CN111675295A - Preparation method of efficient flocculant for purifying acid mine wastewater - Google Patents
Preparation method of efficient flocculant for purifying acid mine wastewater Download PDFInfo
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- CN111675295A CN111675295A CN202010348295.7A CN202010348295A CN111675295A CN 111675295 A CN111675295 A CN 111675295A CN 202010348295 A CN202010348295 A CN 202010348295A CN 111675295 A CN111675295 A CN 111675295A
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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
- C02F1/5245—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents using basic salts, e.g. of aluminium and iron
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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
- C02F1/56—Macromolecular 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
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/10—Nature of the water, waste water, sewage or sludge to be treated from quarries or from mining activities
Abstract
The invention discloses a preparation method of a high-efficiency flocculating agent for purifying acid mine wastewater, which comprises the following main steps of A, according to parts by weight, preparing ferrous sulfate solution by reacting 10-15 parts of cleaned waste iron scraps and 90-130 parts of sulfuric acid solution; B. according to the mass fraction, 100 parts of ferrous sulfate and 10-15 parts of oxidant are included to prepare polymeric ferric sulfate solution; C. according to the mass fraction, the high-efficiency flocculant solution is prepared by reacting 100-130 parts of polyferric sulfate and 30-40 parts of polyacrylamide solution. According to the high-efficiency flocculating agent for purifying the mine acidic wastewater, which is prepared by the invention, the organic polymer is introduced into the molecular structure, so that the high-molecular flocculating agent with the inorganic polymer and the organic polymer integrated is obtained, and the indexes such as impurity removal rate, alumen ustum settling velocity and the like are greatly improved when the high-efficiency flocculating agent is used for treating the mine acidic wastewater.
Description
Technical Field
The invention relates to the technical field of chemical reagents, in particular to a preparation method of a high-efficiency flocculating agent for purifying acid mine wastewater.
Background
According to data statistics, the discharge amount of various mine wastewater in China accounts for about 10% of the total discharge amount of industrial wastewater in China. The acidic waste water discharged from mines is the acid waste water with the widest pollution range and the greatest harm degree in the mine waste water, and is one of the most serious environmental problems in mining or abandoned mines.
The metal mine ore body acidic wastewater is mainly generated by mining sulfide minerals contained in metal ore body ores, and the sulfide minerals are subjected to a series of physical and chemical reactions such as leaching, oxidation, hydrolysis and the like under the action of air, water and microorganisms to form acidic wastewater. The pH value of the acidic water is generally 2-4, the components are complex, the acidic water contains various heavy metals, and the ion content in each liter of water is from dozens to hundreds of milligrams. Meanwhile, the acid wastewater generated by mines is large, acid water is discharged by thousands to tens of thousands of tons every day in some mines, and the water quantity and the water quality change greatly under the conditions of mining conditions and abundant rainwater in different seasons. The treatment of acid mine waste water is increasingly strict.
At present, the method for treating acid mine wastewater mainly comprises a neutralization precipitation method, a vulcanization precipitation method, an oxidation-reduction method, a microbial treatment method and the like. In these treatment processes, flocculants must be used. Flocculants are mainly groups with positive (negative) electrical properties and particles or granules with negative (positive) electrical properties which are difficult to separate, are close to each other, lower their potential, make them unstable, and use their polymeric nature to concentrate and separate them by physical or chemical means. Flocculants can be classified into inorganic flocculants and organic flocculants according to the total chemical composition. Wherein the inorganic flocculant also comprises an inorganic coagulant and an inorganic polymeric flocculant; the organic flocculant also comprises a synthetic organic polymer flocculant, a natural organic polymer flocculant and a microbial flocculant.
Polyferric sulfate is an inorganic polymeric flocculant which has many complex ions in aqueous solution, namely OH-The compound is used as a bridge to form multi-nuclear complex ions, so that the compound becomes a larger inorganic macromolecular compound, and has the characteristics of wide pH application range, high impurity removal rate, low residue concentration, high alum blossom settling speed, good decoloration effect and the like. Because the polymerization degree of the polymeric ferric sulfate is not high, compared with the organic polymeric flocculant, the polymeric ferric sulfate still has a plurality of defects.
Disclosure of Invention
The invention aims to provide a preparation method of a high-efficiency flocculating agent for purifying acid mine wastewater. According to the method, organic polymers are introduced into polymeric ferric sulfate molecules, so that the using amount of a flocculating agent can be reduced, the sewage purification effect can be greatly improved, and the effect is particularly obvious in the aspect of treating acid mine wastewater.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a preparation method of a high-efficiency flocculating agent for purifying acid mine wastewater comprises the following steps:
s1, scrap iron cleaning: weighing 100 parts of scrap iron, 200 parts of water and 10 parts of surfactant in a reactor with a stirring device by mass, stirring and washing for 0.5h, filtering, and washing the scrap iron for 2 times to obtain the cleaned scrap iron.
