CN113754359B - All-solid-waste-fiber-reinforced geopolymer composite material suitable for 3D printing technology - Google Patents
All-solid-waste-fiber-reinforced geopolymer composite material suitable for 3D printing technology Download PDFInfo
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- 238000010146 3D printing Methods 0.000 title claims abstract description 29
- 229920000876 geopolymer Polymers 0.000 title claims abstract description 26
- 239000002131 composite material Substances 0.000 title claims abstract description 24
- 238000005516 engineering process Methods 0.000 title claims abstract description 19
- 239000000463 material Substances 0.000 claims abstract description 73
- 239000003513 alkali Substances 0.000 claims abstract description 57
- 239000012190 activator Substances 0.000 claims abstract description 55
- 239000000835 fiber Substances 0.000 claims abstract description 53
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 39
- 239000002041 carbon nanotube Substances 0.000 claims abstract description 33
- 229910021393 carbon nanotube Inorganic materials 0.000 claims abstract description 33
- 239000002893 slag Substances 0.000 claims abstract description 31
- 239000010881 fly ash Substances 0.000 claims abstract description 29
- 238000002360 preparation method Methods 0.000 claims abstract description 27
- 229910021487 silica fume Inorganic materials 0.000 claims abstract description 26
- 239000002910 solid waste Substances 0.000 claims abstract description 25
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000004576 sand Substances 0.000 claims abstract description 10
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 108
- 238000003756 stirring Methods 0.000 claims description 27
- 239000002002 slurry Substances 0.000 claims description 23
- 239000007787 solid Substances 0.000 claims description 23
- 239000000203 mixture Substances 0.000 claims description 22
- 239000007864 aqueous solution Substances 0.000 claims description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- 239000004115 Sodium Silicate Substances 0.000 claims description 18
- 238000002156 mixing Methods 0.000 claims description 18
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 18
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 18
- 239000002245 particle Substances 0.000 claims description 8
- 238000007639 printing Methods 0.000 claims description 6
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 3
- 239000002356 single layer Substances 0.000 claims 1
- 239000002994 raw material Substances 0.000 abstract description 21
- 229920003041 geopolymer cement Polymers 0.000 abstract description 5
- 239000002699 waste material Substances 0.000 abstract description 4
- 238000007599 discharging Methods 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 35
- 239000000047 product Substances 0.000 description 25
- 239000011734 sodium Substances 0.000 description 16
- 230000004913 activation Effects 0.000 description 15
- 239000008367 deionised water Substances 0.000 description 15
- 229910021641 deionized water Inorganic materials 0.000 description 15
- 238000000034 method Methods 0.000 description 15
- 239000007788 liquid Substances 0.000 description 13
- 239000004567 concrete Substances 0.000 description 10
- 238000004519 manufacturing process Methods 0.000 description 6
- 239000003795 chemical substances by application Substances 0.000 description 3
- 229910021389 graphene Inorganic materials 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 239000002109 single walled nanotube Substances 0.000 description 3
- 229920002430 Fibre-reinforced plastic Polymers 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000004568 cement Substances 0.000 description 2
- 239000011151 fibre-reinforced plastic Substances 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
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- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 239000002518 antifoaming agent Substances 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
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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
- C04B28/006—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 mineral polymers, e.g. geopolymers of the Davidovits type
-
- 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
- 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
- C04B2201/52—High compression strength concretes, i.e. with a compression strength higher than about 55 N/mm2, e.g. reactive powder concrete [RPC]
-
- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
- Y02P40/10—Production of cement, e.g. improving or optimising the production methods; Cement grinding
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Ceramic Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Structural Engineering (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Organic Chemistry (AREA)
- Environmental & Geological Engineering (AREA)
- Civil Engineering (AREA)
- Composite Materials (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
Abstract
The invention relates to the technical field of solid waste resource utilization and geopolymer concrete preparation, in particular to a full-solid waste fiber reinforced geopolymer composite material suitable for a 3D printing technology; the raw materials comprise 20-30 parts of aggregate, 70-80 parts of cementing material, carbon nano tube, PVA fiber and alkali activator; wherein, the gelled material comprises the following components in percentage by mass: 15-30% of fly ash, 55-65% of slag and 10-25% of silica fume; the aggregate is reclaimed machine-made sand. The all-solid-waste ultrahigh-performance geopolymer concrete provided by the invention can reach initial setting within 10-25 minutes of discharging, and meets the 3D printing requirement; in addition, the fly ash, the slag and the reclaimed machine-made sand are all derived from industrial building solid waste, so that the waste of the solid waste can be effectively reduced, the sustainability of the building is improved, and an efficient, environment-friendly and energy-saving solution is provided for the treatment after the building is dismantled.
