CN110527221A - A kind of graphene 3D printing material and preparation method thereof - Google Patents
A kind of graphene 3D printing material and preparation method thereof Download PDFInfo
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- CN110527221A CN110527221A CN201910972464.1A CN201910972464A CN110527221A CN 110527221 A CN110527221 A CN 110527221A CN 201910972464 A CN201910972464 A CN 201910972464A CN 110527221 A CN110527221 A CN 110527221A
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- 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
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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
- C08L27/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers
- C08L27/02—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L27/04—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
- C08L27/06—Homopolymers or copolymers of vinyl chloride
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Abstract
The present invention provides a kind of preparation method of graphene 3D printing material, and a kind of preparation method of graphene 3D printing material: removing moisture removal with the way of distillation for tetrahydrofuran, is divided into A, two parts of solution of B, and the mass ratio of solution A and B solution is (2-3): 1；In solution A put into silica white after stirring to dissolve after, then again by graphene dispersion wherein；After polyvinyl chloride and maleic anhydride polymer are mixed, puts into B solution and sufficiently dissolve；By above-mentioned two parts of solution after 30-60 DEG C is sufficiently mixed, then 120 DEG C are warming up to fully reacting, and collect the tetrahydrofuran of volatilization, solution is subjected to deep cooling powder, the 3D printing material that diameier is 20-200nm is obtained, separately can be made into 3D printing wire rod, realizes the diversification of material application.
Description
Technical field
The present invention relates to 3D printing material manufacturing fields, in particular to a kind of graphene 3D printing material and its system
Preparation Method.
Background technique
Three-dimensional (3D) printing technique is also known as increases material manufacturing technology, and basic principle is layered manufacturing, successively increases material next life
At the technology of 3D solid, actually a kind of emerging technology of rapid shaping field, it is a kind of is with digital model file
Basis constructs the technology of object by layer-by-layer printing with adhesive materials such as powdery metal or plastics.Mesh
Before, three-dimensional printing technology is applied primarily to product prototype, mold manufactures and the fields such as artistic creation, jewelry-making, substitution
The retrofit technique that these tradition rely on, in addition, three-dimensional printing technology is gradually applied to medicine, bioengineering, building, clothes
Wide space has been opened up for innovation in the fields such as dress, aviation.
Graphene has the characteristics that excellent optics, mechanics, and conductive effect is excellent, can be widely used for microelectronics, boat
Empty space flight, machinery field.Silica gel and polyvinyl chloride in high molecular material have importantly in plastic industry, instrument manufacturing etc.
Position.But will by these high molecular materials and graphene it is compound be used as 3D printing material when, between graphene and macromolecule be easy
It separates, uniformity is poor, it is difficult to which the accurate expression for designing 3D printing causes to obtain the uneven precision of 3D printing interiors of products
Low, rough surface, mechanical property is undesirable.
Summary of the invention
In order to overcome drawbacks described above, there is integrally formed property the present invention provides one kind and controllability is good, simple process, power
Learn high graphene 3D printing material of performance and preparation method thereof.
The technical solution solved the problems, such as of the invention is that a kind of preparation method of graphene 3D printing material, feature exists
In, comprising the following steps:
1) prepare raw material: 10-20 parts of polyvinyl chloride, 10-40 parts of silica white, 10-30 parts of graphene, maleic acid by weight
1-3 parts of anhydride polymer, 80-100 parts of tetrahydrofuran；
2) tetrahydrofuran is removed into moisture removal with the way of distillation, is divided into A, the mass ratio of two parts of solution of B, solution A and B solution is
(2-3): 1；
3) in solution A put into silica white after stirring to dissolve after, then again by graphene dispersion wherein；
4) it after mixing polyvinyl chloride and maleic anhydride polymer, puts into B solution and sufficiently dissolves；
5) by 3) and after 4) two parts of solution are sufficiently mixed at 30-60 DEG C, then 120 DEG C are warming up to fully reacting, and collect
The tetrahydrofuran of volatilization；
6) 5) solution is subjected to deep cooling powder, obtains the 3D printing material that diameier is 20-200nm.
Preferably, the partial size of graphene is 10-30nm.
In some embodiments, graphene dispersion is that ultrasonic disperse or microwave disperse in the step 2).
In some embodiments, step 6) deep cooling powder is carried out in liquid nitrogen environment.
The present invention also utilizes above-mentioned manufacturing method, provides graphene 3D printing material powder, is used for powder-type 3D printer.
