CN109913300B - Biodegradable environment-friendly lubricant and preparation method thereof - Google Patents
Biodegradable environment-friendly lubricant and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a biodegradable environment-friendly lubricant and a preparation method thereof, wherein the lubricant comprises the following components: vegetable oil, an antioxidant, an emulsifier, sodium carbonate, hydrochloric acid and ionic liquid; the preparation method of the lubricant comprises the following steps: preparing vegetable oil fatty acid methyl ester; preparing primary modified vegetable oil; preparing epoxidized primary modified vegetable oil; preparing secondary modified vegetable oil; sequentially adding the secondary modified vegetable oil, the ionic liquid, the antioxidant, the emulsifier, the sodium carbonate and the hydrochloric acid into a reactor, and stirring to obtain a lubricant; after the vegetable oil is subjected to primary modification and secondary modification, C = C double bonds in the vegetable oil are eliminated, and glycerin in vegetable oil molecules is replaced, so that the modified vegetable oil with better oxidation stability is obtained.
Description
Technical Field
The invention relates to the technical field of lubricants, in particular to a biodegradable environment-friendly lubricant and a preparation method thereof.
Background
The lubricant plays a key role in reducing mechanical wear, prolonging the service life of equipment and the like, can be divided into liquid lubricants (mineral oil, synthetic oil, water-based oil, animal and vegetable oil), lubricating grease, solid lubricants (graphite, molybdenum disulfide) and gas lubricants (air, helium, nitrogen, hydrogen and the like) according to the material forms of the lubricant, has the characteristics of wider viscosity range, low noise, high thermal conductivity and the like compared with other lubricants, is widely applied to liquid lubricants, can be suitable for friction pairs and moving parts under various working conditions, and has the advantages of abundant product resources, low price and easy obtainment.
At the end of the 19 th century, mineral oil has gradually become the mainstream of lubricants, and after the 20 th century, the development of internal combustion engine and automobile industries, friction pairs need to work under severe conditions of high temperature and high pressure for a long time, which requires that lubricating oil have high working temperature range and performance stability, so synthetic oil has been widely used, wherein, silicone oil has wide temperature range and high viscosity index, and is widely used in the aerospace field, PAO (poly alpha olefin) and polyester, etc. are also used in the aircraft industry, these synthetic lubricants expand the use temperature range of liquid film lubrication from-70 ℃ to 300 ℃, but in the use process of synthetic lubricating oil, the defects of the synthetic lubricating oil, such as low polarity, poor boundary lubrication capability, limited high temperature use, etc., are discovered, and people are required to continuously strive for high performance lubricants. The environmental problems caused by the infiltration, leakage, overflow and improper treatment of a large amount of lubricating oil in the production, use and discharge processes seriously pollute soil and water resources and destroy the ecological environment and ecological balance, the environmental problems are more and more emphasized along with the increasing enhancement of the environmental crisis consciousness of people, and the development of the environment-friendly lubricating oil with biodegradability is an effective way for solving the problem and is a development direction of the future lubricating oil industry.
The vegetable oil-based lubricating oil has good sustainable productivity and biodegradability, low volatility and high flash point, is widely concerned by people, but the vegetable oil-based lubricating oil in the prior art has poor oxidation stability and needs to be further improved in lubricating effect, and the defects limit the further development of the vegetable oil-based lubricating oil.
Disclosure of Invention
The invention aims to provide a biodegradable environment-friendly lubricant and a preparation method thereof, which aim to solve the problems in the prior art.
In order to achieve the purpose, the invention provides the following technical scheme:
a biodegradable environment-friendly lubricant comprises the following components in 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.
Preferably, the novel lubricating oil also comprises 1-10 parts by weight of ionic liquid, wherein the ionic liquid is any one of 1-ethyl-3-methylimidazolium tetrafluoroborate ionic liquid, 1-butyl-3-methylimidazolium chloride ionic liquid, 1-butyl-3-methylimidazolium hexafluorophosphate ionic liquid, quaternary phosphonium phosphate ionic liquid or 1-hexyl-3-methylimidazolium hexafluorophosphate ionic liquid. When the lubricant is used for mechanical equipment, the ionic liquid in the lubricant is easy to generate a layer of friction reaction film on the surface of the mechanical equipment through complex friction chemical reaction, and the friction reaction film has lower shear strength and is relatively flat and smooth, so that the novel lubricating oil has a good lubricating effect.
Preferably, the vegetable oil is modified vegetable oil, and the modified vegetable oil is prepared by modifying vegetable oil with methanol, trimethylolethane, glacial acetic acid, hydrogen peroxide and organic acid. The modified vegetable oil is adopted as the base oil, has good biodegradability, and after a series of modifications, the vegetable oil eliminates C = C double bonds in the vegetable oil and replaces glycerin in the vegetable oil molecules, so that the modified vegetable oil with good oxidation stability is obtained.
Preferably, the vegetable oil is any one of linseed oil, cottonseed oil, rice bran oil, camellia seed oil or coconut oil.
