CN113149579A - Preparation method of super-gelling cement for 3D printing and super-gelling cement for 3D printing - Google Patents
Preparation method of super-gelling cement for 3D printing and super-gelling cement for 3D printing Download PDFInfo
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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
- C04B28/02—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 hydraulic cements other than calcium sulfates
- C04B28/06—Aluminous cements
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y70/00—Materials specially adapted for additive manufacturing
- B33Y70/10—Composites of different types of material, e.g. mixtures of ceramics and polymers or mixtures of metals and biomaterials
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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
- 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
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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
- 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
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Abstract
The invention provides a preparation method of super-gelling cement for 3D printing and the super-gelling cement for 3D printing prepared by the method. The preparation method of the super-gelling cement for 3D printing provided by the invention comprises the following steps: the method comprises the following steps: putting 100-150 parts by weight of aluminate cement, 400-600 parts by weight of water and 2-8 parts by weight of grinding aid into a ball mill, and wet-grinding to obtain nano slurry A; step two: carrying out liquid phase grinding on 380-475 parts by weight of silicate cement clinker, 20-25 parts by weight of gypsum, 120-180 parts by weight of water, 10-30 parts by weight of superfine ceramic fiber and 1-5 parts by weight of water reducer to obtain slurry B; step three: and adding the nano slurry A, 1-10 parts by weight of interface reinforcing agent and 15-40 parts by weight of basalt fiber into the slurry B, and mixing to obtain the super-gelling cement for 3D printing. The super-gelling cement for 3D printing provided by the invention is easy to realize mass production, is efficient in wet grinding, and can enable 3D printing to have quick-setting and easy-printing performance, high compressive strength and excellent later-period performance.
Description
Technical Field
The invention belongs to the technical field of building materials, and relates to a preparation method of super-gelling cement for 3D printing and the super-gelling cement for 3D printing prepared by the method.
Background
The 3D printing technology is a new material preparation technology developed in the last 30 years, and is considered as an important production tool of the third industrial revolution. Meanwhile, 3D printing of cement-based materials is also remarkably developed and popularized, and the method is successfully applied to the building fields of house construction, underground engineering, roads, bridges and the like and has great development potential. The 3D printing technology and the traditional material preparation technology have the greatest advantages that the speed is high, templates and a large number of workers are not needed, integral forming can be achieved, a series of complex steps are reduced, the preparation efficiency is greatly improved, and the waste of resources is reduced.
However, at present, the cement-based 3D printing technology is still in the beginning stage, and there is no comprehensive research on materials, equipment, process systems, and the like, especially on materials. The existing 3D printing cement material has some defects, which are mainly shown in that the problems of collapse, deformation and the like of the printing material are easy to occur after the printing material falls due to the defects of low early strength, long setting time, poor material fluidity, difficulty in adhesion and the like, and in the later stage of cement hydration, the volume stability and the durability of a 3D printing component are influenced due to shrinkage cracks caused by the volume shrinkage of hardened cement paste.
CN105731942A discloses a cement-based composite material for 3D printing, and a preparation method and an application thereof, wherein the cement-based composite material comprises the following components in percentage by weight: composite gelled material: 19 to 25 percent; shrinkage inhibitor: 0.2 to 0.6 percent; anti-carbonization agent: 1 to 2 percent; aggregate: 57-66%; fiber reinforced material: 0.3-1.1%; liquid alkali-free accelerator: 0.9 to 1.8 percent; retarder: 0.8-1.7%; thickening agent: 0.02-2%; plastic-keeping agent: 0.2 to 0.4 percent; defoaming agent: 0.04-0.09%; water reducing agent: 0.04-0.2%; water: 5 to 14 percent. The cement-based composite material for 3D printing provided by the invention has various components, is complex in dosage, is difficult to control and is inconvenient for large-area production.
CN111393046A discloses a high performance 3D printing cement, which comprises, by weight, 80% -100% of silicate gel material and 0% -20% of high belite sulphoaluminate cement. The preparation method of the high-performance 3D printing cement comprises the following steps: mixing the mixture of the special cement clinker and the gypsum and the mixed material, and adding a grinding aid to grind into a silicate cementing material; extracting the high belite sulphoaluminate cement according to the corresponding formula amount; and uniformly mixing the silicate cementing material and the high belite sulphoaluminate cement to prepare the high-performance 3D printing cement. Said invention adopts mixing dry grinding, and its grinding efficiency is low, energy consumption is high and economic benefit is low.
