CN1376633A - Process for concentrating diluted sulfuric acid and removing impurities - Google Patents
Process for concentrating diluted sulfuric acid and removing impurities Download PDFInfo
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- CN1376633A CN1376633A CN 02113704 CN02113704A CN1376633A CN 1376633 A CN1376633 A CN 1376633A CN 02113704 CN02113704 CN 02113704 CN 02113704 A CN02113704 A CN 02113704A CN 1376633 A CN1376633 A CN 1376633A
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Abstract
A process for concentrating diluted sulfuric acid while removing impurities includes such steps as counter-current contact between hot air and atomized diluted sulfuric acid in drying-concentrating tower for heating, evaporating and concentrating, cooling, and separating the educed or deposited impurities for sulfuric acid. Its advantages are low cost and simple process.
Description
Belongs to the technical field of:
the invention relates to a concentration and impurity removal method of dilute sulfuric acid.
Background art:
when the titanium dioxide is produced by using a sulfuric acid method, a large amount of dilute sulfuric acid is generated no matter titanium concentrate is used as a raw material or high-titanium slag is used as a raw material to produce the titanium dioxide. The amount and content of dilute sulfuric acid produced varies with the separation technology of the process. The method is generally divided into two types: namely filtrate after metatitanic acid hydrolysis separation, the sulfuric acid content of the filtrate is 17-25%; and a filtered cake wash having a sulfuric acid content of 1-5%. The former has useful value after recovery and can be returned to production for use orProduction of other products; the latter is usually added into lime because the concentration is too low and the recovery value is not great
And disposed of after precipitation. The concentrated dilute sulfuric acid belongs to the former, and typical components of the concentrated dilute sulfuric acid are as follows:
| Components | Content (%) | Components | Content (%) |
| Specific gravity of | 1.32(g/cm3) | H2SO4 | 22.26 |
| Fe2O3 | 5.03 | Al2O3 | 0.2 |
| MgO | 0.40 | TiO2 | 0.68 |
| V | 0.03 | Cr | 0.006 |
| Nb | 0.004 | Pb | 0.015 |
| P | 0.005 | CaO | 0.43 |
since, in addition to sulfuric acid, this acid also contains a large amount of other impurities, such as Fe in the form of ferrous sulfate2O3Metatitanic acidForm of TiO2And magnesium sulfate, aluminum sulfate, calcium sulfate, and the like. Brings great difficulty to the production and utilization of evaporation concentration, and simultaneously, the discharge causes harm to the environment. The methods and disadvantages of the existing common processing are as follows: A. and (5) carrying out vacuum evaporation and concentration to recover the dilute acid. The problem is that the ferrous sulfate and oxygen contained in the waste acid are used as the final effect of the multi-effect evaporation in the initial stage of the evaporationThe impurity compounds such as titanium and calcium sulfate precipitate and scale quickly, so that the graphite heat exchanger is blocked and needs to be mechanically cleaned, and the heat exchanger can be damaged carelessly; the production is not normal, and the equipment cost and investment are expensive. B. In order to solve the problem of heat exchanger blockage in the vacuum evaporation concentration method, the invention method disclosed in the patent CN1042527A adopts two-stage concentration and three-time separation to remove impurities in acid. In the first stage, 20-24% of dilute sulfuric acid is pre-concentrated to 26-29% by using tail gas of a titanium dioxide calcining kiln, residues separated out are separated out for the first time, filtrate obtained by separation is cooled to separate out ferrous sulfate heptahydrate, secondary separation is carried out, and a solid phase substance, namely the ferrous sulfate heptahydrate, is separated out to obtain dilute sulfuric acid containing 30-35%; then, carrying out secondary concentration on the obtained dilute sulfuric acid containing 30-35% by using a vacuum evaporation concentration method to obtain a sulfuric acid concentration of 60-71%; and finally, carrying out third separation on the secondary precipitate in the acid to obtain about 70 percent sulfuric acid. The process has more equipment and long process flow; the surface seems to be energy-saving, and through the long process of two-stage concentration and three-time separation, the equipment investment and the cost of direct evaporation concentration are not reduced but greatly increased, the number of working procedures is large, and the operation cost is also large. C. The literature (the third phase of 2000 years for phosphate fertilizer and compound fertilizer, the fifteenth volume in general) is entitled research on titanium white waste acid for producing common calcium phosphate, and the author directly mixes 20% titanium white powder production dilute sulfuric acid with 