CN114890727A - 3D printing method for high-calcium silicon-based solid waste cementing material - Google Patents
3D printing method for high-calcium silicon-based solid waste cementing material Download PDFInfo
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- CN114890727A CN114890727A CN202210562509.XA CN202210562509A CN114890727A CN 114890727 A CN114890727 A CN 114890727A CN 202210562509 A CN202210562509 A CN 202210562509A CN 114890727 A CN114890727 A CN 114890727A
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- printing
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- solid waste
- based solid
- retarder
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- 239000000463 material Substances 0.000 title claims abstract description 67
- 238000010146 3D printing Methods 0.000 title claims abstract description 50
- 239000002910 solid waste Substances 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title claims abstract description 30
- 239000011575 calcium Substances 0.000 title claims abstract description 28
- 229910052791 calcium Inorganic materials 0.000 title claims abstract description 28
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 28
- 239000010703 silicon Substances 0.000 title claims abstract description 28
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 25
- 239000010881 fly ash Substances 0.000 claims abstract description 18
- 238000007639 printing Methods 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000011812 mixed powder Substances 0.000 claims abstract description 9
- 238000003756 stirring Methods 0.000 claims abstract description 8
- 239000000701 coagulant Substances 0.000 claims abstract description 7
- 238000000465 moulding Methods 0.000 claims abstract description 6
- 239000002562 thickening agent Substances 0.000 claims abstract description 5
- 230000009471 action Effects 0.000 claims abstract description 4
- 150000003839 salts Chemical class 0.000 claims abstract description 4
- 239000007921 spray Substances 0.000 claims abstract description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid group Chemical group C(CC(O)(C(=O)O)CC(=O)O)(=O)O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 60
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 24
- 239000008103 glucose Substances 0.000 claims description 24
- 239000002002 slurry Substances 0.000 claims description 23
- AEQDJSLRWYMAQI-UHFFFAOYSA-N 2,3,9,10-tetramethoxy-6,8,13,13a-tetrahydro-5H-isoquinolino[2,1-b]isoquinoline Chemical compound C1CN2CC(C(=C(OC)C=C3)OC)=C3CC2C2=C1C=C(OC)C(OC)=C2 AEQDJSLRWYMAQI-UHFFFAOYSA-N 0.000 claims description 15
- 239000000176 sodium gluconate Substances 0.000 claims description 15
- 229940005574 sodium gluconate Drugs 0.000 claims description 15
- 235000012207 sodium gluconate Nutrition 0.000 claims description 15
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 6
- 229910052802 copper Inorganic materials 0.000 claims description 6
- 239000010949 copper Substances 0.000 claims description 6
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical group [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims description 6
- 230000005284 excitation Effects 0.000 claims description 5
- 239000003365 glass fiber Substances 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- -1 polypropylene Polymers 0.000 claims description 5
- 239000004743 Polypropylene Substances 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- 239000000835 fiber Substances 0.000 claims description 4
- 125000002791 glucosyl group Chemical group C1([C@H](O)[C@@H](O)[C@H](O)[C@H](O1)CO)* 0.000 claims description 4
- JQJCSZOEVBFDKO-UHFFFAOYSA-N lead zinc Chemical compound [Zn].[Pb] JQJCSZOEVBFDKO-UHFFFAOYSA-N 0.000 claims description 4
- 229920001155 polypropylene Polymers 0.000 claims description 4
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 3
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 3
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 3
- 239000004917 carbon fiber Substances 0.000 claims description 3
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 3
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 claims description 3
- 229910000360 iron(III) sulfate Inorganic materials 0.000 claims description 3
- 229910052698 phosphorus Inorganic materials 0.000 claims description 3
- 239000011574 phosphorus Substances 0.000 claims description 3
- 150000002505 iron Chemical class 0.000 claims description 2
- 230000008901 benefit Effects 0.000 abstract description 3
- 229910000831 Steel Inorganic materials 0.000 abstract 1
- 239000010959 steel Substances 0.000 abstract 1
- 239000000203 mixture Substances 0.000 description 22
- 230000008569 process Effects 0.000 description 8
- 239000002994 raw material Substances 0.000 description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 229910004298 SiO 2 Inorganic materials 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 3
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000000839 emulsion Substances 0.000 description 3
