CN115521708B - Super-lubricating coating based on polydimethylsiloxane polymer molecular brush and preparation method thereof - Google Patents

Super-lubricating coating based on polydimethylsiloxane polymer molecular brush and preparation method thereof Download PDF

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CN115521708B
CN115521708B CN202211283011.6A CN202211283011A CN115521708B CN 115521708 B CN115521708 B CN 115521708B CN 202211283011 A CN202211283011 A CN 202211283011A CN 115521708 B CN115521708 B CN 115521708B
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polydimethylsiloxane
super
epoxy resin
polymer molecular
molecular brush
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CN115521708A (en
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宋浩杰
王潼
魏千竣
杨进
贾晓华
王思哲
李永
邵丹
冯雷
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Shaanxi University of Science and Technology
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
    • C09D183/10—Block or graft copolymers containing polysiloxane sequences
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D5/00—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures
    • B05D5/08—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures to obtain an anti-friction or anti-adhesive surface
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
    • B05D7/50—Multilayers
    • B05D7/52—Two layers
    • B05D7/54—No clear coat specified
    • B05D7/548—No curing step for the last layer
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
    • C08G77/42—Block-or graft-polymers containing polysiloxane sequences

Abstract

The invention relates to the technical field of preparation of super-lubricating coating materials, and in particular discloses a super-lubricating coating based on a polydimethylsiloxane polymer molecular brush and a preparation method thereof, wherein the preparation method comprises the following steps: adding an organic solvent into the epoxy resin, stirring, adding a curing agent and polydimethylsiloxane, and dispersing the component 1; adding an organic solvent into epoxy resin, stirring, adding polydimethylsiloxane, and dispersing to obtain a component 2; mixing the component 1 and the component 2, and stirring to obtain a mixture; and (3) spraying the mixture on the surface of a substrate, solidifying, then dropwise adding nonpolar liquid C on the surface of the coating, and standing to obtain the super-lubrication coating based on the polydimethylsiloxane polymer molecular brush. The lubricating coating obtained by the preparation method of the super lubricating coating based on the polydimethylsiloxane polymer molecular brush has the advantages of high wear resistance and low friction coefficient.

