CN111892222B - Ammonium sulfate wastewater recycling method - Google Patents
Ammonium sulfate wastewater recycling method Download PDFInfo
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- CN111892222B CN111892222B CN202010754919.5A CN202010754919A CN111892222B CN 111892222 B CN111892222 B CN 111892222B CN 202010754919 A CN202010754919 A CN 202010754919A CN 111892222 B CN111892222 B CN 111892222B
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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
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
- C02F1/041—Treatment of water, waste water, or sewage by heating by distillation or evaporation by means of vapour compression
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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
- C02F1/20—Treatment of water, waste water, or sewage by degassing, i.e. liberation of dissolved gases
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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
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
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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
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/16—Nitrogen compounds, e.g. ammonia
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Abstract
The invention discloses a recycling method of ammonium sulfate wastewater, which comprises the following steps: the ammonium sulfate wastewater is treated by a membrane, concentrated to obtain ammonium sulfate concentrated water, and then reacted with sodium hydroxide until the pH value is 10-12; separating ammonia from liquid by adopting an air stripping method, absorbing the obtained ammonia with water or ammonia water, recycling the ammonia to the neutralization of the meta-titanic acid and the ammonia water, and carrying out wet desulfurization; carrying out MVR treatment on the solution after the stripping treatment, and separating and concentrating to obtain sodium sulfate; and (2) preparing high-salt water from sodium sulfate, further preparing sodium hydroxide from the high-salt water, and recycling the sodium hydroxide to the step (S2). According to the invention, ammonium sulfate which is often used as a fertilizer is recycled, so that the waste side is recycled while the environment-friendly treatment pressure of high ammonia nitrogen wastewater is reduced, the corresponding raw material cost is reduced, and the recycling of waste side in production is promoted.
Description
Technical Field
The invention belongs to the technical field of waste side recycling, and particularly relates to a recycling method of ammonium sulfate wastewater.
Background
Ammonia nitrogen refers to ammonia (NH) in water in free form 3 ) And ammonium ion (NH) 4 + ) Excessive ammonia nitrogen is discharged into the water body, so that the water body is eutrophicated, and aquatic plants and animals die. The traditional treatment method of ammonia nitrogen in the water body comprises a stripping method, a zeolite deamination method, a break point chlorination method and the like. The stripping method (comprising air or water vapor) has simple process and stable effect, but high energy consumption, particularly the stripping process (adopting water vapor stripping), and the ammonia nitrogen in the effluent is still higher; the zeolite deamination method needs to consider the regeneration problem of zeolite; the break point chlorination process has high cost and can produceHarmful gas is generated.
Titanium dioxide is widely applied to the fields of paint, plastics, paper making, printing ink and the like due to the characteristics of excellent whiteness, hiding power, weather resistance, chemical stability and the like.
The traditional sulfuric acid process titanium dioxide production process comprises the following steps:
(1) Acidolysis: acidolysis reaction is carried out on the titanium concentrate or acid-soluble waste residue and sulfuric acid to obtain titanyl sulfate;
(2) Hydrolysis: hydrolyzing titanyl sulfate to obtain metatitanic acid slurry;
(3) And (3) washing: washing the hydrolyzed metatitanic acid slurry with water;
(4) Bleaching and secondary washing: bleaching and washing the first washed meta-titanic acid with calcined seed crystal to obtain qualified meta-titanic acid slurry;
(5) Salt treatment: performing salt treatment and filter pressing on the qualified meta-titanic acid subjected to water washing to obtain a filter cake before a kiln;
(6) Calcining: delivering the filter cake before the kiln into a rotary kiln for calcination to obtain a kiln falling product;
(7) Post-treatment: and (3) carrying out organic/inorganic coating and other technological treatments on the kiln falling products to obtain titanium dioxide finished products.
In the step (6), the calcination process is divided into four stages of dehydration, desulfurization, crystal form transformation and particle growth, and in production practice, it is found that the qualified meta-titanic acid subjected to bleaching and washing in the step (4) still contains about 7% of chemisorbed sulfuric acid (including a part of bound acid), and the part of sulfuric acid cannot be removed in the water washing process, can be removed only at high temperature in a calcining kiln, and can inhibit the conversion of rutile and the growth of particles, so that the cost of tail gas treatment and the energy consumption of calcination are increased, and the material is easy to sinter at high temperature and difficult to grind at later stage.
