CN107141686A - A kind of preparation method of polypropylene material - Google Patents

A kind of preparation method of polypropylene material Download PDF

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Publication number
CN107141686A
CN107141686A CN201710310378.5A CN201710310378A CN107141686A CN 107141686 A CN107141686 A CN 107141686A CN 201710310378 A CN201710310378 A CN 201710310378A CN 107141686 A CN107141686 A CN 107141686A
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polypropylene
section
preparation
special fibre
machine barrel
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CN201710310378.5A
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Inventor
方万漂
朱雪梅
朱进平
方少章
王爱绿
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Wenzhou Win Innovation Material Technology Co Ltd
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Wenzhou Win Innovation Material Technology Co Ltd
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Priority to CN201710310378.5A priority Critical patent/CN107141686A/en
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    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L53/00—Compositions of block copolymers containing at least one sequence of a polymer obtained by reactions only involving carbon-to-carbon unsaturated bonds; Compositions of derivatives of such polymers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B9/00—Making granules
    • B29B9/02—Making granules by dividing preformed material
    • B29B9/06—Making granules by dividing preformed material in the form of filamentary material, e.g. combined with extrusion
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25—Component parts, details or accessories; Auxiliary operations
    • B29C48/36—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die
    • B29C48/395—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders
    • B29C48/40—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders using two or more parallel screws or at least two parallel non-intermeshing screws, e.g. twin screw extruders
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
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    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
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    • B29C59/00—Surface shaping of articles, e.g. embossing; Apparatus therefor
    • B29C59/14—Surface shaping of articles, e.g. embossing; Apparatus therefor by plasma treatment
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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    • B29C69/00—Combinations of shaping techniques not provided for in a single one of main groups B29C39/00 - B29C67/00, e.g. associations of moulding and joining techniques; Apparatus therefore
    • B29C69/02—Combinations of shaping techniques not provided for in a single one of main groups B29C39/00 - B29C67/00, e.g. associations of moulding and joining techniques; Apparatus therefore of moulding techniques only
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    • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
    • C08J9/12—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent
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    • C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
    • C08J9/12—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent
    • C08J9/14—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent organic
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    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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    • B29C2948/00—Indexing scheme relating to extrusion moulding
    • B29C2948/92—Measuring, controlling or regulating
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    • B29C2948/92704—Temperature
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
    • B29K2023/00—Use of polyalkenes or derivatives thereof as moulding material
    • B29K2023/10—Polymers of propylene
    • B29K2023/12—PP, i.e. polypropylene
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
    • B29K2105/00—Condition, form or state of moulded material or of the material to be shaped
    • B29K2105/06—Condition, form or state of moulded material or of the material to be shaped containing reinforcements, fillers or inserts
    • B29K2105/08—Condition, form or state of moulded material or of the material to be shaped containing reinforcements, fillers or inserts of continuous length, e.g. cords, rovings, mats, fabrics, strands or yarns
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29L—INDEXING SCHEME ASSOCIATED WITH SUBCLASS B29C, RELATING TO PARTICULAR ARTICLES
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    • C08J2203/00—Foams characterized by the expanding agent
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    • C08J2203/22—Expandable microspheres, e.g. Expancel®
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    • C08J2353/00—Characterised by the use of block copolymers containing at least one sequence of a polymer obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers
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    • C08J2461/00—Characterised by the use of condensation polymers of aldehydes or ketones; Derivatives of such polymers
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Abstract

The invention provides a kind of special fibre RPP material and its preparation method and application, comprising 50~90 parts of polypropylene；10~50 parts of special fibre；1.0~2.0 parts of compatilizer；0.3~0.5 part of coupling agent；0.5~1.0 part of antioxidant；0.5~0.8 part of doping silicon dioxide；0.5~3.0 part of nano imvite；0.5~2.0 part of fretting map polymer；Extruded using double screw extruder, the polypropylene material of low-k and electrical breakdown withstand function admirable is prepared for by special screw combinations and fiber coal addition position technological means, the polypropylene film of specific use is prepared using the material, plasma treatment is carried out to film surface simultaneously, the film can apply to the special dimension particular component such as military project, microelectronic industry.

Description

A kind of preparation method of polypropylene material
Technical field
The invention belongs to technical field of polymer materials, and in particular to a kind of TRPP material and preparation method And its application.
