CN107793750A - A kind of quick preparation method for preparing graphene polyamide compoiste material - Google Patents
A kind of quick preparation method for preparing graphene polyamide compoiste material Download PDFInfo
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- CN107793750A CN107793750A CN201710953017.2A CN201710953017A CN107793750A CN 107793750 A CN107793750 A CN 107793750A CN 201710953017 A CN201710953017 A CN 201710953017A CN 107793750 A CN107793750 A CN 107793750A
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- CN
- China
- Prior art keywords
- graphene
- compoiste material
- polyamide compoiste
- graphite
- caprolactam
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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
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
- C08G69/02—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
- C08G69/08—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from amino-carboxylic acids
- C08G69/14—Lactams
- C08G69/16—Preparatory processes
-
- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Polyamides (AREA)
Abstract
The invention discloses a kind of quick method for preparing graphene polyamide compoiste material, this method includes Graphite processing, and monomer and modified graphite are carried out into mixing and absorption, obtain being adsorbed with the modified graphite of monomer, under activator effect, polymerization obtains graphene polyamide compoiste material.Chemical substance need not be added in graphene polyamide compoiste material preparation process prepared by this method, it is environmentally friendly, quick, and graphene is uniformly dispersed in the polymer, while the graphene polyamide compoiste material combination property prepared is good.
Description
Technical field
The invention belongs to Material Field, more particularly to a kind of quick preparation method for preparing graphene-polyamide compoiste material.
Background technology
Graphene is the carbon atomic layer of monoatomic thickness, is the most thin material having now been found that.The special single original of graphene
Sublayer structure makes it have many unique physicochemical properties, and these excellent performances make graphene have in field of compound material
The application prospect of light.But graphenic surface does not have functional group, so it has limited disperse in organic solvent
Property, this severely limits application prospect of the graphene in functional material is prepared.
In prepared by graphene chemical method, typically using oxidant by graphite oxidation into graphite oxide, then with reducing agent also
Originally it was graphene, but graphene is easily clumped together, it is not easy to prepare the graphene of individual layer or few layer, seriously constrain stone
The application of black alkene.
Monomer cast nylon (MC nylon) is one of current most widely used general-purpose plastics, and it is at normal temperatures by caprolactam
Decompression dehydration, and be further dehydrated under catalyst action, add activator and be well mixed, injected under certain polymerization temperature
It is polymerized in specific mould.It has low cost, high yield, high reaction rate, HMW and good mechanical performance
The advantages that.MC nylon is widely used at present prepares bearing, gear, pulley etc., especially prepare some can not by compression moulding or
Large-scale device prepared by person's extrusion molding.In recent years, MC nylon progressively substitutes some metal materials in many fields, as copper,
Aluminium, steel and iron etc..But non-modified MC nylon is deposited and worn no resistance under high pressure, impact strength is low, and the bad grade of thermostabilization lacks
Point, with the reach of science and the demand of commercial Application, people propose more performance requirements to MC nylon, so these shortcomings
So that the application of MC nylon materials is limited, therefore many scientific research personnel have been carried out extensively in the antifriction of MC nylon, enhancing, toughness reinforcing etc.
Research.
Graphene-the polyamide compoiste material prepared at present prepares graphene using chemical method more, and this method can be a large amount of
Various acid and chemical reagent are used, preparation method is complicated, seriously polluted, and preparation technology is complicated.
The content of the invention
The technical problem to be solved in the present invention is to provide a kind of simple to operate, acidic materials are not added in preparation process, and
Preparation technology simple possible, the graphene-polyamide compoiste material prepared using this method have excellent combination property, hardness
It is significantly increased with wearability, while tensile strength maintains stabilization with impact strength.
In order to solve the above technical problems, the technical solution adopted in the present invention is as follows：
A kind of quick method for preparing graphene-polyamide compoiste material, this method comprise the following steps：
A, graphite is mixed with surfactant, obtains modified graphite；
B, caprolactam monomer is mixed with the modified graphite in the step (1), adsorbed, obtain being adsorbed with oneself
The modified graphite of amide monomer；
C, NaOH is added into step B, mechanical agitation, is evaporated under reduced pressure out water byproduct, temperature is slowly increased to 130 DEG C, instead
Answer 0.5h；
D, TDI is added into step C, stirs 30s rapidly, reaction solution is poured into rapidly to preheating temperature for 150 DEG C -170 DEG C
Mould in, 150 DEG C -170 DEG C polymerization 1h-3h, be made graphene-polyamide compoiste material.
Wherein, in step A, surfactant includes OPEO, NPE, fatty acid polyglycol
One or more in oxygen ethene fat.
Wherein, the mass ratio of surfactant and graphite is 1 in step B：(5-50).
Wherein, in step B, the mass ratio of modified graphene and caprolactam is 1:(50-100).