A method of neutralization and wet sulfur removal with aqueous ammonia is disclosed in the publication CN108408770 a. In the method, ammonia water is used for neutralizing the meta-titanic acid, so that the sulfur content in the titanium dioxide is reduced. In the process, although the content of sulfur oxide generated in the calcination process is reduced, the pressure for treating the calcination tail gas is reduced, a large amount of ammonium sulfate wastewater is generated, and the pressure for treating the ammonium sulfate wastewater is brought. At present, more treatment methods are adopted as membrane treatment methods, and although the ammonium sulfate wastewater can be treated by using membrane treatment, the method is simple and convenient to operate and has no secondary pollution, but the treatment concentration is limited and the yield is not high due to the requirement of the upper limit of ammonia nitrogen in water entering a filtering membrane in the membrane treatment process.
Disclosure of Invention
The invention aims to provide a recycling method of ammonium sulfate wastewater, which aims to solve the defects in the prior art.
The invention aims at realizing the following technical scheme:
the method for recycling the ammonium sulfate wastewater comprises the following steps:
s1: firstly, performing membrane treatment on the ammonium sulfate wastewater, and concentrating to obtain ammonium sulfate concentrated water;
s2: taking the ammonium sulfate concentrated water obtained in the step S1 to react with sodium hydroxide until the pH value is 10-12, and generating ammonia gas;
s3: separating ammonia from liquid by adopting an air stripping method, absorbing the obtained ammonia with water or ammonia water, recycling the ammonia to the neutralization of the meta-titanic acid and the ammonia water, and carrying out wet desulfurization;
s4: carrying out MVR evaporation concentration system treatment on the solution subjected to the stripping treatment in the step S3, and separating and concentrating to obtain sodium sulfate;
s5: and (3) preparing high-salt water from the sodium sulfate processed by the evaporation and concentration system of the step S4 MVR, and further preparing sodium hydroxide from the high-salt water, and recycling the sodium hydroxide to the step S2.
Preferably, the ammonia nitrogen content in the ammonium sulfate concentrated water after the membrane treatment in the step S1 is 7000-12000 mg/L.
Preferably, the mass fraction of sodium hydroxide adopted in the step S2 is 20-50%.
Preferably, the air stripping method in step S3 is performed by air stripping.
Preferably, the ammonia removal rate of the solution after the stripping treatment in the step S3 is 50-90%.
Preferably, the membrane treatment in step S1 is a reverse osmosis membrane treatment.
Preferably, the ammonium sulfate wastewater is ammonium sulfate wastewater generated in the wet desulfurization process by neutralizing meta-titanic acid with ammonia water
According to the invention, ammonium sulfate which is often used as a fertilizer is recycled on the basis of the prior art, so that the waste side is recycled while the environment-friendly treatment pressure of high ammonia nitrogen wastewater is reduced, the corresponding raw material cost is reduced, and the recycling of the waste side in production is promoted.
Detailed Description
The invention provides a recycling method of ammonium sulfate wastewater, which comprises the following steps:
s1: firstly, carrying out membrane treatment on the ammonium sulfate wastewater, and improving the concentration of ammonium sulfate to obtain ammonium sulfate concentrated water;
s2: taking the concentrated ammonium sulfate water obtained in the step S1 to react with sodium hydroxide generated by a chlor-alkali process until the pH value is 10-12, and generating ammonia gas;
s3: separating ammonia from liquid by adopting an air stripping method, absorbing the obtained ammonia with water or ammonia water, recycling the ammonia to the neutralization of the meta-titanic acid and the ammonia water, and carrying out wet desulfurization; ammonia is removed by an air stripping method, and the removal rate is 50-90%; specifically, the ammonia-containing ammonium sulfate concentrated water is blown off by air or steam, ammonia continuously escapes from the solution in the blowing-off process, and is discharged from an ammonia outlet, and most ammonia nitrogen in the solution is removed after blowing-off, and the solution also contains a small amount of ammonia nitrogen and a large amount of sulfate radicals and sodium ions;
