CN110759380A - Low-temperature low-acidity metatitanic acid bleaching process - Google Patents
Low-temperature low-acidity metatitanic acid bleaching process Download PDFInfo
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- CN110759380A CN110759380A CN201911054250.2A CN201911054250A CN110759380A CN 110759380 A CN110759380 A CN 110759380A CN 201911054250 A CN201911054250 A CN 201911054250A CN 110759380 A CN110759380 A CN 110759380A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
- C01G23/0532—Producing by wet processes, e.g. hydrolysing titanium salts by hydrolysing sulfate-containing salts
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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Abstract
The invention belongs to the technical field of titanium dioxide production, and particularly relates to a low-temperature low-acidity metatitanic acid bleaching process. Aiming at the problem that in the prior art, the bleaching condition of metatitanic acid is excessive in acid, and only the bleaching cost and the pressure of sewage treatment are increased, the technical scheme of the invention is as follows: in a bleaching process, the temperature and acidity of the process conditions are reduced while stringent requirements are placed on the rate of temperature rise and the rate and sequence of bleach addition. The invention adopts the low-temperature low-acidity bleaching process to produce the titanium dioxide, which not only can reduce the treatment cost of waste and side products, but also can reduce the consumption of non-renewable energy sources, thereby bringing certain economic benefits. The process can produce qualified titanium dioxide products, and provides a new idea for the whole chemical production industry in the aspects of energy conservation, consumption reduction and environmental protection.
Description
Technical Field
The invention belongs to the technical field of titanium dioxide production, and particularly relates to a low-temperature low-acidity metatitanic acid bleaching process.
Background
The process for producing titanium dioxide by a sulfuric acid method mainly comprises the steps of crushing, acidolysis, sedimentation, heat filtration, crystallization, ferrous separation, hydrolysis, primary washing (primary washing), bleaching, secondary washing (secondary washing), salt treatment, pre-kiln pressure filtration, calcination, intermediate crushing, coating, tertiary washing, drying, airflow crushing and the like. Wherein, the bleaching process is an important step for improving the whiteness of the titanium dioxide product.
At present, the temperature and the acidity of the metatitanic acid after the first washing are respectively controlled to be 60 ℃ and 80g/l (after bleaching) during bleaching, but the purpose of adding sulfuric acid in the bleaching process is only to provide an acidic environment for the reduction of ferric iron and not to participate in the reaction according to literature examination. Therefore, current bleaching conditions use too much acid, only increasing bleaching costs and pressure on wastewater treatment.
Disclosure of Invention
Aiming at the problems that in the prior art, the bleaching condition of metatitanic acid is excessive in acid, and only the bleaching cost and the pressure of sewage treatment are increased, the invention provides a low-temperature low-acidity metatitanic acid bleaching process, which aims to: the temperature and acidity in the bleaching process are reduced, and the consumption of sulfuric acid and energy is reduced, thereby reducing the cost and reducing the pressure of sewage treatment.
The technical scheme adopted by the invention is as follows:
a low-temperature low-acidity metatitanic acid bleaching process comprises the following steps:
[1] feeding materials to a bleaching tank at a washing station, determining the acidity after bleaching to be 55-65g/l, and calculating the addition amount of sulfuric acid according to the acidity before bleaching and the determined acidity after bleaching of washing slurry;
[2] adding sulfuric acid into the bleaching tank according to the addition amount calculated in the step (1);
[3] after the sulfuric acid is completely added, heating the slurry in the bleaching tank to 40-50 ℃, and then adding seed crystals;
[4] after adding seed crystal, stirring at a constant temperature, and then adding a trivalent titanium solution;
[5] adding a trivalent titanium solution, keeping the temperature and stirring until the slurry reaction is stable, sampling and analyzing the concentration of the trivalent titanium, supplementing the trivalent titanium solution into the bleaching tank if the concentration of the trivalent titanium is low, and repeating the operations of sampling, analyzing and supplementing the trivalent titanium solution again until the concentration of the trivalent titanium reaches the standard;
[6] and (5) feeding the slurry treated in the step (5) to a secondary washing post.
After the technical scheme is adopted, compared with the prior art, the addition amount of sulfuric acid and the heat preservation temperature are reduced simultaneously, and the heating and the addition sequence of various components are strictly controlled, so that a product with the same whiteness specification as that of the titanium dioxide obtained by the prior art can be finally prepared. And the process cost and the sewage treatment pressure are also greatly reduced due to the reduction of the use amount of the sulfuric acid and the reduction of the energy (heating steam) consumption.
