CN111672337B - Preparation method of hydrophilic PTFE (polytetrafluoroethylene) filter membrane suitable for treating oil-containing anionic dye wastewater and filter membrane - Google Patents
Preparation method of hydrophilic PTFE (polytetrafluoroethylene) filter membrane suitable for treating oil-containing anionic dye wastewater and filter membrane Download PDFInfo
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- CN111672337B CN111672337B CN202010403123.5A CN202010403123A CN111672337B CN 111672337 B CN111672337 B CN 111672337B CN 202010403123 A CN202010403123 A CN 202010403123A CN 111672337 B CN111672337 B CN 111672337B
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- B01D71/06—Organic material
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Abstract
The invention relates to a preparation method of a hydrophilic PTFE filter membrane suitable for treating oil-containing anionic dye wastewater and the filter membrane, and belongs to the technical field of membrane modification. The preparation method comprises the following steps: a) preparing a chitosan acetic acid aqueous solution; b) adding citric acid and potassium dihydrogen phosphate into the chitosan acetic acid aqueous solution to dissolve so as to form a first reaction solution; c) adding a fluorocarbon surfactant into the first reaction liquid to form a second reaction liquid; d) and (3) immersing the PTFE filter membrane into the second reaction solution for reaction, and obtaining the hydrophilic PTFE filter membrane after the reaction is finished. The filter membrane is suitable for treating oily wastewater, is particularly suitable for treating oily dye wastewater, and has the advantages of high hydrophilicity, strong oil-water separation capability and good anionic dye removal capability.
Description
Technical Field
The invention relates to the technical field of membrane modification, in particular to a preparation method of a hydrophilic PTFE filter membrane suitable for treating oil-containing anionic dye wastewater and the filter membrane.
Background
Nowadays, the pollution of oily wastewater due to the increasing discharge amount of industrial oily wastewater and the frequent oil leakage accidents have attracted extensive attention, seriously threatening the ecological environment and human health.
Among the various oil forms present, oil/water emulsions (in particular oils stabilized by surfactants) are the most difficult to separate due to good stability and small droplet size (< 20 μm). Membrane separation techniques have proven to be a more promising separation method due to their high separation efficiency, low cost and ease of operation, compared to traditional separation methods, including skimming, air flotation and chemical flocculation. The PTFE micro-filtration membrane has the advantages of high porosity, high mechanical strength, low price and the like, and is widely applied to the field of membrane separation. However, the PTFE membrane has high hydrophobicity and is limited in use in the field of oil-water separation.
In recent years, there have been many reports on hydrophilic modification of PTFE membranes, and chinese patent publication No. CN 104998562 a discloses a hydrophilic modification method of a polytetrafluoroethylene membrane, in which a PTFE membrane is treated with plasma under a nitrogen atmosphere, acrylic acid is grafted, and then titanium dioxide is fixed on the surface of the membrane by coordination of carboxyl and Ti4+, thereby providing the membrane with hydrophilic and photocatalytic properties. Chinese patent publication No. CN 105854638A discloses a permanent hydrophilic PTFE hollow fiber membrane and a method for preparing the same, which adopts a cross-linking reaction of dopamine and a hydrophilic or amphoteric polymer to improve the hydrophilicity of the PTFE membrane, but the dopamine is expensive, thereby increasing the production cost. Chinese patent publication No. CN 104353370 a discloses a method for preparing a hydrophilic polytetrafluoroethylene composite microporous membrane, which comprises blending hydrophilic nano inorganic particles into PTFE powder and then stretching the mixture to prepare a hydrophilic membrane, but the nano inorganic particles are not uniformly dispersed, resulting in non-uniform hydrophilicity on the membrane surface.
