CN107057353A - A kind of porous PPS films and preparation method thereof - Google Patents
A kind of porous PPS films and preparation method thereof Download PDFInfo
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- CN107057353A CN107057353A CN201710034298.1A CN201710034298A CN107057353A CN 107057353 A CN107057353 A CN 107057353A CN 201710034298 A CN201710034298 A CN 201710034298A CN 107057353 A CN107057353 A CN 107057353A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/28—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by elimination of a liquid phase from a macromolecular composition or article, e.g. drying of coagulum
- C08J9/286—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by elimination of a liquid phase from a macromolecular composition or article, e.g. drying of coagulum the liquid phase being a solvent for the monomers but not for the resulting macromolecular composition, i.e. macroporous or macroreticular polymers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/30—Sulfur-, selenium- or tellurium-containing compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2381/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing sulfur with or without nitrogen, oxygen, or carbon only; Polysulfones; Derivatives of such polymers
- C08J2381/02—Polythioethers; Polythioether-ethers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/30—Sulfur-, selenium- or tellurium-containing compounds
- C08K2003/3009—Sulfides
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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
- C08L2203/00—Applications
- C08L2203/16—Applications used for films
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- Chemical & Material Sciences (AREA)
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- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
Abstract
The present invention relates to a kind of porous PPS films and preparation method thereof, it is characterized in that polyphenylene sulfide of the porous PPS films using percentage by weight as 70~80%, percentage by weight is 15~25% molybdenum disulfide, the silica that percentage by weight is 2~15% is raw material, it is molded using spraying process, handles and be prepared from through immersion oil.Porous PPS films material porosity prepared by the present invention is more than 15%, aperture is 1~10 μm, temperature in use scope is 50~260 DEG C, and coefficient of friction is 0.05~0.09, with pore size is uniform, temperature in use scope is wide, intensity is high, wear-resisting and excellent greasy property the characteristics of.
Description
Technical field
The present invention relates to a kind of thin-film material and preparation method thereof, and in particular to belongs to a kind of porous film material and its system
Preparation Method.
Background technology
Polyphenylene sulfide (PPS) full name is polyphenylene thioether, is the thermoplastic resin with thiophenyl in molecular backbone.PPS
Macromolecular chain is connected by the phenyl ring of rigid structure with flexible thioether bond, and it has crystallinity high, hard and crisp, fire retardant, thermally-stabilised
Good, resistant to chemical etching, the hot and humid lower dimensionally stable of property, excellent electrical properties, high abrasion resistance and melt fluidity are excellent etc. excellent
Point.In addition, it also has, molding shrinkage is small (about 0.08%), and water absorption rate is low (about 0.02%), and it is excellent that the tired property of vibration resistance is good etc.
Point.Heat endurance, PPS is one of best kind of heat endurance in engineering plastics, and its heat distortion temperature is generally higher than 260 degree；
Chemical resistance, PPS resin resistance to chemical corrosion can compare favourably with being known as the polytetrafluoroethylene (PTFE) of " kings of plastics ", 200
Below DEG C, almost no solvent can dissolve it；Dimensional stability, PPS injection-molded items have good creep resistance, line expansion
Coefficient is low, and dimensional stability is very good；Electrical property, PPS have very low dielectric constant, electric inductivity and dielectric loss because
Element, has excellent insulating properties and dielectric property etc. under the environment such as high temperature, high humidity；Adhesive property, PPS is to glass, aluminium, stainless
Steel etc. has very high adhesive strength, and the adhesive strength to glass is even greater than the cohesive force of glass, due to good resistance to
Corrosivity and adhesive property, extremely preferably make the lining of chemical industry equipment；In addition, PPS itself chemical constitution makes it have good difficulty
Combustibility, without adding fire retardant.Because PPS has an impayable combination property, thus Aero-Space, nuclear industry,
It is electric to wait the traditional industry such as high-technology field and machinery, automobile, household electrical appliance, office automation field to obtain extensively
Using.
