CN113426308A - Acid-base-resistant and high-temperature-resistant PASS/PP high-flux tubular ultrafiltration membrane - Google Patents
Acid-base-resistant and high-temperature-resistant PASS/PP high-flux tubular ultrafiltration membrane Download PDFInfo
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- CN113426308A CN113426308A CN202110640355.7A CN202110640355A CN113426308A CN 113426308 A CN113426308 A CN 113426308A CN 202110640355 A CN202110640355 A CN 202110640355A CN 113426308 A CN113426308 A CN 113426308A
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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
- B01D71/66—Polymers having sulfur in the main chain, with or without nitrogen, oxygen or carbon only
- B01D71/68—Polysulfones; Polyethersulfones
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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
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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
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/04—Tubular membranes
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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
- B01D69/10—Supported membranes; Membrane supports
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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
- B01D71/26—Polyalkenes
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Abstract
The invention discloses an acid-base-resistant and high-temperature-resistant PASS/PP high-flux tubular ultrafiltration membrane, and belongs to the field of organic separation membranes. The separation membrane comprises a modified polypropylene (PP) porous support layer and a polyarylene sulfide sulfone (PASS) separation membrane layer. The invention firstly prepares the PP porous membrane supporting tube by ultrasonic welding of special equipment, then synchronously and uniformly coats the casting membrane liquid containing PASS on the inner wall of the prepared supporting tube, and prepares the PASS/PP high-flux tubular ultrafiltration membrane by adopting a phase inversion method. The membrane has excellent performances of good hydrophilicity, high flux, high temperature resistance, acid and alkali resistance and the like, and can be widely used in the fields of medicine, food, acid and alkali recovery, industrial water treatment, petrochemical industry and the like.
Description
Technical Field
The invention belongs to the field of organic separation membranes, and relates to a preparation method of an acid-base-resistant and high-temperature-resistant PASS/PP high-flux tubular ultrafiltration membrane.
Technical Field
The ultrafiltration technology is used as a membrane separation technology, most membranes are porous asymmetric structures, the filtration process is a separation process based on a mechanical screening principle by taking differential pressure on two sides of the membranes as mass transfer power, and the ultrafiltration membrane has the characteristics of normal-temperature operation, no phase change in the process, low energy consumption, high separation precision and the like.
Polyarylene sulfide sulfone (PASS) is a novel polymer material with a great development prospect, and has excellent heat resistance (the glass transition temperature reaches 220 ℃), corrosion resistance and excellent mechanical properties. PASS is soluble in a specific solvent at room temperature, can be conveniently characterized in a solution state and can be processed by a solution method, and is further characterized by the PASS, so that the PASS is an ideal phase transfer film-forming material. Most of filtering membranes in the current market use Polyester (PET) non-woven fabrics as supporting layers to prepare ultrafiltration membranes, the heat resistance and the acid and alkali resistance are influenced by the performance of PET materials, the industrial application range of the ultrafiltration membranes is greatly limited, and the PASS/PP high-flux tubular ultrafiltration membrane resistant to acid and alkali is designed based on the reason.
Disclosure of Invention
According to the invention, a PASS ultrathin filtering compact layer is prepared by using a porous PP material as a supporting base material of a tubular membrane and coating the inner wall of a PP base material tube by a phase inversion method, so that the high-flux PASS/PP tubular ultrafiltration membrane with good acid and alkali resistance and high temperature resistance is prepared.
The invention is realized by the following technical scheme:
1) preparing a casting solution: mixing PASS, a pore-forming agent, lithium chloride and a solvent according to a formula, stirring to completely dissolve all components to obtain a membrane casting solution, and standing and defoaming the membrane casting solution under a vacuum condition for later use;
2) uniformly coating the casting solution prepared in the previous step on the inner wall of the PP porous support membrane tube;
3) and 2, standing the PP porous supporting membrane tube coated in the step 2 in the air, then immersing the PP porous supporting membrane tube into a coagulating bath, and performing phase separation on a membrane casting liquid layer coated on the surface of the PP porous material by using a phase inversion method to form a separation membrane to obtain the target product.
Further selection is carried out: in the step 1), the mixed components are heated to 60-75 ℃ in a water bath and stirred to be completely dissolved.
