CN116002750A - TiO (titanium dioxide) recovery by leaching of fused salt chloride slag 2 Is a method of (2) - Google Patents
TiO (titanium dioxide) recovery by leaching of fused salt chloride slag 2 Is a method of (2) Download PDFInfo
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- CN116002750A CN116002750A CN202211692489.4A CN202211692489A CN116002750A CN 116002750 A CN116002750 A CN 116002750A CN 202211692489 A CN202211692489 A CN 202211692489A CN 116002750 A CN116002750 A CN 116002750A
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- tio
- salt chloride
- chloride slag
- molten salt
- leaching
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- 239000002893 slag Substances 0.000 title claims abstract description 64
- -1 salt chloride Chemical class 0.000 title claims abstract description 55
- 238000000034 method Methods 0.000 title claims abstract description 43
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 238000002386 leaching Methods 0.000 title claims abstract description 19
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 11
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 5
- 238000011084 recovery Methods 0.000 title claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 35
- 238000001354 calcination Methods 0.000 claims abstract description 28
- 229910010413 TiO 2 Inorganic materials 0.000 claims abstract description 18
- 239000012065 filter cake Substances 0.000 claims abstract description 15
- 238000004064 recycling Methods 0.000 claims abstract description 15
- 238000005406 washing Methods 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 9
- 239000012141 concentrate Substances 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims abstract description 8
- 238000000926 separation method Methods 0.000 claims abstract description 6
- 239000007788 liquid Substances 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 239000008399 tap water Substances 0.000 claims description 5
- 235000020679 tap water Nutrition 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 abstract description 13
- 239000010936 titanium Substances 0.000 abstract description 12
- 229910052719 titanium Inorganic materials 0.000 abstract description 12
- 150000003839 salts Chemical class 0.000 abstract description 7
- 239000002699 waste material Substances 0.000 abstract description 6
- 238000005660 chlorination reaction Methods 0.000 abstract description 3
- 229910004298 SiO 2 Inorganic materials 0.000 description 9
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 9
- 239000000203 mixture Substances 0.000 description 9
- 238000004090 dissolution Methods 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 239000011780 sodium chloride Substances 0.000 description 4
- 238000005265 energy consumption Methods 0.000 description 3
- 235000010215 titanium dioxide Nutrition 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 229910052681 coesite Inorganic materials 0.000 description 2
- 229910052906 cristobalite Inorganic materials 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- 229910052682 stishovite Inorganic materials 0.000 description 2
- 229910052905 tridymite Inorganic materials 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 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
- 239000006227 byproduct Substances 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- XENVCRGQTABGKY-ZHACJKMWSA-N chlorohydrin Chemical compound CC#CC#CC#CC#C\C=C\C(Cl)CO XENVCRGQTABGKY-ZHACJKMWSA-N 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000013505 freshwater Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
Classifications
-
- 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
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Landscapes
- Manufacture And Refinement Of Metals (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The invention belongs to the technical field of metallurgical harmful waste residue resource recycling, and particularly discloses a method for leaching and recycling TiO (titanium dioxide) from molten salt chloride residues 2 Is a method of (2). The method comprises the following steps: step 1: mixing molten salt chloride slag with water, fully stirring and dissolving, and carrying out solid-liquid separation to obtain filter residues; step 2: washing and drying the filter residues obtained in the step 1 to obtain a dried filter cake; step 3: calcining the dried filter cake obtained in the step 2 to obtain calcined residues; step 4: reselecting the calcined residue obtained in the step 3 to obtain TiO 2 Concentrate. By adopting the method provided by the invention, unreacted titanium-rich ore in the molten salt chlorination process can be recovered, the utilization rate of titanium-rich ore can be improved, and the waste of resources is reduced.
Description
Technical Field
The invention belongs to the technical field of metallurgical harmful waste residue resource recycling, and in particular relates to a method for leaching and recycling TiO (titanium dioxide) from molten salt chloride residues 2 Is a method of (2).
Background
At present, the titanium sponge is produced by a molten salt chlorination method in the metallurgical industry, and a large amount of molten salt is inevitably produced by the production methodSalt-chlorinated slag, which is often accompanied by a large amount of unreacted TiO 2 Typically these unreacted utilized TiO 2 Often together with other impurities of the fused salt chlorinated slag, is discarded from the slag field. This not only causes the waste of resources of high titanium slag, but also pollutes the environment.
