CN110240799A - 3D printing composition and its preparation method and application - Google Patents
3D printing composition and its preparation method and application Download PDFInfo
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- CN110240799A CN110240799A CN201810198187.9A CN201810198187A CN110240799A CN 110240799 A CN110240799 A CN 110240799A CN 201810198187 A CN201810198187 A CN 201810198187A CN 110240799 A CN110240799 A CN 110240799A
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- 238000010146 3D printing Methods 0.000 title claims abstract description 94
- 239000000203 mixture Substances 0.000 title claims abstract description 85
- 238000002360 preparation method Methods 0.000 title claims description 9
- 239000000463 material Substances 0.000 claims abstract description 50
- 239000004626 polylactic acid Substances 0.000 claims abstract description 41
- 229920000747 poly(lactic acid) Polymers 0.000 claims abstract description 40
- 229920002401 polyacrylamide Polymers 0.000 claims abstract description 40
- 238000000034 method Methods 0.000 claims abstract description 38
- 239000004677 Nylon Substances 0.000 claims abstract description 30
- 229920001778 nylon Polymers 0.000 claims abstract description 30
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 28
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 27
- 239000011256 inorganic filler Substances 0.000 claims abstract description 27
- 229910003475 inorganic filler Inorganic materials 0.000 claims abstract description 27
- -1 compatilizer Substances 0.000 claims abstract description 13
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 26
- 239000011521 glass Substances 0.000 claims description 13
- 239000000377 silicon dioxide Substances 0.000 claims description 13
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 7
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 claims description 6
- 230000004927 fusion Effects 0.000 claims description 6
- 239000013049 sediment Substances 0.000 claims description 6
- 229920002292 Nylon 6 Polymers 0.000 claims description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 4
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 claims description 4
- 229920002302 Nylon 6,6 Polymers 0.000 claims description 3
- 238000005469 granulation Methods 0.000 claims description 3
- 230000003179 granulation Effects 0.000 claims description 3
- 150000002500 ions Chemical class 0.000 claims description 3
- 235000019260 propionic acid Nutrition 0.000 claims description 3
- 239000011863 silicon-based powder Substances 0.000 claims description 3
- 239000004408 titanium dioxide Substances 0.000 claims description 3
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 claims description 2
- 229910052901 montmorillonite Inorganic materials 0.000 claims description 2
- GLDOVTGHNKAZLK-UHFFFAOYSA-N n-octadecyl alcohol Natural products CCCCCCCCCCCCCCCCCCO GLDOVTGHNKAZLK-UHFFFAOYSA-N 0.000 claims description 2
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 claims description 2
- FGHOOJSIEHYJFQ-UHFFFAOYSA-N (2,4-ditert-butylphenyl) dihydrogen phosphite Chemical class CC(C)(C)C1=CC=C(OP(O)O)C(C(C)(C)C)=C1 FGHOOJSIEHYJFQ-UHFFFAOYSA-N 0.000 claims 1
- 125000000129 anionic group Chemical group 0.000 claims 1
- 150000001768 cations Chemical class 0.000 claims 1
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 claims 1
- 239000000835 fiber Substances 0.000 claims 1
- 238000010521 absorption reaction Methods 0.000 abstract description 11
- 238000013461 design Methods 0.000 abstract description 8
- 238000000465 moulding Methods 0.000 abstract description 7
- 238000007639 printing Methods 0.000 abstract description 5
- 239000003086 colorant Substances 0.000 abstract description 4
- 235000006708 antioxidants Nutrition 0.000 description 20
- 235000013339 cereals Nutrition 0.000 description 20
- 238000001179 sorption measurement Methods 0.000 description 12
- BGYHLZZASRKEJE-UHFFFAOYSA-N [3-[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxy]-2,2-bis[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxymethyl]propyl] 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)OCC(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 BGYHLZZASRKEJE-UHFFFAOYSA-N 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 8
- 239000000178 monomer Substances 0.000 description 7
- 230000001151 other effect Effects 0.000 description 7
- 239000000126 substance Substances 0.000 description 6
- 239000007921 spray Substances 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 238000001125 extrusion Methods 0.000 description 4
- 239000002131 composite material Substances 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 230000008021 deposition Effects 0.000 description 3
- 239000000975 dye Substances 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- JHWNWJKBPDFINM-UHFFFAOYSA-N Laurolactam Chemical compound O=C1CCCCCCCCCCCN1 JHWNWJKBPDFINM-UHFFFAOYSA-N 0.000 description 2
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 2
- 229920000299 Nylon 12 Polymers 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 235000009508 confectionery Nutrition 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- VOZRXNHHFUQHIL-UHFFFAOYSA-N glycidyl methacrylate Chemical compound CC(=C)C(=O)OCC1CO1 VOZRXNHHFUQHIL-UHFFFAOYSA-N 0.000 description 2
