CN103849147B - Biaxial orientation polyphenyl sulfide composite film - Google Patents
Biaxial orientation polyphenyl sulfide composite film Download PDFInfo
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- CN103849147B CN103849147B CN201410093993.1A CN201410093993A CN103849147B CN 103849147 B CN103849147 B CN 103849147B CN 201410093993 A CN201410093993 A CN 201410093993A CN 103849147 B CN103849147 B CN 103849147B
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Abstract
The present invention relates to specialty films preparing technical field, a kind of good toughness, the biaxial orientation polyphenyl sulfide composite film of excellent heat resistance, this laminated film has a following component: film polyphenylene sulfide resin, organic elastomer, inorganic filler, wherein, film polyphenylene sulfide resin comprises masterbatch film polyphenylene sulfide resin and slab film polyphenylene sulfide resin.The biaxial orientation polyphenyl sulfide composite film using technical scheme to prepare has thermostability, dimensional stability, hot formability and the toughness of excellence, and the biaxial orientation polyphenyl sulfide composite film of the present invention can be applicable to the field such as the electrically insulating materials such as motor, transformator, insulated cable or moulding material, circuit base material and mobile phone speaker diaphragm.
Description
Technical field
The present invention relates to specialty films preparing technical field, a kind of good toughness, excellent heat resistance double
Axle orientation polyphenyl sulfide composite film and preparation method thereof.
Background technology
Along with development and the continuous progress of science and technology of society, new technique and new material are opened by people
Sending out more and more extensive, the application to the insulant such as electronics, electrical equipment requires more and more higher, and especially electricity is absolutely
Edge Material Field there is high heat resistance, hydrolytic resistance, water absorption is low and moisture absorption is low new material.
Polyphenylene sulfide (PPS) have excellence chemical resistance and high temperature under heat stability, water absorption,
Moisture absorption is relatively low, and has anti-flammability, insulating properties, radiation resistance and good mechanical performance, can extensively answer
For automobile, Aero-Space, electronics and Food Engineering Development aspect.PPS thin film has the heat-resisting of excellence
Property, anti-flammability, rigidity, chemical reagent resistance, excellent electrical insulating property excellence, the feature such as agent of low hygroscopicity,
Can be used as the basement membrane of magnetic recording medium, capacitor, other electronic components or the insulant of equipment.But
It is that toughness and the intensity of single PPS material product are poor, are easier to embrittlement, especially PPS thin film system
Product, toughness and elongation at break are relatively low, it is difficult to meet the use requirement of modern society.
Summary of the invention
The technical problem to be solved in the present invention is: exist for single PPS film article of the prior art
Toughness and elongation at break are relatively low, it is difficult to meet modern society uses the problem required, it is provided that a kind of each side
Biaxial orientation polyphenyl sulfide composite film that face performance is the most excellent and preparation method thereof.
The technical solution adopted for the present invention to solve the technical problems is: a kind of biaxial orientation polyphenylene sulfide is combined
Thin film, this laminated film has a following component: film polyphenylene sulfide resin, organic elastomer, inorganic fill out
Material, wherein, film polyphenylene sulfide resin comprises masterbatch film polyphenylene sulfide resin and slab thin film
Level polyphenylene sulfide, according to mass ratio meter, masterbatch film polyphenylene sulfide resin and organic elastomer
Proportioning is 85～99: 1～15, the total amount sum of masterbatch film polyphenylene sulfide resin and organic elastomer with
The proportioning of inorganic filler is 100: 0.2～0.6；Masterbatch film polyphenylene sulfide resin, organic elastomer,
Inorganic filler three's total amount sum is 1～3: 7～9 with the proportioning of slab film polyphenylene sulfide resin；Institute
Stating organic elastomer is the one in polyethylene, polypropylene, politef, polyester, Merlon, nothing
The particle diameter of machine filler is 0.1～3 μm.
Further, described film polyphenylene sulfide resin molecular weight is 4～50,000, when 315 DEG C, and melt flows
Speed 100g/10min, described inorganic filler be silicon dioxide, glass microballoon, calcium carbonate, barium sulfate, two
One in titanium oxide.
