CN108587081A - A kind of preparation method of fusion sediment 3D printing new material - Google Patents
A kind of preparation method of fusion sediment 3D printing new material Download PDFInfo
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- CN108587081A CN108587081A CN201810362984.6A CN201810362984A CN108587081A CN 108587081 A CN108587081 A CN 108587081A CN 201810362984 A CN201810362984 A CN 201810362984A CN 108587081 A CN108587081 A CN 108587081A
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- 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
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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
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/02—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds
- C08G63/12—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/16—Dicarboxylic acids and dihydroxy compounds
- C08G63/18—Dicarboxylic acids and dihydroxy compounds the acids or hydroxy compounds containing carbocyclic rings
- C08G63/181—Acids containing aromatic rings
- C08G63/183—Terephthalic acids
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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
- C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
- C08L67/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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- 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
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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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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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
- C08L2207/00—Properties characterising the ingredient of the composition
- C08L2207/06—Properties of polyethylene
- C08L2207/062—HDPE
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Abstract
The present invention relates to field of new material preparation, particularly with regard to a kind of preparation method of fusion sediment 3D printing new material；70 90 parts of polypropylene terephthalate pellet and 10 15 parts of high density polyethylene (HDPE) are dried into 5 10h, then the talcum powder with 0.5 1.5 parts, 10 15 parts of nano barium titanate calcium, 0.5 1.0 parts of N, N ethylenebis stearic amides, the auxiliary agents such as 0.4 0.9 parts of coupling agent and 0.1 0.5 parts of antioxidant are blended molding and obtain 3D printing new material in an extruder；There is higher mechanical strength by 3D printing new material prepared by this programme, good thermal stability and molding processibility, pass through the modification to raw material, prepare a kind of low melting point polypropylene terephthalate, prepared 3D printing material melting point decreases, with lower melt viscosity, it is more applicable for 3D printing technique.
Description
Technical field
The present invention relates to field of material preparation, particularly with regard to a kind of preparation method of fusion sediment 3D printing new material.
Background technology
Fused glass pellet is a kind of 3D printing technique that developed by Stratasys companies, is by Filamentous thermosol
Property plastic heating melt, wire-feed motor squeezed out by print head, becomes a solid three-dimensional by stacked in multi-layers
Object is one of most widely used 3D forming techniques in the world, has been widely used in manufacturing industry, education and housed device etc.
Field.
CN106042374A discloses a kind of method solving fusion sediment 3D printing intensity, belongs to 3D printing technique neck
Domain.Technical scheme of the present invention includes：One layer of suction wave material is coated on the common surface applied to fusion sediment 3D printing wire rod
Material, then gets designed model using 3D printer, model is put into micro-wave oven and carries out microwave treatment, in specific wavelength
Under the action of, absorbing material generates high temperature, controls microwave intensity and microwave time, reaches the wire rod office for making to stack between layers
Portion's high temperature melt is to viscoelastic state, then bonding between layers will more securely, rather than just the bonding on surface.The invention carries
The technical solution of confession will solve fusion sediment printout significantly, and bonding is not tight between layers, is easy the problem of cracking, fracture etc.,
It can be widely applied to 3D printing technique field.
CN106393716A discloses a kind of dredging fused glass pellet technique 3d printer nozzles method and is suitable for
The device of the dredging method.Include fixing heated seats for integrated nozzle is fixed and calorified to nozzle, to fusion sediment at
The jackscrew mechanism of type technique 3d printer nozzles dredging.Resistance heating stick in fixed nozzle hole carries out temperature controlled
Temperature controller, and control the controllor for step-by-step motor of jackscrew mechanism movement.The invention may be implemented to fusion sediment needed for user
The direct dredging of moulding process 3d printing nozzles.The inventive method is not necessarily to dismantle fused glass pellet technique 3d printer nozzles,
And adjustable temperature firm banking is additionally arranged to complete the heating to plug nozzle, jackscrew mechanism used in heat dredging nozzle is completed with this
Elevating movement, to simplify dredging flow, be conducive to save time and materials cost.