Preferably, the antioxidant is any one of zinc dialkyl dithiophosphate, dioctadecyl thiodipropionate, dodecyl selenium, 2, 6-di-tert-butyl-p-cresol or zinc dialkyl dithiocarbamate, and the emulsifier is any one of lignosulfonate, methyl cellulose, diglycerol polypropylene glycol ether, polyoxyethylene oleate or fatty amide polyoxyethylene ether. The antioxidant can inhibit peroxide and decompose the peroxide on one hand, and can remove peroxy radicals on the other hand, and the antioxidant can react with the peroxy radicals to prevent the generation and transfer of the peroxide in the oxidation reaction process of a hydrocarbon chain, so that the lubricant has good antioxidant effect; the emulsifier can enhance the compatibility of the ionic liquid, the antioxidant, the sodium carbonate and the hydrochloric acid with the modified vegetable oil, is beneficial to uniform dispersion of all components, is easy to biodegrade, and is more environment-friendly.
A preparation method of a biodegradable environment-friendly lubricant comprises the following steps:
(1) Preparing vegetable oil fatty acid methyl ester;
(2) Preparing primary modified vegetable oil;
(3) Preparing epoxidized primary modified vegetable oil;
(4) Preparing secondary modified vegetable oil;
(5) And (4) sequentially adding the secondary modified vegetable oil obtained in the step (4), the ionic liquid, the antioxidant, the emulsifier, the sodium carbonate and the hydrochloric acid into a reactor, and stirring to obtain the lubricant.
As optimization, the preparation method of the biodegradable environment-friendly lubricant comprises the following steps:
(1) Adding vegetable oil into a flask, adding methanol and sodium hydroxide into the flask under the condition of stirring, heating for reaction, cooling, separating liquid, and distilling under reduced pressure to obtain vegetable oil fatty acid methyl ester;
(2) Adding the vegetable oil fatty acid methyl ester obtained in the step (1) into a flask, adding trimethylolethane into the flask under the stirring condition, rapidly adding sodium ethoxide, heating for reaction, cooling, separating liquid, and distilling under reduced pressure to obtain primary modified vegetable oil;
(3) Adding the primary modified vegetable oil obtained in the step (2) into a flask, respectively and simultaneously dropwise adding glacial acetic acid, hydrogen peroxide and concentrated sulfuric acid into the flask under the condition of stirring, heating for reaction, cooling, separating liquid, and collecting epoxidized primary modified vegetable oil;
(4) Pouring the epoxidized primary modified vegetable oil collected in the step (3) into a flask, adding organic acid and concentrated sulfuric acid into the flask, stirring, heating for reaction, cooling, separating liquid, and distilling under reduced pressure to obtain secondary modified vegetable oil;
(5) And (5) sequentially adding the secondary modified vegetable oil obtained in the step (4), the ionic liquid, the antioxidant, the emulsifier, the sodium carbonate and the hydrochloric acid into a reactor, heating and stirring to obtain the lubricant.
As optimization, the preparation method of the biodegradable environment-friendly lubricant comprises the following steps:
(1) Adding vegetable oil into a flask, heating to 50-70 ℃, adding methanol and sodium hydroxide into the flask under the stirring condition, wherein the mass ratio of the vegetable oil to the methanol is 1-4, and the mass of the sodium hydroxide is 0.5-1% of the total mass of the vegetable oil and the methanol, reacting at 50-70 ℃ for 60-90min, naturally cooling to room temperature, transferring the reaction mixed solution into a separating funnel, adding dilute hydrochloric acid into the separating funnel to neutralize to neutrality, standing for layering, separating out a lower-layer aqueous phase, and carrying out reduced pressure distillation on an upper-layer vegetable oil fatty acid methyl ester solution at the vacuum degree of 0.01-0.03MPa and the temperature of 30-40 ℃ to obtain the vegetable oil fatty acid methyl ester; the invention firstly carries out ester exchange reaction between vegetable oil and methanol, replaces glyceryl on long-chain fatty acid with methyl, and breaks triglyceride to generate long-chain fatty acid methyl ester, thereby reducing the length of a carbon chain, but reducing the viscosity of oil;