Combination property excellent PPS is widely used it.PPS films on the market mainly have blowing at present
Film, calendered film and biaxial stretching film, it is hard and crisp because PPS crystallization rates are fast, so thin during using blow moulding production
Film is easily broken so that the PPS films of preparation have many defects；And rolling process is to extrude PPS resin by extruder,
Roller is sent to, then certain thickness PPS films are produced by controlling the gap between roller, through rolling legal system
The surface flatness and roller of the film obtained have direct relation.Although PPS films on the market have less friction system at present
Number is 0.25~0.43, but the lubriation material under the conditions of still cannot function as oil-free is used.
The content of the invention
It is a kind of with the porous PPS films material that coefficient of friction is low, greasy property is excellent, this hair in order to prepare
Bright to add molybdenum disulfide and silica thereto using polyphenylene sulfide as matrix material, wherein molybdenum disulfide coefficient of friction is low, can
Used as kollag, silica microstructural is spherical, is added into as additive in high polymer, can improve high polymer
Anti-wear performance and greasy property.
It is an object of the invention to provide a kind of porous PPS films, its concrete scheme is as follows：
A kind of porous PPS films, the film includes matrix material and filler, and described matrix material is polyphenylene sulfide
Ether, the filler is silica and molybdenum disulfide.
A kind of porous PPS films as described above, it is preferable that the percentage by weight of the polyphenylene sulfide is 70~
80%, the percentage by weight of the molybdenum disulfide is 15~25%.
A kind of porous PPS films as described above, it is preferable that the percentage by weight of the silica is 2~
15%, the particle diameter of the polyphenylene sulfide is 20~100 μm, and the particle diameter of the molybdenum disulfide is 1~200 μm, the silica
Particle diameter be 20~100nm.
A kind of porous PPS films as described above, it is preferable that described surface-modified dose of processing of silica.
A kind of porous PPS films as described above, it is preferable that the surface modifier be N- β-aminoethyl-γ-
Aminopropyl trimethoxysilane, the porous PPS films are molded using spraying process.
It is a further object to provide a kind of preparation method of porous PPS films, comprise the following steps：
(1) percentage by weight is weighed for 70~80% polyphenylene sulfides, weigh that percetage by weight is 15~25% two
Molybdenum sulfide, weighs the silica that weight fraction is 2~15%, mixing；
(2) mixed material is dispersed in easy volatile solvent of the boiling point less than 100 DEG C, stock dispersion liquid is made；
(3) obtained stock dispersion liquid is sprayed on ground, the air pressure of spraying process is 0~0.5MPa；
(4) material for obtaining step (3) is sintered, and obtains porous PPS films intermediate；
(5) porous PPS films intermediate is placed in progress immersion oil processing in fluid.
A kind of preparation method of porous PPS films as described above, it is preferable that step (2) described solvent is anhydrous
Ethanol, dispersion liquid is added to the proportional arrangement in 100~300mL absolute ethyl alcohols according to 100g raw materials.
A kind of preparation method of porous PPS films as described above, it is preferable that the sintering process in step (4)
For：By room temperature to 300~400 DEG C, and 10~60min is incubated at 300~400 DEG C, freely cools after terminating, enter one
Step, the more excellent condition of sintering process is：By room temperature to 350~365 DEG C, and 10~30min is incubated at 350~365 DEG C,
Freely cool after terminating.
A kind of preparation method of porous PPS films as described above, it is preferable that the immersion oil processing bar in step (5)
Part is that temperature is 60~100 DEG C, and vacuum is 0.05~0.09MPa, and the immersion oil time is 20~100h.
A kind of porous PPS films material that the present invention is provided is using polyphenylene sulfide, molybdenum disulfide and silica as original
Material, is molded using spraying method, is handled and is prepared from through immersion oil, and the porous PPS films aperture is 1~10 μm, hole
Rate is more than 15%, and coefficient of friction is 0.05~0.09, and density is 0.8~1.5g/cm3, temperature in use scope is -50~260 DEG C,
It is excellent with high intensity, high abrasion, greasy property, the wide advantage of temperature in use scope.
Embodiment
To make the object, technical solutions and advantages of the present invention clearer, technical scheme will be carried out below
Detailed description.Obviously, described embodiment is only a part of embodiment of the invention, rather than whole embodiments.Base
Embodiment in the present invention, those of ordinary skill in the art are resulting on the premise of creative work is not made to be owned
Other embodiment, belongs to the scope that the present invention is protected.