The difficulty of wastewater purification has been further exacerbated by dyes (e.g., azo compounds) produced in the printing, textile and semiconductor industries in recent years. In view of their high toxicity, carcinogenicity and non-degradability, it is important to effectively remove these water-soluble dyes from the wastewater prior to discharge. Chinese patent with patent publication No. CN 110064376A discloses a spongy magnesium chitosan adsorbent for removing dye wastewater and a preparation method thereof, wherein a chitosan acetic acid solution and magnesium chloride are mixed to prepare the magnesium chitosan adsorbent, and the magnesium chitosan adsorbent has good adsorption capacity on anionic dye. Chinese patent publication No. CN 110124635 a discloses an aliphatic polyamide-amine polymer grafted chitosan dye adsorbent and a preparation method thereof, wherein a self-made aliphatic polyamide-amine polymer is grafted on chitosan by genipin, so that the content of active groups is increased, and the adsorption capacity is increased. The above prior art reflects the importance of chitosan in dye adsorption.
It is noteworthy that actual industrial effluents often contain a variety of complex contaminants. For example, oil-containing waste water containing dyes, multifunctional materials capable of separating insoluble oil and water-soluble dyes by specific wettability are very attractive, but have been rarely reported.
Disclosure of Invention
Aiming at the problems, the invention provides a preparation method of a hydrophilic PTFE filter membrane and the filter membrane by using chitosan and citric acid as raw materials and carrying out ultraviolet radiation treatment, which are suitable for treating oily wastewater, in particular to oily dye wastewater, and have the advantages of high hydrophilicity, strong oil-water separation capability and good anionic dye removal capability.
The technical scheme for solving the problems is as follows:
the preparation method of the hydrophilic PTFE filter membrane suitable for treating the oil-containing anionic dye wastewater comprises the following steps:
a) preparing a chitosan acetic acid aqueous solution with the pH of 3.5-4.5;
b) adding citric acid and potassium dihydrogen phosphate into the chitosan acetic acid aqueous solution to dissolve so as to form a first reaction solution;
c) adding a fluorocarbon surfactant into the first reaction liquid to form a second reaction liquid;
d) and (3) immersing the PTFE filter membrane into the second reaction solution, heating and reacting under the condition of ultraviolet radiation, and obtaining the hydrophilic PTFE filter membrane suitable for treating the oil-containing anionic dye wastewater after the reaction is finished.
The invention firstly mixes chitosan and citric acid to prepare pre-reaction liquid, and forms a hydrophilic layer containing a large amount of hydroxyl and amino on the surface of the PTFE membrane under the catalysis of monopotassium phosphate and the initiation of ultraviolet radiation, so that the membrane has good oil-water separation capability and anionic dye removal capability.
Preferably, in the step a), the mass ratio of the chitosan to the chitosan acetic acid aqueous solution is 0.1-1%.
Preferably, the above-described aspect further includes: in the step a), the concentration of acetic acid in the chitosan acetic acid aqueous solution is 0.1-0.7%.
Preferably, in the step b), the mass ratio of the citric acid to the chitosan acetic acid aqueous solution is 0.1-1%, and the mass ratio of the potassium dihydrogen phosphate to the chitosan acetic acid aqueous solution is 0.08-0.12%.
Preferably, in step b), citric acid and potassium dihydrogen phosphate are added into the chitosan acetic acid aqueous solution in the form of powder.
Preferably, in step c), the fluorocarbon surfactant is perfluoroundecanecarboxylic acid.
Preferably, in the step b), the amount of the perfluoroundecanecarboxylic acid added is 0.8 to 1.2% by mass of the first reaction solution.
Preferably, in the step d), the reaction temperature is 40-80 ℃, and the power of the ultraviolet lamp is 100-1500W.
Preferably, in the step d), the reaction time is 1 to 10 hours.
The filter membrane is prepared by adopting the preparation method in any one of the technical schemes.
In summary, the embodiment of the present application has the following beneficial effects:
1) the chitosan and the citric acid react under the catalysis of potassium dihydrogen phosphate and the initiation of ultraviolet radiation to form a three-dimensional network structure layer on the surface of the PTFE membrane, so that a large number of hydroxyl groups and amino groups are endowed on the surface of the PTFE membrane, and the hydrophilicity of the membrane surface is greatly improved.
2) Hydroxyl and amino on the surface of the modified membrane combine water molecules on the surface of the membrane through hydrogen bond action, so that a hydration layer is formed on the surface of the membrane, and the membrane has good oil-water separation capacity.
3) Hydroxyl on the surface of the modified membrane is combined with the anionic dye through hydrogen bond action, and amino adsorbs the anionic dye through electrostatic attraction action, so that the membrane has good anionic dye removing capacity.
