CN109913300A - A kind of biodegradable environment protective lubricant and preparation method thereof - Google Patents
A kind of biodegradable environment protective lubricant and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of biodegradable environment protective lubricants and preparation method thereof, which includes following components: vegetable oil, antioxidant, emulsifier, sodium carbonate, hydrochloric acid and ionic liquid；The lubricant the preparation method comprises the following steps: the preparation of Plant Oil Fatty Acid Methyl Ester；The preparation of modified vegetable oil；The preparation of modified vegetable oil of epoxidation；The preparation of twice-modified vegetable oil；Twice-modified vegetable oil, ionic liquid, antioxidant, emulsifier, sodium carbonate and hydrochloric acid are sequentially added in reactor, stirs, obtains lubricant；Vegetable oil is after being once modified and is twice-modified, both C=C double bond in vegetable oil had been eliminated, the glycerol in vegetable oil molecule has been replaced again, to obtain the preferable modified vegetable oil of oxidation stability, the experimental results showed that lubricant obtained by the present invention has good biological degradability and lubricant effect.
Description
Technical field
The present invention relates to technical field of lubricant, specifically a kind of biodegradable environment protective lubricant and its preparation side
Method.
Background technique
Lubricant plays key effect in terms of reducing mechanical wear, extending, and lubricant presses its object
Matter form can be divided into fluid lubricant (mineral oil, synthetic oil, it is water base oil, vegetable and animals oils), lubricating grease, solid lubricant (graphite,
Molybdenum disulfide) and gas lubricant (air, helium, nitrogen, hydrogen etc.), compared with other lubricants, fluid lubricant is answered
With relatively broad, it has the features such as wider range of viscosities, low noise, high heat conductance, is applicable under a variety of operating conditions
Friction is secondary and moving component, and product resource is abundant, cheap, is easy to get.
At the end of the 19th century, mineral oil has gradually become the mainstream of lubricant, into after 20th century, internal combustion engine and auto industry
Development, friction pair need long-term work under the conditions of the bad working environments of high temperature and high pressure, and this requires lubricating oil higher work
Make temperature range and stability, thus synthetic oil is widely used, wherein silicon class oil has wider temperature model
Enclose with high viscosity index (VI), be used widely in aerospace field, PAO(polyalphaolefin) and polyester etc. be also applied to aircraft
Manufacturing industry, these syntholubes expand the use temperature range of fluid film lubrication, from -70 DEG C to 300 DEG C, but are closing
At itself in the use process of lubricating oil, is found there are some defects, such as lower polarity, boundary lubrication ability is poor and high
For temperature using limited etc., this requires people to be continuing effort to explore high performance lubricant.A large amount of lubricating oil are being produced, using and are being arranged
During putting due to infiltration, leakage, overflow and deal with improperly, and caused by environmental problem seriously pollute soil and water resource,
Ecological environment and the ecological balance are destroyed, these environmental problems are with being increasingly enhanced of realizing of people's environmental crisis and increasingly
It is taken seriously, it is the following lubrication that it is the effective way for solving the problems, such as this that developing, which has the environment-friendly lubricating oil of biological degradability,
The developing direction of oily industry.
Vegetable oil based lubricating oil has good sustainable productivity, biodegradable performance, volatility is low, high-flash by
To the extensive concern of people, but vegetable oil based lubricating oil oxidation stability in the prior art is poor, and lubricant effect need into one
Step improves, these defects limit the further development of vegetable oil based lubricating oil.
Summary of the invention
The purpose of the present invention is to provide a kind of biodegradable environment protective lubricants and preparation method thereof, existing to solve
There is the problems in technology.
To achieve the above object, the invention provides the following technical scheme:
A kind of biodegradable environment protective lubricant, the lubricant include the component of following parts by weight: vegetable oil 30-50
Part, 3-8 parts of antioxidant, 2-10 parts of emulsifier, 1-3 parts of sodium carbonate and 3-5 parts of hydrochloric acid.
As optimization, which further includes the ionic liquid of 1-10 parts by weight, and ionic liquid is 1- ethyl -3-
Methyl imidazolium tetrafluoroborate ionic liquid, 1- butyl -3- methylimidazole villaumite ionic liquid, 1- butyl -3- methylimidazole six
In fluorophosphate ionic liquid, quaternary phosphonium salt phosphate ion liquid or 1- hexyl -3- methylimidazole hexafluorophosphoric acid ionic liquid
Any one.When the lubricant is used for mechanical equipment, the ionic liquid in the lubricant is easy on mechanical equipment surface
Complicated friction chemical reaction occurs and generates one layer of friction reaction film, which has lower shear strength and relatively
It is flat and smooth, to make the new lubricant that there is good lubricant effect.
As optimization, vegetable oil is modified vegetable oil, modified vegetable oil by vegetable oil by methanol, trimethylolethane,
Glacial acetic acid, hydrogen peroxide and modified with organic acids are made.The present invention uses oil based on modified vegetable oil, has good biology
Degradability, vegetable oil pass through after a series of modification, have not only eliminated C=C double bond in vegetable oil, but also replaced vegetable oil
Glycerol in molecule, to obtain the preferable modified vegetable oil of oxidation stability.
As optimization, vegetable oil is any one in linseed oil, cottonseed oil, rice bran oil, camellia seed oil or coconut oil.
As optimization, antioxidant is zinc dialkyl dithiophosphate, thio-2 acid double octadecyl esters, dodecyl selenium, 2,
Any one in 6- di-tert-butyl p-cresol or zinc dialkyl dithiocarbamate, emulsifier are lignosulfonates, contracting
Any one in methylcellulose, diglycerol polypropylene glycol ether, polyoxyethylene oleic acid ester or fatty amide polyoxyethylene ether.It is anti-
On the one hand oxygen agent can inhibit peroxide, and peroxynitrite decomposition compound, on the other hand, antioxidant can remove peroxy radical,
Antioxidant is reacted with peroxy radical, can be prevented the generation and transfer of peroxide in aliphatic oxygenation reaction process, be made to lubricate
Agent has good antioxidant effect；Emulsifier can enhance ionic liquid, antioxidant, sodium carbonate and hydrochloric acid and modified vegetable oil
Compatibility, it is evenly dispersed to be conducive to each component, and the emulsifier is easily biodegradable, it is more environmentally-friendly.
A kind of preparation method of biodegradable environment protective lubricant, the preparation method of the lubricant include following step
It is rapid:
(1) preparation of Plant Oil Fatty Acid Methyl Ester；
The preparation of (2) modified vegetable oils；
(3) preparation of modified vegetable oil of epoxidation；
(4) preparation of twice-modified vegetable oil；
(5) by the obtained twice-modified vegetable oil of step (4), ionic liquid, antioxidant, emulsifier, sodium carbonate and hydrochloric acid according to
In secondary addition reactor, stirring obtains lubricant.
