CN108905656B - Preparation method and application of grafted poly (sodium polystyrene sulfonate) polysulfone microporous filter membrane - Google Patents
Preparation method and application of grafted poly (sodium polystyrene sulfonate) polysulfone microporous filter membrane Download PDFInfo
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- CN108905656B CN108905656B CN201810764259.1A CN201810764259A CN108905656B CN 108905656 B CN108905656 B CN 108905656B CN 201810764259 A CN201810764259 A CN 201810764259A CN 108905656 B CN108905656 B CN 108905656B
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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
- B01D71/76—Macromolecular material not specifically provided for in a single one of groups B01D71/08 - B01D71/74
- B01D71/78—Graft polymers
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- B01D67/0002—Organic membrane manufacture
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- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
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- B01D67/0006—Organic membrane manufacture by chemical reactions
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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
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
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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
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Abstract
The invention relates to the field of heavy metal ion filtration, adsorption and interception in a water system. Preparation method and application of grafted poly (sodium polystyrene sulfonate) polysulfone microporous filter membrane in ethanol, water and waterN,N‑Adding chloromethylated polysulfone, HEDA and acid-binding agent Na into a mixed solvent of dimethylformamide2CO3Stirring at constant temperature for reaction, and precipitating and drying to obtain a PSF-DEA modified polysulfone membrane; adding PSF-DEA modified polysulfone membrane intoN,N‑Swelling in a mixed solvent of dimethylformamide, ethanol and water, adding a monomer of sodium styrene sulfonate SSS and an initiator Ammonium Persulfate (APS), initiating graft polymerization of the SSS on the surface of polysulfone in a redox initiation system consisting of DEA/APS, and reacting under constant-temperature stirring to obtain the graft polymerization membrane PSF-g-PSSS. The invention also relates to the application of the graft sodium poly (p-styrene sulfonate) polysulfone microporous filter membrane.
Description
Technical Field
The invention relates to the field of heavy metal ion filtration, adsorption and interception in a water system, in particular to preparation and application of a microporous filter membrane for adsorbing and intercepting lead, zinc and mercury ions.
Background
Water pollution caused by heavy metal ions is a serious environmental problem, most of the heavy metal pollution sources are derived from industrial wastewater, and the toxicity and accumulation of heavy metal ions in the water in organs seriously harm human health and the environment. In particular, the uptake of lead causes damage to the kidney, nerves and immune system; zinc is a micronutrient for cell growth and metabolism, but too much zinc can cause damage to the nervous system, kidney disease and cancer; mercury causes brain disease, nerve damage, and disturbances of the renal and endocrine systems. Currently, the removal of these heavy metal ions from water is a serious task. Up to now, chemical precipitation, ion exchange, reverse osmosis, adsorption and the like have been generally used for removing heavy metal pollutants from water. However, these methods have disadvantages, such as high costs, secondary contamination and limited removal rates (Oussama K, C lines P B, Jos E S M, Jos E S M. Separation and Purification Technology, 2017,183: 153). Therefore, it is necessary to develop a material that can be used many times to effectively remove heavy metal ions from water.
Membrane separation technology is one of the most promising methods to remove heavy metal ions from water. Advantages of membrane technology include high efficiency, ease of operation, space saving and environmental friendliness (Mizushima H, Yoshikawa M, Li N, Robertson G P, Guiver M D. European Polymer Journal, 2012, 48: 1717). However, the separation function of macroporous membranes is based on a capture mechanism or on a size exclusion effect. Even nanofiltration membranes smaller than 0.5-2 nm may have larger pore sizes than hydrated ion sizes of metal ions, which will easily pass through membranes (Chitpong N, Husson S M. Journal of Membrane Science, 2017, 523: 418), and commercial pore membranes cannot effectively trap and remove heavy metal ions. Thus, a functional composite Membrane has been obtained by subjecting an existing Membrane to modification work, and a chelate composite Membrane and an ion exchange composite Membrane can be produced (Han K N, Yu B Y, Kwak S Y. Journal of Membrane Science,2012, 396: 83). Such a membrane can effectively trap heavy metal ions by chelation and ion exchange, however, the coupling force between the functional membrane and the support membrane of such a composite membrane is physical, and the stability of the functional membrane is poor. In contrast, grafted functional composite films are preferred, and currently UV irradiation, gamma-ray initiation, low temperature plasma treatment (Chittrakarn T, Tirawanickul Y, Sirijarukul S, Yuenyao C. Surface & Coatings Technology, 2016, 296: 157) are commonly used. These methods are not only complicated, demanding and expensive to operate, but also the substrate membrane is often damaged to some extent during installation, especially in membranes prepared by high energy radiation.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: how to provide a preparation method of a microporous filter membrane which has simple preparation process and high interception capability to heavy metal ions.