- 239000004519 grease Substances 0.000 description 2
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 2
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000000110 selective laser sintering Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 235000010215 titanium dioxide Nutrition 0.000 description 2
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 description 1
- JKIJEFPNVSHHEI-UHFFFAOYSA-N Phenol, 2,4-bis(1,1-dimethylethyl)-, phosphite (3:1) Chemical compound CC(C)(C)C1=CC(C(C)(C)C)=CC=C1OP(OC=1C(=CC(=CC=1)C(C)(C)C)C(C)(C)C)OC1=CC=C(C(C)(C)C)C=C1C(C)(C)C JKIJEFPNVSHHEI-UHFFFAOYSA-N 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 125000002252 acyl group Chemical group 0.000 description 1
- 150000001408 amides Chemical class 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 150000001450 anions Chemical group 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 238000005094 computer simulation Methods 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 235000013312 flour Nutrition 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 239000004310 lactic acid Substances 0.000 description 1
- 235000014655 lactic acid Nutrition 0.000 description 1
- 238000001459 lithography Methods 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000006855 networking Effects 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- SSDSCDGVMJFTEQ-UHFFFAOYSA-N octadecyl 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CCCCCCCCCCCCCCCCCCOC(=O)CCC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 SSDSCDGVMJFTEQ-UHFFFAOYSA-N 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 150000008301 phosphite esters Chemical class 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
- 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
- C08L67/04—Polyesters derived from hydroxycarboxylic acids, e.g. lactones
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
- C08L77/02—Polyamides derived from omega-amino carboxylic acids or from lactams thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
- C08L77/06—Polyamides derived from polyamines and polycarboxylic acids
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
Abstract
The present invention relates to polymeric material fields, it discloses the present invention and a kind of 3D printing composition is provided, the composition contains polylactic acid, nylon, polyacrylamide, compatilizer, inorganic filler and antioxidant, on the basis of the total weight of the composition, the content of the polylactic acid is 10-60 weight %, the content of the nylon is 30-80 weight %, the content of the polyacrylamide is 1-20 weight %, the content of the compatilizer is 1-20 weight %, the content of the inorganic filler is 0.1-2 weight %, the content of the antioxidant is 0.05-1.0 weight %.3D printing material of the invention has many advantages, such as high absorption, high-dimensional stability, and suitable for the colorful printing device of 3D, satisfaction fixed point design colours, one-pass molding go out the requirement of colorful product, it is made to have broad application prospects in 3D printing technique.
Description
Technical field
The present invention relates to polymeric material fields, and in particular, to a kind of 3D printing composition and preparation method thereof and answers
With.
Background technique
3D printing, also known as increasing material manufacturing are one kind of rapid shaping technique.Its principle be first pass through computer modeling or
Scan prototype, obtain digital model, then threedimensional model resolves into the two-dimensional section data of multilayer, then by software with
Digital control system is successively printed material, ultimately forms 3D solid.As push tertiary industry revolution core technology,
3D printing has the characteristics that networking, digitlization, personalization, former in defense military, aerospace, industry pattern design, product
The fields such as type design, biologic medical have a wide range of applications.The mainstream forming method of 3D printing includes melting deposition modeling
(FusedDeposition Modeling, FDM), stereolithography apparatus (Stereo Lithography Apparatus,
SLA), selective laser sintering (Selective Laser Sintering, SLS) etc..
3D printing product needs not move through injection molding, can be obtained intensity height, the forming part of good toughness.It can directly use
In the inspection for carrying out intensity, performance to model, the reasonability of product design structure, the feasibility of manufacturing process, moulding are verified
Aesthetics, can time update, improve product design, to meet the needs in market, thus greatly shorten new product exploitation week
Phase reduces development cost, enterprise is made to have stronger competitiveness.
At present in the colorful printing field 3D, it there is no and can satisfy the tool that fixed point design colours, one-pass molding go out colorful product
There is the macromolecule printing consumables of high absorption, high-dimensional stability.
Summary of the invention
The purpose of the invention is to overcome drawbacks described above of the existing technology, provide a kind of with high adsorption, height
The 3D printing composition preparation method of dimensional stability and application.
