CN110790411A - Treatment method of industrial lead smelting wastewater - Google Patents
Treatment method of industrial lead smelting wastewater Download PDFInfo
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- CN110790411A CN110790411A CN201911209730.1A CN201911209730A CN110790411A CN 110790411 A CN110790411 A CN 110790411A CN 201911209730 A CN201911209730 A CN 201911209730A CN 110790411 A CN110790411 A CN 110790411A
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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
- C02F1/001—Processes for the treatment of water whereby the filtration technique is of importance
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/14—Ultrafiltration; Microfiltration
- B01D61/145—Ultrafiltration
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0002—Organic membrane manufacture
- B01D67/0006—Organic membrane manufacture by chemical reactions
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/66—Polymers having sulfur in the main chain, with or without nitrogen, oxygen or carbon only
- B01D71/68—Polysulfones; Polyethersulfones
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
- C02F1/444—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by ultrafiltration or microfiltration
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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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- 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
- C02F2103/16—Nature of the water, waste water, sewage or sludge to be treated from metallurgical processes, i.e. from the production, refining or treatment of metals, e.g. galvanic wastes
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Abstract
The invention discloses a method for treating industrial lead smelting wastewater, which comprises the following steps: step one, preparing a rare earth filter solution: adding polyether sulfone into dimethyl sulfoxide, stirring at a low speed of 100-. The invention takes dimethyl sulfoxide and polyether sulfone as main materials to prepare the polyether sulfone ultrafiltration membrane, the activity and the strength performance of the ultrafiltration membrane are changed by modifying the ultrafiltration membrane, the added nano-cellulose has the performances of high elastic membrane amount, high strength and the like, and a cross-linked network structure can be formed by the added cross-linked starch and the nano-cellulose.
Description
Technical Field
The invention relates to the technical field of industrial wastewater treatment, in particular to a treatment method of industrial lead smelting wastewater.
Background
Lead is widely used in the industry at present, and is used most in the electrical industry sector, mainly for manufacturing storage batteries, various cable protection sheaths, fusing fuses, and the like. Lead plates and pipes are often used as acid-resistant linings and corrosion-resistant covers for corrosion protection of smelting and chemical equipment, and lead is also used as a protective layer and a protective screen for atomic energy industry and X-ray. Lead compounds are used in the pigment industry, the glass industry, the petroleum industry, the medical sector, etc. A large amount of waste liquid is generated in a plurality of working procedures of lead smelting treatment, the waste liquid contains grease, high molecular compounds, solid particle impurities, heavy metal ions and the like, the waste liquid can be discharged only after reaching the national standard after being treated, otherwise, the waste liquid can bring serious harm to the environment.
The removal rate of metal impurities in the existing lead smelting wastewater is not very high, and the adopted removal method is mostly matched with an adsorption method and a chemical method for use, so that innovation is still needed to be carried out, and the removal efficiency of the wastewater is improved.
Chinese patent document CN107352708B discloses a method for treating lead smelting wastewater, comprising the following steps: (1) the method can achieve the method for effectively removing the wastewater through primary filtration treatment, (2) secondary filtration treatment, (3) electrochemical treatment and (4) filtration treatment, but different process effects and technical schemes are different, and the brought effects are different.
Disclosure of Invention
The invention aims to provide a method for treating industrial lead smelting wastewater, which aims to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme:
a treatment method of industrial lead smelting wastewater comprises the following steps:
step one, preparing a rare earth filter solution: adding polyether sulfone into dimethyl sulfoxide, stirring at a low speed of 100-;
step two, preparing the rare earth filter membrane: flatly paving the filter membrane liquid in a membrane piece, and then conveying the membrane piece into a vacuum drying oven, wherein the drying temperature is 25-35 ℃, and the drying time is 18-24 hours, so as to obtain a rare earth filter membrane;
step three, preparing a filtering agent: firstly, carrying out heat treatment on illite, then carrying out ultraviolet irradiation for 10-20min, wherein the irradiation power is 100-;
step four, treating the filtering agent: adding the filtering agent prepared in the third step into the wastewater, stirring at the rotating speed of 200-300r/min for 20-30min, standing for 1-2h, and applying pulse current during standing;
step five: filtering the rare earth filter solution: and (4) slowly flowing the filtrate treated by the filtering agent in the step four into the rare earth filtrate liquid, repeating for 2-3 times, and then obtaining the filtrate.
