CN109912924A - A kind of preparation of the composite modified filler of graphene-nanometer polytetrafluoroethylcomposite and its application method - Google Patents
A kind of preparation of the composite modified filler of graphene-nanometer polytetrafluoroethylcomposite and its application method Download PDFInfo
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Abstract
The invention discloses a kind of preparation of composite modified filler of graphene-nanometer polytetrafluoroethylcomposite and its application methods, the present invention carries out modified graphene with the spherical polytetrafluoroethylene packing of nanometer compound, it is using binder that nanometer spherical polytetrafluoroethylene (PTFE) and flake graphite alkene uniform filling is compound using the method for spray drying simultaneously, compounded mix obtained is allowed both to possess the wear-resisting property of graphene, again with the greasy property of nanometer polytetrafluoroethylcomposite, the compounded mix using when method also it is fairly simple only need to be added to together in polymeric matrix with a small amount of small molecule grease then stir evenly, then it is granulated by pelletizer, compared to the coefficient of friction and wear rate that existing material can effectively reduce material, and the mechanical property of material can be improved.
Description
Technical field
The present invention relates to new material technology fields, and in particular to a kind of graphene-nanometer polytetrafluoroethylcomposite is composite modified to be filled out
The preparation of material and its application method.
Background technique
With advances in technology and industrial expansion, automation equipment is more and more applied and all trades and professions at present, from
The process of dynamicization be unable to do without the operating and movement of component of machine mechanism, and component of machine is inevitable during operation
Friction, abrasion can occur.Research is pointed out, is rubbed and is consumed the non-renewable energy in 1/3 or more the world, and 60% component of machine
Damage is all therefore, to study wear-resisting lubricating composite as caused by wearing and have important practical significance, and develops a drop and wears away
The filler that rubs is particularly critical.And the primary study object that mill antifriction material is always tribological field drops, in real industry, life
It is chiefly used in being processed into transmission parts in work；Drop mill means the elongate member service life, improves resource utilization, and antifriction means to save
The energy reduces energy loss.And macromolecule polymer material can conveniently be processed into various shapes with its superior deformability characteristics
Shape, and have the advantages that conventional metals are incomparable in some aspects.
Currently, the drop in polymer, which wears away the filler that rubs, still mainly is limited to some conventional fillers, as graphite, molybdenum disulfide,
Polytetrafluoroethylene (PTFE) etc..These conventional fillers can improve certain tribological properties of polymer material to a certain extent, but it changes
It is apt to fairly limited, and it needs a large amount of fillings, this causes to significantly reduce to the mechanical performance of basis material.With traditional material phase
Than graphene has excellent mechanical property, in the case where few loading, Ji Kexian as a kind of two-dimension nano materials
The wearability for improving material is write, is a kind of efficient drop mill filler.But its greasy property is poor, needs to change graphene
Into making it have certain lubricating function.Polytetrafluoroethylene (PTFE) has excellent greasy property, and nanometer polytetrafluoroethylcomposite is added to
It can make composite material that there is preferable self-lubricating property in polymer.Therefore as can graphene and nanometer polytetrafluoroethylcomposite are carried out
It is compound, synergistic effect is played, then can be improved the lubricating and wear-resisting characteristic of polymer material.
Since graphene and nanometer polytetrafluoroethylcomposite are nanometer sized materials, it is added to conventional mechanical mixing poly-
It closes in object material, is easy to reunite, it is difficult to realize uniform and stable dispersion, therefore, effect is difficult to reach desirable level.Patent of invention
201410088554.1 point out, graphene and ptfe surface difference amination and carboxylated are handled, then pass through condensation
The covalent key connection that graphene and nanometer polytetrafluoroethylcomposite can be achieved is reacted, uniform graphene-nanometer polytetrafluoroethylcomposite is made
Compounded mix.Although this method can make graphene evenly dispersed with nanometer polytetrafluoroethylcomposite, it needs to introduce many chemistry examinations
Agent, environmental-protecting performance remain to be discussed, and complex process, and removal of impurities and reaction efficiency are low, are difficult to realize industrialized production at present.For
This is proposed it is proposed that a kind of drop the preparation for wearing away the composite modified filler of graphene-nanometer polytetrafluoroethylcomposite for function of rubbing and its answer
Use method
Summary of the invention
In view of the above existing problems in the prior art, the present invention provides a kind of easy to operate practical, effect it is obvious, it can be achieved that
The preparation of the composite modified filler of graphene-nanometer polytetrafluoroethylcomposite of large-scale production and its application method, by solving graphene
Dispersion with nanometer polytetrafluoroethylcomposite and problem is combined, the drop mill friction reduction characteristics of reisn base material can be effectively improved.
