CN103113225A - Preparation method of base oil of ultralow temperature lubricating oil - Google Patents
Preparation method of base oil of ultralow temperature lubricating oil Download PDFInfo
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- CN103113225A CN103113225A CN201310043322XA CN201310043322A CN103113225A CN 103113225 A CN103113225 A CN 103113225A CN 201310043322X A CN201310043322X A CN 201310043322XA CN 201310043322 A CN201310043322 A CN 201310043322A CN 103113225 A CN103113225 A CN 103113225A
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Abstract
The invention provides a preparation method of base oil of ultralow temperature lubricating oil. The preparation method comprises the steps of preparing a compound shown in a formula 1, preparing a compound shown in a formula 2 and preparing the base oil of the ultralow temperature lubricating oil. For the base oil of the ultralow temperature lubricating oil prepared by adopting the preparation method, kinematic viscosities at the temperatures of 40 DEG C and 100 DEG C are determined according to GB/T265-1988(2004) petroleum products--determination of kinematic viscosity and calculation of dynamic viscosity, a pour point is determined according to GB/T3535-2006 petroleum products-determination of pour point, low temperature dynamic viscosity (-25 DEG C) is determined according to GB/T6538-2010 determination of apparent viscosity of engine oils using the cold-cranking simulator, a comparison test between the base oil of the ultralow temperature lubricating oil and a lubricating oil pentaerythritol ester commodity sold on the market is carried out, and the test result shows that the base oil of the ultralow temperature lubricating oil is better than the lubricating oil pentaerythritol ester commodity and can serve as the base oil of lubricating oil.
Description
Technical field
The invention belongs to field of lubricant, be specifically related to the preparation of the friendly lubricant base of a kind of ultra-low temperature surroundings.
Background technology
Lubricating oil is one of important petroleum chemicals, have very widely in industry and a plurality of industries such as civilian and use, and traditional lubricating oil take mineral oil as base oil flows into environment, to the larger harm of environment structure, some countries are own in the world forbids using the nonconforming lubricating oil of biodegradability at environmentally sensitive area through legislation.Simultaneously, petroleum resources reduce just gradually, be to alleviate Pressure on Energy and protection of the environment, development and development of new, biodegradable lubricant base proxy mineral oil has great society and economic implications.
Viscotrol C is yellow thickness vegetables oil, belong to not drier oil class, its main component is 12-hydroxyl ricinolic acid glyceryl ester (containing ricinoleate acid more than 80%), Duo an OH group than general vegetables oil, therefore has the character of many uniquenesses, as good in lubricity, the general grease of viscosity ratio is high, zero pour low (35 ℃), burning-point is high, have nontoxic with this base oil as environmentally friendly lubricating oil, biological degradation rate is high, lubricity is good and viscosity index is high, the advantages such as regenerative power is strong, but also exist oxidation stability poor simultaneously, the shortcoming such as the high and range of viscosities of pour point is narrower, this has limited vegetables oil to a great extent as continuous high temperature, application under the particular surroundingss such as low cold or difference variation is large.
Summary of the invention
Technical problem to be solved by this invention is to overcome the shortcoming that above-mentioned Viscotrol C exists, and provides that a kind of product application scope is wide, thermal oxidation stable, the preparation method of the base oil of good product quality, very low temperature lubricating oil that production cost is low.
Solving the problems of the technologies described above the technical scheme that adopts is made by following step:
1, preparation formula 1 compound
Viscotrol C, properties-correcting agent are added in the there-necked flask that reflux condensing tube and constant speed stirrer are housed, be warming up to 90～100 ℃, then to add disodium-hydrogen catalyzer, the mol ratio of Viscotrol C and properties-correcting agent, disodium-hydrogen be 1:2.0～3.0:0.0657～0.1313,200 rev/mins of isothermal reactions 2.0～3.5 hours, be cooled to room temperature, standing demix is emitted lower clear liquid, upper strata liquid is washed till neutrality with boiling water, 0.02MPa dehydration, a preparation accepted way of doing sth 1 compound, its chemical equation is as follows:
Formula 1
R in following formula
1Be glycerine ester group, R
2Be CH
3-, CH
3CH
2-, CH
3CH
2CH
2-in any one.
Above-mentioned properties-correcting agent is any one in diacetyl oxide, propionic anhydride, butyryl oxide.