Description
Technical Field
The invention relates to the technical field of solid waste resource utilization and geopolymer concrete preparation, in particular to a full-solid waste fiber reinforced geopolymer composite material suitable for a 3D printing technology.
Background
With the rise of computer technology, 3D printing technology has been rapidly developed and has gradually been widely applied in a plurality of fields such as medical treatment, aerospace, architecture, electronics, clothing, food, etc. In the aspect of the building industry, due to the advantages of no mould, refinement and the like of the 3D printing technology, the application level of the technology also promotes the progress of the whole industry. In addition, with the production of a large amount of industrial solid particle waste in the production process, the possibility of sustainable green development of the industry is provided by using slag, fly ash and other substitutes as cementing materials. In recent decades, the continuous and deep knowledge of geopolymer composites in academia and industry has also provided the possibility of their application in 3D printing technology.
Document 1 (Zhouzonghui, kingjinbang, chengxin, etc.; a 3D-printed alkali slag cement concrete and a preparation method thereof; publication No. CN 108178567A) discloses a 3D-printed alkali slag cement concrete and a preparation method thereof. The method is simple to prepare and easy to implement. However, the aggregate in the invention has a particle size of 5-10 mm, which easily causes hollow voids and uneven surface roughness, and limits the mechanical properties and the aesthetic degree of the finished product.
Document 2 (li zhi, qian qiao, deng xiao fang, etc.; concrete based on 3D printing and preparation method thereof, 3D printing column template; publication No. CN 113372075A) discloses concrete based on 3D printing and preparation method thereof. According to the formula provided by the invention, the mechanical property of 3D printing concrete is improved and the printing blockage can be effectively avoided by introducing the carbon fiber. However, in order to make the invention have better thixotropy and fluidity, the expanding agent, the defoaming agent, the air entraining agent and the cellulose are added into the formula, so the preparation process is more complicated and is not suitable for practical engineering application.
Document 3 (Dinghuaming, huangmingyang, nie Jizhen, etc.; a nano graphene concrete material for 3D printing of buildings and a preparation method thereof; publication No. CN 113264744A) discloses a 3D printing concrete scheme capable of freely regulating and controlling the setting time. The nano graphene water has a regulation function on a muddy water product and an aggregation state, so that the product has good fluidity, and the phenomenon of material breakage cannot occur in the printing process. However, the nano graphene is expensive in manufacturing cost, and is not beneficial to mass application in engineering.
Based on the above, a need exists for a full solid waste fiber reinforced polymer composite material with wide and cheap raw material source and suitable for 3D printing technology.
Disclosure of Invention
The invention aims to provide a full-solid waste fiber reinforced geopolymer composite material suitable for a 3D printing technology. The method has the advantages of effective utilization of waste resources, low cost, simple preparation and excellent performance, and the surface of the finished product is smooth like ceramic.
The all-solid waste fiber reinforced geopolymer composite material suitable for the 3D printing technology comprises, by mass, 20-30 parts of aggregate, 70-80 parts of a cementing material, carbon nanotubes, PVA fibers and an alkali activator;
wherein, the gelled material comprises the following components in percentage by mass: 15-30% of fly ash, 55-65% of slag and 10-25% of silica fume;
the aggregate is reclaimed machine-made sand.
Further, the adding amount of the carbon nano tube is 1-3% of the total mass of the aggregate and the cementing material.
Furthermore, the adding amount of the PVA fiber is 0.5-4% of the volume mixing amount.
Further, the proportion of the total mass of the aggregate and the cementing material to the addition of the alkali activator is 1kg:600-700mL.
According to the invention, the fly ash, slag and silica fume mixture is used as a cementing material, and a proper amount of carbon nano tubes and PVA fibers are added in a matching manner, so that the material has short coagulation time, can obtain early strength, and is suitable for 3D printing; meanwhile, the material disclosed by the invention is higher in toughness, can meet the requirement of 3D printing on 'reinforcement-free' and improves the durability of a printing structure.
Further, the particle size of the reclaimed machine-made sand is 0.3-2.36mm.
Further, the carbon nano tube is a single-wall carbon nano tube, and the density at room temperature is 2.1g/cm 3 。
Further, the PVA fiber has the length of 5-15mm, the diameter of 28-32 μm and the elongation of 6-8%.
