CN107601718B - Method for removing organic antimony in industrial wastewater of typical industry - Google Patents
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Abstract
The invention relates to a method for removing organic antimony in industrial wastewater, in particular to a method for treating organic antimony in industrial wastewater with high temperature and high pH value. The treatment method fully utilizes the high waste heat and OH of the wastewater through the operation flows of organic antimony dissociation-precipitation and organic antimony oxidation-precipitation‑The characteristic of high concentration realizes the high-efficiency removal of organic antimony in water and reduces the treatment cost, and the organic antimony, inorganic antimony and COD in the water are treated by the methodCrThe method has the advantages of good removal effect on various pollutants, good application feasibility on the industrial wastewater with complex pollutants, simple treatment process, no need of adding treatment structures and easy popularization and application.
Description
Technical Field
The invention relates to a wastewater treatment process, in particular to a method for removing harmful metal pollutants in wastewater, which is particularly applied to the technical field of industrial wastewater treatment generated by production enterprises such as dyes, plastics, adhesives and the like.
Background
Antimony (Antimony, Sb) has an atomic number of 51, an atomic weight of 121.75, and valence states of-3, +3, +4 and +5, and is mainly present in natural Antimony-containing minerals, such as stibnite (Sb)2S3) Antimony white ore (Sb)2O3) And the like. These minerals are mainly associated with copper, silver and lead ores. Many industrial products contain antimony, including batteries, man-made alloys, tracking missiles, textile thermal protection and barrier agents, plastics, adhesives, paint pigments, catalysts and the like, and related antimony-related industries can become a source of antimony pollution in the environment. Environmental sources of antimony include mainly: (1) artificial pollution mainly comes from antimony-containing domestic garbage, mining dust, waste water, waste residues, gasoline combustion, coal combustion and the like; (2) natural pollution, which is mainly caused by geological conditions such as hot springs, geothermy and the like in antimony mine areas, causes higher antimony content in the surrounding environment.
Antimony and its compounds can bind with sulfhydryl in human body, interfere enzyme activity in vivo or destroy ion balance in cell to make cell lack of oxygen to cause metabolism disorder in human body. The continuous contact of the human body with high concentration of antimony can cause irritation to the skin and mucous membranes; improper antimony intake can cause disorder of stomach and intestine and emesis; side effects of antimony as a pharmaceutical agent include metabolic disorders and degeneration of the liver and heart. Antimony poisoning events have been reported in recent years by exposure of the human body to industrial waste dust, contaminated rain or ingestion of excess antimony-containing drugs. The maximum allowable concentration levels of antimony in drinking water in the European Union, the United states and Japan are 10, 6 and 2. mu.g/L, respectively. The limited concentration of antimony is also set as 5 mug/L in the surface water environmental quality standard and the sanitary standard of drinking water in China.
Antimony is present in aqueous solution predominantly in the trivalent and pentavalent forms. Wherein the antimony trioxide is neutral molecules (Sb (OH)) in the pH range of 2.0-10.03SbO (OH) and HSbO2) The form exists; in the presence of SbO under strong acidic condition+Or Sb (OH)2 +The form exists; in the presence of SbO under strong alkaline condition2 -Or Sb (OH)4The form exists. Pentavalent antimony in the weak, neutral and basic range as Sb (OH)6 -Or SbO3 -Exists in the form of (1); in the form of SbO under strongly acidic conditions2 +. In addition, some industries also produce organic antimony such as antimony acetate, ethylene glycol antimony and the like and place the antimony in the environment. In addition to antimony which hydrolyzes in water to form hydroxyl complexes, it can also form complexes with a number of other ligands, such as citric acid, tartaric acid, and the like. Antimony can also form less stable complexes with EDTA, which are susceptible to decomposition in the presence of tartaric acid or hydrofluoric acid (HF).