Standing the casting solution in the step 1) under a vacuum condition for 12-15H;
the pore-forming agent in the step 1) is selected from one or more of PVPk12-50 and PEG200-20000 related series products, preferably PVPK12, PVPK15, PVPK30, PEG2000, PEG6000 and the like;
the solvent is selected from DMF, DMAc or NMP, preferably DMAc;
the casting solution comprises the following components in percentage by weight: PASS 10-20%, pore-forming agent 10-20%, lithium chloride 1-5%, and the balance solvent.
The coagulating bath in the step 3) is composed of 20-70% of ethanol water solution by mass percentage.
The material used for the ultrasonic welding support tube is PP porous membrane or PP non-woven fabric.
The innovation point of the application is as follows: the pore-forming agent and the additive are added in the preparation process of the membrane casting solution, and the addition of the pore-forming agent and the additive can influence the mutual diffusion speed between the solvent and water in the phase inversion process, so that the addition amount of the pore-forming agent and the additive is optimized, and the separation membrane has a good pore structure.
This application advantage: the membrane has excellent performances of good hydrophilicity (the contact angle is less than or equal to 30 degrees), high temperature resistance (-20-180 ℃), acid and alkali resistance (pH 1-13) and the like, and can be widely applied to the fields of medicine, food, acid and alkali recovery, industrial water treatment, petrochemical industry and the like.
Drawings
FIG. 1 is an electron microscope picture of the PASS/PP tubular ultrafiltration membrane prepared by the present application.
Detailed Description
The present invention will be described in detail with reference to examples, which are not specifically described below, and the percentages given below are by mass.
Example 1:
the components with the mass percentage of 20 percent of PASS, 1510 percent of PVPK, 20002 percent of PEG and 3 percent of lithium chloride are placed in a three-hole flask, 65 percent of DMAc is added to mix the components, the mixture is heated to 75 ℃ in a water bath and stirred for 8 hours at constant speed and constant temperature, and the components are fully mixed to obtain the casting solution. And standing and defoaming the casting solution for 12 hours under a vacuum condition, uniformly coating the casting solution on the inner wall of a porous PP supporting tube prepared by synchronous ultrasonic welding, quickly immersing the inner wall of the porous PP supporting tube into a 20% ethanol water solution coagulating bath at the temperature of 45 ℃ to form a film, taking out the film tube in the coagulating bath, and immersing the film tube in pure water at the temperature of 25 ℃ for 2 days. Then flux and retention rate tests are carried out on the prepared tubular membrane product, and the result shows that the membrane water flux is 550L/m under 0.1Mpa2h, the bovine serum albumin retention rate is about 52%.
Example 2:
15 percent of PASS, 3010 percent of PVPK, 60003 percent of PEG and 2 percent of lithium chloride are put into a three-hole flask by mass percent, and then 70 percent of DMAc is added to mix the components, the mixture is heated to 75 ℃ in a water bath and stirred for 8 hours at constant speed and constant temperature, so that the components are fully mixed to obtain the casting solution. And standing and defoaming the casting solution for 12 hours under a vacuum condition, uniformly coating the casting solution on the inner wall of a porous PP supporting tube prepared by synchronous ultrasonic welding, quickly immersing the inner wall of the porous PP supporting tube into a 20% ethanol water solution coagulating bath at the temperature of 45 ℃ to form a film, taking out the film tube in the coagulating bath, and immersing the film tube in pure water at the temperature of 25 ℃ for 2 days. Then flux and retention rate tests are carried out on the prepared tubular membrane product, and the result shows that the membrane water flux is 670L/m under 0.1Mpa2h, the bovine serum albumin retention rate is about 45%.
Example 3:
placing PASS 12%, PVPK 3012%, PEG 60005% and lithium chloride 1% in a three-hole flask, adding DMAc 70% to mix the components, heating the mixture in a water bath to 75 ℃, stirring the mixture for 8 hours at a constant speed and a constant temperature to fully mix the components to obtain a casting solution. And standing and defoaming the casting solution for 12 hours under a vacuum condition, uniformly coating the casting solution on the inner wall of a porous PP supporting tube prepared by synchronous ultrasonic welding, quickly immersing the porous PP supporting tube into 20% ethanol water solution coagulating bath at the temperature of 45 ℃ to form a film, taking out the film tube in the coagulating bath, and immersing the film tube in pure water at the temperature of 25 ℃ for 2 days. Then flux and retention rate tests are carried out on the prepared tubular membrane product, and the result shows that the membrane water flux is 780L/m under 0.1Mpa2h, the bovine serum albumin retention rate is about 25%.
