CN108640383B - Process and system for improving operation period of vanadium pentoxide stripping deamination tower - Google Patents
Process and system for improving operation period of vanadium pentoxide stripping deamination tower Download PDFInfo
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Abstract
A process for increasing the running period of stripping deaminizing tower of vanadium pentoxide includes such steps as loading the waste water from depositing vanadium in acidic ammonium salt to the first-class desiliconizing tank, adding lime powder as desiliconizing agent, first desiliconizing, solid-liquid separation by press filter, adding calcium chloride as desiliconizing agent, secondary desiliconizing, solid-liquid separation by microporous ultrafilter, loading it to the first-class dechromizing calcium tank, adding concentrated sulfuric acid, regulating pH value, adding sodium pyrosulfite as reducer, reaction, adding soda and sodium hydroxide as dechromizing agent, solid-liquid separation by press filter, loading it to the second-class decalcifying tank, adding sodium phosphate as decalcifying agent, and solid-liquid separation by microporous ultrafilter. The advantages are that: by selectively removing harmful ions such as silicon, calcium and the like, the operation cycle of a stripping deamination tower system is improved by 4 times and reaches more than 150 days, the steam overhaul cleaning cost and the production stop loss are reduced, the continuous production operation target of vanadium pentoxide is realized, and the deamination standard discharge of vanadium precipitation wastewater is ensured.
Description
Technical Field
The invention belongs to the field of vanadium slag vanadium extraction wastewater treatment, and particularly relates to a process and a system for improving the operation period of a vanadium pentoxide stripping deamination tower.
Background
The vanadium-titanium magnetite is smelted into molten iron containing vanadium by a blast furnace, the molten iron is oxidized and blown by a converter, and vanadium enters a slag phase after being enriched to obtain vanadium slag. The vanadium extraction process of the vanadium slag is to bake the vanadium slag into clinker, extract the clinker with water to obtain vanadium solution, add sulfuric acid and ammonium sulfate into the vanadium solution, heat and precipitate vanadium with steam to prepare ammonium polyvanadate, and the ammonium polyvanadate is dried, calcined, decomposed, melted and cooled by a melting furnace to prepare the flaky vanadium pentoxide product. In the vanadium precipitation process, excessive ammonium sulfate is added into a vanadium solution, vanadium is converted into ammonium polyvanadate precipitate, the ammonium polyvanadate is subjected to filter pressing and solid-liquid separation by a filter press, hexavalent chromium and a large number of ammonium groups are contained in vanadium precipitation wastewater, after the hexavalent chromium in the vanadium precipitation wastewater is detoxified by a reducing agent, the ammonium group-containing wastewater is adjusted to a pH value of more than 12 by sodium hydroxide, steam is heated to boiling by a stripping deamination tower to remove ammonia nitrogen, sulfuric acid is adopted to absorb ammonia gas and obtain a byproduct ammonium sulfate liquid, the ammonium sulfate liquid is returned to a vanadium precipitation process for vanadium precipitation production, and the vanadium precipitation wastewater is discharged after being deaminated and reaches the.
Because the vanadium precipitation wastewater entering the stripping deamination tower contains harmful impurity ions such as silicon (0.3-0.9g/L), calcium (0.1-0.4g/L) and the like, the deamination tower gradually scales to destroy the vapor-liquid balance in the tower in the steam stripping heating deamination process, the continuous operation period of the stripping deamination tower is generally less than 10 days, and a deamination tower system is forced to stop for maintenance for more than one week to clean the scales, thereby seriously influencing the continuous production operation of vanadium pentoxide. At present, domestic vanadium extraction enterprises generally adopt a mode of adding an efficient scale inhibition dispersant into vanadium precipitation wastewater to delay scaling time, and the continuous operation period of a stripping deamination tower system is improved, but the method has the defects that the operation period of the stripping deamination tower system is short and still less than 40 days, vanadium pentoxide cannot be continuously produced, and the production stoppage and maintenance of the stripping deamination tower of the vanadium extraction enterprises often bring huge economic loss and environmental protection pressure.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a process and a system for improving the operation period of a vanadium pentoxide stripping deamination tower, wherein harmful ions such as silicon, calcium and the like are selectively removed, so that the operation period of the stripping deamination tower system is improved by 4 times and reaches more than 150 days, the overhaul and cleaning cost and production stop loss of the stripping deamination tower system are reduced, the continuous production operation target of vanadium pentoxide is realized, and the deamination emission of vanadium precipitation wastewater is ensured to reach the standard.
