CN106563360A - Preparation method of low-charge reverse osmosis composite film - Google Patents
Preparation method of low-charge reverse osmosis composite film Download PDFInfo
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- CN106563360A CN106563360A CN201610943710.7A CN201610943710A CN106563360A CN 106563360 A CN106563360 A CN 106563360A CN 201610943710 A CN201610943710 A CN 201610943710A CN 106563360 A CN106563360 A CN 106563360A
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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
- B01D71/76—Macromolecular material not specifically provided for in a single one of groups B01D71/08 - B01D71/74
- B01D71/82—Macromolecular material not specifically provided for in a single one of groups B01D71/08 - B01D71/74 characterised by the presence of specified groups, e.g. introduced by chemical after-treatment
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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
- B01D67/0006—Organic membrane manufacture by chemical reactions
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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
- B01D69/10—Supported membranes; Membrane supports
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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
- B01D2325/14—Membrane materials having negatively charged functional groups
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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
- B01D2325/16—Membrane materials having positively charged functional groups
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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
- B01D2325/18—Membrane materials having mixed charged functional groups
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- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention relates to a low-charge reverse osmosis composite film and a preparation method thereof. The low-charge reverse osmosis composite film comprises non-woven fabric, a polysulfone supporting layer and a low-charge polyamide separation layer. The technical scheme is that acyl chloride groups remaining on the surface of an aromatic polyamide reverse osmosis film during the forming early period of the aromatic polyamide reverse osmosis film and macromolecules containing active groups react, so that a low-charge protective layer is introduced on the surface of the aromatic polyamide reverse osmosis composite film in a chemical bond form. The preparation method has the advantages that chemical bonds of the polyamide separation layer and the protective layer are connected, the purpose of permanently protecting the aromatic polyamide reverse osmosis composite film is achieved, the interfacial polymerization process is not affected, and high desalinization rate of the aromatic polyamide reverse osmosis composite film is guaranteed. The low-charge reverse osmosis composite film has wide application and the preparation method is simple.
Description
Technical field
The invention belongs to water-treatment technology field, and in particular to a kind of preparation method of low electric charge reverse osmosis composite membrane.
Background technology
Since the 1950's, Reid is made after reverse osmosis membrane with the homogenizing acetate fiber of 6 μ m-thicks, reverse osmosis membrane separation
Technology has been widely used in the fields such as sea-water brackish water desalination, the preparation of pure water ultra-pure water, drink water purifying, Treated sewage reusing.Its
In, there is height by the aromatic polyamides reverse osmosis composite membrane that interfacial polymerization is prepared from by m-diaminobenzene., pyromellitic trimethylsilyl chloride
The advantages of desalination, big flux, it has also become the main product in reverse osmosiss field.But in actual use, tie including inorganic matters
Dirt, biological pollution, colloid pollution have seriously restricted further should for aromatic polyamides reverse osmosis composite membrane in interior fouling membrane
With.Correlational study shows that most pollutant are to adsorb deposition to film surface by electrostatic interaction or hydrophobic interaction.Therefore
Prepare a kind of low electric charge, high hydrophilic reverse osmosis composite membrane and be of great significance to improving its antifouling property tool.
At present, common polyamide functional layer process for modifying surface is mainly, in existing reverse osmosis composite membrane surface physics
Coating or processes for chemically crosslinked polyethylene alcohol macromole, form hydration layer and protect reverse osmosis membrane not contaminated, such as CN1213985,
CN101130444 etc., but the polyvinyl alcohol protective layer adhesion deposited due to polyamide stratum disjunctum and surface is weaker, easily in reality
Fall off in the running of border, the separating property even basic so as to lose antifouling property.For improve anti-pollution layer with it is anti-
The adhesion of osmosis composite membrane, patent CN102228809, CN102553458 etc. at high temperature can be with polyamides using epoxide group
The characteristics of active group reacts in amine layer, anti-pollution layer, polyamide stratum disjunctum are connected in the form of chemical bond, so as to effectively change
The weak problem of kind anti-pollution layer cohesive force, but the method needs to prepare the aromatic polyamides reverse osmosis composite membrane that completes and enters again
Row high-temperature heat treatment, easily affects microstructure or the physico-chemical property of polyamide stratum disjunctum or polysulfone supporting layer, reduces reverse osmosiss
The separating property of composite membrane, such as permeation flux reduce or inorganic salt rejection rate declines etc..Additionally, patent CN102921315 then exists
Polyvinyl alcohol molecule is introduced in aqueous phase solution containing polyfunctional group amine, reaction is carried out with polynary acyl chlorides and is formed after polyamide desalination layer
It is chemically crosslinked again, polyamide desalination layer is chemically bound together with polyvinyl alcohol crosslinked coating, is improved poly- second
The adhesive force of enol coating, but as polyvinyl alcohol is polymer-function material, polyamine can be affected to carry out boundary with polynary acyl chlorides
Face is polymerized, and forms more loose polyamide desalination layer, final to limit interception capacity of the reverse osmosis composite membrane to high salinity solution.
