CN112791596B - Preparation method of acid-resistant, alkali-resistant and ethanol-resistant polyvinylidene fluoride hydrophilic membrane - Google Patents
Preparation method of acid-resistant, alkali-resistant and ethanol-resistant polyvinylidene fluoride hydrophilic membrane Download PDFInfo
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- CN112791596B CN112791596B CN202011522870.7A CN202011522870A CN112791596B CN 112791596 B CN112791596 B CN 112791596B CN 202011522870 A CN202011522870 A CN 202011522870A CN 112791596 B CN112791596 B CN 112791596B
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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
- B01D67/0079—Manufacture of membranes comprising organic and inorganic components
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/02—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor characterised by their properties
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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
- B01D71/30—Polyalkenyl halides
- B01D71/32—Polyalkenyl halides containing fluorine atoms
- B01D71/34—Polyvinylidene fluoride
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2323/00—Details relating to membrane preparation
- B01D2323/02—Hydrophilization
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/36—Hydrophilic membranes
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
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Abstract
The invention discloses a preparation method of a polyvinylidene fluoride hydrophilic membrane with acid resistance, alkali resistance and ethanol resistance, which comprises the following steps of (1) dissolving PVDF and TBAC in DMF, heating and stirring for 3-4h, then not heating and stirring for 18-20h to obtain a PVDF solution, and performing electrostatic spinning to obtain a PVDF nano membrane; (2) adding PVP and KH560 into deionized water according to a certain amount, and stirring to prepare a hydrophilic finishing agent; (3) and soaking the PVDF nano-film in ethanol, then placing the soaked PVDF nano-film in a hydrophilic finishing agent, and drying the PVDF nano-film to obtain the polyvinylidene fluoride hydrophilic film. The polyvinylidene fluoride membrane obtained by the method has excellent hydrophilic effect, has good acid resistance (sodium hypochlorite solution of 3-4%), alkali resistance (NaOH solution of 0.4%) and ethanol resistance (absolute ethanol), and can be used in the fields of liquid filtration, water filtration and the like.
Description
Technical Field
The invention belongs to a preparation method of a functional nano-film, and particularly relates to a preparation method of a polyvinylidene fluoride hydrophilic film with acid resistance, alkali resistance and ethanol resistance.
Background
In recent years, nonwoven fabrics have been developed rapidly, and among them, electrospun nanofiber membranes have attracted more and more attention and are applied in various fields, and the growth rate is extremely high. The electrostatic spinning polyvinylidene fluoride (PVDF) fiber membrane has the advantages of large specific surface area, high porosity, good electrolyte wettability, good acid and alkali resistance and the like, but the polyvinylidene fluoride has no hydrophilic group, so that the PVDF nano membrane is hindered in the fields of water filtration, mask cloth and the like requiring products to have hydrophilic performance.
The method for post-finishing the polyvinylidene fluoride nano-film by post-finishing means to endow the polyvinylidene fluoride nano-film with hydrophilicity has the advantages of simple operation process, low requirement on equipment, high efficiency and the like, and brings attention to researchers. However, most researchers select the post-finishing hydrophilic finishing agent as the surfactant, the polyvinylidene fluoride nano-film treated by the surfactant has good initial hydrophilicity, but has the problem of poor acid, alkali and ethanol resistance after finishing, and many polyvinylidene fluoride nano-films are used for water filtration or oil-water separation and the like, and are in need of contacting acid, alkali, ethanol and the like in industrial use.
Disclosure of Invention
The invention aims to provide a preparation method of a polyvinylidene fluoride hydrophilic membrane with acid resistance, alkali resistance and ethanol, which comprises the steps of firstly preparing a polyvinylidene fluoride (PVDF) and tetrabutylammonium chloride (TBAC) blended membrane, then preparing a hydrophilic finishing agent of polyvinylpyrrolidone (PVP) and Y-glycidyl ether oxypropyl trimethoxy silane (KH560), wetting the PVDF membrane, putting the PVDF membrane into the hydrophilic finishing agent, then taking out and baking for post finishing, fully utilizing the KH560 to connect the TBAC and the PVP, endowing the polyvinylidene fluoride nano membrane with hydrophilicity and enabling the polyvinylidene fluoride nano membrane to have the performances of acid resistance, alkali resistance and ethanol resistance, and the finished polyvinylidene fluoride nano membrane with acid resistance, alkali resistance and ethanol resistance can be suitable for the fields of water filtration, mask cloth and the like.