In view of the above, there is provided a method for recovering TiO from molten salt chloride slag 2 The method of (2) is urgent.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a method for leaching and recycling TiO from fused salt chloride slag 2 According to the method, unreacted titanium-rich ore in the fused salt chloride slag can be recovered, and the recovered titanium-rich slag can be returned to the furnace for use, so that the waste of high titanium slag is reduced, and the utilization rate of fused salt chloride to the high titanium slag is improved.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
according to the invention, a method for leaching and recycling TiO from fused salt chloride slag is provided 2 Comprising the steps of: step 1: mixing molten salt chloride slag with water, fully stirring and dissolving, and carrying out solid-liquid separation to obtain filter residues; step 2: washing and drying the filter residues obtained in the step 1 to obtain a dried filter cake; step 3: calcining the dried filter cake obtained in the step 2 to obtain calcined residues; step 4: reselecting the calcined residue obtained in the step 3 to obtain TiO 2 Concentrate.
According to one embodiment of the present invention, in step 1, the molten salt chloride slag is subjected to a crushing treatment before the molten salt chloride slag is mixed with water.
According to one embodiment of the invention, the molten salt chloride slag is crushed to a diameter of 3cm or less.
According to one embodiment of the invention, in the step 1, when the molten salt chloride slag is mixed with water, the mass ratio of the molten salt chloride slag to the water is 1:1-5.
According to one embodiment of the invention, in the step 1, the molten salt chloride slag is stirred and dissolved in water for more than or equal to 2 hours.
According to one embodiment of the invention, in step 2, the filter residue obtained in step 1 is subjected to multistage countercurrent washing by adopting deionized water or tap water.
According to one embodiment of the invention, the amount of wash water is 3-6 times the mass of the filter residue.
According to one embodiment of the invention, in step 2, the filter residue obtained in step 1 is washed to Cl in the filter residue - And drying when the percentage content is less than or equal to 0.3 percent.
According to one embodiment of the invention, in step 3, the calcination temperature is 400-1000 ℃ and the calcination time is 4-16 h.
According to one embodiment of the invention, in step 3, the calcination temperature is 400-600 ℃ and the calcination time is 6-8 hours.
By adopting the technical scheme, the invention has the following beneficial effects:
TiO is recovered by leaching the fused salt chloride slag provided by the invention 2 According to the method, unreacted titanium-rich ore in the molten salt chlorination process can be recovered, so that the utilization rate of the titanium-rich ore can be improved, and the waste of resources is reduced. In addition, the invention provides the method for leaching and recycling TiO from the fused salt chloride slag 2 The method has simple and convenient process and is easy to realize.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
As required, detailed embodiments of the present invention are disclosed in the present specification; however, it is to be understood that the embodiments disclosed herein are merely exemplary of the invention that may be embodied in various and alternative forms. In the following description, a number of operating parameters and components are described in terms of various embodiments contemplated. These specific parameters and components are presented as examples and are not meant to be limiting.
The invention provides a method for leaching and recycling TiO from fused salt chloride slag 2 Comprising the steps of: step 1: mixing molten salt chloride slag with water, stirring and dissolving, and separating solid from liquid to obtainFiltering residues; step 2: washing and drying the filter residues obtained in the step 1 to obtain a dried filter cake; step 3: calcining the dried filter cake obtained in the step 2 to obtain calcined residues; step 4: reselecting the calcined residue obtained in the step 3 to obtain TiO 2 Concentrate.
The fused salt chloride slag adopted by the invention is a common byproduct in the titanium white industry and contains NaCl and FeCl 2 、FeCl 3、 MgCl 2、 MnCl 2 、CaCl 2、 AlCl 3、 TiO 2 SiO2, C, etc. In the method, the fused salt chloride slag is mixed with water and fully stirred, so that NaCl and FeCl which are easy to dissolve in water are obtained 2 、FeCl 3、 MgCl 2、 MnCl 2 、CaCl 2、 AlCl 3 Is dissolved in water, naCl and FeCl which are easy to dissolve in water are separated by solid-liquid separation 2 、FeCl 3、 MgCl 2、 MnCl 2 、CaCl 2、 AlCl 3 And TiO which enters the filtrate but is not easily dissolved in water 2 The SiO2, the C and the like enter filter residues, thereby realizing NaCl and FeCl 2 、FeCl 3、 MgCl 2、 MnCl 2 、CaCl 2、 AlCl 3 Equivalent to TiO 2 、SiO 2 Separation of C and the like; by mixing TiO-containing materials 2 、SiO 2 Washing and drying the filter residues of C and the like to remove redundant Cl in the filter residues - The main component of the obtained baking filter cake is SiO 2 、C、TiO 2 A small amount of alumina; the C in the dried filter cake is removed by calcining, and the main component of the obtained calcined residue is SiO 2 、TiO 2 The method comprises the steps of carrying out a first treatment on the surface of the By reselecting the calcination residues, siO is realized 2 With TiO 2 Is separated to obtain TiO 2 Concentrate.
