CN110092941A - The composite lubricated material of three-dimensional grapheme based on physical absorption, preparation method and application - Google Patents
The composite lubricated material of three-dimensional grapheme based on physical absorption, preparation method and application Download PDFInfo
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- CN110092941A CN110092941A CN201910389638.1A CN201910389638A CN110092941A CN 110092941 A CN110092941 A CN 110092941A CN 201910389638 A CN201910389638 A CN 201910389638A CN 110092941 A CN110092941 A CN 110092941A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/36—After-treatment
- C08J9/40—Impregnation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/36—After-treatment
- C08J9/40—Impregnation
- C08J9/42—Impregnation with macromolecular compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2375/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
- C08J2375/04—Polyurethanes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2477/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
- C08J2477/02—Polyamides derived from omega-amino carboxylic acids or from lactams thereof
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Abstract
The present invention relates to the composite lubricated materials of three-dimensional grapheme based on physical absorption, preparation method and application, belong to composite lubricated Material Field, the composite lubricated material of three-dimensional grapheme is using flexibel polyurethane sponge as matrix, it is prepared after adsorbing graphene/paraffin of different content using the method for in-situ polymerization, the composite lubricated material technology is simple, graphene (GO) used is less, it can volume production, the material has good tribological property as lubrication pad, has a extensive future.
Description
Technical field
The invention belongs to composite lubricated Material Fields, and in particular, to a kind of three-dimensional grapheme based on physical absorption is multiple
Close lubriation material, preparation method and application.
Background technique
Lubriation material is widely used in various mechanical equipments, for reducing the friction of equipment, and prevents mechanical equipment certainly
The abrasion of body improves machine security runnability.Graphene is as known most thin and strongest lubriation material in the world, lubrication
Characteristic is mainly derived from three aspects: one is the friction that its own piece interlayer is minimum, theoretical research is found between graphene layer
Nano friction power depends primarily on the lattice commensurability (mispairing angle) between graphene layer, wherein non-commensurability (lattice mismatch) shape
The interformational sliding frictional force of the graphene of formula stacking is very small, or even ultra-low friction (super lubrication) occurs, and the multilayer stone stacked
Ink is easier to be changed into non-commensurability state, can become significantly more efficient nano lubricating agent theoretically；The second is graphene film surface compared with
Small sliding friction, it is main including wrinkle mechanism outside Electron-phonon coupling mechanism, face, flexible deformation energy dissipation mechanism and
Shear-deformable mechanism；The third is combining to form a more excellent profit with other lubricants by its preferable adsorption capacity
Gliding mass system.
However, at present it has been reported that material obtained by graphene is only used only in the polymer matrix graphene lubriation material of application
The coefficient of friction of material is usually larger, this may have a negative impact in the During Process of Long-term Operation of slide unit.Therefore, many texts
Report is offered to reduce friction using the synergistic effect with other lubricants and improve wearability.Such as Chinese invention patent
CN201610094019.6 discloses a kind of polycaprolactam lubriation material comprising graphene lubricant, and optimal dosage is up to
10% (i.e. about 4% pure graphene), this increases material cost to a certain extent.In addition, the graphene reported at present all needs
To pass through many and diverse process of surface treatment, to obtain fine dispersion in the matrix being modified to play graphene lubricating action
Maximum efficiency, in this context, need to seek a kind of graphene dosage it is less and can obtain fine dispersion and but maintain
The lubriation material of its excellent frictional performance.
Summary of the invention
In order to solve deficiency in the prior art, the purpose of the present invention one is to provide a kind of three-dimensional based on physical absorption
The composite lubricated material of graphene, purpose two be to provide the preparation method of above-mentioned composite lubricated material, and purpose three is to provide
State application of the composite lubricated material in monomer cast nylon material pad.The composite lubricated material is with flexibel polyurethane sponge (PU)
It for matrix, is obtained after adsorbing graphene/paraffin of different content, the composite lubricated material technology is simple, graphene (GO) used
It is less, can volume production, as polyamide pad modifying agent have good tribological property, have a extensive future.
To achieve the goals above, the present invention use the specific scheme is that
The preparation method of the composite lubricated material of three-dimensional grapheme based on physical absorption, comprising the following steps:
Step 1: taking polyurethane sponge, dried after cleaning, the sponge after drying is weighed；It is subsequently placed in graphene solution
In, squeezing sponge makes it suck graphene solution, then impregnates 12h and takes out, and drying obtains PU/GO sponge；
Step 2: weighing to PU/GO sponge, it is subsequently placed in the paraffin of 80-100 DEG C of thawing and carries out immersion 3-9h, obtain
Primary sponge material；The mass ratio of PU/GO sponge and paraffin is 1:1.5-1:3 in the primary sponge material；
Step 3: caprolactam is melted, it is stirred under vacuum 30-50min, catalyst is added, continues to be stirred under vacuum 30-50min, obtain
Active liquid；
Step 4: primary sponge material obtained by step 2 is placed in mold；It is added and is acylated into active liquid obtained by step 3
Agent is cast into mold rapidly after rocking 10-15s, and liquid level is made to cover primary sponge material, after 160-180 DEG C of polymerization 1-3h oneself
It is so cooling, obtain the composite lubricated material of three-dimensional grapheme.
