CN110963547A - Preparation method of hollow fiber membrane for removing heavy metals from industrial wastewater - Google Patents
Preparation method of hollow fiber membrane for removing heavy metals from industrial wastewater Download PDFInfo
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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
- C02F1/42—Treatment of water, waste water, or sewage by ion-exchange
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J47/00—Ion-exchange processes in general; Apparatus therefor
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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
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
- C02F2101/22—Chromium or chromium compounds, e.g. chromates
Abstract
The invention discloses a preparation method of a hollow fiber membrane for removing heavy metals from industrial wastewater. The method comprises the steps of grinding ion exchange resins such as D314, D405 and amino phosphonic acid LSC-500 to 300 meshes and 500 meshes, blending with a membrane casting solution of the membrane material, and spinning by a phase inversion method to obtain the hollow fiber membrane material with the function of removing heavy metals. Compared with other materials for removing heavy metals, the method combines the ion exchange technology and the membrane technology, combines the characteristics of high selectivity, high adsorptivity, high reproducibility and the like of the ion exchange material with the characteristics of high specific surface area, high separation efficiency and the like of the membrane material, and the prepared hollow fiber membrane can specifically adsorb and separate heavy metals such as Cr, Hg, Pb and the like in water, and can play an important role in removing the heavy metals in industrial wastewater.
Description
Technical Field
The invention belongs to the field of membrane materials for water treatment, and particularly relates to a preparation method of a hollow fiber membrane for removing heavy metals in industrial wastewater.
Background
In recent years, with the development of economy, the living standard of people is remarkably improved. However, the pollution problem is particularly obvious, especially the heavy metal pollution and overproof problem in the water environment are more and more serious, and immeasurable harm and damage are caused to ecological environment systems such as rivers, lakes, even oceans and the like. Heavy metal ions are highly toxic and non-degradable, and stay through food chains and accumulate in animals and plants, causing irreversible damage. Heavy metal pollutants are numerous, and a few common water body heavy metal pollutants which are harmful to water bodies are introduced below.
Among the numerous heavy metal pollution sources, chromium (Cr) is considered as one of the most toxic heavy metals, and therefore, the treatment of heavy metal pollutants in water is an important problem to be solved urgently, especially the removal of Cr and its compounds.
Cr and its compounds are used in various fields of production, including metallurgy, tanning, printing and dyeing, paints, pharmaceuticals, pigments, etc. Cr compounds mainly exist in the forms of Cr (III) and Cr (VI), and the toxicity of Cr (VI) is the strongest among compounds with different valence states, wherein the toxicity of Cr (VI) is more than 100 times that of Cr (III), and the Cr (VI) has strong oxidizing property and high permeability, excessive intake of Cr (VI) can cause damage to liver and kidney, generate spasm and generate carcinogenesis and mutagenesis effects on human bodies, and Cr (III) has higher toxicity than Cr (VI) for fishes, so the Cr (VI) is also important for removing water bodies of Cr (III). Cr (VI) is one of carcinogen metal substances recognized by the international center for anticancer research and the U.S. toxicological organization and is also one of key pollutants recognized by the U.S. environmental protection agency in 129. When the Cr (VI) content in the water is 1mg/L, the growth of crops can be stimulated, the chromium content is 1-10mg, the crops grow slowly, and when the chromium content exceeds 100mg/L, the growth is stopped and the crops are in a state of dying.
Mercury (Hg), the most toxic and polluting accumulating heavy metal pollutant in water+And Hg2 +Many organic and inorganic compounds can form in the environment. Hg is a mercury vapor2+The compounds are generally water soluble. Inorganic mercury can be converted into organic mercury (methyl mercury or alkyl mercury) with stronger toxicity after entering water, which causes brain damage, causes water guarantee and seriously harms human health.
Lead (Pb) is a toxic heavy metal which is extremely harmful to human bodies, a small part of metal lead is discharged out of the bodies along with the metabolism of the bodies after entering the human bodies, and the rest of metal lead is deposited in the bodies, so that the lead and compounds thereof can cause harm to a plurality of systems such as nerves, hematopoiesis, digestion, kidneys, cardiovascular and endocrine after entering the human bodies, and lead poisoning can be caused if the content of the lead is too high. The toxicity of lead to living bodies is mainly shown in the following aspects: leading to hyperactivity and growth retardation of infants and children; causing kidney damage, neurological disorder, intellectual disturbance, cancer, etc. in the middle aged and the elderly. If the water containing lead exceeding the standard is drunk for a long time, abortion, fetal deformity and the like of pregnant women can be caused.