Preferably, the preparation method of the rare earth gadolinium chloride solution in the first step is to calcine the rare earth gadolinium chloride at a high temperature of 500-.
Preferably, the corona treatment power is 10-20Kw, and the treatment time is 10-20 min.
Preferably, the corona treatment power is 15Kw and the treatment time is 15 min.
Preferably, the heat treatment in the third step comprises the specific steps of firstly raising the temperature to 300 ℃ at the speed of 5 ℃/min, then preserving the heat for 20-30min, then continuously raising the temperature to 650 ℃ at the speed of 1 ℃/min, continuously preserving the heat for 20-30min, and finally reducing the temperature to room temperature at the speed of 2 ℃/min.
Preferably, the modifier comprises the following raw materials in parts by weight: 30-60 parts of hydroxyl phosphoryl acetic acid, 10-20 parts of 2-amino-8-naphthol-3, 6-disulfonic acid and 45-55 parts of 5-10% chitosan acetic acid solution.
Preferably, the modifier comprises the following raw materials in parts by weight: 45 parts of hydroxyl phosphoryl acetic acid, 15 parts of 2-amino-8-naphthol-3, 6-disulfonic acid and 50 parts of 5-10% chitosan acetic acid solution.
Preferably, the conditions for applying the pulse current in the fourth step are as follows: the frequency of the electric field is 50-70Hz, the pulse width is 45-55us, and the battery intensity is 35-45 v/m.
Preferably, the electric field frequency is 60Hz, the pulse width is 50us, and the battery intensity is 40 v/m.
Compared with the prior art, the invention has the following beneficial effects:
(1) the invention takes dimethyl sulfoxide and polyether sulfone as main materials to prepare the polyether sulfone ultrafiltration membrane, the activity and the strength performance of the polyether sulfone ultrafiltration membrane are changed by modifying the polyether sulfone, the added nano-cellulose has the performances of high elastic membrane quantity, high strength and the like, and the added cross-linked starch and the nano-cellulose can form a cross-linked network structure, so that the strength performance of the ultrafiltration membrane can be improved in the ultrafiltration membrane, and meanwhile, the added rare earth gadolinium chloride solution can activate the ultrafiltration membrane to enhance the activity of the ultrafiltration membrane after modification treatment, so that the filtering agent is matched, and the treatment effect of wastewater is improved.
(2) The main agent in the filtering agent adopts illite which has the characteristics of no expansion and looseness after being placed in water for a long time, the illite is modified, heat treatment is carried out firstly, then ultraviolet irradiation is carried out, the service life of the illite is prolonged, and sodium pyrophosphate, a silane coupling agent and a modifying liquid are added, so that the illite filtering agent has the capability of being hydrophilic to waste water, and arsenic, lead and the like are removed more easily.