It is advanced optimized as to above scheme, the 2-5min before casting of mold described in step 4 is put into 160-180
Preheating in DEG C baking oven.
It is advanced optimized as to above scheme, caprolactam melting is referred to described in step 3 and is added in 140 DEG C of oil baths
Caprolactam is melted under heat.
It is advanced optimized as to above scheme, the temperature condition of drying described in step 1 is 80 DEG C, the time is
12h。
It is advanced optimized as to above scheme, the specific gravity of polyurethane sponge described in step 1 is 0.012-0.036.
It is advanced optimized as to above scheme, the concentration of graphene solution described in step 1 is 1.5 mg/ml-
4.5 mg/ml。
It is advanced optimized as to above scheme, the catalyst is sodium hydroxide, and the acylating agent is that toluene two is different
Cyanate.
A kind of composite lubricated material of three-dimensional grapheme, the composite lubricated material of three-dimensional grapheme is also claimed in the present invention
It is to be prepared using above-mentioned preparation method.
In addition application of the composite lubricated material of above-mentioned three-dimensional grapheme as lubrication pad is claimed in the present invention.
The utility model has the advantages that
1, the three-dimensional grapheme of physical absorption self assembly of the present invention meets the excellent performance that lubriation material maintains graphene,
The operation of physical absorption self-assembling method is easy, required simple process, energy conservation and environmental protection.
2, the polyurethane sponge that the present invention is added has good adsorptivity and toughness, and graphene can be made uniformly to be divided
It dissipates, and greatly reduces the dosage of expensive graphene, and avoid for raising interface compatibility energy and for graphene itself
Many and diverse surface treatment.
3, three-dimensional grid system of the composite lubricated material prepared by the present invention based on sponge can quickly conduct friction and generate
Heat, and can cooperate with and be acted on using the anti-friction wear-resistant of graphene and paraffin, wear-resisting property and the friction of matrix can be effectively improved
Coefficient, to effectively improve the performance of the lubrication pad using material production.
Specific embodiment
Below in conjunction with the embodiment of the present invention, technical scheme in the embodiment of the invention is clearly and completely described.
The instrument and equipment of this field routine is used in the following example.The experiment of actual conditions is not specified in the following example
Method, usually according to normal condition, or according to the normal condition proposed by manufacturer.Various raw materials are used in the following example, are removed
It is non-otherwise indicated, all use conventional commercial product.
Embodiment 1:
It takes PU sponge that specific gravity is 0.012 respectively to clean three times with ethyl alcohol and deionized water respectively, then dries 12h at 80 DEG C, it will
The sponge of drying is weighed, and is subsequently placed in the GO solution of 3mg/ml；Squeeze to sponge makes its internal sucking GO solution,
It is taken out after impregnating 12h, dries 12h at 80 DEG C, PU/GO sponge is made；The PU/GO sponge prepared is taken, weighs quality, then
It is put in the paraffin of 90 DEG C of thawings and carries out immersion 6h, the mass ratio for obtaining PU/GO sponge and paraffin is the three-dimensional grapheme of 1:1.5
Lubriation material.
Polyamide-based three-dimensional graphene composite material is prepared using the method for in-situ polymerization: in 140 DEG C of oil bath heating conditions
It is lower to melt 100g caprolactam, it is stirred under vacuum 40min, 0.8g NaOH is then added, continues to be stirred under vacuum 40min；It will be three-dimensional
Graphene lubriation material 3min before casting is put into 160 DEG C of molds.After the completion of caprolactam is stirred under vacuum, three-necked flask is taken out
Be added 1ml toluene di-isocyanate(TDI), cast rapidly after quickly rocking 10 seconds, make caprolactam matrix liquid level cover sponge, 170
DEG C polymerization 2h after natural cooling, demoulding obtain sample, i.e. three-dimensional graphene composite material.
Embodiment 2:
It takes PU sponge that specific gravity is 0.019 respectively to clean three times with ethyl alcohol and deionized water respectively, then dries 12h at 80 DEG C, it will
The sponge of drying is weighed, and is subsequently placed in the GO solution of 1.5mg/ml；Squeeze to sponge keeps its internal sucking GO molten
Liquid takes out after impregnating 12h, dries 12h at 80 DEG C.The PU/GO sponge prepared is taken, quality is weighed, is then put in 80 DEG C and melts
Immersion 9h is carried out in the paraffin of change, the mass ratio for obtaining sponge and paraffin is the three-dimensional grapheme lubriation material of 1:1.5.