Further, the alkali activator is prepared from a sodium hydroxide aqueous solution and a sodium silicate aqueous solution according to the mass ratio of 3; wherein the concentration of the sodium hydroxide aqueous solution is 6-10mol/L, and the sodium silicate aqueous solution is Na 2 O·nSiO 2 The modulus n is 0.5-3.5.
Further, al in the fly ash 2 O 3 And SiO 2 More than 50wt% and specific surface area of 600-800 m 2 The screen residue of a 45 mu m square hole sieve is less than 1 percent per kg.
Go toStep one, the water content of the slag is less than 1 percent, and the specific surface area is 400-450m 2 /kg。
Furthermore, the particle size of the silica fume is 0.1-0.3 μm, and the specific surface area is 15000-25000m 2 /kg。
In the second technical scheme of the invention, the preparation method of the all-solid waste fiber reinforced geopolymer composite material suitable for the 3D printing technology comprises the following steps:
(1) Uniformly stirring the fly ash, the slag, the silica fume and the carbon nano tube at a low speed, adding the aggregate and uniformly mixing to obtain a solid powdery mixture;
(2) Adding an alkali activator into the solid powdery mixture, uniformly stirring, adding PVA fibers in several times, uniformly stirring to obtain a full-solid waste fiber reinforced geopolymer slurry;
(3) And transferring the all-solid waste fiber reinforced geopolymer slurry into a 3D printer, and printing according to a set program to obtain the all-solid waste fiber reinforced geopolymer composite material suitable for the 3D printing technology.
Further, natural curing (25 ℃,70% humidity) was performed after the 3D printing was completed.
Further, the low-speed stirring in the step (1) is specifically 300-500r/min; and (3) adding the PVA fiber in the step (2) in a divided manner, specifically adding the PVA fiber in 3-5 times.
Compared with the prior art, the invention has the beneficial effects that:
in the all-solid-waste ultra-high-performance geopolymer concrete provided by the invention, clinker calcination is not needed in the production of geopolymer gelled materials, so that the production energy consumption and CO can be greatly reduced 2 The amount of discharge of (c). In addition, the fly ash, the slag and the reclaimed machine-made sand are all derived from industrial building solid waste, so that the waste of the solid waste can be effectively reduced, the sustainability of the building is improved, and an efficient, environment-friendly and energy-saving solution is provided for the treatment after the building is dismantled.
Due to the characteristic of rapid forming of the 3D printing structure, when the upper layer structure is printed, the lower layer material has enough strength in a short time to maintain the original form and cannot collapse and deform, so that the 3D printing material has high early strength to meet the requirement of the structure printing height. The all-solid-waste-fiber-reinforced geopolymer composite material can achieve initial setting within 10-25 minutes of discharging, and the performance of the all-solid-waste-fiber-reinforced geopolymer composite material is far beyond that of the same type of invention (30-100 minutes).
Compared with other geopolymer materials, the tensile property of the prepared all-solid-waste fiber reinforced geopolymer composite material is 500 times that of common silicate concrete, and the composite material has considerable ductility, compact and smooth surface and good corrosion resistance, and can be used for various thin shell structures or used as a protective layer on the surface of a member.
The carbon nano tube used by the all-solid-waste ultra-high-performance geopolymer concrete provided by the invention has good mechanical properties, the tensile strength reaches 50-200 GPa, is 100 times of that of steel, and is at least one order of magnitude higher than that of the conventional graphite fiber; its elastic modulus can reach 1TPa, which is equivalent to that of diamond, about 5 times that of steel. For carbon nanotubes with a single wall, the tensile strength is about 800GPa. Meanwhile, the carbon nano tube has extremely stable structure and is the material with the highest specific strength which can be prepared at present. The invention prepares the composite material by the geopolymer-based concrete matrix, can lead the composite material to show good strength, elasticity, fatigue resistance and isotropy, and brings great improvement to the performance of the composite material.
Drawings
FIG. 1 is a schematic view of the microstructure of a single-walled carbon nanotube used in an embodiment of the present invention;
fig. 2 is a schematic flow chart of the process for preparing the all-solid-waste-fiber-reinforced polymer composite material suitable for the 3D printing technology according to example 1 of the present invention.
Detailed Description
Reference will now be made in detail to various exemplary embodiments of the invention, the detailed description should not be construed as limiting the invention but rather as a more detailed description of certain aspects, features and embodiments of the invention.
