CN107162010A - The hydrated calcium silicate for synthesizing the method for hydrated calcium silicate and being synthesized by this method - Google Patents
The hydrated calcium silicate for synthesizing the method for hydrated calcium silicate and being synthesized by this method Download PDFInfo
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- CN107162010A CN107162010A CN201710379479.8A CN201710379479A CN107162010A CN 107162010 A CN107162010 A CN 107162010A CN 201710379479 A CN201710379479 A CN 201710379479A CN 107162010 A CN107162010 A CN 107162010A
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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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
Abstract
This disclosure relates to a kind of method for synthesizing hydrated calcium silicate and the hydrated calcium silicate synthesized by this method.This method comprises the following steps：A, drift-sand is pre-processed, the granularity of the drift-sand powder by pretreatment is 5 20 μm, SiO2Content is not less than 90 weight %；B, thermal reduction processing is carried out to desulfurated plaster in the presence of a reducing agent, and the quick lime of gained is cleared up, obtain lime white；C, drift-sand powder, the lime white that the process is pre-processed mix progress first with optional water and reacted, and obtain the first reactant；D, addition activator and optional water into first reactant, carry out second and react, obtain the second reactant containing hydrated calcium silicate.The developing low-cost of this method, pollutes small, realizes the combination of sand industry and green material, and synthesized hydrated calcium silicate added value is high, and market application foreground is good.
Description
Technical field
This disclosure relates to new material synthesis technical field, in particular it relates to a kind of method for synthesizing hydrated calcium silicate and by
The hydrated calcium silicate of this method synthesis.
Background technology
Hydrated calcium silicate is with CaO-SiO2-H2The general designation for the ternary compound that O systems are present, due to its composition and structure
Complexity it is different with cleanliness factor, the species of hydrated calcium silicate is varied.In general, when temperature, higher than 100 DEG C, (pressure is high
In 1 standard atmospheric pressure) when Hydrothermal Synthesiss hydrated calcium silicate crystalline state it is good, mainly include eakleite and Tuo Beimo come
Stone；When temperature is less than 100 DEG C, generally resulting calcium silicates crystallinity is poor.Tobermorite (6CaO5SiO2·
6H2O it is) a kind of higher hydrated calcium silicate of crystallinity, with stronger heat endurance, but tobermorite is in 300 DEG C of conditions
Under can lose intermediary water, when temperature reaches 750 DEG C, its crystal structure can be destroyed, and switch to amorphous unformed material.
Eakleite crystal belongs to monoclinic system, and chemical formula is (6CaO6SiO2·H2O), crystallization can form threadiness or needle-like is brilliant
Body.Eakleite is a kind of mineral that crystal water content is minimum, temperature tolerance is best in all hydrated calcium silicate mineral, is used
Temperature can reach 1000 DEG C, and with good characteristics such as high temperature resistant, low-density, and xonotlite fiber is easily by body fluid absorption,
With bio-soluble, its toxicity to human body is not only far below asbestos mineral fiber, also resistance to significantly lower than general alumina silicate
Fiery fiber, is a kind of new energy-saving material of environmental protection using safety.
The synthetic method of hydrated calcium silicate mainly includes the precipitation method, sol-gal process and hydrothermal synthesis method.The precipitation method and molten
The raw material of sol-gel is generally pure compound, the raw material with the complex material such as cement in practice, slag and flyash composition
Difference is larger.The raw material type of hydrothermal synthesis method, water-solid ratio and actual relatively uniform, are the preferable aquations of laboratory synthetic crystallization
The ideal method of calcium silicates, but generation hydrated calcium silicate in terms of chemical composition and microscopic appearance according to reaction bar
Larger difference is presented in the change of part, is subject to certain restrictions in actual applications.
The content of the invention
The purpose of the disclosure is to provide a kind of method for synthesizing hydrated calcium silicate and the hydrated calcium silicate synthesized by this method,
The developing low-cost of this method, pollutes small, realizes the combination of sand industry and green material, synthesized hydrated calcium silicate
Added value is high, and market application foreground is good.
To achieve these goals, disclosure first aspect：A kind of method for synthesizing hydrated calcium silicate, this method bag are provided
Include following steps：
A, drift-sand is pre-processed, obtain the drift-sand powder by pretreatment, the aeolian accumulation by pretreatment
The granularity of husky powder is 5-20 μm, SiO2Content is not less than 90 weight %；
B, thermal reduction processing is carried out to desulfurated plaster in the presence of a reducing agent, and the quick lime of gained cleared up,
Obtain lime white；
C, the lime white obtained by the drift-sand powder by pretreatment obtained in step a, in step b with
Optional water mixing carries out first and reacted, and obtains the first reactant, with molar ratio computing, CaO in first reactant：SiO2：
H2O=(1-1.5)：1：(0.5-2.0)；
Activator and optional water are added in d, first reactant obtained into step c, second is carried out and reacts, obtain
To the second reactant containing hydrated calcium silicate, with molar ratio computing, CaO in second reactant：SiO2：H2O=(0.95-
1.1)：1：(0.1-1.5), the activator is selected from least one of flyash, silicon powder and floating bead.
Alternatively, in step a, the pretreatment includes cleaning；Described clean includes drift-sand and water and cleans auxiliary agent
It is stirred and then rinses after mixing, the drift-sand after being cleaned is described on the basis of the drift-sand of 100 parts by weight
The consumption for cleaning auxiliary agent is 0.01-0.5 parts by weight, and the consumption of the water is 50-100 parts by weight, the scouring auxiliary agent be selected from
At least one of sodium metasilicate, calcium chloride, sodium chloride and sodium pyrophosphate, the time of the scouring is 10-20 minutes.
