CN104987657B - A kind of nanometer antiwear material modification phenolic resin and preparation method thereof - Google Patents
A kind of nanometer antiwear material modification phenolic resin and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to phenol-formaldehyde resin modified field, and in particular to a kind of nanometer antiwear material modification phenolic resin and preparation method thereof.The nano material modified phenolic resins are prepared via a method which：(1) surface modification of nano material：Surfactant is dissolved in organic solvent, adds nano-particle, after carrying out mechanical agitation, ball milling, ultrasonic reaction processing successively, obtains the nanoparticle suspension by surface modification；The nano-particle is nano-graphite, nano-graphene, fullerene, nanometer MoS2With the one or more in CNT；(2) phenolic resin is added in above-mentioned nanoparticle suspension, ultrasonic reaction processing is carried out after being sufficiently stirred, after reaction terminates, after through vacuum drying and crushing, obtain super abrasive nano material modified phenolic resins.The nano material modified phenolic resins have stronger thermal stability, excellent wearability, and wear rate is extremely low, can be widely applied to prepare high-quality friction material.
Description
Technical field
The invention belongs to phenol-formaldehyde resin modified field, and in particular to a kind of nanometer antiwear material modification phenolic resin and its system
Preparation Method.
Background technology
Phenolic resin has good mechanical performance, against weather, corrosion-resistant as one of three big synthesis thermosetting resins
Property, water resistance and certain heat resistance, are widely used in the industries such as communications and transportation, Aviation Industry, military equipment, electronic apparatus.
But with technological innovations such as industrial expansion, particularly auto industry and bullet trains, High Performance Phenolic Resins are proposed newly
Requirement.Friction material (such as vehicle brake piece, clutch) using phenolic resin as base material needs good wearability, higher
Heat decomposition temperature, enough coefficient of friction and relatively low noise, and traditional pure phenolic resin heat-resistant stability is poor, and fragility is big,
Toughness is bad, is increasingly not suitable with the demand for development of friction material.At present, high-quality friction material phenolic resin in China's is main
By import, the development of China's friction material industry strongly limit.
The content of the invention
The present invention in view of the shortcomings of the prior art, and it is an object of the present invention to provide a kind of nanometer antiwear material modification phenolic resin and its
Preparation method.
For achieving the above object, the technical solution adopted in the present invention is：
A kind of preparation method of nanometer antiwear material modification phenolic resin, comprises the following steps：
(1) surface modification of nano material：Surfactant is dissolved in organic solvent, adds nano-particle thereto,
Mechanical agitation is carried out first, then carries out ball milling, is finally entered ultrasonic reactor processing, is obtained the nanoparticle by surface modification
Sub- suspension；The nano-particle is nano-graphite, nano-graphene, nanometer fullerene, nanometer MoS2In CNT
One or more；
(2) phenolic resin is added in step (1) described nanoparticle suspension by surface modification, be sufficiently stirred
Enter ultrasonic reactor afterwards to handle, after processing terminates, after through vacuum drying and crushing, obtain nanometer antiwear material modification phenolic aldehyde tree
Fat.
In such scheme, the surfactant is neopelex, catechol, polyethylene glycol, dodecane
One or more in base sodium sulphate and cetyl trimethylammonium bromide.
In such scheme, the mass parts ratio of the phenolic resin, nano-particle and surfactant is 100:10~20:10
~100.
In such scheme, step (1) the churned mechanically time is 0.5~3h, the rotating speed of the ball milling for 300~
1000rmp, ratio of grinding media to material 3:2~4:1；Step (1) processing time into ultrasonic reactor processing is 0.5~2h, ultrasound
Power is 0.5~3KW.
In such scheme, the mixing time of step (2) described stirring is 0.1~1.5h, and step (2) is described to enter ultrasound instead
The processing time for answering device to handle is 0.1~2h, and ultrasonic power is 0.5~3KW.
In such scheme, the quality of the organic solvent is 0.1~10 times of phenolic resin quality.
In such scheme, the organic solvent is that can dissolve the conventional organic solvent of the surfactant, as ethanol,
Toluene, acetone.
