CN102140246A - Method for preparing nylon powder for selective laser sintering - Google Patents
Method for preparing nylon powder for selective laser sintering Download PDFInfo
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- CN102140246A CN102140246A CN2010105975298A CN201010597529A CN102140246A CN 102140246 A CN102140246 A CN 102140246A CN 2010105975298 A CN2010105975298 A CN 2010105975298A CN 201010597529 A CN201010597529 A CN 201010597529A CN 102140246 A CN102140246 A CN 102140246A
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- nylon powder
- laser sintering
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Abstract
The invention provides a method for preparing nylon powder for selective laser sintering. The method is used for preparing nylon powder materials by steps of heat treatment, powder preparation in a solvent method, addition of an appropriate addition agent and the like, wherein the nylon powder materials have excellent performances and can be effectively applied to a selective laser sintering (SLS for short) process for preparing SLS pieces. The method has simple and convenient process, is environmental friendly and is easy to implement.
Description
Technical field
The present invention relates to a kind of method for preparing nylon powder, relate in particular to a kind of method for preparing selective laser sintering with nylon powder.
Background technology
Selective laser sintering (Selective Laser Sintering, be called for short SLS) be one of present widely used rapid shaping technique, it is raw material with the pressed powder, adopt layering-superposition theorem directly to make 3D solid from cad model, in theory, the powder that viscosity reduces during any heating can be as the SLS agglomerated material, and scope of selecting material extensively is that SLS technology can be widely used in one of the important factor in each field.Nylon is a kind of crystalline polymer, and its SLS product all has more excellent performance at aspects such as intensity, densityes, is a kind of macromolecular material that is suitable for very much SLS technology.Solvent precipitation be utilization at present more prepare one of method of nylon powder, be that nylon is dissolved in the suitable solvent, make material uniform distribution and cooling in solvent separate out Powdered precipitation by high degree of agitation.But the nylon powder of existing solvent precipitation preparation is based on the purposes of Nylon powder coating(s) and nylon injection-molding spare mostly, and SLS technology is to every demands for higher performance of powdered material.The nylon powder of existing method preparation is used for still existing when the SLS moulding is made many defectives, as powder particle shape and size distribution inadequately evenly, poor, the powdered material sintering window narrows of powder resistance toheat etc., existing nylon powder material is to sintering process and equipment requirements strictness, sintering temperature control is improper will to cause the fusing of sintering process powder to be difficult to control or parts owing to buckling deformation takes place internal stress, thereby influence the SLS parts quality.
Summary of the invention
The objective of the invention is to overcome the defective of prior art, a kind of method for preparing selective laser sintering with nylon powder is provided, easy, the easy enforcement of this method technology, the gained nylon powder can adapt to the SLS process requirements, the SLS product that manufacturing property is good.
A kind of selective laser sintering for preparing provided by the invention is with the method for nylon powder, is to be raw material with the nylon pellet, may further comprise the steps:
A, in certain solvent, under certain pressure, at a certain temperature, nylon pellet heat-insulation pressure keeping in high pressure vessel is stirred for some time, material is taken out carry out vacuum-drying then, obtain through heat treated nylon pellet;
B, the nylon pellet of a certain amount of steps A thermal treatment gained and crystallization auxiliary, solvent are added in the high pressure vessel, stirring, ultrasonic for some time under certain temperature and pressure, cooling decompression is separated out powder to normal temperature and pressure then, filtration, washing, drying obtain nylon powder;
C, step B gained nylon powder and flow promotor, oxidation inhibitor are mixed stirring according to a certain ratio, the back material that stirs sieves, and obtains a kind of selective laser sintering nylon powder.
Above-mentioned nylon pellet is selected from one or more in nylon 6, nylon 66, Ni Long11, nylon 12 or the nylon 1010.
Solvent among the above-mentioned steps A is a water, and described heat treated pressure is 0.5～2MPa, and temperature is 110～180 ℃, and the time is 1～7h, and the weight proportion of nylon pellet and solvent is 1: 5～1: 50.
Solvent among the above-mentioned steps B is selected from one or more among methyl alcohol, ethanol, DMF, the DMA, the ultransonic pressure of described stirring is 0.5～2MPa, described temperature is 150～200 ℃, the consumption of described crystallization auxiliary is 0.1%～0.5% of a nylon pellet weight, and the consumption of described solvent is 5～25 times of nylon pellet weight.
Among the above-mentioned steps C, the consumption of described flow promotor is 0.1%～1% of a nylon powder weight, and the consumption of described oxidation inhibitor is 0.1%～2% of a nylon powder weight.Flow promotor described in the above-mentioned steps C and oxidation inhibitor are this area common agents; Wherein flow promotor is preferably one or more in nano carborundum powder, nano silicon, nano aluminium oxide and the nano-titanium oxide; Oxidation inhibitor is preferably the composite antioxidant of Hinered phenols antioxidant and phosphite ester kind antioxidant composition, wherein Hinered phenols antioxidant is preferably 1,3,5-trimethylammonium-2,4,6-three (3, the 5-di-tert-butyl-4-hydroxyl benzyl) benzene, 2,6-di-t-butyl-4-methyl-phenol, N, N '-two (3,5-di-tert-butyl-hydroxy phenyl propionic acid amide), 2,2 '-two (4-methyl-6-tert butyl-phenol) methane, 2,2 '-in two (the 4-ethyl-6-tertiary butyl-phenol) methane one or more, phosphite ester kind antioxidant is preferably 2,2 '-ethylenebis (4, the 6-di-tert-butyl-phenyl) fluorophosphite, four (2, the 4-di-tert-butyl-phenyl)-4,4 '-in the xenyl bis-phosphite one or more.
The solvent that relates among steps A and the B all can carry out recycle and reuse after use, operation employing public technology known in this field such as the heating that the present invention relates to, pressurization, stirring, mixed, drying, screening.The technical scheme that reaches the object of the invention according to content disclosed by the invention all belongs to scope of the present invention.
Technology of the present invention is easy, environmental friendliness, implement easily, adopt method provided by the invention can obtain having the nylon powder of good physicochemical property, compare with original nylon powder, the nylon powder particle form and the good fluidity of the present invention's preparation, possessed better resistance toheat and bigger sintering window simultaneously, the thermostability of material, SLS sintering precision etc. has obtained effective improvement, the product that the nylon powder material that adopts the present invention to prepare obtains through the SLS moulding possesses good physicochemical property, mechanical property and visual appearance can satisfy aviation, automobile, medicine equipment, electronic machine, machine die, the SLS product demand in fields such as artwork.
Embodiment
Embodiment 1
100g nylon 12 pellets and 1000g water are added in the reactor, be forced into 0.8MPa, temperature rises to 120 ℃, stirs 5h, material is taken out carry out vacuum-drying then, obtains through heat treated nylon pellet;
80g is added in the reactor through nylon pellet, 0.1g crystallization auxiliary, the 2000g DMF of thermal treatment gained, be forced into 0.8MPa, be warming up to 160 ℃, stirring, ultrasonic 1h are uniformly dispersed material, cooling decompression is to normal temperature and pressure then, separate out powder, filtration, washing, drying obtain nylon powder;
Get step gained nylon powder 50g, and flow promotor 0.1g, oxidation inhibitor 0.1g, in vertical stirrer, stirring mixed 1h, 150 mesh sieves are crossed in the mixed evenly back of material, obtain being used for the nylon powder of selective laser sintering.
Embodiment 2
500g nylon 12 pellets and 2500g water are added in the reactor, be forced into 1.5MPa, temperature rises to 130 ℃, stirs 4h, material is taken out carry out vacuum-drying then, obtains through heat treated nylon pellet;
300g is added in the reactor through nylon pellet, 0.5g crystallization auxiliary, the 3000g DMA of thermal treatment gained, be forced into 1MPa, be warming up to 170 ℃, stirring, ultrasonic 2h are uniformly dispersed material, and cooling decompression is separated out powder to normal temperature and pressure then, filtration, washing, drying obtain nylon powder;
Get step gained nylon powder 200g, and flow promotor 0.2g, oxidation inhibitor 0.5g, in vertical stirrer, stirring mixed 1h, 150 mesh sieves are crossed in the mixed evenly back of material, obtain being used for the nylon powder of selective laser sintering.
Claims (10)
1. a kind of selective laser sintering for preparing provided by the invention is with the method for nylon powder, is to be raw material with the nylon pellet, it is characterized in that may further comprise the steps:
A, in certain solvent, under certain pressure, at a certain temperature, nylon pellet heat-insulation pressure keeping in high pressure vessel is stirred for some time, material is taken out carry out vacuum-drying then, obtain through heat treated nylon pellet;
B, the nylon pellet of a certain amount of steps A thermal treatment gained and crystallization auxiliary, solvent are added in the high pressure vessel, stirring, ultrasonic for some time under certain temperature and pressure, cooling decompression is separated out powder to normal temperature and pressure then, filtration, washing, drying obtain nylon powder;
C, step B gained nylon powder and flow promotor, oxidation inhibitor are mixed according to a certain ratio, mixed evenly back screening obtains a kind of selective laser sintering nylon powder.
2. a kind of method for preparing selective laser sintering with nylon powder according to claim 1 is characterized in that described nylon pellet is selected from one or more in nylon 6, nylon 66, Ni Long11, nylon 12 or the nylon 1010.
3. a kind of method for preparing selective laser sintering with nylon powder according to claim 1 is characterized in that the solvent in the described steps A is a water, and the weight proportion of nylon pellet and solvent is 1: 5～1: 50.
4. a kind of method for preparing selective laser sintering with nylon powder according to claim 1 is characterized in that heat treated pressure is 0.5～2MPa in the described steps A, and temperature is 110～180 ℃, and the time is 1～7h.
5. a kind of method for preparing selective laser sintering with nylon powder according to claim 1, it is characterized in that solvent among the described step B is selected from one or more among methyl alcohol, ethanol, DMF, the DMA, the consumption of solvent is 5～25 times of nylon pellet weight.
6. a kind of method for preparing selective laser sintering with nylon powder according to claim 1 is characterized in that stirring ultransonic pressure among the described step B is 0.5～2MPa, and temperature is 150～250 ℃.
7. a kind of method for preparing selective laser sintering with nylon powder according to claim 1, the consumption that it is characterized in that crystallization auxiliary among the described step B is 0.1%～0.5% of a nylon pellet weight.
8. a kind of method for preparing selective laser sintering with nylon powder according to claim 1, the consumption that it is characterized in that the flow promotor among the described step C is 0.1%～1% of a nylon powder weight, and the consumption of described oxidation inhibitor is 0.1%～2% of a nylon powder weight.
9. according to claim 1 or 8 described a kind of methods that prepare selective laser sintering with nylon powder, it is characterized in that flow promotor described in the described step C is preferably one or more in nano carborundum powder, nano silicon, nano aluminium oxide and the nano-titanium oxide.
According to claim 1 or 8 described a kind of selective laser sinterings that prepare with the methods of nylon powder, it is characterized in that oxidation inhibitor among the described step C is preferably the composite antioxidant that Hinered phenols antioxidant and phosphite ester kind antioxidant are formed; Wherein Hinered phenols antioxidant is preferably 1,3,5-trimethylammonium-2,4,6-three (3, the 5-di-tert-butyl-4-hydroxyl benzyl) benzene, 2,6-di-t-butyl-4-methyl-phenol, N, N '-two (3,5-di-tert-butyl-hydroxy phenyl propionic acid amide), 2,2 '-two (4-methyl-6-tert butyl-phenol) methane, 2,2 '-in two (the 4-ethyl-6-tertiary butyl-phenol) methane one or more, phosphite ester kind antioxidant is preferably 2,2 '-ethylenebis (4, the 6-di-tert-butyl-phenyl) fluorophosphite, four (2, the 4-di-tert-butyl-phenyl)-4,4 '-in the xenyl bis-phosphite one or more.
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| CN2010105975298A CN102140246A (en) | 2010-12-21 | 2010-12-21 | Method for preparing nylon powder for selective laser sintering |
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| CN2010105975298A CN102140246A (en) | 2010-12-21 | 2010-12-21 | Method for preparing nylon powder for selective laser sintering |
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| CN105462244A (en) * | 2014-09-10 | 2016-04-06 | 中国科学院理化技术研究所 | Preparation method of carbon fiber reinforced nylon composite micro-powder for selective laser sintering |
| CN105585720A (en) * | 2014-10-24 | 2016-05-18 | 中国石油化工股份有限公司 | Polylactic resin powder for selective laser sintering and a preparation method thereof |
| CN105585717A (en) * | 2014-10-24 | 2016-05-18 | 中国石油化工股份有限公司 | Polycaprolactone resin powder for selective laser sintering and a preparation method thereof |
| CN105585719A (en) * | 2014-10-24 | 2016-05-18 | 中国石油化工股份有限公司 | Polypropylene resin powder for selective laser sintering and preparation method thereof |
| CN105754334A (en) * | 2016-04-06 | 2016-07-13 | 广东波斯科技股份有限公司 | Selective low-power laser sintered nylon powder and preparation method thereof |
| CN105860514A (en) * | 2016-05-11 | 2016-08-17 | 广东银禧科技股份有限公司 | Toughening material for SLS and preparation method of toughening material |
| CN106147220A (en) * | 2016-09-27 | 2016-11-23 | 广东银禧科技股份有限公司 | Long-chain nylon and nylon66 fiber alloy powder material preparation method for SLS |
| CN106243705A (en) * | 2016-09-27 | 2016-12-21 | 广东银禧科技股份有限公司 | Long-chain nylon and the alloy powder material preparation method of nylon 6 for SLS |
| CN106478964A (en) * | 2015-08-28 | 2017-03-08 | 比亚迪股份有限公司 | A kind of nylon powder and preparation method thereof and nylon composite materials |
| CN106589860A (en) * | 2015-10-13 | 2017-04-26 | 中国石油化工股份有限公司 | Polylactic acid resin powder for selective laser sintering as well as preparation method and application thereof |
| CN106674550A (en) * | 2015-11-06 | 2017-05-17 | 中国石油化工股份有限公司 | Polyethylene resin powder used for selective laser sintering and preparation method and application thereof |
| CN106674551A (en) * | 2015-11-06 | 2017-05-17 | 中国石油化工股份有限公司 | Antibacterial polycaprolactone resin powder used for selective laser sintering, and preparation method thereof |
| CN106675010A (en) * | 2015-11-06 | 2017-05-17 | 中国石油化工股份有限公司 | Nylon resin powder for selective laser sintering, and preparation method thereof |
| CN106674552A (en) * | 2015-11-06 | 2017-05-17 | 中国石油化工股份有限公司 | Polyformaldehyde resin powder used for selective laser sintering and preparation and application thereof |
| CN106700453A (en) * | 2015-11-06 | 2017-05-24 | 中国石油化工股份有限公司 | Glass fiber enhanced polycaprolactone resin powder for selective laser sintering and preparation of glass fiber enhanced polycaprolactone resin powder |
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| CN106751767A (en) * | 2015-11-24 | 2017-05-31 | 中国科学院理化技术研究所 | A kind of selective laser sintering nylon alloy composite micro-powder and preparation method thereof |
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| CN109291302A (en) * | 2018-09-21 | 2019-02-01 | 中国科学院重庆绿色智能技术研究院 | A kind of semi-crystalline polymer powder sintering window widens method |
| 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 |
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