- 239000012188 paraffin wax Substances 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 235000019353 potassium silicate Nutrition 0.000 description 3
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 3
- 238000005507 spraying Methods 0.000 description 3
- 229920001909 styrene-acrylic polymer Polymers 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000000725 suspension Substances 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000004568 cement Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000005345 coagulation Methods 0.000 description 2
- 230000015271 coagulation Effects 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000004570 mortar (masonry) Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000007712 rapid solidification Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- CSDREXVUYHZDNP-UHFFFAOYSA-N alumanylidynesilicon Chemical compound [Al].[Si] CSDREXVUYHZDNP-UHFFFAOYSA-N 0.000 description 1
- 229910000323 aluminium silicate Inorganic materials 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- OSMSIOKMMFKNIL-UHFFFAOYSA-N calcium;silicon Chemical compound [Ca]=[Si] OSMSIOKMMFKNIL-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000002367 phosphate rock Substances 0.000 description 1
- OJMIONKXNSYLSR-UHFFFAOYSA-N phosphorous acid Chemical compound OP(O)O OJMIONKXNSYLSR-UHFFFAOYSA-N 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000011435 rock Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
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- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B28—WORKING CEMENT, CLAY, OR STONE
- B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
- B28B1/00—Producing shaped prefabricated articles from the material
- B28B1/001—Rapid manufacturing of 3D objects by additive depositing, agglomerating or laminating of material
-
- 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
- B33Y10/00—Processes of additive manufacturing
-
- 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
- B33Y70/10—Composites of different types of material, e.g. mixtures of ceramics and polymers or mixtures of metals and biomaterials
-
- 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
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
-
- 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
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
- C04B41/5024—Silicates
-
- 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
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/60—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only artificial stone
- C04B41/61—Coating or impregnation
- C04B41/65—Coating or impregnation with inorganic materials
- C04B41/68—Silicic acid; Silicates
-
- 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
- C04B7/00—Hydraulic cements
- C04B7/14—Cements containing slag
- C04B7/147—Metallurgical slag
-
- 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
- C04B7/00—Hydraulic cements
- C04B7/24—Cements from oil shales, residues or waste other than slag
- C04B7/26—Cements from oil shales, residues or waste other than slag from raw materials containing flue dust, i.e. fly ash
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/91—Use of waste materials as fillers for mortars or concrete
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Inorganic Chemistry (AREA)
- Mechanical Engineering (AREA)
- Civil Engineering (AREA)
- Composite Materials (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The invention discloses a 3D printing method of a high-calcium silicon-based solid waste cementing material, which comprises the steps of mixing the high-calcium silicon-based solid waste with fly ash, and adding a thickening agent and a trivalent ferric salt into dry mixed powder after the dry mixed powder is actively excited under the action of high-voltage current and corresponding pulse frequency to obtain a printing material; adding water into the printing material, stirring and uniformly mixing, sequentially passing the 3D printing cementing material through 4 temperature zones, and then extruding and molding by using a 3D printing spray head, wherein the retarder is respectively added in the first 3 temperature zones, and the coagulant is added at the 4 th temperature; the method has the advantages that the fluidity of the gel material is good, the fluidity can reach 200-250 mm, the curing speed is high, the gel material is suitable for 3D building printing, the mechanical property is excellent, the initial setting time reaches 80-85 min, and the final setting time can reach 90-100 min; after curing for 3 days, the compressive strength of the steel is about to reach 50-60 MPa, the ultimate strain is 1.3% -3.00%, and the tensile strength reaches 6-7 MPa.
Description
Technical Field
The invention belongs to the technical field of 3D printing technology and solid waste recycling, and particularly relates to a 3D printing method for a high-calcium silicon-based solid waste cementing material.
