CN112794488A - Method for synergistic harmless treatment of electrolytic manganese slag leachate and phosphogypsum leachate - Google Patents

Method for synergistic harmless treatment of electrolytic manganese slag leachate and phosphogypsum leachate Download PDF

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Publication number
CN112794488A
CN112794488A CN201911109613.8A CN201911109613A CN112794488A CN 112794488 A CN112794488 A CN 112794488A CN 201911109613 A CN201911109613 A CN 201911109613A CN 112794488 A CN112794488 A CN 112794488A
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leachate
electrolytic manganese
phosphogypsum
manganese slag
liquid separation
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Inventor
舒建成
赵俊杰
罗迪
陈梦君
蔡林宏
邓亚玲
雷天涯
王瑞
严秋玲
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Southwest University of Science and Technology
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Southwest University of Science and Technology
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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
    • C02F1/66—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
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
    • C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
    • 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
    • C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
    • C02F1/54—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using organic material
    • C02F1/56—Macromolecular compounds
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
    • C02F2103/16—Nature of the water, waste water, sewage or sludge to be treated from metallurgical processes, i.e. from the production, refining or treatment of metals, e.g. galvanic wastes
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
    • C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
    • 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

Abstract

The invention discloses a method for synergistically and harmlessly treating electrolytic manganese slag leachate and phosphogypsum leachate, which is mainly characterized in that firstly, the electrolytic manganese slag leachate and the phosphogypsum leachate are conveyed to a mixing device according to a certain mass ratio, after being uniformly mixed, alkaline materials are adopted to adjust the pH value of a mixing system, and after full reaction, solid-liquid separation is carried out; then adding magnesium salt and phosphate into the filtrate according to a certain mass ratio of N to Mg to P, and carrying out solid-liquid separation after full reaction; and finally, adding a small amount of calcium oxide and polyacrylamide into the filtrate, fully reacting, and then carrying out solid-liquid separation, wherein the filtrate can reach the first-class standard GB8978-1996 of sewage comprehensive discharge. Compared with the prior art, the method has the advantages of mild reaction conditions, simple and convenient operation and easily obtained equipment, can greatly reduce manpower and equipment cost, and provides a new method for low-cost treatment of the electrolytic manganese slag leachate and the phosphogypsum leachate in the future.

