol monooleate, the metal deactivator is a thiadiazole derivative, and the demulsifier is ethylene glycol ester.
Compared with the prior art, the invention has the following beneficial effects:
According to the invention, the trimethylolpropane oleate prepared by taking trimethylolpropane and self-made oleic acid as raw materials is used as the base oil of the hydraulic oil, so that the oxidation resistance of the hydraulic oil can be enhanced, and the prepared hydraulic oil has excellent anti-wear performance and extreme pressure performance by adding the graphene modified by the oleylamine; secondly, the polyether phosphate antistatic component prepared by taking the prepared ethylene oxide propylene oxide block polyether and phosphorus pentoxide as raw materials has excellent antistatic performance, and the polyether phosphate antistatic component is taken as a main antistatic additive component to be added into base oil, so that the antistatic performance of the prepared hydraulic oil can be obviously improved; finally, the antiwear agent, the antioxidant, the antirust agent, the metal deactivator, the demulsifier and the trimethylolpropane oleate base oil are mixed to prepare the composite additive, and then the composite additive is added into the base oil, so that the auxiliary agent can be dispersed in the base oil more uniformly, and the performance of the prepared hydraulic oil is improved.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be clearly and completely described below. It will be apparent that the described embodiments are some, but not all, embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The invention is further described below with reference to examples.
Example 1
The composition of the antistatic hydraulic oil in this embodiment includes: trimethylolpropane oleate base oil, modified graphene additive component, polyether phosphate antistatic component and composite additive;
The preparation method of the antistatic hydraulic oil comprises the following steps: 90 parts of trimethylolpropane oleate base oil, 0.01 part of modified graphene additive component, 0.5 part of polyether phosphate antistatic component and 0.7 part of composite additive are weighed according to parts by weight, added into a reaction kettle, and stirred for 4 hours at 58 ℃ at a stirring speed of 100r/min, thus obtaining the antistatic hydraulic oil.
The preparation method of the trimethylolpropane oleate base oil comprises the following steps:
Step one, according to 1:3, weighing the calculated amount of trimethylolpropane and self-made oleic acid according to the molar ratio, pouring the calculated amount of trimethylolpropane and self-made oleic acid into a flask, adding a catalyst accounting for 4% of the total weight of the trimethylolpropane and the self-made oleic acid, an inhibitor accounting for 0.08% and an entrainer accounting for 40%, and marking the mixture as a mixed system;
Heating the oil bath of the mixed system to 80 ℃, then carrying out heat preservation reaction for 6 hours, filtering, separating and refining the crude ester by molecular distillation, and separating unreacted oleic acid to obtain the trimethylolpropane oleate base oil.
In the first step, the preparation method of self-made oleic acid comprises the following steps: according to 3:1:1, weighing and mixing calculated amount of oleic acid, maleic anhydride and methyl acrylate according to the molar ratio, stirring for 5min at the stirring speed of 150r/min, adding elemental iodine with the weight of 2% of that of the oleic acid, heating to 200 ℃, reacting for 3h, naturally cooling, and separating and refining by molecular distillation to obtain self-made oleic acid.
In the first step, the catalyst is phosphotungstic acid, the inhibitor is hydroquinone, and the entrainer is petroleum ether.
The preparation steps of the modified graphene additive component are as follows:
Step I, according to 1: dispersing graphene in N, N-dimethylformamide in a solid-liquid ratio of 500g/mL, adjusting the pH value to 8 after primary ultrasonic treatment, dripping oleylamine with a weight half that of the graphene, carrying out ultrasonic treatment again, and then reacting for 6 hours at the temperature of 80 ℃ under the protection of nitrogen;
and II, carrying out suction filtration on the reaction liquid in the step I, sequentially washing a filter membrane by using N, N-dimethylformamide, absolute ethyl alcohol and petroleum ether after removing filtrate, and carrying out vacuum drying at the temperature of 60 ℃ for 12 hours to obtain the modified graphene additive component.
In the step I, the frequency of the primary ultrasonic treatment is 22kHz, the time of the primary ultrasonic treatment is 30min, the pH value is adjusted by using a sodium hydroxide solution with the concentration of 1.0mol/L, the frequency of the secondary ultrasonic treatment is 22kHz, and the time of the secondary ultrasonic treatment is 15min.
