CN101717580A - High-performance polyphenylene sulfide insulating composite material and preparation method thereof - Google Patents
High-performance polyphenylene sulfide insulating composite material and preparation method thereof Download PDFInfo
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- CN101717580A CN101717580A CN200910265048A CN200910265048A CN101717580A CN 101717580 A CN101717580 A CN 101717580A CN 200910265048 A CN200910265048 A CN 200910265048A CN 200910265048 A CN200910265048 A CN 200910265048A CN 101717580 A CN101717580 A CN 101717580A
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- 239000004734 Polyphenylene sulfide Substances 0.000 title claims abstract description 53
- 229920000069 polyphenylene sulfide Polymers 0.000 title claims abstract description 53
- 239000002131 composite material Substances 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 230000008878 coupling Effects 0.000 claims abstract description 27
- 238000010168 coupling process Methods 0.000 claims abstract description 27
- 238000005859 coupling reaction Methods 0.000 claims abstract description 27
- 230000002209 hydrophobic effect Effects 0.000 claims abstract description 19
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 19
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000003365 glass fiber Substances 0.000 claims abstract description 15
- 239000000463 material Substances 0.000 claims abstract description 12
- 238000012545 processing Methods 0.000 claims abstract description 11
- 238000011282 treatment Methods 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims abstract description 5
- 238000005469 granulation Methods 0.000 claims abstract description 5
- 230000003179 granulation Effects 0.000 claims abstract description 5
- 239000011256 inorganic filler Substances 0.000 claims abstract description 5
- 229910003475 inorganic filler Inorganic materials 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 5
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical group [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 37
- 239000007822 coupling agent Substances 0.000 claims description 26
- 239000012764 mineral filler Substances 0.000 claims description 24
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 19
- 239000013078 crystal Substances 0.000 claims description 19
- 238000000034 method Methods 0.000 claims description 16
- 239000010445 mica Substances 0.000 claims description 13
- 229910052618 mica group Inorganic materials 0.000 claims description 13
- 239000000843 powder Substances 0.000 claims description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 8
- -1 siloxanes Chemical class 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 4
- 238000013019 agitation Methods 0.000 claims description 4
- 238000007580 dry-mixing Methods 0.000 claims description 4
- 238000011068 loading method Methods 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 238000006557 surface reaction Methods 0.000 claims description 4
- 238000005303 weighing Methods 0.000 claims description 4
- 239000011521 glass Substances 0.000 claims description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 2
- 239000003513 alkali Substances 0.000 claims description 2
- 150000004645 aluminates Chemical class 0.000 claims description 2
- 229920001296 polysiloxane Polymers 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims description 2
- 239000004408 titanium dioxide Substances 0.000 claims description 2
- 229920005989 resin Polymers 0.000 abstract description 8
- 239000011347 resin Substances 0.000 abstract description 8
- 238000004381 surface treatment Methods 0.000 abstract description 6
- 238000005516 engineering process Methods 0.000 abstract description 4
- 239000000203 mixture Substances 0.000 abstract description 3
- 238000002844 melting Methods 0.000 abstract 1
- 230000008018 melting Effects 0.000 abstract 1
- 239000011159 matrix material Substances 0.000 description 12
- 150000001875 compounds Chemical class 0.000 description 3
- 239000012774 insulation material Substances 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 239000004033 plastic Substances 0.000 description 3
- 229920003023 plastic Polymers 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 239000011810 insulating material Substances 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 229920006389 polyphenyl polymer Polymers 0.000 description 2
- 150000003568 thioethers Chemical class 0.000 description 2
- 229910017083 AlN Inorganic materials 0.000 description 1
- 239000005995 Aluminium silicate Substances 0.000 description 1
- PIGFYZPCRLYGLF-UHFFFAOYSA-N Aluminum nitride Chemical compound [Al]#N PIGFYZPCRLYGLF-UHFFFAOYSA-N 0.000 description 1
- 235000012211 aluminium silicate Nutrition 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 229920006351 engineering plastic Polymers 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000005543 nano-size silicon particle Substances 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
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Abstract
The invention discloses a high-performance polyphenylene sulfide insulating composite material and a preparation method thereof. The high-performance polyphenylene sulfide insulating composite material comprises the following components in percentage by weight: 59 percent of polyphenylene sulfide, 30 percent of glass fibers, 1-10 percent of inorganic filler after coupling surface treatment and 1-5 percent of hydrophobic nano-silica. The preparation method comprises the following steps of: throwing polyphenylene sulfide resins, the inorganic filler after the coupling surface treatment and the hydrophobic nano-silica into a feed hopper of a twin-screw extruder after being uniformly mixed; adding the glass fibers from a side feeding hole; controlling the rotational speed of screws at 70-100rpm; processing the temperature of each region from 250 DEG C to 330 DEG C with the residence time of 2min and the die orifice pressure of 5MPa; and carrying out the treatments of melting, extruding and water cooling on the mixture and pulling the mixture to a dicer cutter for granulation. The invention has the advantages of high and stable mechanical performance and insulating performance of the materials, simple processing technology, wide material application field and the like.