To solve the problems, such as the dispersion of graphene and nanometer polytetrafluoroethylcomposite and combining, the present invention proposes that a kind of graphene-is received
The preparation method of the rice composite modified filler of polytetrafluoroethylene (PTFE), particular content includes the following steps,
Step I takes graphene that deionized water is added, and heating stirring obtains solution A under water bath condition；
Step II takes coupling agent, ethyl alcohol, deionized water to be stirred to obtain solution B
Step III, solution A and solution B are mixed and carries out coupling reaction under conditions of water-bath, material surface is presented
Lipophilic out, cold filtration washing obtains graphene filler M modified；
Step IV, appropriate graphene filler M modified and nanometer polytetrafluoroethylcomposite is taken to be added to the mixing of water-ethanol
It is mixed in solution, and appropriate aqueous binders is added, carried out dispersion mixing, obtain emulsion N；
Step V, the dispersibility of emulsion N is maintained, and is dehydrated to obtain graphene-nanometer polytetrafluoroethylcomposite multiple
Close modified filler.
Preferably, in the step I each component weight ratio are as follows: 800 parts of deionized water, 10 parts of graphene, and water-bath
Temperature is 80 DEG C, and the graphene is powdered watersoluble plumbago alkene；
The weight ratio of each component in the step II are as follows: 2 parts of coupling agent, 15 parts of ethyl alcohol, 1 part of deionized water；
The weight ratio of solution A and solution B in the step III are as follows: 810 parts of solution A, 5 parts of solution B, and the coupling
The condition of reaction be 80 DEG C water-bath 3 hours.
Preferably, the coupling agent be one of organochromium complexes, silanes, titanate ester and aluminic acid compound or
Person is several.
Preferably, the weight ratio range of graphene filler M and polytetrafluoroethylene (PTFE) is 1:5 to 1:25 in the step IV.
Preferably, the aqueous binders in the step IV are polyethylene pyrrole network alkanone (PVP), polyvinyl alcohol (PVA), fourth
One or more of tetrol, and the weight content of the aqueous binders is that graphene-nanometer polytetrafluoroethylcomposite is composite modified
1%-the 5% of filler.
Preferably, the drying mode in the step V is spray drying, and the parameter of the spray drying is, mouth temperature
At 120-150 DEG C, charging rate is controlled in 10-25 atmospheric pressure, outlet temperature at 70-90 DEG C in 5%-35%, air pressure
In range.
Preferably, the mixed solution weight ratio of the water-ethanol in the step IV is 3 parts of water, 2 parts of ethyl alcohol.
The present invention improves a kind of application method of composite modified filler of graphene-nanometer polytetrafluoroethylcomposite, poly- in order to improve
Wear-resisting, the lubricity for closing object matrix, reduce the coefficient of friction and wear rate of material, the resulting graphene-nanometer of step V are gathered
The composite modified filler of tetrafluoroethene is added in polymeric matrix material with the weight ratio of 5%-30%, while weight point is added
Number is 0.1-1% small molecule grease, then by being stirred and obtaining graphene-nanometer polytetrafluoroethyl-ne by extruding pelletization
Composite granule is obtained the product of required structure using injection molding or hot pressing mode by the modified polymer composite granule of alkene.
Preferably, the small molecule grease is paraffin oil, and the polymeric matrix material is polyformaldehyde, nylon, polyethers
One or more of ether ketone, ultra-high molecular weight polyethylene.