It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. In addition, for numerical ranges in the present disclosure, it is understood that each intervening value, to the upper and lower limit of that range, is also specifically disclosed. Every smaller range between any stated value or intervening value in a stated range and any other stated or intervening value in a stated range is encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention. All documents mentioned in this specification are incorporated by reference herein for the purpose of disclosing and describing the methods and/or materials associated with the documents. In case of conflict with any incorporated document, the present specification will control.
It will be apparent to those skilled in the art that various modifications and variations can be made in the specific embodiments of the present disclosure without departing from the scope or spirit of the disclosure. Other embodiments will be apparent to those skilled in the art from consideration of the specification. The description and examples are intended to be illustrative only.
As used herein, the terms "comprising," "including," "having," "containing," and the like are open-ended terms that mean including but not limited to.
The raw materials used in the following examples of the invention are as follows:
aggregate: regenerating machine-made sand, wherein the source of the machine-made sand is a building demolition object, and the machine-made sand is crushed into the grain diameter of 0.3-2.36mm before use;
fly ash: the source is power plant, al 2 O 3 And SiO 2 50 percent of the total weight of the powder, and the specific surface area of the powder is 600-800 m 2 Kg, the residue of a square hole sieve with the size of 45 mu m is less than 1 percent;
slag: drying the raw materials in an iron-making plant until the water content is less than 1 percent, and grinding the raw materials to the specific surface area of 400 to 450m 2 /kg；
Silica fume: the mineral powder factory has particle distribution range of 0.1-0.3 μm and specific surface area of 15000-25000m 2 /kg；
The carbon nanotube is a single-wall carbon nanotube and purchased in the market, and the schematic view of the microstructure is shown in figure 1; the density at room temperature is 2.1g/cm 3 。
PVA fiber: the length of the product is 5-15mm, the diameter is 28-32 μm, and the elongation is 6-8%.
Example 1
Weighing the following raw materials in parts by weight: 25 parts of aggregate, 75 parts of cementing material (calculated by mass fraction, 30% of fly ash, 60% of slag and 10% of silica fume), PVA fiber (2% of volume mixing amount), carbon nano tube (2% of total mass of aggregate and cementing material), and alkali activator (650 mL of alkali activator is added into each kilogram of mixture of aggregate and cementing material);
the preparation method of the alkaline activator comprises the following steps: dissolving NaOH solid in deionized water according to a certain proportion to prepare 6mol/L sodium hydroxide solution, standing at normal temperature for 24 hours until the solution is cooled to room temperature, and adding sodium silicate aqueous solution (Na) according to a mass ratio of 3 2 O·nSiO 2 N = 1.5), and uniformly stirring to obtain alkali activation liquid for later use;
the preparation method is as follows (fig. 2 is a schematic flow chart of the concrete composite material prepared by the embodiment):
(1) Adding the fly ash, the slag, the silica fume and the carbon nano tube into a stirrer, stirring at a low speed of 500r/min for 2 minutes, adding the aggregate, and stirring for 1 minute to obtain a solid powdery mixture;
(2) Adding an alkali activator into the solid powdery mixture, uniformly stirring for 6 minutes (any value within the range of 4-6 min), uniformly scattering PVA fibers for 5 times, and stirring for 4 minutes (any value within the range of 2-4 min) to obtain full-solid waste fiber reinforced geopolymer slurry; measuring the initial setting time of the slurry to be 10min;
(3) And pouring the all-solid waste fiber reinforced geopolymer slurry into a printer, and obtaining a finished product according to a set program. The compressive strength of the product after natural curing (25 ℃,70 percent of humidity) for 28 days is 45MPa.
Example 2
The difference from the example 1 is that the raw materials are weighed according to the parts by weight: 25 parts of aggregate, 75 parts of cementing material (calculated by mass fraction, 30% of fly ash, 60% of slag and 10% of silica fume), PVA fiber (2% of volume mixing amount), carbon nano tube (2% of total mass of aggregate and cementing material), and alkali activator (650 mL of alkali activator is added into each kilogram of mixture of aggregate and cementing material);
the preparation method of the alkaline activator comprises the following steps: dissolving NaOH solid in deionized water according to a certain proportion to prepare 8mol/L sodium hydroxide solution, standing at normal temperature for 24 hours until the solution is cooled to room temperature, and adding sodium silicate aqueous solution (Na) according to a mass ratio of 3 2 O·nSiO 2 And n = 1.5), and uniformly stirring to obtain the alkali activation liquid for later use. Measuring the initial setting time of the slurry to be 10 minutes; the compressive strength of the product is detected to be 54MPa after natural curing (25 ℃,70 percent of humidity) for 28 days.
