CN110627279A - Treatment method of high-concentration salt-containing waste sulfuric acid - Google Patents
Treatment method of high-concentration salt-containing waste sulfuric acid Download PDFInfo
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- CN110627279A CN110627279A CN201910790618.5A CN201910790618A CN110627279A CN 110627279 A CN110627279 A CN 110627279A CN 201910790618 A CN201910790618 A CN 201910790618A CN 110627279 A CN110627279 A CN 110627279A
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- sulfuric acid
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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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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F11/00—Treatment of sludge; Devices therefor
- C02F11/12—Treatment of sludge; Devices therefor by de-watering, drying or thickening
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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
- C02F9/00—Multistage treatment of water, waste water or sewage
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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
- 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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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/101—Sulfur compounds
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Removal Of Specific Substances (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention provides a method for treating high-concentration salt-containing waste sulfuric acid, which is characterized by comprising the following steps of: (1) preparing quicklime or limestone and water into slurry with a certain concentration; (2) adding a proper amount of inducer into a reaction tank containing high-concentration salt-containing waste sulfuric acid; (3) adding the slurry into the reaction tank, stirring and measuring the pH value, stopping adding the slurry when the pH value is increased to be within the range of 3-5, and continuing stirring for a period of time; (4) adding a proper amount of calcium chloride into the reaction tank, and stirring for a period of time; (5) and filtering the solution in the reaction tank, evaporating and crystallizing the filtrate, and drying the filter residue to obtain the calcium sulfate dihydrate. Therefore, the method for treating the high-concentration salt-containing waste sulfuric acid can greatly reduce the salt content of the wastewater entering the evaporator, save the evaporation energy consumption, greatly reduce the output of the salt slurry, obtain the calcium sulfate dihydrate and realize the resource utilization of the high-concentration salt-containing waste sulfuric acid.
Description
Technical Field
The invention relates to the technical field of waste sulfuric acid treatment, in particular to a treatment method of high-concentration salt-containing waste sulfuric acid.
Background
The waste sulfuric acid containing salt is mainly from the production process flow of industrial enterprises engaged in metal surface treatment, electronic element manufacturing and the like. In the manufacturing process of electronic elements, acid is needed to be used for processes such as electrolytic degreasing, acid etching, sensitization before activation, catalysis, polishing and the like, and a large amount of high-salt-content waste acid liquor is generated in the manufacturing process; also, in the production of liquid crystal displays or integrated circuit boards, oxide etching using acid etchants is required, and a large amount of highly salt-containing spent acid solution is also generated. For example, in metal surface treatment and other industries, it is necessary to use acid for surface cleaning, and sulfuric acid for acid etching, electrolytic degreasing, surface sensitization, acid carbonization, electrolytic polishing, catalysis, etc., which all generate salt-containing waste acid.
In the process, the production amount of the salt-containing waste sulfuric acid is large, and the production amount of enterprises with integrated circuit boards reaches 2000-3000 tons/month. The waste liquid has strong acidity, and the pH value is between 1 and 2, sometimes even lower than 1. The sulfate radical concentration is large and is between 20 and 60g/L, the chloride ion concentration is between 10 and 30g/L, the total salt content is between 40 and 100g/L, and ions such as sodium, potassium, magnesium, copper, calcium and the like are usually contained.
The salt-containing waste sulfuric acid belongs to high-concentration salt-containing waste liquid, and is classified as dangerous waste due to the strong corrosiveness of the waste sulfuric acid. Therefore, the sewage is required to be subjected to harmless treatment and can be discharged into a corresponding receiving water body after meeting the requirements of relevant discharge standards. The state also provides relevant regulations, for example, salt-containing waste sulfuric acid belongs to HW34 waste acid hazardous waste in national hazardous waste records (2016), and requires harmless treatment according to a hazardous waste management system.
At present, in hazardous waste disposal enterprises, the waste liquid is generally treated by a method of neutralization and other pretreatment and then evaporative crystallization. Due to the high salt content, salt substances exist in the form of salt mud after evaporation and crystallization. Due to complex components and more impurities, the produced salt mud cannot be effectively utilized. The method considers that the leachate has too high salinity due to leaching of the salinity, so that the normal operation of a leachate treatment system is influenced, and a landfill site is unwilling to receive salt mud for landfill. Therefore, the salt mud cannot be disposed and is stacked in a warehouse due to the fact that the salt mud is treated by the evaporation crystallization method after neutralization.
Therefore, it is necessary to provide a method for treating waste sulfuric acid containing salt at high concentration to solve the above-mentioned disadvantages of the prior art.
