CN111908653B - Slow-release arsenic and antimony removal medicament, preparation method thereof and method for deeply treating heavy metal wastewater by adopting slow-release arsenic and antimony removal medicament - Google Patents
Slow-release arsenic and antimony removal medicament, preparation method thereof and method for deeply treating heavy metal wastewater by adopting slow-release arsenic and antimony removal medicament Download PDFInfo
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- CN111908653B CN111908653B CN202010668645.8A CN202010668645A CN111908653B CN 111908653 B CN111908653 B CN 111908653B CN 202010668645 A CN202010668645 A CN 202010668645A CN 111908653 B CN111908653 B CN 111908653B
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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
- C02F1/28—Treatment of water, waste water, or sewage by sorption
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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
- C02F1/00—Treatment of water, waste water, or sewage
- C02F2001/007—Processes including a sedimentation step
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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 belongs to the technical field of sewage and wastewater treatment, and particularly relates to a slow-release arsenic and antimony removal medicament, a preparation method thereof and a method for deeply treating heavy metal wastewater by adopting the slow-release arsenic and antimony removal medicament, wherein the slow-release arsenic and antimony removal medicament comprises the following components: iron manganese complexes and polyethyleneimines; wherein the mass volume ratio g/L of the iron-manganese compound to 1-20% of polyethyleneimine solution is 10-200: 1. after the heavy metal wastewater is treated by the method, the special emission limit requirement of the industry can be met, the medicament adding amount is small, the hazardous waste generation amount is small, and the secondary pollution risk is reduced.
Description
Technical Field
The invention belongs to the technical field of sewage and wastewater treatment, and particularly relates to a slow-release arsenic and antimony removal medicament, a preparation method thereof and a method for deeply treating heavy metal wastewater by adopting the slow-release arsenic and antimony removal medicament, which are used for deeply treating arsenic-antimony-containing heavy metal wastewater, and are particularly suitable for deeply treating waste water related to non-ferrous metal mining, selection, smelting and other industries.
Background
At present, in the aspect of arsenic-antimony heavy metal wastewater treatment, a lime-iron salt treatment method is mainly adopted, and in order to achieve a treatment effect, a large amount of medicament needs to be excessively added in a treatment process, so that the problems of large medicament consumption, large sludge (hazardous waste) generation amount and the like are caused. Therefore, the conventional lime-iron salt technology can not meet increasingly strict environmental protection requirements, and a new arsenic and antimony-containing heavy metal wastewater advanced treatment method needs to be developed urgently, so that the concentrations of arsenic and antimony in wastewater can be stably reduced to the special discharge limit value of the industry from 100-200 mg/L and 10-20 mg/L respectively, the removal rate reaches more than 99%, and the treatment requirement of the heavy metal wastewater is met.
Chinese patent application CN104193043A discloses a dearsenification treatment process and method for high-concentration arsenic-containing alkaline wastewater, but the dearsenification agent used in the method is still traditional inorganic high molecular polymer, such as one or more of polymeric ferric sulfate, polymeric ferrous sulfate, polymeric aluminum chloride and polymeric aluminum iron.
Chinese patent CN105858958B discloses a method for treating mine wastewater containing arsenic, antimony and cyanogen, but the arsenic and antimony removing agent used in the method is one or a compound of more of traditional ferric sulfate, ferrous sulfate, polymeric ferric sulfate, ferric chloride, ferrous chloride and ferric nitrate.
The traditional heavy metal treatment agent has the advantages of large dosage, low removal rate, large hazardous waste generation amount and easy secondary pollution when treating heavy metal wastewater.
Disclosure of Invention
The invention aims to provide a slow-release arsenic and antimony removal medicament and an advanced treatment method of heavy metal wastewater containing arsenic and antimony by adopting the slow-release arsenic and antimony removal medicament.
In order to achieve the purpose, the invention is realized by the following technical scheme:
the slow-release arsenic and antimony removal medicament comprises the following components: iron manganese complexes and polyethyleneimines;
wherein the mass volume ratio g/L of the iron-manganese compound to the polyethyleneimine solution with the mass fraction of 1-20% is 10-200: 1.
the invention also provides a preparation method of the sustained-release arsenic and antimony removal medicament, which comprises the following steps:
a) carrying out aeration reaction on potassium permanganate and ferrous sulfate in a solution according to a molar ratio of 1: 3-10 for 1-3 h, then adding sodium hydroxide into the solution to enable the pH of the solution to reach 3-5, drying the mixed solution at 600-800 ℃ for 1-3 h, and preparing a matrix material-iron-manganese compound;
b) preparing 1-20% polyethyleneimine solution, namely coating material solution;
c) stirring and mixing the substrate material and the coating material solution according to the mass volume ratio of 10-200 g/L for 10-30 min to prepare a mixed substance of the substrate material and the coating material;
d) and drying the mixed substance of the substrate material and the coating material at the drying temperature of 150-300 ℃ for 6-12 h, and then cooling to room temperature to obtain the slow-release arsenic and antimony removal medicament.