As optimization, a kind of preparation method of biodegradable environment protective lubricant, the preparation method packet of the lubricant
Include following steps:
(1) it takes vegetable oil to be added in flask, methanol and sodium hydroxide is added in flask under stirring conditions, heating reaction,
Cooling, liquid separation, vacuum distillation obtains Plant Oil Fatty Acid Methyl Ester；
(2) the resulting Plant Oil Fatty Acid Methyl Ester of step (1) is added in flask, under stirring conditions by trimethylolethane
It is added in flask, then is rapidly added sodium ethoxide, heating reaction is cooling, and liquid separation is evaporated under reduced pressure, obtains a modified vegetable oil；
(3) the resulting modified vegetable oil of step (2) is added in flask, under stirring conditions, by glacial acetic acid, peroxidating
Hydrogen and the concentrated sulfuric acid are added dropwise in flask simultaneously respectively, heating reaction, cooling, and modified vegetable oil of epoxidation is collected in liquid separation；
(4) modified vegetable oil of epoxidation that step (3) are collected is refunded in flask, then organic acid and dense is added into flask
Sulfuric acid, stirring, heating reaction, cooling, liquid separation, vacuum distillation obtain twice-modified vegetable oil；
(5) by the obtained twice-modified vegetable oil of step (4), ionic liquid, antioxidant, emulsifier, sodium carbonate and hydrochloric acid according to
It in secondary addition reactor, heats, stirring obtains lubricant.
As optimization, a kind of preparation method of biodegradable environment protective lubricant, the preparation method packet of the lubricant
Include following steps:
(1) it takes vegetable oil to be added in flask, after being heated to 50-70 DEG C, methanol and sodium hydroxide is added under stirring conditions
In flask, the ratio between amount of substance of vegetable oil and methanol is 1:4-6, and the quality of sodium hydroxide is vegetable oil and methanol gross mass
0.5-1% reacts 60-90min at 50-70 DEG C, and reaction mixture is transferred in separatory funnel by cooled to room temperature, to
Dilute hydrochloric acid is added in separatory funnel and is neutralized to neutrality, stratification first separates lower layer's water phase, by upper layer Plant Oil Fatty Acid Methyl Ester
Solution is evaporated under reduced pressure in the case where vacuum degree is 0.01-0.03MPa, temperature is 30-40 DEG C, obtains Plant Oil Fatty Acid Methyl Ester；
First ester exchange reaction is occurred for vegetable oil and methanol by the present invention, replaces the glyceryl in long chain fatty acids with methyl, by glycerol three
Ester fracture generates long chain fatty acids methyl esters, to shorten carbon chain lengths, but can reduce the viscosity of oil plant in this way；
(2) the resulting Plant Oil Fatty Acid Methyl Ester of step (1) is added in flask, is heated to 60-80 DEG C, under stirring conditions
Trimethylolethane is added in flask, is then rapidly added sodium ethoxide, Plant Oil Fatty Acid Methyl Ester and trimethylolethane again
The ratio between the amount of substance be 3-5:1, the quality of sodium ethoxide is Plant Oil Fatty Acid Methyl Ester and trimethylolethane gross mass
0.8-1.2% reacts 1-2h at 60-80 DEG C, and reaction mixture is transferred in separatory funnel by cooled to room temperature, to point
Dilute hydrochloric acid is added in liquid funnel and is neutralized to neutrality, stratification first separates lower layer's water phase, and the modified vegetable oil of upper layer one time is mixed
Solution is evaporated under reduced pressure in the case where vacuum degree is 0.01-0.03MPa, temperature is 60-80 DEG C, obtains a modified vegetable oil；This
The Plant Oil Fatty Acid Methyl Ester that step (1) obtains after ester exchange reaction and trimethylolethane are carried out transesterification by invention again
Reaction, obtains a modified vegetable oil, to replace the glycerol in vegetable oil molecule with the polyalcohol without β-H, makes vegetable oil
Stability be improved；
(3) the resulting modified vegetable oil of step (2) is added in flask, is heated to 40-60 DEG C, under stirring conditions,
Glacial acetic acid, hydrogen peroxide and the concentrated sulfuric acid are added dropwise in flask simultaneously respectively, rate of addition is 20-25 drop/minute, is once changed
Property vegetable oil, glacial acetic acid and hydrogen peroxide the ratio between the amount of substance be 1:4-5:4-5, the quality of the concentrated sulfuric acid is an improved plant
The 0.5-1% of oil, glacial acetic acid and hydrogen peroxide gross mass, after being added dropwise, reacts 3-5h at 60-70 DEG C, naturally cools to room
Reaction mixture is transferred in separatory funnel by temperature, and sodium hydroxide solution is added into separatory funnel and is neutralized to neutrality, stands and divides
Layer first separates lower layer's water phase, collects modified vegetable oil of upper layer epoxidation；But also contain C=C in a modified vegetable oil
Double bond, the present invention, which is reacted using glacial acetic acid with hydrogen peroxide, generates Peracetic acid, and a modified vegetable oil is reacted with Peracetic acid
Modified vegetable oil of epoxidation is generated, to eliminate the double bond in vegetable oil, but epoxy group is three-membered ring, with height
Power, only open loop could release tension；
(4) modified vegetable oil of epoxidation that step (3) are collected is refunded in flask, then organic acid and dense is added into flask
The ratio between amount of substance of sulfuric acid, modified vegetable oil of epoxidation and organic acid is 1:4-5, and the quality of the concentrated sulfuric acid is epoxidation one
The 0.2-0.5% of secondary modified vegetable oil and organic acid gross mass reacts 2-4h, natural cooling under conditions of stirring, 70-80 DEG C
To room temperature, reaction mixture is transferred in separatory funnel, sodium hydroxide solution is added into separatory funnel and is neutralized to neutrality, it is quiet
Layering is set, lower layer's water phase is first separated, by the twice-modified vegetable oil solution in upper layer vacuum degree is 0.01-0.03MPa, temperature is
It is evaporated under reduced pressure at 60-80 DEG C, obtains twice-modified vegetable oil；The present invention is by modified vegetable oil of epoxidation in acid item
Under part, addition reaction occurs with organic acid, epoxy ring-opening obtains twice-modified vegetable oil, vegetable oil by primary modified and
After twice-modified, C=C double bond in vegetable oil was not only eliminated, but also replaced the glycerol in vegetable oil molecule, to obtain oxygen
Change the preferable modified vegetable oil of stability；
(5) by the obtained twice-modified vegetable oil of step (4), ionic liquid, antioxidant, emulsifier, sodium carbonate and hydrochloric acid according to
In secondary addition reactor, 30-60min is stirred at 80-100 DEG C, 300-500r/min, obtains lubricant.Sodium carbonate and hydrochloric acid
Reaction is exothermic reaction and generates gas, the heat of releasing can speed up ionic liquid, antioxidant, emulsifier and modified plant
Object oil is uniformly mixed, while the gas generated can remove the impurity in modified vegetable oil, makes the quality of lubricant obtained
It is more excellent.
As optimization, the mass fraction of dilute hydrochloric acid is 5-15% in step (1) and step (2).
As optimization, the mass fraction of sodium hydroxide solution is 5-10% in step (3) and step (4).
