CN109251495A - The method of 3D printing molded graphite alkene composite material - Google Patents
The method of 3D printing molded graphite alkene composite material Download PDFInfo
- Publication number
- CN109251495A CN109251495A CN201811059824.0A CN201811059824A CN109251495A CN 109251495 A CN109251495 A CN 109251495A CN 201811059824 A CN201811059824 A CN 201811059824A CN 109251495 A CN109251495 A CN 109251495A
- Authority
- CN
- China
- Prior art keywords
- mixed liquor
- mixed
- composite material
- printing
- obtains
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- 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
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y70/00—Materials specially adapted for additive manufacturing
-
- 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
- C08K3/042—Graphene or derivatives, e.g. graphene oxides
-
- 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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
-
- 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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
-
- 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
- C08K2201/011—Nanostructured additives
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Carbon And Carbon Compounds (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a kind of method of 3D printing molded graphite alkene composite material, include the following steps: the alcohol mixeding liquid for configuring silane coupling agent；Nano aluminium oxide is added into the alcohol mixeding liquid of silane coupling agent, and carries out mechanical stirring, obtains the second mixed liquor；Graphene nanometer sheet is added into the second mixed liquor, be stirred by ultrasonic then progress ball milling, obtains the 5th mixed liquor；Polylactic acid powder is provided；Polylactic acid is dissolved in ethyl alcohol, obtains mixed liquor A；The 5th mixed liquor is added into mixed liquor A, obtains mixed liquid B；Mechanical stirring is carried out to mixed liquid B, obtains mixed liquor C；Ball milling is carried out to mixed liquor C, obtains mixed liquor D；Mixed liquor D is dried, the mixed-powder of polydactyl acid is obtained；The mixed-powder of polydactyl acid is subjected to extrusion molding, obtains the graphene composite material pellet for 3D printing；And the graphene composite material pellet for being used for 3D printing is formed into graphene composite material using 3D printing.
Description
Technical field
The present invention relates to 3D printing technique fields, especially with regard to a kind of side of 3D printing molded graphite alkene composite material
Method.
Background technique
In recent years, 3D printing is in a manner of its special increasing material manufacturing, in product prototype, jewelry-making, bioengineering and doctor
Etc. fields are quickly grown.3D printing is that it mainly utilizes calculating mechanism with traditional " removal type " manufacture difference
It makes the model of three-dimensional structure and controls material and form object in next one layer heap of the layer product of instruction of computer code to realize increasing material
Manufacture.Currently, the molding mode multiplicity of 3D printing, such as precinct laser sintering, Stereolithography, fused glass pellet (FDM)
[7], easily operated and become domestic the most widely used technology wherein since FDM molding equipment is simple.Suitable for FDM 3D
The material category of printing is based on plastics, such as polylactic acid (PLA), acrylonitrile-butadiene-polyglass, polycarbonate,
Extensive concern of the middle PLA due to the characteristic with fully biodegradable and by researcher, but that there are prices is high by PLA
Disadvantage.
The information disclosed in the background technology section is intended only to increase the understanding to general background of the invention, without answering
When being considered as recognizing or imply that the information constitutes the prior art already known to those of ordinary skill in the art in any form.
Summary of the invention
The purpose of the present invention is to provide a kind of methods of 3D printing molded graphite alkene composite material, can overcome existing
The shortcomings that technology.
To achieve the above object, the present invention provides a kind of methods of 3D printing molded graphite alkene composite material, including such as
Lower step: the alcohol mixeding liquid of silane coupling agent is configured；Nano aluminium oxide is added into the alcohol mixeding liquid of silane coupling agent, obtains
To the first mixed liquor, wherein in the first mixed liquor, silane coupling agent concentration is 0.1-0.3g/mL, and nano oxidized aluminum concentration is
1-2g/mL；Mechanical stirring is carried out to the first mixed liquor, obtains the second mixed liquor；Graphene nano is added into the second mixed liquor
Piece obtains third mixed liquor wherein, and in third mixed liquor, graphene nanometer sheet concentration is 0.1-0.2g/mL；Third is mixed
Liquid is stirred by ultrasonic, and the 4th mixed liquor is obtained；Ball milling is carried out to the 4th mixed liquor, obtains the 5th mixed liquor；Polylactic acid is provided
Powder；Polylactic acid is dissolved in ethyl alcohol, obtains mixed liquor A, wherein PLA concentration is 1-2g/mL；The 5th is added into mixed liquor A
Mixed liquor obtains mixed liquid B, wherein the 5th mixed liquor 10-15g is added in every 100g mixed liquor A；Mixed liquid B is carried out mechanical
Stirring, obtains mixed liquor C；Ball milling is carried out to mixed liquor C, obtains mixed liquor D；Mixed liquor D is dried, modified poly- cream is obtained
The mixed-powder of acid；The mixed-powder of polydactyl acid is put into double screw extruder and carries out extrusion molding, obtains beating for 3D
The graphene composite material pellet of print；And the graphene composite material pellet for being used for 3D printing is formed into graphite using 3D printing
Alkene composite material.
