CN112573495A - Sulfur-titanium-phosphorus integrated wastewater treatment process for sulfuric acid method titanium dioxide device - Google Patents
Sulfur-titanium-phosphorus integrated wastewater treatment process for sulfuric acid method titanium dioxide device Download PDFInfo
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- CN112573495A CN112573495A CN202011360511.6A CN202011360511A CN112573495A CN 112573495 A CN112573495 A CN 112573495A CN 202011360511 A CN202011360511 A CN 202011360511A CN 112573495 A CN112573495 A CN 112573495A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/18—Phosphoric acid
- C01B25/22—Preparation by reacting phosphate-containing material with an acid, e.g. wet process
- C01B25/222—Preparation by reacting phosphate-containing material with an acid, e.g. wet process with sulfuric acid, a mixture of acids mainly consisting of sulfuric acid or a mixture of compounds forming it in situ, e.g. a mixture of sulfur dioxide, water and oxygen
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/08—Compounds containing halogen
- C01B33/10—Compounds containing silicon, fluorine, and other elements
- C01B33/103—Fluosilicic acid; Salts thereof
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/14—Sulfates
Abstract
The invention discloses a process for integrally treating wastewater of a sulfate process titanium dioxide device by sulfur, titanium and phosphorus, which relates to the fields of comprehensive utilization of resources and clean production, and specifically comprises the following steps: s1: 1 percent of sulfuric acid wastewater washed by a first washing device and a second washing device of the sulfuric acid method titanium dioxide and 2.5 percent of sulfuric acid wastewater washed by acidolysis and calcination tail gas enter a ground phosphate rock repulping tank of the device, the solid content of phosphorus-containing ore pulp is about 45 percent according to the wastewater amount, a cyclone thickener is added to meet the requirement of the phosphoric acid slurry on the water content, the solid content of the outlet slurry is controlled to be about 54 percent, and after the process, the wastewater containing 1 percent and 2.5 percent of sulfuric acid discharged by the sulfuric acid method titanium dioxide device is consumed. The invention can achieve the comprehensive utilization of water, sulfur and sodium resources and the zero discharge of the sewage of the sulfur-titanium-phosphorus integrated device, can use the salt-containing sewage discharged by a circulating water station and a desalted water station of a sulfate process titanium dioxide device, and simultaneously, the discharged water contains no sulfuric acid and only contains partial calcium salt and is used as a phosphoric acid concentration circulating water station for supplement.
Description
Technical Field
The invention relates to the fields of comprehensive utilization of resources and clean production, in particular to a process for integrally treating wastewater of a sulfate process titanium dioxide device by sulfur, titanium and phosphorus.
Background
A large amount of acidic wastewater can be generated in the production process of the titanium dioxide device by the sulfuric acid method, and data obtained by the existing production device show that the amount of wastewater generated by producing 1t of titanium dioxide by the sulfuric acid method is 40-60 t, and meanwhile, the wastewater discharged in different processes is different in components, and the main components are sulfuric acid, ferrous sulfate and sodium sulfate, so that the wastewater cannot be directly discharged.
At present, most titanium dioxide factories of sulfuric acid process adopt a method of neutralizing with alkaline substances to treat titanium dioxide wastewater, and the obtained neutralized products are common precipitated titanium gypsum and iron-containing filtrate, but the titanium gypsum obtained by the method contains a large amount of iron ion hydrate, has high water content and high viscosity, is difficult to apply, occupies a large amount of land during stacking, and pollutes the environment.
The production process of the phosphoric acid device consumes sulfuric acid and a large amount of water, wherein the sulfuric acid is a production raw material, the consumption of water is not only a part of acid product, but also saturated water discharged by reaction washing tail gas, phosphogypsum crystal water and water evaporated by a phosphoric acid concentration circulating water station are all consumed, in addition, if the phosphoric acid device adopts a wet-process slag-off process, a large amount of water can be evaporated in a phosphogypsum yard, the water source of the phosphoric acid device mainly comprises water brought by raw material phosphorite or powdered rock phosphate and water brought by sulfuric acid, but the quantity is very limited, so that the phosphoric acid device needs to be supplemented with a large amount of water during normal production, and according to the production condition of the existing phosphoric acid device, 35-45 t of water needs to be supplemented every 1t of phosphoric acid is produced.
