CN107739512A - A kind of material for 3D printing and preparation method thereof - Google Patents
A kind of material for 3D printing and preparation method thereof Download PDFInfo
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- CN107739512A CN107739512A CN201711095426.XA CN201711095426A CN107739512A CN 107739512 A CN107739512 A CN 107739512A CN 201711095426 A CN201711095426 A CN 201711095426A CN 107739512 A CN107739512 A CN 107739512A
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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
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
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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
-
- 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
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
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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
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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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
-
- 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
- C08L2205/08—Polymer mixtures characterised by other features containing additives to improve the compatibility between two polymers
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- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a kind of material for 3D printing, and it includes the silicon rubber of SY 1, c-type silicon rubber and Aided Modification material, wherein the weight percent of each component is：The silicon rubber 75%~100% of SY 1, the Aided Modification material of c-type silicon rubber 0%~25% and 1%~4%, the Aided Modification material mainly include crosslinking agent 5% 22%, compounding ingredient 38% 57%, antioxidant 8% 17%, toughener 4% 7%, hydrolysis-resisting agent 8% 17%, melt fusion reinforcing agent 5% 20%.In addition, the invention further relates to the preparation method of the material.The 3D printing material of the present invention has the characteristics that small toxicity, pollution is small, fidelity is high, mobility is high, toughness is high, shrinkage factor is low, printing precision is high, suitable for fusion sediment 3D printing rapid shaping.
Description
Technical field
The invention belongs to 3D printing technique field, and in particular to a kind of material for 3D printing and preparation method thereof.
Background technology
In recent years, 3D printing method has stepped into application field, in Aero-Space, furniture item, biologic medical, big
The fields such as type equipment have obtained more and more extensive application.Develop 3D printing method, can produce various has specific function
Personalized product, and large batch of personalized customization will be promoted to turn into important production model, lifting product development is horizontal, adds
The development of fast advanced manufacturing industry, has extremely important meaning to optimizing the structure of production.
The core of 3D printing is that it is overturned to conventionally manufactured pattern.Therefore, the process for printing most critical is to establish
Material development process in Fundamental Course of Mechanic Manufacturing.In print procedure, after material melts under driven by program, it is extruded or tiles,
Each lamella is frozen into, recombines material with such method, completes shaping.
The manufacture method of 3D printing refers to based on mathematical model, with a variety of hardness such as metal dust or plastic powders
The larger material of threshold value, on the basis of original 3D printing technique, the hardness gradient material of human body and biology is printed, makes what is printed
Possesses different hardness gradients in same model.Different from conventional cast industry, Method of printing is without designing and manufacturing in advance
Mould, it is not necessary to substantial amounts of material is lost during formed product.In terms of material usage, material has been saved, has improved utilization
Rate, print the tissue such as bone, cartilage, muscle by a certain percentage using multiple material, can be realized in same model different
Hardness gradient.
Point out that 3D printing is mainly by acrylonitrile butadiene styrene copolymer, PLA, Buddhist nun according to a newest report
The metal dust such as the thin polymer films such as dragon and fibrous material, titanium or titanium alloy, duralumin, hard alumin ium alloy, cast magnesium alloy, aluminum oxide, carbon
SiClx ceramic particle etc. forms.The wherein demand of polymeric material is apparently higher than other materials, and with the use of poly-lactic acid material
Amount is maximum, purposes is the most extensive.For printing human body and the organization structural model of animal, metal material poor plasticity, hardness mistake
It is high, it is clear that inapplicable.The material fragilities such as ceramics are big, frangible, are not also suitable for the printing of institutional framework.
At present, it is domestic production, spinning, the paper of film forming and the patent for being largely related to 3D printing material, discomfort to be present
Institutional framework for medical domain prints.Such as：(1) patent of invention " beat by 3D printing material and 3D based on graphene oxide
Print product and their preparation method " refer in (publication number CN106315575A) based on graphene oxide and aniline
Polymeric material, although formability is good, be easy to preserve for a long time, fused glass pellet technology can not be used, and aniline is to people
The toxic effect of body.(2) patent of invention " a kind of composition for 3D printing, the 3D printing material containing it and its preparation side
Thermoplastic resin, the alloyed powder containing rare earth element referred in method, application and 3D printing equipment " (publication number CN105713362A)
Although the advantages that end can be directly used for fused glass pellet, and cost is low, and preparation technology is simple, safe, hard in finished product
Still there is very big difference with the mechanics of biological tissue of medical domain on degree.