The removal technology of common inorganic trivalent antimony and pentavalent antimony in natural water is researched more at home and abroad and mainly comprises adsorption, precipitation, oxidation reduction, ion exchange and the like. The different methods each have advantages and disadvantages, and have suitable optimum concentration ranges. In contrast, antimony-containing industrial wastewater produced in industrial wastewater often has a high organic antimony proportion, and some wastewater is even up to more than 85%. The organic antimony has more complex molecular structure and form, different molecular electrical characteristics and is more difficult to remove by a single or certain fixed combined processes. Because the discharge standard of the industrial wastewater is calculated by total antimony, the strengthened removal of the organic antimony becomes a precondition and a key for realizing the standard reaching of the antimony of the industrial wastewater. In addition, in some industrial wastewater generation processes, operations such as heating are often required, so that the temperature of the generated wastewater is high, and if the residual heat in water can be fully utilized for reaction, the antimony removal effect is expected to be improved, and the operation cost is expected to be reduced. Aiming at the requirements, the invention provides a method for removing organic antimony in an enhanced manner by combining the characteristics of generation, treatment and discharge of certain industrial wastewater, and has good application value.
Disclosure of Invention
The invention aims to provide a method for effectively removing organic antimony in industrial wastewater by utilizing the characteristics of high temperature and high pH value of the industrial wastewater.
The technical principle of the method for removing the organic antimony in the industrial wastewater provided by the invention is as follows: under the condition of high pH value, the organic antimony generated by antimony and the complex is subjected to ligand dissociation and release and is converted into inorganic antimony; inorganic antimony is further hydrolyzed under alkaline conditions to form hydroxyl complexes, so that precipitates are formed and separated out. In addition, some organic antimony such as ethylene glycol antimony is still very stable under strong alkaline conditions and is difficult to precipitate. Aiming at the situation, high-concentration OH is utilized under the strong alkaline condition-And the persulfate can be activated under the high-temperature condition to generate sulfate free radicals with extremely strong oxidizing capability, the organic antimony in the stable state is oxidized into inorganic antimony, and the generated inorganic antimony can be rapidly precipitated and separated out under the alkaline pH value condition. If the temperature is lower, the persulfate activator can be used for strengthening the generation of sulfate free radicals, and the removal of organic antimony can also be realized.
In order to realize the aim, the invention realizes the treatment of the antimony-containing industrial wastewater by the following technical scheme:
i. adjusting the pH value of the antimony-containing wastewater to be more than 12 by using alkali liquor, stirring and reacting for 10-60min, and removing suspended matters in water by adopting a solid-liquid separation method;
ii, measuring the water temperature T of the antimony-containing wastewater, adding persulfate when the temperature T is higher than 45 ℃, and stirring for reaction for 10-60 min; when the T is less than or equal to 45 ℃, adding persulfate and persulfate activator, and reacting for 20-120 min; removing suspended matters in water by a solid-liquid separation method;
wherein the molar equivalent of the persulfate is determined by calculation as follows:
m persulfate ═ 1.2 x [ Mtot-Sb+(CODCr-BOD5)/16]/[(T-45)/(T+45)]
Mtot-SbIs the molar equivalent of the total antimony in the antimony-containing wastewater;
adding a mixed solution of calcium salt, magnesium salt, ferric salt, ferrous salt and aluminum salt, reacting for 5-15min, and adding acid liquor in the reaction process to enable the reaction equilibrium pH value range to be 6-9; and removing suspended matters in water by adopting a solid-liquid separation method.
Wherein the persulfate is selected from one or more of sodium persulfate, potassium persulfate, ammonium persulfate and potassium hydrogen persulfate;
wherein the persulfate activator is a mixed solution of Mn (II), Fe (II), Cu (II) and Co (II), and the molar ratio of any two of the elements of Fe, Mn, Co and Cu is in the range of 3: 1-1: 3; and the range of the ratio of the sum of the molar concentrations of the iron, manganese, cobalt and copper elements in the persulfate activator to the molar concentration of the persulfate is 1: 50-1: 5.
wherein the alkali liquor is selected from one or more of calcium hydroxide, sodium hydroxide, calcium oxide and potassium hydroxide;
wherein the acid solution is selected from one or more of sulfuric acid, hydrochloric acid and nitric acid;
wherein the calcium salt is selected from one or more of calcium chloride, calcium sulfate and calcium nitrate;
wherein the magnesium salt is selected from one or more of magnesium chloride, magnesium sulfate and magnesium nitrate;
wherein, the ferric salt can be one or more selected from ferric chloride, ferric sulfate, ferric nitrate, polymeric ferric chloride, polymeric ferric sulfate, polymeric ferric nitrate and the like;
wherein the aluminum salt solution is selected from one or more of aluminum sulfate solution, aluminum chloride solution, polyaluminum sulfate solution, polyaluminum chloride solution, aluminum nitrate solution, polyaluminum nitrate solution, alum solution and the like;
wherein, the ferrous salt solution comprises one or more of ferrous chloride, ferrous sulfate, ferrous nitrate and other solutions;
wherein, the solid-liquid separation method can be one or more of concentration, precipitation and filtration.