The technical scheme adopted by the invention is as follows: a preparation method of a grafted poly (sodium polystyrene sulfonate) polysulfone microporous filter membrane comprises the following steps
Step one, in ethanol, water andN,N-adding chloromethylated polysulfone (CMPSF) into a mixed solvent of dimethylformamide for swelling, and then adding HDEA and an acid-binding agent Na2CO3，N2Under protection, stirring and reacting at constant temperature, alternately washing the precipitate with ethanol and distilled water, and drying the precipitate to constant weight to obtain a PSF-DEA modified polysulfone membrane;
step two, adding the PSF-DEA modified polysulfone membrane intoN,N-Swelling in a mixed solvent of dimethylformamide, ethanol and water, adding a monomer of sodium styrene sulfonate SSS and an initiator Ammonium Persulfate (APS), initiating graft polymerization of the SSS on the surface of polysulfone in a redox initiation system consisting of DEA/APS, and reacting under constant-temperature stirring to obtain the graft polymerization membrane PSF-g-PSSS.
As a preferred mode: in the first step, ethanol, water and water are addedN,N-Mixed solvent of dimethyl formamide, ethanol, water andN,N-the volume ratio of the dimethyl formamide is 1:1:2, and each 60mL of ethanol, water and waterN,N-The amount of chloromethylated polysulfone (CMPSF) added to the mixed solvent of dimethylformamide was 0.1g, the amount of HDEA added was 0.132g, and Na was added2CO3Is added in an amount of0.127g。
As a preferred mode: in the first step, in ethanol, water andN,N-chloromethyl polysulphone (CMPSF) is added into a mixed solvent of dimethyl formamide to swell for 2 hours, the constant-temperature stirring reaction refers to stirring at the temperature of 80 ℃ for 6 hours, and the precipitate is dried to constant weight and is carried out in vacuum.
As a preferred mode: in the second step, the first step is carried out,N,N-in a mixed solvent of dimethylformamide, ethanol and water,N,N-dimethylformamide, ethanol and water in a volume ratio of 3:1:1, and 0.1g of PSF-DEA modified polysulfone membrane was addedN,N-The amount of a mixed solvent of dimethylformamide, ethanol and water is 75mL, the amount of sodium styrene sulfonate SSS added is 7-11 g, the amount of initiator ammonium persulfate APS added is 0.21-0.33 g, and the reaction is carried out under constant-temperature stirring for 8-12 h at the temperature of 45-60 ℃.
An application of graft poly (sodium p-styrene sulfonate) polysulfone microporous filter membrane in heavy ion adsorption and interception.
As a preferred mode: the graft poly (sodium p-styrenesulfonate) polysulfone microporous filter membrane is used for determining the Pb content by adopting an adsorption method and a permeation method2 +Ions, Zn2+Ions and Hg2+Adsorption and rejection properties of ions.
