CN107841104A - High temperature resistant PLA graphene composite material and preparation method thereof - Google Patents
High temperature resistant PLA graphene composite material and preparation method thereof Download PDFInfo
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- CN107841104A CN107841104A CN201610834238.3A CN201610834238A CN107841104A CN 107841104 A CN107841104 A CN 107841104A CN 201610834238 A CN201610834238 A CN 201610834238A CN 107841104 A CN107841104 A CN 107841104A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
- C08L67/04—Polyesters derived from hydroxycarboxylic acids, e.g. lactones
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
Abstract
The invention provides a kind of high temperature resistant PLA graphene composite material, it is characterised in that it is made up of the raw material of following parts by weight：50~100 parts of PLA, 4~10 parts of chitosan, 2~8 parts of graphene nanometer sheet, 5~14 parts of carbon fiber, 8~14 parts of glass fibre, 6~12 parts of talcum powder, 1~5 part of Ludox, 1~5 part of four glycidyl amine of MDA, 1~3 part of silane coupler；Wherein, the specific surface area of the graphene nanometer sheet reaches 80~100m2/ g, and treated by the glycidyl amine of MDA four.The present invention also provides a kind of preparation method of above-mentioned high temperature resistant PLA graphene composite material.High temperature resistant PLA graphene composite material provided by the invention has the advantages of excellent toughness, resistance to elevated temperatures are good, comprehensive mechanical intensity is high.
Description
Technical field
The present invention relates to a kind of lactic acid composite material, and in particular to a kind of high temperature resistant PLA graphene composite material and
Its preparation method.
Background technology
PLA（English abbreviation：PLA）It is a kind of thermoplastic aliphatic's polyester, produces the lactic acid and third required for PLA
Lactide can be fermented by renewable resource, be dehydrated, be obtained after purification, resulting PLA typically have good machinery and
Processing characteristics, and poly-lactic acid products it is discarded after can be that one kind possesses good performance by various mode fast degradations
Green plastic.But PLA material is more crisp in itself, and heat resistance is poor, and this significantly limit its application.
Graphene nanometer sheet, guide number Ss（Graphene nanosheets）Or GNFs (Graphene
NanoFlakes), it is to be formed by single layer of carbon atom planar structure graphene stacking, thickness is the bidimensional Nano graphite of nanoscale
Material, its extreme case are single-layer graphenes, and it has larger specific surface area and layer structure, can be formed in the base very
Good supporting network structure, there is far-reaching Research Significance for improving PLA properties.
The content of the invention
In view of this, it is necessory to provide it is a kind of with excellent toughness, that resistance to elevated temperatures is good, comprehensive mechanical intensity is high is resistance to
High temperature PLA graphene composite material and preparation method thereof, to solve the above problems.
The present invention provides a kind of high temperature resistant PLA graphene composite material, is made up of the raw material of following parts by weight：Poly- breast
50~100 parts of acid, 4~10 parts of chitosan, 2~8 parts of graphene nanometer sheet, 5~14 parts of carbon fiber, 8~14 parts of glass fibre, cunning
6~12 parts of stone flour, 1~5 part of Ludox, 1~5 part of four glycidyl amine of MDA, 1~3 part of silane coupler；Its
In, the specific surface area of the graphene nanometer sheet reaches 80~100m2/ g, and pass through the glycidol of MDA four
Amine treats.
Based on above-mentioned, it is made up of the raw material of following parts by weight：70~90 parts of PLA, 5~8 parts of chitosan, graphene
3~6 parts of nanometer sheet, 7~11 parts of carbon fiber, 9~12 parts of glass fibre, 8~10 parts of talcum powder, 2~4 parts of Ludox, diaminourea
2~4 parts of four glycidyl amine of diphenyl-methane, 1~3 part of silane coupler.
Based on above-mentioned, the silane coupler is Silane coupling agent KH550, silane coupler KH560, silane coupler
KH570 or silane coupler KH792.
Based on above-mentioned, the weight average molecular weight of the PLA is 100,000~800,000, and fusing point is 60 DEG C.
Based on above-mentioned, the carbon fiber is treated through silane coupler.
Based on above-mentioned, the glass fibre is treated through silane coupler.
Wherein, the particle diameter of the silicon dioxide granule in the Ludox is 580nm, and the content of silicon dioxide granule is
20%~30%.Based on above-mentioned, the particle diameter of the talcum powder is less than 40 μm.