(2) Adding the vegetable oil fatty acid methyl ester obtained in the step (1) into a flask, heating to 60-80 ℃, adding trimethylolethane into the flask under the stirring condition, then quickly adding sodium ethoxide, wherein the mass ratio of the vegetable oil fatty acid methyl ester to the trimethylolethane is 3-5, the mass of the sodium ethoxide is 0.8-1.2% of the total mass of the vegetable oil fatty acid methyl ester and the trimethylolethane, reacting at 60-80 ℃ for 1-2h, naturally cooling to room temperature, transferring the reaction mixed solution into a separating funnel, adding dilute hydrochloric acid into the separating funnel to neutralize to neutrality, standing for layering, firstly separating out a lower-layer water phase, and carrying out reduced pressure distillation on the upper-layer primary modified vegetable oil mixed solution at the vacuum degree of 0.01-0.03MPa and the temperature of 60-80 ℃ to obtain primary modified vegetable oil; the vegetable oil fatty acid methyl ester obtained by the ester exchange reaction in the step (1) and the trimethylolethane are subjected to the ester exchange reaction to obtain the primary modified vegetable oil, so that the polyhydric alcohol without beta-H is used for replacing the glycerol in the vegetable oil molecule, and the stability of the vegetable oil is improved;
(3) Adding the primary modified vegetable oil obtained in the step (2) into a flask, heating to 40-60 ℃, respectively and simultaneously dropwise adding glacial acetic acid, hydrogen peroxide and concentrated sulfuric acid into the flask under the stirring condition, wherein the dropwise adding speed is 20-25 drops/minute, the mass ratio of the primary modified vegetable oil to the glacial acetic acid to the hydrogen peroxide is 1-4-5, the mass of the concentrated sulfuric acid is 0.5-1% of the total mass of the primary modified vegetable oil to the glacial acetic acid to the hydrogen peroxide, reacting at 60-70 ℃ for 3-5h after the dropwise adding is finished, naturally cooling to room temperature, transferring the reaction mixed solution into a separating funnel, adding a sodium hydroxide solution into the separating funnel to neutralize to neutrality, layering, separating out a lower-layer water phase, and collecting an upper-layer epoxidized primary modified vegetable oil; the primary modified vegetable oil also contains C = C double bonds, the invention utilizes the reaction of glacial acetic acid and hydrogen peroxide to generate peroxyacetic acid, and the primary modified vegetable oil and the peroxyacetic acid react to generate epoxidized primary modified vegetable oil so as to eliminate the double bonds in the vegetable oil, but an epoxy group is a three-membered ring and has high tension, and the tension can be relieved only by opening the ring;
(4) Pouring the epoxidized primary modified vegetable oil collected in the step (3) into a flask, adding organic acid and concentrated sulfuric acid into the flask, wherein the mass ratio of the epoxidized primary modified vegetable oil to the organic acid is 1-5, the mass of the concentrated sulfuric acid is 0.2-0.5% of the total mass of the epoxidized primary modified vegetable oil and the organic acid, reacting for 2-4h under the conditions of stirring and 70-80 ℃, naturally cooling to room temperature, transferring the reaction mixed solution into a separating funnel, adding a sodium hydroxide solution into the separating funnel to neutralize to be neutral, standing for layering, separating out a lower-layer water phase, and carrying out reduced pressure distillation on an upper-layer secondary modified vegetable oil solution at the vacuum degree of 0.01-0.03MPa and the temperature of 60-80 ℃ to obtain secondary modified vegetable oil; according to the invention, the epoxidized primary modified vegetable oil is subjected to addition reaction with organic acid under an acidic condition, and an epoxy group is subjected to ring opening to obtain secondary modified vegetable oil, and after the primary modification and the secondary modification of the vegetable oil, the C = C double bond in the vegetable oil is eliminated, and the glycerin in the vegetable oil molecule is replaced, so that the modified vegetable oil with better oxidation stability is obtained;
(5) And (3) sequentially adding the secondary modified vegetable oil obtained in the step (4), the ionic liquid, the antioxidant, the emulsifier, the sodium carbonate and the hydrochloric acid into a reactor, and stirring for 30-60min at 80-100 ℃ and 300-500r/min to obtain the lubricant. The reaction of the sodium carbonate and the hydrochloric acid is exothermic and generates gas, the emitted heat can accelerate the uniform mixing of the ionic liquid, the antioxidant, the emulsifier and the modified vegetable oil, and the generated gas can remove impurities in the modified vegetable oil, so that the quality of the prepared lubricant is better.
As optimization, the mass fraction of the dilute hydrochloric acid in the step (1) and the step (2) is 5-15%.
And (4) optimally, the mass fraction of the sodium hydroxide solution in the step (3) and the step (4) is 5-10%.
