CN109233272A - Nylon/attapulgite/carbon fiber composite granule and preparation method thereof and the application in Selective Laser Sintering - Google Patents
Nylon/attapulgite/carbon fiber composite granule and preparation method thereof and the application in Selective Laser Sintering Download PDFInfo
- Publication number
- CN109233272A CN109233272A CN201811128108.3A CN201811128108A CN109233272A CN 109233272 A CN109233272 A CN 109233272A CN 201811128108 A CN201811128108 A CN 201811128108A CN 109233272 A CN109233272 A CN 109233272A
- Authority
- CN
- China
- Prior art keywords
- nylon
- attapulgite
- carbon fiber
- powder
- composite powder
- 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.)
- Withdrawn
Links
Classifications
-
- 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
-
- 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
- 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
- C08K13/06—Pretreated ingredients and ingredients covered by the main groups C08K3/00 - C08K7/00
-
- 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
- C08K3/346—Clay
-
- 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
- C08K5/134—Phenols containing ester groups
- C08K5/1345—Carboxylic esters of phenolcarboxylic 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
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/06—Elements
-
- 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
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
-
- 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
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
Abstract
Application the invention discloses a kind of nylon/attapulgite/carbon fiber composite powder and preparation method thereof and in Selective Laser Sintering, the preparation method includes nylon powder, concave and convex rod stone powder being decompressed compound method by liquid phase mixing, heating dissolved under pressure, cooling nylon/attapulgite composite powder is prepared, then the nylon/attapulgite composite powder and carbon fiber, flow promortor, antioxidant are obtained nylon/attapulgite/carbon fiber composite powder by mechanical mixture.The present invention provides a kind of preparation methods of nylon/attapulgite/carbon fiber composite powder, nylon/attapulgite/carbon fiber the composite powder prepared in this way is raw material, and the laser sintered part that chosen property laser sintering technology obtains has good comprehensive mechanical performance.
Description
Technical field
The present invention relates to selective laser sintering fields, and in particular to a kind of nylon/attapulgite/carbon fiber composite powder
And preparation method thereof and the application in Selective Laser Sintering.
Background technique
Selective Laser Sintering (SLS) is also known as precinct laser sintering, comes across the eighties in last century, is a kind of base
In the 3D printing technique of increasing material manufacturing.Its principle is to spread one layer of dusty material on the table in advance, and laser is in computer control
Under system, according to interface profile information, solid section powder is sintered, then constantly circulation, layer upon layer form.The technology
It is required that the particle diameter distribution of dusty material is uniform, mobility is preferable, be conducive to powder bed powder laying in this way.Such forming method has manufacture
The features such as simple process, degree of flexibility are high, material selection range is wide, stock utilization is high, shaping speed is fast, for the above feature
SLS method is mainly used in foundry industry, and can be used to directly make fast mould etc..
In addition, SLS technique biggest advantage is that selection is relatively broad, as nylon, wax, ABS, resin wrap sand (overlay film
Sand), polycarbonate (poly carbonates), metal and ceramic powders etc. all can serve as sintering object.It is not burnt on powder bed
Knot is divided into the support construction of sintering part, because without regard to support system (hardware and software).
Nylon material is a kind of semi-crystalline polymer, has good sintering character and lower melt viscosity, can pass through
SLS technique straight forming consistency is higher, the preferable function part of mechanical property, become the SLS that is most widely used at present at
One of profile material.But it is lower by the molding pure nylon product intensity of SLS technology and rigidity, it is mechanical that it is not able to satisfy certain molded parts
The performance requirement that performance test is required or used directly as final products.
Summary of the invention
The object of the present invention is to provide a kind of nylon/attapulgite/carbon fiber composite powder and preparation method thereof and selecting
Application in selecting property laser sintering technology, the nylon/attapulgite/carbon fiber composite powder prepared in this way are raw material, warp
The laser sintered part that Selective Laser Sintering obtains has good comprehensive mechanical performance.
The technical solution of the invention is as follows: nylon/attapulgite/carbon fiber composite powder preparation method includes such as
Lower step:
(1) attapulgite, coupling agent are mixed with organic solvent A, obtains modified attapulgite dispersion liquid;
(2) nylon, antitack agent are mixed with organic solvent B, obtains nylon mixed liquor;
(3) the modified attapulgite dispersion liquid, the nylon mixed liquor are placed in autoclave, are solved after heating reaction
It presses, be cooled to room temperature, then post-treated obtain nylon/attapulgite composite powder;
(4) after mixing evenly by nylon/attapulgite composite powder, carbon fiber, flow promortor and the antioxidant of step (3) preparation
Obtain the nylon/attapulgite/carbon fiber composite powder.