Polyamide-based three-dimensional graphene composite material is prepared using the method for in-situ polymerization: will under 140 DEG C of oil bath heatings
The melting of 100g caprolactam, is stirred under vacuum 30min, and 0.5g NaOH is then added, and continues to be stirred under vacuum 30min；By three-dimensional graphite
Alkene lubriation material 2min before casting is put into 170 DEG C of molds.After the completion of caprolactam is stirred under vacuum, takes out three-necked flask and be added
0.5ml toluene di-isocyanate(TDI) is cast rapidly after quickly rocking 12 seconds, make caprolactam matrix liquid level cover sponge, 180 DEG C
Natural cooling after polymerization 1h, demoulding obtain sample, i.e. three-dimensional graphene composite material.
Embodiment 3:
It takes PU sponge that specific gravity is 0.026 to clean three times with ethyl alcohol and deionized water respectively, then dries 12h at 80 DEG C, will dry
Dry sponge is weighed, and is subsequently placed in the GO solution of 4.5mg/ml, and squeeze to sponge makes its internal sucking GO solution,
It is taken out after impregnating 12h, dries 12h at 80 DEG C.The PU/GO sponge prepared is taken, quality is weighed, is then put in 100 DEG C of thawings
Paraffin in carry out immersion 3h, the mass ratio for obtaining sponge and paraffin is the three-dimensional grapheme lubriation material of 1:1.5.
Polyamide-based three-dimensional graphene composite material is prepared using the method for in-situ polymerization, i.e. it will under 140 DEG C of oil bath heatings
The melting of 100g caprolactam, is stirred under vacuum 30min, and 0.5g NaOH is then added, and continues to be stirred under vacuum 30min；By three-dimensional graphite
Alkene lubriation material 2min before casting is put into 170 DEG C of molds.After the completion of caprolactam is stirred under vacuum, takes out three-necked flask and be added
1.5ml toluene di-isocyanate(TDI) is cast rapidly after quickly rocking 15 seconds, make caprolactam matrix liquid level cover sponge, 160 DEG C
Natural cooling after polyase 13 h, demoulding obtain sample, i.e. three-dimensional graphene composite material.
Embodiment 4:
It takes PU sponge that specific gravity is 0.036 to clean three times with ethyl alcohol and deionized water respectively, then dries 12h at 80 DEG C, will dry
Dry sponge is weighed, and is subsequently placed in the GO solution of 3mg/ml, and squeeze to sponge makes its internal sucking GO solution, leaching
It is taken out after bubble 12h, dries 12h at 80 DEG C.The PU/GO sponge prepared is taken, quality is weighed, is then put in the stone of 90 DEG C of thawings
Immersion 6h is carried out in wax, the mass ratio for obtaining sponge and paraffin is respectively the three-dimensional grapheme lubriation material of 1:3.
Polyamide-based three-dimensional graphene composite material is prepared using the method for in-situ polymerization: will under 140 DEG C of oil bath heatings
The melting of 100g caprolactam, is stirred under vacuum 30min, and 1.1g NaOH is then added, and continues to be stirred under vacuum 30min；By three-dimensional graphite
Alkene lubriation material 3min before casting is put into 170 DEG C of molds.After the completion of caprolactam is stirred under vacuum, takes out three-necked flask and be added
1ml toluene di-isocyanate(TDI) is cast rapidly after quickly rocking 10 seconds, and caprolactam matrix liquid level is made to cover sponge, and 160 DEG C poly-
Natural cooling after conjunction 2h, demoulding obtain sample, i.e. three-dimensional graphene composite material.
Comparative example 1:
It weighs caprolactam to be placed in three-necked flask, 140 DEG C are heated in oil bath pan melts caprolactam completely, then side
Stirring side vacuumizes.After reacting half an hour, sodium hydrate solid is added into three-necked flask, continues to vacuumize.After half an hour, to
It is added in three-necked flask a small amount of acylating agent (Toluene-2,4-diisocyanate, 4- diisocyanate), it immediately will be in three-necked flask after concussion three-necked flask
Liquid is transferred in mold preheated in advance, is heated two hours at 160 DEG C, natural cooling obtains polycaprolactam.
Friction testing operating condition, in dry condition, loads 180N using MM-2HL plastic sliding frictional wear testing machine,
Test rate is 200r/min, test period 60min, and antithesis uses diameter for the steel loop of 40mm.Embodiment 1-4 measurement rubs
The results are shown in Table 1 for wiping coefficient and wear rate.