Compared with prior art, the beneficial effects of the present invention are:
First is that a kind of preparation method of biodegradable environment protective lubricant of the present invention, the present invention is first by vegetable oil and methanol
Ester exchange reaction occurs, the glyceryl in long chain fatty acids, the plant that secondly will be obtained after ester exchange reaction are replaced with methyl
Object soyate and trimethylolethane carry out ester exchange reaction again, replace vegetable oil molecule with the polyalcohol without β-H
In glycerol, be improved the stability of vegetable oil, again using glacial acetic acid reacted with hydrogen peroxide generation Peracetic acid, by one
Secondary modified vegetable oil is reacted with Peracetic acid generates modified vegetable oil of epoxidation, to eliminate the double bond in vegetable oil, finally
In acid condition by modified vegetable oil of epoxidation, addition reaction occurs with organic acid, obtains twice-modified vegetable oil, plant
Object oil had not only eliminated C=C double bond in vegetable oil, but also replaced in vegetable oil molecule after being once modified and is twice-modified
Glycerol, to obtain the preferable modified vegetable oil of oxidation stability；
Second is that a kind of biodegradable environment protective lubricant of the present invention, the present invention use oil based on modified vegetable oil, tool
There is good biological degradability, antioxidant can not only inhibit peroxide, and peroxynitrite decomposition compound, and can remove again
Oxygen radical is reacted with peroxy radical, is prevented the generation and transfer of peroxide in aliphatic oxygenation reaction process, is made lubricant
With good antioxidant effect；Emulsifier can enhance the compatibility of each component and modified vegetable oil, and it is equal to be conducive to each component
Even dispersion；When the lubricant is used for mechanical equipment, the ionic liquid in the lubricant is easy to occur on mechanical equipment surface
Complicated friction chemical reaction and generate one layer of friction reaction film, to make the new lubricant with good lubricant effect.
Specific embodiment
Below in conjunction with the embodiment of the present invention, technical scheme in the embodiment of the invention is clearly and completely described,
Obviously, described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based in the present invention
Embodiment, every other embodiment obtained by those of ordinary skill in the art without making creative efforts, all
Belong to the scope of protection of the invention.
Embodiment 1:
A kind of biodegradable environment protective lubricant, the lubricant include the component of following parts by weight: modified linseed oil 30
Part, 3 parts of zinc dialkyl dithiophosphate, 2 parts of lignosulfonates, 1 part of sodium carbonate, 3 parts of hydrochloric acid and 1- ethyl-3-methylimidazole
1 part of tetrafluoroborate ion liquid, modified linseed oil passes through methanol, trimethylolethane, glacial acetic acid, hydrogen peroxide by linseed oil
It is made with modified with organic acids.
Prepare a kind of biodegradable environment protective lubricant using above-mentioned raw materials, the preparation method of the lubricant include with
Lower step:
(1) it takes linseed oil to be added in flask, after being heated to 50 DEG C, flask is added in methanol and sodium hydroxide under stirring conditions
In, the ratio between amount of substance of linseed oil and methanol is 1:4, and the quality of sodium hydroxide is the 0.5% of linseed oil and methanol gross mass,
60min is reacted at 50 DEG C, reaction mixture is transferred in separatory funnel by cooled to room temperature, is added into separatory funnel
Enter dilute hydrochloric acid and be neutralized to neutrality, the mass fraction of dilute hydrochloric acid is 5%, and stratification first separates lower layer's water phase, by upper layer linseed oil
Fatty acid methyl ester solution is evaporated under reduced pressure in the case where vacuum degree is 0.01MPa, temperature is 30 DEG C, obtains linseed oil fatty acid first
Ester；
(2) the resulting linseed oil fatty acid methyl esters of step (1) is added in flask, is heated to 60 DEG C, under stirring conditions will
Trimethylolethane is added in flask, is then rapidly added sodium ethoxide again, linseed oil fatty acid methyl esters and trimethylolethane
The ratio between amount of substance is 3:1, and the quality of sodium ethoxide is the 0.8% of linseed oil fatty acid methyl esters and trimethylolethane gross mass,
1h is reacted at 60 DEG C, reaction mixture is transferred in separatory funnel by cooled to room temperature, and dilute salt is added into separatory funnel
Acid is neutralized to neutrality, and the mass fraction of dilute hydrochloric acid is 5%, and stratification first separates lower layer's water phase, and upper layer is once modified flax
Oily mixed solution is evaporated under reduced pressure in the case where vacuum degree is 0.01MPa, temperature is 60 DEG C, obtains once being modified linseed oil；
(3) the resulting primary modified linseed oil of step (2) is added in flask, 40 DEG C is heated to, under stirring conditions, by ice
Acetic acid, hydrogen peroxide and the concentrated sulfuric acid are added dropwise in flask simultaneously respectively, and rate of addition is 20 drops/minute, are once modified flax
The ratio between amount of substance of oil, glacial acetic acid and hydrogen peroxide is 1:4:4, and the quality of the concentrated sulfuric acid is primary modified linseed oil, glacial acetic acid
With the 0.5% of hydrogen peroxide gross mass, after being added dropwise, 3h, cooled to room temperature, by reaction mixture are reacted at 60 DEG C
It is transferred in separatory funnel, sodium hydroxide solution is added into separatory funnel and is neutralized to neutrality, the quality point of sodium hydroxide solution
Number is 5%, and stratification first separates lower layer's water phase, collects upper layer epoxidation and is once modified linseed oil；
(4) epoxidation that step (3) are collected once is modified linseed oil to refund in flask, then organic acid and dense is added into flask
Sulfuric acid, the ratio between the amount of substance that epoxidation is once modified linseed oil and organic acid is 1:4, and the quality of the concentrated sulfuric acid is that epoxidation is primary
The 0.2% of modified linseed oil and organic acid gross mass reacts 2h under conditions of stirring, 70 DEG C, and cooled to room temperature will be anti-
It answers mixed liquor to be transferred in separatory funnel, sodium hydroxide solution is added into separatory funnel and is neutralized to neutrality, sodium hydroxide solution
Mass fraction be 5%, stratification first separates lower layer's water phase, is in vacuum degree by the twice-modified flax oil solution in upper layer
0.01MPa, temperature are to be evaporated under reduced pressure at 60 DEG C, obtain twice-modified linseed oil；
(5) by obtained 30 parts of the modified linseed oil of step (4), 3 parts of zinc dialkyl dithiophosphate, 2 parts of lignosulfonates,
1 part of 1 part of sodium carbonate, 3 parts of hydrochloric acid and 1- ethyl-3-methylimidazole tetrafluoroborate ion liquid sequentially add in reactor,
80 DEG C, stir 30min under 300r/min, obtain lubricant.
Embodiment 2:
A kind of biodegradable environment protective lubricant, the lubricant include the component of following parts by weight: modified cottonseed oil 35
Part, double 4 parts of the octadecyl esters of thio-2 acid, 3 parts of contracting methylcellulose, 1.5 parts of sodium carbonate, 3.5 parts of hydrochloric acid and 1- butyl -3- methyl
2 parts of imidazoles chloride salt ions liquid, modified cottonseed oil by cottonseed oil by methanol, trimethylolethane, glacial acetic acid, hydrogen peroxide and
Modified with organic acids is made.