Wherein, in step (1):
The attapulgite is the nanofiber that draw ratio is greater than 40;
The organic solvent A selects at least one of ethylene glycol, isopropanol, n-butanol, N,N-dimethylformamide;
The coupling agent is aluminate coupling agent;
The mass ratio of the attapulgite and coupling agent is 1:0.03 ~ 0.5, further preferably 1:0.2;
In the modified attapulgite dispersion liquid mass percent concentration of attapulgite be 1 ~ 30%, further preferably 10 ~
15%。
Wherein, in step (2):
The nylon does not have particular/special requirement, selects the common nylon kinds such as nylon 6, nylon66 fiber, nylon 11, nylon 12;
The antitack agent in oleamide, erucyl amide, ethyl alcohol bis-stearamides, the double lauramides of ethyl alcohol at least one
Kind;
The organic solvent B is selected from least one of ethylene glycol, isopropanol, n-butanol N,N-dimethylformamide;
The quality of the antitack agent is the 0.1 ~ 1% of nylon quality;
The mass percent concentration of nylon is 1 ~ 25% in the mixed liquor.
Wherein, in step (3):
The mass ratio of the nylon in attapulgite and the mixed liquor in the modified attapulgite dispersion liquid is 1:5 ~ 100.
Wherein, in step (3), the temperature of the heating reaction is 130 ~ 200 DEG C, and the time is 0.5 ~ 2h, further preferably
Temperature be 150 ~ 180 DEG C;
The rate of the cooling be 2 ~ 5 DEG C/min, in order to make more uniform 4 DEG C of the further preferred rate of temperature fall of particle diameter distribution/
min;
The post-processing includes filtering, dried and screened, removes the bulky grain of reunion by being sieved.
Wherein, in step (4):
The diameter of the carbon fiber is 5 ~ 20 μm, and length is 10 ~ 100 μm;
The flow promortor in fumed silica, gaseous oxidation aluminium, nano-titanium oxide, nanometer silicon carbide at least one
Kind;
The antioxidant be irgasfos 168 (three [2.4- di-tert-butyl-phenyl] phosphite esters), antioxidant 1098(N, N '-it is bis--
(3-(3,5- di-tert-butyl-hydroxy phenyl) propiono) hexamethylene diamine), antioxidant 1076 (β-(3,5- di-t-butyl -4- hydroxyl
Phenyl) propionic acid octadecanol ester), antioxidant 1010 (four [β-(3,5- di-t-butyl -4- hydroxyl) benzenpropanoic acid] pentaerythritol esters)
One of;
The nylon/attapulgite composite powder, carbon fiber, flow promortor and antioxidant mass fraction be respectively 60 ~
98.4%, 1 ~ 35%, 0.5 ~ 4% and 0.1 ~ 1%.
The invention also discloses the nylon/attapulgite/carbon fiber composite powders prepared according to the above method.
The invention also discloses a kind of Selective Laser Sinterings, using nylon/attapulgite/carbon fiber as described above
Dimension composite powder is raw material powder, specifically: by raw material powder be fitted into selective laser molding machine in powder cabin, powdering scraper
Raw material powder is equably layered on processing platform to and is heated to processing temperature, laser issues laser, then controls program control
Laser processed is scanned on processing platform according to two-dimensional slice, after laser beam flying, moves down a powder layer thickness, scraper
Powdering is carried out, laser beam flying is repeated, and obtains laser sintered part;It is characterized in that: the mode of the laser beam flying is certainly
It is interior and outer, laser power be 30-80 w, scanning speed 6m/s, powder layer thickness be 0.08 ~ 0.15 mm, processing temperature be 170 ~
185℃。
Further preferably, the powder layer thickness is 0.10 ~ 0.11 mm.
Further preferably, the processing temperature is 180 DEG C.
Compared with prior art, the present invention has the advantage that
1, in the preparation method of nylon/attapulgite/carbon fiber composite powder disclosed by the invention, with natural-nanometer fiber bumps
Stick stone is raw material, has the advantages that material source is wide, green safe, application cost is low etc..
2, aluminate coupling agent is added and processing is modified to attapulgite, keep attapulgite good by functional group
In conjunction with nylon particles, humidification well is played, while the hygroscopicity of composite material can also be reduced, improve printing adaptation
Property.
It 3, is to make composite powder using pressurization-heating, pressure release-cooling when nylon/attapulgite composite powder preparation
Particle diameter distribution is more uniform, is suitable for SLS method and prints.