At present, in biologic medical field, main research concentrates on the 3D printing of bone, and is used for the material of muscle 3D printing
Rare report.In order to print a complete biological model, the 3D printing of bone, cartilage and muscle is indispensable.
The content of the invention
It is an object of the invention to provide a kind of material for 3D printing and preparation method thereof, it is mainly used in human muscle
The 3D printing of model, the hardness of musculature is simulated, meet the needs of medical 3D printing consumptive material, realize bulk individualization
Production, reduces cost.Concrete technical scheme is as follows.
A kind of material for 3D printing, it includes SY-1 silicon rubber, c-type silicon rubber and Aided Modification material, wherein respectively
The weight percent of individual component is：SY-1 silicon rubber 75%~100%, c-type silicon rubber 0%~25% and 1%~4% aid in
Material modified, the Aided Modification material mainly includes crosslinking agent, compounding ingredient, antioxidant, toughener, hydrolysis-resisting agent, melt
Reinforcing agent is merged, the weight percent of each component of the Aided Modification material is：Crosslinking agent 5%-22%, compounding ingredient
38%-57%, antioxidant 8%-17%, toughener 4%-7%, hydrolysis-resisting agent 8%-17%, melt fusion reinforcing agent 5%-
20%.
Further, the compatilizer be Research of Grafting Malaic Anhydride Onto Polyethylene, styrene-propene it is fine-Glycidyl methacrylate
The mixture of glyceride terpolymer and ethylene butyl acrylate copolymer, it can further improve the toughness of composite.
Further, the antioxidant is tetrapentaerythritol ester, triphosphite ester, 1,3,5- tri- isocyanuric acids, double seasons
The mixture of penta tetrol diphosphites, their mass percent are respectively：Tetrapentaerythritol ester 40%~50%, three phosphorous
Acid esters 10%~20%, the isocyanuric acids 30%~40% of 1,3,5- tri-, bipentaerythrite diphosphites 10%~15%；It is excellent
Selection of land, tetrapentaerythritol ester：Triphosphite ester：The isocyanuric acids of 1,3,5- tri-：Bipentaerythrite diphosphites are 45%：
15%：30%：10%.
Further, the toughener is transparent butylbenzene anti-impact resin, poly butylene succinate, terephthalic acid (TPA) fourth two
The mixture of ester, their mass percent are respectively：Transparent butylbenzene anti-impact resin 40%~60%, poly butylene succinate
15%~25%, butylene terephthalate 30%~35%；Preferably, transparent butylbenzene anti-impact resin：Poly-succinic acid-butanediol
Ester：Butylene terephthalate is 50%：20%：30%.
Further, described hydrolysis-resisting agent is N, N '-two (2,6- diisopropyl phenyl) carbodiimide.
Further, described melt fusion reinforcing agent is rosin resin, terpene resin, one kind in Petropols or more
The mixture of kind.
Based on same inventive concept, the invention further relates to a kind of preparation method of the material for 3D printing, it include with
Lower step：
S1：By weight percent be respectively 75%~100%SY-1 silicon rubber, 0%~25%C types silicon rubber, 1%~
The mixture of 4% Aided Modification material, which is added in mixer, to be carried out mixing 2-4 hours, and the temperature in the mixer is more than
140 DEG C, the weight percent of each component of the Aided Modification material is：Crosslinking agent 2%-10%, compounding ingredient 40%-
60%th, antioxidant 8%-20%, toughener 4%-7%, hydrolysis-resisting agent 8%-20%, melt fusion reinforcing agent 2%-10%；
S2：Obtained mixing material in step S1 is added in screw extruder and carries out melting heat refining, by screw extruder
Squeeze out linear material and be cooled and shaped by tank.