To achieve the goals above, in a first aspect, the present invention provides a kind of 3D printing composition, the composition contains poly-
Lactic acid, nylon, polyacrylamide, compatilizer, inorganic filler and antioxidant, it is described on the basis of the total weight of the composition
The content of polylactic acid is 10-60 weight %, the content of the nylon is 30-80 weight %, the content of the polyacrylamide is
1-20 weight %, the compatilizer content be 1-20 weight %, the content of the inorganic filler is 0.1-2 weight %, described
The content of antioxidant is 0.05-1.0 weight %.
Second aspect, the present invention provides a kind of preparation methods of 3D printing material, this method comprises: by said combination
Object is successively mixed, is granulated and formed.
The third aspect, the present invention provides 3D printing materials made from the above method.
Fourth aspect, the present invention provides the application of above-mentioned composition or printed material in fusion sediment method 3D printing.
Compared with prior art, technical solution of the present invention has the advantage that
3D printing material of the invention has many advantages, such as high absorption, high-dimensional stability, is suitable for the colorful printing device of 3D
In, satisfaction fixed point design colours, one-pass molding go out the requirement of colorful product, it is made to have wide answer in 3D printing technique
Use prospect.
Other features and advantages of the present invention will the following detailed description will be given in the detailed implementation section.
Specific embodiment
Detailed description of the preferred embodiments below.It should be understood that described herein specific
Embodiment is merely to illustrate and explain the present invention, and is not intended to restrict the invention.
The endpoint of disclosed range and any value are not limited to the accurate range or value, these ranges herein
Or value should be understood as comprising the value close to these ranges or value.For numberical range, the endpoint value of each range it
Between, can be combined with each other between the endpoint value and individual point value of each range, and individually between point value and obtain one
Or multiple new numberical ranges, these numberical ranges should be considered as specific open herein.
The present invention provides a kind of high absorption 3D printing composition, the composition contains polylactic acid, nylon, polypropylene
Amide, compatilizer, inorganic filler and antioxidant, on the basis of the total weight of the composition, the content of the polylactic acid is
10-60 weight %, the nylon content be 30-80 weight %, the content of the polyacrylamide is 1-20 weight %, institute
The content for stating compatilizer is 1-20 weight %, the content of the inorganic filler is 0.1-2 weight %, the antioxidant contains
Amount is 0.05-1.0 weight %.
In 3D printing composition of the invention, under preferable case, the melt mass flow rate of the polylactic acid is 1-
20g/10min, further preferably 3-10g/10min.
In 3D printing composition of the invention, on the basis of the total weight of the composition, the polylactic acid contains measurer
It can be body 10 weight %, 20 weight %, 30 weight %, 35 weight %, 40 weight %, 45 weight %, 50 weight %, 55
The arbitrary value in range that any two in weight %, 60 weight % and these point values are constituted.It is highly preferred that described
The content of polylactic acid is 20-50 weight %, further preferably 30-45 weight %.
When the polylactic acid melt mass flow rate and dosage within the above range, can make 3D printing material have
There are better high adsorption, high-dimensional stability and other effects.
In 3D printing composition of the invention, under preferable case, the nylon is nylon-6, nylon -66, nylon-
1010, at least one of Nylon-12 12.It is highly preferred that the nylon be nylon-6 and/or nylon -66, further preferably
For nylon-6.
In 3D printing composition of the invention, on the basis of the total weight of the composition, the content of the nylon is specific
Ground can be 30 weight %, 40 weight %, 42 weight %, 50 weight %, 55 weight %, 60 weight %, 65 weight %, 70 weights
The arbitrary value in range that any two in amount %, 80 weight % and these point values are constituted.It is highly preferred that the Buddhist nun
The content of dragon is 40-70 weight %, further preferably 42-55 weight %.
In 3D printing composition of the invention, under preferable case, the viscosity of the nylon is 1-8PaS, more preferably
For 2.4-4.5PaS.
When the composition of the nylon, dosage and viscosity within the above range, 3D printing material can be made to have preferably high
Adsorptivity, high-dimensional stability and other effects.
In 3D printing composition of the invention, under preferable case, the polyacrylamide is anion pp acyl
At least one of amine, cationic polyacrylamide, non-ionic polyacrylamide and amphoteric ion polyacrylamide.More preferably
Ground, the polyacrylamide be non-ionic polyacrylamide and/or amphoteric ion polyacrylamide, it is further preferably non-from
Sub- polyacrylamide.
