CN113336244A - Method for removing ammonium from brine prepared from waste chlorination residues for ionic membrane caustic soda - Google Patents
Method for removing ammonium from brine prepared from waste chlorination residues for ionic membrane caustic soda Download PDFInfo
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- CN113336244A CN113336244A CN202110732837.5A CN202110732837A CN113336244A CN 113336244 A CN113336244 A CN 113336244A CN 202110732837 A CN202110732837 A CN 202110732837A CN 113336244 A CN113336244 A CN 113336244A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/04—Chlorides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/14—Purification
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/0018—Mixed oxides or hydroxides
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Abstract
The method relates to an ammonium removal method for preparing brine from chlorination residues for ionic membrane caustic soda, which comprises the following steps: a. adding tap water into the chlorination residues according to the slag-water ratio of about 1.0: 1.0-2.0, stirring, filtering and separating to obtain filtrate; b. adding alkali liquor into the filtrate, wherein the volume ratio of the filtrate to the alkali liquor is 1.0: 0.8-1.0, and stirring; c. rapidly adding a sodium hypochlorite solution into the mixed solution, wherein the volume ratio of the mixed solution to the sodium hypochlorite solution is 1.0: 0.4-0.8, and stirring at 500-1000 rpm; d. and after continuously aerating for 1-3 h, standing the solution for 48-72 h, and filtering to obtain brine. According to the method, monochloramine and dichloramine are generated by reacting hypochlorite radicals with ammonium radicals, and can be blown out by means of aeration and air blowing. Solves the problems that the ammonium content in the salt water prepared from the waste of the molten salt chlorination and the waste of the chlorination residues is higher, and the ammonium salt is easy to react in the ion membrane alkali preparation process to generate explosives.
Description
Technical Field
The invention relates to an ammonium removal method for preparing brine from waste chlorination residues for ionic membrane caustic soda, and belongs to the technical field of recycling of waste chlorination residues.
Background
The vanadium-titanium resources in Panxi areas are rich, wherein the titanium reserves account for about 90 percent of the total amount of the titanium resources in China. In order to fully develop Panxi titanium resources, Panxi steel adopts a relatively advanced molten salt chlorination method to produce TiCl4, the process has the characteristics of low production cost and high product quality, but also has the problems of large yield of waste salt (quasi-hazardous waste) and waste salt water (hazardous waste) and serious pollution, and the popularization of the molten salt chlorination technology and the application of primary titanium ore are seriously restricted. Meanwhile, the composition of a large amount of chlorination residue waste brine generated by the process for extracting titanium from blast furnace slag is similar to that of molten salt chlorination waste brine, and the pollution to the environment is serious.
Therefore, a whole set of wastewater treatment process is independently developed in Panzhihua steel, ions such as Fe, Mn and Mg in wastewater are recycled step by step, and finally the waste salt water is used for preparing chlorine and caustic soda by an ion membrane caustic soda process, so that the full resource utilization of the waste salt and the chlorination residues in the molten salt chlorination is realized. The ionic membrane caustic soda process has to strictly control various ionic indexes in initial brine, particularly when the ammonium content is too high, ammonium ions in the brine can generate nitrogen trichloride in the electrolytic process, and the following reaction occurs under the condition that the pH value of an electrolytic bath anolyte is 2-4: NH (NH)3+3HClO→NCl3+3H2And O. The natural explosion temperature of nitrogen trichloride is 95 ℃, the explosion possibility exists when the volume fraction of nitrogen trichloride in chlorine reaches 5.0-6.0%, the nitrogen trichloride can be decomposed and exploded under the conditions of vibration or ultrasonic waves at 60 ℃, and the nitrogen trichloride can be instantaneously exploded under the irradiation of sunlight and magnesium light.
Disclosure of Invention
The invention aims to solve the technical problem that the ammonium content in the salt water prepared from the waste chlorination residue and the waste chlorination salt is high, and the ammonium salt is easy to react in the ion membrane alkali preparation process to generate explosives.
