CN107337793A - Copolymer nylon dusty material for selective laser sintering and preparation method thereof - Google Patents
Copolymer nylon dusty material for selective laser sintering and preparation method thereof Download PDFInfo
- Publication number
- CN107337793A CN107337793A CN201710636091.1A CN201710636091A CN107337793A CN 107337793 A CN107337793 A CN 107337793A CN 201710636091 A CN201710636091 A CN 201710636091A CN 107337793 A CN107337793 A CN 107337793A
- Authority
- CN
- China
- Prior art keywords
- salt
- nylon
- copolymer nylon
- copolymer
- dusty material
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
- C08G69/02—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
- C08G69/26—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from polyamines and polycarboxylic acids
- C08G69/28—Preparatory processes
-
- 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
- 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
-
- 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
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/02—Organic and inorganic ingredients
-
- 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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
-
- 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
-
- 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
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/13—Phenols; Phenolates
-
- 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
- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/20—Carboxylic acid amides
-
- 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
- C08K5/00—Use of organic ingredients
- C08K5/49—Phosphorus-containing compounds
- C08K5/51—Phosphorus bound to oxygen
- C08K5/52—Phosphorus bound to oxygen only
- C08K5/524—Esters of phosphorous acids, e.g. of H3PO3
- C08K5/526—Esters of phosphorous acids, e.g. of H3PO3 with hydroxyaryl compounds
-
- 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
- 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
-
- 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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
-
- 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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
Landscapes
- Chemical & Material Sciences (AREA)
- 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)
- Processing And Handling Of Plastics And Other Materials For Molding In General (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
- Polyamides (AREA)
Abstract
The invention provides a kind of copolymer nylon dusty material for selective laser sintering and preparation method thereof, by using the principle of copolyreaction, the progress copolyreaction such as a kind of short chain nylon raw material and long carbon chain nylon raw material is obtained into copolymer polyamide resin, copolymer polyamide resin is passed through into deep cooling crush technique, after drying and sieving, the copolymer nylon material for selective laser sintering is obtained after adding flow promortor and antioxidant.The preparation method technique of the present invention is simple, and easily controllable, copolymer nylon powder diameter of the invention has the characteristics of particle diameter distribution is narrow, can perform well in post forming, be suitable for material increasing field.
Description
Technical field
The invention belongs to increases material manufacturing technology field, and in particular to a kind of copolymer nylon powder for selective laser sintering
Powder material and preparation method thereof.
Background technology
Selective laser sintering (Selective Laser Sintering, SLS) technology has begun to be applied to industry life
In production.Different from the method for traditional subtractive processes, splicing and combination forming, selective laser sintering technique is to utilize to increase material system
The method rapidoprint made.SLS technologies are not influenceed by material shape, can manufacture labyrinth, so being widely applied to vapour
The fields such as car, medical treatment, building and space flight.
Nylon is a kind of semicrystalline polymeric, has wider sintering window, extensively should have been obtained in SLS technologies
With.Because long carbon chain nylon has relatively low fusing point, the relatively short carbon chain nylon of crystallinity is lower, easier to process, so SLS technologies
Middle application is more.But long carbon chain nylon intensity is relatively low, and price is higher, the present application of nylon.Short carbon chain nylon has higher
Intensity, price is also relatively inexpensive, but its fusing point is high, and crystal property is more preferable so that limits it and is applied to SLS moulding process.
The content of the invention
The invention provides a kind of copolymer nylon dusty material and preparation method for selective laser sintering, cost
It is low, it is easy to accomplish, it is easily applied to industrial production.The present invention controls the ratio of two kinds of nylon salts in copolymer nylon since salt manufacturing,
Copolymer nylon salt disposably is obtained, copolymer nylon fusing point can be efficiently controlled and eliminate the separation of salt, drying process, improved
Technology stability, save preparation time.Preparation cost has not only been saved, and has improved copolymer nylon dusty material performance
Stability.