Alternatively, in step a, the pretreatment is additionally included in the step of carrying out wet-milling again after the progress scouring, described
Wet-milling includes being ground after the drift-sand after the scouring is mixed with grinding aid, after the scouring of 100 parts by weight
On the basis of drift-sand, the consumption of the grinding aid is 0.2-3 parts by weight, and the grinding aid is selected from sodium chloride, enuatrol and ring
At least one of alkanoic acid sodium, the time of the wet-milling is 30-50 minutes.
Alternatively, in step b, the reducing agent be selected from least one of coke, coal and CO, the desulfurated plaster with
The mol ratio of reducing agent is 1：(0.1-5), the desulfurated plaster is with CaSO4Meter, the reducing agent is in terms of C.
Alternatively, the condition of the thermal reduction processing is：Temperature is 800-1200 DEG C, and the time is 10-30 minutes.
Alternatively, in step b, it is described clear up including：The quick lime is mixed with water, lime white, the raw stone is obtained
The weight ratio of ash and water is 1：(10-30), it is described to clear up so that the lime white contains particle diameter and is not higher than 0.1 μm, specific surface area
For 10-30m2/ g Ca (OH)2Particle.
Alternatively, the condition cleared up is：Temperature is 50-100 DEG C, and the time is 50-90 minutes.
Alternatively, this method also includes：In step c, by it is described by pretreatment drift-sand powder, lime white with it is additional
Agent mixing carries out first and reacted, and the mol ratio of the additive and the drift-sand powder by pretreatment is (0.001-0.1)：1,
The drift-sand powder by pretreatment is with SiO2Meter, the additive is selected from BaCl2, KCl and SrCl2In at least one
Kind.
Alternatively, the condition of first reaction in step c is：Reaction temperature is 160-200 DEG C, and pressure is 1-
2MPa, the stir speed (S.S.) that the temperature rise period of the reaction temperature is risen to by room temperature is 200-400rpm, reaches the reaction temperature
The stir speed (S.S.) of holding stage afterwards is 50-100rpm, and the reaction time is 3-4 hours
Alternatively, in step d, on the basis of the drift-sand powder by pretreatment of 100 parts by weight, the activation
The consumption of agent is 1-30 parts by weight.
Alternatively, in step d, the condition of second reaction is：Reaction temperature is 180-230 DEG C, and pressure is 2-3MPa,
The stir speed (S.S.) that the temperature rise period of the reaction temperature is risen to by room temperature is 200-400rpm, reaches the guarantor after the reaction temperature
The stir speed (S.S.) of thermophase is 50-100rpm, and the reaction time is 6-12 hours.
Alternatively, in step d, the condition of second reaction is：Reaction temperature is 200-220 DEG C, pressure 2-3MPa, instead
It is 8-10 hours between seasonable
Alternatively, this method also includes：The second reactant containing hydrated calcium silicate is carried out described in being obtained in step d
The step of extrusion forming and steam press maintenance, the condition of the extrusion forming is：Temperature is 10-30 DEG C, and pressure is 15-25MPa, when
Between be 1-5 minutes, the condition of the steam press maintenance is：Temperature is 160-200 DEG C, and pressure is 1-2MPa, and the time is 6-10 hours.
Disclosure second aspect：The hydrated calcium silicate that a kind of method by described in disclosure first aspect is synthesized is provided.
By above-mentioned technical proposal, the disclosure, as raw material, develops one using drift-sand, desulfurated plaster and flyash etc.
Set low cost, the new energy-saving material hydrated calcium silicate synthetic method of low stain treatment technology, realize the regeneration of industrial waste
Using and sand industry and green material combination, the hydrated calcium silicate added value that is produced is high, and market application foreground is good.
Other feature and advantage of the disclosure will be described in detail in subsequent embodiment part.
Brief description of the drawings
Accompanying drawing is, for providing further understanding of the disclosure, and to constitute a part for specification, with following tool
Body embodiment is used to explain the disclosure together, but does not constitute limitation of this disclosure.In the accompanying drawings：
Fig. 1 is a kind of flow chart of embodiment of the method for the synthesis hydrated calcium silicate that the disclosure is provided；
Fig. 2 is the electromicroscopic photograph of the calcium silicate board product prepared in embodiment 1；
Fig. 3 is the XRD of the calcium silicate board product prepared in embodiment 1-5.
Embodiment
It is described in detail below in conjunction with accompanying drawing embodiment of this disclosure.It should be appreciated that this place is retouched
The embodiment stated is merely to illustrate and explained the disclosure, is not limited to the disclosure.
Disclosure first aspect：A kind of method for synthesizing hydrated calcium silicate is provided, Fig. 1 is a kind of specific implementation of this method
The flow chart of mode.This method comprises the following steps：
A, drift-sand is pre-processed, obtain the drift-sand powder by pretreatment, the aeolian accumulation by pretreatment
The granularity of husky powder is 5-20 μm, SiO2Content is not less than 90 weight %；
B, thermal reduction processing is carried out to desulfurated plaster in the presence of a reducing agent, and the quick lime of gained cleared up,
Obtain lime white；
C, the lime white obtained by the drift-sand powder by pretreatment obtained in step a, in step b with
Optional water mixing carries out first and reacted, and obtains the first reactant, with molar ratio computing, CaO in first reactant：SiO2：
H2O=(1.0-1.5)：1：(0.5-2.0)；
Activator and optional water are added in d, first reactant obtained into step c, second is carried out and reacts, obtain
To the second reactant containing hydrated calcium silicate, with molar ratio computing, CaO in second reactant：SiO2：H2O=(0.95-
1.1)：1：(0.1-1.5), the activator is selected from least one of flyash, silicon powder and floating bead.