Background technology
With the development of super large-scale integration, interconnection RC delay is increasingly severe, seriously constrains high-speed cruising Performance, conventional insulating layer silica causes selfcapacity to increase due to the continuous diminution of thickness, reduces the reliability of circuit, is This problem is solved, the material of application low-k, high electrical breakdown withstand is replaced traditional silica by microelectronics industry Insulating materials.It is 2.25~2.50 (being tested under 106Hz) under polyacrylic dielectric constant normal temperature, and cost is low, but with rigidity The problem of low, poor heat resistance, therefore multi-purpose glass carries out enhanced modification to it, to improve the mechanical strength of material and heat-resisting Performance, but the elongation of fiber glass reinforced polypropylene is greatly lowered, and is difficult to prepare the small film of thickness, and the material after fiberglass reinforced Dielectric constant is also increased as to 3.5~40, electrical breakdown hydraulic performance decline, while being not suitable for blowfilm shaping, it is difficult to apply in army The special dimensions such as work, communication electronics.
The content of the invention
In order to overcome the problem of existing fiber glass reinforced polypropylene material is present, an object of the present invention is to provide a kind of tool There are the special fibre RPP material of low-k, high electrical breakdown withstand, of a relatively high elongation at break, the army of being exclusively used in The particular component of the special dimensions such as work, communication electronics.
It is a further object to provide a kind of preparation method of special fibre RPP material.
The present invention a further object is that offer is a kind of and prepare special type PP films product and method using the polypropylene material.
Technical scheme is as follows：
A kind of special fibre RPP material, is prepared from by weight by following components：
50~90 parts of polypropylene；
10~50 parts of special fibre；
1.0~2.0 parts of compatilizer；
0.3~0.5 part of coupling agent；
0.5~1.0 part of antioxidant；
0.5~0.8 part of doping silicon dioxide；
0.5~3.0 part of nano imvite；
Described special fibre be polyether-ketone (PEK), polyether-ether-ketone (PEEK), one kind in PEKK (PEKK) or A variety of, compared with glass, they have lower dielectric constant；Doping silicon dioxide is carbon-doped silicon oxide, fluorine doped silica One or both of composition with boron doped silica, doping silicon dioxide, which is added, there is collaboration to make reduction dielectric constant With；The nano imvite can improve material electrical breakdown performance.
A kind of described special fibre RPP material, in addition to a kind of fretting map polymer, fretting map polymerization Thing is a kind of core shell structure, and shell is that thermoplastic acrylic resin is birdsed of the same feather flock together compound, and kernel is the spherical modeling that alkanes gas is constituted Expect particle, content is 0.5~2.0 part, has synergy to reduction dielectric constant.
Described special fibre 0.1~1.0mm of filament diameter, preferably 0.5~0.8mm of filament diameter, too thin monofilament is straight Footpath is unfavorable for improving tensile strength, the bending strength of material.
Described doping silicon dioxide is preferably the composition of fluorine doped silica and boron doped silica, both compositions Optimal mixing ratio is 2: 1.
Described polypropylene under 230 DEG C/2.16Kg melting means for 10~100g/10min highly crystalline HOPP or The comonomer of at least one of block copolymerization polypropylene, wherein block copolymerization polypropylene be ethene, contents of ethylene be 5~ 8mol%；The crystallinity of highly crystalline HOPP is not less than 80%, isotacticity not less than 95%.
Described compatilizer for the copolymer, wherein maleic anhydride of maleated polypropylene content 10~60%, it is and general Logical maleic anhydride inoculated polypropylene is compared, it is easier to improve the compatibility of fiber and PP resins.
Described antioxidant be 1.3.5- tri- (3,5- di-t-butyls, 4- hydroxybenzyls) s-triazine (3114), 4.4 '-it is thio Double (the 6- tert-butyl group -3- methylphenols) (300), thio-2 acid two (18) ester (DSTP) and three [2.4- di-tert-butyl-phenyls] Phosphite ester (168) carries out compounding use according to mass ratio 1: 1: 2: 1, and the thermo-oxidative stability of processing is provided for PP.
Described coupling agent is one kind in silane coupler, aluminate coupling agent, titanate coupling agent, and preferably silane is even Join agent, be conducive to further improving the compatibility between fiber and polypropylene.
Described nano imvite powder size is no more than 300 nanometers.The addition of nano imvite can improve material Electrical breakdown withstand performance.
