CN104877283A - Method for preparing anti-static carbon nanomaterial-polytetrafluoroethylene composite material - Google Patents
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/04—Ingredients characterised by their shape and organic or inorganic ingredients
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- 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
- B29C67/00—Shaping techniques not covered by groups B29C39/00 - B29C65/00, B29C70/00 or B29C73/00
- B29C67/02—Moulding by agglomerating
- B29C67/04—Sintering
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- C—CHEMISTRY; METALLURGY
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/30—Sulfur-, selenium- or tellurium-containing compounds
- C08K2003/3009—Sulfides
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- C08K2201/004—Additives being defined by their length
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- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/04—Antistatic
Abstract
The invention discloses a method for preparing an anti-static carbon nanomaterial-polytetrafluoroethylene composite material. The method comprises the following steps that after a carbon nanomaterial is dispersed in a liquid medium and then is mixed with polytetrafluoroethylene powder and other raw materials according to the mass percentage of 0.5%-2%, then the mixture is dried at the temperature ranging from 40 DEG C to 100 DEG C, the dried mixed material is placed in a mould, is extruded at the pressure ranging from 45 MPa to 70 MPa and is sintered at the temperature ranging from 360 DEG C to 385 DEG C, and then the anti-static carbon nanomaterial-polytetrafluoroethylene composite material is obtained. According to the method, only the low-content carbon nanomaterial needs to be introduced, the high conductivity of the carbon nanomaterial such as a grapheme or carbon nano tube and the dimensionality characteristic which can effectively constitute a conductive network are used, and a basic preparation method without changing a PTFE forming piece and a film material is provided, namely, the anti-static composite material low in surface resistivity can be prepared; meanwhile, benefiting from the toughness effect of the carbon nanomaterial, the mechanical property and the friction abrasion resistance of the composite material are not affected at all.
Description
technical field:
The present invention relates to a kind of preparation method of antistatic carbon nanomaterial-ptfe composite, be applied in the purposes such as packing film, antiadhesion barrier, self-lubricating parts, belong to resin base functional composite material field.
background technology:
Polytetrafluoroethylene (PTFE) is the (per) fluoropolymer that tetrafluoroethylene obtains through copolymerization, and its molecular chain is-[CF
2-CF
2]-, the molecular weight of tetrafluoroethylene is high, degree of crystallinity is higher, unbranched in molecular chain, carbon fluorine atom arrangement closely and the Z-shaped distortion of its atomchain, fluorine atom can play shielding effect to main chain, carbon-fluorine bond chemistry bond energy is high, due to its special construction and character, the hydrophobicity of tetrafluoroethylene, oleophobic property, resistivity against fire, chemical resistance, weathering resistance, dielectricity are all very good, and have lower frictional coefficient.Therefore, it is widely used in fields such as electronics, chemical industry, machinery, aviations, is often used as self-lubricating parts, corrosion-resistant heatproof substrate material, wrapping material, anti-stick coating etc.
But PTFE is as typical high dielectric property macromolecular material, and resistivity is high.PTFE film easily produces buildup of static electricity in the air of drying, causes adhesion of film, and may cause security incident occurs.Therefore, reduce the surface resistivity of PTFE, increase its static resistance, improve the use properties as packaging film, self-lubricating material etc., become and modification is carried out to PTFE material and expands the important technical of its Application Areas.
The metal-powders such as bronze powder are the composite modification materials of the most frequently used PTFE.Bronze powder not only can reduce the surface resistivity of material, also has obvious reinforcing effect to material, and the frictional coefficient of matrix material can reduce further simultaneously, and wear resistance can further improve.
Mineral filler application also can realize reducing the effect of material surface resistivity, as Graphite Powder 99, carbon fiber, carbon dust etc.But because the interface compatibility of mineral filler and PTFE matrix is often poor, inorganic materials more easily occurs from reuniting, and thus, obtain lower surface resistivity, the content of mineral filler often needs very high.Too high inorganic filler content often causes the decline of the strength of materials, toughness and wear resistance.