In a preferred embodiment, mechanical stirring specific process parameter is carried out to the first mixed liquor are as follows: whipping temp
It is 50-70 DEG C, mixing time 40-60min, mixing speed 800-1000rpm.
In a preferred embodiment, ultrasonic agitation specific process parameter is carried out to third mixed liquor are as follows: whipping temp
It is 50-70 DEG C, mixing time 20-40min, ultrasonic frequency 20-30kHz.
In a preferred embodiment, ball milling specific process parameter is carried out to the 4th mixed liquor are as follows: drum's speed of rotation is
500-800rpm, milling atmosphere are argon atmosphere, Ball-milling Time 20-30h, ratio of grinding media to material 15:1-20:1.
In a preferred embodiment, mechanical stirring specific process parameter is carried out to mixed liquid B are as follows: whipping temp is
40-60 DEG C, mixing time 40-60min, mixing speed 1000-1200rpm.
In a preferred embodiment, ball milling specific process parameter is carried out to mixed liquor C are as follows: drum's speed of rotation is
1000-1200rpm, milling atmosphere are argon atmosphere, Ball-milling Time 20-30h, ratio of grinding media to material 10:1-15:1.
In a preferred embodiment, specific process parameter is dried to mixed liquor D are as follows: drying temperature 90-100
DEG C, drying time 2-8h.
In a preferred embodiment, the mixed-powder of polydactyl acid double screw extruder is put into be extruded into
Type specific process parameter are as follows: extruder the firstth area temperature is 160-165 DEG C, and extruder the secondth area temperature is 165-170 DEG C, is squeezed out
Machine third area's temperature is 170-175 DEG C, and the 4th area's temperature of extruder is 185-190 DEG C, and the 5th area's temperature of extruder is 180-185
DEG C, twin-screw revolving speed is 30-40r/min when extrusion, and feed inlet pressure is 40-50MPa, and discharge port pressure is 20-30MPa.
In a preferred embodiment, the graphene composite material pellet for being used for 3D printing is formed into stone using 3D printing
The specific process parameter of black alkene composite material are as follows: print speed 800-1000mm/min, the high 0.4-0.5mm of layer print spacing
0.2-0.3mm, 60-80 DEG C of hott bed temperature.
Compared with prior art, the method for 3D printing molded graphite alkene composite material of the invention has the advantages that mesh
Before had already appeared some household grade 3D printers, household grade 3D printer generally uses plastics as raw material, and polylactic acid is
A kind of mechanical property preferably, moderate cost and polymer material from a wealth of sources, be suitable as 3D printer raw material.It is worth
It is noted that pure polylactic acid can not fully meet the needs of 3D printing, need to be modified it.It is deposited in currently available technology
In the technology for improving poly-lactic acid material toughness using glycerol, but in general, be added after glycerol, the tensile strength of material with
And the problem of bending strength all will significantly reduce, this will lead to printed product poor mechanical property.For problem of the prior art,
The invention proposes a kind of technologies that polylactic acid toughening is carried out using graphene, inventors have found that passing through particular step and technique
It is added after graphene, the toughness of poly-lactic acid material increases considerably, while cooperating and second-phase strength particle, the drawing of material is added
Stretching intensity and bending strength can be also greatly enhanced simultaneously, and therefore, the invention proposes one kind to improve simultaneously
The method of a variety of mechanical properties of poly-lactic acid material, is with a wide range of applications.
Detailed description of the invention
Fig. 1 is the method flow diagram of 3D printing molded graphite alkene composite material according to an embodiment of the present invention.
Specific embodiment
With reference to the accompanying drawing, specific embodiments of the present invention will be described in detail, it is to be understood that guarantor of the invention
Shield range is not limited by the specific implementation.
Unless otherwise explicitly stated, otherwise in entire disclosure and claims, term " includes " or its change
Changing such as "comprising" or " including " etc. will be understood to comprise stated element or component, and not exclude other members
Part or other component parts.
