CN107236294A - A kind of selective laser sintering polyamide 66 powder material preparation method - Google Patents
A kind of selective laser sintering polyamide 66 powder material preparation method Download PDFInfo
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Abstract
The invention provides a kind of selective laser sintering polyamide 66 powder material preparation method, including：Polyamide 66 resin and solvent are pressed 1:4~20 mass ratio is blended in closed reactor; add inorganic nucleator; reactor is vacuumized; then filling with inert gas is protected; material reaction maximum temperature is heated to 150~200 DEG C under continuous agitation, soaking time is 5~300min, then material is cooled to less than 5 10 DEG C of material Precipitation Temperature with 0.1~2.0 DEG C/min rate of temperature fall in kettle; fast cooling to room temperature, centrifugation, dry, screening obtains PA66 powder；By with following components of mass percent：PA66 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 for 30~180 μm of polyamide 66 dusty materials suitable for selective laser sintering.The polyamide 66 dusty material preparation technology that the present invention is provided, with low cost, technique simple possible, resulting powder is particularly suitable for use in SLS moulding process.
Description
Technical field
The invention belongs to increases material manufacturing technology field, and in particular to a kind of selective laser sintering polyamide 66 powder material
Preparation method for material
Background technology
SLS (Selective Laser Sintering, selective laser sintering) is by optionally fusing multiple powder
Last layer 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 is by multiple overlapping layers of laser sintering powder, to obtain 3D solid.This method is mainly polymerize using thermoplasticity
Thing is completed.The method that patent US6136948 and WO9606881 manufactures three-dimensional body to this use polymer powder is entered
Detailed description is gone.
Polyamide 66 powder-product is molded there is presently no the ripe selective laser that is used for, is further broadening selectivity
One of laser sintering technology application, the important directions studied at present when PA66 is as raw material.Current polyamide 66 powder
The main mode of production is cryogenic freezing disintegrating process, and its principle is that polymer and low-temperature receiver are carried out into heat exchange, cools to material
Brittle state, the shock that the material after embrittlement is carried out many times in crushing chamber by disintegrating mechanism finally turns into fine particle
Shape, the powder particle particle diameter distribution that the process is obtained is wide, and yield is relatively low；Sphericity is poor, and powder flowbility is relatively low.
The content of the invention
It is used for laser sintered polyamide 66 powder material preparation method, this method work it is an object of the invention to provide a kind of
Skill process is simple, with low cost, and polyamide 66 powder diameter distribution concentration, the sphericity of acquisition are high, are particularly suitable for use in selectivity
Laser sintering technology.
A kind of selective laser sintering polyamide 66 powder material preparation method, comprises the following steps：
(1) polyamide 66 resin and solvent, are pressed 1:4~20 mass ratio is blended in closed reactor, adds nothing
Machine nucleator, is evacuated to air pressure for ﹣ 0.2~﹣ 0.6Mpa by reactor, then passes in inert gas shielding to reactor
Air pressure is 0.2~0.4Mpa, and material reaction maximum temperature is heated into 150~200 DEG C, insulation under continuous agitation
Time is 5~300min；Then material is cooled to less than material Precipitation Temperature with 0.1~2.0 DEG C/min rate of temperature fall in kettle
5-10 DEG C, room temperature is cooled to 2.0~5.0 DEG C/min rate of temperature fall, centrifugation, dry, screening obtain PA66 powder；
(2), by with following components of mass percent：PA66 powder 96~99.98%, powder flow aid 0.01~
2.0%th, the mixing of powder antioxidant 0.01~2.0%, sieving obtain average grain diameter for 30~180 μm suitable for selective laser
The polyamide 66 dusty material of sintering.
As present invention further optimization scheme, the inorganic nucleator is silica powder, titanium oxide powder, carborundum
One or more in powder, talcum powder, Paris white, mica powder and alumina powder.
As present invention further optimization scheme, the addition of the inorganic nucleation powder is polyamide 66 resin quality
0.1~1.0%.
