CN106674952A - 3D printing PC-AES material and preparation method thereof - Google Patents

3D printing PC-AES material and preparation method thereof Download PDF

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Publication number
CN106674952A
CN106674952A CN201611060202.0A CN201611060202A CN106674952A CN 106674952 A CN106674952 A CN 106674952A CN 201611060202 A CN201611060202 A CN 201611060202A CN 106674952 A CN106674952 A CN 106674952A
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China
Prior art keywords
consumption
weight portions
aes
preparation
printing
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Pending
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CN201611060202.0A
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Chinese (zh)
Inventor
黄仲佳
王心生
杨军
姚春
李思文
郑兰斌
吴志华
吕晨
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Anhui Chungu 3D Printing Technology Research Institute of Intelligent Equipment Industry
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Anhui Chungu 3D Printing Technology Research Institute of Intelligent Equipment Industry
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Priority to CN201611060202.0A priority Critical patent/CN106674952A/en
Publication of CN106674952A publication Critical patent/CN106674952A/en
Pending legal-status Critical Current

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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
    • C08L69/00—Compositions of polycarbonates; Compositions of derivatives of polycarbonates
    • 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
    • C08K2201/00—Specific properties of additives
    • C08K2201/011—Nanostructured additives
    • 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
    • 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

Abstract

The invention discloses a 3D printing PC-AES material and a preparation method of the 3D printing PC-AES material. The preparation method comprises the following steps: 1) soaking PC in an acid solution and filtering, taking a filter cake, and melting furfuryl alcohol, sodium laurylsulfate, polyether-ether-ketone, methylcellulose, calcium carbonate, coal ash, propolis, zirconium oxide, aminopropyltriethoxysilane, chitosan and the filter cake to prepare a first melt; 2) melting AES, pentaerythritol, palm oil, ferrocene, borax, carbon nano tube and polyether ketone to prepare a second melt; 3) blending the first melt and the second melt, molding and pelletizing to prepare a PC-AES particle; 4) grinding the PC-AES particle to prepare the 3D printing PC-AES material. The 3D printing PC-AES material is excellent in strength, toughness and heat resistance, and meanwhile, the preparation method has the characteristics that the raw materials are easy to get and the process is simple.