92% concentrated sulfuric acid into sulfuric acid with the concentration of about 60%; then separating to remove impurity compounds such as iron, titanium and the like, and directly using the impurity compounds in the production of common superphosphate. Although the process is simplified and the equipment investment is less, the water content in 20 percent of dilute sulfuric acid is taken away by the common calcium superphosphate product, and the production capacity of the calcium superphosphate matched with the water content is necessarily 20 to 30 times of that of the titanium pigment; matching the production scale of titanium dioxide by sulfuric acid process with calcium superphosphate and water waggonIt is difficult to satisfy. And the calcium superphosphate is a low-concentration phosphate fertilizer with lower value, is limited by the transportation radius and the fertilizer using radius, and cannot obtain better economic benefit. Furthermore, since the dilute sulfuric acid brings about excess water, the production of calcium superphosphate must be carried out by a dry process, i.e. bakingDry phosphate ore, dry ground phosphate ore and the like, and increases the investment, energy consumption and operation production cost of processing equipment of the calcium superphosphate. In addition, 92% sulfuric acid is diluted and then filtered, impurity removal and filtration equipment is doubled, and the load of impurity separation is increased.
The invention content is as follows:
the invention aims to provide a production method for concentrating dilute sulfuric acid and removing impurities. The production method shortens the process flow, and solves the problem of precipitation, scaling and blockage of the heat exchanger due to no use of the heat exchanger; because the process flow is simplified, impurities separated out and precipitated in the acid are separated only once; and the low-price corrosion-resistant and temperature-resistant material is adopted, so that the investment of a dilute sulfuric acid concentration device is reduced, and the processing operation cost is also reduced.
The purpose of the invention is realized as follows:
the production principle of the invention is as follows: the dilute sulfuric acid and high-temperature hot gas are in countercurrent contact in an empty tower for instantaneous evaporation and concentration, and impurity compounds contained in the acid are precipitated and separated out along with the increase of the temperature and the concentration of the acid. The principle is as follows:
the specific process of the invention is as follows: carrying out atomization spraying on dilute sulfuric acid from the top of a drying and concentrating tower, and carrying out countercurrent contact heating on the dilute sulfuric acid and hot air entering from the bottom of the tower in the tower to finish the evaporation and concentration process; the steam of concentration evaporation is got rid of from the top of the tower, and the tail gas fan is got rid of into the atmosphere from the chimney after the defroster defogging. The concentrated sulfuric acid liquid containing precipitated impurities is discharged from the tower bottom, is subjected to heat exchange and temperature reduction through a cooler, and then enters a filter press for solid-liquid separation, and the filtrate is concentrated sulfuric acid which can be returned to titanium dioxide production or used for phosphorus chemical production and other production; the filter cake is washed by dilute sulfuric acid, the washing acid returns to the evaporation and concentration process, and the filter cake is used for producing ferrous salt or is sent to a sulfuric acid factory for producing sulfuric acid. The invention is therefore characterized in that the method comprises:
A. carrying out atomization spraying on dilute sulfuric acid in a concentration tower;
B. the atomized dilute sulfuric acid and hot gas are subjected to countercurrent contact heat exchange in an empty tower and are quickly evaporated and concentrated;
C. in the concentration process of the dilute sulphuric acid feed liquid, impurity compounds contained in the dilute sulphuric acid feed liquid are precipitated and separated out and are discharged from the bottom of the tower along with the concentrated feed liquid;
D. cooling the concentrated feed liquid;
E. cooling the feed liquid, and performing filter pressing separation to obtain filtrate, namely concentrated sulfuric acid;
F. washing the filter cake with dilute sulfuric acid before concentration, and returning the washing acid to atomizing spray for concentration;
G. the washed filter cake is sent to ferrous salt production or sulfuric acid factory to produce sulfuric acid.
The spray atomization of the dilute sulfuric acid is pressure atomization or centrifugal atomization, and preferably pressure atomization.
The hot air contacted with the dilute sulfuric acid comprises coal-fired purified tail gas, boiler high-temperature tail gas, natural gas and fuel-fired hot air.
