CN113072155A - Preparation of ionic liquid sustained-release agent and method for purifying arsenic and heavy metal wastewater - Google Patents
Preparation of ionic liquid sustained-release agent and method for purifying arsenic and heavy metal wastewater Download PDFInfo
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- CN113072155A CN113072155A CN202110341292.5A CN202110341292A CN113072155A CN 113072155 A CN113072155 A CN 113072155A CN 202110341292 A CN202110341292 A CN 202110341292A CN 113072155 A CN113072155 A CN 113072155A
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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
- C02F1/52—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
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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
- C02F1/52—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
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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
- C02F2101/103—Arsenic compounds
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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
- C02F2101/20—Heavy metals or heavy metal compounds
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Abstract
The invention discloses a method for purifying waste water containing arsenic and heavy metal by using an ionic liquid slow-release agent, which comprises the steps of introducing hydrogen sulfide gas into an organic alcohol amine aqueous solution for absorbing hydrogen sulfide to obtain the ionic liquid slow-release agent; and heating the ionic liquid slow-release agent to perform a hydrogen sulfide desorption reaction, introducing the desorbed hydrogen sulfide into the acidic wastewater containing arsenic and heavy metal to perform a vulcanization reaction, and obtaining arsenic and heavy metal sulfide precipitate. The method can realize deep purification of heavy metal acidic wastewater and recovery of valuable metals, and avoids H2S pollutes the environment and the danger and instability of the hydrogen sulfide gas in the storage and transportation processes, and the operation process of the method is simpleIs convenient and is beneficial to industrialized application.
Description
Technical Field
The invention relates to a method for treating wastewater containing arsenic and heavy metals, in particular to a method for realizing deep removal and purification of heavy metals and arsenic in industrial acidic waste liquid by absorbing and slowly releasing hydrogen sulfide by using organic alcohol amine, belonging to the technical field of heavy metal wastewater treatment.
Background
In recent years, with the development of economy and the further improvement of the living standard of people, various industrial production activities are also accelerated continuously, and the common industrial production processes mainly comprise mineral smelting and processing, chemical engineering, mechanical manufacturing, pharmaceutical electronics, pigments and the like. In the industrial production process, a large amount of waste water containing heavy metal ions, namely heavy metal waste water, can be discharged. Particularly, a large amount of flue gas is generated in the smelting of nonferrous metals such as copper, lead and zinc, a large amount of strong acid wastewater containing heavy metals is generated in the process, the components of the wastewater are complex, and the wastewater contains harmful metal ions such as arsenic, copper, lead, zinc, cadmium, bismuth and the like, and the wastewater needs to be subjected to advanced treatment and is discharged after reaching the standard.
The currently adopted iron salt neutralization method not only has large slag quantity but also can cause the waste of valuable metal resources, the valuable metals in the wastewater mostly exist in the form of divalent metal ions, and the arsenic is arsenous acid H3AsO3The specific reaction equation of the method can be used for realizing selective precipitation separation of heavy metal and arsenic in wastewater according to different sulfide solubilities by a sulfidation method as follows:
M2++S2-↓ (M refers to metal element)
2H3AsOs+3H2S＝As2S3↓+6H2O
Currently, most of the industry uses vulcanizing agents such as Na2S and NaHS, which are easily to cause a large amount of H when directly used under acidic conditions2S escapes, and the purification efficiency is low due to the excessively high dissolution rate, and the purification is tightThe double image affects the filtration properties of the vulcanized product. Using H2S replaces vulcanizing agents such as sodium sulfide and the like, so that the introduction of sodium ions and other impurity ions can be avoided, and the recycling of waste water and waste acid is facilitated. But H2S is used as a highly toxic gas, the storage and the use of the S need strict supervision and administration, and H is given2The popularization and use of S gas brings great difficulty, and therefore, there is an urgent need to develop a safe and reliable method or technique for utilizing H in the field of wastewater treatment more safely and efficiently2S。
The raw material gas for synthesizing ammonia and the gas generated in natural gas and smelting plant inevitably have some acidic gas, such as H2S、CO2、SO2And the like. In these acid gases H2The harm of S is the most serious, pipelines and equipment are corroded, the environment is polluted, the production of factories and the occupational safety of workers are seriously affected, and if the harmful gas hydrogen sulfide in the industrial waste gas can be fully absorbed and the resource utilization is realized, the method is an ideal way.