Disclosure of Invention
The invention aims to provide a method for treating high-concentration salt-containing waste sulfuric acid, which can greatly reduce the salt content of waste water entering an evaporator, save evaporation energy consumption, greatly reduce the production amount of salty mud, obtain calcium sulfate dihydrate and realize the resource utilization of the high-concentration salt-containing waste sulfuric acid.
In order to realize the aim, the invention provides a method for treating high-concentration salt-containing waste sulfuric acid, which comprises the following steps:
(1) preparing quicklime or limestone and water into slurry with a certain concentration;
(2) adding a proper amount of inducer into a reaction tank containing high-concentration salt-containing waste sulfuric acid;
(3) adding the slurry into the reaction tank, stirring and measuring the pH value, stopping adding the slurry when the pH value is increased to be within the range of 3-5, and continuing stirring for a period of time;
(4) adding a proper amount of calcium chloride into the reaction tank, and stirring for a period of time;
(5) and filtering the solution in the reaction tank, evaporating and crystallizing the filtrate, and drying the filter residue to obtain the calcium sulfate dihydrate.
Compared with the prior art, in the method for treating the high-concentration salt-containing waste sulfuric acid, quicklime or limestone and water are prepared into slurry with a certain concentration, and the slurry is added into the high-concentration salt-containing waste sulfuric acid, so that the accuracy of the quicklime or limestone required in the neutralization reaction is improved; adding an inducer to crystallize the product, controlling the reaction speed by controlling the pH value to generate crystals, supplementing calcium ions by adding calcium chloride, and crystallizing more sulfate ions to generate calcium sulfate dihydrate, wherein the prepared product is the calcium sulfate dihydrate, and the quality can meet the requirements of first-grade products in GB/T23456-2009 phosphogypsum. Therefore, the method for treating the high-concentration salt-containing waste sulfuric acid can greatly reduce the salt content of the wastewater entering the evaporator, save the evaporation energy consumption, greatly reduce the output of the salt slurry, obtain the calcium sulfate dihydrate and realize the resource utilization of the high-concentration salt-containing waste sulfuric acid.
Preferably, the inducer is a sulfate. Wherein the sulfate is selected from at least one of sodium sulfate, calcium sulfate or potassium sulfate.
Preferably, the concentration of the slurry is 50 g/L-300 g/L. For example, the slurry concentration is 50g/L, 100g/L, 150g/L, 200g/L, 250g/L, or 300 g/L.
Preferably, the addition amount of the calcium chloride is 2-8% of the mass of the sulfate in the high-concentration salt-containing waste sulfuric acid. For example, the addition amount of calcium chloride is 2%, 4%, 6%, 8% of the mass of sulfate in the high-concentration salt-containing waste sulfuric acid.
Preferably, the calcium chloride is in a powder state or prepared into a solution.
Preferably, the stirring speed is 50 r/min-150 r/min. For example, the stirring speed is 50r/min, 70r/min, 90r/min, 110r/min, 130r/min, 150 r/min.
Preferably, the filtration in the step (5) is performed by pressure filtration by using a plate-and-frame filter press.
Preferably, the drying temperature of the filter residue is 105 ℃, and the drying time is 0.5-2 h.
Drawings
FIG. 1 is a process flow chart of the method for treating high-concentration salt-containing waste sulfuric acid.
Detailed Description
FIG. 1 is a process flow chart of the method for treating high-concentration salt-containing waste sulfuric acid, and as can be seen from FIG. 1, the method for treating high-concentration salt-containing waste sulfuric acid comprises the following steps:
s1: adding a proper amount of water into the slurry tank, introducing a proper amount of quicklime or limestone into the slurry tank from a storage bin through a meter, starting a stirrer to stir for a period of time, and uniformly mixing the slurry to obtain slurry.
S2: and (3) sending the waste sulfuric acid containing high-concentration salt into a reaction tank from a waste acid storage tank by using a pump, adding a proper amount of an inducer, and starting a stirrer to stir for a period of time to uniformly mix the solution.
S3: and (3) sending the slurry from the slurry tank into a reaction tank by using a pump through a flowmeter, starting a stirrer to stir at a certain rotating speed, measuring the pH value of the feed liquid in real time, stopping adding the slurry when the pH value is increased to be within a range of 3-5, and continuously stirring for a period of time.
S4: adding a proper amount of calcium chloride powder or solution into the reaction tank, and starting a stirrer to stir at a certain rotating speed for a period of time.
S5: and (3) introducing the feed liquid in the reaction tank into a plate-and-frame filter press by using a pump, opening the plate-and-frame filter press for filter pressing, and collecting filtrate in a storage tank.
S6: drying the filter residue at 105 ℃ for a certain time by using a dryer.
S7: and packaging and storing the dried filter residue.