Compared with the prior art, the invention has the beneficial effects that:
firstly, vegetable oil and methanol are subjected to transesterification reaction, glyceryl on long-chain fatty acid is replaced by methyl, then vegetable oil methyl ester obtained after the transesterification reaction and trimethylolethane are subjected to transesterification reaction, polyhydric alcohol without beta-H is used for replacing glycerol in vegetable oil molecules, the stability of the vegetable oil is improved, glacial acetic acid and hydrogen peroxide are used for reacting to generate peroxyacetic acid, the primary modified vegetable oil and the peroxyacetic acid are reacted to generate epoxidized primary modified vegetable oil so as to eliminate double bonds in the vegetable oil, finally the epoxidized primary modified vegetable oil and organic acid are subjected to addition reaction under an acidic condition to obtain secondary modified vegetable oil, and after the primary modification and the secondary modification of the vegetable oil, the C = C double bonds in the vegetable oil are eliminated, and the glycerol in the vegetable oil molecules is replaced, so that the modified vegetable oil with better oxidation stability is obtained;
the modified vegetable oil is used as base oil, so that the biodegradable lubricating agent has good biodegradability, and the antioxidant can inhibit peroxide, decompose the peroxide, remove peroxy radicals, react with the peroxy radicals, prevent the generation and transfer of the peroxide in the oxidation reaction process of a hydrocarbon chain and have good antioxidant effect; the emulsifier can enhance the compatibility of each component and the modified vegetable oil, and is beneficial to uniform dispersion of each component; when the lubricant is used for mechanical equipment, the ionic liquid in the lubricant is easy to generate a layer of friction reaction film on the surface of the mechanical equipment through complex friction chemical reaction, so that the novel lubricating oil has a good lubricating effect.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
a biodegradable environment-friendly lubricant comprises the following components in parts by weight: 30 parts of modified linseed oil, 3 parts of zinc dialkyl dithiophosphate, 2 parts of lignosulfonate, 1 part of sodium carbonate, 3 parts of hydrochloric acid and 1 part of 1-ethyl-3-methylimidazole tetrafluoroborate ionic liquid, wherein the modified linseed oil is prepared by modifying linseed oil through methanol, trimethylolethane, glacial acetic acid, hydrogen peroxide and organic acid.
The preparation method of the biodegradable environment-friendly lubricant comprises the following steps:
(1) Adding linseed oil into a flask, heating to 50 ℃, adding methanol and sodium hydroxide into the flask under the stirring condition, wherein the mass ratio of substances of the linseed oil to the methanol is 1;
(2) Adding the linseed oil fatty acid methyl ester obtained in the step (1) into a flask, heating to 60 ℃, adding trimethylolethane into the flask under the stirring condition, then quickly adding sodium ethoxide, wherein the mass ratio of substances of the linseed oil fatty acid methyl ester to the trimethylolethane is 3;
(3) Adding the primary modified linseed oil obtained in the step (2) into a flask, heating to 40 ℃, respectively and simultaneously dropwise adding glacial acetic acid, hydrogen peroxide and concentrated sulfuric acid into the flask under the stirring condition, wherein the dropwise adding speed is 20 drops/minute, the mass ratio of the primary modified linseed oil, the glacial acetic acid and the hydrogen peroxide is 1;
(4) Pouring the epoxidized primary modified linseed oil collected in the step (3) into a flask, adding organic acid and concentrated sulfuric acid into the flask, wherein the mass ratio of the epoxidized primary modified linseed oil to the organic acid is 1;
(5) And (3) sequentially adding 30 parts of modified linseed oil obtained in the step (4), 3 parts of zinc dialkyl dithiophosphate, 2 parts of lignosulfonate, 1 part of sodium carbonate, 3 parts of hydrochloric acid and 1 part of 1-ethyl-3-methylimidazolium tetrafluoroborate ionic liquid into a reactor, and stirring at 80 ℃ and 300r/min for 30min to obtain the lubricant.
Example 2:
a biodegradable environment-friendly lubricant comprises the following components in parts by weight: 35 parts of modified cottonseed oil, 4 parts of dioctadecyl thiodipropionate, 3 parts of methyl cellulose, 1.5 parts of sodium carbonate, 3.5 parts of hydrochloric acid and 2 parts of 1-butyl-3-methylimidazolium chloride ionic liquid, wherein the modified cottonseed oil is prepared by modifying cottonseed oil by methanol, trimethylolethane, glacial acetic acid, hydrogen peroxide and organic acid.