Disclosure of Invention
Aiming at the problems of high cost, low efficiency and H existing in the method for recovering or removing heavy metal and arsenic-containing components in the solution in the prior art2The invention aims to provide a method for realizing deep removal and recovery of heavy metals and arsenic-containing components in arsenic-and heavy metal-containing acidic wastewater by using organic alcohol amine as a slow-release donor for adsorbing, storing and slowly releasing hydrogen sulfide, wherein the method can realize purification of H in the environment by using the organic alcohol amine2S, can slowly release H2S, thereby selectively recovering valuable metals from industrial waste liquid with high efficiency and low cost and deeply removing arsenic, and slowly releasing H through the ionic liquid slow-release agent2S is beneficial to the selective separation of metal ions and arsenic, simultaneously avoids the generation of amorphous products due to the excessively high crystallization speed of the products, and enhances the filtering performance of the products. Compared with the existing vulcanizing agent, the ionic liquid slow-release agent can be repeatedly utilized, is safe and reliable, is convenient to store and transport, can avoid the introduction of sodium ions and other impurity ions in the using process, and is beneficial to the recycling of waste water and waste acid.
In order to realize the technical purpose, the invention provides a method for purifying acidic wastewater containing arsenic and heavy metal by using an ionic liquid slow-release agent, which comprises the steps of introducing hydrogen sulfide gas into an organic alcohol amine aqueous solution for a reaction of absorbing hydrogen sulfide to obtain the ionic liquid slow-release agent; and heating the ionic liquid slow-release agent to perform a hydrogen sulfide desorption reaction, introducing the desorbed hydrogen sulfide into the acidic wastewater containing arsenic and heavy metal to perform a vulcanization reaction, and obtaining arsenic and heavy metal sulfide precipitate.
According to the technical scheme, the organic alcohol amine is used as a slow release donor for hydrogen sulfide adsorption storage and slow release, so that gaseous hydrogen sulfide can be converted into stable liquid hydrogen sulfide, the storage and the transportation are convenient, the slow and stable release of hydrogen sulfide gas can be controlled in the process of treating the acid wastewater containing arsenic and heavy metals, the deep vulcanization precipitation of the arsenic and the heavy metals in the acid wastewater containing arsenic and heavy metals is realized, the arsenic and the heavy metals are converted into metal sulfides with high crystallinity, and the separation and the recovery are facilitated.
In a preferred embodiment, the organic alcohol amine is at least one of N-methyldiethanolamine, triethanolamine, diethanolamine and diisopropanolamine. The preferred organic alcohol amines are effective in binding hydrogen sulfide gas and converting to compounds that are stable at room temperature.
As a preferred scheme, the reaction conditions for absorbing hydrogen sulfide are as follows: and (3) reacting in an autoclave at the temperature of 20-40 ℃ and under the pressure of 4-5 MPa for more than 30 min. The hydrogen sulfide can be efficiently combined under the preferable reaction condition, but the hydrogen sulfide is combined with the hydrogen sulfide less efficiently and the utilization rate of the organic alcohol amine is low under the preferable reaction condition.
Preferably, the mass percentage concentration of the organic alcohol amine aqueous solution is 30-40%.
As a preferred scheme, the reaction conditions for desorbing hydrogen sulfide are as follows: the temperature is controlled within the range of 110-120 ℃. The temperature is the key to controlling the release of hydrogen sulfide gas, and the slow and stable release of hydrogen sulfide can be controlled under the optimized reaction conditions.
As a preferred embodiment, the conditions of the sulfurization reaction are: the temperature is 50-60 ℃, and the stirring speed is 300-500 r/min.
As a preferable scheme, heavy metal sulfide and arsenic sulfide are sequentially recovered in the sulfurization reaction process by controlling the oxidation-reduction potential to be reduced from high. And the final point of the vulcanization reaction is based on the oxidation-reduction potential of the solution, namely the removal of the valuable metals and arsenic which are selectively recovered is realized according to the final oxidation-reduction potential of the solution, the desorbed organic amine solution can be returned for cyclic utilization after being cooled, and the ionic liquid slow-release agent is continuously prepared.