Preferably, described masterbatch film polyphenylene sulfide resin is 85: 15 with the proportioning of organic elastomer,
The total amount sum of masterbatch film polyphenylene sulfide resin and organic elastomer with the proportioning of inorganic filler is
100∶0.4；Masterbatch film polyphenylene sulfide resin, organic elastomer, inorganic filler three's total amount sum
It is 2: 8 with the proportioning of slab film polyphenylene sulfide resin.
A kind of preparation method of biaxial orientation polyphenyl sulfide composite film, this preparation method has following steps:
(1) material is prepared
Prepare film polyphenylene sulfide resin, organic elastomer, inorganic filler, wherein, film-grade polyphenylene sulfide
Ether resin comprises masterbatch film polyphenylene sulfide resin and slab film polyphenylene sulfide resin, according to matter
Amount is 85～99: 1～15 than meter, masterbatch film polyphenylene sulfide resin with the proportioning of organic elastomer, female
The total amount sum of material film polyphenylene sulfide resin and organic elastomer and the proportioning of inorganic filler are 100:
0.2～0.6；Masterbatch film polyphenylene sulfide resin, organic elastomer, inorganic filler three's total amount sum
It is 1～3: 7～9 with the proportioning of slab film polyphenylene sulfide resin；
(2) prepared by masterbatch
By above-mentioned material according to masterbatch film polyphenylene sulfide resin, organic elastomer, the elder generation of inorganic filler
Rear charging sequence, makes masterbatch by mixed material after double screw extruder is extruded, and wherein extruder temperature exists
Between 310～330 DEG C；
(3) curtain coating slab
Masterbatch step (2) obtained and slab film polyphenylene sulfide resin are with mass ratio 1～3: 7～9
Ratio mixing, through double screw extruder melt blending extrude, to the applying that surface temperature is 30～40 DEG C
Carry out closely sealed cooling and solidifying while the conveying of electrostatic charge cold roller, obtain non-stretched polyphenylene sulfide tape casting diaphragm；
Wherein, rate of feeding 25～50r/min, screw speed 150～250r/min, dosing pump rotating speed 25～
50r/min, fusion plastification temperature is 310～340 DEG C, and die head temperature is 315～345 DEG C；
(4) stretching film forming
Non-stretched polyphenylene sulfide tape casting diaphragm step (3) obtained carries out biaxial stretch-formed, and drawing process is adopted
With first longitudinal stretching the most in the longitudinal direction, then carry out the biaxial stretching process successively of cross directional stretch in the direction of the width,
Specific as follows:
A, longitudinal stretching: tape casting diaphragm is sent into longitudinal stretching roller, stretches on the longitudinal direction of film,
Stretching ratio is 2.0～4.0 times, and draft temperature is 90～110 DEG C, then by the chill roll group of 20～50 DEG C
Cooling；
B, cross directional stretch: the sheet through longitudinal stretching is sent into transverse drawing mill and carries out cross directional stretch, preheating
Temperature 95 DEG C～120 DEG C, preheating time 15～30s；Draft temperature is 100 DEG C～130 DEG C, stretching ratio
3.0～5.0 times；Carrying out thermal finalization while carrying out in the direction of the width relaxing to this stretched film subsequently, heat is fixed
Type temperature 250 DEG C～270 DEG C, the time 10～20s, relaxation rate 2～7%, it is finally cooled to room temperature, obtains double
Axle orientation polyphenyl sulfide composite film.
Preferably, the extruder temperature in described step (2) is 310 DEG C；Rate of feeding in step (3)
For 35r/min, screw speed is 205r/min, dosing pump rotating speed 38r/min, and fusion plastification temperature is
310 DEG C, die head temperature is 315 DEG C；In step (4) a, longitudinal stretching multiplying power is 3.5 times, draft temperature
It it is 93 DEG C；In step (4) b, cross directional stretch preheating temperature be 113 DEG C, preheating time 15s；Stretching temperature
Degree is 113 DEG C, stretching ratio 3.5 times, and heat setting temperature is 270 DEG C, time 15s, relaxation rate 5%.
