CN106621865A - Polyamide nano-filtration separation membrane and preparation method thereof - Google Patents
Polyamide nano-filtration separation membrane and preparation method thereof Download PDFInfo
- Publication number
- CN106621865A CN106621865A CN201611170788.6A CN201611170788A CN106621865A CN 106621865 A CN106621865 A CN 106621865A CN 201611170788 A CN201611170788 A CN 201611170788A CN 106621865 A CN106621865 A CN 106621865A
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- parts
- separation membrane
- seperation film
- filtration separation
- basement membrane
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Classifications
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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
-
- 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
-
- 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
- B01D69/12—Composite membranes; Ultra-thin membranes
- B01D69/125—In situ manufacturing by polymerisation, polycondensation, cross-linking or chemical reaction
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/30—Chemical resistance
Abstract
The invention relates to a polyamide nano-filtration separation membrane and a preparation method thereof and belongs to the technical field of nano-filtration separation membranes. The polyamide nano-filtration separation membrane comprises a cut polysulfone basal membrane and is prepared from the following raw materials in parts by weight: 40 to 50 parts of a m-phenylenediamine water solution, 5 to 10 parts of trimesoyl chloride, 3 to 5 parts of sodium dodecyl sulfate, 40 to 50 parts of distilled water, 2 to 3 parts of camphorsulfonic acid, 3 to 5 parts of an isopropyl alcohol water solution and 30 to 50 parts of n-hexane. By adopting the polyamide nano-filtration separation membrane provided by the invention, process conditions of interface polymerization are improved, and the polyamide nano-filtration separation membrane which has relatively good comprehensive mechanical properties, relatively reasonable pore structure, large flux and high rejection rate is prepared. The oxidization resistance, anti-scaling and anti-pollution capabilities and chlorine resistance of the separation membrane are greatly improved.
Description
Technical field
The present invention relates to a kind of seperation film and preparation method thereof, it is more particularly related to a kind of polyamide nanofiltration
Seperation film and preparation method thereof, belongs to nanofiltration separation technical field of membrane.
Background technology
In recent decades, polymeric membrane is widely used in various gases, liquid separation field, such as micro-filtration, ultrafiltration, counter-infiltration
Obtain a wide range of applications with nanofiltration.NF membrane (Nanofiltration membranes) is to come out the eighties in 20th century
Novel separation film, its separating property is between counter-infiltration and ultrafiltration, and operating pressure is relatively low, has different choosings to one, divalent ion
Selecting property, there is higher retention characteristic to small organic molecule.NF membrane has been widely used in food, petrochemical industry, medicine, metallurgy etc.
In field.Membrane material is the core of membrane technology.The ultra-thin one polymer of the composite membrane of commercial successful Application is mostly fragrant polyamides
Amine.
Aromatic polyamide film has that salt rejection rate is high, flux is big, chemical stability is excellent, using pH wide ranges (4-11),
Resistance to biodegradable, operating pressure requires low advantage, but not resistance to oxidation, and ant-scaling and pollution capacity are poor, and chlorine resistance is poor.Exploitation is new
Type functional polymer membrane material, strengthen and activating technology ultra-thin to hymeniderm layer research, prepare resistance to oxidation, resistance to free chlorine and antipollution
Composite membrane tool is of great significance.
The content of the invention
Present invention seek to address that polyamide nanofiltration membrane of the prior art not resistance to oxidation, ant-scaling and pollution capacity are poor, resistance to
The problem of chlorine difference, there is provided a kind of polyamide nanofiltration seperation film, the oxidative resistance of the polyamide nanofiltration seperation film, ant-scaling and dirt
Dye ability and chlorine resistance are obtained for very big raising.
In order to realize foregoing invention purpose, its specific technical scheme is as follows：
A kind of polyamide nanofiltration seperation film, it is characterised in that：Including the polysulfones basement membrane for cutting, using following according to parts by weight
The raw material of meter is made：
M-phenylene diamine (MPD) aqueous solution 40-50 parts
Pyromellitic trimethylsilyl chloride 5-10 parts
Lauryl sodium sulfate 3-5 part
Distilled water 40-50 parts
Camphorsulfonic acid 2-3 parts
Isopropanol aqueous 3-5 part
N-hexane 30-50 parts.
The concentration of the m-phenylene diamine (MPD) aqueous solution of the present invention is 3-5%.
