CN109133650A - A method of devitrified glass is prepared using titanium slag is mentioned containing chlorine - Google Patents
A method of devitrified glass is prepared using titanium slag is mentioned containing chlorine Download PDFInfo
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- CN109133650A CN109133650A CN201811088051.9A CN201811088051A CN109133650A CN 109133650 A CN109133650 A CN 109133650A CN 201811088051 A CN201811088051 A CN 201811088051A CN 109133650 A CN109133650 A CN 109133650A
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- titanium slag
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
- C03C10/0063—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition containing waste materials, e.g. slags
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B1/00—Preparing the batches
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B1/00—Preparing the batches
- C03B1/02—Compacting the glass batches, e.g. pelletising
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/06—Other methods of shaping glass by sintering, e.g. by cold isostatic pressing of powders and subsequent sintering, by hot pressing of powders, by sintering slurries or dispersions not undergoing a liquid phase reaction
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
- Y02P40/50—Glass production, e.g. reusing waste heat during processing or shaping
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- Crystallography & Structural Chemistry (AREA)
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- Life Sciences & Earth Sciences (AREA)
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- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Manufacturing & Machinery (AREA)
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Abstract
The method that titanium slag prepares devitrified glass is proposed using containing chlorine the present invention provides a kind of.The method includes the steps: it chlorine will be contained mentions titanium slag and be dried, crush, or will contain that chlorine mentions titanium slag and ingredient pre-processes, and obtain base powder, wherein mention the mass fraction of titanium slag 85% or more containing chlorine in base powder；Base pressed by powder is formed, devitrified glass green body is obtained；Green body is heat-treated to obtain devitrified glass.The beneficial effect comprise that it is high to propose titanium slag utilization rate containing chlorine；Addition Nucleating Agent, granulating agent and binder are not required in preparation process；Production process three-waste free discharge.
Description
Technical field
The present invention relates to Solid Waste Treatment and Resources utilization and inorganic non-metallic functional material preparation fields, especially
Ground is related to a kind of utilize and proposes the method that titanium slag prepares devitrified glass containing chlorine.
Background technique
Containing chlorine mention titanium slag be titanium-containing blast furnace slag obtained after high temperature cabonization-low temperature chlorination mention titanium slag, chlorinity is higher,
Danger slag is had been cited as, it is very big to harm such as soil, environment.Therefore, the processing of titanium slag is proposed containing chlorine and comprehensively utilize critically important.
Devitrified glass also known as glass ceramics, micro-crystalline ceramic are to pass through control based on glass and ceramic forming technique
Heat treating regime, obtained crystallite phase and glass phase and a kind of polycrystalline material deposited are high hard because it is with good mechanical performance
Degree, high abrasion and acid-alkali-corrosive-resisting etc. can be used as high-grade construction decoration material and multiple functions material etc..Existing devitrified glass
Production technology specifically includes that whole crystallization method, molten sintering method and sol-gel method, for industrial residue devitrified glass, master
Wanting production technology is first two.The production procedure of whole crystallization method be cooperation raw material → high-temperature fusion → pouring molding → annealing →
Nucleus crystallization → polishing trimming → product, the production procedure of molten sintering method are cooperation raw material → high-temperature fusion → water quenching → ball milling
→ tabletting → nucleus crystallization → polishing trimming → product.Whole crystallization method and molten sintering method contain high temperature melting process, together
Shi Erzhe is both needed to secondary high-temperature treatment process, thus there are energy consumption height, and process flow is long, process is tedious, and industrial residue benefit
With the low drawback of rate or defect.
In conclusion there are production energy consumption height, process flow length, waste residue utilization for existing devitrified glass mainstream production technology
The problems such as rate is low.In addition, high because mentioning titanium slag chlorinity containing chlorine, it is difficult to be directly used in building material, it is necessary to be removed by washing roasting
It could be used after chlorine or addition antichlor roasting dechlorination, and added value of product is lower after dechlorination.
Currently, there has been no the methods for only needing a high-temperature process that can prepare devitrified glass, and during the preparation process
It can dechlorinate to titanium slag is mentioned containing chlorine.
Summary of the invention
For the deficiencies in the prior art, it is an object of the invention to solve above-mentioned one existing in the prior art
Or multiple problems.For example, one of the objects of the present invention is to provide a kind of utilize to propose the method that titanium slag prepares devitrified glass containing chlorine,
Chloride can be recycled simultaneously during the preparation process.
To achieve the goals above, one aspect of the present invention provides a kind of utilize and mentions the side that titanium slag prepares devitrified glass containing chlorine
Method.The method can comprise the following steps that will mention titanium slag containing chlorine is dried, crushes, and obtains base powder；By base powder pressure
Type is made, obtains green body；The green body is heated to 800~1000 DEG C, keeps the temperature to promote green body nucleation and crystallization, is again heated to
1100~1200 DEG C of sintering, are cooled down after the completion of to be sintered, obtain devitrified glass.
Another aspect of the present invention also provides a kind of utilize and proposes the method that titanium slag prepares devitrified glass containing chlorine.The method can
The following steps are included: will contain, chlorine will mention titanium slag and ingredient pre-processes, and obtain base powder, wherein in base powder, contains chlorine
The mass fraction of titanium slag is mentioned 85% or more, the ingredient includes fluxing agent and/or devitrified glass ingredient replenishers；By base powder
Body compression moulding, obtains green body；The green body is heated to 800~1000 DEG C, keeps the temperature to promote green body nucleation and crystallization, reheats
It is sintered to 1100~1200 DEG C, is cooled down after the completion of to be sintered, obtain the devitrified glass.
One or more exemplary embodiment according to the present invention, the ingredient can include: quartz, potassium feldspar, nepheline, boron
At least one of sand, soda ash and cullet.Wherein, borax, soda ash can be fluxing agent, quartz sand can be replenishers, potassium feldspar,
Nepheline and cullet can be replenishers and fluxing agent simultaneously.