The present invention also provides a kind of preparation method of above-mentioned high temperature resistant PLA graphene composite material, specific preparation method
Step is as follows：
（1）The processing of graphene nanometer sheet
Graphene nanometer sheet is positioned in DMF solvent together with the glycidyl amine of MDA four, mechanical agitation is held
It is continuous 1~3 hour, 500~1500rpm of rotating speed, after being well mixed, it is positioned in drying oven, temperature control is at 45 DEG C~55 DEG C
Persistently dry 6 hours, obtain the graphene nanometer sheet of surface modification；
（2）The graphene nanometer sheet that the surface is modified and PLA mix particles is uniform, in three-roll grinder grind 20~
30 min, obtain PLA graphene mixture；
（3）By the PLA graphene mixture and chitosan, talcum powder, silane coupler, Ludox, diaminourea hexichol first
In the min of high-speed mixer and mixing 10~30, double screw extruder is added after well mixed according to said ratio for the glycidyl amine of alkane four
Hopper in, by carbon fiber and glass fibre by a certain percentage from double screw extruder plus added in fine mouth, through melting altogether
Mixed extrusion, extruded material dry up pelletizing after cold go, and the high temperature resistant PLA graphene composite material is made.
Compared with prior art, high temperature resistant PLA graphene composite material provided by the invention has advantages below：It is first
First, the graphene nanometer sheet of the glycidyl amine of MDA four surface treatment is prepared using solution blended process, can
Make graphene nanometer sheet and matrix resin that there is good compatibility；Secondly, the glycidyl amine of MDA four possesses
Larger relative molecular mass, very low viscosity is but shown, therefore be used to reduce the melt viscosity of polymer, improve polymerization
The fluidity of molten of thing；In addition, having active hydroxyl and amino in chitosan macromolecular, they have stronger chemical reaction energy
Power, by producing interaction with other radical reactions or with matrix, toughening effect is splendid；The addition of talcum powder can then improve
Mechanical strength, creep resistance and the pliability of polymer；Ludox can increase the heat resistance and intensity of polymer；Graphene
There is high temperature resistant, excellent pliability and high intensity；Therefore, high temperature resistant PLA graphene provided by the invention is compound
Material has the advantages that excellent toughness, resistance to elevated temperatures are good, comprehensive mechanical intensity is high.
Embodiment
Below by embodiment, technical scheme is described in further detail.
Embodiment 1
The embodiment of the present invention provides a kind of high temperature resistant PLA graphene composite material, and it is made up of the raw material of following parts by weight：
50 parts of PLA, 4 parts of chitosan, 2 parts of graphene nanometer sheet, 5 parts of carbon fiber, 8 parts of glass fibre, 6 parts of talcum powder, Ludox 1
1 part of part, 1 part of four glycidyl amine of MDA and Silane coupling agent KH550；Wherein, the PLA is divided equally again
Son amount is 100,000, and fusing point is 60 DEG C；Carbon fiber and glass fibre are all treated by Silane coupling agent KH550.
The preparation method for the above-mentioned high temperature resistant PLA graphene composite material that the present embodiment provides comprises the following steps：
（1）Graphene nanometer sheet is positioned in DMF solvent together with the glycidyl amine of MDA four, mechanical agitation
Continue 1 hour, the rpm of rotating speed 700, after being well mixed, be positioned in drying oven, temperature control 45 DEG C persistently drying it is 6 small
When, the graphene nanometer sheet of surface modification is obtained, and its specific surface area reaches 86 m2/g；
（2）The graphene nanometer sheet that the surface is modified and PLA mix particles is uniform, 20 are ground in three-roll grinder
Min, obtain PLA graphene mixture；
（3）By the PLA graphene mixture and chitosan, talcum powder, Silane coupling agent KH550, Ludox, diaminourea
In the min of high-speed mixer and mixing 10, twin-screw extrusion is added after well mixed according to said ratio for the glycidyl amine of diphenyl-methane four
In the hopper of machine, carbon fiber and glass fibre are added from adding in fine mouth for double screw extruder by a certain percentage, through melting
Blending extrusion, extruded material dry up pelletizing after cold go, and the high temperature resistant PLA graphene composite material is made.
