CN108069694B - 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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- CN108069694B CN108069694B CN201711334112.0A CN201711334112A CN108069694B CN 108069694 B CN108069694 B CN 108069694B CN 201711334112 A CN201711334112 A CN 201711334112A CN 108069694 B CN108069694 B CN 108069694B
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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
-
- 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 field, a kind of method for specifically disclosing calcium silicate board；It is obtained by the repressed molding of hydrated calcium silicate fiber.Hydrated calcium silicate fiber of the present invention is prepared under 120~260 DEG C of hydrothermal condition by the slurry that siliceous raw material, calcareous raw material, alkali and water are prepared.The bulk density of calcium silicate board produced by the present invention is 0.8~1.5g/cm3, thermal coefficient 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 technique
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, bulk density is low, and have good
Good machinability and noninflammability, so it is 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 " determines fiber reinforced calcium silicate board
Justice: cementing with siliceous-calcium materials as main part using the loose staple fiber such as inorganic mineral fiber or cellulose fibre as reinforcing material
Material through slurrying, molding, accelerates curing reaction in high temperature and high pressure saturated steam, forms calcium silicate gel and manufactured plate
Material.Definition to steam press maintenance: referring in calcium silicate board with microporous production process, and 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 tobermorite crystal plus fiber reinforcement.If siliceous-calcareous raw material is during steam pressure
It reacts insufficient, cause the forming amount of tobermorite crystal not enough or forms other substitution ingredients, will result in silicic acid
The mechanical strength of calcium panel products is not high, or even becomes waste product (soft board).
To solve drawbacks described above existing for existing calcium silicate board production technology, the prior art mainly passes through addition cement substitution
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 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%, defoaming agent 0.5~1%.
The purpose of addition cement is to increase the intensity of calcium silicate board using the intensity of hydrated cementitious formation, and utilize water
The characteristics of mud is calcic raw material substitutes part quick lime, to reduce production cost.But cement is in calcium silicate board production
Additive amount is not easy to control, and cement consumption is few, does not have humidification to the mechanical strength of calcium silicate board；Dosage is excessive, will cause
Calcium silicate board product colour deepens and reduces quality, and will increase the deformation coefficient of calcium silicate board, makes product that use be not achieved
It is required that.
Summary of the invention
To solve technical problem of the existing technology, 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 molding of hydrated calcium silicate fiber.
The study found that being raw material using the hydrated calcium silicate fiber of hydrothermal synthesis, bulk density can be made in direct pressing molding
It is small, thermal coefficient is low, the calcium silicate board product of excellent thermal insulation performance；In addition, under lower bulk density of the present invention, moreover it is possible to
Ensure that the indices such as the mechanical strength of calcium silicate board all meet and uses standard.
Preferably, the diameter of the hydrated calcium silicate fiber is 0.01~1 μm；Length is 0.5~20 μm.The present invention
People also the study found that using the preferred diameter and length range hydrated calcium silicate fiber, not only can satisfy calcium silicate products
The requirement of middle tobermorite content, can also unexpectedly play the role of it is fibre-reinforced, to avoid using other mines
Fibres or industrial chemicals, economize on resources, and protect environment, environmentally protective.
Further preferably, the diameter of the hydrated calcium silicate fiber is 0.05~0.2 μm；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 bulk density and thermal coefficient 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 be tobermorite, the pattern of tobermorite is the aggregate of threadiness, tool
There is the features such as hole is flourishing, thermal coefficient and bulk density 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, cooperate preferred draw ratio, facilitates the performance for further promoting 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, finally obtained aquation
Ca silicate fibre is particularly suitable for preparing calcium silicate board.Studies have shown that fine using hydrated calcium silicate obtained under the temperature range
Dimension, the indices such as thermal coefficient and bulk density of calcium silicate board obtained can meet requirement.
The siliceous raw material can mainly contain the material of silica for quartz, flyash, slag etc..
The calcareous raw material can mainly contain the material of CaO for lime, carbide slag etc..
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.
It is main raw material(s) that hydrated calcium silicate fiber used in the present invention, which is using flyash and quick lime, anti-by hydro-thermal
It should be prepared；Principle is simple, is easy to promote and apply, may advantageously facilitate comprehensive utilization and the energy-saving building material product of fly ash
Resource regeneration.
