CN109499387A - A kind of compound forward osmosis membrane of high throughput and preparation method thereof - Google Patents

A kind of compound forward osmosis membrane of high throughput and preparation method thereof Download PDF

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Publication number
CN109499387A
CN109499387A CN201810136062.3A CN201810136062A CN109499387A CN 109499387 A CN109499387 A CN 109499387A CN 201810136062 A CN201810136062 A CN 201810136062A CN 109499387 A CN109499387 A CN 109499387A
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China
Prior art keywords
preparation
forward osmosis
osmosis membrane
woven fabrics
layer
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CN201810136062.3A
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Chinese (zh)
Inventor
薛立新
汤依莲
林旭杰
林玉生
高从堦
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Wenzhou Environmental Protection Technology Co Ltd Lotus
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Wenzhou Environmental Protection Technology Co Ltd Lotus
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Priority to CN201810136062.3A priority Critical patent/CN109499387A/en
Publication of CN109499387A publication Critical patent/CN109499387A/en
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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
    • B01D69/12—Composite membranes; Ultra-thin membranes
    • 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
    • B01D61/002—Forward osmosis or direct osmosis
    • 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
    • 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
    • Y02A20/00—Water conservation; Efficient water supply; Efficient water use
    • Y02A20/124—Water desalination
    • Y02A20/131—Reverse-osmosis

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Water Supply & Treatment (AREA)
  • Manufacturing & Machinery (AREA)
  • Separation Using Semi-Permeable Membranes (AREA)

Abstract

The invention discloses a kind of compound forward osmosis membranes of high throughput and preparation method thereof, which includes: non-woven fabrics supporting layer；With the poly aromatic amide separating layer being attached directly on the non-woven fabrics supporting layer.Wherein, poly aromatic amide dense separation layers are generated by amine and aroyl chloride with more than one functional group by the interfacial polymerization of one or more steps on the non-woven fabrics supporting layer.It can cause the ultrafiltration middle layer of interior concentration difference structure due on the support structure, eliminating, forward osmosis membrane of the invention has very high water flux and high salt rejection rate under conditions of maintaining the high retention of aramid layer.In preparation method, preparation step is simplified, has saved cost.Prepared forward osmosis membrane can be used for the fields such as first aid water bag, concentration of juices, pharmacy, plant protection case, sea water desalination, water softening, industrial wastewater.