CN205969972U discloses a kind of safety-type 3D printer using fusion sediment formula technology.The safety-type 3D
Printer includes 3D printing fuselage, Z axis protective shell, X-axis protective shell and the nozzle protective shell using fusion sediment formula technology.Pass through
The design that full packaging type is carried out to the 3D printing fuselage of application fusion sediment formula technology, can not only protect in 3D printing fuselage
The positions such as circuit and feeding-passage, prevent leads to problems such as short circuit or feeding-passage be obstructed because the external world touches, and protects
The service life for hindering 3D printer is also prevented from human body touching circuit and discharging spray nozzle, avoids the occurrence of electric shock or scald human body
Accident, ensure human-body safety, thus the safety of 3D printer can be made to increase substantially, be highly suitable for the application scenarios such as teaching
In.In addition, the safety-type 3D printer also has, additional function is more, stable work in work, simple in structure low with processing cost
The advantages that, it is convenient for practical promotion and application.
Polypropylene terephthalate is a kind of novel thermoplastic polyester, has higher intensity, good thermostabilization
Performance, excellent molding processibility also have the advantages that good pollution resistance and wearability, especially suitable for fused glass pellet
3D printing material.But the fusing point of the polypropylene terephthalate 3D printing material of prior art production is too high, it is excessively high
Print temperature, it is possible to cause polymer to decompose, generate poisonous and harmful substance, pollute environment.
Invention content
To solve the above-mentioned problems, the invention provides a kind of preparation methods of fusion sediment 3D printing new material.
A kind of preparation method of fusion sediment 3D printing new material, synthetic technology scheme are as follows：
According to mass fraction, the high density polyethylene (HDPE) of 70-90 parts of polypropylene terephthalate pellets and 10-15 part is put
Enter dry 5-10h in 80-90 DEG C of baking oven, then the talcum powder with 0.5-1.5 parts, 10-15 parts of nano barium titanate calcium, 0.5-
1.0 parts of N, N- ethylenebis stearic amide, 0.001-0.006 parts of polyaminopropyl biguanide, 0.5-1.0 parts of hydrogenation of benzene second
Alkene/methyl styrene/indene copolymer, 0.4-0.9 parts of coupling agent isopropyl three（Dioctylphyrophosphoric acid acyloxy）Titanate esters and
0.1-0.5 parts of antioxidant 2,6 di tert butyl 4 methyl phenol is added in extruder to be blended to be molded and obtain after mixing
A kind of fusion sediment 3D printing new material；It is characterized in that the polypropylene terephthalate pellet is a kind of low melting point
Polypropylene terephthalate.
In the extruder three sections of processing temperatures of blending extrusion machine be respectively set as 150-160 DEG C, 165-175 DEG C and
175-180℃；Screw speed 80-100r/min.
The polypropylene terephthalate of the low melting point is a kind of wire rod of a diameter of 0.20-0.35mm.
The polypropylene terephthalate of the low melting point is prepared as follows：
According to mass fraction, by 23-28 parts of terephthalic acid (TPA), 10-15 parts of M-phthalic acid, 0.4-1.0 parts of decanedioic acid,
23-30 parts of 1,3-PD, 0.01-0.06 parts of poly- hydroxyterephthalic acid's zinc, 0.0002-0.0008 parts three (2,2,
6,6- tetramethyl -3,5- pimelic acid) europium, 0.02-0.06 parts of bismuth hexafluoro -2,4- pentanedionate, 0.01-0.05 parts of catalyst
It is added in reaction kettle, then begins to warm up, start to stir when system temperature rises to 90-100 DEG C, mixing speed 120-
It 150 turns/min, then proceedes to be warming up to 160-210 DEG C, reacts 120-240min, the water generated in reaction process is distilled off；
0.02-0.06 parts of antioxidant 2,6 di tert butyl 4 methyl phenol, 3.2-5.1 parts of nano-calcium carbonate is added after completing reaction
Then calcium and 0.1-0.5 parts of stearic acid vacuumize reaction, keep pressure in kettle to be not more than 80Pa, be warming up to 240-260 DEG C,
React 180-240min；It then passes to nitrogen and releases vacuum, product is poured into cold water while hot, is then taken out, at 70-80 DEG C
Dry 18-24h, is cut into pellet, you can obtain a kind of low melting point polypropylene terephthalate in baking oven.
The catalyst is the mixture of tetra-n-butyl titanate or tetraethyl titanate or both.
A kind of preparation method of fusion sediment 3D printing new material disclosed in the method for the present invention, the 3D prepared by this programme
Printing new material has higher mechanical strength, good thermal stability and molding processibility, passes through the modification to raw material, system
For a kind of low melting point polypropylene terephthalate is gone out, prepared 3D printing material melting point decreases, and has lower
Melt viscosity is more applicable for 3D printing technique.
