CN112759164A - Method for recycling waste slag water generated in dust collection of titanium dioxide by chlorination process - Google Patents
Method for recycling waste slag water generated in dust collection of titanium dioxide by chlorination process Download PDFInfo
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- CN112759164A CN112759164A CN202011639933.7A CN202011639933A CN112759164A CN 112759164 A CN112759164 A CN 112759164A CN 202011639933 A CN202011639933 A CN 202011639933A CN 112759164 A CN112759164 A CN 112759164A
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- titanium dioxide
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- wastewater
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 104
- 238000000034 method Methods 0.000 title claims abstract description 80
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 44
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 43
- 238000004064 recycling Methods 0.000 title claims abstract description 39
- 238000005660 chlorination reaction Methods 0.000 title claims abstract description 37
- 239000002699 waste material Substances 0.000 title claims abstract description 37
- 239000002893 slag Substances 0.000 title claims abstract description 26
- 239000000428 dust Substances 0.000 title claims abstract description 24
- 239000002351 wastewater Substances 0.000 claims abstract description 91
- 238000000926 separation method Methods 0.000 claims abstract description 42
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 39
- 238000011084 recovery Methods 0.000 claims abstract description 34
- 229910052751 metal Inorganic materials 0.000 claims abstract description 32
- 239000002184 metal Substances 0.000 claims abstract description 30
- 239000000126 substance Substances 0.000 claims abstract description 24
- 239000011780 sodium chloride Substances 0.000 claims abstract description 20
- 239000010936 titanium Substances 0.000 claims abstract description 13
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 12
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000011329 calcined coke Substances 0.000 claims abstract description 11
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 101
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 75
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 57
- 238000006243 chemical reaction Methods 0.000 claims description 41
- 239000006228 supernatant Substances 0.000 claims description 21
- 239000003054 catalyst Substances 0.000 claims description 20
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims description 19
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims description 19
- 238000001728 nano-filtration Methods 0.000 claims description 19
- 238000007885 magnetic separation Methods 0.000 claims description 13
- 238000007670 refining Methods 0.000 claims description 13
- 238000002425 crystallisation Methods 0.000 claims description 11
- 230000008025 crystallization Effects 0.000 claims description 11
- 239000012528 membrane Substances 0.000 claims description 11
- 238000010517 secondary reaction Methods 0.000 claims description 11
- 238000001914 filtration Methods 0.000 claims description 9
- 229910000000 metal hydroxide Inorganic materials 0.000 claims description 9
- 150000004692 metal hydroxides Chemical class 0.000 claims description 9
- 238000001704 evaporation Methods 0.000 claims description 8
- 230000008020 evaporation Effects 0.000 claims description 8
- 230000005484 gravity Effects 0.000 claims description 8
- 238000006460 hydrolysis reaction Methods 0.000 claims description 8
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 5
- 238000000108 ultra-filtration Methods 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 4
- 229910010270 TiOCl2 Inorganic materials 0.000 claims description 3
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 3
- 229960004887 ferric hydroxide Drugs 0.000 claims description 2
- IEECXTSVVFWGSE-UHFFFAOYSA-M iron(3+);oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Fe+3] IEECXTSVVFWGSE-UHFFFAOYSA-M 0.000 claims description 2
- 229910021506 iron(II) hydroxide Inorganic materials 0.000 claims description 2
- NCNCGGDMXMBVIA-UHFFFAOYSA-L iron(ii) hydroxide Chemical compound [OH-].[OH-].[Fe+2] NCNCGGDMXMBVIA-UHFFFAOYSA-L 0.000 claims description 2
- 230000001376 precipitating effect Effects 0.000 claims description 2
- 239000003513 alkali Substances 0.000 abstract description 9
- 229910052742 iron Inorganic materials 0.000 abstract description 8
- 150000003839 salts Chemical class 0.000 abstract description 8
- 230000008901 benefit Effects 0.000 abstract description 5
- 229910052749 magnesium Inorganic materials 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 3
- 239000010842 industrial wastewater Substances 0.000 abstract description 2
- 238000011144 upstream manufacturing Methods 0.000 abstract description 2
- 238000004065 wastewater treatment Methods 0.000 abstract description 2
- 230000007613 environmental effect Effects 0.000 abstract 1
- 235000010215 titanium dioxide Nutrition 0.000 description 30
- 239000000243 solution Substances 0.000 description 24
- 239000002244 precipitate Substances 0.000 description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 16
- 238000001035 drying Methods 0.000 description 14
- 239000007789 gas Substances 0.000 description 14
- -1 salt ions Chemical class 0.000 description 13
- 239000012266 salt solution Substances 0.000 description 10
- 239000000047 product Substances 0.000 description 9
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 8
- 239000012535 impurity Substances 0.000 description 7
- 238000010521 absorption reaction Methods 0.000 description 6
- 239000000706 filtrate Substances 0.000 description 6
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 5
- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical compound [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 description 5
