CN110482983A - A kind of gypsum base 3D printing material and preparation method thereof - Google Patents
A kind of gypsum base 3D printing material and preparation method thereof Download PDFInfo
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- CN110482983A CN110482983A CN201910711676.4A CN201910711676A CN110482983A CN 110482983 A CN110482983 A CN 110482983A CN 201910711676 A CN201910711676 A CN 201910711676A CN 110482983 A CN110482983 A CN 110482983A
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- Prior art keywords
- gypsum
- printing
- slurry
- parts
- material structure
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Links
- 239000010440 gypsum Substances 0.000 title claims abstract description 168
- 229910052602 gypsum Inorganic materials 0.000 title claims abstract description 168
- 238000010146 3D printing Methods 0.000 title claims abstract description 70
- 239000000463 material Substances 0.000 title claims abstract description 48
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 239000011257 shell material Substances 0.000 claims abstract description 34
- 238000000034 method Methods 0.000 claims abstract description 22
- 239000011162 core material Substances 0.000 claims abstract description 19
- 230000005855 radiation Effects 0.000 claims abstract description 8
- 239000002002 slurry Substances 0.000 claims description 85
- 239000011347 resin Substances 0.000 claims description 28
- 229920005989 resin Polymers 0.000 claims description 28
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 claims description 24
- 238000001125 extrusion Methods 0.000 claims description 18
- 239000002250 absorbent Substances 0.000 claims description 17
- 230000002745 absorbent Effects 0.000 claims description 17
- 239000003795 chemical substances by application Substances 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 239000003607 modifier Substances 0.000 claims description 13
- 239000013008 thixotropic agent Substances 0.000 claims description 13
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 12
- 239000001175 calcium sulphate Substances 0.000 claims description 12
- 235000011132 calcium sulphate Nutrition 0.000 claims description 12
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 12
- 230000008719 thickening Effects 0.000 claims description 12
- 239000002994 raw material Substances 0.000 claims description 11
- YTPLMLYBLZKORZ-UHFFFAOYSA-N Thiophene Chemical compound C=1C=CSC=1 YTPLMLYBLZKORZ-UHFFFAOYSA-N 0.000 claims description 10
- 239000011159 matrix material Substances 0.000 claims description 10
- 239000003085 diluting agent Substances 0.000 claims description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 8
- 229910021389 graphene Inorganic materials 0.000 claims description 8
- 239000004575 stone Substances 0.000 claims description 8
- -1 acrylic ester Chemical class 0.000 claims description 7
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 6
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 6
- FGRVOLIFQGXPCT-UHFFFAOYSA-L dipotassium;dioxido-oxo-sulfanylidene-$l^{6}-sulfane Chemical compound [K+].[K+].[O-]S([O-])(=O)=S FGRVOLIFQGXPCT-UHFFFAOYSA-L 0.000 claims description 6
- 239000007789 gas Substances 0.000 claims description 6
- 229920000609 methyl cellulose Polymers 0.000 claims description 6
- 239000001923 methylcellulose Substances 0.000 claims description 6
- 230000008569 process Effects 0.000 claims description 6
- 239000000377 silicon dioxide Substances 0.000 claims description 6
- 230000010148 water-pollination Effects 0.000 claims description 6
- 125000006309 butyl amino group Chemical group 0.000 claims description 5
- 125000004494 ethyl ester group Chemical group 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- 239000011505 plaster Substances 0.000 claims description 5
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 claims description 5
- 229930192474 thiophene Natural products 0.000 claims description 5
- MOMKYJPSVWEWPM-UHFFFAOYSA-N 4-(chloromethyl)-2-(4-methylphenyl)-1,3-thiazole Chemical compound C1=CC(C)=CC=C1C1=NC(CCl)=CS1 MOMKYJPSVWEWPM-UHFFFAOYSA-N 0.000 claims description 4
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 4
- 125000001931 aliphatic group Chemical group 0.000 claims description 4
- 150000004645 aluminates Chemical class 0.000 claims description 4
- 239000007822 coupling agent Substances 0.000 claims description 4
- 235000019983 sodium metaphosphate Nutrition 0.000 claims description 4
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 claims description 4
- 235000019345 sodium thiosulphate Nutrition 0.000 claims description 4
- MYWOJODOMFBVCB-UHFFFAOYSA-N 1,2,6-trimethylphenanthrene Chemical compound CC1=CC=C2C3=CC(C)=CC=C3C=CC2=C1C MYWOJODOMFBVCB-UHFFFAOYSA-N 0.000 claims description 3
- 239000004258 Ethoxyquin Substances 0.000 claims description 3
- 229960000892 attapulgite Drugs 0.000 claims description 3
- 239000000440 bentonite Substances 0.000 claims description 3
- 229910000278 bentonite Inorganic materials 0.000 claims description 3
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims description 3
- 150000001875 compounds Chemical class 0.000 claims description 3
- VFHVQBAGLAREND-UHFFFAOYSA-N diphenylphosphoryl-(2,4,6-trimethylphenyl)methanone Chemical group CC1=CC(C)=CC(C)=C1C(=O)P(=O)(C=1C=CC=CC=1)C1=CC=CC=C1 VFHVQBAGLAREND-UHFFFAOYSA-N 0.000 claims description 3