The technical scheme adopted by the invention is as follows:
a preparation method of a polyvinylidene fluoride hydrophilic membrane with acid resistance, alkali resistance and ethanol comprises the following steps:
(1) dissolving PVDF and TBAC in DMF, heating to 70 ℃ and stirring for 3-4h to make PVDF powder easier to dissolve, then stirring for 18-20h without heating, fully stirring to obtain PVDF solution, and performing electrostatic spinning to obtain a PVDF nano-film;
(2) adding PVP and KH560 into deionized water, and stirring to obtain hydrophilic finishing agent;
(3) and (3) soaking the PVDF nano membrane obtained in the step (1) in ethanol for 1-2min, then placing the PVDF nano membrane in the hydrophilic finishing agent obtained in the step (2), taking out the PVDF nano membrane, and baking and drying the PVDF nano membrane to obtain the acid, alkali and ethanol resistant polyvinylidene fluoride hydrophilic membrane.
In the above technical solution, further, the conductivity of the PVDF solution obtained in the step (1) is 100-102(μ s/cm), and since the addition of the TABC can effectively increase the conductivity, the fiber diameter can be thinned.
Further, in the step (1), PVDF and TBAC were added to DMF so that the concentration of PVDF was 10% by weight.
Further, the concentration of PVP in the hydrophilic finishing agent in the step (2) is 0.5-2 wt%.
Further, the concentration of KH560 in the hydrophilic finishing agent in the step (2) is 2-6 g/L.
Further, the soaking time of the PVDF nano-film in the hydrophilic finishing agent in the step (3) is 5-10 min.
Due to the adoption of the technical scheme, the method has the following beneficial effects:
according to the invention, inorganic particle tetrabutylammonium chloride (TBAC) is utilized to effectively increase the conductivity of the PVDF solution, so that the fiber diameter is smaller, the pore diameter is smaller, the filtering efficiency is higher, meanwhile, the TBAC is also inorganic particles, and the silane coupling agent KH560 is utilized to connect the hydrophilic PVP with the inorganic particle TBAC, so that the hydrophilic PVP is firmly connected to the surface of the polyvinylidene fluoride nano-membrane, and the polyvinylidene fluoride nano-membrane is endowed with good acid, alkali and ethanol resistance. The method has simple and convenient operation process, low requirement on equipment and convenient popularization and use.
Drawings
The invention will be further described with reference to the accompanying drawings in which:
FIG. 1 is a scanning electron microscope image of the hydrophilic polyvinylidene fluoride nano-film obtained in example 1;
fig. 2 shows the contact angle change of the hydrophilic polyvinylidene fluoride nano-film obtained in example 1 in different time periods when the contact angle is tested after the hydrophilic polyvinylidene fluoride nano-film is sequentially soaked in acid, alkali and ethanol for 12 hours.
Detailed Description
The invention is further illustrated by the following examples:
in the following examples, reagents, materials and devices used were each commercially available or prepared by a conventional method, unless otherwise specified.
Example 1
(1) Dissolving 10 wt% of PVDF and TBAC in DMF, heating and stirring for 4h, then stirring for 20h without heating, fully stirring to ensure that the conductivity of the solution is 102 (mu s/cm), and then carrying out electrostatic spinning to obtain a PVDF nano film;
(2) 1 wt% of PVP and 2g/L KH560 are added into deionized water and stirred to prepare a hydrophilic finishing agent;
(3) and (3) hydrophilic after-finishing of the polyvinylidene fluoride nano-membrane, namely soaking the PVDF membrane in ethanol for 1min, putting the PVDF membrane in a hydrophilic finishing agent for 6min, taking out the PVDF membrane, putting the PVDF membrane in a 70 ℃ blast drying oven for baking for 35min, and drying to obtain the hydrophilic polyvinylidene fluoride nano-membrane.