The method for treating organic antimony in industrial wastewater has the following advantages:
1. the characteristics of wastewater in certain industries are comprehensively considered, the characteristics of high temperature, high pH value and the like of the wastewater are fully utilized and exerted, the effect can be obviously improved, and the cost can be greatly reduced;
2. can be flexibly designed according to the characteristics of the water quality, the water quantity, the coexisting pollutants and the like of the industrial wastewater to meet the requirements of different types of water quality, and has broad-spectrum adaptability;
3. the treatment process is simple, no treatment structure is required to be added, and the method is easy to popularize and apply;
4. for organic antimony, inorganic antimony and COD in waterCrAnd various pollutants have good removal effect, and the method has good application feasibility for industrial wastewater with complex pollutants.
Detailed Description
The technical solutions of the present invention will be described in detail with reference to specific examples, which should be understood as merely illustrative and not restrictive, and various equivalent modifications of the present invention, which fall within the scope of the appended claims, will be suggested to those skilled in the art after reading the present invention.
The antimony solution (i.e., the specifically treated simulated wastewater) used in the examples of the present invention was obtained by diluting with 1000. mu.g/mL of an antimony standard solution as a mother liquor, and the antimony content: 1.0mg/L, pH 10, wastewater temperature 50 ℃.
Example 1: the method comprises the following specific steps of removing organic antimony in industrial wastewater under a high-temperature condition (T >45 ℃):
i. adjusting the pH value of the antimony-containing wastewater to be more than 12.5 by using alkali liquor, stirring and reacting for 10min, and removing suspended matters in water by adopting a solid-liquid separation method;
ii, measuring the water temperature T of the antimony-containing wastewater, and when T is reached>And at 50 ℃, persulfate is added. Wherein, the persulfate dosage MPersulfate-1Calculated using the following formula.
MPersulfates＝1.2*[Mtot-Sb+(CODCr-BOD5)/16]/[(T-45)/(T+45)]
Adding persulfate into water, and fully stirring for reaction for 10 min; removing suspended matters in water by a solid-liquid separation method;
adding a mixed solution of calcium salt, magnesium salt, ferrous salt and aluminum salt, reacting for 5min, and adding acid liquor in the reaction process to ensure that the reaction equilibrium pH value range is 6; and removing suspended matters in water by adopting a solid-liquid separation method.
And measuring the content of antimony in the supernatant, wherein the removal rate of antimony can reach more than 80%, and the content of antimony after treatment is less than 200 mug/L.
Example 2: the method comprises the following specific steps of removing organic antimony in industrial wastewater under a high-temperature condition (T >45 ℃):
i. adjusting the pH value of the antimony-containing wastewater to be more than 12.0 by using alkali liquor, stirring and reacting for 60min, and removing suspended matters in water by adopting a solid-liquid separation method;
ii, measuring the water temperature T of the antimony-containing wastewater, and when T is reached>Persulfate is added at the temperature of 45 ℃. Wherein, the persulfate dosage MPersulfate-1Calculated using the following formula.
MPersulfates＝1.2*[Mtot-Sb+(CODCr-BOD5)/16]/[(T-45)/(T+45)]
Adding persulfate into water, and fully stirring for reaction for 60 min; removing suspended matters in water by a solid-liquid separation method;
adding a mixed solution of ferrous salt and aluminum salt, reacting for 15min, and adding acid liquor in the reaction process to enable the reaction balance pH value range to be 9; and removing suspended matters in water by adopting a solid-liquid separation method.
And (3) measuring the content of antimony in the supernatant, wherein the removal rate of antimony can reach more than 90%, and the content of antimony after treatment is less than 100 mug/L.
Example 3: the method comprises the following specific steps of removing organic antimony in industrial wastewater under a high-temperature condition (T >45 ℃):
i. adjusting the pH value of the antimony-containing wastewater to be more than 12.0 by using alkali liquor, stirring for reacting for 30min, and removing suspended matters in water by adopting a solid-liquid separation method;
ii, measuring the water temperature T of the antimony-containing wastewater, and when T is reached>Persulfate is added at the temperature of 45 ℃. Wherein, the persulfate dosage MPersulfate-1Calculated using the following formula.