Background
3D printing is also called additive manufacturing, has the characteristics of digitalization and customizability, and is used in the field of buildings without the need of adding materials
The template saves manpower, has high construction speed, has higher building efficiency and economic benefit, and can print various profiled bars. The raw materials used in current 3D printing mainly include polymer materials, metal materials, ceramic materials, and the like. Three printing processes are distinguished according to the characteristics of materials and are divided into the following three types: fused deposition modeling (FMD), Stereolithography (SLA), and three-dimensional printing processes (3 DP). The 3DP process is widely used in the 3D building printing industry due to low material cost. The building materials for 3D printing mostly adopt cement-based mortar at present, and the 3D printing building mortar is prepared by using high-silicon calcium-based solid wastes as raw materials. According to the reports of saving and comprehensive utilization of mineral resources in China (2018), the stock of tailings in China is 195 hundred million t by the end of 2017, and 82% of tailings and waste rocks generated by the mining and separation of iron ore, copper ore, gold ore and phosphorite are shown. Meanwhile, the comprehensive utilization rate of the industrial solid waste is generally low, the added value is not high, and the environmental benefit in the production process is poor, so that the method is a main problem facing the current development of circular economy, promotes the development of the industrial solid waste resource utilization to scale, high-valued and intensive development, and develops a novel solid waste resource technology, so that the method is an effective means for solving the problem of the existing solid waste utilization.
Based on the current situation, a plurality of researchers use the tailings as raw materials to apply in the aspect of 3D printing technology, mainly representing that artware and buildings are printed by using the tailings as raw materials by using the 3D printing technology. The performance requirements of the 3D printing material comprise fluidity, setting time, strength performance, viscosity and the like, and the proper fluidity ensures that the material is smoothly extruded and molded through a printing nozzle through a material conveying pipeline to complete the layer-by-layer stacking of the material; the appropriate setting time ensures that the material will not collapse and deform in the process of stacking, and the material will not block the transportation pipeline. Therefore, the following problems mainly exist in the current 3D printing method by using tailings as raw materials to prepare the cementing material: the poor coagulation performance leads to the difficult adjustment of the coagulation time; the early strength of the material is not high; the material has poor fluidity and is easy to cause pipe blockage.
Disclosure of Invention
Aiming at the problems that the setting time of a high-calcium-based solid waste 3D printing material is difficult to control, the fluidity is low, the material cannot be effectively utilized, the construction period is long, the cost is high and the like, the invention provides a 3D printing method of the high-calcium-silicon-based solid waste cementing material;
the 3D printing method of the high-calcium silicon-based solid waste cementing material comprises the following steps:
(1) mixing 100-150 parts by weight of high-calcium silicon-based solid waste with 40-50 parts by weight of fly ash, and after the dry mixed powder is subjected to active excitation for 25-35 min under the action of high-voltage current and corresponding pulse frequency, adding 3-5 parts by weight of a thickening agent and 10-30 parts by weight of a trivalent iron salt to obtain a printing material;
the high-calcium silicon-based solid waste comprises copper tailings, lead-zinc tailings and phosphorus tailings, the particle size of the high-calcium silicon-based solid waste is 0.3-2.36mm, the water content of the high-calcium silicon-based solid waste is 2-4%, and the fineness modulus of the fly ash is 2.4-2.7;
the high-voltage current is 100-200 kV, and the pulse frequency is 40-80 Hz; the ferric salt is selected from ferric nitrate, ferric sulfate and ferric chloride; the thickening agent is one or more of polypropylene fibers, glass fibers and carbon fibers with the length of 6-9 mm;
(2) adding water into the printing material, and stirring for 10-20 min at 20-60 ℃ to obtain a 3D printing cementing material, wherein the water accounts for 30-40% of the mass of the 3D printing cementing material;
(3) and (3) sequentially passing the 3D printing cementing material through temperature zones of 30-35 ℃, 35-40 ℃, 40-45 ℃ and 20-25 ℃ and then extruding and molding by a 3D printing spray head, wherein a retarder is respectively added in the first 3 temperature zones, a coagulant is added at the 4 th temperature, the molded product is cured, a curing agent is sprayed once every 24 hours, and the final 3D printing product is obtained after curing for 3 days.