The technical solution of the invention is as follows:
a process for improving the operation period of a vanadium pentoxide stripping deamination tower system comprises the following specific steps:
(1) opening a valve a, sending the acidic ammonium salt vanadium precipitation wastewater with the temperature of 50-70 ℃ into a primary desiliconization tank, closing the valve a, starting a stirring paddle, adding a desiliconization agent lime powder, reacting for 20-30 min, controlling the pH value to be 9.0-10.5, carrying out primary desiliconization, and carrying out solid-liquid separation on the primary desiliconization solution through a filter press after analyzing and detecting that the silicon content of the solution in the primary desiliconization tank is less than or equal to 0.1 g/L;
(2) opening a valve b, sending filtrate filtered by the filter press into a secondary desiliconization tank, closing the valve b, starting a stirring paddle, adding a desiliconization agent calcium chloride, reacting for 10-30 min, carrying out secondary desiliconization, and carrying out solid-liquid separation on the secondary desiliconization solution through a microporous precision filter after analyzing and detecting that the solution in the secondary desiliconization tank contains silicon less than or equal to 0.05 g/L;
(3) opening a valve c, sending filtrate filtered by a microporous precise filter into a first-stage chromium-removing calcium tank, closing the valve c, starting a stirring paddle, opening a valve d, adding concentrated sulfuric acid into the first-stage chromium-removing calcium tank, adjusting the pH value of the solution to be less than or equal to 2.5, adding a reducing agent sodium metabisulfite into the first-stage chromium-removing calcium tank, reacting for 20-30 min, adding a chromium-removing calcium agent sodium carbonate and sodium hydroxide into the first-stage chromium-removing calcium tank, neutralizing the pH value of 9.5-10.5, reacting for 10-30 min, after primary calcium removal, analyzing and detecting that the calcium content of the solution in the first-stage chromium-removing calcium tank is less than or equal to 0.06g/L, and performing solid-liquid separation on the primary calcium-removing solution through a filter press;
(4) opening a valve e, sending filtrate filtered by the filter press into a secondary decalcification tank, closing the valve e, starting a stirring paddle, adding a decalcification agent sodium phosphate into the secondary decalcification tank, reacting for 10-30 min, analyzing and detecting that the calcium content of the solution in the secondary decalcification tank is less than or equal to 0.0005g/L, carrying out solid-liquid separation on the reacted solution through a microporous precision filter, and then conveying the filtrate, namely the ammonium-containing vanadium precipitation wastewater to a stripping deamination tower system to remove ammonia nitrogen.
Further, in the step (1), the particle size of the silica remover lime powder is 100-400 meshes, and the mass content of active CaO is more than or equal to 40%.
Further, the mass ratio of the calcium content in the calcium chloride serving as the silicon removing agent in the step (2) to the silicon content in the primary silicon removing liquid is 3.0: 1-7.0: 1.
Further, in the step (3), the chromium and calcium removing agent comprises sodium carbonate and sodium hydroxide, and the mass ratio of the sodium carbonate to the sodium hydroxide is 0.6: 1-3.0: 1.
Further, the mass ratio of the phosphorus content in the calcium removing agent sodium phosphate in the step (4) to the calcium content in the primary calcium removing liquid is 1.0: 1-4.0: 1.
Further, the particle size of the silicon removing agent lime powder in the step (1) is 200-350 meshes, the mass ratio of calcium in calcium chloride serving as a silicon removing agent to silicon in primary silicon removing liquid in the step (2) is 3.5: 1-6.0: 1, the mass ratio of soda ash serving as a chromium removing agent to sodium hydroxide in the step (3) is 0.9: 1-1.5: 1, and the mass ratio of phosphorus in sodium phosphate serving as a calcium removing agent to calcium in primary calcium removing liquid in the step (4) is 2.0: 1-3.5: 1.
The utility model provides an improve vanadium pentoxide strip deamination tower operating cycle's acid ammonium salt pretreatment systems, has one-level desiliconization jar, second grade desiliconization jar, one-level dechromization calcium jar, second grade decalcification jar, its special character lies in: the one-level desiliconization jar liquid outlet is linked together through pipeline and second grade desiliconization jar, is equipped with pressure filtration pump I, pressure filter I in proper order on the pipeline between one-level desiliconization jar and the second grade desiliconization jar, the second grade desiliconization jar is linked together through pipeline and one-level dechromization calcium jar, is equipped with transfer pump I, micropore precision filter I in proper order on the pipeline between second grade desiliconization jar and the one-level dechromization calcium jar, the one-level dechromization calcium jar is linked together through pipeline and second grade desiliconization jar, is equipped with pressure filtration pump II, pressure filter II in proper order on the pipeline between one-level dechromization calcium jar and the second grade dechromization jar, the second grade decalcification jar is linked together through pipeline and micropore precision filter II, is equipped with transfer pump II on the pipeline between second grade desiliconization jar and micropore precision filter II, II exports of micropore precision.