s4: carrying out MVR evaporation concentration system treatment on the solution subjected to the air stripping treatment in the step S3, separating ammonia nitrogen, sulfate radicals and sodium ions, enabling the ammonia nitrogen to enter an evaporation condensate water system, separating out sodium sulfate in a solid salt form, and centrifuging to obtain sodium sulfate solids and mother liquor containing sodium sulfate, so that the solution subjected to the air stripping treatment can be separated and concentrated to obtain sodium sulfate and evaporation condensate water containing ammonia nitrogen after the MVR treatment; specifically, the MVR evaporation concentration system generally comprises a preheater, an evaporator, a gas-liquid separator, a crystallizer, a centrifuge, a compressor, a pump set and other components, secondary steam subjected to compression, temperature rise and pressure rise is recycled, ammonia nitrogen can be evaporated into an evaporation condensate water system under the alkaline high-temperature condition, and further separation of the ammonia nitrogen and sodium sulfate solution is realized; concentrating the sodium sulfate solution after separating ammonia nitrogen, when the solution reaches a certain saturation state, enabling the solution to flow into a crystallizer for crystallization, and then further separating the solution by a centrifugal machine to obtain sodium sulfate solid and sodium sulfate mother liquor; the MVR evaporation concentration system fully utilizes the latent heat of steam, so that the heat exchange efficiency is high, and the energy consumption and the operation cost are low;
s5: the sodium sulfate solid obtained after the treatment of the MVR evaporation concentration system in the step S4 is basically free of ammonia nitrogen, can be recycled to a chlor-alkali process, high-salt water is prepared, sodium hydroxide is further prepared from the high-salt water, and the sodium hydroxide is recycled to the step S2; the ammonia nitrogen content in the sodium sulfate mother liquor after the sodium sulfate solid is separated out is also low, and the sodium sulfate mother liquor can be conveyed to an evaporation concentration system again for circular treatment; the evaporated condensate water containing ammonia nitrogen can be recycled to step S3 for absorbing ammonia gas.
The ammonium sulfate wastewater can be produced by neutralizing the meta-titanic acid slurry with ammonia water and carrying out wet desulfurization as disclosed in the patent with the publication number of CN 108408770A.
The chlor-alkali process is to prepare sodium hydroxide (NaOH) and chlorine (Cl) by industrial method of electrolysis saturated sodium chloride solution 2 ) And hydrogen (H) 2 ). In the production process of titanium dioxide, a chlor-alkali workshop is not separated for producing sodium hydroxide and chlorine.
The invention firstly carries out membrane treatment concentration on high-concentration ammonium sulfate wastewater generated in the wet desulfurization process of the meta-titanic acid to obtain high-concentration ammonium sulfate concentrated water, then uses sodium hydroxide to adjust pH, and then carries out stripping to separate ammonia in liquid. The concentration of ammonium sulfate in the high-concentration ammonium sulfate wastewater is further improved by adopting membrane treatment, so that on one hand, the reaction efficiency with sodium hydroxide can be improved, the alkali consumption can be saved, on the other hand, the stripping efficiency can be improved, the energy consumption can be reduced, and the ammonia gas with higher concentration can be obtained. The ammonia gas after stripping and separation is absorbed by water or ammonia water and then recycled to the wet desulfurization process of the meta-titanic acid. The solution after stripping still contains ammonia nitrogen with higher concentration, so the invention processes the solution after stripping through an MVR evaporation concentration system, separates and concentrates to obtain sodium sulfate. The obtained sodium sulfate is basically free of ammonia nitrogen and high in purity, and is recycled to the chlor-alkali process to prepare high-salt water, and then sodium hydroxide is prepared from the high-salt water, and the sodium hydroxide can be recycled to the step S2. And step S2, adjusting the pH value by adopting sodium hydroxide, wherein compared with the prior art, more calcium hydroxide is used, the generated calcium sulfate has lower solubility, the generated calcium sulfate precipitation needs to be separated from the solution, and the solution cannot be recycled to the chlor-alkali process to prepare high-salt water.
Compared with the prior art which only adopts the stripping method, the method adopts the membrane treatment before stripping, so that the concentration of ammonium sulfate is concentrated, the ammonia gas with high concentration can be quickly and efficiently separated after the subsequent stripping, the ammonia nitrogen removal rate is improved, the ammonia nitrogen content in the liquid after stripping is lower, and the ammonia nitrogen in the sodium sulfate solution is separated after the stripping by adopting the MVR treatment, so that the later stripping time can be reduced (the stripping efficiency is lower and lower along with the reduction of the ammonia nitrogen concentration). And if only adopt MVR evaporation concentration system, be less than the stripping to high concentration ammonia nitrogen desorption efficiency, consequently with membrane treatment, stripping and MVR evaporation concentration system joint use, can synthesize the stripping to high concentration ammonia nitrogen desorption efficiency higher, and MVR processing system energy consumption lower advantage, and can solve prior art and only adopt membrane treatment, have the requirement to the ammonia nitrogen upper limit of intaking, the treatment concentration is limited, the not high problem of yield.
