CN104987659A - Heat-resistant antistatic conductive polymer composite material and preparation method therefor and application thereof - Google Patents
Heat-resistant antistatic conductive polymer composite material and preparation method therefor and application thereof Download PDFInfo
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- CN104987659A CN104987659A CN201510483664.2A CN201510483664A CN104987659A CN 104987659 A CN104987659 A CN 104987659A CN 201510483664 A CN201510483664 A CN 201510483664A CN 104987659 A CN104987659 A CN 104987659A
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Abstract
The present invention provides a heat-resistant antistatic conductive polymer composite material and a preparation method therefor and application thereof. The composite material comprises the following compositions in percentage by mass: 30-60% of polyether-ether-ketone (PEEK); 30-60% of polyphenylene sulfide (PPS); 1-10% of carbon nanotubes (CNT); and 1-10% of conductive carbon black. According the present invention, the PEEK, PPS, CNT and conductive carbon black are optimally combined, and particles in different size stack together compactly to form an interlocked and controllable net structure, so the mechanical property can be guaranteed; the antistatic requirement of lower than 1012 ohm.cm is met with lower content of the conductive additive; the conductive requirement of 108 ohm.cm is met with appropriate carbon material content; and recycling and reuse of the PEEK material are implemented. According the invention, the physical blending-injection molding method used to obtain the composite material and is simpler and more adjustable than the melt blending-injection molding method in the prior art.
Description
Technical field
The invention belongs to conductive polymers technical field, more specifically, relate to conducting polymer composite material of a kind of high-temperature resistant and antistatic and its preparation method and application.
Background technology
Polyether-ether-ketone (PEEK) is a kind of high-performance crystallinity special engineering plastics, performance is similar to polyphenylene sulfide (PPS), it has the physical and chemical performances such as high temperature resistant, corrosion-resistant, and there is excellent mechanical property and electrical property, be widely used in aerospace, the fields such as field such as automotive industry, electric and medicine equipment.High melting temperature and high viscosity make PEEK forming process difficulty, and its waste material is block particle, and difficulty is processed again, and it is high to take out the difficult energy consumption of grain, is not easy to recycle.
PPS fragility is large, the processing of PEEK difficulty, and application is very restricted, at present existing correlative study, both composite modified good mechanical properties co-mixing systems that can obtain, but its conductivity after compound still can not satisfy the demands.
Therefore, the present invention is directed to above-mentioned deficiency, further expand it at high-temperature resistant and antistatic, and the application in conductivity higher material field.
Summary of the invention
The present invention, according to the deficiency in current conducting polymer materials, provides a kind of conducting polymer composite material of high-temperature resistant and antistatic.
Another object of the present invention is to the preparation method and application that above-mentioned conducting polymer composite material is provided.
Technical purpose of the present invention is achieved through the following technical solutions:
The invention provides a kind of conducting polymer composite material of high-temperature resistant and antistatic, comprise following component by mass percentage:
Polyether-ether-ketone 30-60%
Polyphenylene sulfide 30-60%
Carbon nanotube 1-10%
Graphitized carbon black 1-10%.
The present invention PEEK powder and PPS powder blended, and add carbon nanotube (CNT) and graphitized carbon black and make matrix material form the controlled network morphology of interlocking, thus improve the conductivity of co-mixing system.The multi-component collocation of the present invention and many particle diameters pile up the interface making conducting particles be in polymer particle, set up matrix material interlocking controllable network form, thus reach good conductivity, can be used as antistatic and electro-conductive material and use.
Preferably, described conducting polymer composite material comprises following component by mass percentage:
Polyether-ether-ketone 35-60%
Polyphenylene sulfide 35-60%
Carbon nanotube 2-8%
Graphitized carbon black 2-8%.
More preferably, described conducting polymer composite material comprises following component by mass percentage:
Polyether-ether-ketone 56%
Polyphenylene sulfide 36%
Carbon nanotube 3%
Graphitized carbon black 5%.
Preferably, the order number of described polyether-ether-ketone is 150 ~ 300 orders, and the order number of described polyphenylene sulfide is 80 ~ 120 orders; The particle diameter of described carbon nanotube is 20 ~ 40nm, and the particle diameter of described conductive carbon black is 15 ~ 30nm.
Preferably, the order number of described polyether-ether-ketone is 200 orders, and the order number of described polyphenylene sulfide is 100 orders; The particle diameter of described carbon nanotube is 30nm, and the particle diameter of described conductive carbon black is 20nm.