Fig. 1 is the method flow diagram of 3D printing molded graphite alkene composite material according to an embodiment of the present invention.Such as figure
Shown, the method for 3D printing molded graphite alkene composite material of the invention includes the following steps:
Step 101: configuring the alcohol mixeding liquid of silane coupling agent；
Step 102: nano aluminium oxide is added into the alcohol mixeding liquid of silane coupling agent, obtains the first mixed liquor, wherein
In the first mixed liquor, silane coupling agent concentration is 0.1-0.3g/mL, and nano oxidized aluminum concentration is 1-2g/mL；
Step 103: mechanical stirring being carried out to the first mixed liquor, obtains the second mixed liquor；
Step 104: graphene nanometer sheet is added into the second mixed liquor, obtains third mixed liquor wherein, is mixed in third
In liquid, graphene nanometer sheet concentration is 0.1-0.2g/mL；
Step 105: third mixed liquor being stirred by ultrasonic, the 4th mixed liquor is obtained；
Step 106: ball milling being carried out to the 4th mixed liquor, obtains the 5th mixed liquor；
Step 107: polylactic acid powder is provided；
Step 108: polylactic acid being dissolved in ethyl alcohol, obtains mixed liquor A, wherein PLA concentration is 1-2g/mL；
Step 109: the 5th mixed liquor being added into mixed liquor A, obtains mixed liquid B, wherein add in every 100g mixed liquor A
Enter the 5th mixed liquor 10-15g；
Step 110: mechanical stirring being carried out to mixed liquid B, obtains mixed liquor C；
Step 111: ball milling being carried out to mixed liquor C, obtains mixed liquor D；
Step 112: mixed liquor D being dried, the mixed-powder of polydactyl acid is obtained；
Step 113: the mixed-powder of polydactyl acid being put into double screw extruder and carries out extrusion molding, is obtained for 3D
The graphene composite material pellet of printing；And
Step 114: the graphene composite material pellet for being used for 3D printing being formed into graphene composite material using 3D printing.
Embodiment 1
The method of 3D printing molded graphite alkene composite material of the invention includes the following steps: the second for configuring silane coupling agent
Alcohol mixed liquor；Nano aluminium oxide is added into the alcohol mixeding liquid of silane coupling agent, obtains the first mixed liquor, wherein first
In mixed liquor, silane coupling agent concentration is 0.1g/mL, and nano oxidized aluminum concentration is 1g/mL；Machinery is carried out to the first mixed liquor to stir
It mixes, obtains the second mixed liquor；Graphene nanometer sheet is added into the second mixed liquor, obtains third mixed liquor wherein, it is mixed in third
It closes in liquid, graphene nanometer sheet concentration is 0.1g/mL；Third mixed liquor is stirred by ultrasonic, the 4th mixed liquor is obtained；To
Four mixed liquors carry out ball milling, obtain the 5th mixed liquor；Polylactic acid powder is provided；Polylactic acid is dissolved in ethyl alcohol, obtains mixed liquor A,
Wherein PLA concentration is 1g/mL；The 5th mixed liquor is added into mixed liquor A, obtains mixed liquid B, wherein every 100g mixed liquor
The 5th mixed liquor 10g is added in A；Mechanical stirring is carried out to mixed liquid B, obtains mixed liquor C；Ball milling is carried out to mixed liquor C, is obtained
Mixed liquor D；Mixed liquor D is dried, the mixed-powder of polydactyl acid is obtained；The mixed-powder of polydactyl acid is put into
Double screw extruder carries out extrusion molding, obtains the graphene composite material pellet for 3D printing；It will be used for using 3D printing
The graphene composite material pellet of 3D printing forms graphene composite material.Mechanical stirring concrete technology is carried out to the first mixed liquor
Parameter are as follows: whipping temp is 50 DEG C, mixing time 40min, mixing speed 800rpm.Third mixed liquor is stirred by ultrasonic
Specific process parameter are as follows: whipping temp is 50 DEG C, mixing time 20min, ultrasonic frequency 20kHz.To the 4th mixed liquor
Carry out ball milling specific process parameter are as follows: drum's speed of rotation 500rpm, milling atmosphere are argon atmosphere, Ball-milling Time 20h, ball
Material is than being 15:1.Mechanical stirring specific process parameter is carried out to mixed liquid B are as follows: whipping temp is 40 DEG C, and mixing time is
40min, mixing speed 1000rpm.Ball milling specific process parameter is carried out to mixed liquor C are as follows: drum's speed of rotation 1000rpm, ball
Mill atmosphere is argon atmosphere, Ball-milling Time 20h, ratio of grinding media to material 10:1.Specific process parameter is dried to mixed liquor D are as follows:
Drying temperature is 90 DEG C, drying time 2h.The mixed-powder of polydactyl acid is put into double screw extruder to be extruded into
Type specific process parameter are as follows: extruder the firstth area temperature is 160 DEG C, and extruder the secondth area temperature is 165 DEG C, extruder third area
Temperature is 170 DEG C, and the 4th area's temperature of extruder is 185 DEG C, and the 5th area's temperature of extruder is 180 DEG C, twin-screw revolving speed when extrusion
For 30r/min, feed inlet pressure is 40MPa, and discharge port pressure is 20MPa.The graphene of 3D printing will be used for using 3D printing
The specific process parameter of composite material pellet formation graphene composite material are as follows: print speed 800mm/min, the high 0.4mm of layer are beaten
Print spacing 0.2mm, hott bed temperature 60 C.
