CN112619286A - Method for purifying and crystallizing titanium dioxide solution - Google Patents
Method for purifying and crystallizing titanium dioxide solution Download PDFInfo
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- CN112619286A CN112619286A CN202011497394.8A CN202011497394A CN112619286A CN 112619286 A CN112619286 A CN 112619286A CN 202011497394 A CN202011497394 A CN 202011497394A CN 112619286 A CN112619286 A CN 112619286A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D37/00—Processes of filtration
- B01D37/02—Precoating the filter medium; Addition of filter aids to the liquid being filtered
- B01D37/025—Precoating the filter medium; Addition of filter aids to the liquid being filtered additives incorporated in the filter
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- C—CHEMISTRY; METALLURGY
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- C01G23/00—Compounds of titanium
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Abstract
The invention discloses a method for purifying and crystallizing titanium dioxide by acidolysis, which belongs to the technical field of titanium dioxide acidolysis, and is characterized in that a tubular filter is adopted for filtration, a filter aid is perlite, and the temperature of titanium dioxide feed liquid entering the tubular filter is 50-65 ℃. By improving the tubular filter and the filtering operation steps, the invention not only solves the problem of poor filtering effect caused by crystallization and the like, but also improves the efficiency by 56 percent compared with the prior plate-and-frame filter press, and the same is 450m when 15 ten thousand tons of titanium dioxide are produced per year2The tubular filter can meet the production of titanium dioxide with the annual output of 15 ten thousand tons, and the plate-and-frame filter press can only meet the production requirement of 6 to 8 ten thousand tons per year.
Description
Technical Field
The invention belongs to the technical field of titanium dioxide acidolysis, and particularly relates to a method for purifying and crystallizing acidolysis titanium liquid.
Background
Since the production of the titanium dioxide by the sulfuric acid method in 20 th century began in 50 s, particularly, the production process technology is continuously developed and innovated in recent ten years, and a plurality of novel improved equipment devices are widely applied to the titanium dioxide industry, so that the titanium dioxide production industry is rapidly developed. In the production process of titanium dioxide by a sulfuric acid method, clear titanium liquid settled by a thickener still contains colloids, fine crystals and mechanical impurities, heavy metal ions are adsorbed on the surfaces of the colloids, and if the heavy metal ions are not removed, poor crystal centers can be formed during hydrolysis, and the size and the shape of metatitanic acid particles are influenced, so that the quality (particularly whiteness and decolorization) of a finished product is influenced finally. The plate-and-frame filter press applied to the working procedure has the advantages of low manufacturing cost, simple structure, simple operation and the like, but also has the defects of large degree of manual intervention on the filtering quality, large occupied area, high labor intensity, poor labor environment, low automation degree and the like.
The patent publication No. CN106966427A discloses a method for purifying titanium acidolysis solution and a filter used in the method, and proposes that a tubular filter is used for replacing the operation of a traditional plate-and-frame filter press, titanium solution is added into the tubular filter for filtration, qualified filtrate enters the next process, when the pressure in the tubular filter reaches 0.35MPa or the outlet flow is reduced by half or the set filtration time is reached (temporarily set for 6 hours), the filtration is automatically stopped, and the pressure discharge stage is entered. And (3) discharging the diatomite sludge into a pulping tank by using air pressure, opening a total manual valve of the sand filter pipe to clean the tubular filter, and sending the cleaned diatomite slurry to secondary filter pressing. The tubular filter is characterized mainly by the following aspects: 1. the filtering quality is stable and is less interfered by manual work, and the filtering precision can reach 10 x 10-6The following; 2. the tubular filter has high automation degree, can realize various control modes, has less operation workload, only needs to operate a control button and has low labor intensity; 3. the tubular filter has small floor area and effectively utilizes narrow space.
However, in the actual operation process, the following problems are found in the titanium liquid filtered by using the tubular filter:
1. the titanium liquid is easy to crystallize and block the tubular filter during filtration, so that the problem of poor filtration effect is caused;
2. the diatomite carries a large amount of iron and calcium ions, and the filtering effect is further influenced;
3. the titanium oxysulfate solution has high sulfuric acid content and strong acidity, and the filtering cloth is corroded for a long time to cause penetration, so that the solid content of the titanium liquid is unqualified, and in addition, after the titanium oxysulfate solution is used for a long time, the holes of the filtering bag are gradually blocked, the filtering performance is also reduced, and the tubular filter belongs to a closed filtering container, so that the filtering cloth is more complicated to replace, and the service life of the filtering cloth is particularly important.
Disclosure of Invention
The invention aims to provide a method for purifying and crystallizing acidolysis titanium liquid, which aims to solve the technical problem of poor filtering effect caused by crystallization and problems in the process of filtering the titanium liquid by using a tubular filter.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a method for purifying and crystallizing titanium liquid by acidolysis adopts a tubular filter for filtration, the filter aid adopts perlite, and the temperature of titanium liquid feeding liquid entering the tubular filter is 50-65 ℃.