The present invention is further illustrated below by embodiment.In the examples below, this hair is determined according to GB10006-88
The coefficient of friction of the film of bright offer, coefficient of friction represents the greasy property of material, and this numerical value is lower, illustrates that greasy property is got over
It is good；The porosity for the porous membrane that the present invention is provided is determined using weight method, porosity (%) represents the pore-forming performance of material, this
One numerical value is bigger, and explanation pore-forming is more；Using the aperture of electronic scanner microscope direct measurement porous membrane, aperture (μm) is represented
The size in the hole of porous material；The density for the porous PPS films that the present invention is provided is measured using density tester, it is close
Spend (g/cm2) there is conclusive influence to many physical and mechanical properties of perforated membrane.
Embodiment 1
A kind of porous PPS films, preparation process is as follows：Weigh the polyphenylene sulfide resin cosmetics that particle diameter is 20~100 μm
Last 70g, particle diameter is 50 ± 10 μm of molybdenum disulfide 25g, and particle diameter is 30 ± 5nm silica 5g, in stirred type mixer
Mixing, the powder mixed is added in 200mL absolute ethyl alcohols, and 10min is disperseed in ultrasonic wave separating apparatus, air gun is used
Dispersion liquid is sprayed on the copperplate ground of surfacing, sintering in sintering furnace is then placed in and obtains porous PPS films
Intermediate, sintering process is：By room temperature to 350 DEG C, and 30min is incubated at 350 DEG C, freely cooled after terminating.Most
The porous PPS films intermediate prepared is placed in fluid afterwards, then one is placed in vacuum drying chamber, wherein very
Empty drying box temperature is 60 DEG C, and vacuum is 0.06MPa, immersion oil 72h.
Embodiment 2
A kind of porous PPS films, preparation process is as follows：First, nano silicon is carried out using wet-process modified
Surface modification treatment, detailed process is as follows：Weighing the nano silicon that 10g particle diameters are 30 ± 5nm, to be added to 200mL toluene molten
In liquid, ultrasonic disperse 30min is made suspension, weighs 0.526gN- β-aminoethyl-γ-aminopropyltrimethoxysilane and add
Enter into suspension, ultrasonic mixing 10min, by mixed liquor in 90 DEG C of heated at constant temperature 6h, then under conditions of 10000r/min
Sediment is centrifuged to obtain, is washed sediment 3 times with absolute ethyl alcohol, dries, that is, obtains modified manometer silicon dioxide.Secondly, weigh
Particle diameter is 20~100 μm of polyphenylene sulfide powder 80g, and particle diameter is 50 ± 10 μm of molybdenum disulfide 15g, modified nano-silica
SiClx 5g, is mixed in stirred type mixer.The powder mixed is added into 200mL absolute ethyl alcohols, in ultrasonic wave separating apparatus
Dispersion liquid, is sprayed on the copperplate ground of surfacing by scattered 20min using air gun, is then placed in sintering furnace and is burnt
Knot, obtains the intermediate of porous PPS films, sintering process is：By room temperature to 355 DEG C, and in 355 DEG C of insulations
20min, freely cools after terminating.The porous PPS films intermediate prepared is placed in fluid, then in the lump
It is placed in vacuum drying chamber, wherein vacuum drying chamber temperature is 80 DEG C, vacuum 0.08MPa, immersion oil 48h.
Embodiment 3
A kind of porous PPS films material, preparation process is as follows：Weigh the polyphenylene sulfide resin that particle diameter is 20~100 μm
Cosmetics end 70g, particle diameter is 50 ± 10 μm of molybdenum disulfide 18g, and modified manometer silicon dioxide 12g be (modified manometer silicon dioxide
Method is same as Example 2), mixed in stirred type mixer.The powder mixed is added into 150mL absolute ethyl alcohols, super
Disperse 20min in sound wave separating apparatus, dispersion liquid is sprayed on the copperplate ground of surfacing using air gun, is then placed in
Sintered in sintering furnace, obtain the intermediate of porous PPS films, sintering process is：By room temperature to 360 DEG C, and
360 DEG C of insulation 15min, freely cool after terminating.The porous PPS films intermediate prepared is placed in fluid,
Then one it is placed in vacuum drying chamber, wherein vacuum drying chamber temperature is 100 DEG C, vacuum 0.07MPa, immersion oil 24h.