Embodiment 2
The method of 3D printing molded graphite alkene composite material of the invention includes the following steps: the second for configuring silane coupling agent
Alcohol mixed liquor；Nano aluminium oxide is added into the alcohol mixeding liquid of silane coupling agent, obtains the first mixed liquor, wherein first
In mixed liquor, silane coupling agent concentration is 0.3g/mL, and nano oxidized aluminum concentration is 2g/mL；Machinery is carried out to the first mixed liquor to stir
It mixes, obtains the second mixed liquor；Graphene nanometer sheet is added into the second mixed liquor, obtains third mixed liquor wherein, it is mixed in third
It closes in liquid, graphene nanometer sheet concentration is 0.2g/mL；Third mixed liquor is stirred by ultrasonic, the 4th mixed liquor is obtained；To
Four mixed liquors carry out ball milling, obtain the 5th mixed liquor；Polylactic acid powder is provided；Polylactic acid is dissolved in ethyl alcohol, obtains mixed liquor A,
Wherein PLA concentration is 2g/mL；The 5th mixed liquor is added into mixed liquor A, obtains mixed liquid B, wherein every 100g mixed liquor
The 5th mixed liquor 15g is added in A；Mechanical stirring is carried out to mixed liquid B, obtains mixed liquor C；Ball milling is carried out to mixed liquor C, is obtained
Mixed liquor D；Mixed liquor D is dried, the mixed-powder of polydactyl acid is obtained；The mixed-powder of polydactyl acid is put into
Double screw extruder carries out extrusion molding, obtains the graphene composite material pellet for 3D printing；It will be used for using 3D printing
The graphene composite material pellet of 3D printing forms graphene composite material.Mechanical stirring concrete technology is carried out to the first mixed liquor
Parameter are as follows: whipping temp is 70 DEG C, mixing time 60min, mixing speed 1000rpm.Ultrasound is carried out to third mixed liquor to stir
Mix specific process parameter are as follows: whipping temp is 70 DEG C, mixing time 40min, ultrasonic frequency 30kHz.It is mixed to the 4th
Liquid carries out ball milling specific process parameter are as follows: and drum's speed of rotation 800rpm, milling atmosphere are argon atmosphere, Ball-milling Time 30h,
Ratio of grinding media to material is 20:1.Mechanical stirring specific process parameter is carried out to mixed liquid B are as follows: whipping temp is 60 DEG C, and mixing time is
60min, mixing speed 1200rpm.Ball milling specific process parameter is carried out to mixed liquor C are as follows: drum's speed of rotation 1200rpm, ball
Mill atmosphere is argon atmosphere, Ball-milling Time 30h, ratio of grinding media to material 15:1.Specific process parameter is dried to mixed liquor D are as follows:
Drying temperature is 100 DEG C, drying time 8h.The mixed-powder of polydactyl acid is put into double screw extruder to be extruded into
Type specific process parameter are as follows: extruder the firstth area temperature is 165 DEG C, and extruder the secondth area temperature is 170 DEG C, extruder third area
Temperature is 175 DEG C, and the 4th area's temperature of extruder is 190 DEG C, and the 5th area's temperature of extruder is 185 DEG C, twin-screw revolving speed when extrusion
For 40r/min, feed inlet pressure is 50MPa, and discharge port pressure is 30MPa.The graphene of 3D printing will be used for using 3D printing
The specific process parameter of composite material pellet formation graphene composite material are as follows: print speed 1000mm/min, the high 0.5mm of layer,
Print spacing 0.3mm, 80 DEG C of hott bed temperature.
Embodiment 3
The method of 3D printing molded graphite alkene composite material of the invention includes the following steps: the second for configuring silane coupling agent
Alcohol mixed liquor；Nano aluminium oxide is added into the alcohol mixeding liquid of silane coupling agent, obtains the first mixed liquor, wherein first
In mixed liquor, silane coupling agent concentration is 0.15g/mL, and nano oxidized aluminum concentration is 1.2g/mL；Machine is carried out to the first mixed liquor
Tool stirring, obtains the second mixed liquor；Graphene nanometer sheet is added into the second mixed liquor, obtains third mixed liquor wherein,
In three mixed liquors, graphene nanometer sheet concentration is 0.13g/mL；Third mixed liquor is stirred by ultrasonic, the 4th mixing is obtained
Liquid；Ball milling is carried out to the 4th mixed liquor, obtains the 5th mixed liquor；Polylactic acid powder is provided；Polylactic acid is dissolved in ethyl alcohol, is mixed
Liquid A is closed, wherein PLA concentration is 1.2g/mL；The 5th mixed liquor is added into mixed liquor A, obtains mixed liquid B, wherein is every
The 5th mixed liquor 12g is added in 100g mixed liquor A；Mechanical stirring is carried out to mixed liquid B, obtains mixed liquor C；To mixed liquor C into
Row ball milling obtains mixed liquor D；Mixed liquor D is dried, the mixed-powder of polydactyl acid is obtained；By polydactyl acid
Mixed-powder is put into double screw extruder and carries out extrusion molding, obtains the graphene composite material pellet for 3D printing；It utilizes
The graphene composite material pellet for being used for 3D printing is formed graphene composite material by 3D printing.First mixed liquor is carried out mechanical
Stir specific process parameter are as follows: whipping temp is 55 DEG C, mixing time 45min, mixing speed 850rpm.To third mixed liquor
Carry out ultrasonic agitation specific process parameter are as follows: whipping temp is 55 DEG C, mixing time 25min, ultrasonic frequency 22kHz.