The retarder is citric acid with the mass concentration of 2% -5%, glucose with the mass concentration of 45% -50% and sodium gluconate, the ratio of the mass of the glucose solution to the flow mass of the slurry in unit time is 0.10-0.12 in a temperature area of 30-35 ℃ when the retarder is the glucose solution, if the retarder is the sodium gluconate, the addition amount of the sodium gluconate is 0.2% -0.3% of the flow mass of the slurry in unit time, and if the retarder is the citric acid solution, the ratio of the mass of the citric acid solution to the flow mass of the slurry in unit time is 0.3-0.35; in a temperature zone of 35-40 ℃, when the retarder is glucose solution, the ratio of the mass of the glucose solution to the flow mass of the pulp in unit time is 0.07-0.08, if the retarder is sodium gluconate, the addition amount of the sodium gluconate is 0.1-0.15% of the flow mass of the pulp in unit time, and if the retarder is citric acid solution, the ratio of the mass of the citric acid solution to the flow mass of the pulp in unit time is 0.2-0.25; in a temperature zone of 40-45 ℃, when the retarder is glucose solution, the ratio of the mass of the glucose solution to the flow mass of the pulp in unit time is 0.03-0.05, if the retarder is sodium gluconate, the addition amount of the sodium gluconate is 0.03-0.05% of the flow mass of the pulp in unit time, and if the retarder is citric acid solution, the ratio of the mass of the citric acid solution to the flow mass of the pulp in unit time is 0.1-0.15;
the coagulant is fly ash with fineness modulus of 2.5, and the addition amount of the coagulant is 3-5% of the flowing mass of slurry in unit time.
The curing agent is one of paraffin suspension, high polymer styrene-acrylic emulsion and water glass solution, wherein the mass concentration of the paraffin suspension is 40-45%, the mass concentration of the high polymer styrene-acrylic emulsion is 30-35%, and the mass concentration of the water glass solution is 3
5~45%。
Because the high-calcium silicon-based solid waste and the fly ash contain a large amount of silicon and calcium elements, the fly ash has potential active excited substances; after the high-calcium silicon-based solid waste and the fly ash are mechanically ground and sieved, a certain dielectric medium still exists, and according to the electrical property of the dielectric medium, the dry-mixed powder is gradually heated under the action of high-voltage current and corresponding pulse frequency, and then the dry-mixed powder is fed into the reactorThe chemical bonds of the internal structure of the material are broken to achieve the aim of aluminosilicate recombination, and a structural unit consisting of silicon-aluminum-oxygen tetrahedron is formed, but the proportion of silicon dioxide and aluminum oxide is difficult to react completely. The ferric salt added at this time provided Fe 3+ Replacing part of Al in silicon-aluminum tetrahedron structure 3+ Replacing tetrahedral sites in the polymer structure, thus enabling the conversion of industrial solid waste to cementitious materials. For most 3D printing materials, the gelled material has three stages inside a printer conveying pipeline, namely a high-flow dynamic stage, a rapid solidification stage and a stable forming stage, and the chemical condition and the physical condition applied to the outside of the fluidity of each stage are related, so that the fluidity of the slurry in pipeline conveying is controlled by adding a retarder or an accelerant and controlling the temperature. The 3D printing cementing material is in a high-flow state at the initial stage of entering a conveying pipeline, the fluidity is high at the stage, and only part of organic retarder needs to be added to keep the fluidity of the cementing material in the pipeline; the slurry enters a rapid solidification stage along with the passage of time, a retarder needs to be added to prolong the time of the first stage, when the slurry is to be extruded and formed through a 3D printing nozzle, the slurry needs to be rapidly formed, the ratio of raw materials is increased, and the solidification rate is accelerated; after the material is extruded and formed, partial active reaction still exists inside the material, and a certain curing agent is applied, so that the material formed preliminarily can be ensured to be gradually stable.
The gel material has good fluidity, the fluidity can reach 200-250 mm, the curing speed is high, the gel material is suitable for 3D building printing, the mechanical property is excellent, the initial setting time reaches 80-85 min, the final setting time can reach 90-100 min, the compressive strength of the gel material after curing for 3 days is about to reach 50-60 MPa, the ultimate strain is 1.2% -3.00%, and the tensile strength reaches 8-10 MPa.