Therefore, the invention provides a process for integrally treating wastewater of a sulfate process titanium dioxide device by using sulfur, titanium and phosphorus, which is necessary for solving the problems.
Disclosure of Invention
The invention aims to provide a process for integrally treating wastewater of a sulfate process titanium dioxide device by using sulfur, titanium and phosphorus, and aims to solve the problem that according to the production condition of the existing phosphoric acid device, 35-45 t of water needs to be supplemented every 1t of phosphoric acid is produced, and a large amount of water resources are wasted in the background art.
In order to achieve the purpose, the invention provides the following technical scheme: the process for integrally treating the wastewater of the sulfate process titanium dioxide device by using sulfur, titanium and phosphorus comprises the following steps:
s1: 1% sulfuric acid wastewater washed by a first washing device and a second washing device of a sulfuric acid method titanium dioxide device and 2.5% sulfuric acid wastewater washed by acidolysis and calcination tail gas enter a ground phosphate rock repulping tank of the device, the solid content of phosphorus-containing ore pulp is about 45% according to the wastewater amount, a cyclone thickener is added to meet the requirement of phosphoric acid slurry on the water content, the solid content of outlet slurry is controlled to be about 54%, after the process, the 1% and 2.5% sulfuric acid-containing wastewater discharged by the sulfuric acid method titanium dioxide device is consumed, and process water required to be supplemented for preparing the ore pulp of the phosphoric acid device is saved;
s2: firstly, mixing 98% of sulfuric acid added into a phosphoric acid reaction tank with 25% of sulfuric acid-containing wastewater washed from a sulfuric acid method titanium dioxide device according to a ratio, adjusting the ratio to enable the concentration of the mixed sulfuric acid to be 55%, mixing in an external circulation mixer, after the 98% of sulfuric acid is mixed and diluted, emitting a large amount of dilution heat to enable the mixed acid to flow in a circulating pipe, enabling the mixed sulfuric acid to enter a settling tank, naturally cooling to 50 ℃, collecting cooled FeSO4 in a stirring rake, then conveying to a filter press 6 by a slurry pump to perform filter pressing and separating out FeSO4, returning the filtrate which is the mixed sulfuric acid to the settling tank, and after the working procedure, completely utilizing the sulfuric acid in the wastewater and simultaneously separating out FeSO 4;
s3: the Na2SO4 content in the initial salt-containing wastewater of the sulfuric acid process titanium dioxide three-washing is 1.5%, but the wastewater amount accounts for about 45% of the discharge amount of the sulfuric acid process titanium dioxide wastewater, in order to be better utilized, the wastewater can be simply treated by using membrane separation to obtain 11% NaSO4 concentrated phase wastewater, phosphoric acid devices are generally matched with sodium fluosilicate production, the concentrated wastewater containing NaSO4 after separation can be directly conveyed to a sodium fluosilicate device for utilization by a pump, and the generated wastewater is dilute sulfuric acid solution;
s4: the salt-containing sewage discharged by the circulating water station and the desalted water station of the sulfate process titanium dioxide device is collected by a collecting tank and is conveyed to a phosphoric acid filtering section by a pump to replace phosphogypsum and re-slurry for water supplement.
Preferably, in the step S1, the clear solution after the rotational flow thickening contains substantially no sulfuric acid, and can be used as make-up water for a concentrated circulating water station of a phosphoric acid plant.
Preferably, in S2, the settler is provided with a rotating rabble.
Preferably, in the S2, the phosphoric acid extraction reaction theoretically requires not too high a concentration of sulfuric acid to normally maintain the temperature of the reaction tank, but too low a concentration of sulfuric acid affects the reaction speed.
Preferably, in the step S2, the sulfuric acid premixing, vacuum evaporation cooling and cooling processes are adopted, so that the existing high-concentration sulfuric acid can be mixed with the waste water to increase the sulfuric acid concentration, and simultaneously, the FeSO4 is separated by external cooling and settling after self-circulation vacuum evaporation.
Preferably, in S2, the external circulation mixer is provided with a flash chamber, the flash chamber is under negative pressure, and the temperature is controlled to be 85 ℃.