In 3D printing composition of the invention, on the basis of the total weight of the composition, the polyacrylamide contains
Amount specifically can be 1 weight %, 2 weight %, 3 weight %, 5 weight %, 8 weight %, 10 weight %, 12 weight %, 15 weights
The arbitrary value in range that any two in amount %, 18 weight %, 20 weight % and these point values are constituted.More preferably
Ground, the content of the polyacrylamide are 2-15 weight %, further preferably 5-10 weight %.
In 3D printing composition of the invention, under preferable case, the granularity of the polyacrylamide is 50-200 mesh,
More preferably 50-100 mesh.
When the composition of the polyacrylamide, dosage and granularity within the above range, can make 3D printing material have more
High adsorption well, high-dimensional stability and other effects.
In the present invention, to the component selection of the compatilizer, there is no particular limitation, can routinely select for this field
It selects.Under preferable case, the compatilizer is the graft of polylactic acid, is specifically as follows polylactic acid grafted maleic anhydride and/or gathers
Lactic acid graft glycidyl methacrylate.It is highly preferred that the compatilizer is that the shrink of polylactic acid grafted methacrylic acid is sweet
Grease.
In the present invention, under preferable case, the grafting rate of graft is 0-1 weight %, more preferably 0.5-1 in compatilizer
Weight %.Wherein, grafting rate=[grafted monomers quality/(grafted monomers quality+grafted monomers homopolymerization amount of substance)] ×
100%.Grafted monomers homopolymerization amount of substance refers to non-grafted monomer mass.By taking polylactic acid grafted maleic anhydride as an example, grafting
Rate refers to the polylactic acid quality being grafted divided by the gross mass of polylactic acid monomer, and the gross mass of polylactic acid monomer is equal to
Grafting with the quality of non-grafted polylactic acid and.
In the present invention, to the selection of the dosage of the compatilizer, there is no particular limitation, can routinely select for this field
It selects.In 3D printing composition of the invention, on the basis of the total weight of the composition, the content of the compatilizer is specific
It can be 1 weight %, 2 weight %, 3 weight %, 5 weight %, 8 weight %, 10 weight %, 12 weight %, 15 weight %, 18
The arbitrary value in range that any two in weight %, 20 weight % and these point values are constituted.It is highly preferred that described
The content of compatilizer is 2-15 weight %, further preferably 5-10 weight %.
When the component of the compatilizer, grafting rate and dosage within the above range, 3D printing material can be made to have more preferable
High adsorption, high-dimensional stability and other effects.
In the present invention, it can be this field conventional selection that the component of the inorganic filler, there is no particular limitation.It is excellent
In the case of choosing, in 3D printing composition of the invention, the inorganic filler is silica, titanium dioxide, glass microballoon, cunning
At least one of mountain flour, barium sulfate, montmorillonite and silicon powder.It is highly preferred that the inorganic filler is silica, titanium white
At least one of powder and glass microballoon.In the present invention, silicon powder can be super-fine silicon micro-powder.
In a kind of preferred embodiment of the present invention, the inorganic filler is the mixture of glass microballoon and silica,
And the weight ratio of the two is 1: 1-2.
In the present invention, it can be this field conventional selection that the dosage of the inorganic filler, there is no particular limitation.?
In 3D printing composition of the invention, on the basis of the total weight of the composition, the inorganic filler content is specifically as follows
0.1 weight %, 0.2 weight %, 0.3 weight %, 0.4 weight %, 0.6 weight %, 0.8 weight %, 1 weight %, 1.2 weights
It is any in the range that any two in amount %, 1.5 weight %, 1.8 weight %, 2 weight % and these point values are constituted
Value.It is highly preferred that the content of the inorganic filler is 0.2-1 weight %, further preferably 0.3-0.6 weight %.
In the present invention, to the average grain diameter of the inorganic filler, there is no particular limitation, can routinely select for this field
It selects.Under preferable case, in 3D printing composition of the invention, the average grain diameter of the inorganic filler is 500-5000 mesh, tool
Body, for example, can for 500 mesh, 800 mesh, 1000 mesh, 1300 mesh, 1500 mesh, 1800 mesh, 2000 mesh, 2500 mesh, 3000 mesh,
The arbitrary value in range that any two in 3500 mesh, 4000 mesh, 4500 mesh, 5000 mesh and these point values are constituted.More
Preferably, the average grain diameter of the inorganic filler is 800-2000 mesh.
When the inorganic filler component, dosage and average grain diameter within the above range, 3D printing material can be made to have
Better high adsorption, high-dimensional stability and other effects.