The nanometer of material and nano combinedization are the important channels realizing all kinds of excellent properties synthesization of material.When the powder granularity of PTFE is reduced to 2 ~ 50nm by Zhao Deyao etc. [Zhao Deyao: a kind of polytetrafluoroethylnanoscale nanoscale powder material and preparation method thereof, number of patent application is: 200910195197.8], achieve the decline of material friction coefficient and the lifting of anti-extreme pressure ability.Li Tongsheng [Li Tongsheng, Wang Hongyan, Lv Renguo: polytetrafluoroethylnano nano particle modified phenolic resin wear-resistant material and preparation method thereof, application number is: 201010540271.8] etc. application PTFE nano particle modified alkyd resin, the wear resistance of resol can be significantly improved, reduce frictional coefficient.Nano-scale carbon material also can carry out compound with PTFE.Mei Ju etc. [lift, Bao Chunrong: a kind of application of novel polytetrafluoroethylnano nano material by plum, application number is 201210199779.5] self-assembled film of composite carbon nanometer tube in the substrate of PTFE, be applied to artificial blood vessel, vascellum endometrial hyperplasia degree after implantation can be alleviated, improve unobstructed blood vessel rate.But the method being improved the antistatic property of PTFE by nanometer or composite Nano method is not all proposed in above-mentioned several document.
The present invention proposes by carbon nanomaterial compound, reduces the surface resistivity of PTFE, improves the method for its antistatic property, thus improves and expand the application performance in fields such as packing film, antiadhesion barrier, self-lubricating parts, can effectively take precautions against electrostatic safety problem.
summary of the invention:
Technical problem to be solved by this invention is: the preparation method providing a kind of antistatic carbon nanomaterial-ptfe composite, by introducing carbon nanotube, the graphene carbon nano material of low levels, anti-static composite material is obtained by the PTFE preparation method of routine, the high conductivity of these materials of carbon nanometer such as the method using mineral carbon alkene, carbon nanotube and efficiently can form the dimensional properties of conductive network, simultaneously due to the highly malleablized effect of carbon nanomaterial, mechanical property and the friction and abrasion of matrix material are not all affected.
The technical scheme that the present invention takes for technical solution problem is:
A preparation method for antistatic carbon nanomaterial-ptfe composite, its concrete preparation process is as follows:
A, disperseed in liquid medium by carbon nanomaterial, the consumption of carbon nanomaterial and liquid medium is 1 by its mass ratio: (40 ~ 100), obtain liquid mixture A;
B, by liquid mixture A and tetrafluoroethylene mixing, blending ratio by its mass ratio be (0.5 ~ 2): (98 ~ 99.5), obtain total mixture B;
C, total mixture B is dry under the temperature condition of 40 ~ 100 DEG C, obtain dry pack C;
D, dry pack C is placed in mould, suppresses under 45 ~ 70MPa, obtain sample green compact;
E, sample green compact are placed in sintering oven, under the sintering temperature of 370 ~ 385 DEG C, sinter 100 ~ 300 minutes, obtain antistatic carbon nanomaterial-ptfe composite.
In step, described carbon nanomaterial is one in carbon nanotube, Graphene or mixing, and described carbon nanomaterial can be passed through or without surface treatment.
In step, the dispersing method of described carbon nanomaterial in liquid medium is one in high speed shear, ultrasonic disperse or mixing; Described liquid medium is organic solvent.
In stepb, also can add other raw materials when liquid mixture A and tetrafluoroethylene mixing, other raw material described is one or several mixing in bronze powder, molybdenumdisulphide, Graphite Powder 99, carbon fiber; Blending ratio is as follows by its mass ratio, liquid mixture A: tetrafluoroethylene: other raw material=1:(10 ~ 14): (85 ~ 89).
In stepb, the blending means of described liquid mixture A and tetrafluoroethylene be ball milling, mixing tank mixing, stir in one or mixing.
In step e, described sintering is at N
2or carry out in Ar atmosphere.