Another goal of the invention of the present invention is to provide above-mentioned RPP material preparation method, and step is as follows：
(1) by proportioning, by polypropylene, compatilizer, coupling agent, antioxidant, doping silicon dioxide, fretting map polymer successively It is added in high mixer, mixes 3-5 minutes, obtains grain powder mixture；
(2) using equidirectional parallel double-screw extruder equipment, the draw ratio 44: 1~60: 1 of double screw extruder, preferably 48: 1~52: 1, double screw extruder sets side forced feeding along extrusion direction Section 7 machine barrel, is set between Section 6 and Section 7 Thickness 3mm asbestos or polytetrafluoroethylene (PTFE) heat insulating mattress are put, along the screw rod group of 1~Section 6 machine barrel position in extrusion direction Close the one kind taken in following a combinations, b combinations, three kinds of combinations of c combinations：
A is combined：36/36、36/36、X90/90、X90/90、GD90/45、56/56、56/56、 90/5-45°、90/5- 45°、56/56、90/5-45°、90/5-45°、56/56、 90/5-45°、90/5-45°、56/56、56/5-45°、56/5-45°、 48/4-60°、 48/5-90°、56/56、240/60、L240/60；
B is combined：36/36、36/36、X90/90、X90/90、GD90/45、56/56、90/5-45°、 90/5-45°、56/ 56、90/5-45°、90/5-45°、C36/36、C36/36、90/5-45°、 56/56、90/5-45°、56/5-45°、56/5- 45°、56/56、48/4-60°、 48/5-90°、90/7-30°；
C is combined：36/36、36/36、62-X90/90、62-X90/90、62-GD90/45、90/5-45°、 90/5-45°、 CXL56/28、90/5-45°、62-CXL56/28、90/5-45°、 90/5-45°、56/56、56/5-45°、56/5-45°、48/ 4-60°、L56/28、 90/7-30°、48/5-90°、56/56、C36/36、C36/36。
(3), Section 1 machine barrel (i.e. main feed opening) aperture position of the special fibre along extrusion direction is rotated with extruder draws Enter, while part grain powder mixture is added in Section 1 machine barrel (i.e. main feed opening) aperture position, by weighing the unit interval respectively The weight of the RPP material inside obtained and in the unit interval special fibre reduction Weight control special fibre with passing through The weight ratio that Section 1 machine barrel (i.e. main feed opening) aperture position adds both part grain powder mixtures is 1: 2.
(4), after debugging completes main feed opening special fibre and part grain powder mixture feeding ratio, remaining grain is mixed Mixture sets side forced feeding mouthful to feed by Section 7 machine barrel.Feeding is realized by adjusting the rotating speed of lateral feeding machine Ratio.
(5), in extrusion, the temperature along Section 1~Section 6 machine barrel position in extrusion direction is set as 110~130 ℃.Section 7 to die temperature is set as 180~220 DEG C.
(6), in extrusion, control extruder negative-pressure vacuum degree is not less than 0.05MPa.
(7), extrusion material strip is cooled down through tank, and control tank temperature is no more than 25 DEG C, is crossed water length and is not less than 15m, it is ensured that The surface temperature of material strip road pelleter mouthful after entering is less than 35 DEG C, and a kind of special fibre enhancing poly- third is obtained through pelleter pelletizing Alkene material.
Super face can also be injected at the mouth mold of double screw extruder by gas phase assistant formation equipment in extrusion Boundary N2、CO2、H2One kind in inert gas, prepares the polypropylene material of fretting map, preferably CO2Gas.
Another goal of the invention of the present invention is to provide one kind and prepares PP films product and method using the polypropylene material, Step is as follows：
(1), by a kind of above-mentioned special fibre RPP material be placed in baking oven dry, drying condition be 80~ 110 DEG C, 1~3h of drying time.
(2), the extruded Blown Film of dried pellet or through rolling film forming, extrusion and blow molding or calendering formation process Processing temperature be set as 180~220 DEG C.
(3) film of preparation, is subjected to plasma treatment, the gas used using plasma processor to the surface of PP films Including N2、He、H2、NH3Or the mixed gas between them, gas flow 200sccm, rf frequency is 13.56MHZ, cavity Air pressure is 100mTorr, and processing time is 3~5min, and radio-frequency power is 360w, and special PP film products are made.
