CN110028851A - A kind of solid lubrication barrier material with self-repair function - Google Patents
A kind of solid lubrication barrier material with self-repair function Download PDFInfo
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- CN110028851A CN110028851A CN201910305224.6A CN201910305224A CN110028851A CN 110028851 A CN110028851 A CN 110028851A CN 201910305224 A CN201910305224 A CN 201910305224A CN 110028851 A CN110028851 A CN 110028851A
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- 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
- C08G77/04—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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- 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
- 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
- C09D127/18—Homopolymers or copolymers of tetrafluoroethene
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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
- 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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- 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
- 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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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- 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 kind of preparation methods of lubrication protection coating with unique self-repair function, it is using polyamide-imide resin as adhesive, eight-polyhedral oligomeric silsesquioxane of sulphur (S8-POSS) is selfreparing and reinforcing function additive, polytetrafluoroethylene (PTFE) is lubricant, N, dinethylformamide is diluent, and ground dispersion is prepared.The present invention does not give only the excellent comprehensive performance of lubrication protection coating, and it is made to have unique self-repair function using the S8-POSS for containing reversible cystine linkage as reparation and reinforcing function additive.The performance test results, which show the material not only, has good adhesive force, shock resistance, flexibility, heat resistance, and has unique self-repair function, can effectively improve the friction and wear behavior of material, extends coating service life.
Description
Technical field
The present invention relates to a kind of lubrication protection coating material more particularly to a kind of solid lubrication with self-repair function
Barrier material belongs to intelligent lubricating protective coating technique field.
Background technique
Bonded solid lubricant coating, be it is a kind of disperse solid lubricant in resin system, then be similar to paint
Coating process is formed a film on friction member surface to reduce one kind of its friction and wearing properties special lubriation material and technology.
The convenience that this kind of material is used by it, thus it is very widely used, throughout the fields such as the aerospace of high-tech to daily life
Various aspects living.Since it belongs to sacrificial protection coating, how to prolong its service life always concerned by people
Focus.Under normal circumstances lubrication protection coating in use, in addition to wear can also be heated, the shadow of the factors such as mechanically and chemically
It rings, so that reduced service life and friction and wear behavior be caused to reduce.In order to extend the service life of coating, develop a series of
Technology, including by resin modified improve properties of coating and by Recompounded multielement functional stuffing improve coating friction mill
Damage performance etc..In recent years, as the appearance of selfreparing concept, self-healing polymers material are come into being, selfreparing concept is drawn
Enter lubrication protection coating and is undoubtedly an effective way for extending coating service life.The study found that the polymerization containing cystine linkage
Object can realize the self-repair function of material by carrying out reversible exchange reaction, and external intervene (such as heating or light having
According to etc.) in the case where, the progress of selfreparing can be further speeded up.
S8, the simple substance of element sulphur are the allotropes of sulphur, each S atom and other 2 S atom shapes in molecular crystal
At S-S singly-bound.The fracture of key occurs for S8 at high temperature, forms reversible dynamic disulfide bond, covalent bond is easily broken off and other
Sulphur atom carry out chemical bond recombination and between sulfydryl reacting realize self-healing properties.Polyhedral oligomeric silsesquioxane
Alkane (POSS) is a kind of novel organic/inorganic hybridization material with nanostructure occurred in recent years, since its is unique
The design feature of nanometer hybrid, molecule Modulatory character and hollow cage modle, can be on a molecular scale to polymer
It is modified, it realizes the inorganic and abundant hydridization of organic component, forms uniform heterogeneous material, modified polymer is made not only to remain height
The excellent processability of molecular material, toughness and low cost, while also there is inorganic material heat-resisting, oxidative resistance outstanding and excellent
Different mechanical property.S8 is grafted on POSS by inverse vulcanization reaction, the S8-POSS containing dynamic cystine linkage is introduced into profit
In sliding protective materials, properties of coating is not only increased, and introduce self-repair function, effectively increase the friction of material
Polishing machine extends coating service life.
Summary of the invention
The purpose of the present invention is to provide a kind of excellent solid lubrication barrier materials with self-repair function.
(1) with the lubrication protection coating material of self-repair function
1. selfreparing and the preparation of reinforcing function additive S8-POSS
Using diethylene glycol dimethyl ether as solvent, octavinyl-POSS and S8 are stirred with the molar ratio of 1:3 ~ 1:6 in 160 ~ 180 DEG C of xia
It mixes and evaporates 0.5 ~ 2h of back flow reaction and obtain.
Fig. 1 is the synthetic route that the present invention uses S8-POSS.As shown in Figure 1, eight ethylene POSS have with Si-O-Si
Key is the hollow cage structure of inorganic skeleton, and eight vinyl groups are connected on eight angles of structure can occur inverse sulphur with S8
Change reaction, obtain the S8-POSS with cystine linkage, which is 120 DEG C.
