CN111117724A - Preparation method of modified PTFE (Polytetrafluoroethylene) ultrafine powder, modified PTFE ultrafine powder and nano energy-saving antiwear agent - Google Patents
Preparation method of modified PTFE (Polytetrafluoroethylene) ultrafine powder, modified PTFE ultrafine powder and nano energy-saving antiwear agent Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M147/00—Lubricating compositions characterised by the additive being a macromolecular compound containing halogen
- C10M147/02—Monomer containing carbon, hydrogen and halogen only
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M169/00—Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
- C10M169/04—Mixtures of base-materials and additives
- C10M169/044—Mixtures of base-materials and additives the additives being a mixture of non-macromolecular and macromolecular compounds
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2203/00—Organic non-macromolecular hydrocarbon compounds and hydrocarbon fractions as ingredients in lubricant compositions
- C10M2203/003—Organic non-macromolecular hydrocarbon compounds and hydrocarbon fractions as ingredients in lubricant compositions used as base material
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2203/00—Organic non-macromolecular hydrocarbon compounds and hydrocarbon fractions as ingredients in lubricant compositions
- C10M2203/10—Petroleum or coal fractions, e.g. tars, solvents, bitumen
- C10M2203/1006—Petroleum or coal fractions, e.g. tars, solvents, bitumen used as base material
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- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2205/00—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions
- C10M2205/02—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers
- C10M2205/028—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers containing aliphatic monomers having more than four carbon atoms
- C10M2205/0285—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers containing aliphatic monomers having more than four carbon atoms used as base material
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2213/00—Organic macromolecular compounds containing halogen as ingredients in lubricant compositions
- C10M2213/06—Perfluoro polymers
- C10M2213/062—Polytetrafluoroethylene [PTFE]
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
- C10M2215/086—Imides
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2223/00—Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions
- C10M2223/02—Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions having no phosphorus-to-carbon bonds
- C10M2223/04—Phosphate esters
- C10M2223/045—Metal containing thio derivatives
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2225/00—Organic macromolecular compounds containing phosphorus as ingredients in lubricant compositions
- C10M2225/04—Organic macromolecular compounds containing phosphorus as ingredients in lubricant compositions obtained by phosphorisation of macromolecualr compounds not containing phosphorus in the monomers
Abstract
The invention discloses a preparation method of modified PTFE (polytetrafluoroethylene) ultrafine powder, which comprises the following steps: (1) crushing and separating the irradiated cross-linked PTFE powder to obtain PTFE superfine powder with the particle size range of 0.4-0.6 mu m; (2) dissolving PTFE superfine powder in dialkyl dithiophosphoric acid, controlling the reaction temperature to be 90-150 ℃, keeping stirring, reacting for 3-5 hours at constant temperature, then carrying out solid-liquid separation, and drying to obtain modified PTFE superfine powder; the mass ratio of the dialkyl dithiophosphoric acid to the PTFE superfine powder is (2-5) to 1. Also provides modified PTFE superfine powder prepared by the method, and a nano energy-saving antiwear agent prepared by taking the modified PTFE superfine powder as a key component. The modified PTFE superfine powder has good dispersibility and anti-settling property in an organic solvent, and is not easy to settle and agglomerate for the second time, so that the modified PTFE superfine powder can not cause the secondary abrasion to mechanical equipment when being used as a lubricating oil anti-wear agent, and can not increase the friction coefficient, thereby ensuring that the mechanical equipment runs smoothly, prolonging the service life and greatly reducing the energy consumption for running.
Description
Technical Field
The invention belongs to the technical field of lubricating oil, and particularly relates to a preparation method of modified PTFE (polytetrafluoroethylene) ultrafine powder, the modified PTFE ultrafine powder and a nano energy-saving antiwear agent.
Background
The lubricating oil is a liquid or semisolid lubricating agent used on various types of automobiles and mechanical equipment to reduce friction and protect machines and workpieces, and mainly plays roles in lubrication, cooling, rust prevention, cleaning, sealing, buffering and the like. The quality of the lubricating effect of the lubricating oil plays an important role in the service life of mechanical equipment and whether energy is saved or not. Lubricating oils are prepared by adding various additives, such as: antiwear agents, antioxidants, dispersants, and the like form a well-balanced formulation for lubricating oil products. The antiwear agent is an important lubricating oil additive, and can reduce the friction of a metal surface, reduce the energy consumption of mechanical equipment in operation and prolong the service life of the mechanical equipment.