Preferably, in the S3, the main raw materials for producing sodium fluosilicate are fluosilicic acid and sodium salt, and the sodium salt can be NaCL or Na2SO4, wherein the NaCL is gradually eliminated due to the difficulty in treating the HCL-producing wastewater.
The invention has the technical effects and advantages that:
1. on the basis of analyzing the amount and components of wastewater discharged by each process of the titanium white by the sulfuric acid process, aiming at the characteristics of water used by a phosphoric acid device, the invention grasps the balance relationship of sulfur, phosphorus and water in the production process of phosphoric acid, follows the principle of quality-grading and gradient utilization, and utilizes the wastewater discharged by the titanium white device by the sulfuric acid process and sulfuric acid and sodium resources to the maximum extent, so that the production of sulfur, titanium and phosphorus is integrated, and finally the comprehensive utilization of the water, sulfur and sodium resources is achieved, and the zero discharge of the wastewater of the sulfur, titanium and phosphorus integrated device is realized.
2. The main components of the salt-containing sewage discharged by the circulating water station and the desalted water station of the titanium dioxide device by the sulfuric acid process are COD and sulfates containing calcium and iron, the components are similar to those of phosphogypsum which is a reaction product of phosphoric acid, when the phosphogypsum is repulped, besides part of water returned from a slag yard is utilized, because the water is carried by the evaporation of the slag yard and the sedimentation of the phosphogypsum, the returned water is far less than the supplemented water during repulping, a large amount of water is supplemented by the repulping, and therefore the salt-containing sewage discharged by the circulating water station and the desalted water station of the titanium dioxide device by the sulfuric acid process can be.
3. The invention utilizes the principle that phosphate ore can react with sulfuric acid, 1 percent and 2.5 percent of dilute sulfuric acid wastewater is used for replacing process water for pulping phosphate ore pulp, the sulfuric acid in the wastewater reacts with the phosphate ore to be consumed, one part of the rest water enters an ore pulp system, the other part of the rest water is treated as clarification on the upper layer after passing through a cyclone thickener and is also discharged, the discharged water does not contain sulfuric acid, only contains partial calcium salt, and is used as a phosphoric acid concentration circulating water station for supplement.
4. According to the invention, after the sulfate process titanium dioxide three-washing salt-containing wastewater is subjected to preliminary treatment in a titanium dioxide device, 150g/lNa2SO4 wastewater is obtained, Na2SO4 is used for producing sodium fluosilicate, the operation of the existing device is not influenced, and simultaneously, a certain amount of dilute H2SO4 is contained in the generated mother liquor, SO that comprehensive cyclic utilization is realized.
5. The phosphoric acid extraction reaction in the invention theoretically has no high requirement on the concentration of sulfuric acid, the temperature of a reaction tank can be normally maintained, but the sulfuric acid with the excessively low concentration influences the reaction speed, and meanwhile, the waste water contains FeSO4, if the waste water is directly used, the normal operation of the subsequent working procedures of a phosphoric acid device is influenced, so that FeSO4 needs to be separated before use.