Disclosure of Invention
The invention aims to provide a super-cementing material for 3D printing, which is easy to produce in quantity, high in wet grinding efficiency, and capable of enabling 3D printing to have quick-setting and easy-printing performance, high compressive strength and excellent later-period performance, aiming at the problems that the existing cement-based material cementing material for 3D printing has various components, is complex in dosage, difficult to control and inconvenient to produce in quantity, and the grinding efficiency is low, the energy consumption is high and the economic benefit is low due to dry grinding.
The invention provides a preparation method of super-gelling cement for 3D printing, which comprises the following steps:
the method comprises the following steps: putting 100-150 parts by weight of aluminate cement, 400-600 parts by weight of water and 2-8 parts by weight of grinding aid into a ball mill, and wet-grinding to obtain nano slurry A;
step two: carrying out liquid phase grinding on 380-475 parts by weight of silicate cement clinker, 20-25 parts by weight of gypsum, 120-180 parts by weight of water, 10-30 parts by weight of superfine ceramic fiber and 1-5 parts by weight of water reducer to obtain slurry B;
step three: and adding the nano slurry A, 1-10 parts by weight of interface reinforcing agent and 15-40 parts by weight of basalt fiber into the slurry B, and mixing to obtain the super-gelling cement for 3D printing.
The invention also provides the super-gelling cement for 3D printing, which is prepared by the preparation method of the super-gelling cement for 3D printing.
The beneficial effects of the invention include:
1. the 3D printing super-gelled cement can accurately regulate and control the setting time and flow thixotropy, and has excellent building performance. The fresh slurry of the material has good plasticity, adhesive force and plastic deformation resistance, the phenomena of flowing and collapsing can not occur in the lamination application construction, the lateral deformation of the printing component is controllable, good bonding can be formed between the printing layers, and the potential safety hazard caused by the existence of interlayer gaps of the printed building component due to poor bonding is reduced.
2. After the aluminate cement is wet-milled to reach the nanometer level, a large amount of hydrated calcium aluminate in a metastable state is obtained, the whole system is in a prehydration state, the hydration rate of the portland cement is obviously improved, the setting time is effectively improved, the viscosity of the superfine portland cement and the aluminate cement is improved, and excellent thixotropy can be achieved without a thixotropic agent.
3. The calcium sulfate in the wet-milled gypsum can react with the hydration product tricalcium aluminate after the aluminate cement is prehydrated to generate a large amount of needle-rod-shaped calcium sulphoaluminate crystals with extremely low solubility, so that the skeleton supporting function is provided, and the constructability and the early strength are improved.
4. The aluminate cement has high setting and hardening speed, the strength can reach 80 percent of the highest strength in 1 day, and the early strength of the building is improved; the gypsum can prevent the hydration of the portland cement in the liquid phase grinding process and slow down the hydration of early portland cement, so that a large amount of portland cement in the early stage is not hydrated and can be continuously hydrated in the later stage, the defects of poor later strength and easiness in collapse of aluminate cement are overcome, the later strength is effectively ensured, and the comprehensive mechanical property of the whole material is excellent.
5. The superfine ceramic fiber is an environment-friendly A1-grade flame-retardant product, the fire-resistant temperature of the superfine ceramic fiber is above 1300 ℃, the temperature resistance and the fire-resistant time of the prepared super-gelling cement can be improved, and the fire resistance of the 3D printing cement-based material is effectively improved.
6. The basalt fiber is a natural material, and no boron or other alkali metal oxides are discharged in the production process, so that no harmful substances are separated out from the smoke dust, and the atmosphere is not polluted. And the product has long service life and excellent tensile strength, and can effectively improve the breaking strength of the super-gelled cement.
Detailed Description
The invention provides a preparation method of super-gelling cement for 3D printing, which comprises the following steps:
the method comprises the following steps: putting 100-150 parts by weight of aluminate cement, 400-600 parts by weight of water and 2-8 parts by weight of grinding aid into a ball mill, and wet-grinding to obtain nano slurry A;
step two: carrying out liquid phase grinding on 380-475 parts by weight of silicate cement clinker, 20-25 parts by weight of gypsum, 120-180 parts by weight of water, 10-30 parts by weight of superfine ceramic fiber and 1-5 parts by weight of water reducer to obtain slurry B;
step three: and adding the nano slurry A, 1-10 parts by weight of interface reinforcing agent and 15-40 parts by weight of basalt fiber into the slurry B, and mixing to obtain the super-gelling cement for 3D printing.