Ball milling specific process parameter is carried out to the 4th mixed liquor are as follows: drum's speed of rotation 600rpm, milling atmosphere are argon atmosphere, ball milling
Time is 25h, ratio of grinding media to material 16:1.Mechanical stirring specific process parameter is carried out to mixed liquid B are as follows: whipping temp is 45 DEG C, is stirred
Mixing the time is 45min, mixing speed 1050rpm.Ball milling specific process parameter is carried out to mixed liquor C are as follows: drum's speed of rotation is
1050rpm, milling atmosphere are argon atmosphere, Ball-milling Time 25h, ratio of grinding media to material 11:1.Specific work is dried to mixed liquor D
Skill parameter are as follows: drying temperature is 95 DEG C, drying time 3h.By the mixed-powder of polydactyl acid be put into double screw extruder into
Row extrusion molding specific process parameter are as follows: extruder the firstth area temperature is 162 DEG C, and extruder the secondth area temperature is 168 DEG C, is squeezed out
Machine third area's temperature is 172 DEG C, and the 4th area's temperature of extruder is 186 DEG C, and the 5th area's temperature of extruder is 183 DEG C, double when extrusion
Screw speed is 35r/min, and feed inlet pressure is 45MPa, and discharge port pressure is 25MPa.3D printing will be used for using 3D printing
Graphene composite material pellet form the specific process parameter of graphene composite material are as follows: print speed 850mm/min, layer are high
0.45mm, print spacing 0.25mm, 65 DEG C of hott bed temperature.
Embodiment 4
The method of 3D printing molded graphite alkene composite material of the invention includes the following steps: the second for configuring silane coupling agent
Alcohol mixed liquor；Nano aluminium oxide is added into the alcohol mixeding liquid of silane coupling agent, obtains the first mixed liquor, wherein first
In mixed liquor, silane coupling agent concentration is 0.2g/mL, and nano oxidized aluminum concentration is 1.5g/mL；First mixed liquor is carried out mechanical
Stirring, obtains the second mixed liquor；Graphene nanometer sheet is added into the second mixed liquor, third mixed liquor is obtained wherein, in third
In mixed liquor, graphene nanometer sheet concentration is 0.15g/mL；Third mixed liquor is stirred by ultrasonic, the 4th mixed liquor is obtained；
Ball milling is carried out to the 4th mixed liquor, obtains the 5th mixed liquor；Polylactic acid powder is provided；Polylactic acid is dissolved in ethyl alcohol, is mixed
Liquid A, wherein PLA concentration is 1.5g/mL；The 5th mixed liquor is added into mixed liquor A, obtains mixed liquid B, wherein every 100g
The 5th mixed liquor 12g is added in mixed liquor A；Mechanical stirring is carried out to mixed liquid B, obtains mixed liquor C；Ball is carried out to mixed liquor C
Mill, obtains mixed liquor D；Mixed liquor D is dried, the mixed-powder of polydactyl acid is obtained；By the mixing of polydactyl acid
Powder is put into double screw extruder and carries out extrusion molding, obtains the graphene composite material pellet for 3D printing；It is beaten using 3D
The graphene composite material pellet for being used for 3D printing is formed graphene composite material by print.Mechanical stirring is carried out to the first mixed liquor
Specific process parameter are as follows: whipping temp is 60 DEG C, mixing time 50min, mixing speed 900rpm.Third mixed liquor is carried out
Specific process parameter is stirred by ultrasonic are as follows: whipping temp is 60 DEG C, mixing time 30min, ultrasonic frequency 25kHz.To
Four mixed liquors carry out ball milling specific process parameter are as follows: drum's speed of rotation 600rpm, milling atmosphere are argon atmosphere, Ball-milling Time
For 25h, ratio of grinding media to material 18:1.Mechanical stirring specific process parameter is carried out to mixed liquid B are as follows: whipping temp is 50 DEG C, when stirring
Between be 50min, mixing speed 1100rpm.Ball milling specific process parameter is carried out to mixed liquor C are as follows: drum's speed of rotation is
1100rpm, milling atmosphere are argon atmosphere, Ball-milling Time 25h, ratio of grinding media to material 12:1.Specific work is dried to mixed liquor D
Skill parameter are as follows: drying temperature is 95 DEG C, drying time 5h.By the mixed-powder of polydactyl acid be put into double screw extruder into
Row extrusion molding specific process parameter are as follows: extruder the firstth area temperature is 163 DEG C, and extruder the secondth area temperature is 168 DEG C, is squeezed out
Machine third area's temperature is 173 DEG C, and the 4th area's temperature of extruder is 188 DEG C, and the 5th area's temperature of extruder is 182 DEG C, double when extrusion
Screw speed is 35r/min, and feed inlet pressure is 45MPa, and discharge port pressure is 25MPa.3D printing will be used for using 3D printing
Graphene composite material pellet form the specific process parameter of graphene composite material are as follows: print speed 900mm/min, layer are high
0.45mm prints spacing 0.25mm, hott bed temperature 70 C.