Description

Method for synergistic harmless treatment of electrolytic manganese slag leachate and phosphogypsum leachate
Technical Field
The invention belongs to the field of environmental protection, and relates to the field of electrolytic manganese and phosphate industrial leachate treatment.
Background
Phosphogypsum is a byproduct generated in the process of producing phosphoric acid by a wet method, has a grey-white or grey-black color, belongs to the second general industrial solid waste, and mainly comprises CaSO4·2H2And O. At present, the global phosphogypsum stockpiling reaches 60 hundred million t, and is still increased at the speed of 10 percent each year. The stockpiling of a large amount of phosphogypsum not only occupies a large amount of cultivated land, but also causes serious pollution to the surrounding environment because the stock dump percolate contains a large amount of phosphorus, fluoride and heavy metal. Therefore, how to treat the phosphogypsum leachate with low cost and harmlessness is a problem to be solved urgently at present, and has important practical significance for green environmental protection and sustainable development of phosphate fertilizer industry.
At present, most of domestic phosphogypsum leachate treatment is recycled, but the device is complex, the cost is high, for example, in a method for recycling phosphogypsum yard leachate in the patent CN 109942112A, although the method has high removal rate of phosphate and fluoride in the phosphogypsum leachate, the process flow is complex; patent CN 109485175A discloses an in-situ treatment system for leachate in a phosphogypsum yard, which can reduce the content of fluoride ions, phosphate ions, total iron and manganese ions in leachate groundwater, but has special requirements on the geographical position of enterprises.
The electrolytic manganese slag is a high-water-content industrial solid waste generated in the production process of electrolytic manganese metal, and contains a large amount of soluble manganese sulfate and ammonium sulfate. At present, 8-10 t of electrolytic manganese slag is generated when 1 t of metal manganese is produced in China. The quantity of the electrolytic manganese slag in China is over 1 hundred million tons, and more than 1000 million tons are newly added every year. The main chemical composition of the electrolytic manganese slag is CaSO4、SiO2、Al2 O3、Fe2 O3MnO and SO3And the phase composition thereof is mainly composed of dihydrate gypsum and silica. The electrolytic manganese slag has high manganese and ammonia nitrogen contents, the highest contents respectively reach 34762 mg/kg and 2987 mg/kg, and in addition, the electrolytic manganese slag also contains sulfate, the content of which reaches 38378 mg/kg. For electrolytic manganese enterprises, electrolytic manganese slag is mostly treated by adopting a stacking or direct landfill mode, and a large amount of leachate containing high-concentration heavy metal and ammonia nitrogen is generated in the stacking process of the electrolytic manganese slag, so that surface water, underground water, rivers and the like around the electrolytic manganese enterprises are seriously polluted.
At present, a great deal of research is carried out on harmless treatment of the electrolytic manganese slag leachate in China, for example, in the method of patent CN 106186455A, saturated clarified lime water, sodium silicate, sodium chloride and an electric field are sequentially added, so that the harmless treatment of the electrolytic manganese slag leachate is realized, but the method has complex process flow and higher cost; patent CN 106242180A discloses an electrolytic manganese slag leachate advanced treatment and recycling device and a method, the method uses an iron scrap micro-electrolysis bed to remove chromium in the electrolytic manganese slag leachate, a stripping tower is used to remove ammonia nitrogen, a reaction tank and an inclined tube sedimentation tank are used to remove heavy metal ions, and a microorganism manganese removal tank is used to remove manganese.
In fact, phosphogypsum leachate contains soluble metal ions, such as Ca2+、Mg2+、PO4 3-、F-、Zn2+、Fe2+、Pb2+、Al3+、Cu2+、Cr6+、As2+. Mn in electrolytic manganese slag leachate2+、NH4 +The plasma soluble ions can react with PO in phosphogypsum leachate4 3-、F-Reacting soluble ions at normal temperature to generate insoluble precipitate; simultaneously electrolyze OH in manganese slag leachate-Can be matched with H in phosphogypsum percolate+Neutralization is carried out, the pH of the mixed stockpiling system can be increased, and Mn is promoted2+、NH4 +、PO4 3-And F-Stable curing of (2). The method is characterized in that the respective characteristics of the electrolytic manganese slag percolate and the phosphogypsum percolate are utilized, phosphate, magnesium salt and alkaline materials are supplemented for harmless treatment, and the problem of percolate pollution caused by respective stockpiling of two industrial wastes in the phosphorization industry and the electrolytic manganese metal industry is solved. The main reaction equations involved are shown below:
OH-+H+=H2O （1）
Mn2++2OH-=Mn(OH)2 （2）
4Mn2++O2+6H2O = 4MnOOH+ 8H+ （3）
xMn2++yPO4 3-+zH2O →MnxH(PO4)y·zH2O↓ （4）
NH4++Mg2++PO4 3-+6H2O→NH4MgPO4·6H2O↓ （5）
(Mn2+, Ca2+, Mg2+) +F-→(Mn, Ca, Mg)F2↓ （6）
NH4+ + Mn2+ + PO4 3- + 6H2O→ NH4MnPO4·6H2O↓ （7）
(Mn2+, Ca2+, Mg2+) + PO4 3-→ (Mn, Ca, Mg)3(PO4)2 （8）
(Mn2+, Ca2+, Mg2+) + HPO4 2-→ (Mn, Ca, Mg)HPO4 （9）
Ca2++PO4 3-+ OH- +2H2O→Ca(PO4)(OH)·2H2O↓ （10）。
disclosure of Invention
The technical problem to be solved by the invention is as follows: the method for harmlessly treating the electrolytic manganese slag leachate and the phosphogypsum leachate in a synergistic manner is provided, the problem of pollution of the electrolytic manganese slag leachate and the phosphogypsum leachate is solved, and the pollution of the electrolytic manganese slag and the phosphogypsum caused by separate accumulation is treated. The technical scheme of the invention is a method for harmlessly treating electrolytic manganese slag leachate and phosphogypsum leachate in a synergistic manner, which comprises the following specific steps:
