CN114409335B - Low-density interior calcium silicate board and preparation method and application thereof - Google Patents

Low-density interior calcium silicate board and preparation method and application thereof Download PDF

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CN114409335B
CN114409335B CN202210084691.2A CN202210084691A CN114409335B CN 114409335 B CN114409335 B CN 114409335B CN 202210084691 A CN202210084691 A CN 202210084691A CN 114409335 B CN114409335 B CN 114409335B
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calcium silicate
low
silicate board
density
plate
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CN114409335A (en
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王阳
李建新
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Zhaoqing Sanle Integrated Housing Manufacturing Co ltd
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    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B28/00Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
    • C04B28/02Compositions 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
    • C04B28/04Portland cements
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B14/00Use of inorganic materials as fillers, e.g. pigments, for mortars, concrete or artificial stone; Treatment of inorganic materials specially adapted to enhance their filling properties in mortars, concrete or artificial stone
    • C04B14/02Granular materials, e.g. microballoons
    • C04B14/04Silica-rich materials; Silicates
    • C04B14/06Quartz; Sand
    • C04B14/062Microsilica, e.g. colloïdal silica
    • EFIXED CONSTRUCTIONS
    • E04BUILDING
    • E04FFINISHING WORK ON BUILDINGS, e.g. STAIRS, FLOORS
    • E04F13/00Coverings or linings, e.g. for walls or ceilings
    • E04F13/07Coverings or linings, e.g. for walls or ceilings composed of covering or lining elements; Sub-structures therefor; Fastening means therefor
    • E04F13/08Coverings or linings, e.g. for walls or ceilings composed of covering or lining elements; Sub-structures therefor; Fastening means therefor composed of a plurality of similar covering or lining elements
    • E04F13/14Coverings or linings, e.g. for walls or ceilings composed of covering or lining elements; Sub-structures therefor; Fastening means therefor composed of a plurality of similar covering or lining elements stone or stone-like materials, e.g. ceramics concrete; of glass or with an outer layer of stone or stone-like materials or glass
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/20Resistance against chemical, physical or biological attack
    • C04B2111/28Fire resistance, i.e. materials resistant to accidental fires or high temperatures
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    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/76Use at unusual temperatures, e.g. sub-zero
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2201/00Mortars, concrete or artificial stone characterised by specific physical values
    • C04B2201/20Mortars, concrete or artificial stone characterised by specific physical values for the density
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2201/00Mortars, concrete or artificial stone characterised by specific physical values
    • C04B2201/50Mortars, concrete or artificial stone characterised by specific physical values for the mechanical strength
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/74Physical characteristics
    • C04B2235/77Density
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02WCLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00Technologies for solid waste management
    • Y02W30/50Reuse, recycling or recovery technologies
    • Y02W30/91Use of waste materials as fillers for mortars or concrete

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
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  • Chemical Kinetics & Catalysis (AREA)
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Abstract

The invention discloses a low-density interior calcium silicate board and a preparation method and application thereof. The preparation method comprises the following steps: (1) preparing hollow silicon dioxide microspheres by an emulsion method; (2) Mixing hollow silica microspheres, siliceous materials, calcareous materials, cement and plant fibers to prepare mixed blank slurry with solid content of 10-15 wt%; (3) And (3) carrying out net surfing molding on the mixed blank slurry to prepare a wet plate blank, then carrying out plate compacting treatment on the wet plate blank under the compacting pressure of not less than 23MPa, and carrying out autoclaved curing to obtain a molded plate, namely the low-density interior calcium silicate plate. According to the invention, the hollow silicon dioxide microspheres are added in the preparation process of the calcium silicate board, so that a large number of hollow gaps are still formed in the board after the board is compacted, the density of the board can be flexibly adjusted, and the application range of the calcium silicate board is favorably expanded.

Description

Low-density interior calcium silicate board and preparation method and application thereof
Technical Field
The invention belongs to the field of building materials, and particularly relates to a low-density interior calcium silicate board and a preparation method and application thereof.