Description
Technical field
The invention belongs to polymer composite, especially polyphenylene sulfide insulating composite material is made the field.
Background technology
Polyphenylene sulfide (be called for short PPS) claims polyphenylene sulfide, poly-phenylene thioether again, is a kind of thermoplastic engineering plastic of excellent combination property, and its outstanding feature is high temperature resistant, corrosion-resistant, radiation hardness, do not fire, mechanical property and electrical property excellence.Be mainly used in automobile making, electronic apparatus, mechanical industry, chemical industry instrument and space industry etc.But because the PPS rigidity is strong, performance is crisp, impelling strength is not high, application is restricted, and the PPS product of practical application all is to pass through modification.Though the PPS material of modification has certain insulating property, in air, expose to the open air for a long time or (as: hot and humid condition) use in particular environment, resistance value can descend very fast, and for example: PPS matrix material volume specific resistance under normal conditions is 10
17Ω .m, surface resistivity are 10
14Ω, but in the environment of 95 ℃ of temperature, humidity 90% the resistivity several magnitude that descends rapidly, this certainly will influence the PPS matrix material and be applied in hot and humid insulating material field.
At present, it is mainly compound based on machinery to prepare the method for PPS matrix material.The machinery complex method is meant the insulation modified filler is filled in the plastics in the mode of mechanical blending and goes that the main insulation modified filler of using has mica, nano silicon, aluminium nitride, kaolin, nano-calcium carbonate, calcium carbonate crystal whisker, calcium sulfate crystal whiskers, glass microballon etc.The insulating material that this mechanical recombining process is just simply crossed coupling agent treatment adds in the plastics and disperses, fusion in forcing machine then, extrude, obtain the polyphenyl thioether composite material of modification at last, cause product in actual applications, under particularly long-term exposed to air or process high temperature, the super-humid conditions, insulating property significantly descend.
Above shortcoming in view of prior art the objective of the invention is, and studies a kind of high-performance polyphenylene sulfide insulating composite material preparation method, makes it overcome the above shortcoming of prior art.
The present invention also aims to develop a kind of high-performance polyphenylene sulfide insulating composite material, make it to have that mechanical property and insulativity are high and stable, complete processing is easy, material Application Areas advantage widely.
Summary of the invention,
The high-performance polyphenylene sulfide insulating composite material preparation method, its raw material composition is by weight ratio: polyphenylene sulfide 59%, glass fibre 30% is through coupling surface-treated mineral filler 1～10%, hydrophobic nano-silica 1～5%; Technology comprises following key step:
1) the coupling surface treatment of mineral filler: 10～20min is fully soaked in mineral filler in the mixing solutions of coupling agent, dehydrated alcohol, 30～50 ℃ of treatment temps, make and the abundant and inorganic filler surface reaction of coupling agent obtain the mineral filler of described coupling surface-treated through hot-air dry; Wherein three's proportioning is: 70～80% mineral filler, 1～2.5% coupling agent, 10～20% dehydrated alcohol;
2) taking by weighing polyphenylene sulfide and 1 by weight ratio) mineral filler of coupling surface-treated and hydrophobic nano-silica put into high-speed mixer for dry mixing 5～10 minutes together, the control stirring velocity is 1000～2000rpm, and the agitation vat temperature is 30～50 ℃;
3) with step 2) in mixed material put in the loading hopper of twin screw extruder; glass fibre is added by the side spout; control screw speed 70～100rpm; processing is respectively distinguished temperature from 250～330 ℃; residence time 2min; die orifice pressure is 5MPa, through melt extrude, water cooling, be drawn to the dicing machine granulation.
Adopt technical scheme of the present invention, have following beneficial effect:
1, the present invention adopts novel insulating packing p-poly-phenyl thioether matrix material to carry out filling-modified, new insulation material is uniformly dispersed in the polyphenylene sulfide matrix resin, insulativity is high and stable, and characteristics such as addition is few, easily compound, easy processing, Application Areas are extensive.
When 2, the present invention improves insulated with material, also improve the toughness of polyphenylene sulfide, improved the mechanical property such as bending, stretching of matrix material.
3, the preparation technology of the high electric-insulating polyphenyl thioether matrix material of the present invention's proposition is simple, and can satisfy the processing requirement of plastic shapings processing such as injection moulding, extrusion molding or mold pressing repeatedly, can be widely used in fields such as electronic product, Communication Equipment, safety precaution.
Description of drawings
Fig. 1 is a process route chart of the present invention.