Preferably, the calcium silicon mol ratio of flyash and quick lime is 0.3~1.5 in slurry；Further preferably 0.4
~1.0.The calcium silicon mol ratio in slurry is controlled, the calcium silicate board haveing excellent performance is facilitated.
The inventors discovered that water-heat process exogenously added alkali, cooperates the hydrothermal reaction condition, the material that such hydro-thermal obtains
It is thermally conductive to reduce its for example, further helping in the bulk density for reducing calcium silicate board for the performance for helping to be promoted calcium silicate board obtained
Coefficient promotes thermal insulation property.
Preferably, the alkali is alkali metal hydroxide；Preferably potassium hydroxide and/or sodium hydroxide；Further
Preferably sodium hydroxide.
Preferably, the concentration of alkali is less than or equal to 100g/L in slurry.The alkali for adding the concentration facilitates 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 bulk density of calcium silicate board obtained is lower, and thermal insulation property is more excellent.
Most preferably, in slurry, the concentration of alkali is 5~20g/L.
It that is to say, the pH of control slurry (starting slurry of hydro-thermal reaction) is 11~14；Further preferably 13~14.
Preferably, liquid-solid ratio is 5~30mL/g in slurry；Further preferably 10~20mL/g.Described in the present inventor
Slurry be calcareous raw material, siliceous raw material alkaline aqueous solution, by it is carried out it is described under the conditions of hydro-thermal reaction, facilitate
Hydrated calcium silicate fiber must be made in high yield, additionally aid the performance for promoting subsequent obtained calcium silicate board.
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 also passes through the study found that by the temperature of hydrothermal reaction process, pH, liquid-solid ratio control described preferred
In range, it can help to obtain more conducively tobermorite by the collaboration of the parameter and form and then further promoted silicic acid
The hydrated calcium silicate fiber of calcium plate performance.
Hydrated calcium silicate fiber it is preferred the preparation method comprises the following steps: 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, the pH value that the NaOH less than or equal to 30g/L adjusts slurry is added
(13~14).High-pressure closed vessel is added in prepared suspension slurry, 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 sufficiently dehydrated；Then repressed molding is to get the calcium silicate board.
Preferably, the pressure of compression moulding process is 1~100MPa.Further preferred compression moulding pressure be 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, includes 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, according to calcium silicon mol ratio be 0.4~1.0 and liquid-solid ratio is 10~20mL/g formulation in step (1)
Slurry, the NaOH that 5~20g/L is added 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,
Slurry is taken out, arrives satisfactory hydrated calcium silicate fiber after separation of solid and liquid, washing and drying
Preferably, in step (2): by the sufficiently drying of hydrated calcium silicate fiber obtained in step (1) and mixing, weighing
After be added 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 bulk density made from the preparation method described in one kind3；Into
One step is preferably 0.8~1.2g/cm3.Material of the invention, has lower bulk density, and material is light.
Preferably, thermal coefficient is 0.02~0.5W/ (mK)；Further preferably 0.08~0.2W/ (mK).This
The calcium silicate board of invention has lower thermal coefficient, has good thermal insulation property.
Calcium silicate board of the present invention, thickness are preferably 2~30mm；Further preferably 5~20mm.
Under bulk density 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；Sufficiently meet requirement.
Preferably, the preparation method of the calcium silicate board, briquetting pressure is 10~50MPa, the dwell time is 10~
30min, calcium silicate board product thickness are 5~20mm, and bulk density is 0.8~1.2g/cm3, thermal coefficient 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 the lime, calcium carbide 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, is easy to promote and apply, may advantageously facilitate the Resource regeneration of energy-saving building material product.
The present invention not only solves present in traditional calcium silicates board production technology since tobermorite production quantity 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 beneficial effect that the present invention can obtain:
Calcium silicate board is prepared using hydrated calcium silicate fiber direct pressing molding, prepares calcium silicate board with traditional steam press maintenance
Technique compare, preparation principle is simple, process is short, product quality is easy to get control, equipment investment and production cost are low, be easy
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 existed with the fibers form of crystal whisker-shaped, avoid using
Mineral fibres and other industrial chemicals, product quality is controllable, energy conservation and environmental protection, and the comprehensive development and utilization of Industrial Solid Waste may be implemented.