Wherein, the aluminate cement used in the first step can be aluminate cement commonly used in the field, generally, the aluminate cement is prepared by calcining bauxite and limestone as raw materials, and the main component is aluminateCalcium. In the invention, the preferred aluminate cement is Al2O3More than 55% by weight of aluminate cement. The aluminate cements used in the examples and comparative examples of the present invention were aluminate cements purchased from Huaxin cement plant, whose main components were aluminates, and Al2O3The content of (B) is 58% by weight.
The grinding aid used in the first step is a high-efficiency grinding aid, can be a high-efficiency grinding aid commonly used in the field, and is preferably one or more selected from the group consisting of triethanolamine grinding aid, triisopropanolamine grinding aid and glycol grinding aid, and the high-efficiency grinding aid used in the examples and comparative examples of the invention is triethanolamine grinding aid purchased from knoway commercial company limited of Tianjin city.
In the first step, the nano-slurry A is obtained by wet grinding for 60-120 minutes at the rotation speed of 400-800r/min by using a wet grinding preparation technology, the wet grinding is preferably carried out in a planetary ball mill, and the median particle diameter of the obtained nano-slurry A is 50-300 nm.
The portland cement clinker used in the second step can be a portland cement clinker commonly used in the field, and the main components of the portland cement clinker are CaO and SiO2、Al2O3、Fe2O3. In the present invention, the portland cement clinker is preferably a portland cement clinker having a calcium silicate mineral content of not less than 66% by weight and a calcium oxide/silicon oxide mass ratio of not less than 2.0. The portland cement clinker used in the examples and comparative examples of the present invention was portland cement purchased from watson cement plant, which is portland cement clinker having a calcium silicate mineral content of 66% by weight and a calcium oxide to silicon oxide mass ratio of 2.0.
The gypsum in the second step is waste flue gas desulfurization gypsum which is an industrial byproduct gypsum obtained by coal-fired or oil-fired industrial enterprises after treating sulfur dioxide in flue gas, preferably CaSO4·2H2The weight content of O is more than or equal to 90 percent, and the pH value of the leaching solution is 7.8-9. The gypsum used in the examples and comparative examples of the present invention was desulfurized gypsum purchased from Guohui mineral processing plants in Lingshou county, which was CaSO4·2H2The content of O is 90 wt%, and the leaching solutionThe desulfurized gypsum having a pH of 8.
The superfine ceramic fiber in the second step can be the superfine ceramic fiber commonly used in the field, and the main component of the superfine ceramic fiber is Al2O3、Cr2O3、ZrO2Preferably the fibres have a diameter of less than 100 μm and a length of no more than 10 mm. The superfine ceramic fibers used in the examples and comparative examples of the present invention were those available from Guangxin refractory ceramic fiber manufacturers and the major component thereof was Al2O3、Cr2O3、ZrO2The fibers had a diameter of 80 μm and a length of 7 mm.
The water reducing agent in the second step may be a water reducing agent commonly used in the art, and for example, may be one or more selected from the group consisting of a polycarboxylic acid high-efficiency water reducing agent, a naphthalene-based high-efficiency water reducing agent, and an aliphatic high-efficiency water reducing agent. The water reducing agent is a concrete admixture capable of reducing the mixing water consumption under the condition of maintaining the slump constant of concrete, and is usually a polymerization product of various organic matters. The high-efficiency water reducing agent used in the examples and comparative examples of the present invention is a polycarboxylic acid water reducing agent available from Nanchangdefen technologies, Inc.
The slurry B in the second step is obtained by wet grinding for 20-40 minutes at the rotating speed of 400-600r/min by using a wet grinding preparation technology, wherein the median particle size is 1-5 mu m.
The interfacial reinforcing agent in the third step may be an interfacial reinforcing agent commonly used in the art, and is ethylene vinyl acetate copolymer (EVA) redispersible latex powder, and the interfacial reinforcing agent used in the embodiments and comparative examples of the present invention is EVA redispersible latex powder available from te lese chemical ltd.
The basalt fiber in the third step can be basalt fiber commonly used in the field, and the main component of the basalt fiber is SiO2、Al2O3、Fe4O3MgO, CaO, nano SiO is added after the surface of the fiber is modified2The particles and fibers have rough surfaces, and preferably have monofilament diameters of less than 10 μm and a density of less than 2.8g/cm3And a basalt fiber having a thermal conductivity of 0.031-0.038W/m.K. The basalt fibers used in the examples and comparative examples of the present invention were obtained from Qifeng oreBasalt fiber of QF type from Biofiber Ltd, which has a filament diameter of 7 μm and a density of 2.5g/cm3And a basalt fiber having a heat conductivity of 0.035W/m.K.