Preferably, the filtration with the tubular filter specifically comprises the following operating steps:
(1) liquid charging and gas discharging: filling the raw material liquid into the tubular filter until the liquid level reaches a high liquid level;
(2) pre-blowback: compressed air is firstly introduced for scrubbing, and then compressed air is introduced for back blowing the filter element from inside to outside;
(3) pre-scrubbing: pre-coating liquid formed by premixing raw material liquid and perlite is filled in a tubular filter until the liquid level reaches a high liquid level;
(4) pre-coating circulation: opening a pre-coating liquid reflux valve to enable the pre-coating liquid to circulate in the tubular filter for 30-45 minutes, and entering the next step when the solid content of the filtrate is qualified;
(5) pre-filtering: stopping the pre-coating circulation, introducing a raw material liquid, performing pre-filtration for 5-10 minutes, and refluxing the pre-filtered clear liquid into the raw material liquid;
(6) and (3) filtering: starting filtering, regularly monitoring the solid content of filtrate, feeding the filtered qualified clear liquid into the next procedure, refluxing unqualified filtrate into the raw material liquid, alarming when the pressure value fed back by a pressure transmitter of the tubular filter reaches a preset value of 0.25-0.40 MPa, or continuously filtering for 5-6 hours, and stopping filtering;
(7) pressure drainage and filtration: stopping introducing the raw material liquid, discharging the liquid in the tubular filter by applying air pressure, and refluxing the discharged liquid into the raw material liquid;
(8) back flushing: compressed air is firstly introduced for scrubbing, and then compressed air is introduced for back blowing the filter element from inside to outside;
(9) deslagging: discharging perlite sludge in the tubular filter;
(10) and (4) spraying, namely spraying and washing the tubular filter by using clear water or dilute acid, and then performing the next round of use after the tubular filter is washed.
Preferably, in the step (3), the pre-coating solution is prepared by mixing and stirring the titanium solution and the perlite at 50-60 ℃, and the stirring time is at least 30 minutes.
Preferably, in the steps (5) and (6), the feeding amount of the raw material liquid is 40-70 m3/h。
Preferably, the filter cloth of the tubular filter is soaked by dilute acid periodically, and is cleaned by clean water after soaking.
Compared with the prior art, the invention has the following beneficial effects:
1. by improving the tubular filter and the filtering operation steps, the invention not only solves the problem of poor filtering effect caused by crystallization and the like, but also improves the efficiency by 56 percent compared with the prior plate-and-frame filter press, and the same is 450m when 15 ten thousand tons of titanium dioxide are produced per year2The tubular filter can meet the production of titanium dioxide with the annual output of 15 ten thousand tons, and the plate-and-frame filter press can only meet the production requirement of 6 to 8 ten thousand tons per year;
2. the profit of the single tubular filtering, purifying and crystallizing device obtained in the aspect of automation improvement is about 16.2 ten thousand yuan per year, the filtering efficiency is improved, and the cost can be reduced by about 45.48 ten thousand yuan per year in water resource saving. The total economic benefit of a single creation is about 61.68 ten thousand yuan;
3. the invention can improve the service life of the filter cloth of the tubular filter by at least more than 50 percent by soaking the filter cloth of the tubular filter with dilute acid and cleaning the filter cloth with clean water after soaking.
Detailed Description
The present invention is further illustrated by the following examples, which include, but are not limited to, the following examples.
Example 1
In this example, the filter aid was perlite and the temperature of the titanium feed solution entering the tubular filter was 60 ℃ to 65 ℃. The filter aid is prepared by mixing and stirring titanium liquid at 55-60 ℃ and perlite, the dosage of the perlite in a single batch is 80-100 Kg, namely 4-5 bags (one bag with 20Kg), the stirring time is at least 30 minutes, the filter aid is uniformly prepared, and the quality of a filter aid layer is ensured.
The specific filtering steps are as follows:
1. preparation of precoated filter aid
1.1 manually opening a titanium liquid valve of a perlite slurry storage tank and a filter aid preparation tank, adding titanium liquid into the filter aid preparation tank, and starting the filter aid preparation tank to stir when the titanium liquid submerges a stirring paddle;
1.2 when the titanium liquid reaches 70% of the liquid level of the filter aid preparation tank, stopping feeding the filter aid preparation tank, closing a titanium liquid valve and stopping discharging;
1.3 adding perlite with a specified technical amount into a filter aid preparation tank and stirring for 30 min;
2. normal filtration step
2.1, filling and exhausting of the filter: opening a turbid liquid valve XV01 at the inlet of the tubular filter pump, an air-operated valve XV24 at the outlet of the tubular filter pump and an inlet valve XV23, starting a liquid supply pump, conveying the stock solution to the filter by the liquid supply pump, when the liquid level reaches a high liquid level, alarming by a liquid level switch LS01, closing the turbid liquid valve XV01, the inlet valve XV23 and the liquid supply pump, and ending the liquid filling of the filter at the moment. After the preparation is completed, the filter enters an automatic operation stage.
2.2, pre-back flushing of a filter: and opening the gas scrubbing valve XV03, introducing compressed air for scrubbing for 90s (adjustable), and closing the gas scrubbing valve XV 03. Opening an air back-blowing valve XV09, opening grouping valves XV 11-XV 16 one by one (back-blowing time is 10s each time, interval is 5s is adjustable, back-blowing is performed for 1 time in each group), introducing compressed air to back-blow the filter element from inside to outside, and closing an air back-blowing valve XV09 after pre-back blowing is finished.
2.3 filter refill liquid: the precoating liquid valve XV02, pump outlet pneumatic valve XV24 and inlet valve XV23 of the filter are opened, and the liquid feed pump is started (the feed flow is set to 80 m)3And h, the frequency converter automatically controls instantaneous flow in an interlocking manner), the liquid supply pump conveys the precoating liquid into the filter, and when the liquid level reaches a high liquid level, the liquid level switch LS01 gives an alarm to enter a precoating circulation stage.
