CN105566902B - A kind of selective laser sintering nylon powder preparation method - Google Patents
A kind of selective laser sintering nylon powder preparation method Download PDFInfo
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- CN105566902B CN105566902B CN201610097283.5A CN201610097283A CN105566902B CN 105566902 B CN105566902 B CN 105566902B CN 201610097283 A CN201610097283 A CN 201610097283A CN 105566902 B CN105566902 B CN 105566902B
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- laser sintering
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- nylon powder
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
- C08L77/06—Polyamides derived from polyamines and polycarboxylic acids
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- 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
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- 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
- C08G69/30—Solid state polycondensation
Abstract
The invention discloses a kind of selective laser sintering nylon powder preparation methods.The stability of the fusing point of nylon powder material made from this method is high, greatly improves the quality and performance of selective laser sintering product.Method of the invention mainly comprises the steps that enough binary acid, diamine and ethyl alcohol are put into reaction vessel by (1), and reacted obtained nylon salt solution, centrifugal filtration obtains copolymer nylon salt；(2) obtained nylon salt is placed in microwave drying instrument under the conditions of 30 ~ 40 DEG C of temperature dry 10-30min, the dry nylon salt that obtains that treated；(3) dry nylon salt, molecular weight regulator, deionized water are added in closed polymerization reaction kettle, obtain copolymer nylon pellet through copolyreaction；(4) copolymer nylon powder is made by solvent precipitation in the copolymer nylon pellet prepared；(5) copolymer nylon powder, flow promortor, antioxidant are mixed again, obtains a kind of selective laser sintering nylon powder.
Description
Technical field
The present invention provides a kind of nylon powder preparation method, and in particular to a kind of selective laser sintering nylon powder system
Preparation Method.
Background technique
Selective Laser Sintering (Selective Laser Sintering) be at present it is a kind of be widely used it is fast
Fast forming technique, moulding process principle is: the electronic 3-D model of target part is initially set up, it then will with delamination software
Threedimensional model carries out slicing treatment, obtains the data information of each processing level, under the control of the computer, according to slice level
Information successively scans sintering to heat-fusible dusty material using laser beam, is finally completed the processing and manufacturing of target part.Selection
The property applicable material ranges of laser sintering technology are very wide, including polymer, metal and ceramics etc..
In selective laser sintering technique, dusty material is the key factor for influencing part performance.Due to polymeric material
Material has many advantages, such as that forming temperature is low, sintering power is small compared with metal and ceramic material, thus most as application at present
Selective laser sintering material.Nylon-based resin material is a kind of semi-crystalline polymer, have good sintering character and compared with
Low melt viscosity, can, mechanical property preferable function part higher by Selective Laser Sintering straight forming consistency,
One of moulding material as the selective laser sintering technique being most widely used at present.But selective laser sintering technique is wanted
Its agglomerated material performance is asked to stablize, the especially stability of material melting point, stable fusing point advantageously reduces to be generated when sintering
Viscous powder and warpage issues, to improve the quality of selective laser sintering product.And influence the pass of nylon material fusing point stability
Key factor is the control after copolymer nylon salt is prepared, to the humidity size of nylon salt, and nylon salt humid control is being closed
The stability of the fusing point of nylon powder material can be greatly improved in the range of reason.Nylon is reduced using seasoning in the prior art
Salt humidity, but by the dry nylon salt of common or vacuum oven, often it is merely able to dry nylon salt surface, drying efficiency
It is low, and drying process is it is easier that nylon salt flavescence and agglomeration, can change the color of nylon salt, and then affect the property of sintered part
Can, in addition, more by dissolvent residual in the common or nylon salt of vacuum drying treatment, it is difficult to recycle, cause to waste.
Summary of the invention
The present invention solve the problems, such as deficiency present in above-mentioned technology and, provide a kind of selective laser sintering nylon
The fusing point stability of the preparation method of powder, nylon powder material made from this method is greatly improved, so as to pole
The earth improves the quality and performance of selective laser sintering product, while the preparation method greatly improves nylon powder material
Preparation efficiency and solvent the rate of recovery.
A kind of selective laser sintering nylon powder preparation method, which comprises the following steps:
(1) enough binary acid, diamine and ethyl alcohol are put into reaction vessel, reacted obtained nylon salt solution, from
Copolymer nylon salt is obtained by filtration in the heart；
(2) obtained nylon salt is placed in microwave drying instrument dry 10-30min under the conditions of 30 ~ 40 DEG C of temperature, obtained
The dry nylon salt to treated；
(3) dry nylon salt, molecular weight regulator, deionized water are added in closed polymerization reaction kettle, it is anti-through being copolymerized
It should obtain copolymer nylon pellet；
(4) copolymer nylon powder is made by solvent precipitation in the copolymer nylon pellet prepared；
(5) copolymer nylon powder, flow promortor, antioxidant are mixed again, obtains a kind of selective laser sintering and uses Buddhist nun
Imperial powder.