The invention provides a kind of copolymer nylon dusty material for selective laser sintering, the copolymer nylon powder
Material is polymerized by long carbon chain nylon salt and short carbon chain nylon salt, the quality of long carbon chain nylon salt and the short carbon chain nylon salt
Than for 9~1: 1~9.
As present invention further optimization scheme, the copolymer nylon dusty material is by long carbon chain nylon salt and short carbon chain
Nylon salt is polymerized, and the mass ratio of long carbon chain nylon salt and the short carbon chain nylon salt is 3~7: 7~3.
As present invention further optimization scheme, the long carbon chain nylon salt is PA1010 salt, PA1012 salt, PA1212
Any of salt, PA1014 salt, PA1214 salt, lauric lactam and omega-amino undecanoic acid.
As present invention further optimization scheme, the short carbon chain nylon salt is caprolactam or PA66 salt.
As present invention further optimization scheme, the copolymer nylon dusty material also includes antioxidant, described anti-
Oxidant is Hinered phenols oxidant or phosphorous acid lipid antioxidant, and wherein hindered phenol anti-oxidants are 1,3,5- front threes
Base -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) in one or more, the phosphorous acid lipid antioxidant be 2,2 '-ethylidene
Double (4,6- di-tert-butyl-phenyl) fluorophosphites, four (2,4- di-tert-butyl-phenyls) -4, in 4 '-xenyl bis-phosphite
One or more.
The copolymer nylon dusty material also includes molecular weight regulator, and the molecular weight regulator is SA, 12
Any of carbon diacid, 14 carbon diacid, thapsic acid and 18 carbon diacid.
As present invention further optimization scheme, the copolymer nylon dusty material also includes flow promortor, the stream
Dynamic auxiliary agent is aerosil, gas phase alundum (Al2O3) or nano titanium oxide.
Present invention also offers a kind of copolymer nylon powder material preparation method for selective laser sintering, including such as
Lower step：
Step 1：Deionized water and long carbon chain nylon salt, short carbon chain nylon salt, molecular weight regulator, antioxidant are added
Enter into polymeric kettle, wherein, both long carbon chain nylon salt, short carbon chain nylon salt quality sum and molecular weight regulator, deionization
Water, the ratio of antioxidant quality are 58.4%~88.4%: 0.4%~1.0%: 10%~40%: 0.4%~1.0%, close
Close, vacuumize, it is 0.10~0.15MPa to then pass to pressure in carbon dioxide to reactor, is warming up to 190~235 DEG C,
Pressure pressurize 0.5-3h, is then slowly deflated to normal pressure up to 1.1~1.6MPa, be warming up to 238~270 DEG C keep reaction 0.2~
3h, stop heating, the discharging of water cooling tie rod, pelletizing, obtain copolymer nylon pellet；
Step 2：Copolymer nylon powder is prepared by the method for deep cooling crush；
Step 3：Copolymer nylon powder passes through drying, screening, obtains copolymer nylon powder of the average grain diameter at 45~65 μm
End；
Step 4：Sieve, obtain after copolymer nylon powder made from step 3 is well mixed with flow promortor, antioxidant
To a kind of selective laser sintering nylon powder.
As present invention further optimization scheme, the method for the deep cooling crush is specially：For selecting the crushing
For the crushing temperature control of pulverizing chamber between -160~-125 DEG C, regulation rotor clearance is 0.5~2.5mm in technique, and main frame turns
Speed is 2000~6000r/min, and feed rate is controlled at 2~20kg/ (kWh).
As present invention further optimization scheme, copolymer nylon powder, flow promortor and antioxygen described in step 4
The proportioning of agent is 1: 0.5%~3%: 0.2%~0.5%.
A kind of selective laser sintering of the present invention has below beneficial to effect with static resistant polyamide powder and preparation method
Fruit：
1. being copolymerized using long carbon chain nylon and short carbon chain nylon, change the structure of nylon from molecular structure, so as to prepare
Obtain relative to the higher material of long carbon chain nylon intensity.