China be desert distributional region extensively, by the serious country of desertification hazard.Flyash and desulfurated plaster are China
The larger industrial residue of current discharge capacity, huge pressure is caused to the development of the national economy and ecological environment, and it is comprehensively utilized, and is become
Waste be changed into values, turns bane into boon, and is the important means for solving contradiction between China's power generation environmental pollution and scarcity of resources.The disclosure
With drift-sand, desulfurated plaster and flyash etc. for raw material, developing low-cost, the hydrated calcium silicate synthesis side of low stain treatment technology
Method, realizes the regeneration of industrial waste and the combination of sand industry and green material.
According to the disclosure, in step a, the purpose of the pretreatment is that drift-sand is processed as into specific specified particle size and SiO2
The drift-sand powder of content, to improve the solubility of silica, is more beneficial for the synthesis of hydrated calcium silicate.The pretreatment can
With including cleaning.The scouring can include being stirred and then rinsing after drift-sand is mixed with water and scouring auxiliary agent, obtain
Drift-sand after scouring.The scouring can be carried out in the conventional equipment of this area, for example, can be carried out in swaging machine.It is real
When border is operated, drift-sand can be placed in swaging machine, add appropriate water and scouring auxiliary agent, in the presence of mechanical force constantly
Stir, stir, shock, scouring mutually between sand grains, the mud point and loose sull for being attached to sand grain surface is stripped, then
Rinsed with clear water, go to desilt point and particulate, the drift-sand after being cleaned.Can be by mechanical force and aeolian accumulation by cleaning
The thin-films Oxygen compound and mud impure mineral of shearing force to remove drift-sand surface between husky sand grains etc., and wipe broken not into monomer
Mineral aggregate, reaches refining effect.As needed, the step of can also being classified after rinsing, to filter out suitable production
Product, the step is the conventional steps of this area, and the disclosure is repeated no more.The swaging machine can by this area routine use
, it is commercially available, the SP100 model swaging machines that can be for example produced for Yu Kuang Machinery Manufacturing Co., Ltd.s of Henan Province.
In the scouring, solid concentration is very big to the influential effect of scouring, and solid material content is too high, does not have scouring work
With, solid material content is low, then hit between sand grains, the chance of scouring it is few, the effect of scouring is poor.According to disclosed method, with 100
On the basis of the drift-sand of parts by weight, the consumption for cleaning auxiliary agent can be 0.01-0.5 parts by weight, the consumption of the water
It can be 50-100 parts by weight, ideal scrub effect can be reached under above-mentioned consumption.In order to further be had
The hydrated calcium silicate of the good characteristics such as high temperature resistant, low-density, on the basis of the drift-sand of 100 parts by weight, the scouring is helped
The consumption of agent is preferably 0.02-0.1 parts by weight, and the consumption of the water is preferably 55-65 parts by weight.It is described scouring auxiliary agent can be
Selected from least one of sodium metasilicate, calcium chloride, sodium chloride and sodium pyrophosphate.Clean the bioactive molecule in auxiliary agent in drift-sand and
Chemistry and Characteristic Adsorption can occur for impure mineral particle surface, can and be improved so as to significantly reduce mineral particle surface
Intergranular electric repulsion, serves to the peptizaiton of particulate and splitting between mineral grain is allocated as to use, can further improve
Scrub effect.In order to reduce equipment attrition, cost is reduced, the time of scouring can be controlled at 10-20 minutes.
In order to which the drift-sand after scouring to be further ground into the superfine powder for meeting granularity requirements, the pretreatment may be used also
To be included in the step of carrying out carrying out wet-milling again after the scouring.The wet-milling is included the drift-sand after the scouring and grinding aid
It is ground after agent mixing.The grinding can be this area conventional method, for example can be with Ball-stirring mill and vibromill, on
The operating procedure for stating Ginding process is well known to those skilled in the art, and is usually to be placed in material to be ground in friction device simultaneously
Milling medium, water etc. are added, milling apparatus is started, milling medium spheroid is produced centrifugal force, revolving force and up and down motion, passes through
The compound action of impact, shearing, compression and friction etc. can with it is very effective by crushing material into superfine powder.The mill used
The requirement of ore deposit medium be wear away less, hardness it is high, diameter can be 1-10mm, can be from different size in practical operation
Milling medium carries out collocation and used.Milling apparatus can be the conventional equipment of this area, in order to prevent milling apparatus cylinder inboard wall
The pollution and loss of machinery iron, the inwall of friction device can make the polyester barrel of high abrasion.The milling apparatus can be
This area institute is conventional use of, is commercially available, for example, can be produced for Luoyang Qi Xing technological development Co., Ltd
MJS1000 model friction devices.
According to the disclosure, during wet-milling, addition has the material of grind -aiding effect to drift-sand as grinding aid, can drop
The surface energy of low aeolian accumulation sand grain, accelerates the crushing of drift-sand, improves mill efficiency, reduce energy consumption.In order to farthest send out
The grind -aiding effect of grinding aid is waved, the consumption of the grinding aid is described on the basis of the drift-sand after the scouring of 100 parts by weight
The consumption of grinding aid can be 0.2-3 parts by weight.The grinding aid can be in sodium chloride, enuatrol and sodium naphthenate
It is at least one.The time of the wet-milling can be 30-50 minutes.