The present invention with 200 object PEEK powder and 100 object PPS powder blended, and the graphitized carbon black of the carbon nanotube (CNT) and 20nm that add 30nm makes matrix material form the controlled network morphology of interlocking, thus improving the conductivity of co-mixing system, its volume specific resistance reaches 4.5*10
4, prior art of comparing prepares little 4 ~ 6 orders of magnitude of volume specific resistance of PEEK matrix material, demonstrates the conductivity that it is outstanding.
The preparation method of the conducting polymer composite material of high-temperature resistant and antistatic of the present invention, comprises the steps:
S1. carry out dispersion treatment to carbon nanotube: mixed with concentrated acid by carbon nanotube, after reflux, washing and filtering, dries;
S2. carry out surface modification to conductive carbon black: mixed with ammonium persulfate solution by conductive carbon black, ultrasonic post-heating stirs, and washing is dry;
S3. polyether-ether-ketone and polyphenylene sulfide are tentatively mixed in mixing machine, and slowly add the graphitized carbon black processed in the carbon nanotube and S2 step of dispersion treatment in S1 step, after injection moulding, namely obtain described conducting polymer composite material.
Polymer composites is without twin screw extruder, and direct injection moulding, preparation method is more simple, and the modification of the low PPS powder of viscosity makes PEEK easily process and reclaim.
Preferably, in described S1, nitration mixture is the dense H of volume ratio 1:1
2sO
4with dense HNO
3, described return time is 0.5 ~ 1h.
Preferably, in described S2, ultrasonic time is 2 ~ 4h, and Heating temperature is 340 ~ 360 DEG C, and churning time is 16 ~ 20h.
Preferably, in described S3, injection temperature is 360 ~ 380 DEG C.
Compared with prior art, the present invention has following beneficial effect:
The present invention adopts PEEK, PPS, CNT and graphitized carbon black optimization collocation, and different-grain diameter is closely piled up, and can form the network morphology that interlocking is controlled, while guarantee mechanical property, under lower conductive additive content, realizes 10
12the antistatic requirement of below Ω ㎝, under suitable carbon material content, realize 10
8the conduction of Ω ㎝ requires (volume specific resistance prepares little 4 ~ 6 orders of magnitude of the volume specific resistance of PEEK matrix material than prior art), meet the recycling requirement of PEEK simultaneously.Adopt physical blending-injection moulding of the present invention method obtain matrix material, than prior art melt blending-injection molding forming method obtain matrix material preparation on more simple, controllability is higher.The conducting polymer composite material of high-temperature resistant and antistatic provided by the invention, in aerospace, automotive industry, electric and medical instruments field, possess application prospect widely.
Accompanying drawing explanation
The conducting polymer composite material form schematic diagram of the high-temperature resistant and antistatic that Fig. 1 provides for the embodiment of the present invention 1.
Embodiment
Below by embodiment, the present invention is specifically described; what be necessary to herein means out is that the present embodiment is only used to further illustrate the present invention; but can not be interpreted as limiting the scope of the invention, the person skilled in the art in this field can make some nonessential improvement and adjustment according to the content of the invention described above.
Unless stated otherwise, the present invention adopts reagent, method and apparatus are the art conventional reagent, method and apparatus.
Volume specific resistance: adopt EST121 type numeral ultra-high resistance, micro current instrument, according to GB/T1410-2006 test
Shock strength: adopt shock-testing machine, according to GB/T1043 test
Tensile strength: adopt universal testing machine, according to ASTM/D638 test
Flexural strength: adopt universal testing machine, according to ASTM/D790 test
embodiment 1:
Carry out proportioning according to each component concentration of embodiment in table 11, wherein preparation process is as follows:
S1. the dispersion treatment of carbon nanotube: CNT powder is positioned over 500ml balloon, measures excessive dense H
2sO
4dense HNO
3mixed solution (volume ratio H
2sO
4: HNO
3=3:1) pour in balloon until flood powder completely, on insert the prolong of recirculated water, heat in electric mantle, acid solution boiling reflux is made under the condition of logical water coolant, continue 0.5h, it is neutral for then under the condition vacuumized, carrying out washing and filtering to pH value with place mat every the ceramic funnel of pore membrane, dries at being positioned in baking oven DEG C.
S2. the surface modification of graphitized carbon black: be positioned over by graphitized carbon black in 500ml balloon, measure excessive ammonium persulfate aqueous solution and pour into until flood powder completely in balloon, ultrasonic 3h, stirs 18h at 350 DEG C of lower magnetic forces, centrifuge washing, vacuum-drying 24h.