2.4 Pre-coat cycle: opening grouping valves XV 11-XV 16 and a precoating liquid return valve XV08 of the filter, closing an exhaust valve XV06D, and enabling the filter to enter a precoating cycle stage. The circulation time is 30-45 minutes (adjustable), and samples are taken to detect whether the solid content of the filtrate is qualified (qualified below 0.03 g/L), and the qualified filtrate enters the next procedure.
2.5, pre-filtering: the filtrate turbidity valve XV01 was opened (feed flow 50 m)3H) and a clear liquid reflux valve XV17, closing a pre-coating liquid reflux valve XV08 after 10s, closing a pre-coating liquid reflux valve XV02 after 20s, enabling a filter to enter a pre-filtering state, wherein the pre-filtering time is 5-10 minutes (adjustable), and the filter stage is started after the pre-filtering time is up.
2.6, filtering: the clear liquid outlet valve XV10 of the filter is opened, and after 5s, the clear liquid return valve XV17 is closed to start filtration. During the filtration, a filtrate sample is taken in real time at a post for suction filtration, the solid content condition of the filter paper is monitored (qualified below 0.03 g/L), and unqualified titanium liquid is prevented from entering the next procedure.
2.7, gradually increasing the pressure difference between the inlet and the outlet of the filter along with the filtering, alarming when the pressure value fed back by the pressure transmitter PI T01 on the tank body reaches a preset value of 0.25-0.40 MPa (adjustable), or continuously filtering for 5-6 hours (adjustable), stopping filtering at this moment, and entering a pressure discharge filtering stage; or manually triggering the stop filter, which then completes the rest of the steps in the automatic run.
2.8 pressure filtration: the method comprises the steps of firstly opening a gas squeezing valve XV04 and a clear liquid return valve XV17, stopping a liquid supply pump after 5s, closing a filter turbid liquid valve XV01, a pump outlet pneumatic valve XV24 and a clear liquid outlet valve XV10, carrying out pressure drainage for a period of time (10min, adjustable), opening a bottom drain valve XV19, returning liquid in the filter to a washing liquid storage tank, carrying out pressure drainage for a period of time (3min, adjustable), closing a gas squeezing valve XV04, delaying 60s, and closing a clear liquid return valve XV17, a grouping valve XV 11-XV 16 and a bottom drain valve XV 19.
2.9 back flushing and slag discharging: opening an exhaust valve XV06 of the filter, opening a slag discharge valve XV21 and XV22 after an interval of 5s, opening an air back-flushing valve XV09 and a grouping valve XV11 after an interval of 5s, closing a grouping valve XV11 after 10s, opening a grouping valve XV12 after an interval of 5s, closing a grouping valve XV12 after 10s, opening a grouping valve XV13 after 5s, performing back flushing on other groups respectively (the grouping back flushing is performed for one time, three back flushing is performed, and the back flushing frequency is adjustable) according to the operation, and closing all grouping valves XV16 and the air back-flushing valve XV09 after the back flushing is finished; discharging perlite sludge.
2.10 spraying: opening a clean water inlet valve XV01Q (whether to open a dilute acid inlet valve HV01S can be determined according to field conditions), opening a spray valve XV05 after delaying for 5s, closing a clean water inlet valve XV01 after lasting for 5min, closing the spray valve XV05 at an interval of 5s, and closing an exhaust valve XV06 and deslagging valves XV21 and XV22 after delaying for 3 min.
2.11 at this point, one filtration cycle of the clean titanium liquid is over and the tube filter can be used for the next time.
In the embodiment, the filtering effect is good, the solid content of the filtrate is maintained below 0.03g/L, the filtering operation is not stopped by alarming after continuous filtering for 6 hours, the requirement of the next procedure can be met, and the trial operation effect of the next procedure is good.
Example 2
In this example, the filter aid was perlite and the temperature of the titanium feed solution entering the tubular filter was 50 ℃ to 55 ℃. The filter aid is prepared by mixing and stirring titanium liquid at 50-55 ℃ and perlite, the dosage of the perlite in a single batch is 80-100 Kg, namely 4-5 bags (one bag with 20Kg), the stirring time is at least 30 minutes, the filter aid is uniformly prepared, and the quality of a filter aid layer is ensured.
The specific filtering steps are as follows:
1. preparation of precoated filter aid
1.1 manually opening a titanium liquid valve of a perlite slurry storage tank and a filter aid preparation tank, adding titanium liquid into the filter aid preparation tank, and starting the filter aid preparation tank to stir when the titanium liquid submerges a stirring paddle;
1.2 when the titanium liquid reaches 70% of the liquid level of the filter aid preparation tank, stopping feeding the filter aid preparation tank, closing a titanium liquid valve and stopping discharging;
1.3 adding perlite with a specified technical amount into a filter aid preparation tank and stirring for 30 min;
2. normal filtration step
2.1, filling and exhausting of the filter: opening a turbid liquid valve XV01 at the inlet of the tubular filter pump, an air-operated valve XV24 at the outlet of the tubular filter pump and an inlet valve XV23, starting a liquid supply pump, conveying the stock solution to the filter by the liquid supply pump, when the liquid level reaches a high liquid level, alarming by a liquid level switch LS01, closing the turbid liquid valve XV01, the inlet valve XV23 and the liquid supply pump, and ending the liquid filling of the filter at the moment. After the preparation is completed, the filter enters an automatic operation stage.