Beneficial effect: in technical scheme, the addition of organic elastomer can be effectively improved later stage polyphenyl
The structural strength of thioether laminated film, toughness and elongation at break；The addition of inorganic filler can be effectively improved thin
The thermostability of film, thermal dimensional stability and crystallinity, the insulating properties of gained composite are substantially dropped
Low；Organic elastomer and inorganic filler in the preparation method of the present invention add with the form of masterbatch, and pass through
Melt extrude for twice, make resin dispersion in mixed material be more uniformly distributed, be effectively controlled reunion, make
The surface property obtaining later stage PPS films is more stable homogeneous, and is substantially reduced production cost, improves
Productivity effect.The biaxial orientation polyphenyl sulfide composite film using technical scheme to prepare has excellence
Thermostability, thermal dimensional stability, hot formability and toughness, can be applicable to motor, transformator, insulated electro
The fields such as the electrically insulating materials such as cable or moulding material, circuit base material and mobile phone speaker diaphragm.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention will be further described.Polypropylene in following embodiment by
Petrochemical industry Yang Zi petrochemical industry company limited of state provides, and Merlon is provided by Korea S's LG chemistry, politef
Thered is provided by du pont company.
Embodiment one
A kind of preparation method of biaxial orientation polyphenyl sulfide composite film, this preparation method has following steps:
(1) material is prepared
Prepare film polyphenylene sulfide resin, polypropylene, silicon dioxide, wherein, film-grade polyphenylene sulfide resin
Fat comprises masterbatch film polyphenylene sulfide resin and slab film polyphenylene sulfide resin, according to mass ratio
Meter, masterbatch film polyphenylene sulfide resin and polyacrylic proportioning are 85: 15, masterbatch film-grade polyphenyl
The proportioning of sulfide resin and polyacrylic total amount sum and silicon dioxide is 100: 0.4；Masterbatch film-grade is gathered
Diphenyl sulfide resin, polypropylene, silicon dioxide three's total amount sum and slab film polyphenylene sulfide resin
Proportioning is 2: 8；
(2) prepared by masterbatch
By above-mentioned material according to masterbatch film polyphenylene sulfide resin, polypropylene, silicon dioxide charging suitable
Sequence, makes masterbatch after twin-screw extrusion, and extruder temperature is 310 DEG C；
(3) curtain coating slab
The masterbatch that step (2) obtained and slab film polyphenylene sulfide resin are with the ratio of mass ratio 2: 8
Example mixes, and extrudes through double screw extruder melt blending, to the applying electrostatic that surface temperature is 30～40 DEG C
Carry out closely sealed cooling and solidifying while the conveying of lotus cold roller, obtain non-stretched polyphenylene sulfide tape casting diaphragm；
Wherein, rate of feeding 35r/min, screw speed 205r/min, dosing pump rotating speed 38r/min, melted
Plasticization temperature is 310 DEG C, and die head temperature is 315 DEG C；
(4) stretching film forming
Non-stretched polyphenylene sulfide tape casting diaphragm step (3) obtained carries out biaxial stretch-formed, and drawing process is adopted
With first longitudinal stretching the most in the longitudinal direction, then carry out the biaxial stretching process successively of cross directional stretch in the direction of the width,
Specific as follows:
A, longitudinal stretching: tape casting diaphragm is sent into longitudinal stretching roller, stretches on the longitudinal direction of film,
Stretching ratio is 3.5 times, and draft temperature is 93 DEG C, then cools down by the chill roll group of 20～50 DEG C；
B, cross directional stretch: the sheet through longitudinal stretching is sent into transverse drawing mill and carries out cross directional stretch, preheating
Temperature 113 DEG C, preheating time 15s；Draft temperature is 113 DEG C, stretching ratio 3.5 times；Subsequently this is drawn
Stretch and while film carries out relaxing in the direction of the width, carry out thermal finalization, heat setting temperature 270 DEG C, time 15s,
Relaxation rate 5%, is finally cooled to room temperature, obtains biaxial orientation polyphenyl sulfide composite film.
Embodiment two
A kind of preparation method of biaxial orientation polyphenyl sulfide composite film, this preparation method has following steps:
(1) material is prepared
Prepare film polyphenylene sulfide resin, polypropylene, calcium carbonate, wherein, film polyphenylene sulfide resin
Comprise masterbatch film polyphenylene sulfide resin and slab film polyphenylene sulfide resin, according to mass ratio meter,
Masterbatch film polyphenylene sulfide resin and polyacrylic proportioning are 90: 10, masterbatch film-grade polyphenylene sulfide
The proportioning of resin and polyacrylic total amount sum and calcium carbonate is 100: 0.2；Masterbatch film-grade polyphenylene sulfide
Resin, polypropylene, calcium carbonate three's total amount sum are 1 with the proportioning of slab film polyphenylene sulfide resin:
9；
Remaining step is with embodiment one.
