CN105176084A - Composite 3D printing material and preparation method thereof - Google Patents
Composite 3D printing material and preparation method thereof Download PDFInfo
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- CN105176084A CN105176084A CN201510714300.0A CN201510714300A CN105176084A CN 105176084 A CN105176084 A CN 105176084A CN 201510714300 A CN201510714300 A CN 201510714300A CN 105176084 A CN105176084 A CN 105176084A
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- polyetherimide
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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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L63/00—Compositions of epoxy resins; Compositions of derivatives of epoxy resins
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
Abstract
The invention provides a composite 3D printing material and a preparation method thereof. The composite 3D printing material is characterized by being prepared from, by weight, 40-100 parts of polyetherimide, 40-100 parts of epoxy resin, 5-10 parts of inorganic fillers, 5-20 parts of coupling agents, 0.1-0.5 part of light stabilizers, 0.1-2 parts of flatting agents, 0.1-2 parts of antioxidants, 0.1-2 parts of degassing agents and 1-6 parts of dispersed lubricants. Compared with a traditional polyetherimide material, the polyetherimide composite 3D printing material has higher strength and hardness and can be used at high temperature.
Description
Technical field
The invention belongs to field of compound material, be specifically related to a kind of preparation method of compound 3D printed material.
Background technology
It is a kind of based on digital model file that 3D prints, and applying powder last current state metal or plastics etc. can the rapid shaping techniques of jointing material, are described as the Industrial Revolution again of overturning traditional manufacture.This technology is at jewelry, footwear, industrial design, building, engineering and construction (AEC), dentistry and medical industries, education, geographical information system(GIS), civil engineering work, automobile, and aerospace, gun and other field are applied all to some extent.Since 3D prints birth, change to functional and service product from industry, BUILDINGS MODELS print.And under the intelligence manufacture background in future, 3D printing technique will with other modern technique fusion developments such as internet, cloud computing, Internet of Things, large data.But existing 3D printed material is applied in the problem that the fields such as aerospace automobile also exist insufficient strength, therefore urgently exploitation is a kind of comparatively mates with 3D printer mobility, formability, has the 3D printed material of sufficient intensity and hardness simultaneously.
Summary of the invention
The object of the present invention is to provide a kind of compound 3D printed material and preparation method thereof, the present invention effectively can improve mechanical property, dimensional stability, thermotolerance, the ageing-resistant performance of 3D printing matrix material.Expand polyamide material high-end applications scope in automobile, aerospace.
For realizing above object, technical scheme of the present invention is:
A kind of compound 3D printed material, is characterized in that, be made up of the raw material of following weight part:
Described polyetherimide compound 3D printed material, each component is preferably made up of the raw material of following weight part:
Described polyetherimide is oxygen index is 47%, and density is the commercially available polyetherimide of 1.28 ~ 1.42g/cm3; Described epoxy resin is commercially available glycidyl amine epoxy resin, and described Gum Rosin is commercial rosin resin, and described mineral filler is potassium titanate crystal whisker or Graphene, and described coupling agent is zirconium class coupling agent; Described flow agent is polydimethylsiloxane or butyl cellulose, described photostabilizer is ESCALOL 567 or 5-chlorination benzotriazole, described flow agent is polydimethylsiloxane, butyl cellulose or isopropyl cellulose, described oxidation inhibitor is 2,6-tri-grades of butyl-4-methylphenols, described air release agent is Viscotrol C or butylbenzene rubber cement, and described dispersed lubricant is polyethylene wax or bis-fatty acid amides.
Further, described potassium titanate crystal whisker is diameter 0.1 ~ 5 micron, and length is 5 ~ 100 microns, and density is 4g/cm3, the potassium titanate crystal whisker that purity (wt%) is 90-99.9%.
