CN108069694A - A kind of calcium silicate board and preparation method thereof - Google Patents
A kind of calcium silicate board and preparation method thereof Download PDFInfo
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- CN108069694A CN108069694A CN201711334112.0A CN201711334112A CN108069694A CN 108069694 A CN108069694 A CN 108069694A CN 201711334112 A CN201711334112 A CN 201711334112A CN 108069694 A CN108069694 A CN 108069694A
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- calcium silicate
- silicate board
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- slurry
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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
- C04B30/00—Compositions for artificial stone, not containing binders
- C04B30/02—Compositions for artificial stone, not containing binders containing fibrous materials
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/20—Silicates
- C01B33/24—Alkaline-earth metal silicates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
-
- 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
- C04B2201/20—Mortars, concrete or artificial stone characterised by specific physical values for the density
-
- 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
- C04B2201/30—Mortars, concrete or artificial stone characterised by specific physical values for heat transfer properties such as thermal insulation values, e.g. R-values
- C04B2201/32—Mortars, concrete or artificial stone characterised by specific physical values for heat transfer properties such as thermal insulation values, e.g. R-values for the thermal conductivity, e.g. K-factors
-
- 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
Abstract
The invention belongs to green energy-conserving construction material technical fields, specifically disclose a kind of method of calcium silicate board；It is obtained by the repressed shaping of hydrated calcium silicate fiber.The slurry that hydrated calcium silicate fiber of the present invention is prepared by siliceous raw material, calcareous raw material, alkali and water is prepared under 120~260 DEG C of hydrothermal condition.The unit weight of calcium silicate board produced by the present invention is 0.8~1.5g/cm3, thermal conductivity factor is 0.02~0.5W/ (mK), and flexural strength is 1~15MPa, and compression strength is 1~50MPa.The present invention prepares hydrated calcium silicate fiber source that calcium silicate board uses in Industrial Solid Waste flyash, and cost of material is low；Using hydrated calcium silicate fiber as raw material, calcium silicate board is prepared using compression moulding technique, compared with traditional steaming pressuring curing process, production procedure is short, and preparation efficiency is high, and product quality is easy to get control, is conducive to the high value added utilization of fly ash.
Description
Technical field
The present invention relates to the preparation methods of calcium silicate board；Belong to green energy-conserving construction material technical field.
Background technology
Calcium silicate board is that (main ingredient is SiO by siliceous material2, such as silica flour, flyash, diatomite), calcareous material
Material (main ingredient is CaO, such as lime, carbide slag, cement), reinforcing fiber, auxiliary agent etc. mix according to a certain percentage, through mould
It presses, copy and take or flow a kind of novel energy-conserving building materials made of the processes such as slurry, steam press maintenance.Because its intensity is high, unit weight is low, and with good
Good machinability and noninflammability, so be widely used the shifting board in ship, furred ceiling and building non-bearing wall body and
There are other places of fire protection requirement.JC/T564.1-2008《Fiber reinforced calcium silicate board》Fiber reinforced calcium silicate board is determined
Justice：It is cementing based on siliceous-calcareous material using the loose staple fiber such as inorganic mineral fiber or cellulose fibre as reinforcing material
Material through slurrying, shaping, accelerates curing reaction in high temperature and pressure saturated vapor, forms calcium silicates gel and manufactured plate
Material.Definition to steam press maintenance：Refer in calcium silicate board with microporous production process, manufactured material base (water content is generally below 1mL/g) is sent into pressure
It steams in kettle, through about (0.8~1.0) MPa, 180 DEG C or so of high pressure, high temperature action, promotes to excite siliceous-calcareous material in raw material
Activity, promote that hydration reaction occurs, generate main hydration products and a certain number of adhesive bonds and generate the process of intensity.Cause
This, calcium silicate board is actually that tobermorite crystal adds fiber reinforcement.If siliceous-calcareous raw material is during steam pressure
It reacts insufficient, causes the forming amount of tobermorite crystal not enough or form other to substitute ingredient, will result in silicic acid
The mechanical strength of calcium panel products is not high or even as waste product (soft board).