Specific implementation mode
The invention is described further below by specific embodiment：
Embodiment 1
A kind of preparation method of fusion sediment 3D printing new material, synthetic technology scheme are as follows：
According to mass fraction, 80 parts of polypropylene terephthalate pellet and 13 parts of high density polyethylene (HDPE) are put into 85 DEG C
Baking oven in dry 8h, the then talcum powder with 1.0 parts, 13 parts of nano barium titanate calcium, 0.8 part of N, N- ethylenebis stearic acid
Amide, 0.003 part of polyaminopropyl biguanide, 0.8 part of hydrogenated styrene/methyl styrene/indene copolymer, 0.6 part of coupling
Agent isopropyl three（Dioctylphyrophosphoric acid acyloxy）Titanate esters and 0.3 part of antioxidant 2,6 di tert butyl 4 methyl phenol are mixed
It is added in extruder to be blended to be molded after closing uniformly and obtains a kind of fusion sediment 3D printing new material；It is characterized in that described is poly-
Propylene glycol ester terephthalate's pellet is a kind of polypropylene terephthalate of low melting point.
Three sections of processing temperatures of blending extrusion machine are respectively set as 155 DEG C, 170 DEG C and 180 DEG C in the extruder；Screw rod
Rotating speed 90r/min.
The polypropylene terephthalate of the low melting point is a kind of wire rod of a diameter of 0.25mm.
The polypropylene terephthalate of the low melting point is prepared as follows：
According to mass fraction, by 25 parts of terephthalic acid (TPA), 13 parts of M-phthalic acid, 0.7 part of decanedioic acid, the 1,3- of 26 parts
Propylene glycol, 0.02 part of poly- hydroxyterephthalic acid's zinc, 0.0006 part three (2,2,6,6- tetramethyl -3,5- pimelic acid) europiums,
0.05 part of bismuth hexafluoro -2,4- pentanedionate, 0.03 part of catalyst are added in reaction kettle, then begin to warm up, and work as system
Start to stir when temperature rise is to 95 DEG C, 130 turns/min of mixing speed, then proceedes to be warming up to 180 DEG C, react 180min, instead
The water that should be generated in the process is distilled off；Complete reaction after be added 0.04 part antioxidant 2,6 di tert butyl 4 methyl phenol,
Then 4.1 parts of nano-calcium carbonate and 0.3 part of stearic acid vacuumize reaction, keep pressure in kettle to be not more than 80Pa, be warming up to
250 DEG C, react 210min；It then passes to nitrogen and releases vacuum, product is poured into cold water while hot, is then taken out, at 75 DEG C
Dry 20h, is cut into pellet, you can obtain a kind of low melting point polypropylene terephthalate in baking oven.
The catalyst is tetra-n-butyl titanate.
Sample number into spectrum is KD-1.
Embodiment 2
A kind of preparation method of fusion sediment 3D printing new material, synthetic technology scheme are as follows：
According to mass fraction, 70 parts of polypropylene terephthalate pellet and 10 parts of high density polyethylene (HDPE) are put into 80 DEG C
Baking oven in dry 5h, the then talcum powder with 0.5 part, 10 parts of nano barium titanate calcium, 0.5 part of N, N- ethylenebis stearic acid
Amide, 0.001 part of polyaminopropyl biguanide, 0.5 part of hydrogenated styrene/methyl styrene/indene copolymer, 0.4 part of coupling
Agent isopropyl three（Dioctylphyrophosphoric acid acyloxy）Titanate esters and 0.1 part of antioxidant 2,6 di tert butyl 4 methyl phenol are mixed
It is added in extruder to be blended to be molded after closing uniformly and obtains a kind of fusion sediment 3D printing new material；It is characterized in that described is poly-
Propylene glycol ester terephthalate's pellet is a kind of polypropylene terephthalate of low melting point.
Three sections of processing temperatures of blending extrusion machine are respectively set as 150 DEG C, 165 DEG C and 175 DEG C in the extruder；Screw rod
Rotating speed 80r/min.
The polypropylene terephthalate of the low melting point is a kind of wire rod of a diameter of 0.20mm.