A preparation method for compound 3D printed material, comprises the following steps:
1) epoxy resin, oxidation inhibitor, dispersed lubricant, coupling agent are put into material-compound tank according to described formula ratio, in heating unit, rapid stirring 1 ~ 3h, obtains product A;
2) mineral filler added in the product A of above-mentioned melting, ultrasonic vibration 10 ~ 30min, obtains product B;
3) at 100 ~ 200 DEG C, in product B, add polyetherimide, photostabilizer, flow agent, air release agent, continue the product C of stirring 1 ~ 2h;
4) product C is cooled to room temperature, pulverizes, can obtain compound 3D printed material after screening with ball mill grinding.
Described step 1) in Heating temperature be 100 DEG C, stirring velocity is 600r/min, step 3) in stirring velocity be 800r/min, step 4) in grind and the median size of sieve afterwards described compound 3D printed material is 20 μm.
This materials'use EOSP396 model 3D printer, adopts powder sintered shaping (SelectedLaserSintering is called for short SLS) technology, utilizes infrared laser to carry out powdered material powder sintered shaping.
The invention has the beneficial effects as follows:
Beneficial effect:
(1) a kind of compound 3D printed material of the present invention is compared with traditional polyamide material, and compound 3D printed material of the present invention has higher bending elastic modulus, tensile strength, dimensional stability and thermal distoftion temperature, can at high temperature use.
(2) a kind of compound 3D printed material process of the present invention is simple, is easy to suitability for industrialized production
(3) a kind of compound 3D printed material raw material of the present invention is cheap, wide material sources, and has good environmental benefit and economic benefit.
Embodiment
The present invention is described in further detail by embodiment.
Embodiment 1
Raw material is prepared according to the raw material of following weight part:
Polyetherimide 40; Glycidyl amine epoxy resin 40; Mineral filler 10; Zirconium class coupling agent 5; ESCALOL 567 0.1; Polydimethylsiloxane 0.1; 2,6-, tri-grades of butyl-4-methylphenols 0.1; Butylbenzene rubber cement 0.1; Polyethylene wax 1.
Described mineral filler is diameter 0.1 ~ 5 micron, and length is 5 ~ 100 microns, and density is 4g/cm3, the potassium titanate crystal whisker that purity (wt%) is 90-99.9%.
Described polyetherimide is oxygen index is 47%, and density is the commercially available polyetherimide of 1.28 ~ 1.42g/cm3.
Preparation process is:
1) epoxy resin, oxidation inhibitor, dispersed lubricant, coupling agent are put into material-compound tank according to described formula ratio, in heating unit, 600r/min stirs 1 ~ 3h, and Heating temperature 100 DEG C, obtains product A;
2) mineral filler added in the product A of above-mentioned melting, ultrasonic vibration 10 ~ 30min, obtains product B;
3) at 100 ~ 200 DEG C, in product B, add polyetherimide, photostabilizer, flow agent, air release agent, continue the product C of stirring 1 ~ 2h, stirring velocity 800r/min;
4) product C is cooled to room temperature, pulverizes with ball mill grinding, and pulverizing the median size obtained is 20 μm, can obtain compound 3D printed material after screening.
Embodiment 2
Raw material is prepared according to the raw material of following weight part:
Polyetherimide 100; Glycidyl amine epoxy resin 100; Mineral filler 20; Zirconium class coupling agent 20; ESCALOL 567 0.5; Polydimethylsiloxane 2; 2,6-, tri-grades of butyl-4-methylphenols 2; Butylbenzene rubber cement 2; Polyethylene wax 6.
Described mineral filler is diameter 0.1 ~ 5 micron, and length is 5 ~ 100 microns, and density is 4g/cm3, the potassium titanate crystal whisker that purity (wt%) is 90-99.9%.
Described polyetherimide is oxygen index is 47%, and density is the commercially available polyetherimide of 1.28 ~ 1.42g/cm3.
