CN112588123A - Aramid loose nanofiltration membrane as well as preparation method and application thereof - Google Patents
Aramid loose nanofiltration membrane as well as preparation method and application thereof Download PDFInfo
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- CN112588123A CN112588123A CN202011324803.4A CN202011324803A CN112588123A CN 112588123 A CN112588123 A CN 112588123A CN 202011324803 A CN202011324803 A CN 202011324803A CN 112588123 A CN112588123 A CN 112588123A
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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
- 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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- 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
- B01D71/56—Polyamides, e.g. polyester-amides
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
- C02F1/442—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by nanofiltration
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D2325/00—Details relating to properties of membranes
- B01D2325/24—Mechanical properties, e.g. strength
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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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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
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Abstract
The invention provides an aramid loose nanofiltration membrane for efficient dye salt separation and a preparation method and application thereof3C2TxAnd (3) carrying out ice bath ultrasonic treatment on the two-dimensional nanosheet under an alkaline condition to obtain the aramid loose nanofiltration membrane. The preparation of the membrane is based on the three-dimensional interconnected space characteristic of the aramid fiber framework, has the characteristic of high porosity, and further has the separation of the nanofiltration membraneCharacteristics and good self-cleaning ability. The membrane is used for efficiently recovering dyes after separation of dyeing salts, realizes efficient separation and interception of dyes such as Congo red, rose bengal, alcian blue and the like under low pressure by utilizing the screening performance of an aramid fiber framework after intercalation of a rigid two-dimensional nanosheet and a reconstructed nano water channel, and is suitable for rapid treatment and dye recovery of high-salt printing and dyeing wastewater.
Description
Technical Field
The invention belongs to the technical field of membrane separation, and particularly relates to an aramid loose nanofiltration membrane for efficient dye salt separation, and a preparation method and application thereof.
Background
At present, the problems of high salinity of the waste water in the printing and dyeing industry, difficult direct biological treatment and the like in China become bottleneck problems which restrict the high-efficiency treatment of the waste water in the printing and dyeing textile industry. Toxic and harmful byproducts can be generated in the process of treating the water body by ozone oxidation and other technologies, so that secondary pollution is caused. The separation effect of technologies such as ion exchange and electrodialysis on organic matters and salt in water is poor, the energy consumption is high, the stability is poor, and the method is not suitable for large-scale printing and dyeing wastewater treatment. The search for the removal of salts and the recovery of dyes from printing and dyeing wastewater is a hot spot of current attention and research and development.
The nanofiltration method can realize the high-efficiency separation of the dye salt in the high-salinity wastewater under higher water flux. However, the nanofiltration membrane has a certain retention capacity on salt ions, so that the purity of the recovered dye is low. Meanwhile, the operating pressure of the existing nanofiltration membrane is high, and the problems of high energy consumption and the like possibly exist in the separation process of the dye salt. Therefore, the research and development of a membrane material which can remarkably improve the separation efficiency of the dye salt and reduce the nanofiltration operation pressure is an urgent problem to be solved in the prior printing and dyeing wastewater treatment technology.
Disclosure of Invention
Aiming at the defects, the invention provides the aramid loose nanofiltration membrane for efficiently separating the salt, which can not only efficiently recover the dye, but also realize higher water production rate and membrane flux under lower operation pressure, has obvious pollution resistance and long service life, and the preparation method and the application thereof.
The invention provides the following technical scheme: a preparation method of an aramid loose nanofiltration membrane comprises the following steps:
1) preparing an aramid nano-fiber spinning solution: crushing the para-aramid fiber yarn, adding the crushed para-aramid fiber yarn into a potassium hydroxide solution with the mass fraction of 1%, stirring the solution at the temperature of 80 ℃ for 2 hours, washing the solution with deionized water, and drying the washed solution; adding the dried fiber fragments into dimethylformamide, and continuously stirring for 1-3 h at the rotation speed of 200-500 rpm to obtain an aramid nanofiber spinning solution;
2) preparing hydrophilic aramid nanofiber sol: dropwise adding the aramid nano-fiber spinning solution obtained in the step 1) into a phosphoric acid solution with the mass fraction of 3% -10%, standing for 2-12 h, continuously stirring at the rotating speed of 100-300 rpm for 1-2 h, and then carrying out ultrasonic treatment for 2-5 h to obtain hydrophilic aramid nano-fiber sol;
3) preparing an aramid loose nanofiltration membrane: adding Ti into hydrophilic aramid nano-fiber sol3C2TxAnd (3) adjusting the pH value of the solution to 9-10 by using a two-dimensional nano sheet, continuously performing ultrasonic treatment for 1-3 h under an ice bath condition, and performing suction filtration on the obtained dispersion liquid to obtain the aramid loose nanofiltration membrane.