(3) From examples 1-3 and comparative examples 1-2, it is shown that in example 3 of the present invention, the cadmium removal rate can reach 99.9%, the arsenic removal rate can reach 99.9%, and in comparative example 2, the cadmium removal rate is 97.6%, and the arsenic removal rate is 95.2%, and it can be seen that compared with comparative example 2, the cadmium removal rate is increased by 2.3%, and the arsenic removal rate is increased by 4.7%, and the present invention has a certain improvement effect on wastewater treatment.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below with reference to specific embodiments, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
the method for treating the industrial lead smelting wastewater comprises the following steps:
step one, preparing a rare earth filter solution: adding polyether sulfone into dimethyl sulfoxide, stirring at a low speed of 100r/min, stirring until the solution is clear, then adding a rare earth gadolinium chloride solution, then adding nanocellulose, stirring at a medium speed of 450r/min for 30min, then adding crosslinked starch, and continuing stirring at a speed of 1000r/min for 30min to obtain a filter membrane solution;
step two, preparing the rare earth filter membrane: flatly paving the filter membrane liquid in a membrane piece, and then conveying the membrane piece into a vacuum drying oven, wherein the drying temperature is 25 ℃, and the drying time is 18 hours, so as to obtain the rare earth filter membrane;
step three, preparing a filtering agent: firstly, carrying out heat treatment on illite, then carrying out ultraviolet irradiation for 10min with the irradiation power of 100-200W, then sending the illite into a ball mill for ball milling for 1 time until the particle size is 200 meshes, then sending the illite into a magnetic stirrer, then adding sodium pyrophosphate and a silane coupling agent into the illite, starting the stirrer, increasing the rotating speed to 5000r/min, continuing stirring for 20min, then adding a modification solution, and continuing stirring for 1 h;
step four, treating the filtering agent: adding the filtering agent prepared in the third step into the wastewater, stirring at the rotating speed of 200r/min for 20min, standing for 1h, and applying pulse current during standing;
step five: filtering the rare earth filter solution: and (4) slowly flowing the filtrate treated by the filtering agent in the step four into the rare earth filtrate liquid, repeating for 2-3 times, and then obtaining the filtrate.
In the first step of this embodiment, the preparation method of the rare earth gadolinium chloride solution includes calcining the rare earth gadolinium chloride at a high temperature of 500 ℃ for 20min, performing corona treatment, adding the calcined rare earth gadolinium chloride and tetrafluoroborate ions into an acetone solution, adding ammonium chloride, stirring at a rotation speed of 500r/min for 20min, and obtaining the rare earth gadolinium chloride solution after stirring.
The corona treatment power of this example was 10Kw, and the treatment time was 10 min.
The specific steps of the heat treatment in the third step of this embodiment are to raise the temperature to 300 ℃ at a rate of 5 ℃/min, then to keep the temperature for 20min, then to continue to raise the temperature to 650 ℃ at a rate of 1 ℃/min, to continue to keep the temperature for 20min, and finally to lower the temperature to room temperature at a rate of 2 ℃/min.
The modifier of the embodiment comprises the following raw materials in parts by weight: 30 parts of hydroxyl phosphoryl acetic acid, 10 parts of 2-amino-8-naphthol-3, 6-disulfonic acid and 45 parts of 5-10% chitosan acetic acid solution.
The conditions for applying the pulse current in the fourth step of this embodiment are: the frequency of the electric field is 50Hz, the pulse width is 45us, and the battery intensity is 35 v/m.
Example 2:
the method for treating the industrial lead smelting wastewater comprises the following steps:
step one, preparing a rare earth filter solution: adding polyether sulfone into dimethyl sulfoxide, stirring at a low speed of 200r/min, stirring until the solution is clear, then adding a rare earth gadolinium chloride solution, then adding nanocellulose, stirring at a medium speed of 550r/min for 40min, then adding crosslinked starch, and continuously stirring at a speed of 1200r/min for 40min to obtain a filter membrane solution;
step two, preparing the rare earth filter membrane: flatly paving the filter membrane liquid in a membrane piece, and then conveying the membrane piece into a vacuum drying oven, wherein the drying temperature is 35 ℃, and the drying time is 24 hours, so as to obtain the rare earth filter membrane;
step three, preparing a filtering agent: firstly, carrying out heat treatment on illite, then carrying out ultraviolet irradiation for 20min with the irradiation power of 200W, then sending the illite into a ball mill for ball milling for 2 times until the particle size is 500 meshes, then sending the illite into a magnetic stirrer, then adding sodium pyrophosphate and a silane coupling agent into the illite, starting the stirrer, increasing the rotating speed to 700r/min, continuing stirring for 30min, then adding a modification solution, and continuing stirring for 2 h;
step four, treating the filtering agent: adding the filtering agent prepared in the third step into the wastewater, stirring at the rotating speed of 300r/min for 30min, standing for 2h, and applying pulse current during standing;
step five: filtering the rare earth filter solution: and (4) slowly flowing the filtrate treated by the filtering agent in the step four into the rare earth filtrate liquid, repeating for 3 times, and then obtaining the filtrate.