Example 3
The method is the same as example 1 except that the raw materials are weighed according to the parts by weight: 25 parts of aggregate, 75 parts of cementing material (calculated by mass fraction, 30% of fly ash, 60% of slag and 10% of silica fume), PVA fiber (2% of volume mixing amount), carbon nano tube (2% of total mass of aggregate and cementing material), and alkali activator (650 mL of alkali activator is added in per kilogram of mixture of aggregate and cementing material);
the preparation method of the alkaline activator comprises the following steps: dissolving NaOH solid in deionized water according to a certain proportion to prepare 10mol/L sodium hydroxide solution, standing at normal temperature for 24 hours until the solution is cooled to room temperature, and adding sodium silicate aqueous solution (Na) according to a mass ratio of 3 2 O·nSiO 2 And n = 1.5), and uniformly stirring to obtain the alkali activation liquid for later use. The initial setting time of the slurry is 10 minutes by measurement; after natural curing (25 ℃,70 percent of humidity) for 28 days, the compressive strength of the product is 63MPa.
Example 4
The method is the same as example 1 except that the raw materials are weighed according to the parts by weight: 25 parts of aggregate, 75 parts of cementing material (calculated by mass fraction, 20% of fly ash, 60% of slag and 20% of silica fume), PVA fiber (2% of volume mixing amount), carbon nano tube (2% of total mass of aggregate and cementing material), and alkali activator (650 mL of alkali activator is added in per kilogram of mixture of aggregate and cementing material);
the preparation method of the alkaline activator comprises the following steps: dissolving NaOH solid in deionized water according to a certain proportion to prepare 6mol/L sodium hydroxide solution, standing at normal temperature for 24 hours until the solution is cooled to room temperature, and adding sodium silicate aqueous solution (Na) according to a mass ratio of 3 2 O·nSiO 2 And n = 1.5), and uniformly stirring to obtain the alkali activation liquid for later use. The initial setting time of the slurry is measured to be 12 minutes; after natural curing (25 ℃,70 percent of humidity) for 28 days, the compressive strength of the product is detected to be 58MPa.
Example 5
The method is the same as example 1 except that the raw materials are weighed according to the parts by weight: 25 parts of aggregate, 75 parts of cementing material (calculated by mass fraction, 20% of fly ash, 60% of slag and 20% of silica fume), PVA fiber (2% of volume mixing amount), carbon nano tube (2% of total mass of aggregate and cementing material), and alkali activator (650 mL of alkali activator is added into each kilogram of mixture of aggregate and cementing material);
the preparation method of the alkaline activator comprises the following steps: dissolving NaOH solid in deionized water according to a certain proportion to prepare 8mol/L sodium hydroxide solution, standing at normal temperature for 24 hours until the solution is cooled to room temperature, and adding sodium silicate aqueous solution (Na) according to a mass ratio of 3 2 O·nSiO 2 And n = 1.5), and uniformly stirring to obtain the alkali activation liquid for later use. The initial setting time of the slurry is 10 minutes by measurement; after natural curing (25 ℃,70 percent of humidity) for 28 days, the compressive strength of the product is detected to be 68MPa.
Example 6
The method is the same as example 1 except that the raw materials are weighed according to the parts by weight: 25 parts of aggregate, 75 parts of cementing material (calculated by mass fraction, 20% of fly ash, 60% of slag and 20% of silica fume), PVA fiber (2% of volume mixing amount), carbon nano tube (2% of total mass of aggregate and cementing material), and alkali activator (650 mL of alkali activator is added in per kilogram of mixture of aggregate and cementing material);
the preparation method of the alkaline activator comprises the following steps: dissolving NaOH solid in deionized water according to a certain proportion to prepare 10mol/L sodium hydroxide solution, standing at normal temperature for 24 hours until the solution is cooled to room temperature, and adding the NaOH solid into the solution according to a mass ratio of 3Aqueous sodium silicate solution (Na) 2 O·nSiO 2 And n = 1.5), and uniformly stirring to obtain the alkali activation liquid for later use. The initial setting time of the slurry is measured to be 10 minutes; after natural curing (25 ℃,70 percent of humidity) for 28 days, the compressive strength of the product is 80MPa.
It can be seen from comparing the data of examples 1-3 and 4-6 that different sodium hydroxide concentrations have an effect on the compressive strength of the final product without changing the gel material ratio, because the degree of polymerization of the geopolymer reaction is higher in a strong alkaline environment; the data of example 1 and example 4, example 2 and example 5, and example 3 and example 6 show that under the premise of no change of the alkali-activating agent, the adjustment of the proportion of slag, fly ash and silica fume in the cementing material also affects the performance of the product, because the fillers with different particle sizes improve the compactness of the product.