Embodiment 2
The embodiment of the present invention provides a kind of high temperature resistant PLA graphene composite material, and it is made up of the raw material of following parts by weight：
70 parts of PLA, 5 parts of chitosan, 3 parts of graphene nanometer sheet, 7 parts of carbon fiber, 9 parts of glass fibre, 8 parts of talcum powder, Ludox 2
Part, 2 parts of four glycidyl amine of MDA, 2 parts of silane coupler KH560；Wherein, the PLA is divided equally again
Son amount is 300,000, and fusing point is 60 DEG C；Carbon fiber and glass fibre are all treated by silane coupler KH560.
The preparation method for the above-mentioned high temperature resistant PLA graphene composite material that the present embodiment provides comprises the following steps：
（1）Graphene nanometer sheet is positioned in DMF solvent together with the glycidyl amine of MDA four, mechanical agitation
Continue 2 hours, the rpm of rotating speed 800, after being well mixed, be positioned in drying oven, temperature control 50 DEG C persistently drying it is 6 small
When, the graphene nanometer sheet of surface modification is obtained, and its specific surface area reaches 92 m2/g；
（2）The graphene nanometer sheet that the surface is modified and PLA mix particles is uniform, 20 are ground in three-roll grinder
Min, obtain PLA graphene mixture；
（3）By the PLA graphene mixture and chitosan, talcum powder, silane coupler KH560, Ludox, diaminourea
In the min of high-speed mixer and mixing 15, twin-screw extrusion is added after well mixed according to said ratio for the glycidyl amine of diphenyl-methane four
In the hopper of machine, carbon fiber and glass fibre are added from adding in fine mouth for double screw extruder by a certain percentage, through melting
Blending extrusion, extruded material dry up pelletizing after cold go, and the high temperature resistant PLA graphene composite material is made.
Embodiment 3
The embodiment of the present invention provides a kind of high temperature resistant PLA graphene composite material, and it is made up of the raw material of following parts by weight：
80 parts of PLA, 7 parts of chitosan, 5 parts of graphene nanometer sheet, 9 parts of carbon fiber, 11 parts of glass fibre, 9 parts of talcum powder, Ludox 3
Part, 4 parts of four glycidyl amine of MDA, 2 parts of silane coupler KH570；Wherein, the PLA is divided equally again
Son amount is 500,000, and fusing point is 60 DEG C；Carbon fiber and glass fibre are all treated by silane coupler KH570.
The preparation method for the above-mentioned high temperature resistant PLA graphene composite material that the present embodiment provides comprises the following steps：
（1）Graphene nanometer sheet is positioned in DMF solvent together with the glycidyl amine of MDA four, mechanical agitation
Continue 2 hours, the rpm of rotating speed 1000, after being well mixed, be positioned in drying oven, temperature control 50 DEG C persistently drying it is 6 small
When, the graphene nanometer sheet of surface modification is obtained, and its specific surface area reaches 99 m2/g；
（2）The graphene nanometer sheet that the surface is modified and PLA mix particles is uniform, 25 are ground in three-roll grinder
Min, obtain PLA graphene mixture；
（3）By the PLA graphene mixture and chitosan, talcum powder, silane coupler KH570, Ludox, diaminourea
In the min of high-speed mixer and mixing 20, twin-screw extrusion is added after well mixed according to said ratio for the glycidyl amine of diphenyl-methane four
In the hopper of machine, carbon fiber and glass fibre are added from adding in fine mouth for double screw extruder by a certain percentage, through melting
Blending extrusion, extruded material dry up pelletizing after cold go, and the high temperature resistant PLA graphene composite material is made.
Embodiment 4
The embodiment of the present invention provides a kind of high temperature resistant PLA graphene composite material, and it is made up of the raw material of following parts by weight：
90 parts of PLA, 8 parts of chitosan, 6 parts of graphene nanometer sheet, 11 parts of carbon fiber, 12 parts of glass fibre, 12 parts of talcum powder, silicon are molten
4 parts of glue, 4 parts of four glycidyl amine of MDA, 3 parts of silane coupler KH792；Wherein, the weight of the PLA is equal
Molecular weight is 700,000, and fusing point is 60 DEG C；Carbon fiber and glass fibre are all treated by silane coupler KH792.