Compared with prior art, technical superiority of the present invention is:
The method only need introduce the carbon material of low levels, the high conductivity of these materials of carbon nanometer such as using mineral carbon alkene, carbon nanotube and efficiently can form the dimensional properties of conductive network, do not change the basic preparation method of PTFE profiled member and mould material, the antistatic carbon nanomaterial-ptfe composite with low surface resistivity can be obtained.Meanwhile, benefit from the highly malleablized effect of carbon nanomaterial, mechanical property and the friction and wear behavior of matrix material are not affected.
embodiment:
embodiment 1:a preparation method for antistatic carbon nanomaterial-ptfe composite, its concrete steps are as follows:
The cloth pouch-type Graphene of the multi-walled carbon nano-tubes of diameter 10 ~ 30mm, length 1 ~ 100 μm and 1 ~ 6 layer, diameter 200 ~ 300nm is added in acetone according to the mass ratio of 1:4, solid-liquid mass ratio is 1:49, knife up speed decollator is pulverized with the ultrasonic dispersers ultrasonic disperse 30min of the dispersion of the VELOCITY SHEAR of 8000r/min 60min, rear frequency 40KHz, power 100W, volume 3L with stainless steel;
According to carbon nanomaterial: polytetrafluoroethylene (PTFE) mass ratio is the ratio of 1:99, above-mentioned carbon nanomaterial slurry is mixed with PTFE, stirs 30min with homogenizer, be placed in vacuum drying oven, at 50 DEG C, dry 60min.The mixing raw material of drying is proceeded in mould, pre-molding under 50MPa, obtain sample green compact; Green compact are left standstill 24 hours, fully to discharge internal stress, is then placed in sintering oven, sinter under an ar atmosphere, sintering temperature is 370 DEG C, and sintering time is 180min, obtains the antistatic carbon nanomaterial-ptfe composite prepared by the present invention after sintering.
Gained matrix material cuts, and can obtain carbon nanomaterial/polytetrafluoroethylene film that thickness is 0.2mm, the surface resistivity of this film is less than 1 × 10
6Ω, tensile strength is 15.6MPa, and elongation rate of tensile failure is 142%.
As a comparison, according to same process, apply the surface resistivity of pure polytetrafluoroethylene film prepared by identical tetrafluoroethylene raw material (PTFE) higher than 1 × 10
11Ω, tensile strength is 14.8MPa, and elongation rate of tensile failure is 136%.
embodiment 2: a kind of preparation method of antistatic carbon nanomaterial-ptfe composite, its concrete steps are as follows:
The multi-walled carbon nano-tubes of diameter 20 ~ 40mm, length 40 ~ 400 μm is added in dehydrated alcohol, solid-liquid mass ratio is 1:99, knife up speed decollator is pulverized with the ultrasonic dispersers ultrasonic disperse 45min of the dispersion of the VELOCITY SHEAR of 1200r/min 30min, rear frequency 40KHz, power 100W, volume 3L with stainless steel;
Get the multi-walled carbon nano-tubes of 3g diameter 20 ~ 40mm, length 40 ~ 400 μm, join (sulfuric acid, nitric acid volume ratio are 3:1), ultrasonic disperse 15min in 500ml mixed acid solution, then at room temperature magnetic agitation 24h, repeatedly clean with deionized water again, suction filtration, until pH is 7, by filter cake dry 24h in 80 DEG C of vacuum drying ovens, obtain carboxylation carbon nanotube; Getting a certain amount of dehydrating agent dicyclohexylcarbodiimide is dissolved in 150 ml dehydrated alcohols, the carboxylation carbon nanotube getting 2g again adds wherein, ultrasonic disperse 10min, the aqueous solution 150ml of Sulphanilic Acid is added again in system, in the water-bath of 50 DEG C, react 24h, then use ethanol, deionized water repetitive scrubbing, suction filtration, until pH is 7, obtain aminated carbon nano tube slurry.
According to carbon nanomaterial: PTFE mass ratio is the ratio of 0.5:99.5, mixed by above-mentioned carbon nanomaterial slurry with PTFE, in ball mill, ball milling 120min under 500r/min, is placed in vacuum drying oven, at 40 DEG C, dry 120min.The mixing raw material of drying is proceeded in mould, pre-molding under 45MPa, obtain sample green compact; Green compact are left standstill 24 hours, fully to discharge internal stress, is then placed in sintering oven, at N
2sinter under atmosphere, sintering temperature is 385 DEG C, and sintering time is 120min, obtains the antistatic carbon nanomaterial-ptfe composite prepared by the present invention after sintering.