The invention also provides the super-gelling cement for 3D printing, which is prepared by the preparation method of the super-gelling cement for 3D printing.
Examples
In order to make the objects, technical solutions and advantageous performances of the present invention more clear, four examples and two comparative examples are listed below, further illustrating the present invention. These examples and comparative examples are only for explaining the present invention and are not intended to limit the present invention. In the examples and comparative examples, "parts" means "parts by weight" unless otherwise specified.
Example 1
The method comprises the following steps: taking 100 parts of aluminate cement, 400 parts of water and 2 parts of triethanolamine high-efficiency grinding aid, and carrying out liquid phase grinding for 60 minutes at the rotating speed of 400r/min to obtain slurry A with the median particle size of 300 nm;
step two: putting 380 parts of portland cement clinker, 20 parts of gypsum, 120 parts of water, 10 parts of superfine ceramic fiber and 1 part of polycarboxylic acid type high-efficiency water reducing agent into a planetary ball mill, and wet-milling for 20 minutes at the rotating speed of 400r/min to obtain slurry B, wherein the median particle size is 5 microns;
step three: adding the slurry A, 2 parts of the interface reinforcing agent and 15 parts of basalt fiber into the slurry B, and uniformly mixing to obtain super-gelled cement C1 for 3D printing in example 1;
step four: the super-gelling cement C1, 80 parts of water and 750 parts of river sand are uniformly stirred to obtain a 3D printing mixture E1, and then the mixture is printed and molded through a printer.
Example 2
The method comprises the following steps: taking 120 parts of aluminate cement, 450 parts of water and 4 parts of triethanolamine high-efficiency grinding aid, and carrying out liquid-phase grinding for 80 minutes at the rotating speed of 600r/min to obtain slurry A with the median particle size of 200 nm;
step two: putting 428 parts of portland cement clinker, 22 parts of gypsum, 140 parts of water, 15 parts of superfine ceramic fiber and 2 parts of polycarboxylic acid type high-efficiency water reducing agent into a planetary ball mill, and wet-milling for 20 minutes at the rotating speed of 500r/min to obtain slurry B, wherein the median particle size is 4 microns;
step three: adding the slurry A, 4 parts of interface reinforcing agent and 25 parts of basalt fiber into the slurry B, and uniformly mixing to obtain super-gelled cement C2 for 3D printing;
step four: the super-gelled cement C2, 80 parts of water and 750 parts of river sand are uniformly stirred to obtain a 3D printing mixture E2, and then the mixture is printed and molded by a printer.
Example 3
The method comprises the following steps: taking 130 parts of aluminate cement, 550 parts of water and 6 parts of triethanolamine high-efficiency grinding aid, and carrying out liquid-phase grinding for 100 minutes at the rotating speed of 600r/min to obtain slurry A with the median particle size of 100 nm;
step two: putting 452 parts of portland cement clinker, 23 parts of gypsum, 160 parts of water, 23 parts of superfine ceramic fiber and 4 parts of polycarboxylic acid type high-efficiency water reducing agent into a planetary ball mill, and wet-milling for 40 minutes at the rotating speed of 500r/min to obtain slurry B, wherein the median particle size is 3 mu m;
step three: adding the slurry A, 7 parts of interface reinforcing agent and 30 parts of basalt fiber into the slurry B, and uniformly mixing to obtain super-gelled cement C3 for 3D printing;
step four: the super-gelling cement C3, 80 parts of water and 750 parts of river sand are uniformly stirred to obtain a 3D printing mixture E3, and then the mixture is printed and molded through a printer.
Example 4
The method comprises the following steps: taking 150 parts of aluminate cement, 600 parts of water and 8 parts of triethanolamine high-efficiency grinding aid, and carrying out liquid-phase grinding for 120 minutes at the rotating speed of 800r/min to obtain slurry A with the median particle size of 50 nm;
step two: placing 475 parts of portland cement clinker, 25 parts of gypsum, 180 parts of water, 30 parts of superfine ceramic fiber and 5 parts of polycarboxylic acid type high-efficiency water reducing agent into a planetary ball mill, and wet-milling for 40 minutes at the rotating speed of 600r/min to obtain slurry B, wherein the median particle size is 1 mu m;
step three: adding the slurry A, 10 parts of interface reinforcing agent and 40 parts of basalt fiber into the slurry B, and uniformly mixing to obtain super-gelled cement C4 for 3D printing;
step four: the super-gelling cement C4, 80 parts of water and 750 parts of river sand are uniformly stirred to obtain a 3D printing mixture E4, and then the mixture is printed and molded through a printer.
