CN115838492A - Super-hydrophilic polyphenylene sulfide composite membrane and preparation method thereof - Google Patents
Super-hydrophilic polyphenylene sulfide composite membrane and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a super-hydrophilic polyphenylene sulfide composite membrane and a preparation method thereof, wherein the super-hydrophilic polyphenylene sulfide composite membrane comprises the following components in parts by weight: 50-150 parts of polyphenylene sulfide, 30-90 parts of benzophenone, 20-80 parts of catechol, 10-30 parts of polyethyleneimine, 130-390 parts of dibutyl phthalate, 10-60 parts of tris (hydroxymethyl) aminomethane and 5-30 parts of gamma-glycidyl ether oxypropyl trimethoxysilane. According to the super-hydrophilic polyphenylene sulfide composite membrane with the structure and the preparation method thereof, the surface coating method and the surface grafting method are adopted to carry out hydrophilic modification on the PPS membrane, catechol is used for replacing dopamine substitutes, the modified layer is firmly adhered to the surface of the membrane, and reactive active groups are grafted on the surface of the membrane, so that an excellent modification effect is achieved, and the cost is reduced.
Description
Technical Field
The invention relates to the technical field of composite membranes, in particular to a super-hydrophilic polyphenylene sulfide composite membrane and a preparation method thereof.
Background
Membrane separation is known as a technique for efficient separation, concentration, purification and purification. The novel water treatment method has the advantages of safety, no pollution, simplicity, feasibility, excellent treatment effect and the like. The existing conventional membrane materials mainly comprise polysulfone, polyethersulfone, polyvinylidene fluoride, polyacrylonitrile and the like. Although the polyvinylidene fluoride membrane has stronger acid resistance, the polyvinylidene fluoride membrane loses the mechanical property in a strong alkaline solution; the polyethersulfone membrane can be dissolved in 1-methyl-2-pyrrolidone, and the integrity and the filtering performance are lost; the polyacrylonitrile membrane can be seriously corroded in a sodium hypochlorite solution, and the integrity and the mechanical property are lost; most of the conventional membrane materials can only be used in a mild environment, and in a severe environment with strong acidity and alkalinity and the like, the membrane materials cannot maintain the original performance or even completely lose the original performance. Therefore, a new film material with acid resistance and alkali resistance needs to be found.
Polyphenylene Sulfide (PPS) is a novel membrane material with a plurality of excellent performances such as acid and alkali resistance, solvent resistance, dimensional stability, high temperature resistance and the like, and can keep excellent performances in severe environment. However, the PPS film has strong hydrophobicity, and is easily contaminated by hydrophobic interaction with organic substances, microorganisms, and the like in water during water treatment and use. Membrane fouling not only reduces membrane performance but also shortens the membrane lifetime, and therefore hydrophilic modification of the membrane is required. The hydrophilic modification can not only improve the wettability and the permeability of the membrane, but also improve the pollution resistance of the membrane.
The hydrophilic modification method mainly comprises blending modification, surface coating modification, plasma treatment method, surface grafting method and the like. Although the blending modification is simple to operate, the bonding force between the polymer and the modified particles is not strong, and the modified particles are also easily coated in the main body of the membrane, so that the modification effect is poor; the plasma method is not uniform in treatment, and the phenomenon that the membrane surface is hydrophilic but the pores are hydrophobic is often caused only on the membrane surface; the modification of the surface coating method generally occurs on the surface of the film, and the stability between the coating and the surface of the film is poor and the film is easy to fall off. The mussel bionic method is a surface coating modification method which is developed rapidly in recent years, a modified layer formed by dopamine can be firmly adhered to the surface of a membrane, but the application of the method is limited by the high price of the dopamine.
Disclosure of Invention
The invention aims to provide a super-hydrophilic polyphenylene sulfide composite membrane and a preparation method thereof.