In the prior art, the antiwear agent mainly comprises a sulfur-containing antiwear agent, a phosphorus-containing antiwear agent, a chlorine-containing antiwear agent, a metal antiwear agent and the like. The sulfur-containing antiwear agent has a plurality of varieties, and mainly comprises sulfurized isobutylene, sulfurized grease, thioester, xanthate, thiocarbonate, dithiocarbamate, polysulfide and the like. Phosphorus-containing antiwear agents include T304(P), T305(S/P/N), dibutyl phosphite and the like. The chlorine-containing antiwear agent mainly comprises chlorinated paraffin and chlorinated fatty acid. The chlorinated paraffin has strong extreme pressure activity and good abrasion resistance, and is particularly suitable for metals difficult to process. However, chlorinated paraffin easily emits chlorine atoms under the conditions of heat and hydrolysis, and further emits hydrogen chloride, which causes iron corrosion and reduces the service life of mechanical equipment. Typical representatives of metal antiwear agents are lead naphthenate, zinc dialkyldithiophosphate, antimony dialkyldithiocarbamate, and the like. The zinc dialkyl dithiophosphate is a multi-effect additive with oxidation resistance, corrosion resistance and wear resistance, and is widely used in engine oil, wear-resistant hydraulic oil, industrial gear oil and other oil products. Zinc dialkyldithiophosphates are limited in their use because they can produce particulate ash in the exhaust gas, resulting in environmental regulations not being met.
With the continued development of antiwear agents, the use of nano-scaled Polytetrafluoroethylene (PTFE) to reduce wear is increasingly recognized and used. The nano polytetrafluoroethylene has various good characteristics:
(1) high temperature resistance, and the working temperature of the product can reach 250 ℃.
(2) Low temperature resistance, good mechanical toughness, 5 percent of elongation rate maintenance even if the temperature is reduced to-196 ℃, and good tensile strength.
(3) Corrosion resistance, inertness to most chemicals and solvents, strong acid and alkali resistance, water and various organic solvents.
(4) Weather resistance, is the best aging life in plastics.
(5) High lubrication is the lowest friction coefficient of solid materials.
(6) Non-stick, is the smallest surface tension in a solid material, and does not stick any substance.
(7) And does not generate cold flow when being pressed.
However, in the prior art, the nano polytetrafluoroethylene is easily agglomerated and settled in an organic solvent under the influence of van der waals force among particles, so that lubricating oil using the nano polytetrafluoroethylene as an anti-wear agent is easy to cause secondary wear to mechanical equipment, and the friction coefficient is increased, thereby reducing the service life of the mechanical equipment and increasing the energy consumption of the equipment. At present, the product application of taking nano polytetrafluoroethylene as a lubricating oil antiwear agent does not exist in the market.
The nano polytetrafluoroethylene antiwear agent in the prior art has unstable wear resistance and friction reduction performance, is easy to agglomerate and precipitate to cause secondary wear to mechanical equipment, and increases the friction coefficient, thereby reducing the service life and increasing the energy consumption of the equipment. Therefore, it is necessary to develop a new nano-polytetrafluoroethylene antiwear agent to solve the above technical problems.
Disclosure of Invention
The invention aims to provide a preparation method of a nano energy-saving antiwear agent, which aims to solve the problems that in the prior art, a nano polytetrafluoroethylene antiwear agent is easy to agglomerate and precipitate in an organic solvent, so that mechanical equipment generates secondary wear, the service life of the mechanical equipment is shortened, and the energy consumption is increased.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of modified PTFE (polytetrafluoroethylene) ultrafine powder comprises the following steps:
(1) crushing and separating the irradiated cross-linked PTFE powder to obtain PTFE superfine powder with the particle size range of D90 of 0.4-0.6 mu m;
(2) dissolving the PTFE superfine powder obtained in the step (1) in a formula amount in dialkyl dithiophosphoric acid in a formula amount, controlling the reaction temperature to be 90-150 ℃, keeping stirring, reacting at a constant temperature for 3-5 hours, then carrying out solid-liquid separation, and drying to obtain modified PTFE superfine powder;
the mass ratio of the dialkyl dithiophosphoric acid to the PTFE superfine powder is (2-5) to 1.