The preparation method of the biodegradable environment-friendly lubricant comprises the following steps:
(1) Adding cottonseed oil into a flask, heating to 55 ℃, adding methanol and sodium hydroxide into the flask under the stirring condition, wherein the mass ratio of substances of the cottonseed oil to the methanol is 1.5, the mass of the sodium hydroxide is 0.6 percent of the total mass of the cottonseed oil and the methanol, reacting for 65min at 55 ℃, naturally cooling to room temperature, transferring the reaction mixed solution into a separating funnel, adding dilute hydrochloric acid into the separating funnel to neutralize to neutrality, keeping the dilute hydrochloric acid at 6 percent by mass, standing for layering, separating out a lower-layer water phase, and carrying out reduced pressure distillation on an upper-layer cottonseed oil fatty acid methyl ester solution at the vacuum degree of 0.015MPa and the temperature of 32 ℃ to obtain cottonseed oil fatty acid methyl ester;
(2) Adding the cottonseed oil fatty acid methyl ester obtained in the step (1) into a flask, heating to 65 ℃, adding trimethylolethane into the flask under the condition of stirring, then quickly adding sodium ethoxide, wherein the mass ratio of substances of the cottonseed oil fatty acid methyl ester to the trimethylolethane is 3.5;
(3) Adding the primary modified cottonseed oil obtained in the step (2) into a flask, heating to 45 ℃, respectively and simultaneously dropwise adding glacial acetic acid, hydrogen peroxide and concentrated sulfuric acid into the flask under the condition of stirring, wherein the dropwise adding speed is 21 drops/min, the mass ratio of the primary modified vegetable oil to the glacial acetic acid to the hydrogen peroxide is 1.2;
(4) Pouring the epoxidized primary modified cottonseed oil collected in the step (3) back into the flask, adding organic acid and concentrated sulfuric acid into the flask, wherein the mass ratio of the epoxidized primary modified cottonseed oil to the organic acid is 1.2, the mass of the concentrated sulfuric acid is 0.25% of the total mass of the epoxidized primary modified cottonseed oil and the organic acid, reacting for 2.5h under the conditions of stirring and 72 ℃, naturally cooling to room temperature, transferring the reaction mixed solution into a separating funnel, adding a sodium hydroxide solution into the separating funnel to neutralize to neutrality, the mass fraction of the sodium hydroxide solution is 6%, standing for layering, separating a lower-layer water phase, and carrying out reduced pressure distillation on an upper-layer secondary modified cottonseed oil solution at the temperature of 65 ℃ under the vacuum degree of 0.015MPa to obtain secondary modified cottonseed oil;
(5) And (3) sequentially adding 35 parts of modified cottonseed oil obtained in the step (4), 4 parts of dioctadecyl thiodipropionate, 3 parts of methyl cellulose, 1.5 parts of sodium carbonate, 3.5 parts of hydrochloric acid and 2 parts of 1-butyl-3-methylimidazolium chloride ionic liquid into a reactor, and stirring at 85 ℃ and 350r/min for 35min to obtain the lubricant.
Example 3:
a biodegradable environment-friendly lubricant comprises the following components in parts by weight: 40 parts of modified 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 5 parts of 1-butyl-3-methylimidazolium hexafluorophosphate ionic liquid, wherein the modified rice bran oil is prepared by modifying rice bran oil through methanol, trimethylolethane, glacial acetic acid, hydrogen peroxide and organic acid.
The preparation method of the biodegradable environment-friendly lubricant comprises the following steps:
(1) Adding rice bran oil into a flask, heating to 60 ℃, adding methanol and sodium hydroxide into the flask under the stirring condition, wherein the mass ratio of the rice bran oil to the methanol is 1;
(2) Adding the rice bran oil fatty acid methyl ester obtained in the step (1) into a flask, heating to 70 ℃, adding trimethylolethane into the flask under the stirring condition, then quickly adding sodium ethoxide, wherein the mass ratio of the rice bran oil fatty acid methyl ester to the trimethylolethane is 4;
(3) Adding the primary modified rice bran oil obtained in the step (2) into a flask, heating to 50 ℃, respectively and simultaneously dropwise adding glacial acetic acid, hydrogen peroxide and concentrated sulfuric acid into the flask under the condition of stirring, wherein the dropwise adding speed is 23 drops/min, the mass ratio of the primary modified rice bran oil, the glacial acetic acid and the hydrogen peroxide is 1;
(4) Pouring the epoxidized primary modified rice bran oil collected in the step (3) into a flask, adding organic acid and concentrated sulfuric acid into the flask, wherein the mass ratio of the epoxidized primary modified rice bran oil to the organic acid is 1;
(5) And (3) sequentially adding 40 parts of the modified rice bran oil obtained in the step (4), 5 parts of dodecyl selenium, 6 parts of diglycerol polypropylene glycol ether, 1.5 parts of sodium carbonate, 4 parts of hydrochloric acid and 5 parts of 1-butyl-3-methylimidazolium hexafluorophosphate ionic liquid into a reactor, and stirring at 90 ℃ and 400r/min for 45min to obtain the lubricant.
Example 4:
a biodegradable environment-friendly lubricant comprises the following components in parts by weight: 45 parts of modified camellia seed oil, 7 parts of 2, 6-di-tert-butyl-p-cresol, 8 parts of oleic acid polyoxyethylene ester, 2.5 parts of sodium carbonate, 4.5 parts of hydrochloric acid and 9 parts of quaternary phosphonium salt phosphate ionic liquid, wherein the modified camellia seed oil is prepared by modifying camellia seed oil through methanol, trimethylolethane, glacial acetic acid, hydrogen peroxide and organic acid.