Embodiment 4
A kind of porous PPS films material, preparation process is as follows：Weigh the polyphenylene sulfide resin that particle diameter is 20~100 μm
Cosmetics end 75g, particle diameter is 50 ± 10 μm of molybdenum disulfide 20g, the modified manometer silicon dioxide 5g (sides of modified manometer silicon dioxide
Method is same as Example 2), mixed in stirred type mixer.The powder mixed is added into 200mL absolute ethyl alcohols, in ultrasound
Disperse 20min in ripple separating apparatus, dispersion liquid is sprayed on the copperplate ground of surfacing using air gun, burning is then placed in
Sintered in freezing of a furnace, obtain porous polyphenylene sulfide intermediate, sintering process is：By room temperature to 365 DEG C, and in 365 DEG C of insulations
10min, freely cools after terminating.The porous PPS films intermediate prepared is placed in fluid, then in the lump
It is placed in vacuum drying chamber, wherein vacuum drying chamber temperature is 90 DEG C, vacuum 0.09MPa, immersion oil 24h.
Comparative example 1
The polyphenylene sulfide powder 100g that particle diameter is 20~100 μm is weighed, the mould of surfacing is placed in, in 30MPa
Pressure under be cold-pressed, then sintering obtain porous PPS films, sintering process is：By room temperature to 365 DEG C, and
365 DEG C of insulation 10min, freely cool after terminating.
The porous PPS films data of table 1
| Each film performance | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Comparative example 1 |
| Coefficient of friction | 0.07 | 0.06 | 0.07 | 0.05 | 0.25 |
| Porosity (%) | 17 | 18 | 17 | 16 | 2.7 |
| Aperture (μm) | 1-15 | 1-10 | 1-10 | 1-10 | 3-20 |
| Density (g/cm2) | 1.38 | 1.35 | 1.38 | 1.37 | 1.5 |
Embodiment 2,3 and 4 is can be seen that from the data of above-mentioned table 1 more to concentrate than the pore-size distribution of embodiment 1, it is grand
Explanation is disperseed more uniform in the film by modified silica in sight；The coefficient of friction data explanation of above-mentioned table 1, with poly-
Diphenyl sulfide, molybdenum disulfide, nano silicon oxide are raw material, the porous PPS films material friction system prepared using above method
Number is less than 0.1, far below the coefficient of friction 0.25 of PPS films in comparative example 1, and it is porous poly- that this explanation present invention is provided
Diphenyl sulfide film has good greasy property.The porous PPS films that the present invention is provided are compared with comparative example, one-tenth porosity
Height, pore-size distribution is concentrated.The density for the embodiment film that the present invention is provided is small compared with comparative example, is also demonstrated from side and utilizes this hair
The pore-forming performance of the porous PPS films of raw material and the preparation method shaping of bright offer is better than utilizing commonsense method shaping
Porous PPS films.The porosity of embodiment film is more than 15% in above-mentioned table 1, and aperture is at 1-10 μm, due to porous
PPS films porosity is moderate, and aperture is larger, during immersion oil processing, can be deposited in the hole of porous polyphenylene sulfide
The fluid of a part is stored up, so as to improve the greasy property of porous PPS films.
The foregoing is only a specific embodiment of the invention, but protection scope of the present invention is not limited thereto, any
Those familiar with the art the invention discloses technical scope in, change or replacement can be readily occurred in, should all be contained
Cover within protection scope of the present invention.Therefore, protection scope of the present invention should be based on the protection scope of the described claims.
Claims (10)
1. a kind of porous PPS films, it is characterised in that：The film includes matrix material and filler, described matrix material
For polyphenylene sulfide, the filler is silica and molybdenum disulfide.
2. porous PPS films according to claim 1, it is characterised in that：The percentage by weight of the polyphenylene sulfide
For 70~80%, the percentage by weight of the molybdenum disulfide is 15~25%, the percentage by weight of the silica for 2~
15%.