In the present invention, the irradiation-crosslinked PTFE powder is obtained by irradiation-crosslinking PTFE powder. The radiation crosslinking method in the prior art can be adopted by the person skilled in the art.
According to a preferred technical scheme of the invention, in the step (1), the irradiation cross-linked PTFE powder is obtained by irradiation cross-linking raw PTFE powder, and the method comprises the following preparation steps: placing raw material PTFE powder into an irradiation box, replacing air in the irradiation box with nitrogen, controlling the temperature of the irradiation box to be 335 +/-5 ℃, placing the irradiation box into an irradiation range of a 60Co source, and controlling the absorption dose to be 300-500 kGy to obtain the irradiation crosslinking PTFE powder; the particle size range of D90 of the raw material PTFE powder is 80-200 μm.
In the present invention, a commercially available product can be used as the raw material PTFE powder.
Preferably, in the step (1), the irradiation crosslinked PTFE powder is pulverized using an ultra-low temperature freezing type jet mill under the conditions: the pressure of a gas source main pipe is 0.18-0.25 MPa, the pressure of a feeding valve is 0.16-0.22 MPa, the crushing pressure is 0.18-0.32 MPa, the temperature of high-speed airflow is-165 +/-5 ℃, and the crushing time is 45-60 min; the separation mode is cyclone separation.
Preferably, in the step (2), the reaction temperature is 110-130 ℃, and the reaction is carried out for 4-5 hours at a constant temperature;
in the step (2), the drying conditions are as follows: vacuum drying is carried out, the vacuum degree is-0.10 to-0.15 MPa, and the drying temperature is 90 to 105 ℃.
Further preferably, in the step (2), the reaction temperature is 125 ℃, and the reaction is carried out for 4 hours at constant temperature.
In the step (2), the solid-liquid separation method is a conventional method in the prior art, such as filtration, suction filtration, and freeze drying.
The second purpose of the invention is to provide modified PTFE superfine powder which is prepared by the preparation method of the modified PTFE superfine powder.
The third purpose of the invention is to provide a nano energy-saving antiwear agent, which comprises the following components in parts by weight:
modified PTFE superfine powder: 20-30 parts by weight;
base oil: 55-65 parts by weight;
dispersing agent: 5-10 parts by weight;
antioxidant: 5-10 parts by weight;
the modified PTFE superfine powder is the modified PTFE superfine powder.
Preferably, the nanometer energy-saving antiwear agent comprises the following components in parts by weight:
modified PTFE superfine powder: 22-26 parts by weight;
base oil: 58-64 parts by weight;
dispersing agent: 5-10 parts by weight;
antioxidant: 5 to 10 parts by weight.
Preferably, the base oil is selected from: one or more of poly-alpha-olefin (PAO), hydroisomerization base oil, UCBO;
the dispersant is selected from: one or more of mono-succinimide T151, bis-succinimide T152 and T154;
the antioxidant is selected from: one or more of sulfur phosphorus dioctyl alkaline zinc salts T203, T202 and T205.
Further preferably, the base oil is a polyalphaolefin, PAO; the dispersant is mono-succinimide T151; the antioxidant is alkaline zinc salt T203 of sulfur, phosphorus and dioctyl.
Preferably, the D90 particle size range of the nano energy-saving antiwear agent is 40-70 nm.
The fourth purpose of the invention is to provide a preparation method of the nanometer energy-saving antiwear agent, which comprises the following preparation steps: stirring and mixing the components according to the formula ratio to form slurry, then placing the slurry into a nano grinder to grind, and controlling the grinding time to be 6-8 hours.
Preferably, the parameter conditions of the nanomilling machine are: the rotating speed is 600r/m, the output current is 60A, the maximum linear speed is 14m/s, and the air pressure is 2-4 bar.
The fifth purpose of the invention is to provide the application of the nano energy-saving antiwear agent as an antiwear agent of lubricating oil.
It should be noted that, a person skilled in the art can properly adjust the addition amount of the nano energy-saving antiwear agent in the lubricating oil according to actual needs.