(1) conveying the electrolytic manganese slag leachate and the phosphogypsum leachate into a reaction tank according to different mass ratios, and stirring and mixing uniformly. Wherein the mass ratio of the electrolytic manganese slag leachate to the phosphogypsum leachate is 1: (0.2 to 12);
(2) and (3) adjusting the pH value of the mixed system in the step (1) to (8-10) by using an alkaline material, and fully stirring at room temperature for (0.5-2) hours. Wherein the alkaline material is one or more of low-grade magnesium oxide, quicklime, burning raw materials and sodium hydroxide;
(3) carrying out solid-liquid separation on the suspension liquid in the claim (2), recycling filter residues, adding magnesium salt and phosphate into the filtrate to enable the mass ratio N to Mg to P =1 (0.5-1) to (0.8-2.4), adjusting the pH value to (8.5-9.5) by using sodium hydroxide, carrying out solid-liquid separation after fully reacting for (0.5-1) hours, and recycling the filter residues. Wherein the phosphate is Na2HPO4、NaH2PO4、Na3PO4Wherein the magnesium salt is one or more of low-grade magnesium oxide and MgCl2、MgSO4One or more of them;
(4) adding calcium oxide into the obtained filtrate in the claim (3), reacting for 0.5-1 hour, adding polyacrylamide, reacting for 15-30 min, and performing solid-liquid separation to obtain a filtrate which reaches the first-level wastewater comprehensive discharge standard GB 8978-1996. Wherein the mass ratio of the calcium oxide to the percolate is (0.05-0.5): 100, the mass concentration of the polyacrylamide is 2 mg/L-10 mg/L.
The invention has the following remarkable advantages: the method solves the problem of pollution of the electrolytic manganese slag percolate and the phosphogypsum percolate essentially, controls the pollution of the independent accumulation of the electrolytic manganese slag and the phosphogypsum to the environment, realizes the synergistic harmless treatment of the electrolytic manganese slag percolate and the phosphogypsum percolate, and reduces the cost of independently treating the electrolytic manganese slag percolate and the phosphogypsum percolate. The alkaline material, the magnesium salt and the phosphate treating agent have the advantages of low cost and easy acquisition, and have popularization value in the phosphorus chemical industry and the electrolytic manganese metal industry.
Example 1:
(1) conveying 10 kg of electrolytic manganese slag leachate and 40kg of phosphogypsum leachate into a reaction tank, and stirring and mixing uniformly;
(2) adjusting the pH value of the mixed system in the step (1) to 9 by adopting low-grade magnesium oxide, and fully stirring for 0.5 hour at room temperature;
(3) performing solid-liquid separation on the suspension in the claim (2), recycling the filter residue, and adding 47.2g MgSO to the filtrate4And 93.6 g Na2HPO4The mass ratio of N to Mg to P =1 to 1 is met, the pH is adjusted to 9 by sodium hydroxide, solid-liquid separation is carried out after the full reaction is carried out for 1 hour, and the filter residue can be recycled;
(4) adding 0.5% of calcium oxide into the obtained filtrate in the step (3), reacting for 0.5 hour, adding 3mg/L polyacrylamide, reacting for 15-30 min, and performing solid-liquid separation to obtain a filtrate which reaches the first-level wastewater comprehensive discharge standard GB 8978-1996.
Example 2:
(1) conveying 10 kg of electrolytic manganese slag leachate and 40kg of phosphogypsum leachate into a reaction tank, and stirring and mixing uniformly;
(2) adjusting the pH value of the mixed system in the step (1) to 9.5 by adopting low-grade magnesium oxide, and fully stirring for 0.5 hour at room temperature;
(3) performing solid-liquid separation on the suspension in the claim (2), recycling the filter residue, and adding 48.0g MgSO to the filtrate4，140.4g Na2HPO4So that the mass ratio of N to Mg to P =1 to 1.5, adjusting the pH to 9.5 with sodium hydroxide,after the reaction is carried out for 1 hour, solid-liquid separation is carried out, and the filter residue can be recycled;
(4) adding 0.2% of calcium oxide into the obtained filtrate in the step (3), reacting for 0.5 hour, performing solid-liquid separation, adding 5 mg/L of polyacrylamide, reacting for 15-30 min, and making the filtrate reach the first-level wastewater comprehensive discharge standard GB 8978-1996.
Example 3:
(1) conveying 10 kg of electrolytic manganese slag leachate and 40kg of phosphogypsum leachate into a reaction tank, and stirring and mixing uniformly;
(2) adjusting the pH value of the mixed system in the step (1) to 9.5 by adopting low-grade magnesium oxide, and fully stirring for 0.5 hour at room temperature;
(3) performing solid-liquid separation on the suspension in the claim (2), recycling the filter residue, and adding 48.0g MgSO4，74.88 g Na2HPO4The mass ratio of N to Mg to P =1 to 0.8 is met, the pH is adjusted to 9.5 by sodium hydroxide, solid-liquid separation is carried out after the full reaction is carried out for 1 hour, and the filter residue can be recycled;
(4) adding 0.4% of calcium oxide into the obtained filtrate in the step (3), reacting for 0.5 hour, performing solid-liquid separation, adding 3mg/L of polyacrylamide, reacting for 15-30 min, and making the filtrate reach the first-level wastewater comprehensive discharge standard GB 8978-1996.
Verification Table 1
Figure DEST_PATH_IMAGE001
As can be seen from the above examples, after the electrolytic manganese slag leachate is mixed with the phosphogypsum leachate for reaction, the concentration of soluble phosphorus is not higher than 0.5 mg/L, the concentration of fluorine ions is not higher than 6.0 mg/L, the concentration of ammonia nitrogen is not higher than 15.0 mg/L, the concentration of manganese ions is less than 1.0 mg/L, and the pH value of the leachate is maintained at 6-9. That is, after the phosphogypsum leachate and the electrolytic manganese slag leachate are mixed and reacted, the fluorine ions, the phosphates, the ammonia nitrogen, the manganese ions and the pH concentration of the leachate meet the primary standard of the Integrated wastewater discharge Standard GB 8978-1996. Therefore, the treatment method can be used for simultaneously and synergistically treating the two solid waste percolates, and is simple, low in cost and high in efficiency.