In the present invention, to the component selection of the antioxidant, there is no particular limitation, can routinely select for this field
It selects.Under preferable case, in 3D printing composition of the invention, antioxidant can be four [β-(3,5- di-t-butyl -4- hydroxyls
Base phenyl) propionic acid] pentaerythritol ester (also known as antioxidant 1010), phosphite ester is (also known as three [2,4- di-tert-butyl-phenyls]
Irgasfos 168) and β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid n-octadecyl alcohol ester (also known as antioxidant 1076) in
At least one.It is highly preferred that the antioxidant is antioxidant 1010, at least one of antioxidant 168.Into one
Preferably, the antioxidant is the mixture of antioxidant 1010 and irgasfos 168, weight ratio 1: 2 to step.
In the present invention, to the selection of the dosage of the antioxidant, there is no particular limitation, can routinely select for this field
It selects.Under preferable case, in 3D printing composition of the invention, on the basis of the total weight of the composition, described is anti-oxidant
Agent content is 0.05-1 weight %, specifically, such as can be 0.05 weight %, 0.1 weight %, 0.2 weight %, 0.3 weight
Measure %, 0.4 weight %, 0.5 weight %, 0.6 weight %, 0.7 weight %, 0.8 weight %, 0.9 weight %, 1 weight % and
The arbitrary value in range that any two in these point values are constituted.It is highly preferred that the content of the antioxidant is 0.1-
0.8 weight %, further preferably 0.2-0.5 weight %.
When the antioxidant component and dosage within the above range, 3D printing material can be made to have preferably high
Adsorptivity, high-dimensional stability and other effects.
In order to make 3D printing material that there is better high adsorption, high-dimensional stability and other effects, under preferable case, institute
The 3D printing composition stated, on the basis of the total weight of the composition, the content of the polylactic acid is 20-50 weight %, described
The content of nylon is 40-70 weight %, the content of the polyacrylamide is 2-15 weight %, and the content of the compatilizer is
2-15 weight %, the content of the inorganic filler are 0.2-1%, and the content of the antioxidant is 0.1-0.8 weight %.
It is further preferred that the 3D printing composition, on the basis of the total weight of the composition, the polylactic acid
Content be 30-45 weight %, the content of the nylon is 42-55 weight %, the content of the polyacrylamide be 5-10 weight
% is measured, the content of the compatilizer is 5-10 weight %, and the content of the inorganic filler is 0.3-0.6%, the antioxidant
Content be 0.2-0.5 weight %.
Second aspect, the present invention provides a kind of preparation methods of 3D printing material, this method comprises: above-mentioned 3D is beaten
Print composition is successively mixed, is granulated extrusion and forming processes.
In method of the invention, the equipment being used in mixed way can be high-speed mixer, and the mixed time is not special
Restriction, as long as be made above-mentioned composition each component be uniformly mixed.
In method of the invention, it is granulated the selection of equipment that uses to described there is no particular limitation, can be this field
Middle conventional selection.Such as can be double screw extruder, under preferable case, the draw ratio of double screw extruder can be 30:
1-53: 1, the revolving speed of double screw extruder can be 200-400rpm.
In method of the invention, to the selection of the condition of the granulation, there is no particular limitation, can be conventional in this field
Selection.Under preferable case, the condition of the granulation may include: that extrusion temperature is 190-240 DEG C, preferably 200-230
℃.Prilling temperature in the present invention refers to that the temperature in double screw extruder controls in above-mentioned preferred scope, i.e. composition
Temperature when by double screw extruder can gradually rise, but its maximum temperature is not higher than 240 DEG C, and minimum temperature is not less than
190℃。
In method of the invention, forms the selection of equipment that uses to described there is no particular limitation, can be this field
Middle conventional selection, such as can be 3D twine machine.
In method of the invention, to the molding condition selection, there is no particular limitation, can be conventional in this field
Selection.Under preferable case, the molding condition may include: that processing temperature is 230 DEG C, extruded velocity 50r/min,
Leading speed is 100r/min.
The third aspect, the present invention provides 3D printing materials made from the above method.
In the present invention, to the selection of the specification of the 3D printing material, there is no particular limitation, can in this field often
The selection of rule.Under preferable case, the specification of 3D printing material produced by the present invention can be diameter 1.7-1.8mm.