Fig. 2 is the thermogravimetric curve of S8-POSS.By the compound of S8 and POSS, the thermal stability of S8-POSS is significantly improved.
Fig. 3 is the DSC curve of S8-POSS, it can be seen from DSC curve POSS at 150 DEG C or less there is no phase transformation, and S8 due to
The presence of allotrope fusing point containing there are two, and after compound, the fusing point of S8-POSS is stablized at 120 DEG C, therefore in height
Heat treatment is carried out in 120 DEG C can be improved the selfreparing rate of coating.
2. the preparation of lubrication protection coating material
It is adhesive with polyamidoimide (PAI), eight-polyhedral oligomeric silsesquioxane of sulphur (S8-POSS) is modified reinforcement
And self-repair function filler, polytetrafluoroethylene (PTFE) are lubricant, N,N-Dimethylformamide (DMF) is diluent, through height
Speed is dispersed with stirring uniformly and obtains.
Above-mentioned each component is matched by following weight percent content: polyamidoimide (PAI) 5.0 ~ 12.0% gathers
Tetrafluoroethene (PTFE) 6.00 ~ 15.00%, eight-polyhedral oligomeric silsesquioxane of sulphur (S8-POSS) 4.0 ~ 9.0%, remaining content
For solvent N,N-dimethylformamide.
Wherein adhesive polyamidoimide (PAI) is commercial paraphernalia, and solid content is between 30 ± 3%；Lubricant is poly-
Granularity≤10 μm of tetrafluoroethene (PTFE), purity >=98%.The solid component content of the selfreparing slip coating of preparation is 25
±5%。
(2) preparation and performance test of the lubrication protection coating with self-repair function
1. the preparation of selfreparing lubricant coating
Configured coating is sprayed on piece surface under compressed air (oil-free) or compressed nitrogen with spray gun.Piece surface needs
The surface treatments such as preparatory oil removing, derusting, sandblasting, ultrasound.The part sprayed should place 1-3 h surface drying at room temperature, be put into
Solidification in convection oven.Condition of cure: 150 ± 5 DEG C, 1 h of constant temperature；It 280 ± 5 DEG C, 1 h of constant temperature, can be used after taking-up.
2. the performance indexes of selfreparing lubricant coating
2.1. appearance of coat: flat and smooth flawless.
2.2 adhesive force: it is tested by GB/T 9286: 0 grade.
2. 3 flexibilities: being tested by GB/T 1731: 1/mm.
2.4. it impact resistance: is tested by GB/T1732: 50cm.
2.5. tribological property: friction test carries out on CSM ball disk friction wear testing machine.Experiment condition: load is
10N, rate 10cm/s, steel ball radius 3mm, amplitude 2.5cm.Test result: μ=0.06 ~ 0.10, W=0.6 ~ 3.0 × 10-6 mm3/
Nm。
2.6. the self-healing properties test of coating
Fig. 4 is wear rate comparison before and after the selfreparing of S8-POSS modified coating.As shown in Figure 4, the polishing scratch of coating is passing through 200 DEG C
After lower heat preservation 3h heat treatment, the depth and width of polishing scratch have to be reduced to a certain degree, and wear rate reduces 65%.Therefore, the painting
After Overheating Treatment, the degree of wear of coating is substantially reduced layer, shows good self-healing properties.
In conclusion the present invention is using containing the S8-POSS of reversible cystine linkage as repairing and reinforcing function additive, no
It gives only the excellent comprehensive performance of lubrication protection coating: not only there is good adhesive force, shock resistance, flexibility, heat resistance,
And has unique self-repair function, the friction and wear behavior of material can be effectively improved, extend coating service life.
Detailed description of the invention
Fig. 1 is the synthetic route of S8-POSS.
Fig. 2 is the thermogravimetric curve of S8-POSS.
Fig. 3 is the DSC curve of S8-POSS.
Fig. 4 is wear rate comparison before and after the selfreparing of S8-POSS modified coating.
Specific embodiment
In order to better understand the present invention, the preparation and property below by specific embodiment to selfreparing lubrication protection coating
It can further illustrate.
Embodiment 1
80 g of PAI, PTFE 100g, S8-POSS 25g, solvent N,N-Dimethylformamide 800ml are weighed respectively.By original used
It is uniformly dispersed after material mixing through high-speed stirred, scattered slip coating is sprayed under compressed air (oil-free) or compressed nitrogen
Piece surface (piece surface needs the surface treatment such as preparatory oil removing, derusting, sandblasting, ultrasound).The part sprayed is first in room temperature
1 ~ 3 h surface drying of lower placement places into solidification in convection oven.Condition of cure: 150 ± 5 DEG C, 1 h of constant temperature；280 ± 5 DEG C, constant temperature 1
H can be used after taking-up.The main performance index of product is shown in Table 1.Show by 3h selfreparing experiment at friction and 200 DEG C
The modified coating coefficient of friction of S8-POSS is basically unchanged, and coating shows good self-repairability after Overheating Treatment
Can, the wear rate variation of heat treatment front and back polishing scratch is shown in Table 2.