Further, the mass ratio of the para-aramid fiber yarn in the step 1) to the potassium hydroxide in the potassium hydroxide solution is 1: 0.5-4.
Further, the dosage ratio of the para-aramid fiber yarn to the dimethylformamide in the step 1) is 1g:300 mL-800 mL.
Further, the dosage ratio of the aramid nano-fiber spinning solution to the phosphoric acid solution in the step 2) is 1g:1000 mL-3000 mL.
Further, the hydrophilic aramid nano-fiber sol obtained in the step 3) and the Ti3C2TxThe mass ratio of the two-dimensional nano sheets is 1: 0.05-0.3.
The invention also provides the aramid loose nanofiltration membrane prepared by the preparation method, and the porosity of the nanofiltration membrane is 40-70%.
The invention also provides the application of the loose aramid nanofiltration membrane in the efficient recovery of dye after the separation of the dye, wherein the operation pressure is 1.5-2.5 bar.
Further, the flux was 150Lm-2h-1bar-1～200Lm-2h-1bar-1。
The invention has the beneficial effects that:
1. the preparation method is simple, and the prepared aramid loose nanofiltration membrane has good hydrophilicity and mechanical strength, has obvious interception effect on dye molecules such as Congo red, rose bengal, Alsinoblue and the like, and is suitable for rapid treatment of high-salt printing and dyeing wastewater.
2. The aramid loose nanofiltration membrane obtained by the preparation method is based on the spatial characteristic of three-dimensional interconnection of aramid fiber frameworks, has the characteristic of high porosity, is low in salt rejection rate and high in water yield, and can realize efficient separation of dyeing salt under lower operation pressure (1.5-2.5 bar).
3. The aramid fiber membrane prepared by the method has the separation characteristic of a nanofiltration membrane and good self-cleaning capability. The membrane mainly aims at separating the dye salt and efficiently recovering the dye, and realizes efficient separation of the dye salt under low pressure by utilizing the sieving performance of the aramid fiber framework after the rigid two-dimensional nanosheet intercalation and the reconstructed nano-water channel. According to the invention, the aramid loose nanofiltration membrane has remarkable rejection performance of Congo red, rose bengal and Alsinoblue under the operation pressure of 2bar, and is suitable for rapid treatment and dye recovery of high-salt printing and dyeing wastewater.
Drawings
The invention will be described in more detail hereinafter on the basis of embodiments and with reference to the accompanying drawings. Wherein:
FIG. 1 is an aramid loose nanofiltration membrane entity prepared in example 1;
FIG. 2 is a scanning electron microscope picture of the front surface and the cross section of the aramid loose nanofiltration membrane prepared in example 1;
FIG. 3 is a schematic diagram of an apparatus for separating a dye salt in examples 4 to 6.
Detailed description of the preferred embodiments
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The embodiment provides a preparation method of an aramid loose nanofiltration membrane, which comprises the following steps:
1) preparing an aramid nano-fiber spinning solution: soaking 1g of para-aramid fiber in 200mL of 1% by mass potassium hydroxide solution, stirring at 80 ℃ for 2h, washing with deionized water and drying; adding 500mL of dimethylformamide into the dried fiber fragments, and continuously stirring at a rotating speed of 200rpm for 3 hours to obtain an aramid fiber spinning solution;
2) preparing hydrophilic aramid fiber sol: dripping the aramid nano-fiber spinning solution obtained in the step 1) into a phosphoric acid solution with the mass fraction of 3% according to the dosage ratio of 1g to 1000mL, standing for 12h, continuously stirring at the rotating speed of 300rpm for 1h, and then carrying out ultrasonic treatment for 2h to obtain hydrophilic aramid nano-fiber sol;
3) preparing an aramid loose nanofiltration membrane: taking a certain mass of the hydrophilic aramid nano-fiber sol obtained in the step 2), and adding Ti with the mass ratio of 0.1:1 to the aramid fiber3C2TxAnd (3) performing two-dimensional nanosheet, adjusting the pH of the solution to 10, and then performing continuous ultrasonic treatment for 1h under the ice bath condition. And (3) carrying out suction filtration on the dispersion liquid to obtain the aramid loose nanofiltration membrane with the porosity of 40%. The object is shown in figure 1, and the micro-topography of the front surface and the cross section of the film is shown in figure 2.