Preferably, the addition amount of the nano energy-saving antiwear agent is 5-10 wt% of the mass of the lubricating oil. Within the addition range, the prepared lubricating oil has excellent wear resistance and friction reduction performance and excellent energy-saving performance.
Further preferably, the addition amount of the nano energy-saving antiwear agent is 5-7 wt% of the mass of the lubricating oil.
When the addition amount of the nano energy-saving antiwear agent is 5 wt% of the mass of the lubricating oil, the addition amount of the modified PTFE superfine powder is 1.0-1.5 wt% of the mass of the lubricating oil according to the formula.
When the addition amount of the nano energy-saving antiwear agent is 7 wt% of the mass of the lubricating oil, the addition amount of the modified PTFE superfine powder is 1.4-2.1 wt% of the mass of the lubricating oil according to the formula.
Further preferably, the addition amount of the nano energy-saving antiwear agent is 7 wt% of the mass of the lubricating oil.
Compared with the prior art, the invention has the following beneficial technical effects:
according to the preparation method of the modified PTFE superfine powder, the modified irradiation crosslinking PTFE superfine powder is modified by dialkyl dithiophosphoric acid, and the modified PTFE superfine powder modified by HDDP is obtained. The modified PTFE superfine powder has the advantages that a long-chain organic hydrophobic layer is formed on the surface of the modified PTFE superfine powder, the modified PTFE superfine powder has good dispersibility and anti-settling property in an organic solvent (base oil), and is not easy to settle and agglomerate secondarily, and when the nano energy-saving antiwear agent prepared from the modified PTFE superfine powder is used as a lubricating oil antiwear agent, secondary wear cannot be caused to mechanical equipment, and the friction coefficient cannot be increased. Meanwhile, the nano energy-saving antiwear agent disclosed by the invention does not cause environmental pollution, has a good environment-friendly effect, does not have corrosivity on mechanical equipment, and is beneficial to prolonging the service life of the mechanical equipment.
Detailed Description
The present invention will be further described with reference to the following examples. It should be understood that the following examples are illustrative only and are not intended to limit the scope of the present invention.
In the following examples, the particle diameter of D90 in the raw PTFE powder was 80 to 200. mu.m. Other raw materials are all commercially available.
In the invention, the ultra-low temperature freezing type jet mill adopts a German JSM jet mill. The crushing conditions are as follows: the pressure of a gas source main pipe is 0.18MPa, the pressure of a feeding valve is 0.16MPa, the crushing pressure is 0.18MPa, the temperature of high-speed airflow is-165 +/-5 ℃, and the crushing time is 45-60 min.
Particle size detection equipment: laser particle analyzer.
Preparation example 1 preparation of radiation-crosslinked PTFE powder
Placing raw material PTFE powder into a sealable galvanizing irradiation box, replacing air in the irradiation box with high-purity nitrogen, controlling the temperature of the irradiation box to be 335 +/-5 ℃, placing the irradiation box into an irradiation range of a 60Co source, controlling the absorption dose to be 300-500 kGy, and enabling molecular chains of the PTFE powder to generate crosslinking to obtain the irradiation crosslinked PTFE powder.
Example 1 preparation of ultrafine modified PTFE powder
(1) Crushing the irradiated cross-linked PTFE powder by a JSM jet mill, and then performing cyclone separation to obtain PTFE superfine powder with the particle size range of D90 of 0.4-0.6 mu m;
the radiation cross-linked absorption dose of the radiation cross-linked PTFE powder is 500 kGy; the crushing conditions are as follows: the pressure of a gas source main pipe is 0.18MPa, the pressure of a feeding valve is 0.16MPa, the crushing pressure is 0.18MPa, the temperature of high-speed airflow is-165 +/-5 ℃, and the crushing time is 60 min.
(2) Dissolving PTFE superfine powder in a proper amount of dialkyl dithiophosphoric acid, controlling the reaction temperature to be 125 ℃, keeping stirring, reacting for 4 hours at constant temperature, and filtering to obtain a solid mixture; then putting the solid mixture into a vacuum drier for drying, controlling the vacuum degree to be-0.10 to-0.15 MPa, and the drying temperature to be 90-105 ℃ to obtain modified PTFE superfine powder A1; the mass ratio of the PTFE superfine powder to the dialkyl dithiophosphoric acid is 3: 1.
