CN214115239U - Titanium white powder dust collection waste residue water resourceful treatment system by chlorination process - Google Patents
Titanium white powder dust collection waste residue water resourceful treatment system by chlorination process Download PDFInfo
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- CN214115239U CN214115239U CN202023335269.5U CN202023335269U CN214115239U CN 214115239 U CN214115239 U CN 214115239U CN 202023335269 U CN202023335269 U CN 202023335269U CN 214115239 U CN214115239 U CN 214115239U
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Abstract
The utility model provides a titanium white powder dust collection waste residue water resourceful treatment system of chlorination method, include that insoluble substance separating element, hydrochloric acid strip unit, titanium dioxide recovery unit, iron oxide recovery unit, metal catalyst recovery unit and sodium chloride recovery unit that set gradually according to the technology step. The titanium dioxide dust-collecting waste residue water recycling treatment system adopting the chlorination method is used for recycling the multivalent metal salt in the waste water respectively by aiming at different impurities and adopting different principles and selecting a multi-stage treatment device, and the obtained metal oxide can be applied to a plurality of technical fields, especially can be used as a raw material of a chlor-alkali enterprise after the final product sodium chloride is purified and forms an upstream and downstream circular economy industrial chain with the chlor-alkali enterprise. The utility model discloses a to recovery and resource utilization of chlorination legal system titanium white powder waste residue aquatic all impurity that gathers dust, the zero release of the sediment waste water that gathers dust that the chlorination process of titanium white powder preparation produced has very strong environmental protection benefit.
Description
Technical Field
The utility model belongs to the industrial wastewater treatment field especially relates to a titanium white powder dust collection waste residue water resourceful treatment system of chlorination legal system.
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, printing ink, 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, and 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 titanium tetrachloride preparation, titanium tetrachloride oxidation and titanium dioxide surface treatment, wherein, the titanium tetrachloride preparation mostly adopts rutile ore, chlorine and coke to react at 1800 ℃ to generate titanium tetrachloride, the condensation point of titanium tetrachloride is very low, the purification of titanium tetrachloride can be realized by cooling, but because the rutile ore contains a large amount of metal elements such as iron, magnesium, manganese and the like, the chlorides of the elements can be preferentially crystallized in the cooling process, and enter 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 wastewater mainly comprises alkali adjustment and neutralization precipitation, for example, the alkali adjustment is carried out by using sodium hydroxide to finally treat the wastewater into a sodium chloride product, the alkali adjustment is carried out by using lime to finally treat the wastewater into a calcium chloride product, and the alkali adjustment is carried out by using ammonia water to finally treat the wastewater into an ammonium chloride product. Although the method realizes reasonable treatment of the wastewater, a large amount of chemical washing sludge is generated by neutralization and precipitation, and the chemical washing sludge cannot be properly treated and comprehensively utilized and finally becomes solid waste, so that resource waste and treatment cost are increased.
SUMMERY OF THE UTILITY MODEL
The embodiment of the utility model provides a technical problem that solves provides a chlorination legal system titanium white powder waste residue water resourceful treatment system that gathers dust, aims at solving among the prior art and gathers dust the sediment to the chlorination legal system and handle unreasonable, produces a large amount of solid useless, causes the technical problem of wasting of resources.