- DECIPOUIJURFOJ-UHFFFAOYSA-N ethoxyquin Chemical compound N1C(C)(C)C=C(C)C2=CC(OCC)=CC=C21 DECIPOUIJURFOJ-UHFFFAOYSA-N 0.000 claims description 3
- 235000019285 ethoxyquin Nutrition 0.000 claims description 3
- 229940093500 ethoxyquin Drugs 0.000 claims description 3
- UHESRSKEBRADOO-UHFFFAOYSA-N ethyl carbamate;prop-2-enoic acid Chemical compound OC(=O)C=C.CCOC(N)=O UHESRSKEBRADOO-UHFFFAOYSA-N 0.000 claims description 3
- 229910052625 palygorskite Inorganic materials 0.000 claims description 3
- 239000004375 Dextrin Substances 0.000 claims description 2
- 229920001353 Dextrin Polymers 0.000 claims description 2
- 229920002472 Starch Polymers 0.000 claims description 2
- 239000006229 carbon black Substances 0.000 claims description 2
- 235000019425 dextrin Nutrition 0.000 claims description 2
- 239000008107 starch Substances 0.000 claims description 2
- 235000019698 starch Nutrition 0.000 claims description 2
- 125000005396 acrylic acid ester group Chemical group 0.000 claims 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims 1
- 239000006210 lotion Substances 0.000 claims 1
- 239000000203 mixture Substances 0.000 claims 1
- 229910052760 oxygen Inorganic materials 0.000 claims 1
- 239000001301 oxygen Substances 0.000 claims 1
- 238000007639 printing Methods 0.000 abstract description 19
- 238000009833 condensation Methods 0.000 abstract description 5
- 230000005494 condensation Effects 0.000 abstract description 5
- 238000009825 accumulation Methods 0.000 abstract description 4
- 238000001723 curing Methods 0.000 description 16
- 238000007711 solidification Methods 0.000 description 10
- 230000008023 solidification Effects 0.000 description 10
- 238000007599 discharging Methods 0.000 description 8
- 238000010168 coupling process Methods 0.000 description 7
- 238000005859 coupling reaction Methods 0.000 description 7
- 230000000694 effects Effects 0.000 description 7
- 238000007600 charging Methods 0.000 description 6
- MZRQZJOUYWKDNH-UHFFFAOYSA-N diphenylphosphoryl-(2,3,4-trimethylphenyl)methanone Chemical compound CC1=C(C)C(C)=CC=C1C(=O)P(=O)(C=1C=CC=CC=1)C1=CC=CC=C1 MZRQZJOUYWKDNH-UHFFFAOYSA-N 0.000 description 6
- 230000009257 reactivity Effects 0.000 description 5
- XVZXOLOFWKSDSR-UHFFFAOYSA-N Cc1cc(C)c([C]=O)c(C)c1 Chemical group Cc1cc(C)c([C]=O)c(C)c1 XVZXOLOFWKSDSR-UHFFFAOYSA-N 0.000 description 4
- 230000008878 coupling Effects 0.000 description 4
- 238000000465 moulding Methods 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 3
- 239000011230 binding agent Substances 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 239000012530 fluid Substances 0.000 description 3
- WKGDNXBDNLZSKC-UHFFFAOYSA-N oxido(phenyl)phosphanium Chemical compound O=[PH2]c1ccccc1 WKGDNXBDNLZSKC-UHFFFAOYSA-N 0.000 description 3
- 230000001360 synchronised effect Effects 0.000 description 3
- 238000005979 thermal decomposition reaction Methods 0.000 description 3
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 2
- XYFCBTPGUUZFHI-UHFFFAOYSA-N Phosphine Chemical compound P XYFCBTPGUUZFHI-UHFFFAOYSA-N 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 239000006071 cream Substances 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- 239000003805 procoagulant Substances 0.000 description 2
- 238000007493 shaping process Methods 0.000 description 2
- 238000010008 shearing Methods 0.000 description 2
- 125000004469 siloxy group Chemical group [SiH3]O* 0.000 description 2
- 239000002689 soil Substances 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 206010021703 Indifference Diseases 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000000740 bleeding effect Effects 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- CDNGYFJXHJQTJJ-UHFFFAOYSA-N diphenylphosphorylformaldehyde 1,3,5-trimethylbenzene Chemical group C(=O)P(C1=CC=CC=C1)(C1=CC=CC=C1)=O.CC1=CC(=CC(=C1)C)C CDNGYFJXHJQTJJ-UHFFFAOYSA-N 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000010365 information processing Effects 0.000 description 1
- 239000011256 inorganic filler Substances 0.000 description 1
- 229910003475 inorganic filler Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000013178 mathematical model Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 229910000073 phosphorus hydride Inorganic materials 0.000 description 1
- 238000000016 photochemical curing Methods 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002195 synergetic effect Effects 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
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/14—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing calcium sulfate cements
- C04B28/145—Calcium sulfate hemi-hydrate with a specific crystal form
- C04B28/146—Calcium sulfate hemi-hydrate with a specific crystal form alpha-hemihydrate
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/46—Polymerisation initiated by wave energy or particle radiation
- C08F2/48—Polymerisation initiated by wave energy or particle radiation by ultraviolet or visible light
- C08F2/50—Polymerisation initiated by wave energy or particle radiation by ultraviolet or visible light with sensitising agents
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/006—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polymers provided for in C08G18/00
- C08F283/008—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polymers provided for in C08G18/00 on to unsaturated polymers