MPersulfates＝1.2*[Mtot-Sb+(CODCr-BOD5)/16]/[(T-45)/(T+45)]
Adding persulfate into water, and fully stirring for reaction for 60 min; removing suspended matters in water by a solid-liquid separation method;
adding a ferrous salt solution, reacting for 10min, and adding an acid solution in the reaction process to enable the reaction balance pH value range to be 8; and removing suspended matters in water by adopting a solid-liquid separation method.
And measuring the content of antimony in the supernatant, wherein the removal rate of antimony can reach more than 70%, and the content of antimony after treatment is less than 300 mug/L.
Example 4: the specific method for removing the organic antimony in the industrial wastewater under the low temperature condition (T is less than or equal to 45 ℃), which comprises the following steps:
i. adjusting the pH value of the antimony-containing wastewater to be more than 12 by using alkali liquor, stirring and reacting for 60min, and removing suspended matters in water by adopting a solid-liquid separation method;
ii, measuring the water temperature T of the antimony-containing wastewater, and when the temperature T is less than or equal to 45 ℃, adding persulfate and a persulfate activator, wherein the adding amount M of the persulfatePersulfate-1Calculated using the following formula.
MPersulfates＝1.2*[Mtot-Sb+(CODCr-BOD5)/16]/[(T-45)/(T+45)]
Adding persulfate into water, and fully stirring for reaction for 120 min; removing suspended matters in water by a solid-liquid separation method;
iii, adding a mixed solution of ferric salt, ferrous salt and aluminum salt, reacting for 15min, and adding acid liquor in the reaction process to ensure that the reaction equilibrium pH value range is 9; and removing suspended matters in water by adopting a solid-liquid separation method.
And (3) measuring the content of antimony in the supernatant, wherein the removal rate of antimony can reach more than 90%, and the content of antimony after treatment is less than 100 mug/L.
Example 5: the specific method for removing the organic antimony in the industrial wastewater under the low temperature condition (T is less than or equal to 45 ℃), which comprises the following steps:
i. adjusting the pH value of the antimony-containing wastewater to be more than 13 by using alkali liquor, stirring and reacting for 20min, and removing suspended matters in water by adopting a solid-liquid separation method;
ii, measuring the water temperature T of the antimony-containing wastewater, and when the temperature T is less than or equal to 45 ℃, adding persulfate and a persulfate activator, wherein the adding amount M of the persulfatePersulfate-1Calculated using the following formula.
MPersulfates＝1.2*[Mtot-Sb+(CODCr-BOD5)/16]/[(T-45)/(T+45)]
Adding persulfate into water, and fully stirring for reaction for 20 min; removing suspended matters in water by a solid-liquid separation method;
adding aluminum salt mixed solution, reacting for 5min, and adding acid liquor in the reaction process to ensure that the reaction equilibrium pH value range is 6; and removing suspended matters in water by adopting a solid-liquid separation method.
And measuring the content of antimony in the supernatant, wherein the removal rate of antimony can reach more than 80%, and the content of antimony after treatment is less than 200 mug/L.
Example 6: the specific method for removing the organic antimony in the industrial wastewater under the low temperature condition (T is less than or equal to 45 ℃), which comprises the following steps:
i. adjusting the pH value of the antimony-containing wastewater to be more than 12 by using alkali liquor, stirring and reacting for 10min, and removing suspended matters in water by adopting a solid-liquid separation method;
ii, measuring the water temperature T of the antimony-containing wastewater, and when the temperature T is less than or equal to 35 ℃, adding persulfate and a persulfate activator, wherein the adding amount M of the persulfatePersulfate-1Calculated using the following formula.
MPersulfates＝1.2*[Mtot-Sb+(CODCr-BOD5)/16]/[(T-45)/(T+45)]
Adding persulfate into water, and fully stirring for reaction for 20 min; removing suspended matters in water by a solid-liquid separation method;
adding a mixed solution of calcium salt and magnesium salt, reacting for 15min, and adding acid liquor in the reaction process to ensure that the reaction equilibrium pH value range is 7; and removing suspended matters in water by adopting a solid-liquid separation method.
And (3) measuring the content of antimony in the supernatant, wherein the removal rate of antimony can reach more than 95%, and the content of antimony after treatment is less than 50 mu g/L.
