CN112441676A - Method for treating acid wastewater of titanium dioxide by sulfuric acid process - Google Patents
Method for treating acid wastewater of titanium dioxide by sulfuric acid process Download PDFInfo
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- CN112441676A CN112441676A CN201910823806.3A CN201910823806A CN112441676A CN 112441676 A CN112441676 A CN 112441676A CN 201910823806 A CN201910823806 A CN 201910823806A CN 112441676 A CN112441676 A CN 112441676A
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F9/00—Multistage treatment of water, waste water or sewage
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/46—Sulfates
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/001—Processes for the treatment of water whereby the filtration technique is of importance
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- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
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- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2301/00—General aspects of water treatment
- C02F2301/08—Multistage treatments, e.g. repetition of the same process step under different conditions
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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Abstract
The invention relates to the technical field of titanium dioxide acid wastewater treatment, and provides a method for treating titanium dioxide acid wastewater by a sulfuric acid process, which comprises the following steps: s1, under stirring treatment, enabling a mixed solution of the acidic wastewater and clear water containing 3% -8% of sulfuric acid to automatically flow into a neutralization tank through a fall, pumping limestone slurry into the neutralization tank for first-stage neutralization, and enabling the pH value at the end point of the reaction to be 4.0-5.0; s2, continuously stirring, pumping the digested lime slurry, and performing second-stage neutralization, wherein the pH value at the end of the reaction is 7.0-8.5, so as to obtain reaction slurry; pumping the qualified neutralized reaction slurry of S3 into a filter press for filter pressing, wherein the pH value of the reaction slurry is 6.5-8.5; s4, naturally drying the filter cake after filter pressing, aerating and filtering the filter liquor after filter pressing, and discharging qualified water reaching the standard through detection or using the qualified water as process water. The invention has the technical effects of high neutralization efficiency, good aeration effect and low cost.
Description
Technical Field
The invention belongs to the technical field of titanium dioxide acid wastewater treatment, and particularly relates to a method for treating titanium dioxide acid wastewater.
Background
A large amount of acidic wastewater is generated in the production of titanium dioxide by a sulfuric acid method, and the conventional treatment method is to neutralize the acidic wastewater in a calcium oxide-calcium hydroxide combined mode, and then to obtain the wastewater and gypsum which reach the standard through the working procedures of aeration, filter pressing and the like.
The waste water is neutralized by combining calcium oxide and calcium hydroxide, and the following disadvantages exist: (1) the lime is used as the raw material to treat the wastewater, so the cost is high; (2) lime which is not digested by the digestion water can only be treated as waste, which causes resource waste; (3) stirring and aerating in a mode of blowing air, so that the neutralization process is not thorough and the sewage treatment efficiency is low; (4) solid-phase substances are continuously deposited at the bottom of the neutralization aeration tank, and the neutralization aeration tank needs to be stopped for cleaning, so that the service efficiency of the neutralization aeration tank is reduced, and the titanium dioxide production process is restricted.
Therefore, how to improve the cost for treating the wastewater and improve the wastewater treatment efficiency is an urgent problem to be solved in the current titanium dioxide acidic wastewater treatment process.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a method for treating acid wastewater of titanium dioxide by a sulfuric acid process, which can achieve the technical effects of high neutralization efficiency, good aeration effect and low cost.
In order to achieve the above purpose, the solution adopted by the invention is as follows:
a method for treating acid wastewater of titanium dioxide by a sulfuric acid process comprises the following steps:
s1, under stirring treatment, enabling a mixed solution of the acidic wastewater and clear water containing 3% -8% of sulfuric acid to automatically flow into a neutralization tank through a fall, pumping limestone slurry into the neutralization tank for first-stage neutralization, and enabling the pH value at the end point of the reaction to be 4.0-5.0;
s2, continuously stirring, pumping the digested lime slurry, and performing second-stage neutralization, wherein the pH value at the end of the reaction is 7.0-8.5, so as to obtain reaction slurry;
pumping the qualified neutralized reaction slurry of S3 into a filter press for filter pressing, wherein the pH value of the reaction slurry is 6.5-8.5;
s4, naturally drying the filter cake after filter pressing, aerating and filtering the filter liquor after filter pressing, and discharging qualified water reaching the standard through detection or using the qualified water as process water.