One or more exemplary embodiment according to the present invention, the method may further comprise the step of: to be obtained described
Devitrified glass carries out trimming and/or polishing.
It is according to the present invention one or more exemplary embodiment, the method may further comprise the step of: by the trimming and/
Or the waste material that polishing generates is returned for making the base powder.In the step of returning to front, re-use, waste material is in institute
The mass fraction stated in base powder can be 0~2%.
One or more exemplary embodiment according to the present invention, the pretreatment includes dry, crushing and mixing, described
The step of crushing may include broken and grinding, can be also classified after the pulverizing.
One or more exemplary embodiment according to the present invention, the granularity of the base powder can be 40~100 μm, into
One step, it can be 45~96 μm.The water content of the base powder is 3~6%.
The step of one or more exemplary embodiment according to the present invention, the compression moulding can include: by the system
Base powder is evenly laid out in a mold, in 250~720kgf/cm2Pressure under 15~30s of pressure maintaining, then demould after obtain base
Body；Further, pressure can be 255~714kgf/cm2。
It is according to the present invention one or more exemplary embodiment, the method may further comprise the step of: to it is described heating and
The gas that holding stage generates is collected and condenses, to recycle chloride, wherein the temperature of condensation can be 400~500 DEG C.
One or more exemplary embodiment according to the present invention, the method may further comprise the step of: to be heated to described
It 800~1000 DEG C and keeps the temperature the gas that generates of 30~60min stage and is collected and condenses, to recycle chloride, wherein condense
Temperature can be 400~500 DEG C.
The step of one or more exemplary embodiment according to the present invention, the green body is heated to 800~1000 DEG C, can
It include: that the green body is heated to 800~1000 DEG C with the heating rate of 5~15 DEG C/min；It is described to be heated to 1100~1200
DEG C the step of can include: be heated to 1100~1200 DEG C with the heating rate of 3~5 DEG C/min.
One or more exemplary embodiment according to the present invention, the mass fraction for mentioning Cl element in titanium slag containing chlorine can
For 2~5%, TiO2Mass fraction can be 2~10%.
One or more exemplary embodiment according to the present invention, the temperature of the drying can be 80~120 DEG C, dry
Time can be 7~13 hours.
Compared with prior art, it the beneficial effect comprise that the process of devitrified glass preparation more simplifies, avoids
The complex processes such as high-temperature fusion and water quenching are not required to addition Nucleating Agent, without addition granulating agent and binder during the preparation process
It directly carries out dry-pressing formed；It can be good at mentioning titanium slag using containing chlorine, proposing titanium slag utilization rate containing chlorine is 85~100%；Heat treatment
Process can be re-used without noxious gas emission, waste material, and production process three-waste free discharge meets green manufacturing technology and wants
It asks.
Detailed description of the invention
By the description carried out with reference to the accompanying drawing, above and other purpose of the invention and feature will become more clear
Chu, in which:
The utilization that Fig. 1 shows an illustrative embodiment of the invention proposes the process that titanium slag prepares devitrified glass method containing chlorine
Schematic diagram；
Fig. 2 shows the utilizations of another exemplary embodiment of the invention to mention the stream that titanium slag prepares devitrified glass method containing chlorine
Journey schematic diagram；
Fig. 3 is the X-ray diffractogram for the devitrified glass sample that example 1 proposes titanium slag preparation containing chlorine；
Fig. 4 is the X-ray diffractogram for the devitrified glass sample that example 2 proposes titanium slag preparation containing chlorine；
Fig. 5 is the scanning electron microscope (SEM) photograph for the devitrified glass sample that example 2 proposes titanium slag preparation containing chlorine；
Fig. 6 is the X-ray diffractogram for the devitrified glass sample that example 5 proposes titanium slag preparation containing chlorine.
Specific embodiment
Hereinafter, utilization of the invention will be described in detail in conjunction with attached drawing and exemplary embodiment and proposes titanium slag preparation containing chlorine
The method of devitrified glass.
Mentioning titanium slag containing chlorine is the one kind obtained after the processing of " high temperature cabonization-low temperature chlorination " titanium extracting technology by titanium-containing blast furnace slag
Low titanium type industry danger slag containing chlorine.Inventor's discovery: the main component for mentioning titanium slag containing chlorine is CaO, SiO2、Al2O3Deng meeting system
The main component of standby devitrified glass, at the same its contain can be directly as the TiO of the Nucleating Agent ingredient of devitrified glass2、Fe2O3；Containing chlorine
Mention Cl in titanium slag-Content be 2~5%, Cl-It mentions in titanium slag containing chlorine mainly with CaCl2Form exists, this will make to mention titanium containing chlorine
Slag has certain room temperature moisture absorption, it can play the role of granulation and bonding during preparing base powder in this way.
Therefore, the invention proposes a kind of methods for preparing devitrified glass as raw material to mention titanium slag containing chlorine.The method
It need to be only collected by a high-temperature process, and to generated chloride during firing devitrified glass, make devitrified glass
Without noxious gas emission in preparation process.The preparation method is that solid waste utilizes, reduces environmental pollution and save in production
The green manufacturing technique that can be lowered consumption with three-waste free discharge.
One aspect of the present invention provides a kind of utilize and proposes the method that titanium slag prepares devitrified glass containing chlorine.Fig. 1 shows this hair
The utilization of a bright exemplary embodiment mentions the flow diagram that titanium slag prepares devitrified glass method containing chlorine.