2. copolymer nylon crystallinity is low simultaneously, crystalline rate is slow so that its sintering window is wider, is suitable for selective laser
Sintering.Simultaneously because its crystallinity is low, copolymer nylon sintered part, elongation at break is higher, and its toughness is more preferable.
3. because the market price of short carbon chain nylon that the present invention uses is lower relative to long carbon chain nylon material, by itself and
Long-chain nylon raw material, which carries out copolymerization, can significantly reduce the preparation cost of alloy powder, have a good application prospect.
4. preparing copolymer nylon powder by cryogenic technology, powder diameter can be effectively controlled, while add flow promortor
Can solve the irregular factor for causing poor fluidity of its pattern, this preparation method technique is simple, easy to operate, prepares cost
It is low.
Brief description of the drawings
Fig. 1 is the DCS curve maps of the copolymer nylon dusty material embodiment three of selective laser sintering of the present invention.
Embodiment
The present invention is described in further detail below by specific embodiment.
Embodiment one：
Step 1：PA1010 salt, caprolactam, molecular weight regulator, deionized water, antioxidant are added to polymeric kettle
In.Wherein the mass ratio of PA1010 salt and caprolactam is 3:7 (by 10 parts of calculating), both PA1010 salt, caprolactam quality
Sum and molecular weight regulator, deionized water, the ratio of antioxidant quality are 88.4%: 0.8%: 10%: 0.8%；It is closed, take out
Vacuum, CO 2 gas-shielded 0.18MPa is then passed to, be warming up to 210 DEG C, pressure reaches 1.5MPa, pressurize 0.5h, Ran Houhuan
Slowly normal pressure is deflated to, is warming up to 250 DEG C and keeps reaction 2.5h, stopped heating, the discharging of water cooling tie rod, pelletizing, obtain being copolymerized Buddhist nun
Imperial pellet.
Step 2：Copolymer nylon powder is prepared by the method for deep cooling crush, the crushing of pulverizing chamber in the disintegrating process
For temperature control at -125 ± 5 DEG C, regulation rotor clearance is 0.5mm, engine speed 6000r/min, and feed rate, which controls, to exist
20kg/kW.h。
Step 3：Obtain copolymer nylon powder and pass through drying, sieve, obtain copolymer nylon powder of the average grain diameter at 40 μm
End.
Step 4：Copolymer nylon powder will be obtained with flow promortor, antioxidant by 1:3%:0.2% proportioning mixing, is mixed
Sieved after closing uniformly, obtain a kind of selective laser sintering nylon powder.
Embodiment two：
Step 1：PA1010 salt, caprolactam, molecular weight regulator, deionized water, antioxidant are added to polymeric kettle
In.Wherein the mass ratio of PA1010 salt and caprolactam is 7:3 (by 10 parts of calculating), both PA1010 salt, caprolactam quality
Sum and molecular weight regulator, deionized water, the ratio of antioxidant quality are 79.2%: 0.4%: 20%: 0.4%；It is closed, take out
Vacuum, then pass to CO 2 gas-shielded 0.18MPa.220 DEG C are warming up to, pressure reaches 1.6MPa, pressurize 1h, then slowly
Normal pressure is deflated to, 260 DEG C is warming up to and keeps reaction 1h, stops heating, the discharging of water cooling tie rod, pelletizing, obtains copolymer nylon grain
Material.
Step 2：Copolymer nylon powder is prepared by the method for deep cooling crush, the crushing of pulverizing chamber in the disintegrating process
Temperature control is between -130 ± 5 DEG C, and regulation rotor clearance is 2.0mm, engine speed 5000r/min, feed rate control
In 16kg/kW.h.
Step 3：Obtain copolymer nylon powder and pass through drying, sieve, obtain copolymer nylon powder of the average grain diameter at 50 μm
End.
Step 4：Copolymer nylon powder will be obtained with flow promortor, antioxidant by 1:2.5%:0.3% proportioning mixing,
Sieved after well mixed, obtain a kind of selective laser sintering nylon powder.