Further, the binary acid be adipic acid, decanedioic acid, 11 carbon diacid, dodecanedioic acid, hendecane dicarboxylic acid,
One or more of 14 carbon diacid.
Further, the diamine be hexamethylene diamine, decamethylene diamine, 11 carbon diamines, 12 carbon diamines, 13 carbon diamines,
One or more of 14 carbon diamines.
Further, the nylon salt humidity being dried to obtain in the step (2) is 0.1 ~ 5.0%.
Further, the molecular weight regulator in the step (3) is adipic acid, decanedioic acid, 11 carbon diacid, 12 carbon
One or more of diacid, hendecane dicarboxylic acid, 14 carbon diacid.
Further, the antioxidant in the step (5) is Hinered phenols antioxidant and phosphite ester antioxidant group
At composite antioxidant.
Further, the Hinered phenols antioxidant is preferably 1,3,5- trimethyls -2,4, (3, the 5- di-t-butyls-of 6- tri-
4- hydroxybenzyl) benzene, one of 2,6- di-t-butyl -4- methyl-phenol.
Further, the phosphite ester antioxidant is preferably that bis- (4, the 6- di-tert-butyl-phenyl) fluoro of 2 '-ethyls are sub-
One of phosphate, four (2,4- di-tert-butyl-phenyl) -4,4 '-xenyl bis-phosphites.
Compared with prior art the invention has the following advantages:
The present invention handles nylon salt using micro-wave drying method, and the humidity for the nylon salt being dried to obtain is 0.1 ~ 5.0%, dry
When dry, microwave energy directly acts on medium molecule and is converted to thermal energy, since there is microwave penetration performance to make inside and outside medium simultaneously
Heating has saved the time so heating speed is fast without heat transfer, has greatly improved the drying efficiency of nylon salt, in addition,
Due to heating simultaneously inside and outside medium, medium internal-external temperature difference is small, is heated evenly, and is not in shape scorched outside and underdone inside in conventional heating
Condition, the nylon salt after drying will not turn yellow, and pH value will not change, so that dry mass greatly improves, and do
Dry obtained solvent can recycle again, improve the rate of recovery of solvent, saved cost.It is placed in microwave drying instrument
In, in 30 ~ 40 DEG C of conditions, the phenomenon that both having eliminated the solvent in nylon salt, and also nylon salt avoided to turn to be yellow, treated Buddhist nun
Imperial salt can accurately obtain nylon salt dry weight, and the fusing point for matching the nylon pellet of preparation is stablized, and considerably reduce time of product
Product rate improves the quality of sintered part.
Specific embodiment
In order to enable those skilled in the art more fully understands and realizes technical solution of the present invention, below in conjunction with specific
Embodiment is described in further details.
A kind of selective laser sintering nylon powder preparation method, which comprises the following steps:
1) enough binary acid, diamine and ethyl alcohol are put into reaction vessel, reacted obtained nylon salt solution, are centrifuged
Copolymer nylon salt is obtained by filtration, the binary acid is adipic acid, decanedioic acid, 11 carbon diacid, dodecanedioic acid, 13 carbon two
Acid, one or more of 14 carbon diacid, the diamine be hexamethylene diamine, decamethylene diamine, 11 carbon diamines, 12 carbon diamines,
One or more of 13 carbon diamines, 14 carbon diamines；
2) obtained nylon salt is placed in microwave drying instrument dry 10-30min under the conditions of 30 ~ 40 DEG C of temperature, obtained
The dry nylon salt to treated, the nylon salt humidity being dried to obtain are 0.1 ~ 5.0%；
3) dry nylon salt, molecular weight regulator, deionized water are added in closed polymerization reaction kettle, through copolyreaction
Copolymer nylon pellet is obtained, the molecular weight regulator is adipic acid, decanedioic acid, 11 carbon diacid, dodecanedioic acid, 13 carbon
One or more of diacid, 14 carbon diacid；
4) copolymer nylon powder is made by solvent precipitation in the copolymer nylon pellet prepared, is used in the step
Solvent is one kind of methanol, ethyl alcohol, ethylene glycol；
5) copolymer nylon powder, flow promortor, antioxidant are mixed again, obtains a kind of selective laser sintering nylon
Powder, the antioxidant is the composite antioxidant of Hinered phenols antioxidant and phosphite ester antioxidant composition, described to be obstructed
Phenolic antioxidant is preferably 1,3,5- trimethyls -2,4,6- tri- (3,5- di-tert-butyl-4-hydroxyl benzyl) benzene, the tertiary fourth of 2,6- bis-
One of base -4- methyl-phenol, the phosphite ester antioxidant are preferably that 2 '-ethyls are bis- (4,6- di-tert-butyl-phenyl)
One of fluorophosphite, four (2,4- di-tert-butyl-phenyl) -4,4 '-xenyl bis-phosphites.