Description

A kind of compound forward osmosis membrane of high throughput and preparation method thereof
Technical field
The present invention relates to the sides that a kind of compound forward osmosis membrane of high throughput and interfacial polymerization method prepare the forward osmosis membrane Method.
Background technique
Positive infiltration (Forward Osmosis, FO) technology is the osmotic drive of a kind of chemical potential difference or osmotic pressure guidance Membrane process has the characteristics that low energy consumption, low pollution, Gao Huishou, and in sea water desalination, wastewater treatment, the energy generates electricity, food processing, There are reality or potential application prospect in the fields such as drug concentration.However, greatly being restricted due to lacking efficient FO membrane material The development of FO technology.Membrane material currently used for FO process all has unsymmetric structure, by thin selection separating layer and porous branch Support layer composition.All there is outer concentration polarization and interior concentration polarization during FO, especially interior concentration polarization causes FO film practical Water flux is far smaller than theoretical water flux.Under normal conditions, outer concentration polarization occurs to pass through in the interface of film and solution Increase the hydrodynamics such as flow velocity to be alleviated；Interior concentration polarization is phenomenon specific to FO process, during FO according to The orientation of film, solute are accumulated or are diluted in film porous support layer, are formed concentration and diluted interior concentration polarization, be can be greatly reduced The osmotic pressure,effective of film two sides is poor.Interior concentration polarization occurs in porous support layer, it is difficult to slow by changing external condition Solution.Research shows that interior concentration polarization and film porous support layer structure (porosity, hole curvature, film thickness) and membrane material itself Physicochemical properties (hydrophilic and hydrophobic, selectivity) have very big relationship.Supporting layer thickness is smaller, and porosity is higher, hole bending Spend smaller, hydrophily is better, then membrane structure parameter is then smaller, and interior concentration polarization is smaller.
Interfacial polymerization is to prepare the height containing polyamide separating layer to shut off the method for permeable membrane, but existing interfacial polymerization The method for preparing forward osmosis membrane has copied the process of preparation high pressure reverse osmosis membrane.Its process includes first in non-woven fabrics support surface By polymer supermicro filtration membrane being applied and separating supporting layer as isolation technics, then, carrying out interface party, in conjunction with upper polyamide Positive permeability and separation layer.In this kind of traditional structure, the polymer supermicro filtration membrane being incorporated between non-woven fabrics and aramid layer is separated Supporting layer, resulting in forward osmosis membrane, not only preparation process is complicated, but also during application, interior concentration polarization is big, and infiltration is logical Measure less than normal, practical performance is bad.
Therefore, urgent need is developed forward osmosis membrane of a kind of high-efficient high performance and preparation method thereof and is wanted in practical application to meet It asks.
Summary of the invention
The purpose of the present invention is to provide a kind of high-throughput forward osmosis membranes and preparation method thereof.
The first aspect of the present invention provides a kind of forward osmosis membrane, comprising:
Non-woven fabrics supporting layer；With
The poly aromatic amide separating layer being attached directly on the non-woven fabrics supporting layer.
In another preferred example, poly aromatic amide separating layer is poly aromatic amide dense separation layers.
In another preferred example, the non-woven fabrics supporting layer is by polyester, polyamide, prepared by polyolefin or polyether sulfone etc. and At.
In another preferred example, poly aromatic amide dense separation layers can pass through amine and virtue with more than one functional group Fragrant acyl chlorides is generated by the interfacial polymerization of one or more steps.
The second aspect of the present invention provides the preparation method of forward osmosis membrane described in first aspect, comprising the following steps:
(i) amine aqueous solution and aroyl chloride solution are provided；
(ii) amine aqueous solution is dispersed in acquisition amine aqueous solution layer on non-woven fabrics supporting layer；
(iii) the aroyl chloride solution is dispersed on amine aqueous solution layer and carries out interfacial polymerization acquisition poly aromatic amide separation Layer is to obtain forward osmosis membrane.
In another preferred example, step ii) dispersing method include but is not limited to that non-woven fabrics is immersed liquid or liquid to lead to Surface coating or spray are crossed to nonwoven surface.
In another preferred example, step iii) dispersing method include but is not limited to will be loaded with amine aqueous solution layer non-woven fabrics leaching Enter liquid or liquid to apply or sprayed to the nonwoven surface for being loaded with amine aqueous solution layer by surface.
In another preferred example, the amine is selected from: m-phenylene diamine (MPD), o-phenylenediamine, diethylenetriamine, triethylene tetramine, piperazine The mixture that any one in piperazine or derivatives thereof or two kinds of mass ratioes are 1:1~1:4.
In another preferred example, the aroyl chloride is selected from: pyromellitic trimethylsilyl chloride, m-phthaloyl chloride, paraphenylene terephthalamide The mixture that one of chlorine, polynary sulfonic acid chloride or any two kinds of mass ratioes are 1:1~1:4.
