CN113368691A - Preparation method of aramid fiber organic solvent-resistant nanofiltration membrane - Google Patents
Preparation method of aramid fiber organic solvent-resistant nanofiltration membrane Download PDFInfo
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- CN113368691A CN113368691A CN202110619592.5A CN202110619592A CN113368691A CN 113368691 A CN113368691 A CN 113368691A CN 202110619592 A CN202110619592 A CN 202110619592A CN 113368691 A CN113368691 A CN 113368691A
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/02—Reverse osmosis; Hyperfiltration ; Nanofiltration
- B01D61/027—Nanofiltration
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- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0002—Organic membrane manufacture
- B01D67/0009—Organic membrane manufacture by phase separation, sol-gel transition, evaporation or solvent quenching
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0002—Organic membrane manufacture
- B01D67/0009—Organic membrane manufacture by phase separation, sol-gel transition, evaporation or solvent quenching
- B01D67/0011—Casting solutions therefor
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/56—Polyamides, e.g. polyester-amides
Abstract
The invention discloses a preparation method of an aramid fiber organic solvent-resistant nanofiltration membrane, which comprises the following steps: (1) sequentially adding potassium hydroxide, deionized water and dimethyl sulfoxide into a round-bottom flask at room temperature, and ultrasonically dissolving; after 10-30 minutes, adding the amino polystyrene microsphere solution into a round-bottom flask for ultrasonic dissolution; after 1-3 hours, adding aramid fiber into a round-bottom flask; placing the round-bottom flask in a constant-temperature water bath at 30-35 ℃, and mechanically stirring for 12-36 hours; vacuumizing and defoaming the obtained mixed membrane casting solution for 6-18 hours, and then uniformly scraping the membrane casting solution on a glass plate to form a membrane; (2) immediately immersing the scraped film into deionized water for 5-20 minutes by using a phase conversion method for phase conversion to obtain a hydrogel film; washing the hydrogel film with pure water until the pH value is 5-8; and taking out the membrane, draining, and drying in vacuum at 35-75 ℃ for 10-14 hours to obtain the aramid fiber organic solvent-resistant nanofiltration membrane. The aramid fiber organic solvent-resistant nanofiltration membrane prepared by the invention has high flux, high organic solvent tolerance and high selectivity.
Description
Technical Field
The invention belongs to the field of membrane separation under pressure driving, and particularly relates to a preparation method of an aramid fiber organic solvent-resistant nanofiltration membrane.
Technical Field
In the separation process of chemical substances, such as separation and recovery of organic solvents, medical intermediates, gases and the like in industry, the separation and recovery mainly depend on traditional phase change separation processes such as distillation, evaporation and the like. These processes are energy intensive and cause severe environmental pollution. Organic Solvent Nanofiltration (OSN) is a novel, efficient, low-energy-consumption, and stably-operated green separation process, is mainly used for separating solutes from a solvent, and plays an important role in chemical processes such as catalyst recovery and organic matter extraction. At present, all commercial solvent-resistant nanofiltration membranes are organic polymer nanofiltration membranes, and in order to solve the problems that the organic polymer nanofiltration membranes are easily swelled by organic solvents and reduced in membrane performance, membrane materials with stable chemical structures are generally selected and then modified to improve the solvent resistance of the membrane materials, so that the solvent-resistant organic nanofiltration membranes are finally prepared.
The nano aramid fiber is a one-dimensional organic nano material consisting of poly (p-phenylene terephthalamide) (PPTA), and has excellent mechanical property, extremely high thermal stability and tolerance to various common organic solvents. However, the hydrogen bonds between PPTA chains are easily regenerated, and the formed aramid-based film limits the industrial application of the PPTA-based film in the separation field due to low flux. Therefore, the basic performance of the base membrane is kept, and meanwhile, the solvent-resistant nanofiltration membrane with high flux and high selectivity is designed by adjusting the structure of the base membrane, so that the solvent-resistant nanofiltration membrane is beneficial to wide application in the industrial field.
Disclosure of Invention
The invention aims to provide a preparation method of an aramid fiber organic solvent-resistant nanofiltration membrane.