Embodiment three：
Step 1：PA1010 salt, PA66 salt, molecular weight regulator, deionized water, antioxidant are added in polymeric kettle.
The mass ratio of wherein PA1010 salt and PA66 salt is 3:7 (by 10 parts of calculating), both PA1010 salt, PA66 salt quality sum are with dividing
Son amount conditioning agent, deionized water, the ratio of antioxidant quality are 68.8%: 0.6%: 30%: 0.6%；It is closed, vacuumize, so
After be passed through CO 2 gas-shielded 0.18MPa.230 DEG C are warming up to, pressure reaches 1.7MPa, pressurize 1.5h, then slowly deflates
To normal pressure, it is warming up to 270 DEG C and keeps reaction 1.5h, stops heating, the discharging of water cooling tie rod, pelletizing, obtain copolymer nylon pellet.
Step 2：Copolymer nylon powder is prepared by the method for deep cooling crush, the crushing of pulverizing chamber in the disintegrating process
Temperature control is between -140 ± 5 DEG C, and regulation rotor clearance is 1.5mm, engine speed 4000r/min, feed rate control
In 12kg/kW.h.
Step 3：Obtain copolymer nylon powder and pass through drying, sieve, obtain copolymer nylon powder of the average grain diameter at 60 μm
End.
Step 4：Copolymer nylon powder will be obtained with flow promortor, antioxidant by 1:2.0%:0.4% proportioning mixing,
Sieved after well mixed, obtain a kind of selective laser sintering nylon powder.
Example IV：
Step 1：PA1212 salt, caprolactam, molecular weight regulator, deionized water, antioxidant are added to polymeric kettle
In.Wherein the mass ratio of PA1212 salt and caprolactam is 1:9 (by 10 parts of calculating), both PA1212 salt, caprolactam quality
Sum and molecular weight regulator, deionized water, the ratio of antioxidant quality are 58.4%: 0.8%: 40%: 0.8%；It is closed, take out
Vacuum, then pass to CO 2 gas-shielded 0.18MPa.240 DEG C are warming up to, pressure reaches 1.8MPa, pressurize 2.0h, Ran Houhuan
Slowly normal pressure is deflated to, is warming up to 280 DEG C and keeps reaction 2.0h, stopped heating, the discharging of water cooling tie rod, pelletizing, obtain being copolymerized Buddhist nun
Imperial pellet.
Step 2：Copolymer nylon powder is prepared by the method for deep cooling crush, the crushing of pulverizing chamber in the disintegrating process
Temperature control is between -150 ± 5 DEG C, and regulation rotor clearance is 1.0mm, engine speed 3000r/min, feed rate control
In 8kg/kW.h.
Step 3：Obtain copolymer nylon powder and pass through drying, sieve, obtain copolymer nylon powder of the average grain diameter at 60 μm
End.
Step 4：Copolymer nylon powder will be obtained with flow promortor, antioxidant by 1:1.0%:0.5% proportioning mixing,
Sieved after well mixed, obtain a kind of selective laser sintering nylon powder.
Embodiment five：
Step 1：Lauric lactam, PA66 salt, molecular weight regulator, deionized water, antioxidant are added to polymeric kettle
In.The mass ratio of wherein lauric lactam and PA66 salt is 5:5 (by 10 parts of calculating), both lauric lactam, PA66 salt quality
Sum and molecular weight regulator, deionized water, the ratio of antioxidant quality are 78%: 1.0%: 20%: 1.0%；It is closed, take out true
Sky, then pass to CO 2 gas-shielded 0.18MPa.260 DEG C are warming up to, pressure reaches 2.0MPa, pressurize 2.5h, then slowly
Normal pressure is deflated to, 300 DEG C is warming up to and keeps reaction 2.5h, stops heating, the discharging of water cooling tie rod, pelletizing, obtains copolymer nylon
Pellet.