Comparative example 1
Difference from Example 1 is: in the first mixed liquor, silane coupling agent concentration is 0.05g/mL, nano oxygen
Change aluminum concentration is 0.5g/mL.
Comparative example 2
Difference from Example 1 is: in third mixed liquor, graphene nanometer sheet concentration is 0.05g/mL.
Comparative example 3
Difference from Example 1 is: carrying out mechanical stirring to third mixed liquor, obtains the 4th mixed liquor；Machinery stirs
Mix parameter are as follows: whipping temp is 50 DEG C, mixing time 40min, mixing speed 800rpm.
Comparative example 4
Difference from Example 1 is: the 5th mixed liquor 5g being added in every 100g mixed liquor A.
Comparative example 5
Difference from Example 1 is: carrying out mechanical stirring specific process parameter to the first mixed liquor are as follows: whipping temp
It is 40 DEG C, mixing time 30min, mixing speed 700rpm.
Comparative example 6
Difference from Example 1 is: carrying out ultrasonic agitation specific process parameter to third mixed liquor are as follows: whipping temp
It is 40 DEG C, mixing time 10min, ultrasonic frequency 10kHz.
Comparative example 7
Difference from Example 1 is: carrying out ball milling specific process parameter to the 4th mixed liquor are as follows: drum's speed of rotation is
1000rpm, milling atmosphere are argon atmosphere, Ball-milling Time 40h, ratio of grinding media to material 10:1.
Comparative example 8
Difference from Example 1 is: carrying out mechanical stirring specific process parameter to mixed liquid B are as follows: whipping temp is
70 DEG C, mixing time 70min, mixing speed 1300rpm.
Comparative example 9
Difference from Example 1 is: carrying out ball milling specific process parameter to mixed liquor C are as follows: drum's speed of rotation is
1300rpm, milling atmosphere are argon atmosphere, Ball-milling Time 35h, ratio of grinding media to material 20:1.
Comparative example 10
Difference from Example 1 is: the mixed-powder of polydactyl acid being put into double screw extruder and is squeezed out
Form specific process parameter are as follows: extruder the firstth area temperature is 170 DEG C, and extruder the secondth area temperature is 175 DEG C, extruder third
Area's temperature is 180 DEG C, and the 4th area's temperature of extruder is 185 DEG C.
Comparative example 11
Difference from Example 1 is: the mixed-powder of polydactyl acid being put into double screw extruder and is squeezed out
Form specific process parameter are as follows: twin-screw revolving speed is 45r/min when extrusion, and feed inlet pressure is 20MPa, and discharge port pressure is
10MPa。
Comparative example 12
Difference from Example 1 is: being formed the graphene composite material pellet for being used for 3D printing using 3D printing
The specific process parameter of graphene composite material are as follows: print speed 900mm/min, the high 0.3mm of layer print spacing 0.1mm, hott bed
90 DEG C of temperature.
To the lactic acid composite material of embodiment 1-4 and comparative example 1-12 carry out bending strength, elongation at break and
(tension test is carried out by GB/T 1040.2-2006 for the test of tensile strength；Bend test is carried out by GB/T 9341-2008),
Test result is shown in Table 1.
Table 1
The aforementioned description to specific exemplary embodiment of the invention is in order to illustrate and illustration purpose.These descriptions
It is not wishing to limit the invention to disclosed precise forms, and it will be apparent that according to the above instruction, can much be changed
And variation.The purpose of selecting and describing the exemplary embodiment is that explaining specific principle of the invention and its actually answering
With so that those skilled in the art can be realized and utilize a variety of different exemplary implementation schemes of the invention and
Various chooses and changes.The scope of the present invention is intended to be limited by claims and its equivalents.
