CN107915997A - A kind of silicon rubber composite material for SLS and its preparation method and application - Google Patents
A kind of silicon rubber composite material for SLS and its preparation method and application Download PDFInfo
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- CN107915997A CN107915997A CN201711262027.8A CN201711262027A CN107915997A CN 107915997 A CN107915997 A CN 107915997A CN 201711262027 A CN201711262027 A CN 201711262027A CN 107915997 A CN107915997 A CN 107915997A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y70/00—Materials specially adapted for additive manufacturing
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K3/04—Carbon
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- 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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08K7/06—Elements
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/0831—Gold
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08K2201/001—Conductive additives
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K2201/011—Nanostructured additives
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Abstract
The present invention relates to processing of high molecular material technical field, and in particular to a kind of silicon rubber composite material for SLS and its preparation method and application, including following raw material is in parts by weight：100 parts of silicon rubber, 0.1~10 part of conductive filler, 0.1~0.2 part of light stabilizer, 0.1~0.3 part of antioxidant, 0.1~0.5 part of flow ability modifying agent；Its preparation method is prepared into powder for raw material is uniformly mixed, and obtains silicon rubber composite material, and the average grain diameter of its dusty material is 10~150 μm.The preparation process of the present invention is simple, it is of low cost, silicon rubber composite material powder printing product, which is made, has good dimensional accuracy, and there is excellent electric conductivity and electromagnetic performance, flexible electrode and wearable electronic etc. are can be applied to, basis material is silicon rubber, it is with good flexibility, it is only capable of obtaining rigid articles for the material such as nylon used in current SLS, it has widened the application range of SLS technologies significantly.
Description
Technical field
The present invention relates to processing of high molecular material technical field, and in particular to a kind of silicon rubber composite material for SLS
And its preparation method and application.
Background technology
Selective laser sintering (Selective Laser Sintering), it be with Computerized three-dimensional design a model for
Source, one kind of product is obtained with metal dust, ceramic powders, polymer powder materials by successively printing, being superimposed shaping
New material molding technology.Have the advantages that high without supporting structure, printing product intensity.
Selective laser sintering technique is the 3D printing technique being most widely used, its basic thought is by Texas ,Usa
The C.R.Dechard of university's Austin was proposed in 1986, and successfully developed selective laser sintering work in 1989
Skill.The technique is with fastest developing speed, the most successful and commercialized 3D printing method, can not only be produced using the technology
Accurate model and original shape, the metal parts that can also be formed with reliable structure are used as direct functor.Selectivity swashs
Light sintering technology has many advantages, such as, as powder selection is extensive, applicability is wide, manufacturing process is fairly simple, forming accuracy is high, nothing
Need supporting structure, can direct sintering part, therefore be subject to more and more extensive attention in modern manufacturing industry.
However, the greatest problem of selective laser sintering technique is extremely limited for the polymeric material of sintering, and
Price is relatively expensive, therefore develops new polymeric material and be suitable for selective laser sintering and be extremely necessary.Market
On can be used for that laser sintered polymeric material is seldom, and the most widely used for nylon material, including nylon 12, nylon at present
11st, nylon 6 etc., accounts for more than 95%, and other can be used for laser sintered polymeric material such as makrolon, polystyrene, gather
The application such as ether ether ketone is less.The performance and traditional processing for the product that these materials are obtained by selective laser sintering technique at the same time
Technique, such as injection, extrusion compare also larger gap with the performance for casting obtained product, and cost is much higher,
So the 3D printing technique based on selective laser sintering technique also and is not used for the industrialized production of product.
In addition, using the polymeric material based on Nylon-12, obtain is rigid articles through laser sintered at present, its is hard
Degree is big, flexible poor.So if a kind of new flexible material that can be used for SLS processing and formings can be developed, will widen significantly
The application range of 3D printing technique based on laser sintered.
The content of the invention
It is an object of the invention to overcome the deficiencies of the prior art and provide a kind of silicon rubber composite material for SLS and
Its preparation method and application, its main feature is that the silicon rubber composite material can be used for SLS 3D printings, printing product has good
Electric conductivity and electromagnetic performance, silicon rubber have good pliability, it is used successfully to the application that 3D printing has been widened in 3D printing
Scope.