2.2, pre-back flushing of a filter: and opening the gas scrubbing valve XV03, introducing compressed air for scrubbing for 90s (adjustable), and closing the gas scrubbing valve XV 03. Opening an air back-blowing valve XV09, opening grouping valves XV 11-XV 16 one by one (back-blowing time is 10s each time, interval is 5s is adjustable, back-blowing is performed for 1 time in each group), introducing compressed air to back-blow the filter element from inside to outside, and closing an air back-blowing valve XV09 after pre-back blowing is finished.
2.3 filter refill liquid: the precoating liquid valve XV02, pump outlet pneumatic valve XV24 and inlet valve XV23 of the filter are opened, and the liquid feed pump is started (the feed flow is set to 80 m)3And h, the frequency converter automatically controls instantaneous flow in an interlocking manner), the liquid supply pump conveys the precoating liquid into the filter, and when the liquid level reaches a high liquid level, the liquid level switch LS01 gives an alarm to enter a precoating circulation stage.
2.4 Pre-coat cycle: opening grouping valves XV 11-XV 16 and a precoating liquid return valve XV08 of the filter, closing an exhaust valve XV06D, and enabling the filter to enter a precoating cycle stage. The circulation time is 30-45 minutes (adjustable), and samples are taken to detect whether the solid content of the filtrate is qualified (qualified below 0.03 g/L), and the qualified filtrate enters the next procedure.
2.5, pre-filtering: the filtrate turbidity valve XV01 was opened (feed flow 50 m)3H) and a clear liquid reflux valve XV17, closing a pre-coating liquid reflux valve XV08 after 10s, closing a pre-coating liquid reflux valve XV02 after 20s, enabling a filter to enter a pre-filtering state, wherein the pre-filtering time is 5-10 minutes (adjustable), and the filter stage is started after the pre-filtering time is up.
2.6, filtering: the clear liquid outlet valve XV10 of the filter is opened, and after 5s, the clear liquid return valve XV17 is closed to start filtration. During the filtration, a filtrate sample is taken in real time at a post for suction filtration, the solid content condition of the filter paper is monitored (qualified below 0.03 g/L), and unqualified titanium liquid is prevented from entering the next procedure.
2.7, gradually increasing the pressure difference between the inlet and the outlet of the filter along with the filtering, alarming when the pressure value fed back by the pressure transmitter PI T01 on the tank body reaches a preset value of 0.25-0.40 MPa (adjustable), or continuously filtering for 5-6 hours (adjustable), stopping filtering at this moment, and entering a pressure discharge filtering stage; or manually triggering the stop filter, which then completes the rest of the steps in the automatic run.
2.8 pressure filtration: the method comprises the steps of firstly opening a gas squeezing valve XV04 and a clear liquid return valve XV17, stopping a liquid supply pump after 5s, closing a filter turbid liquid valve XV01, a pump outlet pneumatic valve XV24 and a clear liquid outlet valve XV10, carrying out pressure drainage for a period of time (10min, adjustable), opening a bottom drain valve XV19, returning liquid in the filter to a washing liquid storage tank, carrying out pressure drainage for a period of time (3min, adjustable), closing a gas squeezing valve XV04, delaying 60s, and closing a clear liquid return valve XV17, a grouping valve XV 11-XV 16 and a bottom drain valve XV 19.
2.9 back flushing and slag discharging: opening an exhaust valve XV06 of the filter, opening a slag discharge valve XV21 and XV22 after an interval of 5s, opening an air back-flushing valve XV09 and a grouping valve XV11 after an interval of 5s, closing a grouping valve XV11 after 10s, opening a grouping valve XV12 after an interval of 5s, closing a grouping valve XV12 after 10s, opening a grouping valve XV13 after 5s, performing back flushing on other groups respectively (the grouping back flushing is performed for one time, three back flushing is performed, and the back flushing frequency is adjustable) according to the operation, and closing all grouping valves XV16 and the air back-flushing valve XV09 after the back flushing is finished; discharging perlite sludge.
2.10 spraying: opening a clean water inlet valve XV01Q (whether to open a dilute acid inlet valve HV01S can be determined according to field conditions), opening a spray valve XV05 after delaying for 5s, closing a clean water inlet valve XV01 after lasting for 5min, closing the spray valve XV05 at an interval of 5s, and closing an exhaust valve XV06 and deslagging valves XV21 and XV22 after delaying for 3 min.
2.11 at this point, one filtration cycle of the clean titanium liquid is over and the tube filter can be used for the next time.
In the embodiment, the filtering effect is good, the solid content of the filtrate is maintained below 0.03g/L, the filtering operation is stopped by alarming after 5 hours of filtering, the requirement of the next procedure can be met, and the trial operation effect of the next procedure is good.
Example 3
In this example, the filter aid was perlite and the temperature of the titanium feed solution entering the tubular filter was 40 ℃ to 45 ℃. The filter aid is prepared by mixing and stirring titanium liquid at 45-50 ℃ and perlite, the dosage of the perlite in a single batch is 80-100 Kg, namely 4-5 bags (one bag with 20Kg), the stirring time is at least 30 minutes, the filter aid is uniformly prepared, and the quality of a filter aid layer is ensured.