In some cases, in step 1 of the method, before the molten salt chloride slag is mixed with water, the molten salt chloride slag is crushed, which is beneficial to increasing the specific surface area of the molten salt chloride slag and improving the dissolution efficiency. In some embodiments, the fused salt chloride slag is crushed to a diameter less than or equal to 3cm, and the dissolving efficiency and the energy consumption sum of the fused salt chloride slag in the particle size range are obviously better than those of the fused salt chloride slag with other particle sizes.
In the step 1 of the method, when the fused salt chloride slag is mixed with water, the mass ratio of the fused salt chloride slag to the water is 1:1-5. That is, if the molten salt is 1kg of the slag chloride, the required water is 1 to 5kg (i.e., 1 to 5L). Specifically, the mass ratio of molten salt chloride slag to water may be 1:1, 1:2, 1:3, 1:4, 1:5. Compared with other ranges, the mass ratio of the fused salt chloride slag to water can obviously improve the dissolution efficiency of sodium, iron, manganese, magnesium and calcium in the fused salt chloride slag, and simultaneously save energy consumption. Preferably, the mass ratio of the fused salt chloride slag to the water is 1:2.
In step 1 of the method, in order to ensure that the fused salt chloride slag is fully dissolved, the fused salt chloride slag is stirred in water for more than or equal to 2 hours. Specifically, the stirring dissolution time may be 2 hours, 3 hours, 4 hours, or the like. In the present invention, the rotation speed of stirring is not particularly limited, and may be selected by those skilled in the art according to actual needs. The stirring dissolution time provided by the application can improve the dissolution efficiency and save the energy consumption.
In the step 2 of the method, deionized water or tap water is adopted to wash the filter residue obtained in the step 1, and the washing water quantity is about 3-6 times of the mass (dry basis) of the filter residue. Specifically, the amount of wash water may be about 3 times, 4 times, 5 times, 6 times the mass (dry basis) of the filter residue. Preferably, the amount of wash water may be about 4 times the mass (dry basis) of the filter residue. In the washing process, a multi-stage countercurrent washing mode can be adopted to reduce the consumption of new water. For example, a three-stage countercurrent washing mode can be adopted. To ensure that the consumption of fresh water is reduced, cl is washed into filter residues - After the content of the percent (dry basis) is less than or equal to 0.3 percent, the method can carry out filter pressing and drying to obtain a dried filter cake. Preferably, it can be washed into the filter residue Cl - And (3) after the content of the (dry basis) is 0.16-0.27%, performing filter pressing and drying.
In step 3 of the method, the dried filter cake is put into a muffle furnace for calcination, the calcination temperature is 400-1000 ℃, and the calcination time is 4-16 h. Preferably, the calcination temperature is 400-600 ℃ and the calcination time is 6-8 h. Specifically, the calcination temperature may be 400 ℃, 450 ℃, 500 ℃, 550 ℃, 600 ℃, and the calcination time may be 6h, 6.5h, 7h, 7.5h, 8h. In some cases, the dried filter cake is ground prior to calcination to facilitate adequate removal of C therein during calcination.
In step 4 of the method of the invention, the calcination residue obtained in step 3 is subjected to reselection in a shaking table. In some cases, the calcination residues are ground before being fed into the shaker to facilitate adequate separation of SiO 2 With TiO 2 。
The present invention will be specifically described with reference to the following examples. It should be noted that these examples are merely illustrative and do not limit the invention in any way.
The composition of a typical molten salt chloride slag is shown in table 1. The content of each component fluctuates depending on the production conditions. The invention is given by taking the example as the following to leach and recycle TiO from the fused salt chloride slag 2 By way of introduction, the scope of applicability of the present invention includes, but is not limited to, the compositions of Table 1.