S8: the filtrate is sent to an evaporator by a pump from a filtrate storage tank for evaporation crystallization.
The method for treating waste sulfuric acid containing high concentration salt according to the present invention will be described below with reference to specific examples.
Example 1
The method for treating the high-concentration salt-containing waste sulfuric acid in the embodiment comprises the following steps:
(1) taking quicklime as a neutralizer, and preparing the quicklime and water into slurry with the concentration of 200 g/L;
(2) 2m is added into the reaction tank3The pH value of the high-concentration salt-containing waste sulfuric acid is 1.6, the concentration of sulfate ions is 51.9g/L, and chloride ions are detectedThe seed concentration is 12.8g/L, 7kg of inducer is added into the reaction tank, and the mixture is stirred uniformly;
(3) gradually adding the slurry into a reaction tank, continuously stirring in the reaction process at a stirring speed of 100r/min, measuring the pH value of the feed liquid in real time, stopping adding the slurry when the pH value is 4, and continuously stirring for 1 hour;
(4) adding 4.4kg of calcium chloride powder into a reaction tank, and uniformly stirring at the stirring speed of 100r/min for 1 hour;
(5) and (3) conveying the solution in the reaction tank to a plate-and-frame filter press for filter pressing, conveying the filtrate to an evaporator for evaporation crystallization, conveying the filter residue to a dryer for drying at 105 ℃ for 1 hour, and then packaging to obtain a product, namely the calcium sulfate dihydrate with the weight of 178 kg.
Example 2
The method for treating the high-concentration salt-containing waste sulfuric acid in the embodiment comprises the following steps:
(1) taking quicklime as a neutralizer, and preparing the quicklime and water into slurry with the concentration of 200 g/L;
(2) 2m is added into the reaction tank3Measuring the pH value of the high-concentration salt-containing waste sulfuric acid to be 1.1, the sulfate ion concentration to be 58.5g/L and the chloride ion concentration to be 18.3g/L, adding 15kg of inducer into a reaction tank, and uniformly stirring;
(3) gradually adding the slurry into a reaction tank, continuously stirring in the reaction process at a stirring speed of 100r/min, measuring the pH value of the feed liquid in real time, stopping adding the slurry when the pH value is 3, and continuously stirring for 1 hour;
(4) adding 2.0kg of calcium chloride powder into a reaction tank, and uniformly stirring at the stirring speed of 100r/min for 1 hour;
(5) and (3) conveying the solution in the reaction tank to a plate-and-frame filter press for filter pressing, conveying the filtrate to an evaporator for evaporation crystallization, conveying the filter residue to a dryer for drying at 105 ℃ for 2 hours, and then packaging to obtain a product, namely calcium sulfate dihydrate with the weight of 210 kg.
Comparative example 1
The method for treating the high-concentration salt-containing waste sulfuric acid in the comparative example comprises the following steps:
the original process comprises the following steps: the same high-concentration salt-containing waste sulfuric acid as in example 1 was neutralized with NaOH solution to a pH of 7 to 8, and the neutralized solution was subjected to evaporative crystallization to obtain a salt slurry.
Comparative example 2
The method for treating the high-concentration salt-containing waste sulfuric acid in the comparative example comprises the following steps:
the original process comprises the following steps: the same high-concentration salt-containing waste sulfuric acid as in example 2 was neutralized with NaOH solution to a pH of 7 to 8, and the neutralized solution was subjected to evaporative crystallization to obtain a salt slurry.
Comparative example 3
The method for treating the high-concentration salt-containing waste sulfuric acid in the comparative example comprises the following steps:
(1) taking quicklime as a neutralizer, and preparing the quicklime and water into slurry with the concentration of 200 g/L;
(2) 2m is added into the reaction tank3The pH value of the high-concentration salt-containing waste sulfuric acid is 1.1, the sulfate ion concentration is 58.5g/L, and the chloride ion concentration is 18.3 g/L;
(3) gradually adding the slurry into a reaction tank, continuously stirring in the reaction process at a stirring speed of 100r/min, measuring the pH value of the feed liquid in real time, stopping adding the slurry when the pH value is 3, and continuously stirring for 1 hour;
(4) adding 2.0kg of calcium chloride powder into a reaction tank, and uniformly stirring at the stirring speed of 100r/min for 1 hour;
(5) and (3) conveying the solution in the reaction tank to a plate-and-frame filter press for filter pressing, conveying the filtrate to an evaporator for evaporation crystallization, and conveying the filter residue to a dryer for drying at 105 ℃ for 2 hours to obtain calcium sulfate dihydrate.