Drawings
FIG. 1 is a flow chart of the present invention for utilizing 1% and 2.5% waste water containing sulfuric acid;
FIG. 2 is a flow chart of the utilization of 25% sulfuric acid-containing wastewater according to the present invention;
FIG. 3 is a flow chart of the sulfuric acid process titanium dioxide three-washing treatment of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a process for integrally treating wastewater of a sulfate process titanium dioxide device by using sulfur, titanium and phosphorus, which comprises the following steps:
s1: 1% sulfuric acid wastewater washed by a first washing device and a second washing device of a sulfuric acid method titanium dioxide device and 2.5% sulfuric acid wastewater washed by acidolysis and calcination tail gas enter a ground phosphate rock repulping tank of the device, the solid content of phosphorus-containing ore pulp is about 45% according to the wastewater amount, a cyclone thickener is added to meet the requirement of phosphoric acid slurry on the water content, the solid content of outlet slurry is controlled to be about 54%, after the process, the 1% and 2.5% sulfuric acid-containing wastewater discharged by the sulfuric acid method titanium dioxide device is consumed, and process water required to be supplemented for preparing the ore pulp of the phosphoric acid device is saved;
meanwhile, clear liquid after rotational flow thickening basically does not contain sulfuric acid, and can be used as water replenishing of a concentration circulating water station of a phosphoric acid device;
s2: firstly, mixing 98% of sulfuric acid added into a phosphoric acid reaction tank with 25% of sulfuric acid-containing wastewater washed from a sulfuric acid method titanium dioxide device according to a ratio, adjusting the ratio to enable the concentration of the mixed sulfuric acid to be 55%, mixing in an external circulation mixer, after the 98% of sulfuric acid is mixed and diluted, emitting a large amount of dilution heat to enable the mixed acid to flow in a circulating pipe, enabling the mixed sulfuric acid to enter a settling tank, naturally cooling to 50 ℃, collecting cooled FeSO4 in a stirring rake, then conveying to a filter press 6 by a slurry pump to perform filter pressing and separating out FeSO4, returning the filtrate which is the mixed sulfuric acid to the settling tank, and after the working procedure, completely utilizing the sulfuric acid in the wastewater and simultaneously separating out FeSO 4;
in addition, the settling tank is provided with a rotary stirring rake;
then, the phosphoric acid extraction reaction theoretically has no high requirement on the concentration of sulfuric acid, and the temperature of the reaction tank can be normally maintained, but the sulfuric acid with too low concentration can influence the reaction speed;
in addition, the existing high-concentration sulfuric acid can be mixed with the waste water to improve the concentration of the sulfuric acid by adopting the processes of sulfuric acid premixing, vacuum evaporation cooling and cooling, and simultaneously FeSO4 is separated by external cooling and settling after self-circulation vacuum evaporation;
more specifically, the external circulation mixer is provided with a flash evaporation chamber, the flash evaporation chamber is under negative pressure, and the temperature is controlled to be 85 ℃;
s3: the Na2SO4 content in the initial salt-containing wastewater of the sulfuric acid process titanium dioxide three-washing is 1.5%, but the wastewater amount accounts for about 45% of the discharge amount of the sulfuric acid process titanium dioxide wastewater, in order to be better utilized, the wastewater can be simply treated by using membrane separation to obtain 11% NaSO4 concentrated phase wastewater, phosphoric acid devices are generally matched with sodium fluosilicate production, the concentrated wastewater containing NaSO4 after separation can be directly conveyed to a sodium fluosilicate device for utilization by a pump, and the generated wastewater is dilute sulfuric acid solution;
it should be noted that the main raw materials for producing sodium fluosilicate are fluosilicic acid and sodium salt, the sodium salt can be NaCL or Na2SO4, wherein the NaCL is gradually eliminated because the produced HCL wastewater is difficult to treat;
s4: the salt-containing sewage discharged by the circulating water station and the desalted water station of the sulfate process titanium dioxide device is collected by a collecting tank and is conveyed to a phosphoric acid filtering section by a pump to replace phosphogypsum and re-slurry for water supplement.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications may be made to the embodiments or portions thereof without departing from the spirit and scope of the invention.