Nanometer antiwear material modification phenolic resin is prepared in above-mentioned preparation method.
For in Conventional nano phenol-formaldehyde resin modified, scattered and distribution and its and base of the nano-particle in macromolecule matrix
The interface compatibility of body is bad, and the problems such as so as to cause the mechanical property of material and poor frictional behaviour, the application is according to high score
The feature of subbase body is directed to the suitable nano-particle of Sexual behavior mode, and modifies the surface of nano-particle, suppresses the reunion of nano-particle
And improve the distribution of nano-particle in the base, the interfacial interaction between nanoparticle surface and matrix is improved, realization is received
Nano composite material system is wear-resisting and the General Promotion of mechanical property；It is of the present invention using nano particle modified alkyd resin as matrix
Friction material friction pair face can be promoted to form uniform and thin and strong adhesion strength transfer membrane, the carrying of material can be significantly improved
Ability and tribological property.
Beneficial effects of the present invention are as follows：
(1) present invention, which is directed to, has surface modification effect difference when carrying out the surface modification of nano-particle using conventional method
Problem, surface modification is carried out to nano-particle using organic surface active agent, during nanoparticle surface modified, passes through machine
Tool stirring, ball milling, Oscillatory Flow Reactor is scattered and is ultrasonically treated, and it is anti-to form mechanical agitation, ball milling (macro-scale), ultrasound
The dispersion technology that becomes more meticulous of the integrated application of device processing (meso-scale and micro-scale) is answered, can effectively lift surfactant pair
The modification effect of nano-particle.
(2) the problem of present invention is for nano-particle and phenolic compatible difference, using fine integrated dispersion technology,
By mechanical agitation, ultrasonic reactor processing etc. process, efficiently solve nano-particle disperse in macromolecule matrix it is uneven, steady
Qualitative poor problem.
(3) mechanical property and heat for the nano material modified phenolic resins being prepared using preparation method of the present invention
Stability has to be lifted by a relatively large margin, has excellent wearability, and wear rate is extremely low, be can be widely applied to preparation high-performance and is rubbed
Wipe material.
Brief description of the drawings
Fig. 1 is that phenol-formaldehyde resin modified TG schemes in the embodiment of the present invention 1.
Fig. 2 is that phenol-formaldehyde resin modified TG schemes in the embodiment of the present invention 2.
Fig. 3 is that phenol-formaldehyde resin modified TG schemes in the embodiment of the present invention 3.
Fig. 4 is that phenol-formaldehyde resin modified TG schemes in the embodiment of the present invention 4.
Fig. 5 schemes for common 2123 phenolic resin TG.
Embodiment
For a better understanding of the present invention, with reference to the embodiment content that the present invention is furture elucidated, but the present invention
Content is not limited solely to the following examples.
In following examples, the organic solvent is that can dissolve the conventional organic solvent of the surfactant, such as second
Alcohol, toluene, acetone.
Embodiment 1
A kind of nanometer antiwear material modification phenolic resin, is prepared via a method which to obtain：10 parts are added by mass parts
Organic solvent, 10 parts of polyethylene glycol, 15 parts of nano-graphite are into stirred tank, at room temperature, after mechanical agitation 1.5h, are added to
Ball milling (rotational speed of ball-mill 300rpm, ratio of grinding media to material 4 in ball mill:1), finally entering ultrasonic reactor processing 0.5h, (ultrasonic power is
3KW), the nano-graphite suspension by surface modification is obtained, 100 parts of phenolic resin are added in this suspension, fully stirred
After mixing 0.5h, into ultrasonic reactor processing 0.1h (ultrasonic power 3KW), vacuum drying, crushing material obtain to 200 mesh
A kind of graphite modified phenolic resin of nanometer antiwear.The TG figures for the phenol-formaldehyde resin modified being prepared in the present embodiment are shown in Fig. 1.