Furthermore, a sulfuric acid inlet of the first-stage chromium-removing calcium tank is connected with a sulfuric acid storage tank through a pipeline, and a sulfuric acid delivery pump is arranged on the pipeline between the first-stage chromium-removing calcium tank and the sulfuric acid storage tank.
An acidic ammonium salt vanadium precipitation wastewater inlet of the primary silicon removal tank is provided with an acidic ammonium salt vanadium precipitation wastewater pipeline, and a valve a is arranged on the acidic ammonium salt vanadium precipitation wastewater inlet pipeline of the primary silicon removal tank.
The inlet pipeline of the second-stage dechromization tank is provided with a valve b, the secondary dechromization solution inlet pipeline of the first-stage dechromization calcium tank is provided with a valve c, the sulfuric acid inlet pipeline of the first-stage dechromization calcium tank is provided with a valve d, and the inlet pipeline of the second-stage dechromization tank is provided with a valve e.
The invention has the beneficial effects that:
(1) the process is simple, the equipment structure is reasonable, and the operation is convenient;
the silicon removal tank is used for removing silicon twice, so that the silicon removal effect is good; the calcium removal tank is used for removing calcium twice, the calcium removal effect is good, and the concentration of harmful impurity ions such as silicon, calcium and the like in the vanadium precipitation wastewater is greatly reduced.
(2) The operation period of the stripping deamination tower system is increased by 4 times from less than 40 days to more than 150 days.
The process and the system thereof can thoroughly remove silicon, calcium and other ions without adding a high-efficiency scale inhibition dispersing agent into the vanadium precipitation wastewater, greatly improve the operation period of a stripping deamination tower system, realize continuous production operation of vanadium pentoxide and ensure that the vanadium precipitation wastewater is deaminated and discharged up to the standard.
(3) The suspended particles of silicon, calcium, chromium and the like in the solution are greatly reduced by using the microporous precise filter.
The process and the system thereof not only greatly improve the operation period of a stripping deamination tower system, but also greatly reduce the suspended matters in the discharged wastewater, so that the SS of the suspended matters is less than or equal to 10mg/L and is far lower than the national allowable vanadium industrial discharge standard (the SS is less than or equal to 50 mg/L).
Drawings
FIG. 1 is a schematic structural diagram of an acidic ammonium salt pretreatment system for increasing the operation period of a vanadium pentoxide stripping deamination tower.
In the figure: 1-first-stage desiliconization tank, 2-filter press I, 3-second-stage desiliconization tank, 4-microporous precise filter I, 5-first-stage chromium calcium removal tank, 6-filter press II, 7-second-stage desiliconization tank, 8-microporous precise filter II, 9-filter press pump I, 10-infusion pump I, 11-filter press pump II, 12-infusion pump II, 13-sulfuric acid storage tank and 14-sulfuric acid delivery pump.
Detailed Description
Example 1
As shown in the figure, the acidic ammonium salt pretreatment system for improving the operation cycle of the vanadium pentoxide stripping deamination tower comprises a primary desiliconization tank 1, a secondary desiliconization tank 3, a primary chromium and calcium removal tank 5 and a secondary calcium removal tank 7, wherein a liquid outlet of the primary desiliconization tank 1 is communicated with the secondary desiliconization tank 3 through a pipeline, an acidic ammonium salt vanadium precipitation wastewater pipeline is arranged at an acidic ammonium salt vanadium precipitation wastewater inlet of the primary desiliconization tank 1, and a valve a is arranged at the acidic ammonium salt vanadium precipitation wastewater inlet pipeline of the primary desiliconization tank; a pressure filtration pump I9 and a pressure filter I2 are sequentially arranged on a pipeline between the primary desiliconization tank 1 and the secondary desiliconization tank 3, the secondary desiliconization tank 3 is communicated with the primary dechromization calcium tank 5 through a pipeline, an infusion pump I10 and a microporous precision filter I4 are sequentially arranged on the pipeline between the secondary desiliconization tank 3 and the primary dechromization calcium tank 5, a valve b is arranged on an inlet pipeline of the secondary desiliconization tank 3, the primary dechromization calcium tank 5 is communicated with the secondary dechromization tank 7 through a pipeline, a pressure filtration pump II 11 and a pressure filter II 6 are sequentially arranged on the pipeline between the primary dechromization calcium tank 5 and the secondary dechromization tank 7, a sulfuric acid inlet of the primary dechromization calcium tank 5 is connected with a sulfuric acid storage tank 13 through a pipeline, and a sulfuric acid delivery pump 14 is arranged on the pipeline between the primary dechromization calcium tank 5 and the sulfuric acid storage tank; the secondary of one-level chromium calcium jar 5 is removed the siliconization solution inlet pipe and is equipped with valve c, sulphuric acid inlet pipe and is equipped with valve d, the second grade removes calcium jar 7 and is linked together through pipeline and II 8 of micropore precision filter, is equipped with transfer pump II 12 on the pipeline between second grade calcium jar 7 and II 8 of micropore precision filter to the inlet pipe that removes the calcium jar at the second grade is equipped with valve e, II 8 exports of micropore precision filter pass through the pipeline with strip deamination tower system entry and link to each other.