Drawings
FIG. 1 is a graph of the 0s static water contact angle of the membrane in a comparative example of the invention;
FIG. 2 is a graph showing the 0s static water contact angle of the film obtained in example 3 of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. The embodiments of the present invention, and all other embodiments obtained by those skilled in the art without any inventive step, are within the scope of the present invention.
The present invention will be described in detail below by way of examples with reference to the accompanying drawings.
The multifunctional hydrophilic PTFE membrane is obtained by reacting chitosan and citric acid on the surface of the PTFE membrane under the catalysis of monopotassium phosphate and ultraviolet radiation, has high flux and efficiency for oil-water emulsion separation, and has good effect on anionic dye removal.
Example 1:
a) preparing a chitosan acetic acid aqueous solution with pH =4 and the mass fraction of chitosan being 0.1%;
b) adding citric acid with the mass fraction of 1% of the chitosan acetic acid solution and monopotassium phosphate with the content of one thousandth of the chitosan acetic acid solution into the step a), and stirring for dissolving.
c) Adding perfluoroundecanecarboxylic acid as one percent of the total solution to step b);
d) and c), putting the PTFE membrane into the reaction solution prepared in the step c), and reacting for 10 hours at the temperature of 80 ℃ and the power of an ultraviolet lamp of 100W to obtain the multifunctional hydrophilic PTFE membrane M1.
Example 2:
a) preparing a chitosan acetic acid aqueous solution with pH =4 and the mass fraction of chitosan of 1%;
b) adding citric acid with the mass fraction accounting for 0.1 percent of the chitosan acetic acid solution and monopotassium phosphate with the content accounting for one thousandth of the chitosan acetic acid solution into the step a), and stirring and dissolving.
c) Adding perfluoroundecanecarboxylic acid as one percent of the total solution to step b);
d) and c), putting the PTFE membrane into the reaction solution prepared in the step c), and reacting for 1h at the temperature of 40 ℃ and the ultraviolet lamp power of 1500W to obtain the multifunctional hydrophilic PTFE membrane M2.
Example 3:
a) preparing a chitosan acetic acid aqueous solution with pH =4.5 and the mass fraction of chitosan of 0.5%;
b) adding citric acid with the mass fraction accounting for 0.3 percent of the chitosan acetic acid solution and monopotassium phosphate with the content accounting for one thousandth of the chitosan acetic acid solution into the step a), and stirring and dissolving.
c) Adding perfluoroundecanecarboxylic acid as one percent of the total solution to step b);
d) and c), putting the PTFE membrane into the reaction solution prepared in the step c), and reacting for 3 hours at the temperature of 50 ℃ and the ultraviolet lamp power of 1000W to obtain the multifunctional hydrophilic PTFE membrane M3.
Example 4:
a) preparing a chitosan acetic acid aqueous solution with pH =3.5 and a chitosan mass fraction of 0.3%;
b) adding citric acid with the mass fraction of 0.5 percent of the chitosan acetic acid solution and monopotassium phosphate with the content of one thousandth of the chitosan acetic acid solution into the step a), stirring and dissolving.
c) Adding perfluoroundecanecarboxylic acid as one percent of the total solution to step b);
d) and c), putting the PTFE membrane into the reaction solution prepared in the step c), and reacting for 5 hours at the temperature of 70 ℃ and the ultraviolet lamp power of 800W to obtain the multifunctional hydrophilic PTFE membrane M4.
Example 5:
a) preparing a chitosan acetic acid aqueous solution with pH =4 and the mass fraction of chitosan being 0.7%;
b) adding citric acid with the mass fraction of 0.7 percent of the chitosan acetic acid solution and monopotassium phosphate with the content of one thousandth of the chitosan acetic acid solution into the step a), stirring and dissolving.
c) Adding perfluoroundecanecarboxylic acid as one percent of the total solution to step b);
d) and c), putting the PTFE membrane into the reaction solution prepared in the step c), and reacting for 7 hours at the temperature of 60 ℃ and under the ultraviolet lamp power of 1200W to obtain the multifunctional hydrophilic PTFE membrane M5.
