CN107841106A - Flame-proof polylactic acid graphene composite material and preparation method thereof - Google Patents
Flame-proof polylactic acid graphene composite material and preparation method thereof Download PDFInfo
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- CN107841106A CN107841106A CN201610834262.7A CN201610834262A CN107841106A CN 107841106 A CN107841106 A CN 107841106A CN 201610834262 A CN201610834262 A CN 201610834262A CN 107841106 A CN107841106 A CN 107841106A
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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
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
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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
- C08K2201/00—Specific properties of additives
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
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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
- C08L2201/02—Flame or fire retardant/resistant
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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 flame-proof polylactic acid 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, 6~12 parts of chitosan, 2~8 parts of graphene nanometer sheet, 4~12 parts of carbon fiber, 8~14 parts of glass fibre, 4~8 parts of wollastonite in powder, 1~5 part of Ludox, 10~18 parts of expanded graphite, 2~6 parts of attapulgite, 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 flame-proof polylactic acid graphene composite material.Flame-proof polylactic acid graphene composite material provided by the invention has the advantages of excellent fire-retardancy, 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 flame-proof polylactic acid 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 a kind of good, comprehensive with excellent fire-retardancy, excellent toughness, resistance to elevated temperatures it is necessory to provide
Flame-proof polylactic acid graphene composite material of high mechanical strength and preparation method thereof, to solve the above problems.
The present invention provides a kind of flame-proof polylactic acid graphene composite material, is made up of the raw material of following parts by weight：PLA
50~100 parts, 6~12 parts of chitosan, 2~8 parts of graphene nanometer sheet, 5~15 parts of carbon fiber, 4~12 parts of glass fibre, glass
8~14 parts of fiber, 4~8 parts of wollastonite in powder, 1~5 part of Ludox, 10~18 parts of expanded graphite, 2~6 parts of attapulgite, diamino
1~5 part of four glycidyl amine of base diphenyl-methane, 1~3 part of silane coupler；Wherein, the specific surface area of the graphene nanometer sheet
Reach 80~100m2/ g, and treated by the glycidyl amine of MDA four.
Based on above-mentioned, it is made up of the raw material of following parts by weight：70~90 parts of PLA, 8~10 parts of chitosan, graphene
3~6 parts of nanometer sheet, 6~10 parts of carbon fiber, 10~12 parts of glass fibre, 5~7 parts of wollastonite in powder, 2~4 parts of Ludox, expansion
12~16 parts of graphite, 3~5 parts of attapulgite, 2~4 parts of four glycidyl amine of MDA, silane coupler 1~3
Part.
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 wollastonite in powder is less than 40 μm.
The present invention also provides a kind of preparation method of above-mentioned flame-proof polylactic acid graphene composite material, specific preparation method step
It is rapid 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, wollastonite in powder, silane coupler, Ludox, expanded graphite,
Attapulgite, the glycidyl amine of MDA four are according to said ratio in the min of high-speed mixer and mixing 10~30, mixing
Added after uniformly in the hopper of double screw extruder, by carbon fiber and glass fibre by a certain percentage from double screw extruder
Add and added in fine mouth, extruded through melt blending, extruded material dries up pelletizing after cold go, and the flame-proof polylactic acid graphene is made
Composite.
Compared with prior art, flame-proof polylactic acid graphene composite material provided by the invention has advantages below：First,
The graphene nanometer sheet of the glycidyl amine of MDA four surface treatment is prepared using solution blended process, stone can be made
Black alkene nanometer sheet has good compatibility with matrix resin；Secondly, the glycidyl amine of MDA four possesses larger
Relative molecular mass, but show very low viscosity, thus be used to reduce polymer melt viscosity, improve polymer
Fluidity of molten；In addition, having active hydroxyl and amino in chitosan macromolecular, they have stronger chemical reaction ability,
By producing interaction with other radical reactions or with matrix, toughening effect is splendid；The addition of wollastonite in powder can then improve
The mechanical strength of polymer；Ludox can increase the heat resistance and intensity of polymer；Expanded graphite is expansion type flame retardant
With attapulgite phyllosilicate nano material compositional flame-retardant, continuous and fine and close layer of charcoal can be formed in matrix surface, and
It will not produce and melt drop；Graphene has the advantages that high temperature resistant, excellent pliability and high intensity；Therefore, resistance provided by the invention
Combustion PLA graphene composite material has good, comprehensive mechanical intensity height of excellent fire-retardancy, excellent toughness, resistance to elevated temperatures etc.
Advantage.
Embodiment
Below by embodiment, technical scheme is described in further detail.