The present invention compared with the existing technology, has the advantages that：
1st, the present invention does reinforcing agent using special fibre, while adding a certain amount of doping silicon dioxide, nano imvite And fretting map polymer, make made polypropylene material that there is relatively low dielectric constant and higher electrical breakdown withstand performance, simultaneously Material flexibility is good, with higher extensibility, is applicable to blowfilm shaping or calendering formation；
2nd, present invention uses special double-screw structure and screw combinations so that is squeezed using slightly improved parallel dual-screw Special fibre can be clipped to the microscopic dimensions of needs by going out machine, the mechanical property required for obtaining；
3rd, the present invention is surface-treated using using plasma processing method to PP films, improves the dielectric strength of film, So that obtained thin film surface planeness is high, Step Coverage performance is good, so as to be conducive to the process stabilizing of follow-up integrated circuit；
4th, the present invention uses thermoplastic polypropylene for resin matrix, and the cost of material is low, recoverable, does not result in environment Pollution.
Polypropylene material prepared by the present invention have dielectric constant it is low, it is easily processed into type the features such as, can be applied to military project And the special dimension such as Communication Equipment.
Brief description of the drawings
Fig. 1 is screw combinations (a combinations) figure.
Fig. 2 is screw combinations (b combinations) figure.
Fig. 3 is screw combinations (c combinations) figure.
Embodiment
With reference to embodiment, the present invention is further detailed explanation.Performance evaluation mode and implementation standard：Stretching Performance test is carried out according to ASTM D638, draw speed 5mm/min, gauge length 115mm, batten size：Total length 175mm, parallel portion Point：10mm×4mm；Crooked test is carried out according to ASTM D790, rate of bending 5mm/min, span 100mm, batten size： 127mm×12.7mm×6.4mm；Impact property test is carried out according to ASTM D256, batten size：80mm×10mm×4mm (molding breach)；The test of dielectric constant is carried out according to GB/T 1409-2006, and test frequency is 1MHz, and test bars size is 8mm × 3.2mm × 1.6mm, the dielectric strength of film is according to ASTM D-149.
Table 1, comparative example 1 and embodiment 1~implementation 8 are formulated
Polypropylene in table 1 is block copolymerization polypropylene, and wherein the comonomer of block copolymerization polypropylene is ethene, ethene Base content be 5mo1%, glass be alkali-free E glasses, filament diameter 13um, special fibre be PEEK fibers, filament diameter 0.7mm, The compatilizer of embodiment 3 is maleic anhydride graft PP, grafting rate 1%, and comparative example and other embodiment compatilizer are maleic acid in table 1 The polyacrylic copolymer of acid anhydride, maleic anhydride content 30%, coupling agent is Silane coupling agent KH550, antioxidant is 3114,300, DSTP and 168 mixture, its ratio is that 3114: 300: DSTP: 168 ratios are 1: 1: 2: 1, and fretting map polymer is Acker Revive a kind of core shell structure of production, shell is that thermoplastic acrylic resin is birdsed of the same feather flock together compound, and kernel is the ball that alkanes gas is constituted Shape plastic grain, nano imvite is commercially available prod, and powder size is within 300 nanometers, embodiment 2, embodiment 3, embodiment 5th, the doping silicon dioxide of embodiment 8 is the composition of carbon-doped silicon oxide and boron doped silica silica, the two mixing Than 1: 1, embodiment 4, embodiment 6, embodiment 7 are the composition of fluorine doped silica and boron doped silica silica, two Person's mixture, its mixed proportion is respectively 1: 1,3: 2 and 2: 1.Embodiment 8 and embodiment 9 are auxiliary by gas phase at extrusion neck ring mold Former is helped to inject supercritical CO2Gas, embodiment 9 its difference is that embodiment 9 takes 0.3mm monofilament with embodiment 8 The PEEK fibers of diameter.
Above-mentioned RPP material preparation method, step is as follows：
(1) by proportioning, by polypropylene, compatilizer, coupling agent, antioxidant, doping silicon dioxide, fretting map polymer successively It is added in high mixer, mixes 4 minutes, obtains grain powder mixture.
