CN110028851B - Solid lubrication protective coating material with self-repairing function - Google Patents
Solid lubrication protective coating material with self-repairing function Download PDFInfo
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- 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
- C08G77/04—Polysiloxanes
- C08G77/38—Polysiloxanes modified by chemical after-treatment
- C08G77/382—Polysiloxanes modified by chemical after-treatment containing atoms other than carbon, hydrogen, oxygen or silicon
- C08G77/392—Polysiloxanes modified by chemical after-treatment containing atoms other than carbon, hydrogen, oxygen or silicon containing sulfur
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- 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
- C09D127/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers
- C09D127/02—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment
- C09D127/12—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
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- 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
- C09D179/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen, with or without oxygen, or carbon only, not provided for in groups C09D161/00 - C09D177/00
- C09D179/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
- C09D179/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
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- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/18—Fireproof paints including high temperature resistant paints
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- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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Abstract
The invention discloses a preparation method of a lubricating protective coating with a unique self-repairing function, which is prepared by grinding and dispersing polyamide-imide resin as an adhesive, sulfur-octa-polyhedral oligomeric silsesquioxane (S8-POSS) as a self-repairing and reinforcing functional additive, polytetrafluoroethylene as a lubricant and N, N-dimethylformamide as a diluent. The invention utilizes the S8-POSS containing reversible disulfide bond as the repairing and reinforcing functional additive, thereby not only endowing the lubricating protective coating with excellent comprehensive performance, but also leading the lubricating protective coating to have unique self-repairing function. The performance test result shows that the material not only has good adhesive force, impact resistance, flexibility and heat resistance, but also has a unique self-repairing function, so that the frictional wear performance of the material can be effectively improved, and the service life of the coating is prolonged.
Description
Technical Field
The invention relates to a lubricating protective coating material, in particular to a solid lubricating protective coating material with a self-repairing function, and belongs to the technical field of intelligent lubricating protective coatings.
Background
The solid lubricating coating is a special lubricating material and technology which disperses solid lubricant in resin system and then forms film on the surface of friction part by coating process similar to paint to reduce its friction and wear performance. Due to the convenience of use, the material is widely applied and extends from the fields of high-technology aerospace and the like to various aspects of daily life. Because it is a sacrificial protective coating, it has been a focus of attention on how to extend its useful life. In general, the lubricating protective coating is affected by factors such as heat, machinery and chemistry besides abrasion in the using process, so that the service life is shortened and the frictional wear performance is reduced. In order to prolong the service life of the coating, a series of technologies are developed, including improving the comprehensive performance of the coating through resin modification, improving the frictional wear performance of the coating through multi-component functional filler, and the like. In recent years, with the emergence of self-repairing concepts, self-repairing polymer materials are produced, and the introduction of the self-repairing concept into a lubricating protective coating is undoubtedly an effective way for prolonging the service life of the coating. Researches show that the polymer containing disulfide bonds can realize the self-repairing function of the material by performing reversible exchange reaction, and can further accelerate the self-repairing in the presence of external intervention (such as heating, illumination and the like).
S8, the simple substance of sulfur element is an allotrope of sulfur, and each S atom in the molecular crystal forms an S-S single bond with the other 2S atoms. And S8 is subjected to bond breakage at high temperature to form a reversible dynamic disulfide bond, and the covalent bond is easily broken to perform chemical bond recombination with other sulfur atoms and react with sulfydryl to realize self-repairing performance. Polyhedral oligomeric silsesquioxane (POSS) is a novel organic/inorganic hybrid material with a nano structure in recent years, and due to the unique nano organic/inorganic hybrid, molecular controllability and hollow cage-shaped structural characteristics, the polyhedral oligomeric silsesquioxane (POSS) can modify a polymer at a molecular level, realize full hybridization of inorganic and organic components, form a uniform multi-phase material, ensure that the modified polymer not only maintains the excellent processability, toughness and low cost of a high-molecular material, but also has the outstanding heat resistance, oxidation resistance and excellent mechanical properties of the inorganic material. S8 is grafted to POSS through inverse vulcanization reaction, and S8-POSS containing dynamic disulfide bonds is introduced into the lubricating protective material, so that the comprehensive performance of the coating is improved, the self-repairing function is introduced, the frictional wear performance of the material is effectively improved, and the service life of the coating is prolonged.
Disclosure of Invention
The invention aims to provide a solid lubrication protective coating material with an excellent self-repairing function.
Lubricating protective coating material with self-repairing function
1. Preparation of self-repairing and reinforcing functional additive S8-POSS
The catalyst is prepared by stirring octavinyl POSS and S8 at a molar ratio of 1: 3-1: 6 at 160-180 ℃ of xia by using diethylene glycol dimethyl ether as a solvent and carrying out evaporation reflux reaction for 0.5-2 h.