At present, methods for removing heavy metals mainly include chemical precipitation, ion exchange, biological, adsorption, coagulation and precipitation methods, and the like. However, these methods have certain limitations in the application process. Such as: the content of the heavy metal remained after the heavy metal containing the complexing agent is treated by a chemical precipitation method is far beyond the standard; the ion exchange resin has different specific surface area, surface groups and different pore diameters and porosity, so that the selectivity, the adsorption capacity and the regeneration performance of the material are instable, and the satisfactory effect is difficult to achieve.
As a novel separation technology, the membrane separation technology has the characteristics of simple and convenient operation, high separation efficiency, low energy consumption, environmental protection, easy amplification and the like and is widely applied to the water treatment industry. However, the membrane separation material, whether the microfiltration, ultrafiltration, nanofiltration or reverse osmosis membrane separation process, mainly screens ions depending on the size of the membrane pore size, has poor selectivity, and is difficult to effectively separate or remove heavy metals and compounds thereof.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention aims to provide a preparation method of a hollow fiber membrane for removing heavy metals in industrial wastewater.
In order to achieve the purpose of the invention, the following technical scheme is provided.
A method for preparing a hollow fiber membrane for removing heavy metals from industrial wastewater comprises the steps of grinding ion exchange resin such as D314, D405 and amino phosphonic acid LSC-500 to 300 meshes and 500 meshes, blending with a membrane casting solution of a membrane material, and spinning by a phase inversion method to obtain the hollow fiber membrane material with the function of removing the heavy metals from a water body.
The ion exchange resin such as D314, D405 and LSC-500 is the ion exchange resin material existing in the field, and the adsorption mechanism of the ion exchange resin material is realized by a special functional group contained in the resin, such as R-N (CH) contained in D3143)2+The structure, the-SH structure contained in D405 has a special coordination ability, and the aminophosphonic acid resin contains coordination atoms such as N and O. Grinding the ion exchange resin to 300-500 meshes to meet the stability and uniformity of the resin in the membrane casting solution and prevent the resin from settling in the membrane casting solution and separating phases.
A preparation method of a hollow fiber membrane for removing heavy metals from industrial wastewater comprises the following steps:
a. grinding commercially purchased ion exchange resin to a particle size of 300-500 mesh;
b. adding 20-30% of polymer material A, 5-15% of polyvinylpyrrolidone, 0.1-10% of ion exchange resin with the size of 300-500 meshes in the step a and 60-70% of organic solvent according to mass percent, uniformly mixing, stirring for 10-24h at the temperature of 60-80 ℃, standing and defoaming at room temperature to obtain a membrane casting solution; the polymer material A is polysulfone, polyethersulfone or polyvinylidene fluoride with the molecular weight of 10000-100000;
c. passing the casting solution obtained in the step (2) through a stainless steel spinning nozzle by a hollow fiber membrane preparation device, wherein the inner diameter of the spinning nozzle is 0.1-2 mm; the feeding speed is controlled to be 0.1-5 ml/min; the distance between the spinning nozzle and the coagulating bath is 1-20 cm; the solution in the coagulating bath is water, alcohol compound or the mixture; the winding speed of the winding device is 0.5-20/min, the mixed membrane casting solution is spun into membrane filaments by a phase inversion method, and the spinning process is carried out in a room temperature environment;
d. and (3) soaking the hollow fiber membrane filaments prepared in the step (3) in deionized water for more than 24 hours for removing residual organic solvents in the membrane materials, soaking in 30-80 wt% of glycerol aqueous solution for 10 hours, airing at room temperature, and storing.
The commercially available ion exchange resins are D314, D405, aminophosphonic acid LSC-500.
The average molecular weight of polyvinylpyrrolidone in the membrane casting solution is 1000-150000; the organic solvent is N, N-dimethylacetamide or N-methylpyrrolidone.
