CN111909764B - High-cleanness high-pressure anti-wear hydraulic oil and preparation method thereof - Google Patents
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- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
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- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
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Abstract
The invention relates to high-cleanness high-pressure anti-wear hydraulic oil and a preparation method thereof, and the preparation method comprises the following steps of firstly, adding palladium acetate into a solution melted by high carbonic acid to prepare a high carbonic acid palladium-high carbonic acid homogeneous waxy solid catalyst; step two, mixing ethylenediamine and high-carbon alcohol, adding a high-palladium carbonate-high-carbonic acid homogeneous waxy solid catalyst, heating, uniformly stirring, and preparing a 2-alkyl imidazoline compound under the condition of introducing air; and step three, mixing the 2-alkyl imidazoline compound, the high-carbon alcohol, the high-methyl carbonate and the base oil to obtain the high-cleanness high-pressure anti-wear hydraulic oil. The high-cleanness high-pressure anti-wear hydraulic oil does not need to be additionally added with a metal anticorrosive agent and an extreme pressure anti-wear agent. The high-temperature high-pressure wear-resistant cleaning agent is not degraded after long-term use under the high-temperature high-pressure condition, does not generate oil sludge, achieves the high-pressure wear-resistant high-cleaning effect, and has the quality indexes which all accord with the hydraulic oil standard.
Description
Technical Field
The invention belongs to the technical field of hydraulic oil, and relates to high-cleanness high-pressure anti-wear hydraulic oil and a preparation method thereof.
Background
The hydraulic oil is a medium for transferring energy in hydraulic transmission and is widely used for automobile brake systems, hoisting systems, bulldozer systems, airplanes, ships and the like. For excellent hydraulic oil, the oil should have good oxidation resistance, corrosion resistance of metal materials, emulsification resistance, high-pressure wear resistance, good high-temperature deterioration resistance and good low-temperature fluidity. The conventional hydraulic oil is usually formed by adding additives such as a metal preservative, an anti-emulsifier, an extreme pressure anti-wear agent, a high pressure anti-wear agent and the like on the basis of base oil. Typical friction reducers typically incorporate phosphites, phosphates, and zinc alkyl dithiophosphates. The additives can be degraded quickly under the high-temperature aerobic condition, so that oil sludge is generated, the cleaning is difficult, and the time and the labor are wasted during the cleaning. The market needs hydraulic oil which has stable chemical performance, does not produce oil sludge and is wear-resistant under the condition of long-term aerobic high temperature; and can meet the standard detection of GB 11118.1-2011.
Disclosure of Invention
Object of the Invention
In order to solve the problems in the prior art, the invention provides high-cleanness high-pressure anti-wear hydraulic oil meeting GB11118.1-2011 standard and a preparation method thereof. Has stable chemical performance under the condition of long-term aerobic high temperature, does not generate oil sludge, and achieves high cleanness, high pressure and abrasion resistance of engineering requirements.
Technical scheme
A high-cleanness high-pressure anti-wear hydraulic oil is prepared by mixing a 2-alkyl imidazoline compound, high-carbon alcohol, high-carbonic acid monomethyl ester and base oil;
the mass ratio of the 2-alkyl imidazoline compound to the high-carbon alcohol to the high-carbon monomethyl ester to the base oil is (10 to 30): (10 to 30): (5 to 20): (30 to 50);
the structural formula of the 2-alkyl imidazoline compound is as follows:
-R has the formula: - (CH) 2 ) n-2 CH 3 ；
Where n is a positive integer from 10 to 24.
Further, the molecular structural formula of the higher alcohol is as follows:
HO-(CH 2 ) n-1 CH 3 ；
wherein n is a positive integer of 10 to 24;
the molecular structural formula of the high carbonic acid monomethyl ester is as follows:
wherein n is a positive integer of 10 to 24.
The preparation method of the high-cleaning high-pressure anti-wear hydraulic oil comprises the following steps:
step one, adding palladium acetate into a high-carbonic acid molten solution to prepare a high-carbonic acid palladium-high-carbonic acid homogeneous waxy solid catalyst;
step two, mixing ethylenediamine and high-carbon alcohol, adding a high-palladium carbonate-high-carbonic acid homogeneous waxy solid catalyst, heating, uniformly stirring, and preparing a 2-alkyl imidazoline compound under the condition of introducing air;
and step three, mixing the 2-alkyl imidazoline compound, the high-carbon alcohol, the high-methyl carbonate and the base oil to obtain the high-cleanness high-pressure anti-wear hydraulic oil.
