CN107151443A - A kind of PEI base graphene 3D printing composite and preparation method thereof - Google Patents
A kind of PEI base graphene 3D printing composite and preparation method thereof Download PDFInfo
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- CN107151443A CN107151443A CN201710390041.XA CN201710390041A CN107151443A CN 107151443 A CN107151443 A CN 107151443A CN 201710390041 A CN201710390041 A CN 201710390041A CN 107151443 A CN107151443 A CN 107151443A
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- pei
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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
- C08L79/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen or carbon only, not provided for in groups C08L61/00 - C08L77/00
- C08L79/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
- C08L79/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
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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
- 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
Abstract
The invention belongs to graphene composite material technology of preparing, it is related to a kind of PEI base graphene composite material and preparation method thereof.The mass percent of PEI base graphene 3D printing composite each component of the present invention is:Graphene powder:0.1%~15%;Coupling agent:0.1%~5%;Lubricant:0.1%~5%;Surplus is polyetherimide resin.The step of preparation, is as follows:Prepare PEI base graphene composite material master batch;Prepare PEI base graphene composite wire rod.The present invention improves the use temperature upper limit and use environment scope of 3D printing composite, improves mechanical strength, and emphasis improves its impact strength, has expanded the application of PEI and graphene in terms of 3D printing.
Description
Technical field
The invention belongs to graphene composite material technology of preparing, be related to a kind of PEI base graphene composite material and
Its preparation method.
Background technology
3D printing technique is also known as increasing material manufacturing, can be realized and successively added by 3D printer directly according to three-dimensional data
Work, the technique of superposition forming, entity is generated with this;It is different from the preparation method of traditional moulds processing, this without mold freedom
The technology of shaping has broken away from the constraint of space geometry and design technology, any creative design can be changed into entity products, expands
Huge space for the creativity.And compared with conventional resins processing mode, the R&D cycle is shortened, reduce R&D costs;Open up
Wide material selection range and product applications;Molding part can directly manufacture terminal parts;Also disappearing for material is just reduced
The production of consumption, especially small lot can substantially reduce product cost.In recent years, 3D printing technique is developed rapidly, receives the country
Outer being widely recognized as and paying close attention to.
In 3D printing technique, be used widely have laser powder sinter (SLS), fused glass pellet (FDM) and
This is several for Stereolithography (SLA), wherein, fused glass pellet (FDM) technology is that one kind can be by various thermoplastic polymers silk
Material heating fusing and then the printing technique method of accumulation molding, this method principle compared with it is simple, printing cost is low, operation is simple,
It is most widely used in numerous 3D printing techniques, while having vital status in 3D printing field.
At present, the polymer silk material applied to FDM printing techniques is main with conventional engineering thermoplastic's modeling such as ABS, PLA, PC
Material is in the majority, but these polymer generally existing temperature in use are low, and mechanical strength is poor, the problem of practical ranges are limited, especially
It is that in terms of the engineer applieds such as Aero-Space, existing 3D printing material has been difficult to meet the growing market demand.
PEI (PEI) is a kind of prepattern high-performance polymer, while be also a kind of conventional aeronautical material, its
With excellent mechanical property, outstanding high temperature resistant is presented, intensity is good, modulus is big, wide spectrum chemical resistance, fire resistance and low cause
Cigarette, creep resistant and excellent size stability, can apply to fireman's helmet, aircraft interior trim, out of my cabin Aero-Space component, vapour
Each position component of car etc..It possesses maximum heat resistance, chemical resistance and the mechanical strength for any FDM thermoplastics, is
It is used as the optimal selection of high performance 3 d printing composite material polymeric matrix;But its shock resistance is still not excellent enough, has
Treat in further improvement.
Graphene is as a kind of new material, with special two-dimensional structure, superior electricity, calorifics, mechanical property, compared with
High chemical stability, due to the above-mentioned excellent mechanical and functional form performance of graphene, generally adds as enhancing filler
Enter into polymeric matrix, and then effectively improve every correlated performance of polymeric matrix.