4, after high speed agitator stirs, it is uniformly mixed powder, the bulky grain of reunion is removed in sieving, in order to avoid to subsequent
Powder bed impacts, and facilitates attapulgite, carbon fiber is evenly distributed in nylon during the sintering process, formation attapulgite carbon
Fibrillar meshwork structure.
5, laser power is low in selective laser sintering technique disclosed by the invention, less energy consumption, with nylon/attapulgite/
Carbon fiber composite powder is raw material, by adding attapulgite and carbon fiber in the feed, after laser sintered, is burnt in laser
It ties and forms attapulgite/carbon fiber network in part, so that the mechanical performance of the laser sintered part of preparation greatly improves.
Specific embodiment
The present invention is made into one with reference to embodiments for the purposes, technical schemes and advantages that the present invention is furture elucidated
The detailed description of step, but protection scope not thereby limiting the invention.
Embodiment 1:
(1) 750 g nylon, 12 powder, 80g concave and convex rod stone powder, 140 g carbon fiber powders, the flowing of 20g nanometer silicon carbide are weighed
Auxiliary agent and 10g antioxidant 1010;
(2) above-mentioned attapulgite and aluminate coupling agent are added in n,N-Dimethylformamide with the mass ratio of 1:0.3, are made into
The dispersion liquid that attapulgite mass concentration is 15%, ultrasonic vibration 2-4 h obtain modified attapulgite dispersion liquid;
(3) N, N- dimethyl methyl is added with the mass ratio of 1:0.005 in above-mentioned nylon powder and the double lauramide antitack agents of ethyl alcohol
In amide, it is made into the mixed liquor that nylon mass concentration is 15%;
(4) the nylon mixed liquor of the modified attapulgite dispersion liquid of above-mentioned steps (2) preparation and above-mentioned steps (3) preparation is placed in
In autoclave, it is passed through nitrogen and is forced into 1MPa, and high-speed stirred (630rpm);Temperature is risen to 175 DEG C, heat preservation 2h to Buddhist nun
Dragon 12 is completely dissolved;High pressure is released after being completely dissolved, and room temperature is cooled the temperature to the speed of 4 DEG C/min, obtains nylon micron
Grain suspension;
(5) the nylon micron particles vacuum dried processing again for preparing step (4) crosses 200 meshes, obtains nylon/concave convex rod
Stone composite powder material;
(6) by the nylon prepared/attapulgite composite powder, weighed nanometer silicon carbide flow promortor and antioxidant 1010
It is placed in closed container and is uniformly mixed, weighed carbon fiber powder is then added, under conditions of revolving speed is 630 turns, stirring
20 min obtain nylon/attapulgite/carbon fiber composite powder;
(7) by nylon/attapulgite/carbon fiber composite powder be added to selective laser sintering and moulding machine in powder cabin, paving
Nylon/attapulgite/carbon fiber composite powder is equably layered on processing platform by powder scraper, and laser issues laser, powdering 6
Mm, setting processing temperature is 180 DEG C, processing platform temperature is 130 DEG C, dries 2 h of powder in advance;Start to process after drying powder, count
Calculation machine controls the switch of laser and the angle of scanner, so that laser beam is in processing plane according to corresponding two-dimensional slice
Form scan, after laser beam is inswept, workbench moves down a thickness, then powdering, and laser beam flying is swashed repeatedly
Light sintered part;The mode that wherein laser beam scans on processing platform is from-inner-to-outer, laser power 50W, scanning speed 6
M/s, powder layer thickness 0.11mm.