The invention has the beneficial effects that: (1) the polysulfone microfiltration membrane is taken as a base membrane, and the grafted microfiltration membrane PSF-g-PSSS is taken as a functional membrane for adsorbing and intercepting heavy metal ions. The grafted microporous filter membrane prepared by the method can keep high water flow and can efficiently adsorb heavy metal ions so as to realize interception of the heavy metal ions. The grafted microporous filter membrane prepared by the method is used for treating Pb2 +Ions, Zn2+Ions and Hg2+The adsorption capacity of the ions can reach 2.18 mu mol/cm2, 1.62μmol/cm2And 0.66. mu. mol/cm2 ；Pb2 +Ions, Zn2+Ions and Hg2+Ion concentration of 0.2 mmol/L, passing through 4 cm2The grafted microporous filter membrane PSF-g-PSSS is 0-45 ml, and the rejection rate of the grafted membrane to heavy metal ions is almost 100%. (2) The preparation process of the invention takes the polysulfone membrane as a substrate membrane,the polysulfone membrane has good chemical stability, thermal stability and mechanical property, and is suitable for the requirement of industrial production. The preparation process is simple, the cost is low, and the control is easy. (3) The invention constructs an initiating system in a substrate membrane and a solution, and initiates functional monomers to graft and polymerize onto a substrate under mild conditions to prepare the high-performance graft polymerization membrane. Aromatic tertiary amine on a polysulfone membrane (PSF) and ammonium persulfate in the solution form a redox initiation system to initiate monomer Sodium Styrene Sulfonate (SSS) to graft and polymerize on the surface of the polysulfone membrane to form a novel graft functional polymerization composite membrane, PSF-g-PSSS. The preparation method is simple, easy to operate, mild in condition, good in membrane stability and strong in adsorption and interception capacity on heavy metal ions.
Detailed Description
Example 1:
in a four-necked flask, 60mL of ethanol, water andN,N-0.1g of chloromethylated polysulfone (CMPSF) is added into a mixed solvent of dimethylformamide (volume ratio is 1:1: 2) to swell for 2 hours, and then 0.132g of HDEA and 0.127g of acid-binding agent Na are added2CO3，N2Stirring at 80 ℃ under the protection of the solution, reacting for 6 hours at constant temperature, precipitating by using ethanol and distilled water, and alternately washing the precipitate to obtain the PSF-DEA modified polysulfone membrane. 0.1g of PSF-DEA-modified polysulfone membrane was added to 75mLN,N-Swelling in a mixed solvent of dimethylformamide, ethanol and water (volume ratio is 3:1: 1) for 2h, adding 9 g of monomer Sodium Styrene Sulfonate (SSS) and 0.27 g of initiator ammonium persulfate, initiating graft polymerization of SSS on the surface of polysulfone in a redox initiation system consisting of DEA/APS, and reacting at constant temperature of 55 ℃ for 10 h under stirring to obtain a graft polymerization membrane PSF-g-PSSS with the grafting degree of 1.45mg/cm2. Pb at a concentration of 0.2 mmol/L, pH of 5.02 +Ionic, pH 5.5 Zn2+Ions and Hg at pH 2.02+Ions permeate through 4 cm each2When the grafted microporous filter membrane PSF-g-PSSS is used, the flow is within the range of 0-45 ml, the rejection rate of the grafted membrane to heavy metal ions is almost 100%, and the rejection rate is about 95% within the range of 70 ml.
Example 2
In a four-mouth bottle, 60ml of ethanol, water andN,N-two-agent0.1g of chloromethylated polysulfone (CMPSF) is added into a mixed solvent of the formamide (the volume ratio is 1:1: 2) to swell for 2 hours, and then 0.132g of HDEA and 0.127g of acid-binding agent Na are added2CO3，N2Stirring at 80 ℃ under the protection of the solution, reacting for 6 hours at constant temperature, precipitating by using ethanol and distilled water, and alternately washing the precipitate to obtain the PSF-DEA modified polysulfone membrane. 0.1g of PSF-DEA-modified polysulfone membrane was added to 75mLN,N-Swelling in a mixed solvent of dimethylformamide, ethanol and water (volume ratio is 3:1: 1) for 2h, adding 7g of monomer Sodium Styrene Sulfonate (SSS) and 0.21 g of initiator ammonium persulfate, initiating graft polymerization of SSS on the surface of polysulfone in a redox initiation system consisting of DEA/APS, and reacting at constant temperature for 8 h under stirring at 60 ℃ to obtain a graft polymerization membrane PSF-g-PSSS with the grafting degree of 0.8 mg/cm2. Pb at a concentration of 0.2 mmol/L, pH of 5.02 +Ionic, pH 5.5 Zn2+Ions and Hg at pH 2.02+Ions permeate through 4 cm each2When the grafted microporous filter membrane PSF-g-PSSS is used, the flow is within the range of 0-45 ml, the rejection rate of the grafted membrane to heavy metal ions is almost 100%, and the rejection rate is about 95% within the range of 70 ml.