The method improves the fluidity of the 3D printing material, increases the mechanical property of the material, reduces the use of cement, reduces the preparation cost, reduces the carbon emission, and realizes the transition from industrial solid waste to the value of the 3D printing cementing material of the high-silicon calcium-based material.
The 3D printing method adopted by the material effectively controls the setting time of slurry in the 3D printing process, solves the contradiction between the high flow state performance of the slurry and the stability of the material, and provides a feasible method for controlling the setting time of the cementing material.
Detailed Description
The invention is further illustrated by the following examples, but the scope of the invention is not limited to the following examples, in which the copper tailings mainly comprise: 20-45 wt% of CaO and Al 2 O 3 5~10wt%、SiO 2 35-50 wt% of MgO, 5-10 wt%; the lead-zinc tailings mainly comprise the following components: 30-35 wt% of CaO and Al 2 O 3 5~10wt%、SiO 2 45-50 wt% of ZnO, and 5-10 wt% of ZnO; the phosphorus tailings mainly comprise the following components: 50-55 wt% of CaO, 20-25 wt% of MgO, and SiO 2 10~15wt%、P 2 O 5 5-10 wt%; the fly ash comprises the following main components: SiO 2 2 35~60wt%、Al 2 O 3 15~35wt%、CaO 1~20wt%、Fe 2 O 3 1~15wt%。
Example 1, the method for 3D printing of the high calcium silicon-based solid waste cementing material is as follows:
(1) taking 100g of copper tailings with the particle size of 0.3-2.36mm and 40g of fly ash, feeding the copper tailings and the fly ash into a dry powder stirrer, stirring and mixing at room temperature, wherein the rotating speed of the stirrer is 70 revolutions per minute, the time is 1min, and the dry mixed powder acts for 30min under the conditions of 100kV high-voltage current generated by a pulse high-voltage generator and pulse frequency of 80Hz to perform activity excitation;
(2) adding 12g of ferric sulfate, 3g of polypropylene fiber with the length of 9mm, 1g of glass fiber with the length of 6mm and 1g of carbon fiber with the length of 8mm into the mixture obtained in the step (1), stirring and mixing uniformly, then 100g of water is added and mixed evenly, the mixture is conveyed to a 3D printing platform through a lifting pump and a pipeline, in the conveying process, the mixture passes through temperature zones of 30 ℃, 35 ℃, 40 ℃ and 25 ℃ in sequence, the flow rate is controlled at 2m/s, adding 45 mass% glucose solution into the mixture at 30 deg.C temperature region, wherein the ratio of glucose solution mass to flow mass of the slurry in 1min is 0.10, adding 45 mass% glucose solution into the mixture at 35 deg.C temperature region, wherein the ratio of glucose solution mass to flow mass of the slurry in 1min is 0.07, adding a glucose solution with the mass concentration of 45% into the mixture in a temperature area of 40 ℃, wherein the ratio of the mass of the glucose solution to the flow mass of the slurry in 1min is 0.03; adding fly ash with fineness modulus of 2.5 in a temperature zone of 25 ℃, wherein the addition amount is 3% of the flowing mass of the slurry in 1 min; finally, extruding and molding the mixture from a 3D printing nozzle, wherein the rotating speed of an extruder is 80 r/min;
(3) and (5) curing the molded test block obtained in the step (4) at 20 ℃, spraying 45% paraffin suspension liquid once every 24 hours, and curing for 3 days to obtain a final printed sample.
As a result: testing the cementing material, wherein the initial setting time is 80min, and the final setting time is 90 min; after curing for 3 days, the compressive strength reaches 50MPa, the ultimate strain is 1.3 percent, the tensile strength is 6.3MPa, and the fluidity is 200 mm.