Comparative example 1:
the original PTFE separation membrane M0.
Comparative example 2:
a) preparing a chitosan acetic acid aqueous solution with pH =4 and the mass fraction of chitosan being 0.5%;
b) adding citric acid with the mass fraction accounting for 0.3 percent of the chitosan acetic acid solution and monopotassium phosphate with the content accounting for one thousandth of the chitosan acetic acid solution into the step a), and stirring and dissolving.
c) Adding perfluoroundecanecarboxylic acid as one percent of the total solution to step b);
d) and (c) putting the PTFE membrane into the reaction solution prepared in the step c), and reacting for 3 hours at the temperature of 50 ℃ to obtain the multifunctional hydrophilic PTFE membrane M6.
Comparative example 3:
a) preparing a chitosan acetic acid aqueous solution with pH =4 and the mass fraction of chitosan being 0.5%;
b) adding citric acid with the mass fraction accounting for 0.3 percent of the chitosan acetic acid solution into the step a), stirring and dissolving.
c) Adding perfluoroundecanecarboxylic acid as one percent of the total solution to step b);
d) and c), putting the PTFE membrane into the reaction solution prepared in the step c), and reacting for 3 hours at the temperature of 50 ℃ and the ultraviolet lamp power of 1200W to obtain the multifunctional hydrophilic PTFE membrane M7.
Test example:
an aqueous emulsion containing an anionic dye was prepared using 0.1% (M machine oil/M water) of a machine oil and 20% Tween-80 (MT-80/M machine oil) as an emulsifier, and having a methyl blue concentration of 1 mg/L. The mixture was then stirred at 10000 rpm for 1.0 h. The droplet size of the emulsion was determined by Dynamic Light Scattering (DLS) (LB 550, HORIBA). The average particle size of the final emulsion is 90-442 nm.
The area of the effective membrane is 13.85cm2The permeation and separation performance of the membrane is studied by the dead-end filtration experiment, and the membrane flux is calculated by the formula (1):
wherein J is permeation flux, V is permeation volume, A is effective area, and Δ t is test time.
All membranes were pre-stressed at 0.2MPa with deionized water for at least 0.5h before measurement to give a stable membrane flux, while pure water flux (Jw) was measured at 0.1 MPa. The pure water was then replaced by an oil-in-water emulsion and filtered under gravity for 30 min. The oil content in the water was measured at 280nm using a UV-vis spectrophotometer (Lambda 900, USA), and the separation efficiency was calculated from the oil discard efficiency according to equation (2).
R1 is the retention rate in oil-water emulsion separation, CpAs concentration of filtrate oil, CfThe concentration of the original oil-water emulsion.
The effective membrane area adopted in the dye adsorption experiment is 13.85cm2The dead-end filtration experiment, adsorption experiment, 200 mL of a 1mg/L methyl blue aqueous solution dye solution was poured onto the upper surface of the membrane and the filtrate was collected. The whole separation process is only driven by gravity. The maximum absorption wavelength of the dye in the solution before and after adsorption was measured by a UV-vis spectrophotometer (Lambda 900, USA), and the concentration of the dye in the solution after filtration was obtained from the calibration curve. Therefore, the removal efficiency of the dye (R2) was calculated according to formula (3).
R2 is methyl blue removal rate, C1Concentration of methyl blue as filtrate, C0Is the original methyl blue concentration.
TABLE 1 multifunctional hydrophilic PTFE Membrane oil-water separation and dye removal efficiency
As can be seen from Table 1, the multifunctional hydrophilic PTFE membrane obtained by the method has good oil-water separation efficiency and anion dye removal efficiency, and the oil-water separation efficiency and the anion dye removal efficiency can be remarkably improved by adding potassium dihydrogen phosphate and ultraviolet radiation.
As shown in FIG. 1, which is a graph of the 0s static water contact angle of the membrane of comparative example 1 of the present invention, and as shown in FIG. 2, which is a graph of the 0s static water contact angle of the membrane of example 3 of the present invention, the multifunctional hydrophilic PTFE membrane obtained according to the present invention has a greatly reduced water contact angle on the surface of the membrane and a greatly increased hydrophilicity as compared with the original PTFE membrane.