Example 7
The difference from example 6 is that the raw materials are weighed according to parts by mass: 20 parts of aggregate, 80 parts of cementing material (calculated by mass fraction, 20% of fly ash, 60% of slag and 20% of silica fume), PVA fiber (2% of volume mixing amount), carbon nano tube (2% of total mass of aggregate and cementing material), and alkali activator (650 mL of alkali activator is added in per kilogram of mixture of aggregate and cementing material);
the preparation method of the alkaline activator comprises the following steps: dissolving NaOH solid in deionized water according to a certain proportion to prepare 10mol/L sodium hydroxide solution, standing at normal temperature for 24 hours until the solution is cooled to room temperature, and adding sodium silicate aqueous solution (Na) according to a mass ratio of 3 2 O·nSiO 2 And n = 1.5), and uniformly stirring to obtain the alkali activation liquid for later use.
The initial setting time of the slurry is 10 minutes, and the compressive strength after initial setting is 16MPa; the compressive strength of the product is detected to be 75MPa after natural curing (25 ℃,70 percent of humidity) for 28 days.
Example 8
The method is the same as example 6 except that the raw materials are weighed according to the parts by weight: 30 parts of aggregate, 70 parts of cementing material (calculated by mass fraction, 20% of fly ash, 60% of slag and 20% of silica fume), PVA fiber (2% of volume mixing amount), carbon nano tube (2% of total mass of aggregate and cementing material), and alkali activator (650 mL of alkali activator is added in per kilogram of mixture of aggregate and cementing material);
the preparation method of the alkaline activator comprises the following steps: dissolving NaOH solid in deionized water according to a certain proportion to prepare 10mol/L sodium hydroxide solution, standing at normal temperature for 24 hours until the solution is cooled to room temperature, and adding sodium silicate aqueous solution (Na) according to a mass ratio of 3 2 O·nSiO 2 And n = 1.5), and uniformly stirring to obtain an alkali activation solution for later use.
The initial setting time of the slurry is measured to be 8 minutes, and the compressive strength after initial setting is 21MPa; after natural curing (25 ℃,70 percent of humidity) for 28 days, the compressive strength of the product is 81MPa.
Example 9
The method is the same as example 6 except that the raw materials are weighed according to the parts by weight: 40 parts of aggregate, 60 parts of cementing material (calculated by mass fraction, 20% of fly ash, 60% of slag and 20% of silica fume), PVA fiber (2% of volume mixing amount), carbon nano tube (2% of total mass of aggregate and cementing material), and alkali activator (650 mL of alkali activator is added in per kilogram of mixture of aggregate and cementing material);
the preparation method of the alkaline activator comprises the following steps: dissolving NaOH solid in deionized water according to a certain proportion to prepare 10mol/L sodium hydroxide solution, standing at normal temperature for 24 hours until the solution is cooled to room temperature, and adding sodium silicate aqueous solution (Na) according to a mass ratio of 3 2 O·nSiO 2 And n = 1.5), and uniformly stirring to obtain the alkali activation liquid for later use.
The initial setting time of the slurry is determined to be 10 minutes, and the compressive strength after initial setting is 23MPa; after natural curing (25 ℃,70 percent of humidity) for 28 days, the compressive strength of the product is detected to be 71MPa.
Example 10
The method is the same as example 6 except that the raw materials are weighed according to the parts by weight: 25 parts of aggregate, 75 parts of cementing material (calculated by mass fraction, 20% of fly ash, 60% of slag and 20% of silica fume), PVA fiber (2% of volume mixing amount), carbon nano tube (3% of total mass of aggregate and cementing material), and alkali activator (650 mL of alkali activator is added into each kilogram of mixture of aggregate and cementing material);
the preparation method of the alkaline activator comprises the following steps: dissolving NaOH solid in deionized water according to a certain proportion to prepare 10mol/L sodium hydroxide solution, standing at normal temperature for 24 hours until the solution is cooled to room temperature, and adding sodium silicate aqueous solution (Na) according to a mass ratio of 3 2 O·nSiO 2 And n = 1.5), and uniformly stirring to obtain an alkali activation solution for later use.
The initial setting time of the slurry is determined to be 12 minutes, and the compressive strength after initial setting is 16MPa; after natural curing (25 ℃,70 percent of humidity) for 28 days, the compressive strength of the product is 65MPa.