In an exemplary embodiment of the present invention, the method can comprise the following steps that
To mention titanium slag as raw material containing chlorine, or to propose titanium slag and ingredient as raw material containing chlorine, raw material is pre-processed, is obtained
To the base powder that water content is 3%~6%, granularity is 40~100 μm, step S01 as shown in figure 1.When raw material only contains chlorine
When mentioning titanium slag, pretreatment may include crushing, being dry；When raw material includes raw material and ingredient, pretreatment may include dry, crushing
With mixing etc. links.The mass fraction of titanium slag is mentioned in base powder (or raw material) containing chlorine 85% or more, this can satisfy solid
Useless high usage demand.The granularity control of base powder at 40~100 μm, granularity control be conducive in the range green body at
Type, while can be avoided the meticulous institute of grinding increased time and energy consumption；Further, the granularity of base powder can be 45~96 μ
m.The ingredient may include one or more of quartz, potassium feldspar, nepheline, borax, soda ash, cullet.Wherein, it adds
Ingredient one kind more preferably selects, for example, the ingredient can not only play fluxing effect, and provides liquid under the high temperature conditions
Phase promotes green body dense sintering, additionally it is possible to complementary element.Ingredient may include fluxing agent and/or devitrified glass ingredient replenishers,
In, some can be used as fluxing agent, have plenty of both to be considered as replenishers, some and have concurrently in ingredient.It can be considered fluxing agent
For borax and soda ash；It can be considered that replenishers are quartz sand, the effect of replenishers is complementary element, enables the devitrified glass produced
It is more stable；It is both replenishers and fluxing agent is potassium feldspar, nepheline and cullet, this three can supplement devitrified glass burning
At required chemical component, while fluxing effect can be provided again.Wherein, devitrified glass ingredient replenishers are in design crystallite glass
When glass formula or devitrified glass composition proportion, the insufficient chemical component of content can be supplemented, microcrystalline glass formula or ingredient are met
Proportion enables more stable prepared devitrified glass, more excellent performance of natural material or chemical reagent.
Base pressed by powder is formed, the green body of devitrified glass is obtained, step S02 as shown in figure 1.The step of compression moulding
Can include: the base powder is evenly laid out in a mold, in 250~720kgf/cm2Pressure under 15~30s of pressure maintaining, so
The green body of the devitrified glass is obtained after demoulding afterwards, it further, can be in 255~714kgf/cm2Pressure under pressure maintaining.Pressure
Be conducive to blank forming and demoulding within the above range with dwell time state modulator, for example, pressure controllable system 310 or
680kgf/cm2, the time can be controlled in 17 or 28s.Wherein, the environmental condition of base can be room temperature, or the temperature of slightly above room temperature
Degree, such as 30~100 DEG C.
Green body is heat-treated to obtain devitrified glass, step S03 as shown in figure 1.Wherein, it is heat-treated can include: by base
Body is heated to 800~1000 DEG C (cold stages), can be 800~950 DEG C further, such as 810 DEG C, 910 DEG C etc., then
To promote green body nucleation and crystallization, it is further continued for being heated to 1100~1200 DEG C (hot stage or sintering stage) sintering, further may be used
It is 1130~1185 DEG C, for example, 1140 DEG C, 1170 DEG C etc., it is cooling after the completion of to be sintered.Wherein, the soaking time of cold stage
It can be 30~60min, the soaking time of hot stage can be 30~90min.The heating rate for being heated to cold stage is controllable
In 5~15 DEG C/min, volatile material (such as CO in green body can quickly and be farthest excluded in cold stage in this way2、
Chloride etc.), be conducive to the collection of chloride and the sintering of green body；Further, the heating rate of cold stage can be 5~10
℃/min.The heating rate for being heated to the heating process of hot stage can be controlled in 3~5 DEG C/min, in this way can be in high temperature rank
The problems such as deformation of blank sintering caused by section prevents heating rate too fast or uneven sintering, i.e., heating rate is too fast influences whether to burn
The quality of knot, and the too low energy consumption that will cause of heating rate is high, low efficiency.The temperature and time of cold stage is controlled 800
~1000 DEG C and 30~60min, be conducive to the nucleation and crystallization of green body；By the control of the temperature and time of hot stage 1100~
1200 DEG C and 30~90min, blank sintering can be enabled fine and close.Cooling step may include slow cooling to room temperature (or environment temperature),
Or first slow cooling rapid cooling again.Wherein, rapid cooling is specific again for first slow cooling can include: heat preservation terminates (i.e. hot stage under firing temperature
Heat preservation terminates) after, carry out slow cooling processing, by firing temperature slow cooling to 300~500 DEG C, rate of temperature fall can for 1~4 DEG C/
Min, the rate of temperature fall can reduce quartz crystal conversion or be sintered the unstable influence to devitrified glass；Then by 300~500
DEG C fast cooling is not affected by temperature to 200 DEG C hereinafter, such as 30~100 DEG C in the devitrified glass performance of this temperature range, because
This can be rapidly cooled, such as directly drum cold wind is rapidly cooled to reduce energy consumption, which can be 5~10
℃/min。
Heat treatment process can carry out in oxygen containing gas, such as air or oxygen rich gas.
In the present embodiment, the present invention directly can mention titanium slag containing chlorine using cinder field accumulation, containing chlorine mention titanium slag include according to
The following ingredient of mass fraction meter: 28~33%CaO, 20~25%SiO2, 10~14%Al2O3, 2~7%MgO, 2~10%
TiO2, 2~4%Fe2O3, 2~5%Cl element.Cinder field accumulation proposes the content of water in titanium slag by ambient humidity and season shadow containing chlorine
Sound is larger, for example, the water content in titanium slag is proposed up to 8%~10% containing chlorine in humidity biggish summer, and it is lesser in humidity
Autumn, water content also have 6~8%.