Further, the structural formula of the high carbonic acid in the first step is as follows:
wherein n is a positive integer of 10 to 24.
Further, in the first step, the molar ratio of palladium acetate to high carbonic acid: 1 to 1, adding palladium acetate into a high-carbonic acid molten solution, uniformly stirring, raising the temperature from normal temperature to 120 to 200 ℃, vacuumizing for 50 to 200mmHg, keeping the temperature for 3 to 5 hours, steaming out a by-product acetic acid generated in the reaction, transferring the reaction liquid into a stainless steel disc, and naturally cooling to obtain the high-carbonic acid palladium-high-carbonic acid homogeneous waxy solid catalyst.
Further, in the second step, the molar ratio of the higher alcohol to the ethylenediamine is more than or equal to 1, the mixture is stirred uniformly in a reactor, a palladium carbonate-carbonic acid homogeneous wax solid catalyst is added, the mass of the palladium carbonate-carbonic acid homogeneous wax solid catalyst is 1/100000-3/100 of the sum of the mass of the higher alcohol and the mass of the ethylenediamine, then air is introduced, the temperature is controlled to 100 ℃ -150 ℃, the mixture is stirred uniformly, the vacuum pumping is carried out for 50-200mmHg, the reaction is carried out for 8-12 hours, water generated by the reaction is distilled out, and a 2-alkylimidazoline compound is obtained, wherein the structural formula is as follows:
further, in the third step, the mass ratio of the 2-alkyl imidazoline compound, the high carbon alcohol, the high methyl carbonate and the base oil is (10 to 30): (10 to 30): (5 to 20): (30 to 50), heating to be more than or equal to 100 ℃ from the normal temperature, uniformly stirring, and cooling to the room temperature to obtain the high-cleaning high-pressure anti-wear hydraulic oil;
the base oil refers to: a class of mineral base oils ISOVG32, a class of mineral base oils ISOVG46, paraffinic class I or paraffinic class II base oils.
Further, the reactor includes reactor main part, cooling tube and byproduct receiving tank, reactor main part inserts and fixes being equipped with pressure detector and temperature detector, the reactor main part outside is equipped with the heating jacket, be equipped with the cavity that holds the heat carrier between heating jacket and the reactor main part, one side lower extreme of heating jacket is equipped with the heat carrier entry, the opposite side upper end of heating jacket is equipped with the heat carrier export, one side upper end of reactor main part is equipped with raw materials entry, the opposite side upper end of reactor main part is equipped with air inlet, the lower extreme of reactor main part is equipped with the product export, the upper end outside of reactor main part is fixed with the rotating electrical machines, the reactor main part has been passed to the rotating electrical machines's rotation axis, the rotating electrical machines's rotation axis lower extreme is connected with the stirring rake, the upper end of reactor main part still communicates with the one end of distillation tower, the one end at the cooling tube is connected to the other end of distillation tower, the other end and the inside intercommunication of byproduct receiving tank of cooling tube, the periphery of cooling tube is fixed with the cooling tank, lower extreme one side of cooling tank is equipped with the coolant inlet, the upper end opposite side of cooling tank is equipped with the coolant liquid export, the byproduct receiving tank, the coolant outlet, the byproduct receiving tank is equipped with the vacuum tube.
Furthermore, a water receiving tank is arranged under the cooling tank, one end of the spraying pipe is arranged at the bottom of the water receiving tank, the main body of the spraying pipe is fixed with the cooling pipe, a pump capable of pumping liquid on the net is arranged on the spraying pipe, the main body at the upper part of the spraying pipe is in a horizontal state, a spraying head is arranged on the main body at the upper part of the spraying pipe, and the spraying head is positioned above the cooling tank and can spray towards the cooling tank.
Furthermore, the cooling pipe is provided with two downward flow guide blocks, and the two flow guide blocks are respectively positioned at two ends of the cooling tank.
Advantages and effects
The high-cleanness high-pressure anti-wear hydraulic oil does not need to be additionally added with a metal anticorrosive agent and an extreme pressure anti-wear agent. The product is not degraded after long-term use under the conditions of high temperature and high pressure, does not generate oil sludge, and achieves the effects of high pressure, wear resistance and high cleanness.