Fourth aspect, the present invention provides above-mentioned 3D printing compositions or 3D printing material to beat in fusion sediment method in 3D
The application of India and China.Such as it can be melted to heat the 3D printing material of Filamentous (diameter about 1.75mm) by spray head, spray head bottom
Portion has minute nozzle (diameter is generally 0.2-0.6mm), is squeezed and is gushed out with certain pressure for material；Spray head is along water simultaneously
Square to movement, and workbench moves along the vertical direction.The material squeezed out in this way is together with previous level clinkering, and one
After the completion of level deposition, workbench is declined the thickness of a layer by scheduled increment, is further continued for fusion sediment, until completing whole
A solid modelling.
Below will by embodiment and comparative example, the present invention will be described in detail, but be not intended to limit the present invention.With
In lower embodiment and comparative example, unless otherwise instructed, used material can be commercially available.
Polylactic acid in embodiment 1-3 is purchased from U.S. NatureWorks company, trade mark PLA4032D, and major parameter is
Melt mass flow rate is 5g/10min.
Nylon-6 is purchased from, trade mark 5033B, and major parameter is that viscosity is 3.5PaS.
Nylon-12 12 is purchased from Ube company, and trade mark 3020U, major parameter is that viscosity is 3.0PaS.
Non-ionic polyacrylamide is purchased from Peng Yu chemical company, and major parameter is that granularity is 100 mesh.
Anion-polyacrylamide is purchased from Peng Yu chemical company, and major parameter is that granularity is 100 mesh.
Polylactic acid graft glycidyl methacrylate, purchased from French Arkema, trade mark CP5001, mainly
Parameter is that grafting rate is 0.8%.
Antioxidant 1010 is purchased from Shijiazhuang Jia Tuo Chemical Industry Science Co., Ltd, the trade mark 1010.
Irgasfos 168 is purchased from Shijiazhuang Jia Tuo Chemical Industry Science Co., Ltd, the trade mark 168.
Inorganic filler silica is purchased from Qingdao Niu Senke new material, trade mark VN3.
Inorganic filler glass microballoon is purchased from Shanghai Ming Bo new material Co., Ltd, trade mark MH.
Embodiment 1
The present embodiment is for illustrating 3D printing composition and 3D printing material and its preparation method and application of the invention.
(1) 3D printing composition is put into high-speed mixer and mixes 10min, be uniformly mixed, obtain mixture；Wherein,
The composition of 3D printing composition are as follows: 380g polylactic acid, 500g nylon, 60g non-ionic polyacrylamide, 53gPLA-g-GMA, 2g
Glass microballoon (average grain diameter is 1000 mesh), 2g silica (average grain diameter is 1000 mesh), 3g compound antioxidant (are resisted by 1g
Oxygen agent 1010 and 2g irgasfos 168 form)；
(2) mixture obtained in step (1) is added twin-screw extrude, coupled extrusion, obtains high absorption modeling
Expect grain, the process conditions of double screw extruder are as follows: extrusion temperature is 200-230 DEG C, and the draw ratio of double screw extruder is 40:
1, the revolving speed of double screw extruder is 300rpm；
(3) 3D twine machine is added in high adsorption plastic grain obtained in step (2), linear 3D printing material is prepared.
(4) the 3D printing material that step (3) obtains is made to the product of specific shape using fusion sediment method.Specifically
Method are as follows: the 3D printing material of Filamentous (diameter about 1.75mm) is heated by spray head and is melted, head of the nozzle has minute nozzle
(diameter is generally 0.3mm) is squeezed with certain pressure for material and is gushed out；Spray head moves in the horizontal direction simultaneously, and workbench
It moves along the vertical direction.The material squeezed out in this way is together with previous level clinkering, after the completion of a level deposition, work
Platform is declined the thickness of a layer by scheduled increment, is further continued for fusion sediment, until completing entire solid modelling.
Embodiment 2
3D printing material is prepared according to the method for embodiment 1, unlike, the group of the 3D printing composition in step (1)
Become: 450g polylactic acid, 420g nylon, 70g non-ionic polyacrylamide, 53g polylactic acid grafted methacrylic acid glycidol
Ester (PLA-g-GMA), 2g glass microballoon (average grain diameter is 1000 mesh), 2g silica (average grain diameter is 1000 mesh), 3g are multiple
It (is made of 1g antioxidant 1010 and 2g irgasfos 168) with antioxidant.