- 229910001448 ferrous ion Inorganic materials 0.000 description 5
- 229910001425 magnesium ion Inorganic materials 0.000 description 5
- 229910001437 manganese ion Inorganic materials 0.000 description 5
- 239000000463 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
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 238000000605 extraction Methods 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 239000006004 Quartz sand Substances 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- RHZUVFJBSILHOK-UHFFFAOYSA-N anthracen-1-ylmethanolate Chemical compound C1=CC=C2C=C3C(C[O-])=CC=CC3=CC2=C1 RHZUVFJBSILHOK-UHFFFAOYSA-N 0.000 description 3
- 239000003830 anthracite Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000000571 coke Substances 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000006386 neutralization reaction Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 239000002910 solid waste Substances 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 1
- 240000007049 Juglans regia Species 0.000 description 1
- 235000009496 Juglans regia Nutrition 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 235000011941 Tilia x europaea Nutrition 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 239000001110 calcium chloride Substances 0.000 description 1
- 229910001628 calcium chloride Inorganic materials 0.000 description 1
- 150000001805 chlorine compounds Chemical class 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 239000004571 lime Substances 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
- 239000011707 mineral Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000010979 pH adjustment Methods 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000010802 sludge Substances 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 235000020234 walnut Nutrition 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F9/00—Multistage treatment of water, waste water or sewage
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B7/00—Halogens; Halogen acids
- C01B7/01—Chlorine; Hydrogen chloride
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/04—Chlorides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
- C01G23/0536—Producing by wet processes, e.g. hydrolysing titanium salts by hydrolysing chloride-containing salts
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/06—Ferric oxide [Fe2O3]
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/001—Processes for the treatment of water whereby the filtration technique is of importance
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
- C02F1/048—Purification of waste water by evaporation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
- C02F1/442—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by nanofiltration
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
- C02F1/444—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by ultrafiltration or microfiltration
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/58—Treatment of water, waste water, or sewage by removing specified dissolved compounds
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
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- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- Engineering & Computer Science (AREA)
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- General Life Sciences & Earth Sciences (AREA)
- Materials Engineering (AREA)
- Hydrology & Water Resources (AREA)
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- Treatment Of Water By Oxidation Or Reduction (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
- Removal Of Specific Substances (AREA)
Abstract
The invention belongs to the field of industrial wastewater treatment, and particularly relates to a method for recycling waste slag water generated in the process of titanium dioxide dust collection by a chlorination method, which realizes the separation and recovery of insoluble substances, namely high titanium slag and calcined coke in the waste slag water by the chlorination method and the control of the pH value of wastewater, separates Ti, Fe, Mg and other polyvalent metal salts in the waste slag water, converts the Ti, Fe, Mg and other polyvalent metal salts into respective oxides to be recovered, and finally purifies sodium chloride to be used as a raw material in the chlor-alkali industry to form an upstream and downstream circular economic industry chain with the chlor-alkali industry, thereby really realizing the zero emission and the complete recycling of the waste slag water generated in the chlorination process of titanium dioxide dust collection by the chlorination method, and having good environmental protection benefits.
Description
Technical Field
The invention belongs to the field of industrial wastewater treatment, and particularly relates to a method for recycling waste slag water generated by dust collection of titanium dioxide by a chlorination process.
Background
Titanium dioxide (TiO)2) The titanium dioxide is one of white raw materials with the best performance in the world, has extremely wide application in the fields of coating, plastic papermaking, humor, rubber, chemical fiber and the like, and the method for preparing the titanium dioxide in the prior art can be divided into a sulfuric acid method and a chlorination method, wherein the chlorination method has great advantages compared with the sulfuric acid method: advanced technology, short flow and few working procedures; the method is easy to realize continuity and automation, and the single set of device has large capacity and high labor productivity; less three wastes are discharged, the chlorine gas is recycled, and the three wastes pollution is less; the product has excellent quality, less impurities, uniform particle size, large decolorizing power, good dispersibility and good quality; low energy consumption, low production cost and good economic benefit.