In order to achieve the above object, the utility model adopts the following technical scheme: the system comprises an insoluble substance separation unit, a hydrochloric acid stripping unit, a titanium dioxide recovery unit, an iron oxide recovery unit, a metal catalyst recovery unit and a sodium chloride recovery unit which are sequentially arranged according to the process steps;
the titanium dioxide recovery unit comprises a second separation device connected with a wastewater outlet of the hydrochloric acid stripping unit through a first pipeline, wherein a pH adjusting port is formed in the first pipeline and used for adjusting the pH to 4.2-4.8, and the second separation device is used for separating and recovering TiO generated by hydrolysis in wastewater2；
The ferric oxide recovery unit comprises a first-stage reaction tank and a third separation device, wherein the first-stage reaction tank is connected with the water outlet end of the second separation device and is used for adjusting the pH value to 7-10 to separate out ferric hydroxide or ferrous hydroxide, and the third separation device is used for separating and recovering the ferric hydroxide or the ferrous hydroxide;
the metal catalyst recovery unit comprises a secondary reaction tank and a fourth separation device, wherein the secondary reaction tank is communicated with the supernatant of the reaction tank, the secondary reaction tank is used for adjusting the pH value to 10-12.5 so that metal in the wastewater generates hydroxide to be separated out, and the fourth separation device is used for separating and recovering the metal hydroxide;
the sodium chloride recovery unit comprises a nanofiltration device and an evaporation crystallization device, wherein the nanofiltration device is communicated with the supernatant of the secondary reaction tank, the nanofiltration device is used for separating monovalent salt from divalent salt, and the evaporation crystallization device is used for evaporation crystallization of monovalent salt solution.
In one embodiment, the system for recycling water containing waste residues from dust collection of titanium dioxide by chlorination process further comprises:
a drying device: for the drying of the ferric hydroxide or ferrous hydroxide, or for the drying of the metal hydroxide;
and the roasting device is used for dehydrating ferric hydroxide to generate ferric oxide or dehydrating the metal hydroxide to prepare the metal catalyst.
In one embodiment, the iron oxide recovery unit further comprises a magnetic separation refining mechanism for purifying iron oxide.
In one embodiment, the metal catalyst recovery unit is further provided with a forming device for press-forming the metal oxide between the second drying device and the second calcining device.
In one embodiment, the intercepted divalent salt concentrated solution in the nanofiltration device flows back to the inlet of the primary reaction tank through a pipeline.
In one embodiment, the insoluble substance separation unit comprises a first separation device, a gravity separation device and a filtrate buffer tank, wherein the first separation device is used for filtering high titanium slag and calcined coke in wastewater, and a filter press is adopted as the first separation device;
the gravity separation device is used for separating the high titanium slag and the calcined coke;
the filtrate buffer pool is used for storing the separated filtrate.
In one embodiment, the hydrochloric acid stripping unit comprises a hydrochloric acid stripping tower and a hydrochloric acid absorption device, the hydrochloric acid stripping tower is provided with a steam inlet, a mixed gas outlet connected with the hydrochloric acid absorption device and a waste water outlet, and the steam inlet is communicated with a secondary steam outlet of the evaporative crystallization device through an insulated pipeline.
In one embodiment, the second separation device is a tubular membrane, a bag filter, an ultrafiltration membrane, or a multimedia filter.
In one embodiment, the nanofiltration device is further provided with: the filter material in the multi-medium filter is at least two of active carbon, quartz sand, anthracite and walnut slag.
In one embodiment, the third separation device or the fourth separation device is a plate and frame filter press.
The utility model provides a titanium white powder waste residue water resourceful treatment system that gathers dust of chlorination legal system's beneficial effect lies in: the utility model provides a chlorination legal system titanium white powder waste residue water resourceful treatment system that gathers dust is to different impurity, adopt different principles, select for use multi-stage treatment device, has realized the recycle of all impurity in the chlorination legal system titanium white powder waste residue water that gathers dust. The insoluble substance separation unit realizes the separation and reutilization of insoluble high-carbon residue and calcined coke by adopting the principles of filtration and gravity separation; the method comprises the steps of separating and recovering multivalent metal salt in the wastewater through adjustment and control of the pH value of the wastewater, wherein ferric oxide can be used as an industrial raw material and applied to various fields, oxides of magnesium, aluminum and manganese belong to efficient catalysts, and a final product sodium chloride can be used as a raw material of a chlor-alkali enterprise after purification, so that an upstream-downstream circular economic industrial chain is formed with the chlor-alkali enterprise. The system for recycling the titanium dioxide powder dust collection waste slag water by the chlorination method realizes zero emission of the dust collection slag waste water generated in the chlorination process of titanium dioxide preparation, and realizes complete recycling of substances in the dust collection slag waste water in the chlorination process of titanium dioxide preparation.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the following briefly introduces the embodiments or the drawings required in the prior art, and obviously, the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
Fig. 1 is a schematic structural diagram of a processing system according to an embodiment of the present invention;
wherein, in the figures, the respective reference numerals:
10-insoluble substance separation unit, 11-first separation device, 12-gravity separation device, and 13-filtrate buffer pool; 20-hydrochloric acid stripping unit, 21-hydrochloric acid stripping tower and 22-hydrochloric acid absorption device; 30-a titanium dioxide recovery unit; 40-iron oxide recovery unit, 41-first-stage reaction tank, 42-third separation device, 43-first drying device, 44-first roasting device, 45-magnetic separation refining mechanism, 50-metal catalyst recovery unit, 51-second-stage reaction device, 52-fourth separation device, 53-second drying device, 54-forming device, 55-second roasting device; 60-sodium chloride recovery unit, 61-nanofiltration device and 62-evaporative crystallization device.