Example 2
The embodiment provides a preparation method of an aramid loose nanofiltration membrane, which comprises the following steps:
1) preparing an aramid nano-fiber spinning solution: soaking 1g of para-aramid fiber in 400mL of potassium hydroxide solution with the mass fraction of 1%, stirring for 1h at 80 ℃, washing with deionized water and drying; adding 800mL of dimethylformamide into the dried fiber fragments, and continuously stirring at a rotating speed of 500rpm for 2 hours to obtain an aramid fiber spinning solution;
2) preparing hydrophilic aramid fiber sol: dripping the aramid nano-fiber spinning solution obtained in the step 1) into a phosphoric acid solution with the mass fraction of 5% according to the dosage ratio of 1g to 2000mL, standing for 8h, continuously stirring at the rotating speed of 100rpm for 2h, and then carrying out ultrasonic treatment for 5h to obtain hydrophilic aramid nano-fiber sol;
3) preparing an aramid loose nanofiltration membrane: taking a certain mass of the hydrophilic aramid nano-fiber sol obtained in the step 2)Adding Ti with the mass ratio of 0.05:1 to the aramid fiber3C2TxAnd (3) performing two-dimensional nanosheet, adjusting the pH of the solution to 9, and then performing continuous ultrasonic treatment for 3h under the ice bath condition. And (3) carrying out suction filtration on the dispersion liquid to obtain the aramid loose nanofiltration membrane with the porosity of 55%.
Example 3
The embodiment provides a preparation method of an aramid loose nanofiltration membrane, which comprises the following steps:
1) preparing an aramid nano-fiber spinning solution: soaking 1g of para-aramid fiber in 400mL of potassium hydroxide solution with the mass fraction of 1%, stirring for 1h at 80 ℃, washing with deionized water and drying; adding the dried fiber fragments into 300mL of dimethylformamide, and continuously stirring at a rotating speed of 3500rpm for 1h to obtain an aramid fiber spinning solution;
2) preparing hydrophilic aramid fiber sol: dropwise adding the aramid nano-fiber spinning solution obtained in the step 1) into a phosphoric acid solution with the mass fraction of 10% according to the dosage ratio of 1g to 3000mL, standing for 12h, continuously stirring at the rotating speed of 200rpm for 1.5h, and then carrying out ultrasonic treatment for 3.5h to obtain hydrophilic aramid nano-fiber sol;
3) preparing an aramid loose nanofiltration membrane: taking a certain mass of the hydrophilic aramid nano-fiber sol obtained in the step 2), and adding Ti with the mass ratio of 0.3:1 to the aramid fiber3C2TxAnd (3) performing two-dimensional nanosheet, adjusting the pH of the solution to 9.5, and then performing continuous ultrasonic treatment for 2h under the ice bath condition. And (3) carrying out suction filtration on the dispersion liquid to obtain the aramid loose nanofiltration membrane with the porosity of 70%.
Example 4
By using the aramid loose nanofiltration membrane prepared in the embodiment 1 and adopting a structural device shown in fig. 3, a mixed solution of sodium sulfate and congo red is filtered within an operating pressure range of 2bar, wherein 1 in fig. 3 is a water inlet of the device, 2 is the aramid loose nanofiltration membrane prepared in the embodiment 1 of the invention, and 3 is a water outlet of the device. The concentration of sodium sulfate was 5.0gL when the separation of the dye salt was carried out-1Congo Red concentration of 1.0gL-1The membrane flux is 180Lm-2h-1bar-1. The result shows that the rejection rate of Congo red is up to 96 percent, and sodium sulfateThe retention rate of (a) is less than 0.2%.
Example 5
By using the aramid loose nanofiltration membrane prepared in the embodiment 1 and adopting a structural device shown in fig. 3, a mixed solution of sodium chloride and rose bengal is filtered under an operating pressure of 1.5bar, wherein 1 in fig. 3 is a water inlet of the device, 2 is the aramid loose nanofiltration membrane prepared in the embodiment 1 of the invention, and 3 is a water outlet of the device. The concentration of sodium chloride was 1.0gL when the separation of the dye salts was carried out-1Rose bengal concentration of 1.0gL-1The membrane flux is 150Lm-2h-1bar-1. The result shows that the rose bengal retention rate is as high as 98%, and the sodium chloride retention rate is lower than 0.1%.