The content of the invention
To solve above-mentioned technical problem, the present invention provides a kind of low electric charge reverse osmosis composite membrane and preparation method thereof, existing
On the basis of having conventional interface polymerization to prepare aromatic polyamides reverse osmosis composite membrane, the initial stage is formed using aromatic polyamides molecule residual
The acid chloride groups stayed, are reacted with the macromole containing active group, so as to not affect polyamine poly- with polynary acyl chlorides interface
On the premise of conjunction, light current macromole is introduced on polyamide molecule surface in the form of chemical bond, with original polyamide molecule
Low electric charge polyamide stratum disjunctum is formed together, the high desalination layer function of aramid layer had both been ensure that, realizes permanent protection virtue again
The purpose of fragrant polyamide reverse osmosis composite film.
The preparation method of the low electric charge reverse osmosis composite membrane of the present invention, including non-woven fabrics, polysulfone supporting layer, low electric charge polyamides
Amine stratum disjunctum, the polysulfones microporous membrane that described low electric charge polyamide stratum disjunctum is made up of non-woven fabrics and polysulfone supporting layer successively with
Aqueous phase solution containing m-diaminobenzene., the organic phase solution containing pyromellitic trimethylsilyl chloride, the contact of the aqueous solution containing light current macromole, and
Carry out heat treatment and be obtained.
The preparation method of the low electric charge reverse osmosis composite membrane of the present invention, the light current macromole is containing in amino, hydroxyl
One or two functional groups water-soluble macromolecule.
Light current macromole described in the preparation method of the low electric charge reverse osmosis composite membrane of the present invention is polyvinyl alcohol, gathers
The mixture of one or more in ethylene glycol or polyethyleneimine.
Described in the preparation method of the low electric charge reverse osmosis composite membrane of the present invention, the quality of light current macromolecular aqueous solution is dense
Spend for 0.001%～1.0%.Used as more preferably selecting, the mass concentration of light current macromolecular aqueous solution is 0.1%.
The low electric charge reverse osmosis composite membrane of the present invention, described heat treatment temperature are 50 DEG C～100 DEG C.As optimum temperature
Temperature is selected, and data result when heat treatment temperature is 80 DEG C is best.
Beneficial effect：
Compared with prior art：The present invention forms acyl chlorides of the initial stage in film remained on surface using aromatic polyamides reverse osmosis membrane
Group, and is reacted containing the macromole of active group, so as in the form of chemical bond in aromatic polyamides reverse osmosis composite membrane
Surface introduces light current macromole.On the one hand, realize that polyamide stratum disjunctum is chemical bonded with protective layer, effectively solving polyamides
The weak problem of cohesive force between amine stratum disjunctum and protective layer, it is ensured that its stability in actual use, reaches permanent
The purpose of protection aromatic polyamides reverse osmosis composite membrane；On the other hand, polyamine is not being affected with polynary acyl chlorides interfacial polymerization shape
Into stratum disjunctum on the premise of, do not increase extra heat treatment, realize that interfacial polymerization heat treatment is same with surface functional layer heat treatment
Step is carried out, and advantageously ensures that the equipment with high desalinization and easy preparative of aromatic polyamides reverse osmosis composite membrane.
Specific embodiment
Enforcement to the present invention below is illustrated；
Comparative example 1
The complex reverse osmosis membrane comprising nonwoven layer, polysulfone supporting layer and aramid layer is prepared according to a conventional method.
First by the polysulfones microporous membrane being made up of non-woven fabrics, polysulfone supporting layer water phase of the immersion containing 2.0wt% m-diaminobenzene .s
In solution, the polysulfones microporous membrane being had with 0.2wt% pyromellitic trimethylsilyl chlorides are contained after the solution of excess surface is removed with rubber rollers
Machine phase solution is contacted 1 minute, and heat treatment 10 minutes in 80 DEG C of baking oven, obtains polyamide reverse osmosis composite film.
Determine film surface water contact angle and Zeta potential (pH=7.0), then pressure be 225PSI, temperature be 25 DEG C,
PH value is the initial desalination of test compound reverse osmosis membrane under conditions of 6.5～7.5, charging is 2000mg/l sodium-chloride water solutions
Rate and water flux, acquired results are shown in Table 1.