Detailed Description
In order to make the technical problem, technical solution and advantageous effects to be solved by the present invention more clearly understood, the following description is given in conjunction with the accompanying drawings and embodiments to illustrate the present invention in further detail. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Please refer to fig. 1, which illustrates the recycling system for titanium dioxide dust-collecting waste water produced by chlorination process. The system for recycling the titanium dioxide dust collection waste residue water by the chlorination process in the embodiment comprises an insoluble substance separation unit 10, a hydrochloric acid stripping unit 20, a titanium dioxide recovery unit 30, an iron oxide recovery unit 40, a metal catalyst recovery unit 50 and a sodium chloride recovery unit 60 which are sequentially arranged according to the process steps.
In this embodiment, the titanium dioxide recovery unit 30 includes a second separation device connected to the wastewater outlet of the hydrochloric acid stripping unit 20 via a first pipeline, the first pipeline is provided with a pH adjusting port for adjusting the pH to 4.2-4.8, and the second separation device is used for separating and recovering TiO generated by hydrolysis in wastewater2(ii) a The ferric oxide recovery unit 40 comprises a first-stage reaction tank 41 and a third separation device 42 which are connected with a water outlet end of the second separation device, wherein the first-stage reaction tank 41 is used for adjusting the pH value to 7-10 to separate out ferric hydroxide or ferrous hydroxide, and the third separation device 42 is used for separating and recovering the ferric hydroxide or ferrous hydroxide; the metal catalyst recovery unit 50 comprises a secondary reaction tank 51 and a fourth separation device 52, wherein the secondary reaction tank 51 is communicated with the supernatant of the primary reaction tank 41, the secondary reaction tank 51 is used for adjusting the pH value to 10-12.5 so that metal in the wastewater generates hydroxide and is separated out, and the fourth separation device 52 is used for separating and recovering the metal hydroxide; the sodium chloride recovery unit 60 comprises a nanofiltration device 61 communicated with the supernatant of the secondary reaction tank and an evaporative crystallization device 62, wherein the nanofiltration device 61 is used for separating monovalent salt from divalent salt, and the evaporative crystallization device 62 is used for evaporative crystallization of monovalent salt solution. As an alternative configuration, the third separation device 52 or the fourth separation device 52 is a plate and frame filter press.