Claims (9)
1. a kind of method of 3D printing molded graphite alkene composite material, it is characterised in that: the 3D printing molded graphite alkene is compound
The method of material includes the following steps:
Configure the alcohol mixeding liquid of silane coupling agent；
Nano aluminium oxide is added into the alcohol mixeding liquid of the silane coupling agent, obtains the first mixed liquor, wherein described
In one mixed liquor, the silane coupling agent concentration is 0.1-0.3g/mL, and the nano oxidized aluminum concentration is 1-2g/mL；
Mechanical stirring is carried out to first mixed liquor, obtains the second mixed liquor；
Graphene nanometer sheet is added into second mixed liquor, obtains third mixed liquor wherein, in the third mixed liquor,
The graphene nanometer sheet concentration is 0.1-0.2g/mL；
The third mixed liquor is stirred by ultrasonic, the 4th mixed liquor is obtained；
Ball milling is carried out to the 4th mixed liquor, obtains the 5th mixed liquor；
Polylactic acid powder is provided；
The polylactic acid is dissolved in ethyl alcohol, obtains mixed liquor A, wherein PLA concentration is 1-2g/mL；
The 5th mixed liquor is added into the mixed liquor A, obtains mixed liquid B, wherein it is mixed that the 5th is added in every 100g mixed liquor A
Close liquid 10-15g；
Mechanical stirring is carried out to mixed liquid B, obtains mixed liquor C；
Ball milling is carried out to the mixed liquor C, obtains mixed liquor D；
The mixed liquor D is dried, the mixed-powder of polydactyl acid is obtained；
The mixed-powder of the polydactyl acid is put into double screw extruder and carries out extrusion molding, obtains the stone for 3D printing
Black alkene composite material pellet；And
The graphene composite material pellet for being used for 3D printing is formed into graphene composite material using 3D printing.
2. passing through the method for 3D printing formation lactic acid composite material as described in claim 1, it is characterised in that: to described the
One mixed liquor carries out mechanical stirring specific process parameter are as follows: whipping temp is 50-70 DEG C, mixing time 40-60min, stirring
Speed 800-1000rpm.
3. passing through the method for 3D printing formation lactic acid composite material as claimed in claim 2, it is characterised in that: to described the
Three mixed liquors carry out ultrasonic agitation specific process parameter are as follows: whipping temp is 50-70 DEG C, mixing time 20-40min, ultrasound
Wave frequency rate is 20-30kHz.
4. passing through the method for 3D printing formation lactic acid composite material as claimed in claim 3, it is characterised in that: to described the
Four mixed liquors carry out ball milling specific process parameter are as follows: drum's speed of rotation 500-800rpm, milling atmosphere are argon atmosphere, ball milling
Time is 20-30h, ratio of grinding media to material 15:1-20:1.
5. the method as claimed in claim 4 for forming lactic acid composite material by 3D printing, it is characterised in that: to mixed liquor
B carries out mechanical stirring specific process parameter are as follows: whipping temp is 40-60 DEG C, mixing time 40-60min, mixing speed
1000-1200rpm。
6. the method as claimed in claim 5 for forming lactic acid composite material by 3D printing, it is characterised in that: to described mixed
It closes liquid C and carries out ball milling specific process parameter are as follows: drum's speed of rotation 1000-1200rpm, milling atmosphere are argon atmosphere, ball milling
Time is 20-30h, ratio of grinding media to material 10:1-15:1.
7. the method as claimed in claim 6 for forming lactic acid composite material by 3D printing, it is characterised in that: to described mixed
It closes liquid D and specific process parameter is dried are as follows: drying temperature is 90-100 DEG C, drying time 2-8h.
8. the method as claimed in claim 7 for forming lactic acid composite material by 3D printing, it is characterised in that: change described
Property polylactic acid mixed-powder be put into double screw extruder carry out extrusion molding specific process parameter are as follows: the firstth area of extruder temperature
It is 160-165 DEG C, extruder the secondth area temperature is 165-170 DEG C, and extruder third area's temperature is 170-175 DEG C, extruder the
Four area's temperature are 185-190 DEG C, and the 5th area's temperature of extruder is 180-185 DEG C, and twin-screw revolving speed is 30-40r/min when extrusion,
Feed inlet pressure is 40-50MPa, and discharge port pressure is 20-30MPa.