Embodiment 1：
First by the polysulfones microporous membrane being made up of non-woven fabrics, polysulfone supporting layer water phase of the immersion containing 2.0wt% m-diaminobenzene .s
In solution, the polysulfones microporous membrane being had with 0.2wt% pyromellitic trimethylsilyl chlorides are contained after the solution of excess surface is removed with rubber rollers
Machine phase solution contact 1 minute, with rubber rollers remove excess surface solution after again with containing 0.1wt% polyvinyl alcohol aqueous solution
Contact 1 minute, and heat treatment 10 minutes in 80 DEG C of baking oven, obtain low electric charge polyamide reverse osmosis composite film.
Determine film surface water contact angle and Zeta potential (pH=7.0), then pressure be 225PSI, temperature be 25 DEG C,
PH value is the initial desalination of test compound reverse osmosis membrane under conditions of 6.5～7.5, charging is 2000mg/l sodium-chloride water solutions
Rate and water flux, acquired results are shown in Table 1.
Embodiment 2：
First by the polysulfones microporous membrane being made up of non-woven fabrics, polysulfone supporting layer water phase of the immersion containing 2.0wt% m-diaminobenzene .s
In solution, the polysulfones microporous membrane being had with 0.2wt% pyromellitic trimethylsilyl chlorides are contained after the solution of excess surface is removed with rubber rollers
Machine phase solution contact 1 minute, with rubber rollers remove excess surface solution after again with containing 0.5wt% polyvinyl alcohol aqueous solution
Contact 1 minute, and heat treatment 10 minutes in 80 DEG C of baking oven, obtain low electric charge polyamide reverse osmosis composite film.
Determine film surface water contact angle and Zeta potential (pH=7.0), then pressure be 225PSI, temperature be 25 DEG C,
PH value is the initial desalination of test compound reverse osmosis membrane under conditions of 6.5～7.5, charging is 2000mg/l sodium-chloride water solutions
Rate and water flux, acquired results are shown in Table 1.
Embodiment 3：
First by the polysulfones microporous membrane being made up of non-woven fabrics, polysulfone supporting layer water phase of the immersion containing 2.0wt% m-diaminobenzene .s
In solution, the polysulfones microporous membrane being had with 0.2wt% pyromellitic trimethylsilyl chlorides are contained after the solution of excess surface is removed with rubber rollers
Machine phase solution contact 1 minute, with rubber rollers remove excess surface solution after again with containing 0.1wt% Polyethylene Glycol aqueous solution
Contact 1 minute, and heat treatment 10 minutes in 80 DEG C of baking oven, obtain low electric charge polyamide reverse osmosis composite film.
Determine film surface water contact angle and Zeta potential (pH=7.0), then pressure be 225PSI, temperature be 25 DEG C,
PH value is the initial desalination of test compound reverse osmosis membrane under conditions of 6.5～7.5, charging is 2000mg/l sodium-chloride water solutions
Rate and water flux, acquired results are shown in Table 1.
Embodiment 4：
First by the polysulfones microporous membrane being made up of non-woven fabrics, polysulfone supporting layer water phase of the immersion containing 2.0wt% m-diaminobenzene .s
In solution, the polysulfones microporous membrane being had with 0.2wt% pyromellitic trimethylsilyl chlorides are contained after the solution of excess surface is removed with rubber rollers
Machine phase solution is contacted 1 minute, removed with rubber rollers after the solution of excess surface again with it is water-soluble containing 0.1wt% polyethyleneimine
Liquid is contacted 1 minute, and heat treatment 10 minutes in 80 DEG C of baking oven, obtains low electric charge polyamide reverse osmosis composite film.
Determine film surface water contact angle and Zeta potential (pH=7.0), then pressure be 225PSI, temperature be 25 DEG C,
PH value is the initial desalination of test compound reverse osmosis membrane under conditions of 6.5～7.5, charging is 2000mg/l sodium-chloride water solutions
Rate and water flux, acquired results are shown in Table 1.
Table 1：Composite film surface characteristic and separating property
From table 1 it follows that after introducing light current macromole, the water contact on aromatic polyamides reverse osmosis composite membrane surface
There is different degrees of decline in angle, elecrtonegativity, water contact angle decline be due to introduced macromole contain abundant hydroxyl or
Amino, with good hydrophilic；And after elecrtonegativity decline is then because that film surface introduces light current macromole, aromatic polyamides
Reverse osmosis composite membrane surface forms uniform light current protective layer, on the one hand consumes the acid chloride groups of residual, prevent its hydrolysis and
The stronger carboxyl of electronegativity is produced, the protective layer of another aspect light current can effectively shield the electronegativity of polyamide molecule, so as to
Realize the preparation of low electric charge reverse osmosis composite membrane.