Example 11
The difference from example 6 is that the raw materials are weighed according to parts by mass: 25 parts of aggregate, 75 parts of cementing material (calculated by mass fraction, 20% of fly ash, 60% of slag and 20% of silica fume), PVA fiber (2% of volume mixing amount), carbon nano tube (1% of total mass of aggregate and cementing material), and alkali activator (650 mL of alkali activator is added into each kilogram of mixture of aggregate and cementing material);
the preparation method of the alkaline activator comprises the following steps: dissolving NaOH solid in deionized water according to a certain proportion to prepare 10mol/L sodium hydroxide solution, standing at normal temperature for 24 hours until the solution is cooled to room temperature, and adding sodium silicate aqueous solution (Na) according to a mass ratio of 3 2 O·nSiO 2 And n = 1.5), and uniformly stirring to obtain the alkali activation liquid for later use.
The initial setting time of the slurry is 10 minutes, and the compressive strength after initial setting is 22MPa; after natural curing (25 ℃,70 percent of humidity) for 28 days, the compressive strength of the product is detected to be 72MPa.
Example 12
The difference from example 6 is that the raw materials are weighed according to parts by mass: 25 parts of aggregate, 75 parts of cementing material (calculated by mass fraction, 20% of fly ash, 60% of slag and 20% of silica fume), PVA fiber (2% of volume mixing amount), carbon nano tube (5% of total mass of aggregate and cementing material), and alkali activator (650 mL of alkali activator is added in per kilogram of mixture of aggregate and cementing material);
the preparation method of the alkaline activator comprises the following steps: dissolving NaOH solid in deionized water according to a certain proportion to prepare 10mol/L sodium hydroxide solution, standing at normal temperature for 24 hours until the solution is cooled toAdding sodium silicate aqueous solution (Na) according to the mass ratio of 3 2 O·nSiO 2 And n = 1.5), and uniformly stirring to obtain the alkali activation liquid for later use.
The initial setting time of the slurry is determined to be 14 minutes, and the compressive strength after initial setting is 18MPa; the compressive strength of the product is detected to be 62MPa after natural curing (25 ℃,70 percent of humidity) for 28 days.
Example 13
The difference from example 6 is that the addition of carbon nanotubes was omitted as the starting material.
The initial setting time of the slurry is determined to be 15 minutes, and the compressive strength after initial setting is 14MPa; the compressive strength of the product is 43MPa after natural curing (25 ℃,70% humidity) for 28 days.
Example 14
The method is the same as example 6 except that the raw materials are weighed according to the parts by weight: 25 parts of aggregate, 75 parts of cementing material (calculated by mass fraction, 20% of fly ash, 60% of slag and 20% of silica fume), PVA fiber (2.5% of volume), carbon nanotube (2% of total mass of aggregate and cementing material), and alkali activator (650 mL of alkali activator is added in each kilogram of mixture of aggregate and cementing material);
the preparation method of the alkaline activator comprises the following steps: dissolving NaOH solid in deionized water according to a certain proportion to prepare 10mol/L sodium hydroxide solution, standing at normal temperature for 24 hours until the solution is cooled to room temperature, and adding sodium silicate aqueous solution (Na) according to a mass ratio of 3 2 O·nSiO 2 And n = 1.5), and uniformly stirring to obtain the alkali activation liquid for later use.
The initial setting time of the slurry is determined to be 16 minutes, and the compressive strength after initial setting is 18MPa; the compressive strength of the product is detected to be 62MPa after natural curing (25 ℃,70 percent of humidity) for 28 days.
Example 15
The difference from example 6 is that the raw materials are weighed according to parts by mass: 25 parts of aggregate, 75 parts of cementing material (calculated by mass fraction, 20% of fly ash, 60% of slag and 20% of silica fume), PVA fiber (0.5% of volume mixing amount), carbon nano tube (2% of total mass of aggregate and cementing material), and alkali activator (650 mL of alkali activator is added in each kilogram of mixture of aggregate and cementing material);
the preparation method of the alkaline activator comprises the following steps: dissolving NaOH solid in deionized water according to a certain proportion to prepare 10mol/L sodium hydroxide solution, standing at normal temperature for 24 hours until the solution is cooled to room temperature, and adding sodium silicate aqueous solution (Na) according to a mass ratio of 3 2 O·nSiO 2 And n = 1.5), and uniformly stirring to obtain the alkali activation liquid for later use.
The initial setting time of the slurry is determined to be 13 minutes, and the compressive strength after initial setting is 15MPa; the compressive strength of the product is 60MPa after natural curing (25 ℃,70% humidity) for 28 days.