S3. the preparation of conducing composite material: after dried PEEK powder and PPS powder are tentatively mixed in high-speed mixer, the graphitized carbon black of CNT and the S2 process through S1 dispersion treatment is slowly added on mixing limit, limit inward, and then at injection moulding machine 370 DEG C, injection moulding obtains conducing composite material.
Wherein, the particle diameter of PEEK powder, PPS powder, CNT, graphitized carbon black is respectively 200 orders, 100 orders, 30nm, 20nm.
As shown in Figure 1, the conducting polymer composite material form schematic diagram of the high-temperature resistant and antistatic that the embodiment of the present invention 1 provides, wherein the particle diameter ratio PPS powder of PEEK powder is slightly large, the carbon material that CNT tubular structure and spherical graphitized carbon black composition conduction are formed, above-mentioned substance has been mixed to form the fine and close form of the controlled network of interlocking.
embodiment 2:
Preparation method is with embodiment 1, and component proportion is in table 1.
embodiment 3:
Preparation method is with embodiment 1, and component proportion is in table 1.
embodiment 4:
Preparation method is with embodiment 1, and component proportion is in table 1.
embodiment 5:
Preparation method is with embodiment 1, and component proportion is in table 1.
embodiment 6:
Preparation method is with embodiment 1, and component proportion is in table 1.
embodiment 7:
Preparation method is with embodiment 1, and component proportion is in table 1, and wherein, the particle diameter of PEEK powder, PPS powder, CNT, graphitized carbon black is respectively 300 orders, 120 orders, 40nm, 30nm.
embodiment 8:
Preparation method is with embodiment 1, and component proportion is in table 1, and wherein, the particle diameter of PEEK powder, PPS powder, CNT, graphitized carbon black is respectively 150 orders, 80 orders, 20nm, 15nm.
embodiment 9:
Preparation method is with embodiment 1, and component proportion is with embodiment 6.Wherein, wherein, the particle diameter of PEEK powder, PPS powder, CNT, graphitized carbon black is respectively 200 orders, 100 orders, 20nm, 30nm.
comparative example 1:
Comparative example 1 adopts traditional preparation method: after PEEK pellet, PPS powder and carbon material just mix according to a certain percentage, melt blending at twin screw extruder 360 DEG C, extruding pelletization, blended pellet is dry 6h at 100 DEG C, the 370 DEG C of injection mouldings of rear injection moulding machine.
Its component proportion is in table 1.
comparative example 2:
Preparation method is with comparative example 1, and component proportion is in table 1.
comparative example 3:
Preparation method is with comparative example 1, and component proportion is with embodiment 6.Wherein, wherein, the particle diameter of PEEK powder, PPS powder, CNT, graphitized carbon black is respectively 100 orders, 200 orders, 30nm, 20nm.
comparative example 4:
Preparation method is with comparative example 1, and component particle diameter is with embodiment 1, and component proportion is PEEK powder in mass ratio: PPS powder: CNT=56:36:8, does not add conductive carbon black.
comparative example 5:
Preparation method is with comparative example 1, and component particle diameter is with embodiment 1, and component proportion is PEEK powder in mass ratio: PPS powder: conductive carbon black=56:36:8, does not add CNT.
Table 1
Embodiment 6 and embodiment 9 are due to the difference of carbon nanotube and graphitized carbon black particle diameter, larger on the volume specific resistance impact of the final electrically conductive composite formed.
And embodiment 7 and 8 is compared to other embodiments, its volume specific resistance exceeds several order of magnitude, and the component proportion showing specific order number and specific order number all exists larger impact to the conductivity of final material.
Because carbon nanotube particle diameter is less than graphitized carbon black particle diameter in comparative example 3, the more each embodiment inequality of its conductivity.
Comparative example 4 and 5 illustrates that the compound (cooperation of carbon nanotube and conductive carbon black) of carbon material of the present invention significantly can improve conductivity.
Above embodiment and comparative example prove again, the present invention adopts PEEK powder and the collocation of PPS powder of different-grain diameter size, and the former particle diameter need be larger than the latter, in its mixing, space is occupied by carbon material (carbon nanotube of specific proportioning and particle diameter and conductive carbon black), form the fine and close form of the controlled network of interlocking, directly after mixing, compression moulding is easy to obtain the good material of conductive network.Such particle diameter design, the matrix material prepared can be made to pile up tightr, closely pile up bubble-free when ensureing compression moulding, conductivity is better.