Example 2 preparation of ultrafine modified PTFE powder
(1) Crushing the irradiated cross-linked PTFE powder by a JSM jet mill, and then performing cyclone separation to obtain PTFE superfine powder with the particle size range of D90 of 0.4-0.6 mu m;
the radiation-crosslinked absorbed dose of the radiation-crosslinked PTFE powder was 400 kGy; the crushing conditions are as follows: the pressure of a gas source main pipe is 0.25MPa, the pressure of a feeding valve is 0.22MPa, the crushing pressure is 0.32MPa, the temperature of high-speed airflow is-165 +/-5 ℃, and the crushing time is 45 min.
(2) Dissolving PTFE superfine powder in a proper amount of dialkyl dithiophosphoric acid, controlling the reaction temperature to be 130 ℃, keeping stirring, reacting for 5 hours at constant temperature, and filtering to obtain a solid mixture; then putting the solid mixture into a vacuum drier for drying, controlling the vacuum degree to be-0.10 to-0.15 MPa, and the drying temperature to be 90-105 ℃ to obtain modified PTFE superfine powder A2; the mass ratio of the PTFE superfine powder to the dialkyl dithiophosphoric acid is 5: 1.
Example 3 preparation of ultrafine modified PTFE powder
(1) Crushing the irradiated cross-linked PTFE powder by a JSM jet mill, and then performing cyclone separation to obtain PTFE superfine powder with the particle size range of D90 of 0.4-0.6 mu m;
the radiation-crosslinked absorbed dose of the radiation-crosslinked PTFE powder is 300 kGy; the crushing conditions are as follows: the pressure of a gas source main pipe is 0.20MPa, the pressure of a feeding valve is 0.20MPa, the crushing pressure is 0.25MPa, the temperature of high-speed airflow is-165 +/-5 ℃, and the crushing time is 50 min.
(2) Dissolving PTFE superfine powder in a proper amount of dialkyl dithiophosphoric acid, controlling the reaction temperature to be 110 ℃, keeping stirring, reacting for 5 hours at constant temperature, and filtering to obtain a solid mixture; then putting the solid mixture into a vacuum drier for drying, controlling the vacuum degree to be-0.10 to-0.15 MPa, and the drying temperature to be 90-105 ℃ to obtain modified PTFE superfine powder A3; the mass ratio of the PTFE superfine powder to the dialkyl dithiophosphoric acid is 2: 1.
Example 4 preparation of ultrafine modified PTFE powder
The basic steps and parameters are the same as those of example 1, except that in the step (2), the reaction temperature is controlled to be 90 ℃, stirring is kept, the reaction is carried out for 5 hours at constant temperature, and then filtration is carried out to obtain a solid mixture;
finally, modified PTFE superfine powder A4 is obtained.
Example 5 preparation of ultrafine modified PTFE powder
The basic steps and parameters are the same as those of example 1, except that in the step (2), the reaction temperature is controlled to be 150 ℃, stirring is kept, the reaction is carried out for 3 hours at constant temperature, and then filtration is carried out to obtain a solid mixture;
finally, modified PTFE superfine powder A5 is obtained.
Examples 6-11, Nano energy-saving antiwear Agents
The formulations of the nano energy-saving antiwear agents of examples 6-11 are shown in Table 1.
TABLE 1 nanometer energy-saving antiwear agent formulation
The preparation method of the nanometer energy-saving antiwear agent of the embodiment 6 to 11 comprises the following preparation steps:
stirring and mixing the components according to the formula ratio to form slurry, then placing the slurry into a nano grinder to grind, and controlling the grinding time to be 6-8 hours. The parameter conditions of the nano-grinder are as follows: the rotating speed is 600r/m, the output current is 60A, the maximum linear speed is 14m/s, and the air pressure is 2-4 bar.
The nano energy-saving antiwear agents of examples 6-11 are respectively counted as antiwear agents B1-B6. The D90 particle size range of the antiwear agent B1-B6 detected by a laser particle sizer is 40-70 nm.