The solution in step a) is an aqueous solution.
Preferably, the 1% -20% polyethyleneimine solution in step b) of the invention can be obtained by mixing a polyethyleneimine aqueous solution with a mass fraction of 50% in ethanol, or can be obtained by directly diluting the polyethyleneimine aqueous solution with a mass fraction of 50% in water.
The invention further provides an advanced treatment method of the heavy metal wastewater containing arsenic and antimony, which comprises the following steps:
1) adding the slow-release arsenic and antimony removal agent into heavy metal wastewater containing arsenic and antimony, carrying out full stirring reaction, and carrying out flocculation reaction on the wastewater after the reaction;
2) carrying out precipitation treatment on the wastewater after the flocculation reaction;
3) in the process of precipitation treatment, precipitates containing heavy metals such as arsenic and antimony are subjected to precipitation and solid-liquid separation, the separated wastewater is discharged after reaching the standard, and the generated sludge is safely treated.
Preferably, in the step 1), the mass-to-volume ratio of the slow-release arsenic and antimony removal agent to the arsenic and antimony-containing heavy metal wastewater is 300 mg-500 mg/L, and the stirring reaction time is 30-60 min.
Preferably, in the step 2), the flocculation reaction time is 5-15 min.
Preferably, in the step 3), the precipitation time is 1-3 h.
Specifically, the slow-release arsenic and antimony removal medicament, the preparation method thereof and the method for deeply treating heavy metal wastewater by adopting the slow-release arsenic and antimony removal medicament comprise the following steps:
1) the slow-release arsenic and antimony removal medicament is added in an amount of 300 mg-500 mg/L (waste water) Adding the heavy metal wastewater containing arsenic and antimony into the wastewater, fully stirring and reacting for 30-60 min, and allowing the wastewater after reaction to enter a flocculation reaction unit;
2) in the flocculation reaction unit, carrying out flocculation reaction by utilizing flocculation of substances in the arsenic and antimony removal medicament for 5-15 min, and allowing the wastewater after the flocculation reaction to enter a precipitation treatment unit;
3) in the precipitation treatment unit, solid-liquid separation is carried out on precipitates containing heavy metals such as arsenic and antimony through precipitation, the precipitation time is 1-3 hours, the treated wastewater is discharged after reaching the standard, and the generated sludge is safely treated.
In the step 1), the preparation method of the slow-release arsenic and antimony removal medicament comprises the following steps:
a) carrying out an aeration reaction on potassium permanganate and ferrous sulfate in an aqueous solution for 1-3 h according to a molar ratio of 1: 3-10, then adding sodium hydroxide into the solution to enable the pH of the solution to reach 3-5, and drying the mixed solution at 600-800 ℃ for 1-3 h to prepare a matrix material;
b) preparing 1-20% polyethyleneimine solution, namely coating material solution, by adding 50% polyethyleneimine aqueous solution into 99.97% industrial ethanol;
c) the matrix material of the slow-release arsenic and antimony removal medicament is added by 10g to 200g/L (coating material solution) Stirring and mixing the solution of the coating material and the solution of the coating material for 10-30 min to prepare a slow-release arsenic and antimony removal medicament matrix material and a coating material mixed substance;
d) heating the mixed substance of the substrate material and the coating material of the slow-release arsenic and antimony removal medicament to 150-300 ℃ in a blast drying oven, drying for 6-12 h, and cooling to room temperature to obtain the prepared slow-release arsenic and antimony removal medicament.
In the present invention, "%" refers to mass percent concentration unless otherwise specified.
The iron-manganese compound is a mixture of hydrated iron-manganese oxide compound and excessive ferric sulfate, and has synergistic effect of adsorption and flocculation when treating heavy metals; the coating material adopts polyethyleneimine, has a slow release effect, is also a good adsorbent for treating heavy metals, and therefore has a good treatment effect under the comprehensive effect. The invention adds excessive ferrous sulfate when preparing the iron-manganese compound, and excessive ferric sulfate can be generated after reaction, thereby playing a role in flocculation.
Compared with the prior art, the invention has the beneficial effects that:
1) aiming at the water quality characteristics of the arsenic-antimony-containing heavy metal wastewater, the invention adopts the slow-release arsenic-antimony removal medicament, the dosage of the medicament is small (more than 20 percent reduction), the generation amount of hazardous waste is small, and the secondary pollution risk is reduced.