As present invention further optimization scheme, the particle size range of the inorganic nucleator is 20~40 μm.
As present invention further optimization scheme, the solvent is made up of first alcohol and water, and the methanol quality accounts for solvent
The 40%~60% of gross mass.
As present invention further optimization scheme, the mass ratio of the polyamide 66 resin and solvent is 1：8~12.
As present invention further optimization scheme, the material reaction maximum temperature is 155~165 DEG C, soaking time
For 30~120min.
As present invention further optimization scheme, the rate of temperature fall described in temperature-fall period is 0.5~1.2 DEG C/min.
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 is by Hinered phenols antioxidant and phosphorous acid lipid
Antioxidant is constituted, and wherein Hinered phenols antioxidant is 1,3,5- trimethyls -2,4, (3, the 5- di-t-butyl -4- hydroxyl benzyls of 6- tri-
Base) benzene, 2,6- di-t-butyl -4- methyl-phenols, N, N '-two (3,5- di-tert-butyl-hydroxy phenyl propionamide), phosphorous acid
Lipid antioxidant is 2,2 '-ethylenebis (4,6- di-tert-butyl-phenyl) fluorophosphite, four (2,4- di-tert-butyls
Base) -4,4 '-xenyl bis-phosphite, the Hinered phenols antioxidant accounts for the 40%-90% of powder antioxidant gross mass.
A kind of selective laser sintering of the present invention is had the advantages that with polyamide 66 powder material 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 66 resin is blended in closed reactor with solvent by certain mass ratio, is added inorganic nucleator, is vacuumized, fills lazy
Property gas shield, experience first heat up after decrease temperature crystalline process.In temperature-fall period, polyamide 66 strand is relatively low in temperature
The reduction of regional activity ability, and inorganic nucleator making contact, be evenly distributed using it as nucleus further growth into particle diameter and
The high powder particle of concentration, particle sphericity.Inorganic nucleator is by changing polyamide 66 resin in polyamide 66 solution
Crystallization behavior, makes it be changed into heterogeneous nucleation by homogeneous nucleation, accelerate the crystalline rate of polyamide 66 microballoon, add it is micro-
The crystal density of ball and promote Microsphere Size distribution more homogeneous, reach that polyamide 66 powder particle sphericity is high, particle diameter distribution
Effect that is uniform and concentrating；
(2), selective laser sintering of the present invention with polyamide 66 dusty material by comprising above-mentioned each component and content, making
Obtaining finally obtained polyamide 66 dusty material also has good fluidity, sintering process stabilization, mechanical performance excellent, so that
The parts that surface quality is good, dimensional accuracy is high can be preferably manufactured, SLS moulding process is especially suitable for；
(3), preparation method of the present invention is simple.
Brief description of the drawings
Fig. 1 is 20 times of micro- shapes in a kind of selective laser sintering polyamide 66 powder material preparation method embodiment 1
Looks；
Fig. 2 is 20 times of micro- shapes in a kind of selective laser sintering polyamide 66 powder material preparation method embodiment 2
Looks；
Fig. 3 is 20 times of micro- shapes in a kind of selective laser sintering polyamide 66 powder material preparation method embodiment 3
Looks；
Fig. 4 is 20 times of micro- shapes in a kind of selective laser sintering polyamide 66 powder material preparation method embodiment 4
Looks；
Fig. 5 is 20 times of micro- shapes in a kind of selective laser sintering polyamide 66 powder material preparation method embodiment 5
Looks；
Fig. 6 is 20 times of micro- shapes in a kind of selective laser sintering polyamide 66 powder material preparation method embodiment 6
Looks；
Fig. 7 is DCS curves in a kind of selective laser sintering polyamide 66 powder material preparation method embodiment 1；
Fig. 8 is DCS curves in a kind of selective laser sintering polyamide 66 powder material preparation method embodiment 2；
Fig. 9 is DCS curves in a kind of selective laser sintering polyamide 66 powder material preparation method embodiment 3；
Figure 10 is DCS curves in a kind of selective laser sintering polyamide 66 powder material preparation method embodiment 4；
Figure 11 is DCS curves in a kind of selective laser sintering polyamide 66 powder material preparation method embodiment 5；
Figure 12 is DCS curves in a kind of selective laser sintering polyamide 66 powder material preparation method embodiment 6.