(2) equidirectional parallel double-screw extruder equipment, the draw ratio 48: 1 of double screw extruder, twin-screw extrusion are used Machine sets side forced feeding, Section of 6 setting thickness 3mm between Section 7 asbestos insulation along extrusion direction Section 7 machine barrel Pad, following screw combinations (a combinations) are taken along the screw combinations of Section of the 1st~6 machine barrel position in extrusion direction：36/36、 36/36、 X90/90、X90/90、GD90/45、56/56、56/56、90/5-45°、90/5-45°、 56/56、90/5-45°、 90/5-45°、56/56、90/5-45°、90/5-45°、56/56、 56/5-45°、56/5-45°、48/4-60°、48/5-90°、 56/56、240/60、 L240/60。
(3), Section 1 machine barrel (i.e. main feed opening) aperture position of the special fibre along extrusion direction is rotated with extruder draws Enter, while part grain powder mixture is added in Section 1 machine barrel (i.e. main feed opening) aperture position, by weighing the unit interval respectively The weight of the RPP material inside obtained and in the unit interval special fibre reduction Weight control special fibre with passing through The weight ratio that Section 1 machine barrel (i.e. main feed opening) aperture position adds both part grain powder mixtures is 1: 2.
(4), after debugging completes main feed opening special fibre and part grain powder mixture feeding ratio, remaining grain is mixed Mixture sets side forced feeding mouthful to feed by Section 7 machine barrel.Feeding is realized by adjusting the rotating speed of lateral feeding machine Ratio.
(5), in extrusion, the temperature along Section 1~Section 6 machine barrel position in extrusion direction is set as 110~130 ℃.Section 7 to die temperature is set as 180~220 DEG C.
(6), in extrusion, control extruder negative-pressure vacuum degree is not less than 0.05MPa.
(7), extrusion material strip is cooled down through tank, and control tank temperature is no more than 25 DEG C, is crossed water length and is not less than 15m, it is ensured that The surface temperature of material strip road pelleter mouthful after entering is less than 35 DEG C, and a kind of special fibre enhancing poly- third is obtained through pelleter pelletizing Alkene material.
When preparing embodiment 8 and embodiment 9, inject overcritical by gas phase assistant formation equipment at extrusion neck ring mold CO2Gas.
Comparative example 1 and the testing result of embodiment 1~8 are shown in Table 2：
Table 2, comparative example 1 and embodiment 1~testing result of implementation 8
Found from table 2 in comparative example 1 and embodiment 1, simple glass fiber reinforcement PP, dielectric are substituted using special fibre Constant, breakdown voltage, elongation, Izod notch shocks are increased substantially, tensile strength and bending strength reduction, i.e., material is soft Toughness and electrical property are significantly improved, while the rigidity of expendable material.Found from embodiment 2, add doping titanium dioxide After silicon, the dielectric constant of material is further reduced, and is found from embodiment 3, is added after nano imvite, the breakdown voltage of material Further improve, from embodiment 3 and the contrast of embodiment 4 it can be found that using the improvement of maleic anhydride inoculated polypropylene relative consistency It is big to be much worse than using maleic anhydride and polyacrylic copolymer, it is clear that copolymer due to the maleic anhydride ratios containing high content, Be more beneficial for solve material compatibility issues, from the contrast of embodiment 4 and embodiment 5 it can be found that fretting map polymer plus Enter so that the dielectric constant of material is down to 1.5, the contrast of embodiment 4 and embodiment 6 and embodiment 7 is it can be found that different mixes The combination of miscellaneous silica has considerable influence, fluorine doped silica: the combination of boron doped silica silica to dielectric constant Thing is optimal case, and shown through many experiments that optimal Mixing ratio by weight between the two is 2: 1.From embodiment 8 and embodiment 5 contrasts, it can be seen that without fretting map polymer, but by injecting gas in extrusion neck ring mold, form material internal Minute pores reach same effect with addition fretting map aggregation, show from the contrast of embodiment 8 and embodiment 9, thinner single The fiber of silk diameter is unfavorable for improving the strength and stiffness of material, but is conducive to improving the pliability of material.