The operation process of the acidic ammonium salt pretreatment system for improving the operation period of the vanadium pentoxide stripping deamination tower is as follows: before the process system is started, all valves are in a closed state;
(1) opening a valve a, sending acidic ammonium salt vanadium precipitation wastewater (0.6 g/L of silicon, 0.3g/L of calcium and 1.2g/L of hexavalent chromium) with the temperature of 50 ℃ into a primary desiliconization tank 1, closing the valve a, starting a stirring paddle, adding lime powder (the granularity is 100 meshes and the active CaO content is 40%), controlling the pH value to be 9.0, reacting for 20min, carrying out primary desiliconization, analyzing and detecting that a solution in the primary desiliconization tank contains 0.1g/L of silicon, starting a filter press pump I9, and carrying out solid-liquid separation on the primary desiliconization solution through a filter press I2;
(2) opening a valve b, sending filtrate filtered by the filter press filter I2 into a secondary desiliconization tank 3, closing the valve b, starting a stirring paddle, adding calcium chloride (the mass ratio of the calcium content in the desiliconization agent calcium chloride to the silicon content in the primary desiliconization liquid is 3.0:1), reacting for 30min, carrying out secondary desiliconization, analyzing and detecting that the solution in the secondary desiliconization tank 3 contains 0.05g/L silicon, starting an infusion pump I10, and carrying out solid-liquid separation on the secondary desiliconization solution through a microporous precision filter I4;
(3) opening a valve c, sending filtrate filtered by a microporous precise filter I4 into a primary chromium-removing calcium tank 5, closing the valve c, starting a stirring paddle, opening a valve d, adding concentrated sulfuric acid into the primary chromium-removing calcium tank 5, adjusting the pH value of the solution to 2.5, adding sodium metabisulfite into the primary chromium-removing calcium tank 5, reacting for 20min, adding soda and sodium hydroxide (the mass ratio of the soda to the sodium hydroxide is 0.6:1) into the tank 5, neutralizing the pH value to 9.5, reacting for 10min, analyzing and detecting the calcium content of the solution in the primary chromium-removing calcium tank 5 to be 0.06g/L after primary calcium removal, starting a filter press pump II 11, and performing solid-liquid separation on the primary calcium-removed solution through a filter press II 6;
(4) opening a valve e, sending filtrate filtered by the filter press II 6 into a secondary decalcification tank 7, closing the valve e, starting a stirring paddle, adding sodium phosphate (the mass ratio of phosphorus in a decalcification agent sodium phosphate to calcium in a primary decalcification solution is 1.0:1) into the secondary decalcification tank 7, reacting for 10min, analyzing and detecting the calcium content of the solution in the secondary decalcification tank 7 to be 0.0005g/L, carrying out solid-liquid separation on the reacted solution through a microporous precision filter II 8, then conveying the filtrate, namely the ammonium-containing vanadium precipitation wastewater to a stripping deamination tower system to remove ammonia nitrogen, and carrying out ammonia nitrogen removal on the deamination wastewater NH3N2.5mg/L, suspension SS 8.5 mg/L.
Example 2
The acidic ammonium salt pretreatment system for improving the operation period of the vanadium pentoxide stripping deamination tower is the same as that in the embodiment 1.
