CN107022167A - A kind of fiberglass reinforced polyether-ether-ketone 3D printing consumptive material and preparation method thereof - Google Patents
A kind of fiberglass reinforced polyether-ether-ketone 3D printing consumptive material and preparation method thereof Download PDFInfo
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- CN107022167A CN107022167A CN201610069556.5A CN201610069556A CN107022167A CN 107022167 A CN107022167 A CN 107022167A CN 201610069556 A CN201610069556 A CN 201610069556A CN 107022167 A CN107022167 A CN 107022167A
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- peek
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B13/00—Conditioning or physical treatment of the material to be shaped
- B29B13/06—Conditioning or physical treatment of the material to be shaped by drying
- B29B13/065—Conditioning or physical treatment of the material to be shaped by drying of powder or pellets
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/92—Measuring, controlling or regulating
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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
- C08L61/00—Compositions of condensation polymers of aldehydes or ketones; Compositions of derivatives of such polymers
- C08L61/04—Condensation polymers of aldehydes or ketones with phenols only
- C08L61/16—Condensation polymers of aldehydes or ketones with phenols only of ketones with phenols
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92504—Controlled parameter
- B29C2948/9258—Velocity
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92504—Controlled parameter
- B29C2948/92704—Temperature
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92819—Location or phase of control
- B29C2948/92828—Raw material handling or dosing, e.g. active hopper or feeding device
Abstract
The invention provides a kind of fiberglass reinforced polyether-ether-ketone 3D printing consumptive material and preparation method thereof, polyether-ether-ketone 3D printing consumptive material component is by roving glass fiber (GL), polyether-ether-ketone(PEEK)Resin viscosity conditioning agent, PEEK mixed with resin are constituted.The preparation method of polyether-ether-ketone 3D printing consumptive material, comprises the following steps:Raw material drying;Mixed at high speed, melting extrusion, cooling, traction and winding.The present invention adds PEEK resin viscosity conditioning agents in PEEK, can effectively reduce processing of the viscosity so as to fit 3D consumptive materials of PEEK matrix resins.PEEK resin viscosities conditioning agent is constituted using the poly aromatic ether ketone liquid crystal copolymer close with polyether-ether-ketone structure, because structure is similar, is solved and polyether-ether-ketone matrix resin consistency problem.PEEK is again in itself special engineering plastics, is combined with 3D printing forming method, it is more suitable for the making of sophisticated functions part, increases the application field of material.
Description
Technical field
The invention of this reality is related to a kind of 3D printing consumptive material, more particularly to a kind of fiberglass reinforced polyether-ether-ketone 3D printing consumptive material and preparation method thereof.
Background technology
In the development of 3D printing manufacturing technology, material is the key of skill upgrading.3D printing manufacturing technology is a kind of brand-new manufacturing philosophy, and big industrial scale is most applied at last and is intelligently produced.Now, due to the limitation of plastics self-strength so that application of the plastic material in 3D printing is only limitted to common product.In future, plastic material will develop towards high intensity.PEEK is by excellent combination properties such as high-fire resistance, high intensity, high-modulus, high-fracture toughness, it is considered to be the most possible material for being directly used to manufacture all kinds of complex components instead of metal.Most of traditional PEEK products are made using high-temperature injection, simple in construction, and personalized and practicality is not high, and the introducing of 3D printing forming technique will improve material practicality and personalized designs.And PEEK resin viscosities are big, being not easy to must be added to viscosity modifier in the production of 3D consumptive materials, therefore 3D consumptive material production processes reduces its viscosity, makes it suitable for 3D manufacturing industry.
The content of the invention
The technical problem to be solved
The technical problem to be solved in the present invention is to develop a kind of fiberglass reinforced polyether-ether-ketone 3D printing consumptive material, solves tradition PEEK because viscosity cannot be used for greatly 3D printing consumptive material industry, increases its practicality and personalized designs, expand its application field.
Technical scheme
In order to solve the above-mentioned technical problem, the technical solution adopted by the present invention is:A kind of fiberglass reinforced polyether-ether-ketone 3D printing consumptive material and preparation method thereof, is made up of roving glass fiber (GL), PEEK resin viscosities conditioning agent and PEEK mixed with resin.
As currently preferred technical scheme, roving glass fiber (GL) mass percent is that 10 ~ 20%, PEEK resin viscosity conditioning agents mass percent is that 2 ~ 10%, PEEK mass percents are 70 ~ 88%.
As currently preferred technical scheme, PEEK melt index is 2 ~ 10.
As currently preferred technical scheme, the stretch modulus of roving glass fiber (GL) is more than 80GPa.
As currently preferred technical scheme, PEEK resin viscosities conditioning agent is poly aromatic ether ketone liquid crystal copolymer.