The invention has the following beneficial effects:
the invention adopts a blending mode, combines the resin for efficiently removing heavy metal with the membrane material to prepare the hollow fiber membrane material, and enhances the adsorption performance of heavy metal in water. The method is simple, low in cost, suitable for large-scale purification of wastewater industry and easy to operate. According to the technology, the hollow fiber membrane material is introduced, so that the specific surface area of the traditional ion exchange resin material is increased, the contact area of the wastewater and the resin material for removing the heavy metals is increased, the adsorption kinetic reaction of the resin material is accelerated, the balance time for removing the heavy metals is reduced, and the working efficiency is improved. The hollow fiber membrane prepared by the technology is easy to clean, has stable regeneration performance, and has good application prospect in industrial heavy metal removal wastewater.
Compared with other heavy metal removal technologies, the technology combines the ion exchange technology with the membrane technology, namely combines the characteristics of high selectivity, high adsorptivity, high reproducibility and the like of the ion exchange resin and the characteristics of high specific surface area, high separation efficiency and the like of the membrane material to prepare the heavy metal removal hollow fiber membrane, so that the heavy metal removal hollow fiber membrane has the characteristics of targeted adsorption and separation on heavy metal ions such as Cr, Hg, Pb and the like in water and plays an important role in removing heavy metals from industrial wastewater.
Drawings
FIG. 1 is an SEM front view of a hollow fiber membrane for removing heavy metals from industrial wastewater prepared in example 1;
FIG. 2 is a SEM sectional view of a hollow fiber membrane for removing heavy metals from industrial wastewater prepared in example 2;
FIG. 3 is a graph showing the regeneration performance of a hollow fiber membrane for removing heavy metals from industrial wastewater obtained in example 3.
Detailed Description
The present invention will be described in detail with reference to specific embodiments. Wherein the following description is merely exemplary in nature and is in no way intended to limit the scope of the invention, its application, or uses.
In the following examples:
the hollow fiber membrane for removing heavy metals from industrial wastewater prepared in the example was tested as follows:
and (3) testing the surface hydrophilicity of the hollow fiber membrane, and characterizing the surface hydrophilicity of the chromium-removed hollow fiber membrane by using a dynamic water contact angle tester DSA 100. Wherein, for the hydrophilic characterization, the smaller the water contact angle is, the better the wetting property of the hollow fiber membrane is.
Testing the surface and section morphology of the hollow fiber membrane by using a field emission Scanning Electron Microscope (SEM) Hitachi S-4800;
the water flux performance of the hollow fiber membrane is tested by utilizing the conventional hollow fiber membrane testing device. Where water flux is defined as the volume of water that permeates a unit area of membrane per unit time. The water flux test conditions of the hollow fiber membrane are as follows: the test pressure was 0.1MPa, the temperature was controlled at room temperature, and the flux change value of the hollow fiber membrane was calculated according to the formula F ═ V/(a ﹡ t).
The regeneration performance of the hollow fiber membrane for removing heavy metals is subjected to adsorption and desorption processes according to different existing forms of chromium in a solution. For example:
1. regeneration of hollow fiber membrane for removing chromium
Under acidic condition, Cr (VI) is mainly Cr2O7 2-In the form of Cr (VI) and at neutral or low concentrations, Cr (VI) is predominantly present as Cr2O4 2-Form exists and adsorption is carried out:
CrO4 2-+R2SO4→R2CrO4+SO4 2-
Cr2O7 2-+R2SO4→R2Cr2O7+SO4 2-
when the chromium adsorption of the hollow fiber membrane is saturated, 0.1mol of NaOH can be used for regeneration, and the regeneration reaction can be expressed as:
2R-N(CH3)2Cr2O7+2NaOH→2R-N(CH3)2OH+Na2Cr2O7
the ion exchange resin in the regenerated hollow fiber membrane is in an OH type and needs to be further transformed into R-SO4In a form that contributes to an increase in the adsorption capacity for chromium.
2. Mercury removal hollow fiber membrane regeneration
The hollow fiber membrane adsorbs mercury at a low acidity and desorbs mercury at a high acidity
3. Lead-removing hollow fiber membrane
The LSC-500 resin belongs to cation chelating resin, and hydrochloric acid or EDTA can be selected for eluting the hollow fiber membrane.