Claims (7)
1. The process for integrally treating the wastewater of the sulfate process titanium dioxide device by using sulfur, titanium and phosphorus is characterized by comprising the following steps of:
s1: 1% sulfuric acid wastewater washed by a first washing device and a second washing device of a sulfuric acid method titanium dioxide device and 2.5% sulfuric acid wastewater washed by acidolysis and calcination tail gas enter a ground phosphate rock repulping tank of the device, the solid content of phosphorus-containing ore pulp is about 45% according to the wastewater amount, a cyclone thickener is added to meet the requirement of phosphoric acid slurry on the water content, the solid content of outlet slurry is controlled to be about 54%, after the process, the 1% and 2.5% sulfuric acid-containing wastewater discharged by the sulfuric acid method titanium dioxide device is consumed, and process water required to be supplemented for preparing the ore pulp of the phosphoric acid device is saved;
s2: firstly, mixing 98% of sulfuric acid added into a phosphoric acid reaction tank with 25% of sulfuric acid-containing wastewater washed from a sulfuric acid method titanium dioxide device according to a ratio, adjusting the ratio to enable the concentration of the mixed sulfuric acid to be 55%, mixing in an external circulation mixer, after the 98% of sulfuric acid is mixed and diluted, emitting a large amount of dilution heat to enable the mixed acid to flow in a circulating pipe, enabling the mixed sulfuric acid to enter a settling tank, naturally cooling to 50 ℃, collecting cooled FeSO4 in a stirring rake, then conveying to a filter press 6 by a slurry pump to perform filter pressing and separating out FeSO4, returning the filtrate which is the mixed sulfuric acid to the settling tank, and after the working procedure, completely utilizing the sulfuric acid in the wastewater and simultaneously separating out FeSO 4;
s3: the Na2SO4 content in the initial salt-containing wastewater of the sulfuric acid process titanium dioxide three-washing is 1.5%, but the wastewater amount accounts for about 45% of the discharge amount of the sulfuric acid process titanium dioxide wastewater, in order to be better utilized, the wastewater can be simply treated by using membrane separation to obtain 11% NaSO4 concentrated phase wastewater, phosphoric acid devices are generally matched with sodium fluosilicate production, the concentrated wastewater containing NaSO4 after separation can be directly conveyed to a sodium fluosilicate device for utilization by a pump, and the generated wastewater is dilute sulfuric acid solution;
s4: the salt-containing sewage discharged by the circulating water station and the desalted water station of the sulfate process titanium dioxide device is collected by a collecting tank and is conveyed to a phosphoric acid filtering section by a pump to replace phosphogypsum and re-slurry for water supplement.
2. The process for integrally treating wastewater of a sulfuric acid process titanium dioxide device according to claim 1, which is characterized in that: in the step S1, the clear liquid after the rotational flow thickening basically does not contain sulfuric acid, and can be used as the water replenishing of a concentration circulating water station of a phosphoric acid device.
3. The process for integrally treating wastewater of a sulfuric acid process titanium dioxide device according to claim 1, which is characterized in that: in said S2, the settler is provided with a rotating rabble.
4. The process for integrally treating wastewater of a sulfuric acid process titanium dioxide device according to claim 1, which is characterized in that: in the S2, the phosphoric acid extraction reaction theoretically requires no high concentration of sulfuric acid, and the temperature of the reaction tank can be normally maintained, but the reaction speed is influenced by the sulfuric acid with too low concentration.
5. The process for integrally treating wastewater of a sulfuric acid process titanium dioxide device according to claim 1, which is characterized in that: in the S2, the sulfuric acid premixing, vacuum evaporation cooling and cooling processes are adopted, the existing high-concentration sulfuric acid can be mixed with the waste water to improve the sulfuric acid concentration, and simultaneously, FeSO4 is separated out through external cooling and settling after self-circulation vacuum evaporation.
6. The process for integrally treating wastewater of a sulfuric acid process titanium dioxide device according to claim 1, which is characterized in that: in the step S2, the external circulation mixer is provided with a flash chamber, the flash chamber is under negative pressure, and the temperature is controlled to be 85 ℃.
7. The process for integrally treating wastewater of a sulfuric acid process titanium dioxide device according to claim 1, which is characterized in that: in the S3, the main raw materials for producing the sodium fluosilicate are fluosilicic acid and sodium salt, the sodium salt can be NaCL or Na2SO4, wherein the NaCL is gradually eliminated because the generated HCL wastewater is difficult to treat.
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1376635A (en) * | 2002-05-09 | 2002-10-30 | 四川龙蟒集团有限责任公司 | Process for preparing phosphoric acid from waste sulfuric acid as by-product of titanium oxide powder by wet method |
| CN101759166A (en) * | 2009-12-31 | 2010-06-30 | 四川龙蟒钛业股份有限公司 | Method for pre-treating phosphorite by using acidic waste water in the production process of titanium pigment |
| CN103723765A (en) * | 2014-01-20 | 2014-04-16 | 韶关学院 | Method for preparing titanium dioxide through sulfuric acid method |
| CN107902823A (en) * | 2015-08-19 | 2018-04-13 | 石家庄工大化工设备有限公司 | The recovery and treatment method of the high-salt wastewater of sodium chloride-containing and sodium sulphate |
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