To solve drawbacks described above existing for existing calcium silicate board production technology, the prior art is mainly substituted by adding cement
Part quick lime.For example, the Chinese patent literature of Publication No. CN102786278A discloses a kind of non-asbestos fibre silicon
Sour calcium plate, it is characterised in that：Each composition of the non-asbestos fibre calcium silicate board is matched somebody with somebody by following weight percent
Than：Waste ceramic powder 15~25%, cement 35~40%, konilite 20~30%, quick lime 8~10%, organic fiber 7~
10%, inorganic thickening agent 1~2%, antifoaming agent 0.5~1%.
The purpose of addition cement is the intensity for increasing calcium silicate board using the intensity of hydrated cementitious formation and utilizes water
The characteristics of mud is calcic raw material substitutes part quick lime, so as to reduce production cost.But cement is in calcium silicate board production
Additive amount is difficult to control, and cement consumption is few, and humidification is not had to the mechanical strength of calcium silicate board；Dosage is excessive, can cause
Calcium silicate board product colour deepens and reduces quality, and can increase the deformation coefficient of calcium silicate board, makes product that use be not achieved
It is required that.
The content of the invention
To solve technical problem existing in the prior art, the present invention provides a kind of preparation methods of calcium silicate board, it is intended to
It is raw material using the hydrated calcium silicate fiber, prepares calcium silicate board novel energy-conserving building materials, promote the synthesis of fly ash
It utilizes.
A kind of preparation method of calcium silicate board is obtained by the repressed shaping of hydrated calcium silicate fiber.
The study found that it is raw material using the hydrated calcium silicate fiber of hydrothermal synthesis, unit weight can be made in direct pressing shaping
It is small, thermal conductivity factor is low, the calcium silicate board product of excellent thermal insulation performance；In addition, under relatively low unit weight of the present invention, moreover it is possible to
Ensure that the indices such as the mechanical strength of calcium silicate board all meet using standard.
Preferably, a diameter of 0.01~1 μm of the hydrated calcium silicate fiber；Length is 0.5~20 μm.The present invention
People can not only meet calcium silicate products also the study found that using the preferred diameter and the hydrated calcium silicate fiber of length range
The requirement of middle tobermorite content, can also unexpectedly play the role of it is fibre-reinforced, so as to avoid using other ore deposits
Fibres or industrial chemicals, economize on resources, and environmental protection is environmentally protective.
Further preferably, a diameter of 0.05~0.2 μm of the hydrated calcium silicate fiber；Length is 3~20 μm.
Preferably, the draw ratio of hydrated calcium silicate fiber is 10~200.Using the aquation silicic acid of the preferred draw ratio
Calcium fiber, the unit weight and thermal conductivity factor for the calcium silicate board suppressed are lower, and calcium silicate board is lighter, more keeps the temperature.
Further preferably, the draw ratio of hydrated calcium silicate fiber is 50~200.
Preferably, the calcium silicon atom ratio (elemental mole ratios) of hydrated calcium silicate fiber is 0.3~2.Under the preferred proportion
Hydrated calcium silicate fiber main mineral constituent for tobermorite, the pattern of tobermorite is the aggregate of threadiness, tool
There is the features such as hole is flourishing, thermal conductivity factor and unit weight are low.
The study found that the calcium silicon atom ratio (elemental mole ratios) of hydrated calcium silicate fiber is 0.5~1.In the preferred calcium
Under silicon atom ratio, coordinate preferred draw ratio, help further to promote the performance of calcium silicate board.
Preferably, the hydrated calcium silicate fiber is existed by the slurry that siliceous raw material, calcareous raw material, alkali and water are prepared
It is prepared under 120~260 DEG C of hydrothermal condition.
It is found by numerous studies, under the temperature range, carries out the hydro-thermal reaction, the aquation finally obtained
Ca silicate fibre is particularly suitable for preparing calcium silicate board.Research shows fine using hydrated calcium silicate obtained under the temperature range
The indices such as dimension, the thermal conductivity factor and unit weight of calcium silicate board obtained can meet requirement.