The preparation method of the biodegradable environment-friendly lubricant by adopting the raw materials comprises the following steps:
(1) Adding camellia oleosa seed oil into a flask, heating to 65 ℃, adding methanol and sodium hydroxide into the flask under the stirring condition, wherein the mass ratio of camellia oleosa seed oil to methanol is 1.5, the mass of sodium hydroxide is 0.9% of the total mass of the plant oil and methanol, reacting at 65 ℃ for 85min, naturally cooling to room temperature, transferring the reaction mixed solution into a separating funnel, adding dilute hydrochloric acid into the separating funnel to neutralize to neutrality, the mass fraction of the dilute hydrochloric acid is 12%, standing for layering, separating a lower-layer aqueous phase, and carrying out reduced pressure distillation on an upper-layer plant oil fatty acid methyl ester solution at the vacuum degree of 0.025MPa and the temperature of 38 ℃ to obtain camellia oleosa seed oil fatty acid methyl ester;
(2) Adding the camellia seed oil fatty acid methyl ester obtained in the step (1) into a flask, heating to 78 ℃, adding trimethylolethane into the flask under the condition of stirring, then quickly adding sodium ethoxide, wherein the mass ratio of substances of the camellia seed oil fatty acid methyl ester to the trimethylolethane is 4.5;
(3) Adding the primary modified camellia oleosa seed oil obtained in the step (2) into a flask, heating to 55 ℃, respectively and simultaneously dripping glacial acetic acid, hydrogen peroxide and concentrated sulfuric acid into the flask under the condition of stirring, wherein the dripping speed is 24 drops/min, the mass ratio of the primary modified camellia oleosa seed oil to the glacial acetic acid to the hydrogen peroxide is 1;
(4) Pouring the epoxidized primary modified camellia seed oil collected in the step (3) back into the flask, adding organic acid and concentrated sulfuric acid into the flask, wherein the mass ratio of the epoxidized primary modified camellia seed oil to the organic acid is 1:4.8, the mass of the concentrated sulfuric acid is 0.45% of the total mass of the epoxidized primary modified camellia seed oil and the organic acid, reacting for 3.5 hours under the condition of stirring and 78 ℃, naturally cooling to room temperature, transferring the reaction mixed solution into a separating funnel, adding a sodium hydroxide solution into the separating funnel to neutralize to neutrality, keeping the sodium hydroxide solution at 9% by mass, standing for layering, firstly separating a lower-layer water phase, and carrying out reduced pressure distillation on an upper-layer secondary modified camellia seed oil solution at the temperature of 75 ℃ under the vacuum degree of 0.025MPa to obtain secondary modified camellia seed oil;
(5) And (5) sequentially adding 45 parts of the modified camellia oleosa seed oil obtained in the step (4), 7 parts of 2, 6-di-tert-butyl-p-cresol, 8 parts of oleic acid polyoxyethylene ester, 2.5 parts of sodium carbonate, 4.5 parts of hydrochloric acid and 9 parts of quaternary phosphonium phosphate ionic liquid into a reactor, and stirring at 95 ℃ and 450r/min for 55min to obtain the lubricant.
Example 5:
a biodegradable environment-friendly lubricant comprises the following components in parts by weight: 50 parts of modified coconut oil, 8 parts of zinc dialkyl dithiocarbamate, 10 parts of fatty amide polyoxyethylene ether, 3 parts of sodium carbonate, 5 parts of hydrochloric acid and 10 parts of 1-hexyl-3-methylimidazole hexafluorophosphate ionic liquid, wherein the modified coconut oil is prepared by modifying coconut oil through methanol, trimethylolethane, glacial acetic acid, hydrogen peroxide and organic acid.
The preparation method of the biodegradable environment-friendly lubricant comprises the following steps:
(1) Adding coconut oil into a flask, heating to 70 ℃, adding methanol and sodium hydroxide into the flask under the stirring condition, wherein the mass ratio of the coconut oil to the methanol is 1;
(2) Adding the coconut oil fatty acid methyl ester obtained in the step (1) into a flask, heating to 80 ℃, adding trimethylolethane into the flask under the stirring condition, then quickly adding sodium ethoxide, wherein the mass ratio of the coconut oil fatty acid methyl ester to the trimethylolethane is 5;
(3) Adding the primary modified coconut oil obtained in the step (2) into a flask, heating to 60 ℃, respectively and simultaneously dropwise adding glacial acetic acid, hydrogen peroxide and concentrated sulfuric acid into the flask under the condition of stirring, wherein the dropwise adding speed is 25 drops/min, the mass ratio of the primary modified coconut oil, the glacial acetic acid and the hydrogen peroxide is 1;
(4) Pouring the epoxidized primary modified vegetable oil collected in the step (3) into a flask, adding organic acid and concentrated sulfuric acid into the flask, wherein the mass ratio of the epoxidized primary modified vegetable oil to the organic acid is 1;
(5) And (5) sequentially adding 50 parts of modified coconut oil obtained in the step (4), 8 parts of zinc dialkyl dithiocarbamate, 10 parts of fatty amide polyoxyethylene ether, 3 parts of sodium carbonate, 5 parts of hydrochloric acid and 10 parts of 1-hexyl-3-methylimidazole hexafluorophosphate ionic liquid into a reactor, and stirring at 100 ℃ and 500r/min for 60min to obtain the lubricant.
Comparative example 1:
a novel lubricant comprises the following components in parts by weight: 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 5 parts of 1-butyl-3-methylimidazolium hexafluorophosphate ionic liquid.