Description

Super-lubricating coating based on polydimethylsiloxane polymer molecular brush and preparation method thereof
Technical Field
The invention relates to the technical field of preparation of super-lubricating coating materials, in particular to a super-lubricating coating based on a polydimethylsiloxane polymer molecular brush and a preparation method thereof.
Background
The friction and abrasion cause the damage faults of devices, the service life is shortened, the fuel oil resources are used in an aggravated mode, and the resource energy is wasted seriously. While a lubricious coating is critical to minimize damage to the underlying materials and ensure low energy dissipation in the mechanical system. Polymer molecular brushes (e.g., polydimethylsiloxane molecular brushes), which are biomimetic to the natural synovial joint microstructure and lubrication mechanism, polymer chains form brush structures on the surface of high grafting density in good solvents due to exclusion of volume-dominated inter-chain interactions. The polymer molecular brush as a lubricating coating can reduce the dynamic friction coefficient of the modified surface by several orders of magnitude compared to a bare or oil lubricated surface, thereby attracting widespread attention of researchers.
The preparation method of the polymer molecular brush super-lubricating coating comprises a surface grafting method and a coating method, and PDMS brush is introduced into thermosetting resin such as epoxy resin, polyurethane resin and the like. During the curing process, PDMS is grafted in an epoxy resin system through ring-opening polymerization reaction, and the PDMS tends to aggregate towards the surface of the coating due to the low surface energy and high flow property of the PDMS, so that a compact polymer molecular brush layer is formed on the surface of the coating.
However, the inventors found that the abrasion resistance of the polymer molecular brush super-lubricating coating in the related art needs to be improved, and a super-lubricating coating having high abrasion resistance and low friction coefficient is highly demanded.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention aims to provide the super-lubricating coating based on the polydimethylsiloxane polymer molecular brush and the preparation method thereof, and the epoxy super-lubricating coating can have high wear resistance and low friction coefficient.
In order to achieve the above purpose, the invention is realized by adopting the following technical scheme:
in a first aspect, the present invention provides a method of preparing a super-lubricious coating based on a polydimethylsiloxane polymer molecular brush.
A method for preparing a super-lubricating coating based on a polydimethylsiloxane polymer molecular brush, comprising the following steps:
step one, preparing a component 1:
adding an organic solvent into epoxy resin, stirring, adding a curing agent and polydimethylsiloxane, and performing ultrasonic dispersion to obtain a component 1; based on the total mass of the epoxy resin, the polydimethylsiloxane and the curing agent, the mass percent of the epoxy resin is 50-56%, the mass percent of the polydimethylsiloxane is 4-8%, and the balance is the curing agent;
step two, preparing a component 2:
adding an organic solvent into epoxy resin, stirring, adding polydimethylsiloxane, and performing ultrasonic dispersion to obtain a component 2; based on the total mass of the epoxy resin and the polydimethylsiloxane, the mass percent of the epoxy resin is 80-90%, and the mass percent of the polydimethylsiloxane mixture is 10-20%;
preparing a super-lubricating coating based on a polydimethylsiloxane polymer molecular brush:
mixing the component 1 and the component 2, and stirring to obtain a mixture; and (3) spraying the mixture on the surface of a substrate, solidifying, then dropwise adding nonpolar liquid C on the surface of the coating, and standing to obtain the super-lubrication coating based on the polydimethylsiloxane polymer molecular brush.
Further, the epoxy resin is one or more of bisphenol A type epoxy resin, bisphenol F type epoxy resin, aliphatic glycidyl ether type epoxy resin, glycidyl ester type epoxy resin or glycidyl amine type epoxy resin.
Further, the polydimethylsiloxane is one or more of monoglycidyl ether end-capped polydimethylsiloxane, diglycidyl ether end-capped polydimethylsiloxane and trimethylsiloxane end-capped polydimethylsiloxane; the concentration of the polydimethylsiloxane molecular brush solution is 0.8-1 mol/L.
Further, the curing agent in the first step is one of polyamide, ethylenediamine, polyetheramine and diethylenetriamine.
Further, the nonpolar liquid C in the third step is one of methyl silicone oil, ethyl silicone oil, phenyl silicone oil, methyl hydroxyl silicone oil, hydroxyl hydrogen silicone oil, dodecane, hexadecane, poly alpha olefin, toluene, isopropanol and dimethylformamide.
Further, the organic solvent in the first step is one or more of ethyl acetate and ethanol; the organic solvent in the second step is one or more of acetone, toluene and xylene.
Further, in the third step, the curing temperature is 120-130 ℃ and the curing time is 2-3 h.
Further, the spraying pressure in the third step is 1500-1900 Psi.
Further, the standing environment after the nonpolar liquid C is dripped in the third step is a ventilated dust-free environment.
In a second aspect, the present invention provides a super-lubricious coating based on a polydimethylsiloxane polymer molecular brush.
A super-lubricating coating based on a polydimethylsiloxane polymer molecular brush is prepared by the method.
Compared with the prior art, the invention has the following technical effects:
the fluidity and extensibility of the polymer molecular brush affect the surface friction performance, while the nonpolar liquid (such as methyl silicone oil, phenyl silicone oil, hexadecane, poly alpha olefin, toluene, isopropanol and the like) in the invention has good miscibility with the polymer chain, which can cause the expansion of the polymer chain to increase the liquid fluidity of the polymer chain, thereby being beneficial to remarkably improving the bearing capacity and lubricity of the friction surface by reducing the shear strength of the coating and improving the friction performance of the coating.