The operation process of the process system for improving the operation period of the vanadium pentoxide stripping deamination tower is as follows: before the process system is started, all valves are in a closed state;
(1) opening a valve a, sending acidic ammonium salt vanadium precipitation wastewater (0.7 g/L of silicon, 0.4g/L of calcium and 1.3g/L of hexavalent chromium) with the temperature of 70 ℃ into a primary desiliconization tank 1, closing the valve a, starting a stirring paddle, adding a desiliconization agent lime powder (the granularity is 400 meshes and the active CaO content is 64%), controlling the pH value to be 10.5, reacting for 30min, carrying out primary desiliconization, analyzing and detecting the solution of the primary desiliconization tank to contain 0.06g/L of silicon, starting a filter press pump I9, and carrying out solid-liquid separation on the primary desiliconization solution through a filter press I2;
(2) opening a valve b, sending filtrate filtered by the filter press filter I2 into a secondary desiliconization tank 3, closing the valve b, starting a stirring paddle, adding calcium chloride (the mass ratio of the calcium content in the desiliconization agent calcium chloride to the silicon content in the primary desiliconization liquid is 7.0:1), reacting for 10min, carrying out secondary desiliconization, analyzing and detecting that the solution in the secondary desiliconization tank 3 contains 0.01g/L silicon, starting an infusion pump I10, and carrying out solid-liquid separation on the secondary desiliconization solution through a microporous precision filter I4;
(3) opening a valve c, sending filtrate filtered by a microporous precise filter I4 into a primary chromium-removing calcium tank 5, closing the valve c, starting a stirring paddle, opening a valve d, adding concentrated sulfuric acid into the primary chromium-removing calcium tank 5, adjusting the pH value of the solution to be 1.8, adding sodium metabisulfite into the primary chromium-removing calcium tank 5, reacting for 30min, adding a chromium-calcium removing agent of soda and sodium hydroxide (the mass ratio of the soda to the sodium hydroxide is 3.0:1) into the tank 5, neutralizing the pH value to be 10.5, reacting for 30min, analyzing and detecting that the solution in the primary chromium-removing calcium tank 5 contains 0.05g/L of calcium after primary calcium removal, starting a filter press pump II 11, and separating the primary calcium-removed solution through a filter press II 6;
(4) opening a valve e, sending filtrate filtered by the filter press II 6 into a secondary decalcification tank 7, closing the valve e, starting a stirring paddle, adding sodium phosphate (the mass ratio of phosphorus in the calcium phosphate as a decalcification agent to calcium in the primary decalcification solution is 4.0:1) into the secondary decalcification tank 7, reacting for 30min, analyzing and detecting 0.0001g/L of calcium in the solution in the secondary decalcification tank 7, carrying out solid-liquid separation on the reacted solution through a microporous precision filter II 8, then conveying the filtrate, namely the ammonium-containing vanadium precipitation wastewater to a stripping deamination tower system to remove ammonia nitrogen, and carrying out NH deamination on the wastewater32.9mg/L of N, and 6.4mg/L of suspended substance SS.
Example 3
The acidic ammonium salt pretreatment system for improving the operation period of the vanadium pentoxide stripping deamination tower is the same as that in the embodiment 1.
The operation process of the process system for improving the operation period of the vanadium pentoxide stripping deamination tower is as follows: before the process system is started, all valves are in a closed state;
(1) opening a valve a, sending acidic ammonium salt vanadium precipitation wastewater (0.3 g/L of silicon, 0.1g/L of calcium and 1.6g/L of hexavalent chromium) with the temperature of 60 ℃ into a primary desiliconization tank 1, closing the valve a, starting a stirring paddle, adding lime powder (the granularity is 350 meshes and the active CaO content is 76%), controlling the pH value to be 9.8, reacting for 25min, carrying out primary desiliconization, analyzing and detecting that a solution in the primary desiliconization tank contains 0.06g/L of silicon, starting a filter press pump I9, and carrying out solid-liquid separation on the primary desiliconization solution through a filter press I2;
(2) opening a valve b, sending filtrate filtered by the filter press filter I2 into a secondary desiliconization tank 3, closing the valve b, starting a stirring paddle, adding calcium chloride (the mass ratio of the calcium content in the desiliconization agent calcium chloride to the silicon content in the primary desiliconization liquid is 6.0:1), reacting for 25min, carrying out secondary desiliconization, analyzing and detecting that the solution in the secondary desiliconization tank 3 contains 0.009g/L silicon, starting an infusion pump I10, and carrying out solid-liquid separation on the secondary desiliconization solution through a microporous precision filter I4;
(3) opening a valve c, sending filtrate filtered by a microporous precise filter I4 into a primary chromium-removing calcium tank 5, closing the valve c, starting a stirring paddle, opening a valve d, adding concentrated sulfuric acid into the primary chromium-removing calcium tank 5, adjusting the pH value of the solution to 1.5, adding sodium metabisulfite into the primary chromium-removing calcium tank 5, reacting for 26min, adding a chromium-calcium removing agent, namely soda and sodium hydroxide (the mass ratio of the soda to the sodium hydroxide is 1.5:1) into the tank 5, neutralizing the pH value to 10.0, reacting for 25min, analyzing and detecting that the solution in the primary chromium-removing calcium tank 5 contains 0.02g/L of calcium after primary calcium removal, starting a filter press pump II 11, and carrying out solid-liquid separation on the primary calcium-removing solution through a filter press II 6;
(4) opening a valve e, sending the filtrate filtered by the filter press II 6 into a secondary decalcification tank 7, closing the valve e, starting a stirring paddle, and adding sodium phosphate (the phosphorus content in the decalcification agent sodium phosphate and the primary decalcification solution) into the secondary decalcification tank 7Calcium mass ratio of 3.5:1), reacting for 20min, analyzing and detecting that the solution in the secondary calcium removal tank 7 contains 0.0001g/L calcium, performing solid-liquid separation on the reacted solution through a microporous precision filter II 8, conveying the filtrate, namely the ammonium-containing vanadium precipitation wastewater to a stripping deamination tower system to remove ammonia nitrogen, and performing deamination on the wastewater NH36.5mg/L of N and 5.7mg/L of suspended substance SS.