Fig. 2 is an embodiment of the invention material property table.
Embodiment
Below in conjunction with accompanying drawing process of the present invention is described in further detail.
As shown in Figure 1, the coupling surface treatment of mineral filler: 10～20min is fully soaked in mineral filler in the mixing solutions of coupling agent, dehydrated alcohol, 30～50 ℃ of treatment temps, make and the abundant and inorganic filler surface reaction of coupling agent behind hot-air dry, obtain the mineral filler of described coupling surface-treated; Wherein three's proportioning is: 70～80% mineral filler, 1～2.5% coupling agent, 10～20% dehydrated alcohol; Mineral filler is calcium carbonate crystal whisker or is that calcium carbonate crystal whisker and two kinds of mica powders are compound.Used mica powder is a mica powder of wet process, and radius-thickness ratio is 80～120, and its coupling surface treatment method is consistent with the processing of calcium carbonate crystal whisker.Used calcium carbonate crystal whisker mean length 30～40 μ m, length-to-diameter ratio 20～50.Coupling agent is at least a in titanate coupling agent, aluminate coupling agent, the siloxanes coupling agent, is preferably the siloxanes coupling agent.
Take by weighing polyphenylene sulfide and the mineral filler of above coupling surface-treated and hydrophobic nano-silica by weight ratio and put into high-speed mixer for dry mixing 5～10min together, the control stirring velocity is 1000～2000rpm, and the agitation vat temperature is 30～50 ℃.Wherein, the polyphenylene sulfide weight-average molecular weight is 50000, and chloride ion content is below 1000ppm; As nanometer titanium dioxide silicone content 96% in the hydrophobic nano-silica of new insulation material interpolation, median size is at 13～16nm.
At last above-mentioned mixed material is put in the loading hopper of twin screw extruder; glass fibre (adopting the non-alkali glass macrofiber) adds by extruding the pusher side spout; control screw speed 70～100rpm; processing is respectively distinguished temperature from 250～330 ℃; residence time 2min; die orifice pressure is 5MPa, through melt extrude, water cooling, be drawn to the dicing machine granulation.
Coupling agent all adopts siloxanes coupling agent KH-550 in following examples.
In the present embodiment 1, described high-performance PPS insulating composite material has comprised 59% PPS resin, 30% glass fibre, 10% coupling surface-treated calcium carbonate crystal whisker, 1% hydrophobic nano-silica.Implementing process is as follows:
The coupling surface treatment of mineral filler: calcium carbonate crystal whisker is fully soaked into 15min in the mixing solutions of siloxanes coupling agent KH-550, dehydrated alcohol, 40 ℃ of treatment temps, make and the abundant and calcium carbonate crystal whisker surface reaction of coupling agent KH-550 behind hot-air dry, obtain described coupling surface-treated calcium carbonate crystal whisker; Wherein three's proportioning is: 80% mineral filler, 2% coupling agent, 18% dehydrated alcohol.
Take by weighing polyphenylene sulfide and above coupling surface-treated calcium carbonate crystal whisker and hydrophobic nano-silica by weight ratio and put into high-speed mixer for dry mixing 5min together, the control stirring velocity is 1500rpm, and the agitation vat temperature is 40 ℃.
At last above-mentioned mixed material is put in the loading hopper of twin screw extruder, glass fibre adds by extruding the pusher side spout, control screw speed 90rpm; processing is respectively distinguished temperature and is: a district is 250 ℃, and two districts are 280 ℃, and three districts are 300 ℃; four districts are 300 ℃; five districts are 295 ℃, and six districts are 290 ℃, and head is 285 ℃; residence time 2min; die orifice pressure is 5MPa, through melt extrude, water cooling, be drawn to the dicing machine granulation.
Embodiment 2:
In the present embodiment 2, described high-performance PPS insulating composite material has comprised 59% PPS resin, 30% glass fibre, 8% coupling surface-treated calcium carbonate crystal whisker, 2% coupling surface-treated mica powder, 1% hydrophobic nano-silica.Implementing process is with described in the embodiment 1.
Embodiment 3:
In the present embodiment 3, described high-performance PPS insulating composite material has comprised 59% PPS resin, 30% glass fibre, 5% coupling surface-treated calcium carbonate crystal whisker, 5% coupling surface-treated mica powder, 1% hydrophobic nano-silica.Implementing process is with described in the embodiment 1.
Embodiment 4:
In the present embodiment 4, described high-performance PPS insulating composite material has comprised 59% PPS resin, 30% glass fibre, 5% coupling surface-treated calcium carbonate crystal whisker, 4% coupling surface-treated mica powder, 2% hydrophobic nano-silica.Implementing process is with described in the embodiment 1.