In the super-lubricating coating based on the polydimethylsiloxane polymer molecular brush, PDMS and epoxy resin are subjected to ring-opening polymerization reaction at high temperature and are orderly and densely connected together, so that a compact polydimethylsiloxane chain brush is formed on the surface of the coating. Non-polar liquids such as silicone oils have low surface tension. Has good compatibility with PDMS chains. When they come into contact, the surface of the coating is dissolved by a non-polar liquid such as silicone oil, which causes the polymer chains to move and rotate, just like a brush. Meanwhile, the PDMS chain is connected with the coating through a covalent bond, so that the compact polydimethylsiloxane chain brush layer has good mechanical strength and stability.
In addition, the good miscibility of the polymer chain and nonpolar liquid such as silicone oil can lead to the expansion of the polymer chain, increase the liquid fluidity of the polymer chain, be favorable for the coating to obviously improve the bearing capacity and lubricity of the friction surface by reducing the shear strength, and improve the friction performance of the coating. Finally, the liquid lubrication layer generated by dripping nonpolar liquid such as silicone oil on the surface of the coating plays a role in lubrication, and can cover the defects existing on the surface of the coating and not covered by the PDMS chain brush, so that the stability and the wear resistance of the coating are enhanced.
Thus, the polydimethylsiloxane polymer molecular brush super-lubricating coating prepared by the method has good wear resistance, lubricating performance and stability and good operability.
Drawings
FIG. 1 is a physical view of the coating in example 1 of the present invention;
FIG. 2 is a scanning electron microscope image of a polydimethylsiloxane polymer molecular brush super-lubricious coating prepared in example 1 of the present invention;
FIG. 3 is a graph showing the abrasion mark and 3D morphology of the polydimethylsiloxane polymer molecular brush super-lubricating coating prepared in example 1 of the present invention after friction test;
FIG. 4 is a graph showing the friction coefficients of the lubricating coatings prepared in examples 1, 2, and 3 of the present invention;
FIG. 5 is a graph showing the friction coefficient of the lubricating coatings prepared in examples 4 and 5 of the present invention;
FIG. 6 is a bar graph of the average friction coefficient of the lubricating coatings prepared in examples 1, 2, 3, 4, 5 of the present invention;
FIG. 7 is a bar graph of wear rates of the lubricating coatings prepared in examples 1, 2, 3, 4, 5 of the present invention;
FIG. 8 is a bar graph of the average coefficient of friction of the super slip coatings prepared in inventive example 1 and comparative examples 1 and 2.
Detailed Description
The following examples illustrate the invention in further detail.
The substrate used in the embodiment of the invention is 1060 aluminum plate, and the substrate is provided with pretreatment steps before spraying, and the pretreatment steps of the substrate are specifically that absolute ethyl alcohol is adopted for wiping before spraying.
Examples
Example 1
A method for preparing a super-lubricating coating based on a polydimethylsiloxane polymer molecular brush, comprising the following steps:
step one, preparing a component 1:
2.6g of tetraglycidyl amine type epoxy resin, 25ml of absolute ethyl alcohol and 25ml of ethyl acetate are added into a 100ml beaker, stirred and dispersed for 40min at a rotating speed of 2000r/min on a magnetic stirrer, and then 2.2g of polyamide and 0.2g of monoglycidyl ether end-capped polydimethylsiloxane are added, and ultrasonic dispersion is carried out for 20min, so that a coating component 1 is prepared;
step two, preparing a component 2:
adding 0.9g of tetraglycidyl amine type epoxy resin, 25ml of acetone and 25ml of dimethylbenzene into a 100ml beaker, stirring and dispersing for 35min at a rotating speed of 1500r/min on a magnetic stirrer, adding 0.05g of mono-glycidyl ether end-capped polydimethylsiloxane and 0.05g of diglycidyl ether end-capped polydimethylsiloxane, and performing ultrasonic dispersion for 15min to obtain a coating component 2;
preparing a super-lubricating coating based on a polydimethylsiloxane polymer molecular brush:
firstly, mixing the component 1 and the component 2 in a 200ml beaker, and dispersing for 45min on magnetic stirring at a rotating speed of 2000r/min to obtain a mixture; then, the mixture was added to a spraying apparatus, sprayed onto the substrate surface at a pressure of 1500Psi, and the coating was cured at 120 ℃ for two hours; and finally, dripping 5ml of methyl silicone oil on the surface of the cured coating by using a dropper, and standing for 2 hours in a ventilated dust-free environment to obtain the super-lubrication coating based on the polydimethylsiloxane polymer molecular brush.
From FIG. 1, it can be seen that the polydimethylsiloxane polymer molecular brush prepared by the invention has a smooth and flat super-lubrication coating; as can be seen from FIG. 2, the surface of the coating is distributed with silicone oil pools having diameters varying from 8 to 77 μm.
Example 2
A method for preparing a super-lubricating coating based on a polydimethylsiloxane polymer molecular brush, comprising the following steps:
step one, preparing a component 1:
2.55g of bisphenol A epoxy resin and 50ml of absolute ethyl alcohol are added into a 100ml beaker, stirred and dispersed for 45min at a rotating speed of 1800r/min on a magnetic stirrer, and then 2.15g of polyether amine and 0.3g of monoglycidyl ether end-capped polydimethylsiloxane are added, and ultrasonic dispersion is carried out for 20min, so that a coating component 1 is prepared;
step two, preparing a component 2:
adding 0.85g bisphenol A epoxy resin and 50ml acetone into a 100ml beaker, stirring and dispersing for 30min on a magnetic stirrer at a rotating speed of 1600r/min, adding 0.15g monoglycidyl ether end-capped polydimethylsiloxane, and performing ultrasonic dispersion for 15min to prepare a coating component 2;
preparing a super-lubricating coating based on a polydimethylsiloxane polymer molecular brush:
firstly, mixing the component 1 and the component 2 in a 200ml beaker, and dispersing for 50min on magnetic stirring at a rotation speed of 1800r/min to obtain a mixture; then, the mixture was added to a spraying apparatus, sprayed onto the substrate surface at a pressure of 1700Psi, and the coating was cured at 120 ℃ for two hours; finally, dripping 5ml of poly alpha olefin on the surface of the cured coating by using a dropper, and standing for 2 hours in a ventilated dust-free environment to obtain the polydimethylsiloxane polymer molecular brush super-lubrication coating 。
Example 3
A method for preparing a super-lubricating coating based on a polydimethylsiloxane polymer molecular brush, comprising the following steps:
step one, preparing a component 1:
2.5g of bisphenol F epoxy resin and 50ml of absolute ethyl alcohol are added into a 100ml beaker, stirred and dispersed for 50min at a rotating speed of 1600r/min on a magnetic stirrer, and then 2.1g of ethylenediamine and 0.4g of trimethyl siloxane end-capped polydimethylsiloxane are added, and ultrasonic dispersion is carried out for 20min, so that a coating component 1 is prepared;
step two, preparing a component 2:
adding 0.8g bisphenol F epoxy resin and 50ml xylene into a 100ml beaker, stirring and dispersing for 25min on a magnetic stirrer at a rotating speed of 1700r/min, adding 0.2g monoglycidyl ether end-capped polydimethylsiloxane, and performing ultrasonic dispersion for 15min to prepare a coating component 2;
preparing a super-lubricating coating based on a polydimethylsiloxane polymer molecular brush:
firstly, mixing the component 1 and the component 2 in a 200ml beaker, and dispersing for 45min on magnetic stirring at a rotating speed of 1600r/min to obtain a mixture; then, the mixture was fed into a spraying apparatus, sprayed onto the surface of a substrate at a pressure of 1900Psi, and the coating was cured at 120 ℃ for two hours; and finally, dripping 5ml of phenyl silicone oil on the surface of the cured coating by using a dropper, and standing for 2 hours in a ventilated dust-free environment to obtain the polydimethylsiloxane polymer molecular brush super-lubrication coating.
Example 4
A preparation method of a super-lubricating coating based on a polydimethylsiloxane polymer molecular brush is carried out according to the method in the embodiment 1, and is characterized in that epoxy resin in raw materials is aliphatic glycidyl ether type epoxy resin, a curing agent is polyether amine, an organic solution B is toluene, and a nonpolar liquid C is hexadecane; the addition amount of the aliphatic glycidyl ether type epoxy resin is 2.8g, the addition amount of polyether amine is 2g, the addition amount of mono-glycidyl ether end-capped polydimethylsiloxane is 0.2g, and the curing temperature in the third step is 130 ℃ and the curing time is 3h.
Example 5
A preparation method of a super-lubricating coating based on a polydimethylsiloxane polymer molecular brush is carried out according to the method in the embodiment 1, except that epoxy resin in raw materials is glycidyl ester type epoxy resin, a curing agent is diethylenetriamine, and nonpolar liquid C is isopropanol.
Example 6
A preparation method of a super-lubricating coating based on a polydimethylsiloxane polymer molecular brush is carried out according to the method in the embodiment 1, except that epoxy resin in raw materials is glycidylamine type epoxy resin, and nonpolar liquid C is dimethylformamide.
Comparative example
Comparative example 1
A preparation method of a super-lubricating coating based on a polydimethylsiloxane polymer molecular brush is carried out according to the method in the example 1, except that the dimethyl silicone oil is not dripped on the surface of the cured coating in the step three.
Comparative example 2
A preparation method of a super-lubricating coating based on a polydimethylsiloxane polymer molecular brush is carried out according to the method in the example 1, except that polydimethylsiloxane is not added in the step one and the step two.
Performance detection
The lubricating coatings of examples 1 to 5 and comparative examples 1 to 2 were subjected to friction test under the following conditions: the super-lubricating coating and the steel ball are subjected to opposite grinding, and friction test conditions are as follows: the load is 3N, the rotating speed is 5cm/s, the running time is 1.0h, and the friction coefficient and the wear rate are the average value of 3-5 tests.
Referring to fig. 3 to 8, fig. 3 is a graph showing the abrasion mark and 3D morphology of the polydimethylsiloxane polymer molecular brush super-lubricating coating prepared in example 1 according to the present invention after a friction test; FIG. 4 is a graph showing the friction coefficient of the lubricating coatings prepared in examples 1, 2 and 3 according to the present invention, and FIG. 5 is a graph showing the friction coefficient of the lubricating coatings prepared in examples 4 and 5; FIG. 6 is a bar graph of the average friction coefficient of the lubricating coatings prepared in examples 1, 2, 3, 4, 5 of the present invention; FIG. 7 is a bar graph of wear rates of the lubricating coatings prepared in examples 1, 2, 3, 4, 5 of the present invention; FIG. 8 is a bar graph of the average coefficient of friction of the super slip coatings prepared in inventive example 1 and comparative examples 1 and 2.
As can be seen from fig. 3, the coating remains intact after 1h of friction under a 3N load, leaving only slight wear marks on the surface of the coating, the wear resistance being higher than most super-lubricious coatings; as can be seen from FIGS. 3 to 7, the lubricating coatings prepared in examples 1 to 5 exhibited low friction coefficients and wear rates after friction for 1 hour under a load of 3N, the average friction coefficient was maintained at 0.01 to 0.035, and the wear rate was at least 1.7X10 -4 mm 3 ·N·m -1 And example 1 preparation of a lubricating coating left only slight grinding marks on the surface, the average depth of the grinding marks was 1.59 μm, the average width of the grinding marksThe degree is 87.14 mu m, which shows that the polydimethylsiloxane polymer molecular brush super-lubricating coating prepared by the invention has excellent wear resistance and antifriction performance; from fig. 8, it can be shown from example 1 and comparative examples 1 to 2 that the polydimethylsiloxane chain brush and the simethicone in the coating prepared by the invention have a remarkable improvement effect on the friction performance of the lubricating coating.