A kind of preparation method of polyamide nanofiltration seperation film, it is characterised in that：Comprise the following steps that：
It is A, with alcohol or acetone that the polysulfones membrane surface for cutting process is clean, it is standby；
B, each group component is accurately weighed by recipe requirements, and prepared respectively；M-phenylene diamine (MPD) is dissolved in into cushioning liquid isophthalic is obtained
Two amine aqueous solutions are water phase；Pyromellitic trimethylsilyl chloride is dissolved in n-hexane oil phase is obtained, it is standby；
C, by the upper surface of the polysulfones basement membrane for cleaning in advance immersion water phase；Polysulfones basement membrane is taken out, the unnecessary aqueous solution is discharged；
Polysulfones basement membrane is immersed in oil phase and is reacted the 20-30 seconds, quickly removed, drain；
D, 12h is dried in atmosphere, interfacial chemical reaction 3-5h is continued at 40-60 DEG C, obtain final product polyamide nanofiltration seperation film.
The Advantageous Effects that the present invention brings：
The present invention is that new aqueous phase monomers constitute the reaction system of interfacial polymerization with pyromellitic trimethylsilyl chloride with m-phenylene diamine (MPD), and is added
Various auxiliary agents, improve the process conditions of interfacial polymerization, prepare comprehensive mechanics preferably, pore structure relatively reasonable flux
Greatly, the high polyamide nanofiltration seperation film of rejection.The oxidative resistance of the seperation film, ant-scaling and pollution capacity and chlorine resistance are all
It is greatly improved.
Specific embodiment
Embodiment 1
A kind of polyamide nanofiltration seperation film, including the polysulfones basement membrane for cutting, using following raw materials by weight system
Into：
40 parts of the m-phenylene diamine (MPD) aqueous solution
5 parts of pyromellitic trimethylsilyl chloride
3 parts of lauryl sodium sulfate
40 parts of distilled water
2 parts of camphorsulfonic acid
3 parts of isopropanol aqueous
30 parts of n-hexane.
Embodiment 2
A kind of polyamide nanofiltration seperation film, including the polysulfones basement membrane for cutting, using following raw materials by weight system
Into：
50 parts of the m-phenylene diamine (MPD) aqueous solution
10 parts of pyromellitic trimethylsilyl chloride
5 parts of lauryl sodium sulfate
50 parts of distilled water
3 parts of camphorsulfonic acid
5 parts of isopropanol aqueous
50 parts of n-hexane.
Embodiment 3
A kind of polyamide nanofiltration seperation film, including the polysulfones basement membrane for cutting, using following raw materials by weight system
Into：
45 parts of the m-phenylene diamine (MPD) aqueous solution
7 parts of pyromellitic trimethylsilyl chloride
4 parts of lauryl sodium sulfate
45 parts of distilled water
2.5 parts of camphorsulfonic acid
4 parts of isopropanol aqueous
40 parts of n-hexane.
Embodiment 4
A kind of preparation method of polyamide nanofiltration seperation film, comprises the following steps that：
It is A, with alcohol or acetone that the polysulfones membrane surface for cutting process is clean, it is standby；
B, each group component is accurately weighed by recipe requirements, and prepared respectively；M-phenylene diamine (MPD) is dissolved in into cushioning liquid isophthalic is obtained
Two amine aqueous solutions are water phase；Pyromellitic trimethylsilyl chloride is dissolved in n-hexane oil phase is obtained, it is standby；
C, by the upper surface of the polysulfones basement membrane for cleaning in advance immersion water phase；Polysulfones basement membrane is taken out, the unnecessary aqueous solution is discharged；
Polysulfones basement membrane is immersed in oil phase and is reacted 20 seconds, quickly removed, drain；
D, 12h is dried in atmosphere, interfacial chemical reaction 3h is continued at 40 DEG C, obtain final product polyamide nanofiltration seperation film.
Embodiment 5
A kind of preparation method of polyamide nanofiltration seperation film, comprises the following steps that：
It is A, with alcohol or acetone that the polysulfones membrane surface for cutting process is clean, it is standby；
B, each group component is accurately weighed by recipe requirements, and prepared respectively；M-phenylene diamine (MPD) is dissolved in into cushioning liquid isophthalic is obtained
Two amine aqueous solutions are water phase；Pyromellitic trimethylsilyl chloride is dissolved in n-hexane oil phase is obtained, it is standby；
C, by the upper surface of the polysulfones basement membrane for cleaning in advance immersion water phase；Polysulfones basement membrane is taken out, the unnecessary aqueous solution is discharged；
Polysulfones basement membrane is immersed in oil phase and is reacted 30 seconds, quickly removed, drain；
D, 12h is dried in atmosphere, interfacial chemical reaction 3-5h is continued at 60 DEG C, obtain final product polyamide nanofiltration seperation film.