Embodiment 1
The embodiment of the present invention provides a kind of flame-proof polylactic acid graphene composite material, and it is made up of the raw material of following parts by weight：It is poly-
50 parts of lactic acid, 6 parts of chitosan, 2 parts of graphene nanometer sheet, 4 parts of carbon fiber, 8 parts of glass fibre, 4 parts of wollastonite in powder, Ludox 1
Part, 10 parts of expanded graphite, 2 parts of attapulgite, 1 part of four glycidyl amine of MDA and Silane coupling agent KH550 1
Part；Wherein, the weight average molecular weight of the PLA is 100,000, and fusing point is 60 DEG C；Carbon fiber and glass fibre are all by silane
What coupling agent KH550 was treated.
The preparation method for the above-mentioned flame-proof polylactic acid 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 87 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, wollastonite in powder, Silane coupling agent KH550, Ludox, expansion
Graphite, attapulgite, the glycidyl amine of MDA four are according to said ratio in the min of high-speed mixer and mixing 10, mixing
Added after uniformly in the hopper of double screw extruder, by carbon fiber and glass fibre by a certain percentage from double screw extruder
Add and added in fine mouth, extruded through melt blending, extruded material dries up pelletizing after cold go, and the flame-proof polylactic acid graphene is made
Composite.
Embodiment 2
The embodiment of the present invention provides a kind of flame-proof polylactic acid graphene composite material, and it is made up of the raw material of following parts by weight：It is poly-
70 parts of lactic acid, 8 parts of chitosan, 3 parts of graphene nanometer sheet, 6 parts of carbon fiber, 10 parts of glass fibre, 5 parts of wollastonite in powder, Ludox 2
Part, 12 parts of expanded graphite, 3 parts of attapulgite, 2 parts of four glycidyl amine of MDA, silane coupler KH560 2
Part；Wherein, the weight average molecular weight of the PLA is 300,000, and fusing point is 60 DEG C；Carbon fiber and glass fibre are all by silane
What coupling agent KH560 was treated.
The preparation method for the above-mentioned flame-proof polylactic acid 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 91 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, wollastonite in powder, silane coupler KH560, Ludox, expansion
Graphite, attapulgite, the glycidyl amine of MDA four are according to said ratio in the min of high-speed mixer and mixing 15, mixing
Added after uniformly in the hopper of double screw extruder, by carbon fiber and glass fibre by a certain percentage from double screw extruder
Add and added in fine mouth, extruded through melt blending, extruded material dries up pelletizing after cold go, and the flame-proof polylactic acid graphene is made
Composite.
Embodiment 3
The embodiment of the present invention provides a kind of flame-proof polylactic acid graphene composite material, and it is made up of the raw material of following parts by weight：It is poly-
80 parts of lactic acid, 9 parts of chitosan, 5 parts of graphene nanometer sheet, 8 parts of carbon fiber, 11 parts of glass fibre, 6 parts of wollastonite in powder, Ludox 3
Part, 14 parts of expanded graphite, 4 parts of attapulgite, 4 parts of four glycidyl amine of MDA, silane coupler KH570 2
Part；Wherein, the weight average molecular weight of the PLA is 500,000, and fusing point is 60 DEG C；Carbon fiber and glass fibre are all by silane
What coupling agent KH570 was treated.
The preparation method for the above-mentioned flame-proof polylactic acid 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 98 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, wollastonite in powder, silane coupler KH570, Ludox, expansion
Graphite, attapulgite, the glycidyl amine of MDA four are according to said ratio in the min of high-speed mixer and mixing 20, mixing
Added after uniformly in the hopper of double screw extruder, by carbon fiber and glass fibre by a certain percentage from double screw extruder
Add and added in fine mouth, extruded through melt blending, extruded material dries up pelletizing after cold go, and the flame-proof polylactic acid graphene is made
Composite.
Embodiment 4
The embodiment of the present invention provides a kind of flame-proof polylactic acid graphene composite material, and it is made up of the raw material of following parts by weight：It is poly-
90 parts of lactic acid, 10 parts of chitosan, 6 parts of graphene nanometer sheet, 10 parts of carbon fiber, 12 parts of glass fibre, 8 parts of wollastonite in powder, silicon are molten
4 parts of glue, 16 parts of expanded graphite, 5 parts of attapulgite, 4 parts of four glycidyl amine of MDA, silane coupler KH792
3 parts；Wherein, the weight average molecular weight of the PLA is 700,000, and fusing point is 60 DEG C；Carbon fiber and glass fibre are all by silane
What coupling agent KH792 was treated.
The preparation method for the above-mentioned flame-proof polylactic acid 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 81 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, wollastonite in powder, silane coupler KH792, Ludox, expansion
Graphite, attapulgite, the glycidyl amine of MDA four are according to said ratio in the min of high-speed mixer and mixing 25, mixing
Added after uniformly in the hopper of double screw extruder, by carbon fiber and glass fibre by a certain percentage from double screw extruder
Add and added in fine mouth, extruded through melt blending, extruded material dries up pelletizing after cold go, and the flame-proof polylactic acid graphene is made
Composite.