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/00008—Obtaining or using nanotechnology related materials
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/00034—Physico-chemical characteristics of the mixtures
- C04B2111/00181—Mixtures specially adapted for three-dimensional printing (3DP), stereo-lithography or prototyping
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/50—Mortars, concrete or artificial stone characterised by specific physical values for the mechanical strength
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Health & Medical Sciences (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Structural Engineering (AREA)
- Manufacturing & Machinery (AREA)
Abstract
The present invention provides a kind of gypsum base 3D printing material and preparation method thereof, which is made of shell material structure and the core material structure for being solidificated in shell material inside configuration；Shell material structure is formed during 3D printing through ultraviolet radiation-curable by photopolymer system；Core material structure is formed by curing during 3D printing through infrared radiation by gypsum system；Photopolymer system and gypsum system coaxially squeeze out during 3D printing.Gypsum base 3D printing material of the invention is using the photopolymer system by ultraviolet radiation-curable as shell material structure, using by the cured gypsum system of infrared radiation as core material structure, and using the method coaxially squeezed out while squeezing out photopolymer system and gypsum system, it greatly improves the pure gypsum of tradition and squeezes out the interlaminar strength after condensation, and preferably accumulation property is able to achieve in three-dimensional structure especially Z-direction, simultaneously, it is light-initiated to solidify and the combination of infrared thermal-curable, it is greatly improved printing precision.
Description
Technical field
The present invention relates to 3D printing technique field, in particular to a kind of gypsum base 3D printing material and preparation method thereof.
Background technique
3D printing technique, that is, three-dimensional fast shaping printing, by the input of mathematical model, and the layering to solid figure
Discrete processes possess a variety of molding modes such as extrusion, powder bed, liquid bed, photocuring.3D printing technique be related to material science,
The multi-disciplinary intersection such as information processing, Electromechanical Control, by computer to the journey of the accurate drafting and 3D printer of moulded dimension
Sequence control forms to realize that indifference is positioned with accurate.And all have broad application prospects in industries such as building, traffic, medical treatment,
It is the new industry plan of 21 century.
Currently, organic polymer class material has many advantages, such as that wear-resisting, plasticity is strong and printing precision is high, but its tensile strength
It is low with heat distortion temperature so that using have significant limitation；Metal material mechanics performance and chemical property are excellent, and material is high
It is expensive, generally from great and improve printing difficulty to temperature requirement is higher；Inorganic non-metallic material gypsum source is wide, price is low
Honest and clean, mechanical strength and good biocompatibility, but it is easy to appear during gypsum base 3D printing extrusion molding that accumulation property is poor, beats
Print the problems such as precision is low low with bond strength between layers after solidification.
Summary of the invention
In view of this, the present invention is directed to propose a kind of gypsum base 3D printing material, to solve existing gypsum base 3D printing material
Expect accumulation property is poor, printing precision is low during extrusion molding, solidify after the low problem of bond strength between layers.
In order to achieve the above objectives, the technical scheme of the present invention is realized as follows:
A kind of gypsum base 3D printing material, by shell material structure and the core material structure group for being solidificated in the shell material inside configuration
At；The shell material structure is formed during 3D printing through ultraviolet radiation-curable by photopolymer system；The core material structure
It is formed by curing during 3D printing through infrared radiation by gypsum system；The photopolymer system and the gypsum system exist
It is coaxial during 3D printing to squeeze out.
Optionally, by weight, the photopolymer system includes following components: photosensitive resin matrix: 30-50 parts,
Photoinitiator: 0.1-1.2 parts, UV blockers: 0.05-1.0 parts, reactive diluent: 15-25 parts, oligomer: 35-45 parts,
Resin-gypsum interface modifier: 0.6-6.0 parts.
Optionally, the photosensitive resin matrix is acrylic ester prepolymer；The photoinitiator is 2,4,6- trimethylbenzene
Formyl diphenyl phosphine oxide；The UV blockers are bis- (5- tert-butyl -2- benzoxazoles) thiophene of 2,5-；The activity is dilute
Releasing agent is 2- acrylic acid -2- [[(butylamino)-carbonyl] oxo] ethyl ester；The oligomer is aliphatic polyurethane acrylic acid
One of ester, ethoxyquin pentaerythritol tetraacrylate；The resin-gypsum interface modifier is silane coupling agent, liquid
One of aluminate coupling agent.