Claims (7)

1. A method for preparing a super-lubricating coating based on a polydimethylsiloxane polymer molecular brush, which is characterized by comprising the following steps:
step one, preparing a component 1:
adding an organic solvent into epoxy resin, stirring, adding a curing agent and polydimethylsiloxane, and performing ultrasonic dispersion to obtain a component 1; based on the total mass of the epoxy resin, the polydimethylsiloxane and the curing agent, the mass percent of the epoxy resin is 50% -56%, the mass percent of the polydimethylsiloxane is 4% -8%, and the balance is the curing agent;
step two, preparing a component 2:
adding an organic solvent into epoxy resin, stirring, adding polydimethylsiloxane, and performing ultrasonic dispersion to obtain a component 2; based on the total mass of the epoxy resin and the polydimethylsiloxane, the mass percent of the epoxy resin is 80% -90%, and the mass percent of the polydimethylsiloxane mixture is 10% -20%;
preparing a super-lubricating coating based on a polydimethylsiloxane polymer molecular brush:
mixing the component 1 and the component 2, and stirring to obtain a mixture; spraying the mixture on the surface of a substrate, solidifying, then, dripping liquid C on the surface of the coating, and standing to obtain the super-lubrication coating based on the polydimethylsiloxane polymer molecular brush; the liquid C is one of methyl silicone oil, ethyl silicone oil, phenyl silicone oil, methyl hydroxyl silicone oil, hydroxyl hydrogen silicone oil, dodecane, hexadecane, poly alpha olefin, toluene, isopropanol and dimethylformamide;
the polydimethylsiloxane is one or more of monoglycidyl ether end-capped polydimethylsiloxane, diglycidyl ether end-capped polydimethylsiloxane and trimethylsiloxane end-capped polydimethylsiloxane;
the epoxy resin is one or more of bisphenol A epoxy resin, bisphenol F epoxy resin, aliphatic glycidyl ether epoxy resin, glycidyl ester epoxy resin or glycidyl amine epoxy resin.
2. The method for preparing a super-lubricating coating based on a polydimethylsiloxane polymer molecular brush as recited in claim 1, wherein the curing agent in the first step is one of polyamide, ethylenediamine, polyetheramine and diethylenetriamine.
3. The method for preparing a super-lubricating coating based on a polydimethylsiloxane polymer molecular brush as defined in claim 1, wherein the organic solvent in the first step is one or more of ethyl acetate and ethanol; the organic solvent in the second step is one or more of acetone, toluene and xylene.
4. The method for preparing a super-lubricating coating based on a polydimethylsiloxane polymer molecular brush as set forth in claim 1, wherein the curing temperature in the third step is 120-130 ℃ and the curing time is 2-3 h.
5. The method for preparing the super-lubricating coating based on the polydimethylsiloxane polymer molecular brush according to claim 1, wherein the spraying pressure in the third step is 1500-1900 psi.
6. The method for preparing a super-lubricating coating based on a polydimethylsiloxane polymer molecular brush as recited in claim 1, wherein the standing environment after the liquid C is dropped in the third step is a ventilated dust-free environment.
7. A super-lubricious coating based on a polydimethylsiloxane polymer molecular brush prepared by the method of any one of claims 1-6.
CN202211283011.6A 2022-10-20 2022-10-20 Super-lubricating coating based on polydimethylsiloxane polymer molecular brush and preparation method thereof Active CN115521708B (en)

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