The specific filtering steps are as follows:
1. preparation of precoated filter aid
1.1 manually opening a titanium liquid valve of a perlite slurry storage tank and a filter aid preparation tank, adding titanium liquid into the filter aid preparation tank, and starting the filter aid preparation tank to stir when the titanium liquid submerges a stirring paddle;
1.2 when the titanium liquid reaches 70% of the liquid level of the filter aid preparation tank, stopping feeding the filter aid preparation tank, closing a titanium liquid valve and stopping discharging;
1.3 adding perlite with a specified technical amount into a filter aid preparation tank and stirring for 30 min;
2. normal filtration step
2.1, filling and exhausting of the filter: opening a turbid liquid valve XV01 at the inlet of the tubular filter pump, an air-operated valve XV24 at the outlet of the tubular filter pump and an inlet valve XV23, starting a liquid supply pump, conveying the stock solution to the filter by the liquid supply pump, when the liquid level reaches a high liquid level, alarming by a liquid level switch LS01, closing the turbid liquid valve XV01, the inlet valve XV23 and the liquid supply pump, and ending the liquid filling of the filter at the moment. After the preparation is completed, the filter enters an automatic operation stage.
2.2, pre-back flushing of a filter: and opening the gas scrubbing valve XV03, introducing compressed air for scrubbing for 90s (adjustable), and closing the gas scrubbing valve XV 03. Opening an air back-blowing valve XV09, opening grouping valves XV 11-XV 16 one by one (back-blowing time is 10s each time, interval is 5s is adjustable, back-blowing is performed for 1 time in each group), introducing compressed air to back-blow the filter element from inside to outside, and closing an air back-blowing valve XV09 after pre-back blowing is finished.
2.3 filter refill liquid: the precoating liquid valve XV02, pump outlet pneumatic valve XV24 and inlet valve XV23 of the filter are opened, and the liquid feed pump is started (the feed flow is set to 80 m)3And h, the frequency converter automatically controls instantaneous flow in an interlocking manner), the liquid supply pump conveys the precoating liquid into the filter, and when the liquid level reaches a high liquid level, the liquid level switch LS01 gives an alarm to enter a precoating circulation stage.
2.4 Pre-coat cycle: opening grouping valves XV 11-XV 16 and a precoating liquid return valve XV08 of the filter, closing an exhaust valve XV06D, and enabling the filter to enter a precoating cycle stage. The circulation time is 30-45 minutes (adjustable), and samples are taken to detect whether the solid content of the filtrate is qualified (qualified below 0.03 g/L), and the qualified filtrate enters the next procedure.
2.5, pre-filtering: the filtrate turbidity valve XV01 was opened (feed flow 50 m)3H) and a clear liquid reflux valve XV17, closing a pre-coating liquid reflux valve XV08 after 10s, closing a pre-coating liquid reflux valve XV02 after 20s, enabling a filter to enter a pre-filtering state, wherein the pre-filtering time is 5-10 minutes (adjustable), and the filter stage is started after the pre-filtering time is up.
2.6, filtering: the clear liquid outlet valve XV10 of the filter is opened, and after 5s, the clear liquid return valve XV17 is closed to start filtration. During the filtration, a filtrate sample is taken in real time at a post for suction filtration, the solid content condition of the filter paper is monitored (qualified below 0.03 g/L), and unqualified titanium liquid is prevented from entering the next procedure.
2.7, gradually increasing the pressure difference between the inlet and the outlet of the filter along with the filtering, alarming when the pressure value fed back by the pressure transmitter PI T01 on the tank body reaches a preset value of 0.25-0.40 MPa (adjustable), or continuously filtering for 5-6 hours (adjustable), stopping filtering at this moment, and entering a pressure discharge filtering stage; or manually triggering the stop filter, which then completes the rest of the steps in the automatic run.
2.8 pressure filtration: the method comprises the steps of firstly opening a gas squeezing valve XV04 and a clear liquid return valve XV17, stopping a liquid supply pump after 5s, closing a filter turbid liquid valve XV01, a pump outlet pneumatic valve XV24 and a clear liquid outlet valve XV10, carrying out pressure drainage for a period of time (10min, adjustable), opening a bottom drain valve XV19, returning liquid in the filter to a washing liquid storage tank, carrying out pressure drainage for a period of time (3min, adjustable), closing a gas squeezing valve XV04, delaying 60s, and closing a clear liquid return valve XV17, a grouping valve XV 11-XV 16 and a bottom drain valve XV 19.
2.9 back flushing and slag discharging: opening an exhaust valve XV06 of the filter, opening a slag discharge valve XV21 and XV22 after an interval of 5s, opening an air back-flushing valve XV09 and a grouping valve XV11 after an interval of 5s, closing a grouping valve XV11 after 10s, opening a grouping valve XV12 after an interval of 5s, closing a grouping valve XV12 after 10s, opening a grouping valve XV13 after 5s, performing back flushing on other groups respectively (the grouping back flushing is performed for one time, three back flushing is performed, and the back flushing frequency is adjustable) according to the operation, and closing all grouping valves XV16 and the air back-flushing valve XV09 after the back flushing is finished; discharging perlite sludge.
2.10 spraying: opening a clean water inlet valve XV01Q (whether to open a dilute acid inlet valve HV01S can be determined according to field conditions), opening a spray valve XV05 after delaying for 5s, closing a clean water inlet valve XV01 after lasting for 5min, closing the spray valve XV05 at an interval of 5s, and closing an exhaust valve XV06 and deslagging valves XV21 and XV22 after delaying for 3 min.
2.11 at this point, one filtration cycle of the clean titanium liquid is over and the tube filter can be used for the next time.
In the embodiment, the filtering effect is good, the solid content of the filtrate is maintained below 0.03g/L, the filtering operation is stopped by alarming after 2 hours of filtering, the requirement of the next procedure can be met, and the trial operation effect of the next procedure is good.