Gained matrix material cuts, and can obtain carbon nanomaterial/polytetrafluoroethylene film that thickness is 0.2mm, the surface resistivity of this film is less than 1 × 10
7Ω, tensile strength is 16.1MPa, and elongation rate of tensile failure is 166%.
embodiment 3:a preparation method for antistatic carbon nanomaterial-ptfe composite, its concrete steps are as follows:
By thickness 0.8 ~ 1.2 μm (individual layer rate >80%), the graphene microchip 1g that diameter is 0.5 ~ 2 μm joins in 200g dehydrated alcohol, add the silane coupling agent KH570 of 1.5g again, knife up speed decollator is pulverized with the VELOCITY SHEAR of 1200r/min dispersion 30min with stainless steel, use the ultrasonic dispersers ultrasonic disperse 30min of frequency 40KHz, power 100W, volume 3L afterwards, obtain functionalization graphene slurry;
According to carbon nanomaterial: PTFE mass ratio is the ratio of 2:98, above-mentioned carbon nanomaterial slurry is mixed with PTFE, in V-type blender, mixes 18h, be placed in vacuum drying oven, at 100 DEG C, dry 30min; The mixing raw material of drying is proceeded in mould, pre-molding under 70MPa, obtain sample green compact; Green compact are left standstill 24 hours, fully to discharge internal stress, is then placed in sintering oven, sinter under an ar atmosphere, sintering temperature is 345 DEG C, and sintering time is 300min, obtains the antistatic carbon nanomaterial-ptfe composite prepared by the present invention after sintering.
The surface resistivity of gained matrix material is less than 5 × 10
5Ω, tensile strength is 12.2MPa, and elongation rate of tensile failure is 122%, is 0.12. with the dish pin friction wear testing machine frictional coefficient recorded under friction load 20N between this composite wood charging tray and 45# draw point of surface hardness 43HRC
As a comparison, according to same process, apply the surface resistivity of pure PTFE material prepared by identical PTFE raw material higher than 1 × 10
11Ω, tensile strength is 11.9MPa, and elongation rate of tensile failure is 109%, is 0.12 with the frictional coefficient that dish pin friction wear testing machine records between this pure PTFE dish and 45# draw point of surface hardness 43HRC under friction load 20N.
embodiment 4:a preparation method for antistatic carbon nanomaterial-ptfe composite, its concrete steps are as follows:
By the multi-walled carbon nano-tubes of diameter 10 ~ 30mm, length 1 ~ 100 μm and 1 ~ 6 layer, the cloth pouch-type Graphene of diameter 200 ~ 300nm is added in acetone according to the mass ratio of 1:4, solid-liquid mass ratio is 1:49, knife up speed decollator is pulverized with the ultrasonic dispersers ultrasonic disperse 30min of the dispersion of the VELOCITY SHEAR of 8000r/min 60min, rear frequency 40KHz, power 100W, volume 3L with stainless steel;
According to carbon nanomaterial: molybdenumdisulphide: bronze powder: PTFE mass ratio is the ratio of 1:3:9:87, above-mentioned carbon nanomaterial slurry is mixed with PTFE powder, in ball mill, ball milling 120min under 500r/min, be placed in vacuum drying oven, at 50 DEG C, dry 60min; The mixing raw material of drying is proceeded in mould, pre-molding under 50MPa, obtain sample green compact; Green compact are left standstill 24 hours, fully to discharge internal stress, is then placed in sintering oven, sinter under an ar atmosphere, sintering temperature is 370 DEG C, and sintering time is 180min, obtains the antistatic carbon nanomaterial-ptfe composite prepared by the present invention after sintering.
Prepared antistatic carbon nanomaterial-ptfe composite, obtains multiple profiled member by mechanical workouts such as sawing, turning, borings.The surface resistivity of gained matrix material is less than 1 × 10
6Ω, tensile strength is 16.3MPa, and elongation rate of tensile failure is 108%, is 0.11 with the frictional coefficient that dish pin friction wear testing machine records between this pure PTFE dish and 45# draw point of surface hardness 43HRC under friction load 20N.
As a comparison, according to same process, application same materials, according to molybdenumdisulphide: bronze powder: PTFE mass ratio be 3:9:88 prepare not containing the surface resistivity of PTFE matrix material of carbon nanomaterial higher than 1 × 10
10Ω, tensile strength is 16.0MPa, and elongation rate of tensile failure is 96%, is 0.12 with the frictional coefficient that dish pin friction wear testing machine records between this pure PTFE dish and 45# draw point of surface hardness 43HRC under friction load 20N.