Background
The calcium silicate board is a novel building and decoration board taking calcium and siliceous materials as continuous phases and plant fibers, chemical fibers or glass fibers and the like as reinforcing phases. The preparation process mainly comprises the processes of pulp flowing/net hanging forming, plate blank compacting, pre-curing, steam pressure curing, sanding, edge cutting and the like. The calcium silicate board has the advantages of high strength, small wet expansion rate, low heat conductivity coefficient, good fireproof performance, no toxicity, no harm and the like, and is an inorganic board with great development potential. At present, the medium-high density calcium silicate board (950-1400 kg/m) 3 ) The production and application of the calcium silicate board in the outer wall are quite common, but the calcium silicate board has the problems of heavy weight, poor toughness of the board and the like, and the application of the calcium silicate board in the aspect of decorative inner walls is severely limited.
At present, the research and development and production of low-density calcium silicate boards are not mature yet in China, and the density of the low-density calcium silicate boards meeting the performance requirements is still generally higher than 1000kg/m 3 . Generally, in order to ensure that the calcium silicate board has lower density, each production enterprise does not adopt a board blank compaction process, which directly results in the defects of poor flexural strength (6-8 MPa), more surface voids, low strength, further sudden increase of water absorption rate of the board, poor freeze-thaw resistance and the like of the board, and seriously influences the actual use effect of the calcium silicate board. Chinese patent application with application number of 202010427750.2 entitled "preparation of high-strength high-toughness low-density wood fiber calcium silicate board and formulation thereof" adopts alkaliThe wood fiber after the activation of the metal oxide replaces more than 50 percent of paper pulp to prepare the light calcium silicate board, but the density still reaches 900-1100 kg/m 3 . The Chinese patent with the application number of 201510319908.3, named as a low-density fiber-reinforced calcium silicate fireproof plate and a preparation method thereof prepares a low-density calcium silicate plate by a method of increasing the content (8-12%) of imported plant fibers in the plate and not compacting the plate blank, but the plant fiber dosage in the method is obviously higher than the conventional dosage (5-7%), so that the production cost is greatly increased and the surface strength of the plate is low.
In view of the problems encountered in the production and application of the low-density calcium silicate board, there is a need to find a more reasonable method for producing a low-density calcium silicate board with low density, high strength and low cost, which is more suitable for interior decoration.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide a preparation method of a low-density interior calcium silicate board.
The invention also aims to provide the low-density interior calcium silicate board prepared by the method.
It is a further object of the present invention to provide the use of said low density interior calcium silicate board.
The purpose of the invention is realized by the following technical scheme:
a preparation method of a low-density interior calcium silicate board comprises the following steps:
(1) Preparing hollow silica microspheres by an emulsion method:
(1) adding nano silicon dioxide particles into the oil phase to obtain a nano silicon dioxide suspension with the solid content of 20-50 wt%, and fully and uniformly stirring at the temperature of 60 +/-5 ℃ to obtain a suspension A;
(2) adding the suspension A obtained in the step (1) into an aqueous solution containing a surfactant under the condition of continuous stirring, and adjusting the pH value of the system to 12-14 to obtain a pre-reaction emulsion B;
(3) heating the pre-reaction emulsion B to 180-220 ℃, preserving heat for pre-polymerization reaction, centrifuging and washing to obtain a solid silicon dioxide microsphere prepolymer; then calcining the solid silica microsphere prepolymer at 600 ℃ to obtain hollow silica microspheres;
(2) Preparation of Mixed Green stock
Mixing the hollow silicon dioxide microspheres obtained in the steps (1) and (3), a siliceous material, a calcareous material, cement and plant fibers to prepare mixed blank slurry with the solid content of 10-15 wt%; wherein the total silicon-calcium ratio is 0.8-1.0;
(3) Preparation of low-density interior calcium silicate board
And (3) forming the mixed blank slurry obtained in the step (2) into a wet plate blank by netting, then carrying out plate compaction treatment on the wet plate blank under the compaction pressure of not less than 23MPa, and then carrying out autoclaved curing to obtain a formed plate, namely the low-density interior calcium silicate plate.
The particle size of the nano silicon dioxide particles in the step (1) is 10-100 nm.
The oil phase in the step (1) comprises one or more of silicone oil, cyclohexane and kerosene; preferably silicone oil, cyclohexane, or a mixture of silicone oil, cyclohexane and kerosene; more preferably a silicone oil, cyclohexane, or an oil phase obtained by mixing a silicone oil, cyclohexane and kerosene in a mass ratio of 5.
