CN107236295A - A kind of selective laser sintering polyamide 610 dusty material and preparation method - Google Patents
A kind of selective laser sintering polyamide 610 dusty material and preparation method Download PDFInfo
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- CN107236295A CN107236295A CN201710359095.XA CN201710359095A CN107236295A CN 107236295 A CN107236295 A CN 107236295A CN 201710359095 A CN201710359095 A CN 201710359095A CN 107236295 A CN107236295 A CN 107236295A
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
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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
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/12—Powdering or granulating
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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
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/13—Phenols; Phenolates
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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
- C08K5/00—Use of organic ingredients
- C08K5/49—Phosphorus-containing compounds
- C08K5/51—Phosphorus bound to oxygen
- C08K5/53—Phosphorus bound to oxygen bound to oxygen and to carbon only
- C08K5/5393—Phosphonous compounds, e.g. R—P(OR')2
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- C08J2377/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
- C08J2377/06—Polyamides derived from polyamines and polycarboxylic acids
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Abstract
A kind of selective laser sintering polyamide 610 dusty material that the present invention is provided and preparation method thereof; polyamide 610 resin and solvent are blended in by 1: 4~20 mass ratio in closed reactor; vacuumize, nitrogen charging gas shielded; material reaction maximum temperature is heated to 140~180 DEG C under continuous agitation; soaking time is 1~300min; then the material reaction maximum temperature is brought down below 5~10 DEG C of material Precipitation Temperature; required temperature fall time is 60~180min, then obtains PA610 powder through centrifugation, dry and screening；By following components by percentage to the quality：PA610 powder 96~99.98%, powder flow aid 0.01~2.0%, the mixing of powder antioxidant 0.01~2.0%, sieving obtain average grain diameter and are applied to selective laser sintering polyamide 610 dusty material for 30~120 μm.Uniform and concentrate by the made polyamide 610 dusty material particle diameter distribution obtained of the present invention, particle sphericity is high, and its preparation technology is simple, with low cost, is especially suitable for SLS moulding process.
Description
Technical field
The present invention relates to a kind of polyamide 610 dusty material and preparation method, and in particular to a kind of selective laser sintering
With polyamide 610 dusty material and preparation method.
Background technology
Selective laser sintering (Selective Laser Sintering, abbreviation SLS) is many by optionally fusing
Individual powder bed manufactures a kind of method of three-dimensional body, and this method allows only need to be according to object to be produced without using tool processes
3-D view by multiple overlapping layers of laser sintering powder, to obtain 3D solid.This method mainly uses thermoplastic poly
Compound is completed, and patent US61013610948 and WO96100610881 manufactures three-dimensional body to this use polymer powder
Method be described in detail.
Current selective laser technology, mainly using polyamide 11 and polyamide 12 as main raw material, is further
Extended Technology application extends, and is one of direction for studying at present using polyamide 610 material as raw material.At present
PA610 powder prepares and mainly uses cryogenic freezing disintegrating process, and its principle is that polymer and low-temperature receiver are carried out into heat exchange, makes material
Brittle state is cooled to, the shock that the material after embrittlement is carried out many times in crushing chamber by disintegrating mechanism finally turns into tiny
Graininess.The powder particle shape prepared using the technique is irregular, flow of powder sexual deviation；Its powder diameter is distributed
Width, and suitable for selective laser sintering the preferable particle size range of powder particle at 30~120 microns, after screening process yield drop
It is low, material is caused to waste.
The content of the invention
The above-mentioned technical problem existed for prior art, it is an object of the invention to provide a kind of particle diameter distribution is uniform and collection
In, selective laser sintering polyamide 610 dusty material and the system that particle sphericity is high, preparation technology is simple, with low cost
Preparation Method.