Embodiment 2
90 g of PAI, PTFE 100g, S8-POSS 20g, solvent N,N-Dimethylformamide 750ml are weighed respectively.By original used
It is uniformly dispersed after material mixing through high-speed stirred, scattered slip coating is sprayed under compressed air (oil-free) or compressed nitrogen
Piece surface (piece surface needs the surface treatment such as preparatory oil removing, derusting, sandblasting, ultrasound).The part sprayed is first in room temperature
1 ~ 3 h surface drying of lower placement places into solidification in convection oven.Condition of cure: 150 ± 5 DEG C, 1 h of constant temperature；280 ± 5 DEG C, constant temperature 1
H can be used after taking-up.The main performance index of product is shown in Table 1.Show by 3h selfreparing experiment at friction and 200 DEG C
The modified coating coefficient of friction of S8-POSS is basically unchanged, and coating shows good self-repairability after Overheating Treatment
Can, the wear rate variation of heat treatment front and back polishing scratch is shown in Table 2.
Embodiment 3
90 g of PAI, PTFE 120g, S8-POSS 30g, solvent N,N-Dimethylformamide 700ml are weighed respectively.By original used
It is uniformly dispersed after material mixing through high-speed stirred, scattered slip coating is sprayed under compressed air (oil-free) or compressed nitrogen
Piece surface (piece surface needs the surface treatment such as preparatory oil removing, derusting, sandblasting, ultrasound).The part sprayed should be in room temperature
1 ~ 3 h surface drying of lower placement places into solidification in convection oven.Condition of cure: 150 ± 5 DEG C, 1 h of constant temperature；280 ± 5 DEG C, constant temperature 1
H can be used after taking-up.The main performance index of product is shown in Table 1.Show by 3h selfreparing experiment at friction and 200 DEG C
The modified coating coefficient of friction of S8-POSS is basically unchanged, and coating shows good self-repairability after Overheating Treatment
Can, the wear rate variation of heat treatment front and back polishing scratch is shown in Table 2.
Embodiment 4
90 g of PAI, PTFE 100g, S8-POSS 35g, solvent N,N-Dimethylformamide 800ml are weighed respectively.By original used
It is uniformly dispersed after material mixing through high-speed stirred, scattered slip coating is sprayed under compressed air (oil-free) or compressed nitrogen
Piece surface (piece surface needs the surface treatment such as preparatory oil removing, derusting, sandblasting, ultrasound).The part sprayed is first in room temperature
1 ~ 3 h surface drying of lower placement places into solidification in convection oven.Condition of cure: 150 ± 5 DEG C, 1 h of constant temperature；280 ± 5 DEG C, constant temperature 1
H can be used after taking-up.The main performance index of product is shown in Table 1.Show by 3h selfreparing experiment at friction and 200 DEG C
The modified coating coefficient of friction of S8-POSS is basically unchanged, and coating shows good self-repairability after Overheating Treatment
Can, the wear rate variation of heat treatment front and back polishing scratch is shown in Table 2.
Embodiment 5
80 g of PAI, PTFE 110g, S8-POSS 40g, solvent N,N-Dimethylformamide 850ml are weighed respectively.By original used
It is uniformly dispersed after material mixing through high-speed stirred, scattered slip coating is sprayed under compressed air (oil-free) or compressed nitrogen
Piece surface (piece surface needs the surface treatment such as preparatory oil removing, derusting, sandblasting, ultrasound).The part sprayed is first in room temperature
1 ~ 3 h surface drying of lower placement places into solidification in convection oven.Condition of cure: 150 ± 5 DEG C, 1 h of constant temperature；280 ± 5 DEG C, constant temperature 1
H can be used after taking-up.The main performance index of product is shown in Table 1.Show by 3h selfreparing experiment at friction and 200 DEG C
The modified coating coefficient of friction of S8-POSS is basically unchanged, and coating shows good self-repairability after Overheating Treatment
Can, the wear rate variation of heat treatment front and back polishing scratch is shown in Table 2.