3. porous PPS films according to claim 1, it is characterised in that：The particle diameter of the polyphenylene sulfide be 20~
100 μm, the particle diameter of the molybdenum disulfide is 1~200 μm, and the particle diameter of the silica is 20~100nm.
4. the porous PPS films according to one of claim 1-3, it is characterised in that：The silica is through surface
Modifier treatment.
5. porous polyphenylene sulfide according to claim 4, it is characterised in that：The surface modifier is N- β-aminoethyls-
γ-aminopropyltrimethoxysilane.
6. porous PPS films according to claim 1, it is characterised in that：The porous PPS films are used
Spraying process is molded.
7. prepare the method for the porous PPS films described in one of claim 1-6, it is characterised in that：Including following step
Suddenly：
(1) polyphenylene sulfide, molybdenum disulfide and silica are mixed, obtains mixed material；
(2) mixed material is dispersed in easy volatile solvent of the boiling point less than 100 DEG C, dispersion liquid is made；
(3) dispersion liquid is sprayed on ground；
(4) material for obtaining step (3) is sintered, and obtains porous PPS films intermediate；
(5) porous PPS films intermediate is placed in fluid, immersion oil, obtains a kind of porous PPS films.
8. method according to claim 7, it is characterised in that：Sintering process in step (4) is：By room temperature extremely
300~400 DEG C, and 10~60min is incubated at 300~400 DEG C, freely cool after terminating.
9. method according to claim 8, it is characterised in that：Sintering process in step (4) is：By room temperature extremely
350~365 DEG C, and 10~30min is incubated at 350~365 DEG C, freely cool after terminating.
10. method according to claim 7, it is characterised in that：Carried out in step (5) in vacuum drying chamber at immersion oil
Reason, temperature is 60~100 DEG C, 0.05~0.09MPa of vacuum, 20~100h of immersion oil.
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| CN201710034298.1A CN107057353A (en) | 2017-01-18 | 2017-01-18 | A kind of porous PPS films and preparation method thereof |
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| CN201710034298.1A CN107057353A (en) | 2017-01-18 | 2017-01-18 | A kind of porous PPS films and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2020007387A (en) * | 2018-07-03 | 2020-01-16 | ポリプラスチックス株式会社 | Porous molded article and method for producing the same |
| CN114989721A (en) * | 2022-04-28 | 2022-09-02 | 浙江新和成特种材料有限公司 | Polyphenylene sulfide compound coating and preparation method thereof |
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| JPH0257332A (en) * | 1988-08-22 | 1990-02-27 | Toyobo Co Ltd | Felt laminate |
| CN101234305A (en) * | 2007-02-02 | 2008-08-06 | 中国科学院化学研究所 | Polyphenylene sulfide porous film and preparation thereof |
| CN102516767A (en) * | 2011-11-24 | 2012-06-27 | 东北石油大学 | Polyphenyl thioether sweating type lubricating friction-resistant composite material and preparation method thereof |
| CN103205123A (en) * | 2013-03-06 | 2013-07-17 | 珠海市赛纬电子材料有限公司 | Production method of polyphenylene sulfide diaphragm in lithium ion batteries |
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|---|---|---|---|---|
| JPH0257332A (en) * | 1988-08-22 | 1990-02-27 | Toyobo Co Ltd | Felt laminate |
| CN101234305A (en) * | 2007-02-02 | 2008-08-06 | 中国科学院化学研究所 | Polyphenylene sulfide porous film and preparation thereof |
| CN102516767A (en) * | 2011-11-24 | 2012-06-27 | 东北石油大学 | Polyphenyl thioether sweating type lubricating friction-resistant composite material and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2020007387A (en) * | 2018-07-03 | 2020-01-16 | ポリプラスチックス株式会社 | Porous molded article and method for producing the same |
| JP7071235B2 (en) | 2018-07-03 | 2022-05-18 | ポリプラスチックス株式会社 | Porous molded body and its manufacturing method |
| CN114989721A (en) * | 2022-04-28 | 2022-09-02 | 浙江新和成特种材料有限公司 | Polyphenylene sulfide compound coating and preparation method thereof |
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