The content of the invention
The purpose of the present invention is:A kind of PEI base graphene composite material and preparation method thereof is provided, to carry
The use temperature upper limit and use environment scope of high 3D printing composite, improve mechanical strength, and emphasis improves its shock resistance
Intensity, expands the application of PEI and graphene in terms of 3D printing, creates remarkable economic benefit and social benefit.
The technical scheme is that:A kind of PEI base graphene 3D printing composite, it is characterised in that it
The mass percent of each component be:Graphene powder:0.1%~15%;Coupling agent:0.1%~5%;Lubricant:0.1%
~5%;Surplus is polyetherimide resin;Described coupling agent is silane coupler, titanate coupling agent, aluminate coupling agent
One of them;Described lubricant is one of OPE, polypropylene, stearic acid, butyl stearate;The polyethers
The weight average molecular weight Mw of imide resin is the g/mol of 40,000 g/mol~50,000.
The preparation method of PEI base graphene 3D printing composite as described above, it is characterised in that system
Standby step is as follows:
1st, PEI base graphene composite material master batch is prepared:
The graphene weighed up, coupling agent and lubricant are added in dried polyetherimide resin, stirred repeatedly
Through double screw extruder after well mixed, melt blending and extruding pelletization are carried out under conditions of temperature is 350 DEG C~420 DEG C,
Obtain composite master batch;
2nd, PEI base graphene composite wire rod is prepared:
After composite master batch desiccant dehumidification, PEI based composites wire rod, institute is made through resin wire drawing machine
The addition temperature for stating wire drawing machine is 320 DEG C~400 DEG C, a diameter of 1mm~4mm of wire rod.
It is an advantage of the invention that:There is provided a kind of PEI base graphene composite material and preparation method thereof, improve
The use temperature upper limit and use environment scope of 3D printing composite, improves mechanical strength, and emphasis improves it and resisted
Impact strength, has expanded the application of PEI and graphene in terms of 3D printing, creates economic benefit and the society of brilliance
Can benefit.
Embodiment
The present invention is described in further details below.A kind of PEI base graphene 3D printing composite, its
It is characterised by, the mass percent of its each component is:Graphene powder:0.1%~15%;Coupling agent:0.1%~5%;Profit
Lubrication prescription:0.1%~5%;Surplus is polyetherimide resin;Described coupling agent is silane coupler, titanate coupling agent, aluminium
One of acid esters coupling agent;Described lubricant be OPE, polypropylene, stearic acid, butyl stearate wherein it
One;The weight average molecular weight Mw of the polyetherimide resin is the g/mol of 40,000 g/mol~50,000.
The preparation method of PEI base graphene 3D printing composite as described above, it is characterised in that system
Standby step is as follows:
1st, PEI base graphene composite material master batch is prepared:
The graphene weighed up, coupling agent and lubricant are added in dried polyetherimide resin, stirred repeatedly
Through double screw extruder after well mixed, melt blending and extruding pelletization are carried out under conditions of temperature is 350 DEG C~420 DEG C,
Obtain composite master batch;
2nd, PEI base graphene composite wire rod is prepared:
After composite master batch desiccant dehumidification, PEI based composites wire rod, institute is made through resin wire drawing machine
The addition temperature for stating wire drawing machine is 320 DEG C~400 DEG C, a diameter of 1mm~4mm of wire rod.
The present invention operation principle be:Combination process is simple and easy to apply, safe operation, be easily achieved batch steady production, multiple
Additive is few, environment-protecting and non-poisonous during conjunction, and prepared PEI base graphene composite wire rod is uniform, can directly answer
For 3D printing, the R&D cycle is short, cost is low, material consumption is few, there is prominent advantage compared with traditional processing manufacture;It is resulting
PEI base graphene composite material, mechanical property significantly improved, and especially shock resistance is obviously improved, and compensate for
The deficiency of pure PEI shock resistance difference, and can persistently be used under the adverse circumstances such as high-temp and high-strength high corrosion, make
For a kind of novel high-performance composite, it is more suitable for applying in Aero-Space, machine-building etc. has material the phase of high request
Pass field, lays a good foundation to expand the application of PEI and graphene in terms of 3D printing.