The surfactant in the step (2) comprises one or more of sodium dodecyl sulfate, polyethylene glycol monolaurate and polyoxyethylene lauryl ether.
The concentration of the aqueous solution containing the surfactant in the step (2) is 10-20% by mass; preferably 10% by mass.
The addition amount of the surfactant-containing aqueous solution in the step (2) is 50% of the volume of the oil phase.
The pH value of the adjusting system in the step (2) is adjusted by adopting a sodium hydroxide solution; preferably, the sodium hydroxide solution with the mass percent of 4-12% is adopted for adjustment.
The pH value of the adjusting system in the step (2) is preferably adjusted to 13.
The temperature of the prepolymerization reaction in the step (3) is preferably 200 ℃.
The prepolymerization reaction time (namely the heat preservation time) in the step (3) is 1-5 h; preferably for 2 hours.
The calcining time in the step (3) is 4-8 h; preferably 6h.
The hollow silica microspheres in the step (2) account for 10-20% of the weight of the siliceous material.
The siliceous material in the step (2) is quartz sand.
The calcareous material in the step (2) is quicklime.
The cement in the step (2) is Portland cement; preferably portland cement 425#.
The cement in the step (2) accounts for 10-15 wt% of the total solid content of the mixed blank slurry.
The plant fiber in the step (2) is one or more of unbleached softwood pulp, hemp pulp and waste cement bag paper pulp; preferably unbleached softwood pulp, waste water mud bag paper pulp, or mixed pulp of jute pulp and waste water mud bag paper; more preferably unbleached softwood pulp, waste cement sack pulp, hemp pulp and waste cement sack paper, and the mass ratio of the mixed pulp to the waste cement sack paper is 1.
The plant fiber in the step (2) accounts for 5 to 7 weight percent of the total solid content of the mixed blank slurry.
The wet plate blank in the step (3) is preferably made into the wet plate blank by adopting a long-wire pulp flowing process or a cylinder mould picking process.
The compaction pressure of the plate compaction treatment in the step (3) is preferably 23-25 MPa; more preferably 25MPa.
The compacting time of the plate compacting treatment in the step (3) is 10-30 min; preferably 20min.
The steam pressure curing in the step (3) is realized by the following mode: curing the wet plate blank subjected to the plate compacting treatment at 40 ℃ for 4-12 h (preferably 4 h), and then placing the wet plate blank into a steam curing kettle at 150-170 ℃ for steam curing for 12-15 h.
The preparation method of the low-density interior calcium silicate board further comprises the steps of demoulding, edge trimming and sanding the obtained formed board after the step (3).
A low density interior calcium silicate board prepared by any one of the above methods.
The low-density interior calcium silicate board is applied to building materials.
The building material comprises a decorative inner wall.
Compared with the prior art, the invention has the following advantages and effects:
1. the invention provides a high-strength, compactable and low-density interior calcium silicate board, aiming at the problems that the light board has poor flexural strength and more surface voids, and further the board has suddenly increased water absorption rate, poor freeze-thaw resistance and the like caused by the technology of reducing board density without compacting a board blank in the preparation process of the existing low-density calcium silicate board.
2. The density of the low-density interior calcium silicate board provided by the invention can be reduced to 700-900 kg/m 3 The method adopts the hollow silica microspheres to partially replace siliceous materials, allows the wet plate blank to be compacted, greatly improves the strength of the low-density calcium silicate plate, ensures that a large amount of hollow gaps are still formed in the plate after the plate is compacted by adding the hollow silica microspheres, and can flexibly adjust the density of the plate.
3. The hollow silica microspheres with high specific surface are introduced in the invention, and the nucleation and growth of tobermorite can be accelerated in the steam curing process, so that the steam curing time is reduced, the heat energy consumption is reduced, and the production cost is reduced.
4. The method provided by the invention can be suitable for preparing low-density calcium silicate boards with various purposes, and provides a powerful guarantee for the innovative development and the expansion of the application range of the calcium silicate boards.
Detailed Description
The present invention will be described in further detail with reference to examples, but the embodiments of the present invention are not limited thereto. The experimental methods in the following examples, which are not specified under specific conditions, are generally performed under conventional conditions. The raw materials and reagents used in the following examples are commercially available unless otherwise specified.
In the present invention, all percentages (%) are mass percentages (wt%) unless otherwise specified.