The technological process of producing titanium white powder by chlorination process mainly includes three major steps of chlorination of titanium dioxide, oxidation of titanium tetrachloride and surface treatment of titanium dioxide, in which the preparation of titanium tetrachloride mostly adopts rutile ore, chlorine gas and coke are reacted at 1800 deg.C to produce titanium tetrachloride, the condensation point of titanium tetrachloride is very low, and the purification of titanium tetrachloride can be implemented by means of cooling, but because the rutile ore contains lots of metal elements of iron, magnesium and manganese, etc., the chlorides of these elements can be preferentially crystallized in the course of cooling, and can be fed into dust-collecting slag together with unreacted mineral powder and coke.
The prior art adopts the treatment method of dust-collecting slag to dissolve chloride in water slurry mixing, but the water quality of the slurry wastewater after the slurry mixing of the chlorination dust-collecting slag is treated by the dust-collecting slag is complex, and the treatment difficulty is higher. At present, the treatment of the waste water mainly comprises alkali adjustment and neutralization precipitation, for example, sodium hydroxide is used for alkali adjustment to finally treat the waste water into a sodium chloride product, lime is used for alkali adjustment to finally treat the waste water into a calcium chloride product, and ammonia water is used for alkali adjustment to finally treat the waste water into an ammonium chloride product. Although the method realizes reasonable treatment of the wastewater, the chemical washing sludge generated by the neutralization precipitation is not properly treated and comprehensively utilized, and a large amount of solid waste is generated, so that the resource waste and the treatment cost are increased.
Disclosure of Invention
The invention provides a method for recycling waste water generated by dust collection of titanium dioxide by a chlorination process, aiming at the technical problem of resource waste caused by a large amount of solid waste due to unreasonable treatment of the dust collection slag by the chlorination process in the prior art.
In order to achieve the purpose of the invention, the embodiment of the invention adopts the following technical scheme:
a method for recycling waste slag water generated in dust collection of titanium dioxide by a chlorination process comprises the following steps:
separating and recovering insoluble substances, and separating and recovering high titanium slag and calcined coke from the waste slag water to be treated through a first filtering device;
hydrogen chloride is recovered, and the wastewater after passing through the first filtering device enters a hydrochloric acid stripping tower to extract hydrogen chloride;
recovering titanium dioxide, wherein the effluent of the hydrochloric acid stripping tower enters a second separation device through a pipeline, the pH of the wastewater in the pipeline is adjusted to 4.2-4.8, and TiOCl2Hydrolysis to separate out TiO2TiO in waste water2Separating and recovering by a second separation device;
recycling ferric oxide, enabling effluent of the second separation device to enter a first-stage reaction tank, adjusting the pH of the first-stage reaction tank to 7-10, precipitating ferric hydroxide or ferrous hydroxide, separating by a third separation device, drying and roasting to obtain ferric oxide;
recovering the metal catalyst, wherein the supernatant of the primary reaction tank flows into the secondary reaction tank, the pH is adjusted to 10-12.5, and the metal hydroxide in the wastewater is completely precipitated, separated by a fourth separation device, dehydrated, molded and roasted to obtain the metal catalyst;
and (3) recovering sodium chloride, wherein the supernatant of the secondary reaction tank passes through a nanofiltration device, and after nanofiltration water production, the sodium chloride is recovered through an evaporation crystallization device.
Compared with the prior art: according to the invention, through the process design of the titanium dioxide waste residue water prepared by the chlorination method and the control of the pH value of the wastewater, the separation and recovery of insoluble substances, namely high titanium residue and calcined coke in the waste residue water are realized, the Ti element, the Fe element, the Mg element and other polyvalent metal salts in the wastewater are separated and converted into respective oxides to be recovered, the final product sodium chloride can be used as a raw material in the chlor-alkali industry after being purified, an upstream and downstream circular economic industry chain is formed with the chlor-alkali industry, the zero emission and all resource utilization of the dust collection waste residue water prepared in the chlorination process of titanium dioxide prepared by the chlorination method are really realized, and the environment-friendly benefit is good.
Preferably, the step of separating and recovering the insoluble substances further comprises the step of gravity separation of the high titanium slag and the calcined coke, and the separation step adopts gravity separation or manual separation.
Preferably, the steam required by the hydrochloric acid stripping tower is secondary steam generated by the evaporative crystallization device.
Preferably: and in the step of recovering titanium dioxide, the pH value is adjusted to 4.5-4.8 by using a sodium hydroxide solution with the mass concentration of 5-10%.
The proper concentration of the sodium hydroxide solution can realize the accurate regulation and control of the pH value of the wastewater and ensure the TiOCl2Hydrolysis to produce TiO2And simultaneously prevent other metal elements in the wastewater from generating hydroxide precipitates.