Optionally, the acrylic ester prepolymer is 80%-90% to the transmitance of infrared ray.
Optionally, by weight, the gypsum system includes following components: gypsum: 50-70 parts, water: and 15-30 parts, stone
Cream retarder: 0.1-5.0 parts, gypsum thickening water-retaining agent: 0.5-6.0 parts, gypsum thixotropic agent: 1.0-8.0 parts, the infrared heat absorption of gypsum
Agent: 1.0-6.0 parts, the thermotropic accelerator of gypsum: 0.8-6.0 parts.
Optionally, the gypsum is alpha-semi water plaster stone；The calcium sulphate retarder is that sodium metaphosphate, citric acid, protide are multiple
Close one of retarder or a variety of；The gypsum thickening water-retaining agent is one of methylcellulose, dextrin, bentonite or more
Kind；The gypsum thixotropic agent is one of attapulgite, hydrophily gas phase nano silica, starch ether or a variety of；It is described
The infrared heat absorbent of gypsum is one of carbon black, graphene oxide or a variety of；The thermotropic accelerator of gypsum be potassium thiosulfate,
One of sodium thiosulfate.
Optionally, absorptivity >=95% of the infrared heat absorbent of the gypsum to infrared wavelength light source.
The second object of the present invention is to provide a kind of method for preparing above-mentioned gypsum base 3D printing material, the preparation method
The following steps are included:
1) raw material of the photopolymer system is mixed to form slurry A, the raw material of the gypsum system is mixed to form
Slurry B；
2) 3D printer is used, squeezes out the slurry A in a manner of pressurizeing and squeeze out, is squeezed out in a manner of Screw Extrusion described
Slurry B, the slurry A and the slurry B are coaxially squeezed out, and in extrusion process, the slurry A is through ultraviolet around 3D printing platform
Light irradiation is formed by curing shell material structure, and the slurry B is radiated at the shell material structure through infrared light supply around 3D printing platform
Internal curing forms core material structure.
Optionally, the feed rate of the slurry A is 0.157-2.512mL/min, and the feed rate of the slurry B is
6.28-15.7mL/min。
Compared with the existing technology, gypsum base 3D printing material of the present invention has the advantage that
1, gypsum base 3D printing material of the invention is using the photopolymer system by ultraviolet radiation-curable as shell material knot
Structure, as core material structure, and using the method coaxially squeezed out while being squeezed out photosensitive by the cured gypsum system of infrared radiation
Resin system and gypsum system, on the one hand, can make greatly to improve tradition by photosensitive resin solidification bonding between layers
Pure gypsum squeezes out the interlaminar strength after condensation and is on the other hand able to achieve better accumulation in three-dimensional structure especially Z-direction
Property, good technical foundation is provided for extensive component or ornament printing, and coaxial squeeze out is greatly improved gypsum base 3D
The shaping efficiency of printed material, meanwhile, it is light-initiated to solidify and the combination of infrared thermal-curable, it is greatly improved printing precision, separately
Outside, the present invention can avoid causing to collapse because of the self weight of printed material using cured photopolymer system as shell material structure,
And then realize the printing of hanging structure.
2, the preparation method of gypsum base 3D printing material of the present invention is simple, easy to industrialized production.
Detailed description of the invention
The attached drawing for constituting a part of the invention is used to provide further understanding of the present invention, schematic reality of the invention
It applies example and its explanation is used to explain the present invention, do not constitute improper limitations of the present invention.In the accompanying drawings:
Fig. 1 is coaxially to squeeze out single unit system top view in gypsum base 3D printing material preparation process of the present invention；
Fig. 2 is extruder, charging, discharging and printing equipment figure in gypsum base 3D printing material preparation process of the present invention；
Fig. 3 is coaxial extruder head sectional view in gypsum base 3D printing material preparation process of the present invention.
Description of symbols:
1- is ultraviolet-infrared light supply, 2- extruder, charging, discharging and printing equipment, 3-3D print platform, the charging of 4- gypsum
Mouth, 5- resin feeding mouth, the coaxial extruder head of 6-, 7- extruder, 8- shaft coupling, 9- screw rod, 10- gypsum discharge port, 11- resin go out
Material mouth.
Specific embodiment
It should be noted that in the absence of conflict, the feature in embodiment and embodiment in the present invention can phase
Mutually combination.
Below in conjunction with drawings and examples, the present invention will be described in detail.
Embodiment 1
A kind of gypsum base 3D printing material is made of shell material structure and the core material structure for being solidificated in shell material inside configuration；Shell
Material structure is formed during 3D printing through ultraviolet radiation-curable by photopolymer system；Core material structure is by gypsum system in 3D
It is formed by curing in print procedure through infrared radiation；Photopolymer system and gypsum system coaxially squeeze out during 3D printing.