2, preparation formula 2 compounds
formula 1 compound and acetic acid are added in the there-necked flask that reflux condensing tube and constant speed stirrer are housed, hydrogen peroxide, the biphosphate sodium catalyst joins dissolving in beaker, 40 ℃ are added dropwise in there-necked flask, formula 1 compound and acetic acid, hydrogen peroxide, the mass ratio of SODIUM PHOSPHATE, MONOBASIC is 1:0.10～0.20:0.80～0.90:0.01～0.02, be warming up to 60～65 ℃, 400 rev/mins of isothermal reactions 2.5～3.5 hours, be cooled to room temperature, standing demix, emit lower clear liquid, product is washed till neutrality with boiling water, 0.02MPa dehydration, a preparation accepted way of doing sth 2 compounds, its chemical equation is as follows:
Formula 2
R3 in following formula is CH3-.
3, the base oil of preparation very low temperature lubricating oil
Formula 2 compounds and alcohol are added in the there-necked flask that reflux condensing tube and constant speed stirrer are housed, be warming up to 85～95 ℃, add again phosphoric acid catalyst, formula 2 compounds are 1:8.0～10.0:0.3514～0.4686,300 rev/min isothermal reaction 8.0～9.0 hours with the mol ratio of alcohol, phosphoric acid, are cooled to room temperature, product is washed till neutrality with boiling water, 0.02MPa dewater, be prepared into the base oil of very low temperature lubricating oil, its chemical equation is as follows:
Formula 3
R4 in following formula is any one in (CH3) 2CH-, CH3CH (CH3) CH2CH2-, CH3CH2CH2CH2CH2CH2CH2-.
Above-mentioned alcohol is any one in Virahol, primary isoamyl alcohol, n-Heptyl alcohol.
In preparation 1 formula compound step 1 of the present invention, Viscotrol C, properties-correcting agent are added in the there-necked flask that reflux condensing tube and constant speed stirrer are housed, optimum temperature rise to 100 ℃, then add the disodium-hydrogen catalyzer, the optimum mole ratio of Viscotrol C and properties-correcting agent, disodium-hydrogen is 1:2.5:0.0985,200 rev/mins of isothermal reactions 2.0～3.5 hours are cooled to room temperature, standing demix, emit lower clear liquid, upper strata liquid is washed till neutrality with boiling water, 0.02MPa dehydration, a preparation accepted way of doing sth 1 compound.
In preparation 2 formula compound steps 2 of the present invention, formula 1 compound and acetic acid are added in the there-necked flask that reflux condensing tube and constant speed stirrer are housed, hydrogen peroxide, biphosphate sodium catalyst join dissolving in beaker, 40 ℃ are added dropwise in there-necked flask, the optimum quality ratio of formula 1 compound and acetic acid, hydrogen peroxide, SODIUM PHOSPHATE, MONOBASIC is 1:0.15:0.85:0.015, optimum temperature rise to 60 ℃, 400 rev/mins of isothermal reactions 2.5～3.5 hours, be cooled to room temperature, product is washed till neutrality with boiling water, 0.02MPa dehydration, a preparation accepted way of doing sth 2 compounds.
In the base oil step 3 of preparation very low temperature lubricating oil of the present invention, formula 2 compounds and alcohol are added in the there-necked flask that reflux condensing tube and constant speed stirrer are housed, optimum temperature rise to 85 ℃, add phosphoric acid catalyst, formula 2 compounds are 1:9.0:0.4100 with the optimum mole ratio of alcohol, phosphoric acid, 300 rev/mins of isothermal reactions 8.0～9.0 hours again, be cooled to room temperature, product is washed till neutrality with boiling water, and 0.02MPa dewaters, and is prepared into the base oil of very low temperature lubricating oil.
adopt the base oil of the very low temperature lubricating oil of the present invention's preparation, measure the kinematic viscosity of 40 ℃ and 100 ℃ according to GB/T265-1988 (2004) " petroleum products kinematic viscosity assay method and kinetic viscosity computing method ", GB/T3535-2006 " petroleum products pour point assay method " measures pour point, GB/T6538-2010 " the mensuration cold start-up analog machine method of engine oil apparent viscosity " measures the commercial lubricant pentaerythritol ester of selling on low-temperature dynamic viscosity (25 ℃) and market and has carried out contrast test, test result shows, adopt the base oil of the very low temperature lubricating oil of the present invention's preparation to be better than the commercial lubricant pentaerythritol ester, can be used as the base oil of lubricating oil.