Embodiment 3
3D printing material is prepared according to the method for embodiment 1, unlike, the group of the 3D printing composition in step (1)
Become: 300g polylactic acid, 550g nylon, 90g non-ionic polyacrylamide, 53g polylactic acid grafted methacrylic acid glycidol
Ester (PLA-g-GMA), 2g glass microballoon (average grain diameter is 1000 mesh), 2g silica (average grain diameter is 1000 mesh), 3g are multiple
It (is made of 1g antioxidant 1010 and 2g irgasfos 168) with antioxidant.
Embodiment 4
3D printing material is prepared according to the method for embodiment 1, unlike, the group of the 3D printing composition in step (1)
Become: 200g polylactic acid, 700g nylon, 20g non-ionic polyacrylamide, 73gPLA-g-GMA, 2g glass microballoon (average grain
Diameter is 1000 mesh), 2g silica (average grain diameter is 1000 mesh), 3g compound antioxidant is (by 1g antioxidant 1010 and 2g antioxygen
Agent 168 forms).
Embodiment 5
3D printing material is prepared according to the method for embodiment 1, unlike, the group of the 3D printing composition in step (1)
Become: 500g polylactic acid, 400g nylon, 20g non-ionic polyacrylamide, 73g polylactic acid grafted methacrylic acid glycidol
Ester (PLA-g-GMA), 2g glass microballoon (average grain diameter is 1000 mesh), 2g silica (average grain diameter is 1000 mesh), 3g are multiple
It (is made of 1g antioxidant 1010 and 2g irgasfos 168) with antioxidant.
Embodiment 6
3D printing material is prepared according to the method for embodiment 1, unlike, the group of the 3D printing composition in step (1)
Become: 600g polylactic acid, 300g nylon, 10g non-ionic polyacrylamide, 83g polylactic acid grafted methacrylic acid glycidol
Ester (PLA-g-GMA), 2g glass microballoon (average grain diameter is 1000 mesh), 2g silica (average grain diameter is 1000 mesh), 3g are multiple
It (is made of 1g antioxidant 1010 and 2g irgasfos 168) with antioxidant.
Embodiment 7
3D printing material is prepared according to the method for embodiment 1, unlike, the group of the 3D printing composition in step (1)
Become: 100g polylactic acid, 680g nylon, 200g non-ionic polyacrylamide, 13g polylactic acid grafted methacrylic acid shrink sweet
Grease (PLA-g-GMA), 2g glass microballoon (average grain diameter is 1000 mesh), 2g silica (average grain diameter is 1000 mesh), 3g
Compound antioxidant (is made of) 1g antioxidant 1010 and 2g irgasfos 168.
Embodiment 8
3D printing material is prepared according to the 3D printing composition material and method of embodiment 1, unlike, in step (1)
3D printing composition composition in polylactic acid melt mass flow rate 19g/10min (trade mark PLA6302D, is purchased from
NatureWorks company, the U.S.).
Embodiment 9
3D printing material is prepared according to the 3D printing composition material and method of embodiment 1, unlike, in step (1)
3D printing composition composition in nylon be nylon 1212.
Embodiment 10
3D printing material is prepared according to the 3D printing composition material and method of embodiment 1, unlike, in step (1)
3D printing composition composition in polyacrylamide be anion-polyacrylamide.
Comparative example 1
3D printing material is prepared according to the method for embodiment 1, unlike, the group of the 3D printing composition in step (1)
Polylactic acid is free of in.
Comparative example 2
3D printing material is prepared according to the method for embodiment 1, unlike, the group of the 3D printing composition in step (1)
Nylon is free of in.
Comparative example 3
3D printing material is prepared according to the method for embodiment 1, unlike, the group of the 3D printing composition in step (1)
Polyacrylamide is free of in.
Comparative example 4
3D printing material is prepared according to the method for embodiment 1, unlike, gather in the 3D printing composition in step (1)
The granularity of acrylamide is 200 mesh.
The 3D printing composition component of above-described embodiment and comparative example accounts for weight ratio and is listed in the table below in 1.
Table 1
Test case
3D printing material in embodiment and comparative example is detected as follows respectively:
1, absorption property is tested, and test method is as follows: preparation 60mm × 30mm × 3mm cuboid exemplar, electronic scale are surveyed
Test mass amount is M1.It impregnates in acrylic compounds dyestuff (being purchased from Zhuhai martial prowess new material limited liability company, yellow) and uses afterwards for 24 hours
Filter paper gently dries surface dye, and it is M2, adsorption rate=(M2-M1)/M1 × 100%, the present invention that electronic scale, which tests weight,
In, the judgment mode for the absorption property tested according to the method described above is as follows: when adsorption rate >=10%, color absorption property is very
Good, when 5% < adsorption rate < 10%, color absorption property is good, and when 2% < adsorption rate≤5%, color absorption property is poor, when
When adsorption rate≤2%, almost without color adsorptivity；It when dyestuff is dried, visually observes color (color and gloss), then by sample
Part room temperature for 24 hours, compares color and maintains effect.