In the present invention, under without outer doping, it still can unexpectedly obtain that bulk density is low, the silicic acid of excellent thermal insulation performance
Calcium plate, test show bulk density up to 0.8~1.5g/cm3, thermal coefficient can be 0.02~0.5W/ (mK).
Detailed description of the invention
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 figure 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.
From Fig. 1 and Fig. 2 it can be seen that being Tuo Beimo using the main component of water of coal ash thermal synthesis hydrated calcium silicate product
Carry out stone, occurs 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 relatively flat, is 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 that 5g/L is added 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 group of product becomes mullite, quartz and aquation
Gel of calcium silicate.The diameter of hydrated calcium silicate fiber is 0.01~0.1 μm, and length is 1~3 μm, and draw ratio is 20~30；Aquation
The calcium silicon atom ratio of ca silicate fibre is 0.4.
Step (2):
It is hydrated calcium silicate fiber obtained in step (1) is sufficiently dry and mix, be added after weighing it is framed, in 10MPa
Briquetting pressure under maintain 5min, obtain calcium silicate board (thickness 5mm).The bulk density of calcium silicate board product is 1.4g/cm3, thermally conductive
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 that 15g/L is added 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
Stone, hydrated calcium silicate gel.The diameter of hydrated calcium silicate fiber be 0.05~0.3 μm, length be 3~5 μm, draw ratio be 50~
100；The calcium silicon atom ratio of hydrated calcium silicate fiber is 0.7.
Step (2):
It is hydrated calcium silicate fiber obtained in step (1) is sufficiently dry and mix, be added after weighing it is framed, in 20MPa
Briquetting pressure under maintain 20min, obtain calcium silicate board (thickness 10mm).The bulk density 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 that 30g/L is added 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
The diameter of calcium fiber is 0.05~0.2 μm, and length is 10~20 μm, and draw ratio is 50~200；The calcium silicon of hydrated calcium silicate fiber
Atomic ratio is 0.9.
Step (2):
It is hydrated calcium silicate fiber obtained in step (1) is sufficiently dry and mix, be added after weighing it is framed, in 30MPa
Briquetting pressure under maintain 30min, obtain calcium silicate board (thickness 15mm).The bulk density 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 that 50g/L is added 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.
The diameter of hydrated calcium silicate fiber is 0.1~0.5 μm, and length is 5~10 μm, and draw ratio is 10~50；Hydrated calcium silicate fiber
Calcium silicon atom than 1.3.
Step (2):
It is hydrated calcium silicate fiber obtained in step (1) is sufficiently dry and mix, be added after weighing it is framed, in 50MPa
Briquetting pressure under maintain 50min, obtain calcium silicate board (thickness 20mm).The bulk density 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 that 100g/L is added 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.The diameter of hydrated calcium silicate fiber be 0.01~0.1 μm, length be 1~2 μm, draw ratio be 10~
50；The calcium silicon atom ratio of hydrated calcium silicate fiber is 1.5.
Step (2):
It is hydrated calcium silicate fiber obtained in step (1) is sufficiently dry and mix, be added after weighing it is framed, in 100MPa
Briquetting pressure under maintain 60min, obtain calcium silicate board (thickness 25mm).The bulk density 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 that 20g/L is added 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
The diameter of sour calcium fiber is 0.01~0.1 μm, and length is 10~20 μm, and draw ratio is 50~200；The calcium of hydrated calcium silicate fiber
Silicon atom ratio is 0.75.
Step (2):
It is hydrated calcium silicate fiber obtained in step (1) is sufficiently dry and mix, be added after weighing it is framed, in 100MPa
Briquetting pressure under maintain 60min, obtain calcium silicate board (thickness 30mm).The bulk density 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 is, alkali is not added in feed liquid, and concrete operations are as follows:
Step (1):
According to calcium silicon mol ratio be 1.0 and liquid-solid ratio is that 30mL/g prepares slurry, and NaOH (pH 11) is not added；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
Diameter is 0.01~0.1 μm, and 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):
It is hydrated calcium silicate fiber obtained in step (1) is sufficiently dry and mix, be added after weighing it is framed, in 30MPa
Briquetting pressure under maintain 30min, obtain calcium silicate board (thickness 12mm).The bulk density 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
It is comprehensively compared in Examples 1 to 6 and is found using the process that hydrated calcium silicate fiber prepares calcium silicate board, adjust 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 be 0.5~1.0, reach or close to tobermorite molecule calcium silicon atom ratio；Again when suitable control hydro-thermal reaction
Between in preferred range, the available biggish hydrated calcium silicate fiber of draw ratio.