Embodiment 1
Weigh 0.3g graphene powder, 0.3g coupling agent, 0.3g lubricant and 299.1g PEI
Resin;
Through double screw extruder after above-mentioned raw materials are uniformly mixed repeatedly, under conditions of temperature is 380 DEG C fully
Extruding pelletization after melt blending, obtains composite master batch;After composite master batch desiccant dehumidification temperature will be being added through wire drawing machine
Spend that PEI based composites wire rod is made under conditions of 350 DEG C.
Embodiment 2
Weigh 3g graphene powder, 3g coupling agent, 3g lubricant and 291g polyetherimide resin;
Through double screw extruder after above-mentioned raw materials are uniformly mixed repeatedly, under conditions of temperature is 400 DEG C fully
Extruding pelletization after melt blending, obtains composite master batch;After composite master batch desiccant dehumidification temperature will be being added through wire drawing machine
Spend that PEI based composites wire rod is made under conditions of 370 DEG C.
Embodiment 3
Weigh 15g graphene powder, 4.5g coupling agent, 4.5g lubricant and 276g PEI tree
Fat;
Through double screw extruder after above-mentioned raw materials are uniformly mixed repeatedly, under conditions of temperature is 420 DEG C fully
Extruding pelletization after melt blending, obtains composite master batch;After composite master batch desiccant dehumidification temperature will be being added through wire drawing machine
Spend that PEI based composites wire rod is made under conditions of 400 DEG C.
Embodiment 4
Weigh 30g graphene powder, 7.5g coupling agent, 7.5g lubricant and 255g PEI tree
Fat;
Through double screw extruder after above-mentioned raw materials are uniformly mixed repeatedly, under conditions of temperature is 350 DEG C fully
Extruding pelletization after melt blending, obtains composite master batch;After composite master batch desiccant dehumidification temperature will be being added through wire drawing machine
Spend that PEI based composites wire rod is made under conditions of 320 DEG C.
Embodiment 5
Weigh 45g graphene powder, 15g coupling agent, 15g lubricant and 225g polyetherimide resin;
Through double screw extruder after above-mentioned raw materials are uniformly mixed repeatedly, under conditions of temperature is 370 DEG C fully
Extruding pelletization after melt blending, obtains composite master batch;After composite master batch desiccant dehumidification temperature will be being added through wire drawing machine
Spend that PEI based composites wire rod is made under conditions of 340 DEG C.
Claims (2)
1. a kind of PEI base graphene 3D printing composite, it is characterised in that the mass percent of its each component
For:Graphene powder:0.1%~15%;Coupling agent:0.1%~5%;Lubricant:0.1%~5%;Surplus is polyetherimide
Polyimide resin;Described coupling agent is one of silane coupler, titanate coupling agent, aluminate coupling agent;Described lubrication
Agent is one of OPE, polypropylene, stearic acid, butyl stearate;The polyetherimide resin is divided equally again
Son amount Mw is the g/mol of 40,000 g/mol~50,000.
2. the preparation method of PEI base graphene 3D printing composite as claimed in claim 1, it is characterised in that
The step of preparation, is as follows:
2.1st, PEI base graphene composite material master batch is prepared:
The graphene weighed up, coupling agent and lubricant are added in dried polyetherimide resin, repeatedly stirring mixing
Through double screw extruder after uniform, melt blending and extruding pelletization are carried out under conditions of temperature is 350 DEG C~420 DEG C, is obtained
Composite master batch;
2.2nd, PEI base graphene composite wire rod is prepared:
After composite master batch desiccant dehumidification, PEI based composites wire rod, the drawing is made through resin wire drawing machine
The addition temperature of silk machine is 320 DEG C~400 DEG C, a diameter of 1mm~4mm of wire rod.