Step 2：Copolymer nylon powder is prepared by the method for deep cooling crush, the crushing of pulverizing chamber in the disintegrating process
Temperature control is between -160 ± 5 DEG C, and regulation rotor clearance is 0.5mm, engine speed 2000r/min, feed rate control
In 2kg/kW.h.
Step 3：Obtain copolymer nylon powder and pass through drying, sieve, obtain copolymer nylon powder of the average grain diameter at 70 μm
End.
Step 4：Copolymer nylon powder will be obtained with flow promortor, antioxidant by 1:0.5%:0.5% proportioning mixing,
Sieved after well mixed, obtain a kind of selective laser sintering nylon powder.
The selective laser sintering 3 d part prepared using the copolymer nylon dusty material of above-described embodiment one to five
Correlation performance parameters are as described in Table 1, copolymeric material melting temperature Tm in table 1, in sintering window in Selective Laser Sintering
In, polyamide powder incipient melting temperature Tmo and FCTA temprature Tco difference are defined as, is represented using △ T, such as Fig. 1 institutes
Show, be the DCS curve maps of copolymer nylon dusty material.
Table 1：The performance of selective laser sintering 3 d part prepared by the copolymer nylon dusty material of embodiment one to five
Parameter
Claims (10)
- A kind of 1. copolymer nylon dusty material for selective laser sintering, it is characterised in that the copolymer nylon powder material Material is polymerized by long carbon chain nylon salt and short carbon chain nylon salt, the mass ratio of long carbon chain nylon salt and the short carbon chain nylon salt For 9~1: 1~9.
- 2. copolymer nylon dusty material according to claim 1, it is characterised in that the copolymer nylon dusty material is by growing Carbon chain nylon salt and short carbon chain nylon salt are polymerized, and the mass ratio of long carbon chain nylon salt and the short carbon chain nylon salt is 3~7 : 7~3.
- 3. copolymer nylon dusty material according to claim 1 or 2, it is characterised in that the long carbon chain nylon salt is Appointing in PA1010 salt, PA1012 salt, PA1212 salt, PA1014 salt, PA1214 salt, lauric lactam and omega-amino undecanoic acid It is a kind of.
- 4. copolymer nylon dusty material according to claim 3, it is characterised in that the short carbon chain nylon salt is acyl in oneself Amine or PA66 salt.
- 5. copolymer nylon dusty material according to claim 4, it is characterised in that the copolymer nylon dusty material also wraps Antioxidant is included, the antioxidant is Hinered phenols oxidant or phosphorous acid lipid antioxidant, wherein Hinered phenols antioxygen Agent is 1,3,5- trimethyls -2,4,6- tri- (3,5- di-tert-butyl-4-hydroxyl benzyl) benzene, 2,6- di-t-butyls -4- methyl-benzene Phenol, N, the one or more in N '-two (3,5- di-tert-butyl-hydroxy phenyl propionamide), the phosphorous acid lipid are anti-oxidant Agent is 2,2 '-ethylenebis (4,6- di-tert-butyl-phenyl) fluorophosphite, four (2,4- di-tert-butyl-phenyl) -4,4 '-connection One or more in phenyl bis-phosphite.
- 6. copolymer nylon dusty material according to claim 5, it is characterised in that the copolymer nylon dusty material also wraps Molecular weight regulator is included, the molecular weight regulator is SA, dodecanedioic acid, 14 carbon diacid, thapsic acid and ten Any of eight carbon diacid.
- 7. copolymer nylon dusty material according to claim 6, it is characterised in that the copolymer nylon dusty material also wraps Flow promortor is included, the flow promortor is aerosil, gas phase alundum (Al2O3) or nano titanium oxide.