The siliceous raw material can be the material that quartz, flyash, slag etc. mainly contain silica.
The calcareous raw material can be the material that lime, carbide slag etc. mainly contain CaO.
In preparation method of the present invention, hydrothermal temperature is more crucial.Preferably, the temperature of hydro-thermal reaction is 200~220
℃.The hydrated calcium silicate fiber that hydro-thermal obtains at such a temperature is more conducive to the promotion of calcium silicate board overall performance.
In the present invention, the hydro-thermal reaction carries out in closed container.Under the hydrothermal condition, hydro-thermal reaction
Pressure is preferably 0.2~5MPa；Preferably 1.5MPa~2.5MPa.
Hydrated calcium silicate fiber used in the present invention is to utilize flyash and quick lime as main raw material(s), anti-by hydro-thermal
It should be prepared；Principle is simple, easily promotes and applies, may advantageously facilitate the comprehensive utilization of fly ash and energy-saving building material product
Resource regeneration.
Preferably, in slurry, the calcium silicon mol ratio of flyash and quick lime is 0.3~1.5；Further preferably 0.4
~1.0.The calcium silicon mol ratio in slurry is controlled, contributes to the calcium silicate board haveing excellent performance.
The inventors discovered that water-heat process exogenously added alkali, coordinates the hydrothermal reaction condition, the material that such hydro-thermal obtains
Contribute to the performance of calcium silicate board made from being promoted, for example, further helping in the unit weight for reducing calcium silicate board, reduce its heat conduction
Coefficient promotes heat-insulating property.
Preferably, the alkali is alkali metal hydroxide；Preferably potassium hydroxide and/or sodium hydroxide；Further
Preferably sodium hydroxide.
Preferably, in slurry, the concentration of alkali is less than or equal to 100g/L.The alkali of the concentration is added, is contributed into one
Step promotes the formation efficiency of hydrated calcium silicate fiber, helps to obtain the aquation that draw ratio is more excellent, is more suitable for calcium silicate board preparation
Ca silicate fibre.
Further preferably, in slurry, the concentration of alkali is 5~30g/L.Under the preferred concentration, obtained aquation silicic acid
Calcium fiber is more suitable for the preparation of calcium silicate board, and the unit weight of calcium silicate board obtained is lower, and heat-insulating property is more excellent.
Most preferably, in slurry, the concentration of alkali is 5~20g/L.
It that is to say, the pH for controlling slurry (starting slurry of hydro-thermal reaction) is 11~14；Further preferably 13~14.
Preferably, in slurry, liquid-solid ratio is 5~30mL/g；Further preferably 10~20mL/g.Described in the present inventor
Slurry be calcareous raw material, the alkaline aqueous solution of siliceous raw material, by it is carried out it is described under the conditions of hydro-thermal reaction, contribute to
Hydrated calcium silicate fiber must be made in high yield, additionally aid the performance for promoting the calcium silicate board subsequently obtained.
Under the hydrothermal condition, suitable the hydro-thermal reaction time is controlled, further promotion can prepare calcium silicate board
Performance helps further to promote the application prospect that calcium silicate board is made.
Preferably, the hydro-thermal reaction time is 0.5~12h；Further preferably 1~5h.
The present inventor is also by the study found that by the temperature of hydrothermal reaction process, pH, liquid-solid ratio control described preferred
In the range of, it can help to obtain more conducively tobermorite by the collaboration of the parameter and formed and then further promote silicic acid
The hydrated calcium silicate fiber of calcium plate performance.
The preferred preparation method of hydrated calcium silicate fiber is：By siliceous raw material, calcareous raw material, water according to calcium silicon mol ratio
It is that 5~30mL/g prepares slurry for 0.3~1.5 and liquid-solid ratio, adds in the pH value that the NaOH less than or equal to 30g/L adjusts slurry
(13~14).Prepared suspension slurry is added in into high-pressure closed vessel, temperature be 120~260 DEG C, the time be 0.5~
12h, mixing speed carry out hydrothermal synthesis under conditions of being 100~300rpm.