The preparation steps of the polyether phosphate antistatic component are as follows:
step 1, pouring 2mL of ethylene glycol and 0.1g of potassium hydroxide into a flask, heating an oil bath to 100 ℃, sequentially dripping 20g of ethylene oxide and 22g of propylene oxide, and recording the mixture as ethylene oxide propylene oxide block polyether after the dripping is completed;
and 2, adding ethylene oxide and propylene oxide block polyether into the flask, heating to 45 ℃ under stirring, then adding phosphorus pentoxide in 3 times, stirring and reacting for 3 hours under constant temperature at 65 ℃, and obtaining the antistatic component marked as polyether phosphate.
In the step 2, the feeding mole ratio of the ethylene oxide propylene oxide block polyether to the phosphorus pentoxide is 3:1, the stirring speeds are 200r/min.
The preparation method of the composite additive comprises the following steps: adding 60% of antiwear agent, 20% of antioxidant, 6% of antirust agent, 3% of metal deactivator, 0.5% of demulsifier and 10.5% of trimethylolpropane oleate base oil into a reaction kettle according to weight percentage, stirring and heating to 50 ℃ at a stirring speed of 150r/min, and continuously stirring for 5 hours at a temperature of 50 ℃ to obtain the composite additive.
In the preparation method of the composite additive, the antiwear agent is phosphorothioate, the antioxidant is alkyl diphenylamine, the antirust agent is alkene butyl diacid, the metal deactivator is thiadiazole derivative, and the demulsifier is glycol ester.
Example 2
The composition of the antistatic hydraulic oil in this embodiment includes: trimethylolpropane oleate base oil, modified graphene additive component, polyether phosphate antistatic component and composite additive;
the preparation method of the antistatic hydraulic oil comprises the following steps: 90 parts of trimethylolpropane oleate base oil, 0.01 part of modified graphene additive component, 0.5 part of polyether phosphate antistatic component and 0.7 part of composite additive are weighed according to parts by weight, added into a reaction kettle, and stirred for 5 hours at the temperature of 65 ℃ at the stirring speed of 100r/min, thus obtaining the antistatic hydraulic oil.
The preparation method of the trimethylolpropane oleate base oil comprises the following steps:
Step one, according to 1:3, weighing the calculated amount of trimethylolpropane and self-made oleic acid according to the molar ratio, pouring the calculated amount of trimethylolpropane and self-made oleic acid into a flask, adding a catalyst accounting for 4% of the total weight of the trimethylolpropane and the self-made oleic acid, an inhibitor accounting for 0.08% and an entrainer accounting for 40%, and marking the mixture as a mixed system;
Heating the oil bath of the mixed system to 82 ℃, then carrying out heat preservation reaction for 8 hours, filtering, separating and refining the crude ester by molecular distillation, and separating unreacted oleic acid to obtain the trimethylolpropane oleate base oil.
In the first step, the preparation method of self-made oleic acid comprises the following steps: according to 3:1:1, weighing and mixing calculated amount of oleic acid, maleic anhydride and methyl acrylate according to the molar ratio, stirring for 5min at the stirring speed of 150r/min, adding elemental iodine with the weight of 2% of that of the oleic acid, heating to 200 ℃, reacting for 3h, naturally cooling, and separating and refining by molecular distillation to obtain self-made oleic acid.
In the first step, the catalyst is phosphotungstic acid, the inhibitor is hydroquinone, and the entrainer is petroleum ether.
The preparation steps of the modified graphene additive component are as follows:
Step I, according to 1: dispersing graphene in N, N-dimethylformamide in a solid-liquid ratio of 500g/mL, adjusting the pH value to 10 after primary ultrasonic treatment, dripping oleylamine with a weight half that of the graphene, carrying out ultrasonic treatment again, and then reacting for 6 hours at the temperature of 80 ℃ under the protection of nitrogen;
and II, carrying out suction filtration on the reaction liquid in the step I, sequentially washing a filter membrane by using N, N-dimethylformamide, absolute ethyl alcohol and petroleum ether after removing filtrate, and carrying out vacuum drying at the temperature of 60 ℃ for 12 hours to obtain the modified graphene additive component.
In the step I, the frequency of the primary ultrasonic treatment is 23kHz, the time of the primary ultrasonic treatment is 30min, the pH value is adjusted by using a sodium hydroxide solution with the concentration of 1.0mol/L, the frequency of the secondary ultrasonic treatment is 23kHz, and the time of the secondary ultrasonic treatment is 15min.