The polypropylene terephthalate of the low melting point is prepared as follows：
According to mass fraction, by 23 parts of terephthalic acid (TPA), 10 parts of M-phthalic acid, 0.4 part of decanedioic acid, the 1,3- of 23 parts
Propylene glycol, 0.01 part of poly- hydroxyterephthalic acid's zinc, 0.0002 part three (2,2,6,6- tetramethyl -3,5- pimelic acid) europiums,
0.02 part of bismuth hexafluoro -2,4- pentanedionate, 0.01 part of catalyst Ti acetoacetic ester are added in reaction kettle, then start to add
Heat starts to stir when system temperature rises to 90 DEG C, 120 turns/min of mixing speed, then proceedes to be warming up to 160 DEG C, reaction
120min, the water generated in reaction process are distilled off；Complete the antioxidant 2,6- di-t-butyls -4- of 0.02 part of addition after reacting
Then methylphenol, 3.2 parts of nano-calcium carbonate and 0.1 part of stearic acid vacuumize reaction, pressure in kettle is kept to be not more than
80Pa is warming up to 240 DEG C, reacts 180min；It then passes to nitrogen and releases vacuum, product is poured into cold water while hot, then
It takes out, dry 18h, is cut into pellet, you can obtain a kind of low melting point polypropylene terephthalate in 70 DEG C of baking ovens.
Sample number into spectrum KD-2.
Embodiment 3
A kind of preparation method of fusion sediment 3D printing new material, synthetic technology scheme are as follows：
According to mass fraction, 90 parts of polypropylene terephthalate pellet and 15 parts of high density polyethylene (HDPE) are put into 80-
10h is dried in 90 DEG C of baking oven, then the talcum powder with 1.5 parts, 15 parts of nano barium titanate calcium, 1.0 parts of N, N- ethylenebis
Stearic amide, 0.006 part of polyaminopropyl biguanide, 1.0 parts of hydrogenated styrene/methyl styrene/indene copolymer, 0.9 part
Coupling agent isopropyl three（Dioctylphyrophosphoric acid acyloxy）Titanate esters and 0.5 part of antioxidant 2,6- di-t-butyl -4- methyl
Phenol is added in extruder to be blended to be molded after mixing obtains a kind of fusion sediment 3D printing new material；It is characterized in that institute
The polypropylene terephthalate pellet stated is a kind of polypropylene terephthalate of low melting point.
Three sections of processing temperatures of blending extrusion machine are respectively set as 1160 DEG C, 175 DEG C and 180 DEG C in the extruder；Spiral shell
Bar rotating speed 100r/min.
The polypropylene terephthalate of the low melting point is a kind of wire rod of a diameter of 0.35mm.
The polypropylene terephthalate of the low melting point is prepared as follows：
According to mass fraction, by 28 parts of terephthalic acid (TPA), 15 parts of M-phthalic acid, 1.0 parts of decanedioic acid, the 1,3- of 30 parts
Propylene glycol, 0.06 part of poly- hydroxyterephthalic acid's zinc, 0.0008 part three (2,2,6,6- tetramethyl -3,5- pimelic acid) europiums,
0.06 part of bismuth hexafluoro -2,4- pentanedionate, 0.05 part of catalyst tetra-n-butyl titanate are added in reaction kettle, then start
Heating, starts to stir when system temperature rises to 100 DEG C, and mixing speed 120-150 turns/min, then proceedes to be warming up to 210
DEG C, 240min is reacted, the water generated in reaction process is distilled off；The antioxidant 2 of 0.02-0.06 parts of addition after reacting is completed,
Then 6- di-tert-butyl-4-methy phenols, 5.1 parts of nano-calcium carbonate and 0.1-0.5 parts of stearic acid vacuumize reaction, protect
It holds pressure in kettle and is not more than 80Pa, be warming up to 260 DEG C, react 240min；It then passes to nitrogen and releases vacuum, while hot fall product
Enter into cold water, then take out, is dried for 24 hours in 80 DEG C of baking ovens, be cut into pellet, you can obtain a kind of poly- terephthaldehyde of low melting point
Acid propylene glycol ester.
Sample number into spectrum KD-3.
Comparative example 1
It is not added with M-phthalic acid, the other the same as in Example 1, obtained sample number into spectrum KD-4.
Comparative example 2
It is not added with hydrogenated styrene/methyl styrene/indene copolymer, the other the same as in Example 1, obtained sample number into spectrum KD-5.