The applicant declares that the above description is only a specific embodiment of the present invention, but the scope of the present invention is not limited thereto, and it should be understood by those skilled in the art that any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are within the scope and disclosure of the present invention.
Claims (9)
1. The preparation method of the hydrophilic PTFE filter membrane suitable for treating the oil-containing anionic dye wastewater is characterized by comprising the following steps:
a) preparing a chitosan acetic acid aqueous solution with the pH of 3.5-4.5;
b) adding citric acid and potassium dihydrogen phosphate into the chitosan acetic acid aqueous solution to dissolve so as to form a first reaction solution;
c) adding a fluorocarbon surfactant into the first reaction liquid to form a second reaction liquid;
d) and (3) immersing the PTFE filter membrane into the second reaction liquid, heating and reacting under the condition of ultraviolet radiation, wherein the power of an ultraviolet lamp is 100-1500W, the reaction time is 1-10 hours, and the hydrophilic PTFE filter membrane suitable for treating the oil-containing anionic dye wastewater is obtained after the reaction is finished.
2. The method for preparing a hydrophilic PTFE filter membrane suitable for treating oil-containing anionic dye wastewater according to claim 1, wherein the method comprises the following steps: in the step a), the mass ratio of the chitosan to the chitosan acetic acid aqueous solution is 0.1-1%.
3. The method for preparing a hydrophilic PTFE filter membrane suitable for treating oil-containing anionic dye wastewater according to claim 1 or 2, wherein the method comprises the following steps: in the step a), the concentration of acetic acid in the chitosan acetic acid aqueous solution is 0.1-0.7%.
4. The method for preparing a hydrophilic PTFE filter membrane suitable for treating oil-containing anionic dye wastewater according to claim 1, wherein the method comprises the following steps: in the step b), the mass ratio of citric acid to the chitosan acetic acid aqueous solution is 0.1-1%, and the mass ratio of potassium dihydrogen phosphate to the chitosan acetic acid aqueous solution is 0.08-0.12%.
5. The method for preparing a hydrophilic PTFE filter membrane suitable for treating oil-containing anionic dye wastewater according to claim 1, wherein the method comprises the following steps: in step b), citric acid and potassium dihydrogen phosphate are added into the chitosan acetic acid aqueous solution in the form of powder.
6. The method for preparing a hydrophilic PTFE filter membrane suitable for treating oil-containing anionic dye wastewater according to claim 1, wherein the method comprises the following steps: in the step c), the fluorocarbon surfactant is perfluoroundecanecarboxylic acid.
7. The method for preparing a hydrophilic PTFE filter membrane suitable for treating oil-containing anionic dye wastewater according to claim 6, wherein the method comprises the following steps: in the step b), the adding mass of the perfluoroundecanecarboxylic acid is 0.8-1.2% of the mass of the first reaction solution.
8. The method for preparing a hydrophilic PTFE filter membrane suitable for treating oil-containing anionic dye wastewater according to claim 1, wherein the method comprises the following steps: in the step d), the reaction temperature is 40-80 ℃.
9. A filter membrane, characterized in that: the preparation method is characterized by being prepared by the preparation method of any one of claims 1-8.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102671631A (en) * | 2012-04-24 | 2012-09-19 | 三元控股集团有限公司 | Preparation method of adsorbent for acid dye wastewater treatment |
| WO2018208902A1 (en) * | 2017-05-10 | 2018-11-15 | Northwestern University | Porous polyelectrolyte complex films and foams and related methods |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102671631A (en) * | 2012-04-24 | 2012-09-19 | 三元控股集团有限公司 | Preparation method of adsorbent for acid dye wastewater treatment |
| WO2018208902A1 (en) * | 2017-05-10 | 2018-11-15 | Northwestern University | Porous polyelectrolyte complex films and foams and related methods |
Non-Patent Citations (2)
| Title |
|---|
| β-环糊精/壳聚糖膜的制备及在废水处理中的应用;俞丹等人;《印染》;20130131(第2期);第56-60页 * |
| 酸性染料对壳聚糖改性腈纶的染色;郝凤岭等人;《毛纺科技》;20150630;第43卷(第6期);第15-18页 * |
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