The oil phase comprises one or more of silicone oil, cyclohexane, kerosene and the like; among them, the silicone oil referred to in the examples is a conventional commercially available methyl silicone oil.
The siliceous material related to the embodiment of the invention is quartz sand; the calcareous material is quicklime; the cement is Portland cement No. 425.
The plant fiber in the invention can be one or more of unbleached softwood pulp, hemp pulp and waste water mud bag paper pulp; the examples relate to vegetable fibres as unbleached softwood pulp (rainbow brand), waste bag pulp (domestic waste pulp), or mixed pulp of hemp pulp (selisar brand) and waste bag pulp (domestic waste pulp), all of which are purchased from national trade ltd.
Example 1 preparation of Low Density interior calcium silicate Board
(1) Preparing hollow silica microspheres:
(1) preparing hollow silica microsphere emulsion by adopting an emulsion method, firstly adding nano silica particles with the particle size of 10nm into an oil phase (silicone oil) to obtain nano silica suspension with the solid content of 20wt%, and fully stirring at 60 ℃ to obtain suspension A;
(2) gradually adding a 10wt% aqueous solution of a surfactant (sodium dodecyl sulfate) into the suspension A obtained in the step (1) under the condition of continuous stirring, wherein the addition amount of the aqueous solution is 50% (v/v) of the volume of an oil phase (silicone oil), then adding a sodium hydroxide solution (mass fraction is 4%), and adjusting the pH value of the system to be 13 to obtain a pre-reaction emulsion B;
(3) heating the pre-reaction emulsion B to 200 ℃, preserving the heat for 2 hours to complete the pre-polymerization reaction of the hollow silica microspheres, centrifuging and washing to obtain a solid silica microsphere prepolymer, and calcining the obtained solid silica microsphere prepolymer at 600 ℃ for 6 hours to finally obtain the hollow silica microspheres.
(2) Mixing raw materials: mixing the hollow silica microspheres obtained in the step (1) with a siliceous material, a calcareous material, cement and plant fibers (unbleached softwood pulp), and adding water to prepare a mixed blank slurry with the solid content of 10wt%; wherein the total silicon-calcium ratio (the ratio of calcium element to silicon element) is 0.8, the hollow silicon dioxide microspheres account for 10wt% of the siliceous material, the cement accounts for 10wt% of the total solid content, and the unbleached softwood pulp accounts for 5wt% of the total solid content.
(3) And (3) net surfing molding: and (3) preparing the mixed blank slurry obtained in the step (2) into a wet plate blank by adopting a fourdrinier pulp flowing process or a cylinder mould picking process.
(4) Plate compacting: compacting the wet plate blank obtained in the step (3) on a press for 20min, wherein the compacting pressure is not lower than 23MPa (the pressure is set to be 25MPa in the experiment).
(5) Steam pressure curing: and (4) curing the compacted wet plate blank obtained in the step (4) at 40 ℃ for 4 hours, and then placing the wet plate blank in a steam curing kettle at 150 ℃ for steam curing for 12 hours to obtain a formed plate.
(6) And (5) demolding, trimming and sanding the formed plate obtained in the step (5) to obtain the low-density interior calcium silicate plate.
Example 2 preparation of Low Density interior calcium silicate Board
(1) Preparing hollow silica microspheres:
(1) preparing hollow silica microsphere emulsion by adopting an emulsion method, firstly adding nano silica particles with the particle size of 50nm into an oil phase (cyclohexane) to obtain nano silica suspension with the solid content of 35wt%, and fully stirring at 60 ℃ to obtain suspension A;
(2) gradually adding a 10wt% aqueous solution of a surfactant (polyethylene glycol monolaurate) into the suspension A obtained in the step (1) under the condition of continuous stirring, adding 50% (v/v) of the volume of the oil phase (cyclohexane), then adding a sodium hydroxide solution (mass fraction is 8%), and adjusting the pH value of the system to be 13 to obtain a pre-reaction emulsion B;
(3) heating the pre-reaction emulsion B to 200 ℃, preserving heat for 2h to complete the pre-polymerization reaction of the hollow silica microspheres, centrifuging and washing to obtain a solid silica microsphere prepolymer, and calcining the obtained solid silica microsphere prepolymer at 600 ℃ for 6h to finally obtain the hollow silica microspheres.