Embodiment three
A kind of preparation method of biaxial orientation polyphenyl sulfide composite film, this preparation method has following steps:
(1) material is prepared
Prepare film polyphenylene sulfide resin, Merlon, silicon dioxide, wherein, film-grade polyphenylene sulfide
Resin comprises masterbatch film polyphenylene sulfide resin and slab film polyphenylene sulfide resin, according to quality
Than meter, masterbatch film polyphenylene sulfide resin is 95: 5 with the proportioning of Merlon, and masterbatch film-grade is gathered
The total amount sum of diphenyl sulfide resin and Merlon and the proportioning of silicon dioxide are 100: 0.6；Masterbatch thin film
Level polyphenylene sulfide, Merlon, silicon dioxide three's total amount sum and slab film-grade polyphenylene sulfide
The proportioning of resin is 3: 7；
Remaining step is with embodiment one.
Embodiment four
A kind of preparation method of biaxial orientation polyphenyl sulfide composite film, this preparation method has following steps:
(1) material is prepared
Prepare film polyphenylene sulfide resin, politef, calcium carbonate, wherein, film-grade polyphenylene sulfide
Resin comprises masterbatch film polyphenylene sulfide resin and slab film polyphenylene sulfide resin, according to quality
Than meter, masterbatch film polyphenylene sulfide resin is 99: 1 with the proportioning of politef, masterbatch film-grade
The total amount sum of polyphenylene sulfide and politef and the proportioning of calcium carbonate are 100: 0.6；Masterbatch is with thin
Film level polyphenylene sulfide, politef, calcium carbonate three's total amount sum and slab film-grade polyphenylene sulfide
The proportioning of ether resin is 3: 7；
Remaining step is with embodiment one.
Comparative example one
Polyphenylene sulfide is obtained non-stretched polyphenylene sulfide stream through double screw extruder melt blending extrusion
Prolonging diaphragm, wherein fusion plastification temperature is at 310 DEG C, die head temperature 315 DEG C, cold roll temperature 30～40 DEG C, feeds
Material speed 35r/min, screw speed 205r/min, dosing pump rotating speed 38r/min.
Curtain coating is cast sheet successively longitudinally, laterally side be pulled up, wherein longitudinal stretching multiplying power 3.5 times,
Draft temperature 92 DEG C；Laterally preheating temperature 113 DEG C, preheating time 20s, draft temperature 113 DEG C, stretching times
Rate 3.5 times, heat setting temperature 270 DEG C, heat-setting time 15s, relaxation rate 5%；It is finally cooled to room temperature obtain
To PPS films.
The performance of the PPS thin film of above-described embodiment and comparative example gained is as shown in the table:
From the data of upper table, compared with comparative example 1, answering of the technical scheme gained of employing embodiment 1
The combination property closing film is optimal, and electric insulation breakdown strength is without substantially reducing；The component formula pair of laminated film
The impact of heat distortion temperature, surface roughness and insulation breakdown intensity is bigger.