Comparative example 3
It is not added with polyaminopropyl biguanide, the other the same as in Example 1, sample number into spectrum KD-6.
Comparative example 4
Not addition polymerization hydroxyterephthalic acid zinc, the other the same as in Example 1, obtained sample number into spectrum KD-7.
Comparative example 5
It is not added with three (2,2,6,6- tetramethyl -3,5- pimelic acid) europiums, the other the same as in Example 1, obtained sample number into spectrum KD-8.
Comparative example 6
It is not added with bismuth hexafluoro -2,4- pentanedionate, the other the same as in Example 1, sample number into spectrum KD-9.
Table：The performance for the test specimen that different process is made compares.
Claims (5)
1. a kind of preparation method of fusion sediment 3D printing new material, synthetic technology scheme are as follows：
According to mass fraction, the high density polyethylene (HDPE) of 70-90 parts of polypropylene terephthalate pellets and 10-15 part is put
Enter dry 5-10h in 80-90 DEG C of baking oven, then the talcum powder with 0.5-1.5 parts, 10-15 parts of nano barium titanate calcium, 0.5-
1.0 parts of N, N- ethylenebis stearic amide, 0.001-0.006 parts of polyaminopropyl biguanide, 0.5-1.0 parts of hydrogenation of benzene second
Alkene/methyl styrene/indene copolymer, 0.4-0.9 parts of coupling agent isopropyl three（Dioctylphyrophosphoric acid acyloxy）Titanate esters and
0.1-0.5 parts of antioxidant 2,6 di tert butyl 4 methyl phenol is added in extruder to be blended to be molded and obtain after mixing
A kind of fusion sediment 3D printing new material；It is characterized in that the polypropylene terephthalate pellet is a kind of low melting point
Polypropylene terephthalate.
2. a kind of preparation method of fusion sediment 3D printing new material according to claim 1, it is characterised in that：Described
Three sections of processing temperatures of blending extrusion machine are respectively set as 150-160 DEG C, 165-175 DEG C and 175-180 DEG C in extruder；Screw rod turns
Fast 80-100r/min.
3. a kind of preparation method of fusion sediment 3D printing new material according to claim 1, it is characterised in that：Described
The polypropylene terephthalate of low melting point is a kind of wire rod of a diameter of 0.20-0.35mm.
4. a kind of preparation method of fusion sediment 3D printing new material according to claim 1, it is characterised in that：Described
The polypropylene terephthalate of low melting point is prepared as follows：
According to mass fraction, by 23-28 parts of terephthalic acid (TPA), 10-15 parts of M-phthalic acid, 0.4-1.0 parts of decanedioic acid,
23-30 parts of 1,3-PD, 0.01-0.06 parts of poly- hydroxyterephthalic acid's zinc, 0.0002-0.0008 parts three (2,2,
6,6- tetramethyl -3,5- pimelic acid) europium, the catalysis of 0.02-0.06 parts of bismuth hexafluoro -2,4- pentanedionate and 0.01-0.05 part
Agent is added in reaction kettle, is then begun to warm up, and starts to stir when system temperature rises to 90-100 DEG C, mixing speed 120-
It 150 turns/min, then proceedes to be warming up to 160-210 DEG C, reacts 120-240min, the water generated in reaction process is distilled off；
0.02-0.06 parts of antioxidant 2,6 di tert butyl 4 methyl phenol, 3.2-5.1 parts of nano-calcium carbonate is added after completing reaction
Then calcium and 0.1-0.5 parts of stearic acid vacuumize reaction, keep pressure in kettle to be not more than 80Pa, be warming up to 240-260 DEG C,
React 180-240min；It then passes to nitrogen and releases vacuum, product is poured into cold water while hot, is then taken out, at 70-80 DEG C
Dry 18-24h, is cut into pellet, you can obtain a kind of low melting point polypropylene terephthalate in baking oven.
5. a kind of preparation method of fusion sediment 3D printing new material according to claim 4, it is characterised in that：Described
Catalyst is the mixture of tetra-n-butyl titanate or tetraethyl titanate or both.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109599479A (en) * | 2018-11-16 | 2019-04-09 | 清华大学深圳研究生院 | A kind of thermoelectric material and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109599479A (en) * | 2018-11-16 | 2019-04-09 | 清华大学深圳研究生院 | A kind of thermoelectric material and preparation method thereof |
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Application publication date: 20180928 |