S2, preparing a ferrous sulfate solution: adding 10-15 parts of weighed scrap iron cleaned by S1 and 90-130 parts of sulfuric acid solution into a reactor equipped with a stirring and heating device according to parts by weight, stirring, keeping the reaction temperature at 60-70 ℃, reacting for 1.5-2h, cooling to room temperature, filtering, and taking filtrate, namely ferrous sulfate solution;
s3, preparation of polyferric sulfate: adding 100 parts by mass of ferrous sulfate solution prepared by S2 into a reactor equipped with a stirring and heating device, dropwise adding 10-15 parts by mass of oxidant, controlling the reaction temperature at 20-30 ℃ and the reaction time at 1.5-2h, cooling to room temperature, and filtering to obtain polymeric ferric sulfate solution;
s4, preparing the high-efficiency flocculant: according to the mass portion, 130 portions of polymeric ferric sulfate solution prepared by S3 is added into a reactor equipped with a stirring and heating device, 30-40 portions of polyacrylamide solution is dripped, the reaction time is 1h, the temperature is reduced to room temperature, and the high-efficiency flocculant solution is prepared by filtering.
Preferably, the iron filings in S1 are derived from wastes generated in the machining process of a mechanical processing plant.
Preferably, the surfactant in S1 is at least one of sodium fatty alcohol polyoxyethylene ether sulfate (AES) or nonylphenol polyoxyethylene ether (TX-10);
preferably, the mass percent concentration of the sulfuric acid solution in the S2 is 20-25%;
preferably, the oxidant in S3 is at least one of potassium chlorate or hydrogen peroxide;
preferably, the polyacrylamide in the S4 is non-ionic, and the model is VN835.
Preferably, the mass percentage concentration of the polyacrylamide solution in the S4 is 5%.
The high-efficiency flocculant prepared by the invention takes industrial waste scrap iron as a raw material, firstly prepares polymeric ferric sulfate, and then modifies the polymeric ferric sulfate by using an organic polymeric flocculant. The main chemical reaction equation is as follows:
FeSO4+1/2SO4 2-→1/2Fe2(SO4)3
Fe2(SO4)3+nH2O→Fe2(OH)n(SO4)3-n/2+n/2H2SO4wherein n is less than or equal to 2)
m[Fe2(OH)n(SO4)3-n/2]→[Fe2(OH)n(SO4)3-n/2]m
Wherein n is less than or equal to 2, m is more than or equal to f (n)
According to the high-efficiency flocculant for purifying mine acidic wastewater, which is prepared by the invention, an organic polymer is introduced into a molecular structure, so that the high-molecular flocculant integrating an inorganic polymer and the organic polymer is obtained, and the indexes such as impurity removal rate, alum blossom settling velocity and the like are greatly improved when the high-efficiency flocculant is used for treating mine acidic wastewater.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The invention is described in further detail below with reference to the figures and specific examples.
Example 1
A preparation method of a high-efficiency flocculating agent for purifying acid mine wastewater comprises the following steps:
s1, scrap iron cleaning: weighing 100 parts of scrap iron, 200 parts of water and 10 parts of nonylphenol polyoxyethylene ether (TX-10) in a reactor with a stirring device by mass, stirring and washing for 0.5h, filtering, and washing the scrap iron for 2 times to obtain the cleaned scrap iron.
S2, preparing a ferrous sulfate solution: adding 10 parts of weighed scrap iron cleaned by S1 and 90 parts of sulfuric acid solution with the mass percentage concentration of 20% into a reactor equipped with a stirring and heating device according to the parts by mass, stirring, keeping the reaction temperature at 60 ℃, reacting for 1.5h, cooling to room temperature, filtering, and taking filtrate, namely the ferrous sulfate solution;
s3, preparation of polyferric sulfate: adding 100 parts by mass of ferrous sulfate solution prepared in S2 into a reactor equipped with a stirring and heating device, dropwise adding 10 parts by mass of potassium chlorate, controlling the reaction temperature at 20 ℃, reacting for 1.5h, cooling to room temperature, and filtering to obtain polymeric ferric sulfate solution;
s4, preparing the high-efficiency flocculant: adding 100 parts by mass of polymeric ferric sulfate solution prepared by S3 into a reactor equipped with a stirring and heating device, dropwise adding 30 parts by mass of polyacrylamide solution with the mass percentage concentration of 5%, reacting for 1h, cooling to room temperature, and filtering to obtain the high-efficiency flocculant solution.