After hydro-thermal reaction, hydro-thermal reaction liquid is cooled to room temperature, after separation of solid and liquid, washing and drying, i.e.,
Obtain satisfactory hydrated calcium silicate fiber.
Hydrated calcium silicate fiber obtained is fully dehydrated；Then repressed shaping is to get the calcium silicate board.
Preferably, the pressure of compression moulding process is 1~100MPa.Further preferred compression moulding pressure for 10~
30MPs。
The dwell time is 1~60min at this pressure.
A kind of preparation method of preferred calcium silicate board of the present invention, comprises the following steps：
Step (1)：
The slurry that siliceous raw material, calcareous raw material, alkali and water are prepared is in 120~260 DEG C, the hydro-thermal that pressure is 0.2~5MPa
Under the conditions of hydrated calcium silicate fiber is prepared；
Step (2)：By hydrated calcium silicate fiber compression moulding made from step (1), calcium silicate board is obtained.
Preferably, in step (1), according to calcium silicon mol ratio be 0.4~1.0 and liquid-solid ratio is 10~20mL/g formulations
Slurry, the NaOH for adding in 5~20g/L adjust the pH value of slurry；Gained suspension slurry is put into pressure reaction still, stirring is warming up to
200 DEG C~220 DEG C, 1~5h of isothermal reaction under 1.5MPa~2.5MPa pressure；After reaction, slurry is cooled to room temperature,
Take out slurry, by separation of solid and liquid, washing and it is dry after to get to satisfactory hydrated calcium silicate fiber
Preferably, in step (2)：By the hydrated calcium silicate fiber obtained in step (1) fully drying and mixing, weigh
After add in it is framed, under the briquetting pressure of 10~50MPa maintain 10~30min, that is, the calcium silicate board being prepared.
It is 0.8~1.5g/cm the present invention also provides calcium silicate board unit weight made from a kind of preparation method3；Into
One step is preferably 0.8~1.2g/cm3.The material of the present invention, has relatively low unit weight, and material is light.
Preferably, thermal conductivity factor is 0.02~0.5W/ (mK)；Further preferably 0.08~0.2W/ (mK).This
The calcium silicate board of invention has relatively low thermal conductivity factor, has good heat-insulating property.
Calcium silicate board of the present invention, thickness are preferably 2~30mm；Further preferably 5~20mm.
Under unit weight of the present invention, it is 1~15MPa that calcium silicate board of the present invention, which still has flexural strength, is resisted
Compressive Strength is the performance of 1~50MPa；Fully meet requirement.
Preferably, the preparation method of the calcium silicate board, briquetting pressure is 10~50MPa, the dwell time for 10~
30min, calcium silicate board product thickness are 5~20mm, and unit weight is 0.8~1.2g/cm3, thermal conductivity factor is 0.08~0.2W/ (m
K), flexural strength is 5~15MPa, and compression strength is 10~30MPa.
Hydrated calcium silicate fiber used in the present invention is to utilize siliceous raw materials and lime, the calcium carbides such as quartz, flyash, slag
The calcareous raw materials such as slag are main raw material(s) (the siliceous and calcareous raw material of production calcium silicate board), are prepared by the method for hydrothermal synthesis
It obtains；Principle is simple, easily promotes and applies, may advantageously facilitate the Resource regeneration of energy-saving building material product.
The present invention is not only solved present in traditional calcium silicates board production technology since tobermorite growing amount is inadequate
And the problem of influencing product quality, meanwhile, using Industrial Solid Waste as raw material, be conducive to the comprehensive utilization of fly ash.
It is using the advantageous effect of the invention that can be obtained：
Calcium silicate board is prepared using hydrated calcium silicate fiber direct pressing shaping, calcium silicate board is prepared with traditional steam press maintenance
Technique compare, preparation principle is simple, flow is short, product quality is easy to get control, equipment investment and production cost are low, easily
It promotes and applies.