Wherein, step B is comprised the following steps that：Caprolactam is heated and melted, by modified graphite dissolving in organic solvent,
Modified graphite solution after dissolving is slowly added into liquid caprolactam solution, stirred, caprolactam heating-up temperature
For 80-120 DEG C.
Further, methods described further comprises step E, and chain extender is added in the reaction solution obtained to step C.
Wherein, the chain extender includes the one or more in diethylene glycol (DEG), triethylene glycol, glycerine, sorbierite.Beneficial to effect
Fruit：The present invention compared with prior art, has following advantage：
1st, in the inventive method, not using strong acid, highly basic, catalyst preparation graphene, reduce environmental pollution, simplify system
Standby technique
2nd, the present invention is surfactant-modified using being carried out to graphite, then mixes modified graphite and caprolactam solution
Close, because graphite surface has organic group, therefore, modified graphite can be with caprolactam monomer quick adsorption, modified graphite surface
It is adsorbed with caprolactam monomer
3rd, during caprolactam monomer polymerize, polymerization stress can realize stone rapidly by graphite layers away from increasing
Glass acts between layer of ink, meanwhile, graphite is peeled off the graphene to be formed and can be uniformly dispersed in polyamide polymer, avoids existing
There is the phenomenon that graphene dispersion is uneven in technology.
4th, the present invention can further add chain extender in modified graphite and caprolactam reaction solution, and chain extender can enter one
The increase graphite layers of step are away from preparing more preferable graphene..
5th, the graphene-polyamide compoiste material prepared using the present invention has excellent mechanical property and wearability, stone
Black alkene is evenly distributed in polyamide, and interface is good.
Brief description of the drawings：
Fig. 1 (a) is polyamide polarisation test chart,
Fig. 1 (b) is graphene-polyamide compoiste material polarisation test chart；
Fig. 2 (a) schemes for polyamide SEM；
Fig. 2 (b) is graphene-polyamide wear surface SEM figures.
Embodiment
(1) in parts by weight, 5g crystalline flake graphites are mixed with 1g NPEs, obtains being modified crystalline flake graphite；
(2) 300g caprolactam monomers are added in reactor, is heated to 80 degrees Celsius, will after caprolactam melting
Modified crystalline flake graphite is added in above-mentioned solution, stirring reaction 1 hour.
(3) 90 DEG C are maintained the temperature at, adds 0.5g sodium hydroxides, reacts 1 hour, is evaporated under reduced pressure out water byproduct, is added
0.5gTDI, 30s is stirred rapidly, reaction solution is poured into rapidly in the mould that preheating temperature is 170 DEG C, polymerize 1h at 170 DEG C.Instead
It should terminate.
Mechanical test is carried out to graphene-polyamide compoiste material, the impact strength of composite is 9.12KJm-2, than
The impact strength of pure polyamide improves 260%
It is that polyamide and graphene-polyamide POM scheme as shown in Fig. 1 (a), Fig. 1 (b), Fig. 1 (a) surveys for polyamide polarisation
Attempt, Fig. 1 (b) is graphene-polyamide compoiste material polarisation test chart.From scheming a, stabilization in polyamide be present
Spherocrystal.From scheming b, add graphene and polyamide spherulite size is reduced, the increase of spherocrystal density.Illustrate graphene for oneself
Implementing anionic lactam polymerisation has nucleation.
If Fig. 2 (a), Fig. 2 (b) are polyamide and graphene-polyamide wear surface SEM figures, Fig. 2 (a) is polyamide SEM
Figure, Fig. 2 (b) are graphene-polyamide wear surface SEM figures, show that serious table occurs in the wear surface of polyamide by scheming a
Face melts and surface tear phenomenon, and this also embodies the characteristics of polyamide wears no resistance at high loads.Graphite is shown by scheming b
The wear surface of alkene-polyamide nano-composite (b) has slight surface breakdown phenomenon, shows that graphene-polyamide is compound
The wearability of material significantly improves.
Graphene-polyamide compoiste material prepared by the present invention has excellent mechanical property and wearability, preparation method
Simple possible.
By above-mentioned implementation column, the present invention reduces environment without using strong acid, highly basic, catalyst preparation graphene
Pollution, simplify preparation technology, and it is surfactant-modified using being carried out to graphite, then by modified graphite and caprolactam solution
Mixing, because graphite surface has organic group, therefore, modified graphite can be with caprolactam monomer quick adsorption, modified graphite table
Face is adsorbed with caprolactam monomer；Caprolactam monomer polymerize during, polymerization stress can rapidly by graphite layers away from
Increase, realize that graphite layers glass acts on, meanwhile, graphite, which peels off the graphene to be formed, can be uniformly dispersed in polyamide polymer
In, avoid the uneven phenomenon of graphene dispersion in the prior art.