(2) Mixing raw materials: mixing the hollow silica microspheres obtained in the step (1) with a siliceous material, a calcareous material, cement and plant fibers (waste water sludge bag pulp), and adding water to prepare a mixed blank slurry with the solid content of 13 wt%; wherein the total silicon-calcium ratio is 0.9, the hollow silicon dioxide microspheres account for 15wt% of the siliceous material, the cement accounts for 7wt% of the total solid content, and the waste cement bag pulp accounts for 6wt% of the total solid content.
(3) And (3) net surfing molding: and (3) preparing the mixed blank slurry obtained in the step (2) into a wet plate blank by adopting a long-net pulp flowing process or a cylinder mould copying process.
(4) Plate compacting: compacting the wet plate blank obtained in the step (3) on a press for 20min, wherein the compacting pressure is not lower than 23MPa (the pressure is set to be 25MPa in the experiment).
(5) Steam pressure curing: and (4) curing the compacted wet plate blank obtained in the step (4) at 40 ℃ for 4 hours, and then placing the wet plate blank in a steam curing kettle at 160 ℃ for steam curing for 13 hours to obtain a formed plate.
(6) And (5) demolding, trimming and sanding the formed plate obtained in the step (5) to obtain the low-density interior calcium silicate plate.
Example 3 preparation of Low Density interior calcium silicate Board
(1) Preparing hollow silica microspheres:
(1) preparing hollow silica microsphere emulsion by adopting an emulsion method, firstly adding nano silica particles with the particle size of 100nm into an oil phase (a mixed solution of silicone oil, cyclohexane and kerosene, wherein the mass ratio is methyl silicone oil: cyclohexane: kerosene =5: 2) to obtain a nano silica suspension with the solid content of 50wt%, and fully stirring at the temperature of 60 ℃ to obtain a suspension A;
(2) gradually adding 10wt% of surfactant (polyoxyethylene lauryl ether) aqueous solution into the suspension A obtained in the step (1) under the condition of continuous stirring, wherein the adding amount is 50% (v/v) of the volume of the oil phase (cyclohexane), and then adding sodium hydroxide solution (the mass fraction is 12%), and adjusting the pH value of the system to be 13 to obtain pre-reaction emulsion B;
(3) heating the pre-reaction emulsion B to 200 ℃, preserving heat for 2h to complete the pre-polymerization reaction of the hollow silica microspheres, centrifuging and washing to obtain a solid silica microsphere prepolymer, and calcining the obtained solid silica microsphere prepolymer at 600 ℃ for 6h to finally obtain the hollow silica microspheres.
(2) Mixing raw materials: mixing the hollow silica microspheres obtained in the step (1) with a siliceous material, a calcareous material, cement and plant fibers (gunite and waste water mud bag paper mixed pulp, the mass ratio of the gunite to the waste water mud bag paper pulp = 1), and adding water to prepare a mixed blank slurry with a solid content of 15 wt%; wherein the total silicon-calcium ratio is 1.0, the hollow silicon dioxide microspheres account for 20wt% of the siliceous material, the cement accounts for 5wt% of the total solid content, and the hemp pulp and the waste cement bag paper mixed pulp account for 7wt% of the total solid content.
(3) And (3) net surfing molding: and (3) preparing the mixed blank slurry obtained in the step (2) into a wet plate blank by adopting a long-net pulp flowing process or a cylinder mould copying process.
(4) Plate compacting: compacting the wet plate blank obtained in the step (3) on a press for 20min, wherein the compacting pressure is not lower than 23MPa (the pressure is set to be 25MPa in the experiment).
(5) Steam pressure curing: and (5) curing the compacted wet plate blank obtained in the step (4) at 40 ℃ for 4 hours, and then placing the wet plate blank in a steam curing kettle at 170 ℃ for steam curing for 15 hours to obtain a formed plate.
(6) And (5) demolding, trimming and sanding the formed plate obtained in the step (5) to obtain the low-density interior calcium silicate plate.