Embodiment 6
80 g of PAI, PTFE 110g, S8-POSS 40g, solvent N,N-Dimethylformamide 750ml are weighed respectively.By original used
It is uniformly dispersed after material mixing through high-speed stirred, scattered slip coating is sprayed under compressed air (oil-free) or compressed nitrogen
Piece surface (piece surface needs the surface treatment such as preparatory oil removing, derusting, sandblasting, ultrasound).The part sprayed is first in room temperature
1 ~ 3 h surface drying of lower placement places into solidification in convection oven.Condition of cure: 150 ± 5 DEG C, 1 h of constant temperature；280 ± 5 DEG C, constant temperature 1
H can be used after taking-up.The main performance index of product is shown in Table 1.Show by 3h selfreparing experiment at friction and 200 DEG C
The modified coating coefficient of friction of S8-POSS is basically unchanged, and coating shows good self-repairability after Overheating Treatment
Can, the wear rate variation of heat treatment front and back polishing scratch is shown in Table 2.
Embodiment 7
100 g of PAI, PTFE 100g, S8-POSS 30g, solvent N,N-Dimethylformamide 900ml are weighed respectively.It will be used
It is uniformly dispersed after raw material mixing through high-speed stirred, scattered slip coating is sprayed under compressed air (oil-free) or compressed nitrogen
It is coated in piece surface (piece surface needs the surface treatment such as preparatory oil removing, derusting, sandblasting, ultrasound).The part sprayed is first in room
Temperature is lower to place 1 ~ 3 h surface drying, solidifies being put into convection oven.Condition of cure: 150 ± 5 DEG C, 1 h of constant temperature；It is 280 ± 5 DEG C, permanent
1 h of temperature can be used after taking-up.The main performance index of product is shown in Table 1.Table is tested by 3h selfreparing at friction and 200 DEG C
Bright, the modified coating coefficient of friction of S8-POSS is basically unchanged, and coating shows good selfreparing after Overheating Treatment
The wear rate variation of performance, heat treatment front and back polishing scratch is shown in Table 2.
In the various embodiments described above, the specific preparation process of S8-POSS: accurate to measure diethylene glycol dimethyl ether 50ml, Xiang Qi
Middle addition 25g (0.1mol) S8,12.66g (0.02mol) octavinyl-POSS, is heated to 160 DEG C, mechanical stirring is simultaneously evaporated back
Stream 0.5 ~ 2h of reaction, is grafted to S8 on POSS, to obtain S8-POSS.
Claims (5)
1. a kind of lubrication protection coating material with self-repair function is the sulphur eight-using polyamide-imide resin as adhesive
Polyhedral oligomeric silsesquioxane S8-POSS is selfreparing and reinforcing function additive, and polytetrafluoroethylene (PTFE) is lubricant, N, N- bis-
Methylformamide is diluent, is uniformly dispersed and obtains through high-speed stirred；
The selfreparing and the preparation of reinforcing function additive S8-POSS are eight vinyl using diethylene glycol dimethyl ether as solvent
POSS and S8 is with the molar ratio of 1:3 ~ 1:6, in 160 ~ 180 DEG C, stir and evaporate 0.5 ~ 2h of back flow reaction to get.
2. as described in claim 1 with the lubrication protection coating material of self-repair function, it is characterised in that: each component
It is matched by following weight percent: selfreparing and reinforcing function additive S8-POSS 4.0 ~ 9.0%, polyamidoimide
For 5.00 ~ 12.00%, polytetrafluoroethylene (PTFE) be 6.00 ~ 15.00%, remaining is solvent N,N-dimethylformamide.
3. as claimed in claim 1 or 2 with the lubrication protection coating material of self-repair function, it is characterised in that: adhesive is poly-
The solid content of amide imide resin is between 30 ± 3%.
4. as claimed in claim 1 or 2 with the lubrication protection coating material of self-repair function, it is characterised in that: lubricant is poly-
Granularity≤10 μm of tetrafluoroethene, purity >=98%.
5. as claimed in claim 1 or 2 with the lubrication protection coating material of self-repair function, it is characterised in that: solid lubrication
The solid component content of coating is 25 ± 5%.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110591554A (en) * | 2019-08-05 | 2019-12-20 | 广州中国科学院工业技术研究院 | Protective coating with self-repairing characteristic |
| CN114685996A (en) * | 2022-04-24 | 2022-07-01 | 华南理工大学 | Elastomer composite material and preparation method and application thereof |
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| HO-KENG LIN等: "Reactive Hybrid of Polyhedral Oligomeric Silsesquioxane (POSS) and Sulfur as a Building Block for Self-Healing Materials", 《MACROMOLECULAR RAPID COMMUNICATIONS》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110591554A (en) * | 2019-08-05 | 2019-12-20 | 广州中国科学院工业技术研究院 | Protective coating with self-repairing characteristic |
| CN114685996A (en) * | 2022-04-24 | 2022-07-01 | 华南理工大学 | Elastomer composite material and preparation method and application thereof |
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| CN110028851B (en) | 2021-05-28 |
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