As a preferable scheme, the organic alcohol amine regenerated after desorbing the hydrogen sulfide is recycled and returned to the reaction process of absorbing the hydrogen sulfide.
The hydrogen sulfide gas related to the invention can be derived from waste gas containing hydrogen sulfide, or can be prepared by reacting metal sulfide with acid. Specifically, the sodium sulfide is obtained by dripping sodium sulfide with the concentration of 1-1.5 mol/L into a dilute hydrochloric acid solution with the concentration of 30-40 wt% at the speed of 20-50 mL/min, and stirring and reacting under the condition that the stirring speed is 300-500 r/min.
The ionic liquid slow-release agent can change the state of hydrogen sulfide from a gaseous state to a liquid state, is convenient to store and transport, and can realize desorption of hydrogen sulfide and slowly release H again by controlling the temperature condition when needed2S。
The source of the acidic waste liquid containing arsenic and heavy metal is that a large amount of waste water containing heavy metal ions and arsenic is discharged in the production processes of mineral smelting processing, chemical engineering, mechanical manufacturing, pharmaceutical electronics and pigment industry.
Compared with the prior art, the technical scheme of the invention has the beneficial technical effects that:
1) the technical scheme provided by the invention utilizes the organic alcohol amine as a slow release donor for storing and slowly releasing the hydrogen sulfide, not only can efficiently combine the hydrogen sulfide, but also has the function of slowly releasing H2Characteristic of S, H2The S has high utilization rate, can be repeatedly utilized, can greatly reduce the use cost of the vulcanizing agent, and reduces the harm to the environment; solves the problem of the sulfur of the traditional vulcanizing agents such as sodium sulfide and the likeLarge consumption of the sulfurating agent in the process of removing impurities, low utilization rate and easy escape of H2S harms the environment and the like, can also avoid the introduction of sodium ions and other impurity ions, and is beneficial to the recycling of waste water and waste acid.
2) The ionic liquid sustained-release agent has the advantages of simple preparation method, wide raw material source, safety, reliability, convenience for transportation and storage and contribution to industrial production.
3) The technical scheme provided by the invention utilizes the ionic liquid slow-release agent to treat the acidic wastewater containing arsenic and heavy metal, can realize the selective recovery of valuable metal elements and the proper treatment of arsenic, has less impurity inclusion in a vulcanized product, can avoid the generation of an amorphous product due to the over-high crystallization speed of the product, improves the filtering performance of the product, and is beneficial to the separation and recovery of metal sulfide and arsenic sulfide.
Drawings
FIG. 1 is a flow chart of slow-release vulcanization purification of industrial waste liquid.
Detailed Description
The following examples are intended to further illustrate the present disclosure, but not to limit the scope of the claims.
Example 1
The method for treating the copper smelting waste acid water comprises the following specific steps of taking a certain amount of waste acid water (H)2SO48% in content, 0.5g/L in copper content and 2g/L in arsenic content), dropping 1.2mol/L sodium sulfate solution into prepared 35% dilute hydrochloric acid at 10mL/min to prepare hydrogen sulfide, introducing 35% N-methyldiethanolamine solution to synthesize ionic liquid slow release agent, wherein the synthesis conditions are as follows: the synthesis pressure is 4MPa, the temperature is 25 ℃, and the synthesis time is 45 min; controlling the temperature of a desorption oil bath at 110 ℃, slowly introducing desorption gas into waste acid for a vulcanization reaction at 60 ℃, controlling the stirring speed at 300r/min, simultaneously monitoring the potential of reaction change by using an oxidation-reduction potentiometer, when the oxidation-reduction potential is reduced from initial 450mV to 252mV, which means that copper ions are basically removed, taking out reaction liquid for filtration to obtain first-stage copper-removed slag, continuously returning the filtrate to the reaction, stopping the reaction when the oxidation-reduction potential is reduced to 93mV, taking out the filtrate for filtration to obtain second-stage arsenic-removed slag and clean and pureAnd (4) forming the solution. The first-stage slag contains valuable metals and can be recycled, the second-stage high-arsenic slag can be properly cured, and the purifying liquid can be recycled or the waste acid can be recycled.