Preferably, in the step S1, the ratio of the acidic wastewater to the clear water containing 3% -8% of sulfuric acid is 1: 25-40.
Preferably, in the step S1, the stirring speed is 40 to 60 r/min.
Preferably, in S2, the lime slurry is prepared by mixing lime with slaking water after the lime is slaked by a slaking machine or a ball mill, and cooling the mixture with water at 30-40 ℃ to obtain the lime slurry; the part of lime which is not digested by the digestion water enters a ball mill to be ground together with the limestone raw material into limestone slurry; the digestion water is press filtration water.
Preferably, 4 to 8 tons of slaking water are added to each ton of lime for slaking.
Preferably, in S4, the filtration is performed by plate and frame filtration.
Preferably, in S4, continuous aeration is performed in a manner that a plurality of aeration tanks are connected in series, and the aeration time is 1 to 3 hours.
Preferably, in S4, the process water is used for the slaking water in the lime slurry, the grinding water used for the lime slurry, and the water for life of titanium white.
The technical principle of the invention is as follows:
lime-limestone is adopted to neutralize the acid wastewater, firstly, limestone and sulfuric acid in the acid wastewater are subjected to first-stage neutralization, and a part of sulfuric acid is consumed; secondly, slaking lime and slaked water to generate slaked lime, carrying out second-stage neutralization, and carrying out acid wastewater treatment in a two-stage neutralization mode, wherein the neutralization efficiency is high, and the cost is effectively controlled.
The acid wastewater is mixed with the clear water with low sulfuric acid concentration, the acid wastewater to be neutralized is uniformly blended, and the problems that when the acidity is too high and is neutralized with limestone slurry and lime slurry, the slurry is thick, the reaction rate is reduced, the stirring difficulty is high, the subsequent operation process is influenced and the like are solved.
The pH value of the neutralization end point of the first section is controlled to be 4.0-5.0, and is suitable for the acidity of the acidic wastewater. If the pH value is too high, the neutralization speed is slowed, and the utilization rate of limestone is reduced; if the pH is too low, the effective reactivity of the limestone is low, resulting in an increase in the amount of slaked lime used in the second stage neutralization. The pH value of the neutralization end point of the second section is controlled to be 7.0-8.5, the pH value of discharged water is 6-9, and gypsum precipitates generated by the neutralization reaction of the second section grow up uniformly, so that filter pressing is facilitated; and is beneficial to the requirement of hydrolyzing the pH value of calcium, magnesium, manganese and other ions during aeration. If the pH value is too low, the metal ions are not fully hydrolyzed and do not reach the standard of external drainage; if the pH value is too high, the lime consumption is increased, and the cost is increased.
The first section neutralization and the second section neutralization are both treated by mechanical stirring, the slurry has strong fluidity in the neutralization process, the pumped lime slurry can be rapidly and uniformly dispersed, the reaction is sufficient, the precipitate is not easy to aggregate, and the neutralization effect is obvious.
And continuous aeration is carried out in a white clear water state, aeration is carried out in a mode of connecting a plurality of aeration tanks in series, qualified neutralized wastewater continuously flows into an inlet of each aeration tank, and the wastewater is discharged from an overflow port of each aeration tank until COD of external drainage is less than 100 mg/L. By adopting the aeration method, the aeration effect is good, and the efficiency is obviously improved; compared with aeration treatment in the neutralization process, the treatment capacity of the wastewater is improved by more than 50% by aeration after neutralization and filter pressing.