Claims (10)
1. a conducting polymer composite material for high-temperature resistant and antistatic, is characterized in that, comprises following component by mass percentage:
Polyether-ether-ketone 30-60%
Polyphenylene sulfide 30-60%
Carbon nanotube 1-10%
Graphitized carbon black 1-10%.
2. the conducting polymer composite material of high-temperature resistant and antistatic according to claim 1, is characterized in that, described conducting polymer composite material comprises following component by mass percentage:
Polyether-ether-ketone 35-60%
Polyphenylene sulfide 35-60%
Carbon nanotube 2-8%
Graphitized carbon black 2-8%.
3. the conducting polymer composite material of high-temperature resistant and antistatic according to claim 1, is characterized in that, described conducting polymer composite material comprises following component by mass percentage:
Polyether-ether-ketone 56%
Polyphenylene sulfide 36%
Carbon nanotube 3%
Graphitized carbon black 5%.
4. the conducting polymer composite material of the high-temperature resistant and antistatic according to claims 1 to 3 any one claim, is characterized in that, the order number of described polyether-ether-ketone is 150 ~ 300 orders, and the order number of described polyphenylene sulfide is 80 ~ 120 orders; The particle diameter of described carbon nanotube is 20 ~ 40nm, and the particle diameter of described conductive carbon black is 15 ~ 30nm.
5. the conducting polymer composite material of the high-temperature resistant and antistatic according to Claims 1-4 any one claim, is characterized in that, the order number of described polyether-ether-ketone is 200 orders, and the order number of described polyphenylene sulfide is 100 orders; The particle diameter of described carbon nanotube is 30nm, and the particle diameter of described conductive carbon black is 20nm.
6. a preparation method for the conducting polymer composite material of the high-temperature resistant and antistatic described in claim 1 to 5 any one claim, is characterized in that, comprises the steps:
S1. carry out dispersion treatment to carbon nanotube: mixed with concentrated acid by carbon nanotube, after reflux, washing and filtering, dries;
S2. carry out surface modification to conductive carbon black: mixed with ammonium persulfate solution by conductive carbon black, ultrasonic post-heating stirs, and washing is dry;
S3. polyether-ether-ketone and polyphenylene sulfide are tentatively mixed in mixing machine, and slowly add the graphitized carbon black processed in the carbon nanotube and S2 step of dispersion treatment in S1 step, after injection moulding, namely obtain described conducting polymer composite material.
7. the preparation method of the conducting polymer composite material of high-temperature resistant and antistatic according to claim 6, is characterized in that, in described S1, nitration mixture is the dense H of volume ratio 1:1
2sO
4with dense HNO
3, described return time is 0.5 ~ 1h.
8. the preparation method of the conducting polymer composite material of high-temperature resistant and antistatic according to claim 6, is characterized in that, in described S2, ultrasonic time is 2 ~ 4h, and Heating temperature is 340 ~ 360 DEG C, and churning time is 16 ~ 20h.
9. the preparation method of the conducting polymer composite material of high-temperature resistant and antistatic according to claim 6, is characterized in that, in described S3, injection temperature is 360 ~ 380 DEG C.
10. the conducting polymer composite material of the high-temperature resistant and antistatic described in claim 1 to 5 any one claim in aerospace, the application in automotive industry, electric and medical instruments field material.
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| CN105482454A (en) * | 2015-12-04 | 2016-04-13 | 暨南大学 | Polyphenylene ulfide/polyether ether ketone conductive composite material, and preparation method and application thereof |
| CN105504671A (en) * | 2015-12-31 | 2016-04-20 | 广东顺德鲁华光电新材料实业有限公司 | Antistatic polymer material as well as preparation method and application thereof |
| CN107603137A (en) * | 2017-10-18 | 2018-01-19 | 扬州大学 | A kind of semiconductive Polyether-ether-ketocable cable material and preparation method thereof |
| CN109096692A (en) * | 2018-05-30 | 2018-12-28 | 浙江德清科赛塑料制品有限公司 | A kind of antistatic PEEK resin material and preparation method thereof |
| US11118053B2 (en) | 2018-03-09 | 2021-09-14 | Ticona Llc | Polyaryletherketone/polyarylene sulfide composition |
| WO2024063490A1 (en) * | 2022-09-21 | 2024-03-28 | 롯데케미칼 주식회사 | Thermoplastic resin composition and molded article formed therefrom |
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