Prepare a kind of biodegradable environment protective lubricant using above-mentioned raw materials, the preparation method of the lubricant include with
Lower step:
(1) it takes cottonseed oil to be added in flask, after being heated to 55 DEG C, flask is added in methanol and sodium hydroxide under stirring conditions
In, the ratio between amount of substance of cottonseed oil and methanol is 1:4.5, and the quality of sodium hydroxide is cottonseed oil and methanol gross mass
0.6%, 65min is reacted at 55 DEG C, reaction mixture is transferred in separatory funnel by cooled to room temperature, to separatory funnel
Middle addition dilute hydrochloric acid is neutralized to neutrality, and the mass fraction of dilute hydrochloric acid is 6%, and stratification first separates lower layer's water phase, by upper layer cotton
Seed oil fatty acid methyl ester solution is evaporated under reduced pressure in the case where vacuum degree is 0.015MPa, temperature is 32 DEG C, obtains cottonseed oil and fat
Sour methyl esters；
(2) the resulting cottonseed oil fatty acid methyl esters of step (1) is added in flask, is heated to 65 DEG C, under stirring conditions will
Trimethylolethane is added in flask, is then rapidly added sodium ethoxide again, cottonseed oil fatty acid methyl esters and trimethylolethane
The ratio between amount of substance is 3.5:1, and the quality of sodium ethoxide is the 0.9% of cottonseed oil fatty acid methyl esters and trimethylolethane gross mass,
1.2h is reacted at 65 DEG C, reaction mixture is transferred in separatory funnel by cooled to room temperature, is added into separatory funnel
Dilute hydrochloric acid is neutralized to neutrality, and the mass fraction of dilute hydrochloric acid is 6%, and stratification first separates lower layer's water phase, and upper layer is once modified
Cottonseed oil mixed solution is evaporated under reduced pressure in the case where vacuum degree is 0.015MPa, temperature is 65 DEG C, obtains once being modified cottonseed oil；
(3) the resulting primary modified cottonseed oil of step (2) is added in flask, 45 DEG C is heated to, under stirring conditions, by ice
Acetic acid, hydrogen peroxide and the concentrated sulfuric acid are added dropwise in flask simultaneously respectively, and rate of addition is 21 drops/minute, an improved plant
The ratio between amount of substance of oil, glacial acetic acid and hydrogen peroxide is 1:4.2:4.2, and the quality of the concentrated sulfuric acid is primary modified cottonseed oil, ice
The 0.6% of acetic acid and hydrogen peroxide gross mass after being added dropwise, reacts 3.5h at 62 DEG C, and cooled to room temperature will react
Mixed liquor is transferred in separatory funnel, and sodium hydroxide solution is added into separatory funnel and is neutralized to neutrality, sodium hydroxide solution
Mass fraction is 6%, stratification, first separates lower layer's water phase, collects upper layer epoxidation and is once modified cottonseed oil；
(4) epoxidation that step (3) are collected once is modified cottonseed oil to refund in flask, then organic acid and dense is added into flask
Sulfuric acid, the ratio between the amount of substance that epoxidation is once modified cottonseed oil and organic acid is 1:4.2, and the quality of the concentrated sulfuric acid is epoxidation one
The 0.25% of secondary modified cottonseed oil and organic acid gross mass reacts 2.5h under conditions of stirring, 72 DEG C, cooled to room temperature,
Reaction mixture is transferred in separatory funnel, sodium hydroxide solution is added into separatory funnel and is neutralized to neutrality, sodium hydroxide
The mass fraction of solution is 6%, and stratification first separates lower layer's water phase, is in vacuum degree by the twice-modified cottonseed oil solution in upper layer
0.015MPa, temperature are to be evaporated under reduced pressure at 65 DEG C, obtain twice-modified cottonseed oil；
(5) by obtained 35 parts of the modified cottonseed oil of step (4), double 4 parts of the octadecyl ester of thio-2 acid, 3 parts of contracting methylcellulose,
2 parts of ionic liquid of 1.5 parts of sodium carbonate, 3.5 parts of hydrochloric acid and 1- butyl -3- methylimidazole villaumite sequentially add in reactor, 85
DEG C, stir 35min under 350r/min, obtain lubricant.
Embodiment 3:
A kind of biodegradable environment protective lubricant, the lubricant include the component of following parts by weight: modified rice bran oil 40
Part, 5 parts of dodecyl selenium, 6 parts of diglycerol polypropylene glycol ether, 1.5 parts of sodium carbonate, 4 parts of hydrochloric acid and 1- butyl -3- methylimidazole six
5 parts of fluorophosphate ionic liquid, modified rice bran oil by rice bran oil by methanol, trimethylolethane, glacial acetic acid, hydrogen peroxide and
Modified with organic acids is made.
Prepare a kind of biodegradable environment protective lubricant using above-mentioned raw materials, the preparation method of the lubricant include with
Lower step:
(1) it takes rice bran oil to be added in flask, after being heated to 60 DEG C, flask is added in methanol and sodium hydroxide under stirring conditions
In, the ratio between amount of substance of rice bran oil and methanol is 1:5, and the quality of sodium hydroxide is the 0.8% of rice bran oil and methanol gross mass,
75min is reacted at 60 DEG C, reaction mixture is transferred in separatory funnel by cooled to room temperature, is added into separatory funnel
Enter dilute hydrochloric acid and be neutralized to neutrality, the mass fraction of dilute hydrochloric acid is 10%, and stratification first separates lower layer's water phase, by upper layer rice bran oil
Fatty acid methyl ester solution is evaporated under reduced pressure in the case where vacuum degree is 0.02MPa, temperature is 35 DEG C, obtains rice bran oil fatty acid first
Ester；
(2) the resulting rice bran oil fatty acid methyl esters of step (1) is added in flask, is heated to 70 DEG C, under stirring conditions will
Trimethylolethane is added in flask, is then rapidly added sodium ethoxide again, rice bran oil fatty acid methyl esters and trimethylolethane
The ratio between amount of substance is 4:1, and the quality of sodium ethoxide is the 1.0% of rice bran oil fatty acid methyl esters and trimethylolethane gross mass,
1.5h is reacted at 70 DEG C, reaction mixture is transferred in separatory funnel by cooled to room temperature, is added into separatory funnel dilute
Hydrochloric acid is neutralized to neutrality, and the mass fraction of dilute hydrochloric acid is 10%, and stratification first separates lower layer's water phase, and upper layer is once modified rice
Oil extracted from rice husks mixed solution is evaporated under reduced pressure in the case where vacuum degree is 0.02MPa, temperature is 70 DEG C, obtains once being modified rice bran oil；
(3) the resulting primary modified rice bran oil of step (2) is added in flask, 50 DEG C is heated to, under stirring conditions, by ice
Acetic acid, hydrogen peroxide and the concentrated sulfuric acid are added dropwise in flask simultaneously respectively, and rate of addition is 23 drops/minute, are once modified rice bran
The ratio between amount of substance of oil, glacial acetic acid and hydrogen peroxide is 1:4.5:4.5, and the quality of the concentrated sulfuric acid is primary modified rice bran oil, ice
The 0.8% of acetic acid and hydrogen peroxide gross mass after being added dropwise, reacts 4h at 65 DEG C, and cooled to room temperature is mixed by reaction
It closes liquid to be transferred in separatory funnel, sodium hydroxide solution is added into separatory funnel and is neutralized to neutrality, the matter of sodium hydroxide solution
Measuring score is 8%, and stratification first separates lower layer's water phase, collects upper layer epoxidation and is once modified rice bran oil；
(4) epoxidation that step (3) are collected once is modified rice bran oil to refund in flask, then organic acid and dense is added into flask
Sulfuric acid, the ratio between the amount of substance that epoxidation is once modified rice bran oil and organic acid is 1:4.5, and the quality of the concentrated sulfuric acid is epoxidation one
The 0.35% of secondary modified rice bran oil and organic acid gross mass reacts 3h under conditions of stirring, 75 DEG C, and cooled to room temperature will
Reaction mixture is transferred in separatory funnel, and sodium hydroxide solution is added into separatory funnel and is neutralized to neutrality, sodium hydroxide is molten
The mass fraction of liquid is 8%, and stratification first separates lower layer's water phase, is in vacuum degree by the twice-modified rice bran oil solution in upper layer
0.02MPa, temperature are to be evaporated under reduced pressure at 70 DEG C, obtain twice-modified rice bran oil；
(5) by obtained 40 parts of the modified rice bran oil of step (4), 5 parts of dodecyl selenium, 6 parts of diglycerol polypropylene glycol ether, carbonic acid
1.5 parts of sodium, 4 parts of hydrochloric acid and 5 parts of ionic liquid of -3- methylimidazole hexafluorophosphoric acid of 1- butyl sequentially add in reactor, 90
DEG C, stir 45min under 400r/min, obtain lubricant.