The material of step 4) is put into high-speed kneading machine by graphene 3D printing wire rod, and revolving speed 1000-6000rpm is pinched
30-60min is closed, single screw extrusion machine is transferred to and carries out extrusion bracing wire, is made；Wherein, feeding section extrusion temperature is 170-190 DEG C,
Fluxing zone extrusion temperature is 200-250 DEG C, and melt conveying zone extrusion temperature is 190-250 DEG C, and head temperature is 210-260 DEG C.
Inventor's discovery passes through graphene in microwave or the evenly dispersed wherein silica gel-tetrahydrofuran solution of ultrasound, and
Good dispersion stabilization is kept, the graphene 3D printing material haveing excellent performance finally made, present invention process method is simple, grasps
Make easy, yield height, it is at low cost.
Specific embodiment
Son is described in further details the present invention combined with specific embodiments below, but this should not be interpreted as of the invention
Range is only limitted to following instance.
Embodiment 1
1) by weight prepare raw material: 10 parts of polyvinyl chloride, 10 parts of silica white, partial size be 10-30nm 10 parts of graphene,
1 part of maleic anhydride polymer, 80 parts of tetrahydrofuran；
2) tetrahydrofuran is removed into moisture removal with the way of distillation, is divided into A, the mass ratio of two parts of solution of B, solution A and B solution is 2:
1；
3) in solution A put into silica white after stirring to dissolve after, then again by graphene ultrasonic disperse wherein, ultrasonic wave
Frequency be 300-450W；
4) it after mixing polyvinyl chloride and maleic anhydride polymer, puts into B solution and sufficiently dissolves；
3) and 4) 5) by two parts of solution after 45 DEG C are sufficiently mixed, then 120 DEG C are warming up to fully reacting, and collect volatilization
Tetrahydrofuran；
6) 5) solution is subjected to deep cooling powder, obtains the 3D printing material that diameier is 20-200nm.
Embodiment 2
1) by weight prepare raw material: 15 parts of polyvinyl chloride, 10 parts of silica white, partial size be 10-30nm 20 parts of graphene,
3 parts of maleic anhydride polymer, 90 parts of tetrahydrofuran；
2) tetrahydrofuran is removed into moisture removal with the way of distillation, is divided into A, the mass ratio of two parts of solution of B, solution A and B solution is 2:
1；
3) in solution A put into silica white after stirring to dissolve after, then again by graphene ultrasonic disperse wherein, ultrasonic wave
Frequency be 300-450W；
4) it after mixing polyvinyl chloride and maleic anhydride polymer, puts into B solution and sufficiently dissolves；
3) and 4) 5) by two parts of solution after 45 DEG C are sufficiently mixed, then 120 DEG C are warming up to fully reacting, and collect volatilization
Tetrahydrofuran；
6) 5) solution is subjected to deep cooling powder, obtains the 3D printing material that diameier is 20-200nm.
Embodiment 3
1) by weight prepare raw material: 20 parts of polyvinyl chloride, 40 parts of silica white, partial size be 10-30nm 30 parts of graphene,
3 parts of maleic anhydride polymer, 100 parts of tetrahydrofuran；
2) tetrahydrofuran is removed into moisture removal with the way of distillation, is divided into A, the mass ratio of two parts of solution of B, solution A and B solution is 3:
1；
3) in solution A put into silica white after stirring to dissolve after, then again by graphene ultrasonic disperse wherein, ultrasonic wave
Frequency be 300-450W；
4) it after mixing polyvinyl chloride and maleic anhydride polymer, puts into B solution and sufficiently dissolves；
3) and 4) 5) by two parts of solution after 45 DEG C are sufficiently mixed, then 120 DEG C are warming up to fully reacting, and collect volatilization
Tetrahydrofuran；
6) 5) solution is subjected to deep cooling powder, obtains the 3D printing material that diameier is 20-200nm.
By the material of embodiment 1-3 step 4), it is put into high-speed kneading machine, revolving speed 6000rpm mediates 60min, is transferred to list
Screw extruder, feeding section extrusion temperature are 190 DEG C, and fluxing zone extrusion temperature is 250 DEG C, and melt conveying zone extrusion temperature is
250 DEG C, head temperature is 260 DEG C, and squeezing out diameter is that 1.78mm carries out squeezing out the obtained graphene 3D printing line for realizing 4-6 of bracing wire
Material.
To experiment 4-6 wire rod detect, detection the result is as follows:
It can be seen that material of the invention by upper table and shown good mechanical mechanics property and structure precision, have
Standby good electric conductivity.