Present invention also offers the preparation method of above-mentioned fiberglass reinforced polyether-ether-ketone 3D printing consumptive material, comprise the following steps:
Raw material drying:PEEK powder is dried using drying box;
Mixed at high speed:Use high-speed mixer that PEEK resin viscosities conditioning agent, PEEK are carried out into batch mixing with certain mass percent, so that PEEK resin viscosities conditioning agent and PEEK homogeneous blends;
Melting extrusion:Mixed material is carried out in melting extrusion, extrusion engineering using full-automatic twin screw compounding extruder, roving glass fiber is added by extruder upper end plus fine mouth, the consumptive material of extrusion is after air cooling, into hauling machine;
Traction:By adjusting hauling machine drawing rolls optimum distance, pass through PEEK consumptive materials;
Winding:It will be wound by the rolling machine of the consumptive material of hauling machine.
As currently preferred technical scheme, the temperature in raw material drying step is 80 ~ 150 DEG C, and drying time is 0.5 ~ 2h;
As currently preferred technical scheme, mixing time is 0.5 ~ 5min in mixed at high speed step;Described mass percent be PEEK resin viscosities conditioning agent 2 ~ 10%, PEEK be 70 ~ 88%;
It is used as currently preferred technical scheme, it is 350 ~ 370 DEG C that the parameter of extruder, which is set to area's temperature, in melting extrusion step, and two area's temperature are 350 ~ 370 DEG C, and three area's temperature are 350 ~ 370 DEG C, four area's temperature are 350 ~ 370 DEG C, five area's temperature are 350 ~ 370 DEG C, and six area's temperature are 355 ~ 380 DEG C, and seven area's temperature are 355 ~ 380 DEG C, eight area's temperature are 355 ~ 380 DEG C, head temperature is 355 ~ 380 DEG C, and engine speed is 180 ~ 400r/min, and feeding frequency is 5 ~ 20Hz;Glass fiber content is adjusted by adjusting the radical and engine speed of addition roving glass fiber during melting extrusion, it is 10 ~ 20% to make its mass ratio.
As currently preferred technical scheme, the distance of regulation drawing rolls is 1.0 ~ 1.7mm in distraction step.
Beneficial effect
(1) PEEK resin viscosities are big, and melting extrusion is difficult, are unfavorable for the production of 3D printing consumptive material, and the present invention adds PEEK resin viscosity conditioning agents in PEEK, can effectively reduce processing of the viscosity so as to fit 3D consumptive materials of PEEK matrix resins;(2) PEEK resin viscosities conditioning agent is constituted using the poly aromatic ether ketone liquid crystal copolymer close with polyether-ether-ketone structure, because structure is similar, solve and polyether-ether-ketone matrix resin consistency problem, glass can be promoted scattered in matrix resin simultaneously, glass emergence on the surface is reduced, the bright property of wire surface is improved;(3) PEEK sheets are as special engineering plastics, and excellent performance is combined with 3D printing forming method, it is more suitable for the making of sophisticated functions part, increase the application field of material.
Embodiment
Below in conjunction with the embodiment of the present invention, the technical scheme in the embodiment of the present invention is clearly and completely described, it is clear that described embodiment is only a part of embodiment of the invention, rather than whole embodiments.Based on the embodiment in the present invention, the every other embodiment that those of ordinary skill in the art are obtained under the premise of creative work is not made belongs to the scope of protection of the invention.
Embodiment 1
The fiberglass reinforced polyether-ether-ketone 3D printing consumptive material of the present invention is made up of roving glass fiber (GL), PEEK resin viscosities conditioning agent and PEEK mixed with resin, component is that roving glass fiber (GL) mass percent is that 15%, PEEK resin viscosity conditioning agent mass percents are that 2%, PEEK mass percents are 83%, PEEK melt index is 8, stretch modulus 81GPa, the PEEK resin viscosity conditioning agent of roving glass fiber (GL) is poly aromatic ether ketone liquid crystal copolymer.
The problem of fiberglass reinforced polyether-ether-ketone 3D printing consumptive material of the present embodiment solves traditional 3D printing consumptive material limitation, add application of the consumptive material in terms of high-fire resistance, high intensity, high-modulus, high-fracture toughness, it directly will be used to manufacture all kinds of complex components instead of metal, product not only cheap lightweight again, so that fiberglass reinforced polyether-ether-ketone 3D printing consumptive material is widely used in 3D is manufactured.