Description of drawings
Fig. 1 is the infrared spectrogram of base oil of the very low temperature lubricating oil of embodiment 1 preparation.
Embodiment
The present invention is described in more detail below in conjunction with drawings and Examples, but the invention is not restricted to these embodiment.
Embodiment 1
1, preparation formula 1 compound
Viscotrol C 175.00g, propionic anhydride 61.09g are added in the 500mL there-necked flask that reflux condensing tube and constant speed stirrer are housed, be warming up to 100 ℃, add again disodium-hydrogen catalyzer 2.63g, the mol ratio 1:2.5:0.0985 of Viscotrol C and propionic anhydride, disodium-hydrogen, 200 rev/mins of isothermal reactions 2.0～3.5 hours.Be cooled to room temperature, standing demix is emitted lower clear liquid, and upper strata liquid is washed till neutrality with boiling water, 0.02MPa dehydration, a preparation accepted way of doing sth 1 compound.Chemical equation is seen formula 1, and in formula 1, R1 is the glycerine ester group, and R2 is CH3CH2-.
2, preparation formula 2 compounds
Formula 1 compound 160.00g, acetic acid 24.00g are added in the there-necked flask that reflux condensing tube and constant speed stirrer are housed, and hydrogen peroxide 136.00g, biphosphate sodium catalyst 2.40g add fully dissolving in beaker.Being warming up to 40 ℃ is added drop-wise in there-necked flask, the mass ratio of formula 1 compound and acetic acid, hydrogen peroxide, SODIUM PHOSPHATE, MONOBASIC is 1:0.15:0.85:0.015, be warming up to 60 ℃ after dropwising, 400 rev/mins of isothermal reactions 2.5～3.5 hours, be cooled to room temperature, product is washed till neutrality with boiling water, 0.02MPa dehydration, a preparation accepted way of doing sth 2 compounds.Chemical equation is seen formula 2, and in formula 2, R3 is CH3-.
3, the base oil of preparation very low temperature lubricating oil
Formula 2 compound 65.00g, primary isoamyl alcohol 44.92g are placed in the 500mL there-necked flask that reflux condensing tube and constant speed stirrer are housed, be warming up to 85 ℃, add again phosphoric acid catalyst 2.28g, the mol ratio of formula 2 compounds and primary isoamyl alcohol, phosphoric acid is 1:9.0:0.4100,300 rev/mins of isothermal reactions 8.0～9.0 hours are cooled to room temperature, and product is washed till neutrality with boiling water, 0.02MPa dewater, be prepared into the base oil of very low temperature lubricating oil.Chemical equation is seen formula 3, and in formula 3, R4 is CH3CH (CH3) CH2CH2-.
The base oil of prepared very low temperature lubricating oil is tested with infrared spectrometer, and experimental result is seen Fig. 1.As seen from Figure 1, the stretching vibration of O-H has appearred in the 3437cm-1 place, and the absorption peak of strong ether structure has appearred in the 1177cm-1 place, and the expression epoxy bond is opened, and has introduced hydroxyl and ether structure in molecule.
Embodiment 2
In preparation formula 1 compound step 1, Viscotrol C 175.00g, propionic anhydride 48.87g are added in the 500mL there-necked flask that reflux condensing tube and constant speed stirrer are housed, be warming up to 100 ℃, add again disodium-hydrogen catalyzer 1.75g, the mol ratio 1:2.0:0.0657 of Viscotrol C and propionic anhydride, disodium-hydrogen.Other step in this step is identical with embodiment 1, a preparation accepted way of doing sth 1 compound.Chemical equation is seen formula 1, and in formula 1, R1 is the glycerine ester group, and R2 is CH3CH2-.
In preparation formula 2 compound steps 2, formula 1 compound 160.00g, acetic acid 16.00g are added in the there-necked flask that reflux condensing tube and constant speed stirrer are housed, hydrogen peroxide 128.00g, biphosphate sodium catalyst 1.60g add fully dissolving in beaker.Be warming up to 40 ℃ and be added drop-wise in there-necked flask, the mass ratio of formula 1 compound and acetic acid, hydrogen peroxide, SODIUM PHOSPHATE, MONOBASIC is 1:0.10:0.80:0.01.Other step in this step is identical with embodiment 1, a preparation accepted way of doing sth 2 compounds,, chemical equation is seen formula 2, in formula 2, R3 is CH3-.