Further, the preparation method of the Aided Modification material described in step S1 comprises the following steps：
S11：Compounding ingredient (55%), antioxidant (15%), hydrolysis-resisting agent (15%) are mixed and are warming up to 100~120 DEG C,
It is preferred that 115 DEG C, 1~2h is reacted in the case where rotating speed is 120~160r/min, it is standby that mixture is made；
S12：After crosslinking agent (5%), solution fusion reinforcing agent (5%) are added into mixture made from step S11, heating
To 140~160 DEG C, under 250~350r/min of rotating speed, preferably 140r/min, 2~4h is reacted, preferably 3.5h, mixing is made
Thing is standby；
S13：After adding toughener (5%) into mixture made from step S12,110~130 DEG C, preferably 125 are warming up to
DEG C, under 350~450r/min of rotating speed, preferably 420r/min, 1~2h is reacted, preferably 1.5h, Aided Modification material is made.
The present invention has small toxicity, pollution is small, fidelity is high, mobility is high, toughness is high, shrinkage factor is low, printing precision is high
The features such as, suitable for fusion sediment 3D printing rapid shaping.
Brief description of the drawings
Fig. 1 is the graph of a relation of C glue addition and Shore A hardness；
Fig. 2 is the schematic diagram of double screw extruder.
In figure：Vacuum exhaust 1, exhaust 2, loading hopper 3, kneading block 4, plus thread element 5.
Embodiment
With reference to the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clear, complete
Ground describes.Referring to Fig. 1-2, present invention use is largely easy to get, SY-1 silicon rubber, c-type silicon rubber and the Aided Modification material of low cost
Expect that Fig. 2 is SY-1 silicon rubber to prepare the 3D printing material for musculature：Aided Modification quality of materials ratio is 7：1 situation
Under, the relation curve of C type silicon rubber dosages and Shore A hardness.Therefore, Shore A hardness muscle between 75-90 need to such as be printed
Tissue, the dosage of c-type silicon rubber is 0%~25%.
The material for 3D printing of the present invention, it includes SY-1 silicon rubber, c-type silicon rubber and Aided Modification material, its
In the weight percent of each component be：SY-1 silicon rubber 75%~100%, c-type silicon rubber 0%~25% and 1%~4%
Aided Modification material, the Aided Modification material mainly include crosslinking agent, compounding ingredient, antioxidant, toughener, hydrolysis-resisting agent,
Melt merges reinforcing agent, and the weight percent of each component of the Aided Modification material is：Crosslinking agent 5%-22%, coordinate
Agent 38%-57%, antioxidant 8%-17%, toughener 4%-7%, hydrolysis-resisting agent 8%-17%, melt fusion reinforcing agent
5%-20%.
In such scheme, the compatilizer be Research of Grafting Malaic Anhydride Onto Polyethylene, styrene-propene it is fine-methacrylic acid contracting
The mixture of water glyceride terpolymer and ethylene butyl acrylate copolymer, it can further improve the toughness of composite.
In such scheme, the antioxidant is tetrapentaerythritol ester, triphosphite ester, 1,3,5- tri- isocyanuric acids, double
The mixture of pentaerythritol diphosphites, their mass percent are respectively：Tetrapentaerythritol ester 40%~50%, Sanya
Phosphate 10%~20%, the isocyanuric acids 30%~40% of 1,3,5- tri-, bipentaerythrite diphosphites 10%~15%；
Preferably, tetrapentaerythritol ester：Triphosphite ester：The isocyanuric acids of 1,3,5- tri-：Bipentaerythrite diphosphites are 45%：
15%：30%：10%.
In such scheme, the toughener is transparent butylbenzene anti-impact resin, poly butylene succinate, terephthalic acid (TPA) fourth
The mixture of diester, their mass percent are respectively：Transparent butylbenzene anti-impact resin 40%~60%, poly-succinic acid-butanediol
Ester 15%~25%, butylene terephthalate 30%~35%；Preferably, transparent butylbenzene anti-impact resin：Poly-succinic fourth two
Alcohol ester：Butylene terephthalate is 50%：20%：30%.
In such scheme, described hydrolysis-resisting agent is N, N '-two (2,6- diisopropyl phenyl) carbodiimide.
In such scheme, described melt fusion reinforcing agent be rosin resin, terpene resin, one kind in Petropols or
A variety of mixtures.