Preferably, in the step [2], the adding speed of the sulfuric acid is 50-100L/min.
Preferably, in the step [3], the temperature rise rate is 0.5-0.8 ℃/min.
Preferably, the concentration of the trivalent titanium after bleaching is determined to be 0.3-0.6g/l, and the addition amount of the trivalent titanium solution in the step [4] and the addition amount of the trivalent titanium solution in the step [5] are calculated according to the concentration of the trivalent titanium after bleaching.
Preferably, the concentration of the trivalent titanium solution used in the step [4] and the step [5] is 70-90 g/l; the adding speed of the trivalent titanium solution is 200-300L/min.
The preferable scheme optimizes the adding speed and the heating speed of each component, and in the actual process, the specific embodiment is that after the temperature and the addition of the sulfuric acid are adjusted, the opening of a steam valve needs to be recalculated, and a pipeline and a valve for adding the sulfuric acid need to be replaced again to meet the process requirement. The titanium dioxide product with better whiteness can be obtained by the optimized process.
In summary, due to the adoption of the technical scheme, the invention has the beneficial effects that:
1. compared with the prior art, the method simultaneously reduces the addition amount of sulfuric acid and the heat preservation temperature, and strictly controls the heating and the addition sequence of various components, so that the product with the same whiteness specification as the titanium dioxide obtained by the prior art can be finally prepared. And the process cost and the sewage treatment pressure are also greatly reduced due to the reduction of the use amount of the sulfuric acid and the reduction of the energy (heating steam) consumption.
2. The preferred scheme optimizes the adding speed and the heating speed of each component, thereby obtaining the titanium dioxide product with better whiteness.
Detailed Description
All of the features disclosed in this specification, or all of the steps in any method or process so disclosed, may be combined in any combination, except combinations of features and/or steps that are mutually exclusive. In particular, the description of the present invention that the concentration or acidity of a certain component "after bleaching" refers to the concentration or acidity of the component in the slurry in step [6 ]; the concentration or acidity of a component "after bleaching" refers to the concentration or acidity of the component in the slurry in step [1 ].
A low-temperature low-acidity metatitanic acid bleaching process comprises the following steps:
[1] feeding materials to a bleaching tank at a washing station, determining the acidity after bleaching to be 55-65g/l, and calculating the addition amount of sulfuric acid according to the acidity before bleaching and the determined acidity after bleaching of washing slurry; the calculation formula is as follows:
the amount of sulfuric acid added is (acidity after bleaching-acidity before bleaching) x total volume after bleaching ÷ concentration of added sulfuric acid.
[2] Adding sulfuric acid into the bleaching tank according to the addition amount calculated in the step (1), wherein the addition process is slow;
[3] after the sulfuric acid is completely added, heating the slurry in the bleaching tank to 40-50 ℃, and then adding seed crystals;
[4] after adding seed crystal, stirring at a constant temperature, and then adding a trivalent titanium solution; the formula for calculating the seed crystal addition is as follows:
crystal seed addition rate (crystal seed addition ratio) multiplied by slurry TiO2Concentration x slurry volume ÷ seed concentration.
[5] Adding a trivalent titanium solution, keeping the temperature and stirring until the slurry reaction is stable, sampling and analyzing the concentration of the trivalent titanium, supplementing the trivalent titanium solution into the bleaching tank if the concentration of the trivalent titanium is low, and repeating the operations of sampling, analyzing and supplementing the trivalent titanium solution again until the concentration of the trivalent titanium reaches the standard;
[6] and (5) feeding the slurry treated in the step (5) to a secondary washing post.
Preferably, in the step [2], the adding speed of the sulfuric acid is 50-100L/min.
Preferably, in the step [3], the temperature rise rate is 0.5-0.8 ℃/min.
Preferably, the concentration of the trivalent titanium after bleaching is determined to be 0.3-0.6g/l, and the addition amount of the trivalent titanium solution in the step [4] and the addition amount of the trivalent titanium solution in the step [5] are calculated according to the concentration of the trivalent titanium after bleaching. The formula for calculating the addition of the trivalent titanium solution is as follows:
the trivalent titanium addition is the trivalent titanium concentration after bleaching x the total volume after bleaching divided by the trivalent titanium concentration.
Preferably, the concentration of the trivalent titanium solution used in the step [4] and the step [5] is 70-90 g/l; the adding speed of the trivalent titanium solution is 200-300L/min.
The technical solution of the present invention is further illustrated by the following specific examples.