Comparative example 1 preparation of antiwear agent B7 from radiation-crosslinked PTFE micropowder
The antiwear agent B7 formulation was essentially the same as formulation 1 except that the modified PTFE micropowder A1 in formulation 1 was replaced with radiation crosslinked PTFE micropowder. The preparation method is the same as that of example 7, and the antiwear agent B7 taking the irradiation crosslinking PTFE superfine powder as a key component is finally obtained. The D90 particle size of the antiwear agent B7 detected by a laser particle sizer is 55 nm.
Comparative example 2 preparation of antiwear agent B8
The formula of the antiwear agent B8 is basically the same as that of the formula 1, except that 25 parts by weight of equivalent sulfur-containing extreme pressure antiwear agent sulfurized isobutylene T321 is used as a key component to replace the modified PTFE superfine powder A1 in the formula 1. The preparation method comprises the following steps: the components are adjusted and prepared under the condition of constant temperature of 85 ℃.
Comparative example 3 preparation of antiwear agent B9
The formula of the antiwear agent B9 is basically the same as that of the formula 1, except that 25 parts by weight of phosphorus-containing extreme pressure antifriction agent dibutyl phosphite with the same amount is used as a key component to replace the modified PTFE superfine powder A1 in the formula 1. The preparation method comprises the following steps: the components are adjusted and prepared under the condition of constant temperature of 85 ℃.
Example 12 Performance test
(I) Dispersion stability test
The antiwear agents B1-B7 were left to stand for 30 days, and observed to be: the antiwear agent B1-B6 prepared by taking the modified PTFE superfine powder modified by HDDP as a key component has no layering, the antiwear agent B7 prepared by taking the irradiation crosslinking PTFE superfine powder which is not modified by HDDP as a key component has complete layering, and the irradiation crosslinking PTFE superfine powder is completely settled to the bottom of the solution. Therefore, the antiwear agent B7 prepared by using the radiation cross-linked PTFE superfine powder which is not modified by HDDP as a key component has poor dispersion performance, and the antiwear agent B1-B6 prepared by using the modified PTFE superfine powder modified by HDDP as a key component has good dispersion performance.
(II) detection of anti-wear and anti-friction performance
The detection methods of the non-seizing load, the sintering load, the friction coefficient and the wear scar diameter are GB/T3142, GB/T12583 and GB/T0762 respectively.
(1) The antiwear agents B1 to B9 were added to an appropriate amount of the polyalphaolefin PAO40 in an amount of 7 wt% to obtain test samples C1 to C9, and the test samples C1 to C9 were tested for seizure-free load, sintering load, friction coefficient, and wear-leveling diameter, the results of which are shown in Table 2.
TABLE 2 results of the testing of the anti-wear and anti-friction properties
The results in Table 2 show that the friction coefficients of samples C1-C6 are much lower than those of samples C8 and C9, and are also significantly lower than that of sample C7, and the friction coefficients of samples C1-C6 are 51.0% -71.8% of C7, 29.3% -41.5% of C8, and 26.3% -37.2% of C9. The nano energy-saving antiwear agent prepared in the embodiments 1 to 6 of the invention has excellent antifriction performance. The wear-scar diameters of samples C1-C6 are far smaller than those of samples C8 and C9 and are also obviously lower than that of C7, and the wear-scar diameters of samples C1-C6 are 82.6-93.5% of that of C7, 74.5-84.3% of that of C8 and 71.7-81.1% of that of C9. The nano energy-saving antiwear agent prepared in the embodiments 1 to 6 of the invention has excellent antiwear performance.
The non-seizure load and the sintering load of the samples C1-C6 are much higher than those of the samples C8 and C9 and also much higher than that of the samples C7, and the non-seizure load of the samples C1-C6 is 1.1-1.3 times of that of the samples C7, 1.8-2.1 times of that of the samples C8 and 1.7-2.0 times of that of the samples C9. The sintering load of the sample C1-C6 is 1.3-2.0 times of that of C7, 1.6-2.5 times of that of C8, and 1.6-2.5 times of that of C9. The nano energy-saving antiwear agent prepared in the embodiments 1 to 6 of the invention has excellent antiwear and antifriction performances.
(2) Of B1-B6, the anti-wear agent B1 having the best anti-wear and anti-friction effects and the B4 having the relatively poor anti-friction effects were added to an appropriate amount of the polyalphaolefin PAO40 in amounts of 5 wt%, 7 wt%, 8.5 wt% and 10 wt%, respectively, to obtain test samples C1-1, C1-2, C1-3 and C1-4, C4-1, C4-2, C4-3 and C4-4, and the non-seizure load, sintering load, friction coefficient and wear-scar diameter of 8 samples were tested, and the results are shown in Table 3.