FIG. 1 is a synthetic route using S8-POSS according to the present invention. As shown in figure 1, octaethylene POSS has a hollow cage structure with Si-O-Si bond as inorganic framework, eight vinyl groups are connected to eight corners of the structure and can perform inverse vulcanization reaction with S8 to obtain S8-POSS with disulfide bond, and the melting point of the product is 120 ℃.
FIG. 2 is a thermogravimetric plot of S8-POSS. Through the compounding of S8 and POSS, the thermal stability of S8-POSS is obviously improved. FIG. 3 is a DSC curve of S8-POSS, from which it can be seen that POSS has no phase change below 150 ℃, while S8 has two melting points due to the presence of allotropes, and after recombination, the melting point of S8-POSS is stabilized at 120 ℃, so that heat treatment at above 120 ℃ can improve the self-healing rate of the coating.
2. Preparation of lubricating protective coating material
The composite material is prepared by taking polyamide-imide (PAI) as an adhesive, sulfur-octa-polyhedral oligomeric silsesquioxane (S8-POSS) as a modified reinforcing and self-repairing functional filler, Polytetrafluoroethylene (PTFE) as a lubricant and nitrogen-nitrogen Dimethylformamide (DMF) as a diluent through high-speed stirring and uniform dispersion.
The components are mixed according to the following weight percentage: 5.0-12.0% of polyamide imide (PAI), 6.00-15.00% of Polytetrafluoroethylene (PTFE), 4.0-9.0% of sulfur octa-polyhedral oligomeric silsesquioxane (S8-POSS) and the balance of solvent N, N-dimethylformamide.
Wherein the adhesive polyamide imide (PAI) is a commercial product, and the solid content of the adhesive polyamide imide (PAI) is 30 +/-3%; the granularity of the lubricant Polytetrafluoroethylene (PTFE) is less than or equal to 10 mu m, and the purity is more than or equal to 98 percent. The solid component content of the prepared self-repairing lubricating coating is 25 +/-5%.
(II) preparation and performance test of lubricating protective coating with self-repairing function
1. Preparation of self-repairing lubricating coating
The prepared coating is sprayed on the surface of the part by a spray gun under the condition of compressed air (oil-free) or compressed nitrogen. The surface of the part needs to be subjected to surface treatment such as oil removal, rust removal, sand blasting, ultrasound and the like in advance. And (3) placing the sprayed part at room temperature for 1-3 h, drying the part on the surface, and curing the part in a blast oven. Curing conditions are as follows: keeping the temperature at 150 +/-5 ℃ for 1 h; keeping the temperature at 280 plus or minus 5 ℃ for 1 hour, and taking out for use.
2. Various performance indexes of self-repairing lubricating coating
2.1. Appearance of the coating: smooth and crackless.
2.2 adhesion: testing according to GB/T9286: and (4) level 0.
2.3 flexibility: testing according to GB/T1731: 1/mm.
2.4. Impact resistance: testing according to GB/T1732: 50 cm.
2.5. The tribological performance is as follows: the friction test was performed on a CSM ball-and-disc friction wear tester. The experimental conditions are as follows: the load is 10N, the speed is 10cm/s, the radius of the steel ball is 3mm, and the amplitude is 2.5 cm. And (3) testing results: mu = 0.06-0.10, W = 0.6-3.0 x 10-6 mm3/Nm。
2.6. Self-repair performance test of coating
FIG. 4 is a comparison of wear rates before and after self-healing of S8-POSS modified coatings. As can be seen from FIG. 4, after the wear scar of the coating is subjected to heat treatment at 200 ℃ for 3h, the depth and the width of the wear scar are reduced to a certain extent, and the wear rate is reduced by 65%. Therefore, after the coating is subjected to heat treatment, the abrasion degree of the coating is obviously reduced, and good self-repairing performance is shown.
In conclusion, the invention utilizes the S8-POSS containing the reversible disulfide bond as the repairing and reinforcing functional additive, thereby not only endowing the lubricating protective coating with excellent comprehensive performance: the coating has good adhesive force, impact resistance, flexibility and heat resistance, has a unique self-repairing function, can effectively improve the frictional wear performance of the material, and prolongs the service life of the coating.
Drawings
FIG. 1 is a synthetic route for S8-POSS.
FIG. 2 is a thermogravimetric plot of S8-POSS.
FIG. 3 is a DSC curve of S8-POSS.
FIG. 4 is a comparison of wear rates before and after self-healing of S8-POSS modified coatings.
Detailed Description
In order to better understand the present invention, the preparation and performance of the self-healing lubricious protective coating is further illustrated by the following specific examples.