Examples
The embodiment is carried out by adopting a device related to a bleaching process in the existing titanium dioxide production process, and comprises the following specific steps:
step 1, feeding of a density control groove: and (4) informing a washing post to feed, automatically starting stirring when the liquid level submerges the lower layer of blades, and automatically stopping a washing and feeding pump when the liquid level reaches the high limit.
Step 2, feeding of a bleaching tank: opening an outlet valve of the density control tank, opening a feed valve of the bleaching tank to 1/2 degrees of opening, checking and confirming that feed valves of other bleaching tanks are in a closed state, setting the metatitanic acid amount in a batch controller of the metatitanic acid of the bleaching tank, and switching an electric valve to be automatically controlled. And stopping stirring when the liquid level of the density control tank is just lower than the lower paddle. And when the liquid level of the bleaching tank reaches the stirring paddle, starting stirring, automatically closing the batch control valve after the set amount of the metatitanic acid is reached, and closing an outlet valve of the density control tank and a feed valve of the bleaching tank.
And 3, calculating and setting the adding amount of the seed crystal and the sulfuric acid. This example shows that the amount of sulfuric acid added was 30g/l in terms of the degree of acidity after bleaching of 60g/l (as a comparative example, the amount of sulfuric acid added was 50g/l in terms of the degree of acidity after bleaching of 80 g/l).
Step 4, adding sulfuric acid: and opening a tail gas exhaust valve of the bleaching tank, opening a steam inlet valve of a steam pipeline of the bleaching tank, and starting heating. The electric valve of the batch sulfuric acid control valve is opened to 40 percent, the electric valve is switched to be automatically controlled, the outlet valve (double valves) of the sulfuric acid head tank and the sulfuric acid feeding valve of the bleaching tank are opened, the sulfuric acid feeding valves of other bleaching tanks are checked and confirmed to be in a closed state, the sulfuric acid is slowly added, the valves are automatically closed after the set sulfuric acid amount is added in batches, and the outlet valve of the sulfuric acid head tank and the sulfuric acid feeding valve of the bleaching tank are closed.
Step 5, heating and adding seed crystals: the slurry was warmed to 50 ℃. Setting and opening a seed crystal batch control valve, opening a calcining seed crystal feeding valve of the bleaching tank, checking and confirming that seed crystal feeding valves of other bleaching tanks are in a closed state, and starting a seed crystal pump to add seed crystals into the bleaching tank. And when the set amount of the calcined seed crystal is added, the batch control valve is automatically closed, the seed crystal pump is stopped, and the seed crystal feeding valve of the bleaching tank is closed.
Step 6, Ti3+Adding (A): and (4) keeping the temperature and stirring for 10min, and calculating the adding amount of the trivalent titanium according to the concentration of the bleached trivalent titanium solution of 0.3-0.6 g/l. Opening a trivalent titanium feeding valve of a bleaching tank, checking and confirming that seed crystal feeding valves of other bleaching tanks are in a closed state, opening an outlet valve of a trivalent titanium metering tank, setting the adding volume of a trivalent titanium solution, adding a calculated amount of trivalent titanium into the bleaching tank, and closing an outlet valve of the trivalent titanium metering tank and a Ti of the bleaching tank after the adding is finished3+And a feed valve.
Step 7, heat preservation and sampling: adding the trivalent titanium solution, and stirring for 90 minutes at 50 ℃. Sampling and sending to a central control system for analyzing the concentration of the trivalent titanium.
Step 8, if the Ti in the slurry3+If the concentration is lower, replenishing, opening a trivalent titanium feeding valve of the bleaching tank, checking and confirming that seed crystal feeding valves of other bleaching tanks are in a closed state, opening an outlet valve of a trivalent titanium metering tank, setting the volume of replenished trivalent titanium, and adding Ti to be replenished to the bleaching tank3+Metering, closing the outlet valve of the trivalent titanium metering tank and the Ti of the bleaching tank after the feeding3+And a feed valve.
And 9, after the detection is qualified, receiving a second washing and feeding notice, opening a discharge valve of the bleaching tank, opening an inlet valve of a second washing and feeding pump, enabling an outlet valve to have 40% of opening, starting the feeding pump, adjusting the outlet valve to have the required opening, feeding to a second washing post, and stopping stirring when the liquid level of the bleaching tank is just lower than the paddle.
And step 10, after the batch of bleaching materials is fed, closing an outlet valve of the second washing feed pump, stopping the pump, closing an inlet valve of the pump, and closing an outlet valve of the bleaching tank.