Example 2: the 3D printing method of the high-calcium silicon-based solid waste cementing material comprises the following steps:
(1) taking 120g of lead-zinc tailings with the particle size of 0.5-2.0mm and 45g of fly ash, feeding the mixture into a dry powder stirrer, stirring and mixing at room temperature, wherein the rotating speed of the stirrer is 70 revolutions per minute, the time is 1min, and the dry mixed powder acts for 30min under 150kV high-voltage current generated by a pulse high-voltage generator and the pulse frequency of 60Hz to perform activity excitation;
(2) adding 15g of ferric nitrate, 3g of polypropylene fiber with the length of 6mm and 1g of glass fiber with the length of 7mm into the mixture obtained in the step (1), stirring and mixing uniformly, then 90g of water is added and mixed evenly, the mixture is conveyed to a 3D printing platform through a lifting pump and a pipeline, in the conveying process, the mixture passes through temperature zones of 33 ℃, 35 ℃, 40 ℃ and 25 ℃ in sequence, the flow rate is 2m/s, adding sodium gluconate into the mixture at a temperature of 30 deg.C, wherein the addition amount of sodium gluconate is 0.2% of the flowing mass of the slurry within 1min, adding 45% glucose solution into the mixture at 37 deg.C temperature region, wherein the ratio of glucose solution mass to flow mass of the slurry in 1min is 0.08, when citric acid solution with the mass concentration of 2% is added into the mixture in a temperature zone of 42 ℃, the ratio of the mass of the citric acid solution to the flow mass of the slurry in 1min is 0.1; adding fly ash with fineness modulus of 2.5 in a temperature zone of 20 ℃, wherein the addition amount is 4% of the flowing mass of the slurry in 1 min; finally, extruding and molding the mixture from a 3D printing nozzle, wherein the rotating speed of an extruder is 80 r/min;
(3) and (4) curing the molded test block obtained in the step (4) at 20 ℃, spraying a water glass solution with the mass concentration of 40% every 24 hours, and curing for 3 days to obtain a final printed sample.
As a result: the gelled material is tested, the initial setting time is 85min, the final setting time is 95min, the compressive strength reaches 55MPa after curing for 3 days, the ultimate strain is 1.8%, the tensile strength is 7MPa, and the fluidity is 220 mm.
Example 3: the 3D printing method of the high-calcium silicon-based solid waste cementing material comprises the following steps:
(1) taking 150g of phosphate tailings with the particle size of 1.0-2.3mm and 50g of fly ash, wherein the rotating speed of a stirrer is 70 revolutions per minute, the time is 1min, and the dry mixed powder acts for 30min under the conditions of 200kV high-voltage current generated by a pulse high-voltage generator and pulse frequency of 40Hz to carry out activity excitation;
(2) adding 30g of ferric chloride and 5g of glass fiber with the length of 7mm into the mixture obtained in the step (1), uniformly stirring, adding 120g of water, uniformly mixing, conveying the mixture to a 3D printing platform through a lifting pump and a pipeline, wherein in the conveying process, the mixture sequentially passes through temperature regions of 35 ℃, 40 ℃, 45 ℃ and 22 ℃ and has the flow rate of 2m/s, 3% of citric acid solution is added into the mixture in the temperature region of 35 ℃, the ratio of the mass of the citric acid solution to the flow mass of the pulp in unit time is 0.32, 3% of citric acid solution is added into the mixture in the temperature region of 40 ℃, the ratio of the mass of the citric acid solution to the flow mass of the pulp in unit time is 0.25, and when 40% of glucose solution with the mass concentration of 40% is added into the mixture in the temperature region of 45 ℃, the ratio of the mass of the glucose solution to the flow mass of the pulp in unit time is 0.04; adding fly ash with fineness modulus of 2.5 in a temperature zone of 22 ℃, wherein the addition amount is 5% of the flowing mass of the slurry in 1 min; finally, extruding and molding the mixture from a 3D printing nozzle, wherein the rotating speed of an extruder is 80 r/min;
(3) and (4) curing the molded test block obtained in the step (4) at 20 ℃, spraying a styrene-acrylic emulsion with the mass concentration of 35% every 24 hours, and curing for 3 days to obtain a final printed sample.