Through analysis, the copper content in the first-stage copper-removed slag is 41.32 percent, and the arsenic content is 3.46 percent; the arsenic content of the second-stage arsenic removal slag is 24.33 percent; the copper content in the purification liquid is 4.3mg/L, and the removal rate exceeds 99 percent; the arsenic content is 9.8mg/L, the removal rate exceeds 99 percent, and the purification effect is ideal.
Example 2
The method for treating the copper smelting ash leachate comprises the following specific steps of taking a certain amount of leachate (H)2SO4The content is 7%, the copper content is 20g/L, the arsenic content is 8g/L), dilute hydrochloric acid with the concentration of 40% is prepared, 1.2mol/L sodium sulfate solution is dripped into the dilute hydrochloric acid with the concentration of 10mL/min to prepare hydrogen sulfide, 40% N-methyldiethanolamine solution is introduced to synthesize the ionic liquid sustained-release agent, and the synthesis conditions are as follows: the synthesis pressure is 3MPa, the temperature is 25 ℃, and the synthesis time is 60 min; controlling the temperature of a desorption oil bath at 120 ℃, introducing desorption gas into contaminated acid to perform a vulcanization reaction, controlling the reaction temperature at 40 ℃, controlling the stirring speed at 300r/min, simultaneously monitoring the potential of reaction change by using an oxidation-reduction potentiometer, when the oxidation-reduction potential is reduced from 447mV to 262mV, which means that copper ions are basically removed, taking out reaction liquid to perform filtration to obtain first-stage copper-removed slag, continuously returning the filtrate to the reaction, stopping the reaction when the oxidation-reduction potential is reduced to 82mV, taking out the filtration to obtain second-stage arsenic-removed slag and a purified solution. The first-stage slag contains valuable metals and can be recycled, the second-stage high-arsenic slag can be properly cured, and the purifying liquid can be recycled or the waste acid can be recycled.
Through analysis, the copper content in the first-stage copper-removed slag is 38.53 percent, and the arsenic content is 3.02 percent; the arsenic content of the second-stage arsenic removal slag is 33.58%; the copper content in the purification liquid is 5mg/L, and the removal rate exceeds 99 percent; the arsenic content is 2.8mg/L, the removal rate exceeds 99 percent, and the purification effect is ideal.
Comparative example 1
The process method for treating the waste acid wastewater from zinc smelting comprises the following specific steps of taking a certain amount of waste acid wastewater (H)2SO43% of copper content 5mg/L, arsenicContent of 0.5g/L), preparing dilute hydrochloric acid with concentration of 35%, dripping 1.2mol/L sodium sulfate solution into the dilute hydrochloric acid with concentration of 15mL/min to prepare hydrogen sulfide, introducing 30% diisopropanolamine solution to synthesize the ionic liquid slow-release agent, wherein the synthesis conditions are as follows: the synthesis pressure is 2MPa, the temperature is 40 ℃, and the synthesis time is 30 min; controlling the temperature of a desorption oil bath at 95 ℃, introducing desorption gas into contaminated acid to perform a vulcanization reaction, controlling the reaction temperature at 60 ℃, controlling the stirring speed at 300r/min, simultaneously monitoring the potential of reaction change by using an oxidation-reduction potentiometer, directly removing arsenic by adopting a one-step method in a vulcanization manner in view of less copper content, taking out a reaction liquid to filter when the oxidation-reduction potential is reduced from initial 234mV to 185mV, and respectively analyzing and testing obtained filtrate and filter residue.
After analysis, the arsenic content in the arsenic-removed slag is 14.43 percent; the copper content in the purifying liquid is less than 0.1 mg/L; the arsenic content is 306mg/L, the removal rate is only 39.04 percent, and the purification effect is poor.