- 8. the preparation method of a kind of copolymer nylon dusty material for selective laser sintering, it is characterised in that including following Step：Step 1：By the long carbon chain nylon salt any one of deionized water and claim 1 to 7, short carbon chain nylon salt, divide Son amount conditioning agent, antioxidant are added in polymeric kettle, closed, are vacuumized, are then passed in carbon dioxide to reactor Pressure is 0.10~0.15MPa, is warming up to 190~235 DEG C, pressure pressurize 0.5-3h, is then slowly put up to 1.1~1.6MPa Gas is warming up to 238~270 DEG C and keeps 0.2~3h of reaction, stop heating, the discharging of water cooling tie rod, pelletizing, be total to normal pressure Poly- nylon pellet；Step 2：Copolymer nylon powder is prepared by the method for deep cooling crush；Step 3：Copolymer nylon powder passes through drying, screening, obtains copolymer nylon powder of the average grain diameter at 45~65 μm；Step 4：Sieved after copolymer nylon powder made from step 3 is well mixed with flow promortor, antioxidant, obtain one Kind selective laser sintering nylon powder.
- 9. the preparation method of the copolymer nylon dusty material according to claim 8 for selective laser sintering, it is special Sign is that the method for the deep cooling crush is specially：For select the crushing temperature control of pulverizing chamber in the disintegrating process- Between 160~-125 DEG C, regulation rotor clearance is 0.5~2.5mm, and engine speed is 2000~6000r/min, feed rate control System is at 2~20kg/ (kWh).
- 10. the preparation method of the copolymer nylon dusty material for selective laser sintering according to claim 8 or claim 9, Characterized in that, the proportioning of the copolymer nylon powder, flow promortor and antioxidant described in step 4 is 1: 0.5%~3%: 0.2%~0.5%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710636091.1A CN107337793B (en) | 2017-07-28 | 2017-07-28 | Copolymerized nylon powder material for selective laser sintering and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710636091.1A CN107337793B (en) | 2017-07-28 | 2017-07-28 | Copolymerized nylon powder material for selective laser sintering and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107337793A true CN107337793A (en) | 2017-11-10 |
| CN107337793B CN107337793B (en) | 2021-07-02 |
Family
ID=60216591
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710636091.1A Active CN107337793B (en) | 2017-07-28 | 2017-07-28 | Copolymerized nylon powder material for selective laser sintering and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107337793B (en) |
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107974077A (en) * | 2017-11-24 | 2018-05-01 | 湖南华曙高科技有限责任公司 | A kind of nylon composite materials for selective laser sintering and preparation method thereof |
| CN109128133A (en) * | 2018-08-02 | 2019-01-04 | 中广核研究院有限公司 | A kind of recombination radiation protective materials and preparation method |
| CN110591343A (en) * | 2019-09-02 | 2019-12-20 | 湖南华曙高科技有限责任公司 | High-molecular powder material, preparation method thereof and method for preparing workpiece by using material |
| CN113150269A (en) * | 2021-03-31 | 2021-07-23 | 上海庚彩新材料科技有限公司 | Semi-aromatic polyamide copolymer and preparation thereof |
| CN113234319A (en) * | 2021-06-30 | 2021-08-10 | 贺州学院 | Copolymerized nylon/graphene composite microsphere for selective laser sintering and preparation method thereof |
| CN113667130A (en) * | 2021-08-19 | 2021-11-19 | 郑州大学 | Thermoplastic polyamide elastomer powder for selective laser sintering and preparation method thereof |
| CN114262518A (en) * | 2021-12-31 | 2022-04-01 | 湖南华曙高科技股份有限公司 | Nylon powder material for selective laser sintering and preparation method thereof |
| CN115894901A (en) * | 2021-08-20 | 2023-04-04 | 中国石油化工股份有限公司 | Block copolymer nylon and preparation method thereof |