The technical scheme adopted by the invention for solving the technical problems is as follows: the method for removing ammonium from brine prepared from waste chlorination residues for ionic membrane caustic soda comprises the following steps:
a. adding tap water into the chlorination residues according to the slag-water ratio of about 1.0: 1.0-2.0, stirring at 500-1000 rpm for 10-30 min, and filtering and separating after the reaction is finished to obtain filtrate;
b. adding alkali liquor into the filtrate, wherein the volume ratio of the filtrate to the alkali liquor is 1.0: 0.8-1.0, and stirring at 500-1000 rpm;
c. rapidly adding a sodium hypochlorite solution into the mixed solution, wherein the volume ratio of the mixed solution to the sodium hypochlorite solution is 1.0: 0.4-0.8, and stirring at 500-1000 rpm;
d. and after continuously aerating for 1-3 h, standing the solution for 48-72 h, and filtering to obtain brine.
Wherein the chlorination residue in the step a in the method is waste salt or chlorination residue of molten salt chlorination.
Wherein, the alkali liquor in the step a in the method is a sodium carbonate saturated solution of 12 to 17 percent of sodium hydroxide.
Wherein, in the step c of the method, NH is added into the crude brine4+And Fe2+Concentration, in terms of Fe2+:ClO-＝2.0:1.0～1.2，NH4+:ClO-Sodium hypochlorite solution is added at a ratio of 1.0: 1.1-1.2.
Wherein the available chlorine in the sodium hypochlorite solution in the step c in the method is 7-20 g/l.
Wherein the mixed alkali and sodium hypochlorite in the steps b and c in the method are industrial waste alkali liquor or waste brine with the pH value of about 9-13.
The invention has the beneficial effects that: taking climbing steel sponge titanium as an example, the current chlorination waste salt has the annual treatment cost of about 2700 ten thousand yuan per year, and after the invention is adopted, the molten salt chlorination slag has the treatment cost of about 1026 ten thousand yuan per a, the product sale is about 2620 ten thousand yuan per a, and the annual benefit is about 1500 ten thousand yuan. The project not only has good economic benefit, but also has great social benefit. The process comprises the steps of preparing crude brine by water quenching of waste chlorination residues, removing ammonium from the crude brine, further removing impurities from the treated brine for use in ionic membrane caustic soda, and using a ferric hydroxide mixture as a sintering raw material or other alloy production raw materials. The process eliminates the hidden trouble that ammonium in the crude brine generates explosion products in the ion membrane alkali preparation process, is simple, convenient and easy to realize, and provides guarantee for resource utilization of chloride slag. The ammonium content is reduced to below 1mg/l, the ammonium chloride can be used for the ionic membrane caustic soda process through further impurity removal, the resource treatment of different chloride waste residues is realized, the economic benefit is good, the significant significance of eliminating the bottleneck of the application and development of the molten salt chlorination and titanium extraction from blast furnace slag is achieved, the market competitiveness of titanium white chloride and titanium sponge enterprises can be remarkably improved, and the market prospect is wide.
Detailed Description
The present invention will be further described with reference to the following examples.
The method for removing ammonium from brine prepared from waste chlorination residues for ionic membrane caustic soda comprises the following steps:
a. adding tap water into the chlorination residues according to the slag-water ratio of about 1.0: 1.0-2.0, stirring at 500-1000 rpm for 10-30 min, and filtering and separating after the reaction is finished to obtain filtrate;
b. adding alkali liquor into the filtrate, wherein the volume ratio of the filtrate to the alkali liquor is 1.0: 0.8-1.0, and stirring at 500-1000 rpm;
c. rapidly adding a sodium hypochlorite solution into the mixed solution, wherein the volume ratio of the mixed solution to the sodium hypochlorite solution is 1.0: 0.4-0.8, and stirring at 500-1000 rpm;
d. and after continuously aerating for 1-3 h, standing the solution for 48-72 h, and filtering to obtain brine. As will be appreciated by those skilled in the art, the present process converts Fe primarily through hypochlorite2+Oxidation of Fe3+And depositing Fe, Mn, Mg and other ions. Ammonium ions are kept in the alkali liquor, hypochlorite in the added sodium hypochlorite solution reacts with ammonium ions to generate monochloramine and dichloramine, and the monochloramine and dichloramine can be blown out by means of aeration and air blowing and the like, so that the hidden danger of nitrogen trichloride explosion is eliminated.