Embodiment
The present invention is described in further detail below by specific embodiment.
Embodiment 1
Polyamide 66 material 10kg, methanol 50kg, water 50kg, titanium dioxide 30g are put into 100L reactors, will be reacted
Kettle is evacuated to air pressure for ﹣ 0.06Mpa, and it is 0.3Mpa to then pass to air pressure in inert gas shielding to reactor, lasting stirring
Lower heating makes temperature in the kettle be increased to 160 DEG C, and 30min is incubated at this temperature；Cooling water temperature then is used, makes temperature in the kettle
90 DEG C are down to 0.8 DEG C/min cooldown rate, increasing cooling water flow makes temperature in the kettle be down to room temperature, take out material, centrifugation
It is that can obtain polyamide 66 powder sample to separate, dry, crossing 80 eye mesh screens, and carrying out pattern, DSC to powder sample tests, as a result
As shown in Figure 1 and Figure 7.
Embodiment 2
Polyamide 66 material 10kg, methanol 50kg, water 50kg, calcium carbonate 30g are put into 100L reactors, by reactor
Air pressure is evacuated to for ﹣ 0.06Mpa, it is 0.3Mpa to then pass to air pressure in inert gas shielding to reactor, under lasting stirring
Heating makes temperature in the kettle be increased to 160 DEG C, and 30min is incubated at this temperature；Then use cooling water temperature, make temperature in the kettle with
0.8 DEG C/min cooldown rate is down to 90 DEG C, and increasing cooling water flow makes temperature in the kettle be down to room temperature, takes out material, centrifugation point
From, dry, cross 80 eye mesh screens be that can obtain polyamide 66 powder sample, to powder sample carry out pattern, DSC test, as a result such as
Shown in Fig. 2 and Fig. 8.
Embodiment 3
Polyamide 66 material 10kg, methanol 45kg, water 55kg, titanium dioxide 30g are put into 100L reactors, will be reacted
Kettle is evacuated to air pressure for ﹣ 0.06Mpa, and it is 0.3Mpa to then pass to air pressure in inert gas shielding to reactor, lasting stirring
Lower heating makes temperature in the kettle be increased to 160 DEG C, and 30min is incubated at this temperature；Cooling water temperature then is used, makes temperature in the kettle
90 DEG C are down to 0.8 DEG C/min cooldown rate, increasing cooling water flow makes temperature in the kettle be down to room temperature, take out material, centrifugation
It is that can obtain polyamide 66 powder sample to separate, dry, crossing 80 eye mesh screens, and carrying out pattern, DSC to powder sample tests, as a result
As shown in Figure 3 and Figure 9.
Embodiment 4
Polyamide 66 material 10kg, methanol 50kg, water 50kg, titanium dioxide 50g are put into 100L reactors, will be reacted
Kettle is evacuated to air pressure for ﹣ 0.06Mpa, and it is 0.3Mpa to then pass to air pressure in inert gas shielding to reactor, lasting stirring
Lower heating makes temperature in the kettle be increased to 160 DEG C, and 30min is incubated at this temperature；Cooling water temperature then is used, makes temperature in the kettle
90 DEG C are down to 0.8 DEG C/min cooldown rate, increasing cooling water flow makes temperature in the kettle be down to room temperature, take out material, centrifugation
It is that can obtain polyamide 66 powder sample to separate, dry, crossing 80 eye mesh screens, and carrying out pattern, DSC to powder sample tests, as a result
As shown in Fig. 4 and Figure 10.