Description

3D printing PC-AES materials and preparation method thereof
Technical field
The present invention relates to 3D printing material, in particular it relates to 3D printing PC-AES materials and preparation method thereof.
Background technology
3D printing material is the important substance basis of 3D printing technique development, and to a certain extent, the development of material is to determine Can 3D printing be determined the deciding factor being more widely used.At present, 3D printing material mainly include engineering plastics, Photosensitive resin, rubber type of material, metal material and ceramic material.
Engineering plastics refer to be used as the industrial plasticses of industrial part or sheathing material, and its requirement is with excellent Intensity, resistance to impact, heat resistance, hardness and ageing resistace, common are AES plastics, PC plastics and nylon etc..Though So, these materials itself are respectively provided with excellent performance, but there is also certain defect, it is difficult to be competent at wanting for engineering plastics completely Ask；Compatibility simultaneously between these homogenous materials is also poor.
The content of the invention
It is an object of the invention to provide a kind of 3D printing PC-AES materials and preparation method thereof, 3D printing PC-AES materials With excellent intensity, toughness and heat resistance, while there is the preparation method raw material to be easy to get, the characteristics of operation is simple.
To achieve these goals, the invention provides a kind of preparation method of 3D printing PC-AES materials, including：
1) PC (Merlon) is placed in acid solution and soaks, filters to take filter cake, then by furfuryl alcohol, sldium lauryl sulfate, poly- Ether ether ketone, methylcellulose, calcium carbonate, flyash, propolis, zirconium oxide, aminopropyl triethoxysilane, chitin and filter cake enter Row melting is with prepared first fused mass；
2) by AES (acrylonitrile ethylene styrene copolymer), pentaerythrite, palm oil, ferrocene, borax, carbon nanometer Pipe is melted that the second fused mass is obtained with polyether sulfone；
3) the first fused mass and the second fused mass are blended, molding, granulating to be to be obtained PC-AES particles；
4) PC-AES particles are ground that 3D printing PC-AES materials are obtained.
Present invention also offers a kind of 3D printing PC-AES materials, 3D printing PC-AES materials are by above-mentioned preparation side Method is prepared.
In technical scheme is stated, the present invention causes obtained 3D printing by the synergy of each raw material and each step PC-AES materials have excellent intensity, toughness and heat resistance, while there is the preparation method raw material to be easy to get, operation is simply special Point.
Other features and advantages of the present invention will be described in detail in subsequent specific embodiment part.
Specific embodiment
The specific embodiment of the present invention is described in detail below.It should be appreciated that described herein concrete Embodiment is merely to illustrate and explains the present invention, is not limited to the present invention.
The invention provides a kind of preparation method of 3D printing PC-AES materials, including：
1) PC (Merlon) is placed in acid solution and soaks, filters to take filter cake, then by furfuryl alcohol, sldium lauryl sulfate, poly- Ether ether ketone, methylcellulose, calcium carbonate, flyash, propolis, zirconium oxide, aminopropyl triethoxysilane, chitin and filter cake enter Row melting is with prepared first fused mass；
2) by AES (acrylonitrile ethylene styrene copolymer), pentaerythrite, palm oil, ferrocene, borax, carbon nanometer Pipe is melted that the second fused mass is obtained with polyether sulfone；
3) the first fused mass and the second fused mass are blended, molding, granulating to be to be obtained PC-AES particles；
4) PC-AES particles are ground that 3D printing PC-AES materials are obtained.
In the step 1 of the present invention) in, the consumption of each material can be selected in wide scope, but in order that obtained 3D printing PC-AES materials have more excellent intensity, toughness and heat resistance, it is preferable that in step 1) in, immersion at least meets Following condition：Soaking temperature is 50-60 DEG C, and soak time is 4-6h.
In the step 1 of the present invention) in, the actual conditions of acid solution can be selected in wide scope, but in order that be obtained 3D printing PC-AES materials have more excellent intensity, toughness and heat resistance, it is preferable that in step 1) in, acid solution is at least full Be enough to lower condition：PH is 4-6, one or more in aqueous hydrochloric acid solution, phosphate aqueous solution and aqueous sulfuric acid.