In order to realize the purpose, the invention provides a super-hydrophilic polyphenylene sulfide composite film and a preparation method thereof, wherein the super-hydrophilic polyphenylene sulfide composite film comprises the following components in parts by weight: 50 to 150 parts of polyphenylene sulfide, 30 to 90 parts of benzophenone, 20 to 80 parts of catechol, 10 to 30 parts of polyethyleneimine, 130 to 390 parts of dibutyl phthalate, 10 to 60 parts of trihydroxymethyl aminomethane and 5 to 30 parts of gamma-glycidyl ether oxypropyl trimethoxysilane.
Preferably, the mass ratio of the polyphenylene sulfide to the benzophenone to the dibutyl phthalate is 24.
Preferably, the molar ratio of the catechol to the polyethyleneimine is 1, and the mass fraction of the gamma-glycidoxypropyltrimethoxysilane is 1%.
A preparation method of a super-hydrophilic polyphenylene sulfide composite membrane comprises the following steps:
s1, mixing polyphenylene sulfide, benzophenone and dibutyl phthalate in a beaker;
s2, heating and stirring the mixed solution obtained in the step S1, pouring the mixed solution onto an iron plate, scraping the mixed solution with a film scraping rod to form a film, then putting the film into water for cooling and forming, taking the film out, adding ethanol into the film, extracting the residual solvent, washing the film with water after the extraction is finished, and drying the film to obtain a polyphenylene sulfide film;
s3, dissolving trihydroxymethyl aminomethane in water to prepare a buffer solution;
s4, adding pyrocatechol and polyethyleneimine into a buffer solution, and after a solute is completely dissolved, placing the wet PPS membrane into a newly prepared solution for oscillation;
and S5, cleaning the vibrated polyphenylene sulfide membrane with water and ethanol, putting the modified membrane into a gamma-glycidyl ether oxypropyltrimethoxysilane solution for heating, and cleaning, drying and storing the membrane after the reaction is finished to obtain the super-hydrophilic polyphenylene sulfide composite membrane.
Preferably, in the step S2, the three-neck flask is heated to 260 ℃, stirring is started when the temperature of the liquid in the flask rises to 200 ℃, and the flask is allowed to stand for 10min after the polyphenylene sulfide in the flask is completely dissolved.
Preferably, in step S3, the pH of the buffer is 8.5.
Preferably, in step S5, the heating temperature of the gamma-glycidoxypropyltrimethoxysilane is 50 ℃.
The invention has the following beneficial effects:
1. according to the invention, the surface coating method and the surface grafting method are adopted to carry out hydrophilic modification on the polyphenylene sulfide membrane, so that the hydrophilic performance of the polyphenylene sulfide membrane is greatly improved, catechol is used for replacing dopamine substituent, the modified layer is firmly adhered to the surface of the membrane, and the cost is reduced.
2. The invention improves the anti-pollution performance of the polyphenylene sulfide membrane by grafting the gamma-glycidoxypropyltrimethoxysilane to the surface of the membrane, and has good market application prospect.
The technical solution of the present invention is further described in detail by the following examples.
Detailed Description
The present invention will be further described below, and it should be noted that the present embodiment is based on the technical solution, and a detailed implementation manner and a specific operation process are given, but the protection scope of the present invention is not limited to the present embodiment.
The raw materials used in the examples were as follows:
polyphenylene sulfide (Mn = 65000), tacona, usa.
Benzophenone (DPK, 99%), catechol (CA, analytical grade), polyethyleneimine (PEI, mn = 600), shanghai alatin biochem technologies ltd
Dibutyl phthalate (DBP, 99%), tris (Tris, AR), hydrochloric acid, sodium hydroxide, gamma-glycidoxypropyltrimethoxysilane (KH 560, AR), tianjin gloss finishing chemical Co., ltd.
Example 1
The embodiment provides a super-hydrophilic polyphenylene sulfide composite film, which comprises the following components in parts by weight: 50 parts of polyphenylene sulfide, 30 parts of benzophenone, 26 parts of catechol, 10 parts of polyethyleneimine, 130 parts of dibutyl phthalate, 10 parts of tris (hydroxymethyl) aminomethane and 5 parts of gamma-glycidyl ether oxypropyl trimethoxysilane.