In the base oil step 3 of preparation very low temperature lubricating oil, formula 2 compound 65.00g, primary isoamyl alcohol 39.93g are placed in the 500mL there-necked flask that reflux condensing tube and constant speed stirrer are housed, be warming up to 85 ℃, add again phosphoric acid catalyst 1.95g, the mol ratio of formula 2 compounds and primary isoamyl alcohol, phosphoric acid is 1:8.0:0.3514, other step in this step is identical with embodiment 1, is prepared into the base oil of very low temperature lubricating oil.Chemical equation is seen formula 3, and in formula 3, R4 is CH3CH (CH3) CH2CH2-.
Embodiment 3
In preparation formula 1 compound step 1, Viscotrol C 175.00g, propionic anhydride 73.31g are added in the 500mL there-necked flask that reflux condensing tube and constant speed stirrer are housed, be warming up to 100 ℃, add again disodium-hydrogen catalyzer 3.50g, the mol ratio 1:3.0:0.1313 of Viscotrol C and propionic anhydride, disodium-hydrogen.Other step in this step is identical with embodiment 1, a preparation accepted way of doing sth 1 compound.Chemical equation is seen formula 1, and in formula 1, R1 is the glycerine ester group, and R2 is CH3CH2-.
In preparation formula 2 compound steps 2, formula 1 compound 160.00g, acetic acid 32.00g are added in the there-necked flask that reflux condensing tube and constant speed stirrer are housed, hydrogen peroxide 144.00g, biphosphate sodium catalyst 3.20g add fully dissolving in beaker.Be warming up to 40 ℃ and be added drop-wise in there-necked flask, the mass ratio of formula 1 compound and acetic acid, hydrogen peroxide, SODIUM PHOSPHATE, MONOBASIC is 1:0.20:0.90:0.02.Other step in this step is identical with embodiment 1, a preparation accepted way of doing sth 2 compounds, and chemical equation is seen formula 2, in formula 2, R3 is CH3-.
In the base oil step 3 of preparation very low temperature lubricating oil, formula 2 compound 65.00g, primary isoamyl alcohol 49.91g are placed in the 500mL there-necked flask that reflux condensing tube and constant speed stirrer are housed, be warming up to 85 ℃, add again phosphoric acid catalyst 2.60g, the mol ratio of formula 2 compounds and primary isoamyl alcohol, phosphoric acid is 1:10.0:0.4686, other step in this step is identical with embodiment 1, be prepared into the base oil of very low temperature lubricating oil, chemical equation is seen formula 3, in formula 3, R4 is CH3CH (CH3) CH2CH2-.
Embodiment 4
In the preparation formula 1 compound step 1 of above embodiment 1～3, material modification agent propionic anhydride used is replaced with equimolar diacetyl oxide, and in this step, other step is identical with embodiment 1, a preparation accepted way of doing sth 1 compound, in formula 1, R1 is the glycerine ester group, and R2 is CH3-.In the base oil step 3 of preparation very low temperature lubricating oil, raw materials used primary isoamyl alcohol is replaced with equimolar Virahol, and in this step, other step is identical with embodiment 1.Other step is identical with corresponding embodiment, is prepared into the base oil of very low temperature lubricating oil, and in formula 3, R4 is (CH3) 2CH-.
Embodiment 5
In the preparation formula 1 compound step 1 of above embodiment 1～3, material modification agent propionic anhydride used is replaced with equimolar butyryl oxide, and in this step, other step is identical with embodiment 1, a preparation accepted way of doing sth 1 compound, in formula 1, R1 is the glycerine ester group, and R2 is CH3CH2CH2-.In the base oil step 3 of preparation very low temperature lubricating oil, raw materials used primary isoamyl alcohol is replaced with equimolar n-Heptyl alcohol, and in this step, other step is identical with embodiment 1.Other step is identical with corresponding embodiment, is prepared into the base oil of very low temperature lubricating oil, and in formula 3, R4 is CH3CH2CH2CH2CH2CH2CH2-.