Comparative example 4
The method for treating the high-concentration salt-containing waste sulfuric acid in the comparative example comprises the following steps:
(1) taking quicklime as a neutralizer, and preparing the quicklime and water into slurry with the concentration of 200 g/L;
(2) 2m is added into the reaction tank3The pH value of the high-concentration salt-containing waste sulfuric acid is 1.1, the concentration of sulfate ions is 58.5g/L, and the concentration of chloride ions is measuredThe degree is 18.3g/L, 15kg of inducer is added into the reaction tank, and the mixture is stirred uniformly;
(3) gradually adding the slurry into a reaction tank, continuously stirring in the reaction process at a stirring speed of 100r/min, measuring the pH value of the feed liquid in real time, stopping adding the slurry when the pH value is 2, and continuously stirring for 1 hour;
(4) adding 2.0kg of calcium chloride powder into a reaction tank, and uniformly stirring at the stirring speed of 100r/min for 1 hour;
(5) and (3) conveying the solution in the reaction tank to a plate-and-frame filter press for filter pressing, conveying the filtrate to an evaporator for evaporation crystallization, and conveying the filter residue to a dryer for drying at 105 ℃ for 2 hours to obtain calcium sulfate dihydrate.
The amount of the salt sludge and the sulfate ion concentration generated in the treatment methods of examples 1 to 2 and comparative examples 1 to 4 were measured, and the results are shown in Table 1:
as can be seen from the table 1, the treatment method of the high-concentration salt-containing waste sulfuric acid can greatly reduce the salt content of the waste water entering the evaporator, save the evaporation energy consumption, greatly reduce the yield of the salty mud, obtain the calcium sulfate dihydrate and realize the resource utilization of the high-concentration salt-containing waste sulfuric acid. Wherein, the lack of the inducer in the step (2) can cause that the product can not be crystallized, the calcium sulfate dihydrate product can not be obtained, and the resource utilization can not be realized. When the pH value in the step (3) is less than 3, the reaction speed is high, the product is not crystallized, the water content is high, the calcium sulfate dihydrate product cannot be obtained, and the resource utilization cannot be realized.
The present invention has been described in connection with the preferred embodiments, but the present invention is not limited to the embodiments disclosed above, and is intended to cover various modifications, equivalent combinations, which are made in accordance with the spirit of the present invention.
Claims (9)
1. A method for treating waste sulfuric acid containing high concentration salt is characterized by comprising the following steps:
(1) preparing quicklime or limestone and water into slurry with a certain concentration;
(2) adding a proper amount of inducer into a reaction tank containing high-concentration salt-containing waste sulfuric acid;
(3) adding the slurry into the reaction tank, stirring and measuring the pH value, stopping adding the slurry when the pH value is increased to be within the range of 3-5, and continuing stirring for a period of time;
(4) adding a proper amount of calcium chloride into the reaction tank, and stirring for a period of time;
(5) and filtering the solution in the reaction tank, evaporating and crystallizing the filtrate, and drying the filter residue to obtain the calcium sulfate dihydrate.
2. The method for treating waste sulfuric acid containing high concentration salt according to claim 1, wherein the inducer is sulfate.
3. The method for treating waste sulfuric acid containing high concentration salt according to claim 2, wherein the sulfate is at least one selected from sodium sulfate, calcium sulfate and potassium sulfate.
4. The method for treating high-concentration salt-containing spent sulfuric acid according to claim 1, wherein the concentration of the slurry is 50 to 300 g/L.
5. The method for treating waste sulfuric acid containing high concentration salt according to claim 1, wherein the amount of the added calcium chloride is 2-8% of the mass of the sulfate in the waste sulfuric acid containing high concentration salt.
6. The method according to claim 1, wherein the calcium chloride is in a powder state or is prepared into a solution.
7. The method for treating waste sulfuric acid containing high concentration salt as claimed in claim 1, wherein the stirring speed is 50r/min to 150 r/min.
8. The method for treating waste sulfuric acid containing high concentration salt according to claim 1, wherein the drying temperature of the filter residue is 105 ℃, and the drying time is 0.5 h-2 h.
9. The method for treating waste sulfuric acid containing high concentration salts according to claim 1, wherein the filtration in the step (5) is performed by press filtration using a plate and frame filter press.
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Cited By (3)
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CN111362292A (en) * | 2020-03-17 | 2020-07-03 | 中国科学院过程工程研究所 | Continuous production system and method for producing low-water-content calcium sulfate from waste sulfuric acid |
CN112573786A (en) * | 2020-10-12 | 2021-03-30 | 江苏荣信环保科技有限公司 | Treatment process for waste sulfuric acid sludge on surface of metal product |
CN114031104A (en) * | 2021-12-14 | 2022-02-11 | 江西思远再生资源有限公司 | Composite process for producing calcium sulfate and regenerating HCl through solvent replacement |
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