The high-cleanness high-pressure anti-wear hydraulic oil produced by the invention is detected according to GB11118.1-2011 standard, and all quality indexes of the high-cleanness high-pressure anti-wear hydraulic oil meet the hydraulic oil standard. The catalyst does not contain inorganic matters or inorganic ash, is synthesized by all organic compounds, and meets the market demand.
Drawings
The invention is further described with reference to the following figures and detailed description. The scope of the invention is not limited to the following expressions.
FIG. 1 is a schematic view of the reactor structure.
Description of reference numerals: 1. the reactor comprises a reactor main body, a heating jacket, a heat carrier inlet, a heat carrier outlet, a product outlet, a raw material inlet, an air inlet, a rotating motor, a stirring paddle 9, a pressure detector 10, a temperature detector 11, a distillation tower 12, a cooling tower 13, a cooling pipe 14, a cooling tank 15, a cooling liquid inlet, a cooling liquid outlet, a spraying pipe 17, a spraying head 18, a water receiving tank 19, a flow guide block 20, a byproduct receiving tank 21, a byproduct outlet, a vacuum pumping pipe 23, and a pump 24.
Detailed Description
A high-cleanness high-pressure anti-wear hydraulic oil is prepared by mixing a 2-alkyl imidazoline compound, high-carbon alcohol, high-methyl carbonate and base oil;
the mass ratio of the 2-alkyl imidazoline compound to the high-carbon alcohol to the high-carbon monomethyl ester to the base oil is (10 to 30): (10 to 30): (5 to 20): (30 to 50);
the structural formula of the 2-alkyl imidazoline compound is as follows:
-R has the formula: - (CH) 2 ) n-2 CH 3 ；
Where n is a positive integer from 10 to 24.
The molecular structural formula of the higher alcohol is as follows:
HO-(CH 2 ) n-1 CH 3 ；
wherein n is a positive integer of 10 to 24;
the molecular structural formula of the high carbonic acid monomethyl ester is as follows:
wherein n is a positive integer of 10 to 24.
The preparation method of the high-cleanness high-pressure anti-wear hydraulic oil comprises the following steps:
step one, the molar ratio of palladium acetate to high carbonic acid is as follows: 1, adding palladium acetate into a high-carbonic acid molten solution, uniformly stirring, raising the temperature from normal temperature to 120-200 ℃, vacuumizing for 50-200mmHg, keeping the temperature for 3-5 hours, evaporating a by-product acetic acid generated in the reaction, transferring a reaction solution into a stainless steel disc, and naturally cooling to obtain the high-carbonic acid homogeneous waxy solid catalyst.
The structural formula of the high carbonic acid is as follows:
wherein n is a positive integer of 10 to 24.
Step two, mixing and stirring the high carbon alcohol and the ethylenediamine uniformly in a molar ratio of more than or equal to 1, adding a high-palladium carbonate-high-carbonic acid homogeneous wax solid catalyst, wherein the mass of the high-palladium carbonate-high-carbonic acid homogeneous wax solid catalyst is 1/100000 to 3/100 of the sum of the mass of the high carbon alcohol and the mass of the ethylenediamine, introducing air, controlling the temperature to be 100 to 150 ℃, stirring uniformly, vacuumizing for 50 to 200mmHg, reacting for 8 to 12 hours, and evaporating water generated by the reaction to obtain a 2-alkylimidazoline compound, wherein the structural formula is as follows:
step three, the mass ratio of the 2-alkyl imidazoline compound, the high-carbon alcohol, the high-methyl carbonate and the base oil is (10 to 30): (10 to 30): (5 to 20): (30 to 50), heating to more than or equal to 100 ℃ from normal temperature, uniformly stirring, and cooling to room temperature to obtain the high-cleaning high-pressure anti-wear hydraulic oil; the base oil refers to: a class of mineral base oils ISOVG32, a class of mineral base oils ISOVG46, paraffinic class I or paraffinic class II base oils.