The preparation method for the above-mentioned high temperature resistant PLA graphene composite material that the present embodiment provides comprises the following steps：
（1）Graphene nanometer sheet is positioned in DMF solvent together with the glycidyl amine of MDA four, mechanical agitation
Continue 2 hours, the rpm of rotating speed 1100, after being well mixed, be positioned in drying oven, temperature control 50 DEG C persistently drying it is 6 small
When, the graphene nanometer sheet of surface modification is obtained, and its specific surface area reaches 89 m2/g；
（2）The graphene nanometer sheet that the surface is modified and PLA mix particles is uniform, 30 are ground in three-roll grinder
Min, obtain PLA graphene mixture；
（3）By the PLA graphene mixture and chitosan, talcum powder, silane coupler KH792, Ludox, diaminourea
In the min of high-speed mixer and mixing 25, twin-screw extrusion is added after well mixed according to said ratio for the glycidyl amine of diphenyl-methane four
In the hopper of machine, carbon fiber and glass fibre are added from adding in fine mouth for double screw extruder by a certain percentage, through melting
Blending extrusion, extruded material dry up pelletizing after cold go, and the high temperature resistant PLA graphene composite material is made.
Embodiment 5
The embodiment of the present invention provides a kind of high temperature resistant PLA graphene composite material, and it is made up of the raw material of following parts by weight：
100 parts of PLA, 10 parts of chitosan, 8 parts of graphene nanometer sheet, 14 parts of carbon fiber, 14 parts of glass fibre, 12 parts of talcum powder, silicon
5 parts of colloidal sol, 5 parts of four glycidyl amine of MDA, 3 parts of silane coupler KH560；Wherein, the weight of the PLA
Average molecular weight is 800,000, and fusing point is 60 DEG C；Carbon fiber and glass fibre are all treated by silane coupler KH560.
The preparation method for the above-mentioned high temperature resistant PLA graphene composite material that the present embodiment provides comprises the following steps：
（1）Graphene nanometer sheet is positioned in DMF solvent together with the glycidyl amine of MDA four, mechanical agitation
Continue 3 hours, the rpm of rotating speed 1400, after being well mixed, be positioned in drying oven, temperature control 55 DEG C persistently drying it is 6 small
When, the graphene nanometer sheet of surface modification is obtained, and its specific surface area reaches 93 m2/g；
（2）The graphene nanometer sheet that the surface is modified and PLA mix particles is uniform, 30 are ground in three-roll grinder
Min, obtain PLA graphene mixture；
（3）By the PLA graphene mixture and chitosan, talcum powder, silane coupler KH560, Ludox, diaminourea
In the min of high-speed mixer and mixing 30, twin-screw extrusion is added after well mixed according to said ratio for the glycidyl amine of diphenyl-methane four
In the hopper of machine, carbon fiber and glass fibre are added from adding in fine mouth for double screw extruder by a certain percentage, through melting
Blending extrusion, extruded material dry up pelletizing after cold go, and the high temperature resistant PLA graphene composite material is made.
According to national standard, the high temperature resistant PLA graphene composite material that above-described embodiment 1~5 provides is carried out every
Performance test, test result are as shown in the table：
| Project | Tensile strength（MPa） | Bending strength（MPa） | Unnotched impact strength (KJ/m2) | Heat distortion temperature (0.18MPa/ DEG C) | Strength retention（%） |
| Embodiment 1 | 90.7 | 79.6 | 28.7 | 77.9 | 83.5 |
| Embodiment 2 | 97.5 | 85.5 | 32.5 | 84.5 | 80.8 |
| Embodiment 3 | 117.4 | 89.1 | 38.4 | 88.3 | 79.3 |
| Embodiment 4 | 112.1 | 93.3 | 39.1 | 86.9 | 79.1 |
| Embodiment 5 | 101.8 | 81.9 | 35.6 | 80.7 | 78.7 |
Note：It is strong that strength retention refers to that obtained composite soaks 24 h drying process post-tensioning in 80 DEG C of waters bath with thermostatic control
Spend the rate of change relative to untreated composite.
Finally it should be noted that：The above embodiments are merely illustrative of the technical scheme of the present invention and are not intended to be limiting thereof；To the greatest extent
The present invention is described in detail with reference to preferred embodiments for pipe, those of ordinary skills in the art should understand that：Still
The embodiment of the present invention can be modified or equivalent substitution is carried out to some technical characteristics；Without departing from this hair
The spirit of bright technical scheme, it all should cover among the claimed technical scheme scope of the present invention.