Example 3
In a four-mouth bottle, 60ml of ethanol, water andN,N-adding chloromethylated polysulfone (CMPSF) into a mixed solvent of dimethylformamide (volume ratio =1:1: 2) to swell for 2h, 0.132g HDEA and 0.127g acid-binding agent Na2CO3，N2Under protection, stirring and reacting at constant temperature of 80 ℃ for 6 h, precipitating by using ethanol and distilled water and alternately washing to prepare the PSF-DEA modified polysulfone membrane. 0.1g of PSF-DEA-modified polysulfone membrane was added to 75mLN,N-Swelling in a mixed solvent of dimethylformamide, ethanol and water (volume ratio =3:1: 1) for 2h, adding 11g of monomer Sodium Styrene Sulfonate (SSS) and 0.33 g of initiator ammonium persulfate, initiating graft polymerization of SSS on the surface of polysulfone in a redox initiation system consisting of DEA/APS, and reacting at constant temperature of 45 ℃ for 12h under stirring to obtain a graft polymerization membrane PSF-g-PSSS with the grafting degree of 1.2 mg/cm2. Pb at a concentration of 0.2 mmol/L, pH of 5.02 +Ionic, pH 5.5 Zn2+Ions and Hg at pH 2.02+Ions permeate through 4 cm each2When the grafted microporous filter membrane PSF-g-PSSS is used, the flow is within the range of 0-45 ml, the rejection rate of the grafted membrane to heavy metal ions is almost 100%, and the rejection rate is about 95% within the range of 70 ml.
Example 4
In a four-mouth bottle, 60ml of ethanol, water andN,N-0.1g of chloromethylated polysulfone (CMPSF) was added to a mixed solvent of dimethylformamide (volume ratio =1:1: 2) to swell for 2 hours, and then 0.132g of HDEA and 0.127g of acid-binding agent Na were added2CO3，N2Under protection, stirring and reacting at constant temperature of 80 ℃ for 6 h, precipitating by using ethanol and distilled water and alternately washing to prepare the PSF-DEA modified polysulfone membrane. 0.1g of PSF-DEA-modified polysulfone membrane was added to 75mLN,N-Swelling in a mixed solvent of dimethylformamide, ethanol and water (volume ratio =3:1: 1) for 2h, adding 8 g of monomer Sodium Styrene Sulfonate (SSS) and 0.24 g of initiator ammonium persulfate, forming a redox initiation system by DEA/APS to initiate graft polymerization of SSS on the surface of polysulfone, and reacting at constant temperature for 9 h under stirring at 55 ℃ to obtain a graft polymerization membrane PSF-g-PSSS with the grafting degree of 1.1 mg/cm2. Pb at a concentration of 0.2 mmol/L, pH of 5.02 +Ionic, pH 5.5 Zn2+Ions and Hg at pH 2.02+Ions permeate through 4 cm each2When the grafted microporous filter membrane PSF-g-PSSS is used, the flow is within the range of 0-45 ml, the rejection rate of the grafted membrane to heavy metal ions is almost 100%, and the rejection rate is about 95% within the range of 70 ml.
Example 5
In a four-mouth bottle, 60ml of ethanol, water andN,N-adding chloromethylated polysulfone (CMPSF) into a mixed solvent of dimethylformamide (volume ratio =1:1: 2) to swell for 2h, 0.132g HDEA and 0.127g acid-binding agent Na2CO3，N2Under protection, stirring and reacting at constant temperature of 80 ℃ for 6 h, precipitating by using ethanol and distilled water and alternately washing to prepare the PSF-DEA modified polysulfone membrane. 0.1g of PSF-DEA-modified polysulfone membrane was added to 75mLN,N-Swelling in a mixed solvent of dimethylformamide, ethanol and water (volume ratio =3:1: 1) for 2h, adding 10 g of monomer Sodium Styrene Sulfonate (SSS) and 0.3 g of initiator ammonium persulfate, and introducing into a redox initiation system composed of DEA/APSGraft polymerization of the SSS on the surface of polysulfone, and constant temperature reaction for 8 h at 45 ℃ under stirring to obtain a graft polymerization membrane PSF-g-PSSS with the grafting degree of 0.9 mg/cm2. Pb at a concentration of 0.2 mmol/L, pH of 5.02 +Ionic, pH 5.5 Zn2+Ions and Hg at pH 2.02+Ions permeate through 4 cm each2When the grafted microporous filter membrane PSF-g-PSSS is used, the flow is within the range of 0-45 ml, the rejection rate of the grafted membrane to heavy metal ions is almost 100%, and the rejection rate is about 95% within the range of 70 ml.