Above-described embodiment is the present invention's preferably embodiment; but embodiments of the present invention are not restricted to the described embodiments; change, the modification made under other any does not deviate from spirit of the present invention and principle, substitute, combine, simplify; all should be the substitute mode of equivalence, be included in protection scope of the present invention.
Claims (6)
1. a preparation method for antistatic carbon nanomaterial-ptfe composite, its concrete preparation process is as follows:
A, disperseed in liquid medium by carbon nanomaterial, the consumption of carbon nanomaterial and liquid medium is 1 by its mass ratio: (40 ~ 100), obtain liquid mixture A;
B, by liquid mixture A and tetrafluoroethylene mixing, blending ratio by its mass ratio be (0.5 ~ 2): (98 ~ 99.5), obtain total mixture B;
C, total mixture B is dry under the temperature condition of 40 ~ 100 DEG C, obtain dry pack C;
D, dry pack C is placed in mould, suppresses under 45 ~ 70MPa, obtain sample green compact;
E, sample green compact are placed in sintering oven, under the sintering temperature of 370 ~ 385 DEG C, sinter 100 ~ 300 minutes, obtain antistatic carbon nanomaterial-ptfe composite.
2. the preparation method of antistatic carbon nanomaterial-ptfe composite according to claim 1, it is characterized in that: in step, described carbon nanomaterial is one in carbon nanotube, Graphene or mixing, and described carbon nanomaterial can be passed through or without surface treatment.
3. the preparation method of antistatic carbon nanomaterial-ptfe composite according to claim 1, it is characterized in that: in step, the dispersing method of described carbon nanomaterial in liquid medium is one in high speed shear, ultrasonic disperse or mixing; Described liquid medium is organic solvent.
4. the preparation method of antistatic carbon nanomaterial-ptfe composite according to claim 1, it is characterized in that: in stepb, also can add other raw materials when liquid mixture A and tetrafluoroethylene mixing, other raw material described is one or several mixing in bronze powder, molybdenumdisulphide, Graphite Powder 99, carbon fiber; Blending ratio is as follows by its mass ratio, liquid mixture A: tetrafluoroethylene: other raw material=1:(10 ~ 14): (85 ~ 89).
5. the preparation method of antistatic carbon nanomaterial-ptfe composite according to claim 1, it is characterized in that: in stepb, the blending means of described liquid mixture A and tetrafluoroethylene be ball milling, mixing tank mixing, stir in one or mixing.
6. the preparation method of antistatic carbon nanomaterial-ptfe composite according to claim 1, it is characterized in that: in step e, described sintering is at N
2or carry out in Ar atmosphere.
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| CN105924862A (en) * | 2016-06-07 | 2016-09-07 | 扬州大学 | Method for preparing composite polytetrafluoroethene conductive material |
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| CN106380762A (en) * | 2016-08-31 | 2017-02-08 | 温州赵氟隆有限公司 | Graphene and polytetrafluoroethylene composite material conductive belt and production method thereof |
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| CN111253699A (en) * | 2019-12-26 | 2020-06-09 | 江苏亿豪塑业股份有限公司 | Preparation process of polytetrafluoroethylene composite filler |
| CN113897005A (en) * | 2021-08-23 | 2022-01-07 | 宁波风盛新材料科技有限公司 | Production method of inner drainage pipe |
| CN116285172A (en) * | 2023-02-10 | 2023-06-23 | 南京肯特复合材料股份有限公司 | Conductive sealing material for hydraulic system of undercarriage and preparation method thereof |
| CN116355337A (en) * | 2023-06-01 | 2023-06-30 | 山东美氟科技股份有限公司 | Fluorine-containing polymer-carbon nano tube modified polytetrafluoroethylene and preparation process thereof |
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Cited By (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105924862A (en) * | 2016-06-07 | 2016-09-07 | 扬州大学 | Method for preparing composite polytetrafluoroethene conductive material |
| CN105924862B (en) * | 2016-06-07 | 2017-11-21 | 扬州大学 | A kind of preparation method of compound polytetrafluoroethylene (PTFE) conductive material |
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