CN109265026B - Dechlorination method of titanium extraction tailings, product of titanium extraction tailings, slag micro powder, application of slag micro powder and product of slag micro powder - Google Patents
Dechlorination method of titanium extraction tailings, product of titanium extraction tailings, slag micro powder, application of slag micro powder and product of slag micro powder Download PDFInfo
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- CN109265026B CN109265026B CN201811180048.XA CN201811180048A CN109265026B CN 109265026 B CN109265026 B CN 109265026B CN 201811180048 A CN201811180048 A CN 201811180048A CN 109265026 B CN109265026 B CN 109265026B
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- 238000000605 extraction Methods 0.000 title claims abstract description 207
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 199
- 239000010936 titanium Substances 0.000 title claims abstract description 197
- 229910052719 titanium Inorganic materials 0.000 title claims abstract description 197
- 238000006298 dechlorination reaction Methods 0.000 title claims abstract description 97
- 238000000034 method Methods 0.000 title claims abstract description 89
- 239000002893 slag Substances 0.000 title claims abstract description 61
- 239000000843 powder Substances 0.000 title claims abstract description 50
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 79
- 239000000203 mixture Substances 0.000 claims abstract description 36
- 239000007788 liquid Substances 0.000 claims abstract description 33
- 238000010438 heat treatment Methods 0.000 claims abstract description 21
- 238000001816 cooling Methods 0.000 claims abstract description 8
- 239000004566 building material Substances 0.000 claims description 22
- 150000003608 titanium Chemical class 0.000 claims description 22
- 238000001035 drying Methods 0.000 claims description 20
- 230000008569 process Effects 0.000 claims description 20
- 238000001914 filtration Methods 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 14
- 239000004567 concrete Substances 0.000 claims description 12
- 230000009467 reduction Effects 0.000 claims description 12
- 238000000926 separation method Methods 0.000 claims description 11
- 239000004568 cement Substances 0.000 claims description 8
- 230000000382 dechlorinating effect Effects 0.000 claims description 8
- 238000011085 pressure filtration Methods 0.000 claims description 7
- 238000007670 refining Methods 0.000 claims description 6
- 238000005119 centrifugation Methods 0.000 claims description 5
- 238000000967 suction filtration Methods 0.000 claims description 4
- 239000000725 suspension Substances 0.000 claims description 4
- 238000003825 pressing Methods 0.000 claims description 3
- 239000002002 slurry Substances 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 38
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 239000000460 chlorine Substances 0.000 description 57
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 56
- 229910052801 chlorine Inorganic materials 0.000 description 56
- 239000000126 substance Substances 0.000 description 28
- 230000036571 hydration Effects 0.000 description 21
- 238000006703 hydration reaction Methods 0.000 description 21
- 150000001875 compounds Chemical class 0.000 description 15
- 230000000052 comparative effect Effects 0.000 description 11
- 238000002360 preparation method Methods 0.000 description 10
- 239000002699 waste material Substances 0.000 description 9
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 8
- 238000001514 detection method Methods 0.000 description 8
- 238000011534 incubation Methods 0.000 description 6
- 230000009286 beneficial effect Effects 0.000 description 5
- 238000005660 chlorination reaction Methods 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 description 5
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 4
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 4
- 238000004321 preservation Methods 0.000 description 4
- 229910000831 Steel Inorganic materials 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000005265 energy consumption Methods 0.000 description 3
- 238000000227 grinding Methods 0.000 description 3
- 238000010561 standard procedure Methods 0.000 description 3
- 239000010959 steel Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 239000004408 titanium dioxide Substances 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 239000001110 calcium chloride Substances 0.000 description 2
- 229910001628 calcium chloride Inorganic materials 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 239000004035 construction material Substances 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 2
- 229910001629 magnesium chloride Inorganic materials 0.000 description 2
- 238000003801 milling Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- AKEJUJNQAAGONA-UHFFFAOYSA-N sulfur trioxide Chemical compound O=S(=O)=O AKEJUJNQAAGONA-UHFFFAOYSA-N 0.000 description 2
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 1
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 1
- 229910003074 TiCl4 Inorganic materials 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 230000009194 climbing Effects 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- 210000004127 vitreous body Anatomy 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B7/00—Hydraulic cements
- C04B7/14—Cements containing slag
- C04B7/147—Metallurgical slag
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B5/00—Treatment of metallurgical slag ; Artificial stone from molten metallurgical slag
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B7/00—Hydraulic cements
- C04B7/36—Manufacture of hydraulic cements in general
- C04B7/38—Preparing or treating the raw materials individually or as batches, e.g. mixing with fuel
-
- 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
- Y02P40/10—Production of cement, e.g. improving or optimising the production methods; Cement grinding
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention provides a dechlorination method of titanium extraction tailings, a product of the dechlorination method, slag micro powder, application of the slag micro powder and the product of the slag micro powder, and relates to the technical field of metallurgical environmental protection. The dechlorination method of the titanium extraction tailings comprises the steps of heating a mixture of the titanium extraction tailings and water to 250 ℃ in a closed container, preserving the heat for 20-150min, and then cooling to obtain titanium extraction tailings turbid liquid. The dechlorination method of the titanium extraction tailings solves the technical problem that the dechlorination method of the titanium extraction tailings is poor in dechlorination effect and small in influence on activity of the titanium extraction tailings in the prior art, and the dechlorination titanium extraction tailings prepared by the dechlorination method of the titanium extraction tailings are also provided; in addition, the invention also provides slag micro powder, application thereof and a product thereof.
Description
Technical Field
The invention relates to the technical field of metallurgical environmental protection, in particular to a dechlorination method of titanium extraction tailings, a product of the dechlorination method, slag micro powder, application of the slag micro powder and the product of the slag micro powder.
Background
Solid waste generated by the discharge of the titanium-containing blast furnace slag in the metallurgical industry is accumulated, so that the environment is seriously damaged, and simultaneously, the waste of resources is caused. Taking Pan steel as an example, Pan steel discharges about 300 million tons of titanium-containing blast furnace slag every year, the content of titanium dioxide in the titanium-containing blast furnace slag is about 20-26%, the titanium-containing blast furnace slag is generally inactive after water quenching, and the titanium-containing blast furnace slag cannot be directly used as slag micro powder, so that the titanium-containing blast furnace slag is directly stockpiled, and great waste is caused. Therefore, the process of preparing titanium tetrachloride by high-temperature carbonization-low-temperature chlorination is developed in steel climbing. However, the process effectively recycles the titanium element in the titanium-containing blast furnace slag, and realizes resource recycling to a certain extent. But still generates a large amount of titanium extraction tailings after extracting the titanium resource, and the composition of the titanium extraction tailings contains about 2-6% of chlorine element. At present, dechlorination is carried out by a counter-current-water washing process, but the dechlorination has a chlorine content of about 0.2 percent and a poor dechlorination effect; in addition, the dechlorination process can cause the reduction of the hydration activity of the titanium extraction tailings, and the defects seriously affect the large-scale application of the products obtained after dechlorination.
With the development of economy and the acceleration of urban construction, the demand of concrete is more and more increased, and in order to ensure the workability, the hydration activity, the early strength, the later safety, less hydration heat and other properties of concrete, the parameter standards of concrete in the construction field are generally stricter, such as: in the field of building materials, the chlorine content standard is required to be 0.06% or less by referring to the cement standard, and the preparation cost of concrete is high due to the strictness of the parameter standard. Thus, the cost of the concrete is reduced; the titanium extraction tailings dechlorination method with good dechlorination effect is developed, so that the dechlorinated product is more beneficial to large-scale application; the method effectively treats the environmental pollution caused by the massive accumulation of metallurgical wastes, and the aspects are the technical problems which need to be solved at present, and have important economic significance and environmental protection significance.
In view of the above, the present invention is particularly proposed.
Disclosure of Invention
One of the purposes of the invention is to provide a dechlorination method for titanium extraction tailings, which solves the technical problem that the dechlorination method for titanium extraction tailings in the prior art is lack of a dechlorination method which has good dechlorination effect and has small influence on the hydration activity of the titanium extraction tailings after dechlorination.
The invention also aims to provide a dechlorination method for preparing titanium extraction tailings to obtain dechlorinated titanium extraction tailings, and the treated titanium extraction tailings can be used for preparing slag micro powder.
The invention also aims to provide the slag micro powder prepared by the preparation method of the slag micro powder, which has low chlorine content, good hydration activity and low cost.
The fourth purpose of the invention is to provide application of the slag micro powder in preparation of building materials.
The fifth purpose of the invention is to provide a building material containing the dechlorination titanium extraction tailings or the slag micro powder.
In order to achieve the above purpose of the present invention, the following technical solutions are adopted:
a dechlorination method for titanium extraction tailings comprises the following steps:
in a closed container, heating the mixture of the titanium extraction tailings and water to 100-250 ℃, preserving the heat for 20-150min, and then cooling to obtain titanium extraction tailings turbid liquid.
Preferably, on the basis of the scheme of the invention, the temperature of the mixture of the titanium extraction tailings and water is raised to 100-220 ℃, and preferably to 100-200 ℃;
preferably, the heat preservation time is 30-130min, preferably 30-120 min;
preferably, the temperature is reduced to 20-50 ℃ in the temperature reduction treatment step, and preferably to 20-30 ℃;
preferably, the total volume of the mixture of the titanium extraction tailings and the water accounts for 50-90%, preferably 50-80% of the total volume of the closed container;
preferably, the mass ratio of the titanium extraction tailings to the water in the mixture of the titanium extraction tailings and the water is 1: (2-5), preferably 1: (3-4), more preferably 1: 3.
Preferably, on the basis of the scheme of the invention, the turbid liquid of the titanium extraction tailings is subjected to solid-liquid separation to obtain wet dechlorination titanium extraction tailings.
Preferably, on the basis of the scheme of the invention, the solid-liquid separation mode comprises the following steps: filtration or centrifugation, preferably filtration;
preferably, the method of filtration comprises suction filtration or pressure filtration, preferably pressure filtration.
Preferably, on the basis of the scheme of the invention, the method further comprises the step of drying the wet dechlorination titanium extraction tailings to obtain dechlorination titanium extraction tailings;
preferably, the drying temperature is 80-200 ℃, preferably 100-120 ℃, and more preferably 100 ℃;
preferably, the drying time is 20-80min, preferably 20-60min, and more preferably 60 min.
Preferably, on the basis of the scheme of the invention, the dechlorination method further comprises the step of carrying out heavy suspension after temperature reduction treatment to obtain titanium extraction tailings turbid liquid;
preferably, the method of resuspension comprises stirring or shaking, preferably stirring.
In a second aspect, the dechlorination titanium extraction tailings are prepared by a dechlorination method of the titanium extraction tailings.
Thirdly, the slag micro powder is prepared by thinning the dechlorinated titanium extraction tailings to a specific surface area of more than or equal to 400m 2/kg; obtaining slag micro powder;
preferably, the method of refining is milling.
In a fourth aspect, the dechlorination titanium extraction tailings or the slag micro powder are applied to preparation of building materials.
In a fifth aspect, a construction material comprising the above dechlorinated titanium-extracted tailings or the above slag fine powder;
preferably, the building material comprises cement or concrete.
Compared with the prior art, the invention has the following beneficial effects:
(1) the titanium extraction tailings provided by the invention contain Cl2、HCl、AlCl3、FeCl3、MgCl2、CaCl2The chlorine-containing compound and the chlorine simple substance can be dissolved into a part of water to heat the mixture of the titanium extraction tailings and the water, and the micropore expands with heat and contracts with cold in the heating process, more importantly, the heating treatment is carried out in the closed reactor, so that the internal pressure of the system is increased in the heating process, the heating temperature is 100-250 ℃, water is evaporated into steam at the temperature, water molecules easily enter the micropores of the titanium extraction tailings under strong internal pressure along with the increase of the steam, the chlorine-containing compound or the chlorine simple substance in the micropores is further dissolved into the water, and the steam is more easily introduced into the internal gaps of the titanium extraction tailings; the temperature is kept for 20-150min, so that chlorine-containing compounds and chlorine simple substances can be more fully dissolved in water, the dechlorination effect is further improved, then the temperature is reduced, the steam in the system is changed into liquid, the chlorine-containing compounds and chlorine simple substances enter the solution, and the dechlorination of the titanium extraction tailings is realized; meanwhile, the temperature in the whole temperature rise process is relatively low, so that the influence on the physical or chemical properties of the titanium extraction tailings is small, the dechlorinated titanium extraction tailings obtained by dechlorinating by using the method can keep good hydration activity, and chlorine-containing substances in micropores of the titanium extraction tailings raw materials can be more fully dissolved in water by using the method provided by the invention, so that the dechlorinating effect is good. In conclusion, the dechlorination method for the titanium extraction waste residue solves the technical problem that the dechlorination method for the titanium extraction waste residue is lack in the prior art, has good dechlorination effect and less influence on the hydration activity of the titanium extraction waste residue, and is simple in process; in addition, the titanium extraction tailings are used as raw materials, so that the cost is low, and the environment can be improved due to the utilization of the waste titanium extraction tailings.
(2) The dechlorination titanium extraction tailings prepared by the dechlorination method for the titanium extraction tailings provided by the invention have low chlorine content and good hydration activity. In addition, the slag micro powder provided by the invention thins the dechlorination titanium extraction tailings to a specific surface area of more than or equal to 400m2/kg, obtaining slagMicro-powder; the slag micro powder has the same advantages as the dechlorination titanium extraction tailings, and has low chlorine content and good hydration activity. The invention also provides application of the dechlorination titanium extraction tailings or the slag micro powder in preparation of building materials, and the application can greatly reduce the preparation cost of the building materials. In addition, the invention also provides a building material containing the dechlorination titanium extraction tailings or the slag micro powder, and the building material has the same advantages as the dechlorination titanium extraction tailings or the slag micro powder.
Detailed Description
Embodiments of the present invention will be described in detail below with reference to examples, but it will be understood by those skilled in the art that the following examples are only illustrative of the present invention and should not be construed as limiting the scope of the present invention. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer.
According to the first aspect of the invention, the dechlorination method for the titanium extraction tailings comprises the following steps:
in a closed container, heating the mixture of the titanium extraction tailings and water to 100-250 ℃, preserving the heat for 20-150min, and then cooling to obtain titanium extraction tailings turbid liquid.
After the blast furnace slag with the titanium dioxide content of more than 20 percent is subjected to the process of preparing titanium tetrachloride through high-temperature carbonization-low-temperature chlorination, the discharged chlorinated tailings are the titanium extraction tailings. Typical blast furnace slags have a titanium dioxide content of about 20-26%. The titanium tetrachloride prepared by using the blast furnace slag is subjected to high-temperature carbonization and low-temperature chlorination, and the tailings generated in the process belong to titanium extraction tailings. The titanium extraction tailings mainly comprise CaO, MgO and SiO2、TiO2、Al2O3And the like. However, in the titanium extraction tailings, because of the low-temperature chlorination process, the titanium extraction tailings usually contain 2-6% of chlorine, and the content of the chlorine is high, so that the large-scale application of the titanium extraction tailings is limited. In the titanium extraction tailings, chlorine element exists in the form of compound or chlorine simple substance, and typical but non-limiting existence forms are as follows: HCl and AlCl3、FeCl3、MgCl2、CaCl2、Cl2Or TiCl4. Titanium extractionThe tailings generally contain a large amount of micropores, and the micropores are generated by preparing TiCl through high-temperature carbonization-low-temperature chlorination4TiCl in the process4The titanium extraction tailings enter a gas phase in a gas form to be purified, the remained tailings overflow with a large amount of titanium tetrachloride, a large number of pits and gaps are formed at the original titanium element part, chlorine-containing compounds or chlorine simple substances cannot completely escape and remain in micropores or are adsorbed on the surfaces of the micropores, and the titanium extraction tailings contain a large number of micropores, and the residual chlorine element in the micropores is difficult to remove due to the fact that the micropores are nano-scale, so that the application of the titanium extraction tailings is limited.
In the mixture of the titanium extraction tailings and the water, a part of chlorine-containing compounds and chlorine simple substances in the titanium extraction tailings are dissolved in the water, the mixture of the titanium extraction tailings and the water is subjected to temperature rise treatment, the temperature rise can promote the chlorine-containing compounds and chlorine simple substances in the titanium extraction tailings to be further dissolved in the water, meanwhile, the temperature rise makes micropores in the titanium extraction tailings become large due to expansion with heat and contraction with cold, more importantly, the temperature rise treatment is performed in a closed reactor, the air pressure in the closed reactor becomes large due to evaporation of water in the temperature rise process, the temperature rise temperature is up to 100-250 ℃, and typical but non-limiting temperature rise temperatures are, for example: 100 deg.C, 110 deg.C, 120 deg.C, 130 deg.C, 140 deg.C, 150 deg.C, 160 deg.C, 170 deg.C, 180 deg.C, 190 deg.C, 200 deg.C, 210 deg.C, 220 deg.C, 230 deg.C, 240 deg.C or 250 deg.C, etc. At the moment, a large amount of water is evaporated, and under the action of internal pressure, steam and liquid water can enter internal micropores of the titanium extraction tailings more favorably, so that chlorine-containing compounds and chlorine simple substances in the micropores are dissolved in the water; the incubation is carried out for 20-150min, typical but not limiting incubation times are for example: 20min, 30min, 40min, 50min, 60min, 70min, 80min, 90min, 100min, 110min, 120min, 130min, 140min or 150min and the like, keeping the temperature to ensure that the chlorine-containing compound and the chlorine simple substance in the titanium extraction tailings have more sufficient action time with water, so as to ensure that the chlorine-containing compound and the chlorine simple substance in the micropores of the titanium extraction tailings are more fully dissolved in the water, then cooling the water, changing the steam in the system into liquid, and stirring the mixture in the processes of heating, keeping the temperature and cooling the temperature, wherein the stirring speed is 500-800r/min, and a typical but non-limiting stirring speed is, for example: 600 or 700 r/min. Stirring is carried out, which is beneficial to the circulation of water, so that the titanium extraction tailings are more fully contacted with water, and the chlorine-containing compound and the chlorine simple substance can be more fully and uniformly dissolved in the solution. After the temperature reduction treatment, a large amount of chlorine-containing compounds and chlorine simple substances in the titanium extraction tailings are dissolved in the liquid to obtain a titanium extraction tailings turbid liquid, so that dechlorination of the titanium extraction tailings is realized. Meanwhile, the temperature in the whole temperature rise process is relatively low, so that the influence on the physical or chemical properties of the titanium extraction tailings is small, the damage to the physical or chemical properties of the titanium extraction tailings due to overhigh temperature is avoided, and the physical or chemical properties of the titanium extraction tailings are key factors influencing the hydration activity of the titanium extraction tailings, so that the dechlorinated titanium extraction tailings obtained by dechlorinating by using the method can keep better hydration activity, and chlorine-containing substances in micropores of the titanium extraction tailings raw materials can be more fully dissolved into water, so that the dechlorinating effect is good.
According to the invention, the mixture of the titanium extraction tailings and water is subjected to heating treatment, the pressure in the closed container is increased, water molecules enter the titanium extraction tailings more fully, chlorine-containing substances in micropores in the titanium extraction tailings are dissolved in water more fully, the dechlorination effect is improved, the temperature is kept for a period of time, the dechlorination effect is further improved, the chlorine-containing substances in the titanium extraction tailings are dissolved in water more fully, the dechlorination effect is better, then the temperature is reduced to change water vapor into liquid, the temperature in the whole heating process is lower, the physical or chemical properties of the titanium extraction tailings can be better maintained, and the influence on the hydration activity is smaller.
In a preferred embodiment, the temperature of the mixture of the titanium extraction tailings and water is raised to 100-.
The temperature rise is optimized, the full evaporation of water is ensured, the change of physical or chemical properties caused by overhigh temperature is avoided, and the performance, especially the hydration activity, of the raw material for preparing the slag micro powder at the later stage is better ensured. Typical but non-limiting elevated temperatures are for example: 110 deg.C, 115 deg.C, 125 deg.C, 135 deg.C, 145 deg.C, 155 deg.C, 165 deg.C, 175 deg.C, 185 deg.C, 195 deg.C, 215 deg.C or 220 deg.C.
Preferably, the time for heat preservation is 30-130min, preferably 30-120 min.
The optimal heat preservation time can ensure full dissolution and avoid the overlong process time consumption.
Preferably, the temperature is reduced in the temperature reduction treatment step to a temperature of 20 to 50 ℃, preferably 20 to 30 ℃.
A suitable temperature range for the temperature reduction is preferred, which allows the temperature of the system to be moderate for the subsequent addition of further processing steps and subsequent applications, typical but not limiting temperature reduction being for example: 20 ℃, 30 ℃, 40 ℃ or 50 ℃.
Preferably, the total volume of the mixture of the titanium extraction tailings and the water accounts for 50-90%, preferably 50-80% of the total volume of the closed container.
Preferably, the volume ratio of the total volume of the mixture of the titanium extraction tailings and the water to the total volume of the closed container is favorable for increasing the internal pressure of the system and ensuring the safety of the system, and if the total volume of the mixture of the titanium extraction tailings and the water in the closed container is too large, a large amount of steam is evaporated after heating to easily cause the excessive internal pressure of the system, so that the safety is not favorable. If the volume is too small, the titanium extraction tailings and water mixture is not beneficial to efficient treatment, the single batch treatment amount is reduced, the efficiency is reduced, and the increase of the internal pressure of the system is also not beneficial to the increase of the internal pressure of the system due to the too small volume. The ratio of the total volume of the mixture of the titanium extraction tailings and the water to the total volume of the closed container is, for example: 50%, 60%, 70%, 80% or 90%.
Preferably, the mass ratio of the titanium extraction tailings to the water in the mixture of the titanium extraction tailings and the water is 1: (2-5), preferably 1: (3-4), more preferably 1: 3.
The mass ratio of the titanium extraction tailings to the water in the mixture of the titanium extraction tailings and the water is preferably selected, so that the chlorine-containing substances in the titanium extraction tailings can be fully dissolved, the water content is too low, the chlorine-containing substances can not be fully dissolved, the increase of the internal pressure of a system in the heating process can not be facilitated, and the moisture can not fully enter the micropores of the titanium extraction tailings; in a container with the same volume, the titanium extraction tailings is reduced due to the fact that the water content is too large, single batch treatment of a large amount of titanium extraction tailings is not facilitated, water is wasted, heating energy consumption is high, and unnecessary process cost waste is caused. Typical but non-limiting mixing mass ratios of titanium tailings and water are for example: 1:2, 1:3, 1:4, 1:5, etc.
In a preferred embodiment, the titanium extraction tailings turbid liquid is subjected to solid-liquid separation to obtain wet dechlorination titanium extraction tailings.
And (3) carrying out solid-liquid separation on the turbid liquid of the titanium extraction tailings, and separating chlorine-containing compounds and chlorine simple substances dissolved in the liquid along with the separation of the solution to obtain wet dechlorination titanium extraction tailings.
In a preferred embodiment, the solid-liquid separation comprises: filtration or centrifugation, preferably filtration.
The solid-liquid separation mode can use filtration or centrifugation, and the filtration is preferred because the filtration is low in energy consumption in process, and the centrifugation is high in energy consumption and higher in equipment requirement.
Preferably, the method of filtration comprises suction filtration or pressure filtration, preferably pressure filtration.
Both suction filtration and pressure filtration can achieve the liquid removal effect, with pressure filtration being preferred due to its higher efficiency.
In a preferred embodiment, the method further comprises the step of drying the wet dechlorinated titanium extraction tailings to obtain dechlorinated titanium extraction tailings.
And drying the wet dechlorination titanium extraction tailings to further remove water to obtain the dechlorination titanium extraction tailings.
Preferably, the drying temperature is 80 to 200 ℃, preferably 100-120 ℃, and more preferably 100 ℃.
Typical but non-limiting drying temperatures are for example: 80 deg.C, 90 deg.C, 100 deg.C, 110 deg.C, 120 deg.C, 130 deg.C, 140 deg.C, 150 deg.C, 160 deg.C, 170 deg.C, 180 deg.C, 190 deg.C or 200 deg.C, etc. The values are described such that when the heating temperature is less than 100 ℃, although the boiling point of water molecules is not reached, the water is highly volatile due to the high temperature, and the effect of removing water is similarly achieved within a certain period of time. The drying temperature is preferred in order to improve the drying efficiency and shorten the process time.
Preferably, the drying time is 20-80min, preferably 20-60min, and more preferably 60 min.
Heating times are preferred, too short of a heating time, insufficient moisture removal, too long of a heating time resulting in waste of the process-typical but non-limiting heating times are for example: 20min, 40min, 60min or 80min and the like.
In a preferred embodiment, the dechlorination method further comprises the step of carrying out heavy suspension after the temperature reduction treatment to obtain titanium extraction tailings turbid liquid;
resuspend, i.e., allow the pellet to suspend again. And after the temperature reduction treatment, the titanium extraction tailings turbid liquid is subjected to heavy suspension, so that the circulation between the liquid in the micropores and the liquid outside the micropores is facilitated, the solution is more uniform, the concentration of chlorine-containing compounds in the liquid remaining in the micropores is facilitated to be reduced, and the filtration efficiency is facilitated to be improved.
Preferably, the method of resuspension comprises stirring or shaking, preferably stirring.
The shaking or stirring method can ensure that the titanium extraction tailings after water treatment are also resuspended, wherein the stirring is more time-saving and labor-saving.
In a second aspect, the dechlorination titanium extraction tailings are prepared by a dechlorination method of the titanium extraction tailings.
The dechlorination titanium extraction tailings prepared by the titanium extraction tailing dechlorination method have low chlorine content in the obtained titanium extraction tailings because the chlorine-containing substances remained in the micropores in the titanium extraction tailings are sufficiently removed in the process, and the prepared dechlorination titanium extraction tailings have high hydration activity because the temperature in the whole process is low and the influence on the physical or chemical properties of the titanium extraction tailings is small.
Thirdly, the slag micro powder is prepared by thinning the dechlorinated titanium extraction tailings to a specific surface area of more than or equal to 400m 2/kg; and obtaining slag micro powder.
The slag micro powder has the requirement on granularity, so the titanium extraction tailings can be used as the slag micro powder after being refined.
Preferably, the method of refining is milling.
The grinding mode is preferred because the grinding mode is more suitable for large-scale equipment to carry out large-scale refining.
In a fourth aspect, the dechlorination titanium extraction tailings or the slag micro powder are applied to preparation of building materials.
The slag micro powder can be applied to the preparation of building materials, can reduce the cost of the building materials when being used as raw materials, and the building materials comprise cement or concrete.
In a fifth aspect, a construction material comprising the above dechlorinated titanium-extracted tailings or the above slag fine powder;
the building material containing the dechlorination titanium extraction tailings or the slag micro powder also has the advantages of low cost, low chlorine content and good hydration activity, and in addition, the building material has lower cost.
Preferably, the building material comprises cement or concrete.
The cement or concrete containing the dechlorination titanium extraction tailings or the slag micro powder has the same advantages as the dechlorination titanium extraction tailings or the slag micro powder and is low in cost because the dechlorination titanium extraction tailings or the slag micro powder are applied.
The invention is further illustrated by the following specific examples and comparative examples, but it should be understood that these examples are for purposes of illustration only and are not to be construed as limiting the invention in any way.
Example 1
And (3) mixing the titanium extraction tailings and water in a mass ratio of 1:3, pouring a mixture of the titanium extraction tailings and water into a high-pressure reaction kettle, wherein the mixture of the titanium extraction tailings and the water accounts for 65% of the total volume of the high-pressure reaction kettle, adjusting the stirring speed to 600r/min, heating, keeping the temperature of the high-pressure reaction kettle at 100 ℃, carrying out heat preservation for 30min, cooling to 25 ℃ to obtain a titanium extraction tailings turbid liquid, transferring the titanium extraction tailings turbid liquid to a plate-and-frame filter press for filter pressing, heating wet dechlorination titanium extraction tailings obtained after filter pressing to 100 ℃ in an oven, and drying for 60min to obtain dechlorinated titanium extraction tailings.
Example 2
Example 2 differs from example 1 only in that the incubation was carried out for 60 min.
Example 3
Example 3 differs from example 1 only in that the autoclave temperature was raised to 150 ℃.
Example 4
Example 4 differs from example 3 only in that the incubation time was 60 min.
Example 5
Example 5 differs from example 1 only in that the autoclave temperature was raised to 200 ℃.
Example 6
Example 6 differs from example 5 only in that the incubation was for 60 min.
Example 7
Example 7 differs from example 1 only in that the temperature is reduced to 50 ℃.
Example 8
Example 8 differs from example 1 only in the temperature rise to 200 ℃.
Example 9
Example 9 differs from example 1 only in that the incubation time was 120 min.
Example 10
Example 10 differs from example 1 only in that the mass ratio of titanium extraction tailings to water in the mixture of titanium extraction tailings and water is 1: 2.
Example 11
Example 11 differs from example 1 only in that the drying time was 40 min.
Example 2
Example 12 differs from example 1 only in that the titanium extraction tailings slurry after the water treatment is resuspended by stirring before the solid-liquid separation step.
Comparative example 1
Comparative example 2 differs from example 1 only in that the temperature increase is carried out in a non-closed reactor.
Comparative example 2
The comparative example 2 is different from the example 1 only in that the mass ratio of the titanium extraction tailings to the water in the mixture of the titanium extraction tailings and the water is 1: 1.
Test examples
The chlorine content of the dechlorinated titanium extraction tailings obtained in the embodiments 1 to 11 and the comparative examples 1 to 2 of the invention is detected according to an industry standard method of GB/T18046-2008 granulated blast furnace slag powder used in cement and concrete, and the detection result of the chlorine content is shown in the following table 1; then the dechlorinated titanium extraction tailings obtained in the examples 1 to 11 and the comparative examples 1 to 2 are thinned by a grinding mode until the specific surface area is more than or equal to 400m2And/kg, obtaining slag micro powder, detecting the slag micro powder according to an industrial standard method of GB/T18046-2008 'granulated blast furnace slag powder used in cement and concrete', wherein parameters such as density, fluidity ratio, water content, sulfur trioxide content, ignition loss, vitreous body content and the like all accord with industrial standards, and determining hydration activity indexes according to the standard method, wherein detection results are shown in Table 1 below.
TABLE 1 chlorine content of dechlorinated titanium extraction tailings obtained in examples and comparative examples and hydration activity index detection results of slag micro powder prepared from dechlorinated titanium extraction tailings obtained in examples and comparative examples
As can be seen from the test results of examples 1-2 in Table 1, the chlorine content of the dechlorinated titanium tailings obtained in examples 1-11 is low, and the hydration activity is high.
As can be seen from the detection results of the examples 1 to 11 and the detection results of the comparative examples 1 to 2 in the table 1, the dechlorinated titanium extraction tailings obtained by the method of the examples 1 to 11 have low chlorine content, and the slag micro powder obtained by refining has high hydration activity, so that the method is suitable for application in the preparation of building materials; the chlorine content of the dechlorinated titanium extraction tailings prepared in comparative examples 1-2 is too high to be applied to the preparation of building materials.
As can be seen from the comparison of the test results of example 7 and example 1 in Table 1, the effect of the temperature reduction on the chlorine content and the hydration activity is small.
As can be seen from the comparison of the detection results of the embodiment 8 and the embodiment 1 in the table 1, the temperature rise is high, the dechlorination effect is favorably improved, and the chlorine content of the dechlorinated titanium extraction tailings is lower.
As can be seen from the comparison of the detection results of the embodiment 9 and the embodiment 1 in the table 1, the insulation time has influence on the dechlorination effect, the longer the insulation time is, the dechlorination effect is favorably improved, and the chlorine content of the dechlorination titanium extraction tailings obtained after dechlorination is lower.
As can be seen from the comparison between the detection results of example 10 and example 1 in Table 1, the dechlorination effect can be improved by optimizing the ratio of the titanium extraction tailings to the water in the mixture of the titanium extraction tailings and the water.
As can be seen from the comparison of the results of example 11 and example 1 in Table 1, the drying time has little influence on the dechlorination effect and the hydration activity.
While particular embodiments of the present invention have been illustrated and described, it would be obvious that various other changes and modifications can be made without departing from the spirit and scope of the invention. It is therefore intended to cover in the appended claims all such changes and modifications that are within the scope of this invention.
Claims (32)
1. The dechlorination method of the titanium extraction tailings is characterized by comprising the following steps of:
in a closed container, heating the mixture of the titanium extraction tailings and water to 100-250 ℃, preserving the heat for 20-150min, and then cooling to obtain titanium extraction tailings turbid liquid;
the mass ratio of the titanium extraction tailings to the water in the mixture of the titanium extraction tailings and the water is 1: (2-5).
2. The dechlorination method of the titanium extraction tailings as claimed in claim 1, wherein the mixture of the titanium extraction tailings and water is heated to 100-220 ℃.
3. The dechlorination method of the titanium extraction tailings as claimed in claim 2, wherein the mixture of the titanium extraction tailings and water is heated to 100-200 ℃.
4. The dechlorination method of the titanium extraction tailings according to claim 1, wherein the mixture of the titanium extraction tailings and water is kept at the temperature for 30-130 min.
5. The dechlorination method of the titanium extraction tailings according to claim 1, characterized in that the mixture of the titanium extraction tailings and water is kept at the temperature for 30-120 min.
6. The dechlorination method of the titanium extraction tailings according to claim 1, wherein the temperature reduction treatment step is carried out at a temperature of 20 to 50 ℃.
7. The dechlorination method of the titanium extraction tailings according to claim 6, wherein the temperature reduction treatment step is carried out at a temperature of 20 to 30 ℃.
8. The process for dechlorinating titanium extraction tailings according to claim 1, wherein the total volume of the mixture of the titanium extraction tailings and water is 50-90% of the total volume of the closed vessel.
9. The process for dechlorinating titanium extraction tailings according to claim 8, wherein the total volume of the mixture of the titanium extraction tailings and water is 50-80% of the total volume of the closed vessel.
10. The dechlorination method of the titanium extraction tailings according to claim 1, wherein the mass ratio of the mixture of the titanium extraction tailings and the water in the mixture of the titanium extraction tailings and the water is 1: (3-4).
11. The dechlorination method of the titanium extraction tailings according to claim 10, wherein the mass ratio of the titanium extraction tailings to the water in the mixture of the titanium extraction tailings and the water is 1: 3.
12. The dechlorination method of titanium extraction tailings according to any one of claims 1 to 11, characterized in that the slurry of titanium extraction tailings is subjected to solid-liquid separation to obtain wet dechlorinated titanium extraction tailings.
13. The dechlorination method of titanium extraction tailings according to claim 12, wherein the solid-liquid separation mode comprises: filtration or centrifugation.
14. The dechlorination method of titanium extraction tailings according to claim 13, wherein the solid-liquid separation is filtration.
15. The dechlorination method of titanium extraction tailings according to claim 14, wherein the filtration method comprises suction filtration or pressure filtration.
16. The dechlorination method of titanium extraction tailings according to claim 15, wherein the filtration method is filter pressing.
17. The method for dechlorinating titanium extraction tailings of claim 13, wherein the method further comprises the step of drying the wet dechlorinated titanium extraction tailings to obtain dechlorinated titanium extraction tailings.
18. The dechlorination method of titanium extraction tailings according to claim 17, wherein the drying temperature is 80-200 ℃.
19. The dechlorination method of titanium extraction tailings as claimed in claim 18, wherein the drying temperature is 100-120 ℃.
20. The dechlorination method of titanium extraction tailings according to claim 19, wherein the drying temperature is 100 ℃.
21. The dechlorination method of titanium extraction tailings according to claim 17, wherein the drying time is 20-80 min.
22. The dechlorination method of titanium extraction tailings according to claim 21, wherein the drying time is 20-60 min.
23. The dechlorination method of titanium extraction tailings according to claim 22, wherein the drying time is 60 min.
24. The dechlorination method of titanium extraction tailings according to any of claims 1 to 11, further comprising the step of resuspending the titanium extraction tailings slurry after the cooling treatment.
25. The dechlorination method of titanium extraction tailings according to claim 24, wherein the resuspension method comprises stirring or shaking.
26. The method for dechlorinating the titanium extraction tailings according to claim 25, wherein the heavy suspension method is stirring.
27. Dechlorinated titanium extraction tailings prepared by a dechlorination method of the titanium extraction tailings of any one of claims 1 to 26.
28. Fine slag powder characterized by being obtained by refining the dechlorinated titanium-extraction tailings according to claim 27 to a specific surface area of not less than 400m2And/kg, obtaining slag micro powder.
29. Slag micropowder according to claim 28, characterized in that the refining process is pulverising.
30. Use of dechlorinated titanium tailings of claim 27 or slag fines of claim 28 or 29 in the production of building materials.
31. A building material comprising the dechlorinated titanium tailings of claim 27 or the micro slag powder of claim 28 or 29.
32. The building material of claim 31, wherein the building material comprises cement or concrete.
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