Comparative example 1 preparation of Low Density calcium silicate Board
In the comparative example, a conventional manufacturing method of the low-density calcium silicate board is adopted, no hollow silicon dioxide microspheres are added, and the board is not compacted, and the specific steps are as follows:
(1) Mixing raw materials: mixing siliceous materials, calcareous materials, cement and plant fibers (unbleached softwood pulp) to prepare mixed blank slurry with the solid content of 10wt%; wherein the total silicon-calcium ratio is 0.8, the cement accounts for 10wt% of the total solid content, and the unbleached softwood pulp accounts for 7wt% of the total solid content.
(2) And (3) net surfing molding: and (2) preparing the mixed blank slurry obtained in the step (1) into a wet plate blank by adopting a long-net pulp flowing process or a cylinder mould copying process.
(3) Steam pressure curing: and (3) curing the compacted wet plate blank obtained in the step (2) at 40 ℃ for 4 hours, and then placing the wet plate blank in a steam curing kettle at 160 ℃ for steam curing for 12 hours to obtain a formed plate.
(4) And (4) demolding the formed plate obtained in the step (3), trimming and sanding to obtain the low-density calcium silicate plate.
Comparative example 2 preparation of Low Density calcium silicate Board
In this comparative example, a hollow silica microsphere prepared by a template method was used as a comparison, in which a polystyrene microsphere was used as a template and tetraethoxysilane was used as a precursor (refer to the preparation method of the hollow microsphere with porous silica microspheres with a high structural strain via a Sol-Gel process. Journal of Sol-Gel Science and technology. DOI:10.1007/s 10971-015-3691-7.), specifically comprising the following steps:
(1) Mixing raw materials: mixing hollow silica microspheres prepared by a template method, a siliceous material, a calcareous material, cement and plant fibers (gunite and waste water mud bag paper mixed pulp, the mass ratio of the gunite to the waste water mud bag paper pulp = 1); wherein the total silicon-calcium ratio is 1.0, the hollow silicon dioxide microspheres prepared by the template method account for 20wt% of the siliceous material, the cement accounts for 5wt% of the total solid content, and the hemp pulp and waste water mud bag paper mixed pulp accounts for 7wt% of the total solid content.
(2) And (3) net surfing molding: and (2) preparing the mixed blank slurry obtained in the step (1) into a wet plate blank by adopting a long-net pulp flowing process or a cylinder mould copying process.
(3) Plate compacting: compacting the wet plate blank obtained in the step (2) on a press, wherein the compacting time is 20min, and the compacting pressure is 25MPa.
(4) Steam pressure curing: and (4) curing the compacted wet plate blank obtained in the step (3) at 40 ℃ for 4 hours, and then placing the wet plate blank in a steam curing kettle at 160 ℃ for steam curing for 12 hours to obtain a formed plate.
(5) And (5) demolding the formed plate obtained in the step (4), trimming and sanding to obtain the low-density calcium silicate plate.
Effects of the embodiment
The low-density interior calcium silicate boards manufactured in examples 1 to 3 and the low-density calcium silicate boards manufactured in comparative examples 1 to 2 were subjected to tests for flexural strength (GB/T7019-2014), density (GB/T7019-2014), freeze-thaw resistance (GB/T7019-2014), water absorption (GB/T7019-2014), wet swell (GB/T7019-2014), incombustibility (GB/T5465-2010), and dry shrinkage (JC/T564.1-2008), and the results are shown in table 1 below.
TABLE 1 test of the properties of the sheets of the examples and comparative examples
Figure BDA0003487060620000081
Tests prove that the hollow silicon dioxide microspheres prepared by the emulsion method partially replace siliceous materials, the wet plate blank is allowed to be compacted, the strength of the low-density calcium silicate plate is greatly improved, and the density of the low-density calcium silicate plate can be 700-900 kg/m 3 Flexible and reliable control. It is worth noting that the hollow silica microspheres prepared by the conventional template method have poor strength and are difficult to maintain the original shape in the air in the slab compaction process, so that the density of the plate is still high. The data prove that the strength and other performance indexes of the low-density interior calcium silicate board can be improved while the density of the board is reduced by adopting the technology provided by the invention.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.