The hydrated calcium silicate fiber that the present invention uses is using Industrial Solid Waste flyash as primary raw material, by hydrothermal synthesis work
What skill was prepared.Tobermorite component content is high in product, and is the fibers form presence with crystal whisker-shaped, avoids using
Mineral fibres and other industrial chemicals, product quality is controllable, energy conservation and environmental protection, can realize the comprehensive development and utilization of Industrial Solid Waste.
In the present invention, under without outer doping, it still can unexpectedly obtain that unit weight is low, the silicic acid of excellent thermal insulation performance
Calcium plate, test show unit weight up to 0.8~1.5g/cm3, thermal conductivity factor can be 0.02~0.5W/ (mK).
Description of the drawings
Attached drawing 1 is the XRD diagram of hydrated calcium silicate fiber prepared by the embodiment of the present invention 3；
Attached drawing 2 is the SEM figures of hydrated calcium silicate fiber prepared by the embodiment of the present invention 3；
Attached drawing 3 is calcium silicate board figure prepared by the embodiment of the present invention 3.
It can be seen that from Fig. 1 and Fig. 2：Main component using water of coal ash thermal synthesis hydrated calcium silicate product is Tuo Beimo
Carry out stone, occur almost without the diffraction maximum of other object phases, illustrate that the impurity component content of hydrated calcium silicate product is very low；Tuo Beimo
The pattern for carrying out stone is in the fiber of crystal whisker-shaped, and fibre diameter is 0.01~0.2 μm, length is 5~20 μm, and draw ratio is up to 200.From
The calcium silicate board surface that Fig. 3 can be seen that compression moulding is more smooth, in canescence.
Specific embodiment
The chemical phase analysis of hydrated calcium silicate fiber uses x-ray diffractometer, and microstructure analysis uses scanning electron
Microscope.The detection method of calcium silicate board performance parameter, referring to JC_T 564.1-2008《Fiber reinforced calcium silicate board the 1st
Point：Asbestos-free calcium silicate board》Building material industry standard.
Embodiment 1：
Step (1)：
According to calcium silicon mol ratio be 0.3 and liquid-solid ratio is that 5mL/g prepares slurry, and the NaOH for adding in 5g/L adjusts the pH of slurry
Value (pH 13)；Gained suspension slurry is put into pressure reaction still, stirring is warming up to 160 DEG C, the constant temperature under 0.6MPa pressure
React 2h；After reaction, slurry is cooled to room temperature, takes out slurry, after separation of solid and liquid, washing and drying, obtain aquation
Calcium silicate products.Obtained product is subjected to XRD and sem analysis.The essential mineral composition of product is mullite, quartz and aquation
Gel of calcium silicate.A diameter of 0.01~0.1 μm of hydrated calcium silicate fiber, length are 1~3 μm, and draw ratio is 20~30；Aquation
The calcium silicon atom ratio of ca silicate fibre is 0.4.
Step (2)：
By the hydrated calcium silicate fiber obtained in step (1) is fully dry and mixing, added in after weighing it is framed, in 10MPa
Briquetting pressure under maintain 5min, obtain calcium silicate board (thickness 5mm).The unit weight of calcium silicate board product is 1.4g/cm3, heat conduction
Coefficient is 0.5W/ (mK), flexural strength 1MPa, compression strength 3MPa.
Embodiment 2：
Step (1)：
According to calcium silicon mol ratio be 0.6 and liquid-solid ratio is that 15mL/g prepares slurry, and the NaOH for adding in 15g/L adjusts slurry
PH value (pH 13.5)；Gained suspension slurry is put into pressure reaction still, stirring is warming up to 190 DEG C, under 1.5MPa pressure
Isothermal reaction 3h；After reaction, slurry is cooled to room temperature, takes out slurry, after separation of solid and liquid, washing and drying, obtained
Hydrated calcium silicate product.Obtained product is subjected to XRD and sem analysis.The main object of product is mutually mullite, Tuo Beimo comes
Stone, hydrated calcium silicate gel.A diameter of 0.05~0.3 μm of hydrated calcium silicate fiber, length are 3~5 μm, draw ratio for 50~
100；The calcium silicon atom ratio of hydrated calcium silicate fiber is 0.7.