The preparation method of this fiberglass reinforced polyether-ether-ketone 3D printing consumptive material, comprises the following steps successively:
Raw material drying:PEEK powder is dried using drying box;Temperature is 100 DEG C, and drying time is 1h;
Mixed at high speed:Use high-speed mixer that PEEK resin viscosities conditioning agent, PEEK are carried out into batch mixing with certain mass percent, so that mixing time is 0.5min in PEEK resin viscosities conditioning agent and PEEK homogeneous blends, mixed at high speed step;Described mass percent is that PEEK resin viscosities conditioning agent 2%, PEEK are 83%;
Melting extrusion:Mixed material is carried out in melting extrusion, extrusion engineering using full-automatic twin screw compounding extruder, roving glass fiber is added by extruder upper end plus fine mouth, the consumptive material of extrusion is after air cooling, into hauling machine;The parameter of extruder is set to area's temperature for 350 DEG C in melting extrusion step, two area's temperature are 350 DEG C, three area's temperature are 350 DEG C, and four area's temperature are 355 DEG C, and five area's temperature are 355 DEG C, six area's temperature are 355 DEG C, seven area's temperature are 355 DEG C, and eight area's temperature are 355 DEG C, and head temperature is 355 DEG C, engine speed is 250r/min, and feeding frequency is 15Hz;Glass fiber content is adjusted by adjusting the radical and engine speed of addition roving glass fiber during melting extrusion, it is 15% to make its mass ratio.
Traction:By adjusting hauling machine drawing rolls optimum distance, pass through PEEK consumptive materials, the distance that drawing rolls are adjusted in distraction step is 1.6mm.
Winding:It will be wound by the rolling machine of the consumptive material of hauling machine, in winding step, adjust the rotating speed of winding and the rotating speed of main frame, it is 1.7mm to make consumptive material line footpath.
The performance of the fiberglass reinforced polyether-ether-ketone 3D printing consumptive material material of preparation reaches following index:
The performance of the fiberglass reinforced polyether-ether-ketone 3D printing consumptive material material of table 1
Sequence number | Test item | Standard and test condition | Test result |
1 | Simply supported beam unnotched impact strength(KJ/m2) | ISO 179-1:2010 | 64.5(Fracture completely) |
2 | Simply supported beam notch impact strength(KJ/m2) | ISO 179-1:2010 | 6.7(Fracture completely) |
3 | Izod notched impact strength(KJ/m2) | ISO 180:2010 | 7.1 |
4 | Cantilever beam unnotched impact strength(KJ/m2) | ISO 180:2010 | 77.7 |
5 | Tensile strength(MPa) | ISO 527-2:2012 | 118.5 |
6 | It is broken norminal strain(%) | ISO 527-2:2012 | 4 |
7 | Bending strength(MPa) | ISO 178:2010 | 192.4 |
8 | Bending modulus(MPa) | ISO 178:2010 | 5823 |
9 | Ash content(%) | ISO 3451-1:2008 Method A | 16.4 |
10 | Ball indentation hardness | ISO 2039-1:2001 | 234 |
11 | Rockwell hardness | ISO 2039-2:2001 | 121 |
12 | Shao's D hardness | ISO 868:2003 | 86 |
Claims (9)
1. a kind of fiberglass reinforced polyether-ether-ketone 3D printing consumptive material and preparation method thereof, it is characterised in that:Component is made up of roving glass fiber (GL), PEEK resin viscosities conditioning agent and PEEK mixed with resin, roving glass fiber (GL)
Mass percent is that 10 ~ 20%, PEEK resin viscosity conditioning agents mass percent is that 2 ~ 10%, PEEK mass percents are 70 ~ 88%.
2. fiberglass reinforced polyether-ether-ketone 3D printing consumptive material according to claim 1, it is characterised in that:PEEK melt index is 2 ~ 10.
3. fiberglass reinforced polyether-ether-ketone 3D printing consumptive material according to claim 1, it is characterised in that:The stretch modulus of roving glass fiber (GL) is more than 80GPa.
4. fiberglass reinforced polyether-ether-ketone 3D printing consumptive material according to claim 1, it is characterised in that:PEEK resin viscosities conditioning agent is poly aromatic ether ketone liquid crystal copolymer.
5. the preparation method of fiberglass reinforced polyether-ether-ketone 3D printing consumptive material according to claim 1, comprises the following steps:
Raw material drying:PEEK powder is dried using drying box;
Mixed at high speed:Use high-speed mixer that PEEK resin viscosities conditioning agent and PEEK are carried out into batch mixing with certain mass percent, so that PEEK resin viscosities conditioning agent and PEEK homogeneous blends;
Melting extrusion:Mixed material is carried out in melting extrusion, extrusion using full-automatic twin screw compounding extruder, roving glass fiber is added by extruder upper end plus fine mouth, the consumptive material of extrusion is after air cooling, into hauling machine;
Traction:By adjusting hauling machine drawing rolls optimum distance, pass through PEEK consumptive materials;
Winding:It will be wound by the rolling machine of the consumptive material of hauling machine.
6. the preparation method of fiberglass reinforced polyether-ether-ketone 3D printing consumptive material according to claim 1, it is characterised in that:Temperature in raw material drying step is 80 ~ 150 DEG C, and drying time is 0.5 ~ 2h.