Claims (1)
1. a biaxial orientation polyphenyl sulfide composite film, is characterized in that: this laminated film has a following component:
Film polyphenylene sulfide resin, organic elastomer, inorganic filler, wherein, film polyphenylene sulfide resin bag
Containing masterbatch film polyphenylene sulfide resin and slab film polyphenylene sulfide resin, according to mass ratio meter,
Masterbatch film polyphenylene sulfide resin is 85: 15 with the proportioning of organic elastomer, masterbatch film-grade polyphenyl
The total amount sum of sulfide resin and organic elastomer and the proportioning of inorganic filler are 100: 0.4；Masterbatch thin film
Level polyphenylene sulfide, organic elastomer, inorganic filler three's total amount sum and slab film-grade polyphenylene sulfide
The proportioning of ether resin is 2: 8；
Described organic elastomer is polypropylene, and the particle diameter of inorganic filler is 0.1～3 μm；Described inorganic filler is
Silicon dioxide；
This laminated film has a following preparation process:
(1) prepared by masterbatch
By above-mentioned material according to masterbatch film polyphenylene sulfide resin, polypropylene, silicon dioxide charging suitable
Sequence, makes masterbatch after twin-screw extrusion, and extruder temperature is 310 DEG C；
(2) curtain coating slab
The masterbatch that step (1) obtained and slab film polyphenylene sulfide resin are with the ratio of mass ratio 2: 8
Example mixes, and extrudes through double screw extruder melt blending, to the applying electrostatic that surface temperature is 30～40 DEG C
Carry out closely sealed cooling and solidifying while the conveying of lotus cold roller, obtain non-stretched polyphenylene sulfide tape casting diaphragm；Wherein,
Rate of feeding 35r/min, screw speed 205r/min, dosing pump rotating speed 38r/min, fusion plastification temperature is
310 DEG C, die head temperature is 315 DEG C；
(3) stretching film forming
Non-stretched polyphenylene sulfide tape casting diaphragm step (2) obtained carries out biaxial stretch-formed, and drawing process is adopted
With first longitudinal stretching the most in the longitudinal direction, then carry out the biaxial stretching process successively of cross directional stretch in the direction of the width,
Specific as follows:
A, longitudinal stretching: tape casting diaphragm is sent into longitudinal stretching roller, stretches on the longitudinal direction of film,
Stretching ratio is 3.5 times, and draft temperature is 93 DEG C, then cools down by the chill roll group of 20～50 DEG C；
B, cross directional stretch: the sheet through longitudinal stretching is sent into transverse drawing mill and carries out cross directional stretch, preheating
Temperature 113 DEG C, preheating time 15s；Draft temperature is 113 DEG C, stretching ratio 3.5 times；Subsequently this is drawn
Stretch and while film carries out relaxing in the direction of the width, carry out thermal finalization, heat setting temperature 270 DEG C, time 15s,
Relaxation rate 5%, is finally cooled to room temperature, obtains biaxial orientation polyphenyl sulfide composite film.
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| CN106928709B (en) * | 2015-12-30 | 2020-04-14 | 广东生益科技股份有限公司 | Filler-containing polyarylether or polyarylether thioether composite material, filler-containing polyarylether or polyarylether thioether composite material sheet and circuit substrate containing filler-containing polyarylether or polyarylether thioether composite material sheet |
| CN106751829B (en) * | 2016-11-24 | 2019-07-23 | 扬州亚宝新材料科技有限公司 | A kind of polyphenylene sulfide casting films and preparation method thereof |
| CN106497059B (en) * | 2016-11-24 | 2019-04-05 | 扬州亚宝新材料科技有限公司 | Double membranes of a kind of polyphenylene sulfide and preparation method thereof |
| CN116790123A (en) * | 2023-05-26 | 2023-09-22 | 东莞市欣荣天丽科技实业有限公司 | Food deoxidizer and preparation method thereof |
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| CN101797800A (en) * | 2009-12-30 | 2010-08-11 | 四川华通特种工程塑料研究中心有限公司 | Technology for preparing polyphenyl sulfide composite film |
| CN101921486A (en) * | 2008-11-17 | 2010-12-22 | 德阳科吉高新材料有限责任公司 | Polyphenylene sulfide compound film or fiber and manufacture method thereof |
| CN103087524A (en) * | 2013-03-04 | 2013-05-08 | 四川华通特种工程塑料研究中心有限公司 | Polyphenyl thioether sheet with electrical insulation properties and preparation method thereof |
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| CN102250481A (en) * | 2011-05-25 | 2011-11-23 | 上海树普新材料科技有限公司 | Plastic with high thermal conductivity and preparation method thereof |
| CN102558863A (en) * | 2012-01-04 | 2012-07-11 | 四川华通特种工程塑料研究中心有限公司 | Low-dielectric-property polyphenylene sulphide composite material and preparation method thereof |
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| CN101921486A (en) * | 2008-11-17 | 2010-12-22 | 德阳科吉高新材料有限责任公司 | Polyphenylene sulfide compound film or fiber and manufacture method thereof |
| CN101797800A (en) * | 2009-12-30 | 2010-08-11 | 四川华通特种工程塑料研究中心有限公司 | Technology for preparing polyphenyl sulfide composite film |
| CN103087524A (en) * | 2013-03-04 | 2013-05-08 | 四川华通特种工程塑料研究中心有限公司 | Polyphenyl thioether sheet with electrical insulation properties and preparation method thereof |
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