Example 4
The acidic ammonium salt pretreatment system for improving the operation period of the vanadium pentoxide stripping deamination tower is the same as that in the embodiment 1.
The operation process of the process system for improving the operation period of the vanadium pentoxide stripping deamination tower is as follows: before the process system is started, all valves are in a closed state;
(1) opening a valve a, sending acidic ammonium salt vanadium precipitation wastewater (0.5 g/L of silicon, 0.2g/L of calcium and 1.5g/L of hexavalent chromium) with the temperature of 55 ℃ into a primary desiliconization tank 1, closing the valve a, starting a stirring paddle, adding lime powder (the granularity is 200 meshes and the active CaO content is 81%), controlling the pH value to be 10.0, reacting for 20min, carrying out primary desiliconization, analyzing and detecting that a solution in the primary desiliconization tank contains 0.07g/L of silicon, starting a filter press pump I9, and carrying out solid-liquid separation on the primary desiliconization solution through a filter press I2;
(2) opening a valve b, sending filtrate filtered by the filter press filter I2 into a secondary desiliconization tank 3, closing the valve b, starting a stirring paddle, adding calcium chloride (the mass ratio of the calcium content in the desiliconization agent calcium chloride to the silicon content in the primary desiliconization liquid is 4.0:1), reacting for 20min, carrying out secondary desiliconization, analyzing and detecting the solution in the secondary desiliconization tank 3 to contain 0.006g/L silicon, starting an infusion pump I10, and carrying out solid-liquid separation on the secondary desiliconization solution through a microporous precision filter I4;
(3) opening a valve c, sending filtrate filtered by a microporous precise filter I4 into a primary chromium-removing calcium tank 5, closing the valve c, starting a stirring paddle, opening a valve d, adding concentrated sulfuric acid into the primary chromium-removing calcium tank 5, adjusting the pH value of the solution to 2.0, adding sodium metabisulfite into the primary chromium-removing calcium tank 5, reacting for 24min, adding a chromium-calcium removing agent, namely soda and sodium hydroxide (the mass ratio of the soda to the sodium hydroxide is 0.9:1) into the tank 5, neutralizing the pH value to 9.8, reacting for 20min, analyzing and detecting that the solution in the primary chromium-removing calcium tank 5 contains 0.01g/L of calcium after primary calcium removal, starting a filter press pump II 11, and carrying out solid-liquid separation on the primary calcium-removing solution through a filter press II 6;
(4) opening a valve e, sending filtrate filtered by the filter press II 6 into a secondary decalcification tank 7, closing the valve e, starting a stirring paddle, adding sodium phosphate (the mass ratio of phosphorus in the calcium phosphate as a decalcification agent to calcium in the primary decalcification solution is 2.0:1) into the secondary decalcification tank 7, reacting for 18min, analyzing and detecting the calcium content of the solution in the secondary decalcification tank 7 to be 0.0003g/L, carrying out solid-liquid separation on the reacted solution through a microporous precision filter II 8, then conveying the filtrate, namely the ammonium-containing vanadium precipitation wastewater to a stripping deamination tower system to remove ammonia nitrogen, and carrying out NH deamination wastewater3-N8.3 mg/L, suspension SS 6.6 mg/L.
Comparative example 1
Adding acidic ammonium salt vanadium precipitation wastewater (0.5 g/L of silicon, 0.3g/L of calcium and 1.5g/L of hexavalent chromium) with the temperature of 55 ℃ into a chromium removal tank, adding concentrated sulfuric acid to adjust the pH value of the solution to be 2.0, then adding sodium metabisulfite, wherein the mass ratio of chromium to sodium metabisulfite is 3.2, reacting for 30min, adding soda ash into the reaction tank to neutralize the pH value to be 9.2, reacting for 30min, analyzing and detecting the solution to contain 0.26g/L of calcium and contain 0.44g/L of silicon, starting a dynamic pressure filter pump, separating the solution through a solid-liquid filter press, conveying filtrate, namely the ammonium group vanadium precipitation wastewater, to a stripping deamination tower system to remove ammonia nitrogen, and removing NH (NH) of316mg/L of N, 48mg/L of suspended substance SS, and 7.6 days of the operation cycle of the stripping deamination tower system.