Example 1
80 g of PAI, 100g of PTFE, 25g of S8-POSS and 800ml of dimethylformamide as a solvent nitrogen were weighed out respectively. The raw materials are mixed and uniformly dispersed by high-speed stirring, and the dispersed lubricating coating is sprayed on the surface of a part (the surface of the part needs surface treatment such as oil removal, rust removal, sand blasting, ultrasonic treatment and the like in advance) under compressed air (oil-free) or compressed nitrogen. And (3) placing the sprayed part at room temperature for 1-3 h, drying the part, and then placing the part into a blast oven for curing. Curing conditions are as follows: keeping the temperature at 150 +/-5 ℃ for 1 h; keeping the temperature at 280 plus or minus 5 ℃ for 1 hour, and taking out for use. The main performance indexes of the product are shown in table 1. Friction and a self-repairing experiment at 200 ℃ for 3h show that the friction coefficient of the coating modified by S8-POSS is basically unchanged, the coating after heat treatment shows good self-repairing performance, and the change of the wear rate of the wear scar before and after heat treatment is shown in Table 2.
Example 2
PAI 90 g, PTFE 100g, S8-POSS 20g and dimethylformamide as solvent (nitrogen and nitrogen) 750ml were weighed out separately. The raw materials are mixed and uniformly dispersed by high-speed stirring, and the dispersed lubricating coating is sprayed on the surface of a part (the surface of the part needs surface treatment such as oil removal, rust removal, sand blasting, ultrasonic treatment and the like in advance) under compressed air (oil-free) or compressed nitrogen. And (3) placing the sprayed part at room temperature for 1-3 h, drying the part, and then placing the part into a blast oven for curing. Curing conditions are as follows: keeping the temperature at 150 +/-5 ℃ for 1 h; keeping the temperature at 280 plus or minus 5 ℃ for 1 hour, and taking out for use. The main performance indexes of the product are shown in table 1. Friction and a self-repairing experiment at 200 ℃ for 3h show that the friction coefficient of the coating modified by S8-POSS is basically unchanged, the coating after heat treatment shows good self-repairing performance, and the change of the wear rate of the wear scar before and after heat treatment is shown in Table 2.
Example 3
PAI 90 g, PTFE 120g, S8-POSS 30g and dimethylformamide as solvent nitrogen 700ml were weighed out separately. The raw materials are mixed and uniformly dispersed by high-speed stirring, and the dispersed lubricating coating is sprayed on the surface of a part (the surface of the part needs surface treatment such as oil removal, rust removal, sand blasting, ultrasonic treatment and the like in advance) under compressed air (oil-free) or compressed nitrogen. And (3) placing the sprayed part at room temperature for 1-3 h, drying the part, and then placing the part into a blast oven for curing. Curing conditions are as follows: keeping the temperature at 150 +/-5 ℃ for 1 h; keeping the temperature at 280 plus or minus 5 ℃ for 1 hour, and taking out for use. The main performance indexes of the product are shown in table 1. Friction and a self-repairing experiment at 200 ℃ for 3h show that the friction coefficient of the coating modified by S8-POSS is basically unchanged, the coating after heat treatment shows good self-repairing performance, and the change of the wear rate of the wear scar before and after heat treatment is shown in Table 2.
Example 4
90 g of PAI, 100g of PTFE, 35g of S8-POSS and 800ml of dimethylformamide as a solvent nitrogen are weighed respectively. The raw materials are mixed and uniformly dispersed by high-speed stirring, and the dispersed lubricating coating is sprayed on the surface of a part (the surface of the part needs surface treatment such as oil removal, rust removal, sand blasting, ultrasonic treatment and the like in advance) under compressed air (oil-free) or compressed nitrogen. And (3) placing the sprayed part at room temperature for 1-3 h, drying the part, and then placing the part into a blast oven for curing. Curing conditions are as follows: keeping the temperature at 150 +/-5 ℃ for 1 h; keeping the temperature at 280 plus or minus 5 ℃ for 1 hour, and taking out for use. The main performance indexes of the product are shown in table 1. Friction and a self-repairing experiment at 200 ℃ for 3h show that the friction coefficient of the coating modified by S8-POSS is basically unchanged, the coating after heat treatment shows good self-repairing performance, and the change of the wear rate of the wear scar before and after heat treatment is shown in Table 2.
Example 5
80 g of PAI, 110g of PTFE, 40g of S8-POSS and 850ml of dimethylformamide as a solvent nitrogen were weighed out respectively. The raw materials are mixed and uniformly dispersed by high-speed stirring, and the dispersed lubricating coating is sprayed on the surface of a part (the surface of the part needs surface treatment such as oil removal, rust removal, sand blasting, ultrasonic treatment and the like in advance) under compressed air (oil-free) or compressed nitrogen. And (3) placing the sprayed part at room temperature for 1-3 h, drying the part, and then placing the part into a blast oven for curing. Curing conditions are as follows: keeping the temperature at 150 +/-5 ℃ for 1 h; keeping the temperature at 280 plus or minus 5 ℃ for 1 hour, and taking out for use. The main performance indexes of the product are shown in table 1. Friction and a self-repairing experiment at 200 ℃ for 3h show that the friction coefficient of the coating modified by S8-POSS is basically unchanged, the coating after heat treatment shows good self-repairing performance, and the change of the wear rate of the wear scar before and after heat treatment is shown in Table 2.