The beneficial effects of the present invention are: the present invention is pre-processed using coupling agent, on the one hand can to avoid filler because
It is mutually heaped for Van der Waals force, reduces the fillibility of filler；On the other hand, the pretreatment of coupling agent can also improve filler with
The compatibility of matrix reduces composite inner defect as caused by incompatible, uses amination and carboxylic relative to existing
The method of the chemical functional groups such as baseization processing is more simple, and process flow is also more simplified；And made by the way of liquid phase mixing
Graphene and nanometer polytetrafluoroethylcomposite are uniformly dispersed, and avoid reuniting, more preferable compared to standard machinery mixed method dispersion effect, separately
Outer existing industrial mature, the efficient spray drying device of utilization, it is at low cost, there is biggish prospects for commercial application, it is same with this
The form of Shi Caiyong spray drying, makes composite mortar during drying, has both avoided the extensive group of nano material itself
It is poly-, and nanometer polytetrafluoroethylcomposite is made to be adhered to graphene surface by the effect of binder, so preparation side provided by the invention
Method compounded mix obtained had not only possessed the wear-resisting property of graphene, but also the greasy property with nanometer polytetrafluoroethylcomposite, the two
Synergistic effect can be played in conjunction with being present in basis material.Preparation method provided by the invention obtain can with polyformaldehyde, nylon,
The mixing of the multiple polymers basis material such as polyether-ether-ketone, ultra-high molecular weight polyethylene, can be improved the lubricating and wear-resisting of composite material
Can, injection molding and the molding of hot pressing form can be suitable for, had a wide range of application.
Detailed description of the invention
Fig. 1 is graphene-nanometer polytetrafluoroethylcomposite/polyformaldehyde electron microscope I that method of the invention makes；
Fig. 2 is graphene-nanometer polytetrafluoroethylcomposite/polyformaldehyde electron microscope II that method of the invention makes.
Specific embodiment
The present invention is further explained in the light of specific embodiments, it is clear that described embodiment is only this hair
Bright a part of the embodiment, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art are not having
Every other embodiment obtained under the premise of creative work is made, shall fall within the protection scope of the present invention.
Embodiment 1, the present invention are prepared that graphene-nanometer polytetrafluoroethylcomposite is compound to be changed especially by following below scheme technique
Property filler:
It takes the powdered graphene of 10 parts by weight to be added in the deionized water of 800 parts by weight first, and passes through water-bath
It is heated to 80 DEG C and is mixed, allow graphene sufficiently to dissolve and obtain solution A；Take 2 parts by weight of silane coupling agent, ethyl alcohol
15 parts by weight, the mixing of 1 parts by weight of deionized water are sufficiently stirred 30min and obtain solution B, and 5 parts by weight is taken to be added in solution A,
Then keeping reaction temperature is 80 DEG C, water-bath 3 hours, is cooled later to room temperature, is washed with deionized after filtering,
The graphene filler M modified with oil-wet behavior is obtained, it can be to avoid filler because of model using the pretreatment of coupling agent
De Huali and mutually heap, reunite.It is 1:15 progress ingredient according to graphene filler M and nanometer polytetrafluoroethylcomposite weight ratio, and
The water-ethanol mixed solution that suitable quality proportioning is 3:2 is added and is stirred mixing, while adding and accounting for graphene filler M
With the erythrol of nanometer polytetrafluoroethylcomposite gross mass 2%, the amount of water-ethanol mixed solution requires graphene filler M and nanometer poly-
Tetrafluoroethene can be fully dispersed wherein, and when it is 10%-20% that the volume of ethyl alcohol, which accounts for mixed solution ratio, erythrol
Effect as binder is preferable, and nanometer polytetrafluoroethylcomposite bonding on the surface of graphene after can effectively prevent graphene
It returns in the subsequent process folded, avoids the reunion of compounded mix in the polymer.
And stirring forms emulsion N under the conditions of being kept for 60 DEG C, in order to provide the dispersion effect of emulsion N, can be used super
Sound dispersing apparatus disperses emulsion N.
Emulsion N is handled using the form of spray drying later, the parameters of adjustable spraying drying test machine,
Keep inlet temperature at 130 DEG C, charging rate is 15, air pressure 20m3/ h, jet rate are 5S-1, outlet temperature 70-
Under conditions of between 80 DEG C, after equipment pre- thermostabilization, sprayed spray dryer is passed through under the transmission of emulsion N syringe pump
Mist is dry, and collects the dry powder P i.e. composite modified filler of graphene-nanometer polytetrafluoroethylcomposite that obtains that treated.