In another preferred example, the mass percent of the amine aqueous solution is 0.5~5%.
In another preferred example, the mass percent of the aroyl chloride solution is 0.05~1%.
In another preferred example, the time of the interfacial polymerization is 0.1-10 minutes.
In another preferred example, the preparation method further includes that the forward osmosis membrane that will be obtained passes through 30-130 DEG C of heat treatment 1- It after 15min, is floated with deionized water, the step of drying.
The forward osmosis membrane of the application, interfacial polymerization obtains poly aromatic amide dense separation layers on the support structure, eliminates It can cause the ultrafiltration middle layer of interior concentration difference structure.
In another preferred example, the preparation method comprises the following steps:
1) non-woven fabrics supporting layer is directly contacted to the aromatic multi-amine aqueous solution that one is 0.5~5 ﹪ containing mass percent, Remove excess surface liquid；
2) contact quality percentage is the alkane solution of the more acyl chlorides of 0.05~1 ﹪ fragrance again, carries out 0.1-10 minutes boundaries Face polymerization；
3) membrane material obtained is floated after 30-130 DEG C of heat treatment 1-15min with deionized water, and drying is just permeated Film.
The third aspect of the present invention provides the purposes of forward osmosis membrane described in first aspect, dense for first aid water bag, fruit juice Contracting, pharmacy, plant protection case, sea water desalination, water softening or Industrial Wastewater Treatment.
It can cause the ultrafiltration middle layer of interior concentration difference structure, forward osmosis membrane of the invention due on the support structure, eliminating Under conditions of maintaining the high retention of aramid layer, there is very high water flux and high salt rejection rate.In preparation method, simplify Preparation step, has saved cost.Prepared forward osmosis membrane can be used for first aid water bag, concentration of juices, pharmacy, plant protection The fields such as case, sea water desalination, water softening, industrial wastewater.
It should be understood that above-mentioned each technical characteristic of the invention and having in below (eg embodiment) within the scope of the present invention It can be combined with each other between each technical characteristic of body description, to form a new or preferred technical solution.Institute in specification The each feature disclosed can be replaced by any alternative characteristics for providing identical, impartial or similar purpose.As space is limited, exist This is no longer repeated one by one.
Detailed description of the invention
Fig. 1 is the shape appearance figure of structure of composite membrane.
Fig. 2 is the shape appearance figure of structure of composite membrane.
Fig. 3 is the shape appearance figure of structure of composite membrane.
Specific embodiment
Present inventor develops a kind of positive infiltration of high throughput of structure novel by depth studying extensively for the first time Permeable membrane, including non-woven fabrics supporting layer and the poly aromatic amide dense separation layers being attached directly on non-woven fabrics supporting layer.Wherein, gather Aromatic amides dense separation layers are on the non-woven fabrics supporting layer by amine and aroyl chloride with more than one functional group, It is generated by the interfacial polymerization of one or more steps, simplifies preparation step, saved cost.Due on the support structure, removing It can cause the ultrafiltration middle layer of interior concentration difference structure, the condition of forward osmosis membrane of the invention in the high retention for maintaining aramid layer Under, there is very high water flux and high salt rejection rate.On this basis, the present invention is completed.
Present invention will be further explained below with reference to specific examples.It should be understood that these embodiments are merely to illustrate the present invention Rather than it limits the scope of the invention.In the following examples, the experimental methods for specific conditions are not specified, usually according to conventional strip Part or according to the normal condition proposed by manufacturer.Unless otherwise stated, otherwise percentage and number are weight percent and weight Number.
Unless otherwise defined, it anticipates known to all professional and scientific terms as used herein and one skilled in the art Justice is identical.In addition, any method similar to or equal to what is recorded and material can be applied to the method for the present invention.Wen Zhong The preferred implement methods and materials are for illustrative purposes only.
Embodiment 1
Step (1):
The m-phenylene diamine (MPD) that mass percent is 0.5% is dissolved in pure water, m-phenylene diamine (MPD) aqueous solution is made as water phase；
Step (2):
The pyromellitic trimethylsilyl chloride that mass percent is 0.05% is dissolved in Permethyl 99A, pyromellitic trimethylsilyl chloride is configured to Permethyl 99A solution is as organic phase；
Step (3):
M-phenylene diamine (MPD) aqueous solution is uniformly coated on the non-woven fabrics of hygrometric state, fixed 0.5min, then remove it is extra between Phenylenediamine aqueous solution；
Step (4):
Step (2) prepared organic phase solution is uniformly coated on the non-woven fabrics that step (3) is handled well and carries out interface Polymerase 10 .5 minutes, remove extra solution；Then it is heat-treated 15 minutes, rinses at 50 DEG C, drying obtains efficiently positive infiltration Film.
Film pattern is observed under microscope (2000 times), as a result as shown in Figure 1, being structure of composite membrane.