Example 4
In this example, the filter aid was diatomaceous earth, and the temperature of the titanium feed solution entering the tubular filter was 40 ℃ to 45 ℃. The filter aid is prepared by mixing and stirring titanium liquid at 45-50 ℃ and diatomite, wherein the dosage of the diatomite is 80-100 Kg for a single batch, the stirring time is at least 30 minutes, the filter aid is uniformly prepared, and the quality of a filter aid layer is ensured.
The specific filtering steps are as follows:
1. preparation of precoated filter aid
1.1 manually opening a titanium liquid valve of a diatomite slurry storage tank and a filter aid preparation tank, adding titanium liquid into the filter aid preparation tank, and starting the filter aid preparation tank to stir when the titanium liquid submerges a stirring paddle;
1.2 when the titanium liquid reaches 70% of the liquid level of the filter aid preparation tank, stopping feeding the filter aid preparation tank, closing a titanium liquid valve and stopping discharging;
1.3 adding diatomite with a specified technical amount into a filter aid preparation tank and stirring for 30 min;
2. normal filtration step
2.1, filling and exhausting of the filter: opening a turbid liquid valve XV01 at the inlet of the tubular filter pump, an air-operated valve XV24 at the outlet of the tubular filter pump and an inlet valve XV23, starting a liquid supply pump, conveying the stock solution to the filter by the liquid supply pump, when the liquid level reaches a high liquid level, alarming by a liquid level switch LS01, closing the turbid liquid valve XV01, the inlet valve XV23 and the liquid supply pump, and ending the liquid filling of the filter at the moment. After the preparation is completed, the filter enters an automatic operation stage.
2.2, pre-back flushing of a filter: and opening the gas scrubbing valve XV03, introducing compressed air for scrubbing for 90s (adjustable), and closing the gas scrubbing valve XV 03. Opening an air back-blowing valve XV09, opening grouping valves XV 11-XV 16 one by one (back-blowing time is 10s each time, interval is 5s is adjustable, back-blowing is performed for 1 time in each group), introducing compressed air to back-blow the filter element from inside to outside, and closing an air back-blowing valve XV09 after pre-back blowing is finished.
2.3 filter refill liquid: the precoating liquid valve XV02, pump outlet pneumatic valve XV24 and inlet valve XV23 of the filter are opened, and the liquid feed pump is started (the feed flow is set to 80 m)3And h, the frequency converter automatically controls instantaneous flow in an interlocking manner), the liquid supply pump conveys the precoating liquid into the filter, and when the liquid level reaches a high liquid level, the liquid level switch LS01 gives an alarm to enter a precoating circulation stage.
2.4 Pre-coat cycle: opening grouping valves XV 11-XV 16 and a precoating liquid return valve XV08 of the filter, closing an exhaust valve XV06D, and enabling the filter to enter a precoating cycle stage. The circulation time is 30-45 minutes (adjustable), and samples are taken to detect whether the solid content of the filtrate is qualified (qualified below 0.03 g/L), and the qualified filtrate enters the next procedure.
2.5, pre-filtering: the filtrate turbidity valve XV01 was opened (feed flow 50 m)3H) and a clear liquid reflux valve XV17, closing a pre-coating liquid reflux valve XV08 after 10s, closing a pre-coating liquid reflux valve XV02 after 20s, enabling a filter to enter a pre-filtering state, wherein the pre-filtering time is 5-10 minutes (adjustable), and the filter stage is started after the pre-filtering time is up.
2.6, filtering: the clear liquid outlet valve XV10 of the filter is opened, and after 5s, the clear liquid return valve XV17 is closed to start filtration. During the filtration, a filtrate sample is taken in real time at a post for suction filtration, the solid content condition of the filter paper is monitored (qualified below 0.03 g/L), and unqualified titanium liquid is prevented from entering the next procedure.
2.7, gradually increasing the pressure difference between the inlet and the outlet of the filter along with the filtering, alarming when the pressure value fed back by the pressure transmitter PI T01 on the tank body reaches a preset value of 0.25-0.40 MPa (adjustable), or continuously filtering for 5-6 hours (adjustable), stopping filtering at this moment, and entering a pressure discharge filtering stage; or manually triggering the stop filter, which then completes the rest of the steps in the automatic run.
2.8 pressure filtration: the method comprises the steps of firstly opening a gas squeezing valve XV04 and a clear liquid return valve XV17, stopping a liquid supply pump after 5s, closing a filter turbid liquid valve XV01, a pump outlet pneumatic valve XV24 and a clear liquid outlet valve XV10, carrying out pressure drainage for a period of time (10min, adjustable), opening a bottom drain valve XV19, returning liquid in the filter to a washing liquid storage tank, carrying out pressure drainage for a period of time (3min, adjustable), closing a gas squeezing valve XV04, delaying 60s, and closing a clear liquid return valve XV17, a grouping valve XV 11-XV 16 and a bottom drain valve XV 19.
2.9 back flushing and slag discharging: opening an exhaust valve XV06 of the filter, opening a slag discharge valve XV21 and XV22 after an interval of 5s, opening an air back-flushing valve XV09 and a grouping valve XV11 after an interval of 5s, closing a grouping valve XV11 after 10s, opening a grouping valve XV12 after an interval of 5s, closing a grouping valve XV12 after 10s, opening a grouping valve XV13 after 5s, performing back flushing on other groups respectively (the grouping back flushing is performed for one time, three back flushing is performed, and the back flushing frequency is adjustable) according to the operation, and closing all grouping valves XV16 and the air back-flushing valve XV09 after the back flushing is finished; and discharging the diatomite sludge.