In the following examples, high carbonic acid is exemplified by dodecanoic acid, high alcohols by dodecanol, high monomethyl carbonates by monomethyl dodecanoate, and base oils by paraffinic group i base oils:
example 1
Step one, adding 22.45g (0.1 mol) of palladium acetate into a reactor provided with a pressure detector, a temperature detector, a stirring device, a cooling pipe and a byproduct receiving tank, and adding 200.3g (1 mol) of dodecacarbonic acid (molecular formula of the dodecacarbonic acid: CH) 3 （CH 2 ） 10 COOH) in the reactor, raising the temperature and stirring uniformly, raising the temperature to 145 ℃, vacuumizing for 50mmHg, preserving the temperature for 5 hours, evaporating a by-product acetic acid generated in the reaction, transferring the reaction solution to a stainless steel plate, and naturally cooling to room temperature to obtain 210.75g of a solid catalyst containing 50.51g (0.1 mol, calculated as palladium) of palladium dodecacarbonate;
step two, heating and mixing 60.1g (1 mol) of ethylenediamine and 186.3g (1 mol) of dodecanol in a reactor, uniformly stirring in the reactor, adding 3g of palladium dodecacarbonate-dodecane carbonic acid solid catalyst, introducing air, uniformly stirring, controlling the temperature at 100 ℃, vacuumizing to 50mmHg, reacting for 8 hours, evaporating water generated by the reaction to obtain 224g (1 mol) of 2-alkylimidazoline (2-undecylimidazoline)
Molecular weight 224.
Step three, mixing a 2-alkyl imidazoline compound, dodecanol, monomethyl dodecanoate and paraffin I base oil according to a mass ratio of 15.
The product is detected according to GB11118.1-2011 standard that all quality indexes meet the standard.
Example 2
Step one, adding 22.45g (0.1 mol) of palladium acetate into a reactor provided with a pressure detector, a temperature detector, a stirring device, a cooling pipe and a byproduct receiving tank, and adding 40.06g (0.2 mol) of dodecacarbonic acid (molecular formula of the dodecacarbonic acid: CH) 3 （CH 2 ） 10 COOH) in the reactor, heating and stirring uniformly, heating to 185 ℃, vacuumizing to 130mmHg, keeping the temperature for 4 hours, evaporating a by-product acetic acid generated in the reaction, transferring the reaction liquid to a stainless steel plate, and naturally cooling to room temperature to obtain 50.51g of a solid catalyst of the dodecapalladium carbonate-dodecacarbonic acid, wherein the solid catalyst contains 50.51g (0.1 mol, calculated as palladium) of the dodecapalladium carbonate;
step two, heating and mixing 60.1g (1 mol) of ethylenediamine and 372.6g (2 mol) of dodecanol in a reactor, uniformly stirring in the reactor, adding 12.981g of solid catalyst of palladium dodecanecarbonate-dodecane carbonate, introducing air, uniformly stirring, controlling the temperature at 125 ℃, vacuumizing to 120mmHg, reacting for 10 hours, evaporating water generated by the reaction to obtain 2-alkylimidazoline (224 g (1 mol)) of 2-undecylimidazoline
Molecular weight 224.
Step three, mixing the 2-alkyl imidazoline compound, the dodecanol, the monomethyl dodecanoate and the paraffin I base oil according to the mass ratio of 10.
The product is detected according to GB11118.1-2011 standard that all quality indexes meet the standard.
Example 3
Step one, adding 22.45g (0.1 mol) of palladium acetate into a reactor provided with a pressure detector, a temperature detector, a stirring device, a cooling pipe and a byproduct receiving tank, and adding 400.6g (2 mol) of dodecacarbonic acid (molecular formula of the dodecacarbonic acid: CH) 3 （CH 2 ） 10 COOH) in the reactor, heating and stirring uniformly, heating to 225 ℃, vacuumizing to 200mmHg, keeping the temperature for 3 hours, evaporating a by-product acetic acid generated in the reaction, transferring the reaction liquid to a stainless steel plate, and naturally cooling to room temperature to obtain 411.05g of a solid catalyst of dodecapalladium carbonate-dodecacarbonic acid, wherein the solid catalyst contains 50.51g (0.1 mol, calculated as palladium) of dodecapalladium carbonate;
step two, heating and mixing 60.1g (1 mol) of ethylenediamine and 558.9g (3 mol) of dodecanol in a reactor, uniformly stirring in the reactor, and adding 6.19 multiplied by 10 -3 g of solid catalyst of palladium dodecacarbonate to dodecane carbonic acid, introducing air, stirring uniformly, controlling the temperature at 150 ℃, vacuumizing to 200mmHg, reacting for 12 hours, and evaporating water generated in the reaction to obtain 2-alkylimidazoline (224 g (1 mol)) of 2-undecylimidazoline
Molecular weight 224.