Characteristic by pretreated drift-sand powder particle dispersed phase is changed, and specific surface area increased dramatically,
Chemical reaction rate is significantly improved, and significant changes occur for absorption property, optical property, meltdown property etc..Drift-sand is through cleaning
SiO afterwards2Content is not less than 90 weight %, can preferably reach more than 95%, then the drift-sand powder obtained after wet-milling grain
Spend for 5-20 μm, preferably 8-10 μm, particle is uniform in size in spherical.Drift-sand during pretreatment, silica sand particle
Top layer partial amorphism, can improve the solubility of silica, be beneficial to the synthesis of hydrated calcium silicate.
Desulfurated plaster is also known as flue gas desulfurization gypsum, sulphur gypsum or FGD gypsum, and main component is calcium sulphate dihydrate (CaSO4·
2H2O), its content >=90%.According to the disclosure, reducing agent is added in desulfurated plaster, but it is decomposed at low temperature, institute
The product quick lime (CaO) obtained may be used as the reaction raw materials of hydrated calcium silicate synthesis, while the SO of generation2By after purification may be used
For preparing the industrial products such as sulfuric acid, recycling for resource is realized.In step b, the reducing agent can be selected from coke, coal
At least one of with CO, thermal reduction processing is carried out to desulfurated plaster in the presence of a reducing agent, not only contributes to reduce CaSO4
Decomposition temperature, and energy consumption can be greatly lowered.In order to reach preferable effect, the desulfurated plaster and reducing agent rub
Your ratio can be 1：(0.1-5), preferably 1：(0.5-1), the desulfurated plaster is with CaSO4Meter, the reducing agent is in terms of C.It is de-
The granularity of sulphur gypsum can be 10-100 μm, in order to further generate the aquation silicon with good characteristics such as high temperature resistant, low-density
Sour calcium, the granularity of desulfurated plaster is preferably 45-75 μm.When reducing agent is the solids such as coke, coal, the granularity of the reducing agent can
Think no more than 100 mesh, preferably not greater than 200 mesh.
In order to further improve the resolution ratio of desulfurated plaster, the condition of the thermal reduction processing can be：Temperature is 800-
1200 DEG C, preferably 900-1100 DEG C；Time is 10-30 minutes, preferably 15-25 minutes.
According to the disclosure, thermal reduction processing is carried out to desulfurated plaster, quick lime is obtained, then the quick lime of gained is carried out
Clear up, lime white can be obtained.According to the disclosure, in step b, described clear up can include：The quick lime is mixed with water,
Obtain lime white.The weight ratio of the quick lime and water can be 1：(10-30), preferably 1：(10-20), it is described clear up so that
The lime white contains particle diameter and is not higher than 0.1 μm, and further not higher than 0.06 μm, specific surface area is 10-30m2/ g, be preferably
14-18m2/ g Ca (OH)2Particle.The uniform Ca (OH) of gained2Particle further can form Ca in subsequent reactions
(H2O)5(OH)+Hydrated ion is so as to be conducive to the synthesis of hydrated calcium silicate.In order to obtain the fine Ca for meeting above-mentioned condition
(OH)2Particle, described clear up can be carried out under agitation.The condition cleared up can be：Temperature is 50-100 DEG C, is preferably
80-100 DEG C, the time is 50-90 minutes.After the completion of clearing up, lime white sieving can be made to remove impurity, the aperture of sieve can be with
For 100-300 mesh, such as 200 mesh.
CaO can be changed into by the process cleared up by Ca (OH)2, material particle generates volumetric expansion, so as to add
The inner ratio surface area of raw material, improves the reactivity of calcareous raw material, allows more siliceous raw materials and calcareous raw material abundant
Contact.As Ca (OH)2And SiO2In the presence of simultaneously, SiO2Solubility will dramatically increase, due to SiO2In OH-In the presence of more
Easily generate [H2SiO4]2-Anion radical and dissolve, thus the synthetic reaction of hydrated calcium silicate is carried out more abundant,
Be conducive to growing for calcium silicate crystals.
According to the disclosure, in step c, with molar ratio computing, CaO in preferably described first reactant：SiO2：H2O=(1.1-
1.2)：1：(0.7-1.2), can obtain that crystal water content is lower, the more preferable hydrated calcium silicate of temperature tolerance under the proportioning.In order to enter
One step promotes the synthesis of hydrated calcium silicate, and this method can also include：In step c, by the drift-sand powder by pretreatment
Body, lime white mix progress first with additive and reacted.Additive refers to change slurry property, reaction process or prepare not
With the material of performance requirement, and the particular matter quantitatively added.Crystal seed additive can significantly improve Hydrothermal Synthesiss aquation silicic acid
The dynamic process of calcium, plays nucleating agent, improves reactivity, shortens the reaction time, improves the microstructure of product, improves system
The crystallinity and the uniformity of crystalline phase in product, improve the physical and mechanical property of product.The additive and the wind by pretreatment
The mol ratio of sand powder is (0.001-0.1)：1, be preferably (0.01-0.02)：1, the drift-sand powder by pretreatment
Body is with SiO2Meter.The additive can be selected from BaCl2, KCl and SrCl2At least one of.It can be changed by adding additive
Microcellular structure dynamic process in kind course of reaction, promotes gelation, lifts synthetic reaction speed.Ba2+、K+And Sr2+Favorably
In the formation of calcium silicate crystals, the hollow secondary particle of major diameter can be generated, low-density product is obtained.Cl-To product morphology
The key effect of influence is the solution salt effect caused by chlorion, in Cl-Under effect, solution salt effect promotes Ca (OH)2Hair
Raw dissociation so that Ca in solution2+Content increase so that for Ca2+And the combination of silicon-oxy tetrahedron chain creates conditions, and promotes
The generation of calcium silicate crystals.