From the analysis, the high-concentration ammonium sulfate wastewater generated in the production process of the meta-titanic acid is comprehensively utilized by technologies such as sodium hydroxide, a stripping method, membrane treatment, MVR evaporation concentration and the like in the conventional production of the chlor-alkali by the titanium white, the advantages of the conventional stripping method, membrane treatment and MVR evaporation concentration are achieved, the ammonium sulfate is efficiently and rapidly decomposed into recyclable sodium sulfate and ammonia water, the whole treatment process realizes closed loop, no external treatment agent is used, no waste is discharged, and the method has good economic and environmental benefits.
Preferably, the ammonia nitrogen content in the ammonium sulfate concentrated water after the membrane treatment in the step S1 is 7000-12000 mg/L. At the concentration, the method is favorable for rapidly and efficiently separating ammonia by a stripping method.
Preferably, the concentration of sodium hydroxide adopted in the step S2 is 20-50% (mass fraction omega). The concentration of sodium hydroxide generated by the chlor-alkali process is about 30-50%, and the sodium hydroxide can be directly used.
Preferably, the air is adopted for blowing off in the step S3, so that energy consumption can be saved compared with steam.
Preferably, the ammonia removal rate of the solution after the stripping treatment in the step S3 is 50-90%, the stripping time is short, the efficiency is high, the ammonia nitrogen content of the solution after the stripping is proper, and the efficiency of the subsequent MVR treatment can be improved.
Preferably, step S1 is a reverse osmosis membrane treatment. Reverse osmosis is a process of separating solvent from solution by using pressure difference as driving force, and has low energy consumption, no pollution, simple use and wide application; the reverse osmosis membrane can be a polyamide composite reverse osmosis membrane, a cellulose acetate membrane and the like, and the aperture is 0.5-10 nm.
Example 1
S1: according to the method mentioned in the patent with publication number CN108408770A, wet desulfurization is carried out on the meta-titanic acid slurry, and the concentration of ammonium sulfate in the obtained ammonium sulfate wastewater is 9.26g/L, and the ammonia nitrogen content is 2500mg/L; then carrying out reverse osmosis membrane treatment on the ammonium sulfate wastewater to obtain ammonium sulfate concentrated water, wherein the concentration of ammonium sulfate in the ammonium sulfate concentrated water is increased to 25.9g/L after the reverse osmosis membrane treatment, and the ammonia nitrogen content is 7000mg/L;
s2: reacting concentrated ammonium sulfate water with 30% NaOH solution produced by chlor-alkali process until pH is 10.8;
s3: air is adopted for stripping, the stripping time is 3h, the gas-liquid ratio is 2100, ammonia gas is separated from liquid, the ammonia nitrogen content in the solution obtained after the ammonia gas is separated is 1050mg/L, the ammonia nitrogen removal rate is 85%, ammonia water is obtained after the separated ammonia gas is absorbed by water, and the ammonia water enters a storage tank and is used in wet desulfurization in the step S1 of meta-titanic acid desulfurization;
s4: carrying out MVR evaporation concentration system treatment on the liquid subjected to stripping treatment, and further evaporating residual ammonia nitrogen after stripping into an evaporation condensate water system; separating out sodium sulfate, and centrifuging to obtain sodium sulfate solid and sodium sulfate mother liquor;
s5: step S4, sodium sulfate solid obtained after being processed by an MVR evaporation concentration system enters a chlor-alkali process, high-salt water is prepared according to the method mentioned in the publication No. CN108675499A, the high-salt water is further reacted to obtain sodium hydroxide, and the sodium hydroxide is returned to the step S2 to react with ammonium sulfate concentrated water; and the sodium sulfate mother liquor is conveyed to an MVR evaporation concentration system again for cyclic treatment.