The purpose of the present invention is what is be achieved through the following technical solutions：
A kind of silicon rubber composite material for SLS, including following raw material is in parts by weight：
Further, the conductive filler is single-walled carbon nanotube, multi-walled carbon nanotube, graphene, carbon black, gold nano
Any of line, nano silver wire, copper nano-wire.
Further, the light stabilizer for 2,4- benzophenonedicarboxylic acids, 5- chlorinations benzotriazole, 2- hydroxyls -4- just
It is octyloxybenzophenone, ESCALOL 567 or 2- (the 2 ˊ-ˊ of hydroxyl-5-aminomethyl phenyl) benzotriazole, double
(1,2,2,6,6- pentamethyl -4- piperidyls) sebacate, bis(2,2,6,6-tetramethyl-4-piperidyl)sebacate,
Any of (a, a- 3,5-dimethylphenyl) benzotriazole.
Further, the antioxidant is 2,6- three-level butyl -4- methylphenols, four [β-(3,5- di-t-butyl -4- hydroxyls
Base phenyl) propionic acid] pentaerythritol ester, N, N'- be double-(3- (3,5- di-tert-butyl-hydroxy phenyls) propiono) hexamethylene diamine, three
[2,4- di-tert-butyl-phenyl] phosphite ester, double (3,5- three-level butyl -4- hydroxy phenyls) thioethers and β-(3,5- di-t-butyls -
At least one of 4- hydroxy phenyls) the positive octadecanol ester of propionic acid.
Further, the flow ability modifying agent is diallyl bisphenol, phthalic acid two (2- ethyl hexyls) ester, diethyl
Bisbenzoate, dipropylene glycol dibenzoate, propylene glycol dibenzoate, 2,2,4- trimethyl -1,3- pentanediols are double
Any of isobutyrate, sebum dioctyl phthalate.
A kind of preparation method of silicon rubber composite material as described for SLS, comprises the following steps：By silicon rubber, nothing
Machine filler, light stabilizer, antioxidant and flow ability modifying agent agent are uniformly mixed, and are prepared into powder, obtain silicon rubber composite material,
The average grain diameter of its dusty material is 10~150 μm.
Further, the powder is by mechanical milling method, Freezing smashing method, solvent precipitation or spray drying process
Any method be prepared.
Further, the mechanical milling method is to add the raw material into mechanical grinding device ball mill, the crushing of mill structure
In machine, raw material is carried out with 1000~50000 revs/min of rotating speed with 10~500 revs/min of rotating speed, or homogenizer
Crush, it is compound after obtain silicon rubber composite powder material；The Freezing smashing method is freezing will to be added to after raw material melting mixing
In pulverizer, at a temperature of -196~0 DEG C, under 1000~20000 revs/min of rotating speed obtaining silicon rubber after Freezing smashing answers
Close dusty material；The spray drying process is after raw material is mixed progress, to be added in spray drying device, at 150~350 DEG C
Inlet air temperature, lotion is sprayed to obtain silicon rubber composite powder material under 1~20MPa high pressures；The solvent precipitation be by
Silicon rubber is dissolved in organic good solvent and adds inorganic filler powder, is carried out under 80~200 DEG C, the high pressure of 0.5~10MPa
Solvent deposition obtains silicon rubber composite powder material.
Further, organic good solvent is n,N-Dimethylformamide, Isosorbide-5-Nitrae-dioxane, four in the solvent precipitation
Any of hydrogen furans.
A kind of application of silicon rubber composite material as described for SLS, prints as consumptive material for SLS.
The beneficial effects of the invention are as follows：
1st, silicon rubber composite granule is used for SLS 3D printings, and successful print goes out the product of excellent performance；
2nd, the introducing of the conductive filler such as carbon nanotubes improves the laser sintered performance of silicon rubber, and imparts printing product
Good conduction and electromagnetic performance, can be applied to prepare flexible electromagnetism and wearable electronic；
3rd, basis material is silicon rubber, it is with good flexibility, for the material such as nylon used in current 3D printing
It is only capable of obtaining rigid articles, it has widened the application range of 3D printing technique significantly.