Comparative example 2
Adding acidic ammonium salt vanadium precipitation wastewater (0.3 g/L of silicon, 0.2g/L of calcium and 1.3g/L of hexavalent chromium) with the temperature of 55 ℃ into a chromium removal tank, adding concentrated sulfuric acid to adjust the pH value of the solution to be 1.8, then adding sodium metabisulfite, wherein the mass ratio of chromium to sodium metabisulfite is 3.2, reacting for 30min, adding soda ash into the reaction tank to neutralize the pH value to be 9.5, reacting for 20min, analyzing and detecting the solution to contain 0.18g/L of calcium and 0.22g/L of silicon, adding a high-efficiency scale inhibition dispersing agent into the solution, starting a filter press, performing solid-liquid separation on the solution, conveying the filtrate, namely the ammonium-containing vanadium precipitation wastewater to a stripping deamination tower system to remove ammonia nitrogen, and removing ammonia-containing wastewater313mg/L of N, 160mg/L of suspended substance SS, and 38.8 days of the operation cycle of the stripping deamination tower system.
Table 1 index comparison table before acidic ammonium salt vanadium precipitation wastewater enters stripping deamination tower
| Index (I) | Example 1 | Example 2 | Example 3 | Example 4 | Comparative example 1 | Comparative example 2 |
| Silicon, g/L | 0.05 | 0.01 | 0.009 | 0.006 | 0.44 | 0.22 |
| Calcium, g/L | 0.0005 | 0.0001 | 0.0001 | 0.0003 | 0.26 | 0.18 |
| Suspended matter SS, g/L | 8.5 | 6.4 | 5.7 | 6.6 | 48 | 160 |
Table 2 comparison table of operation cycle of stripping deamination tower system for acidic ammonium salt vanadium precipitation wastewater
| Index (I) | Example 1 | Example 2 | Example 3 | Example 4 | Comparative example 1 | Comparative example 2 |
| Period of operation | Not less than 150 days | Not less than 150 days | Not less than 150 days | Not less than 150 days | 7.6 days | 36.8 days |
The above description is only exemplary of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (6)
1. A process for improving the operation cycle of a vanadium pentoxide stripping deamination tower system is characterized by comprising the following steps:
the method comprises the following specific steps:
(1) opening a valve a, sending the acidic ammonium salt vanadium precipitation wastewater with the temperature of 50-70 ℃ into a primary desiliconization tank, closing the valve a, starting a stirring paddle, adding a desiliconization agent lime powder, reacting for 20-30 min, controlling the pH value to be 9.0-10.5, carrying out primary desiliconization, and carrying out solid-liquid separation on the primary desiliconization solution through a filter press after analyzing and detecting that the silicon content of the solution in the primary desiliconization tank is less than or equal to 0.1 g/L;
the granularity of the silica remover lime powder is 100-400 meshes, and the mass content of active CaO is more than or equal to 40%;
(2) opening a valve b, sending filtrate filtered by the filter press into a secondary desiliconization tank, closing the valve b, starting a stirring paddle, adding a desiliconization agent calcium chloride, reacting for 10-30 min, carrying out secondary desiliconization, and carrying out solid-liquid separation on the secondary desiliconization solution through a microporous precision filter after analyzing and detecting that the solution in the secondary desiliconization tank contains silicon less than or equal to 0.05 g/L;
the mass ratio of the calcium content in the calcium chloride serving as the silicon removing agent to the silicon content in the primary silicon removing liquid is 3.0: 1-7.0: 1;
(3) opening a valve c, sending filtrate filtered by a microporous precise filter into a first-stage chromium-removing calcium tank, closing the valve c, starting a stirring paddle, opening a valve d, adding concentrated sulfuric acid into the first-stage chromium-removing calcium tank, adjusting the pH value of the solution to be less than or equal to 2.5, adding a reducing agent sodium metabisulfite into the first-stage chromium-removing calcium tank, reacting for 20-30 min, adding a chromium-removing calcium agent sodium carbonate and sodium hydroxide into the first-stage chromium-removing calcium tank, neutralizing the pH value of 9.5-10.5, reacting for 10-30 min, after primary calcium removal, analyzing and detecting that the calcium content of the solution in the first-stage chromium-removing calcium tank is less than or equal to 0.06g/L, and performing solid-liquid separation on the primary chromium-removing calcium solution through a filter press;
the chromium-removing calcium agent comprises soda ash and sodium hydroxide, wherein the mass ratio of the soda ash to the sodium hydroxide is 0.6: 1-3.0: 1;
(4) opening a valve e, sending filtrate filtered by the filter press into a secondary calcium removal tank, closing the valve e, starting a stirring paddle, and adding a calcium removal agent sodium phosphate into the secondary calcium removal tank, wherein the mass ratio of the phosphorus in the calcium removal agent sodium phosphate to the calcium in the primary chromium removal calcium solution is 1.0: 1-4.0: 1; reacting for 10 min-30 min, analyzing and detecting that the calcium content of the solution in the secondary decalcification tank is less than or equal to 0.0005g/L, carrying out solid-liquid separation on the reacted solution through a microporous precision filter, and conveying the filtrate, namely the ammonium-containing vanadium precipitation wastewater to a stripping deamination tower system to remove ammonia nitrogen.