Embodiment 5
Polyamide 66 material 10kg, methanol 50kg, water 50kg, titanium dioxide 80g are put into 100L reactors, will be reacted
Kettle is evacuated to air pressure for ﹣ 0.06Mpa, and it is 0.3Mpa to then pass to air pressure in inert gas shielding to reactor, lasting stirring
Lower heating makes temperature in the kettle be increased to 160 DEG C, and 30min is incubated at this temperature；Cooling water temperature then is used, makes temperature in the kettle
90 DEG C are down to 0.8 DEG C/min cooldown rate, increasing cooling water flow makes temperature in the kettle be down to room temperature, take out material, centrifugation
It is that can obtain polyamide 66 powder sample to separate, dry, crossing 80 eye mesh screens, and carrying out pattern, DSC to powder sample tests, as a result
As shown in Fig. 5 and Figure 11.
Embodiment 6
Polyamide 66 material 10kg, methanol 50kg, water 50kg, titanium dioxide 100g are put into 100L reactors, will be anti-
Kettle is answered to be evacuated to air pressure for ﹣ 0.06Mpa, it is 0.3Mpa to then pass to air pressure in inert gas shielding to reactor, is persistently stirred
Mixing lower heating makes temperature in the kettle be increased to 160 DEG C, and 30min is incubated at this temperature；Cooling water temperature then is used, is made warm in kettle
Degree is down to 90 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, take out material, from
It is that can obtain polyamide 66 powder sample that the heart, which is separated, dried, crossing 80 eye mesh screens, and carrying out pattern, DSC to powder sample tests, and ties
Fruit is as shown in Fig. 6 and Figure 12.
Above-mentioned polyamide 66 powder sample, powder flow aid, powder antioxidant is taken to be mixed by following quality proportioning respectively：
99 parts of polyamide 66 powder, 0.5 part of aerosil, 2,66- 0.3 part of di-t-butyl -4- methyl-phenols, four (2,4- bis-
Tert-butyl-phenyl) -4,0.2 part of 4 '-xenyl bis-phosphite is obtained for laser sintered polyamide 66 dusty material, right
Dusty material carries out powder all-round property testing.Use Hu'nan Farsoon High-Tech Co., Ltd.'s HT403P equipment sintering polyamides
The dusty material of amine 66, carries out tensile strength to the product that powder is obtained and HDT is tested, as a result as shown in table 1.
In from Fig. 1 to Figure 12, the microstructure and DCS curve comparisons of each embodiment are understood, solvent reclaimed water in embodiment 3
Content is 55%, and powder particle pattern is poor, illustrates that methanol and water quality ratio are 1 in solvent：Pattern is preferable when 1；Embodiment 1,
4,5,6 DSC graphic correlations understand that content of titanium dioxide increases, and fusing point is slightly raised, but peak shape is similar, to sintering process base
This is without influence；Embodiment 1,2 is contrasted, and identical addition, titanium dioxide is smaller than the powder diameter obtained by calcium carbonate, more
Beneficial to SLS selective laser moulding process.In table 1, because particle diameter is smaller, pattern is better, and angle of repose is lower, and mobility is better,
Accumulation effect is better, and tap density is higher, the workpiece mechanics mechanical performance and thermal deformation temperature printed using above-mentioned different powder
Spend difference smaller.
In a word, the polyamide 66 dusty material preparation technology that the present invention is provided, with low cost, technique simple possible, gained
To powder be particularly suitable for use in SLS moulding process.
The polyamide 66 powder of table 1 and part performance
Claims (10)
1. a kind of selective laser sintering polyamide 66 powder material preparation method, it is characterised in that comprise the following steps：
(1) polyamide 66 resin and solvent are pressed 1:4~20 mass ratio is blended in closed reactor, adds inorganic nucleation
Agent, reactor is vacuumized, and then filling with inert gas is protected, and under continuous agitation heats material reaction maximum temperature
To 150~200 DEG C, soaking time is 5~300min, and then material is cooled to 0.1~2.0 DEG C/min rate of temperature fall in kettle
Less than 5-10 DEG C of material Precipitation Temperature, fast cooling to room temperature, centrifugation, dry, screening obtains PA66 powder；
(2) by with following components of mass percent：PA66 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 the poly- of selective laser sintering for 30~180 μm
The dusty material of acid amides 66.