2.10 spraying: opening a clean water inlet valve XV01Q (whether to open a dilute acid inlet valve HV01S can be determined according to field conditions), opening a spray valve XV05 after delaying for 5s, closing a clean water inlet valve XV01 after lasting for 5min, closing the spray valve XV05 at an interval of 5s, and closing an exhaust valve XV06 and deslagging valves XV21 and XV22 after delaying for 3 min.
2.11 at this point, one filtration cycle of the clean titanium liquid is over and the tube filter can be used for the next time.
In the embodiment, the filtering effect is poor, the solid content of the filtrate is difficult to maintain below 0.03g/L, the filtering operation is stopped by alarming after filtering for 0.5 hour, the requirement of the next procedure can be met, and the trial operation effect of the next procedure is good.
Example 5
In this example, the filter aid was diatomaceous earth, and the temperature of the titanium feed solution entering the tubular filter was 60 ℃ to 65 ℃. The filter aid is prepared by mixing and stirring titanium liquid at 55-60 ℃ and diatomite, wherein the dosage of the diatomite is 80-100 Kg for a single batch, the stirring time is at least 30 minutes, the filter aid is uniformly prepared, and the quality of a filter aid layer is ensured.
The specific filtering steps are as follows:
1. preparation of precoated filter aid
1.1 manually opening a titanium liquid valve of a diatomite slurry storage tank and a filter aid preparation tank, adding titanium liquid into the filter aid preparation tank, and starting the filter aid preparation tank to stir when the titanium liquid submerges a stirring paddle;
1.2 when the titanium liquid reaches 70% of the liquid level of the filter aid preparation tank, stopping feeding the filter aid preparation tank, closing a titanium liquid valve and stopping discharging;
1.3 adding diatomite with a specified technical amount into a filter aid preparation tank and stirring for 30 min;
2. normal filtration step
2.1, filling and exhausting of the filter: opening a turbid liquid valve XV01 at the inlet of the tubular filter pump, an air-operated valve XV24 at the outlet of the tubular filter pump and an inlet valve XV23, starting a liquid supply pump, conveying the stock solution to the filter by the liquid supply pump, when the liquid level reaches a high liquid level, alarming by a liquid level switch LS01, closing the turbid liquid valve XV01, the inlet valve XV23 and the liquid supply pump, and ending the liquid filling of the filter at the moment. After the preparation is completed, the filter enters an automatic operation stage.
2.2, pre-back flushing of a filter: and opening the gas scrubbing valve XV03, introducing compressed air for scrubbing for 90s (adjustable), and closing the gas scrubbing valve XV 03. Opening an air back-blowing valve XV09, opening grouping valves XV 11-XV 16 one by one (back-blowing time is 10s each time, interval is 5s is adjustable, back-blowing is performed for 1 time in each group), introducing compressed air to back-blow the filter element from inside to outside, and closing an air back-blowing valve XV09 after pre-back blowing is finished.
2.3 filter refill liquid: the precoating liquid valve XV02, pump outlet pneumatic valve XV24 and inlet valve XV23 of the filter are opened, and the liquid feed pump is started (the feed flow is set to 80 m)3And h, the frequency converter automatically controls instantaneous flow in an interlocking manner), the liquid supply pump conveys the precoating liquid into the filter, and when the liquid level reaches a high liquid level, the liquid level switch LS01 gives an alarm to enter a precoating circulation stage.
2.4 Pre-coat cycle: opening grouping valves XV 11-XV 16 and a precoating liquid return valve XV08 of the filter, closing an exhaust valve XV06D, and enabling the filter to enter a precoating cycle stage. The circulation time is 30-45 minutes (adjustable), and samples are taken to detect whether the solid content of the filtrate is qualified (qualified below 0.03 g/L), and the qualified filtrate enters the next procedure.
2.5, pre-filtering: the filtrate turbidity valve XV01 was opened (feed flow 50 m)3H) and a clear liquid reflux valve XV17, closing a pre-coating liquid reflux valve XV08 after 10s, closing a pre-coating liquid reflux valve XV02 after 20s, enabling a filter to enter a pre-filtering state, wherein the pre-filtering time is 5-10 minutes (adjustable), and the filter stage is started after the pre-filtering time is up.
2.6, filtering: the clear liquid outlet valve XV10 of the filter is opened, and after 5s, the clear liquid return valve XV17 is closed to start filtration. During the filtration, a filtrate sample is taken in real time at a post for suction filtration, the solid content condition of the filter paper is monitored (qualified below 0.03 g/L), and unqualified titanium liquid is prevented from entering the next procedure.
2.7, gradually increasing the pressure difference between the inlet and the outlet of the filter along with the filtering, alarming when the pressure value fed back by the pressure transmitter PI T01 on the tank body reaches a preset value of 0.25-0.40 MPa (adjustable), or continuously filtering for 5-6 hours (adjustable), stopping filtering at this moment, and entering a pressure discharge filtering stage; or manually triggering the stop filter, which then completes the rest of the steps in the automatic run.
2.8 pressure filtration: the method comprises the steps of firstly opening a gas squeezing valve XV04 and a clear liquid return valve XV17, stopping a liquid supply pump after 5s, closing a filter turbid liquid valve XV01, a pump outlet pneumatic valve XV24 and a clear liquid outlet valve XV10, carrying out pressure drainage for a period of time (10min, adjustable), opening a bottom drain valve XV19, returning liquid in the filter to a washing liquid storage tank, carrying out pressure drainage for a period of time (3min, adjustable), closing a gas squeezing valve XV04, delaying 60s, and closing a clear liquid return valve XV17, a grouping valve XV 11-XV 16 and a bottom drain valve XV 19.