Embodiment 4:
A kind of biodegradable environment protective lubricant, the lubricant include the component of following parts by weight: modified camellia seed oil
45 parts, 7 parts of DBPC 2,6 ditertiary butyl p cresol, 8 parts of polyoxyethylene oleic acid ester, 2.5 parts of sodium carbonate, 4.5 parts of hydrochloric acid and quaternary phosphonium salt phosphorus
9 parts of acid esters ionic liquid, modified camellia seed oil by camellia seed oil by methanol, trimethylolethane, glacial acetic acid, hydrogen peroxide and
Modified with organic acids is made.
A kind of preparation method of biodegradable environment protective lubricant, the preparation of the lubricant are prepared using above-mentioned raw materials
Method the following steps are included:
(1) it takes camellia seed oil to be added in flask, after being heated to 65 DEG C, methanol and sodium hydroxide is added burns under stirring conditions
In bottle, the ratio between amount of substance of camellia seed oil and methanol is 1:5.5, and the quality of sodium hydroxide is vegetable oil and methanol gross mass
0.9%, 85min is reacted at 65 DEG C, reaction mixture is transferred in separatory funnel by cooled to room temperature, to separatory funnel
Middle addition dilute hydrochloric acid is neutralized to neutrality, and the mass fraction of dilute hydrochloric acid is 12%, and stratification first separates lower layer's water phase, upper layer is planted
Object soyate solution is evaporated under reduced pressure in the case where vacuum degree is 0.025MPa, temperature is 38 DEG C, obtains tea seed grease
Fatty acid methyl esters；
(2) the resulting camellia seed oil fatty acid methyl ester of step (1) is added in flask, is heated to 78 DEG C, under stirring conditions
Trimethylolethane is added in flask, is then rapidly added sodium ethoxide, camellia seed oil fatty acid methyl ester and trihydroxy methyl second again
The ratio between amount of substance of alkane is 4.5:1, and the quality of sodium ethoxide is camellia seed oil fatty acid methyl ester and trimethylolethane gross mass
1.1%, 1.8h is reacted at 75 DEG C, reaction mixture is transferred in separatory funnel by cooled to room temperature, to liquid separation leak
Dilute hydrochloric acid is added in bucket and is neutralized to neutrality, the mass fraction of dilute hydrochloric acid is 12%, and stratification first separates lower layer's water phase, by upper layer
Primary modified camellia seed oil mixed solution is evaporated under reduced pressure in the case where vacuum degree is 0.025MPa, temperature is 75 DEG C, is obtained primary
Modified camellia seed oil；
(3) the resulting primary modified camellia seed oil of step (2) is added in flask, is heated to 55 DEG C, it under stirring conditions, will
Glacial acetic acid, hydrogen peroxide and the concentrated sulfuric acid are added dropwise in flask simultaneously respectively, and rate of addition is 24 drops/minute, a modified oil
The ratio between amount of substance of tea-seed oil, glacial acetic acid and hydrogen peroxide is 1:4.8:4.8, and the quality of the concentrated sulfuric acid is an improved plant
The 0.9% of oily, glacial acetic acid and hydrogen peroxide gross mass after being added dropwise, reacts 4.5h, cooled to room temperature will at 68 DEG C
Reaction mixture is transferred in separatory funnel, and sodium hydroxide solution is added into separatory funnel and is neutralized to neutrality, sodium hydroxide is molten
The mass fraction of liquid is 9%, and stratification first separates lower layer's water phase, collects upper layer epoxidation and is once modified camellia seed oil；
(4) by step (3) collect epoxidation once be modified camellia seed oil refund in flask, then into flask be added organic acid and
The concentrated sulfuric acid, the ratio between the amount of substance that epoxidation is once modified camellia seed oil and organic acid is 1:4.8, and the quality of the concentrated sulfuric acid is epoxy
Change the 0.45% of primary modified camellia seed oil and organic acid gross mass, reacts 3.5h, natural cooling under conditions of stirring, 78 DEG C
To room temperature, reaction mixture is transferred in separatory funnel, sodium hydroxide solution is added into separatory funnel and is neutralized to neutrality, hydrogen
The mass fraction of sodium hydroxide solution is 9%, and stratification first separates lower layer's water phase, and the twice-modified camellia seed oil solution in upper layer is existed
Vacuum degree is 0.025MPa, temperature is to be evaporated under reduced pressure at 75 DEG C, obtains twice-modified camellia seed oil；
(5) by obtained 45 parts of the modified camellia seed oil of step (4), 7 parts of DBPC 2,6 ditertiary butyl p cresol, polyoxyethylene oleic acid ester
9 parts of 8 parts, 2.5 parts of sodium carbonate, 4.5 parts of hydrochloric acid and quaternary phosphonium salt phosphate ion liquid sequentially add in reactor, 95 DEG C,
55min is stirred under 450r/min, obtains lubricant.
Embodiment 5:
A kind of biodegradable environment protective lubricant, the lubricant include the component of following parts by weight: modified coconut oil 50
Part, 8 parts of zinc dialkyl dithiocarbamate, 10 parts of fatty amide polyoxyethylene ether, 3 parts of sodium carbonate, 5 parts of hydrochloric acid and 1- oneself
10 parts of ionic liquid of base -3- methylimidazole hexafluorophosphoric acid, modified coconut oil by coconut oil by methanol, trimethylolethane,
Glacial acetic acid, hydrogen peroxide and modified with organic acids are made.