The material preparation method for 3D printing musculature of the present invention mainly includes the following steps that：
S1：By weight percent be respectively 75%~100%SY-1 silicon rubber, 0%~25%C types silicon rubber, 1%~
The mixture of 4% Aided Modification material, which is added in mixer, to be carried out mixing 2-4 hours, and the temperature in the mixer is more than
140 DEG C, SY-1 silicon rubber is preferably 75%, and c-type silicon rubber is preferably that 22%, Aided Modification material is preferably 3%, the auxiliary
The weight percent of material modified each component is：Crosslinking agent 2%-10%, compounding ingredient 40%-60%, antioxidant
8%-20%, toughener 4%-7%, hydrolysis-resisting agent 8%-20%, melt fusion reinforcing agent 2%-10%；
S2：Obtained mixing material in step S1 is added in screw extruder and carries out melting heat refining, by screw extruder
Squeeze out linear material and be cooled and shaped by tank.
Further, the preparation method of the Aided Modification material described in step S1 comprises the following steps：
S11：Compounding ingredient (55%), antioxidant (15%), hydrolysis-resisting agent (15%) are mixed and are warming up to 100~120 DEG C,
It is preferred that 115 DEG C, 1~2h is reacted in the case where rotating speed is 120~160r/min, it is standby that mixture is made；
S12：After crosslinking agent (5%), solution fusion reinforcing agent (5%) are added into mixture made from step S11, heating
To 140~160 DEG C, under 250~350r/min of rotating speed, preferably 140r/min, 2~4h is reacted, preferably 3.5h, mixing is made
Thing is standby；
S13：After adding toughener (5%) into mixture made from step S12,110~130 DEG C, preferably 125 are warming up to
DEG C, under 350~450r/min of rotating speed, preferably 420r/min, 1~2h is reacted, preferably 1.5h, Aided Modification material is made.
The screw extruder can be peg type single screw extrusion machine, double screw extruder or reciprocating Single screw extrusion
Machine, and preferably double screw extruder.Fig. 2 shows a kind of preferable double screw extruder, including：Vacuum exhaust 1, exhaust 2,
Loading hopper 3, kneading block 4, plus thread element 5.Between the screw slenderness ratio of the double screw extruder is 32~40, preferably
40, screw combinations are moderate shear rate combinations mode, and extrusion temperature is between 140~190 DEG C, preferably 160 DEG C.
Finally it should be noted that：The above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations；Although
The present invention is described in detail with reference to the foregoing embodiments, it will be understood by those within the art that：It still may be used
To be modified to the technical scheme described in foregoing embodiments, or equivalent substitution is carried out to which part technical characteristic；
And these modification or replace, do not make appropriate technical solution essence depart from various embodiments of the present invention technical scheme spirit and
Scope.
Claims (8)
1. a kind of material for 3D printing, it includes SY-1 silicon rubber, c-type silicon rubber and Aided Modification material, wherein each
The weight percent of component is：SY-1 silicon rubber 75%~100%, the auxiliary of c-type silicon rubber 0%~25% and 1%~4% change
Property material, the Aided Modification material mainly includes crosslinking agent, compounding ingredient, antioxidant, toughener, hydrolysis-resisting agent, melt melt
Reinforcing agent is closed, the weight percent of each component of the Aided Modification material is：Crosslinking agent 5%-22%, compounding ingredient
38%-57%, antioxidant 8%-17%, toughener 4%-7%, hydrolysis-resisting agent 8%-17%, melt fusion reinforcing agent 5%-
20%.
2. a kind of material for 3D printing according to claim 1, it is characterised in that the compatilizer connects for polyethylene
Branch maleic anhydride, styrene-propene be fine-GMA terpolymer and ethylene butyl acrylate copolymer
Mixture, can further improve the toughness of composite.
3. a kind of material for 3D printing according to claim 1, it is characterised in that the antioxidant is the four seasons penta
Four alcohol esters, triphosphite ester, 1,3,5- tri- isocyanuric acids, the mixture of bipentaerythrite diphosphites, their quality hundred
Fraction is respectively：Tetrapentaerythritol ester 40%~50%, triphosphite ester 10%~20%, the isocyanuric acids 30% of 1,3,5- tri-~
40%th, bipentaerythrite diphosphites 10%~15%；Preferably, tetrapentaerythritol ester：Triphosphite ester：1,3,5- tri- is different
Cyanuric acid：Bipentaerythrite diphosphites are 45%：15%：30%：10%.