The novel lubricant is prepared from the raw materials, and the preparation method of the novel lubricant comprises the following steps:
adding 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 5 parts of 1-butyl-3-methylimidazolium hexafluorophosphate ionic liquid into a reactor in sequence, and stirring for 45min at 90 ℃ and 400r/min to obtain the novel lubricant.
Comparative example 1 is the same as example 3 except that the plant oil rice bran oil is not modified.
Comparative example 2:
a novel lubricant comprises the following components in parts by weight: the modified rice bran oil is prepared by modifying rice bran oil with methanol, trimethylolethane, glacial acetic acid, hydrogen peroxide and organic acid, wherein the modified rice bran oil comprises 40 parts of modified rice bran oil, 5 parts of dodecyl selenium, 6 parts of diglycerol polypropylene glycol ether, 1.5 parts of sodium carbonate and 4 parts of hydrochloric acid.
The novel lubricant is prepared by adopting the raw materials, and the preparation method of the novel lubricant comprises the following steps:
(1) Adding rice bran oil into a flask, heating to 60 ℃, adding methanol and sodium hydroxide into the flask under the stirring condition, wherein the mass ratio of the rice bran oil to the methanol is 1;
(2) Adding the rice bran oil fatty acid methyl ester obtained in the step (1) into a flask, heating to 70 ℃, adding trimethylolethane into the flask under the stirring condition, then quickly adding sodium ethoxide, wherein the mass ratio of the rice bran oil fatty acid methyl ester to the trimethylolethane is 4;
(3) Adding the primary modified rice bran oil obtained in the step (2) into a flask, heating to 50 ℃, respectively and simultaneously adding glacial acetic acid, hydrogen peroxide and concentrated sulfuric acid into the flask under the condition of stirring, wherein the adding speed is 23 drops/minute, the mass ratio of the primary modified rice bran oil to the glacial acetic acid to the hydrogen peroxide is 1;
(4) Pouring the epoxidized primary modified rice bran oil collected in the step (3) into a flask, adding organic acid and concentrated sulfuric acid into the flask, wherein the mass ratio of the epoxidized primary modified rice bran oil to the organic acid is 1;
(5) And (3) sequentially adding 40 parts of the modified rice bran oil obtained in the step (4), 5 parts of dodecyl selenium, 6 parts of diglycerol polypropylene glycol ether, 1.5 parts of sodium carbonate and 4 parts of hydrochloric acid into a reactor, and stirring at 90 ℃ and 400r/min for 45min to obtain the novel lubricant.
Comparative example 2 is the same as example 3 except that 1-butyl-3-methylimidazolium hexafluorophosphate ionic liquid was not used in the raw material.
Example of effects:
(1) Experimental samples: the novel lubricants prepared in examples 1 to 5 of the present invention and the novel lubricants prepared in comparative examples 1 and 2.
(2) The experimental method comprises the following steps:
(a) Biodegradability: the test was carried out according to the experimental method of CEC L-33-A-93 (the precursor is CEC L-33-T-82) of the European Union, and the test results are shown in Table 1;
(b) Bowden (horizontal linear reciprocating) stick-slip test: after immersing the test piece in each test sample at room temperature, the test piece was left in a thermostatic bath at 80 ℃ for 20 minutes, and the adhesion strength of the coating was examined using the test piece on which the lubricating coating was formed according to the following items; test piece material quality: SCM440, test piece shape: 100mm × 80mm × 5mm, friction ball: SUJ-2, 3/16 inch φ, test temperature: 100 ℃, load: 3kg, sliding speed: 3.88 mm/sec, evaluation: the average coefficient of friction and the number of slips until ablation occurred were determined and the results are shown in table 1.
TABLE 1
(3) The experimental results are as follows: as can be seen from table 1, the novel lubricants prepared in examples 1 to 5 of the present invention all had a biodegradability of 98% or more, an average coefficient of friction of 0.04 or less, and a sliding frequency until ablation occurred of 208 times or more, while the novel lubricants prepared in comparative examples 1 and 2 had a biodegradability of 90% and 93%, an average coefficient of friction of 0.10 and 0.12, and a sliding frequency until ablation occurred of 90 times and 85 times, respectively, and the experimental results showed that the novel lubricants prepared in examples 1 to 5 of the present invention had excellent biodegradability and lubricating effect.
Comparative example 1 compared with examples 1 to 5 of the present invention, the lubricating effect of the novel lubricant prepared was inferior to that of the novel lubricant prepared in examples 1 to 5 of the present invention because the vegetable oil was not modified.