Embodiment 5:
In the present embodiment 5, described high-performance PPS insulating composite material has comprised 59% PPS resin, 30% glass fibre, 5% coupling surface-treated calcium carbonate crystal whisker, 3% coupling surface-treated mica, 3% hydrophobic nano-silica.Implementing process is with described in the embodiment 1.
Embodiment 6:
In the present embodiment 6, described high-performance PPS insulating composite material has comprised 59% PPS resin, 30% glass fibre, 5% coupling surface-treated calcium carbonate crystal whisker, 2% coupling surface-treated mica powder, 4% hydrophobic nano-silica.Implementing process is with described in the embodiment 1.
Performance test:
Prepared high-performance polyphenylene sulfide insulating composite material, its tensile strength is tested according to GB GB/T 1040; Its flexural strength and modulus in flexure are tested by GB GB 9341/T; Its notched Izod impact strength is tested by GB/T 1043; Its surface resistivity and volume specific resistance are tested according to GB GB/T 1410-2006.
Fig. 2 is seen in the contrast of embodiment 1～6 prescription and material property: go up tabulation embodiment 1～3 as can be seen by figure, the combination of mineral filler can obviously improve the mechanical property of PPS matrix material, increase along with mica powder in the mineral filler, insulating property under the matrix material normality condition improve, but at hot and humid condition lower surface resistivity and volume specific resistance 2～4 orders of magnitude that still will descend.Can see among the embodiment 4～6, raising along with new insulation material hydrophobic nano-silica content, the insulating property of PPS matrix material obviously improve, but the adding of excessive hydrophobic nano-silica causes the mechanical property of matrix material to reduce, and insulating property do not reach optimum value yet.When mineral filler and hydrophobic nano-silica proportioning reached shown in the embodiment 5, the insulating property of matrix material under normality and hot and humid condition reached optimum value, and have kept higher mechanical property.
Claims (9)
1. high-performance polyphenylene sulfide insulating composite material preparation method, its raw material is formed and is by weight ratio: polyphenylene sulfide 59%, glass fibre 30%, coupling surface-treated mineral filler 1～10%, hydrophobic nano-silica 1～5%; Comprise following key step:
1) 10～20min is fully soaked in untreated mineral filler in the mixing solutions of coupling agent, dehydrated alcohol, 30～50 ℃ of treatment temps, make and the abundant and inorganic filler surface reaction of coupling agent obtain the mineral filler of described coupling surface-treated through hot-air dry again.Wherein three's proportioning is: 70～80% mineral filler, 1～2% coupling agent, 10～20% dehydrated alcohol;
2) taking by weighing polyphenylene sulfide and 1 by weight ratio) mineral filler of coupling surface-treated and hydrophobic nano-silica put into high-speed mixer for dry mixing 5～10min together, the control stirring velocity is 1000～2000rpm, and the agitation vat temperature is 30～50 ℃;
3) with step 2) in mixed material put in the loading hopper of twin screw extruder; glass fibre is added by the side spout; control screw speed 70～100rpm; processing is respectively distinguished temperature from 250～330 ℃; residence time 2min; die orifice pressure is 5MPa, through melt extrude, water cooling, be drawn to the dicing machine granulation.
2. the high-performance polyphenylene sulfide insulating composite material preparation method according to claim 1 is characterized in that described polyphenylene sulfide weight-average molecular weight is 50000, and chloride ion content is below 1000ppm; Described glass fibre is the non-alkali glass macrofiber.
3. the high-performance polyphenylene sulfide insulating composite material preparation method according to claim 1 is characterized in that described mineral filler is a calcium carbonate crystal whisker.
4. the high-performance polyphenylene sulfide insulating composite material preparation method according to claim 1 is characterized in that described mineral filler is calcium carbonate crystal whisker and mica powder.
5. the high-performance polyphenylene sulfide insulating composite material preparation method according to claim 1 is characterized in that, nanometer titanium dioxide silicone content 96% in the described hydrophobic nano-silica, and median size is at 13～16nm.
6. the high-performance polyphenylene sulfide insulating composite material preparation method according to claim 1 is characterized in that, described coupling agent is a kind of in titanate coupling agent, aluminate coupling agent, the siloxanes coupling agent.
7. the high-performance polyphenylene sulfide insulating composite material preparation method according to claim 4 is characterized in that described mica powder is a mica powder of wet process, and radius-thickness ratio is 80～120; Described calcium carbonate crystal whisker mean length 30～40 μ m, length-to-diameter ratio 20～50.
8. the high-performance polyphenylene sulfide insulating composite material preparation method according to claim 1 is characterized in that described coupling agent is preferably the siloxanes coupling agent.
9. a high-performance polyphenylene sulfide insulating composite material is characterized in that, this material is made by the method for claim 1 or 2 or 3 or 4 or 5 or 6 or 7 or 8.
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