The invention adopts the following technical scheme:
the invention provides a preparation method of an aramid fiber organic solvent-resistant nanofiltration membrane, which comprises the following steps:
(1) sequentially adding potassium hydroxide, deionized water and dimethyl sulfoxide into a round-bottom flask at room temperature, and ultrasonically dissolving; after 10-30 minutes, adding the amino polystyrene microsphere solution into a round-bottom flask for ultrasonic dissolution; after 1-3 hours, aramid fiber is added into the round-bottom flask to enable the mass percentage of the aramid fiber to be 0.5% -4%; placing the round-bottom flask in a constant-temperature water bath at 30-35 ℃, and mechanically stirring for 12-36 hours; vacuumizing and defoaming the obtained mixed casting solution for 6-18 hours, selecting a scraper with the thickness of 150-250 microns, and uniformly scraping the casting solution on a glass plate to form a film; wherein, the total mass of the potassium hydroxide, the deionized water and the dimethyl sulfoxide is 100 percent, and the mass percentage of the potassium hydroxide, the deionized water and the dimethyl sulfoxide is respectively 1 to 5 percent, 1 to 5 percent and 90 to 98 percent; the mass usage of the amino polystyrene microsphere solution is 0-200% of the usage of the aramid fiber;
(2) immediately immersing the scraped film into deionized water for 5-20 minutes by using a phase conversion method for phase conversion to obtain a hydrogel film; washing the hydrogel film with pure water until the pH value is 5-8; and taking out the membrane, draining, and then placing the membrane at 35-75 ℃ for vacuum drying for 10-14 hours to obtain the aramid fiber organic solvent-resistant nanofiltration membrane.
In the invention, the concentration of the amino polystyrene microsphere solution is 2.5% w/v, the average particle size of the microsphere is 50-100 nm, and the amino polystyrene microsphere solution is purchased from Shanghai Michelin Biotechnology, Inc.
In the invention, the aramid fiber is Kevlar (KEVLAR) fiber, such as aramid fibers of types K29, K49, K49AP and the like produced by Dupont company in the United states.
Further, the mass percentages of the potassium hydroxide, the deionized water and the dimethyl sulfoxide are respectively 2% -3%, 2% -3% and 94% -96%.
Further, in the step (1), potassium hydroxide, deionized water and dimethyl sulfoxide are mixed, and the ultrasonic dissolving time is controlled to be 10-15 minutes, and more preferably 15 minutes.
Further, in the step (1), the mass usage of the amino polystyrene microsphere solution is 50% -200% of the usage of the aramid fiber, more preferably 80-100%, and most preferably 100%; ultrasonic dissolution is carried out for 1 to 1.5 hours, and more preferably for 1.5 hours.
Further, the mass percentage content of the aramid fiber in the mixed system is 1.5% -2%, and more preferably 2%.
Further, in the step (1), the mechanical stirring time is 18 to 24 hours, and more preferably 24 hours.
Further, in the step (1), the time for vacuumizing and defoaming the mixed casting solution is 10-12 hours, and more preferably 12 hours.
Further, in the step (1), the thickness of the scraper is 200 μm to 250 μm, and more preferably 200 μm.
Further, in the step (2), the scraped film is immediately immersed in deionized water for 10-15 minutes to obtain a hydrogel film.
Further, in the step (2), the hydrogel film is washed by pure water until the pH value is 6-7.
Further, in the step (2), the film is vacuum-dried at 45 to 55 ℃ for 12 hours, more preferably at 55 ℃ for 12 hours.
Compared with the prior art, the invention has the advantages that:
(1) the preparation method is simple and convenient in preparation process, easy to operate, low in toxicity, environment-friendly and convenient for industrial application.
(2) The separation performance test result of the prepared amino polystyrene microsphere/aramid fiber organic solvent-resistant nanofiltration membrane on a rose bengal ethanol solution shows that compared with an aramid fiber original membrane KANF-0%, the prepared amino polystyrene microsphere/aramid fiber organic solvent-resistant nanofiltration membrane has higher flux, and when the mass consumption of the amino polystyrene microsphere solution is not higher than 100% of the consumption of aramid fiber, the amino polystyrene microsphere/aramid fiber organic solvent-resistant nanofiltration membrane also has better dye retention rate.
(3) The contact angle of the prepared amino polystyrene microsphere/aramid fiber organic solvent-resistant nanofiltration membrane to ethanol is increased along with the increase of the dosage of the amino polystyrene microsphere.
(4) Compared with an aramid original film KANF-0%, the amino polystyrene microsphere/aramid organic solvent-resistant nanofiltration membrane prepared by the invention has higher flux in different solvents (methanol, ethanol, isopropanol, dimethylformamide, tetrahydrofuran, n-hexane and carbon tetrachloride).