Wherein, by weight, photopolymer system includes following components: photosensitive resin matrix: 40 parts, photoinitiator:
0.4 part, UV blockers: 0.2 part, reactive diluent: 20 parts, oligomer: 36 parts, resin-gypsum interface modifier: 2 parts,
And photosensitive resin matrix is acrylic ester prepolymer, photoinitiator 2,4,6- trimethylbenzoyl two in photopolymer system
Phenyl phosphine oxide (TPO), UV blockers 2, bis- (5- tert-butyl -2- benzoxazoles) thiophene (OB+) of 5-；Reactive diluent
For 2- acrylic acid -2- [[(butylamino)-carbonyl] oxo] ethyl ester；Oligomer is aliphatic urethane acrylate (Ebecryl
8210)；Resin-gypsum interface modifier is silane coupling agent.In addition, in order to have good solidification effect, acrylate prepolymer
Object is preferably 80%-90% to the transmitance of infrared ray；
By weight, gypsum system includes following components: gypsum: 60 parts, water: and 20 parts, calcium sulphate retarder: 4 parts, gypsum
Thickening water-retaining agent: 5 parts, gypsum thixotropic agent: 6 parts, the infrared heat absorbent of gypsum: 3 parts, the thermotropic accelerator of gypsum: 2 parts, and in gypsum
Gypsum is high-strength alpha-semi water plaster stone in system, and calcium sulphate retarder is citric acid, and it is methylcellulose, stone that gypsum, which thickens water-retaining agent,
Cream thixotropic agent is attapulgite, and the infrared heat absorbent of gypsum is graphene oxide, and the thermotropic accelerator of gypsum is sodium thiosulfate, separately
Outside, in order to there is good solidification effect, the infrared heat absorbent of gypsum is preferably >=95% to the absorptivity of infrared wavelength light source.
In conjunction with shown in Fig. 1, Fig. 2 and Fig. 3, above-mentioned gypsum base 3D printing material is made especially by following methods:
1) said ratio is pressed, the raw material of photopolymer system is mixed to form slurry A, the raw material of gypsum system is mixed into shape
The slurry B for being 2.3-2.4kg/L at density, wherein slurry B and slurry A pass through gypsum feed inlet 4 and resin feeding mouth 5 respectively
Feed, extruder, charging, discharging and printing equipment 2 can be synchronous mobile in X, Y, Z axis direction；
2) it drives shaft coupling 8 to rotate using the extruder 7 in 3D printer, squeezes out slurry A in a manner of pressurizeing and squeeze out, and
The feed rate of control slurry A squeezes out slurry B by screw rod 9 for 0.157-2.512mL/min in a manner of Screw Extrusion, and
The feed rate for controlling slurry B is that 6.28-15.7mL/min, slurry A and slurry B are coaxially squeezed out by coaxial extruder head 6, respectively
It discharges from resin discharge port 11 and gypsum discharge port 10, and in extrusion process, slurry A is through ultraviolet-infrared around 3D printing platform 3
Ultraviolet light in light source 1 is formed by curing the shell material structure of some strength in 3s, and slurry B is purple through 3 surrounding of 3D printing platform
The initial set in 4min of Infrared irradiation in outside-infrared light supply 1 is formed by curing core material structure, and is fixed by the support of shell material structure
It is molded over the inside of shell material structure；
3) slurry B, slurry A are constantly conveyed respectively to gypsum feed inlet 4 and resin feeding mouth 5, repeat the above steps, until
Printing terminates, cleaning plant.
In the present embodiment, the siloxy in slurry A as resin-gypsum interface modifier silane coupling agent is to nothing
Machine object has reactivity, and organic functional base has reactivity or compatibility to photosensitive resin, so as to form photosensitive resin-coupling
Agent-gypsum binder course；2,4,6- trimethylbenzoyl diphenyl phosphine oxide (TPO) as photoinitiator can make slurry A quick
Solidification；Sodium thiosulfate as the thermotropic accelerator of gypsum can be discharged procoagulant Factor (sulfate ion) by thermal decomposition, with work
It acts synergistically for the graphene oxide of the infrared heat absorbent of gypsum, makes slurry B can rapid curing；Concave convex rod as gypsum thixotropic agent
Soil can make the extrusion force of slurry B in 0.1-5.0N, apparent viscosity 0.2-14.0PaS, realize that fluid shearing is thinning and stablizes
Discharging molding；The thickening water retention property of slurry B can be improved in methylcellulose as gypsum thickening water-retaining agent, prevents bleeding existing
As occurring；Citric acid as calcium sulphate retarder can prevent condensation during slurry pipeline steel from printing being caused to terminate.
The mechanical property of the gypsum base 3D printing material of the present embodiment is tested.
After tested it is found that the tensile strength of the gypsum base 3D printing material of the present embodiment is 7MPa.
Embodiment 2
A kind of gypsum base 3D printing material is made of shell material structure and the core material structure for being solidificated in shell material inside configuration；Shell
Material structure is formed during 3D printing through ultraviolet radiation-curable by photopolymer system；Core material structure is by gypsum system in 3D
It is formed by curing in print procedure through infrared radiation；Photopolymer system and gypsum system coaxially squeeze out during 3D printing.