According to the disclosure, the condition of first reaction in step c can be：Reaction temperature is 160-200 DEG C, preferably
For 180-200 DEG C；Pressure is 1-2MPa, and the stir speed (S.S.) that the temperature rise period of the reaction temperature is risen to by room temperature is 200-
400rpm, preferably 300-350rpm, the stir speed (S.S.) for reaching the holding stage after the reaction temperature are 50-100rpm, excellent
Elect 60-80rpm as.Reaction time is 3-4 hours.
According to the disclosure, in step d, activator is added into first reactant carry out second and react, can promote
The synthesis of hydrated calcium silicate.The activator can be selected from least one of flyash, silicon powder and floating bead.Flyash is
The fine ash that catching is got off from the flue gas after coal combustion, is the primary solids waste of coal-burning power plant's discharge.Flyash is noncrystal
With the mixture of crystalline mineral, amorphous mineral is mainly amorphous silica, and its content constitutes about more than 50%, due to by
The silica structure of vitreum is converted from polymeric form to monomer in the effect of mechanical force and alkaline solution, flyash, reduces glass
The degree of polymerization of body, makes vitreous surface hydroxylating, it is easy to generate hydrated calcium silicate with calcium hydroxide reaction.In addition to silica,
The main oxides composition of flyash also includes Al2O3、FeO、Fe2O3, CaO and TiO2Deng.Because aluminium element silicon property is close, knot
Structure is similar, during the course of the reaction, Al3+Part Si can be replaced4+Into in crystal structure, when aluminium content is higher in reaction system,
Replacement rate can reach 10-15%, and resulting product is the hydrated calcium silicate containing aluminium.Silicon powder is by natural quartz (SiO2) or
Vitreous silica (amorphous Si O of the natural quartz after high-temperature fusion, cooling2) pass through broken, ball milling (or vibration, airflow milling), float
The micro mist that the multiple tracks techniques such as choosing, pickling purification, high-purity water process are processed, its main component is the silica of crystallization.Drift
When pearl is that coal dust burns in thermal power plant boiler, clayey material melts are into microlayer model, in stove under the hot air acting of turbulent flow
Spin at a high speed and form perfectly round sial spheroid, the gas such as nitrogen, hydrogen and carbon dioxide that burning and cracking reaction are produced, in melting
High temperature silicon aluminium ball body in expand rapidly, under surface tension effects, form hollow glass envelope, it is cold rapidly subsequently into flue
But, after hardening, the glassy state cenosphere as high vacuum, its main chemical compositions are silicon, the wherein oxide of aluminium, SiO2About
For 50-65%, Al2O3About 25-35%.It is described to swash on the basis of the drift-sand powder stated by pretreatment of 100 parts by weight
The consumption of agent living can be 1-30 parts by weight, preferably 8-15 parts by weight.
According to the disclosure, in step d, the condition of second reaction can be：Reaction temperature is 180-230 DEG C, pressure
For 2-3MPa, the reaction time is 6-12 hours.The generation of reaction temperature and soaking time to crystal has important influence, reaction temperature
Degree rises to 180 DEG C, and the calcium silicates hydrated product of raw material reaction generation is tobermorite；Reaction temperature rises to 200 DEG C, and raw material is anti-
The calcium silicates hydrated product that should be generated is eakleite.Under the conditions of temperature satisfaction, soaking time, which is more than 8h, can ensure siliceous material
Material fully reacts with calcareous material, all generation eakleite.Therefore, in order to further generate with high temperature resistant, low-density etc.
The eakleite of good characteristic, second reaction condition be preferably：Temperature is 200-220 DEG C, pressure 2-3MPa, and the reaction time is
8-10h。
According to the disclosure, in order to promote the scattered of heat transfer in reaction, proton migration and reactant, it is ensured that filled between raw material
Divide in reaction, step d, the stir speed (S.S.) that the temperature rise period of the reaction temperature is risen to by room temperature is 200-400rpm, is preferably
300-350rpm, the stir speed (S.S.) for reaching the holding stage after the reaction temperature is 50-100rpm, preferably 60-80rpm.
Holding stage is reacted in Dynamic Hydrothermal, and the average grain diameter for occurring spheroidal particle in operation, slurry is stirred to slurry with stirring speed
Rate increases and reduced.
According to the disclosure, in step d, crystal is generated water-solid ratio and spherical particle microscopic appearance has a major impact,
Appropriate water-solid ratio is kept in second course of reaction, crystal fibre can be made to physically well develop, spherome surface fiber initiation is obvious.It is logical
Cross progress second to react, it is preferable that CaO in second reactant：SiO2：H2O=(0.98-1.0)：1：(0.1-0.2).
According to the disclosure, first reaction and the second reaction can be carried out in conventional hydrothermal synthesis reactor, for example
Autoclave.
The method of synthesis hydrated calcium silicate that the disclosure is provided can also include, will be obtained in step d described in contain water
The step of the second reactant for changing calcium silicates carries out extrusion forming and steam press maintenance.The condition of the extrusion forming can be：Temperature
Spend for 10-30 DEG C, pressure is 15-25MPa, the time is 1-5 minutes, and the condition of the steam press maintenance can be：Temperature is 160-
200 DEG C, pressure is 1-2MPa, and the time is 6-10 hours.Reinforcing material can also be added as needed in forming process, this is this
The conventional method in field, the disclosure is not being repeated.It can be obtained with good characteristic after extrusion forming and steam press maintenance
Calcium silicate board product.
There is provided the hydrated calcium silicate that a kind of method by described in disclosure first aspect is synthesized for disclosure second aspect.