Embodiment 2
A kind of nanometer antiwear material modification phenolic resin, is prepared via a method which to obtain：1000 parts are added by mass parts
Organic solvent, 30 parts of polyethylene glycol, 30 parts neck benzenediol, 40 parts of lauryl sodium sulfate, 5 parts of CNT, 5
Part nano-graphene into stirred tank, at room temperature, after mechanical agitation 0.5h, be added to ball milling in ball mill (rotating speed 500rpm,
Ratio of grinding media to material 3:1) ultrasonic reactor processing 1h (ultrasonic power 2KW), is finally entered, obtains the nano-graphite by surface modification
Alkene suspension, 100 parts of phenolic resin are added in this suspension, are sufficiently stirred 0.1h, it is (super into ultrasonic reactor processing 1h
Acoustical power is 2KW), vacuum drying, crushing material to 200 mesh, that is, obtain a kind of wear-resisting carbon nanotube/nano graphene and be modified
Phenolic resin.The TG figures for the phenol-formaldehyde resin modified being prepared in the present embodiment are shown in Fig. 2.
Embodiment 3
A kind of nanometer antiwear material modification phenolic resin, is prepared via a method which to obtain：500 parts are added by mass parts
Organic solvent, 20 parts of cetyl trimethylammonium bromide, 20 parts of neopelex, 10 parts of polyethylene glycol, 7 parts
Nanometer fullerene, 13 parts of nanometer MoS2Into stirred tank, at room temperature, after mechanical agitation 3h, ball milling in ball mill is added to
(rotating speed 800rpm, ratio of grinding media to material 2:1) ultrasonic reactor processing 2h (ultrasonic power 0.5KW), is finally entered, obtains repairing by surface
The nanometer MoS of decorations2/ fullerene suspension, 100 parts of phenolic resin are added in this suspension, 1h is sufficiently stirred, enters the excess of imports
2h (ultrasonic power 0.5KW) is handled in sound reactor, vacuum drying, crushing material to 200 mesh, that is, obtains a kind of nanometer antiwear
MoS2/ fullerene phenol-formaldehyde resin modified.The TG figures for the phenol-formaldehyde resin modified being prepared in the present embodiment are shown in Fig. 3.
Embodiment 4
A kind of nanometer antiwear material modification phenolic resin, is prepared via a method which to obtain：500 parts are added by mass parts
Organic solvent, 20 parts of lauryl sodium sulfate, 20 parts of cetyl trimethylammonium bromide, 5 parts of nanometer fullerene, 7
The nano-graphene of part at room temperature, after mechanical agitation 2.5h, is added to ball milling (rotating speed in ball mill into stirred tank
1000rpm, ratio of grinding media to material 3:2) ultrasonic reactor processing 1.2h (ultrasonic power 1W), is finally entered, is obtained by surface modification
Nano-graphene/fullerene suspension, 100 parts of phenolic resin are added in this suspension, are sufficiently stirred 1.5h, enter
Ultrasonic reactor processing 1.2h (ultrasonic power 1W), vacuum drying, crushing material to 200 mesh, that is, obtain a kind of nanometer antiwear
Graphene/fullerene phenol-formaldehyde resin modified.The TG figures for the phenol-formaldehyde resin modified being prepared in the present embodiment are shown in Fig. 4.
Using common 2123 phenolic resin as control (the TG figures of common 2123 phenolic resin are shown in Fig. 5), from Fig. 1~Fig. 5 pair
Than can be seen that：The nano material modified phenolic resins that embodiment 1~4 is prepared have in mechanical property and thermal stability
Lifted by a relatively large margin.
Friction material is prepared as bonding agent using the nano particle modified alkyd resin in embodiment 1~4 below and carrys out progressive
Can test.With identical formula, the particle modified phenolic resin of nanometer antiwear and common 2123 prepared respectively with embodiment 1~4
Phenolic resin (production of Shandong holy well Hai Si companies) is that bonding agent prepares automobile brake brake block, according to QCT 227.1-2009
Motorcycle and trail bike brake(-holder) block frictional behaviour test method method of testing carry out constant speed frictional behaviour experiment, as a result such as table
Shown in 1~5.