Wherein, by weight, photopolymer system includes following components: photosensitive resin matrix: 45 parts, photoinitiator:
0.8 part, UV blockers: 0.2 part, reactive diluent: 18 parts, oligomer: 35 parts, resin-gypsum interface modifier: 1 part,
And photosensitive resin matrix is acrylic ester prepolymer, photoinitiator 2,4,6- trimethylbenzoyl two in photopolymer system
Phenyl phosphine oxide (TPO), UV blockers 2, bis- (5- tert-butyl -2- benzoxazoles) thiophene (OB+) of 5-, reactive diluent
For 2- acrylic acid -2- [[(butylamino)-carbonyl] oxo] ethyl ester, oligomer is aliphatic urethane acrylate (Ebecryl
8210), resin-gypsum interface modifier is silane coupling agent.In addition, in order to have good solidification effect, acrylate prepolymer
Object is preferably 80%-90% to the transmitance of infrared ray；
By weight, gypsum system includes following components: gypsum: 60 parts, water: and 20 parts, calcium sulphate retarder: 2 parts, gypsum
Thickening water-retaining agent: 5 parts, gypsum thixotropic agent: 5 parts, the infrared heat absorbent of gypsum: 5 parts, the thermotropic accelerator of gypsum: 3 parts, and in gypsum
Gypsum is high-strength alpha-semi water plaster stone in system, and calcium sulphate retarder is protide compound retarder, and it is swollen that gypsum, which thickens water-retaining agent,
Profit soil, gypsum thixotropic agent are hydrophily gas phase nano silica, and the infrared heat absorbent of gypsum is graphene oxide, the thermotropic speed of gypsum
Solidifying agent is potassium thiosulfate, in addition, in order to have good solidification effect, absorption of the infrared heat absorbent of gypsum to infrared wavelength light source
Rate is preferably >=95%.
In conjunction with shown in Fig. 1, Fig. 2 and Fig. 3, above-mentioned gypsum base 3D printing material is made especially by following methods:
1) said ratio is pressed, the raw material of photopolymer system is mixed to form slurry A, the raw material of gypsum system is mixed into shape
The slurry B for being 2.3-2.4kg/L at density, wherein slurry B and slurry A pass through gypsum feed inlet 4 and resin feeding mouth 5 respectively
Feed, extruder, charging, discharging and printing equipment 2 can be synchronous mobile in X, Y, Z axis direction；
2) it drives shaft coupling 8 to rotate using the extruder 7 in 3D printer, squeezes out slurry A in a manner of pressurizeing and squeeze out, and
The feed rate of control slurry A squeezes out slurry B by screw rod 9 for 0.157-2.512mL/min in a manner of Screw Extrusion, and
The feed rate for controlling slurry B is that 6.28-15.7mL/min, slurry A and slurry B are coaxially squeezed out by coaxial extruder head 6, respectively
It discharges from resin discharge port 11 and gypsum discharge port 10, and in extrusion process, slurry A is through ultraviolet-infrared around 3D printing platform 3
Ultraviolet light in light source 1 is formed by curing the shell material structure of some strength in 2s, and slurry B is purple through 3 surrounding of 3D printing platform
The initial set in 3min of Infrared irradiation in outside-infrared light supply 1 is formed by curing core material structure, and is fixed by the support of shell material structure
It is molded over the inside of shell material structure；
3) slurry B, slurry A are constantly conveyed respectively to gypsum feed inlet 4 and resin feeding mouth 5, repeat the above steps, until
Printing terminates, cleaning plant.
In the present embodiment, the siloxy in slurry A as resin-gypsum interface modifier silane coupling agent is to nothing
Machine object has reactivity, and organic functional base has reactivity or compatibility to photosensitive resin, so as to form photosensitive resin-coupling
Agent-gypsum binder course；2,4,6- trimethylbenzoyl diphenyl phosphine oxide (TPO) as photoinitiator can make slurry A quick
Solidification；Potassium thiosulfate as the thermotropic accelerator of gypsum can be discharged procoagulant Factor (sulfate ion) by thermal decomposition, with work
It acts synergistically for the graphene oxide of the infrared heat absorbent of gypsum, makes slurry B can rapid curing；Hydrophily as gypsum thixotropic agent
Gas phase nano silica can make the extrusion force of slurry B in 0.1-5.0N, apparent viscosity 0.2-14.0PaS, realize fluid
Shear shinning and stable discharging molding；The thickening water retention property of slurry B can be improved in bentonite as gypsum thickening water-retaining agent,
Prevent excreting water phenomenon from occurring；Protide compound retarder as calcium sulphate retarder can prevent condensation during slurry pipeline steel from causing
Printing terminates.
The mechanical property of the gypsum base 3D printing material of the present embodiment is tested.
After tested it is found that the tensile strength of the gypsum base 3D printing material of the present embodiment is 6MPa.