The invention has the beneficial effects that:
(1) the acid wastewater is neutralized by lime-limestone combination, so that the neutralization efficiency is high, and the cost is effectively controlled;
(2) the neutralization process adopts mechanical stirring treatment, the slurry has strong fluidity, the pumped lime slurry can be rapidly and uniformly dispersed, the reaction is sufficient, the precipitate is not easy to aggregate, and the neutralization effect is obvious;
(3) aeration is carried out in a clear water state, the aeration effect is good, and the efficiency is obviously improved.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
Fig. 1 is a process flow chart of a method for treating acidic wastewater of titanium dioxide produced by a sulfuric acid process provided in embodiments 1 to 6 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The following is a detailed description of the method for treating acidic wastewater from titanium dioxide production by sulfuric acid process according to the embodiment of the present invention.
A process flow chart of a method for treating acid titanium dioxide wastewater by a sulfuric acid method, please refer to fig. 1.
Example 1
A method for treating acid wastewater of titanium dioxide by a sulfuric acid process comprises the following steps:
and S1, under stirring treatment, allowing the mixed solution of the acidic wastewater and clear water containing 3-8% of sulfuric acid to automatically flow into a neutralization tank through a fall, pumping limestone slurry into the neutralization tank for first-stage neutralization, wherein the pH value at the end of reaction is 4.0-5.0. Wherein the ratio of the acidic wastewater to the clear water is 1: 25; the stirring speed was 40 r/min.
And S2, continuously stirring, pumping the digested lime slurry, and performing second-stage neutralization, wherein the pH value at the end of the reaction is 7.0-8.5, so as to obtain reaction slurry. The preparation method of the lime slurry comprises the following steps of mixing lime with slaked water after the lime is slaked by a slaking machine or a ball mill, and obtaining the lime slurry, wherein the water temperature is 30-40 ℃; the part of lime which is not digested by the digestion water enters a ball mill to be ground together with the limestone raw material into limestone slurry; the digestion water is press filtration water. Adding 4 tons of slaking water into each ton of lime for slaking; filtering by plate-and-frame filtration.
Pumping the qualified neutralized reaction slurry of S3 into a filter press for filter pressing, wherein the pH value of the reaction slurry is 6.5-8.5;
s4, naturally drying the filter cake after filter pressing, aerating and filtering the filter liquor after filter pressing, and discharging qualified water reaching the standard through detection or using the qualified water as process water. Wherein, continuous aeration is carried out in a mode of connecting a plurality of aeration tanks in series, and the aeration time is 3 h; the process water is used for slaking water in the lime slurry, grinding water for the lime slurry and water for life of titanium white.
Example 2
A method for treating acid wastewater of titanium dioxide by a sulfuric acid process comprises the following steps:
and S1, under stirring treatment, allowing the mixed solution of the acidic wastewater and clear water containing 3-8% of sulfuric acid to automatically flow into a neutralization tank through a fall, pumping limestone slurry into the neutralization tank for first-stage neutralization, wherein the pH value at the end of reaction is 4.0-5.0. Wherein the ratio of the acidic wastewater to the clear water is 1: 40; the stirring speed was 45 r/min.
And S2, continuously stirring, pumping the digested lime slurry, and performing second-stage neutralization, wherein the pH value at the end of the reaction is 7.0-8.5, so as to obtain reaction slurry. The preparation method of the lime slurry comprises the following steps of mixing lime with slaked water after the lime is slaked by a slaking machine or a ball mill, and obtaining the lime slurry, wherein the water temperature is 30-40 ℃; the part of lime which is not digested by the digestion water enters a ball mill to be ground together with the limestone raw material into limestone slurry; the digestion water is press filtration water. Adding 6 tons of slaking water into each ton of lime for slaking; filtering by plate-and-frame filtration.
Pumping the qualified neutralized reaction slurry of S3 into a filter press for filter pressing, wherein the pH value of the reaction slurry is 6.5-8.5;
s4, naturally drying the filter cake after filter pressing, aerating and filtering the filter liquor after filter pressing, and discharging qualified water reaching the standard through detection or using the qualified water as process water. Wherein, continuous aeration is carried out in a mode of connecting a plurality of aeration tanks in series, and the aeration time is 2 h; the process water is used for slaking water in the lime slurry, grinding water for the lime slurry and water for life of titanium white.