Embodiment 6
In the preparation formula 1 compound step 1 of above embodiment 1～5, Viscotrol C, properties-correcting agent are added in the there-necked flask that reflux condensing tube and constant speed stirrer are housed, be warming up to 90 ℃, add the disodium-hydrogen catalyzer, the consumption of Viscotrol C, properties-correcting agent, disodium-hydrogen is identical with corresponding embodiment again, and other step is identical with embodiment 1, a preparation accepted way of doing sth 1 compound, in formula 1, R1 is the glycerine ester group, and R2 is identical with corresponding embodiment.In preparation formula 2 compound steps 2, raw material used and proportioning thereof are identical with corresponding embodiment, are warming up to 62 ℃, 400 rev/mins of isothermal reactions 2.5～3.5 hours.Other step is identical with embodiment 1, the compound of a preparation accepted way of doing sth 2, and in formula 2, R3 is CH3-.In the base oil step 3 of preparation very low temperature lubricating oil, formula 2 compounds and alcohol are added in the there-necked flask that reflux condensing tube and constant speed stirrer are housed, be warming up to 90 ℃, add again phosphoric acid catalyst, the consumption of formula 2 compounds, alcohol, phosphoric acid is identical with corresponding embodiment, other step in this step is identical with embodiment 1, is prepared into the base oil of very low temperature lubricating oil.In formula 3, R4 is identical with corresponding embodiment.
Embodiment 7
In the preparation formula 1 compound step 1 of above embodiment 1～5, Viscotrol C, properties-correcting agent are added in the there-necked flask that reflux condensing tube and constant speed stirrer are housed, be warming up to 95 ℃, add the disodium-hydrogen catalyzer, the consumption of Viscotrol C, properties-correcting agent, disodium-hydrogen is identical with corresponding embodiment again, and other step is identical with embodiment 1, a preparation accepted way of doing sth 1 compound, in formula 1, R1 is the glycerine ester group, and R2 is identical with corresponding embodiment.In preparation formula 2 compound steps 2, raw material used and proportioning thereof are identical with corresponding embodiment, are warming up to 65 ℃, 400 rev/mins of isothermal reactions 2.5～3.5 hours, other step is identical with embodiment 1, the compound of a preparation accepted way of doing sth 2, in formula 2, R3 is CH3-.In the base oil step 3 of preparation very low temperature lubricating oil, formula 2 compounds and alcohol are added in the there-necked flask that reflux condensing tube and constant speed stirrer are housed, be warming up to 95 ℃, add again phosphoric acid catalyst, the consumption of formula 2 compounds, alcohol, phosphoric acid is identical with corresponding embodiment, other step in this step is identical with embodiment 1, is prepared into the base oil of sub-zero oil.In formula 3, R4 is identical with corresponding embodiment.
In order to determine optimised process step of the present invention, the contriver has carried out a large amount of laboratory study tests, and various test situation are as follows:
1, determine the properties-correcting agent of Viscotrol C
Take Viscotrol C 525.00g and divide equally 3 parts, add respectively in 3 there-necked flasks that reflux condensing tube and constant speed stirrer be housed, add respectively diacetyl oxide 47.92g, propionic anhydride 61.09g, butyryl oxide 74.26g properties-correcting agent, the mol ratio of Viscotrol C and diacetyl oxide, propionic anhydride, butyryl oxide is for being respectively 1:2.5; Be heated to 100 ℃, then add respectively 2.63g disodium-hydrogen catalyzer, 200 rev/mins of isothermal reactions 3.0 hours are cooled to room temperature, and standing demix is emitted lower clear liquid, and upper strata liquid is washed till neutrality with boiling water, and the 0.02MPa dehydration gets formula 1 compound.Other step is identical with embodiment 1, is prepared into respectively the base oil (during test, name is called base oil) of 3 kinds of very low temperature lubricating oil, is numbered No. 1, No. 2, No. 3.Prepared base oil and commercially available pentaerythritol ester have carried out contrast test.Measure respectively the kinematic viscosity of 40 ℃, 100 ℃ according to GB/T265-1988 (2004) " petroleum products kinematic viscosity assay method and kinetic viscosity computing method "; Measure pour point according to GB/T3535-2006 " petroleum products pour point assay method ": measure low-temperature dynamic viscosity (25 ℃) according to GB/T6538-2010 " the mensuration cold start-up analog machine method of engine oil apparent viscosity ", test result sees Table 1.