Comparative example 1: according to ratio described in embodiment 1, nylon/attapulgite composite material is prepared
(1) the anti-of 750 g nylon, 12 powder, the concave and convex rod stone powder of 80g, the nanometer silicon carbide flow promortor of 20g and 10g is weighed
Oxygen agent 1010;
(2) above-mentioned attapulgite and aluminate coupling agent are added in n,N-Dimethylformamide with the mass ratio of 1:0.3, are made into
The dispersion liquid that attapulgite mass concentration is 15%, ultrasonic vibration 2-4 h obtain modified attapulgite dispersion liquid;
(3) N, N- dimethyl methyl is added with the mass ratio of 1:0.005 in above-mentioned nylon powder and the double lauramide antitack agents of ethyl alcohol
In amide, it is made into the mixed liquor that nylon mass concentration is 15%;
(4) the nylon mixed liquor of the modified attapulgite dispersion liquid of above-mentioned steps (2) preparation and above-mentioned steps (3) preparation is placed in
In autoclave, it is passed through nitrogen and is forced into 1MPa, and high-speed stirred (630rpm);Temperature is risen to 175 DEG C, heat preservation 2h to Buddhist nun
Dragon 12 is completely dissolved;High pressure is released after being completely dissolved, and room temperature is cooled the temperature to the speed of 4 DEG C/min, obtains nylon micron
Grain suspension;
(5) the nylon micron particles vacuum dried processing again for preparing step (4) crosses 200 meshes, obtains nylon/concave convex rod
Stone composite powder material;
(6) by the nylon prepared/attapulgite composite powder, weighed nanometer silicon carbide flow promortor and antioxidant 1010
It is placed in be uniformly mixed in closed container and obtains nylon/attapulgite composite powder;
(7) by nylon/attapulgite composite powder be added to selective laser sintering and moulding machine in powder cabin, powdering scraper will
Nylon/attapulgite composite powder is equably layered on processing platform, and laser issues laser, 6 mm of powdering, setting processing temperature
Degree is 180 DEG C, processing platform temperature is 130 DEG C, dries 2 h of powder in advance;Start to process after drying powder, computer controlled laser
Switch and scanner angle so that laser beam is in processing plane according to the form scan of corresponding two-dimensional slice, laser
After beam is inswept, workbench moves down a thickness, then powdering, and laser beam flying obtains laser sintered part repeatedly;Wherein
The mode that laser beam scans on processing platform is from-inner-to-outer, and laser power 50W, scanning speed is 6 m/s, powder layer thickness
For 0.11mm.
Comparative example 2: according to ratio described in embodiment 1, nylon/carbon fibre composite is prepared
(1) the anti-of 750 g nylon, 12 powder, the carbon fiber powder of 140 g, the nanometer silicon carbide flow promortor of 20g and 10g is weighed
Oxygen agent 1010;
(2) N, N- dimethyl methyl is added with the mass ratio of 1:0.005 in above-mentioned nylon powder and the double lauramide antitack agents of ethyl alcohol
In amide, it is made into the mixed liquor that nylon mass concentration is 15%;
(3) nylon mixed liquor prepared by above-mentioned steps (2) is placed in autoclave, is passed through nitrogen and is forced into 1MPa, and is high
Speed stirring (630rpm);Temperature is risen to 175 DEG C, heat preservation 2h to nylon 12 is completely dissolved;High pressure is released after being completely dissolved, with 4
DEG C/speed of min cools the temperature to room temperature, obtain nylon micron particles suspension;
(4) 200 meshes are crossed in the nylon micron particles vacuum dried processing again for preparing step (3);
(5) nylon powder prepared, weighed nanometer silicon carbide flow promortor and antioxidant 1010 are placed in closed container
In be uniformly mixed, weighed carbon fiber powder is then added, revolving speed be 630 turns under conditions of, stir 20 min, obtain Buddhist nun
Dragon/carbon fiber composite powder;
(6) by nylon/carbon fiber composite powder be added to selective laser sintering and moulding machine in powder cabin, powdering scraper is by Buddhist nun
Dragon/carbon fiber composite powder is equably layered on processing platform, and laser issues laser, 6 mm of powdering, and setting processing temperature is
180 DEG C, processing platform temperature be 130 DEG C, in advance dry 2 h of powder;Start to process after drying powder, computer controlled laser is opened
Close and the angle of scanner so that laser beam in processing plane according to the form scan of corresponding two-dimensional slice, laser beam is swept
After crossing, workbench moves down a thickness, then powdering, and laser beam flying obtains laser sintered part repeatedly;Wherein laser
The mode that beam scans on processing platform is from-inner-to-outer, and laser power 50W, scanning speed is 6 m/s, and powder layer thickness is
0.11mm。
Embodiment 2:
(1) weigh 800 g nylon, 12 powder, 80g concave and convex rod stone powder, 95 g carbon fiber powders, 20g nano-titanium oxide flowing help