Example 2
A preparation method of a high-efficiency flocculating agent for purifying acid mine wastewater comprises the following steps:
s1, scrap iron cleaning: weighing 100 parts of scrap iron, 200 parts of water and 10 parts of fatty alcohol-polyoxyethylene ether sodium sulfate (AES) in parts by mass in a reactor with a stirring device, stirring and washing for 0.5h, filtering, and washing the scrap iron for 2 times to obtain the cleaned scrap iron.
S2, preparing a ferrous sulfate solution: adding 15 parts of weighed S1 cleaned scrap iron and 130 parts of 25% sulfuric acid solution in parts by mass into a reactor equipped with a stirring and heating device, stirring, keeping the reaction temperature at 70 ℃, reacting for 2 hours, cooling to room temperature, filtering, and taking filtrate, namely the ferrous sulfate solution;
s3, preparation of polyferric sulfate: adding 100 parts by weight of ferrous sulfate solution prepared in S2 into a reactor equipped with a stirring and heating device, dropwise adding 15 parts by weight of hydrogen peroxide, controlling the reaction temperature at 30 ℃, reacting for 2 hours, cooling to room temperature, and filtering to obtain polymeric ferric sulfate solution;
s4, preparing the high-efficiency flocculant: adding 130 parts of polymeric ferric sulfate solution prepared by S3 into a reactor equipped with a stirring and heating device according to parts by weight, dropwise adding 40 parts of polyacrylamide solution with the mass percentage concentration of 5%, reacting for 1h, cooling to room temperature, and filtering to obtain the high-efficiency flocculant solution.
Example 3
A preparation method of a high-efficiency flocculating agent for purifying acid mine wastewater comprises the following steps:
s1, scrap iron cleaning: weighing 100 parts of scrap iron, 200 parts of water, a mixture of 4 parts of nonylphenol polyoxyethylene ether (TX-10) and 6 parts of fatty alcohol polyoxyethylene ether sodium sulfate (AES) in a reactor with a stirring device by mass, stirring and washing for 0.5h, filtering, and washing the scrap iron for 2 times by using water to obtain the cleaned scrap iron.
S2, preparing a ferrous sulfate solution: adding 13 parts of weighed S1 cleaned scrap iron and 110 parts of sulfuric acid solution with the mass percentage concentration of 20% into a reactor equipped with a stirring and heating device according to the parts by mass, stirring, keeping the reaction temperature at 65 ℃, reacting for 1.8h, cooling to room temperature, filtering, and taking filtrate, namely the ferrous sulfate solution;
s3, preparation of polyferric sulfate: adding 100 parts by weight of ferrous sulfate solution prepared in S2 into a reactor equipped with a stirring and heating device, dropwise adding 10 parts by weight of potassium chlorate and 5 parts by weight of hydrogen peroxide, controlling the reaction temperature at 26 ℃ and the reaction time to be 1.8h, cooling to room temperature, and filtering to obtain polymeric ferric sulfate solution;
s4, preparing the high-efficiency flocculant: according to the mass parts, in a reactor equipped with a stirring and heating device, adding 130 parts of polymeric ferric sulfate solution prepared by S3, dripping 35 parts of polyacrylamide solution with the mass percentage concentration of 5%, reacting for 1h, cooling to room temperature, and filtering to obtain the high-efficiency flocculant solution.
Example 4
A preparation method of a high-efficiency flocculating agent for purifying acid mine wastewater comprises the following steps:
s1, scrap iron cleaning: weighing 100 parts of scrap iron, 200 parts of water and 10 parts of fatty alcohol-polyoxyethylene ether sodium sulfate (AES) in parts by mass in a reactor with a stirring device, stirring and washing for 0.5h, filtering, and washing the scrap iron for 2 times to obtain the cleaned scrap iron.