The preparation steps of the polyether phosphate antistatic component are as follows:
step 1, pouring 2mL of ethylene glycol and 0.1g of potassium hydroxide into a flask, heating an oil bath to 100 ℃, sequentially dripping 20g of ethylene oxide and 22g of propylene oxide, and recording the mixture as ethylene oxide propylene oxide block polyether after the dripping is completed;
And 2, adding ethylene oxide and propylene oxide block polyether into the flask, heating to 48 ℃ under stirring, then adding phosphorus pentoxide in 3 times, stirring and reacting for 3 hours under the constant temperature condition of 68 ℃, and obtaining the antistatic component of the polyether phosphate.
In the step 2, the feeding mole ratio of the ethylene oxide propylene oxide block polyether to the phosphorus pentoxide is 3:1, the stirring speeds are 200r/min.
The preparation method of the composite additive comprises the following steps: adding 60% of antiwear agent, 20% of antioxidant, 6% of antirust agent, 3% of metal deactivator, 0.5% of demulsifier and 10.5% of trimethylolpropane oleate base oil into a reaction kettle according to weight percentage, stirring and heating to 70 ℃ at a stirring speed of 150r/min, and continuously stirring at the temperature of 70 ℃ for 6 hours to obtain the composite additive.
In the preparation method of the composite additive, the antiwear agent is sulfurized olefin, the antioxidant is alkylphenyl propionate, the antirust agent is pentaerythritol monooleate, the metal deactivator is thiadiazole derivative, and the demulsifier is glycol ester.
Example 3
The composition of the antistatic hydraulic oil in this embodiment includes: trimethylolpropane oleate base oil, modified graphene additive component, polyether phosphate antistatic component and composite additive;
The preparation method of the antistatic hydraulic oil comprises the following steps: 90 parts of trimethylolpropane oleate base oil, 0.01 part of modified graphene additive component, 0.5 part of polyether phosphate antistatic component and 0.7 part of composite additive are weighed according to parts by weight, added into a reaction kettle, and stirred for 5 hours at the temperature of 62 ℃ at the stirring speed of 100r/min, thus obtaining the antistatic hydraulic oil.
The preparation method of the trimethylolpropane oleate base oil comprises the following steps:
Step one, according to 1:3, weighing the calculated amount of trimethylolpropane and self-made oleic acid according to the molar ratio, pouring the calculated amount of trimethylolpropane and self-made oleic acid into a flask, adding a catalyst accounting for 4% of the total weight of the trimethylolpropane and the self-made oleic acid, an inhibitor accounting for 0.08% and an entrainer accounting for 40%, and marking the mixture as a mixed system;
heating the oil bath of the mixed system to 81 ℃, then carrying out heat preservation reaction for 7 hours, filtering, separating and refining the crude ester by molecular distillation, and separating unreacted oleic acid to obtain the trimethylolpropane oleate base oil.
In the first step, the preparation method of self-made oleic acid comprises the following steps: according to 3:1:1, weighing and mixing calculated amount of oleic acid, maleic anhydride and methyl acrylate according to the molar ratio, stirring for 5min at the stirring speed of 150r/min, adding elemental iodine with the weight of 2% of that of the oleic acid, heating to 200 ℃, reacting for 3h, naturally cooling, and separating and refining by molecular distillation to obtain self-made oleic acid.
In the first step, the catalyst is phosphotungstic acid, the inhibitor is hydroquinone, and the entrainer is petroleum ether.
The preparation steps of the modified graphene additive component are as follows:
step I, according to 1: dispersing graphene in N, N-dimethylformamide in a solid-liquid ratio of 500g/mL, adjusting the pH value to 9 after primary ultrasonic treatment, dripping oleylamine with a weight half that of the graphene, carrying out ultrasonic treatment again, and then reacting for 6 hours at the temperature of 80 ℃ under the protection of nitrogen;
and II, carrying out suction filtration on the reaction liquid in the step I, sequentially washing a filter membrane by using N, N-dimethylformamide, absolute ethyl alcohol and petroleum ether after removing filtrate, and carrying out vacuum drying at the temperature of 60 ℃ for 12 hours to obtain the modified graphene additive component.
In the step I, the frequency of the primary ultrasonic treatment is 23kHz, the time of the primary ultrasonic treatment is 30min, the pH value is adjusted by using a sodium hydroxide solution with the concentration of 1.0mol/L, the frequency of the secondary ultrasonic treatment is 23kHz, and the time of the secondary ultrasonic treatment is 15min.