In the first step of this embodiment, the preparation method of the rare earth gadolinium chloride solution includes calcining the rare earth gadolinium chloride at a high temperature of 700 ℃ for 30min, performing corona treatment, adding the calcined rare earth gadolinium chloride and tetrafluoroborate ions into an acetone solution, adding ammonium chloride, stirring at a rotation speed of 900r/min for 30min, and obtaining the rare earth gadolinium chloride solution after stirring.
The corona treatment power of this example was 20Kw and the treatment time was 20 min.
The specific steps of the heat treatment in the third step of this embodiment are to raise the temperature to 300 ℃ at a rate of 5 ℃/min, then to keep the temperature for 30min, then to continue to raise the temperature to 650 ℃ at a rate of 1 ℃/min, to keep the temperature for 30min, and finally to lower the temperature to room temperature at a rate of 2 ℃/min.
The modifier of the embodiment comprises the following raw materials in parts by weight: 60 parts of hydroxyl phosphoryl acetic acid, 20 parts of 2-amino-8-naphthol-3, 6-disulfonic acid and 55 parts of 10% chitosan acetic acid solution.
The conditions for applying the pulse current in the fourth step of this embodiment are: the frequency of the electric field is 70Hz, the pulse width is 55us, and the battery intensity is 45 v/m.
Example 3:
the method for treating the industrial lead smelting wastewater comprises the following steps:
step one, preparing a rare earth filter solution: adding polyether sulfone into dimethyl sulfoxide, stirring at a low speed of 150r/min, stirring until the solution is clear, then adding a rare earth gadolinium chloride solution, then adding nanocellulose, stirring at a medium speed of 500r/min for 35min, then adding crosslinked starch, and continuing stirring at a speed of 1100r/min for 35min to obtain a filter membrane solution;
step two, preparing the rare earth filter membrane: flatly paving the filter membrane liquid in a membrane piece, and then conveying the membrane piece into a vacuum drying oven, wherein the drying temperature is 30 ℃, and the drying time is 21 hours, so as to obtain the rare earth filter membrane;
step three, preparing a filtering agent: firstly, carrying out heat treatment on illite, then carrying out ultraviolet irradiation for 15min with the irradiation power of 150W, then sending the illite into a ball mill for ball milling for 2 times until the particle size is 350 meshes, then sending the illite into a magnetic stirrer, then adding sodium pyrophosphate and a silane coupling agent into the illite, starting the stirrer, increasing the rotating speed to 600r/min, continuing stirring for 25min, then adding a modification solution, and continuing stirring for 1.5 h;
step four, treating the filtering agent: adding the filtering agent prepared in the third step into the wastewater, stirring at the rotating speed of 250r/min for 25min, standing for 1.5h, and applying pulse current during standing;
step five: filtering the rare earth filter solution: and (4) slowly flowing the filtrate treated by the filtering agent in the step four into the rare earth filtrate liquid, repeating for 3 times, and then obtaining the filtrate.
In the first step of this embodiment, the preparation method of the rare earth gadolinium chloride solution includes calcining the rare earth gadolinium chloride at a high temperature of 500-.
The corona treatment power of this example was 15Kw and the treatment time was 15 min.
The specific steps of the heat treatment in the third step of this embodiment are to raise the temperature to 300 ℃ at a rate of 5 ℃/min, then to keep the temperature for 20-30min, then to continue to raise the temperature to 650 ℃ at a rate of 1 ℃/min, to keep the temperature for 20-30min, and finally to lower the temperature to room temperature at a rate of 2 ℃/min.
The modifier of the embodiment comprises the following raw materials in parts by weight: 45 parts of hydroxyl phosphoryl acetic acid, 15 parts of 2-amino-8-naphthol-3, 6-disulfonic acid and 50 parts of 5-10% chitosan acetic acid solution.
The conditions for applying the pulse current in the fourth step of this embodiment are: the frequency of the electric field is 60Hz, the pulse width is 50us, and the battery intensity is 40 v/m.
Comparative example 1.
The materials and preparation process were substantially the same as those of example 3, except that no filtering agent was used.