Agent and 5g antioxidant 1076;
(2) above-mentioned attapulgite and aluminate coupling agent are added in n-butanol with the mass ratio of 1:0.02, are made into attapulgite
The dispersion liquid that mass concentration is 15%, ultrasonic vibration 2-4 h obtain modified attapulgite dispersion liquid;
(3) above-mentioned nylon powder and ethyl alcohol bis-stearamides antitack agent are added in n-butanol with the mass ratio of 1:0.005, are made into
The mixed liquor that nylon mass concentration is 15%;
(4) the nylon mixed liquor of the modified attapulgite dispersion liquid of above-mentioned steps (2) preparation and above-mentioned steps (3) preparation is placed in
In autoclave, it is passed through nitrogen and is forced into 1MPa, and high-speed stirred (630rpm);Temperature is risen to 180 DEG C, heat preservation 1h to Buddhist nun
Dragon 12 is completely dissolved;High pressure is released after being completely dissolved, and room temperature is cooled the temperature to the speed of 4 DEG C/min, obtains nylon micron
Grain suspension;
(5) the nylon micron particles vacuum dried processing again for preparing step (4) crosses 200 meshes, obtains nylon/concave convex rod
Stone composite powder material;
(6) by the nylon prepared/attapulgite composite powder, weighed nano-titanium oxide flow promortor and antioxidant 1076
It is placed in closed container and is uniformly mixed, add weighed carbon fiber powder, under conditions of revolving speed is 630 turns, stirring 20
Min obtains nylon/attapulgite/carbon fiber composite powder;
(7) by nylon/attapulgite/carbon fiber composite powder be added to selective laser sintering and moulding machine in powder cabin, paving
Nylon/attapulgite/carbon fiber composite powder is equably layered on processing platform by powder scraper, and laser issues laser, powdering 6
Mm, setting processing temperature is 180 DEG C, processing platform temperature is 130 DEG C, dries 2 h of powder in advance;Start to process after drying powder, count
Calculation machine controls the switch of laser and the angle of scanner, so that laser beam is in processing plane according to corresponding two-dimensional slice
Form scan, after laser beam is inswept, workbench moves down a thickness, then powdering, and laser beam flying is swashed repeatedly
Light sintered part;The mode that wherein laser beam scans on processing platform is from-inner-to-outer, laser power 40W, scanning speed 6
M/s, powder layer thickness 0.10mm.
Embodiment 3:
(1) weigh 500 g nylon, 12 powder, 164g concave and convex rod stone powder, 10 g carbon fiber powders, 5g gaseous oxidation aluminium flowing help
Agent and 1g antioxidant 1098;
(2) above-mentioned attapulgite and aluminate coupling agent are added in isopropanol with the mass ratio of 1:0.03, are made into attapulgite
The dispersion liquid that mass concentration is 30%, ultrasonic vibration 2-4 h obtain modified attapulgite dispersion liquid;
(3) above-mentioned nylon powder and erucyl amide antitack agent are added in isopropanol with the mass ratio of 1:0.01, are made into nylon matter
Measure the mixed liquor that concentration is 1%;
(4) the nylon mixed liquor of the modified attapulgite dispersion liquid of above-mentioned steps (2) preparation and above-mentioned steps (3) preparation is placed in
In autoclave, it is passed through nitrogen and is forced into 1MPa, and high-speed stirred (630rpm);Temperature is risen to 200 DEG C, heat preservation 0.5 to
Nylon 12 is completely dissolved;High pressure is released after being completely dissolved, and room temperature is cooled the temperature to the speed of 5 DEG C/min, obtains nylon micron
Particle suspension liquid;
(5) the nylon micron particles vacuum dried processing again for preparing step (4) crosses 200 meshes, obtains nylon/concave convex rod
Stone composite powder material;
(6) by the nylon prepared/attapulgite composite powder, weighed gaseous oxidation aluminium flow promortor and antioxidant 1098
It is placed in closed container and is uniformly mixed, add weighed carbon fiber powder, under conditions of revolving speed is 630 turns, stirring 20
Min obtains nylon/attapulgite/carbon fiber composite powder;
(7) by nylon/attapulgite/carbon fiber composite powder be added to selective laser sintering and moulding machine in powder cabin, paving
Nylon/attapulgite/carbon fiber composite powder is equably layered on processing platform by powder scraper, and laser issues laser, powdering 6
Mm, setting processing temperature is 185 DEG C, processing platform temperature is 130 DEG C, dries 2 h of powder in advance;Start to process after drying powder, count
Calculation machine controls the switch of laser and the angle of scanner, so that laser beam is in processing plane according to corresponding two-dimensional slice
Form scan, after laser beam is inswept, workbench moves down a thickness, then powdering, and laser beam flying is swashed repeatedly
Light sintered part;The mode that wherein laser beam scans on processing platform is from-inner-to-outer, laser power 80W, scanning speed 6
M/s, powder layer thickness 0.08mm.