Comparative example 1
This comparative example is used to illustrate that the super-gelling cement for 3D printing prepared by the preparation method of super-gelling cement for 3D printing provided by the present invention has fast setting and easy printing properties, high compressive strength and excellent later-stage performance, compared to example 4.
The raw material components and the amounts used in this comparative example were the same as those in example 4, except that in this comparative example, slurry B was not prepared, but slurry A was directly mixed with other raw materials except for the raw material used to prepare slurry A to prepare a cement by the following method:
the method comprises the following steps: taking 150 parts of aluminate cement, 600 parts of water and 8 parts of triethanolamine high-efficiency grinding aid, and carrying out liquid-phase grinding for 120 minutes at the rotating speed of 800r/min to obtain slurry A with the median particle size of 50 nm;
step two: 475 parts of portland cement clinker, 25 parts of gypsum, 180 parts of water, 30 parts of superfine ceramic fiber, 5 parts of polycarboxylic acid type high-efficiency water reducing agent, 10 parts of interface reinforcing agent, 40 parts of basalt fiber and slurry A are uniformly mixed to obtain a cementing material;
step three: the above gelled material was uniformly stirred with 80 parts of water and 750 parts of river sand to obtain a mixture EE1 for 3D printing, and then printed and molded by a printer.
Comparative example 2
This comparative example is used to illustrate that the super-gelling cement for 3D printing prepared by the preparation method of super-gelling cement for 3D printing provided by the present invention has fast setting and easy printing properties, high compressive strength and excellent later-stage performance, compared to example 4.
The components and amounts of the raw materials used in this comparative example were the same as those of example 4, except that in this comparative example, the slurry a and the slurry B were not prepared, but the raw materials for preparing the cement for 3D printing were directly mixed with water and river sand and printed, as follows:
150 parts of aluminate cement, 8 parts of triethanolamine-type high-efficiency grinding aid, 475 parts of portland cement clinker, 25 parts of gypsum, 30 parts of superfine ceramic fiber, 5 parts of polycarboxylic acid-type high-efficiency water reducing agent, 10 parts of interface reinforcing agent and 40 parts of basalt fiber are uniformly stirred with 860 parts of water and 750 parts of river sand to obtain a mixture EE2 for 3D printing, and then the mixture is printed and molded by a printer.
The 3D printing mixtures E1-E4 and EE1-EE2 obtained in examples 1-4 and comparative examples 1-2 were subjected to initial set and final set tests, thixotropic ring area, stacking height, uninterrupted length, and strength tests, respectively.
Wherein, the initial setting and final setting experiments are carried out by adopting the national standard GB 1346-.
And (3) testing the area of the thixotropic ring: the rheometer is adopted, and the curve form of the rheometer shows that an upper rheological curve (the shear rate is gradually increased from 0 to 100S 1) is not overlapped with a lower rheological curve (the shear rate is gradually decreased from 100S + to 0) in a rheological curve diagram, but a closed shuttle-type thixotropic ring is formed between the two curves. The size of the area of this "shuttle" thixotropic ring is a measure of thixotropic properties.
Stacking height: quickly loading the mixed mortar into a straight cylinder with the diameter of 15cm and the height of 80cm in two layers, loading the first layer to the position of about two thirds of the height of a truncated cone round die, respectively scribing 5 times in two mutually vertical directions by a knife, and uniformly tamping 15 times from the edge to the center by a tamping rod; then, a second layer of mortar was applied, and the mortar was cut 5 times in two directions perpendicular to each other with a knife, and then uniformly tamped 10 times from the edge to the center with a tamp. And then quickly lifting and measuring the height of the formed mortar.
Length of uninterrupted: using a 350ML syringe, the outer needle was removed, the outer diameter was 8mm, and the extrusion was continued without interruption of the length.
The strength test was carried out using GB/T17671-1999.
The results of the above tests are shown in table 1 below.
TABLE 1
In table 1, "initial setting time" and "final setting time" reflect the setting speed of the 3D printing mixture.
The "thixotropic ring area" reflects the thixotropy of the 3D printing mixture.
The "stack height" reflects the constructability of the 3D printing mix.