The water in titanium slag is mentioned containing chlorine with moisture absorption due to mentioning titanium slag containing chlorine, such as mentions in titanium slag containing chlorine and not being gone by drying
The water removed, and in preprocessing process the secondary moisture absorption water, binder can be played the role of in preprocessing process, meanwhile,
The cementation as caused by water also forms the effect of granulation so that little particle generates agglomeration, and granulation process is practical
Upper is exactly by tiny powder granule by cementation, and aggregation forms bulky grain.
In the present embodiment, if aqueous height can be unfavorable for crushing (such as being unfavorable for ball milling) in raw material, it is equal to will affect powder
Evenness can also have an impact the proportion of raw material, moreover, if aqueous height in raw material, in subsequent compression moulding, water in raw material
It will receive pressure outflow, the corrosion of mold will be increased in this way.Therefore, it is necessary to which raw material is dried, make the water content in raw material
It is reduced to 6% hereinafter, further, being reduced to 5% or less；I.e. in base powder water content should 6% hereinafter, further,
It is reduced to 5% or less.Therefore, it is necessary to especially mention titanium slag containing chlorine and be dried to raw material.
In the present embodiment, water content should be controlled 3%~6% in base powder, further, can 4%~6%,
Further, it can be controlled in 4%~5%.When base powder moisture content is lower than 3%, in base step (i.e. S02 step)
Pressure under (such as 250~720kgf/cm2) pressing blank when, be easy to cause green body that can not be compacted, there is defect in edge,
If improving pressure, easily causes the expansion of residual air and make blank cracking.
In the present embodiment, when raw material, which only contains chlorine, mentions titanium slag, the pretreated step can include: chlorine will be contained and mention titanium
Slag is dried and crushes.
When raw material includes to mention titanium slag and ingredient containing chlorine, the pretreated step can include: chlorine will be contained and mention titanium slag and match
Material first mixes, re-dry, crushing；Alternatively, when in ingredient water content it is less without it is dry when, only containing chlorine, to mention titanium slag dry, then
Titanium slag will be mentioned containing chlorine after drying and ingredient is crushed, mixed, crush and mix can in no particular order sequentially；Alternatively, working as ingredient
It when middle water content is higher, will contain that chlorine mentions titanium slag and ingredient is all dried, and then crush and mix again, crush and mix can be regardless of
Sequencing.
Preferably, it is contemplated that it is higher to mention water content in titanium slag, and drying can crush, before mixing, can reduce in this way or
Avoiding result in each substance finally cooperates result and the proportion planned to generate deviation.
In the present embodiment, if containing ingredient in raw material, except it is described mention titanium slag containing chlorine in addition to, the raw material or base powder
It may also include according to mass percent meter: quartz 0~10%, potassium feldspar 0~7%, nepheline 0~5%, borax 0~3%, pure
Alkali 0~5%, cullet 0~15%.If the waste material also generated containing trimming and/or polishing in raw material, waste material is in raw material or institute
Stating the mass fraction in powder is 0~2%.
In the present embodiment, the method, which may further comprise the step of:, carries out trimming and/or polishing for obtained devitrified glass,
The waste material that the step obtains returns to one kind as raw material.Polishing (can return in reuse after precipitation with cooling water caused by trimming
It receives and utilizes).
In the present embodiment, the method may further comprise the step of: the gas generated to the heat treatment stages and be collected
And condensation may include chloride gas in gas to recycle chloride, chloride may include the chlorate of potassium, sodium, such as chlorination
Sodium, potassium chloride etc..Wherein, can emphasis to first heating period (being heated to 800~1000 DEG C of stage from room temperature) and first
The gas that a holding stage (800~1000 DEG C of holding stages) generates is collected and condenses, this is because when temperature is more than
After 1000 DEG C, by the cooling content for being recovered to chlorine with regard to few, whole chlorine 1~5% are only accounted for.
Wherein, the temperature of condensation is 400~500 DEG C, and condensation temperature control can enable chloride gas obtain in the range
To abundant condensation precipitating, the powder of aggregation is utmostly obtained.For example, when heat treatment process carries out in tunnel oven, in tunnel
Gas collection and condensing unit, condensation temperature are added on the exhaust pipe of the low-temperature heat section (being heated to 800~1000 DEG C) of road kiln
Degree is set in 400~500 DEG C, for recycling chloride.During heating, chloride volatilizees from green body, by draft mechanism
Chloride gas is evacuated in exhaust pipe rapidly, exhaust pipe used can be the pipeline of resistance to acid and alkali gas attack, gas stream
When moving to the Near Pipelines for having condensing unit, the chloride in gas forms aggregation after condensing and is attached on tube wall, together
The upper settable reciprocation type scrapper conveyor of Shi Guanbi carries out cycle operation, cleans in the collecting bag below aggregation to pipeline, can get
The chlorides powder product such as potassium sodium, the innocuous gas after condensation process are introduced in kiln by air-introduced machine, and one side can be to gas in this way
The waste heat of body is used, and on the other hand remaining chloride gas can be made to be adsorbed on green body to be heated, and then is adding
It is again introduced into exhaust pipe in thermal process, and then is further purified.For example, the outlet end of exhaust pipe may be provided at it is low
The entrance of warm heating zone, to be preheated to the green body that will enter low-temperature heat area.
In another exemplary embodiment of the invention, as shown in Fig. 2, preparing devitrified glass using titanium slag is mentioned containing chlorine
Method can contain chlorine and mention titanium slag or to propose titanium slag and ingredient as raw material containing chlorine, base powder be obtained by pretreatment, to powder
Dry-pressing formed obtained devitrified glass green body is carried out, low-temperature heat, high-temperature heating and cooling are carried out to green body in tunnel oven, then pass through
Cross trimming, polishing and etc., finally be made crystallized glass article.