In order to solve the above technical problems, the invention provides a kind of selective laser sintering polyamide 610 dusty material,
Include following components by percentage to the quality：PA610 powder 96~99.98%, powder flow aid 0.01~2.0%, powder
Antioxidant 0.01~2.0%.Current selective laser technology is mainly used as main former material using polyamide 11 and polyamide 12
Material, is further Extended Technology application extension, is the side studied at present using polyamide 610 dusty material as raw material
One of to.PA610 is to contain substantial amounts of amide group in the thermoplastic engineering plastic of a class excellent performance, its macromolecular structure,
Macromolecular end is amino or carboxyl, is a kind of highly polar, can form hydrogen bond and the hemicrystalline with certain reactivity gathers
Compound.PA610 material relative densities are smaller, and water imbibition is less than short chain nylon, and good stability of the dimension, processing and forming is easy.Machinery
Intensity is high, is resistant to highly basic, weak acid.PA 610 is widely used in machine-building, automobile, tractor and makees gear, bearing, pad, close
Closure material, oil vessel, petroleum pipeline, textile machinery part, rope, bristlelike monofilament, smee cell shell etc..Powder flow aid contributes to
Improve the mobility of selective laser sintering polyamide 610 dusty material, it is ensured that the stability that powder paving is sent in sintering process,
So as to improve sintering finished rate, antioxidant is then favorably improved the inoxidizability of powder.Powder antioxidant is used to prevent selection
Property is laser sintered to lose intensity and toughness with polyamide 610 dusty material because of oxidative degradation.
As present invention further optimization scheme, the powder flow aid is nano-calcium carbonate, nanomete talc powder, received
One or more in off-white carbon black, nano zine oxide, nanometer magnesium stearate and nano magnesia.
As present invention further optimization scheme, the powder antioxidant includes：Mass fraction for 40%-90% by
It is 10%~60% phosphite kind antioxidant to hinder phenolic antioxidant and mass fraction, and wherein Hinered phenols antioxidant is 1,3,
5- trimethyls -2,4,6- tri- (3,5- di-tert-butyl-4-hydroxyl benzyl) benzene, 2,6- di-t-butyl -4- methyl-phenols, N, N '-two
One or more in (3,5- di-tert-butyl-hydroxy phenyl propionamide), phosphite kind antioxidant is 2,2 '-ethylenebis
In (4,6- di-tert-butyl-phenyl) fluorophosphite, four (2,4- di-tert-butyl-phenyls) -4,4 '-xenyl bis-phosphite
It is one or more of.
Present invention also offers a kind of preparation method of selective laser sintering with polyamide 610 dusty material, including such as
Lower step：
(1) polyamide 610 resin and solvent are blended in by 1: 4~20 mass ratio in closed reactor, vacuumize,
Nitrogen charging gas shielded, is heated to 140~180 DEG C by material reaction maximum temperature under continuous agitation, and soaking time is 1~
300min, is then brought down below 5~10 DEG C of material Precipitation Temperature by the material reaction maximum temperature, and required temperature fall time is
60~180min, then obtain PA610 powder through centrifugation, dry and screening；
(2) by following components by percentage to the quality：PA610 powder 96~99.98%, powder flow aid 0.01~
2.0%, the mixing of powder antioxidant 0.01~2.0%, sieving obtain average grain diameter and are applied to selective laser burning for 30~120 μm
Knot uses polyamide 610 dusty material.
As present invention further optimization scheme, the solvent is made up of first alcohol and water, and the methanol accounts for the total matter of solvent
The 60%~95% of amount.
As present invention further optimization scheme, the mass ratio of the polyamide 610 resin and solvent is 1: 6~8.
As present invention further optimization scheme, the material reaction maximum temperature is 150~155 DEG C, soaking time
For 30~120min.
As present invention further optimization scheme, the temperature fall time is：80~120min.
As present invention further optimization scheme, the powder flow aid is nano-calcium carbonate, nanomete talc powder, received
One or more in off-white carbon black, nano zine oxide, nanometer magnesium stearate, nano magnesia.
As present invention further optimization scheme, the powder antioxidant includes：Mass fraction for 40%-90% by
It is 10%~60% phosphite kind antioxidant to hinder phenolic antioxidant and mass fraction, and wherein Hinered phenols antioxidant is 1,3,
5- trimethyls -2,4,6- tri- (3,5- di-tert-butyl-4-hydroxyl benzyl) benzene, 2,6- di-t-butyl -4- methyl-phenols, N, N '-two
The one or more of (3,5- di-tert-butyl-hydroxy phenyl propionamide), phosphite kind antioxidant is 2,2 '-ethylenebis
In (4,6- di-tert-butyl-phenyl) fluorophosphite, four (2,4- di-tert-butyl-phenyls) -4,4 '-xenyl bis-phosphite
It is one or more of.