2. The process for improving the operation period of a vanadium pentoxide stripping deamination tower system as claimed in claim 1, wherein the process comprises the following steps: the particle size of the lime powder serving as the silicon removing agent in the step (1) is 200-350 meshes, the mass ratio of calcium in calcium chloride serving as the silicon removing agent in the step (2) to silicon in primary silicon removing liquid is 3.5: 1-6.0: 1, the mass ratio of soda ash serving as the chromium removing agent in the step (3) to sodium hydroxide is 0.9: 1-1.5: 1, and the mass ratio of phosphorus in sodium phosphate serving as the calcium removing agent in the step (4) to calcium in the primary chromium removing calcium liquid is 2.0: 1-3.5: 1.
3. The acidic ammonium salt pretreatment system for improving the operation period of the vanadium pentoxide stripping deamination tower, which implements the process as claimed in claim 1, comprises a first-stage desiliconization tank, a second-stage desiliconization tank, a first-stage dechromization calcium tank and a second-stage decalcification tank, and is characterized in that: the one-level desiliconization jar liquid outlet is linked together through pipeline and second grade desiliconization jar, is equipped with pressure filtration pump I, pressure filter I in proper order on the pipeline between one-level desiliconization jar and the second grade desiliconization jar, the second grade desiliconization jar is linked together through pipeline and one-level dechromization calcium jar, is equipped with transfer pump I, micropore precision filter I in proper order on the pipeline between second grade desiliconization jar and the one-level dechromization calcium jar, the one-level dechromization calcium jar is linked together through pipeline and second grade desiliconization jar, is equipped with pressure filtration pump II, pressure filter II in proper order on the pipeline between one-level dechromization calcium jar and the second grade dechromization jar, the second grade decalcification jar is linked together through pipeline and micropore precision filter II, is equipped with transfer pump II on the pipeline between second grade desiliconization jar and micropore precision filter II, II exports of.
4. The acidic ammonium salt pretreatment system for improving the operation period of the vanadium pentoxide stripping deamination tower as claimed in claim 3, wherein the acidic ammonium salt pretreatment system comprises: the sulfuric acid inlet of the first-stage chromium-removing calcium tank is connected with a sulfuric acid storage tank through a pipeline, and a sulfuric acid delivery pump is arranged on the pipeline between the first-stage chromium-removing calcium tank and the sulfuric acid storage tank.
5. The acidic ammonium salt pretreatment system for improving the operation period of the vanadium pentoxide stripping deamination tower as claimed in claim 3, wherein the acidic ammonium salt pretreatment system comprises: an acidic ammonium salt vanadium precipitation wastewater inlet of the primary silicon removal tank is provided with an acidic ammonium salt vanadium precipitation wastewater pipeline, and a valve a is arranged on the acidic ammonium salt vanadium precipitation wastewater inlet pipeline of the primary silicon removal tank.
6. The acidic ammonium salt pretreatment system for improving the operation period of the vanadium pentoxide stripping deamination tower as claimed in claim 3, wherein the acidic ammonium salt pretreatment system comprises: the inlet pipeline of the second-stage dechromization tank is provided with a valve b, the secondary dechromization solution inlet pipeline of the first-stage dechromization calcium tank is provided with a valve c, the sulfuric acid inlet pipeline of the first-stage dechromization calcium tank is provided with a valve d, and the inlet pipeline of the second-stage dechromization tank is provided with a valve e.
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| CN1724406A (en) * | 2005-06-20 | 2006-01-25 | 李强国 | Process for treating industrial waste water containing chromium, vanadium |
| CN102795721A (en) * | 2012-07-28 | 2012-11-28 | 中信锦州金属股份有限公司 | Treatment method for wastewater after vanadium precipitation |
| KR20130001839A (en) * | 2011-06-28 | 2013-01-07 | 정대준 | Mineral water manufacturing method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1724406A (en) * | 2005-06-20 | 2006-01-25 | 李强国 | Process for treating industrial waste water containing chromium, vanadium |
| KR20130001839A (en) * | 2011-06-28 | 2013-01-07 | 정대준 | Mineral water manufacturing method |
| CN102795721A (en) * | 2012-07-28 | 2012-11-28 | 中信锦州金属股份有限公司 | Treatment method for wastewater after vanadium precipitation |
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