Example 3
A method for treating acid wastewater of titanium dioxide by a sulfuric acid process comprises the following steps:
and S1, under stirring treatment, allowing the mixed solution of the acidic wastewater and clear water containing 3-8% of sulfuric acid to automatically flow into a neutralization tank through a fall, pumping limestone slurry into the neutralization tank for first-stage neutralization, wherein the pH value at the end of reaction is 4.0-5.0. Wherein the ratio of the acidic wastewater to the clear water is 1: 35; the stirring speed was 60 r/min.
And S2, continuously stirring, pumping the digested lime slurry, and performing second-stage neutralization, wherein the pH value at the end of the reaction is 7.0-8.5, so as to obtain reaction slurry. The preparation method of the lime slurry comprises the following steps of mixing lime with slaked water after the lime is slaked by a slaking machine or a ball mill, and obtaining the lime slurry, wherein the water temperature is 30-40 ℃; the part of lime which is not digested by the digestion water enters a ball mill to be ground together with the limestone raw material into limestone slurry; the digestion water is press filtration water. Adding 8 tons of slaking water into each ton of lime for slaking; filtering by plate-and-frame filtration.
Pumping the qualified neutralized reaction slurry of S3 into a filter press for filter pressing, wherein the pH value of the reaction slurry is 6.5-8.5;
s4, naturally drying the filter cake after filter pressing, aerating and filtering the filter liquor after filter pressing, and discharging qualified water reaching the standard through detection or using the qualified water as process water. Wherein, continuous aeration is carried out in a mode of connecting a plurality of aeration tanks in series, and the aeration time is 1.5 h; the process water is used for slaking water in the lime slurry, grinding water for the lime slurry and water for life of titanium white.
Example 4
A method for treating acid wastewater of titanium dioxide by a sulfuric acid process comprises the following steps:
and S1, under stirring treatment, allowing the mixed solution of the acidic wastewater and clear water containing 3-8% of sulfuric acid to automatically flow into a neutralization tank through a fall, pumping limestone slurry into the neutralization tank for first-stage neutralization, wherein the pH value at the end of reaction is 4.0-5.0. Wherein the ratio of the acidic wastewater to the clear water is 1: 30; the stirring speed was 50 r/min.
And S2, continuously stirring, pumping the digested lime slurry, and performing second-stage neutralization, wherein the pH value at the end of the reaction is 7.0-8.5, so as to obtain reaction slurry. The preparation method of the lime slurry comprises the following steps of mixing lime with slaked water after the lime is slaked by a slaking machine or a ball mill, and obtaining the lime slurry, wherein the water temperature is 30-40 ℃; the part of lime which is not digested by the digestion water enters a ball mill to be ground together with the limestone raw material into limestone slurry; the digestion water is press filtration water. Adding 5 tons of slaking water into each ton of lime for slaking; filtering by plate-and-frame filtration.
Pumping the qualified neutralized reaction slurry of S3 into a filter press for filter pressing, wherein the pH value of the reaction slurry is 6.5-8.5;
s4, naturally drying the filter cake after filter pressing, aerating and filtering the filter liquor after filter pressing, and discharging qualified water reaching the standard through detection or using the qualified water as process water. Wherein, continuous aeration is carried out in a mode of connecting a plurality of aeration tanks in series, and the aeration time is 2.5 h; the process water is used for slaking water in the lime slurry, grinding water for the lime slurry and water for life of titanium white.
Example 5
A method for treating acid wastewater of titanium dioxide by a sulfuric acid process comprises the following steps:
and S1, under stirring treatment, allowing the mixed solution of the acidic wastewater and clear water containing 3-8% of sulfuric acid to automatically flow into a neutralization tank through a fall, pumping limestone slurry into the neutralization tank for first-stage neutralization, wherein the pH value at the end of reaction is 4.0-5.0. Wherein the ratio of the acidic wastewater to the clear water is 1: 38; the stirring speed was 55 r/min.