Brief description of the drawings
Fig. 1 obtains 150 times of electron-microscope scanning figures of silicon rubber composite material for the embodiment of the present invention 4；
Fig. 2 obtains 40000 times of electron-microscope scanning figures of silicon rubber composite material for the embodiment of the present invention 4；
Fig. 3 obtains the electric conductivity detection figure of silicon rubber composite material for the embodiment of the present invention 4；
Fig. 4 obtains the capability of electromagnetic shielding detection figure of silicon rubber composite material for the embodiment of the present invention 4.
Embodiment
Technical scheme, but the protection of the present invention are described in further detail with reference to specific embodiments and the drawings
Scope is not limited to as described below.
Embodiment 1
By 100 parts of silicon rubber, 0.1 part of single-walled carbon nanotube, 0.1 part of 2,4-DihydroxyBenzophenone, 0.1 part of 2,6- three-level
Butyl -4- methylphenols, mechanical grinding device is added to after 0.1 part of diallyl bisphenol melting mixing includes ball mill, mill
The silicon rubber composite material powder that average grain diameter is 10 μm is obtained in structure pulverizer etc., after crushing.
Embodiment 2
By 100 parts of silicon rubber, 2 parts of multi-walled carbon nanotubes, 0.2 part of 2,4-DihydroxyBenzophenone, 0.2 part of four [β-(3,5-
Di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester, after 0.2 part of phthalic acid two (2- ethyl hexyls) ester melting mixing plus
Enter into freezing crusher, the silicon rubber composite material powder that average grain diameter is 40 μm is obtained after Freezing smashing.
Embodiment 3
100 parts of silicon rubber are prepared into silicon rubber lotion, by 3 parts of carbon blacks, 0.2 part of 5- chlorination benzotriazole, 0.3 part of N,
N'- pairs-(3- (3,5- di-tert-butyl-hydroxy phenyls) propiono) hexamethylene diamine, 0.3 part of diethylene glycol dibenzoate powder adds
Enter among lotion, lotion is added in spray drying device, under high pressure spray solution, with hot air, remove
Solvent obtains the silicon rubber composite material powder that average grain diameter is 70 μm.
Embodiment 4
100 parts of silicon rubber are dissolved in after good solvent and add 4 parts of nano silver wires, 0.2 part of 5- chlorination benzotriazole, 0.3 part
Three [2,4- di-tert-butyl-phenyl] phosphite esters, 0.4 part of dipropylene glycol dibenzoate powder are then bad molten with silicon rubber
Agent mixing, precipitation, obtain the silicon rubber composite material powder that average grain diameter is 100 μm, to obtained silicon rubber by filtration drying
Glue composite material carries out electron-microscope scanning, as a result as depicted in figs. 1 and 2.
Embodiment 5
5 parts of copper nano-wires, 0.2 part of 2- hydroxyl -4- n-octyloxy hexichol are added after 100 parts of silicon rubber are dissolved in good solvent
Ketone, 0.3 part of double (3,5- three-level butyl -4- hydroxy phenyls) thioether, 0.5 part of propylene glycol dibenzoate, then with silicon rubber
Poor solvent mixing, precipitation, it is 60 μm of silicon rubber composite material powder to obtain average grain diameter by filtration drying.
Embodiment 6
100 parts of silicon rubber are prepared into silicon rubber lotion, by 9 parts of gold, 0.2 part of 2- (the 2 ˊ-ˊ of hydroxyl-5-aminomethyl phenyl) benzene
And triazole, 0.3 part, N'- pairs-(3- (3,5- di-tert-butyl-hydroxy phenyl) propiono) hexamethylene diamine, 0.5 part 2,2,4- tri-
Methyl isophthalic acid, the double isobutyrate powder of 3- pentanediols are added among lotion, lotion are added in spray drying device, in high pressure
It is lower to spray solution, with hot air, remove solvent and obtain the silicon rubber composite material powder that average grain diameter is 90 μm.