The preparation method of the super-hydrophilic polyphenylene sulfide composite membrane comprises the following steps:
s1, mixing polyphenylene sulfide, benzophenone and dibutyl phthalate in a beaker to prepare a mixed solution;
s2, transferring the mixed solution obtained in the step S1 into a three-neck flask, heating the three-neck flask to 260 ℃, starting stirring when the temperature of the mixed liquid in the three-neck flask rises to 200 ℃, standing for 10min after the polyphenylene sulfide in the three-neck flask is completely dissolved, pouring the mixed solution onto an iron plate, scraping the mixed solution to form a film by using a film scraping rod, then putting the film into water for cooling and forming, taking the film out, adding ethanol, extracting the residual solvent, washing with water after extraction is finished, and drying to obtain a polyphenylene sulfide film;
s3, dissolving trihydroxymethyl aminomethane in water to prepare a buffer solution; the pH of the buffer solution was adjusted to 8.5.
S4, adding catechol and polyethyleneimine into a buffer solution, wherein the molar ratio of the catechol to the polyethyleneimine is 1;
and S5, cleaning the vibrated polyphenylene sulfide membrane with water and ethanol, putting the modified membrane into a gamma-glycidyl ether oxypropyltrimethoxysilane solution for heating, wherein the mass fraction of the gamma-glycidyl ether oxypropyltrimethoxysilane in the solution is 1%, the heating temperature is 50 ℃, and cleaning, drying and storing the membrane after the reaction is finished to obtain the super-hydrophilic polyphenylene sulfide membrane composite membrane.
Example 2
The embodiment provides a super-hydrophilic polyphenylene sulfide composite film, which comprises the following components in parts by weight: 100 parts of polyphenylene sulfide, 62.5 parts of benzophenone, 55 parts of catechol, 21 parts of polyethyleneimine, 254 parts of dibutyl phthalate, 30 parts of tris (hydroxymethyl) aminomethane and 15 parts of gamma-glycidyl ether oxypropyl trimethoxysilane.
The preparation method of the super-hydrophilic polyphenylene sulfide composite membrane comprises the following steps:
s1, mixing polyphenylene sulfide, benzophenone and dibutyl phthalate in a beaker to prepare a mixed solution;
s2, transferring the mixed solution obtained in the step S1 into a three-neck flask, heating the three-neck flask to 260 ℃, starting stirring when the temperature of the mixed liquid in the three-neck flask rises to 200 ℃, standing for 10min after the polyphenylene sulfide in the three-neck flask is completely dissolved, pouring the mixed solution onto an iron plate, scraping the mixed solution to form a film by using a film scraping rod, then putting the film into water for cooling and forming, taking the film out, adding ethanol, extracting the residual solvent, washing with water after extraction is finished, and drying to obtain a polyphenylene sulfide film;
s3, dissolving trihydroxymethyl aminomethane in water to prepare a buffer solution; the pH of the buffer solution was adjusted to 8.5.
S4, adding catechol and polyethyleneimine into a buffer solution, wherein the molar ratio of the catechol to the polyethyleneimine is 1;
s5, washing the polyphenylene sulfide membrane after the oscillation is finished with water and ethanol, then putting the modified membrane into a gamma-glycidoxypropyltrimethoxysilane solution for heating, wherein the mass fraction of the gamma-glycidoxypropyltrimethoxysilane in the solution is 1%, the heating temperature is 50 ℃, and after the reaction is finished, washing, drying and storing the membrane to obtain the super-hydrophilic polyphenylene sulfide membrane composite membrane.
Example 3
The embodiment provides a super-hydrophilic polyphenylene sulfide composite film, which comprises the following components in parts by weight: 150 parts of polyphenylene sulfide, 90 parts of benzophenone, 78 parts of catechol, 30 parts of polyethyleneimine, 390 parts of dibutyl phthalate, 60 parts of tris (hydroxymethyl) aminomethane and 30 parts of gamma-glycidyl ether oxypropyl trimethoxysilane.