Claims (6)
1. A preparation method of a grafted poly (sodium polystyrene sulfonate) polysulfone microporous filter membrane is characterized by comprising the following steps: the method comprises the following steps
Step one, in ethanol, water andN,N-adding chloromethylated polysulfone CMPSF into a mixed solvent of dimethylformamide for swelling, and then adding HDEA and an acid-binding agent Na2CO3，N2Under protection, stirring and reacting at constant temperature, alternately washing the precipitate with ethanol and distilled water, and drying the precipitate to constant weight to obtain a PSF-DEA modified polysulfone membrane;
step two, adding the PSF-DEA modified polysulfone membrane intoN,N-Swelling in a mixed solvent of dimethylformamide, ethanol and water, adding a monomer of sodium styrene sulfonate SSS and an initiator of ammonium persulfate APS, initiating graft polymerization of the SSS on the surface of polysulfone in a redox initiation system consisting of DEA/APS, and reacting under constant-temperature stirring to obtain the graft polymerization membrane PSF-g-PSSS.
2. The preparation method of the grafted poly (sodium p-styrenesulfonate) (polysulfone) microporous filtration membrane according to claim 1, wherein the preparation method comprises the following steps: in the first step, ethanol, water and water are addedN,N-Mixed solvent of dimethyl formamide, ethanol, water andN,N-the volume ratio of the dimethyl formamide is 1:1:2, and each 60mL of ethanol, water and waterN,N-The addition amount of chloromethylated polysulfone CMPSF in the mixed solvent of dimethylformamide is 0.1g, the addition amount of HDEA is 0.132g, and Na2CO3The amount added was 0.127 g.
3. According to the claimsThe preparation method of the grafted poly (p-styrene sulfonate) polysulfone microporous filter membrane in claim 1 is characterized by comprising the following steps: in the first step, in ethanol, water andN,N-adding chloromethylated polysulfone CMPSF into a mixed solvent of dimethylformamide to swell for 2h, wherein the constant-temperature stirring reaction refers to stirring at 80 ℃ for 6 h, drying the precipitate to constant weight, and performing in vacuum.
4. The preparation method of the grafted poly (sodium p-styrenesulfonate) (polysulfone) microporous filtration membrane according to claim 1, wherein the preparation method comprises the following steps: in the second step, the first step is carried out,N,N-in a mixed solvent of dimethylformamide, ethanol and water,N,N-dimethylformamide, ethanol and water in a volume ratio of 3:1:1, and 0.1g of PSF-DEA modified polysulfone membrane was addedN,N-The amount of a mixed solvent of dimethylformamide, ethanol and water is 75mL, the amount of sodium styrene sulfonate SSS added is 7-11 g, the amount of initiator ammonium persulfate APS added is 0.21-0.33 g, and the reaction is carried out under constant-temperature stirring for 8-12 h at the temperature of 45-60 ℃.
5. The application of the grafted sodium polyterephnylsulfonate polysulfone microporous filter membrane prepared by the preparation method of the grafted sodium polyterephnylsulfonate polysulfone microporous filter membrane in claim 1 is characterized in that: the application of the graft poly (sodium p-styrenesulfonate) polysulfone microporous filter membrane in heavy ion adsorption and interception.
6. The use of the grafted polysulfones microporous membrane as claimed in claim 5, wherein: the graft poly (sodium p-styrenesulfonate) polysulfone microporous filter membrane is used for determining the Pb content by adopting an adsorption method and a permeation method2 +Ions, Zn2+Ions and Hg2+Adsorption and rejection properties of ions.
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