The preparation steps of the polyether phosphate antistatic component are as follows:
step 1, pouring 2mL of ethylene glycol and 0.1g of potassium hydroxide into a flask, heating an oil bath to 100 ℃, sequentially dripping 20g of ethylene oxide and 22g of propylene oxide, and recording the mixture as ethylene oxide propylene oxide block polyether after the dripping is completed;
And 2, adding ethylene oxide and propylene oxide block polyether into the flask, heating to 47 ℃ under stirring, then adding phosphorus pentoxide in 3 times, stirring and reacting for 3 hours under constant temperature at 67 ℃, and obtaining the polyether phosphate antistatic component.
In the step 2, the feeding mole ratio of the ethylene oxide propylene oxide block polyether to the phosphorus pentoxide is 3:1, the stirring speeds are 200r/min.
The preparation method of the composite additive comprises the following steps: adding 60% of antiwear agent, 20% of antioxidant, 6% of antirust agent, 3% of metal deactivator, 0.5% of demulsifier and 10.5% of trimethylolpropane oleate base oil into a reaction kettle according to weight percentage, stirring and heating to 60 ℃ at a stirring speed of 150r/min, and continuously stirring at the temperature of 60 ℃ for 6 hours to obtain the composite additive.
In the preparation method of the composite additive, the antiwear agent is ammonium thiophosphate, the antioxidant is alkyl phenyl propionate, the antirust agent is oleic acid glycol ester, the metal deactivator is thiadiazole derivative, and the demulsifier is glycol ester.
Comparative example 1
An antistatic hydraulic oil provided in this comparative example is substantially the same as that of example 1, with the main difference that: comparative example 1 the trimethylolpropane oleate base oil of example 1 was replaced with a commercially available base oil of model CTL.
Comparative example 2
An antistatic hydraulic oil provided in this comparative example is substantially the same as that of example 1, with the main difference that: this comparative example 2 replaces the modified graphene additive component in example 1 with unmodified nanographene.
Comparative example 3
An antistatic hydraulic oil provided in this comparative example is substantially the same as that of example 1, with the main difference that: this comparative example 3 replaces the polyether phosphate antistatic component of example 1 with a thiadiazole derivative.
Performance testing
The antistatic hydraulic oils in examples 1 to 3 and comparative examples 1 to 3 were respectively labeled as example 1, example 2, example 3, comparative example 1, comparative example 2 and comparative example 3, and then the properties of examples 1 to 3 and comparative examples 1 to 3 were examined, and the obtained data are recorded in the following table:
detection performance record table
| Detecting items | Kinematic viscosity (40 ℃ C.)/(mm 2/s) | Shear stability (rate of decrease in kinematic viscosity at 40 ℃ after 250 cycles)/% | Air release value (50 ℃ C.)/(min) |
| Detection method | GB/T 265 | SH/T 0103 | SH/T 0308 |
| Example 1 | 47.8 | 0.1 | 5 |
| Example 2 | 47.9 | 0.1 | 5 |
| Example 3 | 48.6 | 0.1 | 6 |
| Comparative example 1 | 39.5 | 0.2 | 8 |
| Comparative example 2 | 42.3 | 0.3 | 8 |
| Comparative example 3 | 45.7 | 0.2 | 7 |
As is evident from the data in the above table, the viscosity decrease rate of the antistatic hydraulic oil in the present examples 1 to 3 was lower than that of the comparative examples 1 to 3, indicating that the stability of the antistatic hydraulic oil in the present examples 1 to 3 was higher. In addition, the modified graphene additive component and the polyether phosphate antistatic component added in the antistatic hydraulic oil in the embodiment 1-3 can play a role in better antistatic and extreme pressure resistance, so that the antistatic hydraulic oil has an excellent market application prospect.
The above embodiments are only for illustrating the technical solution of the present invention, and are not limiting; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present invention.
Claims (10)
1. An antistatic hydraulic oil, characterized in that the composition of the antistatic hydraulic oil comprises: trimethylolpropane oleate base oil, modified graphene additive component, polyether phosphate antistatic component and composite additive;
the preparation method of the antistatic hydraulic oil comprises the following steps: 90 parts of trimethylolpropane oleate base oil, 0.01 part of modified graphene additive component, 0.5 part of polyether phosphate antistatic component and 0.7 part of composite additive are weighed according to parts by weight, added into a reaction kettle, and stirred for 4-5 hours at 58-65 ℃ at a stirring speed of 100r/min, thus obtaining the antistatic hydraulic oil.