The preparation method of the super-hydrophilic polyphenylene sulfide composite membrane comprises the following steps:
s1, mixing polyphenylene sulfide, benzophenone and dibutyl phthalate in a beaker to prepare a mixed solution;
s2, transferring the mixed solution obtained in the step S1 into a three-neck flask, heating the three-neck flask to 260 ℃, starting stirring when the temperature of the mixed liquid in the three-neck flask rises to 200 ℃, standing for 10min after the polyphenylene sulfide in the three-neck flask is completely dissolved, pouring the mixed solution onto an iron plate, scraping the mixed solution to form a film by using a film scraping rod, then putting the film into water for cooling and forming, taking the film out, adding ethanol, extracting the residual solvent, washing with water after extraction is finished, and drying to obtain a polyphenylene sulfide film;
s3, dissolving trihydroxymethyl aminomethane in water to prepare a buffer solution; the pH of the buffer solution was adjusted to 8.5.
S4, adding catechol and polyethyleneimine into a buffer solution, wherein the molar ratio of the catechol to the polyethyleneimine is 1;
and S5, cleaning the vibrated polyphenylene sulfide membrane with water and ethanol, putting the modified membrane into a gamma-glycidyl ether oxypropyltrimethoxysilane solution for heating, wherein the mass fraction of the gamma-glycidyl ether oxypropyltrimethoxysilane in the solution is 1%, the heating temperature is 50 ℃, and cleaning, drying and storing the membrane after the reaction is finished to obtain the super-hydrophilic polyphenylene sulfide membrane composite membrane.
Comparative example 1
The embodiment provides a super-hydrophilic polyphenylene sulfide composite film, which comprises the following components in parts by weight: 100 parts of polyphenylene sulfide, 62.5 parts of benzophenone, 254 parts of dibutyl phthalate and 30 parts of tris (hydroxymethyl) aminomethane.
The preparation method comprises the following steps:
s1, mixing polyphenylene sulfide, benzophenone and dibutyl phthalate in a beaker to prepare a mixed solution;
s2, transferring the mixed solution obtained in the step S1 into a three-neck flask, heating the three-neck flask to 260 ℃, starting stirring when the temperature of the mixed liquid in the three-neck flask rises to 200 ℃, standing for 10min after the polyphenylene sulfide in the three-neck flask is completely dissolved, pouring the mixed solution onto an iron plate, scraping the mixed solution to form a film by using a film scraping rod, then putting the film into water for cooling and forming, taking the film out, adding ethanol, extracting the residual solvent, washing with water after extraction is finished, and drying to obtain a polyphenylene sulfide film;
s3, dissolving trihydroxymethyl aminomethane in water to prepare a buffer solution; the pH of the buffer solution was adjusted to 8.5.
S4, placing the wet polyphenylene sulfide film into a buffer solution to vibrate;
and S5, cleaning the vibrated polyphenylene sulfide film with water and ethanol, drying and storing to obtain the blank polyphenylene sulfide film composite film.
Comparative example 2
The embodiment provides a super-hydrophilic polyphenylene sulfide composite membrane which comprises the following components in parts by weight: 100 parts of polyphenylene sulfide, 62.5 parts of benzophenone, 55 parts of catechol, 21 parts of polyethyleneimine, 254 parts of dibutyl phthalate and 30 parts of tris (hydroxymethyl) aminomethane.