| CN115926441A (en) * | 2022-12-08 | 2023-04-07 | 中国石油化工股份有限公司 | Transparent copolymerized nylon film and biaxial stretching film forming process thereof |
| CN116003782A (en) * | 2022-04-26 | 2023-04-25 | 湖南世博瑞高分子新材料有限公司 | Synthesis method and application of high-flow low-temperature-resistant PA66 resin |
| EP4279536A1 (en) | 2022-05-17 | 2023-11-22 | Ems-Chemie Ag | Materials for selective laser sintering and laser sintering using such materials |
| WO2024074793A1 (en) * | 2022-10-05 | 2024-04-11 | Arkema France | Method for producing a polyamide powder |
| EP4386036A1 (en) | 2022-12-15 | 2024-06-19 | Ems-Chemie Ag | Materials for selective laser sintering and laser sintering using such materials |
| EP4438654A1 (en) | 2023-03-29 | 2024-10-02 | Ems-Chemie Ag | Materials for powder bed fusion technologies and using such materials in a layer-by-layer process |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2650106A1 (en) * | 2012-04-11 | 2013-10-16 | Evonik Industries AG | Polymer powder with adapted melt behaviour |
| CN104559909A (en) * | 2015-01-29 | 2015-04-29 | 上海化工研究院 | Low-melting-point copolyamide hot melt adhesive and preparation method thereof |
-
2017
- 2017-07-28 CN CN201710636091.1A patent/CN107337793B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2650106A1 (en) * | 2012-04-11 | 2013-10-16 | Evonik Industries AG | Polymer powder with adapted melt behaviour |
| CN104559909A (en) * | 2015-01-29 | 2015-04-29 | 上海化工研究院 | Low-melting-point copolyamide hot melt adhesive and preparation method thereof |
Cited By (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107974077A (en) * | 2017-11-24 | 2018-05-01 | 湖南华曙高科技有限责任公司 | A kind of nylon composite materials for selective laser sintering and preparation method thereof |
| CN109128133A (en) * | 2018-08-02 | 2019-01-04 | 中广核研究院有限公司 | A kind of recombination radiation protective materials and preparation method |
| CN110591343A (en) * | 2019-09-02 | 2019-12-20 | 湖南华曙高科技有限责任公司 | High-molecular powder material, preparation method thereof and method for preparing workpiece by using material |
| CN110591343B (en) * | 2019-09-02 | 2022-03-29 | 湖南华曙高科技股份有限公司 | High-molecular powder material, preparation method thereof and method for preparing workpiece by using material |
| CN113150269A (en) * | 2021-03-31 | 2021-07-23 | 上海庚彩新材料科技有限公司 | Semi-aromatic polyamide copolymer and preparation thereof |
| CN113234319A (en) * | 2021-06-30 | 2021-08-10 | 贺州学院 | Copolymerized nylon/graphene composite microsphere for selective laser sintering and preparation method thereof |
| CN113667130A (en) * | 2021-08-19 | 2021-11-19 | 郑州大学 | Thermoplastic polyamide elastomer powder for selective laser sintering and preparation method thereof |
| CN115894901A (en) * | 2021-08-20 | 2023-04-04 | 中国石油化工股份有限公司 | Block copolymer nylon and preparation method thereof |
| CN114262518A (en) * | 2021-12-31 | 2022-04-01 | 湖南华曙高科技股份有限公司 | Nylon powder material for selective laser sintering and preparation method thereof |
| CN116003782A (en) * | 2022-04-26 | 2023-04-25 | 湖南世博瑞高分子新材料有限公司 | Synthesis method and application of high-flow low-temperature-resistant PA66 resin |
| CN116003782B (en) * | 2022-04-26 | 2024-08-06 | 湖南世博瑞高分子新材料有限公司 | Synthesis method and application of high-flow low-temperature-resistant PA66 resin |
| EP4279536A1 (en) | 2022-05-17 | 2023-11-22 | Ems-Chemie Ag | Materials for selective laser sintering and laser sintering using such materials |
| WO2024074793A1 (en) * | 2022-10-05 | 2024-04-11 | Arkema France | Method for producing a polyamide powder |
| FR3140627A1 (en) * | 2022-10-05 | 2024-04-12 | Arkema France | Process for manufacturing polyamide powder |
| CN115926441A (en) * | 2022-12-08 | 2023-04-07 | 中国石油化工股份有限公司 | Transparent copolymerized nylon film and biaxial stretching film forming process thereof |
| CN115926441B (en) * | 2022-12-08 | 2024-03-12 | 中国石油化工股份有限公司 | Transparent copolymerized nylon film and biaxially oriented film forming process thereof |