In the step 1 of the present invention) in, the actual conditions of melting can be selected in wide scope, but in order that be obtained 3D printing PC-AES materials have more excellent intensity, toughness and heat resistance, it is preferable that in step 1) in, melt it is at least full Be enough to lower condition：Melt temperature is 290-305 DEG C, and the melting time is 1-3h.
In the step 1 of the present invention) in, the consumption of each material can be selected in wide scope, but in order that obtained 3D printing PC-AES materials have more excellent intensity, toughness and heat resistance, it is preferable that in step 1) in, relative to 100 weight Part filter cake, the consumption of furfuryl alcohol is 34-42 weight portions, and the consumption of sldium lauryl sulfate is 14-31 weight portions, the use of polyether-ether-ketone Measure as 78-88 weight portions, the consumption of methylcellulose is 9-16 weight portions, the consumption of calcium carbonate is 23-34 weight portions, flyash Consumption be 41-55 weight portions, the consumption of propolis is 18-23 weight portions, and zirconic consumption is 9-17 weight portions, aminopropyl three The consumption of Ethoxysilane is 11-18 weight portions, and the consumption of chitin is 25-35 weight portions.
In the step 2 of the present invention) in, the actual conditions of melting can be selected in wide scope, but in order that be obtained 3D printing PC-AES materials have more excellent intensity, toughness and heat resistance, it is preferable that in step 2) in, melt it is at least full Be enough to lower condition：Melt temperature is 185-195 DEG C, and the melting time is 2-4h.
In the step 2 of the present invention) in, the consumption of each material can be selected in wide scope, but in order that obtained 3D printing PC-AES materials have more excellent intensity, toughness and heat resistance, it is preferable that in step 2) in, relative to 100 weight The AES of part, the consumption of pentaerythrite is 38-45 weight portions, and the consumption of palm oil is 5-12 weight portions, and the consumption of ferrocene is 3- 7 weight portions, the consumption of borax is 15-26 weight portions, and the consumption of CNT is 1-3 weight portions, and the consumption of polyether sulfone is 75-82 Weight portion.
In the step 3 of the present invention) in, the consumption of each material can be selected in wide scope, but in order that obtained 3D printing PC-AES materials have more excellent intensity, toughness and heat resistance, it is preferable that in step 3) in, first melting The weight ratio of thing and the second fused mass is 1：0.7-0.9.
In the step 3 of the present invention) in, the actual conditions of blending can be selected in wide scope, but in order that be obtained 3D printing PC-AES materials have more excellent intensity, toughness and heat resistance, it is preferable that in step 3) in, be blended it is at least full Be enough to lower condition：Blending temperature is 225-250 DEG C, and the blending time is 3-5h.
In the step 4 of the present invention) in, the actual conditions of grinding can be selected in wide scope, but in order that be obtained 3D printing PC-AES materials have more excellent intensity, toughness and heat resistance, it is preferable that in step 4) in, grinding adopt ball The mode of mill is carried out, and ball milling at least meets following condition：Big ball is 2 with the mass ratio of bead：2-2.6, abrading-ball and material Mass ratio is 10：1.4-1.8, rotating speed is 600-1200rpm, and Ball-milling Time is 25-35min.
Present invention also offers a kind of 3D printing PC-AES materials, 3D printing PC-AES materials are by above-mentioned preparation side Method is prepared.
Hereinafter will be described the present invention by embodiment.
Embodiment 1
1) PC is placed in into 55 DEG C, 5h is soaked in the aqueous hydrochloric acid solution that pH is 5, filter cake is filtered to take, then by filter cake, furfuryl alcohol, Sldium lauryl sulfate, polyether-ether-ketone, methylcellulose, calcium carbonate, flyash, propolis, zirconium oxide, aminopropyl-triethoxy silicon Alkane, chitin are according to 100：38：21：84：14：29：48：20：14：15：30 weight ratio melts 2h to be obtained the at 295 DEG C One fused mass；
2) by AES, pentaerythrite, palm oil, ferrocene, borax, CNT and polyether sulfone according to 100：42：9：5： 20：2：78 weight ratio melts 3h the second fused mass is obtained at 190 DEG C；
3) by the first fused mass and the second fused mass according to 1：0.8 weight ratio 4h, molding, granulating are blended at 240 DEG C with Prepared PC-AES particles；
4) (big ball is 2 with the mass ratio of bead PC-AES particles to be carried out into ball milling：2.3, abrading-ball is with the mass ratio of material 10：1.6, rotating speed is 900rpm, and Ball-milling Time is 30min) with prepared 3D printing PC-AES materials As 1.