The coefficient of friction and abrasion loss contrast table of material prepared by 1 embodiment 1-4 of table and comparative example 1
Through table 1 it is found that compared with comparative example 1, using embodiment 1-4 preparation polymeric material coefficient of friction and wear rate compared with
Low, the performance of the polymeric material especially prepared with embodiment 1 is best, and wearability improves 6 times.
Method of the present invention using in-situ polymerization prepares polyamide-based three-dimensional graphene composite material, GO content
About 0.4%, and it is effectively improved wear-resisting property, reduce coefficient of friction.Its mechanism of action is as follows:
Graphene oxide contained by the present invention has minimum nano-scale, biggish specific surface area and surface ruffle pattern,
It can enhance between substrate molecule in combination with PU sponge surface functional group abundant through the mutual of covalent bond and non-covalent bond
Effect is conducive to stress and disperses, and improves its bearing capacity；Three-dimensional grapheme lubriation material grid system can quickly conduct friction
The heat of generation, and can cooperate with and be acted on using the anti-friction wear-resistant of graphene and paraffin, can be effectively improved matrix wear-resisting property and
Coefficient of friction.
It should be noted that embodiment described above is interpreted as illustrative, to be not intended to limit the present invention protection
Range, protection scope of the present invention are subject to claims.To those skilled in the art, without departing substantially from of the invention real
Under the premise of matter and range, some nonessential modifications and adaptations made to the present invention still fall within protection scope of the present invention.
Claims (9)
1. the preparation method of the composite lubricated material of three-dimensional grapheme based on physical absorption, it is characterised in that: the following steps are included:
Step 1: taking polyurethane sponge, dried after cleaning, the sponge after drying is weighed；It is subsequently placed in graphene solution
In, squeezing sponge makes it suck graphene solution, then impregnates 12h and takes out, and drying obtains PU/GO sponge；
Step 2: weighing to PU/GO sponge, it is subsequently placed in the paraffin of 80-100 DEG C of thawing and carries out immersion 3-9h, obtain
Primary sponge material；The mass ratio of PU/GO sponge and paraffin is 1:1.5-1:3 in the primary sponge material；
Step 3: caprolactam is melted, it is stirred under vacuum 30-50min, catalyst is added, continues to be stirred under vacuum 30-50min, obtain
Active liquid；
Step 4: primary sponge material obtained by step 2 is placed in mold；It is added and is acylated into active liquid obtained by step 3
Agent is cast into mold rapidly after rocking 10-15s, and liquid level is made to cover primary sponge material, after 160-180 DEG C of polymerization 1-3h oneself
It is so cooling, obtain the composite lubricated material of three-dimensional grapheme.
2. preparation method according to claim 1, it is characterised in that: the 2-5min before casting of mold described in step 4 is put
Enter preheating in 160-180 DEG C of baking oven.
3. preparation method according to claim 1, it is characterised in that: refer to caprolactam melting described in step 3
Caprolactam is melted under 140 DEG C of oil bath heatings.
4. preparation method according to claim 1, it is characterised in that: the temperature condition of drying described in step 1 is 80
DEG C, time 12h.
5. preparation method according to claim 1, it is characterised in that: the specific gravity of polyurethane sponge described in step 1 is
0.012-0.036。
6. preparation method according to claim 1, it is characterised in that: the concentration of graphene solution described in step 1 is
1.5 mg/ml-4.5 mg/ml。
7. preparation method according to claim 1, it is characterised in that: the catalyst is sodium hydroxide, the acylating agent
For toluene di-isocyanate(TDI).
8. a kind of composite lubricated material of three-dimensional grapheme, it is characterised in that: utilize preparation described in claim 1-7 any one
Method is prepared.
9. application of the composite lubricated material of three-dimensional grapheme according to claim 8 as lubrication pad.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113831576A (en) * | 2021-09-24 | 2021-12-24 | 中国科学院兰州化学物理研究所 | Self-repairing porous lubricating composite material and preparation method thereof |
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| KR100848303B1 (en) * | 2007-05-31 | 2008-07-24 | 주식회사 에스앤엠 | Metal conduit inserted mc nylon support block producing methods and mc nylon support block producing thereof |
| CN102942694A (en) * | 2012-10-17 | 2013-02-27 | 河南科技大学 | Oil-filled monomer casting nylon composite material |
| CN107321306A (en) * | 2017-07-03 | 2017-11-07 | 佛山市高科合创科技有限公司 | The preparation method of three dimension high efficiency graphene sorbing material by template of sponge |
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| KR20020033119A (en) * | 2002-02-16 | 2002-05-04 | 정대원 | The method for preparing antistatic MC nylon with improved frictional properties |
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| CN113831576A (en) * | 2021-09-24 | 2021-12-24 | 中国科学院兰州化学物理研究所 | Self-repairing porous lubricating composite material and preparation method thereof |
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