The spray concentration tower adopts temperature-resistant and acid-resistant ceramic tiles lined with potassium water glass cement for bonding, and hot gas is directly heated.
The inlet temperature of the hot air at the bottom of the spray concentration tower is 300-700 ℃, and the optimal temperature is 450-600 ℃.
The temperature of the outlet of the top of the spray concentration tower is 70-150 ℃, and the optimal temperature is 80-120 ℃.
The cooling temperature of the concentrated sulfuric acid is 40-90 ℃ before solid-liquid separation, namely before the concentrated sulfuric acid enters a filter press, and the optimal temperature is 50-70 ℃.
The filtered cake after solid-liquid separation of the present invention is washed with water or unconcentrated dilute sulfuric acid, preferably dilute sulfuric acid.
Part of the concentrated sulfuric acid is mixed with dilute sulfuric acid before solid-liquid separation and returned to the spray tower for spraying and concentration.
The solid-liquid separation of the impurities in the concentrated sulfuric acid adopts vacuum filtration or filter pressing by a filter press.
The washing liquid returns to the spray concentration process, the washing filter cake is washed by dilute sulfuric acid, and the washed dilute sulfuric acid returns to the spray concentration tower for spraying. The washed filter cake is used for other product processing, such as sending to a sulfuric acid processing plant to produce sulfuric acid or sending to a ferrous salt plant to produce ferric salt.
The invention solves the problem that the equipment scaling problem of indirect heating is avoided by the material and heating mode of the equipment under the conditions of high temperature and high corrosion of the concentration and evaporation of dilute sulfuric acid. The evaporation concentration tower selects the temperature-resistant acid-resistant brick with the material contact part, and the potash water glass cement serves as a bonding agent, so that the potassium water glass acid-resistant concrete is added in the high-temperature area to prevent the damage caused by direct contact of the temperature-resistant acid-resistant brick and the overheated air in the high-temperature area, the direct contact of the hot air and the ceramic tile is prevented, and the effect of protecting the brick is achieved.
The invention adopts the direct spray of dilute sulphuric acid to contact with hot air for heating and concentration, replaces the vacuum evaporation and concentration indirectly heated by an expensive graphite heat exchanger, and reduces the investment of the device; one-time heating and one-time separation, thereby shortening the production flow, simplifyingthe process and greatly reducing the recovery production cost of the dilute sulfuric acid.
The attached drawings and their description:
FIG. 1 is a process flow diagram of the present invention
In the figure: 1. spray concentration tower 2, hot-blast stove 3, concentrated acid pump tank 4, cooler
5. A filter-pressing pump 6, a filter press 7, a concentrated acid storage tank 8, a demister 9 and a fan
10. Demister 11 and chimney
The specific implementation mode is as follows:
the first embodiment is as follows:
by natureGas combustion tail gas is used as heat source, and 133Kg of dilute sulfuric acid (its main composition: H) is fed into the simulated spray concentration tower every hour2SO422.26％、FeSO4·7H2O 20.8％、MnSO41.1％、MgSO41.2％、CaSO4·H2O 1.2％、TiO20.45%), 560 ℃ at the inlet of the column, 103 ℃ at the outlet, 63Kg of water evaporated per hour, and 70Kg of concentrated sulfuric acid slurry obtained per hour from the bottom of the column (the main composition of which is: h2SO442.29％、FeSO4·H2O24.11％、MnSO42.09％、MgSO42.28％、CaSO42.01％、TiO20.85%); thereafter, the concentrated sulfuric acid slurry was cooled to a temperature of 65 ℃ and subjected to vacuum filtration separation to obtain 33.83Kg of wet cake and 36Kg of filtrate (H)2SO459.21％、Fe2O30.30％、MgO0.71％、Al2O3 0.43％、TiO2 0.06％)。
Example two:
spray concentration, separation and, after suction filtration, 33.83Kg of wet cake per hour were washed in portions with 30Kg of 22.26% dilute sulfuric acid to give 27.06Kg of wet cake (H2SO46.50%, H2O 18.5.5%) and 36.77Kg of filtrate containing 35.40% sulfuric acid, which was returned to the spray concentration tower to be combined with the dilute sulfuric acid as the feed for concentration.