Through testing, the water contact angle of the prepared hydrophilic polyvinylidene fluoride nano-film is 28.3 degrees (the hydrophilic polyvinylidene fluoride nano-film is tested after being kept for 3 seconds after dripping water); two pieces of 5X5cm hydrophilically finished polyvinylidene fluoride nano-film are sequentially placed in sodium hypochlorite 3-4% solution, 0.4% NaOH solution and absolute ethyl alcohol for 12 hours respectively, and the water contact angle of the polyvinylidene fluoride nano-film is still less than 23.3 degrees, which shows that the polyvinylidene fluoride nano-film still has good hydrophilicity.
In addition, the electrostatic spinning PVDF nano-film obtained in the step 1) in the example 1 is soaked in 1 wt% PVP aqueous solution, and the good hydrophilicity is found, but after the electrostatic spinning PVDF nano-film is placed in 3-4% sodium hypochlorite solution, 0.4% NaOH solution and absolute ethyl alcohol in sequence for 12 hours respectively, the film is not wet when dropped with water, and the PVDF nano-film soaked in the 1 wt% PVP aqueous solution does not have the performances of acid resistance, alkali resistance, ethyl alcohol resistance and the like.
Example 2
(1) Dissolving 10 wt% of PVDF and TBAC in DMF, heating and stirring for 3h, then stirring for 19h without heating, fully stirring to ensure that the conductivity of the solution is 102 (mu s/cm), and then carrying out electrostatic spinning to obtain a PVDF nano film;
(2) adding 2 wt% of PVP and 6g/L KH560 into deionized water, and stirring to prepare a hydrophilic finishing agent;
(3) and (3) hydrophilic after-finishing of the polyvinylidene fluoride nano-membrane, namely soaking the PVDF membrane in ethanol for 1min, putting the PVDF membrane in a hydrophilic finishing agent for 5min, taking out the PVDF membrane, putting the PVDF membrane in a 70 ℃ blast drying oven for baking for 25min, and drying to obtain the hydrophilic polyvinylidene fluoride nano-membrane.
After testing, the water contact angle position of the prepared hydrophilic polyvinylidene fluoride nano-film is 44.2 degrees (after dropping water, the test is carried out after 3 seconds of water dropping); two 5X5cm hydrophilic polyvinylidene fluoride nano-films are placed in sodium hypochlorite 3-4% solution, 0.4% NaOH solution and absolute ethyl alcohol for 12 hours, and the water contact angle of the polyvinylidene fluoride nano-films is still less than 39.2 degrees, which shows that the polyvinylidene fluoride nano-films still have good hydrophilicity.
Example 3
(1) Dissolving 10 wt% of PVDF and TBAC in DMF, heating and stirring for 4h, then stirring for 18h without heating, fully stirring to ensure that the conductivity of the solution is 102 (mu s/cm), and then carrying out electrostatic spinning to obtain a PVDF nano film;
(2) adding 0.5 wt% of PVP and 4g/L KH560 into deionized water, and stirring to prepare a hydrophilic finishing agent;
(3) and (3) hydrophilic after-finishing of the polyvinylidene fluoride nano-membrane, namely soaking the PVDF membrane in ethanol for 1min, putting the PVDF membrane in a hydrophilic finishing agent for 10min, taking out the PVDF membrane, putting the PVDF membrane in a 70 ℃ blast drying oven for baking for 30min, and drying to obtain the hydrophilic polyvinylidene fluoride nano-membrane.
Through testing, the water contact angle of the prepared hydrophilic polyvinylidene fluoride nano-film is 26.4 degrees (the hydrophilic polyvinylidene fluoride nano-film is tested after being kept for 3 seconds after dripping); two 5X5cm hydrophilically finished polyvinylidene fluoride nano-films are placed in sodium hypochlorite 3-4% solution, 0.4% NaOH solution and absolute ethyl alcohol for 12 hours, and the water contact angle of the polyvinylidene fluoride nano-films is still smaller than 21.4 degrees, which shows that the polyvinylidene fluoride nano-films still have good hydrophilicity.