In the embodiment, insoluble high titanium slag and calcined coke are removed by passing water obtained from the titanium dioxide dust collection waste slag produced by the chlorination process through an insoluble substance separation unit 10, the separated wastewater flows into a hydrochloric acid stripping unit 20, part of hydrogen chloride in the wastewater is recovered, the acidity of the wastewater is reduced, the wastewater generated by the hydrochloric acid stripping unit 20 flows into a second separation device through a first pipeline, the pH is adjusted to 4.2-4.8 through a pH adjusting port arranged on the first pipeline, and a small amount of residual TiOCl in the wastewater is enabled to pass through a small amount of residual TiOCl2Hydrolysis to TiO2The liquid separated in the second separation device flows into an iron oxide recovery unit40, completely precipitating iron elements in the wastewater to realize the recovery of most iron elements in the wastewater, then flowing through the metal catalyst recovery unit 50 to completely precipitate other metal ions in the wastewater to realize the recovery of other metal elements in the wastewater, flowing into the nanofiltration device 61 to realize the analysis of monovalent salt and divalent salt, and the evaporative crystallization device 62 realizes the recovery of monovalent salt sodium chloride. So far, the embodiment realizes the recovery of all impurities in the titanium dioxide dust-collecting waste residue water by a chlorination method by aiming at different impurities, adopting different principles and selecting a multi-stage treatment device, wherein TiO2The iron oxide can be used as an industrial raw material and applied to various fields, the oxides of magnesium, aluminum and manganese belong to efficient catalysts, the purified final product sodium chloride can be used as a raw material of chlor-alkali enterprises, and an upstream and downstream circular economy industrial chain is formed with the chlor-alkali enterprises, and the treatment system of the embodiment realizes zero emission of dust collection slag wastewater generated in the chlorination process of titanium dioxide preparation.
In this embodiment, in order to implement the oxidation, drying and dehydration of the hydroxide of iron, the iron oxide recovery unit is further provided with a first drying device 43 and a first roasting device 44 which are used in a matching manner, and the first drying device 43 is used for primarily dehydrating and drying the wet ferric hydroxide or ferrous hydroxide precipitate separated by the third separation device 42; the first roasting device 44 oxidizes and dehydrates the dried ferric hydroxide to form ferric oxide.
In order to obtain high-purity iron oxide, the iron oxide recovery unit further comprises a magnetic separation refining mechanism 45 for purifying the iron oxide, and residual metal oxides after refining can be combined into the metal catalyst for treatment so as to prepare the metal catalyst.
As a specific embodiment, the metal catalyst recovery unit 50 further includes a second drying device 53 and a second calcining device 55 which are provided in a kit. The second drying device 53 is used for preliminarily dehydrating and drying the wet metal hydroxide precipitate separated by the fourth separating device 52; the second roasting device 55 is used for oxidizing and dehydrating the dried hydroxide to form a metal oxide.
For the convenience of using as a catalyst, a forming device 54 for press forming of metal oxide is further provided between the second drying device 53 and the second calcining device 55. The forming device 54 can press the dried metal hydroxide into a desired shape, such as a sphere, honeycomb, or the like.
In other embodiments, the first drying device 43 and the second drying device 53 may be a set of devices in which the ferric hydroxide treatment is intermittent and concentrated when the lower precipitate of the primary reaction tank 41 is accumulated to a predetermined amount. Similarly, the treatment of other metal oxides is intermittent.
For the same reason, the first roasting device 44 and the second roasting device 55 may share one set.
The insolubles separation unit may employ a variety of equipment combinations, including, as one embodiment, a first separation device 11, a gravity sorting device 12, and a filtrate buffer tank 13. The first separation device 11 is used for filtering the high titanium slag and calcined coke in the wastewater, and can adopt common filtering equipment, such as a plate-and-frame filter press. The gravity separation device 12 is used for separating the high titanium slag from the calcined coke, and various devices for gravity-based separation can be used. The filtrate buffer tank 13 is used for collecting the filtrate of the first separation device 11, so that the subsequent treatment can be continuously carried out.
The hydrochloric acid stripping unit 20 comprises a hydrochloric acid stripping tower 21 and a hydrochloric acid absorption device 22, wherein the hydrochloric acid stripping tower 21 is provided with a steam inlet, a mixed gas outlet and a waste water outlet which are connected with the hydrochloric acid absorption device 22, the steam inlet is communicated with a secondary steam outlet of the evaporative crystallization device 62 through an insulated pipeline, and a heat source for generating steam is waste heat generated by tail gas treatment for preparing titanium tetrachloride by a rutile chlorination method. The comprehensive utilization of heat is realized.
In this embodiment, the second separation device is a tubular membrane, a bag filter, an ultrafiltration membrane, or a multi-media filter.