Claims (7)
1. a kind of high temperature resistant PLA graphene composite material, it is characterised in that it is made up of the raw material of following parts by weight：Poly- breast
50~100 parts of acid, 4~10 parts of chitosan, 2~8 parts of graphene nanometer sheet, 5~14 parts of carbon fiber, 8~14 parts of glass fibre, cunning
6~12 parts of stone flour, 1~5 part of Ludox, 1~5 part of four glycidyl amine of MDA, 1~3 part of silane coupler；Its
In, the specific surface area of the graphene nanometer sheet reaches 80~100m2/ g, and pass through the glycidol of MDA four
Amine treats.
2. high temperature resistant PLA graphene composite material according to claim 1, it is characterised in that it is by following parts by weight
Raw material be made：70~90 parts of PLA, 5~8 parts of chitosan, 3~6 parts of graphene nanometer sheet, 7~11 parts of carbon fiber, glass
9~12 parts of fiber, 8~10 parts of talcum powder, 2~4 parts of Ludox, 2~4 parts of four glycidyl amine of MDA, silane
1~3 part of coupling agent.
3. high temperature resistant PLA graphene composite material according to claim 1 or 2, it is characterised in that the silane is even
Connection agent is Silane coupling agent KH550, silane coupler KH560, silane coupler KH570 or silane coupler KH792.
4. high temperature resistant PLA graphene composite material according to claim 1 or 2, it is characterised in that the PLA
Weight average molecular weight be 100,000~800,000, fusing point be 60 DEG C.
5. high temperature resistant PLA graphene composite material according to claim 1 or 2, it is characterised in that the carbon fiber
It is treated through silane coupler with the glass fibre.
6. high temperature resistant PLA graphene composite material according to claim 1 or 2, it is characterised in that the talcum powder
Particle diameter be less than 40 μm.
7. a kind of preparation method of the high temperature resistant PLA graphene composite material described in any one of claim 1~6, specific system
Preparation Method step is as follows：
（1）Graphene nanometer sheet is positioned in DMF solvent together with the glycidyl amine of MDA four, mechanical agitation
Continue 1~3 hour, 500~1500rpm of rotating speed, after being well mixed, be positioned in drying oven, temperature control is 45 DEG C~55
DEG C persistently dry 6 hours, obtain the graphene nanometer sheet of surface modification；
（2）The graphene nanometer sheet that the surface is modified and PLA mix particles is uniform, in three-roll grinder grind 20~
30 min, obtain PLA graphene mixture；
（3）By the PLA graphene mixture and chitosan, talcum powder, silane coupler, Ludox, diaminourea hexichol first
In the min of high-speed mixer and mixing 10~30, double screw extruder is added after well mixed according to said ratio for the glycidyl amine of alkane four
Hopper in, by carbon fiber and glass fibre by a certain percentage from double screw extruder plus added in fine mouth, through melting altogether
Mixed extrusion, extruded material dry up pelletizing after cold go, and the high temperature resistant PLA graphene composite material is made.
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| CN201610834238.3A CN107841104A (en) | 2016-09-20 | 2016-09-20 | High temperature resistant PLA graphene composite material and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610834238.3A CN107841104A (en) | 2016-09-20 | 2016-09-20 | High temperature resistant PLA graphene composite material and preparation method thereof |
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| CN107841104A true CN107841104A (en) | 2018-03-27 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109021522A (en) * | 2018-07-10 | 2018-12-18 | 济南开发区星火科学技术研究院 | A kind of preparation method of ultrahigh-strength graphene modified polymer material |
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| CN103772926A (en) * | 2013-12-18 | 2014-05-07 | 江苏悦达新材料科技有限公司 | High-performance flame-retardant PLA (polylactic acid)/graphene nano-sheet composite material and preparation method thereof |
| CN105602216A (en) * | 2016-02-02 | 2016-05-25 | 奇瑞汽车股份有限公司 | Carbon fiber reinforced heatproof flame-retardant polylactic acid composite material and preparation method thereof |
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2016
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103772926A (en) * | 2013-12-18 | 2014-05-07 | 江苏悦达新材料科技有限公司 | High-performance flame-retardant PLA (polylactic acid)/graphene nano-sheet composite material and preparation method thereof |
| CN105602216A (en) * | 2016-02-02 | 2016-05-25 | 奇瑞汽车股份有限公司 | Carbon fiber reinforced heatproof flame-retardant polylactic acid composite material and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109021522A (en) * | 2018-07-10 | 2018-12-18 | 济南开发区星火科学技术研究院 | A kind of preparation method of ultrahigh-strength graphene modified polymer material |
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Application publication date: 20180327 |