Embodiment 7
By 100 parts of silicon rubber, 10 parts of graphenes, 0.2 part of 2- (the 2 ˊ-ˊ of hydroxyl-5-aminomethyl phenyl) benzotriazole, 0.3 part
Four or three [2,4- di-tert-butyl-phenyl] phosphite esters, are added to mechanical lapping after 0.5 part of propylene glycol dibenzoate melting mixing
Equipment is included in ball mill, mill structure pulverizer etc., and the silicon rubber composite material powder that average grain diameter is 20 μm is obtained after crushing
End.
Embodiment 8
By 100 parts of silicon rubber, 2 parts of calcium carbonate, 0.2 part of 5- chlorination benzotriazole, 0.2 part of N, N'- be double-(3- (3,5- bis- uncles
Butyl -4- hydroxy phenyls) propiono) hexamethylene diamine, it is added in freezing crusher after 0.5 part of sebum dioctyl phthalate melting mixing,
The silicon rubber composite material powder that average grain diameter is 50 μm is obtained after Freezing smashing.
Application example 1
Silicon rubber composite material powder made from embodiment 4 is layered on the workbench of 3D printer, sets laser power
For 60w, it is 60 DEG C to build cylinder temperature, and powdering thickness is 0.1mm；
Under control of a computer program, the thickness vertically set according to three-dimensional CAD model file carries out laser
The cross-section data of hierarchy slicing, is selectively scanned the compound polyurethane material powder, sinters；
It is heated by the compound polyurethane material powder in the inswept region of laser, material is melted and bonded, one layer of burning
After the completion of knot, working cylinder declines the height of setting, then carries out next layer of powdering and sintering, and is bonded with preceding layer, so anti-
Multiple machine-shaping；Final take out carries out clear powder, polishes to be that can obtain printing product；Printing product is subjected to electric conductivity inspection respectively
Survey and capability of electromagnetic shielding detects, testing result difference is as shown in Figure 3 and Figure 4.
According to above application implementation, the silicon rubber composite material for respectively obtaining embodiment 1~4 carries out equal conditions
Implement operation, and the printing product respectively obtained is subjected to mechanics properties testing, testing result is as shown in table 1.
1 embodiment of table, 1~4 silicon rubber composite material prints the mechanical property table of product
| Project | Tensile strength/MPa | Elongation at break % |
| Embodiment 1 | 2.12 | 236.58 |
| Embodiment 2 | 2.28 | 254.42 |
| Embodiment 3 | 2.34 | 272.31 |
| Embodiment 4 | 2.41 | 283.21 |
The result shows that：Had by the product obtained after the laser sintered processing of the chosen property of silicon rubber composite material of the present invention
Excellent mechanical property；With the increase of inorganic filler content in component, the tensile strength of product increases therewith, elongation at break
Reduce therewith.
The above is only the preferred embodiment of the present invention, it should be understood that the present invention is not limited to described herein
Form, is not to be taken as the exclusion to other embodiment, and can be used for various other combinations, modification and environment, and can be at this
In the text contemplated scope, it is modified by the technology or knowledge of above-mentioned teaching or association area.And those skilled in the art institute into
Capable modifications and changes do not depart from the spirit and scope of the present invention, then all should be in the protection domain of appended claims of the present invention
It is interior.
Claims (10)
1. a kind of silicon rubber composite material for SLS, it is characterised in that including following raw material in parts by weight：
A kind of 2. silicon rubber composite material for SLS according to claim 1, it is characterised in that the conductive filler
For any of single-walled carbon nanotube, multi-walled carbon nanotube, graphene, carbon black, nanowires of gold, nano silver wire, copper nano-wire.
A kind of 3. silicon rubber composite material for SLS according to claim 1, it is characterised in that the light stabilizer
For 2,4- benzophenonedicarboxylic acids, 5- chlorinations benzotriazole, 2-hydroxy-4-n-octoxybenzophenone, 2- hydroxyl -4- methoxyl groups
Benzophenone or 2- (the 2 ˊ-ˊ of hydroxyl-5-aminomethyl phenyl) benzotriazole, double (1,2,2,6,6- pentamethyl-4- piperidyls) last of the ten Heavenly stems two
Any in acid esters, bis(2,2,6,6-tetramethyl-4-piperidyl)sebacate, (a, a- 3,5-dimethylphenyl) benzotriazole
Kind.