Step three, mixing the 2-alkyl imidazoline compound, the dodecanol, the monomethyl dodecanoate and the paraffin I base oil according to the mass ratio of 30.
The product is detected according to GB11118.1-2011 standard that all quality indexes meet the standard.
As shown in fig. 1, the reactor includes a reactor main body 1, a cooling pipe 13 and a byproduct receiving tank 21, the reactor main body 1 is inserted into and fixedly provided with a pressure detector 10 and a temperature detector 11, a heating jacket 2 is provided outside the reactor main body 1, a cavity for accommodating a heat carrier is provided between the heating jacket 2 and the reactor main body 1, a heat carrier inlet 3 is provided at a lower end of one side of the heating jacket 2, a heat carrier outlet 4 is provided at an upper end of the other side of the heating jacket 2, a raw material inlet 6 is provided at an upper end of one side of the reactor main body 1, an air inlet 7 is provided at an upper end of the other side of the reactor main body 1, a product outlet 5 is provided at a lower end of the reactor main body 1, a rotary motor 8 is fixedly provided outside an upper end of the reactor main body 1, a rotary shaft of the rotary motor 8 passes through the reactor main body 1, a stirring paddle 9 is connected to a lower end of the rotary shaft of the rotary motor 8, an upper end of the reactor main body 1 is further communicated with one end of a distillation tower 12, another end of the distillation tower 12 is connected to one end of the cooling pipe 13, another end of the cooling pipe 13 is communicated with an inside of the byproduct receiving tank 21, a byproduct receiving tank 14 is fixed to an outer periphery of the cooling pipe 13, a byproduct receiving tank 14 is provided at one side of the lower end of the cooling tank 14, a side of the cooling tank 14, a cooling tank 14 is provided with an upper end of the cooling tank 14, a vacuum pipe, a cooling tank 21 is provided with a coolant inlet 15, a coolant inlet 16 is provided with a byproduct receiving tank 22, and another side of the byproduct receiving tank 21 is provided with a byproduct receiving tank 21, and another byproduct receiving tank 21. A water receiving tank 19 is arranged right below the cooling tank 14, one end of a spray pipe 17 is arranged at the bottom of the water receiving tank 19, the main body of the spray pipe 17 is fixed with the cooling pipe 13, a pump 24 capable of pumping liquid on the net is arranged on the spray pipe 17, the main body at the upper part of the spray pipe 17 is in a horizontal state, a spray head 18 is arranged on the main body at the upper part of the spray pipe 17, and the spray head 18 is positioned above the cooling tank 14 and can spray towards the cooling tank 14. Two guide blocks 20 facing downwards are arranged on the cooling pipe 13, and the two guide blocks 20 are respectively positioned at two ends of the cooling tank 14. When the water receiving tank 19 is used, water is filled in the water receiving tank 19, the spray pipe 17 pumps the water in and then sprays the water to the outer surface of the cooling tank 14 through the spray head 18, the outer surface of the cooling tank 14 is assisted to carry out physical heat dissipation in hot weather of more than 30 ℃, the water flows down from the cooling tank 14 and the flow guide blocks 20 at the two end parts of the cooling tank 14, and finally returns to the water receiving tank 19 to recycle the water in the water receiving tank 19.
It should be understood that the above-described embodiments of the present invention are merely examples for clearly illustrating the invention and are not intended to limit the embodiments of the present invention, and that various other modifications and changes may be made on the basis of the above description by those skilled in the art.
Claims (1)
1. The high-cleanness high-pressure anti-wear hydraulic oil is characterized in that:
is prepared by mixing a 2-alkyl oxazoline compound, higher alcohol, higher monomethyl carbonate and base oil;
the mass ratio of the 2-alkyl oxazoline compound, the higher alcohol, the higher methyl carbonate and the base oil is (10-30): (10-30):
(5～20)：(30～50)；
the structural formula of the 2-alkyl oxazoline compound is as follows:
-R has the formula: - (CH 2) n -2CH 3 ；
Where n is a positive integer from 10 to 24.
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