Example 6
By using the aramid loose nanofiltration membrane prepared in the embodiment 1 and adopting a structural device shown in fig. 3, a mixed solution of sodium chloride and alcian blue is filtered under an operating pressure of 2.5bar, wherein 1 in fig. 3 is a water inlet of the device, 2 is the aramid loose nanofiltration membrane prepared in the embodiment 1 of the invention, and 3 is a water outlet of the device. The concentration of sodium chloride was 1.0gL when the separation of the dye salts was carried out-1Concentration of alcian blue 0.2gL-1The membrane flux is 200Lm-2h-1bar-1. The result shows that the retention rate of the alcian blue reaches up to 99.05 percent, and the retention rate of the sodium chloride is lower than 0.12 percent.
The above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Furthermore, those skilled in the art will appreciate that while some embodiments herein include some features included in other embodiments, rather than other features, combinations of features of different embodiments are meant to be within the scope of the invention and form different embodiments. For example, in the claims above, any of the claimed embodiments may be used in any combination. The information disclosed in this background section is only for enhancement of understanding of the general background of the invention and should not be taken as an acknowledgement or any form of suggestion that this information forms the prior art already known to a person skilled in the art.
Claims (8)
1. The preparation method of the aramid loose nanofiltration membrane is characterized by comprising the following steps of:
1) preparing an aramid nano-fiber spinning solution: crushing the para-aramid fiber yarn, adding the crushed para-aramid fiber yarn into a potassium hydroxide solution with the mass fraction of 1%, stirring the solution at the temperature of 80 ℃ for 2 hours, washing the solution with deionized water, and drying the washed solution; adding the dried fiber fragments into dimethylformamide, and continuously stirring for 1-3 h at the rotation speed of 200-500 rpm to obtain an aramid nanofiber spinning solution;
2) preparing hydrophilic aramid nanofiber sol: dropwise adding the aramid nano-fiber spinning solution obtained in the step 1) into a phosphoric acid solution with the mass fraction of 3% -10%, standing for 2-12 h, continuously stirring at the rotating speed of 100-300 rpm for 1-2 h, and then carrying out ultrasonic treatment for 2-5 h to obtain hydrophilic aramid nano-fiber sol;
3) preparing an aramid loose nanofiltration membrane: adding Ti into hydrophilic aramid nano-fiber sol3C2TxAnd (3) adjusting the pH value of the solution to 9-10 by using a two-dimensional nano sheet, continuously performing ultrasonic treatment for 1-3 h under an ice bath condition, and performing suction filtration on the obtained dispersion liquid to obtain the aramid loose nanofiltration membrane.
2. The preparation method of the aramid loose nanofiltration membrane as claimed in claim 1, wherein the mass ratio of the para-aramid fiber yarn in the step 1) to the potassium hydroxide in the potassium hydroxide solution is 1: 0.5-4.
3. The preparation method of the aramid loose nanofiltration membrane of claim 1, wherein the dosage ratio of the para-aramid fiber yarn to the dimethylformamide in the step 1) is 1 g/300 mL-800 mL.
4. The preparation method of the aramid loose nanofiltration membrane of claim 1, wherein the dosage ratio of the aramid nano-fiber spinning solution to the phosphoric acid solution in the step 2) is 1g:1000 mL-3000 mL.
5. The preparation method of the aramid loose nanofiltration membrane as claimed in claim 1, wherein the hydrophilic aramid nanofiber sol obtained in the step 3) and the Ti are mixed together to form the hydrophilic aramid nanofiber sol3C2TxThe mass ratio of the two-dimensional nano sheets is 1: 0.05-0.3.
6. The aramid loose nanofiltration membrane prepared by the preparation method according to any one of claims 1 to 5, wherein the porosity of the nanofiltration membrane is 40 to 70 percent.
7. The application of the aramid loose nanofiltration membrane of claim 6 in efficient dye recovery after dye salt separation, wherein the operating pressure is 1.5-2.5 bar.
8. The application of the aramid loose nanofiltration membrane of claim 6 to efficient dye recovery after separation of a dye salt, wherein the flux is 150Lm-2h-1bar-1～200Lm-2h-1bar-1。
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| CN113198332A (en) * | 2021-04-08 | 2021-08-03 | 华南理工大学 | MXene-nanofiber composite membrane and preparation method and application thereof |
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