And S2, continuously stirring, pumping the digested lime slurry, and performing second-stage neutralization, wherein the pH value at the end of the reaction is 7.0-8.5, so as to obtain reaction slurry. The preparation method of the lime slurry comprises the following steps of mixing lime with slaked water after the lime is slaked by a slaking machine or a ball mill, and obtaining the lime slurry, wherein the water temperature is 30-40 ℃; the part of lime which is not digested by the digestion water enters a ball mill to be ground together with the limestone raw material into limestone slurry; the digestion water is press filtration water. Adding 7 tons of slaking water into each ton of lime for slaking; filtering by plate-and-frame filtration.
Pumping the qualified neutralized reaction slurry of S3 into a filter press for filter pressing, wherein the pH value of the reaction slurry is 6.5-8.5;
s4, naturally drying the filter cake after filter pressing, aerating and filtering the filter liquor after filter pressing, and discharging qualified water reaching the standard through detection or using the qualified water as process water. Wherein, continuous aeration is carried out in a mode of connecting a plurality of aeration tanks in series, and the aeration time is 1 h; the process water is used for slaking water in the lime slurry, grinding water for the lime slurry and water for life of titanium white.
In examples 1 to 6, the standard reaching conditions of the qualified water are as follows: SS is less than 70mg/L, COD is less than 100mg/L, and pH is 6.5-8.5.
In conclusion, the invention can achieve the technical effects of high neutralization efficiency, good aeration effect and low cost.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (8)
1. A method for treating acid wastewater of titanium dioxide by a sulfuric acid process is characterized by comprising the following steps:
s1, under stirring treatment, enabling a mixed solution of the acidic wastewater and clear water containing 3% -8% of sulfuric acid to automatically flow into a neutralization tank through a fall, pumping limestone slurry into the neutralization tank for first-stage neutralization, and enabling the pH value at the end point of the reaction to be 4.0-5.0;
s2, continuously stirring, pumping the digested lime slurry, and performing second-stage neutralization, wherein the pH value at the end of the reaction is 7.0-8.5, so as to obtain reaction slurry;
pumping the qualified neutralized reaction slurry of S3 into a filter press for filter pressing, wherein the pH value of the reaction slurry is 6.5-8.5;
s4, naturally drying the filter cake after filter pressing, aerating and filtering the filter liquor after filter pressing, and discharging qualified water reaching the standard through detection or using the qualified water as process water.
2. The method for treating acidic wastewater containing titanium dioxide produced by a sulfuric acid process according to claim 1, wherein the ratio of the acidic wastewater to the clear water containing 3% to 8% sulfuric acid in S1 is 1:25 to 40.
3. The method for treating acidic wastewater containing titanium dioxide produced by a sulfuric acid process according to claim 1, wherein the stirring speed in S1 is 40 to 60 r/min.
4. The method for treating acidic wastewater containing titanium dioxide prepared by a sulfuric acid process according to claim 1, wherein in S2, lime slurry is prepared by mixing lime treated by a lime slaking machine or a ball mill with slaking water at a water temperature of 30-40 ℃ to obtain lime slurry; the part of lime which is not digested by the digestion water enters a ball mill to be ground together with the limestone raw material into limestone slurry; the digestion water is press filtration water.
5. The method for treating acidic wastewater containing titanium dioxide produced by a sulfuric acid process according to claim 4, wherein 4 to 8 tons of slaking water are added per ton of lime to slake the lime.
6. The method for treating acidic wastewater containing titanium dioxide produced by a sulfuric acid process according to claim 1, wherein in the step S4, the acidic wastewater is filtered by a plate-and-frame filtration method.
7. The method for treating acidic wastewater containing titanium dioxide produced by a sulfuric acid process according to claim 1, wherein in S4, continuous aeration is performed by connecting a plurality of aeration tanks in series, and the aeration time is 1 to 3 hours.
8. The method for treating acidic wastewater containing titanium dioxide produced by sulfuric acid process according to claim 1, wherein in S4, process water is used as the digestion water in the lime slurry, grinding water for the lime slurry and the water for domestic use of titanium dioxide.
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Application publication date: 20210305 |