Wherein the heavy metal adsorption capacity q (mg/g) is according to the formula q ═ C0-Ce)V/mM；
The regeneration efficiency formula (RE) of the hollow fiber membrane is:
RE＝q2/q1*100％
wherein q1 and q2 are the first adsorption capacity and the adsorption capacity after regeneration of the hollow fiber membrane, respectively.
Example 1
A hollow fiber membrane for removing heavy metals from industrial wastewater comprises the following steps:
1. grinding commercially available D314 resin to a particle size of 300 mesh;
2. adding 20% of polysulfone material with the molecular weight of 10000, 10% of polyvinylpyrrolidone, 10% of D314 resin with the size of 300 meshes and 60% of N, N-dimethylacetamide according to the mass percent, uniformly mixing, stirring for 10 hours at 60 ℃, standing and defoaming at room temperature to obtain a casting solution;
3. passing the casting solution obtained in the step 2 through a stainless steel spinning nozzle by a hollow fiber membrane preparation device, wherein the inner diameter of the spinning nozzle is 0.8 mm; the feeding speed is controlled to be 1.5 mL/min; the distance between the spinning nozzle and the coagulating bath is 5 cm; the solution in the coagulating bath is; the winding speed of the winding device is 5m/min, the mixed membrane casting solution is spun into membrane filaments by a phase inversion method, and the spinning process is carried out in a room temperature environment;
4. and (3) soaking the hollow fiber membrane filaments prepared in the step (3) in deionized water for more than 24 hours for removing residual organic solvents in the membrane materials, soaking in a glycerol water solution with the mass fraction of 50 wt% for 10 hours, airing at room temperature, and storing.
The structure and the chromium removal performance of the chromium removal hollow fiber membrane prepared in the example 1 were measured as follows:
1. structural observation is carried out on the SEM front side and the section of the chromium-removing hollow fiber membrane: the front view can clearly find that the D314 resin is uniformly dispersed in the hollow fiber membrane; the cross section shows that the original structure of the hollow fiber membrane is not changed by the D314 resin added in the hollow fiber membrane.
2. The water contact angle of the chromium-removing hollow fiber membrane is 50 degrees, and the pure water flux value of the chromium-removing hollow fiber membrane is 530L/m2h。
3. The adsorption capacity of the chromium-removing hollow fiber membrane to chromium is 210 mg/g.
4. After the chromium-removing hollow fiber membrane is circulated for 100 times, the regeneration rate is 98.3 percent.
Example 2
A preparation method of a mercury-removing hollow fiber membrane comprises the following steps:
1. grinding commercially available D405 resin to a particle size of 500 mesh;
2. adding 25% of polyether sulfone with the molecular weight of 10000, 5% of polyvinylpyrrolidone, 10% of D405 resin with the size of 500 meshes and 60% of N-methyl pyrrolidone according to the mass percentage, uniformly mixing, stirring for 10 hours at the temperature of 60 ℃, standing and defoaming at room temperature to obtain a casting solution;
3. passing the casting solution obtained in the step (2) through a stainless steel spinning nozzle by a hollow fiber membrane preparation device, wherein the inner diameter of the spinning nozzle is 1.2 mm; the feeding speed is controlled to be 2.0 mL/min; the distance between the spinning nozzle and the coagulating bath is 3 cm; the solution in the coagulating bath is; the winding speed of the winding device is 4m/min, the mixed membrane casting solution is spun into membrane filaments by a phase inversion method, and the spinning process is carried out in a room temperature environment;
4. and (3) soaking the hollow fiber membrane filaments prepared in the step (3) in deionized water for more than 24 hours for removing residual organic solvents in the membrane materials, soaking in 60 wt% glycerol water solution for 10 hours, airing at room temperature, and storing.
The structure and mercury removal performance of the mercury removal hollow fiber membrane prepared in this example 2 were tested as follows:
1. in the SEM image of the mercury-removing hollow fiber membrane, the D405 resin is uniformly dispersed in the membrane, as shown in FIG. 2.