The preparation method comprises the following steps:
s1, mixing polyphenylene sulfide, benzophenone and dibutyl phthalate in a beaker to prepare a mixed solution;
s2, transferring the mixed solution obtained in the step S1 into a three-neck flask, heating the three-neck flask to 260 ℃, starting stirring when the temperature of the mixed liquid in the three-neck flask rises to 200 ℃, standing for 10min after the polyphenylene sulfide in the three-neck flask is completely dissolved, pouring the mixed solution onto an iron plate, scraping the mixed solution to form a film by using a film scraping rod, then putting the film into water for cooling and forming, taking the film out, adding ethanol, extracting the residual solvent, washing with water after extraction is finished, and drying to obtain a polyphenylene sulfide film;
s3, dissolving trihydroxymethyl aminomethane in water to prepare a buffer solution; the pH of the buffer solution was adjusted to 8.5.
S4, adding pyrocatechol and polyethyleneimine into a buffer solution, and after a solute is completely dissolved, placing the wet PPS membrane into a newly prepared solution for oscillation;
and S5, cleaning the vibrated polyphenylene sulfide film with water and ethanol, drying and storing to obtain the catechol/polyethyleneimine modified polyphenylene sulfide composite film.
And (3) performance testing:
1. pure water flux test
The polyphenylene sulfide composite films obtained in example 2 and comparative examples 1 to 2 were tested by a water flux measuring device having an effective area of 2.54cm 2 . The test sample is pre-pressed for 30min under 0.2MPa, then the sample is tested under 0.1MPa, and the flux value is recorded after being stable. Water flux (J) wl ) According to the formula wherein the effective area of the device is 2.54cm 2 . The test sample is pre-pressed for 30min under 0.2MPa, then the sample is tested under 0.1MPa, and the flux value is recorded after being stable. Water flux (J) wl ) According to the formula
Calculation, wherein A is the area of the film (m) 2 ) (ii) a Δ t is time (min); v is the volume of water. Each set of samples was tested 5 times, averaged, and the test results are shown in table 1:
TABLE 1 pure water flux test meter
| Pure water flux/(L.m) -2 ·h -1 ) | |
| Example 2 | 68 |
| Comparative example 1 | 24 |
| Comparative example 2 | 73.2 |
It can be seen by comparison that the hydrophilic performance of comparative example 2 is significantly better than that of the other examples, and that the hydrophilicity of comparative example 1 is poor, resulting in its pure water flux of only 24L/(m) 2 H). The pure water flux of comparative example 2 after modification was greatly increased, while the pure water flux of example 2 was still reduced by 5.2L/(m) despite the super-hydrophilic surface 2 H). The main reasons are as follows: after catechol and polyethyleneimine are modified, an adhesion layer on the surface of the membrane has good hydrophilicity, and after gamma-glycidoxypropyltrimethoxysilane is grafted, the steric hindrance of membrane pores is reduced and increased, so that the hydrophilicity is slightly reduced. But compared with the blank polyphenylene sulfide original membrane, the super-hydrophilic polyphenylene sulfide composite membrane has higher pure water flux and improves the permeability.
2. And (3) testing the anti-pollution performance:
bovine serum albumin is weighed and dissolved in water to prepare a protein solution with the mass concentration of 1 g/L. The test sample was pre-pressed at 0.2MPa for 30min, and the polyphenylene sulfide composite membranes prepared in example 2 and comparative examples 1-2 were tested at 0.1MPa, and the permeation flux was recorded. After testing for 1h, the membrane was removed, cleaned and tested again. Flux recovery ratio (R) according to the formula
Calculation of, in the formula J w To restore flux; j. the design is a square w1 To test front flux. Each set of samples was tested 5 times, averaged, and the test results are shown in table 2:
TABLE 2 anti-pollution property test meter
| Flux recovery rate/%) | |
| Example 2 | 92.62 |
| Comparative example 1 | 74.25 |
| Comparative example 2 | 85.33 |
The flux recovery rate is one of the important parameters of the membrane's anti-fouling ability. The flux recovery of the pure polyphenylene sulfide membrane of comparative example 1 was tested to be 74.25%, and the flux recovery of both example 2 and comparative example 2 was superior to example 1 because: the original film hydrophilicity of the polyphenylene sulfide modified by catechol and polyethyleneimine is increased, the flux recovery rate of the modified film is increased to 92.62 percent after the gamma-glycidyl ether oxypropyl trimethoxy silane is grafted, and the pollution resistance is further improved. Test results show that the hydrophilic modification not only improves the hydrophilicity of the membrane, but also increases the anti-pollution capacity of the membrane.