Prepare a kind of biodegradable environment protective lubricant using above-mentioned raw materials, the preparation method of the lubricant include with
Lower step:
(1) it takes coconut oil to be added in flask, after being heated to 70 DEG C, flask is added in methanol and sodium hydroxide under stirring conditions
In, the ratio between amount of substance of coconut oil and methanol is 1:6, and the quality of sodium hydroxide is the 1% of coconut oil and methanol gross mass,
90min is reacted at 70 DEG C, reaction mixture is transferred in separatory funnel by cooled to room temperature, is added into separatory funnel
Dilute hydrochloric acid is neutralized to neutrality, and the mass fraction of dilute hydrochloric acid is 15%, and stratification first separates lower layer's water phase, by upper layer coconut grease
Fatty acid methyl esters solution is evaporated under reduced pressure in the case where vacuum degree is 0.03MPa, temperature is 40 DEG C, obtains coconut oil fatty acid methyl ester；
(2) the resulting coconut oil fatty acid methyl ester of step (1) is added in flask, is heated to 80 DEG C, under stirring conditions will
Trimethylolethane is added in flask, is then rapidly added sodium ethoxide again, coconut oil fatty acid methyl ester and trimethylolethane
The ratio between amount of substance is 5:1, and the quality of sodium ethoxide is the 1.2% of coconut oil fatty acid methyl ester and trimethylolethane gross mass,
2h is reacted at 80 DEG C, reaction mixture is transferred in separatory funnel by cooled to room temperature, and dilute salt is added into separatory funnel
Acid is neutralized to neutrality, and the mass fraction of dilute hydrochloric acid is 15%, and stratification first separates lower layer's water phase, and upper layer is once modified coconut
Oily mixed solution is evaporated under reduced pressure in the case where vacuum degree is 0.03MPa, temperature is 80 DEG C, obtains once being modified coconut oil；
(3) the resulting primary modified coconut oil of step (2) is added in flask, 60 DEG C is heated to, under stirring conditions, by ice
Acetic acid, hydrogen peroxide and the concentrated sulfuric acid are added dropwise in flask simultaneously respectively, and rate of addition is 25 drops/minute, are once modified coconut
The ratio between amount of substance of oil, glacial acetic acid and hydrogen peroxide is 1:5:5, and the quality of the concentrated sulfuric acid is primary modified coconut oil, glacial acetic acid
With the 1% of hydrogen peroxide gross mass, after being added dropwise, 5h is reacted at 70 DEG C, cooled to room temperature turns reaction mixture
It moves in separatory funnel, sodium hydroxide solution is added into separatory funnel and is neutralized to neutrality, the mass fraction of sodium hydroxide solution
It is 10%, stratification first separates lower layer's water phase, collects upper layer epoxidation and is once modified coconut oil；
(4) modified vegetable oil of epoxidation that step (3) are collected is refunded in flask, then organic acid and dense is added into flask
The ratio between amount of substance of sulfuric acid, modified vegetable oil of epoxidation and organic acid is 1:5, and the quality of the concentrated sulfuric acid is that epoxidation is primary
The 0.5% of modified vegetable oil and organic acid gross mass reacts 4h under conditions of stirring, 80 DEG C, and cooled to room temperature will be anti-
It answers mixed liquor to be transferred in separatory funnel, sodium hydroxide solution is added into separatory funnel and is neutralized to neutrality, sodium hydroxide solution
Mass fraction be 10%, stratification first separates lower layer's water phase, is in vacuum degree by the twice-modified vegetable oil solution in upper layer
0.03MPa, temperature are to be evaporated under reduced pressure at 80 DEG C, obtain twice-modified vegetable oil；
(5) by obtained 50 parts of the modified coconut oil of step (4), 8 parts of zinc dialkyl dithiocarbamate, fatty acid amide polyoxy
10 parts of vinethene, 3 parts of sodium carbonate, 5 parts of hydrochloric acid and 10 parts of ionic liquid of -3- methylimidazole hexafluorophosphoric acid of 1- hexyl sequentially add
In reactor, 60min is stirred at 100 DEG C, 500r/min, obtains lubricant.
Comparative example 1:
A kind of novel lubricant, the novel lubricant include the component of following parts by weight: 40 parts of rice bran oil, dodecyl selenium 5
Part, 6 parts of diglycerol polypropylene glycol ether, 1.5 parts of sodium carbonate, 4 parts of hydrochloric acid and 1- butyl -3- methylimidazole hexafluorophosphate ionic liquid
5 parts of body.
Prepare a kind of novel lubricant using above-mentioned raw materials, the novel lubricant the preparation method comprises the following steps:
By 40 parts of rice bran oil, 5 parts of dodecyl selenium, 6 parts of diglycerol polypropylene glycol ether, 1.5 parts of sodium carbonate, 4 parts of hydrochloric acid and 1- fourth
5 parts of ionic liquid of base -3- methylimidazole hexafluorophosphoric acid sequentially adds in reactor, stirs at 90 DEG C, 400r/min
45min obtains novel lubricant.
Comparative example 1 with embodiment 3 the difference is that be not modified to vegetable oil rice bran oil, remaining and 3 phase of embodiment
Together.
Comparative example 2:
A kind of novel lubricant, the novel lubricant include the component of following parts by weight: modified 40 parts of rice bran oil, dodecyl
5 parts of selenium, 6 parts of diglycerol polypropylene glycol ether, 1.5 parts of sodium carbonate and 4 parts of hydrochloric acid, modified rice bran oil pass through methanol, three by rice bran oil
Hydroxymethyl ethane, glacial acetic acid, hydrogen peroxide and modified with organic acids are made.