2. The water contact angle of the mercury-removing hollow fiber membrane is 55 degrees, and the pure water flux value of the mercury-removing hollow fiber membrane is 521L/m2h。
3. The adsorption capacity of the mercury-removing hollow fiber membrane to chromium is 560 mg/g.
4. After 100 cycles, the regeneration rate of the mercury-removing hollow fiber membrane is 98.9%.
Example 3
A preparation method of a lead-removing hollow fiber membrane comprises the following steps:
1. grinding commercially available LSC-500 resin to a particle size of 500 mesh;
2. adding 23 mass percent of polysulfone material with the molecular weight of 10000, 7 mass percent of polyvinylpyrrolidone, 10 mass percent of LSC-500 resin with the size of 500 meshes and 60 mass percent of N, N-dimethylacetamide, uniformly mixing, stirring for 10 hours at 60 ℃, standing and defoaming at room temperature to obtain a casting solution;
3. passing the casting solution obtained in the step 2 through a stainless steel spinning nozzle by a hollow fiber membrane preparation device, wherein the inner diameter of the spinning nozzle is 1.1 mm; the feeding speed is controlled to be 2.3 mL/min; the distance between the spinning nozzle and the coagulating bath is 6 cm; the solution in the coagulating bath is; the winding speed of the winding device is 5.5m/min, the mixed membrane casting solution is spun into membrane filaments by a phase inversion method, and the spinning process is carried out in a room temperature environment;
4. and (3) soaking the hollow fiber membrane filaments prepared in the step (3) in deionized water for more than 24 hours for removing residual organic solvents in the membrane materials, soaking in a glycerol water solution with the mass fraction of 50 wt% for 10 hours, airing at room temperature, and storing.
The structure and the lead removal performance of the lead removal hollow fiber membrane prepared in the embodiment 3 are detected as follows:
1. the LSC-500 resin is found to exist and be uniformly distributed in the membrane in the SEM picture of the lead-removing hollow fiber membrane.
2. The water contact angle of the lead-removing hollow fiber membrane is 62 degrees, and the pure water flux value is 533L/m2h。
3. The adsorption capacity of the lead-removing hollow fiber membrane to chromium is 850 mg/g.
4. After 100 cycles, the regeneration rate of the lead-removing hollow fiber membrane is 99.1%, as shown in fig. 3.
Claims (3)
1. A preparation method of a hollow fiber membrane for removing heavy metals in industrial wastewater is characterized by comprising the following steps: the method comprises the following steps:
a. grinding commercially purchased ion exchange resin to a particle size of 300-500 mesh;
b. adding 20-30% of polymer material A, 5-15% of polyvinylpyrrolidone, 0.1-10% of ion exchange resin with the size of 300-500 meshes in the step a and 60-70% of organic solvent according to mass percent, uniformly mixing, stirring for 10-24h at the temperature of 60-80 ℃, standing and defoaming at room temperature to obtain a membrane casting solution; the polymer material A is polysulfone, polyethersulfone or polyvinylidene fluoride with the molecular weight of 10000-100000;
c. passing the casting solution obtained in the step (2) through a stainless steel spinning nozzle by a hollow fiber membrane preparation device, wherein the inner diameter of the spinning nozzle is 0.1-2 mm; the feeding speed is controlled to be 0.1-5 ml/min; the distance between the spinning nozzle and the coagulating bath is 1-20 cm; the solution in the coagulating bath is water, alcohol compound or the mixture; the winding speed of the winding device is 0.5-20/min, the mixed membrane casting solution is spun into membrane filaments by a phase inversion method, and the spinning process is carried out in a room temperature environment;
d. and (3) soaking the hollow fiber membrane filaments prepared in the step (3) in deionized water for more than 24 hours for removing residual organic solvents in the membrane materials, soaking in 30-80 wt% of glycerol aqueous solution for 10 hours, airing at room temperature, and storing.
2. The method for preparing the hollow fiber membrane for removing heavy metals from industrial wastewater according to claim 1, wherein the method comprises the following steps: the commercially available ion exchange resins are D314, D405, aminophosphonic acid LSC-500.
3. The method for preparing the hollow fiber membrane for removing heavy metals from industrial wastewater according to claim 1, wherein the method comprises the following steps: the average molecular weight of polyvinylpyrrolidone in the membrane casting solution is 1000-150000; the organic solvent is N, N-dimethylacetamide or N-methylpyrrolidone.
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Application publication date: 20200407 |