(5) The amino polystyrene microsphere/aramid fiber organic solvent-resistant nanofiltration membrane prepared by the invention shows better solvent resistance than the original aramid fiber membrane KANF-0% in different solvents (methanol, ethanol, isopropanol, dimethylformamide, tetrahydrofuran, n-hexane and carbon tetrachloride).
(6) Compared with an aramid original membrane KANF-0%, the amino polystyrene microsphere/aramid fiber organic solvent-resistant nanofiltration membrane prepared by the invention has better retention rate for dyes and polyethylene glycol with molecular weight less than 800.
Drawings
FIG. 1 shows the permselectivity of five nanofiltration membranes with different content of amino polystyrene microspheres to rose bengal ethanol solution prepared by the invention;
FIG. 2 shows the contact angles (ethanol solutions) of five nanofiltration membranes with different content of the amino polystyrene microspheres prepared by the invention;
FIG. 3 is a graph showing the effect of the invention on the retention of aqueous solutions of polyethylene glycol of different molecular weights by KANF-0% and KANF-2% nanofiltration membranes;
FIG. 4 is a graph showing the effect of the nanofiltration membranes of KANF-0% and KANF-2% on the retention of ethanol solutions of dyes of different molecular weights prepared by the present invention;
FIG. 5 is the permeation flux of KANF-0% and KANF-2% nanofiltration membranes prepared by the present invention for different pure organic solvents;
FIG. 6 shows the swelling degree of the KANF-0% and KANF-2% nanofiltration membranes prepared by the present invention after soaking in different organic solvents for 15 days at normal temperature.
Detailed Description
The present invention will be further illustrated with reference to the following examples, but the present invention is not limited to the following examples. The following examples describe in more detail an aramid organic solvent nanofiltration membrane having high permselectivity and a preparation method thereof according to the present invention, and are given by way of illustration, but do not limit the scope of the present invention. Unless otherwise specified, the experimental method adopted by the invention is a conventional method, and experimental equipment, materials, reagents and the like used in the method can be purchased from chemical companies.
The concentration of the amino polystyrene microsphere solution used in the embodiment of the invention is 2.5% w/v, the average particle size of the microsphere is 50-100 nm, and the microsphere is purchased from Shanghai Michelin Biochemical technology, Inc.; the aramid fiber was K29 manufactured by DuPont, USA.
The invention is described in further detail below with reference to the following figures and embodiments:
example 1:
(1) preparing a solvent-resistant nanofiltration membrane: at room temperature, 2.25g of potassium hydroxide and 2.25g of deionized water (H) were weighed in this order2O) and 69g of dimethyl sulfoxide to a 100mL round-bottom flask, and ultrasonically dissolving for 15 minutes; after 15 minutes, adding 1.5g of an amino polystyrene microsphere solution into the round-bottom flask, ultrasonically dissolving for 1.5 hours, and after 1.5 hours, adding 1.5g of aramid fibers into the round-bottom flask; placing the round-bottom flask in a constant-temperature water bath at 30 ℃, and mechanically stirring for 24 hours; after 24 hours, placing the casting solution in the round-bottom flask in a vacuum drying oven, and removing bubbles for 10 hours; after 10 hours, the clean and dry glass plate was placed in a horizontal constant temperature and humidity cabinet, the thickness of the doctor blade was adjusted to 200 μm and the film was scraped on the glass plate. Immediately immersing the scraped film into deionized water; after completion of the phase inversion for 10 minutes, washing with pure water until the pH reached 7; taking the membrane out of the water by using non-woven fabrics, and then putting the membrane into the air for draining; after draining, the film is flatly placed into a vacuum drying oven, the temperature is set to be 55 ℃, and drying is carried out for 12 hours; after 12 hours, the membrane is taken out to obtain a nanofiltration membrane with excellent solvent resistance and high permselectivity, and the nanofiltration membrane is named as KANF-2%.
(2) And (3) evaluating the separation performance of the nanofiltration membrane: the amino polystyrene microsphere/aramid fiber solvent-resistant nanofiltration membrane prepared by the preparation method of the invention is used as a filtering membrane and is placed in a filtering tankIn the filtering device, different solvents are filtered under the conditions of room temperature and the operating pressure of 0.4MPa, the flux and the retention rate of the membrane are determined by detecting the concentration of the solvent in the filtrate, and the solvent is 0.05g/L rose bengal ethanol solution. The flux of KANF-2% p-rose bengal ethanol solution is 26.16L/(m)2H), rose bengal retention of 98.64%.