The results are shown in Table 2 for test.
2, dimensional stability is tested, and test method is as follows: GB/T 17037.4-2003, the results are shown in Table 2 for test.
Table 2
Can be seen that 3D printing material made from 3D printing composition of the invention as the result of table 2 obviously has height
It the advantages that absorption, high-dimensional stability, has excellent performance and safety and environmental protection is nontoxic, be suitably applied in colorful printing field, it is full
Foot fixed point design colours, one-pass molding go out the requirement of colorful product.
The preferred embodiment of the present invention has been described above in detail, still, during present invention is not limited to the embodiments described above
Detail, within the scope of the technical concept of the present invention, can with various simple variants of the technical solution of the present invention are made,
These simple variants all belong to the scope of protection of the present invention.
It is further to note that specific technical features described in the above specific embodiments, in not lance
It in the case where shield, can be combined in any appropriate way, in order to avoid unnecessary repetition, the present invention is to various
No further explanation will be given for possible combination.
In addition, various embodiments of the present invention can be combined randomly, as long as it is without prejudice to originally
The thought of invention, it should also be regarded as the disclosure of the present invention.
Claims (12)
1. a kind of 3D printing composition, which is characterized in that the composition contain polylactic acid, nylon, polyacrylamide, compatilizer,
Inorganic filler and antioxidant, on the basis of the total weight of the composition, the content of the polylactic acid is 10-60 weight %, institute
The content for stating nylon is 30-80 weight %, the content of the polyacrylamide is 1-20 weight %, the content of the compatilizer is
1-20 weight %, the inorganic filler content be 0.1-2 weight %, the content of the antioxidant be 0.05-1.0 weight
Measure %.
2. composition according to claim 1, wherein the nylon is nylon 6, nylon66 fiber, nylon 1010 and nylon
At least one of 1212.
3. composition according to claim 1, wherein the polyacrylamide is anionic polyacrylamide, cation
At least one of polyacrylamide, non-ionic polyacrylamide and amphoteric ion polyacrylamide.
4. composition according to claim 1, wherein the compatilizer is the graft of polylactic acid.
5. composition according to claim 1, wherein on the basis of the total weight of the composition, the polylactic acid contains
Amount be 20-50 weight %, the content of the nylon is 40-70 weight %, the content of the polyacrylamide be 2-15 weight %,
The content of the compatilizer is 2-15 weight %, the content of the inorganic filler is 0.2-1%, the content of the antioxidant is
0.1-0.8 weight %；
It is highly preferred that the content of the polylactic acid is 30-45 weight %, the nylon on the basis of the total weight of the composition
Content be 42-55 weight %, the content of the polyacrylamide is 5-10 weight %, the content of the compatilizer be 5-10 weight
Measure %, the content of the inorganic filler is 0.3-0.6%, the content of the antioxidant is 0.2-0.5 weight %.
6. composition described in any one of -3 according to claim 1, wherein the average grain diameter of the inorganic filler is 500-
5000 mesh, preferably 800-2000 mesh.
7. composition according to claim 5, wherein the inorganic filler be silica, titanium dioxide, glass microballoon,
In at least one of talcum powder, barium sulfate, montmorillonite and silicon powder, preferably silica, titanium dioxide and glass microballoon
It is at least one.
8. composition described in any one of -5 according to claim 1, wherein the antioxidant is four [β-(3,5- bis- uncles
Butyl -4- hydroxy phenyl) propionic acid] pentaerythritol ester, three [2,4- di-tert-butyl-phenyl] phosphite esters and β-(3,5- bis- tertiary fourths
At least one of base -4- hydroxy phenyl) propionic acid n-octadecyl alcohol ester.
9. a kind of preparation method of 3D printing composition, which is characterized in that this method comprises: by 3D printing with composition successively into
Row mixing is granulated and forms.
10. according to the method described in claim 9, wherein, the condition of the granulation includes: that prilling temperature is 190-240 DEG C, excellent
It is selected as 200-230 DEG C.
11. 3D printing material made from method described in claim 9 or 10.
12. 3D printing material is in fusion sediment described in composition described in any one of claim 1-8 or claim 11
Application in method 3D printing.
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