The formula of embodiment 7 is prepared into RPP by different screw combinations, detection properties are shown in Table 3：
Table 3：Different screw combinations are to strengthening the influence of PP performances
Wherein embodiment 7 is using screw combinations (a combinations)：36/36、36/36、X90/90、 X90/90、GD90/45、56/ 56、56/56、90/5-45°、90/5-45°、56/56、 90/5-45°、90/5-45°、56/56、90/5-45°、90/5-45°、 56/56、 56/5-45°、56/5-45°、48/4-60°、48/5-90°、56/56、240/60、 L240/60。
Wherein embodiment 10 is using screw combinations (b combinations)：36/36、36/36、X90/90、 X90/90、GD90/45、 56/56、90/5-45°、90/5-45°、56/56、90/5-45°、 90/5-45°、C36/36、C36/36、90/5-45°、56/ 56、90/5-45°、56/5-45°、 56/5-45°、56/56、48/4-60°、48/5-90°、90/7-30°。
Wherein embodiment 11 is using screw combinations (c combinations)：36/36、36/36、62-X90/90、 62-X90/90、62- GD90/45、90/5-45°、90/5-45°、CXL56/28、90/5-45°、 62-CXL56/28、90/5-45°、90/5-45°、 56/56、56/5-45°、56/5-45°、 48/4-60°、L56/28、90/7-30°、48/5-90°、56/56、C36/36、C36/ 36。
The intensity of a, b, c screw combinations weakens successively, and can be seen that weaker combination from the data in table 3 improves material The tensile strength and bending strength of the intensity and rigidity of material, i.e. material increase, and the reduction of pliability of material, i.e. material Elongation and impact strength decreased, the dielectric strength on material do not influence, and reduce the electrical breakdown withstand performance of material.
The RPP prepared using embodiment 7, prepares PP film products, and step is as follows：
(1), RPP material is placed in baking oven and dried, and drying condition is 100 DEG C, drying time 2h.
(2), the extruded Blown Film of dried pellet, the temperature of extrusion-blown modling process is set as 180~220 DEG C.
(3) film of preparation, is subjected to plasma treatment using plasma processor, the gas used includes N2、He、H2、 NH3Or the mixed gas between them, gas flow 200sccm, rf frequency is 13.56MHZ, and cavity air pressure is 100mTorr, processing time is 3~5min, and radio-frequency power is 360w, and special PP film products are made.
Test the electrical breakdown withstand performance such as table 4 below of the PP films prepared：
Table 4：Influence of the different disposal technique to PP film electrical breakdown withstand performances
The gas that embodiment 12~14 is used is respectively N2、He、H2、NH3, the time is 3min, embodiment 16 and embodiment 17 gases used is N2, processing time is respectively 4min and 5min.
From table 4 it can be found that for improving electrical breakdown withstand performance, using N2, processing time 3min preferably side Case.For reducing the dielectric constant of film, processing time is without influence, the preferred H of gas of use2, with specific reference to the specific of application Purposes and autotelic selection processing gas.
The above-mentioned description to embodiment is understood that for ease of those skilled in the art and using this hair It is bright.Person skilled in the art obviously easily can make various modifications to these embodiments, and described herein General Principle is applied in other embodiment without passing through performing creative labour.Therefore, the invention is not restricted to implementation here Example, those skilled in the art do not depart from improvement that scope made and change all should be according to the announcement of the present invention Within protection scope of the present invention.

Claims (8)

1. a kind of preparation method of polypropylene material, it is characterised in that the polypropylene prepared by weight by following components and Into：
50~90 parts of polypropylene；
10~50 parts of special fibre；
1.0~2.0 parts of compatilizer；
0.3~0.5 part of coupling agent；
0.5~1.0 part of antioxidant；
0.5~0.8 part of doping silicon dioxide；
0.5~3.0 part of nano imvite；
0.5~2.0 part of fretting map polymer；
Described special fibre is the one or more in polyether-ketone (PEK), polyether-ether-ketone (PEEK), PEKK (PEKK)； Described doping silicon dioxide is the group of one or both of carbon-doped silicon oxide, fluorine doped silica with boron doped silica Compound, described nano imvite powder size is no more than 300 nanometers；Described fretting map polymer is a kind of core shell structure, Shell is that thermoplastic acrylic resin is birdsed of the same feather flock together compound, and kernel is the sphere plastic particle that alkanes gas is constituted；Prepare this poly- third The method of alkene comprises the following steps：
Step (1) is by matching, by polypropylene, compatilizer, coupling agent, antioxidant, doping silicon dioxide, fretting map polymer successively It is added in high mixer, mixes 3-5 minutes, obtains grain powder mixture；