Preferably, in the step of recovering the iron oxide or the step of recovering the metal catalyst, a sodium hydroxide solution with a mass concentration of 30-50% or solid sodium hydroxide is used for adjusting the pH value.
The high-concentration sodium hydroxide solution or sodium hydroxide solid can adjust the pH of the waste liquid without introducing impurities, reduce the treatment capacity of the waste liquid as much as possible and reduce the treatment difficulty of the subsequent sodium chloride recovery process.
Preferably, the step of recovering the ferric oxide further comprises magnetic separation refining of the ferric oxide; wherein the oxides remaining after the refining are combined with the metal hydroxide in the metal catalyst recovery step for treatment.
Preferably, the concentrated solution produced by the nanofiltration device flows back to the primary reaction tank through a pipeline.
The concentrated solution contains residual high-valence metal salt ions and hydroxide ions, and can be used as an alkali liquor to regulate the pH value in the primary reaction tank and further recover the high-valence metal salt ions in the solution.
Preferably, the supernatant of the secondary reaction tank is filtered by a multi-medium filter, a cartridge filter or an ultrafiltration device before entering the nanofiltration device.
Preferably the packing of the multimedia filter is: at least two of quartz sand, active carbon, anthracite and walnut shells.
The preferable treatment liquid filtering device can remove residues and suspended matters in the supernatant of the secondary reaction tank, protect the nanofiltration device, prevent blockage and improve the ion exchange efficiency.
Drawings
FIG. 1 is a schematic process flow diagram of a method for recycling waste water generated in dust collection of titanium dioxide by a chlorination process in the embodiment of the invention.
In the figure:
s10-insoluble substance separation and recovery process, 11-first filtering device, 12-gravity sorting device, 13-filtrate buffer tank, S20-hydrochloric acid recovery process, 21-hydrochloric acid stripping tower, 22-hydrochloric acid absorption device, S30-titanium dioxide recovery process, S40-iron oxide recovery process, 41-first-stage reaction tank, 42-third separation device, 43-first drying device, 44-first roasting device, 45-magnetic separation device, S50-metal catalyst recovery process, 51-second-stage reaction tank, 52-fourth separation device, 53-second drying device, 54-forming device, 55-second roasting device, S60-sodium chloride recovery process, 61-nanofiltration device and 62-evaporative crystallization device.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Referring to fig. 1, a process flow of the method for recycling waste water generated by dust collection of titanium dioxide by a chlorination process provided by the invention will now be described. The process flow comprises the following steps: an insoluble matter separation and collection step S10, a hydrochloric acid collection step S20, a titanium dioxide collection step S30, an iron oxide collection step S40, a metal catalyst collection step S50, and a sodium chloride collection step S60.
S10, an insoluble substance separating and recycling process, wherein after insoluble substances in the waste residue water to be treated are separated by a first filtering device 11, the separation and recycling of high titanium slag and calcined coke which are main components in the insoluble substances are realized by a gravity separation device 12, and the waste water filtered by the first filtering device 11 flows into a filtrate buffer tank 13.
And S20, hydrogen chloride recovery, namely, feeding the wastewater filtered by the first filtering device 11 into a hydrochloric acid stripping tower 21, extracting part of hydrogen chloride gas in the wastewater, and feeding the hydrogen chloride gas into a hydrochloric acid absorption device 22 to obtain a dilute hydrochloric acid solution.
S30, titanium dioxide recovery process, wherein the waste water after hydrochloric acid stripping in the hydrochloric acid stripping tower 12 flows into the titanium dioxide recovery process 30 through a pipeline, sodium hydroxide is added into the material in the pipeline to adjust the pH value, so that TiOCl in the waste water2Hydrolysis to separate out TiO2The titanium dioxide is intercepted and recovered through a titanium dioxide recovery process 30;
s40, an iron oxide recovery process, namely, enabling the wastewater flowing out of the titanium dioxide recovery process 30 to enter a primary reaction tank 41, adding sodium hydroxide into the primary reaction tank 41 to adjust the pH value of the wastewater, converting iron ions and ferrous ions in the wastewater into hydroxide precipitates and separating out, separating the hydroxide precipitates through a third separation device 42, drying the hydroxide precipitates through a first drying device 43, roasting the dried precipitates in a first roasting device 44 to realize dehydration of the hydroxide to generate iron oxide, and refining the iron oxide through a magnetic separation device 45 to obtain high-purity iron oxide.