In order to improve the purity of sodium chloride, the nanofiltration device 61 is also provided with: a multimedia filter, a cartridge filter or an ultrafiltration device.
In summary, as an embodiment, the specific operation flow includes:
introducing the waste slag water generated by dust collection of titanium dioxide produced by a chlorination process into the first separation device 11, allowing the separated solid to enter the gravity separation device 12 to realize separation of high titanium slag and calcined coke, allowing the waste water after solid-liquid separation to enter the filtrate cache tank 13, allowing the waste water to enter the hydrochloric acid stripping tower 21 through the filtrate cache tank 13, taking out part of hydrogen chloride gas in the waste water by using steam heat, and allowing the recovered hydrogen chloride gas to enter the hydrochloric acid absorption device 22 for recovery.
The wastewater after hydrochloric acid stripping enters the second separation device through the first pipeline, and sodium hydroxide solution with the mass concentration of 5% is added through the pH adjusting port of the first pipeline to adjust the pH to 4.2-4.8, so that a small amount of TiOCl remained in the wastewater is adjusted2Hydrolysis to TiO2Separating out and separating by a tubular membrane, a bag filter, an ultrafiltration membrane or a multi-medium filter.
And the separated liquid flows into the primary reaction tank 41, and a sodium hydroxide solution with the mass concentration of 30-50% or a sodium hydroxide solid is added into the primary reaction tank 41 to adjust the pH value to 7-10, so that the iron element in the wastewater is completely precipitated. The supernatant of the first-stage reaction tank 41 flows into the second-stage reaction tank 51; after the bottom sediment of the first-stage reaction tank 41 is separated by the third separation device 42, the obtained sediment is dried by blowing air by the first drying device 43, then is roasted for 3h to 4h in the first roasting device 44 at 550 ℃ to 650 ℃, is treated by the magnetic separation refining mechanism 45 to obtain high-purity iron oxide, and the remainder is combined to the metal catalyst recovery unit and is combined with the metal hydroxide for treatment. The filtrate of the third separation device 42 is returned to the first-stage reaction tank 41 for circular treatment.
And enabling the supernatant in the first-stage reaction tank to flow into the second-stage reaction tank 51, adding a sodium hydroxide solution or sodium hydroxide solid with the mass concentration of 30-50% into the second-stage reaction tank 51, and adjusting the pH value to 10-12.5 to enable other metal ions in the wastewater to be completely precipitated. And (3) the supernatant of the secondary reaction tank 51 enters the next procedure, hydroxide precipitates are separated by the fourth separation device 52, the obtained precipitates are dried by air blowing by the second drying device 53 to reach the water content of 30-35%, and are molded by the molding device 54 and then are calcined in the second calcining device 55 at the temperature of 600-700 ℃ for 3-4 hours to obtain the high-purity metal catalyst. The filtrate from the fourth separation device 52 is returned to the secondary reaction tank 51 for recycling treatment.
The supernatant in the secondary reaction tank 51 flows into the nanofiltration device 61 after being filtered by the filtration device, the separation of monovalent salt and divalent salt is realized in the nanofiltration device 61, the separated divalent salt concentrated solution flows back to the primary reaction tank 41 for treatment, and the separated monovalent salt solution can be treated by the evaporation crystallization device 62 to obtain sodium chloride solid which is used as a raw material in the chlor-alkali industry, so that the process and chlor-alkali enterprises form an upstream and downstream circular economy industrial chain.
The above description is only exemplary of the present invention and should not be taken as limiting the scope of the present invention, as any modifications, equivalents, improvements and the like made within the spirit and principles of the present invention are intended to be included within the scope of the present invention.