The selective laser sintering of the present invention is had the advantages that with polyamide 610 dusty material and preparation method：
(1), the present invention is by solvent legal system powder, and wherein solvent is to include the mixed solvent of a certain proportion of first alcohol and water,
Polyamide 610 resin and solvent are blended in closed reactor by certain mass ratio, are vacuumized, nitrogen charging gas shielded, and experience first rises
The process of decrease temperature crystalline after temperature.In temperature-fall period, polyamide 610 strand is reduced in the relatively low regional activity ability of temperature,
Nucleus is generated, nucleus is evenly distributed and concentrated with strand collision, winding further growth granulating footpath, the powder that particle sphericity is high
Last particle；
(2), selective laser sintering of the present invention with polyamide 610 dusty material by comprising above-mentioned each component and content,
So that final obtained polyamide 610 dusty material also has good fluidity, sintering process stabilization, mechanical performance excellent, from
And the parts that surface quality is good, dimensional accuracy is high can be preferably manufactured, it is especially suitable for SLS moulding process；
(3), preparation method of the present invention is simple.
Brief description of the drawings
Fig. 1 be in a kind of selective laser sintering polyamide 610 dusty material and preparation method embodiment 1 20 times it is micro-
Pattern；
Fig. 2 be in a kind of selective laser sintering polyamide 610 dusty material and preparation method embodiment 2 20 times it is micro-
Pattern；
Fig. 3 be in a kind of selective laser sintering polyamide 610 dusty material and preparation method embodiment 3 20 times it is micro-
Pattern；
Fig. 4 be in a kind of selective laser sintering polyamide 610 dusty material and preparation method embodiment 4 20 times it is micro-
Pattern；
Fig. 5 be in a kind of selective laser sintering polyamide 610 dusty material and preparation method embodiment 5 20 times it is micro-
Pattern；
Fig. 6 is DCS curves in a kind of selective laser sintering polyamide 610 dusty material and preparation method embodiment 1；
Fig. 7 is DCS curves in a kind of selective laser sintering polyamide 610 dusty material and preparation method embodiment 2；
Fig. 8 is DCS curves in a kind of selective laser sintering polyamide 610 dusty material and preparation method embodiment 3；
Fig. 9 is DCS curves in a kind of selective laser sintering polyamide 610 dusty material and preparation method embodiment 4；
Figure 10 is DCS songs in a kind of selective laser sintering polyamide 610 dusty material and preparation method embodiment 5
Line.
Embodiment
Embodiment 1
Polyamide 610 material 10kg, methanol 76kg, water 4kg are put into 100L reactors, high pure nitrogen is passed through to pressure
For 0.3MPa, the lower heating of lasting stirring makes temperature in the kettle be increased to 150 DEG C, 60min is incubated at this temperature；Then using cooling
Water cools, and temperature in the kettle is down to 80 DEG C with 0.8 DEG C/min cooldown rate, and increasing cooling water flow makes temperature in the kettle be down to room
Temperature, taking-up material, centrifugation, drying, 100 eye mesh screens excessively are that can obtain polyamide 610 powder sample, and powder sample is carried out
Pattern, DSC tests, as a result as shown in figures 1 to 6.
Embodiment 2
Polyamide 610 material 10kg, methanol 72kg, water 8kg are put into 100L reactors, high pure nitrogen is passed through to pressure
For 0.3MPa, the lower heating of lasting stirring makes temperature in the kettle be increased to 150 DEG C, 60min is incubated at this temperature；Then using cooling
Water cools, and temperature in the kettle is down to 80 DEG C with 0.8 DEG C/min cooldown rate, and increasing cooling water flow makes temperature in the kettle be down to room
Temperature, taking-up material, centrifugation, drying, 100 eye mesh screens excessively are that can obtain polyamide 610 powder sample, and powder sample is carried out
Pattern, DSC tests, as a result as shown in Figure 2 and Figure 7.