Prepare a kind of novel lubricant using above-mentioned raw materials, the preparation method of the novel lubricant the following steps are included:
(1) it takes rice bran oil to be added in flask, after being heated to 60 DEG C, flask is added in methanol and sodium hydroxide under stirring conditions
In, the ratio between amount of substance of rice bran oil and methanol is 1:5, and the quality of sodium hydroxide is the 0.8% of rice bran oil and methanol gross mass,
75min is reacted at 60 DEG C, reaction mixture is transferred in separatory funnel by cooled to room temperature, is added into separatory funnel
Enter dilute hydrochloric acid and be neutralized to neutrality, the mass fraction of dilute hydrochloric acid is 10%, and stratification first separates lower layer's water phase, by upper layer rice bran oil
Fatty acid methyl ester solution is evaporated under reduced pressure in the case where vacuum degree is 0.02MPa, temperature is 35 DEG C, obtains rice bran oil fatty acid first
Ester；
(2) the resulting rice bran oil fatty acid methyl esters of step (1) is added in flask, is heated to 70 DEG C, under stirring conditions will
Trimethylolethane is added in flask, is then rapidly added sodium ethoxide again, rice bran oil fatty acid methyl esters and trimethylolethane
The ratio between amount of substance is 4:1, and the quality of sodium ethoxide is the 1.0% of rice bran oil fatty acid methyl esters and trimethylolethane gross mass,
1.5h is reacted at 70 DEG C, reaction mixture is transferred in separatory funnel by cooled to room temperature, is added into separatory funnel dilute
Hydrochloric acid is neutralized to neutrality, and the mass fraction of dilute hydrochloric acid is 10%, and stratification first separates lower layer's water phase, and upper layer is once modified rice
Oil extracted from rice husks mixed solution is evaporated under reduced pressure in the case where vacuum degree is 0.02MPa, temperature is 70 DEG C, obtains once being modified rice bran oil；
(3) the resulting primary modified rice bran oil of step (2) is added in flask, 50 DEG C is heated to, under stirring conditions, by ice
Acetic acid, hydrogen peroxide and the concentrated sulfuric acid are added dropwise in flask simultaneously respectively, and rate of addition is 23 drops/minute, are once modified rice bran
The ratio between amount of substance of oil, glacial acetic acid and hydrogen peroxide is 1:4.5:4.5, and the quality of the concentrated sulfuric acid is primary modified rice bran oil, ice
The 0.8% of acetic acid and hydrogen peroxide gross mass after being added dropwise, reacts 4h at 65 DEG C, and cooled to room temperature is mixed by reaction
It closes liquid to be transferred in separatory funnel, sodium hydroxide solution is added into separatory funnel and is neutralized to neutrality, the matter of sodium hydroxide solution
Measuring score is 8%, and stratification first separates lower layer's water phase, collects upper layer epoxidation and is once modified rice bran oil；
(4) epoxidation that step (3) are collected once is modified rice bran oil to refund in flask, then organic acid and dense is added into flask
Sulfuric acid, the ratio between the amount of substance that epoxidation is once modified rice bran oil and organic acid is 1:4.5, and the quality of the concentrated sulfuric acid is epoxidation one
The 0.35% of secondary modified rice bran oil and organic acid gross mass reacts 3h under conditions of stirring, 75 DEG C, and cooled to room temperature will
Reaction mixture is transferred in separatory funnel, and sodium hydroxide solution is added into separatory funnel and is neutralized to neutrality, sodium hydroxide is molten
The mass fraction of liquid is 8%, and stratification first separates lower layer's water phase, is in vacuum degree by the twice-modified rice bran oil solution in upper layer
0.02MPa, temperature are to be evaporated under reduced pressure at 70 DEG C, obtain twice-modified rice bran oil；
(5) by obtained 40 parts of the modified rice bran oil of step (4), 5 parts of dodecyl selenium, 6 parts of diglycerol polypropylene glycol ether, carbonic acid
1.5 parts and 4 parts of hydrochloric acid of sodium sequentially add in reactor, stir 45min at 90 DEG C, 400r/min, obtain novel lubricant.
Comparative example 2 and embodiment 3 are except that be not used 1- butyl -3- methylimidazole hexafluorophosphoric acid salt ion in raw material
Liquid, remaining is same as Example 3.
Effect example:
(1) laboratory sample: new obtained by novel lubricant obtained by the embodiment of the present invention 1 to 5 and comparative example 1, comparative example 2
Type lubricant.
(2) experimental method:
(a) biological degradability: according to the experimental method of the CEC L-33-A-93 of the European Community (predecessor is CEC L-33-T-82) into
Row test, test result are shown in Table 1；
(b) Bowden formula (horizontal linear is reciprocating) adheres to sliding test: test film is immersed in each laboratory sample of room temperature
Afterwards, it places 20 minutes in 80 DEG C of thermostat, using the test film after generation lubricating film coated, is covered according to the investigation of following projects
The dhering strength of film；Test film material: SCM440, experiment plate shape: 100mm × 80mm × 5mm, friction ball: SUJ-2,3/16
Inch φ, test temperature: 100 DEG C, load: 3kg, sliding speed: 3.88mm/ seconds, evaluation: measuring average friction coefficient and arrives hair
Sliding number until raw burn erosion, test result are shown in Table 1.
Table 1
(3) experimental result: from table 1 it follows that the biodegrade of novel lubricant obtained by the embodiment of the present invention 1 to 5
Rate 98% or more, averagely rub coefficient 0.04 and hereinafter, sliding number until ablation occurs at 208 times and
More than, and the biological degradation rate of novel lubricant obtained by comparative example 1 and comparative example 2 is respectively 90% and 93%, average friction
Coefficient is respectively 0.10 and 0.12, and the sliding number until ablation occurs is respectively 90 times and 85 times, the experimental results showed that, this
Novel lubricant obtained by inventive embodiments 1 to 5 has good biological degradability and lubricant effect.
Comparative example 1, due to not being modified to vegetable oil, makes novel lubricating obtained compared with the embodiment of the present invention 1 to 5
The lubricant effect of the lubricant effect of agent novel lubricant not as good as obtained by the embodiment of the present invention 1 to 5.
Comparative example 2, since ionic liquid being not used in raw material, makes novel profit obtained compared with the embodiment of the present invention 1 to 5
The lubricant effect of the lubricant effect of lubrication prescription novel lubricant not as good as obtained by the embodiment of the present invention 1 to 5.
It is obvious to a person skilled in the art that invention is not limited to the details of the above exemplary embodiments, Er Qie
In the case where without departing substantially from spirit or essential attributes of the invention, the present invention can be realized in other specific forms.Therefore, no matter
From the point of view of which point, the present embodiments are to be considered as illustrative and not restrictive, and the scope of the present invention is by appended power
Benefit requires rather than above description limits, it is intended that all by what is fallen within the meaning and scope of the equivalent elements of the claims
Variation is included within the present invention.Any label in claim should not be construed as limiting the claims involved.
Claims (10)
1. a kind of biodegradable environment protective lubricant, which is characterized in that the lubricant includes the component of following parts by weight:
30-50 parts of vegetable oil, 3-8 parts of antioxidant, 2-10 parts of emulsifier, 1-3 parts of sodium carbonate and 3-5 parts of hydrochloric acid.
2. the biodegradable environment protective lubricant of one kind according to claim 1, it is characterised in that: the new lubricant
It further include the ionic liquid of 1-10 parts by weight, the ionic liquid is 1- ethyl-3-methylimidazole tetrafluoroborate ionic liquid
Body, 1- butyl -3- methylimidazole villaumite ionic liquid, 1- butyl -3- methylimidazole hexafluorophosphoric acid ionic liquid, quaternary phosphonium salt phosphorus
Any one in acid esters ionic liquid or 1- hexyl -3- methylimidazole hexafluorophosphoric acid ionic liquid.
3. the biodegradable environment protective lubricant of one kind according to claim 1 or 2, it is characterised in that: the plant
Oil be modified vegetable oil, the modified vegetable oil by vegetable oil by methanol, trimethylolethane, glacial acetic acid, hydrogen peroxide and
Modified with organic acids is made.
4. the biodegradable environment protective lubricant of one kind according to claim 3, it is characterised in that: the vegetable oil is
Any one in linseed oil, cottonseed oil, rice bran oil, camellia seed oil or coconut oil.
5. the biodegradable environment protective lubricant of one kind according to claim 4, it is characterised in that: the antioxidant is
The double octadecyl esters of zinc dialkyl dithiophosphate, thio-2 acid, dodecyl selenium, DBPC 2,6 ditertiary butyl p cresol or dialkyl group two
Any one in zinc thiocarbamate, the emulsifier are lignosulfonates, contracting methylcellulose, diglycerol poly- the third two
Any one in alcohol ether, polyoxyethylene oleic acid ester or fatty amide polyoxyethylene ether.