9. the method as claimed in claim 8 for forming lactic acid composite material by 3D printing, it is characterised in that: beaten using 3D
The graphene composite material pellet for being used for 3D printing is formed the specific process parameter of graphene composite material by print are as follows: print speed
800-1000mm/min, the high 0.4-0.5mm of layer print spacing 0.2-0.3mm, 60-80 DEG C of hott bed temperature.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811059824.0A CN109251495B (en) | 2018-09-12 | 2018-09-12 | Method for 3D printing and molding graphene composite material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811059824.0A CN109251495B (en) | 2018-09-12 | 2018-09-12 | Method for 3D printing and molding graphene composite material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN109251495A true CN109251495A (en) | 2019-01-22 |
| CN109251495B CN109251495B (en) | 2021-03-02 |
Family
ID=65047406
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811059824.0A Active CN109251495B (en) | 2018-09-12 | 2018-09-12 | Method for 3D printing and molding graphene composite material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109251495B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2021095021A1 (en) * | 2019-11-15 | 2021-05-20 | Tor Corporation Ltd | Biodegradable polymer nanocomposite and method for production thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20140357788A1 (en) * | 2013-05-31 | 2014-12-04 | Regents Of The University Of Minnesota | Compositions including poly(hydroxyalkanoates) and graphene |
| CN104194007A (en) * | 2014-09-28 | 2014-12-10 | 中国科学院理化技术研究所 | Preparation method for polymer matrix micron/nanometer packing filling modification compound premix particles |
| CN106589859A (en) * | 2015-10-13 | 2017-04-26 | 中国石油化工股份有限公司 | Antistatic polylactic resin powder used for selective laser sintering, and preparation method thereof |
-
2018
- 2018-09-12 CN CN201811059824.0A patent/CN109251495B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20140357788A1 (en) * | 2013-05-31 | 2014-12-04 | Regents Of The University Of Minnesota | Compositions including poly(hydroxyalkanoates) and graphene |
| CN104194007A (en) * | 2014-09-28 | 2014-12-10 | 中国科学院理化技术研究所 | Preparation method for polymer matrix micron/nanometer packing filling modification compound premix particles |
| CN106589859A (en) * | 2015-10-13 | 2017-04-26 | 中国石油化工股份有限公司 | Antistatic polylactic resin powder used for selective laser sintering, and preparation method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2021095021A1 (en) * | 2019-11-15 | 2021-05-20 | Tor Corporation Ltd | Biodegradable polymer nanocomposite and method for production thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN109251495B (en) | 2021-03-02 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105385124B (en) | Carbon fiber enhanced polylactic acid 3D printing material and preparation method thereof | |
| CN109337086A (en) | A kind of the ternary polymerization composite material and preparation method and dedicated unit of functional graphene in-situ polymerization polyester | |
| CN103665802A (en) | Preparation method of polylactic acid material for 3D (three-dimensional) printing | |
| CN111690240A (en) | Polylactic acid/nano cellulose composite material and preparation method thereof | |
| CN104479267B (en) | A kind of modified bagasse-plastic composite and its preparation method and application | |
| CN109251495A (en) | The method of 3D printing molded graphite alkene composite material | |
| CN106380832A (en) | Nylon-polypropylene-filler modified composite powder, and preparation method and application thereof | |
| CN108017858A (en) | A kind of water-fast PVC wood plastic foam composite material and preparation method thereof | |
| CN109575557B (en) | PC/ABS mixture for three-dimensional printing, preparation method thereof and direct printing method | |
| CN104672826A (en) | 3D printed PLA consumable and preparation method thereof | |
| CN102011017A (en) | Method for extracting tungsten by decomposing tungsten minerals | |
| CN105885406A (en) | High-strength and high-toughness modified nylon 66 composite material and preparation method thereof | |
| CN104163943B (en) | Thermoplastic cellulose composite material and preparation method thereof | |
| CN109337313B (en) | Method for forming gradient composite material by using 3D printing | |
| CN107353476A (en) | A kind of lightweight automotive material and preparation method thereof | |
| CN105086393B (en) | Plastic allowing PLA to be fully degraded and production method thereof | |
| CN112375346A (en) | Biodegradable gloves and preparation method thereof | |
| CN102101924A (en) | Machining method of ultrahigh molecular weight polyethylene pipe | |
| CN106433179A (en) | Preparation method of novel printing plastic material | |
| CN106380833A (en) | Nylon/styrene-based polymer/filler modified composite powder, and preparation method and application thereof | |
| CN107841134A (en) | A kind of preparation method available for increasing material manufacturing activeness and quietness nylon material | |
| CN112608500B (en) | Method for preparing high-performance environment-friendly polyvinyl alcohol film by thermoplastic processing | |
| CN109575502A (en) | PC/ABS compound silk material for 3 D-printing and preparation method thereof and Method of printing | |
| CN113683858A (en) | Preparation method of conductive 3D printing graphene composite material with high mechanical strength | |
| CN202016188U (en) | Double-screw extruder unit for reaction extrusion of polyvinyl alcohol (PVA) |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |