CN105694068B - A kind of polyamide powder and preparation method thereof - Google Patents

A kind of polyamide powder and preparation method thereof Download PDF

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CN105694068B
CN105694068B CN201610253524.0A CN201610253524A CN105694068B CN 105694068 B CN105694068 B CN 105694068B CN 201610253524 A CN201610253524 A CN 201610253524A CN 105694068 B CN105694068 B CN 105694068B
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polyamide
powder
precipitation
temperature
polyamide powder
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CN105694068A (en
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傅轶
洪浩然
王雁国
黄志轩
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GUANGDONG SILVERAGE HOLDINGS Ltd
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00Processes of treating or compounding macromolecular substances
    • C08J3/12Powdering or granulating
    • C08J3/14Powdering or granulating by precipitation from solutions
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/34Silicon-containing compounds
    • C08K3/36Silica
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L77/00Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
    • C08L77/02Polyamides derived from omega-amino carboxylic acids or from lactams thereof
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2377/00Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
    • C08J2377/02Polyamides derived from omega-amino carboxylic acids or from lactams thereof
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2377/00Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
    • C08J2377/06Polyamides derived from polyamines and polycarboxylic acids
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • C08K2003/2237Oxides; Hydroxides of metals of titanium
    • C08K2003/2241Titanium dioxide
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/24Crystallisation aids

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  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Processes Of Treating Macromolecular Substances (AREA)
  • Polyamides (AREA)

Abstract

The present invention relates to polyamide preparing technical field, and in particular to a kind of polyamide powder and preparation method thereof, the preparation method comprises the following steps:Dissolving insulation:Polyamides amine solvent is added in reactor, is heated to higher than polyamide temperature Precipitation Temperature 25 80 DEG C;Cooling powder processed:14 16 DEG C higher than polyamide powder Precipitation Temperature of temperature is cooled to 0.5 2.0 DEG C/min speed, then the Precipitation Temperature of polyamide powder is cooled to 0.1 0.4 DEG C/min speed, the last speed with 15 DEG C/min is cooled to room temperature, and precipitation obtains polyamide precipitation;Dry:Polyamide precipitation precipitation is dried and obtains polyamide powder particle.Polyamide powder particle size concentration degree produced by the present invention is good, and technique is easy, and the technological requirement for the SLS that is particularly suitable for use in, part performance is excellent.

Description

A kind of polyamide powder and preparation method thereof
Technical field
The present invention relates to polyamide preparing technical field, and in particular to a kind of polyamide powder and preparation method thereof.
Background technology
Polyamide is also commonly called as nylon, and it is the general name of the high polymer containing amide group in macromolecular main chain repeat unit. Nylon is widely used in machinery, automobile, electrical equipment, textile equipment, chemical industry equipment, aviation, metallurgy etc. as the engineering plastics of big consumption Field, as indispensable structural material in every profession and trade, its main feature is as follows:1st, excellent mechanical property:The machine of nylon Tool intensity is high, good toughness;2nd, self-lubricity, rub resistance are good:Nylon has good self-lubricity, and coefficient of friction is small, so that, as Its service life of drive disk assembly is long;3rd, excellent heat resistance:The heat distortion temperature of such as nylon 46 high crystalline nylon is very high, can The long-term phase uses at 150 DEG C, and PA66 is after glass fiber reinforcement, and its heat distortion temperature reaches more than 250 DEG C;4th, it is excellent Electrical insulation capability:The volume resistance of nylon is very high, breakdown voltage resistant height, is excellent electric, electrical apparatus insulation material;5th, it is excellent Against weather;6th, water imbibition:Nylon water imbibition is big, and saturation water can reach more than 3%.Product can also be being influenceed to a certain degree Dimensional stability.
Selective laser sintering(SLS)It is that the energy is made using infrared laser, the Modeling Material used mostly dusty material, It is mainly used in working of plastics, casting wax-pattern, exemplar or model.SLS is a kind of 3D printing technique emerging recently.Polyamide is one Crystalline polymer is planted, all there is more excellent performance in terms of intensity, consistency using SLS products made from polyamide, It is a kind of high polymer material for being highly suitable for SLS techniques.
Solvent precipitation is to prepare one of method of nylon powder with more at present, is to be dissolved in nylon suitably In solvent, material is uniformly distributed in a solvent by high degree of agitation and cool down the powdered precipitation of precipitation.Existing solvent precipitation The nylon powder of preparation is the purposes based on Nylon powder coating and rotational moulding mostly, and SLS technologies to the pattern of nylon powder and Particle diameter proposes higher requirement, if powder morphology is poor, and powder powdering effect can be caused in selective laser sintering process It is poor so that powdering out-of-flatness, crack, so as to cause the shaping of sintering product bad.Nylon powder prepared by existing method End is used for SLS shaping manufactures and still suffers from many defects, such as:Powder particle shape is irregular(Such as various special-shaped particles), powder grain Footpath size differs, and powder diameter is distributed too wide and powdered heat-resistant difference etc..So as to influence the rough surface of SLS molded articles Powder removes powdering effect in easy degree and SLS process etc. outside degree, compact dimensions precision, product.
Nylon powder prepared by existing method is in order to be able to obtaining the powder particle of centralized particle diameter so as to suitable for SLS Sintering, generally requires to carry out sieve classification to powder, by the smaller particle in powder(Grain diameter is below 20 microns)And compared with Bulky grain(Grain diameter is more than 80 microns)Remove.And in order to make up asking for the irregular caused poor fluidity of powder particle Topic is, it is necessary to add substantial amounts of flow promortor, to obtain powdering effect preferable in SLS sintering processes.Either in solvent method A certain amount of butanone is added in pulverizing process, so that powder particle regular appearance, with preferable sphericity, but butanone Addition can damage the antioxidant effect of material again, powder can be made to turn yellow, and part performance is deteriorated.
The content of the invention
In order to overcome shortcoming and defect present in prior art, it is an object of the invention to provide a kind of polyamide powder Preparation method, the polyamide powder particle good sphericity obtained using the preparation method, powder particle size concentration degree is good, work Skill is easy, and the technological requirement for the SLS that is particularly suitable for use in, part performance is excellent.
The present invention another goal of the invention be to provide a kind of polyamide powder, the polyamide powder particle good sphericity, Powder particle size concentration degree is good, and the technological requirement for the SLS that is particularly suitable for use in, part performance is excellent.
The purpose of the present invention is achieved through the following technical solutions:
A kind of preparation method of polyamide powder, comprises the following steps:
Dissolving insulation:Polyamides amine solvent is added in reactor, is heated to higher than polyamide temperature Precipitation Temperature 25-80℃;
Three sections of cooling powder processed:
First stage:Temperature of high 20-30 DEG C than polyamide powder Precipitation Temperature is cooled to 0.5-2.0 DEG C/min speed Degree;
Second stage:The Precipitation Temperature of polyamide powder is cooled to 0.1-0.4 DEG C/min speed;
Phase III:The last speed with 1-5 DEG C/min is cooled to room temperature, separates out polyamide precipitation.
The rate of temperature fall of three phases must be strict controlled in certain scope, the polyamide powder obtained beyond the scope Sphericity do not reach the present invention effect.
The Precipitation Temperature of polyamide powder can be measured by conventional method, then carry out three further according to its Precipitation Temperature The cooling powder in stage, obtained powder diameter is uniform, sphericity is high.
This processing step is related to the success of powder processed, the obtained dusty material beyond this temperature process scope, is difficult For the SLS techniques of 3D printing.
The particle diameter distribution that the present invention reaches a good powder particle sphericity using indirect cool-down method and relatively concentrated. If directly being cooled by inner chamber, it is difficult to have good sphericity and centralized particle diameter degree.
Dry:Polyamide precipitation precipitation is dried and obtains polyamide powder particle, can also be carried out before drying from The heart is filtered, and obtains Silon, and powder particle is obtained after drying.
Wherein, there is nitrogen protection in reactor in the dissolving incubation step, soaking time is 0.5-1.5 hours.Insulation Purpose in order that material fully dissolves at high temperature under high pressure, while can also have an impact to strand, improve polyamide powder Sphericity.
Wherein, the pressure in the dissolving incubation step in reactor is 0.8-1.2MPa, and pressure is to polyamide powder Forming degree effect has a significant effect, and simple to the Stress control technique in reactor, easily realizes.
Wherein, uniform stirring solution in reactor in the cooling pulverizing process, mixing speed is 100-1000r/min, Preferably 450-550r/min.Uniform stirring can make the temperature in reactor more uniform, and not interfere with polyamide Precipitation.
Wherein, using controlling the heat conduction oil temperature of reactor to reach temperature control purpose in cooling milling step.It is anti-by control Answer the heat conduction oil temperature of kettle to carry out temperature control, temperature in the kettle is more uniform, and polyamide is obtained in overall cooling in temperature-fall period The sphericity and uniform concentration degree of powder can be more preferable.
Wherein, in the dissolving incubation step, polyamide is dissolved using organic solvent, and organic solvent is alcohols solvent or acyl Amine solvent, preferably uses formamide, dimethylformamide.The mixed proportion of solvent and polyamide is molten according to conventional polyamide The ratio mixed solvent of agent method.
Wherein, the polyamide is PA6, PA11, PA12, PA66, PA610, PA612, PA1010, PA1012, PA1212 Any of.
Wherein, nucleation-accelerant can also be added in the dissolving incubation step, the powder contributed in powder precipitation process Particulate nucleation effect.
Wherein, the nucleation-accelerant is metal oxide, and the addition of nucleation-accelerant is the 0.1-2% of nylon addition, is entered One step is preferably 0.5-1%, and the addition of nucleation-accelerant can reduce the control requirement to rate of temperature fall technique in temperature-fall period, Production technology is easy to control, and product yield is higher, preferably uses titanium dioxide, molybdenum oxide.
Wherein, flow promortor, such as gas-phase silica, gaseous oxidation aluminium etc. can also be added, gas phase titanium dioxide is preferably used Silicon, makes the material good fluidity in reactor, is heated evenly, and Precipitation is more stablized, obtained polyamide sphericity it is high and The uniformity is more concentrated.Its addition is the 0.1-2%, more preferably 0.5-1% that polyamide powder adds quality.
A kind of polyamide powder that utilization above method is prepared, powder particle size is evenly distributed, and grain diameter is 40-60 μm or so, by laser particle size measurement, its D10 is more than 30 μm, and D50 is at 55-65 μm, and D75 is less than 80 μm.In reality Found in, identical nylon material, powder morphology is closer to spherical, and powder particle size is than more uniform, particle diameter distribution More concentrate, its powder flowbility is better, and bulk density is bigger, and apparent density of powder is higher, good fluidity, then part performance is got over Good, article surface is more smooth, and product dimensional accuracy is higher, and the removal of article surface powder is easier.The powder grain of the present invention Footpath distribution is an important parameter for examining dusty material performance, and can be directly connected to be smoothed out processing and processing product Global formation performance.
By the veneer of poly- phthalein amine powder on the level board in room, certain temperature is maintained, according to corresponding to article Geometry, laser makes the powder particle agglomeration in the difference of powder bed, such as by means of computer, and the computer is at it Memory in have article shape and the shape is restored in the form of thin slice.Then, the value pair for reducing the level board New powder bed should be then deposited in layer thickness, and the laser is according to the geometric form of the new thin slice corresponding to the article Shape makes powder particle agglomeration.The process is repeated to complete until prepared by whole article.
The article surrounded by polyamide powder is obtained in the chamber interior, therefore the part not being agglomerated keeps powder shape Formula.Then the assembly is leniently cooled down, after complete cooling, article is separated from powder, the powder can be used again In other operations, high recycling rate, and the sphericity of polyamide powder is better, and the uniformity is higher, obtained product accuracy Will be higher, polyamide powder of the invention passes through laser beam(That is selective laser sintering)Agglomeration process can prepare various three Tie up article, such as master mold and model, especially in automobile, ship, Aeronautics and Astronautics, medical science(Artificial limb, auditory system, cell tissue etc. Deng), in fabric, clothes, fashionable dress, decoration, the shell of electronics, phone, home automation, information technology and lighting field.
The beneficial effects of the present invention are:A kind of powder morphology for being used to improve polyamide powder that the present invention is provided is spherical The method of degree and powder particle size concentration degree, is, using nylon pellet as raw material, using solvent legal system powder, through dissolving, to cool, sink Form sediment and obtain the powder particle that sphericity height and grain size are concentrated.
The present invention utilizes indirect sublevel segmentation cool-down method, and obtained polyamide powder pattern sphericity is high, powder particle Size uniform, centralized particle diameter, therefore powder flowbility are good, and bulk density area is big, and apparent density is high, and part performance is good, Be particularly suitable for use in SLS techniques, and the accuracy of product is high, and powder is easily removed and recycled and reused after product.
The present invention another advantage is that:The polyamide powder particle size distribution of the present invention is uniform, grain diameter For 40-60 μm, by laser particle size measurement, its D10 is more than 30 μm, and D50 is at 55-65 μm, and D75 is less than 80 μm.
The polyamide powder pattern of the present invention is close to spherical, and powder particle size is uniform, centralized particle diameter, its powder Good fluidity, bulk density is big, and good fluidity, part performance is good, and article surface is smooth, and product dimensional accuracy is high, and product table Flour end, which is removed, to be easy for.
Brief description of the drawings
Fig. 1 is the granule-morphology figure that polyamide powder obtained by the embodiment of the present invention 1 amplifies 4 times under the microscope;
Fig. 2 is the granule-morphology figure that polyamide powder obtained by comparative example of the present invention amplifies 4 times under the microscope.
Embodiment
For the ease of the understanding of those skilled in the art, further is made to the present invention with reference to embodiment and accompanying drawing 1-2 Explanation, the content that embodiment is referred to not limitation of the invention.
Embodiment 1
A kind of preparation method of polyamide powder, comprises the following steps:
Dissolving insulation:The formamide of PA12 and 10 parts by volume of 1 parts by weight is added to the reaction of nitrogen protection In kettle, stirred with 500r/min speed, heat the mixture to 40 DEG C higher than PA12 powder Precipitation Temperatures and be incubated 1 hour, instead It is 1.0MPa to answer kettle pressure.
Cooling powder processed:125 DEG C are cooled to 0.5 DEG C/min speed, is then cooled to 0.18 DEG C/min speed 100 DEG C of PA12 Precipitation Temperatures, are finally cooled to room temperature with 2.8 DEG C/min speed, and precipitation obtains PA12 precipitations.
Dry:Polyamide is separated out to precipitate and centrifuged, be dried to obtain PA12 powder particles.The polyamide powder material of gained It is in that spherical particle, good sphericity, and particle be uniform, granularity is concentrated to expect powder particle, and grain diameter is 40-60 μm, by swashing Light granulometry, its D10 is 36.9 μm, and D25 is 48.7 μm, and D50 is 65.3 μm, and D75 is 80 μm, and D90 is 98.2 μm.
Embodiment 2
A kind of preparation method of polyamide powder, comprises the following steps:
Dissolving insulation:PA6 pellets, 1% titanium dioxide are added to the reactor of nitrogen protection using formyl amine solvent In, stirred with 450r/min speed, heat the mixture to 40 DEG C higher than PA6 powder Precipitation Temperatures and be incubated 0.5 hour, reaction Kettle pressure is 1.2MPa.
Cooling powder processed:Temperature of high 20 DEG C than PA6 powder Precipitation Temperatures is cooled to 0.5 DEG C/min speed, then with 0.4 DEG C/min speed is cooled to the Precipitation Temperature of PA6 powder, is finally cooled to room temperature with 5 DEG C/min speed, and precipitation is obtained PA6 is precipitated.
Dry:Polyamide is separated out to precipitate and centrifuged, be dried to obtain PA6 powder particles.The polyamide powder material of gained The pattern powder particle of material is in that spherical particle, good sphericity, and particle be uniform, granularity is concentrated, and grain diameter is a 40-60 μm of left side The right side, by laser particle size measurement, its D10 is 33.7 μm, and D25 is 43.9 μm, and D50 is 58.6 μm, and D75 is 77.2 μm, and D90 is 96.7μm。
Embodiment 3
A kind of preparation method of polyamide powder, comprises the following steps:
Dissolving insulation:PA11 pellets, 0.1% titanium dioxide, 1% aerosil are added using formyl amine solvent Into the reactor for thering is nitrogen to protect, stirred, heated the mixture to than PA11 powder Precipitation Temperatures with 500 r/min speed High 25 DEG C are incubated 1.5 hours, and reactor pressure is 0.8MPa.
Cooling powder processed:Temperature of high 20 DEG C than PA11 powder Precipitation Temperatures is cooled to 2.0 DEG C/min speed, then with 0.1 DEG C/min speed is cooled to the Precipitation Temperature of PA11 powder, is finally cooled to room temperature with 1 DEG C/min speed, separates out To PA11 precipitations.
Dry:Polyamide is separated out to precipitate and centrifuged, be dried to obtain PA11 powder particles.The polyamide powder material of gained The visible powder particle of pattern of material is in that spherical particle, good sphericity, and particle be uniform, granularity is concentrated, and grain diameter is 40-60 μm or so, by laser particle size measurement, its D10 is 33.5 μm, and D25 is 42.5 μm, and D50 is 56.2 μm, and D75 is 73.8 μm, D90 For 92.5 μm.
Embodiment 4
A kind of preparation method of polyamide powder, comprises the following steps:
Dissolving insulation:PA1012 pellets, 1% titanium dioxide are added to the anti-of nitrogen protection using formyl amine solvent Answer in kettle, stirred with 450r/min speed, heat the mixture to 80 DEG C of insulations 0.5 higher than PA1012 powder Precipitation Temperatures small When.
Cooling powder processed:Temperature of high 30 DEG C than PA6 powder Precipitation Temperatures is cooled to 0.5 DEG C/min speed, then with 0.4 DEG C/min speed is cooled to the Precipitation Temperature of PA1012 powder, is finally cooled to room temperature with 5 DEG C/min speed, separates out Obtain PA1012 precipitations.
Dry:Polyamide is separated out to precipitate and centrifuged, be dried to obtain PA1012 powder particles.The polyamide powder of gained The pattern of material is as described in Fig. 2, and visible powder particle is in that spherical particle, good sphericity, and particle be uniform, granularity collection in figure In, grain diameter is 40-60 μm, by laser particle size measurement, and its D10 is 35 μm, and D25 is 45 μm, and D50 is 57.1 μm, and D75 is 77.2 μm, D90 is 94.7 μm.
Embodiment 5
A kind of preparation method of polyamide powder, comprises the following steps:
Dissolving insulation:PA612 pellets, 1% titanium dioxide are added to the reaction of nitrogen protection using formyl amine solvent In kettle, stirred with 480r/min speed, heat the mixture to 60 DEG C higher than PA12 powder Precipitation Temperatures and be incubated 0.8 hour.
Cooling powder processed:Temperature of high 25 DEG C than PA6 powder Precipitation Temperatures is cooled to 1 DEG C/min speed, then with 0.2 DEG C/min speed is cooled to the Precipitation Temperature of PA612 powder, is finally cooled to room temperature with 2 DEG C/min speed, precipitation is obtained PA612 is precipitated.
Dry:Polyamide is separated out to precipitate and centrifuged, be dried to obtain PA612 powder particles.The polyamide powder of gained The pattern powder particle of material is in that spherical particle, good sphericity, and particle be uniform, granularity is concentrated, and grain diameter is 40-60 μm Left and right, by laser particle size measurement, its D10 is 34.1 μm, and D25 is 42.9 μm, and D50 is 56.8 μm, and D75 is 76.8 μm, and D90 is 94.6μm。
Embodiment 6
A kind of preparation method of polyamide powder, comprises the following steps:
Dissolving insulation:PA6 pellets, 1% titanium dioxide are added to the reactor of nitrogen protection using formyl amine solvent In, stirred with 450r/min speed, heat the mixture to 50 DEG C higher than PA6 powder Precipitation Temperatures and be incubated 0.5 hour.
Cooling powder processed:Temperature of high 28 DEG C than PA6 powder Precipitation Temperatures is cooled to 0.5 DEG C/min speed, then with 0.4 DEG C/min speed is cooled to the Precipitation Temperature of PA6 powder, is finally cooled to room temperature with 5 DEG C/min speed, and precipitation is obtained PA6 is precipitated.
Dry:Polyamide is separated out to precipitate and centrifuged, be dried to obtain PA6 powder particles.The polyamide powder material of gained The pattern powder particle of material is in that spherical particle, good sphericity, and particle be uniform, granularity is concentrated, and grain diameter is 40-60 μm, By laser particle size measurement, its D10 is 35.8 μm, and D25 is 45.7 μm, and D50 is 63.2 μm, and D75 is 79.3 μm, and D90 is 97.3 μ m。
Comparative example 1
In the reactor that the formyl amine solvent of PA12 and 10 parts by volume of 1 parts by weight is added to nitrogen protection, Stirred with 450r/min speed, heat the mixture to 150 DEG C and be incubated 0.5 hour.