And 11, when the metatitanic acid collecting tank reaches a certain liquid level, sending the slurry into a density control tank by using a metatitanic acid collecting pump, and stopping the metatitanic acid collecting pump when the liquid level is close to a suction inlet of the metatitanic acid collecting pump.
And 12, discharging the cake after the second washing is finished, and sampling to detect the Fe content of the slurry.
The following table shows the Fe content detected after completion of the second washing of examples and comparative examples:
in the embodiment, the bleaching temperature and the bleached sulfuric acid content are respectively reduced to 50 ℃ and 60g/l from 60 ℃ and 80g/l in the prior art, so that the production cost of titanium dioxide can be reduced by 30 yuan per ton. The iron content of the bleached material obtained after the bleaching process conditions are adjusted to be 19ppm after the bleaching process is carried out, and the iron content of the bleached material is not greatly different from that of the unadjusted iron content of the washed material to be 18ppm, so that the product quality is not influenced. The brightness of the calcined bleached material under the kiln is above 94.0, the brightness of the titanium dioxide product is above 94.4, and the whiteness of blue light can reach above 93.5.
The above-mentioned embodiments only express the specific embodiments of the present application, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present application. It should be noted that, for those skilled in the art, without departing from the technical idea of the present application, several changes and modifications can be made, which are all within the protection scope of the present application.
Claims (5)
1. A low-temperature low-acidity metatitanic acid bleaching process is characterized by comprising the following steps:
[1] feeding materials to a bleaching tank at a washing station, determining the acidity after bleaching to be 55-65g/l, and calculating the addition amount of sulfuric acid according to the acidity before bleaching and the determined acidity after bleaching of washing slurry;
[2] adding sulfuric acid into the bleaching tank according to the addition amount calculated in the step (1);
[3] after the sulfuric acid is completely added, heating the slurry in the bleaching tank to 40-50 ℃, and then adding seed crystals;
[4] after adding seed crystal, stirring at a constant temperature, and then adding a trivalent titanium solution;
[5] adding a trivalent titanium solution, keeping the temperature and stirring until the slurry reaction is stable, sampling and analyzing the concentration of the trivalent titanium, supplementing the trivalent titanium solution into the bleaching tank if the concentration of the trivalent titanium is low, and repeating the operations of sampling, analyzing and supplementing the trivalent titanium solution again until the concentration of the trivalent titanium reaches the standard;
[6] and (5) feeding the slurry treated in the step (5) to a secondary washing post.
2. A low temperature low acidity bleaching process of metatitanic acid according to claim 1, wherein: in the step [2], the adding speed of the sulfuric acid is 50-100L/min.
3. A low temperature low acidity bleaching process of metatitanic acid according to claim 1, wherein: in the step [3], the temperature rise speed is 0.5-0.8 ℃/min.
4. A low temperature low acidity bleaching process of metatitanic acid according to claim 1, wherein: and (3) determining the concentration of the bleached trivalent titanium to be 0.3-0.6g/l, and calculating the addition amount of the trivalent titanium solution in the step [4] and the addition amount of the trivalent titanium solution in the step [5] according to the concentration of the bleached trivalent titanium.
5. A low temperature low acidity bleaching process of metatitanic acid according to claim 1, wherein: the concentration of the trivalent titanium solution used in the step [4] and the step [5] is 70-90 g/l; the adding speed of the trivalent titanium solution is 200-300L/min.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112645383A (en) * | 2020-12-30 | 2021-04-13 | 河南佰利联新材料有限公司 | Utilization method of high-chlorine-content R seed crystal |
| CN114380328A (en) * | 2021-12-28 | 2022-04-22 | 龙佰襄阳钛业有限公司 | Titanium dioxide three-washing process |
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2019
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| CN104477985A (en) * | 2014-12-04 | 2015-04-01 | 攀钢集团钛业有限责任公司 | Bleaching method used in production of titanium dioxide powder by sulfuric acid process |
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| CN112645383A (en) * | 2020-12-30 | 2021-04-13 | 河南佰利联新材料有限公司 | Utilization method of high-chlorine-content R seed crystal |
| CN112645383B (en) * | 2020-12-30 | 2024-02-23 | 河南佰利联新材料有限公司 | Utilization method of high-chlorine-content R seed crystal |
| CN114380328A (en) * | 2021-12-28 | 2022-04-22 | 龙佰襄阳钛业有限公司 | Titanium dioxide three-washing process |
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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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Application publication date: 20200207 |