Example 2:
1.5g of the amino polystyrene microsphere in the example 1 is changed into 0g of the amino polystyrene microsphere and named as KANF-0%, and other steps are not changed to obtain the amino polystyrene microsphere/aramid fiber nanofiltration membrane. By adopting the performance detection method of the embodiment 1, the separation performance of the nanofiltration membrane is as follows: the flux of KANF-0% p-Mengladesh rose red ethanol feed liquid is 7.56L/(m)2H), rose bengal retention of 98.36%.
Example 3:
1.5g of the amino polystyrene microsphere in the example 1 is changed into 0.75g of the amino polystyrene microsphere and named as KANF-1%, and other steps are not changed to obtain the amino polystyrene microsphere/aramid fiber nanofiltration membrane. By adopting the performance detection method of the embodiment 1, the separation performance of the nanofiltration membrane is as follows: the flux of KANF-1% of the rose bengal ethanol feed liquid is 15.0L/(m)2H), rose bengal retention of 98.64%.
Example 4:
1.5g of the amino polystyrene microsphere in the example 1 is changed into 2.25g of the amino polystyrene microsphere and named as KANF-3%, and other steps are not changed to obtain the amino polystyrene microsphere/aramid fiber nanofiltration membrane. By adopting the performance detection method of the embodiment 1, the separation performance of the nanofiltration membrane is as follows: the flux of KANF-3% of the rose bengal ethanol feed liquid is 21.88L/(m)2H), rose bengal retention of 98.34%.
Example 5:
1.5g of the amino polystyrene microsphere in the example 1 is changed into 3.0g of the amino polystyrene microsphere and named as KANF-4%, and other steps are not changed to obtain the amino polystyrene microsphere/aramid fiber nanofiltration membrane. By adopting the performance detection method of the embodiment 1, the separation performance of the nanofiltration membrane is as follows: the flux of KANF-4% of the rose bengal ethanol feed liquid is 18.68L/(m)2H), rose bengal retention of 96.41%.
Example 6:
five nanofiltration membranes prepared by the methods of the embodiments 1 to 5 are selected, and the ethanol contact angles of the five nanofiltration membranes are respectively tested to measure the lyophilic and hydrophobic ethanol performances of the five nanofiltration membranes. The KANF-0% ethanol contact angle is 17.95 +/-0.15 degrees; the contact angle of KANF-1% ethanol is 22.9 +/-0.15 degrees; the KANF-2% ethanol contact angle is 24.1 +/-0.12 degrees; the KANF-3% ethanol contact angle is 32.95 +/-0.55 degrees; the KANF-4% ethanol contact angle is 38.2 +/-0.24 degrees; see figure 2 for details.
Example 7:
the KANF-2% and KANF-0% nanofiltration membranes prepared by the methods of example 1 and example 2 were selected and tested for the rejection of different molecular weight polyethylene glycol aqueous solutions by the two nanofiltration membranes, respectively. Setting initial feed liquid as 50mg/L polyethylene glycol aqueous solution with different molecular weights, testing pressure 0.4Mpa, cross-flow filtering, testing area 22.05cm2. The rejection rate of the nanofiltration membrane KANF-0% to the polyethylene glycol 300 is 20.43 +/-0.24%, the rejection rate to the polyethylene glycol 400 is 40.87 +/-0.24%, the rejection rate to the polyethylene glycol 600 is 80.79 +/-0.9%, and the rejection rate to the polyethylene glycol 800 is 99.2 +/-0.01%; the rejection rate of the nanofiltration membrane KANF-2% to the polyethylene glycol 300 is 32.12 +/-3.04%, the rejection rate to the polyethylene glycol 400 is 54.46 +/-2.06%, the rejection rate to the polyethylene glycol 600 is 84.27 +/-1.21%, and the rejection rate to the polyethylene glycol 800 is 99.46 +/-0.01%. See figure 3 for details.