Example three:
using coal-fired high-temperature gas with the specification of phi 6 multiplied by 22m and the volume of 600m3The spray concentration tower of (2) was charged with 16.41t of dilute sulfuric acid per hour (composition: H2SO423.16%;FeSO4&7H2O 17.6.6%; MnSO41.1%; MgSO41.3%; CaSO 4. H2O 1.2.2%; TiO20.5%) is subjected to spray countercurrent contact heating concentration; the hot air inlet temperature is 600 ℃, the outlet temperature is 95 ℃, and the water evaporation amount per hour is 9.0t, thus obtaining 7.4t of concentrated dilute sulfuric acid (the composition is H2SO451.3%, FeSO 4. H2O 23.8.8%, MnSO42.44%, MgSO42.88%, CaSO42.35%, TiO21.11%).
Example four:
spray concentration is carried out according to the third embodiment, concentrated dilute sulfuric acid from the bottom of the concentration tower is cooled to 65 ℃, and the concentrated dilute sulfuric acid enters a filter press for solid-liquid separation; 4.02t of isolated concentrated sulfuric acid (composition: H2SO470.7%, Fe2O30.30%, MgO 0.71%, Al2O30.43%, TiO20.06%), and 3.38t of wet cake (liquid holdup 35%) were obtained per hour.
Example five:
the wet filter cake separated by the filter press according to the fourth embodiment is washed by 3.5t per hour of dilute sulfuric acid (the composition is H2SO423.16%, FeSO 4.7H 2O 17.6.6%, MnSO41.1%, MgSO41.3%, CaSO 4.H 2O 1.2.2%, TiO20.5%); washing dilute sulfuric acid (H2SO4 content: 37.13%) 3.87t is obtained, and the acid returns to the third embodiment and is combined with the raw material dilute sulfuric acid for spray concentration; meanwhile, 3.01t of filter cake (liquid holdup 31%) is obtained every hour and is used for processing sulfuric acid or delivering ferrous salt to a sulfuric acid plant for production treatment.
Claims (11)
1. A production method for concentrating and removing impurities of dilute sulfuric acid is characterized by comprising the following steps:
A. carrying out spray atomization on dilute sulfuric acid in a concentration tower;
B. the atomized dilute sulfuric acid and hot gas are subjected to countercurrent contact heat exchange in a drying concentration tower and are quickly evaporated and concentrated;
C. in the concentration process of the dilute sulphuric acid feed liquid, impurity compounds contained in the dilute sulphuric acid feed liquid are precipitated and separated out and are discharged from the bottom of the tower along with the concentrated feed liquid;
D. cooling the concentrated feed liquid;
E. cooling the feed liquid for solid-liquid separation to obtain filtrate, namely concentrated sulfuric acid;
F. washing the filter cake with dilute sulfuric acid or water before concentration, and returning the washing acid to the atomizing spray for concentration;
G. the washing filter cake is sent to ferrous salt production or sulfuric acid factory to produce sulfuric acid.
2. The production method of dilute sulfuric acid concentration and impurity removal according to claim 1, which is characterized in that: the spray atomization of the dilute sulfuric acid is pressure atomization or centrifugal atomization, preferably pressure atomization.
3. The production method of dilute sulfuric acid concentration and impurity removal according to claim 1, which is characterized in that: the hot air contacted with the dilute sulfuric acid comprises coal-fired purified tail gas, boiler high-temperature tail gas, natural gas and fuel-fired hot air.
4. The production method of dilute sulfuric acid concentration and impurity removal according to claim 1, which is characterized in that: the spray concentration tower adopts lining temperature-resistant and acid-resistant ceramic tiles, potassium water glass cement for bonding, and hot gas is directly heated.
5. The production method of dilute sulfuric acid concentration and impurity removal according to claim 1, which is characterized in that: the inlet temperature of hot air at the bottom of the spray concentration tower is 300-700 ℃, and the optimal temperature is 450-600 ℃.
6. The production method of dilute sulfuric acid concentration and impurity removal according to claim 1, which is characterized in that: the outlet temperature of the spray concentration tower is 70-150 ℃, and the optimal temperature is 80-120 ℃.
7. The production method of dilute sulfuric acid concentration and impurity removal according to claim 1, which is characterized in that: the cooling temperature of the concentrated sulfuric acid before solid-liquid separation, i.e. before the concentrated sulfuric acid enters a filter press is 40-90 ℃, and the optimal temperature is 50-70 ℃.