S2, preparing a ferrous sulfate solution: adding 12 parts of weighed S1 cleaned scrap iron and 120 parts of 25% sulfuric acid solution in parts by mass into a reactor equipped with a stirring and heating device, stirring, keeping the reaction temperature at 68 ℃, reacting for 2 hours, cooling to room temperature, filtering, and taking filtrate, namely ferrous sulfate solution;
s3, preparation of polyferric sulfate: adding 100 parts by weight of ferrous sulfate solution prepared in S2 into a reactor equipped with a stirring and heating device, dropwise adding 12 parts by weight of hydrogen peroxide, controlling the reaction temperature at 26 ℃ and the reaction time to be 1.5h, cooling to room temperature, and filtering to obtain polymeric ferric sulfate solution;
s4, preparing the high-efficiency flocculant: according to the mass parts, 125 parts of polymeric ferric sulfate solution prepared by S3 is added into a reactor equipped with a stirring and heating device, 36 parts of polyacrylamide solution with the mass percentage concentration of 5% is dripped, the reaction time is 1h, the temperature is reduced to the room temperature, and the high-efficiency flocculant solution is prepared by filtering.
Example 5
A preparation method of a high-efficiency flocculating agent for purifying acid mine wastewater comprises the following steps:
s1, scrap iron cleaning: weighing 100 parts of scrap iron, 200 parts of water and 10 parts of surface nonylphenol polyoxyethylene ether (TX-10) in a reactor with a stirring device by mass, stirring and washing for 0.5h, filtering, and washing the scrap iron for 2 times by using water to obtain the cleaned scrap iron.
S2, preparing a ferrous sulfate solution: adding 15 parts of weighed S1 cleaned scrap iron and 140 parts of 20 mass percent sulfuric acid solution into a reactor equipped with a stirring and heating device according to parts by mass, stirring, keeping the reaction temperature at 60 ℃, reacting for 2 hours, cooling to room temperature, filtering, and taking filtrate, namely ferrous sulfate solution;
s3, preparation of polyferric sulfate: adding 100 parts by weight of ferrous sulfate solution prepared in S2 into a reactor equipped with a stirring and heating device, dropwise adding 10 parts by weight of potassium chlorate, controlling the reaction temperature at 25 ℃, reacting for 2 hours, cooling to room temperature, and filtering to obtain polymeric ferric sulfate solution;
s4, preparing the high-efficiency flocculant: adding 120 parts by mass of polymeric ferric sulfate solution prepared in S3 into a reactor equipped with a stirring and heating device, dropwise adding 38 parts by mass of polyacrylamide solution with the mass percentage concentration of 5%, reacting for 1h, cooling to room temperature, and filtering to obtain the high-efficiency flocculant solution.
Example 6
A preparation method of a high-efficiency flocculating agent for purifying acid mine wastewater comprises the following steps:
s1, scrap iron cleaning: weighing 100 parts of scrap iron, 200 parts of water, a mixture of 7 parts of nonylphenol polyoxyethylene ether (TX-10) and 3 parts of fatty alcohol polyoxyethylene ether sodium sulfate (AES) in a reactor with a stirring device by mass, stirring and washing for 0.5h, filtering, and washing the scrap iron for 2 times to obtain the cleaned scrap iron.
S2, preparing a ferrous sulfate solution: adding 11 parts by weight of the weighed S1 cleaned scrap iron and 90 parts by weight of a 20% sulfuric acid solution into a reactor equipped with a stirring and heating device, stirring, keeping the reaction temperature at 70 ℃, reacting for 1.8h, cooling to room temperature, filtering, and taking filtrate, namely the ferrous sulfate solution;
s3, preparation of polyferric sulfate: adding 100 parts by weight of ferrous sulfate solution prepared in S2 into a reactor equipped with a stirring and heating device, dropwise adding 10 parts by weight of hydrogen peroxide, controlling the reaction temperature at 30 ℃ and the reaction time to be 1.5h, cooling to room temperature, and filtering to obtain polymeric ferric sulfate solution;
s4, preparing the high-efficiency flocculant: adding 130 parts of polymeric ferric sulfate solution prepared in S3 into a reactor equipped with a stirring and heating device according to parts by weight, dropwise adding 34 parts of polyacrylamide solution with the mass percentage concentration of 5%, reacting for 1h, cooling to room temperature, and filtering to obtain the high-efficiency flocculant solution.
In the above embodiments, the iron filings are derived from waste in the machining process of a machining factory. The polyacrylamide is nonionic, and the model is VN835.
The main performance indexes of the high-efficiency flocculant for purifying acid mine wastewater prepared in the embodiment are shown in table 1.
TABLE 1
The above results were tested according to the standard requirements of GB14591-2006 polymeric ferric sulfate Water treatment agent.
According to the high-efficiency flocculating agent for purifying the mine acidic wastewater, which is prepared by the invention, the organic polymer is introduced into the molecular structure, so that the high-molecular flocculating agent with the inorganic polymer and the organic polymer integrated is obtained, and the indexes such as impurity removal rate, alumen ustum settling velocity and the like are greatly improved when the high-efficiency flocculating agent is used for treating the mine acidic wastewater.