Step (2)：
By the hydrated calcium silicate fiber obtained in step (1) is fully dry and mixing, added in after weighing it is framed, in 20MPa
Briquetting pressure under maintain 20min, obtain calcium silicate board (thickness 10mm).The unit weight of calcium silicate board product is 1.2g/cm3, lead
Hot coefficient is 0.3W/ (mK), flexural strength 3MPa, compression strength 15MPa.
Embodiment 3：
Step (1)：
According to calcium silicon mol ratio be 1.0 and liquid-solid ratio is that 30mL/g prepares slurry, and the NaOH for adding in 30g/L adjusts slurry
PH value (pH 14)；Gained suspension slurry is put into pressure reaction still, stirring is warming up to 220 DEG C, permanent under 2.5MPa pressure
Temperature reaction 5h；After reaction, slurry is cooled to room temperature, takes out slurry, after separation of solid and liquid, washing and drying, obtain water
Change calcium silicate products.Obtained product is subjected to XRD and sem analysis.The main object of product is mutually tobermorite.Aquation silicic acid
A diameter of 0.05~0.2 μm of calcium fiber, length are 10~20 μm, and draw ratio is 50~200；The calcium silicon of hydrated calcium silicate fiber
Atomic ratio is 0.9.
Step (2)：
By the hydrated calcium silicate fiber obtained in step (1) is fully dry and mixing, added in after weighing it is framed, in 30MPa
Briquetting pressure under maintain 30min, obtain calcium silicate board (thickness 15mm).The unit weight of calcium silicate board product is 1.0g/cm3, lead
Hot coefficient is 0.1W/ (mK), flexural strength 9MPa, compression strength 30MPa.
Embodiment 4：
Step (1)：
According to calcium silicon mol ratio be 1.2 and liquid-solid ratio is that 50mL/g prepares slurry, and the NaOH for adding in 50g/L adjusts slurry
PH value (pH 14)；Gained suspension slurry is put into pressure reaction still, stirring is warming up to 240 DEG C, permanent under 3.5MPa pressure
Temperature reaction 9h；After reaction, slurry is cooled to room temperature, takes out slurry, after separation of solid and liquid, washing and drying, obtain water
Change calcium silicate products.Obtained product is subjected to XRD and sem analysis.The main object of product is mutually tobermorite and hibschite.
A diameter of 0.1~0.5 μm of hydrated calcium silicate fiber, length are 5~10 μm, and draw ratio is 10~50；Hydrated calcium silicate fiber
Calcium silicon atom than 1.3.
Step (2)：
By the hydrated calcium silicate fiber obtained in step (1) is fully dry and mixing, added in after weighing it is framed, in 50MPa
Briquetting pressure under maintain 50min, obtain calcium silicate board (thickness 20mm).The unit weight of calcium silicate board product is 1.4g/cm3, lead
Hot coefficient is 0.3W/ (mK), flexural strength 6MPa, compression strength 40MPa.
Embodiment 5：
Step (1)：
According to calcium silicon mol ratio be 1.5 and liquid-solid ratio is that 20mL/g prepares slurry, and the NaOH for adding in 100g/L adjusts slurry
PH value (pH 14)；Gained suspension slurry is put into pressure reaction still, stirring is warming up to 120 DEG C, under 0.2MPa pressure
Isothermal reaction 12h；After reaction, slurry is cooled to room temperature, takes out slurry, after separation of solid and liquid, washing and drying, obtained
Hydrated calcium silicate product.Obtained product is subjected to XRD and sem analysis.The main object of product is mutually mullite, quartz, aquation
Gel of calcium silicate, analcime.A diameter of 0.01~0.1 μm of hydrated calcium silicate fiber, length are 1~2 μm, draw ratio for 10~
50；The calcium silicon atom ratio of hydrated calcium silicate fiber is 1.5.