8. The production method of dilute sulfuric acid concentration and impurity removal according to claim 1, which is characterized in that: the filtered cake after solid-liquid separation is washed with water or unconcentrated dilute sulfuric acid, preferably dilute sulfuric acid.
9. The production method of dilute sulfuric acid concentration and impurity removal according to claim 1, which is characterized in that: part of the concentrated sulfuric acid is mixed with dilute sulfuric acid before solid-liquid separation and returned to the spray tower for spraying and concentration.
10. The production method of dilute sulfuric acid concentration and impurity removal according to claim 1, which is characterized in that: the solid-liquid separation of the impurities in the concentrated sulfuric acid adopts vacuum filtration or filter pressing by a filter press.
11. The production method of dilute sulfuric acid concentration and impurity removal according to claim 1, which is characterized in that: the washing liquid returns to the spray concentration process, the washing filter cake is washed by dilute sulfuric acid, and the washed dilute sulfuric acid returns to the spray concentration tower for spraying.
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| CN100395535C (en) * | 2004-04-21 | 2008-06-18 | 浙江大学 | Small spray drying appts. for lab and its application method |
| CN100581994C (en) * | 2008-01-09 | 2010-01-20 | 龚家竹 | Concentrating and impurity removing method for dilute sulfuric acid in titanium dioxide powder production process by employing sulfuric acid process |
| CN102430249A (en) * | 2011-09-27 | 2012-05-02 | 东营方圆有色金属有限公司 | Hot-air concentrating tower for purifying waste acid |
| CN101367507B (en) * | 2007-08-17 | 2012-07-11 | 新疆石河子中发化工有限责任公司 | Gas removing, filtering and extracting method for waste sulphuric acid |
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| CN113277480A (en) * | 2021-06-08 | 2021-08-20 | 安徽金星钛白（集团）有限公司 | Titanium dioxide waste acid treatment method |
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| CN101367507B (en) * | 2007-08-17 | 2012-07-11 | 新疆石河子中发化工有限责任公司 | Gas removing, filtering and extracting method for waste sulphuric acid |
| CN100581994C (en) * | 2008-01-09 | 2010-01-20 | 龚家竹 | Concentrating and impurity removing method for dilute sulfuric acid in titanium dioxide powder production process by employing sulfuric acid process |
| CN102430249A (en) * | 2011-09-27 | 2012-05-02 | 东营方圆有色金属有限公司 | Hot-air concentrating tower for purifying waste acid |
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| CN102674255A (en) * | 2012-05-08 | 2012-09-19 | 安徽锦洋氟化学有限公司 | Production process and equipment for heating feed acid by using aluminum fluoride tail gas |
| CN106145160A (en) * | 2015-04-03 | 2016-11-23 | 东至天孚化工有限公司 | A kind of ammonium acid fluoride production method |
| CN106006806A (en) * | 2016-07-22 | 2016-10-12 | 株洲三特环保节能有限公司 | Hot air and tubular heater combined waste acid concentration treatment method and device |
| CN106986314A (en) * | 2017-03-29 | 2017-07-28 | 扬州祥发资源综合利用有限公司 | A kind of middle temperature carbonizatin method handles the method and device of high COD sulfuric acid |
| CN110683520A (en) * | 2018-07-06 | 2020-01-14 | 中国石油化工股份有限公司 | Process for preparing sulfuric acid by regenerating low-concentration dilute waste sulfuric acid |
| CN110240164A (en) * | 2019-06-26 | 2019-09-17 | 威海恒邦化工有限公司 | The method and device of fluosilicic acid concentration |
| CN110577203A (en) * | 2019-09-29 | 2019-12-17 | 贵州胜威福全化工有限公司 | Process for producing calcium superphosphate by using titanium dioxide byproduct waste acid |
| CN111888831A (en) * | 2020-06-24 | 2020-11-06 | 刘发业 | Waste sulfuric acid recovery processing device and application thereof |
| CN113277480A (en) * | 2021-06-08 | 2021-08-20 | 安徽金星钛白（集团）有限公司 | Titanium dioxide waste acid treatment method |
| CN114632338A (en) * | 2022-03-28 | 2022-06-17 | 河北惠尔信新材料有限公司 | Titanium dioxide washing mother liquor concentration treatment system |
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