Claims (7)
1. A preparation method of a high-efficiency flocculating agent for purifying acid mine wastewater is characterized by comprising the following steps: it comprises the following steps:
s1, scrap iron cleaning: weighing 100 parts of scrap iron, 200 parts of water and 10 parts of surfactant in a reactor with a stirring device by mass, stirring and washing for 0.5h, filtering, and washing the scrap iron for 2 times to obtain the cleaned scrap iron.
S2, preparing a ferrous sulfate solution: adding 10-15 parts of weighed scrap iron cleaned by S1 and 90-130 parts of sulfuric acid solution into a reactor equipped with a stirring and heating device according to parts by weight, stirring, keeping the reaction temperature at 60-70 ℃, reacting for 1.5-2h, cooling to room temperature, filtering, and taking filtrate, namely ferrous sulfate solution;
s3, preparation of polyferric sulfate: adding 100 parts by mass of ferrous sulfate solution prepared by S2 into a reactor equipped with a stirring and heating device, dropwise adding 10-15 parts by mass of oxidant, controlling the reaction temperature at 20-30 ℃ and the reaction time at 1.5-2h, cooling to room temperature, and filtering to obtain polymeric ferric sulfate solution;
s4, preparing the high-efficiency flocculant: according to the mass portion, 130 portions of polymeric ferric sulfate solution prepared by S3 is added into a reactor equipped with a stirring and heating device, 30-40 portions of polyacrylamide solution is dripped, the reaction time is 1h, the temperature is reduced to room temperature, and the high-efficiency flocculant solution is prepared by filtering.
2. The preparation method of the high-efficiency flocculating agent for purifying acid mine wastewater according to claim 1, which is characterized by comprising the following steps: and the iron scraps in the S1 are derived from wastes in the machining process of a mechanical processing plant.
3. The preparation method of the high-efficiency flocculating agent for purifying acid mine wastewater according to claim 1, which is characterized by comprising the following steps: and the surfactant in the S1 is at least one of fatty alcohol polyoxyethylene ether sodium sulfate (AES) or nonylphenol polyoxyethylene ether (TX-10).
4. The preparation method of the high-efficiency flocculating agent for purifying acid mine wastewater according to claim 1, which is characterized by comprising the following steps: the mass percent concentration of the sulfuric acid solution in the S2 is 20-25%.
5. The preparation method of the high-efficiency flocculating agent for purifying acid mine wastewater according to claim 1, which is characterized by comprising the following steps: and the oxidant in the S3 is at least one of potassium chlorate or hydrogen peroxide.
6. The preparation method of the high-efficiency flocculating agent for purifying acid mine wastewater according to claim 1, which is characterized by comprising the following steps: and the polyacrylamide in the S4 is nonionic, and the model is VN835.
7. The preparation method of the high-efficiency flocculating agent for purifying acid mine wastewater according to claim 1, which is characterized by comprising the following steps: the mass percentage concentration of the polyacrylamide solution in the S4 is 5%.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114249407A (en) * | 2021-12-28 | 2022-03-29 | 河北正润环境科技有限公司 | Method for recycling pickling waste liquid in steel finishing |
| CN114477605A (en) * | 2022-02-22 | 2022-05-13 | 浙江宏电环保装备有限公司 | Membrane concentrate treatment facility with settlement treatment structure |
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| CN101274780A (en) * | 2008-05-19 | 2008-10-01 | 山西大学 | Polymeric ferric polysulfate composite coagulant and application thereof |
| CN101786708A (en) * | 2010-03-01 | 2010-07-28 | 株式会社东洋贸易 | Iron-based flocculating agent and preparation method thereof |
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2020
- 2020-04-28 CN CN202010348295.7A patent/CN111675295A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101274780A (en) * | 2008-05-19 | 2008-10-01 | 山西大学 | Polymeric ferric polysulfate composite coagulant and application thereof |
| CN101786708A (en) * | 2010-03-01 | 2010-07-28 | 株式会社东洋贸易 | Iron-based flocculating agent and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114249407A (en) * | 2021-12-28 | 2022-03-29 | 河北正润环境科技有限公司 | Method for recycling pickling waste liquid in steel finishing |
| CN114249407B (en) * | 2021-12-28 | 2024-02-02 | 河北正润环境科技有限公司 | Recycling method of steel finishing pickling waste liquid |
| CN114477605A (en) * | 2022-02-22 | 2022-05-13 | 浙江宏电环保装备有限公司 | Membrane concentrate treatment facility with settlement treatment structure |
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Application publication date: 20200918 |