Table 3 shows the results of the tests on the anti-wear and anti-friction properties of the anti-wear agents B1 and B4 at different addition levels
As can be seen from the data in Table 3, the antiwear agents B1 and B4 were added in the range of 5 wt% to 10 wt% to give samples having good antiwear and antifriction properties. The antiwear agents B1-B6 can achieve good antiwear and antifriction performances when the addition amount is in the range of 5 wt% -10 wt%.
Example 13 Industrial practical application
(1) And the antiwear agent B1-B9 is added into 460# industrial closed gear oil in an addition amount of 7 wt% and is used for lubricating a cement ball mill of a main motor of a cement plant. And under the working condition of the same energy production, detecting the power consumption per hour. When only 460# industrial closed gear oil is adopted, the cement ball mill of the cement ball mill is 3225 KW. The results of the hourly power consumption of the cement ball mill using 460# industrial closed gear oil with antiwear agents B1-B9 added are shown in Table 4.
TABLE 4 energy consumption test results
From the results of Table 4, it is understood that the addition of the antiwear agents B8 and B9 has little effect on the reduction of power consumption; even the power consumption was increased after the addition of B9, and the power consumption was slightly decreased after the addition of B7, but the decrease was as small as about 1.4%. After the antiwear agent B1-B6 is added, the power consumption per hour is reduced from 3225KW to 2930-3072 KW, and the energy consumption is reduced by 4.7% -9.1%. In the industrial application field, the energy consumption is reduced by 4.7-9.1%, and the operation cost can be obviously reduced.
Taking a cement ball mill as an example, the cement ball mill runs for 20 hours every day and 300 days in a year, the total running time in a year is 6000 hours. The antiwear agents B1-B6 have average power consumption of 3010KW per hour, and the energy saving is at least (3180) KW × 6000h (1020000 KW. h) 1020000 degrees. When the price of the industrial level period is 0.725 yuan, 739500 yuan can be saved in total in one year, and about 74 ten thousand yuan can be saved. Therefore, the energy-saving effect of the antiwear agent B1-B6 added into lubricating oil is quite good.
(2) And B1-B6, the antiwear agent B1 with the best energy-saving effect and the B4 with relatively poor energy-saving effect are respectively added into 460# industrial closed gear oil in the addition amounts of 5 wt%, 7 wt%, 8.5 wt% and 10 wt% for lubricating a cement ball mill of a main motor of a cement plant. The results are shown in Table 5.
Table 5 shows the energy consumption detection results of the antiwear agents B1, B4 and B7-B9 at different addition amounts
As can be seen from the data in Table 5, when the antiwear agents B1 and B4 were added in the range of 5 wt% to 10 wt%, the power consumption per hour was significantly lower than that when the same amounts of lubricating oils B7, B8 and B9 were added, indicating that the antiwear agents B1 and B4 were added in the range of 5 wt% to 10 wt% and had good energy saving properties. Further shows that the antiwear agents B1-B6 can achieve good energy-saving performance when the addition amount is in the range of 5 wt% -10 wt%.
However, when the amount of the additive is 7 wt%, not only the abrasion resistance and the friction reducing effect are excellent, but also the reduction of the power consumption per hour is already obvious. When the addition amount is continuously increased, the amount of continuous decrease in the power consumption per hour is insignificant, and the cost of the antiwear agent increases. Thus. Under the premise of comprehensive cost, the addition amount should not exceed 10 wt%.
The embodiments of the present invention have been described in detail, but the embodiments are merely examples, and the present invention is not limited to the embodiments described above. Any equivalent modifications or alterations to this practice will occur to those skilled in the art and are intended to be within the scope of this invention. Accordingly, equivalent changes and modifications made without departing from the spirit and scope of the present invention should be covered by the present invention.