S50, recovering the metal catalyst, wherein the supernatant in the first-stage reaction tank 41 flows into the second-stage reaction tank 51, sodium hydroxide is added into the second-stage reaction tank 51 to adjust the pH value of the wastewater so as to completely precipitate high-valence metal impurities such as magnesium ions, manganese ions and the like in the wastewater, the wastewater is separated by a fourth separation device 52, dried by a second drying device 53 and mechanically formed by a forming device 54, and then is roasted by a second roasting device 55 to prepare a metal catalyst product, and the residual oxides in the magnetic separation device in S40 can be mixed with the dried metal hydroxide in the step to be treated.
And S60, sodium chloride recovery, wherein the supernatant of the secondary reaction tank 51 is subjected to pH adjustment and then flows into a nanofiltration device 61 through a pipeline to realize separation of monovalent salt and high-valence salt ions in the wastewater, and the separated high-valence salt solution flows back to the primary reaction tank 41 through a pipeline for circular treatment. The monovalent salt solution can be made into crude sodium chloride by the evaporation crystallization device 62, and the steam generated in the evaporation crystallization device 62 can be used as the stripping steam of the hydrochloric acid stripping tower 21 in the S20 process.
The following examples are given by way of illustration.
Example 1
A method for recycling waste residue water generated in dust collection of titanium dioxide by a chlorination process specifically comprises the following steps:
s10, an insoluble substance separating and recycling process, wherein after the insoluble substance in the waste residue water to be treated is separated by a filter press, the separation and recycling of the main components of high titanium slag and calcined coke in the insoluble substance are realized by a gravity separation device, and the waste water filtered by the filter press flows into a filtrate buffer pool.
And S20, hydrogen chloride recovery, namely, feeding the waste water filtered by the filter press into a hydrochloric acid stripping tower, extracting part of hydrogen chloride gas dissolved in the waste water, feeding the hydrogen chloride gas into a hydrochloric acid absorption device to obtain a dilute hydrochloric acid solution, wherein the extraction amount of hydrochloric acid is 1% of the water inflow of the hydrochloric acid stripping tower, and the heat for heating the waste water by the stripping tower is derived from the heat generated by the treatment of the tail gas of the rutile chlorination reaction.
S30, a titanium dioxide recovery process, wherein the waste water after hydrochloric acid stripping in the hydrochloric acid stripping tower flows into a tubular membrane filter through a pipeline, sodium hydroxide solution with the mass concentration of 5% is added into the material in the pipeline to adjust the pH value to 4.5, so that TiOCl in the waste water2Hydrolysis to separate out TiO2And (4) intercepting and recovering by a tubular membrane filter.
S40, an iron oxide recovery process, wherein the wastewater flowing out of the outlet of the tubular membrane filter enters a primary reaction tank, sodium hydroxide solution with the mass concentration of 30% is added into the primary reaction tank to adjust the pH value of the wastewater to 9, so that iron ions and ferrous ions in the wastewater are converted into hydroxide precipitate to be separated out, the hydroxide precipitate is separated and dried by a third separation device, the dried precipitate is roasted for 3 hours in a first roasting device at the temperature of 550 ℃, the hydroxide is dehydrated to generate iron oxide, and the iron oxide is refined by magnetic separation refining to obtain high-purity iron oxide.
S50, a metal catalyst recycling process, wherein the supernatant in the first-stage reaction tank flows into a second-stage reaction tank, sodium hydroxide solution with the mass concentration of 30% is added into the second-stage reaction tank to adjust the pH value of the wastewater to 11.5, so that high-valence metal impurities such as magnesium ions, manganese ions and the like in the wastewater are completely precipitated, the wastewater is separated by a fourth separating device and dried by a second drying device until the water content is 30%, the wastewater is mechanically formed and then roasted for 4 hours in a second roasting device at the temperature of 600 ℃ to prepare a metal catalyst product, and the residual oxide after magnetic separation and refining in S40 can be combined into the metal hydroxide after drying in the process.
And S60, sodium chloride recovery, wherein the supernatant of the secondary reaction tank flows into a nanofiltration device through a pipeline, the residue and suspended matters in the supernatant are removed by a multi-medium filter filled with activated carbon, quartz sand and anthracite, and then the supernatant flows into the nanofiltration device, so that the separation of monovalent salt and high-valence salt ions in the wastewater is realized, and the separated high-valence salt solution flows back to the primary reaction tank through the pipeline for circular treatment. The monovalent salt solution can be evaporated and crystallized to obtain crude sodium chloride, and the steam generated in the evaporation and crystallization can be used as the stripping steam of the hydrochloric acid stripping tower in the S20 process.