Embodiment 3
Polyamide 610 material 10kg, methanol 64kg, water 16kg are put into 100L reactors, high pure nitrogen is passed through to pressure
Power is 0.3MPa, and the lower heating of lasting stirring makes temperature in the kettle be increased to 150 DEG C, and 60min is incubated at this temperature；Then using cold
But water cools, and temperature in the kettle is down to 80 DEG C with 0.8 DEG C/min cooldown rate, and increasing cooling water flow is down to temperature in the kettle
Room temperature, taking-up material, centrifugation, drying, 100 eye mesh screens excessively are that can obtain polyamide 610 powder sample, and powder sample is entered
Row pattern, DSC tests, as a result as shown in figures 3 and 8.
Embodiment 4
Polyamide 610 material 10kg, methanol 56kg, water 24kg are put into 100L reactors, high pure nitrogen is passed through to pressure
Power is 0.3MPa, and the lower heating of lasting stirring makes temperature in the kettle be increased to 150 DEG C, and 60min is incubated at this temperature；Then using cold
But water cools, and temperature in the kettle is down to 80 DEG C with 0.8 DEG C/min cooldown rate, and increasing cooling water flow is down to temperature in the kettle
Room temperature, taking-up material, centrifugation, drying, 100 eye mesh screens excessively are that can obtain polyamide 610 powder sample, and powder sample is entered
Row pattern, DSC tests, as a result as shown in figures 4 and 9.
Embodiment 5
Polyamide 610 material 10kg, methanol 48kg, water 32kg are put into 100L reactors, high pure nitrogen is passed through to pressure
Power is 0.3MPa, and the lower heating of lasting stirring makes temperature in the kettle be increased to 150 DEG C, and 60min is incubated at this temperature；Then using cold
But water cools, and temperature in the kettle is down to 80 DEG C with 0.8 DEG C/min cooldown rate, and increasing cooling water flow is down to temperature in the kettle
Room temperature, taking-up material, centrifugation, drying, 100 eye mesh screens excessively are that can obtain polyamide 610 powder sample, and powder sample is entered
Row pattern, DSC tests, as a result as shown in Fig. 5 and Figure 10.
Take above-mentioned polyamide 610 powder sample, powder flow aid, powder antioxidant mixed by following quality proportioning respectively
Close：99 parts of polyamide 610 powder, 0.5 part of aerosil, 2,610- 0.3 part of di-t-butyl -4- methyl-phenols, four (2,
4- di-tert-butyl-phenyls) -4,0.2 part of 4 '-xenyl bis-phosphite is obtained for laser sintered polyamide 610 powder material
Material, powder all-round property testing is carried out to dusty material.Burnt using Hu'nan Farsoon High-Tech Co., Ltd.'s HT403P equipment
Polyamide 610 dusty material is tied, tensile strength is carried out to the product that powder is obtained and HDT is tested, as a result as shown in table 1.
From each embodiments of Fig. 1 to Fig. 5 it was found from microstructure contrast, the content of solvent reclaimed water is fewer of more than 30% pattern
It will be deteriorated, illustrate that the methanol that optimal solvent is 70% mass fraction is mixed with 30% mass fraction water；It is each from Fig. 6 to Figure 10
DCS curve comparisons are understood in embodiment, and fusing point is all kept well as the content of solvent reclaimed water is improved and is slightly raised
DSC curve shape and wider sintering window (Tm-Tc), influence smaller to sintering process.In table 1, due to varying topography, it is stopped
Angle till is variant, and pattern is better, and angle of repose is lower, and mobility is better, and other powder parameters and mechanics mechanical performance difference compared with
It is small.
In a word, polyamide 610 powder is prepared the invention provides a kind of solvent precipitation, its solvent for use is cheap,
Technical process is simple, and obtained powder particle sphericity is high, and powder flowbility is good, and particle diameter distribution is narrow, material high income, sinters window
Mouth wide (Tm-Tc), is particularly suitable for use in selective laser sintering technique.
The polyamide 610 powder of table 1 and part performance
Claims (10)
1. a kind of selective laser sintering polyamide 610 dusty material, it is characterised in that by percentage to the quality including following
Component：PA610 powder 96~99.98%, powder flow aid 0.01~2.0%, powder antioxidant 0.01~2.0%.
2. selective laser sintering according to claim 1 polyamide 610 dusty material, it is characterised in that the powder
Last flow promortor is nano-calcium carbonate, nanomete talc powder, Nano carbon white, nano zine oxide, nanometer magnesium stearate and nano oxygen
Change the one or more in magnesium.