Claims (10)
1. A resourceful treatment system for titanium dioxide dust collection waste residue water by a chlorination method is characterized by comprising an insoluble substance separation unit, a hydrochloric acid stripping unit, a titanium dioxide recovery unit, an iron oxide recovery unit, a metal catalyst recovery unit and a sodium chloride recovery unit which are sequentially arranged according to the process steps;
the titanium dioxide recovery unit comprises a second separation device connected with a wastewater outlet of the hydrochloric acid stripping unit through a first pipeline, wherein a pH adjusting port is formed in the first pipeline and used for adjusting the pH to 4.2-4.8, and the second separation device is used for separating and recovering TiO generated by hydrolysis in wastewater2；
The ferric oxide recovery unit comprises a first-stage reaction tank and a third separation device, wherein the first-stage reaction tank is connected with the water outlet end of the second separation device and is used for adjusting the pH value to 7-10 to separate out ferric hydroxide or ferrous hydroxide, and the third separation device is used for separating and recovering the ferric hydroxide or the ferrous hydroxide;
the metal catalyst recovery unit comprises a secondary reaction tank and a fourth separation device, wherein the secondary reaction tank is communicated with the supernatant of the primary reaction tank, the secondary reaction tank is used for adjusting the pH value to 10-12.5 so that metal in the wastewater generates hydroxide to be separated out, and the fourth separation device is used for separating and recovering the metal hydroxide;
the sodium chloride recovery unit comprises a nanofiltration device and an evaporation crystallization device, wherein the nanofiltration device is communicated with the supernatant of the secondary reaction tank, the nanofiltration device is used for separating monovalent salt from divalent salt, and the evaporation crystallization device is used for evaporation crystallization of monovalent salt solution.
2. The system for recycling waste residue water generated in dust collection of titanium dioxide production by chlorination process according to claim 1, wherein the system further comprises:
a drying device for drying the ferric hydroxide or ferrous hydroxide, or for drying the metal hydroxide;
and the roasting device is used for dehydrating ferric hydroxide to generate ferric oxide or dehydrating the metal hydroxide to prepare the metal catalyst.
3. The system for recycling waste residue water generated in dust collection of titanium dioxide production by chlorination process according to claim 2, wherein the iron oxide recovery unit further comprises: and the magnetic separation refining mechanism is used for purifying the ferric oxide.
4. The system for recycling waste residue water produced in dust collection of titanium dioxide production by chlorination process according to claim 3, wherein the metal catalyst recovery unit is further provided with a forming device for metal oxide press forming between the drying device and the roasting device.
5. The system for recycling waste residue water produced in the dust collection of titanium dioxide production by the chlorination process according to claim 1, wherein the intercepted divalent salt concentrated solution in the nanofiltration device flows back to the inlet of the primary reaction tank through a pipeline.
6. The system for recycling waste residue water generated in dust collection of titanium dioxide production by chlorination process according to claim 1, wherein the insoluble substance separation unit comprises:
the first separation device is used for filtering high titanium slag and calcined coke in the wastewater, and the first separation device adopts a filter press; and/or
The gravity separation device is used for separating the high titanium slag and the calcined coke; and/or
And the filtrate buffer pool is used for storing the separated filtrate.
7. The system for recycling waste residue water from titanium dioxide dust collection by chlorination process according to claim 1, wherein the hydrochloric acid stripping unit comprises a hydrochloric acid stripping tower and a hydrochloric acid absorption device, the hydrochloric acid stripping tower is provided with a steam inlet, a mixed gas outlet communicated with the hydrochloric acid absorption device, and a wastewater outlet, and the steam inlet is communicated with a secondary steam outlet of the evaporative crystallization device through an insulated pipeline.
8. The recycling treatment system for the waste residue water generated in the dust collection of titanium dioxide production by the chlorination process according to claim 1, wherein the second separation device is a tubular membrane, a bag filter, an ultrafiltration membrane or a multi-media filter.
9. The system for recycling waste residue water generated in dust collection of titanium dioxide production by chlorination process according to claim 1, wherein before the nanofiltration device, the system is further provided with: a multimedia filter, a cartridge filter, or an ultrafiltration device.
10. The recycling treatment system for the waste residue water generated in dust collection of titanium dioxide produced by the chlorination process according to claim 1, wherein the third separation device or the fourth separation device is a plate-and-frame filter press.
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