Embodiment 4:
(1) 12 powder of 974.26g nylon, the concave and convex rod stone powder of 9.74g, 350 g carbon fiber powders, 40g gas phase dioxy are weighed
SiClx and 10g irgasfos 168;
(2) above-mentioned attapulgite and aluminate coupling agent are added in ethylene glycol with the mass ratio of 1:0.5, are made into attapulgite
The dispersion liquid that mass concentration is 1%, ultrasonic vibration 2-4 h obtain modified attapulgite dispersion liquid;
(3) it is added in ethylene glycol by above-mentioned nylon powder and from oleamide antitack agent with the mass ratio of 1:0.001, is made into nylon
The mixed liquor that mass concentration is 25%;
(4) the nylon mixed liquor of the modified attapulgite dispersion liquid of above-mentioned steps (2) preparation and above-mentioned steps (3) preparation is placed in
In autoclave, it is passed through nitrogen and is forced into 1MPa, and high-speed stirred (630rpm);Temperature is risen to 130 DEG C, heat preservation 2h to Buddhist nun
Dragon 12 is completely dissolved;High pressure is released after being completely dissolved, and room temperature is cooled the temperature to the speed of 2 DEG C/min, obtains nylon micron
Grain suspension;
(5) the nylon micron particles vacuum dried processing again for preparing step (4) crosses 200 meshes, obtains nylon/concave convex rod
Stone composite powder material;
(6) by the nylon prepared/attapulgite composite powder, weighed fumed silica flow promortor and antioxidant
168 be placed in closed container be uniformly mixed, weighed carbon fiber powder is then added, revolving speed be 630 turns under conditions of, stir
20 min are mixed, nylon/attapulgite/carbon fiber composite powder is obtained;
(7) by nylon/attapulgite/carbon fiber composite powder be added to selective laser sintering and moulding machine in powder cabin, paving
Nylon/attapulgite/carbon fiber composite powder is equably layered on processing platform by powder scraper, and laser issues laser, powdering 6
Mm, setting processing temperature is 170 DEG C, processing platform temperature is 130 DEG C, dries 2 h of powder in advance;Start to process after drying powder, count
Calculation machine controls the switch of laser and the angle of scanner, so that laser beam is in processing plane according to corresponding two-dimensional slice
Form scan, after laser beam is inswept, workbench moves down a thickness, then powdering, and laser beam flying is swashed repeatedly
Light sintered part;The mode that wherein laser beam scans on processing platform is from-inner-to-outer, laser power 30W, scanning speed 6
M/s, powder layer thickness 0.15mm.
Performance characterization: the data of mechanical of 1 the obtained drip molding of embodiment 1-4 and comparative example 1-2 of table
Table 1 obtains the data of mechanical of drip molding by embodiment 1-4 and comparative example 1-2, and provides the power of pure nylon 12
Performance is learned to compare.It can be seen that nylon/attapulgite/carbon fiber composite granule prepared by the present invention from the data in table 1
SLS drip molding good mechanical performance, gained SLS drip molding compared to pure nylon powder, nylon/attapulgite composite granule and
Nylon/carbon fiber powder SLS drip molding has a distinct increment in terms of mechanical property.
The above description is merely a specific embodiment, does not constitute the limitation to the scope of this patent, any
Those familiar with the art can easily think of the change or the replacement, should contain in the technical scope that the present invention discloses
Lid is within protection scope of the present invention.
Claims (10)
1. nylon/attapulgite/carbon fiber composite powder preparation method, it is characterised in that the preparation method packet of the composite powder
Include that steps are as follows:
(1) attapulgite, coupling agent are mixed with organic solvent A, obtains modified attapulgite dispersion liquid;
(2) nylon, antitack agent are mixed with organic solvent B, obtains nylon mixed liquor;
(3) the modified attapulgite dispersion liquid, the nylon mixed liquor are placed in autoclave, are solved after heating reaction
It presses, be cooled to room temperature, then post-treated obtain nylon/attapulgite composite powder;
(4) nylon/attapulgite composite powder, carbon fiber, flow promortor and antioxidant prepared by step (3) is stirred evenly,
Obtain nylon/attapulgite/carbon fiber composite powder.
2. the preparation method of nylon/attapulgite/carbon fiber composite powder according to claim 1, it is characterised in that: step
Suddenly in (1), the attapulgite is the nanofiber that draw ratio is greater than 40;The coupling agent is aluminate coupling agent;It is described
Attapulgite and coupling agent mass ratio be 1:0.03 ~ 0.5;The organic solvent A is selected from ethylene glycol, isopropanol, positive fourth
At least one of alcohol, N,N-dimethylformamide;The mass percent of attapulgite in the modified attapulgite dispersion liquid
Concentration is 1 ~ 30%.
3. the preparation method of nylon/attapulgite/carbon fiber composite powder according to claim 1, it is characterised in that: step
Suddenly in (2), the antitack agent in oleamide, erucyl amide, ethyl alcohol bis-stearamides, the double lauramides of ethyl alcohol extremely
Few one kind;The quality of the antitack agent is the 0.1 ~ 1% of nylon quality;The organic solvent B is selected from ethylene glycol, isopropanol, just
At least one of butanol, N,N-dimethylformamide;The mass percent concentration of nylon is 1 ~ 25% in the mixed liquor.