6. a kind of preparation method of biodegradable environment protective lubricant, which is characterized in that the preparation method packet of the lubricant
Include following steps:
(1) preparation of Plant Oil Fatty Acid Methyl Ester；
The preparation of (2) modified vegetable oils；
(3) preparation of modified vegetable oil of epoxidation；
(4) preparation of twice-modified vegetable oil；
(5) by the obtained twice-modified vegetable oil of step (4), ionic liquid, antioxidant, emulsifier, sodium carbonate and hydrochloric acid according to
In secondary addition reactor, stirring obtains lubricant.
7. the preparation method of the biodegradable environment protective lubricant of one kind according to claim 6, which is characterized in that should
The preparation method of lubricant the following steps are included:
(1) it takes vegetable oil to be added in flask, methanol and sodium hydroxide is added in flask under stirring conditions, heating reaction,
Cooling, liquid separation, vacuum distillation obtains Plant Oil Fatty Acid Methyl Ester；
(2) the resulting Plant Oil Fatty Acid Methyl Ester of step (1) is added in flask, under stirring conditions by trimethylolethane
It is added in flask, then is rapidly added sodium ethoxide, heating reaction is cooling, and liquid separation is evaporated under reduced pressure, obtains a modified vegetable oil；
(3) the resulting modified vegetable oil of step (2) is added in flask, under stirring conditions, by glacial acetic acid, peroxidating
Hydrogen and the concentrated sulfuric acid are added dropwise in flask simultaneously respectively, heating reaction, cooling, and modified vegetable oil of epoxidation is collected in liquid separation；
(4) modified vegetable oil of epoxidation that step (3) are collected is refunded in flask, then organic acid and dense is added into flask
Sulfuric acid, stirring, heating reaction, cooling, liquid separation, vacuum distillation obtain twice-modified vegetable oil；
(5) by the obtained twice-modified vegetable oil of step (4), ionic liquid, antioxidant, emulsifier, sodium carbonate and hydrochloric acid according to
It in secondary addition reactor, heats, stirring obtains lubricant.
8. the preparation method of the biodegradable environment protective lubricant of one kind according to claim 7, which is characterized in that should
The preparation method of lubricant the following steps are included:
(1) it takes vegetable oil to be added in flask, after being heated to 50-70 DEG C, methanol and sodium hydroxide is added under stirring conditions
In flask, the ratio between amount of substance of the vegetable oil and methanol is 1:4-6, and the quality of the sodium hydroxide is vegetable oil and methanol
The 0.5-1% of gross mass, reacts 60-90min at 50-70 DEG C, and reaction mixture is transferred to liquid separation by cooled to room temperature
In funnel, dilute hydrochloric acid is added into separatory funnel and is neutralized to neutrality, stratification first separates lower layer's water phase, by upper layer vegetable oil
Fatty acid methyl ester solution is evaporated under reduced pressure in the case where vacuum degree is 0.01-0.03MPa, temperature is 30-40 DEG C, obtains vegetable fat
Fatty acid methyl esters；
(2) the resulting Plant Oil Fatty Acid Methyl Ester of step (1) is added in flask, is heated to 60-80 DEG C, under stirring conditions
Trimethylolethane is added in flask, is then rapidly added sodium ethoxide, the Plant Oil Fatty Acid Methyl Ester and trihydroxy methyl again
The ratio between amount of substance of ethane is 3-5:1, and the quality of the sodium ethoxide is that Plant Oil Fatty Acid Methyl Ester and trimethylolethane are total
The 0.8-1.2% of quality, reacts 1-2h at 60-80 DEG C, and reaction mixture is transferred to separatory funnel by cooled to room temperature
In, dilute hydrochloric acid is added into separatory funnel and is neutralized to neutrality, stratification first separates lower layer's water phase, by upper layer once modified plant
Object oil mixed solution is evaporated under reduced pressure in the case where vacuum degree is 0.01-0.03MPa, temperature is 60-80 DEG C, obtains once modified plant
Object oil；
(3) the resulting modified vegetable oil of step (2) is added in flask, is heated to 40-60 DEG C, under stirring conditions,
Glacial acetic acid, hydrogen peroxide and the concentrated sulfuric acid are added dropwise in flask simultaneously respectively, rate of addition is 20-25 drop/minute, and described one
The ratio between amount of substance of secondary modified vegetable oil, glacial acetic acid and hydrogen peroxide is 1:4-5:4-5, and the quality of the concentrated sulfuric acid is primary
The 0.5-1% of modified vegetable oil, glacial acetic acid and hydrogen peroxide gross mass after being added dropwise, reacts 3-5h at 60-70 DEG C, natural
It is cooled to room temperature, reaction mixture is transferred in separatory funnel, be added into separatory funnel during sodium hydroxide solution is neutralized to
Property, stratification first separates lower layer's water phase, collects modified vegetable oil of upper layer epoxidation；
(4) modified vegetable oil of epoxidation that step (3) are collected is refunded in flask, then organic acid and dense is added into flask
The ratio between amount of substance of sulfuric acid, modified vegetable oil of the epoxidation and organic acid is 1:4-5, and the quality of the concentrated sulfuric acid is
The 0.2-0.5% of epoxidation a modified vegetable oil and organic acid gross mass reacts 2-4h under conditions of stirring, 70-80 DEG C,
Reaction mixture is transferred in separatory funnel by cooled to room temperature, and sodium hydroxide solution is added into separatory funnel and neutralizes
To neutrality, stratification first separates lower layer's water phase, by the twice-modified vegetable oil solution in upper layer vacuum degree be 0.01-
0.03MPa, temperature are to be evaporated under reduced pressure at 60-80 DEG C, obtain twice-modified vegetable oil；
(5) by the obtained twice-modified vegetable oil of step (4), ionic liquid, antioxidant, emulsifier, sodium carbonate and hydrochloric acid according to
In secondary addition reactor, 30-60min is stirred at 80-100 DEG C, 300-500r/min, obtains lubricant.
9. the preparation method of the biodegradable environment protective lubricant of one kind according to claim 8, it is characterised in that: institute
The mass fraction for stating dilute hydrochloric acid in step (1) and step (2) is 5-15%.
10. the preparation method of the biodegradable environment protective lubricant of one kind according to claim 8 or claim 9, feature exist
In: the mass fraction of sodium hydroxide solution is 5-10% in the step (3) and step (4).
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| CN112552989A (en) * | 2021-01-20 | 2021-03-26 | 安徽联亚新材料有限公司 | Biodegradable plant-based anti-wear lubricating oil and preparation method thereof |
| CN116286148A (en) * | 2023-03-17 | 2023-06-23 | 安徽中天石化股份有限公司 | Biodegradable gear lubricating grease and preparation method and application thereof |
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| CN109913300B (en) | 2022-12-16 |
| CN115746939A (en) | 2023-03-07 |
| CN115746939B (en) | 2023-11-17 |
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