Embodiment 2
1) PC is placed in into 50 DEG C, 4h is soaked in the phosphate aqueous solution that pH is 4, filter cake is filtered to take, then by filter cake, furfuryl alcohol, Sldium lauryl sulfate, polyether-ether-ketone, methylcellulose, calcium carbonate, flyash, propolis, zirconium oxide, aminopropyl-triethoxy silicon Alkane, chitin are according to 100：34：14：78：9：23：41：18：9：11：25 weight ratio melts 1h to be obtained first at 290 DEG C Fused mass；
2) by AES, pentaerythrite, palm oil, ferrocene, borax, CNT and polyether sulfone according to 100：38：5：3： 15：1：75 weight ratio melts 2h the second fused mass is obtained at 185 DEG C；
3) by the first fused mass and the second fused mass according to 1：0.7 weight ratio 3h, molding, granulating are blended at 225 DEG C with Prepared PC-AES particles；
4) (big ball is 2 with the mass ratio of bead PC-AES particles to be carried out into ball milling：2, abrading-ball is with the mass ratio of material 10：1.4, rotating speed is 600rpm, and Ball-milling Time is 25min) with prepared 3D printing PC-AES materials As 2.
Embodiment 3
1) PC is placed in into 60 DEG C, 6h is soaked in the aqueous sulfuric acid that pH is 6, filter cake is filtered to take, then by filter cake, furfuryl alcohol, Sldium lauryl sulfate, polyether-ether-ketone, methylcellulose, calcium carbonate, flyash, propolis, zirconium oxide, aminopropyl-triethoxy silicon Alkane, chitin are according to 100：42：31：88：16：34：55：23：17：18：35 weight ratio melts 3h to be obtained the at 305 DEG C One fused mass；
2) by AES, pentaerythrite, palm oil, ferrocene, borax, CNT and polyether sulfone according to 100：45：12：7： 26：3：82 weight ratio melts 4h the second fused mass is obtained at 195 DEG C；
3) by the first fused mass and the second fused mass according to 1：0.9 weight ratio 5h, molding, granulating are blended at 250 DEG C with Prepared PC-AES particles；
4) (big ball is 2 with the mass ratio of bead PC-AES particles to be carried out into ball milling：2.6, abrading-ball is with the mass ratio of material 10：1.8, rotating speed is 1200rpm, and Ball-milling Time is 35min) with prepared 3D printing PC-AES materials As 3.
Comparative example 1
Method according to embodiment 1 carries out that 3D printing material B1 is obtained, except that, step 1) in polyethers ether is not used Ketone.
Comparative example 2
Method according to embodiment 1 carries out that 3D printing material B2 is obtained, except that, step 1) in fine coal is not used Ash.
Comparative example 3
Method according to embodiment 1 carries out that 3D printing material B3 is obtained, except that, step 1) in aminopropyl is not used Triethoxysilane.
Comparative example 4
Method according to embodiment 1 carries out that 3D printing material B4 is obtained, except that, step 1) in oxidation is not used Zirconium.
Comparative example 5
Method according to embodiment 1 carries out that 3D printing material B5 is obtained, except that, step 2) in polyethers is not used Sulfone.
Comparative example 6
Method according to embodiment 1 carries out that 3D printing material B6 is obtained, except that, step 2) in carbon nanometer is not used Pipe.
Comparative example 7
Method according to embodiment 1 carries out that 3D printing material B7 is obtained, except that, step 2) in be not used two luxuriant Iron.
Detection example 1
Intensity, toughness and the heat resistance of above-mentioned 3D printing material are detected, concrete outcome is shown in Table 1.
Table 1
Tensile strength (MPa) Notch impact strength (KJ/cm2) Heat resisting temperature (DEG C)
A1 120 43.0 277
A2 122 41.9 278
A3 125 42.7 274
B1 77 31.2 217
B2 78 29.0 210
B3 70 27.4 242
B4 73 25.5 225
B5 81 26.7 217
B6 72 27.4 236
B7 83 26.2 224
By above-described embodiment, comparative example and detection example, the 3D printing PC-AES materials that the present invention is provided have excellent Different intensity, toughness and heat resistance.
The preferred embodiment of the present invention described in detail above, but, the present invention is not limited in above-mentioned embodiment Detail, the present invention range of the technology design in, various simple variants can be carried out to technical scheme, this A little simple variants belong to protection scope of the present invention.
It is further to note that each particular technique feature described in above-mentioned specific embodiment, in not lance In the case of shield, can be combined by any suitable means, in order to avoid unnecessary repetition, the present invention to it is various can The combination of energy is no longer separately illustrated.
Additionally, can also be combined between a variety of embodiments of the present invention, as long as it is without prejudice to this The thought of invention, it should equally be considered as content disclosed in this invention.