As a result: the gelled material is tested, the initial setting time is 83min, the final setting time is 92min, the compressive strength of the gelled material reaches 63MPa after curing for 3 days, the ultimate strain is 3.0%, the tensile strength is 6MPa, and the fluidity is 250 mm.
Claims (6)
1. A3D printing method of a high-calcium silicon-based solid waste cementing material is characterized by comprising the following steps:
(1) mixing 100-150 parts by weight of high-calcium silicon-based solid waste with 40-50 parts by weight of fly ash, and after the dry mixed powder is subjected to active excitation for 25-35 min under the action of high-voltage current and corresponding pulse frequency, adding 3-5 parts by weight of a thickening agent and 10-30 parts by weight of a trivalent iron salt to obtain a printing material;
(2) adding water into the printing material, and stirring for 10-20 min at 20-60 ℃ to obtain a 3D printing cementing material, wherein the water accounts for 30-40% of the mass of the 3D printing cementing material;
(3) and (3) sequentially passing the 3D printing cementing material through temperature zones of 30-35 ℃, 35-40 ℃, 40-45 ℃ and 20-25 ℃ and then extruding and molding by a 3D printing spray head, wherein a retarder is respectively added in the first 3 temperature zones, a coagulant is added at the 4 th temperature, finally, the molded product is cured, a curing agent is sprayed once every 24 hours, and the final 3D printing product is obtained after curing for 3 days.
2. The method for 3D printing of the high-calcium silicon-based solid waste cementing material according to claim 1, is characterized in that: the high-calcium silicon-based solid waste comprises copper tailings, lead-zinc tailings and phosphorus tailings, the particle size of the high-calcium silicon-based solid waste is 0.3-2.36mm, the water content of the high-calcium silicon-based solid waste is 2-4%, and the fineness modulus of the fly ash is 2.4-2.7.
3. The method for 3D printing of the high-calcium silicon-based solid waste cementing material according to claim 1, is characterized in that: the high-voltage current is 100-200 kV, and the pulse frequency is 40-80 Hz.
4. The method for 3D printing of the high-calcium silicon-based solid waste cementing material according to claim 1, is characterized in that: the ferric salt is selected from ferric nitrate, ferric sulfate and ferric chloride; the thickening agent is one or more of polypropylene fibers, glass fibers and carbon fibers with the length of 6-9 mm.
5. The method for 3D printing of the high-calcium silicon-based solid waste cementing material according to claim 2, is characterized in that: the retarder is citric acid with the mass concentration of 2% -5%, glucose with the mass concentration of 45% -50% and sodium gluconate, the ratio of the mass of the glucose solution to the flow mass of the slurry in unit time is 0.10-0.12 in a temperature area of 30-35 ℃, if the retarder is the glucose solution, the addition amount of the sodium gluconate is 0.2% -0.3% of the flow mass of the slurry in unit time, and if the retarder is the citric acid solution, the ratio of the mass of the citric acid solution to the flow mass of the slurry in unit time is 0.3-0.35; in a temperature zone of 35-40 ℃, when the retarder is glucose solution, the ratio of the mass of the glucose solution to the flow mass of the pulp in unit time is 0.07-0.08, if the retarder is sodium gluconate, the addition amount of the sodium gluconate is 0.1-0.15% of the flow mass of the pulp in unit time, and if the retarder is citric acid solution, the ratio of the mass of the citric acid solution to the flow mass of the pulp in unit time is 0.2-0.25; in a temperature zone of 40-45 ℃, when the retarder is glucose solution, the ratio of the mass of the glucose solution to the flow mass of the pulp in unit time is 0.03-0.05, if the retarder is sodium gluconate, the addition amount of the sodium gluconate is 0.03-0.05% of the flow mass of the pulp in unit time, and if the retarder is citric acid solution, the ratio of the mass of the citric acid solution to the flow mass of the pulp in unit time is 0.1-0.15.
6. The method for 3D printing of the high-calcium silicon-based solid waste cementing material according to claim 1, is characterized in that: the coagulant is fly ash with fineness modulus of 2.5, and the addition amount of the coagulant is 3-5% of the flowing mass of slurry in unit time.
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