The present invention can further add chain extender in modified graphite and caprolactam reaction solution, and chain extender can be further
Increase graphite layers away from preparing more preferable graphene.And graphene-the polyamide compoiste material prepared using the present invention is had
Excellent mechanical property and wearability, graphene are evenly distributed in polyamide, and interface is good.
Above description is only the preferred embodiment of the application and the explanation to institute's application technology principle.People in the art
Member should be appreciated that invention scope involved in the application, however it is not limited to the technology that the particular combination of above-mentioned technical characteristic forms
Scheme, while should also cover in the case where not departing from the inventive concept, carried out by above-mentioned technical characteristic or its equivalent feature
The other technical schemes for being combined and being formed.Such as features described above has similar work(with (but not limited to) disclosed herein
The technical scheme that the technical characteristic of energy is replaced mutually and formed.
Claims (7)
- A kind of 1. quick method for preparing graphene-polyamide compoiste material, it is characterised in that this method comprises the following steps：A, graphite is mixed with surfactant, obtains modified graphite；B, caprolactam monomer is mixed with the modified graphite in the step (1), adsorbed, obtain being adsorbed with caprolactam The modified graphite of monomer；C, NaOH is added into step B, mechanical agitation, is evaporated under reduced pressure out water byproduct, temperature is slowly increased to 130 DEG C, reaction 0.5h；D, TDI is added into step C, stirs 30s rapidly, reaction solution is poured into rapidly to the mould that preheating temperature is 150 DEG C -170 DEG C In tool, in 150 DEG C of -170 DEG C of polymerization 1h-3h, graphene-polyamide compoiste material is made.
- A kind of 2. quick method for preparing graphene-polyamide compoiste material as claimed in claim 1, it is characterised in that institute State in step A, surfactant is included in OPEO, NPE, aliphatic acid polyethenoxy fat One or more.
- A kind of 3. quick method for preparing graphene-polyamide compoiste material as claimed in claim 1, it is characterised in that institute It is 1 to state the mass ratio of surfactant and graphite in step B：(5-50).
- A kind of 4. method of quick graphene-polyamide compoiste material as claimed in claim 1, it is characterised in that the step In rapid B, the mass ratio of modified graphene and caprolactam is 1:(50-100).
- A kind of 5. quick method for preparing graphene-polyamide compoiste material as claimed in claim 1, it is characterised in that institute Step B is stated to comprise the following steps that：Caprolactam is heated and melted, by modified graphite dissolving in organic solvent, after dissolving Modified graphite solution is slowly added into liquid caprolactam solution, is stirred, and caprolactam heating-up temperature is 80-120 DEG C.
- A kind of 6. quick method for preparing graphene-polyamide compoiste material as claimed in claim 1, it is characterised in that institute The method of stating further comprises step E, and chain extender is added in the reaction solution obtained to step C.
- A kind of 7. quick method for preparing graphene-polyamide compoiste material as claimed in claim 6, it is characterised in that institute Stating chain extender includes the one or more in diethylene glycol (DEG), triethylene glycol, glycerine, sorbierite.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108598437A (en) * | 2018-05-03 | 2018-09-28 | 合肥宸翊商贸有限公司 | Lithium ion battery negative material and preparation method thereof suitable for low temperature |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000007180A (en) * | 1998-06-24 | 2000-01-11 | Ntn Corp | Rolling element for sheet carrier of image forming device |
| CN102108123A (en) * | 2009-12-24 | 2011-06-29 | 上海杰事杰新材料(集团)股份有限公司 | Preparation method of nano cast nylon-6/graphite oxide (GO) conductive and bacteriostatic composite material |
| CN105622929A (en) * | 2014-11-06 | 2016-06-01 | 合肥杰事杰新材料股份有限公司 | Casting nylon/graphene nanocomposite material and preparation method thereof |
| CN106276881A (en) * | 2016-08-23 | 2017-01-04 | 黄云鸿 | The preparation method of a kind of Graphene and Graphene |
-
2017
- 2017-10-13 CN CN201710953017.2A patent/CN107793750A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000007180A (en) * | 1998-06-24 | 2000-01-11 | Ntn Corp | Rolling element for sheet carrier of image forming device |
| CN102108123A (en) * | 2009-12-24 | 2011-06-29 | 上海杰事杰新材料(集团)股份有限公司 | Preparation method of nano cast nylon-6/graphite oxide (GO) conductive and bacteriostatic composite material |
| CN105622929A (en) * | 2014-11-06 | 2016-06-01 | 合肥杰事杰新材料股份有限公司 | Casting nylon/graphene nanocomposite material and preparation method thereof |
| CN106276881A (en) * | 2016-08-23 | 2017-01-04 | 黄云鸿 | The preparation method of a kind of Graphene and Graphene |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108598437A (en) * | 2018-05-03 | 2018-09-28 | 合肥宸翊商贸有限公司 | Lithium ion battery negative material and preparation method thereof suitable for low temperature |
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Application publication date: 20180313 |