Claims (10)

1. a kind of preparation method of 3D printing PC-AES materials, it is characterised in that include：
1) PC (Merlon) is placed in acid solution and soaks, filters to take filter cake, then by furfuryl alcohol, sldium lauryl sulfate, polyethers ether Ketone, methylcellulose, calcium carbonate, flyash, propolis, zirconium oxide, aminopropyl triethoxysilane, chitin enter with the filter cake Row melting is with prepared first fused mass；
2) by AES (acrylonitrile ethylene styrene copolymer), pentaerythrite, palm oil, ferrocene, borax, CNT with Polyether sulfone is melted that the second fused mass is obtained；
3) first fused mass and the second fused mass are blended, molding, granulating to be to be obtained PC-AES particles；
4) the PC-AES particles are ground that the 3D printing PC-AES materials are obtained.
2. preparation method according to claim 1, wherein, in step 1) in, the immersion at least meets following condition：Leaching Bubble temperature is 50-60 DEG C, and soak time is 4-6h.
3. preparation method according to claim 1, wherein, in step 1) in, the acid solution at least meets following condition：pH For 4-6, one or more in aqueous hydrochloric acid solution, phosphate aqueous solution and aqueous sulfuric acid.
4. preparation method according to claim 1, wherein, in step 1) in, the melting at least meets following condition：It is molten Melt temperature for 290-305 DEG C, the melting time is 1-3h.
5. preparation method according to claim 1, wherein, in step 1) in, relative to the filter cake of 100 weight portions, The consumption of the furfuryl alcohol is 34-42 weight portions, and the consumption of the sldium lauryl sulfate is 14-31 weight portions, the polyether-ether-ketone Consumption be 78-88 weight portions, the consumption of the methylcellulose is 9-16 weight portions, and the consumption of the calcium carbonate is 23-34 Weight portion, the consumption of the flyash is 41-55 weight portions, and the consumption of the propolis is 18-23 weight portions, described zirconic Consumption is 9-17 weight portions, and the consumption of the aminopropyl triethoxysilane is 11-18 weight portions, and the consumption of the chitin is 25-35 weight portions.
6. the preparation method according to any one choosing in claim 1-5, wherein, in step 2) in, the melting is at least full Be enough to lower condition：Melt temperature is 185-195 DEG C, and the melting time is 2-4h.
7. preparation method according to claim 6, wherein, in step 2) in, relative to the AES of 100 weight portions, institute The consumption for stating pentaerythrite is 38-45 weight portions, and the consumption of the palm oil is 5-12 weight portions, and the consumption of the ferrocene is 3-7 weight portions, the consumption of the borax is 15-26 weight portions, and the consumption of the CNT is 1-3 weight portions, the polyethers The consumption of sulfone is 75-82 weight portions.
8. the preparation method according to any one in claim 1-5,7, wherein, in step 3) in, first melting The weight ratio of thing and the second fused mass is 1：0.7-0.9；
Preferably, the blending at least meets following condition：Blending temperature is 225-250 DEG C, and the blending time is 3-5h.
9. preparation method according to claim 8, wherein, in step 4) in, the grinding is carried out by the way of ball milling, And the ball milling at least meets following condition：Big ball is 2 with the mass ratio of bead：2-2.6, abrading-ball is with the mass ratio of material 10：1.4-1.8, rotating speed is 600-1200rpm, and Ball-milling Time is 25-35min.
10. a kind of 3D printing PC-AES materials, it is characterised in that the 3D printing PC-AES materials are by claim 1-9 Preparation method described in any one is prepared.
CN201611060202.0A 2016-11-28 2016-11-28 3D printing PC-AES material and preparation method thereof Pending CN106674952A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107739511A (en) * 2017-09-26 2018-02-27 芜湖天梦信息科技有限公司 A kind of 3D printing material using PSU as matrix

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104830040A (en) * 2015-04-28 2015-08-12 上海锦湖日丽塑料有限公司 Polycarbonate composition for 3D printing technology and preparation method thereof
CN105038089A (en) * 2015-07-14 2015-11-11 暨南大学 Conductive ABS/PC composite material for 3D printing and preparation method for conductive ABS/PC composite material for 3D printing and application of conductive ABS/PC composite material for 3D printing
CN105504759A (en) * 2016-02-03 2016-04-20 黑龙江鑫达企业集团有限公司 ABS composite material used for 3D printing and preparation method of ABS composite material

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104830040A (en) * 2015-04-28 2015-08-12 上海锦湖日丽塑料有限公司 Polycarbonate composition for 3D printing technology and preparation method thereof
CN105038089A (en) * 2015-07-14 2015-11-11 暨南大学 Conductive ABS/PC composite material for 3D printing and preparation method for conductive ABS/PC composite material for 3D printing and application of conductive ABS/PC composite material for 3D printing
CN105504759A (en) * 2016-02-03 2016-04-20 黑龙江鑫达企业集团有限公司 ABS composite material used for 3D printing and preparation method of ABS composite material

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107739511A (en) * 2017-09-26 2018-02-27 芜湖天梦信息科技有限公司 A kind of 3D printing material using PSU as matrix

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