Claims (13)
1. The preparation method of the modified PTFE superfine powder is characterized by comprising the following steps:
(1) crushing and separating the irradiated cross-linked PTFE powder to obtain PTFE superfine powder with the particle size range of D90 of 0.4-0.6 mu m;
(2) dissolving the PTFE superfine powder obtained in the step (1) in a formula amount in dialkyl dithiophosphoric acid in a formula amount, controlling the reaction temperature to be 90-150 ℃, keeping stirring, reacting at a constant temperature for 3-5 hours, then carrying out solid-liquid separation, and drying to obtain modified PTFE superfine powder;
the mass ratio of the dialkyl dithiophosphoric acid to the PTFE superfine powder is (2-5) to 1.
2. The preparation method of the modified PTFE submicron powder according to the claim 1, characterized in that in the step (1), the irradiation cross-linked PTFE powder is obtained by irradiation cross-linking the raw PTFE powder, and the preparation method comprises the following preparation steps: placing raw material PTFE powder into an irradiation box, replacing air in the irradiation box with nitrogen, controlling the temperature of the irradiation box to be 335 +/-5 ℃, placing the irradiation box into an irradiation range of a 60Co source, and controlling the absorption dose to be 300-500 kGy to obtain the irradiation crosslinking PTFE powder; the particle size range of D90 of the raw material PTFE powder is 80-200 μm.
3. The method for preparing modified PTFE micropowder of claim 1, wherein in the step (1), the irradiation-crosslinked PTFE powder is pulverized by an ultra-low temperature refrigerated air jet pulverizer under the following conditions: the pressure of a gas source main pipe is 0.18-0.25 MPa, the pressure of a feeding valve is 0.16-0.22 MPa, the crushing pressure is 0.18-0.32 MPa, the temperature of high-speed airflow is-165 +/-5 ℃, and the crushing time is 45-60 min; the separation mode is cyclone separation.
4. The preparation method of the modified PTFE superfine powder according to claim 1, wherein in the step (2), the reaction temperature is 110-130 ℃, and the reaction is carried out for 4-5 hours at a constant temperature;
in the step (2), the drying conditions are as follows: vacuum drying is carried out, the vacuum degree is-0.10 to-0.15 MPa, and the drying temperature is 90 to 105 ℃.
5. Modified PTFE micropowder characterized by being produced by the production method for modified PTFE micropowder according to any one of claims 1 to 4.
6. The nanometer energy-saving antiwear agent is characterized by comprising the following components in parts by weight:
modified PTFE superfine powder: 20-30 parts by weight;
base oil: 55-65 parts by weight;
dispersing agent: 5-10 parts by weight;
antioxidant: 5-10 parts by weight;
the modified PTFE ultrafine powder is the modified PTFE ultrafine powder according to claim 5.
7. The nano energy-saving antiwear agent according to claim 6, characterized by comprising the following components in parts by weight:
modified PTFE superfine powder: 22-26 parts by weight;
base oil: 58-64 parts by weight;
dispersing agent: 5-10 parts by weight;
antioxidant: 5 to 10 parts by weight.
8. The nanometer energy-saving antiwear agent according to claim 6, characterized in that,
the base oil is selected from: one or more of poly-alpha-olefin (PAO), hydroisomerization base oil, UCBO;
the dispersant is selected from: one or more of mono-succinimide T151, bis-succinimide T152 and T154;
the antioxidant is selected from: one or more of sulfur phosphorus dioctyl alkaline zinc salts T203, T202 and T205.
9. The nano energy-saving antiwear agent according to claim 8, wherein the base oil is a polyalphaolefin PAO; the dispersant is mono-succinimide T151; the antioxidant is alkaline zinc salt T203 of sulfur, phosphorus and dioctyl.
10. The nanometer energy-saving antiwear agent according to claim 6, wherein the D90 particle size range of the nanometer energy-saving antiwear agent is 40-70 nm.
11. The preparation method of the nanometer energy-saving antiwear agent of any one of claims 6 to 10, characterized by comprising the following preparation steps: stirring and mixing the components according to the formula ratio to form slurry, then placing the slurry into a nano grinder to grind, and controlling the grinding time to be 6-8 hours.
12. Use of the nano energy-saving antiwear agent according to any one of claims 6 to 10, characterized in that it is used as an antiwear agent for lubricating oil.
13. The application of the nano energy-saving antiwear agent disclosed by any one of claims 6 to 10, wherein the addition amount of the nano energy-saving antiwear agent is 5-10 wt% of the mass of lubricating oil.
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