3. selective laser sintering according to claim 1 or 2 polyamide 610 dusty material, it is characterised in that described
Powder antioxidant includes：The Asia that the Hinered phenols antioxidant and mass fraction that mass fraction is 40%-90% are 10%~60%
Phosphate ester kind antioxidant, wherein Hinered phenols antioxidant are 1,3,5- trimethyls -2,4, (3, the 5- di-t-butyl -4- hydroxyls of 6- tri-
Benzyl) benzene, 2,6- di-t-butyl -4- methyl-phenols, N, one in N '-two (3,5- di-tert-butyl-hydroxy phenyl propionamide)
Kind or it is several, phosphite kind antioxidant be 2,2 '-ethylenebis (4,6- di-tert-butyl-phenyl) fluorophosphite, four (2,
4- di-tert-butyl-phenyls) -4, the one or more in 4 '-xenyl bis-phosphite.
4. a kind of selective laser sintering preparation method of polyamide 610 dusty material, it is characterised in that including following step
Suddenly：
(1) polyamide 610 resin and solvent are blended in by 1: 4~20 mass ratio in closed reactor, vacuumized, nitrogen charging
Gas shielded, is heated to 140~180 DEG C by material reaction maximum temperature under continuous agitation, and soaking time is 1~
300min, is then brought down below 5~10 DEG C of material Precipitation Temperature by the material reaction maximum temperature, and required temperature fall time is
60~180min, then obtain PA610 powder through centrifugation, dry and screening；
(2) by following components by percentage to the quality：PA610 powder 96~99.98%, powder flow aid 0.01~
2.0%, the mixing of powder antioxidant 0.01~2.0%, sieving obtain average grain diameter and are applied to selective laser burning for 30~120 μm
Knot uses polyamide 610 dusty material.
5. selective laser sintering according to claim 4 polyamide 610 powder material preparation method, its feature exists
In the solvent is made up of first alcohol and water, and the methanol accounts for the 60%~95% of solvent gross mass.
6. selective laser sintering according to claim 5 polyamide 610 powder material preparation method, its feature exists
In the mass ratio of the polyamide 610 resin and solvent is 1: 6~8.
7. selective laser sintering according to claim 6 polyamide 610 powder material preparation method, its feature exists
In the material reaction maximum temperature is 150~155 DEG C, and soaking time is 30~120min.
8. selective laser sintering according to claim 7 polyamide 610 powder material preparation method, its feature exists
In the temperature fall time is：80~120min.
9. selective laser sintering according to claim 8 polyamide 610 powder material preparation method, its feature exists
In the powder flow aid is nano-calcium carbonate, nanomete talc powder, Nano carbon white, nano zine oxide, nanometer stearic acid
One or more in magnesium, nano magnesia.
10. the selective laser sintering polyamide 610 powder material preparation method according to claim any one of 4-9,
Characterized in that, the powder antioxidant includes：The Hinered phenols antioxidant and mass fraction that mass fraction is 40%-90% be
10%~60% phosphite kind antioxidant, wherein Hinered phenols antioxidant are 1,3,5- trimethyls -2,4,6- tri- (3,5- bis-
Tertiary butyl-4-hydroxy benzyl) benzene, 2,6- di-t-butyl -4- methyl-phenols, N, (3, the 5- di-tert-butyl-hydroxy phenyls of N '-two
Propionamide) one or more, phosphite kind antioxidant be 2,2 '-ethylenebis (4,6- di-tert-butyl-phenyl) fluoro phosphorous
One or more in acid esters, four (2,4- di-tert-butyl-phenyls) -4,4 '-xenyl bis-phosphite.
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| WO2022007360A1 (en) * | 2020-07-06 | 2022-01-13 | 金发科技股份有限公司 | 3d printing powder and preparation method therefor |
| CN114276566A (en) * | 2021-12-23 | 2022-04-05 | 广东聚石科技研究有限公司 | Nylon powder and preparation method and application thereof |
| CN114276566B (en) * | 2021-12-23 | 2023-11-28 | 广东聚石科技研究有限公司 | Nylon powder and preparation method and application thereof |
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