Embodiment 1
Dodecanedioic acid 6.9Kg, 12 carbon diamines 5.16Kg and 9.6Kg ethyl alcohol are added in reactor, at 75 DEG C
Copolymer nylon salting liquid is generated, centrifugal filtration obtains nylon 1212 salt；
Nylon salt obtained above is placed in microwave drying instrument dry 10min under the conditions of 40 DEG C, after being dried
Nylon salt, the nylon salt humidity being dried to obtain be 0.1%；
Copolymer nylon salt, molecular weight regulator, deionized water are added in polymeric kettle.It is closed, it vacuumizes, then passes to
Carbon-dioxide protecting gas 0.15MPa.200 DEG C are warming up to, pressure reaches 1.2MPa, pressure maintaining 3 hours, is then slowly deflated to often
Pressure is warming up to 245 DEG C of holdings and reacts 3 hours, stops heating, the cooling tie rod discharging of water, and pelletizing obtains copolymer nylon 1212
Material.Then 1212 pellet of copolymer nylon prepared is added in polymerization reaction kettle, DMF solvent is added, in the pressure of 1.6MPa
It is stirred at a temperature of power and 165 DEG C, then cooling decompression to room temperature normal pressure, powder is precipitated, centrifugal filtration obtains copolymerization powder；Again will
Obtained 1212 powder of copolymer nylon is mixed with flow promortor, antioxidant by 1:0.008:0.01 proportion, is sieved after mixing
Point, obtain a kind of selective laser sintering nylon 1212 poweder.
Embodiment 2
Dodecanedioic acid 6.9Kg, 12 carbon diamines 5.16Kg and 9.6Kg ethyl alcohol are added in reactor, at 75 DEG C
Copolymer nylon salting liquid is generated, centrifugal filtration obtains nylon 1212 salt；
Nylon salt obtained above is placed in microwave drying instrument dry 25min under the conditions of 35 DEG C, after being dried
Nylon salt, the nylon salt humidity being dried to obtain be 5%；
Copolymer nylon salt, molecular weight regulator, deionized water are added in polymeric kettle.It is closed, it vacuumizes, then passes to
Carbon-dioxide protecting gas 0.12MPa.220 DEG C are warming up to, pressure reaches 1.5MPa, pressure maintaining 2 hours, is then slowly deflated to often
Pressure is warming up to 260 DEG C of holdings and reacts 2 hours, stops heating, the cooling tie rod discharging of water, and pelletizing obtains copolymer nylon 1212
Material.Then 1212 pellet of copolymer nylon prepared is added in polymerization reaction kettle, DMF solvent is added, in the pressure of 1.6MPa
It is stirred at a temperature of power and 165 DEG C, then cooling decompression to room temperature normal pressure, powder is precipitated, centrifugal filtration obtains copolymerization powder；Again will
Obtained 1212 powder of copolymer nylon is mixed with flow promortor, antioxidant by 1:0.008:0.01 proportion, is sieved after mixing
Point, obtain a kind of selective laser sintering nylon 1212 poweder.
Embodiment 3
Dodecanedioic acid 6.9Kg, 12 carbon diamines 5.16Kg and 9.6Kg ethyl alcohol are added in reactor, at 75 DEG C
Copolymer nylon salting liquid is generated, centrifugal filtration obtains nylon 1212 salt；
Nylon salt obtained above is placed in microwave drying instrument dry 30min under the conditions of 30 DEG C, after being dried
Nylon salt, the nylon salt humidity being dried to obtain be 2.45%；
Copolymer nylon salt, molecular weight regulator, deionized water are added in polymeric kettle.It is closed, it vacuumizes, then passes to
Carbon-dioxide protecting gas 0.1MPa.240 DEG C are warming up to, pressure reaches 1.8MPa, pressure maintaining 1 hour, it is then slowly deflated to normal pressure,
It is warming up to 270 DEG C of holdings and reacts 1 hour, stop heating, the cooling tie rod discharging of water, pelletizing obtains 1212 pellet of copolymer nylon.
Then 1212 pellet of copolymer nylon prepared is added in polymerization reaction kettle, be added DMF solvent, 1.6MPa pressure and
It is stirred at a temperature of 165 DEG C, then cooling decompression to room temperature normal pressure, powder is precipitated, centrifugal filtration obtains copolymerization powder；It will obtain again
1212 powder of copolymer nylon and flow promortor, antioxidant mixed by 1:0.008:0.01 proportion, sieve, obtain after mixing
To a kind of selective laser sintering nylon 1212 poweder, the stability of obtained melting point is tested, fusing point is obtained
Fluctuation range, powder brightness results be shown in Table 1.