Additionally, electronegative fall is also relevant with the concentration and physico-chemical structure of introduced macromole, work as polyvinyl alcohol
When molecular mass concentration is 0.5wt%, the reverse osmosis composite membrane surface electronegativity of preparation is 0.1wt% significantly lower than mass concentration
When reverse osmosis composite membrane, this be likely due to mass concentration it is higher when, the polyvinyl alcohol molecule number in solution is more, more can hold
Easily deposit to reverse osmosis composite membrane surface, form more uniform protective layer；Under identical mass concentration, prepared by polyethyleneimine
The reverse osmosis composite membrane that reverse osmosis composite membrane surface electronegativity is then prepared significantly lower than polyvinyl alcohol, this is mainly due to polyethylene
Imines can consume more acid chloride groups with the higher amino of a large amount of reactivities, and under the conditions of identical pH, amino
Electronegativity is weaker than hydroxyl.
Comparative examples 1 and embodiment 1-4, the present invention prepare low electric charge reverse osmosis composite membrane with routine techniquess system
The same superior salt rejection rate of standby complex reverse osmosis membrane.
Claims (5)
1. a kind of preparation method of low electric charge reverse osmosis composite membrane, including non-woven fabrics, polysulfone supporting layer, low electric charge polyamide separation
Layer, it is characterised in that：Described low electric charge polyamide stratum disjunctum, the polysulfones microporous membrane being made up of non-woven fabrics and polysulfone supporting layer
Successively with the aqueous phase solution containing m-diaminobenzene., the organic phase solution containing pyromellitic trimethylsilyl chloride, the aqueous solution containing light current macromole
Contact, is placed in heat treatment in 50～100 DEG C of baking oven and obtains.
2. the preparation method of low electric charge reverse osmosis composite membrane according to claim 1, it is characterised in that：Described light current
Macromole is the water-soluble macromolecule containing one or two functional groups in amino, hydroxyl.
3. the preparation method of low electric charge reverse osmosis composite membrane according to claim 1, it is characterised in that：Described light current
Macromole is the mixture of one or more in polyvinyl alcohol, Polyethylene Glycol or polyethyleneimine.
4. the preparation method of low electric charge reverse osmosis composite membrane according to claim 1, it is characterised in that：The light current is big
The mass concentration of molecule aqueous solution is 0.001%～1.0%.
5. the preparation method of low electric charge reverse osmosis composite membrane according to claim 4, it is characterised in that：The light current is big
The mass concentration of molecule aqueous solution is 0.1%.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107213804A (en) * | 2017-07-18 | 2017-09-29 | 宁波日新恒力科技有限公司 | A kind of antibacterial reverse osmosis composite membrane and its preparation method and application |
| CN107694357A (en) * | 2017-11-22 | 2018-02-16 | 贵阳时代沃顿科技有限公司 | A kind of preparation method of modified anti-pollution hydridization reverse osmosis membrane |
| CN109692585A (en) * | 2017-10-20 | 2019-04-30 | 中国石油化工股份有限公司 | Nanofiltration membrane and its preparation method and application |
| CN110052179A (en) * | 2019-04-18 | 2019-07-26 | 万华化学集团股份有限公司 | A kind of preparation method of antipollution composite nanometer filtering film |
| CN110201552A (en) * | 2019-05-13 | 2019-09-06 | 湖北大学 | With micropore/meso-hole structure nano-porous fiber film and preparation method thereof |
| CN113351026A (en) * | 2021-05-17 | 2021-09-07 | 浙江理工大学 | Preparation method of polyamide composite membrane with high controllability |
| CN115814609A (en) * | 2022-12-05 | 2023-03-21 | 蓝星（杭州）膜工业有限公司 | High-yield decolorizing membrane for treating printing and dyeing wastewater and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107213804A (en) * | 2017-07-18 | 2017-09-29 | 宁波日新恒力科技有限公司 | A kind of antibacterial reverse osmosis composite membrane and its preparation method and application |
| CN109692585A (en) * | 2017-10-20 | 2019-04-30 | 中国石油化工股份有限公司 | Nanofiltration membrane and its preparation method and application |
| CN107694357A (en) * | 2017-11-22 | 2018-02-16 | 贵阳时代沃顿科技有限公司 | A kind of preparation method of modified anti-pollution hydridization reverse osmosis membrane |
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| CN110201552B (en) * | 2019-05-13 | 2021-07-13 | 湖北大学 | Nano porous fiber membrane with micropore/mesopore structure and preparation method thereof |
| CN113351026A (en) * | 2021-05-17 | 2021-09-07 | 浙江理工大学 | Preparation method of polyamide composite membrane with high controllability |
| CN115814609A (en) * | 2022-12-05 | 2023-03-21 | 蓝星（杭州）膜工业有限公司 | High-yield decolorizing membrane for treating printing and dyeing wastewater and preparation method thereof |
| CN115814609B (en) * | 2022-12-05 | 2023-09-26 | 蓝星（杭州）膜工业有限公司 | High-water-yield decolorizing film for treating printing and dyeing wastewater and preparation method thereof |
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