Step (2)：
By the hydrated calcium silicate fiber obtained in step (1) is fully dry and mixing, added in after weighing it is framed, in 100MPa
Briquetting pressure under maintain 60min, obtain calcium silicate board (thickness 25mm).The unit weight of calcium silicate board product is 1.5g/em3, lead
Hot coefficient is 0.5W/ (mK), flexural strength 2MPa, compression strength 5MPa.
Embodiment 6：
Step (1)：
According to calcium silicon mol ratio be 0.8 and liquid-solid ratio is that 20mL/g prepares slurry, and the NaOH for adding in 20g/L adjusts slurry
PH value (pH 13.5)；Gained suspension slurry is put into pressure reaction still, stirring is warming up to 200 DEG C, under 2.0MPa pressure
Isothermal reaction 3h；After reaction, slurry is cooled to room temperature, takes out slurry, after separation of solid and liquid, washing and drying, obtained
Hydrated calcium silicate product.Obtained product is subjected to XRD and sem analysis.The main object of product is mutually tobermorite.Aquation silicon
A diameter of 0.01~0.1 μm of sour calcium fiber, length are 10~20 μm, and draw ratio is 50~200；The calcium of hydrated calcium silicate fiber
Silicon atom ratio is 0.75.
Step (2)：
By the hydrated calcium silicate fiber obtained in step (1) is fully dry and mixing, added in after weighing it is framed, in 100MPa
Briquetting pressure under maintain 60min, obtain calcium silicate board (thickness 30mm).The unit weight of calcium silicate board product is 1.3g/cm3, lead
Hot coefficient is 0.2W/ (mK), flexural strength 15MPa, compression strength 50MPa.
Embodiment 7
It is compared with embodiment 3, difference lies in be not added with alkali, concrete operations are as follows in feed liquid：
Step (1)：
According to calcium silicon mol ratio be 1.0 and liquid-solid ratio is that 30mL/g prepares slurry, is not added with NaOH (pH 11)；Gained is hanged
Buoyant slurry is put into pressure reaction still, and stirring is warming up to 220 DEG C, the isothermal reaction 5h under 2.5MPa pressure；After reaction, will
Slurry is cooled to room temperature, and takes out slurry, after separation of solid and liquid, washing and drying, obtains hydrated calcium silicate product.The production that will be obtained
Product carry out XRD and sem analysis.The main object of product is mutually mullite, hibschite, tobermorite.Hydrated calcium silicate fiber
A diameter of 0.01~0.1 μm, length is 1~3 μm, and draw ratio is 10~30；The calcium silicon atom ratio of hydrated calcium silicate fiber is
0.8。
Step (2)：
By the hydrated calcium silicate fiber obtained in step (1) is fully dry and mixing, added in after weighing it is framed, in 30MPa
Briquetting pressure under maintain 30min, obtain calcium silicate board (thickness 12mm).The unit weight of calcium silicate board product is 1.3g/cm3, lead
Hot coefficient is 0.25W/ (mK), flexural strength 3MPa, compression strength 15MPa.
To sum up analyze
The process for being prepared calcium silicate board in Integrated comparative Examples 1 to 6 using hydrated calcium silicate fiber is found, adjusts synthesis
The primary condition of hydrated calcium silicate fiber can prepare the hydrated calcium silicate fiber of different type and crystallization shape, work as hydro-thermal
Synthesis temperature, calcium silicon mol ratio and NaOH concentration etc. are in the preferred scope of collaboration, the calcium silicon of the hydrated calcium silicate fiber of synthesis
Atomic ratio is 0.5~1.0, is reached or the calcium silicon atom ratio close to tobermorite molecule；Again during suitable control hydro-thermal reaction
Between in preferred scope, the bigger hydrated calcium silicate fiber of major diameter can be obtained.