Embodiment 3
A kind of gypsum base 3D printing material is made of shell material structure and the core material structure for being solidificated in shell material inside configuration；Shell
Material structure is formed during 3D printing through ultraviolet radiation-curable by photopolymer system；Core material structure is by gypsum system in 3D
It is formed by curing in print procedure through infrared radiation；Photopolymer system and gypsum system coaxially squeeze out during 3D printing.
Wherein, by weight, photopolymer system includes following components: photosensitive resin matrix: 50 parts, photoinitiator:
0.4 part, UV blockers: 0.2 part, reactive diluent: 17 parts, oligomer: 30 parts, resin-gypsum interface modifier: 2 parts,
And photosensitive resin matrix is acrylic ester prepolymer, photoinitiator 2,4,6- trimethylbenzoyl two in photopolymer system
Phenyl phosphine oxide (TPO), UV blockers 2, bis- (5- tert-butyl -2- benzoxazoles) thiophene (OB+) of 5-, reactive diluent
For 2- acrylic acid -2- [[(butylamino)-carbonyl] oxo] ethyl ester, oligomer is ethoxyquin pentaerythritol tetraacrylate
(Sartomer SR 494), resin-gypsum interface modifier are liquid aluminate coupling agent.In addition, in order to there is good solidification
Effect, acrylic ester prepolymer are preferably 80%-90% to the transmitance of infrared ray；
By weight, gypsum system includes following components: gypsum: 60 parts, water: and 20 parts, calcium sulphate retarder: 2 parts, gypsum
Thickening water-retaining agent: 5 parts, gypsum thixotropic agent: 5 parts, the infrared heat absorbent of gypsum: 5 parts, the thermotropic accelerator of gypsum: 3 parts, and in gypsum
Gypsum is high-strength alpha-semi water plaster stone in system, and calcium sulphate retarder is sodium metaphosphate, and it is methylcellulose that gypsum, which thickens water-retaining agent,
Gypsum thixotropic agent is hydrophily gas phase nano silica, and the infrared heat absorbent of gypsum is graphene oxide, the thermotropic accelerator of gypsum
For potassium thiosulfate, in addition, in order to there is good solidification effect, the infrared heat absorbent of gypsum is excellent to the absorptivity of infrared wavelength light source
It is selected as >=95%.
In conjunction with shown in Fig. 1, Fig. 2 and Fig. 3, above-mentioned gypsum base 3D printing material is made especially by following methods:
1) said ratio is pressed, the raw material of photopolymer system is mixed to form slurry A, the raw material of gypsum system is mixed into shape
The slurry B for being 2.3-2.4kg/L at density, wherein slurry B and slurry A pass through gypsum feed inlet 4 and resin feeding mouth 5 respectively
Feed, extruder, charging, discharging and printing equipment 2 can be synchronous mobile in X, Y, Z axis direction；
2) it drives shaft coupling 8 to rotate using the extruder 7 in 3D printer, squeezes out slurry A in a manner of pressurizeing and squeeze out, and
The feed rate of control slurry A squeezes out slurry B by screw rod 9 for 0.157-2.512mL/min in a manner of Screw Extrusion, and
The feed rate for controlling slurry B is that 6.28-15.7mL/min, slurry A and slurry B are coaxially squeezed out by coaxial extruder head 6, respectively
It discharges from resin discharge port 11 and gypsum discharge port 10, and in extrusion process, slurry A is through ultraviolet-infrared around 3D printing platform 3
Ultraviolet light in light source 1 is formed by curing the shell material structure of some strength in 3s, and slurry B is purple through 3 surrounding of 3D printing platform
The initial set in 3min of Infrared irradiation in outside-infrared light supply 1 is formed by curing core material structure, and is fixed by the support of shell material structure
It is molded over the inside of shell material structure；
3) slurry B, slurry A are constantly conveyed respectively to gypsum feed inlet 4 and resin feeding mouth 5, repeat the above steps, until
Printing terminates, cleaning plant.
In the present embodiment, containing in slurry A as resin-gypsum interface modifier liquid aluminate coupling agent can be with
The group of active hydrogen reaction, thus bonding action, You Jiguan can occur with the inorganic filler of hydroxyl, carboxyl or surface adsorption water
Can base to photosensitive resin have reactivity or compatibility, the compatibility that can be effectively improved between gypsum slurry and photosensitive resin interface,
So as to form photosensitive resin-coupling agent-gypsum binder course；2,4,6- trimethylbenzoyl dipheny oxide as photoinitiator
Slurry A rapid curing can be made by changing phosphine (TPO)；Potassium thiosulfate as the thermotropic accelerator of gypsum can be promoted by thermal decomposition release it is solidifying because
Sub (sulfate ion), the graphene oxide synergistic effect with as the infrared heat absorbent of gypsum, makes slurry B can rapid curing；
Hydrophily gas phase nano silica as gypsum thixotropic agent can make the extrusion force of slurry B in 0.1-5.0N, and apparent viscosity is
0.2-14.0PaS realizes the thinning and stable discharging molding of fluid shearing；Methylcellulose as gypsum thickening water-retaining agent
The thickening water retention property that slurry B can be improved, prevents excreting water phenomenon from occurring；Sodium metaphosphate as calcium sulphate retarder can prevent slurry
Condensation causes printing to terminate in transmission process.