Located in advance specifically, the method for preparing devitrified glass can comprise the following steps that 1) to contain chlorine and mention titanium slag with ingredient
Base powder is obtained after reason.Ingredient can be in quartz, potassium feldspar, nepheline, borax, soda ash, cullet, polishing and trimming waste material
One or two or more complex；Preprocessing process includes dry, broken, grinding, classification etc..It mentions titanium slag containing chlorine and matches
Material can be separately dried, be crushed, grinding, be cooperated after classification, can also first cooperate, then dry, crush.It mentions titanium slag containing chlorine and matches
Expect composition batch in each component mass percent are as follows: containing chlorine mention titanium slag 85~100%, quartz 0~10%, potassium feldspar 0~
7%, nepheline 0~5%, borax 0~3%, soda ash 0~5%, cullet 0~15%, polishing and trimming waste material 0~2%.It is described
Ingredient can play fluxing effect, and provide liquid phase under the high temperature conditions, promote green body dense sintering.The base powder of acquisition
The granularity of body is 45~96 μm.
2) by the evenly laid out mold of base powder, dry-pressing is carried out by control pressure and dwell time using press machine
Molding, obtains devitrified glass green body after demoulding.Such as base powder can be tiled and be put into mold, using press machine, 255
~714kgf/cm2Pressure under, pressure maintaining 15~30s is dry-pressing formed, and demoulding obtains devitrified glass green body.
3) devitrified glass green body is put into tunnel oven, heat treatment process and parameter is set, specifically: with 5~10 DEG C/
The heating rate of min rises to 800~950 DEG C by room temperature, keeps the temperature 30~60min；Again with the heating rate of 3~5 DEG C/min, by
800~950 DEG C are warming up to 1130~1185 DEG C, keep the temperature 30~90min；Then with slowly cooling to 300~500 DEG C after, then by
300~500 DEG C of air blast are cooled to 30~100 DEG C fastly；It takes out and it is polished, obtains crystallized glass article after trimming.Polishing
It is re-used with waste recovery obtained by trimming as ingredient, polishing and cooling water reuse after precipitation caused by trimming.
As shown in Fig. 2, in (800~950 DEG C) of the tunnel oven low-temperature heat section settable exhaust pipes in outlet, on exhaust pipe
Settable condensing unit and reciprocation type scrapper conveyor.Tunnel oven is heated at high temperature section (1130~1185 DEG C) and low-temperature heat section air-flow
Direction be it is opposite, high-temperature heating section generate chloride gas can with low temperature presintering (i.e. low-temperature heat) generate gas together with
Into in exhaust pipe, the chlorinations powders such as potassium, sodium are formed after condensing under the action of condensing unit, reciprocation type scrapper conveyor can
To be recycled to chloride.
The object phase of devitrified glass is prepared according to the method for two examples above embodiment can include: glass phase and crystallite
Phase.Prepared devitrified glass includes three kinds.
The first: the mass fraction of the glass phase is 5~15%, and the mass fraction of the crystallite phase is 85~95%,
The crystallite phase may include mass ratio (42~48): (35~45): akermanite phase, diopside phase and the perovskite of (12~16)
Phase.Wherein, akermanite is mutually principal crystalline phase, and diopside phase, Perovskite Phase are secondary crystal phase.
In crystallite phase, mass fraction shared by akermanite phase can be 42~48%, and mass fraction shared by diopside phase can
It is 35~45%, remaining can be Perovskite Phase.Wherein, akermanite phase and diopside phase content are high, help to improve crystallite glass
The mechanical property of glass.For example, mass fraction shared by akermanite phase can be 46 ± 1%, mass fraction shared by diopside phase can be
39 ± 0.5%, surplus can be Perovskite Phase.Wherein, akermanite phase devitrified glass performance opposite with diopside plays a leading role,
Diopside phase content is in 38~41% ranges, such as 39%, akermanite phase content in 43~45% ranges, such as
44%, at this point, devitrified glass performance is best.Due to mentioning, calcium and magnesium aluminium silicone content is higher in titanium slag, be conducive to akermanite phase and thoroughly
The formation of pyroxene phase；And ceramics can be promoted by mentioning the iron in titanium slag, facilitate akermanite and diopside crystal grain
Growth improves the content of akermanite phase and diopside phase；The titanium in titanium slag is mentioned, can also promote ceramics, promote simultaneously
Into the formation of Perovskite Phase.
Crystallite phase morphology is mainly plate, short cylinder and graininess in devitrified glass；Wherein, akermanite is mutually plate,
Diopside is short cylinder, and Perovskite Phase is graininess.The length of plate crystallite phase can be 1.5~3.4 μm, and width can be 1~1.7
μm, such as it is 1.8 μm long, 1.2 μm wide, it is for another example 3.2 μm long, 1.6 μm wide；The length of short cylinder crystallite phase can be 1.4~2.5 μm,
Width can be 1.2~1.7 μm, for example, it is 2.0 ± 0.4 μm long, it is 1.5 ± 0.1 μm wide；The partial size of granular microcrystalline phase can for 0.5~
1.2 μm, for example, 0.8 ± 0.2 μm.Above crystallite phase morphology, that is, crystallite phase size is smaller, and respectively less than 5 μm, the lesser crystallite of size
It mutually interconnects, generated gap is smaller, is conducive to even in liquid phase filling, reduces void count, promote the property of devitrified glass
Energy.
May also include in the devitrified glass has stomata, wherein the volume accounting of stomata is 5% hereinafter, such as 1~5%.
Stomata may include that glass phase is not filled up completely the alternate gap of crystallite in devitrified glass, i.e., the described stomata include the glass phase with
The gap between gap and each crystallite phase between the crystallite phase.The aperture of the stomata can be 1~3 μm, such as 2 ±
0.4μm.In the production process of devitrified glass or ceramics, stomata can not exclude completely, the gas of devitrified glass provided by the invention
Hole accounting is lower, aperture is smaller, this can guarantee the high-performance of devitrified glass.
Second, the crystallite phase of devitrified glass may include principal crystalline phase: diopside phase, secondary crystal phase: akermanite phase, perovskite
Phase and quartzy phase；Wherein, mass fraction shared by diopside phase is 62~67%, mass fraction shared by akermanite phase is 14~
20%, mass fraction shared by Perovskite Phase is 3~5%, and surplus can be quartzy phase；For example, mass fraction shared by diopside phase is
64 ± 1%, mass fraction shared by akermanite phase can be 17 ± 1%, and mass fraction shared by Perovskite Phase can be 4 ± 0.5%, remaining
Amount is quartzy phase.
The third, the crystallite phase of devitrified glass may include principal crystalline phase: diopside phase, secondary crystal phase: aspidelite phase.Wherein, saturating brightness
Mass fraction shared by stone phase can be 95~97%, and surplus is aspidelite phase；Such as mass fraction shared by diopside phase can for 96 ±
0.5%, mass fraction shared by aspidelite phase can be 3.5 ± 0.1%.
The property of prepared devitrified glass is as follows: volume density is 2.60~2.8g/cm2, water absorption rate be 0.05~
0.3%, compression strength is 102~140MPa, and acid resistance is 96% or more, and alkali resistance is 97% or more.
Exemplary embodiments mentioned above for a better understanding of the present invention carries out into one it below with reference to specific example
Walk explanation.
Example 1
It is specific the preparation method is as follows:
1) taking Sichuan somewhere through " high temperature cabonization-low temperature chlorination " titanium extracting technology, treated that mention titanium slag containing chlorine be main former
Material, ingredient are selected as quartz, potassium feldspar and borax, will propose titanium slag and ingredient in 105 DEG C of drying indoor seasoning 8h, then containing chlorine
It is crushed, grinding, classification, is by mass percentage blast furnace slag containing chlorine (mentioning titanium slag containing chlorine) 85%, quartz by each component
5%, potassium feldspar 7%, borax 3% carries out weighing cooperation, takes the powder that granularity is 96 μm as base powder.
2) by the evenly laid out merging mold of base powder, granulating agent and binder are not added, under press machine, with pressure
Power is 714kgf/cm2, the pressing conditions progress of dwell time 20s is dry-pressing formed, then demoulds, obtains devitrified glass green body.
3) devitrified glass green body is put into tunnel oven, sets heat treatment process and parameter, specifically: with 7 DEG C/min's
Heating rate rises to 800 DEG C by room temperature, keeps the temperature 60min；Then with the heating rate of 5 DEG C/min, 1130 DEG C are risen to by 800 DEG C,
60min is kept the temperature, then 400 DEG C of Slow cooling, rate of temperature fall is 2 DEG C/min；Then it is cooled to 50 DEG C fastly by 400 DEG C, rate of temperature fall
For 10 DEG C/min；It takes out and polishes, obtain crystallized glass article after trimming.Wherein, conduct is collected to polishing trimming waste material
Ingredient uses, polishing and the cooling water reuse after precipitation during trimming.In room temperature to unlatching tunnel oven during 800 DEG C
Gas collection and condensing unit, condensation temperature are set as 400 DEG C.In temperature-rise period, the chloride gas that green body generates is evacuated to row
In feed channel, it is attached on tube wall through condensation, while opening the reciprocation type scrapper conveyor on tube wall and carrying out circulation cleaning, by aggregation
It collects into the collecting bag below tube wall, can get potassium na chloride powder.
4) as shown in figure 3, its principal crystalline phase of obtained crystallized glass article is diopside phase, secondary crystal phase is akermanite
Phase, Perovskite Phase and quartzy phase.The crystallized glass article is tested for the property, volume density is 2.64g/cm after tested3, water suction
Rate is 0.20%, compression strength 108MPa, acid resistance 96.7%, alkali resistance 97.2%.
Example 2
It is specific the preparation method is as follows:
1) to mention titanium slag containing chlorine in example 1 as whole raw materials, titanium slag is mentioned in drying 12h in 110 DEG C of hothouses, so containing chlorine
After be crushed, grinding, classification, taking granularity is 96 μm of powder as base powder.
2) tiling of base powder is placed in mold, using press machine, in pressure be 510kgf/cm2, pressure maintaining 20s's
It carries out dry-pressing formed under the conditions of base, then demoulds, obtain devitrified glass green body.It is not added during devitrified glass blank forming
Granulating agent and binder.
3) devitrified glass green body is put into tunnel oven, sets heat treatment process and parameter, specifically: with 5 DEG C/min's
Heating rate rises to 890 DEG C by room temperature, keeps the temperature 30min；Then with the heating rate of 3 DEG C/min, 1185 DEG C are risen to by 890 DEG C,
Keep the temperature 60min；Then 500 DEG C are slowly cooled to, rate of temperature fall is 3 DEG C/min, is then quickly cooled to 30 DEG C by 500 DEG C, drop
Warm 5 DEG C/min of rate；It takes out and polishes after cooling, obtain crystallized glass article after trimming.Room temperature is heated to 850 DEG C
The gas collection and condensing unit of tunnel oven are opened in journey, condensation temperature is set in 450 DEG C, in temperature-rise period, is generated by green body
A small amount of chloride gas fallen on the tube wall of exhaust pipe through condensation, while opening the reciprocation type scrapper conveyor on tube wall and being followed
Ring cleans, and aggregation is collected into collecting bag below tube wall, obtains chlorination powder.
4) crystallized glass article prepared by carries out X-ray diffraction test and analysis, and as shown in Figure 4, principal crystalline phase is magnesium
Melilite phase, secondary crystal phase are diopside and Perovskite Phase.Electronic Speculum (SEM) test is scanned to the crystallized glass article and is divided
Analysis, test results are shown in figure 5, from figure 5 it can be seen that crystallite phase morphology is mainly plate, short cylinder in the devitrified glass
And graininess, devitrified glass are made of crystallite phase, glass phase and Minute pores, glass phase is mutually twisted with crystallite phase, structure compared with
For densification.The crystallized glass article is tested for the property, the volume density of crystallized glass article is 2.70g/cm after tested3, inhale
Water rate is 0.11%, compression strength 120MPa, acid resistance 97.8%, alkali resistance 98.5%.
Example 3
It is specific the preparation method is as follows:
1) titanium slag is mentioned containing chlorine and quartz, nepheline are put into 108 DEG C of drying indoor seasoning 8h, each component is pressed into quality percentage
Than carrying out weighing cooperation for blast furnace slag containing chlorine 85%, quartz 10%, nepheline 5%, then it is crushed, grinding, classification are made
The granularity of base powder is 75 μm.
2) it is placed in base powder is evenly laid out in mold, using press machine, in 357kgf/cm2Under pressure, pressure maintaining
15s progress is dry-pressing formed, then demoulds, and obtains devitrified glass green body.Granulating agent is not added during devitrified glass blank forming
With binder.
3) devitrified glass green body is put into tunnel oven, sets heat treatment process and parameter, specifically: with 5 DEG C/min's
Heating rate rises to 950 DEG C by room temperature, keeps the temperature 30min；Then with the heating rate of 3 DEG C/min, 1160 DEG C are risen to by 950 DEG C,
Keep the temperature 60min；Then 300 DEG C are slowly cooled to, 4 DEG C/min of rate of temperature fall；Then 100 DEG C are quickly cooled to by 300 DEG C, cooling
Rate is 6 DEG C/min；It takes out and polishes after cooling, obtain crystallized glass article after trimming.Room temperature rises to 950 DEG C of process
The middle gas collection and condensing unit for opening tunnel oven, condensation temperature are set as 500 DEG C, are passed through by the chloride gas that green body generates
After condensation, aggregation is formed on the tube wall of exhaust pipe, while being opened the reciprocation type scrapper conveyor on tube wall and being carried out circulation cleaning,
Aggregation is collected into collecting bag below tube wall, potassium na chloride powder is obtained.
4) to prepared crystallized glass article with reference to being tested for the property, after tested, the volume density of crystallized glass article
For 2.68g/cm3, water absorption rate 0.15%, compression strength 114MPa, acid resistance 98%, alkali resistance 97.5%.
Example 4
It is specific the preparation method is as follows:
1) will contain chlorine mentions titanium slag and quartz, soda ash, polishing trimming waste material carry out after dry 10h is put into 110 DEG C of hothouses
It is broken, then grinding, classification, then by each component mass percent be that titanium slag 90%, quartz 3%, soda ash 5%, polishing are proposed containing chlorine
Trimming waste material 2% carries out weighing cooperation, takes the powder that granularity is 75 μm as base powder.
2) base is laid in mold with powder, is 357kgf/cm in pressure using press machine2, the item of pressure maintaining 30s
It is dry-pressing formed under part, it then demoulds, obtains devitrified glass green body.Granulating agent is not added during devitrified glass blank forming and is glued
Tie agent.
3) devitrified glass green body is put into tunnel oven, sets heat treatment process and parameter, specifically: with 5 DEG C/min's
Heating rate rises to 850 DEG C by room temperature, keeps the temperature 60min；Then with the heating rate of 3 DEG C/min, 1180 DEG C are risen to by 850 DEG C,
Keep the temperature 90min；Then with the heating rate of 3 DEG C/min, 1180 DEG C is risen to by 850 DEG C, 90min is kept the temperature, then slowly cools to
450 DEG C, rate of temperature fall is 1 DEG C/min；Then 40 DEG C are quickly cooled to by 450 DEG C, rate of temperature fall is 8 DEG C/min；Cooling terminates
After take out and polish, obtain crystallized glass article after trimming.Room temperature to open during 850 DEG C the gas collection of tunnel oven with
Condensing unit, condensation temperature are set as 450 DEG C.The chloride gas generated by green body falls in the tube wall of exhaust pipe through condensing
On, while opening the reciprocation type scrapper conveyor on tube wall and carrying out circulation cleaning, aggregation is collected into collecting bag below tube wall, is obtained
Obtain potassium na chloride powder.
4) to obtained crystallized glass article with reference to being tested for the property, the volume density of crystallized glass article is after tested
2.62g/cm3, water absorption rate 0.28%, compression strength 105MPa, acid resistance 96%, alkali resistance 99.2%.
Example 5
It is specific the preparation method is as follows:
1) it will contain that chlorine mentions titanium slag and cullet is put into broken, grinding, classification after 105 DEG C of dry indoor seasoning 8h, then press
Mass percent is to mention titanium slag 85%, cullet 15% containing chlorine to carry out weighing cooperation, takes the powder that granularity is 45 μm as base
Use powder.
2) 45 μm of base powder tilings are taken to put into mold, using press machine, in 255kgf/cm2Pressure under, pressure maintaining
30s progress is dry-pressing formed, then demoulds, and obtains devitrified glass green body.Granulating agent is not added during devitrified glass blank forming
With binder.
3) devitrified glass green body is put into tunnel oven, sets heat treatment process and parameter, specifically: with 10 DEG C/min's
Heating rate rises to 850 DEG C by room temperature, keeps the temperature 60min；Then with the heating rate of 3 DEG C/min, 1130 DEG C are risen to by 850 DEG C,
Keep the temperature 90min；Then 350 DEG C are slowly cooled to, rate of temperature fall is 4 DEG C/min；Then 80 DEG C are quickly cooled to by 350 DEG C, drop
Warm 10 DEG C/min of rate；It takes out and polishes after cooling, obtain crystallized glass article after trimming.It is opened when room temperature is to 850 DEG C
The gas collection and condensing unit of tunnel oven, condensation temperature are set as 450 DEG C.To in temperature-rise period green body generate chloride into
Row is collected, and collection process is same as above, and then obtains potassium na chloride powder.