| EP4386036A1 (en) | 2022-12-15 | 2024-06-19 | Ems-Chemie Ag | Materials for selective laser sintering and laser sintering using such materials |
| EP4438654A1 (en) | 2023-03-29 | 2024-10-02 | Ems-Chemie Ag | Materials for powder bed fusion technologies and using such materials in a layer-by-layer process |
Also Published As
| Publication number | Publication date |
|---|---|
| CN107337793B (en) | 2021-07-02 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107337793A (en) | Copolymer nylon dusty material for selective laser sintering and preparation method thereof | |
| CN107337792A (en) | Controllable copolymer nylon dusty material of a kind of fusing point and preparation method thereof | |
| CN104576028B (en) | Methods for manufacturing cerium-rich anisotropy nano-crystalline rare-earth permanent magnets | |
| CN112935252B (en) | Method for preparing high-toughness eutectic high-entropy alloy based on selective laser melting technology | |
| CN101899592B (en) | Method for synthesizing arbitrarily shaped NiTi shape memory alloy in situ | |
| CN107286338A (en) | A kind of selective laser sintering polyamide material and preparation method thereof | |
| JP6242828B2 (en) | Method of manufacturing magnetocaloric element and magnetocaloric element obtained thereby | |
| JP5399081B2 (en) | Method for producing non-sticky granules from a polyester material, and method for further processing the produced granules | |
| EP2698344A1 (en) | Post-sinter conglutination and oxidation-preventative vanadium-nitrogen alloy preparation method | |
| CN104607646B (en) | Production method for sub-micron-order Re-Ni rare earth hydrogen storage alloy powder | |
| CN102950290B (en) | Method for producing nanoscale nickel-manganese alloy powder | |
| CN107974077A (en) | A kind of nylon composite materials for selective laser sintering and preparation method thereof | |
| CN102271791A (en) | Method of producing microporous polymer membrane and microporous polymer membrane produced by the method | |
| RU2718723C1 (en) | Sintering method in discharge plasma for making composite with metal matrix reinforced with single-wall carbon nanotubes, and composite material obtained by such method | |
| CN107722617A (en) | The selective laser sintering powder material preparation method of polyamide 46 | |
| CN102127713A (en) | Oxide dispersion-strengthening ferrite steel with bicrystal structure and production method thereof | |
| CN108659529A (en) | A kind of laser sintered preparation method with polyamide short fibre composite material | |
| CN105949754A (en) | Low-melting-point and low-crystallinity nylon 6 powder for SLS (Selective Laser Sintering) and preparation method of nylon 6 powder | |
| CN105418913A (en) | Process for producing nylon 6 chip for ultra-low-viscosity high-flow engineering plastics | |
| CN109929242A (en) | A kind of nylon polymer powder heat-absorbing material and preparation method thereof | |
| CN104046828A (en) | High energy ball milling process-containing preparation method for nanometer multi-element composite crystal grain growth inhibitor | |
| CN102950289B (en) | Method for producing nanoscale copper-manganese alloy powder | |
| CN115194152A (en) | Preparation method of porous Ni-Mn-Ga shape memory alloy | |
| CN108164730A (en) | A kind of Polywoven Bag of high tensile load | |
| CN108610540A (en) | The method of production of the degradable bubble chamber film of fire resistant antistatic wear-proof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CP01 | Change in the name or title of a patent holder | ||
| CP01 | Change in the name or title of a patent holder |
Address after: No. 181, Linyu Road, national high tech Industrial Development Zone, Changsha City, Hunan Province, 410205 Patentee after: Hunan Huashu High Tech Co.,Ltd. Address before: No. 181, Linyu Road, national high tech Industrial Development Zone, Changsha City, Hunan Province, 410205 Patentee before: HUNAN FARSOON HIGH-TECH Co.,Ltd. |