2) The slow-release arsenic and antimony removal medicament contains ferric sulfate and is high in content, a flocculating agent is not required to be added additionally in the flocculation process, and the flocculation precipitation effect is good.
3) In the process of dissolving the slow-release arsenic and antimony removal medicament in water and slowly releasing, the polyethyleneimine is also released into the wastewater, so that the effect of advanced treatment on heavy metal adsorption can be achieved.
4) According to the invention, the arsenic and antimony concentrations in the wastewater can be stably reduced from 100-200 mg/L and 12-20 mg/L respectively to the specific emission limit removal rate specified by standards such as copper, nickel and cobalt industrial pollutant emission standards (GB25467-2010), lead and zinc industrial pollutant emission standards (GB25466-2010) and tin, antimony and mercury industrial pollutant emission standards (GB30770-2014) and the like, which reaches more than 99%, so that the treatment requirement of the heavy metal wastewater is met.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments.
Example 1
A method for deeply treating heavy metal wastewater by adopting a slow-release arsenic and antimony removal medicament comprises the following steps:
1) the slow-release arsenic and antimony removal medicament is added at 300mg/L (waste water) Adding the additive amount of the compound into heavy metal wastewater containing arsenic and antimony, stirring and reacting for 30min, and allowing the wastewater after reaction to enter a flocculation reaction unit; the heavy metal wastewater containing arsenic and antimony is non-ferrous metal smelting wastewater, and the concentrations of arsenic and antimony are 100mg/L and 12mg/L respectively;
2) in the flocculation reaction unit, flocculation reaction is carried out by utilizing flocculation effect of substances in the slow-release arsenic and antimony removal medicament, the reaction time is 5min, and the wastewater after the flocculation reaction enters the precipitation treatment unit;
3) and carrying out solid-liquid separation on the precipitate containing heavy metals such as arsenic, antimony and the like through precipitation, wherein the precipitation time is 1h, the treated wastewater is discharged after reaching the standard, and the generated sludge is safely treated.
In the step 1), the preparation method of the slow-release arsenic and antimony removal medicament comprises the following steps:
a) carrying out aeration reaction on potassium permanganate and ferrous sulfate in a solution according to a molar ratio of 1:3 for 1h, then adding sodium hydroxide into the solution to enable the pH of the solution to reach 3, and drying the mixed solution at 600 ℃ for 1h to prepare a matrix material; .
b) Mixing 50% of polyethyleneimine water solution into 99.97% of industrial ethanol to prepare 1% of polyethyleneimine solution, namely coating material solution.
c) The matrix material of the slow-release arsenic and antimony removal medicament is added by 10g/L (coating material solution) Stirring and mixing the solution of the coating material for 10min to prepare the slow-release arsenic and antimony removal medicament matrix material and coating material mixed substance.
d) Heating the mixed substance of the substrate material and the coating material of the slow-release arsenic and antimony removal medicament to 150 ℃ in a blast drying oven, drying and drying for 6 hours, and cooling to room temperature to obtain the prepared slow-release arsenic and antimony removal medicament.
The dosage of the slow-release arsenic and antimony removal medicament is reduced by 25% compared with the dosage of the traditional heavy metal wastewater treatment medicament when the same amount of heavy metal wastewater is treated.
The results of advanced treatment of heavy metal wastewater containing arsenic and antimony are shown in Table 1.
TABLE 1 EXAMPLE 1 Effect of removing arsenic and antimony
| Dosage of medicament (mg/L waste water) | 300 | Removal rate |
| Concentration (mg/L) of total arsenic in treated effluent | 0.0203 | 99.98％ |
| Concentration (mg/L) of total antimony in treated effluent | 0.119 | 99％ |
Example 2
A method for deeply treating heavy metal wastewater by adopting a slow-release arsenic and antimony removal medicament comprises the following steps:
1) the slow-release arsenic and antimony removal medicament is added at 500mg/L (waste water) Adding the heavy metal wastewater containing arsenic and antimony into the wastewater, stirring and reacting for 60min, and allowing the wastewater after reaction to enter a flocculation reaction unit; the heavy metal wastewater containing arsenic and antimony is non-ferrous metal mining and dressing wastewater, and the concentrations of arsenic and antimony are 200mg/L and 20mg/L respectively.
2) In the flocculation reaction unit, flocculation reaction is carried out by utilizing the flocculation effect of substances in the slow-release arsenic and antimony removal medicament, the reaction time is 15min, and the wastewater after the flocculation reaction enters the precipitation treatment unit.
3) And carrying out solid-liquid separation on the precipitate containing heavy metals such as arsenic, antimony and the like through precipitation, wherein the precipitation time is 3 hours, the treated wastewater is discharged after reaching the standard, and the generated sludge is safely treated.