The "uninterrupted length" reflects the printability of the 3D printing mix.
The "strength" data indices of "12 h compressive strength", "3D strength", "28D strength", "56D strength", "post-firing strength", etc., reflect the mechanical properties of the 3D printing mixture.
As can be seen from the data in Table 1, the 3D printing mixtures A1-A4 obtained in examples 1-4 using the super-gelling cement for 3D printing provided by the present invention are superior to the 3D printing mixtures C1-C2 obtained in comparative examples 1-2 in both setting time, mechanical properties and printability, wherein comparative example 2 is not formable, resulting in no data and no printing; comparative example 1 although it could be printed, the other effects were far inferior to examples 1 to 4, especially in terms of setting time, thixotropy and mechanical properties.
Therefore, as is apparent from table 1 above, when the 3D printing super-gelling cement prepared by the preparation method of the 3D printing super-gelling cement provided by the invention is used for 3D printing, the 3D printing can have the properties of high early-stage setting speed, high strength, excellent thixotropy and printability, high later-stage strength and good fire resistance.
In addition, the super-gelling cement for 3D printing provided by the invention is also superior to the existing common 3D printing cement-based material. Firstly, the 3D strength of the existing 3D printing mixture prepared by mixing the common 3D printing cement-based material with river sand and water is generally lower than the 3D strength of 25.4-30.6MPa in table 1. In addition, the super-gelling cement for 3D printing provided by the invention can realize quick setting through selection of raw materials and a preparation process, while the initial setting time of the existing common 3D printing cement-based material is about 15 minutes, but an additional coagulant, an accelerator, a retarder, a plasticizer and the like are required to adjust the setting speed of the 3D printing cement-based material (for example, patent document CN105731942A), so that the preparation steps are complicated and the cost is increased. Therefore, the super-gelling cement for 3D printing provided by the invention provides a new idea for 3D printing of buildings, and has remarkable overall benefit.
Claims (9)
1. A preparation method of super-gelling cement for 3D printing comprises the following steps:
the method comprises the following steps: putting 100-150 parts by weight of aluminate cement, 400-600 parts by weight of water and 2-8 parts by weight of grinding aid into a ball mill, and wet-grinding to obtain nano slurry A;
step two: carrying out liquid phase grinding on 380-475 parts by weight of silicate cement clinker, 20-25 parts by weight of gypsum, 120-180 parts by weight of water, 10-30 parts by weight of superfine ceramic fiber and 1-5 parts by weight of water reducer to obtain slurry B;
step three: and adding the nano slurry A, 1-10 parts by weight of interface reinforcing agent and 15-40 parts by weight of basalt fiber into the slurry B, and mixing to obtain the super-gelling cement for 3D printing.
2. The method according to claim 1, wherein the aluminate cement used in step one is prepared by calcining bauxite and limestone as raw materials;
the grinding aid used in the first step is one or more selected from the group consisting of triethanolamine grinding aid, triisopropanolamine grinding aid and ethylene glycol grinding aid.
3. The method according to claim 2, wherein the aluminate cement is Al2O3More than 55% by weight of aluminate cement.
4. The method of claim 1, wherein in step one, the method of wet milling comprises: wet grinding for 60-120 minutes at the rotating speed of 400-800r/min to obtain the nano slurry A with the median particle diameter of 50-300 nm.
5. The method according to claim 1, wherein the portland cement clinker used in the second step is portland cement having a calcium silicate mineral content of not less than 66% by weight and a mass ratio of calcium oxide to silicon oxide of not less than 2.0;
the gypsum in the step two is waste flue gas desulfurization gypsum which is an industrial byproduct gypsum obtained after sulfur dioxide in flue gas is treated by industrial enterprises burning coal or oil;
the diameter of the superfine ceramic fiber in the second step is less than 100 mu m, and the length of the superfine ceramic fiber is not more than 10 mm.
6. The method of claim 5, wherein the gypsum is CaSO4·2H2The weight content of O is more than or equal to 90 percent, and the pH value of the leaching solution is 7.8-9.
7. The method as claimed in claim 1, wherein the slurry B obtained in step two is obtained by wet milling for 20-40 minutes at a rotation speed of 400-600r/min by using a wet milling preparation technique, and the median particle diameter of the slurry B is 1-5 μm.
8. The method of claim 1, wherein the interfacial enhancer in step three is an EVA redispersible latex powder.
9. A super-gelling cement for 3D printing made by the method of any one of claims 1-8.
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