Embodiment 5
The embodiment of the present invention provides a kind of flame-proof polylactic acid graphene composite material, and it is made up of the raw material of following parts by weight：It is poly-
100 parts of lactic acid, 12 parts of chitosan, 8 parts of graphene nanometer sheet, 12 parts of carbon fiber, 12 parts of glass fibre, 8 parts of wollastonite in powder, silicon are molten
5 parts of glue, 18 parts of expanded graphite, 6 parts of attapulgite, 5 parts of four glycidyl amine of MDA, silane coupler KH560
3 parts；Wherein, the weight average molecular weight of the PLA is 800,000, and fusing point is 60 DEG C；Carbon fiber and glass fibre are all by silane
What coupling agent KH560 was treated.
The preparation method for the above-mentioned flame-proof polylactic acid 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 94 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, wollastonite in powder, silane coupler KH560, Ludox, expansion
Graphite, attapulgite, the glycidyl amine of MDA four are according to said ratio in the min of high-speed mixer and mixing 30, mixing
Added after uniformly in the hopper of double screw extruder, by carbon fiber and glass fibre by a certain percentage from double screw extruder
Add and added in fine mouth, extruded through melt blending, extruded material dries up pelletizing after cold go, and the flame-proof polylactic acid graphene is made
Composite.
According to national standard, items are carried out to the flame-proof polylactic acid graphene composite material that above-described embodiment 1~5 provides
It can test, test result is 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（%） | Oxygen index (OI) |
| Embodiment 1 | 95.2 | 82 | 30 | 83 | 83.4 | 29 |
| Embodiment 2 | 98.9 | 87 | 35 | 89 | 80.9 | 30 |
| Embodiment 3 | 117.1 | 92 | 41 | 92 | 79.5 | 32 |
| Embodiment 4 | 112.8 | 96 | 42 | 91 | 79.1 | 33 |
| Embodiment 5 | 106.3 | 84 | 38 | 87 | 78.6 | 34 |
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 flame-proof polylactic acid graphene composite material, it is characterised in that it is made up of the raw material of following parts by weight：PLA
50~100 parts, 6~12 parts of chitosan, 2~8 parts of graphene nanometer sheet, 4~12 parts of carbon fiber, 8~14 parts of glass fibre, silicon ash
4~8 parts of stone flour, 1~5 part of Ludox, 10~18 parts of expanded graphite, 2~6 parts of attapulgite, MDA four shrink
1~5 part of glyceramine, 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.
2. flame-proof polylactic acid graphene composite material according to claim 1, it is characterised in that it is by following parts by weight
Raw material is made：70~90 parts of PLA, 8~10 parts of chitosan, 3~6 parts of graphene nanometer sheet, 6~10 parts of carbon fiber, glass fibers
10~12 parts of dimension, 5~7 parts of wollastonite in powder, 2~4 parts of Ludox, 12~16 parts of expanded graphite, 3~5 parts of attapulgite, diaminourea
2~4 parts of four glycidyl amine of diphenyl-methane, 1~3 part of silane coupler.
3. flame-proof polylactic acid graphene composite material according to claim 1 or 2, it is characterised in that described silane coupled
Agent is Silane coupling agent KH550, silane coupler KH560, silane coupler KH570 or silane coupler KH792.
4. flame-proof polylactic acid graphene composite material according to claim 1 or 2, it is characterised in that the PLA
Weight average molecular weight is 100,000~800,000, and fusing point is 60 DEG C.
5. flame-proof polylactic acid graphene composite material according to claim 1 or 2, it is characterised in that the carbon fiber and
The glass fibre is treated through silane coupler.
6. flame-proof polylactic acid graphene composite material according to claim 1 or 2, it is characterised in that the wollastonite in powder
Particle diameter be less than 40 μm.
7. a kind of preparation method of the flame-proof polylactic acid graphene composite material described in any one of claim 1~6, specific to prepare
Method and 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, wollastonite in powder, silane coupler, Ludox, expanded graphite,
Attapulgite, the glycidyl amine of MDA four are according to said ratio in the min of high-speed mixer and mixing 10~30, mixing
Added after uniformly in the hopper of double screw extruder, by carbon fiber and glass fibre by a certain percentage from double screw extruder
Add and added in fine mouth, extruded through melt blending, extruded material dries up pelletizing after cold go, and the flame-proof polylactic acid graphene is made
Composite.
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| CN201610834262.7A CN107841106A (en) | 2016-09-20 | 2016-09-20 | Flame-proof polylactic acid graphene composite material and preparation method thereof |
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| CN201610834262.7A CN107841106A (en) | 2016-09-20 | 2016-09-20 | Flame-proof polylactic acid graphene composite material and preparation method thereof |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
-
2016
- 2016-09-20 CN CN201610834262.7A patent/CN107841106A/en not_active Withdrawn
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Non-Patent Citations (1)
| Title |
|---|
| 吴改红等: "《聚乳酸纤维及其纺织品》", 31 May 2014, 东华大学出版社 * |
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Application publication date: 20180327 |