Preferably, the chlorination residue in the step a in the method is waste salt or chlorination residue of molten salt chlorination. As can be understood by those skilled in the art, the method is only used for preferably selecting the source of the chlorination residues, and realizes the composition of a large amount of chlorination residue waste brine generated in the titanium extraction process from the Fuco slag and the effective recovery and treatment of the molten salt chlorination waste, thereby reducing pollution.
Preferably, the alkali liquor in step a of the method is 12-17% sodium carbonate saturated solution of sodium hydroxide. As will be appreciated by those skilled in the art, the lye of the process is primarily an increase in pH which maintains the overall mixture in an alkaline environment while allowing the major portion of the manganese to precipitate and a minor portion of the ferrous and magnesium to precipitate. In consideration of economy, reaction effect and convenience in field operation, a saturated solution of sodium carbonate is preferred, the concentration of the saturated solution of sodium carbonate is more preferably 12-17% of alkali solution, and the alkali solution is more preferably 15% of sodium carbonate.
Preferably, the process is carried out according to NH in crude brine as described in step c4 +And Fe2+Concentration, in terms of Fe2+:ClO-＝2.0:1.0～1.2，NH4 +:ClO-Sodium hypochlorite solution is added at a ratio of 1.0: 1.1-1.2. It will be appreciated by those skilled in the art that Fe is added to ensure sodium hypochlorite is added2+Total oxidation to Fe3+Preferably, the hypochlorite solution contains more hypochlorite than Fe2+Therefore, the method is preferably performed according to Fe2+:ClO-Sodium hypochlorite solution was added at a ratio of 2.0: 1.0-1.2. To ensure that hypochlorite reacts well with ammonium to form monochloramine and dichloramine, the process is preferably performed as NH4 +:ClO-Sodium hypochlorite solution is added at a ratio of 1.0: 1.1-1.2.
Preferably, in the method, the available chlorine in the sodium hypochlorite solution in the step c is 7-20 g/l. As can be understood by those skilled in the art, in order to ensure the oxidation and replacement effects of the sodium hypochlorite solution, the effective chlorine in the sodium hypochlorite solution is preferably 7-20 g/l in the method.
Preferably, the alkali mixture and sodium hypochlorite in steps b and c in the method are industrial waste lye or waste brine with the pH value of about 9-13. The technical personnel in the field can understand that, in order to reduce the cost and simultaneously realize the purpose of treating wastes with wastes, the mixed alkali and sodium hypochlorite used in practice are waste alkali liquids generated in other working sections in a plant, wherein the mixed alkali and the sodium hypochlorite contain sodium carbonate, sodium hypochlorite and the like, and the pH value is ensured to meet 9-13.
Example 1
(1) 1kg of fused salt chlorination slag is taken and added into 1.5L of tap water to be stirred and dissolved. And filtering after the molten salt chlorination residues are completely dissolved to obtain 1.34L crude salt water. Crude brine composition and process for producing the sameThe amounts are shown in Table 1-1. Wherein NH4 +The content was 50 mg/l.
TABLE 1-1 crude brine composition (g/l)
| pH | Na+ | Fe2+ | Mg2+ | Mn2+ | Ca2+ | Ti | NH4 + |
| 1.34 | 25.0 | 38.3 | 37.1 | 5.8 | 2.3 | <0.01 | 0.05 |
(2) 1.2L of a saturated solution of sodium carbonate containing 15% sodium hydroxide was slowly added with stirring, and stirring was continued at 800 rpm.
(3) 1L of a sodium hypochlorite solution having an available chlorine content of 18.1g/L was rapidly added to the solution, and stirred at 1000 rpm.
(4) Aerating for 2h, standing the solution for 48h, and filtering to obtain qualified saline water, wherein the components of the qualified saline water are shown in tables 1-2. Qualified Fe in brine2+、Mn2+The content of the NH4+ is less than 1mg/l while the content of the NH4+ is less than 1 mg/l.