The disclosure is described further below by embodiment, but does not therefore limit content of this disclosure.
Used chemicals is that analysis is pure in addition to special indicate in embodiment.
In embodiment, the detection method reference of dioxide-containing silica《GB/T 14506.3-2010 silicate rocks chemistry point
Analysis method third portion：Silica volume is determined》Carry out.Sample is carried out using Rigaku DMAX-RB types X-ray diffractometer (XRD)
Product material phase analysis, test condition is：Cu targetsOperating voltage is 40kV, and operating current is 150mA, scans model
Enclose 5-80 °, 0.02 °/S of sweep speed.Sample is observed using the Sirion200 types SEM (SEM) of Dutch FEI Co.
Pattern, the particle diameter of product, total enlargement ratio of micro- Electronic Speculum select 2000 times.
Embodiment 1
(1) drift-sand 1100kg is taken, 660kg water is added in continuous scrubbing-desliming machine, 500g sodium metasilicate is added as helping
Agent is cleaned, and cleans 20 minutes time, obtains the drift-sand after 1000kg is cleaned.Drift-sand is after cleaning purification, dioxy
SiClx content is detected as 98%.Drift-sand after scouring carries out wet-milling using Ball-stirring mill, using abrasion less, hardness it is high, diameter
Size is 1-10mm ceramic ore grinding medium ball, is stirred and then rinses after addition 2kg sodium chloride auxiliary agent mixing, wet-milling when
Between be 50 minutes, the size indicator of the drift-sand powder after wet-milling reaches 8-10 μm；
(2) desulfurated plaster (CaSO that granularity is 60 μm is taken4·2H2O content is 90%) 2500kg, adds 150kg fixed carbons
Content is 88%, and granularity carries out heat for the coke blacking (being purchased from Shanxi Qingxu coke-oven plant, article number is C90) of 200 mesh for reducing agent
Reduction treatment, carries out the temperature control of thermal reduction processing at 1000-1100 DEG C, the quick lime prepared is used for step (3), by-product
Thing oxidation sulfur cycle is used for industrial production；
(3) the quick lime 1000kg for obtaining step (2) is mixed with 10000kg water, and water temperature is 80 DEG C, in strong stirring bar
Lime white is cleared up under part, and by 200 mesh sieves to remove impurity, the lime white of gained contains particle diameter for 0.06 μm, compares surface
Product is 15m2/ g Ca (OH)2Particle；
(4) the drift-sand powder 800kg obtained by step (1) is taken, by CaO：SiO2(mol ratio) is 1.2 addition steps (3)
The lime white dispensing of gained, adds 40kg barium chlorides as additive, adds the water of requirement, first is carried out into autoclave
Reaction, reaction temperature is 180 DEG C, and temperature rise period stir speed (S.S.) is 300rpm, and holding stage stir speed (S.S.) is 60rpm, and pressure is
1.5MPa, reacts 4h, obtains CaO in the first reactant, the first reactant：SiO2：H2O (mol ratio) is 1.2：1：1.2；Then
The water that the agent of 78kg activating flyashs and requirement are added into autoclave carries out the second reaction, and pressure is 2.3MPa, reaction temperature
For 200 DEG C, temperature rise period stir speed (S.S.) is 300rpm, and holding stage stir speed (S.S.) is 60rpm, and soaking time is 8h, is contained
There is CaO in the second reactant of hydrated calcium silicate, the second reactant：SiO2：H2O (mol ratio) is 0.99：1：0.17；
(5) mould is added after the second reactant slurry containing hydrated calcium silicate is thoroughly mixed, in 20MPa pressure
It is stripped after lower extrusion forming, pressurize 3min, room temperature precuring 5h, prefabricated board is put into still kettle in 1.05MPa, under the conditions of 180 DEG C
Calcium silicate board product S1 is obtained after steam-cured 8h, natural drying.Product S1 electromicroscopic photograph is shown in Fig. 2, XRD such as Fig. 3.Can by Fig. 2
To find out, the present embodiment synthesis calcium silicate products in threadiness, about 5 μm of length, width about 20nm, it, which is interweaved, is wound in
Aggregate, is internally formed many spaces, so that the bulk density of product is smaller.
Embodiment 2
Calcium silicate board product is prepared using the method for embodiment 1, unlike, in step (4), the temperature of the second reaction is
180 DEG C, prepare calcium silicate board product S2.Product S2 electromicroscopic photograph is similar with Fig. 2, XRD such as Fig. 3.
Embodiment 3
Calcium silicate board product is prepared using the method for embodiment 1, unlike, in step (4), the temperature of the second reaction is
190 DEG C, prepare calcium silicate board product S3.Product S3 electromicroscopic photograph is similar with Fig. 2, XRD such as Fig. 3.
Embodiment 4
Calcium silicate board product is prepared using the method for embodiment 1, unlike, in step (4), the temperature of the second reaction is
210 DEG C, prepare calcium silicate board product S4.Product S5 electromicroscopic photograph is similar with Fig. 2, XRD such as Fig. 3.
Embodiment 5
Calcium silicate board product is prepared using the method for embodiment 1, unlike, in step (4), the temperature of the second reaction is
220 DEG C, prepare calcium silicate board product S5.Product S6 electromicroscopic photograph is similar with Fig. 2, XRD such as Fig. 3.