High-throughput forward osmosis membrane prepared by the present embodiment is fitted into film properties evaluating apparatus, then with the chlorination of 2mol/L Sodium water solution is stoste, is to draw liquid, the membrane flux 42L/m of survey with purified water2.h, salt rejection rate 99.57%.
Embodiment 2:
Step (1):
The m-phenylene diamine (MPD) that mass percent is 2 ﹪ is dissolved in pure water, m-phenylene diamine (MPD) aqueous solution is made as water phase；
Step (2):
The pyromellitic trimethylsilyl chloride that mass percent is 0.1 ﹪ is dissolved in normal octane, is being configured to pyromellitic trimethylsilyl chloride just Octane solution is as organic phase；
Step (3):
M-phenylene diamine (MPD) aqueous solution is uniformly coated on the non-woven fabrics of hygrometric state, then fixed 3min removes extra isophthalic Two amine aqueous solutions；
Step (4):
Step (2) prepared organic phase solution is uniformly coated on the non-woven fabrics that step (3) is handled well and carries out interface Polyase 13 minute removes extra solution；Then it is heat-treated 8 minutes, rinses at 85 DEG C, drying obtains efficient forward osmosis membrane.
High-throughput forward osmosis membrane prepared by the present embodiment is fitted into film properties evaluating apparatus, then with the chlorination of 2mol/L Sodium water solution is stoste, is to draw liquid, the membrane flux 38.4L/m of survey with purified water2.h, salt rejection rate 99.83%.
Embodiment 3:
Step (1):
The m-phenylene diamine (MPD) that mass percent is 5 ﹪ is dissolved in pure water, m-phenylene diamine (MPD) aqueous solution is made as water phase；
Step (2):
By mass percent be 1 ﹪ pyromellitic trimethylsilyl chloride be dissolved in n-hexane, be configured to pyromellitic trimethylsilyl chloride just oneself Alkane solution is as organic phase；
Step (3):
M-xylene diamine aqueous solution is uniformly coated on the non-woven fabrics of hygrometric state, fixed 5min, then remove it is extra between Benzene dimethylamine aqueous solution；
Step (4):
Step (2) prepared organic phase solution is uniformly coated on the non-woven fabrics that step (3) is handled well and carries out interface Polymerization 5 minutes, removes extra solution；Then it is heat-treated 2 minutes, rinses at 130 DEG C, drying obtains efficient forward osmosis membrane.
Film pattern is observed under microscope (2000 times), as a result as shown in Fig. 2, being structure of composite membrane.
High-throughput forward osmosis membrane prepared by the present embodiment is fitted into film properties evaluating apparatus, then with the chlorination of 2mol/L Sodium water solution is stoste, is to draw liquid, the membrane flux 53.3L/m of survey with purified water2.h, salt rejection rate 99.67%.
Embodiment 4:
Step (1):
The diethylenetriamine that mass percent is 0.5 ﹪ and the m-phenylene diamine (MPD) that mass percent is 2.5% are dissolved in pure Mixed aqueous solution is made in water as water phase；
Step (2):
The m-phthaloyl chloride that mass percent is 0.05 ﹪ and the pyromellitic trimethylsilyl chloride that mass percent is 0.1% is molten Solution is configured to n-hexane mixed solution as organic phase in n-hexane；
Step (3):
Step (1) is uniformly coated on the non-woven fabrics of hygrometric state, then fixed 3min removes extra water phase；
Step (4): step (2) prepared organic phase solution is uniformly coated on the non-woven fabrics that step (3) is handled well It carries out interfacial polymerization 3 minutes, removes extra solution；Then it is heat-treated 10 minutes, rinses at 85 DEG C, drying obtains efficiently just Permeable membrane.
High-throughput forward osmosis membrane prepared by the present embodiment is fitted into film properties evaluating apparatus, then with the chlorination of 2mol/L Sodium water solution is stoste, is to draw liquid, the membrane flux 52.4L/m of survey with purified water2.h, salt rejection rate 99.71%.
Embodiment 5:
Step (1):
The diethylenetriamine that mass percent is 0.5% is dissolved in pure water, diethylenetriamine aqueous solution is made as water Phase；
Step (2):
The pyromellitic trimethylsilyl chloride that mass percent is 0.05% is dissolved in Permethyl 99A, pyromellitic trimethylsilyl chloride is configured to Permethyl 99A solution is as organic phase；
Step (3):
Diethylenetriamine aqueous solution is uniformly coated on PS membrane counterdie, then fixed 3min removes extra diethyl Three amine aqueous solution of alkene；
Step (4):
Step (2) prepared organic phase solution is uniformly coated on the polysulfones counterdie that step (3) is handled well and carries out boundary Face polymerase 10 .5 minutes, removes extra solution；Then it is heat-treated 10 minutes, rinses at 85 DEG C, drying obtains forward osmosis membrane.
Film pattern is observed under microscope (2000 times), as a result as shown in figure 3, the relatively compact composite membrane result of structure.
Forward osmosis membrane manufactured in the present embodiment is fitted into film properties evaluating apparatus, then with the sodium-chloride water solution of 2mol/L It is to draw liquid, the membrane flux 1.2L/m of survey with purified water for stoste2.h, salt rejection rate 97.23%.
Above-mentioned testing result shows the performance of high-throughput forward osmosis membrane prepared by the present invention, prepares reverse osmosis better than using tradition Forward osmosis membrane prepared by permeable membrane method has more preferable popularization and application foreground using high performance forward osmosis membrane prepared by the present invention With the value of industrialization.
All references mentioned in the present invention is incorporated herein by reference, independent just as each document It is incorporated as with reference to such.In addition, it should also be understood that, after reading the above teachings of the present invention, those skilled in the art can To make various changes or modifications to the present invention, such equivalent forms equally fall within model defined by the application the appended claims It encloses.