The composite modified filler of graphene-nanometer polytetrafluoroethylcomposite prepared can be effectively improved existing polymeric matrix
Wear rate mixes 20 parts by weight of dry powder P of acquisition with the polyformaldehyde powder of 80 parts by weight, and is added and accounts for total weight hundred
Divide the paraffin oil than 0.2%, using the shearing churned mechanically method of tradition, stirs 5min under the conditions of 1000r/min
The polyformaldehyde composite material modified by graphene-nanometer polytetrafluoroethylcomposite is obtained, uses and processes for convenience, it can will be above-mentioned
Graphene-nanometer polytetrafluoroethylcomposite modified polyformaldehyde composite material graphene-nanometer poly- four is prepared by pelletizer
Vinyl fluoride/polyformaldehyde composite granule.
In order to verify the effect that the composite modified filler of graphene-nanometer polytetrafluoroethylcomposite improves the wearability of polyformaldehyde matrix
Fruit is respectively obtained by way of injection molding with the knot of the modified polyformaldehyde composite granule preparation of graphene-nanometer polytetrafluoroethylcomposite
The structural member of the preparation of component and pure polyformaldehyde carries out friction and wear test, this hair of experimental data reality to above-mentioned contrast material
The coefficient of friction of the preparation of bright offer and the resulting structural member of application method is 0.11, wear rate 1.1*10-6mm3/(N*
m)；And the coefficient of friction of pure polyformaldehyde is 0.19, wear rate 2.3*10-6mm3/(N*m).The above results prove, by this hair
A kind of preparation of composite modified filler of graphene-nanometer polytetrafluoroethylcomposite of bright offer and application method can effectively combine graphene
Wear-resisting property and nanometer polytetrafluoroethylcomposite greasy property, and by the two combine exist be applied to existing polymeric matrix in
It is remarkably improved its lubrication and wear resistance property；
In addition graphene-nanometer polytetrafluoroethylcomposite/polyformaldehyde manufacture component is subjected to micro interface observation by Electronic Speculum,
Using the cold field emission scanning electron microscope SU8010 (MDTC-EQ-M18-01) of Hitachi, model specification: HITACHI
SU8010, as shown in Figure 1 and Figure 2 (amplification factor of Fig. 1, Fig. 2 are different), the base material in figure is graphene, ball to electron microscope
Shape particle is the micro-nano powder particles of polytetrafluoroethylene (PTFE), it can be seen that in addition to a small amount of reunion of regional area, nanometer polytetrafluoroethylcomposite
Distribution is more uniform, illustrates that nanometer polytetrafluoroethylcomposite bonding successfully bonds on the surface of graphene, to demonstrate of the invention
The validity of micromorphology.
Embodiment 2
It takes the powdered graphene of 10 parts by weight to be added in the deionized water of 800 parts by weight first, and passes through water-bath
It is heated to 80 DEG C and is mixed, allow graphene sufficiently to dissolve and obtain solution A；Take 2 parts by weight of silane coupling agent, ethyl alcohol
15 parts by weight, the mixing of 1 parts by weight of deionized water are sufficiently stirred 30min and obtain solution B, and 5 parts by weight is taken to be added in solution A,
Then keeping reaction temperature is 80 DEG C, water-bath 3 hours, is cooled later to room temperature, is washed with deionized after filtering,
The graphene filler M modified with oil-wet behavior is obtained, it can be to avoid filler because of model using the pretreatment of coupling agent
De Huali and mutually heap, reunite.It is that 1:5 carries out ingredient, and adds according to graphene filler M and nanometer polytetrafluoroethylcomposite weight ratio
Enter suitable quality proportioning be 3:2 water-ethanol mixed solution be stirred mixing, while add account for graphene filler M and
The amount of the polyethylene pyrrole network alkanone and erythrol of nanometer polytetrafluoroethylcomposite gross mass 1%, water-ethanol mixed solution requires graphene
Filler M can be fully dispersed wherein with nanometer polytetrafluoroethylcomposite, and stirring forms emulsion N under the conditions of being kept for 60 DEG C, then adopts
Emulsion N is handled with the form of spray drying, the parameters of adjustable spraying drying test machine, inlet temperature is kept to exist
130 DEG C, charging rate is 15, air pressure 20m3/ h, jet rate are 5S-1, outlet temperature is the condition between 70-80 DEG C
Under, after equipment pre- thermostabilization, it is spray-dried spray dryer is passed through under the transmission of emulsion N syringe pump, and collect
The dry powder i.e. composite modified filler of graphene-nanometer polytetrafluoroethylcomposite that obtains that treated.