In the step 1), the preparation method of the slow-release arsenic and antimony removal medicament comprises the following steps:
a) performing aeration reaction on potassium permanganate and ferrous sulfate in a solution according to a molar ratio of 1:10 for 3 hours, then adding sodium hydroxide into the solution to enable the pH of the solution to reach 5, and drying the mixed solution at 800 ℃ for 3 hours to prepare a matrix material; .
b) Mixing 50% of polyethyleneimine water solution into 99.97% of industrial ethanol to prepare 20% of polyethyleneimine solution, namely coating material solution.
c) The matrix material of the slow-release arsenic-antimony removing medicament is 200g/L (coating material solution) Stirring and mixing the solution with the coating material solution for 30min to prepare the slow-release arsenic and antimony removal medicament and the coating material mixed substance.
d) Heating the mixed substance of the slow-release arsenic and antimony removal medicament and the coating material in a blast drying oven to 300 ℃, drying for 12h, and cooling to room temperature to obtain the prepared slow-release arsenic and antimony removal medicament.
The dosage of the slow-release arsenic and antimony removal medicament in the embodiment is reduced by 28% compared with the dosage of the traditional heavy metal wastewater treatment medicament.
The results of advanced treatment of heavy metal wastewater containing arsenic and antimony are shown in Table 2.
Table 2 example 2 effect of removing arsenic and antimony
| Dosage of medicament (mg/L waste water) | 500 | Removal rate of |
| Concentration (mg/L) of total arsenic in treated effluent | 0.00644 | 99.99％ |
| Concentration (mg/L) of total antimony in treated effluent | 0.0768 | 99.6％ |
The method can be realized by upper and lower limit values of intervals of process parameters (such as temperature, time and the like) and interval values, and embodiments are not listed.
Conventional technical knowledge in the art can be used for the details which are not described in the present invention.
Any feature disclosed in this specification may be replaced by alternative features serving an equivalent or similar purpose, unless expressly stated otherwise. Unless expressly stated otherwise, each feature is only an example of a generic series of equivalent or similar features. The description is only for the purpose of aiding understanding of the present invention and should not be construed as specifically limiting the present invention.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and are not limited. Although the present invention has been described in detail with reference to the embodiments, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (5)
1. The slow-release arsenic and antimony removal medicament is characterized by comprising the following components in parts by weight: iron manganese complexes and polyethyleneimines; wherein the mass volume ratio g/L of the iron-manganese compound to the polyethyleneimine solution with the mass percentage concentration of 1% -20% is 10-200: 1;
the preparation method of the slow-release arsenic and antimony removal medicament comprises the following steps: a) carrying out aeration reaction on potassium permanganate and ferrous sulfate according to the molar ratio of 1: 3-10 for 1-3 h, then adding sodium hydroxide to enable the pH of the solution to reach 3-5, drying the mixed solution at 600-800 ℃ for 1-3 h, and preparing a matrix material-iron-manganese compound; b) preparing 1-20% polyethyleneimine solution, namely coating material solution; c) stirring and mixing the substrate material and the coating material solution according to the mass volume ratio of 10-200 g/L for 10-30 min to prepare a mixed substance of the substrate material and the coating material; d) and drying the mixed substance of the substrate material and the coating material at the drying temperature of 150-300 ℃ for 6-12 h, and then cooling to room temperature to obtain the slow-release arsenic and antimony removal medicament.
2. The advanced treatment method of heavy metal wastewater containing arsenic and antimony comprises the following steps: 1) the slow-release arsenic and antimony removal medicament of claim 1 is added into heavy metal wastewater containing arsenic and antimony, sufficient stirring reaction is carried out, and flocculation reaction is carried out on the wastewater after reaction; 2) carrying out precipitation treatment on the wastewater after the flocculation reaction; 3) in the precipitation treatment process, heavy metal precipitates containing arsenic and antimony are subjected to precipitation and solid-liquid separation, the separated wastewater is discharged after reaching the standard, and the generated sludge is safely treated.
3. The advanced treatment method for arsenic-antimony-containing heavy metal wastewater as claimed in claim 2, wherein in the step 1), the mass-volume ratio of the slow-release arsenic-antimony removing agent to the arsenic-antimony-containing heavy metal wastewater is 300 mg-500 mg/L, and the stirring reaction time is 30-60 min.
4. The advanced treatment method for arsenic-antimony-containing heavy metal wastewater according to claim 2, wherein in the step 2), the flocculation reaction time is 5-15 min.
5. The advanced treatment method for arsenic-antimony-containing heavy metal wastewater as claimed in claim 2, wherein in the step 3), the precipitation time is 1-3 h.
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