Preparation process is:
1) epoxy resin, oxidation inhibitor, dispersed lubricant, coupling agent are put into material-compound tank according to described formula ratio, in heating unit, 600r/min stirs 1 ~ 3h, and Heating temperature 100 DEG C, obtains product A;
2) mineral filler added in the product A of above-mentioned melting, ultrasonic vibration 10 ~ 30min, obtains product B;
3) at 100 ~ 200 DEG C, in product B, add polyetherimide, photostabilizer, flow agent, air release agent, continue the product C of stirring 1 ~ 2h, stirring velocity 800r/min;
4) product C is cooled to room temperature, pulverizes with ball mill grinding, and pulverizing the median size obtained is 20 μm, can obtain 3D printed material after screening.
Embodiment 3
Raw material is prepared according to the raw material of following weight part:
Polyetherimide 40; Glycidyl amine epoxy resin 40; Mineral filler 10; Zirconium class coupling agent 5; ESCALOL 567 0.1; Polydimethylsiloxane 0.1; 2,6-, tri-grades of butyl-4-methylphenols 0.1; Butylbenzene rubber cement 0.1; Polyethylene wax 1.
Described mineral filler is diameter 0.1 ~ 5 micron, and length is 5 ~ 100 microns, and density is 4g/cm3, the potassium titanate crystal whisker that purity (wt%) is 90-99.9%.
Described polyetherimide is oxygen index is 47%, and density is the commercially available polyetherimide of 1.28 ~ 1.42g/cm3.
Preparation process is:
1) epoxy resin, oxidation inhibitor, dispersed lubricant, coupling agent are put into material-compound tank according to described formula ratio, in heating unit, 600r/min stirs 1 ~ 3h, and Heating temperature 100 DEG C, obtains product A;
2) mineral filler added in the product A of above-mentioned melting, ultrasonic vibration 10 ~ 30min, obtains product B;
3) at 100 ~ 200 DEG C, in product B, add polyetherimide, photostabilizer, flow agent, air release agent, continue the product C of stirring 1 ~ 2h, stirring velocity 800r/min;
4) product C is cooled to room temperature, pulverizes with ball mill grinding, and pulverizing the median size obtained is 20 μm, can obtain compound 3D printed material after screening.
Embodiment 4
Raw material is prepared according to the raw material of following weight part:
Polyetherimide 100; Glycidyl amine epoxy resin 100; Graphene 20; Zirconium class coupling agent 20; 5-chlorination benzotriazole 0.5; Polydimethylsiloxane 2; 2,6-, tri-grades of butyl-4-methylphenols 2; Butylbenzene rubber cement 2; Polyethylene wax 6.
Described polyetherimide is oxygen index is 47%, and density is the commercially available polyetherimide of 1.28 ~ 1.42g/cm3.
Preparation process is:
1) epoxy resin, oxidation inhibitor, dispersed lubricant, coupling agent are put into material-compound tank according to described formula ratio, in heating unit, 600r/min stirs 1 ~ 3h, and Heating temperature 100 DEG C, obtains product A;
2) mineral filler added in the product A of above-mentioned melting, ultrasonic vibration 10 ~ 30min, obtains product B;
3) at 100 ~ 200 DEG C, in product B, add polyetherimide, photostabilizer, flow agent, air release agent, continue the product C of stirring 1 ~ 2h, stirring velocity 800r/min;
4) product C is cooled to room temperature, pulverizes with ball mill grinding, and pulverizing the median size obtained is 20 μm, can obtain compound 3D printed material after screening.
Described mineral filler is the Graphene of diameter 0.1 micron.
Embodiment 5
Raw material is prepared according to the raw material of following weight part:
Polyetherimide 70; Glycidyl amine epoxy resin 70; Mineral filler 18; Zirconium class coupling agent 15; ESCALOL 567 1; Polydimethylsiloxane 1; 2,6-, tri-grades of butyl-4-methylphenols 1; Butylbenzene rubber cement 1; Polyethylene wax 3.
Described mineral filler is diameter 0.1 ~ 5 micron, and length is 5 ~ 100 microns, and density is 4g/cm3, the potassium titanate crystal whisker that purity (wt%) is 90-99.9%.
Described polyetherimide is oxygen index is 47%, and density is the commercially available polyetherimide of 1.28 ~ 1.42g/cm3.