Example 6
80 g of PAI, 110g of PTFE, 40g of S8-POSS and 750ml of dimethylformamide as a solvent nitrogen are weighed respectively. The raw materials are mixed and uniformly dispersed by high-speed stirring, and the dispersed lubricating coating is sprayed on the surface of a part (the surface of the part needs surface treatment such as oil removal, rust removal, sand blasting, ultrasonic treatment and the like in advance) under compressed air (oil-free) or compressed nitrogen. And (3) placing the sprayed part at room temperature for 1-3 h, drying the part, and then placing the part into a blast oven for curing. Curing conditions are as follows: keeping the temperature at 150 +/-5 ℃ for 1 h; keeping the temperature at 280 plus or minus 5 ℃ for 1 hour, and taking out for use. The main performance indexes of the product are shown in table 1. Friction and a self-repairing experiment at 200 ℃ for 3h show that the friction coefficient of the coating modified by S8-POSS is basically unchanged, the coating after heat treatment shows good self-repairing performance, and the change of the wear rate of the wear scar before and after heat treatment is shown in Table 2.
Example 7
100g of PAI, 100g of PTFE, 30g of S8-POSS and 900ml of dimethylformamide as a solvent nitrogen were weighed out, respectively. The raw materials are mixed and uniformly dispersed by high-speed stirring, and the dispersed lubricating coating is sprayed on the surface of a part (the surface of the part needs surface treatment such as oil removal, rust removal, sand blasting, ultrasonic treatment and the like in advance) under compressed air (oil-free) or compressed nitrogen. And (3) placing the sprayed part at room temperature for 1-3 h, drying the part, and curing the part in a blast oven. Curing conditions are as follows: keeping the temperature at 150 +/-5 ℃ for 1 h; keeping the temperature at 280 plus or minus 5 ℃ for 1 hour, and taking out for use. The main performance indexes of the product are shown in table 1. Friction and a self-repairing experiment at 200 ℃ for 3h show that the friction coefficient of the coating modified by S8-POSS is basically unchanged, the coating after heat treatment shows good self-repairing performance, and the change of the wear rate of the wear scar before and after heat treatment is shown in Table 2.
In the above examples, the specific preparation process of S8-POSS was as follows: 50ml of diethylene glycol dimethyl ether is accurately measured, 25g (0.1mol) of S8 and 12.66g (0.02mol) of octavinyl POSS are added into the diethylene glycol dimethyl ether, the mixture is heated to 160 ℃, the mixture is mechanically stirred and is subjected to evaporation reflux reaction for 0.5-2 h, and S8 is grafted onto the POSS, so that S8-POSS is obtained.
Claims (4)
1. A lubricating protective coating material with a self-repairing function is prepared by taking polyamide-imide resin as an adhesive, taking sulfur-octa-polyhedral oligomeric silsesquioxane S8-POSS as a self-repairing and reinforcing functional additive, taking polytetrafluoroethylene as a lubricant and taking N, N-dimethylformamide as a diluent through high-speed stirring and uniform dispersion; the method is characterized in that: the preparation method of the self-repairing and reinforcing functional additive S8-POSS comprises the steps of taking diethylene glycol dimethyl ether as a solvent, stirring and carrying out an evaporation reflux reaction for 0.5-2 hours at 160-180 ℃ by using octavinyl POSS and S8 in a molar ratio of 1: 3-1: 6 to obtain the self-repairing and reinforcing functional additive S8-POSS;
the lubricating protective coating material comprises the following components in percentage by weight: the self-repairing and reinforcing functional additive S8-POSS is 4.0-9.0%, the polyamide-imide resin is 5.00-12.00%, the polytetrafluoroethylene is 6.00-15.00%, and the balance is diluent N, N-dimethylformamide.
2. The lubricant protective coating material of claim 1, wherein: the solid content of the adhesive polyamide-imide resin is 30 +/-3%.
3. The lubricant protective coating material of claim 1 or 2, wherein: the granularity of the lubricant polytetrafluoroethylene is less than or equal to 10 mu m, and the purity of the lubricant polytetrafluoroethylene is more than or equal to 98 percent.
4. The lubricant protective coating material of claim 1 or 2, wherein: the solid component content of the lubricating protective coating material is 25 +/-5%.
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