The mechanical property of the gypsum base 3D printing material of the present embodiment is tested.
After tested it is found that the tensile strength of the gypsum base 3D printing material of the present embodiment is 8MPa.
Comparative example 1
A kind of gypsum base 3D printing material, by weight, including following components: gypsum: 60 parts, water: 40 parts.
The 3D printing method of the gypsum base 3D printing material are as follows: matched according to above-mentioned raw materials, be made into slurry, then, used
3D printer squeezes out slurry in a manner of Screw Extrusion, and the feed rate for controlling slurry is 6.28-15.7mL/min, in 3D
The presetting period of slurry is 8min in print procedure.
The mechanical property of the gypsum base 3D printing material of this comparative example is tested.
After tested it is found that the tensile strength of the gypsum base 3D printing material of this comparative example is 0.6MPa.
The above is merely preferred embodiments of the present invention, be not intended to limit the invention, it is all in spirit of the invention and
Within principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (9)
1. a kind of gypsum base 3D printing material, which is characterized in that by shell material structure and the core for being solidificated in the shell material inside configuration
Material structure composition；The shell material structure is formed during 3D printing through ultraviolet radiation-curable by photopolymer system；It is described
Core material structure is formed by curing during 3D printing through infrared radiation by gypsum system；The photopolymer system and the stone
Lotion ties up to coaxial extrusion during 3D printing.
2. gypsum base 3D printing material according to claim 1, which is characterized in that by weight, the photosensitive resin
System includes following components: photosensitive resin matrix: 30-50 parts, photoinitiator: and 0.1-1.2 parts, UV blockers: 0.05-
1.0 parts, reactive diluent: 15-25 parts, oligomer: 35-45 parts, resin-gypsum interface modifier: 0.6-6.0 parts.
3. gypsum base 3D printing material according to claim 2, which is characterized in that the photosensitive resin matrix is acrylic acid
Ester prepolymer；The photoinitiator is 2,4,6- trimethylbenzoyl diphenyl phosphine oxide；The UV blockers are 2,5-
Bis- (5- tert-butyl -2- benzoxazoles) thiophene；The reactive diluent is 2- acrylic acid -2- [[(butylamino)-carbonyl] oxygen
Generation] ethyl ester；The oligomer is one of aliphatic urethane acrylate, ethoxyquin pentaerythritol tetraacrylate；Institute
Stating resin-gypsum interface modifier is one of silane coupling agent, liquid aluminate coupling agent.
4. gypsum base 3D printing material according to claim 3, which is characterized in that the acrylic ester prepolymer is to infrared
The transmitance of line is 80%-90%.
5. gypsum base 3D printing material according to claim 1, which is characterized in that by weight, the gypsum system
Including following components: gypsum: 50-70 parts, water: 15-30 parts, calcium sulphate retarder: 0.1-5.0 parts, gypsum thickens water-retaining agent: 0.5-
6.0 parts, gypsum thixotropic agent: 1.0-8.0 parts, the infrared heat absorbent of gypsum: 1.0-6.0 parts, the thermotropic accelerator of gypsum: 0.8-6.0 parts.
6. gypsum base 3D printing material according to claim 5, which is characterized in that the gypsum is alpha-semi water plaster stone；Institute
Stating calcium sulphate retarder is one of sodium metaphosphate, citric acid, protide compound retarder or a variety of；The gypsum thickening water conservation
Agent is one of methylcellulose, dextrin, bentonite or a variety of；The gypsum thixotropic agent is attapulgite, hydrophily gas phase
One of nano silica, starch ether are a variety of；The infrared heat absorbent of gypsum is one of carbon black, graphene oxide
Or it is a variety of；The thermotropic accelerator of gypsum is one of potassium thiosulfate, sodium thiosulfate.
7. gypsum base 3D printing material according to claim 6, which is characterized in that the infrared heat absorbent of gypsum is to infrared
Absorptivity >=95% of wavelength light source.
8. the method for preparing the described in any item gypsum base 3D printing materials of claim 1 to 7, which is characterized in that including following
Step:
1) raw material of the photopolymer system is mixed to form slurry A, the raw material of the gypsum system is mixed to form slurry
B；
2) 3D printer is used, the slurry A is squeezed out in a manner of pressurizeing and squeeze out, the slurry is squeezed out in a manner of Screw Extrusion
B, the slurry A and the slurry B are coaxially squeezed out, and in extrusion process, the slurry A is through ultraviolet lighting around 3D printing platform
It penetrates and is formed by curing shell material structure, the slurry B is radiated at the inside of the shell material structure through infrared light supply around 3D printing platform
It is formed by curing core material structure.
9. the preparation method of gypsum base 3D printing material according to claim 8, which is characterized in that the slurry A into
Material rate is 0.157-2.512mL/min, and the feed rate of the slurry B is 6.28-15.7mL/min.
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