The physical and chemical index of table 1 base oil
By as seen from Table 1, the depression of pour point of No. 1, No. 2, No. 3 base oil, has low-temperature performance, use that can be under ultra-low temperature surroundings, the pour point of No. 2 base oils and low-temperature dynamic viscosity are best, be better than the commercial lubricant pentaerythritol ester, it is the properties-correcting agent of Viscotrol C that the present invention selects diacetyl oxide, propionic anhydride, butyryl oxide, and propionic anhydride is best.
2, the alcohol in the base oil of definite preparation very low temperature lubricating oil
According to embodiment 1 preparation formula 1, formula 2 compounds.take formula 2 compound 300g, divide equally 3 parts, be placed in respectively the 500mL there-necked flask that reflux condensing tube and constant speed stirrer are housed, add respectively Virahol 47.09g, primary isoamyl alcohol 69.11g, n-Heptyl alcohol 91.10g, be warming up to 85 ℃, add respectively again phosphoric acid catalyst 3.50g, 300 rev/mins of isothermal reactions 9.0 hours, be cooled to room temperature, product is washed till neutrality with boiling water, 0.02MPa dehydration, be prepared into respectively the base oil of 3 kinds of very low temperature lubricating oil, be numbered No. 4, No. 5, No. 6, the base oil of prepared very low temperature lubricating oil and commercially available pentaerythritol ester have carried out contrast test.Measure respectively the kinematic viscosity of 40 ℃, 100 ℃ according to GB/T265-1988 (2004) " petroleum products kinematic viscosity assay method and kinetic viscosity computing method ", measure pour point according to GB/T3535-2006 " petroleum products pour point assay method ", measure low-temperature dynamic viscosity (25 ℃) according to GB/T6538-2010 " the mensuration cold start-up analog machine method of engine oil apparent viscosity ", test result sees Table 2.
The physical and chemical index of table 2 base oil
By as seen from Table 2, pour point, the low-temperature performance of No. 4, No. 6 base oils are bad, and pour point, the low-temperature performance of No. 5 base oils are better.It is the best alcohol of the base oil of preparation very low temperature lubricating oil that the present invention selects primary isoamyl alcohol.
In order to verify beneficial effect of the present invention, the contriver adopts the base oil of the very low temperature lubricating oil of the embodiment of the present invention 1 preparation to test, and various test situation are as follows:
1, the physical and chemical index of the base oil of test very low temperature lubricating oil
Testing method is identical with experiment 1, and experimental result sees Table the test result of No. 2 base oils in 1.By as seen from Table 1, adopt the base oil of the very low temperature lubricating oil of the present invention's preparation to be better than the commercial lubricant pentaerythritol ester, can be used as the base oil of lubricating oil.
Claims (4)
1. the preparation method of the base oil of a very low temperature lubricating oil is characterized in that it is to be made by following step:
(1) preparation formula 1 compound
Viscotrol C, properties-correcting agent are added in the there-necked flask that reflux condensing tube and constant speed stirrer are housed, be warming up to 90～100 ℃, then to add disodium-hydrogen catalyzer, the mol ratio of Viscotrol C and properties-correcting agent, disodium-hydrogen be 1:2.0～3.0:0.0657～0.1313,200 rev/mins of isothermal reactions 2.0～3.5 hours, be cooled to room temperature, standing demix is emitted lower clear liquid, upper strata liquid is washed till neutrality with boiling water, 0.02MPa dehydration, a preparation accepted way of doing sth 1 compound, its chemical equation is as follows:
Formula 1
R in following formula
1Be glycerine ester group, R
2Be CH
3-, CH
3CH
2-, CH
3CH
2CH
2-in any one;
Above-mentioned properties-correcting agent is any one in diacetyl oxide, propionic anhydride, butyryl oxide;
(2) preparation formula 2 compounds
formula 1 compound and acetic acid are added in the there-necked flask that reflux condensing tube and constant speed stirrer are housed, hydrogen peroxide, the biphosphate sodium catalyst joins dissolving in beaker, 40 ℃ are added dropwise in there-necked flask, formula 1 compound and acetic acid, hydrogen peroxide, the mass ratio of SODIUM PHOSPHATE, MONOBASIC is 1:0.10～0.20:0.80～0.90:0.01～0.02, be warming up to 60～65 ℃, 400 rev/mins of isothermal reactions 2.5～3.5 hours, be cooled to room temperature, standing demix, emit lower clear liquid, product is washed till neutrality with boiling water, 0.02MPa dehydration, a preparation accepted way of doing sth 2 compounds, its chemical equation is as follows:
Formula 2
R in following formula
3Be CH
3-;
(3) base oil of preparation very low temperature lubricating oil
Formula 2 compounds and alcohol are added in the there-necked flask that reflux condensing tube and constant speed stirrer are housed, be warming up to 85～95 ℃, add again phosphoric acid catalyst, formula 2 compounds are 1:8.0～10.0:0.3514～0.4686,300 rev/min isothermal reaction 8.0～9.0 hours with the mol ratio of alcohol, phosphoric acid, are cooled to room temperature, product is washed till neutrality with boiling water, 0.02MPa dewater, be prepared into the base oil of very low temperature lubricating oil, its chemical equation is as follows:
Formula 3
R in following formula
4Be (CH
3)
2CH-, CH
3CH (CH
3) CH
2CH
2-, CH
3CH
2CH
2CH
2CH
2CH
2CH
2-in any one;
Above-mentioned alcohol is any one in Virahol, primary isoamyl alcohol, n-Heptyl alcohol.