2.9 back flushing and slag discharging: opening an exhaust valve XV06 of the filter, opening a slag discharge valve XV21 and XV22 after an interval of 5s, opening an air back-flushing valve XV09 and a grouping valve XV11 after an interval of 5s, closing a grouping valve XV11 after 10s, opening a grouping valve XV12 after an interval of 5s, closing a grouping valve XV12 after 10s, opening a grouping valve XV13 after 5s, performing back flushing on other groups respectively (the grouping back flushing is performed for one time, three back flushing is performed, and the back flushing frequency is adjustable) according to the operation, and closing all grouping valves XV16 and the air back-flushing valve XV09 after the back flushing is finished; and discharging the diatomite sludge.
2.10 spraying: opening a clean water inlet valve XV01Q (whether to open a dilute acid inlet valve HV01S can be determined according to field conditions), opening a spray valve XV05 after delaying for 5s, closing a clean water inlet valve XV01 after lasting for 5min, closing the spray valve XV05 at an interval of 5s, and closing an exhaust valve XV06 and deslagging valves XV21 and XV22 after delaying for 3 min.
2.11 at this point, one filtration cycle of the clean titanium liquid is over and the tube filter can be used for the next time.
In the embodiment, the filtering effect is good, the solid content of the filtrate is maintained below 0.03g/L, but the filtering operation is stopped by alarming after continuous filtering for 1 hour, the filtered filtrate can meet the requirement of the next procedure, and the trial operation effect of the next procedure is good.
The above-mentioned embodiment is only one of the preferred embodiments of the present invention, and should not be used to limit the scope of the present invention, but all the insubstantial modifications or changes made within the spirit and scope of the main design of the present invention, which still solve the technical problems consistent with the present invention, should be included in the scope of the present invention.
Claims (5)
1. A method for purifying and crystallizing titanium acidolysis solution is characterized in that a tubular filter is adopted for filtering, and a filter aid is perlite, and the temperature of a titanium solution feed liquid entering the tubular filter is 50-65 ℃.
2. The method for purifying and crystallizing titanium dioxide solution as claimed in claim 1, wherein the filtering with the tubular filter comprises the following steps:
(1) liquid charging and gas discharging: filling the raw material liquid into the tubular filter until the liquid level reaches a high liquid level;
(2) pre-blowback: compressed air is firstly introduced for scrubbing, and then compressed air is introduced for back blowing the filter element from inside to outside;
(3) pre-scrubbing: pre-coating liquid formed by premixing raw material liquid and perlite is filled in a tubular filter until the liquid level reaches a high liquid level;
(4) pre-coating circulation: opening a pre-coating liquid reflux valve to enable the pre-coating liquid to circulate in the tubular filter for 30-45 minutes, and entering the next step when the solid content of the filtrate is qualified;
(5) pre-filtering: stopping the pre-coating circulation, introducing a raw material liquid, performing pre-filtration for 5-10 minutes, and refluxing the pre-filtered clear liquid into the raw material liquid;
(6) and (3) filtering: starting filtering, regularly monitoring the solid content of filtrate, feeding the filtered qualified clear liquid into the next procedure, refluxing unqualified filtrate into the raw material liquid, alarming when the pressure value fed back by a pressure transmitter of the tubular filter reaches a preset value of 0.25-0.40 MPa, or continuously filtering for 5-6 hours, and stopping filtering;
(7) pressure drainage and filtration: stopping introducing the raw material liquid, discharging the liquid in the tubular filter by applying air pressure, and refluxing the discharged liquid into the raw material liquid;
(8) back flushing: compressed air is firstly introduced for scrubbing, and then compressed air is introduced for back blowing the filter element from inside to outside;
(9) deslagging: discharging perlite sludge in the tubular filter;
(10) and (4) spraying, namely spraying and washing the tubular filter by using clear water or dilute acid, and then performing the next round of use after the tubular filter is washed.
3. The method for purifying and crystallizing titanium dioxide solution as claimed in claim 2, wherein in the step (3), the precoating solution is prepared by mixing and stirring the titanium solution at 50-60 ℃ and perlite, and the stirring time is at least 30 minutes.
4. The method for purifying and crystallizing titanium dioxide solution as claimed in claim 2, wherein the amount of raw material solution fed in steps (5) and (6) is 40 to 70m3/h。
5. The method for purifying and crystallizing titanium dioxide solution as claimed in claim 2, wherein the filter cloth of the tube filter is periodically soaked with dilute acid, and then cleaned with clean water.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113509754A (en) * | 2021-08-09 | 2021-10-19 | 东华工程科技股份有限公司 | Titanium acidolysis solution treatment method and system |
| CN114504879A (en) * | 2021-12-31 | 2022-05-17 | 龙佰襄阳钛业有限公司 | Clear titanium liquid filtration system |
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Address after: 441500 No.1 Bianhe Road, Chengguan Town, Nanzhang County, Xiangyang City, Hubei Province Applicant after: Longbai Xiangyang Titanium Industry Co.,Ltd. Address before: 441500 No.1 Bianhe Road, Chengguan Town, Nanzhang County, Xiangyang City, Hubei Province Applicant before: XIANGYANG LOMON TITANIUM INDUSTRY Co.,Ltd. |
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