Following table is the nylon 1212 poweder as made from existing method and nylon 1212 powder obtained by the method for the invention
The fusing point fluctuation range at end, the comparison of powder whiteness:
Table 1
Claims (5)
1. a kind of selective laser sintering nylon powder preparation method, which comprises the following steps:
1) enough dodecanedioic acids, 12 carbon diamines and ethyl alcohol are put into reaction vessel, reacted obtained nylon salt solution,
Centrifugal filtration obtains copolymer nylon salt；
2) obtained nylon salt is placed in microwave drying instrument dry 10-30min under the conditions of 30 ~ 40 DEG C of temperature, obtained everywhere
Drying nylon salt after reason；
3) dry nylon salt, molecular weight regulator, deionized water are added in closed polymerization reaction kettle, are obtained through copolyreaction
Copolymer nylon pellet；
4) copolymer nylon powder is made by solvent precipitation in the copolymer nylon pellet prepared；
5) copolymer nylon powder, flow promortor, antioxidant are mixed again, obtains a kind of selective laser sintering nylon powder
End, wherein
The nylon salt humidity being dried to obtain in the step 2 is 0.1 ~ 5.0%.
2. a kind of selective laser sintering nylon powder preparation method according to claim 1, which is characterized in that institute
Stating the molecular weight regulator in step 3) is adipic acid, decanedioic acid, 11 carbon diacid, dodecanedioic acid, hendecane dicarboxylic acid, 14
One or more of carbon diacid.
3. a kind of selective laser sintering nylon powder preparation method according to claim 1, which is characterized in that institute
Stating the antioxidant in step 5) is Hinered phenols antioxidant and the composite antioxidant that phosphite ester antioxidant forms.
4. a kind of selective laser sintering nylon powder preparation method according to claim 3, which is characterized in that institute
Stating Hinered phenols antioxidant is 1,3,5- trimethyls -2,4,6- tri- (3,5- di-tert-butyl-4-hydroxyl benzyl) benzene, the tertiary fourth of 2,6- bis-
One of base -4- methyl-phenol.
5. a kind of selective laser sintering nylon powder preparation method according to claim 3, which is characterized in that institute
Stating phosphite ester antioxidant is bis- (4, the 6- di-tert-butyl-phenyl) fluorophosphites of 2 '-ethyls, four (2,4- di-t-butyls
One of phenyl) -4,4 '-xenyl bis-phosphites.
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| CN108395530B (en) * | 2017-02-06 | 2021-12-31 | 中国石油化工股份有限公司 | Method for preparing nylon powder for selective laser sintering based on reversed phase suspension polymerization method |
| CN107337792B (en) * | 2017-07-28 | 2021-07-02 | 湖南华曙高科技有限责任公司 | Melting point-controllable copolymerized nylon powder material and preparation method thereof |
| CN107446130B (en) * | 2017-09-08 | 2020-07-07 | 中央军委后勤保障部军需装备研究所 | Nylon 126 and preparation method thereof |
| CN109517370B (en) * | 2018-09-10 | 2021-07-02 | 湖南华曙高科技有限责任公司 | Preparation method of nylon powder material for selective laser sintering |
| CN109320716B (en) * | 2018-09-10 | 2021-12-10 | 湖南华曙高科技有限责任公司 | Preparation method of nylon powder material applied to selective laser sintering |
| CN111040434A (en) * | 2019-12-30 | 2020-04-21 | 湖南华曙高科技有限责任公司 | Graphene reinforced nylon powder for selective laser sintering and preparation method thereof |
| CN111040444A (en) * | 2019-12-31 | 2020-04-21 | 湖南华曙高科技有限责任公司 | Nylon powder for selective laser sintering and preparation method thereof |
| CN112126086B (en) * | 2020-08-06 | 2022-08-16 | 湖南华曙高科技股份有限公司 | Drying method of nylon powder suspension for selective laser sintering |
| CN111995773B (en) * | 2020-08-06 | 2022-07-05 | 湖南华曙高科技股份有限公司 | Method for drying nylon powder suspension for selective laser sintering |
| CN113527668B (en) * | 2021-07-30 | 2023-04-18 | 会通新材料(上海)有限公司 | Long-chain polyamide and preparation method and application thereof |
| CN115873240A (en) * | 2021-09-29 | 2023-03-31 | 万华化学集团股份有限公司 | Nylon powder for 3D printing with high reuse rate |
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