2. the preparation method of the base oil of very low temperature lubricating oil according to claim 1, it is characterized in that: in preparation 1 formula compound step 1, with Viscotrol C, properties-correcting agent adds in the there-necked flask that reflux condensing tube and constant speed stirrer are housed, be warming up to 100 ℃, add again the disodium-hydrogen catalyzer, Viscotrol C and properties-correcting agent, the mol ratio of disodium-hydrogen is 1:2.5:0.0985, 200 rev/mins of isothermal reactions 2.0～3.5 hours, be cooled to room temperature, standing demix, emit lower clear liquid, upper strata liquid is washed till neutrality with boiling water, 0.02MPa dehydration, a preparation accepted way of doing sth 1 compound.
3. the preparation method of the base oil of very low temperature lubricating oil according to claim 1, it is characterized in that: in preparation 2 formula compound steps 2, formula 1 compound and acetic acid are added in the there-necked flask that reflux condensing tube and constant speed stirrer are housed, hydrogen peroxide, the biphosphate sodium catalyst joins dissolving in beaker, 40 ℃ are added dropwise in there-necked flask, formula 1 compound and acetic acid, hydrogen peroxide, the mass ratio of SODIUM PHOSPHATE, MONOBASIC is 1:0.15:0.85:0.015, be warming up to 60 ℃, 400 rev/mins of isothermal reactions 2.5～3.5 hours, be cooled to room temperature, product is washed till neutrality with boiling water, 0.02MPa dehydration, a preparation accepted way of doing sth 2 compounds.
4. the preparation method of the base oil of very low temperature lubricating oil according to claim 1, it is characterized in that: in the base oil step 3 of preparation very low temperature lubricating oil, formula 2 compounds and alcohol are added in the there-necked flask that reflux condensing tube and constant speed stirrer are housed, be warming up to 85 ℃, add again phosphoric acid catalyst, formula 2 compounds are 1:9.0:0.4100 with the mol ratio of alcohol, phosphoric acid, 300 rev/mins of isothermal reactions 8.0～9.0 hours, be cooled to room temperature, product is washed till neutrality with boiling water, 0.02MPa dewater, be prepared into the base oil of very low temperature lubricating oil.
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| CN104962341A (en) * | 2015-06-26 | 2015-10-07 | 陕西师范大学 | High-temperature-resistant lubricating oil base oil and preparation method thereof |
| CN113293053A (en) * | 2021-06-15 | 2021-08-24 | 诺世(天津)润滑油有限公司 | Lubricating oil with strong wear resistance and preparation method thereof |
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| 李清华: "新型植物油改性润滑剂的研究与开发", 《中国博士学位论文全文数据库 工程科技II辑》 * |
| 耿海军: "生物基润滑油的研究进展", 《河南化工》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104962341A (en) * | 2015-06-26 | 2015-10-07 | 陕西师范大学 | High-temperature-resistant lubricating oil base oil and preparation method thereof |
| CN113293053A (en) * | 2021-06-15 | 2021-08-24 | 诺世(天津)润滑油有限公司 | Lubricating oil with strong wear resistance and preparation method thereof |
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| Publication number | Publication date |
|---|---|
| CN103113225B (en) | 2015-01-14 |
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