Claims (7)

1. A preparation method of a low-density interior calcium silicate board is characterized by comprising the following steps:
(1) Preparing hollow silicon dioxide microspheres by an emulsion method:
(1) adding nano silicon dioxide particles into the oil phase to obtain a nano silicon dioxide suspension with the solid content of 20-50 wt%, and fully and uniformly stirring at the temperature of 60 +/-5 ℃ to obtain a suspension A;
(2) adding the suspension A obtained in the step (1) into an aqueous solution containing a surfactant under the condition of continuous stirring, and adjusting the pH value of the system to 12-14 by using a sodium hydroxide solution to obtain a pre-reaction emulsion B;
(3) heating the pre-reaction emulsion B to 180-220 ℃, preserving heat for pre-polymerization reaction, centrifuging and washing to obtain a solid silicon dioxide microsphere prepolymer; then calcining the solid silica microsphere prepolymer at 600 ℃ to obtain hollow silica microspheres;
(2) Preparation of Mixed Green slurry
Mixing the hollow silicon dioxide microspheres obtained in the steps (1) and (3), a siliceous material, a calcareous material, cement and plant fibers to prepare mixed blank slurry with the solid content of 10-15 wt%; wherein the total silicon-calcium ratio is 0.8-1.0;
(3) Preparation of Low Density interior calcium silicate Board
Forming the mixed blank slurry obtained in the step (2) into a wet plate blank by netting, then carrying out plate compacting treatment on the wet plate blank under the compacting pressure of 23-25 MPa, and then carrying out autoclaved curing to obtain a formed plate, namely the low-density interior calcium silicate plate;
the particle size of the nano silicon dioxide particles in the step (1) is 10-100 nm;
the oil phase in the step (1) comprises one or more of silicone oil, cyclohexane and kerosene;
the surfactant in the step (2) comprises one or more of sodium dodecyl sulfate, polyethylene glycol monolaurate and polyoxyethylene lauryl ether;
the concentration of the aqueous solution containing the surfactant in the step (2) is 10-20% by mass percent;
the addition amount of the aqueous solution containing the surfactant in the step (2) is 50% of the volume of the oil phase;
the siliceous material in the step (2) is quartz sand;
the calcareous material in the step (2) is quicklime;
the cement in the step (2) is Portland cement;
the plant fiber in the step (2) is one or more of unbleached softwood pulp, hemp pulp and waste water mud bag paper pulp;
the hollow silica microspheres in the step (2) account for 10 to 20 percent of the weight of the siliceous material;
the cement in the step (2) accounts for 5wt%, 7wt% or 10wt% of the total solid content of the mixed blank slurry;
the plant fiber in the step (2) accounts for 5 to 7 weight percent of the total solid content of the mixed blank slurry;
the compacting time of the plate compacting treatment in the step (3) is 10-30 min.
2. The method for preparing a low-density interior calcium silicate board according to claim 1, wherein:
the oil phase in the step (1) is silicone oil, cyclohexane, or an oil phase obtained by mixing the silicone oil, the cyclohexane and the kerosene according to a mass ratio of 5;
the cement in the step (2) is Portland cement 425#;
the plant fiber in the step (2) is unbleached softwood pulp, waste water mud bag pulp or mixed pulp obtained by mixing hemp pulp and the waste water mud bag pulp according to the mass ratio of 1.
3. The method for preparing a low-density interior calcium silicate board according to claim 1, wherein:
the steam pressure curing in the step (3) is realized by the following mode: curing the wet plate blank subjected to the plate compacting treatment at 40 ℃ for 4-12 h, and then placing the wet plate blank into a steam curing kettle at 150-170 ℃ for steam curing for 12-15 h.
4. The method for preparing a low-density interior calcium silicate board according to claim 1, wherein:
the pH value of the adjusting system in the step (2) is adjusted to 13;
the temperature of the prepolymerization reaction in the step (3) is 200 ℃;
the prepolymerization reaction time in the step (3) is 1-5 h;
the calcining time in the step (3) is 4-8 h.
5. The method for preparing a low-density interior calcium silicate board according to claim 1, wherein: and (4) after the step (3), the steps of demoulding, edge trimming and sanding are carried out on the obtained formed plate.
6. A low-density interior calcium silicate board is characterized in that: prepared by the method of any one of claims 1 to 5.
7. Use of the low-density interior calcium silicate board of claim 6 in building materials.
CN202210084691.2A 2022-01-25 2022-01-25 Low-density interior calcium silicate board and preparation method and application thereof Active CN114409335B (en)

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CN1350992A (en) * 2000-10-26 2002-05-29 苏州台荣建材有限公司 Light calcium silicate plate and its preparing process
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