Example 2
A method for recycling waste residue water generated by dust collection of titanium dioxide by a chlorination process specifically comprises the following steps;
s10, an insoluble substance separating and recycling process, wherein after the insoluble substance in the waste residue water to be treated is separated by a filter press, the separation and recycling of the main components of high titanium slag and calcined coke in the insoluble substance are realized by a gravity separation device, and the waste water filtered by the filter press flows into a filtrate buffer pool.
And S20, hydrogen chloride recovery, wherein the wastewater filtered by the filter press enters a hydrochloric acid stripping tower, part of hydrogen chloride gas dissolved in the wastewater is extracted, the hydrogen chloride gas enters a hydrochloric acid absorption device to obtain a dilute hydrochloric acid solution, the extraction amount of the hydrochloric acid is 2% of the water inflow of the stripping tower, and the heat for heating the wastewater by the stripping tower is derived from the heat generated by the treatment of the tail gas of the rutile chlorination reaction.
S30, a titanium dioxide recovery process, wherein the waste water after hydrochloric acid stripping in the hydrochloric acid stripping tower flows into a tubular membrane filter through a pipeline, sodium hydroxide solution with the mass concentration of 10% is added into the material in the pipeline to adjust the pH value to 4.8, so that TiOCl in the waste water2Hydrolysis to separate out TiO2And is intercepted and recovered by a bag filter.
S40, an iron oxide recovery process, wherein the wastewater flowing out of the outlet of the tubular membrane filter enters a primary reaction tank, solid sodium hydroxide is added into the primary reaction tank to adjust the pH value of the wastewater to 9, so that iron ions and ferrous ions in the wastewater are converted into hydroxide precipitate, the hydroxide precipitate is separated out, the precipitate is separated, dried and dried by a third separation device and is roasted for 3 hours in a first roasting device at the temperature of 600 ℃, the hydroxide is dehydrated to generate iron oxide, and the iron oxide is refined by magnetic separation refining to obtain high-purity iron oxide.
S50, a metal catalyst recycling process, wherein the supernatant in the first-stage reaction tank flows into a second-stage reaction tank, a sodium hydroxide solution with the mass concentration of 40% is added into the second-stage reaction tank to adjust the pH value of the wastewater to 12, so that high-valence metal impurities such as magnesium ions and manganese ions in the wastewater are completely precipitated, the wastewater is separated by a fourth separating device and dried by a second drying device to the water content of 35%, the wastewater is mechanically formed and then roasted for 4.5 hours in a roasting device at the temperature of 650 ℃ to obtain a metal catalyst product, and the residual oxides after magnetic separation and refining in S40 can be combined into the metal hydroxide after drying in the process.
And S60, sodium chloride recovery, wherein the supernatant of the secondary reaction tank flows into a nanofiltration device through a pipeline, the residue and suspended matters in the supernatant are removed by a security filter and then flow into the nanofiltration device, the pH is adjusted to 9, the separation of monovalent salt and high-valence salt ions in the wastewater is realized, and the separated high-valence salt solution flows back to the primary reaction tank through a pipeline for circular treatment. The monovalent salt solution can be evaporated and crystallized to obtain crude sodium chloride, and the steam generated in the evaporation and crystallization can be used as the stripping steam of the hydrochloric acid stripping tower in the step S20.
Example 3
A method for recycling waste residue water generated by dust collection of titanium dioxide by a chlorination process specifically comprises the following steps;
s10, an insoluble substance separating and recycling process, wherein after the insoluble substance in the waste residue water to be treated is separated by a filter press, the separation and recycling of the main components of high titanium slag and calcined coke in the insoluble substance are realized by a gravity separation device, and the waste water filtered by the filter press flows into a filtrate buffer pool.
And S20, hydrogen chloride recovery, wherein the wastewater filtered by the filter press enters a hydrochloric acid stripping tower, part of hydrogen chloride gas dissolved in the wastewater is extracted, the hydrogen chloride gas enters a hydrochloric acid absorption device to obtain a dilute hydrochloric acid solution, the extraction amount of the hydrochloric acid is 1% of the water inflow of the stripping tower, and the heat for heating the wastewater by the stripping tower is derived from the heat generated by the treatment of the tail gas of the rutile chlorination reaction.