Example 8:
the KANF-2% and KANF-0% nanofiltration membranes prepared by the methods of example 1 and example 2 were selected and tested for retention of ethanol solutions of dyes of different molecular weights. Setting the initial material liquid as 50mg/L ethanol solution of dye with different molecular weight, testing pressure 0.4Mpa, cross-flow filtering, testing area 22.05cm2. The rejection rate of the nanofiltration membrane KANF-0% to methyl orange is 42.78 +/-2.02%, the rejection rate to chrome black T is 52.58 +/-2.38%, the rejection rate to eosin Y is 92.24 +/-0.34%, and the rejection rate to Congo red is 95.26 +/-0.37%; the rejection rate of the nanofiltration membrane KANF-2% to methyl orange is 52.18 +/-2.47%, and the rejection rate to chrome black T is 62.68 +/-2.42%, and has a retention rate of 93.28 +/-0.3% for eosin Y and 96.48 +/-0.34% for congo red. See figure 4 for details.
Example 9:
the KANF-2% and KANF-0% nanofiltration membranes prepared according to the methods of example 1 and example 2 were selected and tested for swelling after soaking in various common organic solvents for 15 days. Setting the initial material liquid as different pure organic solvents including methanol, ethanol, isopropanol, dimethylformamide, tetrahydrofuran, n-hexane and carbon tetrachloride, drying the membrane in a 60 ℃ oven for 24 hours after soaking, weighing the mass change of the sample before and after soaking in the organic solvent, and calculating the swelling degree. The specific swelling degree change is shown in figure 5 in detail, and after 15 days of soaking, the swelling degree of KANF-2% is less than KANF-0%, and the solvent tolerance is more excellent.
Claims (9)
1. A preparation method of an aramid fiber organic solvent-resistant nanofiltration membrane comprises the following steps:
(1) sequentially adding potassium hydroxide, deionized water and dimethyl sulfoxide into a round-bottom flask at room temperature, and ultrasonically dissolving; after 10-30 minutes, adding the amino polystyrene microsphere solution into a round-bottom flask for ultrasonic dissolution; after 1-3 hours, aramid fiber is added into the round-bottom flask to enable the mass percentage of the aramid fiber to be 0.5% -4%; placing the round-bottom flask in a constant-temperature water bath at 30-35 ℃, and mechanically stirring for 12-36 hours; vacuumizing and defoaming the obtained mixed casting solution for 6-18 hours, selecting a scraper with the thickness of 150-250 microns, and uniformly scraping the casting solution on a glass plate to form a film; wherein, the total mass of the potassium hydroxide, the deionized water and the dimethyl sulfoxide is 100 percent, and the mass percentage of the potassium hydroxide, the deionized water and the dimethyl sulfoxide is respectively 1 to 5 percent, 1 to 5 percent and 90 to 98 percent; the mass usage of the amino polystyrene microsphere solution is 0-200% of the usage of the aramid fiber;
(2) immediately immersing the scraped film into deionized water for 5-20 minutes by using a phase conversion method for phase conversion to obtain a hydrogel film; washing the hydrogel film with pure water until the pH value is 5-8; and taking out the membrane, draining, and then placing the membrane at 35-75 ℃ for vacuum drying for 10-14 hours to obtain the aramid fiber organic solvent-resistant nanofiltration membrane.
2. The method of claim 1, wherein: the concentration of the amino polystyrene microsphere solution is 2.5% w/v, and the average particle size of the microspheres is 50-100 nm.
3. The method of claim 1, wherein: the aramid fiber is Kevlar fiber.
4. The method according to any one of claims 1 to 3, wherein: the mass percentages of the potassium hydroxide, the deionized water and the dimethyl sulfoxide are respectively 2-3%, 2-3% and 94-96%.
5. The method according to any one of claims 1 to 3, wherein: in the step (1), the mass amount of the amino polystyrene microsphere solution is 50-200% of the aramid fiber amount, more preferably 80-100%, and most preferably 100%.
6. The method according to any one of claims 1 to 3, wherein: the mass percentage of the aramid fiber in the mixed system is 1.5-2%, and the mass percentage of the aramid fiber in the mixed system is more preferably 2%.
7. The method according to any one of claims 1 to 3, wherein: in the step (1), the mechanical stirring time is 18-24 hours; the time for vacuumizing and defoaming the mixed casting solution is 10-12 hours.
8. The method according to any one of claims 1 to 3, wherein: in the step (1), the thickness of the scraper is 200 μm-250 μm, and more preferably 200 μm.
9. The method according to any one of claims 1 to 3, wherein: in the step (2), immediately immersing the scraped film into deionized water for 10-15 minutes to obtain a hydrogel film; washing the hydrogel film with pure water until the pH value is 6-7; taking out the film, draining, and vacuum drying at 45-55 deg.c for 12 hr.
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