The present invention is described in detail above, its object is to allow the personage for being familiar with this field technology that can understand this
The content of invention is simultaneously implemented, and it is not intended to limit the scope of the present invention, and the present invention is not limited to above-mentioned implementations
, equivalent change or modification made by all Spirit Essences according to the present invention should be covered by the protection scope of the present invention.
Claims (6)
1. a kind of preparation method of graphene 3D printing material, which comprises the following steps:
1) prepare raw material by weight: 10-20 parts of polyvinyl chloride, 10-40 parts of silica white, 10-30 parts of graphene, maleic anhydride are poly-
Close object 1-3 parts, 80-100 parts of tetrahydrofuran；
2) tetrahydrofuran is removed into moisture removal with the way of distillation, is divided into A, the mass ratio of two parts of solution of B, solution A and B solution is (2-3):
1；
3) in solution A put into silica white after stirring to dissolve after, then again by graphene dispersion wherein；
4) it after mixing polyvinyl chloride and maleic anhydride polymer, puts into B solution and sufficiently dissolves；
5) by 3) and after 4) two parts of solution are sufficiently mixed at 30-60 DEG C, then 120 DEG C are warming up to fully reacting, and collect volatilization
Tetrahydrofuran；
6) 5) solution is subjected to deep cooling powder, obtains the 3D printing material that diameier is 20-200nm.
2. the preparation method of graphene 3D printing material according to claim 1, which is characterized in that the grain of the graphene
Diameter is 10-30nm.
3. the preparation method of graphene 3D printing material according to claim 1, which is characterized in that stone in the step 2
Black alkene is separated into ultrasonic disperse or microwave dispersion.
4. the preparation method of graphene 3D printing material according to claim 1, which is characterized in that the step 6) deep cooling
Powder processed is carried out in liquid nitrogen environment.
5. the preparation method of graphene 3D printing material described in -4 according to claim 1, which is characterized in that by the material of step 6)
Material, is put into high-speed kneading machine, and revolving speed 1000-6000rpm mediates 30-60min, is transferred to single screw extrusion machine and carries out extrusion drawing
Graphene 3D printing wire rod is made in line；Wherein, feeding section extrusion temperature is 170-190 DEG C, and fluxing zone extrusion temperature is 200-
250 DEG C, melt conveying zone extrusion temperature is 190-250 DEG C, and head temperature is 210-260 DEG C.
6. a kind of graphene 3D printing material, which is characterized in that be made of any method of claim 1-5.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20170130034A1 (en) * | 2015-11-10 | 2017-05-11 | Korea Institute Of Science And Technology | High strength polymer filament for fdm 3d printer including graphene coated metal nanoparticles, nanocarbons for 3d printer, and preparation method of the same |
| CN107057146A (en) * | 2017-05-15 | 2017-08-18 | 广西丰达三维科技有限公司 | A kind of preparation technology for the 3D printing elastomeric material that graphene is modified |
| CN107964191A (en) * | 2017-12-15 | 2018-04-27 | 深圳恒方大高分子材料科技有限公司 | A 3D-printable soft PVC material and preparation method thereof |
| CN109504093A (en) * | 2018-11-19 | 2019-03-22 | 珠海市扬程玻璃制品有限公司 | A kind of preparation method of conductive pressure sensitive nanometer silicon rubber |
-
2019
- 2019-10-14 CN CN201910972464.1A patent/CN110527221A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20170130034A1 (en) * | 2015-11-10 | 2017-05-11 | Korea Institute Of Science And Technology | High strength polymer filament for fdm 3d printer including graphene coated metal nanoparticles, nanocarbons for 3d printer, and preparation method of the same |
| CN107057146A (en) * | 2017-05-15 | 2017-08-18 | 广西丰达三维科技有限公司 | A kind of preparation technology for the 3D printing elastomeric material that graphene is modified |
| CN107964191A (en) * | 2017-12-15 | 2018-04-27 | 深圳恒方大高分子材料科技有限公司 | A 3D-printable soft PVC material and preparation method thereof |
| CN109504093A (en) * | 2018-11-19 | 2019-03-22 | 珠海市扬程玻璃制品有限公司 | A kind of preparation method of conductive pressure sensitive nanometer silicon rubber |
Non-Patent Citations (1)
| Title |
|---|
| 刘西文: "《塑料挤出工[中、高级]培训教程》", 31 January 2017 * |
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Application publication date: 20191203 |