S30, a titanium dioxide recovery process, wherein the waste water after hydrochloric acid stripping in the hydrochloric acid stripping tower flows into a tubular membrane filter through a pipeline, sodium hydroxide solution with the mass concentration of 7% is added into the material in the pipeline to adjust the pH value to 5, and TiOCl in the waste water is enabled to be2Hydrolysis to separate out TiO2Formed TiO2The coal is separated and recovered by a multi-medium filter filled with active carbon, quartz sand and anthracite.
S40, an iron oxide recovery process, wherein the wastewater flowing out of the outlet of the tubular membrane filter enters a primary reaction tank, a sodium hydroxide solution with the mass concentration of 40% is added into the primary reaction tank to adjust the pH value of the wastewater to 10, so that iron ions and ferrous ions in the wastewater are converted into hydroxide precipitates and separated out, the precipitates are separated, dried and dried by a third separation device and roasted for 3 hours in a first roasting device at 550 ℃, the hydroxide is dehydrated to generate iron oxide, and the iron oxide is refined by magnetic separation refining to obtain high-purity iron oxide.
S50, a metal catalyst recycling process, wherein the supernatant in the first-stage reaction tank flows into a second-stage reaction tank, a sodium hydroxide solution with the mass concentration of 50% is added into the second-stage reaction tank to adjust the pH value of the wastewater to 12, so that high-valence metal impurities such as magnesium ions and manganese ions in the wastewater are completely precipitated, the wastewater is separated by a fourth separating device and dried by a second drying device to the water content of 30%, the wastewater is mechanically formed and then roasted for 4 hours in a second roasting device at the temperature of 600 ℃ to prepare a metal catalyst product, and the residual oxides after magnetic separation and refining in S40 can be combined into the metal hydroxide after drying in the process.
And S60, sodium chloride recovery, wherein the supernatant of the secondary reaction tank flows into a nanofiltration device through a pipeline, the residue and suspended matters in the supernatant are removed through an ultrafiltration filter and then flow into the nanofiltration device, the pH is adjusted to 9, the separation of monovalent salt and high-valence salt ions in the wastewater is realized, and the separated high-valence salt solution flows back to the primary reaction tank through a pipeline for recycling treatment. The monovalent salt solution can be evaporated and crystallized to obtain crude sodium chloride, and the steam generated in the evaporation and crystallization can be used as the stripping steam of the hydrochloric acid stripping tower in the step S20.
Example 4
A method for recycling waste residue water generated by dust collection of titanium dioxide by a chlorination process specifically comprises the following steps;
s10, an insoluble substance separating and recycling process, wherein after the insoluble substance in the waste residue water to be treated is separated by a filter press, the separation and recycling of the main components of high titanium slag and calcined coke in the insoluble substance are realized by a gravity separation device, and the waste water filtered by the filter press flows into a filtrate buffer pool.
And S20, hydrogen chloride recovery, wherein the wastewater filtered by the filter press enters a hydrochloric acid stripping tower, part of hydrogen chloride gas dissolved in the wastewater is extracted, the hydrogen chloride gas enters a hydrochloric acid absorption device to obtain a dilute hydrochloric acid solution, the extraction amount of the hydrochloric acid is 2% of the water inflow of the stripping tower, and the heat for heating the wastewater by the stripping tower is derived from the heat generated by the treatment of the tail gas of the rutile chlorination reaction.
S30, titanium dioxide recovery process, wherein the waste water after hydrochloric acid stripping in the hydrochloric acid stripping tower flows into a tubular membrane filter through a pipeline, and sodium hydroxide with the mass concentration of 5% is added into the materials in the pipelineThe pH of the solution is adjusted to 4.6, so that the TiOCl in the wastewater is adjusted2Hydrolysis to separate out TiO2Formed TiO2Separating with bag filter, and recovering.
S40, an iron oxide recovery process, wherein the wastewater flowing out of the outlet of the tubular membrane filter enters a primary reaction tank, sodium hydroxide solution with the mass concentration of 30% is added into the primary reaction tank to adjust the pH value of the wastewater to 9, so that iron ions and ferrous ions in the wastewater are converted into hydroxide precipitate, the hydroxide precipitate is separated out, the precipitate is separated, dried and dried by a third separation device and is roasted for 3 hours in a first roasting device at the temperature of 550 ℃, the hydroxide is dehydrated to generate iron oxide, and the iron oxide is refined by magnetic separation refining to obtain high-purity iron oxide.