4. the preparation method of nylon/attapulgite/carbon fiber composite powder according to claim 1, it is characterised in that: step
Suddenly in (3), the mass ratio of attapulgite in the modified attapulgite dispersion liquid and the nylon in the mixed liquor be 1:5 ~
100。
5. the preparation method of nylon/attapulgite/carbon fiber composite powder according to claim 1, it is characterised in that: step
Suddenly in (3), the temperature of the heating reaction is 130 ~ 200 DEG C, and the time is 0.5 ~ 2h;The rate of the cooling is 2 ~ 5 DEG C/min;
The post-processing includes filtering, dried and screened.
6. the preparation method of nylon/attapulgite/carbon fiber composite powder according to claim 1, it is characterised in that: step
Suddenly in (4): the diameter of the carbon fiber is 5 ~ 20 μm, and length is 10 ~ 100 μm;The flow promortor is selected from gas phase dioxy
At least one of SiClx, gaseous oxidation aluminium, nano-titanium oxide, nanometer silicon carbide;The antioxidant is selected from irgasfos 168
(three [2.4- di-tert-butyl-phenyl] phosphite esters), antioxidant 1098(N, N '-be bis--(3-(3,5- di-t-butyl -4- hydroxy benzenes
Base) propiono) hexamethylene diamine), antioxidant 1076 (β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid octadecanol ester), antioxygen
At least one of agent 1010(tetra- [β-(3,5- di-t-butyl -4- hydroxyl) benzenpropanoic acid] pentaerythritol ester);The nylon/recessed
In convex stick stone/carbon fiber composite powder, the mass fraction of each component are as follows:
Nylon/attapulgite composite powder 60 ~ 98.4%;
Carbon fiber 1 ~ 35%;
Flow promortor 0.5 ~ 4%;
Antioxidant 0.1 ~ 1%.
7. nylon/attapulgite/carbon fiber composite powder of any method preparation according to claim 1 ~ 6.
8. selective laser sintering method, comprising: by raw material powder be fitted into selective laser molding machine in powder cabin, powdering is scraped
Raw material powder is equably layered on processing platform and is heated to processing temperature by knife, and laser issues laser, then controls laser
It is scanned on processing platform according to two-dimensional slice, after laser beam flying, moves down a powder layer thickness, scraper is spread
Powder, laser beam flying are repeated, and obtain laser sintered part;It is characterized by: raw material powder is Buddhist nun as claimed in claim 7
Dragon/attapulgite/carbon fiber composite powder;The mode of the laser beam flying are as follows: from-inner-to-outer, laser power are 30 ~ 80 w,
Scanning speed is 6 m/s, and powder layer thickness is 0.08 ~ 0.15 mm, and processing temperature is 170 ~ 185 DEG C.
9. selective laser sintering method according to claim 8, it is characterised in that: the powder layer thickness is preferably
0.10~0.11 mm。
10. selective laser sintering method according to claim 8, it is characterised in that: the processing temperature is preferably
180℃。
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201811128108.3A CN109233272A (en) | 2018-09-27 | 2018-09-27 | Nylon/attapulgite/carbon fiber composite granule and preparation method thereof and the application in Selective Laser Sintering |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201811128108.3A CN109233272A (en) | 2018-09-27 | 2018-09-27 | Nylon/attapulgite/carbon fiber composite granule and preparation method thereof and the application in Selective Laser Sintering |
Publications (1)
Publication Number | Publication Date |
---|---|
CN109233272A true CN109233272A (en) | 2019-01-18 |
Family
ID=65056946
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201811128108.3A Withdrawn CN109233272A (en) | 2018-09-27 | 2018-09-27 | Nylon/attapulgite/carbon fiber composite granule and preparation method thereof and the application in Selective Laser Sintering |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN109233272A (en) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN112157909A (en) * | 2020-09-07 | 2021-01-01 | 裕克施乐塑料制品(太仓)有限公司 | Manufacturing process of TPU (thermoplastic polyurethane) -based high-performance automobile instrument panel |
CN115028989A (en) * | 2022-06-27 | 2022-09-09 | 盱眙欧佰特粘土材料有限公司 | Nylon composite powder, preparation method thereof and application thereof in laser sintering |
Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104672890A (en) * | 2014-12-22 | 2015-06-03 | 杭州杭复新材料科技有限公司 | Polymer matrix composite with laser-induced metallization characteristic |
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 |
CN107760018A (en) * | 2016-08-18 | 2018-03-06 | 黑龙江鑫达企业集团有限公司 | A kind of selective laser sintering 3D printing composite powders of PA 12 |