TABLE 1-2 quality brine composition (g/l)
| Na+ | Fe2+ | Mg2+ | Mn2+ | Ca2+ | Al3+ | Ti | NH4 + |
| 63.2 | <0.001 | 26.8 | <0.001 | 0.04 | <0.001 | <0.001 | <0.001 |
Example 2
(1) 1kg of chlorination residue was taken, and 1.5L of tap water was added thereto, and stirred at 1000rpm for 30 min. The solution was filtered to give 1.38L of tailings wash water (crude brine). The composition and content of the crude brine are shown in Table 2-1. The NH4+ content was 160 mg/l.
TABLE 2-1 crude brine composition (g/l)
| pH | Na+ | Fe2+ | Mg2+ | Mn2+ | Ca2+ | Al3+ | Ti | NH4 + |
| 3.1 | 0.60 | 7.10 | 2.31 | 1.01 | 15.4 | 0.07 | <0.001 | 0.16 |
(2) 1.2L of a saturated solution of sodium carbonate containing 15% sodium hydroxide was slowly added with stirring, and stirring was continued at 1000 rpm.
(3) 0.5L of a sodium hypochlorite solution having an available chlorine content of 8.01g/L was rapidly added to the solution, and stirred at 800 rpm.
(4) Aerating for 3h, standing the solution for 72h, and filtering to obtain qualified saline water, wherein the components of the qualified saline water are shown in a table 2-2. Qualified Fe in brine2+、Mn2+The content of the fluorine ions is less than 1 mg/l.
TABLE 2-2 quality brine composition (g/l)
| Fe2+ | Mg2+ | Mn2+ | Ca2+ | Al3+ | Ti | NH4 + |
| <0.001 | 2.23 | <0.001 | 0.02 | <0.001 | <0.001 | <0.001 |
In conclusion, the brine Fe finally prepared by the method2+、Mn2+And the ammonium ions and the like meet the requirements of the ionic membrane caustic soda process on brine, and the waste brine is finally used for preparing chlorine and caustic soda by the ionic membrane caustic soda process, so that the full resource utilization of the waste salt and the chlorination residues in the molten salt chlorination is realized.
Claims (6)
1. The method for removing ammonium from brine prepared from waste chlorination residues for ionic membrane caustic soda is characterized by comprising the following steps:
a. adding tap water into the chlorination residues according to the slag-water ratio of about 1.0: 1.0-2.0, stirring at 500-1000 rpm for 10-30 min, and filtering and separating after the reaction is finished to obtain filtrate;
b. adding alkali liquor into the filtrate, wherein the volume ratio of the filtrate to the alkali liquor is 1.0: 0.8-1.0, and stirring at 500-1000 rpm;
c. rapidly adding a sodium hypochlorite solution into the mixed solution, wherein the volume ratio of the mixed solution to the sodium hypochlorite solution is 1.0: 0.4-0.8, and stirring at 500-1000 rpm;
d. and after continuously aerating for 1-3 h, standing the solution for 48-72 h, and filtering to obtain brine.
2. The method for removing ammonium from brine prepared from waste chlorination residues for ionic membrane caustic soda according to claim 1, which is characterized by comprising the following steps: the chlorination residue in the step a is molten salt chlorination waste salt or chlorination residue.
3. The method for removing ammonium from brine prepared from waste chlorination residues for ionic membrane caustic soda according to claim 1, which is characterized by comprising the following steps: the alkali liquor in the step a is a sodium carbonate saturated solution of 12-17% of sodium hydroxide.
4. The method for removing ammonium from brine prepared from waste chlorination residues for ionic membrane caustic soda according to claim 1, which is characterized by comprising the following steps: according to NH in crude brine in step c4 +And Fe2+Concentration, in terms of Fe2+:ClO-＝2.0:1.0～1.2，NH4 +:ClO-Sodium hypochlorite solution is added at a ratio of 1.0: 1.1-1.2.
5. The method for removing ammonium from brine prepared from waste chlorination residues for ionic membrane caustic soda according to claim 1, which is characterized by comprising the following steps: in the step c, the available chlorine in the sodium hypochlorite solution is 7-20 g/l.
6. The method for removing ammonium from brine prepared from waste chlorination residues for ionic membrane caustic soda according to claim 1, which is characterized by comprising the following steps: the mixed alkali and the sodium hypochlorite in the steps b and c are industrial waste alkali liquor or waste brine with the pH value of about 9-13.
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Application publication date: 20210903 |