Embodiment 6
Calcium silicate board product is prepared using the method for embodiment 1, unlike, step (1) is：Drift-sand 1100kg is taken,
1100kg water is added in continuous scrubbing-desliming machine, 2000g calcium chloride is added and is cleaned as auxiliary agent, clean 20 points of time
Clock, obtains the drift-sand after 980kg is cleaned.Drift-sand is after cleaning purification, and dioxide-containing silica is detected as 92%.Clean
Drift-sand afterwards carries out wet-milling using Ball-stirring mill, using abrasion less, hardness it is high, diameter is 1-10mm ceramic milling medium
Ball, is stirred and then rinses after the auxiliary agent mixing of addition 2kg enuatrols, and the time of wet-milling is 30 minutes, the drift-sand after wet-milling
The size indicator of powder reaches 12-20 μm, and other steps are identical, prepares calcium silicate board product S6.
Embodiment 7
Calcium silicate board product is prepared using the method for embodiment 1, unlike, step (2) is：Take granularity de- for 80 μm
Sulphur gypsum (CaSO4·2H2O content is 90%) 2500kg, and it is 85% to add 60kg and fix carbon content, and granularity is the coke of 100 mesh
Powder (being purchased from Shanxi Qingxu coke-oven plant, article number is C85) carries out thermal reduction processing for reducing agent, carries out the temperature of thermal reduction processing
Control is at 800-850 DEG C, and other steps are identical, prepare calcium silicate board product S7.
Embodiment 8
Calcium silicate board product is prepared using the method for embodiment 1, unlike, step (3) is：Step (2) is obtained
Quick lime 1000kg is mixed with 30000kg water, and water temperature is 50 DEG C, lime white is cleared up under the conditions of strong stirring, and pass through 200
Mesh sieve is to remove impurity, and the lime white of gained contains particle diameter for 0.1 μm, and specific surface area is 30m2/ g Ca (OH)2Particle, other
Step is identical, prepares calcium silicate board product S8.
Embodiment 9
Calcium silicate board product is prepared using the method for embodiment 1, unlike, in step (4), take obtained by step (1)
Drift-sand powder 800kg, by CaO：SiO2(mol ratio) is the lime white dispensing obtained by 1.5 addition steps (3), adds 138kg
Barium chloride adds the water of requirement as additive, and first is carried out into autoclave and is reacted, and reaction temperature is 160 DEG C, heating
Stage stir speed (S.S.) is 200rpm, and holding stage stir speed (S.S.) is 50rpm, and pressure is 1.6MPa, reacts 4h, obtains the first reaction
CaO in thing, the first reactant：SiO2：H2O (mol ratio) is 1.5：1：2；Then 40kg activating flyashs are added into autoclave
The water of agent and requirement carries out second and reacted, and pressure is 2.3MPa, and reaction temperature is 200 DEG C, and temperature rise period stir speed (S.S.) is
300rpm, holding stage stir speed (S.S.) is 60rpm, and soaking time is 8h, obtains the second reactant containing hydrated calcium silicate, the
CaO in two reactants：SiO2：H2O (mol ratio) is 1.1：1：0.6, other steps are identical, prepare calcium silicate board product S9.
Comparative example 1
This comparative example is used to illustrate to synthesize hydrated calcium silicate using existing hydrothermal synthesis method.Specific method is：No. 42.5
The ratio that cement accounts for the weight % of raw material 20 carries out dispensing, and adjustment siliceous raw material and calcareous raw material addition make CaO：SiO2(mole
Than) 1.0~1.2 are reached, the ratio of mud is 0.3~0.5, and slurry is added into mould after being well mixed, in 20MPa forming under the pressure,
Room temperature precuring is stripped, then in 1.05MPa, steam press maintenance 10h under the conditions of 180 DEG C, and calcium silicate board is made after natural drying, passes through
Dicalcium silicate and tricalcium silicate aquation generation C-S-H gels in cement, obtain early strength, and further by steam-cured effect
Aquation, crystallization generation sheet tobermorite, are partially converted into eakleite.This comparative example prepares calcium silicate board product
S10。
Testing example
By standard GB/T7019-2014《Fibre cement product experimental method》Test the close of calcium silicates slab products S1-S11
Degree, moisture content, wet rise rate and percent thermal shrinkage, test result are shown in Table 1.
By standard GB/T10294-2008《Technology of Steady State Thermal Resistance of Thermal Insulating Material and the measure Guarded hot plate about characteristic》Test
Calcium silicate board product S1-S10 thermal conductivity factor, test result is shown in Table 1.
Table 1
From table 1, the calcium silicate board product prepared by the method provided using the disclosure has density low, resistant to elevated temperatures
Good characteristic, is A grades of incombustible materials, with conventional method prepare calcium silicate board product compared to weight gentlier, resistance to elevated temperatures more
It is good.
As seen from Figure 3, the method provided using the disclosure, the second reaction is 200-220 DEG C, pressure 2- preferably in temperature
3MPa, the reaction time is carries out under conditions of 8-10h when, can generate the hard silicon with good characteristics such as high temperature resistant, low-density
Calcium stone.
The preferred embodiment of the disclosure is described in detail above in association with accompanying drawing, still, the disclosure is not limited to above-mentioned reality
The detail in mode is applied, in the range of the technology design of the disclosure, a variety of letters can be carried out with technical scheme of this disclosure
Monotropic type, these simple variants belong to the protection domain of the disclosure.
It is further to note that each particular technique feature described in above-mentioned embodiment, in not lance
In the case of shield, can be combined by any suitable means, in order to avoid unnecessary repetition, the disclosure to it is various can
The combination of energy no longer separately illustrates.
In addition, can also be combined between a variety of embodiments of the disclosure, as long as it is without prejudice to originally
Disclosed thought, it should equally be considered as content disclosed in this invention.