Example 16
The method is the same as example 6 except that the raw materials are weighed according to the parts by weight: 25 parts of aggregate, 75 parts of cementing material (calculated by mass fraction, 20% of fly ash, 60% of slag and 20% of silica fume), PVA fiber (3% of volume mixing amount), carbon nano tube (2% of total mass of aggregate and cementing material), and alkali activator (650 mL of alkali activator is added into each kilogram of mixture of aggregate and cementing material);
the preparation method of the alkaline activator comprises the following steps: dissolving NaOH solid in deionized water according to a certain proportion to prepare 10mol/L sodium hydroxide solution, standing at normal temperature for 24 hours until the solution is cooled to room temperature, and adding sodium silicate aqueous solution (Na) according to a mass ratio of 3 2 O·nSiO 2 And n = 1.5), and uniformly stirring to obtain the alkali activation liquid for later use.
The initial setting time of the slurry is determined to be 16 minutes, and the compressive strength after initial setting is 21MPa; the compressive strength of the product after natural curing (25 ℃,70% humidity) for 28 days was measured to be 46MPa (because too much fiber would introduce voids).
Example 17
The difference from example 6 is that the addition of PVA fibers as a raw material was omitted.
The initial setting time of the slurry is determined to be 14 minutes, and the compressive strength after initial setting is 15MPa; after natural curing (25 ℃,70 percent of humidity) for 28 days, the compressive strength of the product is 65MPa.
By comparing the data of examples 7-17, it can be concluded that PVA fiber and carbon nanotubes can be used as macroscopic fiber and microscopic fiber of the system to form a fiber network, which improves the strength of the composite material. The adjustment of the proportion of the aggregate and the cementing material has great influence on the compressive strength, and the suggested proportion is 20-30 parts of the aggregate and 70-80 parts of the cementing material.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included therein.
Claims (2)
1. The all-solid waste fiber reinforced geopolymer composite material suitable for the 3D printing technology is characterized by comprising 20-30 parts by mass of aggregate, 70-80 parts by mass of cementing material, carbon nanotubes, PVA fiber and an alkali activator;
wherein, the gelled material comprises the following components in percentage by mass: 15-30% of fly ash, 55-65% of slag and 10-25% of silica fume;
the aggregate is reclaimed machine-made sand;
the adding amount of the carbon nano tube is 1-3% of the total mass of the aggregate and the cementing material;
the adding amount of the PVA fiber is 0.5-4% of the volume mixing amount;
the proportion of the total mass of the aggregate and the cementing material to the addition of the alkali activator is 1kg:600-700mL;
the alkali activator is prepared from a sodium hydroxide aqueous solution and a sodium silicate aqueous solution according to the mass ratio of 3; wherein the concentration of the sodium hydroxide aqueous solution is 6-10mol/L;
the particle size of the reclaimed machine-made sand is 0.3-2.36mm; the carbon nano tube is a single-layer wall carbon nano tube, and the density at room temperature is 2.1g/cm 3 (ii) a The length of the PVA fiber is 5-15mm, the diameter is 28-32 mu m, and the elongation is 6-8%;
al in the fly ash 2 O 3 And SiO 2 More than 50wt% and specific surface area of 600-800 m 2 Kg, the residue of a square hole sieve with the size of 45 mu m is less than 1 percent;
the water content of the slag is less than 1 percent, and the specific surface area is 400-450m 2 /kg；
The particle size of the silica fume is 0.1-0.3 mu m, and the specific surface area is 15000-25000m 2 /kg；
The preparation method of the all-solid-waste-fiber-reinforced geopolymer composite material suitable for the 3D printing technology comprises the following steps of:
(1) Uniformly stirring the fly ash, the slag, the silica fume and the carbon nano tube at a low speed, adding the aggregate, and uniformly mixing to obtain a solid powdery mixture;
(2) Adding an alkali activator into the solid powdery mixture, uniformly stirring, adding PVA fibers in several times, uniformly stirring to obtain a full-solid waste fiber reinforced geopolymer slurry;
(3) And transferring the all-solid waste fiber reinforced geopolymer slurry into a 3D printer, and printing according to a set program to obtain the all-solid waste fiber reinforced geopolymer composite material suitable for the 3D printing technology.
2. The all-solid-waste-fiber-reinforced geopolymer composite suitable for 3D printing technology according to claim 1, wherein the low-speed stirring in step (1) is in particular 300-500r/min;
the step (2) of adding PVA fiber in several times is to add PVA fiber in 3-5 times.
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