4. a kind of material for 3D printing according to claim 1, it is characterised in that the toughener is transparent butylbenzene
Anti-impact resin, poly butylene succinate, the mixture of butylene terephthalate, their mass percent are respectively：Thoroughly
Bright butylbenzene anti-impact resin 40%~60%, poly butylene succinate 15%~25%, butylene terephthalate 30%~
35%；Preferably, transparent butylbenzene anti-impact resin：Poly butylene succinate：Butylene terephthalate is 50%：20%：
30%.
A kind of 5. material for 3D printing according to claim 1, it is characterised in that described hydrolysis-resisting agent is N,
N '-two (2,6- diisopropyl phenyls) carbodiimide.
A kind of 6. material for 3D printing according to claim 1, it is characterised in that described melt fusion reinforcing agent
For one or more mixtures in rosin resin, terpene resin, Petropols.
7. a kind of preparation method of material for 3D printing, it comprises the following steps：
S1：It is respectively 75%~100%SY-1 silicon rubber, 0%~25%C types silicon rubber, 1%~4% by weight percent
The mixture of Aided Modification material, which is added in mixer, to be carried out mixing 2-4 hours, and the temperature in the mixer is more than 140
DEG C, the weight percent of each component of the Aided Modification material is：Crosslinking agent 2%-10%, compounding ingredient 40%-60%,
Antioxidant 8%-20%, toughener 4%-7%, hydrolysis-resisting agent 8%-20%, melt fusion reinforcing agent 2%-10%；
S2：Obtained mixing material in step S1 is added in screw extruder and carries out melting heat refining, is extruded by screw extruder
Cutting edge aligned material is simultaneously cooled and shaped by tank.
A kind of 8. preparation method of material for 3D printing according to claim 7, it is characterised in that institute in step S1
The preparation method for the Aided Modification material stated comprises the following steps：
S11：Compounding ingredient (55%), antioxidant (15%), hydrolysis-resisting agent (15%) are mixed and are warming up to 100~120 DEG C, preferably
115 DEG C, 1~2h is reacted in the case where rotating speed is 120~160r/min, it is standby that mixture is made；
S12：After crosslinking agent (5%), solution fusion reinforcing agent (5%) are added into mixture made from step S11, it is warming up to
140~160 DEG C, under 250~350r/min of rotating speed, preferably 140r/min, 2~4h is reacted, preferably 3.5h, it is standby that mixture is made
With；
S13：After adding toughener (5%) into mixture made from step S12,110~130 DEG C, preferably 125 DEG C are warming up to,
Under 350~450r/min of rotating speed, preferably 420r/min, 1~2h is reacted, preferably 1.5h, Aided Modification material is made.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112004656A (en) * | 2018-03-26 | 2020-11-27 | 昕诺飞控股有限公司 | Cross-linked polymer-filled polymer particles for 3D printed articles |
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| CN104559088A (en) * | 2015-01-28 | 2015-04-29 | 上海材料研究所 | Modified composite material suitable for 3D printing and preparation method thereof |
| CN105599311A (en) * | 2016-01-28 | 2016-05-25 | 中国工程物理研究院化工材料研究所 | Method for preparing silicon rubber porous material based on additive manufacturing technology |
| CN107286609A (en) * | 2017-06-20 | 2017-10-24 | 广东波斯科技股份有限公司 | A kind of low-density thermal conductivity PLA 3D printing material and its preparation method and application |
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| US20120059100A1 (en) * | 2010-09-07 | 2012-03-08 | Xiamen Runner Industrial Corporatio | Imitation metal engineering plastic composite material and preparation method of the same |
| CN104559088A (en) * | 2015-01-28 | 2015-04-29 | 上海材料研究所 | Modified composite material suitable for 3D printing and preparation method thereof |
| CN105599311A (en) * | 2016-01-28 | 2016-05-25 | 中国工程物理研究院化工材料研究所 | Method for preparing silicon rubber porous material based on additive manufacturing technology |
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| CN112004656A (en) * | 2018-03-26 | 2020-11-27 | 昕诺飞控股有限公司 | Cross-linked polymer-filled polymer particles for 3D printed articles |
| US11724444B2 (en) | 2018-03-26 | 2023-08-15 | Signify Holding B.V. | Cross-linked polymer filled polymer for 3D printed items |
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Application publication date: 20180227 |