Example 4
(1) Dissolving 10 wt% of PVDF and TBAC in DMF, heating and stirring for 4h, then stirring for 20h without heating, fully stirring to ensure that the conductivity of the solution is 102 (mu s/cm), and then carrying out electrostatic spinning to obtain a PVDF nano film;
(2) 1 wt% of PVP and 4g/L KH560 are added into deionized water and stirred to prepare a hydrophilic finishing agent;
(3) and (3) hydrophilic after-finishing of the polyvinylidene fluoride nano-membrane, namely soaking the PVDF membrane in ethanol for 1min, putting the PVDF membrane in a hydrophilic finishing agent for 8min, taking out the PVDF membrane, putting the PVDF membrane in a 70 ℃ blast drying oven for baking for 35min, and drying to obtain the hydrophilic polyvinylidene fluoride nano-membrane.
Through testing, the water contact angle of the prepared hydrophilic polyvinylidene fluoride nano-film is 37.7 degrees (the hydrophilic polyvinylidene fluoride nano-film is tested after being kept for 3 seconds after dripping); two 5X5cm hydrophilic polyvinylidene fluoride nano-films are placed in sodium hypochlorite 3-4% solution, 0.4% NaOH solution and absolute ethyl alcohol for 12 hours, and the water contact angle of the polyvinylidene fluoride nano-films is still less than 32.7 degrees, which shows that the polyvinylidene fluoride nano-films still have good hydrophilicity.
The sample of example 1 was subjected to a flux test, and it can be seen that the filtration area was taken to be 4. pi. cm2100ml of water are added, the mixture is run through for 9 minutes, and the FLUX FLUX is V/(A T) 0.1L/[ (4 pi/10000 m)2)*(9/60h)]=530.7856Lm-2h-1The prepared membrane has good hydrophilicity and water flux.
The above is merely a concrete implementation of the present invention, but the technical features of the present invention are not limited thereto. Any simple change, equivalent replacement or modification made based on the present invention to solve the substantially same technical problems and achieve the substantially same technical effects all fall within the protection scope of the present invention.
Claims (6)
1. A preparation method of polyvinylidene fluoride hydrophilic membrane with acid resistance, alkali resistance and ethanol resistance is characterized by comprising the following steps: the method comprises the following steps:
(1) dissolving PVDF and TBAC in DMF, heating to 70 ℃ and stirring for 3-4h to make PVDF powder easier to dissolve, then stirring for 18-20h without heating, fully stirring to obtain PVDF solution, and performing electrostatic spinning to obtain a PVDF nano-film;
(2) adding PVP and KH560 into deionized water, and stirring to prepare a hydrophilic finishing agent;
(3) and (3) soaking the PVDF nano membrane obtained in the step (1) in ethanol for 1-2min, then placing the PVDF nano membrane in the hydrophilic finishing agent obtained in the step (2), taking out the PVDF nano membrane, and baking and drying the PVDF nano membrane to obtain the acid, alkali and ethanol resistant polyvinylidene fluoride hydrophilic membrane.
2. The method for preparing the polyvinylidene fluoride hydrophilic membrane with the acid resistance, the alkali resistance and the ethanol resistance as claimed in claim 1, wherein the conductivity of the PVDF solution obtained in the step (1) is 100-102(μ s/cm).
3. The method for preparing a polyvinylidene fluoride hydrophilic membrane with acid, alkali and ethanol resistance according to claim l, wherein the PVDF and TBAC are added into DMF in step (1) to make the concentration of PVDF 10 wt%.
4. The method for preparing polyvinylidene fluoride hydrophilic membrane with acid resistance, alkali resistance and ethanol resistance as claimed in claim I, wherein the concentration of PVP in the hydrophilic finishing agent in the step (2) is 0.5-2 wt%.
5. The method for preparing polyvinylidene fluoride hydrophilic membrane with acid resistance, alkali resistance and ethanol resistance as claimed in claim 1, wherein the concentration of KH560 in the hydrophilic finishing agent in the step (2) is 2-6 g/L.
6. The method for preparing polyvinylidene fluoride hydrophilic membrane with acid, alkali and ethanol resistance as claimed in claim I, wherein the soaking time of the PVDF nano membrane in the hydrophilic finishing agent in the step (3) is 5-10 min.
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