Comparative example 2
The process method for treating the waste acid wastewater from lead smelting comprises the following specific steps of taking a certain amount of waste acid wastewater (H)2SO4The content is 2%, the copper content is 0.01mg/L, the arsenic content is 460.6mg/L), dilute hydrochloric acid with the concentration of 35% is prepared, 1.2mol/L sodium sulfate solution is dripped into 15mL/min to prepare hydrogen sulfide, 30% of mixed solution of diethylenetriamine and diethanol amine is introduced to synthesize the ionic liquid sustained-release agent, and the synthesis conditions are as follows: the synthesis pressure is normal pressure, the temperature is 80 ℃, and the synthesis time is 30 min; the temperature of the desorption oil bath is controlled at 100 ℃, desorption gas is introduced into waste acid for a vulcanization reaction, the reaction temperature is 30 ℃, the stirring speed is 300r/min, an oxidation-reduction potentiometer is used for monitoring the potential of reaction change, in view of less copper content, arsenic is removed by direct one-step vulcanization, the oxidation-reduction potential is reduced from initial 234mV to 165mV without changing, at the moment, reaction liquid is taken out for filtration, and the obtained filtrate and filter residue are respectively analyzed and tested.
After analysis, the arsenic content in the arsenic-removed slag is 16.43 percent; the copper content in the purifying liquid is less than 0.1 mg/L; the arsenic content is 237.5mg/L, the removal rate is 48.4 percent, and the purification effect is poor.
While the present invention has been described in detail with reference to the embodiments shown in the drawings, the present invention is not limited to the embodiments, and various changes can be made without departing from the spirit and scope of the present invention.
Claims (8)
1. A method for purifying wastewater containing arsenic and heavy metal by using ionic liquid slow-release liquid is characterized by comprising the following steps: introducing hydrogen sulfide gas into an organic alcohol amine aqueous solution to perform a reaction of absorbing hydrogen sulfide to obtain an ionic liquid slow release agent; and heating the ionic liquid slow-release agent to perform a hydrogen sulfide desorption reaction, introducing the desorbed hydrogen sulfide into the acidic wastewater containing arsenic and heavy metal to perform a vulcanization reaction, and obtaining arsenic and heavy metal sulfide precipitate.
2. The method for purifying the wastewater containing arsenic and heavy metal by using the ionic liquid slow-release solution as claimed in claim 1, wherein the method comprises the following steps: the organic alcohol amine is at least one of N-methyldiethanolamine, triethanolamine, diethanolamine and diisopropanolamine.
3. The method for purifying the wastewater containing arsenic and heavy metals by using the ionic liquid slow-release solution according to any one of claims 1 to 2, which is characterized in that: the reaction conditions for absorbing hydrogen sulfide are as follows: and (3) reacting in an autoclave at the temperature of 20-40 ℃ and under the pressure of 4-5 MPa for more than 30 min.
4. The method for purifying the wastewater containing arsenic and heavy metal by using the ionic liquid slow-release solution as claimed in claim 1, wherein the method comprises the following steps: the mass percentage concentration of the organic alcohol amine aqueous solution is 30-40%.
5. The method for purifying the wastewater containing arsenic and heavy metal by using the ionic liquid slow-release solution as claimed in claim 1, wherein the method comprises the following steps: the reaction conditions for desorbing the hydrogen sulfide are as follows: the temperature is controlled within the range of 110-120 ℃.
6. The method for purifying the wastewater containing arsenic and heavy metal by using the ionic liquid slow-release solution as claimed in claim 1, wherein the method comprises the following steps: the conditions of the sulfurization reaction are as follows: the temperature is 50-60 ℃, and the stirring speed is 300-500 r/min.
7. The method for purifying the wastewater containing arsenic and heavy metal by using the ionic liquid slow-release solution as claimed in claim 6, wherein the ionic liquid slow-release solution comprises the following steps: in the vulcanization reaction process, heavy metal sulfide and arsenic sulfide are sequentially recovered by controlling the oxidation-reduction potential from high to low.
8. The method for purifying the wastewater containing arsenic and heavy metal by using the ionic liquid slow-release solution as claimed in claim 1, wherein the method comprises the following steps: the organic alcohol amine regenerated after desorbing the hydrogen sulfide is recycled and returned to the reaction process of absorbing the hydrogen sulfide.
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Application publication date: 20210706 |