In addition, research also found, hydrothermal temperature is higher than 1.0 lower than 200 DEG C (embodiments 1,2) or calcium silicon mol ratio
(embodiment 4,5) or the hydrated calcium silicate fiber that alkali (embodiment 7) preparation is not added, tobermorite content is lower, same
The bulk density and thermal coefficient 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 the mechanical strength of the calcium silicate board of preparation obtains under the conditions of briquetting pressure is higher, the dwell time is longer
It is further to be promoted, however its bulk density and thermal coefficient also increased, and the comprehensive quality of product is caused to decline；And form pressure
Power is higher, and the manufacturing cost of molding equipment is 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 (12)
1. a kind of preparation method of calcium silicate board, which is characterized in that obtained by the repressed molding of hydrated calcium silicate fiber；
Hydro-thermal of the slurry that the hydrated calcium silicate fiber is prepared by siliceous raw material, calcareous raw material, alkali and water at 120 ~ 260 DEG C
Under the conditions of be prepared；
The diameter of the hydrated calcium silicate fiber is 0.01 ~ 1 μm, and length is 0.5 ~ 20 μm；Draw ratio is 10 ~ 200.
2. the preparation method of calcium silicate board as described in claim 1, which is characterized in that the draw ratio of hydrated calcium silicate fiber is
50~200。
3. the preparation method of calcium silicate board as described in claim 1, which is characterized in that the calcium silicon atom of hydrated calcium silicate fiber
Than being 0.3 ~ 2.
4. the preparation method of calcium silicate board as described in claim 1, which is characterized in that the calcium silicon atom of hydrated calcium silicate fiber
Than being 0.5 ~ 1.
5. the preparation method of calcium silicate board as described in claim 1, 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 described in claim 1, which is characterized in that the pH for controlling slurry is 13 ~ 14.
7. the preparation method of calcium silicate board as described in claim 1, which is characterized in that in slurry, calcium silicon mol ratio be 0.3 ~
1.5。
8. the preparation method of calcium silicate board as described in claim 1, which is characterized in that in slurry, calcium silicon mol ratio be 0.4 ~
1.0。
9. the preparation method of calcium silicate board as described in claim 1, which is characterized in that the temperature of hydro-thermal reaction is 200 ~ 220
℃。
10. the preparation method of calcium silicate board as described in claim 1, which is characterized in that the siliceous raw material is quartz, powder
At least one of coal ash, slag；
The calcareous raw material is at least one of lime, carbide slag；
The hydro-thermal reaction time is 0.5 ~ 12h.
11. the preparation method of calcium silicate board as described in claim 1, which is characterized in that the pressure of compression moulding process be 1 ~
100MPa；The dwell time is 1 ~ 60min at this pressure.
12. the calcium silicate board as made from any one of claim 1 ~ 11 preparation method, which is characterized in that bulk density is 0.8 ~ 1.5g/
cm3, thermal coefficient is 0.02 ~ 0.5W/ (mK).
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| CN109020248A (en) * | 2018-10-08 | 2018-12-18 | 肇庆三乐集成房屋制造有限公司 | A kind of reinforced fiber enhancing calcium silicate board and preparation method thereof |
| CN113620659A (en) * | 2020-05-08 | 2021-11-09 | 中联环股份有限公司 | Method for preparing non-autoclaved hydrophobic fiber reinforced calcium silicate board by utilizing fly ash |
| 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 |
| CN113231010B (en) * | 2021-06-03 | 2022-07-29 | 中南大学 | Multi-type zeolite/C-S-H composite adsorption material and preparation method and application thereof |
| CN113479898A (en) * | 2021-08-31 | 2021-10-08 | 江苏润邦再生资源科技股份有限公司 | Method for preparing amorphous nano dicalcium silicate by hydrothermal method |
| 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 |
| 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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