4. a kind of silicon rubber composite material for SLS according to claim 1, it is characterised in that the antioxidant is
2,6- three-level butyl -4- methylphenols, four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol esters, N, N'-
It is double-(3- (3,5- di-tert-butyl-hydroxy phenyls) propiono) hexamethylene diamine, three [2,4- di-tert-butyl-phenyls] phosphite esters, double
In (3,5- three-level butyl -4- hydroxy phenyls) thioether and β-positive octadecanol ester of (3,5- di-tert-butyl-hydroxy phenyl) propionic acid
At least one.
A kind of 5. silicon rubber composite material for SLS according to claim 1, it is characterised in that the flow modifier
Agent is diallyl bisphenol, phthalic acid two (2- ethyl hexyls) ester, diethylene glycol dibenzoate, dipropylene glycol hexichol first
Any in acid esters, propylene glycol dibenzoate, 2,2,4- trimethyl -1,3- pentanediols double isobutyrate, sebum dioctyl phthalates
Kind.
6. a kind of preparation method for the silicon rubber composite material for being used for SLS as described in Claims 1 to 5 any one, its feature
It is, comprises the following steps：Silicon rubber, inorganic filler, light stabilizer, antioxidant and flow ability modifying agent agent are uniformly mixed, and
Powder is prepared into, obtains silicon rubber composite material, the average grain diameter of its dusty material is 10~150 μm.
A kind of 7. preparation method of silicon rubber composite material for SLS according to claim 6, it is characterised in that institute
It is by any of mechanical milling method, Freezing smashing method, solvent precipitation or spray drying process method system to state powder
It is standby to obtain.
A kind of 8. silicon rubber composite material for SLS according to claim 7, it is characterised in that the mechanical lapping
Method is added the raw material into mechanical grinding device ball mill, mill structure pulverizer, with 10~500 revs/min of rotating speed, or
Homogenizer crushes raw material with 1000~50000 revs/min of rotating speed, it is compound after obtain silicon rubber composite powder material
Material；The Freezing smashing method is will to be added to after raw material melting mixing in freezing crusher, at a temperature of -196~0 DEG C,
Silicon rubber composite powder material is obtained under 1000~20000 revs/min of rotating speed after Freezing smashing；The spray drying process be by
After raw material mixing carries out, it is added in spray drying device, by breast under the inlet air temperature, 1~20MPa high pressures at 150~350 DEG C
Liquid sprays to obtain silicon rubber composite powder material；The solvent precipitation is that silicon rubber is dissolved in organic good solvent and is added
Inorganic filler powder, progress solvent deposition obtains silicon rubber composite powder material under 80~200 DEG C, the high pressure of 0.5~10MPa
Material.
A kind of 9. silicon rubber composite material for SLS according to claim 8, it is characterised in that the solvent deposition
Organic good solvent is any of N,N-dimethylformamide, 1,4- dioxane, tetrahydrofuran in method.
10. a kind of application for the silicon rubber composite material for being used for SLS as described in Claims 1 to 5 any one, its feature exist
In as consumptive material for SLS printings.
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| CN105238007A (en) * | 2015-09-25 | 2016-01-13 | 四川大学 | Flexible polymer conductor, and preparation method and applications thereof |
| CN106751908A (en) * | 2017-01-09 | 2017-05-31 | 北京工业大学 | A kind of 3D printing flexible conductive composite material and preparation method thereof |
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2017
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104910609A (en) * | 2015-06-03 | 2015-09-16 | 四川大学 | Polyurethane composite material for 3D printing, and preparation method and application thereof |
| CN105111470A (en) * | 2015-08-13 | 2015-12-02 | 四川大学 | Reversible covalent crosslinking polysiloxane elastomer, preparation method therefor and application thereof |
| CN105238007A (en) * | 2015-09-25 | 2016-01-13 | 四川大学 | Flexible polymer conductor, and preparation method and applications thereof |
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