Claims (14)
1. a kind of method for synthesizing hydrated calcium silicate, it is characterised in that this method comprises the following steps：
A, drift-sand is pre-processed, obtain the drift-sand powder by pretreatment, the drift-sand powder by pretreatment
The granularity of body is 5-20 μm, SiO2Content is not less than 90 weight %；
B, thermal reduction processing is carried out to desulfurated plaster in the presence of a reducing agent, and the quick lime of gained is cleared up, obtained
Lime white；
C, the lime white obtained by the drift-sand powder by pretreatment obtained in step a, in step b with it is optional
Water mixing carry out first react, obtain the first reactant, with molar ratio computing, CaO in first reactant：SiO2：H2O=
(1-1.5)：1：(0.5-2.0)；
Activator and optional water are added in d, first reactant obtained into step c, second is carried out and reacts, contained
There is the second reactant of hydrated calcium silicate, with molar ratio computing, CaO in second reactant：SiO2：H2O=(0.95-1.1)：
1：(0.1-1.5), the activator is selected from least one of flyash, silicon powder and floating bead.
2. according to the method described in claim 1, wherein, in step a, it is described pretreatment include scouring；The scouring includes will
Drift-sand is stirred and then rinsed, the drift-sand after being cleaned, with the institute of 100 parts by weight after being mixed with water and scouring auxiliary agent
State on the basis of drift-sand, the consumption for cleaning auxiliary agent is 0.01-0.5 parts by weight, and the consumption of the water is 50-100 parts by weight,
The scouring auxiliary agent is that the time of the scouring is selected from least one of sodium metasilicate, calcium chloride, sodium chloride and sodium pyrophosphate
10-20 minutes.
3. method according to claim 2, wherein, in step a, the pretreatment is additionally included in after the progress scouring again
The step of carrying out wet-milling, the wet-milling includes being ground after the drift-sand after the scouring is mixed with grinding aid, with 100 weights
On the basis of measuring the drift-sand after the scouring of part, the consumption of the grinding aid is 0.2-3 parts by weight, the grinding aid be selected from
At least one of sodium chloride, enuatrol and sodium naphthenate, the time of the wet-milling is 30-50 minutes.
4. according to the method described in claim 1, wherein, in step b, the reducing agent be in coke, coal and CO extremely
Few one kind, the mol ratio of the desulfurated plaster and reducing agent is 1：(0.1-5), the desulfurated plaster is with CaSO4Meter, the reduction
Agent is in terms of C.
5. method according to claim 4, wherein, the condition of the thermal reduction processing is：Temperature is 800-1200 DEG C, when
Between be 10-30 minutes.
6. according to the method described in claim 1, wherein, in step b, it is described clear up including：The quick lime is mixed with water,
Lime white is obtained, the weight ratio of the quick lime and water is 1：(10-30), it is described to clear up so that the lime white contains particle diameter not
Higher than 0.1 μm, specific surface area is 10-30m2/ g Ca (OH)2Particle.
7. method according to claim 6, wherein, the condition cleared up is：Temperature is 50-100 DEG C, and the time is 50-
90 minutes.
8. according to the method described in claim 1, wherein, this method also includes：In step c, by the wind by pretreatment
Sand powder, lime white mix progress first with additive and reacted, the additive and the drift-sand powder by pretreatment
Mol ratio is (0.001-0.1)：1, the drift-sand powder by pretreatment is with SiO2Meter, the additive be selected from
BaCl2, KCl and SrCl2At least one of.
9. the method according to claim 1 or 8, wherein, the condition of first reaction in step c is：Reaction temperature
For 160-200 DEG C, pressure is 1-2MPa, and the stir speed (S.S.) that the temperature rise period of the reaction temperature is risen to by room temperature is 200-
400rpm, the stir speed (S.S.) for reaching the holding stage after the reaction temperature is 50-100rpm, and the reaction time is 3-4 hours.
10. according to the method described in claim 1, wherein, in step d, with 100 parts by weight it is described by pretreatment aeolian accumulation
On the basis of husky powder, the consumption of the activator is 1-30 parts by weight.
11. the method according to claim 1 or 10, wherein, in step d, the condition of second reaction is：Reaction temperature
For 180-230 DEG C, pressure is 2-3MPa, and the stir speed (S.S.) that the temperature rise period of the reaction temperature is risen to by room temperature is 200-
400rpm, the stir speed (S.S.) for reaching the holding stage after the reaction temperature is 50-100rpm, and the reaction time is 6-12 hours.
12. method according to claim 11, wherein, in step d, the condition of second reaction is：Reaction temperature is
200-220 DEG C, pressure 2-3MPa, the reaction time is 8-10 hours.
13. according to the method described in claim 1, wherein, this method also includes：Contain aquation described in being obtained in step d
The step of second reactant of calcium silicates carries out extrusion forming and steam press maintenance, the condition of the extrusion forming is：Temperature is 10-
30 DEG C, pressure is 15-25MPa, and the time is 1-5 minutes, and the condition of the steam press maintenance is：Temperature is 160-200 DEG C, and pressure is
1-2MPa, the time is 6-10 hours.
14. the hydrated calcium silicate that a kind of method in 1-13 by claim described in any one is synthesized.
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| CN109705852A (en) * | 2018-12-25 | 2019-05-03 | 西安建筑科技大学 | A method of strontium silicate powder body material is prepared using strontium hydroxide and silicon ash |
| CN110465260A (en) * | 2019-07-12 | 2019-11-19 | 北京工业大学 | A kind of hydrated calcium silicate and preparation method thereof removing Cu in waste water ion |
| CN114873599A (en) * | 2022-06-09 | 2022-08-09 | 北京科技大学 | Method for preparing calcium silicate from desulfurized gypsum |
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