7. the preparation method of fiberglass reinforced polyether-ether-ketone 3D printing consumptive material according to claim 1, it is characterised in that:Mixing time is 0.5 ~ 5min in mixed at high speed step.
8. the preparation method of fiberglass reinforced polyether-ether-ketone 3D printing consumptive material according to claim 1, it is characterised in that:The parameter of extruder is set to area's temperature for 350 ~ 370 DEG C in melting extrusion step, two area's temperature are 350 ~ 370 DEG C, three area's temperature are 350 ~ 370 DEG C, and four area's temperature are 350 ~ 370 DEG C, and five area's temperature are 350 ~ 370 DEG C, six area's temperature are 355 ~ 380 DEG C, seven area's temperature are 355 ~ 380 DEG C, and eight area's temperature are 355 ~ 380 DEG C, and head temperature is 355 ~ 380 DEG C, engine speed is 180 ~ 400r/min, and feeding frequency is 5 ~ 20Hz.
9. the preparation method of fiberglass reinforced polyether-ether-ketone 3D printing consumptive material according to claim 1, it is characterised in that:The distance that drawing rolls are adjusted in distraction step is 1.0 ~ 1.7mm.
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Cited By (8)
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CN108395672A (en) * | 2018-04-04 | 2018-08-14 | 李垒 | A kind of 3D printing aramid fiber reinforced polyether ether ketone wire rod and preparation method thereof |
CN109605610A (en) * | 2018-12-27 | 2019-04-12 | 陕西恒通智能机器有限公司 | A kind of control method of 3D printing silk material Forming Quality |
CN111424333A (en) * | 2020-05-08 | 2020-07-17 | 广安长明高端产业技术研究院 | Electrostatic spinning PEEK/low-melting-point metal composite fiber, 3D printing consumable material and preparation method thereof |
CN113185801A (en) * | 2021-04-16 | 2021-07-30 | 航天材料及工艺研究所 | Polyether-ether-ketone composite material 3D printing wire material applicable to space environment and preparation method thereof |
CN113248863A (en) * | 2021-04-02 | 2021-08-13 | 南京聚隆科技股份有限公司 | Laser-weldable carbon fiber modified PEEK material and preparation method thereof |
US11118053B2 (en) | 2018-03-09 | 2021-09-14 | Ticona Llc | Polyaryletherketone/polyarylene sulfide composition |
US11352480B2 (en) | 2016-03-18 | 2022-06-07 | Ticona Llc | Polyaryletherketone composition |
US11661521B2 (en) | 2019-12-17 | 2023-05-30 | Ticona Llc | Three-dimensional printing system employing a thermotropic liquid crystalline polymer |
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US11352480B2 (en) | 2016-03-18 | 2022-06-07 | Ticona Llc | Polyaryletherketone composition |
US11118053B2 (en) | 2018-03-09 | 2021-09-14 | Ticona Llc | Polyaryletherketone/polyarylene sulfide composition |
CN108395672A (en) * | 2018-04-04 | 2018-08-14 | 李垒 | A kind of 3D printing aramid fiber reinforced polyether ether ketone wire rod and preparation method thereof |
CN109605610A (en) * | 2018-12-27 | 2019-04-12 | 陕西恒通智能机器有限公司 | A kind of control method of 3D printing silk material Forming Quality |
US11661521B2 (en) | 2019-12-17 | 2023-05-30 | Ticona Llc | Three-dimensional printing system employing a thermotropic liquid crystalline polymer |
CN111424333A (en) * | 2020-05-08 | 2020-07-17 | 广安长明高端产业技术研究院 | Electrostatic spinning PEEK/low-melting-point metal composite fiber, 3D printing consumable material and preparation method thereof |
CN111424333B (en) * | 2020-05-08 | 2022-06-03 | 广安长明高端产业技术研究院 | Electrostatic spinning PEEK/low-melting-point metal composite fiber, 3D printing consumable material and preparation method thereof |
CN113248863A (en) * | 2021-04-02 | 2021-08-13 | 南京聚隆科技股份有限公司 | Laser-weldable carbon fiber modified PEEK material and preparation method thereof |
CN113248863B (en) * | 2021-04-02 | 2024-02-27 | 南京聚隆科技股份有限公司 | Carbon fiber modified PEEK material capable of being welded by laser and preparation method thereof |
CN113185801A (en) * | 2021-04-16 | 2021-07-30 | 航天材料及工艺研究所 | Polyether-ether-ketone composite material 3D printing wire material applicable to space environment and preparation method thereof |
CN113185801B (en) * | 2021-04-16 | 2023-02-03 | 航天材料及工艺研究所 | Polyether-ether-ketone composite material 3D printing wire material applicable to space environment and preparation method thereof |
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Application publication date: 20170808 |