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Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107263855A (en) * | 2017-06-19 | 2017-10-20 | 中国航发北京航空材料研究院 | A kind of high-strength high temperature-resistant 3D printing material, wire rod are prepared and Method of printing |
CN109762336A (en) * | 2019-01-18 | 2019-05-17 | 中国航发北京航空材料研究院 | A kind of 3D printing composite wire and preparation method thereof |
CN110102757A (en) * | 2019-04-15 | 2019-08-09 | 中国航发北京航空材料研究院 | A kind of preparation method of the graphene coated copper conducting powder based on fabricated in situ |
CN110157185A (en) * | 2018-04-12 | 2019-08-23 | 济南开发区星火科学技术研究院 | A kind of graphene 3D printing material with high intensity |
CN112500680A (en) * | 2020-11-10 | 2021-03-16 | 中国航发北京航空材料研究院 | Salt-fog-corrosion-resistant graphene 3D printing material and preparation method thereof |
CN112552683A (en) * | 2020-11-10 | 2021-03-26 | 中国航发北京航空材料研究院 | Anti-aging graphene 3D printing material and preparation method thereof |
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CN105176084A (en) * | 2015-10-28 | 2015-12-23 | 杨洋 | Composite 3D printing material and preparation method thereof |
CN105255179A (en) * | 2015-10-28 | 2016-01-20 | 徐�明 | Polyether imide compound 3D printing material and preparation method thereof |
CN106675028A (en) * | 2017-01-11 | 2017-05-17 | 河南科技大学 | Preparation method of graphene-modified porous polyimide composite material |
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CN105131585A (en) * | 2015-10-21 | 2015-12-09 | 淄博夸克医药技术有限公司 | Polyamide composite silicon carbide heat dissipation material, preparing method and application thereof |
CN105176084A (en) * | 2015-10-28 | 2015-12-23 | 杨洋 | Composite 3D printing material and preparation method thereof |
CN105255179A (en) * | 2015-10-28 | 2016-01-20 | 徐�明 | Polyether imide compound 3D printing material and preparation method thereof |
CN106675028A (en) * | 2017-01-11 | 2017-05-17 | 河南科技大学 | Preparation method of graphene-modified porous polyimide composite material |
Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107263855A (en) * | 2017-06-19 | 2017-10-20 | 中国航发北京航空材料研究院 | A kind of high-strength high temperature-resistant 3D printing material, wire rod are prepared and Method of printing |
CN110157185A (en) * | 2018-04-12 | 2019-08-23 | 济南开发区星火科学技术研究院 | A kind of graphene 3D printing material with high intensity |
CN109762336A (en) * | 2019-01-18 | 2019-05-17 | 中国航发北京航空材料研究院 | A kind of 3D printing composite wire and preparation method thereof |
CN110102757A (en) * | 2019-04-15 | 2019-08-09 | 中国航发北京航空材料研究院 | A kind of preparation method of the graphene coated copper conducting powder based on fabricated in situ |
CN112500680A (en) * | 2020-11-10 | 2021-03-16 | 中国航发北京航空材料研究院 | Salt-fog-corrosion-resistant graphene 3D printing material and preparation method thereof |
CN112552683A (en) * | 2020-11-10 | 2021-03-26 | 中国航发北京航空材料研究院 | Anti-aging graphene 3D printing material and preparation method thereof |
CN112500680B (en) * | 2020-11-10 | 2022-05-27 | 中国航发北京航空材料研究院 | Salt-fog-corrosion-resistant graphene 3D printing material and preparation method thereof |
CN112552683B (en) * | 2020-11-10 | 2022-06-28 | 中国航发北京航空材料研究院 | Anti-aging graphene 3D printing material and preparation method thereof |
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Application publication date: 20170912 |