The composite modified filler of graphene-nanometer polytetrafluoroethylcomposite prepared can be effectively improved existing polymeric matrix
Wear rate mixes 5 parts by weight of dry powder of acquisition with the ultra-high molecular weight polyethylene of 95 parts by weight, and is added and accounts for total weight
The paraffin oil of percentage 0.2% stirs 5min, i.e., using the shearing churned mechanically method of tradition under the conditions of 1000r/min
The composite polyethylene material modified by graphene-nanometer polytetrafluoroethylcomposite can be obtained, uses and processes for convenience, it can will be upper
The modified composite polyethylene material of the graphene stated-nanometer polytetrafluoroethylcomposite is prepared graphene-nanometer by pelletizer and gathers
Tetrafluoroethene/polyethylene composite granule.
In order to verify the effect that the composite modified filler of graphene-nanometer polytetrafluoroethylcomposite improves the wearability of base polyethylene
Fruit is respectively obtained by way of injection molding with the knot of the modified polyformaldehyde composite granule preparation of graphene-nanometer polytetrafluoroethylcomposite
The structural member of the preparation of component and pure polyformaldehyde carries out friction and wear test to above-mentioned contrast material.Specific friction testing item
Part is tested using reciprocating friction mode, and the device model specifically used is Ke Kaihua Science and Technology Development Co., Ltd. in Lanzhou
The high speed reciprocating friction and wear testing machine of HSR-2M type, test parameter are；The GCr15 steel ball for being diameter 6.35mm to flour milling carries
Lotus 20N, reciprocating speed 500rpm, traverse length 5mm, testing time 2h are manufactured using pure ultra-high molecular mass polyethylene
Structural member test as a comparison, result be pure ultra-high molecular mass polyethylene coefficient of friction 0.12, wear rate:
5.6*10-6mm3/ (N*m), and it is added to the friction of graphene of the invention-nanometer polytetrafluoroethylcomposite compounded mix
Coefficient 0.09, wear rate: 3.2*10-6mm3/ (N*m), wear rate reduces 42% in contrast, significant effect.
The coefficient of friction of the preparation provided by the invention of experimental data reality and the resulting structural member of application method is 0.11,
Wear rate is 1.1*10-6mm3/(N*m)；And the coefficient of friction of pure polyformaldehyde is 0.19, wear rate 2.3*10-6mm3/(N*m)。
The above results prove, a kind of preparation of the composite modified filler of graphene-nanometer polytetrafluoroethylcomposite provided through the invention and answer
Can be effectively in conjunction with the greasy property of the wear-resisting property of graphene and nanometer polytetrafluoroethylcomposite with method, and the two is combined and is existed
Applied to being remarkably improved its lubrication and wear resistance property in existing polymeric matrix.
Claims (9)
1. a kind of preparation method of the composite modified filler of graphene-nanometer polytetrafluoroethylcomposite, which is characterized in that including following step
It is rapid:
Step I takes graphene that deionized water is added, and heating stirring obtains solution A under water bath condition；
Step II takes coupling agent, ethyl alcohol, deionized water to be stirred to obtain solution B；
Step III, solution A and solution B are mixed and carries out coupling reaction under conditions of water-bath, material surface is made to show parent
Oiliness, cold filtration washing obtain graphene filler M modified；
Step IV, appropriate graphene filler M modified and nanometer polytetrafluoroethylcomposite is taken to be added to the mixed solution of water-ethanol
In mixed, and appropriate aqueous binders are added, carry out dispersion mixing, obtain emulsion N；
Step V, the dispersibility of emulsion N is maintained, and is dehydrated to obtain that graphene-nanometer polytetrafluoroethylcomposite is compound to be changed
Property filler.