Claims (2)
1. A PASS/PP high-flux tubular ultrafiltration membrane is characterized by being prepared by the following method:
(1) preparing a casting solution: mixing polyarylene sulfide sulfone (PASS), a pore-forming agent, lithium chloride and a solvent according to a formula, stirring and dissolving to obtain a membrane casting solution, and standing and defoaming under a vacuum condition for later use;
(2) uniformly coating the casting solution prepared in the step (1) on the inner wall of the PP porous support membrane tube;
(3) standing the coated PP porous supporting membrane tube in air, then immersing the PP porous supporting membrane tube into a coagulating bath, and carrying out phase separation on a casting membrane liquid layer coated on the surface of the PP porous material to form a separation membrane to obtain a target object;
the casting solution comprises the following components in percentage by weight: PASS10% -20%, pore-forming agent 10% -20%, lithium chloride 1% -5%, and the balance solvent;
the pore-foaming agent in the step 1) is selected from one or more of PVPk12-50 and PEG200-20000 series products;
step 1) the solvent is selected from DMF, DMAc, or NMP;
the coagulating bath in the step 3) is an ethanol water solution with the mass percentage of 20% -70%.
2. The PASS/PP high flux tubular ultrafiltration membrane according to claim 1, wherein the pore-forming agent is selected from one or two of PVPK12, PVPK15, PVPK30, PEG2000 and PEG 6000; the solvent is selected from DMAc.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110640355.7A CN113426308A (en) | 2021-06-09 | 2021-06-09 | Acid-base-resistant and high-temperature-resistant PASS/PP high-flux tubular ultrafiltration membrane |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202110640355.7A CN113426308A (en) | 2021-06-09 | 2021-06-09 | Acid-base-resistant and high-temperature-resistant PASS/PP high-flux tubular ultrafiltration membrane |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102824860A (en) * | 2012-09-10 | 2012-12-19 | 四川大学 | Preparation method of high-corrosion-resistance polyarylene sulfide sulfone separation membrane |
| CN104226130A (en) * | 2014-09-18 | 2014-12-24 | 四川大学 | Method for preparing PASS (polyarylenesulfidesulfone) separation membrane in two coagulating baths |
| US20180085712A1 (en) * | 2016-01-22 | 2018-03-29 | Nanjing University Of Science And Technology | Ultrafiltration membrane and a preparation method thereof |
| CN108355499A (en) * | 2018-03-23 | 2018-08-03 | 海南立昇净水科技实业有限公司 | Double separating layer hollow fiber ultrafiltration membranes of the net containing tubular support and preparation method thereof |
| CN109453673A (en) * | 2018-10-17 | 2019-03-12 | 三达膜科技（厦门）有限公司 | A kind of preparation method of inner support polyethersulfone hollow fiber ultrafiltration membrane |
-
2021
- 2021-06-09 CN CN202110640355.7A patent/CN113426308A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102824860A (en) * | 2012-09-10 | 2012-12-19 | 四川大学 | Preparation method of high-corrosion-resistance polyarylene sulfide sulfone separation membrane |
| CN104226130A (en) * | 2014-09-18 | 2014-12-24 | 四川大学 | Method for preparing PASS (polyarylenesulfidesulfone) separation membrane in two coagulating baths |
| US20180085712A1 (en) * | 2016-01-22 | 2018-03-29 | Nanjing University Of Science And Technology | Ultrafiltration membrane and a preparation method thereof |
| CN108355499A (en) * | 2018-03-23 | 2018-08-03 | 海南立昇净水科技实业有限公司 | Double separating layer hollow fiber ultrafiltration membranes of the net containing tubular support and preparation method thereof |
| CN109453673A (en) * | 2018-10-17 | 2019-03-12 | 三达膜科技（厦门）有限公司 | A kind of preparation method of inner support polyethersulfone hollow fiber ultrafiltration membrane |
Non-Patent Citations (4)
| Title |
|---|
| 何领好等: "《功能高分子材料》", 31 August 2016, 华中科技大学出版社 * |
| 文佩: "聚醚砜（PES）超滤膜的结构与亲水性能的改善", 《中国学位论文全文数据库》 * |
| 王孝军等: "聚芳硫醚砜分离膜的制备――制膜条件对分离性能的影响", 《高分子材料科学与工程》 * |
| 王孝军等: "聚芳硫醚砜分离膜的制备――相图及微观结构", 《四川大学学报(工程科学版)》 * |
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Application publication date: 20210924 |