Preparation process is:
1) epoxy resin, oxidation inhibitor, dispersed lubricant, coupling agent are put into material-compound tank according to described formula ratio, in heating unit, 600r/min stirs 1 ~ 3h, and Heating temperature 100 DEG C, obtains product A;
2) mineral filler added in the product A of above-mentioned melting, ultrasonic vibration 10 ~ 30min, obtains product B;
3) at 100 ~ 200 DEG C, in product B, add polyetherimide, photostabilizer, flow agent, air release agent, continue the product C of stirring 1 ~ 2h, stirring velocity 800r/min;
4) product C is cooled to room temperature, pulverizes with ball mill grinding, and pulverizing the median size obtained is 20 μm, can obtain compound 3D printed material after screening.
Table 1 embodiment 1-5 prepares compound 3D printed material at the substandard performance test table of ISO527-1/-2:
| Test sample | Tensile modulus (pound) | Tensile strength (pound) | Elongation at break (%) |
| Embodiment 1 | 987600 | 69600 | 2.5 |
| Embodiment 2 | 998940 | 70400 | 3.0 |
| Embodiment 3 | 984620 | 67322 | 3.2 |
| Embodiment 4 | 998760 | 69680 | 3.1 |
| Embodiment 5 | 1089100 | 74230 | 3.4 |
Shown by above data, embodiments of the invention 5 tensile modulus, tensile strength are very high, with the obvious advantage.
More than show and describe ultimate principle of the present invention, principal character and advantage of the present invention.The technician of the industry should understand; the present invention is not restricted to the described embodiments; what describe in above-described embodiment and specification sheets just illustrates principle of the present invention; the present invention also has various changes and modifications without departing from the spirit and scope of the present invention, and these changes and improvements all fall in the claimed scope of the invention.Application claims protection domain is defined by appending claims and equivalent thereof.
Claims (6)
1.
a kind of compound 3D printed material, is characterized in that, be made up of the raw material of following weight part: polyetherimide 40 ~ 100; Epoxy resin 40 ~ 100; Mineral filler 5 ~ 10; Coupling agent 5 ~ 20; Photostabilizer 0.1 ~ 0.5; Flow agent 0.1 ~ 2; Oxidation inhibitor 0.1 ~ 2; Air release agent 0.1 ~ 2; Dispersed lubricant 1 ~ 6.
2.
compound 3D printed material according to claim 1, is characterized in that: be made up of the raw material of following weight part: polyetherimide 70; Epoxy resin 70; Mineral filler 8; Coupling agent 15; Photostabilizer 0.3; Flow agent 1; Oxidation inhibitor 1; Air release agent 1; Dispersed lubricant 3.
3.
compound 3D printed material according to claim 1 and 2, described polyetherimide is oxygen index is 47%, and density is the commercially available polyetherimide of 1.28 ~ 1.42g/cm3; Described epoxy resin is commercially available glycidyl amine epoxy resin, and described mineral filler is potassium titanate crystal whisker or Graphene, and described coupling agent is zirconium class coupling agent; Described flow agent is polydimethylsiloxane or butyl cellulose, described photostabilizer is ESCALOL 567 or 5-chlorination benzotriazole, described flow agent is polydimethylsiloxane, butyl cellulose or isopropyl cellulose, described oxidation inhibitor is 2,6-tri-grades of butyl-4-methylphenols, described air release agent is Viscotrol C or butylbenzene rubber cement, and described dispersed lubricant is polyethylene wax or bis-fatty acid amides.
4.
compound 3D printed material according to claim 3, described potassium titanate crystal whisker is diameter 0.1 ~ 5 micron, and length is 5 ~ 100 microns, the potassium titanate crystal whisker that purity (wt%) is 90-99.9%.