TABLE 1 fused salt chlorohydrin composition (content%)
| NaCl | FeCl 2 | FeCl 3 | MgCl 2 | MnCl 2 | CaCl 2 | AlCl 3 | TiO 2 | SiO 2 | C | Others |
| 30.8 | 16.1 | 1.9 | 25.6 | 2.7 | 2.2 | 3.0 | 4.7 | 6.5 | 4.5 | 2.0 |
Example 1
2 kg of fused salt chloride slag (the components are shown in the table 1), crushing (the slag diameter is less than or equal to 2.5 cm), adding 2L of deionized water, stirring, dissolving for 2 hours, and filtering to obtain filter slag. 800mL of tap water is equally divided into three parts, each part of tap water is repeatedly washed for a plurality of times, filter residues are pressed and air-dried, 352.4g of dried filter cakes are obtained, and Cl of the dry basis of the filter cakes is measured - The content was 0.247% (the composition of the dried cake is shown in Table 2). 350g of the dried cake was taken, ground and placed in a muffle furnace, the calcination temperature was set at 600℃and the calcination time was 6 hours, and 221.2g of residue (the residue composition is shown in Table 3) was finally obtained. Grinding the calcined residue again, and sending into a shaking table for reselection to obtain TiO 2 Titanium concentrate with a content of 52.4% (titanium concentrate composition see table 4).
TABLE 2 oven dried cake composition (content%)
| TiO 2 | SiO 2 | C | Others |
| 27.12 | 36.10 | 33.89 | 2.89 |
TABLE 3 residue composition after calcination (content%)
| TiO 2 | SiO 2 | C | Others |
| 39.21 | 54.13 | 2.1 | 4.56 |
TABLE 4 titanium concentrate composition (content%)
| TiO 2 | SiO 2 | C | Others |
| 52.4 | 38.36 | 0.61 | 8.63 |
Claims (10)
1. TiO (titanium dioxide) recovery by leaching of fused salt chloride slag 2 Is characterized by comprising the following steps:
step 1: mixing molten salt chloride slag with water, fully stirring and dissolving, and carrying out solid-liquid separation to obtain filter residues;
step 2: washing and drying the filter residues obtained in the step 1 to obtain a dried filter cake;
step 3: calcining the dried filter cake obtained in the step 2 to obtain calcined residues;
step 4: reselecting the calcined residue obtained in the step 3 to obtain TiO 2 Concentrate.
2. The method for leaching and recycling TiO from molten salt chloride slag according to claim 1 2 In the step 1, before the molten salt chloride slag is mixed with water, the molten salt chloride slag is brokenAnd (5) crushing.
3. The molten salt chloride slag leaching recovery TiO of claim 2 2 The method is characterized in that the fused salt chloride slag is crushed until the diameter is less than or equal to 3cm.
4. The method for leaching and recycling TiO from molten salt chloride slag according to claim 1 2 The method is characterized in that in the step 1, when the fused salt chloride slag is mixed with water, the mass ratio of the fused salt chloride slag to the water is 1:1-5.
5. The method for leaching and recycling TiO from molten salt chloride slag according to claim 1 2 The method is characterized in that in the step 1, the molten salt chloride slag is stirred and dissolved in water for more than or equal to 2 hours.
6. The method for leaching and recycling TiO from molten salt chloride slag according to claim 1 2 In the step 2, deionized water or tap water is adopted to carry out multistage countercurrent washing on the filter residue obtained in the step 1.
7. The method for leaching and recycling TiO from molten salt chloride slag according to claim 6 2 The method is characterized in that the washing water quantity is 3-6 times of the quality of filter residues.
8. The method for leaching and recycling TiO from molten salt chloride slag according to claim 1 2 The method is characterized in that in the step 2, the filter residue obtained in the step 1 is washed to Cl in the filter residue - And drying when the percentage content is less than or equal to 0.3 percent.
9. The method for leaching and recycling TiO from molten salt chloride slag according to claim 1 2 The method is characterized in that in the step 3, the calcination temperature is 400-1000 ℃ and the calcination time is 4-16 h.
10. The molten salt chloride slag leaching recovery TiO of claim 9 2 Is characterized in that in step 3, calcination is performedThe temperature is 400-600 ℃, and the calcination time is 6-8 h.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN118142513A (en) * | 2024-05-09 | 2024-06-07 | 成都先进金属材料产业技术研究院股份有限公司 | Molten salt chloride slag resource utilization method, denitration catalyst and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN118142513A (en) * | 2024-05-09 | 2024-06-07 | 成都先进金属材料产业技术研究院股份有限公司 | Molten salt chloride slag resource utilization method, denitration catalyst and preparation method thereof |
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