Therefore, compared with the prior art, the super-hydrophilic polyphenylene sulfide composite membrane material adopting the structure has the advantages that the catechol and the polyethyleneimine form a hydrophilic coating on the surface of the polyphenylene sulfide membrane through a codeposition method, and the gamma-glycidyl ether oxypropyl trimethoxysilane is grafted to the surface of the membrane, so that the hydrophilicity of the polyphenylene sulfide membrane is greatly improved, the pollution resistance of the polyphenylene sulfide membrane is improved, and the super-hydrophilic polyphenylene sulfide composite membrane material has a good market application prospect.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solutions of the present invention and not for limiting the same, and although the present invention is described in detail with reference to the preferred embodiments, those of ordinary skill in the art should understand that: modifications and equivalents may be made to the invention without departing from the spirit and scope of the invention.
Claims (7)
1. The super-hydrophilic polyphenylene sulfide composite membrane is characterized by comprising the following components in parts by weight: 50-150 parts of polyphenylene sulfide, 30-90 parts of benzophenone, 20-80 parts of catechol, 10-30 parts of polyethyleneimine, 130-390 parts of dibutyl phthalate, 10-60 parts of tris (hydroxymethyl) aminomethane and 5-30 parts of gamma-glycidyl ether oxypropyl trimethoxysilane.
2. The superhydrophilic polyphenylene sulfide composite membrane according to claim 1, wherein: the mass ratio of the polyphenylene sulfide to the benzophenone to the dibutyl phthalate is 24.
3. The superhydrophilic polyphenylene sulfide composite membrane according to claim 1, wherein: the molar ratio of catechol to polyethyleneimine is 1, and the mass fraction of gamma-glycidoxypropyltrimethoxysilane is 1%.
4. A method for preparing a superhydrophilic polyphenylene sulfide composite membrane according to any one of claims 1-3, comprising the steps of:
s1, mixing polyphenylene sulfide, benzophenone and dibutyl phthalate in a beaker;
s2, heating and stirring the mixed solution obtained in the step S1, pouring the mixed solution onto an iron plate, scraping the mixed solution with a film scraping rod to form a film, then putting the film into water for cooling and forming, taking the film out, adding ethanol into the film, extracting the residual solvent, washing the film with water after the extraction is finished, and drying the film to obtain a polyphenylene sulfide film;
s3, dissolving the trihydroxymethyl aminomethane in water to prepare a buffer solution;
s4, adding catechol and polyethyleneimine into a buffer solution, and after a solute is completely dissolved, placing the wet PPS film into a newly prepared solution for oscillation;
and S5, cleaning the vibrated polyphenylene sulfide membrane with water and ethanol, putting the modified membrane into a gamma-glycidyl ether oxypropyltrimethoxysilane solution for heating, and cleaning, drying and storing the membrane after the reaction is finished to obtain the super-hydrophilic polyphenylene sulfide composite membrane.
5. The preparation method of the super-hydrophilic polyphenylene sulfide composite membrane according to claim 4, wherein the preparation method comprises the following steps: in the step S2, the heating is to heat the three-neck flask to 260 ℃, start stirring when the temperature of liquid in the flask rises to 200 ℃, and stand for 10min after the polyphenylene sulfide in the flask is completely dissolved.
6. The preparation method of the super-hydrophilic polyphenylene sulfide composite membrane according to claim 4, wherein the preparation method comprises the following steps: in step S3, the pH value of the buffer is 8.5.
7. The preparation method of the super-hydrophilic polyphenylene sulfide composite membrane according to claim 4, wherein the preparation method comprises the following steps: in step S5, the heating temperature of the gamma-glycidoxypropyltrimethoxysilane is 50 ℃.
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