CN107936547A (en) * | 2017-11-20 | 2018-04-20 | 中国科学院宁波材料技术与工程研究所 | Nylon/graphene/carbon fiber composite powder and preparation method thereof and the application in Selective Laser Sintering |
CN108047687A (en) * | 2017-12-14 | 2018-05-18 | 中国科学院宁波材料技术与工程研究所 | A kind of nylon/attapulgite composite granule, its preparation method and application |
-
2018
- 2018-09-27 CN CN201811128108.3A patent/CN109233272A/en not_active Withdrawn
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
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 |
CN104672890A (en) * | 2014-12-22 | 2015-06-03 | 杭州杭复新材料科技有限公司 | Polymer matrix composite with laser-induced metallization characteristic |
CN107760018A (en) * | 2016-08-18 | 2018-03-06 | 黑龙江鑫达企业集团有限公司 | A kind of selective laser sintering 3D printing composite powders of PA 12 |
CN107936547A (en) * | 2017-11-20 | 2018-04-20 | 中国科学院宁波材料技术与工程研究所 | Nylon/graphene/carbon fiber composite powder and preparation method thereof and the application in Selective Laser Sintering |
CN108047687A (en) * | 2017-12-14 | 2018-05-18 | 中国科学院宁波材料技术与工程研究所 | A kind of nylon/attapulgite composite granule, its preparation method and application |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN112157909A (en) * | 2020-09-07 | 2021-01-01 | 裕克施乐塑料制品(太仓)有限公司 | Manufacturing process of TPU (thermoplastic polyurethane) -based high-performance automobile instrument panel |
CN115028989A (en) * | 2022-06-27 | 2022-09-09 | 盱眙欧佰特粘土材料有限公司 | Nylon composite powder, preparation method thereof and application thereof in laser sintering |
CN115028989B (en) * | 2022-06-27 | 2023-11-24 | 盱眙欧佰特粘土材料有限公司 | Nylon composite powder, preparation method thereof and application thereof in laser sintering |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN107936547A (en) | Nylon/graphene/carbon fiber composite powder and preparation method thereof and the application in Selective Laser Sintering | |
CN104910614B (en) | A kind of 3D printing low-warpage nylon dragon particulate composite and preparation method thereof | |
CN104910609A (en) | Polyurethane composite material for 3D printing, and preparation method and application thereof | |
CN109233272A (en) | Nylon/attapulgite/carbon fiber composite granule and preparation method thereof and the application in Selective Laser Sintering | |
CN105399428B (en) | A kind of ceramic slurry and ceramic material 3D printing forming method | |
CN107309434A (en) | A kind of preparation method and application of the spherical molybdenum powder of high-purity compact | |
CN109400179A (en) | A method of preparing macroscopic view and all controllable material of microstructure | |
CN110981445A (en) | Preparation method of oxide ceramic powder for laser 3D printing | |
CN110194461A (en) | A kind of preparation method of size tunable monodisperse meso-scale preparing spherical SiO 2 | |
CN108841016B (en) | Method for preparing spherical powder for selective laser sintering from high-molecular fibers | |
CN111218191A (en) | Metal powder coating and preparation process thereof | |
CN109534820A (en) | A kind of glass bending molding ceramic mold and preparation method thereof | |
CN106853522B (en) | A kind of hard alloy squeezes the preparation method of feeding | |
CN106046755A (en) | Polyurethane composite material for 3D (three-dimensional) printing | |
CN108384227A (en) | A kind of high speed 3D printing material and preparation method thereof | |
CN108485218A (en) | Shell powder enhances polylactic acid silk material and preparation method thereof and 3D printing | |
CN109014198A (en) | A method of preparing the pure molybdenum part of high-performance | |
CN108465817A (en) | A kind of high-compactness pure tungsten article fabrication methods of even tissue | |
CN105778128B (en) | Method for improving Tf-Tc difference value of polyamide material and polyamide material | |
CN104451222B (en) | A kind of preparation method of nanograined W-Cu composite block material | |
CN104788094B (en) | A kind of preparation method of bismuth titanate ceramics material | |
CN106046754A (en) | Antistatic type thermoplastic polyurethane composite material for 3D (Three Dimensional) printing | |
CN106189186A (en) | The 3D printing compound polyurethane material that a kind of Graphene is modified | |
CN106378447B (en) | A kind of thermoelectric material powder suspension and preparation method thereof for 3D printing | |
CN107304266A (en) | For the polypropylene composite materials powder of selective laser sintering and its preparation |
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 | ||
WW01 | Invention patent application withdrawn after publication | ||
WW01 | Invention patent application withdrawn after publication |
Application publication date: 20190118 |