Cooling powder processed:128 DEG C are cooled to 0.1 DEG C/min speed, then 100 are cooled to 0.5 DEG C/min speed DEG C, room temperature is finally cooled to 2.5 DEG C/min speed, precipitation obtains PA12 precipitations.
Dry:Polyamide is separated out to precipitate and centrifuged, be dried to obtain polyamide powder particle.The polyamide powder of gained The pattern powder of material is shown in that visible powder morphology is very poor in Fig. 2, figure, and powder particle is in irregular shape, and grain edges are very Coarse, fractionlet particle is more.While the particle diameter distribution measured by particle diameter distribution measuring instrument is shown, its little particle and bulky grain More, its D10 is 11.9 μm, and D25 is 22.6 μm, and D50 is 28.9 μm, and D75 is 57.6 μm, and D90 is 106.5 μm.
By contrast, the polyamide granules powder prepared by the present invention is shown in Fig. 1, and the visible powder particle of pattern is in spherical shape Grain, good sphericity, and particle are uniform, granularity is concentrated, and grain diameter is 40-60 μm.
Above-described embodiment is the present invention preferably implementation, and in addition, the present invention can be realized with other manner, Any obvious replacement is within protection scope of the present invention on the premise of not departing from present inventive concept.

Claims (6)

1. a kind of preparation method of polyamide powder, it is characterised in that:Comprise the following steps:
Dissolving insulation:Polyamides amine solvent is added in reactor, is heated to than the high 25-80 of polyamide temperature Precipitation Temperature ℃;
Three sections of cooling powder processed:
First stage:Temperature of high 20-30 DEG C than polyamide powder Precipitation Temperature is cooled to 0.5-2.0 DEG C/min speed;
Second stage:The Precipitation Temperature of polyamide powder is cooled to 0.1-0.4 DEG C/min speed;
Phase III:The last speed with 1-5 DEG C/min is cooled to room temperature, separates out polyamide precipitation;
Dry:Polyamide precipitation precipitation is dried and obtains polyamide powder particle;
Auxiliary agent can also be added in the dissolving incubation step, the addition of auxiliary agent adds the 0.1-2% of quality for polyamide;Institute Stating has nitrogen protection in reactor in dissolving incubation step, soaking time is 0.5-1.5 hours, anti-in the dissolving incubation step It is 0.8-1.2MPa to answer pressure in kettle, and the auxiliary agent is any of nucleation-accelerant or flow promortor or two kinds of combination, Using controlling the heat conduction oil temperature of reactor to reach temperature control purpose in cooling milling step, obtained powder particle passes through laser grain Degree measurement, its D10 is more than 30 μm, and D50 is at 55-65 μm, and D75 is less than 80 μm,.
2. a kind of preparation method of polyamide powder according to claim 1, it is characterised in that:The cooling pulverizing process Uniform stirring solution in middle reactor, mixing speed is 100-1000r/min.
3. a kind of preparation method of polyamide powder according to claim 1, it is characterised in that:The dissolving incubation step In, polyamide is dissolved using organic solvent, and consumption of organic solvent is 8-30 times of volume of polyamide weight.
4. a kind of preparation method of polyamide powder according to claim 3, it is characterised in that:The organic solvent is alcohol Class solvent or amide solvent.
5. a kind of preparation method of polyamide powder according to claim 1, it is characterised in that:The polyamide be PA6, Any of PA11, PA12, PA66, PA610, PA612, PA1010, PA1012, PA1212.
6. a kind of polyamide powder prepared according to any one of claim 1-5 methods described, it is characterised in that:Powder Particle size is evenly distributed, by laser particle size measurement, and its D10 is more than 30 μm, and D50 is at 55-65 μm, and D75 is less than 80 μm.
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CN107189087A (en) * 2017-06-01 2017-09-22 深圳市业天科技有限公司 A kind of preparation method and applications of PLA powder for selective laser sintering
CN110684213B (en) 2018-07-06 2022-04-01 绿点高新科技股份有限公司 Method for producing polyamide powder and composition for producing polyamide powder
CN109199651A (en) * 2018-09-22 2019-01-15 广东兰湾智能科技有限公司 Artificial limb socket of myoelectric hand
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