All of the above mentioned intellectual property rights are not intended to be restrictive to other forms of implementing the new and/or new products. Those skilled in the art will take advantage of this important information, and the foregoing will be modified to achieve similar performance. However, all modifications or alterations are based on the new products of the invention and belong to the reserved rights.
Claims (8)
1. A method for removing organic antimony in industrial wastewater is characterized by comprising the following steps:
i. adjusting the pH value of the antimony-containing wastewater to be more than 12 by using alkali liquor, and stirring and reacting for 10-60 min; removing suspended matters in water by a solid-liquid separation method;
ii, measuring the water temperature T of the antimony-containing wastewater;
when the T is higher than 45 ℃, persulfate is added, and the stirring reaction is carried out for 10-60 min; when the T is less than or equal to 45 ℃, adding persulfate and persulfate activator, and reacting for 20-120 min; removing suspended matters in water by a solid-liquid separation method;
adding a mixed solution of calcium salt, magnesium salt, ferric salt, ferrous salt and aluminum salt, reacting for 5-15min, and adding acid liquor in the reaction process to enable the reaction equilibrium pH value range to be 6-9; removing suspended matters in water by adopting a solid-liquid separation method, wherein the persulfate adding amount is determined by adopting the following method:
m persulfate ═ 1.2 x [ Mtot-Sb+(CODCr-BOD5)/16]/[(T-45)/(T+45)]；
Wherein M persulfate is the molar equivalent of persulfate, Mtot-SbIs the molar equivalent of the total antimony in the antimony-containing wastewater.
2. The method for removing organic antimony in industrial wastewater according to claim 1, characterized in that: wherein the persulfate is selected from one or more of sodium persulfate, potassium persulfate, ammonium persulfate and potassium hydrogen persulfate.
3. The method for removing organic antimony from industrial wastewater according to claim 1 or 2, characterized in that: wherein the persulfate activator is a mixed solution of Mn (II), Fe (II), Cu (II) and Co (II), and the molar ratio of any two of the elements of Fe, Mn, Co and Cu is in the range of 3: 1-1: 3.
4. the method for removing organic antimony from industrial wastewater according to claim 1 or 2, wherein the ratio of the sum of the molar concentrations of iron, manganese, cobalt and copper elements in the persulfate activator to the molar concentration of the persulfate ranges from 1: 50-1: 5.
5. the method for removing organic antimony from industrial wastewater according to claim 1 or 2, characterized in that:
the alkali liquor is selected from one or more of calcium hydroxide, sodium hydroxide, calcium oxide and potassium hydroxide.
6. The method for removing organic antimony from industrial wastewater according to claim 1 or 2, characterized in that: the acid solution is selected from one or more of sulfuric acid, hydrochloric acid and nitric acid; the calcium salt is selected from one or more of calcium chloride, calcium sulfate and calcium nitrate.
7. The method for removing organic antimony from industrial wastewater according to claim 1 or 2, characterized in that: the magnesium salt is selected from one or more of magnesium chloride, magnesium sulfate and magnesium nitrate; the ferric salt can be selected from one or more of ferric chloride, ferric sulfate, ferric nitrate, polymeric ferric chloride, polymeric ferric sulfate and polymeric ferric nitrate.
8. The method for removing organic antimony from industrial wastewater according to claim 1 or 2, characterized in that: the aluminum salt solution is selected from one or more of aluminum sulfate solution, aluminum chloride solution, polyaluminum sulfate solution, polyaluminum chloride solution, aluminum nitrate solution, polyaluminum nitrate solution and alum solution; the ferrous salt solution comprises one or more of ferrous chloride solution, ferrous sulfate solution and ferrous nitrate solution.
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| CN108726799A (en) * | 2018-06-02 | 2018-11-02 | 苏州弘宇水处理工程服务有限公司 | Dyeing waste water efficiently removes antimony technique |
| CN110255696B (en) * | 2019-07-23 | 2022-05-10 | 大连民族大学 | System for utilize surplus alkali waste heat treatment refined cotton black liquid |
| CN112777837B (en) * | 2021-01-05 | 2022-07-05 | 广州大学 | Method for removing aniline, chromium and antimony in wastewater |
| CN114854996A (en) * | 2022-05-07 | 2022-08-05 | 金川集团股份有限公司 | Method for removing antimony by persulfate advanced oxidation method |
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