Claims (4)

1. Conveying the electrolytic manganese slag leachate and the phosphogypsum leachate into a reaction tank according to different mass ratios, and stirring and mixing uniformly. Wherein the mass ratio of the electrolytic manganese slag leachate to the phosphogypsum leachate is 1: (0.2 to 12).
2. And (3) adjusting the pH value of the mixed system in the step (1) to (8-10) by using an alkaline material, and fully stirring at room temperature for (0.5-2) hours. Wherein the alkaline material is one or more of low-grade magnesium oxide, quicklime, burning raw material and sodium hydroxide.
3. Carrying out solid-liquid separation on the suspension liquid in the claim (2), recycling filter residues, adding phosphate and magnesium salt into the filtrate to enable the mass ratio of the phosphate to the magnesium salt to be N, Mg, P =1, (0.5-1) to (0.8-2.4), adjusting the pH value to (8.5-9.5) by using sodium hydroxide, carrying out solid-liquid separation after fully reacting for (0.5-1) hours, and recycling the filter residues. Wherein the phosphate is Na2HPO4、NaH2PO4、Na3PO4Wherein the magnesium salt is one or more of low-grade magnesium oxide and MgCl2、MgSO4One or more of them.
4. Adding calcium oxide into the obtained filtrate in the claim (3), reacting for 0.5-1 hour, adding polyacrylamide, reacting for 15-30 min, and performing solid-liquid separation to obtain a filtrate which reaches the first-level wastewater comprehensive discharge standard GB 8978-1996. Wherein the mass ratio of the calcium oxide to the percolate is (0.05-0.5): 100, the mass concentration of the polyacrylamide is 2 mg/L-10 mg/L.
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