Comparative example 2 compared with examples 1 to 5 of the present invention, the lubricating effect of the novel lubricant prepared was inferior to that of the novel lubricant prepared in examples 1 to 5 of the present invention, since no ionic liquid was used in the raw material.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Claims (6)
1. The preparation method of the biodegradable environment-friendly lubricant is characterized by comprising the following components in 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;
the lubricant further comprises 1-10 parts by weight of ionic liquid, wherein the ionic liquid is any one of 1-ethyl-3-methylimidazole tetrafluoroborate ionic liquid, 1-butyl-3-methylimidazole chloride ionic liquid, 1-butyl-3-methylimidazole hexafluorophosphate ionic liquid, quaternary phosphonium phosphate ionic liquid or 1-hexyl-3-methylimidazole hexafluorophosphate ionic liquid;
the preparation method of the lubricant comprises the following steps:
(1) Adding vegetable oil into a flask, adding methanol and sodium hydroxide into the flask under the condition of stirring, heating for reaction, cooling, separating liquid, and distilling under reduced pressure to obtain vegetable oil fatty acid methyl ester;
(2) Adding the vegetable oil fatty acid methyl ester obtained in the step (1) into a flask, adding trimethylolethane into the flask under the stirring condition, then quickly adding sodium ethylate, heating for reaction, cooling, separating liquid, and distilling under reduced pressure to obtain primary modified vegetable oil;
(3) Adding the primary modified vegetable oil obtained in the step (2) into a flask, respectively and simultaneously dropwise adding glacial acetic acid, hydrogen peroxide and concentrated sulfuric acid into the flask under the condition of stirring, heating for reaction, cooling, separating liquid, and collecting epoxidized primary modified vegetable oil;
(4) Pouring the epoxidized primary modified vegetable oil collected in the step (3) into a flask, adding organic acid and concentrated sulfuric acid into the flask, stirring, heating for reaction, cooling, separating liquid, and distilling under reduced pressure to obtain secondary modified vegetable oil;
(5) And (4) sequentially adding the secondary modified vegetable oil obtained in the step (4), the ionic liquid, the antioxidant, the emulsifier, the sodium carbonate and the hydrochloric acid into a reactor, heating and stirring to obtain the lubricant.
2. The method for preparing a biodegradable, environmentally friendly lubricant according to claim 1, wherein: the vegetable oil is any one of linseed oil, cottonseed oil, rice bran oil, camellia seed oil or coconut oil.
3. The method for preparing a biodegradable environmentally friendly lubricant according to claim 2, wherein: the antioxidant is any one of zinc dialkyl dithiophosphate, dioctadecyl thiodipropionate, dodecyl selenium, 2, 6-di-tert-butyl-p-cresol or zinc dialkyl dithiocarbamate, and the emulsifier is any one of lignosulfonate, methyl cellulose, diglycerol polypropylene glycol ether, oleic acid polyoxyethylene ester or fatty amide polyoxyethylene ether.
4. The method of claim 1, wherein the method comprises the steps of:
(1) Adding vegetable oil into a flask, heating to 50-70 ℃, adding methanol and sodium hydroxide into the flask under the condition of stirring, wherein the mass ratio of the vegetable oil to the methanol is 1;
(2) Adding the vegetable oil fatty acid methyl ester obtained in the step (1) into a flask, heating to 60-80 ℃, adding trimethylolethane into the flask under the condition of stirring, then rapidly adding sodium ethoxide, wherein the mass ratio of the vegetable oil fatty acid methyl ester to the trimethylolethane is 3-5;
(3) Adding the primary modified vegetable oil obtained in the step (2) into a flask, heating to 40-60 ℃, respectively and simultaneously dropwise adding glacial acetic acid, hydrogen peroxide and concentrated sulfuric acid into the flask under the condition of stirring, wherein the dropwise adding speed is 20-25 drops/min, the mass ratio of the substances of the primary modified vegetable oil, the glacial acetic acid and the hydrogen peroxide is 1-4-5, the mass of the concentrated sulfuric acid is 0.5-1% of the total mass of the primary modified vegetable oil, the glacial acetic acid and the hydrogen peroxide, reacting at 60-70 ℃ for 3-5h after the dropwise adding is finished, naturally cooling to room temperature, transferring the reaction into a separating funnel, adding a sodium hydroxide solution into the mixed solution to neutralize to be neutral, standing for layering, firstly separating out a lower-layer water phase, and collecting an upper-layer epoxidized primary modified vegetable oil;
(4) Pouring the epoxidized primary modified vegetable oil collected in the step (3) into a flask, adding organic acid and concentrated sulfuric acid into the flask, wherein the mass ratio of the epoxidized primary modified vegetable oil to the organic acid is 1;
(5) And (3) sequentially adding the secondary modified vegetable oil obtained in the step (4), the ionic liquid, the antioxidant, the emulsifier, the sodium carbonate and the hydrochloric acid into a reactor, and stirring for 30-60min at 80-100 ℃ and 300-500r/min to obtain the lubricant.
5. The method for preparing a biodegradable environmentally friendly lubricant according to claim 4, wherein: the mass fraction of the dilute hydrochloric acid in the step (1) and the step (2) is 5-15%.
6. The method for preparing a biodegradable environmentally friendly lubricant according to claim 4 or 5, wherein: and the mass fraction of the sodium hydroxide solution in the step (3) and the step (4) is 5-10%.
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