2. The antistatic hydraulic oil according to claim 1, wherein the trimethylolpropane oleate base oil is prepared by the steps of:
Step one, according to 1:3, weighing the calculated amount of trimethylolpropane and self-made oleic acid according to the molar ratio, pouring the calculated amount of trimethylolpropane and self-made oleic acid into a flask, adding a catalyst accounting for 4% of the total weight of the trimethylolpropane and the self-made oleic acid, an inhibitor accounting for 0.08% and an entrainer accounting for 40%, and marking the mixture as a mixed system;
Heating the oil bath of the mixed system to 80-82 ℃, then carrying out heat preservation reaction for 6-8h, filtering, separating and refining the crude ester by molecular distillation, and separating unreacted oleic acid to obtain the trimethylolpropane oleate base oil.
3. The antistatic hydraulic oil according to claim 2, wherein in the first step, the preparation method of self-made oleic acid comprises the following steps: according to 3:1:1, weighing and mixing calculated amount of oleic acid, maleic anhydride and methyl acrylate according to the molar ratio, stirring for 5min at the stirring speed of 150r/min, adding elemental iodine with the weight of 2% of that of the oleic acid, heating to 200 ℃, reacting for 3h, naturally cooling, and separating and refining by molecular distillation to obtain self-made oleic acid.
4. An antistatic hydraulic oil according to claim 1, wherein in step one, the catalyst is phosphotungstic acid, the inhibitor is hydroquinone, and the entrainer is petroleum ether.
5. The antistatic hydraulic oil according to claim 1, wherein the preparation steps of the modified graphene additive component are as follows:
step I, according to 1: dispersing graphene in N, N-dimethylformamide in a solid-liquid ratio of 500g/mL, adjusting the pH value to 8-10 after primary ultrasonic treatment, dripping oleylamine with a weight half that of the graphene, performing ultrasonic treatment again, and then reacting for 6 hours at the temperature of 80 ℃ under the protection of nitrogen;
and II, carrying out suction filtration on the reaction liquid in the step I, sequentially washing a filter membrane by using N, N-dimethylformamide, absolute ethyl alcohol and petroleum ether after removing filtrate, and carrying out vacuum drying at the temperature of 60 ℃ for 12 hours to obtain the modified graphene additive component.
6. The antistatic hydraulic oil according to claim 5, wherein in the step I, the primary ultrasonic treatment is performed at a frequency of 22-23kHz, the primary ultrasonic treatment is performed for 30min, the pH value is adjusted by using a sodium hydroxide solution with a concentration of 1.0mol/L, the secondary ultrasonic treatment is performed at a frequency of 22-23kHz, and the secondary ultrasonic treatment is performed for 15min.
7. The antistatic hydraulic oil according to claim 1, wherein the polyether phosphate antistatic component is prepared by the steps of:
step 1, pouring 2mL of ethylene glycol and 0.1g of potassium hydroxide into a flask, heating an oil bath to 100 ℃, sequentially dripping 20g of ethylene oxide and 22g of propylene oxide, and recording the mixture as ethylene oxide propylene oxide block polyether after the dripping is completed;
And 2, adding ethylene oxide and propylene oxide block polyether into the flask, heating to 45-48 ℃ under stirring, then adding phosphorus pentoxide in 3 times, stirring and reacting for 3 hours under constant temperature condition of 65-68 ℃, and obtaining the antistatic component of the polyether phosphate.
8. The antistatic hydraulic oil according to claim 7, wherein in step 2, the feeding mole ratio of ethylene oxide propylene oxide block polyether to phosphorus pentoxide is 3:1, the stirring speeds are 200r/min.
9. The antistatic hydraulic oil according to claim 1, wherein the preparation method of the composite additive comprises the following steps: adding 60% of antiwear agent, 20% of antioxidant, 6% of antirust agent, 3% of metal deactivator, 0.5% of demulsifier and 10.5% of trimethylolpropane oleate base oil into a reaction kettle according to weight percentage, stirring and heating to 50-70 ℃ at a stirring speed of 150r/min, and continuously stirring for 5-6h at a temperature of 50-70 ℃ to obtain the composite additive.
10. The antistatic hydraulic oil according to claim 9, wherein in the preparation method of the composite additive, the antiwear agent is one of thiophosphate, ammonium thiophosphate and sulfurized olefin, the antioxidant is one of alkyl diphenylamine and alkyl phenylpropionate, the antirust agent is one of allyl diacid, glycol oleate and pentaerythritol monooleate, the metal deactivator is a thiadiazole derivative, and the demulsifier is ethylene glycol ester.
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