2. a kind of preparation method of composite modified filler of graphene-nanometer polytetrafluoroethylcomposite according to claim 1, special
Sign is, the weight ratio of each component in the step I are as follows: 800 parts of deionized water, 10 parts of graphene, and bath temperature is 80
DEG C, and the graphene is powdered watersoluble plumbago alkene；
The weight ratio of each component in the step II are as follows: 2 parts of coupling agent, 15 parts of ethyl alcohol, 1 part of deionized water；
The weight ratio of solution A and solution B in the step III are as follows: 810 parts of solution A, 5 parts of solution B, and the coupling reaction
Condition be 80 DEG C water-bath 3 hours.
3. a kind of preparation method of composite modified filler of graphene-nanometer polytetrafluoroethylcomposite according to claim 2, special
Sign is that the coupling agent is one of organochromium complexes, silanes, titanate ester and aluminic acid compound or several.
4. a kind of preparation method of composite modified filler of graphene-nanometer polytetrafluoroethylcomposite according to claim 2, special
Sign is that the weight ratio range of graphene filler M and polytetrafluoroethylene (PTFE) is 1:5 to 1:25 in the step IV.
5. a kind of preparation method of composite modified filler of graphene-nanometer polytetrafluoroethylcomposite according to claim 4, special
Sign is that the aqueous binders in the step IV are polyethylene pyrrole network alkanone (PVP), in polyvinyl alcohol (PVA), erythrol
One or more, and the weight content of the aqueous binders is the composite modified filler of graphene-nanometer polytetrafluoroethylcomposite
1% -5%.
6. a kind of preparation method of composite modified filler of graphene-nanometer polytetrafluoroethylcomposite according to claim 2, special
Sign is that the drying mode in the step V is spray drying, and the parameter of the spray drying is, mouth temperature is in 120-
150 DEG C, charging rate controls within the scope of 70-90 DEG C in 5%-35%, air pressure in 10-25 atmospheric pressure, outlet temperature.
7. a kind of preparation method of composite modified filler of graphene-nanometer polytetrafluoroethylcomposite according to claim 2, special
Sign is that the mixed solution weight ratio of the water-ethanol in the step IV is 3 parts of water, 2 parts of ethyl alcohol.
8. using the application method of composite modified filler made from preparation method described in any claim in claim 1-7,
It is characterized in that, taking the resulting composite modified filler of graphene-nanometer polytetrafluoroethylcomposite of step V with the weight ratio of 5%-30%
Example is added in polymeric matrix material, while it is 0.1-1% small molecule grease that weight fraction, which is added, then mixed by stirring
Merga pass extruding pelletization obtains the modified polymer composite granule of graphene-nanometer polytetrafluoroethylcomposite, and composite granule is used
Injection molding or hot pressing mode obtain the product of required structure.
9. a kind of application method of composite modified filler of graphene-nanometer polytetrafluoroethylcomposite according to claim 8, special
Sign is that the small molecule grease is paraffin oil, and the polymeric matrix material is polyformaldehyde, nylon, polyether-ether-ketone, superelevation
One or more of molecular weight polyethylene.
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| CN110684136A (en) * | 2019-09-27 | 2020-01-14 | 北京石墨烯技术研究院有限公司 | Modified polytetrafluoroethylene, preparation method thereof and modified polytetrafluoroethylene product |
| CN110918007A (en) * | 2019-11-04 | 2020-03-27 | 江苏一夫新材料产业技术研究院有限公司 | PVP polymerized SnO2-graphene aerogels and method for the production thereof |
| CN112300521A (en) * | 2020-11-09 | 2021-02-02 | 河北中科同创科技发展有限公司 | High-thermal-conductivity polytetrafluoroethylene composite material and preparation method and application thereof |
| CN112300521B (en) * | 2020-11-09 | 2022-03-11 | 河北中科同创科技发展有限公司 | High-thermal-conductivity polytetrafluoroethylene composite material and preparation method and application thereof |
| CN112574585A (en) * | 2020-12-11 | 2021-03-30 | 安徽中翰高分子科技有限公司 | Low-hardness thermoplastic vulcanized elastomer material formed by polypropylene three-dimensional blow molding and preparation method thereof |
| CN114752265A (en) * | 2022-04-25 | 2022-07-15 | 中国航空发动机研究院 | Fluorine-containing coating and preparation method and application thereof |
| CN114875393A (en) * | 2022-05-13 | 2022-08-09 | 上海涓微新材料科技有限公司 | High-hardness wear-resistant nickel-phosphorus Teflon plating solution and plating layer |
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