1 embodiment of table, 1 composite nano modified phenolic resin constant speed frictional behaviour test result
2 embodiment of table, 2 composite nano modified phenolic resin constant speed frictional behaviour test result
3 embodiment of table, 3 composite nano modified phenolic resin constant speed frictional behaviour test result
4 embodiment of table, 4 composite nano modified phenolic resin constant speed frictional behaviour test result
The common 2123 phenolic resin constant speed frictional behaviour test result of table 5
The nano material modified phenolic resins that embodiment 1~4 is prepared it can be seen from table 1-5 have excellent resistance to
Mill property, wear rate is extremely low, can be widely applied to prepare high-quality friction material.
Obviously, above-described embodiment is only intended to clearly illustrate made example, and is not the limitation to embodiment.It is right
For those of ordinary skill in the art, can also make on the basis of the above description it is other it is various forms of change or
Change.There is no necessity and possibility to exhaust all the enbodiments.And the obvious change or change therefore amplified
Move within still in the protection domain of the invention.
Claims (4)
1. a kind of preparation method of nanometer antiwear material modification phenolic resin, it is characterised in that comprise the following steps：
（1）The surface modification of nano material：Surfactant is dissolved in organic solvent, adds nano-particle thereto, first
Mechanical agitation is carried out, then carries out ball milling, ultrasonic reactor processing is finally entered, obtains hanging by the nano-particle of surface modification
Supernatant liquid；The nano-particle is nano-graphite, nano-graphene, nanometer fullerene, nanometer MoS2With one in CNT
Kind is several；The surfactant be neopelex, catechol, polyethylene glycol, lauryl sodium sulfate and
One or more in cetyl trimethylammonium bromide；The quality of the organic solvent is the 0.1 ~ 10 of phenolic resin quality
Times；
（2）Phenolic resin is added to step（1）In the nanoparticle suspension by surface modification, it is sufficiently stirred laggard
Enter ultrasonic reactor processing, after processing terminates, after through vacuum drying and crushing, obtain nanometer antiwear material modification phenolic resin；
The mass parts ratio of the phenolic resin, nano-particle and surfactant is 100:10~20: 10~100.
2. preparation method according to claim 1, it is characterised in that step（1）When described churned mechanically
Between be 0.5 ~ 3h, the rotating speed of the ball milling is 300 ~ 1000rpm, ratio of grinding media to material 3:2~4:1；Step（1）It is described to enter ultrasound
The processing time of reactor for treatment is 0.5 ~ 2h, and ultrasonic power is 0.5 ~ 3KW.
3. preparation method according to claim 1, it is characterised in that step（2）During the stirring of the stirring
Between be 0.1 ~ 1.5h, step（2）The processing time into ultrasonic reactor processing is 0.1 ~ 2h.
4. the nanometer antiwear material modification phenolic resin that any preparation method of claim 1 ~ 3 is prepared.
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| CN105782243B (en) * | 2016-03-15 | 2018-12-14 | 江苏大学 | A kind of micro- texture surface solid lubrication processing method of secondary laser of friction |
| CN105950260B (en) * | 2016-05-05 | 2018-12-07 | 西安交通大学 | Obtain the friendly MoS containing lubrication2The method of nano particle lubricating oil |
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| CN106763355A (en) * | 2016-11-10 | 2017-05-31 | 厦门市双晋材料科技有限公司 | A kind of friction material and the brake block with the friction material |
| CN106832352B (en) * | 2017-01-17 | 2020-01-14 | 江苏捷峰钜容新材料有限公司 | Preparation method of carbon nano tube composite resin microspheres |
| CN107057006B (en) * | 2017-05-25 | 2019-10-08 | 成都新柯力化工科技有限公司 | A kind of thermosetting phenolic resin special graphite alkene mother liquor and preparation method |
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| CN108017874A (en) * | 2017-12-05 | 2018-05-11 | 中北大学 | A kind of graphene/hard nanometer particle cooperative phenol-formaldehyde resin modified wear-resistant material |
| CN108251195A (en) * | 2017-12-29 | 2018-07-06 | 赵建平 | A kind of preparation method of binding type solid dry lubricant |
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| CN111022533B (en) * | 2019-12-05 | 2021-09-10 | 铁科纵横（天津）科技发展有限公司 | Powder metallurgy brake pad friction material for high-speed train and preparation method thereof |
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