Embodiment 6
A kind of preparation method of polyamide nanofiltration seperation film, comprises the following steps that：
It is A, with alcohol or acetone that the polysulfones membrane surface for cutting process is clean, it is standby；
B, each group component is accurately weighed by recipe requirements, and prepared respectively；M-phenylene diamine (MPD) is dissolved in into cushioning liquid isophthalic is obtained
Two amine aqueous solutions are water phase；Pyromellitic trimethylsilyl chloride is dissolved in n-hexane oil phase is obtained, it is standby；
C, by the upper surface of the polysulfones basement membrane for cleaning in advance immersion water phase；Polysulfones basement membrane is taken out, the unnecessary aqueous solution is discharged；
Polysulfones basement membrane is immersed in oil phase and is reacted 25 seconds, quickly removed, drain；
D, 12h is dried in atmosphere, interfacial chemical reaction 4h is continued at 50 DEG C, obtain final product polyamide nanofiltration seperation film.
Claims (3)
1. a kind of polyamide nanofiltration seperation film, it is characterised in that：Including the polysulfones basement membrane for cutting, using following according to weight portion
The raw material of number meter is made：
M-phenylene diamine (MPD) aqueous solution 40-50 parts
Pyromellitic trimethylsilyl chloride 5-10 parts
Lauryl sodium sulfate 3-5 part
Distilled water 40-50 parts
Camphorsulfonic acid 2-3 parts
Isopropanol aqueous 3-5 part
N-hexane 30-50 parts.
2. a kind of polyamide nanofiltration seperation film according to claim 1, it is characterised in that：The described m-phenylene diamine (MPD) aqueous solution
Concentration be 3-5%.
3. the preparation method of a kind of polyamide nanofiltration seperation film according to claim 1, it is characterised in that：Including following work
Skill step：
It is A, with alcohol or acetone that the polysulfones membrane surface for cutting process is clean, it is standby；
B, each group component is accurately weighed by recipe requirements, and prepared respectively；M-phenylene diamine (MPD) is dissolved in into cushioning liquid isophthalic is obtained
Two amine aqueous solutions are water phase；Pyromellitic trimethylsilyl chloride is dissolved in n-hexane oil phase is obtained, it is standby；
C, by the upper surface of the polysulfones basement membrane for cleaning in advance immersion water phase；Polysulfones basement membrane is taken out, the unnecessary aqueous solution is discharged；
Polysulfones basement membrane is immersed in oil phase and is reacted the 20-30 seconds, quickly removed, drain；
D, 12h is dried in atmosphere, interfacial chemical reaction 3-5h is continued at 40-60 DEG C, obtain final product polyamide nanofiltration seperation film.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201611170788.6A CN106621865A (en) | 2016-12-16 | 2016-12-16 | Polyamide nano-filtration separation membrane and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611170788.6A CN106621865A (en) | 2016-12-16 | 2016-12-16 | Polyamide nano-filtration separation membrane and preparation method thereof |
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| CN106621865A true CN106621865A (en) | 2017-05-10 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107376674A (en) * | 2017-08-09 | 2017-11-24 | 哈尔滨工业大学 | Improve the method for modifying of fungus resistance in a kind of POSS plate armours polyamide reverse osmose membrane surface |
| CN111569675A (en) * | 2020-05-28 | 2020-08-25 | 西北大学 | Reverse osmosis membrane based on dimethyl carbonate and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103768963A (en) * | 2014-01-23 | 2014-05-07 | 南通苏通分离工程科技有限公司 | Preparation method for polyamide composite nanofiltration membrane |
-
2016
- 2016-12-16 CN CN201611170788.6A patent/CN106621865A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103768963A (en) * | 2014-01-23 | 2014-05-07 | 南通苏通分离工程科技有限公司 | Preparation method for polyamide composite nanofiltration membrane |
Non-Patent Citations (1)
| Title |
|---|
| 王元等: "复合催化剂对聚酰胺纳滤膜结构和性能的影响", 《膜科学与技术》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107376674A (en) * | 2017-08-09 | 2017-11-24 | 哈尔滨工业大学 | Improve the method for modifying of fungus resistance in a kind of POSS plate armours polyamide reverse osmose membrane surface |
| CN107376674B (en) * | 2017-08-09 | 2020-05-26 | 哈尔滨工业大学 | Modification method for improving antibacterial property of POSS armored polyamide reverse osmosis membrane surface |
| CN111569675A (en) * | 2020-05-28 | 2020-08-25 | 西北大学 | Reverse osmosis membrane based on dimethyl carbonate and preparation method thereof |
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Application publication date: 20170510 |