S50, a metal catalyst recycling process, wherein the supernatant in the first-stage reaction tank flows into a second-stage reaction tank, a sodium hydroxide solution with the mass concentration of 40% is added into the second-stage reaction tank to adjust the pH value of the wastewater to 11, so that high-valence metal impurities such as magnesium ions and manganese ions in the wastewater are completely precipitated, the wastewater is separated by a fourth separating device and dried by a second drying device to the water content of 30%, the wastewater is mechanically formed and then roasted for 4 hours in a second roasting device at the temperature of 600 ℃ to prepare a metal catalyst product, and the residual oxides after magnetic separation and refining in S40 can be combined into the metal hydroxide after drying in the process.
And S60, sodium chloride recovery, wherein the supernatant of the secondary reaction tank flows into a nanofiltration device through a pipeline, the residue and suspended matters in the supernatant are removed by an ultrafiltration device and then flow into the nanofiltration device, the pH is adjusted to 9.3, the separation of monovalent salt and high-valence salt ions in the wastewater is realized, and the separated high-valence salt solution flows back to the primary reaction tank through a pipeline for circular treatment. The monovalent salt solution can be evaporated and crystallized to obtain crude sodium chloride, and the steam generated in the evaporation and crystallization can be used as the stripping steam of the hydrochloric acid stripping tower in the step S20.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents or improvements made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (9)
1. A method for recycling waste slag water generated in dust collection of titanium dioxide by a chlorination process is characterized by comprising the following steps:
separating and recovering insoluble substances, and separating and recovering high titanium slag and calcined coke from the waste slag water to be treated through a first filtering device;
hydrogen chloride is recovered, and the wastewater after passing through the first filtering device enters a hydrochloric acid stripping tower to extract hydrogen chloride;
recovering titanium dioxide, wherein the effluent of the hydrochloric acid stripping tower enters a second separation device through a pipeline, the pH of the wastewater in the pipeline is adjusted to 4.2-4.8, and TiOCl2Hydrolysis to separate out TiO2TiO in waste water2Separating and recovering by a second separation device;
recycling ferric oxide, enabling the effluent of the second separation device to enter a first-stage reaction tank, adjusting the pH of the first-stage reaction tank to 7-10, precipitating ferric hydroxide or ferrous hydroxide, separating by a third separation device, dehydrating and roasting to obtain ferric oxide;
recovering the metal catalyst, wherein the supernatant of the primary reaction tank flows into the secondary reaction tank, the pH is adjusted to 10-12.5, and the metal hydroxide in the wastewater is completely precipitated, separated by a fourth separation device, dried, molded and roasted to obtain the metal catalyst;
and (3) recovering sodium chloride, wherein the supernatant of the secondary reaction tank passes through a nanofiltration device, and after nanofiltration water production, the sodium chloride is recovered through an evaporation crystallization device.
2. The method for recycling water from waste residues generated in dust collection of titanium dioxide by a chlorination process according to claim 1, wherein the steps of separating and recovering the insoluble substances further comprise the step of sorting the high titanium slag and calcined coke, and the sorting step adopts gravity sorting or manual sorting.
3. The method for recycling waste residue water generated in dust collection of titanium dioxide production by chlorination process according to claim 1, wherein the steam required by the hydrochloric acid stripping tower is secondary steam of the evaporative crystallization device.
4. The method for recycling the titanium dioxide dust collection waste residue water by the chlorination process according to claim 1, wherein in the titanium dioxide recovery step, the pH is adjusted to 4.5-4.8 by using a sodium hydroxide solution with a mass concentration of 5-10%.
5. The method for recycling waste residue water generated in dust collection of titanium dioxide production by chlorination process according to claim 1 or 4, wherein the second separation device is a tubular membrane, a bag filter, an ultrafiltration membrane or a multi-media filter.
6. The method for recycling water from titanium dioxide dust collection waste residues produced by a chlorination process according to claim 1, wherein in the step of recovering iron oxide or the step of recovering the metal catalyst, a sodium hydroxide solution with a mass concentration of 30-50% or solid sodium hydroxide is used for adjusting the pH value.
7. The method for recycling the waste residue water generated in the dust collection of titanium dioxide by the chlorination process according to claim 6, wherein the step of recovering the iron oxide further comprises magnetic separation and refining of the iron oxide; wherein the oxide remaining after the refining is combined with the metal hydroxide in the step of recovering the metal catalyst.
8. The method for recycling waste residue water generated in dust collection of titanium dioxide by a chlorination process according to claim 1, wherein concentrated solution generated by the nanofiltration device flows back to the primary reaction tank through a pipeline.
9. The method for recycling waste residue water generated in dust collection of titanium dioxide by a chlorination process according to claim 1, wherein the waste water is further filtered by a multi-media filter, a security filter or an ultrafiltration device before entering the nanofiltration device.
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