4) its principal crystalline phase of crystallized glass article obtained by is diopside phase, and secondary crystal phase is aspidelite phase (see Fig. 6).It is micro- to this
Crystal glass is tested for the property, and the volume density of crystallized glass article is 2.74g/cm after tested3, water absorption rate 0.09%, resistance to compression
Intensity is 131MPa, acid resistance 98.5%, alkali resistance 97%.
In conclusion the present invention has significantly compared with the existing technology using proposing the method that titanium slag prepares devitrified glass containing chlorine
The progress of property, its advantages are as follows:
1) technical process that the present patent application uses includes that ingredient → base → low temperature dechlorination → high temperature sintering → polishing is cut
Side → product, only once high-temperature heat treatment process, process more simplify the technology, avoid molten sintering method and entirety
The complex processes such as high-temperature fusion and water quenching in crystallization method sintering process.
2) relative to molten sintering method and whole crystallization method, the TiO used mentioned containing chlorine in titanium slag raw material in the present invention2With
Fe2O3, may act as the effect of complex phase Nucleating Agent, addition Nucleating Agent be not required in preparation process；Containing chlorine mention titanium slag utilization rate be 85~
100%.
3) present invention can be carried out directly using the characteristic for proposing the titanium slag room temperature moisture absorption containing chlorine without adding granulating agent and binder
It is dry-pressing formed, be omitted bonding, be granulated and etc..
4) the present patent application can dechlorinate, without harmful gas during preparing devitrified glass to titanium slag is mentioned containing chlorine
Body discharge, meanwhile, polishing is re-used with trimming waste material as ingredient, and the reuse after precipitation such as cooling water, production process is without three
Useless discharge, is conducive to environmental protection, meets the requirement of green manufacture technology.
5) it is higher than lithotome with the microcrystallite body properties of the method for the invention preparation, can be used as top-grade building
Ornament materials, technique engraving and ceramic material etc..
6) process flow of the invention is simple, low energy consumption, it is environmentally protective, be more advantageous to commercial introduction, be especially suitable for application
In the central and west regions that electric power is sufficient, ecological environment is more fragile.
Although those skilled in the art should be clear above by combining exemplary embodiment to describe the present invention
Chu can carry out exemplary embodiment of the present invention each without departing from the spirit and scope defined by the claims
Kind modifications and changes.
Claims (10)
1. a kind of propose the method that titanium slag prepares devitrified glass using containing chlorine, which is characterized in that the described method comprises the following steps:
It chlorine will be contained mentions titanium slag and be dried, crush, and obtain base powder；
Base pressed by powder is formed, green body is obtained；
The green body is heated to 800~1000 DEG C, keeps the temperature to promote green body nucleation and crystallization, is again heated to 1100~1200 DEG C of burnings
Knot is cooled down after the completion of to be sintered, obtains devitrified glass.
2. a kind of propose the method that titanium slag prepares devitrified glass using containing chlorine, which is characterized in that the described method comprises the following steps:
Titanium slag is mentioned and ingredient pre-processes to containing chlorine, obtains base powder, wherein propose the matter of titanium slag containing chlorine in base powder
Score is measured 85% or more, the ingredient includes fluxing agent and/or devitrified glass ingredient replenishers；
Base pressed by powder is formed, green body is obtained；
The green body is heated to 800~1000 DEG C, keeps the temperature to promote green body nucleation and crystallization, is again heated to 1100~1200 DEG C of burnings
Knot is cooled down after the completion of to be sintered, obtains devitrified glass.
3. according to claim 2 propose the method that titanium slag prepares devitrified glass using containing chlorine, which is characterized in that the ingredient
It include: at least one of quartz, potassium feldspar, nepheline, borax, soda ash and cullet.
4. according to claim 1 or 2 propose the method that titanium slag prepares devitrified glass using containing chlorine, which is characterized in that described
The water content of base powder is 3~6%, granularity is 40~100 μm.
5. according to claim 1 or 2 propose the method that titanium slag prepares devitrified glass using containing chlorine, which is characterized in that described
The step of compression moulding includes:
The base powder is evenly laid out in a mold, in 250~720kgf/cm2Pressure under 15~30s of pressure maintaining, then take off
Mould obtains green body.
6. according to claim 1 or 2 propose the method that titanium slag prepares devitrified glass using containing chlorine, which is characterized in that described
Method further comprises the steps of: the gas generated to the heat treatment stages and is collected and condenses, to recycle chloride, wherein cold
Solidifying temperature is 400~500 DEG C.
7. according to claim 1 or 2 propose the method that titanium slag prepares devitrified glass using containing chlorine, which is characterized in that described
The step of green body is heated to 800~1000 DEG C include: the green body is heated to 800 with the heating rate of 5~15 DEG C/min~
1000℃；Described the step of being heated to 1100~1200 DEG C include: be heated to 1100 with the heating rate of 3~5 DEG C/min~
1200℃。
8. according to claim 1 or 2 propose the method that titanium slag prepares devitrified glass using containing chlorine, which is characterized in that described
The mass fraction for mentioning Cl element in titanium slag containing chlorine is 2~5%, TiO2Mass fraction be 2~10%.
9. according to claim 1 or 2 propose the method that titanium slag prepares devitrified glass using containing chlorine, which is characterized in that described
Method further comprises the steps of:
The obtained devitrified glass is subjected to trimming and/or polishing.
10. according to claim 9 propose the method that titanium slag prepares devitrified glass using containing chlorine, which is characterized in that the side
Method, which is further comprised the steps of:, is used to make the base powder for the waste material return that the trimming and/or polishing generate.
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