In addition, research also found, hydrothermal temperature is higher than 1.0 less than 200 DEG C (embodiments 1,2) or calcium silicon mol ratio
(embodiment 4,5) or the hydrated calcium silicate fiber for being not added with alkali (embodiment 7) preparation, tobermorite content is relatively low, equal
The unit weight and thermal conductivity factor of the calcium silicate board product prepared under briquetting pressure are relatively high.
The present inventor also inquired into briquetting pressure and dwell time to calcium silicate board properties of product influence (embodiment 3,
6)；The study found that under conditions of briquetting pressure is higher, the dwell time is longer, the mechanical strength of the calcium silicate board of preparation obtains
It is further to be promoted, however its unit weight and thermal conductivity factor also increased, and the comprehensive quality of product is caused to decline；And it is molded pressure
Power is higher, and being manufactured into for former is originally higher, and the production cost that the dwell time increases calcium silicate board is consequently increased.Cause
This, selects suitable briquetting pressure and dwell time to have facilitation to the castering action of calcium silicate board product quality.
Claims (10)
1. a kind of preparation method of calcium silicate board, which is characterized in that obtained by the repressed shaping of hydrated calcium silicate fiber.
2. the preparation method of calcium silicate board as described in claim 1, which is characterized in that the hydrated calcium silicate fiber it is straight
Footpath is 0.01~1 μm, and length is 0.5~20 μm；Draw ratio is 10~200.
3. the preparation method of calcium silicate board as claimed in claim 2, which is characterized in that the calcium silicon atom of hydrated calcium silicate fiber
Than for 0.3~2；Preferably 0.5~1.
4. such as the preparation method of claims 1 to 3 any one of them calcium silicate board, which is characterized in that the aquation silicic acid
The slurry that calcium fiber is prepared by siliceous raw material, calcareous raw material, alkali and water is prepared under 120~260 DEG C of hydrothermal condition.
5. the preparation method of calcium silicate board as claimed in claim 4, which is characterized in that in slurry, the concentration of alkali is less than or waits
In 100g/L；Liquid-solid ratio is 5~30mL/g.
6. the preparation method of calcium silicate board as claimed in claim 4, which is characterized in that in slurry, calcium silicon mol ratio for 0.3~
1.5；Preferably 0.4~1.0.
7. the preparation method of calcium silicate board as claimed in claim 4, which is characterized in that the temperature of hydro-thermal reaction is 200~220
℃。
8. the preparation method of calcium silicate board as claimed in claim 4, which is characterized in that the siliceous raw material is quartz, powder
At least one of coal ash, slag；
The calcareous raw material can be at least one of lime, carbide slag；
The hydro-thermal reaction time is 0.5~12h.
9. the preparation method of calcium silicate board as described in claim 1, which is characterized in that the pressure of compression moulding process for 1~
100MPa；The dwell time is 1~60min at this pressure.
10. the calcium silicate board as made from any one of claim 1~9 preparation method, which is characterized in that unit weight is 0.8~1.5g/
cm3, thermal conductivity factor is 0.02~0.5W/ (mK).
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| CN112479663A (en) * | 2020-12-03 | 2021-03-12 | 武汉建筑材料工业设计研究院有限公司 | Calcium silicate board prepared from industrial solid wastes and preparation method thereof |
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| CN112479663A (en) * | 2020-12-03 | 2021-03-12 | 武汉建筑材料工业设计研究院有限公司 | Calcium silicate board prepared from industrial solid wastes and preparation method thereof |
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| CN114988840A (en) * | 2022-06-20 | 2022-09-02 | 广东新元素板业有限公司 | Preparation method of anti-cracking asbestos-fiber-free calcium silicate board |
| CN116375442A (en) * | 2023-03-02 | 2023-07-04 | 武汉理工大学 | High-strength calcium silicate board containing white calcium zeolite and preparation method thereof |
| CN116063055A (en) * | 2023-03-22 | 2023-05-05 | 山东奥科金属制品集团有限公司 | Light calcium silicate board |
| CN116063055B (en) * | 2023-03-22 | 2023-08-18 | 山东奥科金属制品集团有限公司 | Light calcium silicate board |
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