Claims (10)

1. a kind of forward osmosis membrane, which is characterized in that the forward osmosis membrane includes:
Non-woven fabrics supporting layer；With
Poly aromatic amide separating layer is attached directly on the non-woven fabrics supporting layer.
2. forward osmosis membrane as described in claim 1, which is characterized in that the non-woven fabrics supporting layer is by polyester, polyamide, polyene Hydrocarbon or polyether sulfone are prepared.
3. the preparation method of forward osmosis membrane as described in claim 1, which is characterized in that the preparation method includes following step It is rapid:
(i) amine aqueous solution and aroyl chloride solution are provided；
(ii) amine aqueous solution is dispersed in acquisition amine aqueous solution layer on non-woven fabrics supporting layer；
(iii) by the aroyl chloride solution be dispersed on amine aqueous solution layer carry out interfacial polymerization obtain poly aromatic amide separating layer from And obtain forward osmosis membrane.
4. preparation method as claimed in claim 3, which is characterized in that the amine is selected from: m-phenylene diamine (MPD), o-phenylenediamine, diethyl The mixture that any one in alkene triamine, triethylene tetramine, piperazine or derivatives thereof or two kinds of mass ratioes are 1:1~1:4.
5. preparation method as claimed in claim 3, which is characterized in that the aroyl chloride is selected from: pyromellitic trimethylsilyl chloride, isophthalic The mixture that one of dimethyl chloride, paraphthaloyl chloride, polynary sulfonic acid chloride or any two kinds of mass ratioes are 1:1~1:4.
6. preparation method as claimed in claim 3, which is characterized in that the mass percent of the amine aqueous solution is 0.5~5%.
7. preparation method as claimed in claim 3, which is characterized in that the mass percent of the aroyl chloride solution is 0.05 ~1%.
8. preparation method as claimed in claim 3, which is characterized in that the time of the interfacial polymerization is 0.1-10 minutes.
9. preparation method as claimed in claim 3, which is characterized in that the preparation method further includes the forward osmosis membrane that will be obtained It after 30-130 DEG C of heat treatment 1-15min, is floated with deionized water, the step of drying.
10. the purposes of forward osmosis membrane according to claim 1, which is characterized in that be used for first aid water bag, concentration of juices, system Medicine, plant protection case, sea water desalination, water softening or Industrial Wastewater Treatment.
CN201810136062.3A 2018-02-09 2018-02-09 A kind of compound forward osmosis membrane of high throughput and preparation method thereof Pending CN109499387A (en)

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CN201810136062.3A CN109499387A (en) 2018-02-09 2018-02-09 A kind of compound forward osmosis membrane of high throughput and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201810136062.3A CN109499387A (en) 2018-02-09 2018-02-09 A kind of compound forward osmosis membrane of high throughput and preparation method thereof

Publications (1)

Publication Number Publication Date
CN109499387A true CN109499387A (en) 2019-03-22

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Country Status (1)

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