Comparative example 2.
Basically the same materials and preparation process as those in example 3, except that Chinese patent document CN107352708B discloses the raw materials and method in example 2 of a method for treating lead smelting wastewater.
The results of the performance tests of examples 1 to 3 and comparative examples 1 to 2 are as follows
From examples 1-3 and comparative examples 1-2, it is shown that in example 3 of the present invention, the cadmium removal rate can reach 99.9%, the arsenic removal rate can reach 99.9%, and in comparative example 2, the cadmium removal rate is 97.6%, and the arsenic removal rate is 95.2%, and it can be seen that compared with comparative example 2, the cadmium removal rate is increased by 2.3%, and the arsenic removal rate is increased by 4.7%, and the present invention has a certain improvement effect on wastewater treatment.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (9)
1. The method for treating the industrial lead smelting wastewater is characterized by comprising the following steps of:
step one, preparing a rare earth filter solution: adding polyether sulfone into dimethyl sulfoxide, stirring at a low speed of 100-;
step two, preparing the rare earth filter membrane: flatly paving the filter membrane liquid in a membrane piece, and then conveying the membrane piece into a vacuum drying oven, wherein the drying temperature is 25-35 ℃, and the drying time is 18-24 hours, so as to obtain a rare earth filter membrane;
step three, preparing a filtering agent: firstly, carrying out heat treatment on illite, then carrying out ultraviolet irradiation for 10-20min, wherein the irradiation power is 100-;
step four, treating the filtering agent: adding the filtering agent prepared in the third step into the wastewater, stirring at the rotating speed of 200-300r/min for 20-30min, standing for 1-2h, and applying pulse current during standing;
step five: filtering the rare earth filter solution: and (4) slowly flowing the filtrate treated by the filtering agent in the step four into the rare earth filtrate liquid, repeating for 2-3 times, and then obtaining the filtrate.
2. The method as claimed in claim 1, wherein the preparation method of the gadolinium rare earth chloride solution in the first step comprises the steps of calcining gadolinium rare earth chloride at a high temperature of 500-.
3. The method for treating industrial lead smelting wastewater according to claim 2, wherein the corona treatment power is 10-20Kw, and the treatment time is 10-20 min.
4. The method for treating industrial lead smelting wastewater according to claim 3, wherein the corona treatment power is 15Kw, and the treatment time is 15 min.
5. The method for treating the industrial lead smelting wastewater according to claim 1, wherein the heat treatment in the third step comprises the specific steps of firstly raising the temperature to 300 ℃ at a rate of 5 ℃/min, then preserving the heat for 20-30min, then continuously raising the temperature to 650 ℃ at a rate of 1 ℃/min, continuously preserving the heat for 20-30min, and finally reducing the temperature to room temperature at a rate of 2 ℃/min.
6. The method for treating industrial lead smelting wastewater according to claim 1, wherein the modifier comprises the following raw materials in parts by weight: 30-60 parts of hydroxyl phosphoryl acetic acid, 10-20 parts of 2-amino-8-naphthol-3, 6-disulfonic acid and 45-55 parts of 5-10% chitosan acetic acid solution.
7. The method for treating industrial lead smelting wastewater according to claim 6, wherein the modifier comprises the following raw materials in parts by weight: 45 parts of hydroxyl phosphoryl acetic acid, 15 parts of 2-amino-8-naphthol-3, 6-disulfonic acid and 50 parts of 5-10% chitosan acetic acid solution.
8. The method for treating industrial lead smelting wastewater according to claim 1, wherein the conditions for applying the pulse current in the fourth step are as follows: the frequency of the electric field is 50-70Hz, the pulse width is 45-55us, and the battery intensity is 35-45 v/m.
9. The method for treating industrial lead smelting wastewater according to claim 8, wherein the electric field frequency is 60Hz, the pulse width is 50us, and the battery strength is 40 v/m.
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| WO2021237381A1 (en) * | 2020-05-23 | 2021-12-02 | 海门茂发美术图案设计有限公司 | Method for preparing rare earth-modified polyethersulfone ultrafiltration membrane |
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