5.
the preparation method of a kind of compound 3D printed material according to claim 1-4, comprises the following steps:
1) epoxy resin, oxidation inhibitor, dispersed lubricant, coupling agent are put into material-compound tank according to described formula ratio, in heating unit, rapid stirring 1 ~ 3h, obtains product A;
2) mineral filler added in the product A of above-mentioned melting, ultrasonic vibration 10 ~ 30min, obtains product B;
3) at 100 ~ 200 DEG C, in product B, add polyetherimide, photostabilizer, flow agent, air release agent, continue the product C of stirring 1 ~ 2h;
4) product C is cooled to room temperature, pulverizes, can obtain compound 3D printed material after screening with ball mill grinding.
6.
the preparation method of compound 3D printed material according to claim 5, in described step 1), Heating temperature is 100 DEG C, stirring velocity is 600r/min, in step 3), stirring velocity is 800r/min, in step 4) grind and the median size of described compound 3D printed material is 20 μm after sieving.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106905714A (en) * | 2017-03-12 | 2017-06-30 | 广西丰达三维科技有限公司 | A kind of Graphene modified flame retardant type bamboo moulding material, preparation method and applications |
| CN106916469A (en) * | 2017-03-26 | 2017-07-04 | 广西丰达三维科技有限公司 | A kind of environment-friendly materials with high tensile, preparation method and applications |
| CN107151443A (en) * | 2017-05-27 | 2017-09-12 | 中国航发北京航空材料研究院 | A kind of PEI base graphene 3D printing composite and preparation method thereof |
| CN107353644A (en) * | 2017-07-27 | 2017-11-17 | 广州新诚生物科技有限公司 | A kind of 3D printing material and preparation method thereof |
| CN107698919A (en) * | 2017-10-31 | 2018-02-16 | 陕西爱骨医疗股份有限公司 | A kind of 3D printing bio-flexible material and preparation method thereof |
| CN109642082A (en) * | 2016-08-30 | 2019-04-16 | 大塚化学株式会社 | Resin combination, three-dimensional printer long filament and toner and moulder and its manufacturing method |
| 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 |
| US11674030B2 (en) | 2017-11-29 | 2023-06-13 | Corning Incorporated | Highly loaded inorganic filled aqueous resin systems |
| US11912860B2 (en) | 2018-03-29 | 2024-02-27 | Corning Incorporated | Highly loaded inorganic filled organic resin systems |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109642082A (en) * | 2016-08-30 | 2019-04-16 | 大塚化学株式会社 | Resin combination, three-dimensional printer long filament and toner and moulder and its manufacturing method |
| US11718732B2 (en) | 2016-08-30 | 2023-08-08 | Otsuka Chemical Co., Ltd | Resin composition, filament and resin powder for three-dimensional printer, and shaped object and production process therefor |
| CN106905714A (en) * | 2017-03-12 | 2017-06-30 | 广西丰达三维科技有限公司 | A kind of Graphene modified flame retardant type bamboo moulding material, preparation method and applications |
| CN106916469A (en) * | 2017-03-26 | 2017-07-04 | 广西丰达三维科技有限公司 | A kind of environment-friendly materials with high tensile, preparation method and applications |
| CN107151443A (en) * | 2017-05-27 | 2017-09-12 | 中国航发北京航空材料研究院 | A kind of PEI base graphene 3D printing composite and preparation method thereof |
| CN107353644A (en) * | 2017-07-27 | 2017-11-17 | 广州新诚生物科技有限公司 | A kind of 3D printing material and preparation method thereof |
| CN107353644B (en) * | 2017-07-27 | 2020-11-13 | 惠州康脉生物材料有限公司 | 3D printing material and preparation method thereof |
| CN107698919A (en) * | 2017-10-31 | 2018-02-16 | 陕西爱骨医疗股份有限公司 | A kind of 3D printing bio-flexible material and preparation method thereof |
| US11674030B2 (en) | 2017-11-29 | 2023-06-13 | Corning Incorporated | Highly loaded inorganic filled aqueous resin systems |
| US11912860B2 (en) | 2018-03-29 | 2024-02-27 | Corning Incorporated | Highly loaded inorganic filled organic resin systems |
| 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 |
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