Example 2
S1: according to the method mentioned in the patent with publication number CN108408770A, wet desulfurization is carried out on the meta-titanic acid slurry, and the concentration of ammonium sulfate in the obtained ammonium sulfate wastewater is 7.4g/L, and the ammonia nitrogen content is 2000mg/L; then carrying out reverse osmosis membrane treatment on the ammonium sulfate wastewater, concentrating to obtain ammonium sulfate concentrated water, and after membrane treatment, increasing the ammonium sulfate concentration in the ammonium sulfate concentrated water to 33.3g/L and the ammonia nitrogen content to 9000mg/L;
s2: reacting concentrated ammonium sulfate water with 32% NaOH solution produced by chlor-alkali process until pH is 11.4;
s3: air is adopted for stripping, the stripping time is 3h, the gas-liquid ratio is 2100, ammonia gas is separated from liquid, the ammonia nitrogen content in the solution obtained after the ammonia gas is separated is 980mg/L, the ammonia nitrogen removal rate is 89%, ammonia water is obtained after the separated ammonia gas is absorbed by water, and the ammonia water enters a storage tank and is used in wet desulfurization in the step S1 of meta-titanic acid desulfurization;
s4: carrying out MVR evaporation concentration system treatment on the liquid subjected to stripping treatment, and further evaporating residual ammonia nitrogen into an evaporation condensate water system; separating out sodium sulfate, and centrifuging to obtain sodium sulfate solid and sodium sulfate mother liquor;
s5: step S4, sodium sulfate solid obtained after being processed by an MVR evaporation concentration system enters a chlor-alkali process, high-salt water is prepared according to the method mentioned in the publication No. CN108675499A, the high-salt water is further reacted to obtain sodium hydroxide, and the sodium hydroxide is returned to the step S2 to react with ammonium sulfate concentrated water; and the sodium sulfate mother liquor is conveyed to an MVR evaporation concentration system again for cyclic treatment.
Comparative example 1
S1: according to the method mentioned in the patent with publication number CN108408770A, wet desulfurization is carried out on the meta-titanic acid slurry, and the concentration of ammonium sulfate in the obtained ammonium sulfate wastewater is 11.1g/L, and the ammonia nitrogen content is 3000mg/L;
s2: adjusting the pH of the ammonium sulfate solution to 10.8 by using a 30% NaOH solution;
s3: air is adopted for stripping, the stripping time is 12h, the gas-liquid ratio is 2300, ammonia gas is separated from liquid, and the ammonia gas is separated to obtain a solution with the ammonia nitrogen content of 1500mg/L and the ammonia nitrogen removal rate of 50% after testing;
s4: and (3) the sodium sulfate liquid obtained after the stripping in the step (S3) cannot be directly applied to a chlor-alkali process because of higher ammonia nitrogen content in the solution, and deamination treatment is needed to be carried out on the water sample again.
While preferred embodiments of the present invention have been described, additional variations and modifications in those embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. It is therefore intended that the following claims be interpreted as including the preferred embodiments and all such alterations and modifications as fall within the scope of the invention. It will be apparent to those skilled in the art that various modifications and variations can be made to the present invention without departing from the spirit or scope of the invention. Thus, it is intended that the present invention also include such modifications and alterations insofar as they come within the scope of the appended claims or the equivalents thereof.
Claims (1)
1. The method for recycling the ammonium sulfate wastewater is characterized in that the ammonium sulfate wastewater is ammonium sulfate wastewater generated in a wet desulfurization process by neutralizing meta-titanic acid with ammonia water, and the method comprises the following steps of:
s1: firstly, treating ammonium sulfate wastewater by a reverse osmosis membrane, and concentrating to obtain ammonium sulfate concentrated water; the ammonia nitrogen content in the ammonium sulfate concentrated water after membrane treatment is 7000-12000 mg/L;
s2: taking the ammonium sulfate concentrated water obtained in the step S1, and reacting with 20-50% sodium hydroxide by mass fraction until the pH value is 10-12, so as to generate ammonia gas;
s3: separating ammonia from liquid by adopting an air stripping method, absorbing the obtained ammonia with water or ammonia water, recycling the ammonia to the neutralization of the meta-titanic acid and the ammonia water, and carrying out wet desulfurization; blowing off the treated solution, wherein the ammonia gas removal rate is 50-90%;
s4: treating the solution subjected to the stripping treatment in the step S3 through an MVR evaporation concentration system, and separating and concentrating to obtain sodium sulfate solid, mother liquor containing sodium sulfate and evaporation condensate water containing ammonia nitrogen;
s5: preparing high-salt water from the sodium sulfate solid treated by the evaporation and concentration system in the step S4 MVR, and further preparing sodium hydroxide from the high-salt water, and recycling the sodium hydroxide to the step S2; the mother liquor containing sodium sulfate is circularly conveyed to the step S4 for treatment; and recycling the evaporation condensate water containing ammonia nitrogen to the step S3 for absorbing ammonia gas.
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