2. selective laser sintering according to claim 1 polyamide 66 powder material preparation method, it is characterised in that
The inorganic nucleator is in silica powder, titanium oxide powder, carborundum powder, talcum powder, Paris white, mica powder and alumina powder
One or more.
3. selective laser sintering according to claim 2 polyamide 66 powder material preparation method, it is characterised in that
The addition of the inorganic nucleator is the 0.01~5.0% of polyamide 66 resin quality.
4. selective laser sintering according to claim 3 polyamide 66 powder material preparation method, it is characterised in that
The particle size range of the inorganic nucleator is 1~60 μm.
5. the polyamide 66 powder material preparation method of the selective laser sintering according to any one of claim 1-4,
Characterized in that, the solvent is made up of first alcohol and water, the methanol quality accounts for the 40%~60% of solvent gross mass.
6. selective laser sintering according to claim 5 polyamide 66 powder material preparation method, it is characterised in that
The mass ratio of the polyamide 66 resin and solvent is 1：8~12.
7. selective laser sintering according to claim 6 polyamide 66 powder material preparation method, it is characterised in that
The material reaction maximum temperature is 155~165 DEG C, and soaking time is 30~120min.
8. selective laser sintering according to claim 7 polyamide 66 powder material preparation method, it is characterised in that
Rate of temperature fall described in temperature-fall period is 0.5~1.2 DEG C/min.
9. selective laser sintering according to claim 8 polyamide 66 powder material preparation method, it is characterised in that
The powder flow aid is nano-calcium carbonate, nanomete talc powder, Nano carbon white, nano zine oxide, nanometer magnesium stearate, received
One or more in rice magnesia.
10. selective laser sintering according to claim 9 polyamide 66 powder material preparation method, its feature exists
In the powder antioxidant is made up of Hinered phenols antioxidant and phosphite kind antioxidant, and wherein Hinered phenols antioxidant is
1,3,5- trimethyl -2,4,6- tri- (3,5- di-tert-butyl-4-hydroxyl benzyl) benzene, 2,6- di-t-butyl -4- methyl-phenols, N,
N '-two (3,5- di-tert-butyl-hydroxy phenyl propionamide), phosphite kind antioxidant is 2,2 '-ethylenebis (4,6- bis- uncles
Butyl phenyl) fluorophosphite, four (2,4- di-tert-butyl-phenyls) -4,4 '-xenyl bis-phosphite, the Hinered phenols
Antioxidant accounts for the 40%-90% of powder antioxidant gross mass.
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Cited By (7)
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| CN109593355A (en) * | 2018-11-09 | 2019-04-09 | 湖南华曙高科技有限责任公司 | Nylon polymer dusty material and preparation method thereof |
| CN111040443A (en) * | 2019-12-27 | 2020-04-21 | 湖南华曙高科技有限责任公司 | Polyamide powder material for selective laser sintering and preparation method thereof |
| CN111117108A (en) * | 2019-12-25 | 2020-05-08 | 广东祺龙科技有限公司 | High-strength flame-retardant PVC (polyvinyl chloride) and preparation method thereof |
| CN112390965A (en) * | 2019-08-01 | 2021-02-23 | 万华化学集团股份有限公司 | Nylon powder for selective laser sintering, preparation method thereof and three-dimensional printed product |
| CN112442270A (en) * | 2019-09-03 | 2021-03-05 | 中国科学院化学研究所 | Nano material composite polymer powder and preparation method thereof |
| WO2021118589A1 (en) * | 2019-12-13 | 2021-06-17 | Hewlett-Packard Development Company, L.P. | Three-dimensional printing with calcium carbonate particles |
| CN114456409A (en) * | 2021-12-28 | 2022-05-10 | 常州增材制造研究院有限公司 | PA11 material for selective laser sintering 3D printing and preparation method thereof |
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