Step (2) uses equidirectional parallel double-screw extruder equipment, the draw ratio 44: 1~60: 1 of double screw extruder, preferably 48 : 1~52: 1, double screw extruder sets side forced feeding along extrusion direction Section 7 machine barrel, is set between Section 6 and Section 7 Thickness 3mm asbestos or polytetrafluoroethylene (PTFE) heat insulating mattress, along the screw combinations of 1~Section 6 machine barrel position in extrusion direction Take one kind in following a combinations, b combinations, three kinds of combinations of c combinations：
A is combined：36/36、36/36、X90/90、X90/90、GD90/45、56/56、56/56、90/5-45°、90/5-45°、56/ 56、90/5-45°、90/5-45°、56/56、90/5-45°、90/5-45°、56/56、56/5-45°、56/5-45°、48/4- 60°、48/5-90°、56/56、240/60、L240/60；
B is combined：36/36、36/36、X90/90、X90/90、GD90/45、56/56、90/5-45°、90/5-45°、56/56、90/ 5-45°、90/5-45°、C36/36、C36/36、90/5-45°、56/56、90/5-45°、56/5-45°、56/5-45°、56/56、 48/4-60°、48/5-90°、90/7-30°；
C is combined：36/36、36/36、62-X90/90、62-X90/90、62-GD90/45、90/5-45°、90/5-45°、CXL56/ 28、90/5-45°、62-CXL56/28、90/5-45°、90/5-45°、56/56、56/5-45°、56/5-45°、48/4-60°、 L56/28、90/7-30°、48/5-90°、56/56、C36/36、C36/36；
Section 1 machine barrel (the i.e. main feed opening) aperture position of step (3), special fibre along extrusion direction is rotated with extruder to be drawn Enter, while part grain powder mixture is added in Section 1 machine barrel (i.e. main feed opening) aperture position, by weighing the unit interval respectively The weight of the RPP material inside obtained and in the unit interval special fibre reduction Weight control special fibre with passing through The weight ratio that Section 1 machine barrel (i.e. main feed opening) aperture position adds both part grain powder mixtures is 1: 2；
Step (4), after debugging completes main feed opening special fibre and part grain powder mixture feeding ratio, remaining grain is mixed Mixture sets side forced feeding mouthful to feed by Section 7 machine barrel.Feeding is realized by adjusting the rotating speed of lateral feeding machine Ratio；
Step (5), in extrusion, the temperature of Section 1~Section 6 machine barrel position along extrusion direction is set as 110~130 ℃.Section 7 to die temperature is set as 180~220 DEG C；
Step (6), in extrusion, control extruder negative-pressure vacuum degree be not less than 0.05MPa；
Step (7), extrusion material strip are cooled down through tank, and control tank temperature is no more than 25 DEG C, are crossed water length and are not less than 15m, it is ensured that The surface temperature of material strip road pelleter mouthful after entering is less than 35 DEG C, and a kind of special fibre enhancing poly- third is obtained through pelleter pelletizing Alkene material.
2. the preparation method of a kind of polypropylene material according to claim 1, it is characterised in that also including a step：
Step (8), in extrusion can also by gas phase assistant formation equipment, at the mouth mold of double screw extruder inject Overcritical N2、CO2、H2One kind in inert gas, prepares the polypropylene material of fretting map.
3. a kind of preparation method of polypropylene material according to claim 1 or claim 2, described special fibre list 0.5~0.8mm of silk diameter.
4. a kind of preparation method of polypropylene material according to claim 1 or claim 2, described doping titanium dioxide Silicon is a kind of and boron doped silica silicon dioxide compositions in fluorine doped silica, and its mixing ratio is 2: 1.
5. a kind of preparation method of polypropylene material according to claim 1 or claim 2, described polypropylene exists Melt flow rate (MFR) is 10~100g/10min highly crystalline HOPP or block copolymerization polypropylene under 230 DEG C/2.16Kg At least one of, wherein the comonomer of block copolymerization polypropylene is ethene, and contents of ethylene is 5~8mol%；It is highly crystalline The crystallinity of HOPP is not less than 80%, isotacticity not less than 95%.
6. a kind of preparation method of polypropylene material according to claim 1 or claim 2, described compatilizer is horse Carry out the content 10~60% of the polyacrylic copolymer of acid anhydrides, wherein maleic anhydride.
7. a kind of preparation method of polypropylene material according to claim 1 or claim 2, described antioxidant is 1.3.5- three (3,5- di-t-butyls, 4- hydroxybenzyls) s-triazine (3114), 4.4 '-thiobis (the 6- tert-butyl group -3- methylbenzenes Phenol) (300), thio-2 acid two (18) ester (DSTP) and three [2.4- di-tert-butyl-phenyls] phosphite esters (168) are according to matter Amount carries out compounding use than 1: 1: 2: 1.
8. a kind of preparation method of polypropylene material according to claim 1 or claim 2, described coupling agent is silicon One kind in alkane coupling agent, aluminate coupling agent, titanate coupling agent.
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