CN110141982A - A kind of high throughput equipment with high desalinization mixed-matrix reverse osmosis membrane and the preparation method and application thereof - Google Patents
A kind of high throughput equipment with high desalinization mixed-matrix reverse osmosis membrane and the preparation method and application thereof Download PDFInfo
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- CN110141982A CN110141982A CN201910346181.6A CN201910346181A CN110141982A CN 110141982 A CN110141982 A CN 110141982A CN 201910346181 A CN201910346181 A CN 201910346181A CN 110141982 A CN110141982 A CN 110141982A
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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
- B01D61/025—Reverse osmosis; Hyperfiltration
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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
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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
- B01D71/76—Macromolecular material not specifically provided for in a single one of groups B01D71/08 - B01D71/74
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- 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
Abstract
The invention discloses a kind of high-throughput equipment with high desalinization mixed-matrix reverse osmosis membranes and the preparation method and application thereof, the reverse osmosis composite membrane is made of polysulfones support membrane and functional layer, the functional layer is using m-phenylene diamine (MPD) as aqueous phase monomers, using pyromellitic trimethylsilyl chloride as oil phase monomer, dopant material is the terminated hyperbranched polymer of acid chloride groups, by interfacial polymerization on support membrane.The present invention uses simple and easy treatment process, have chosen a kind of dissaving polymer (Hyperbranched polymer), by allowing to its functionalization to participate in interfacial polymerization, it is used for preparing mixed-matrix reverse osmosis membrane, have benefited from the structure of dissaving polymer height cladodification itself, the netted hole number of the aramid layer of mixed-matrix reverse osmosis membrane increases, reduce the resistance to mass tranfer of water, so that prepared mixed-matrix reverse osmosis membrane improves water flux on the basis of keeping higher salt rejection rate.
Description
(1) technical field
The present invention relates to membrane materials and preparation method thereof, and in particular to a kind of high throughput equipment with high desalinization mixed-matrix is reverse osmosis
Film and the preparation method and application thereof.
(2) background technique
Reverse osmosis technology is to realize separation using the selective penetrated property of semi-permeable membrane using the pressure difference of film two sides as motive force
Membrane process.It is not related to that phase transformation, low energy consumption, is played an important role in terms of sea-water brackish water desalination, pure water ultrapure water.
Reverse osmosis membrane is the core of reverse osmosis technology, and the research and application of reverse osmosis membrane, which are always that reverse osmosis technology field is most popular, grinds
Study carefully direction.
Due to it is reverse osmosis be a kind of pressure-actuated separation process, operating pressure has to be larger than the osmotic pressure of strong brine,
So its energy consumption is difficult to reduce.Therefore, under identical operating conditions, while guaranteeing certain equipment with high desalinization, improve reverse osmosis
The water flux of film is the inevitable choice for reducing operating cost, advocates the big of industry energy saving, environmental protection, and sustainable development energetically in country
Under background, further the high-throughput reverse osmosis composite membrane of exploitation is imperative.Some researches show that in reverse osmosis membrane matrix
Introducing mixed substrate membrane containing nano-grade molecular sieve (Mixed matrix membrane) prepared by nanoparticle has excellent separating property, is mesh
Preceding research hotspot.
Hoek etc. is successfully prepared nano zeolite filling by adding nano zeolite in interfacial polymerization oil-phase solution for the first time
The mixed-matrix reverse osmosis membrane of aramid layer, prepared mixed-matrix membrane flux improve about 1 times.[Jeong B-H.Hoke
E.J Membr.Sci.2007,294:1-7].
Chae, H.R.Lee, J. etc. add graphene oxide in aqueous phase solution, and prepared mixed-matrix membrane flux mentions
It is high by about 80%, and maintain higher salt rejection rate.[Chae H-R,Lee J.J Membr.Sci.2015,483:128-
135].
Lee, T.H.Lee, M.Y. etc. will be introduced into reverse osmosis membrane matrix after carbon nanotube oxidation modification, prepared mixing
Matrix membrane flux improves about 35%, and maintains the salt rejection rate close with control group.[Lee T-H,Lee M-Y,J
Membr.Sci.2017,539:441-450].
The research of mixed substrate membrane containing nano-grade molecular sieve is largely focused at present is doped using inorganic nano material, but inorganic nano
Material is easy to produce boundary defect, this brings film longtime running stability since compatibility is poor between polyamide for it
Certain influence.
(3) summary of the invention
In order to solve the problems existing in the prior art, the present invention provides a kind of high-throughput equipment with high desalinization mixed-matrix is reverse osmosis
Film and preparation method thereof.
The present invention adopts the following technical scheme:
A kind of high throughput equipment with high desalinization mixed-matrix reverse osmosis membrane, it is characterised in that: the mixed-matrix reverse osmosis membrane
It is prepared as follows:
(1) carboxy blocking dissaving polymer HBP shown in formula (I) is mixed with thionyl chloride, is heated to 80 DEG C, condensation
Back flow reaction 10h obtains reaction solution revolving removal thionyl chloride, the over-expense of the sealing end of acid chloride groups shown in formula (II) can be obtained
Fluidized polymer HBPAC；
In formula (I) or formula (II), the R are as follows: HO (CH2CH2)nOH, average molecular weight 600；
(2) polysulfones support membrane is soaked in polyamine aqueous phase solution 1-10 minutes, takes out the polysulfones support membrane after impregnating
It dries in the shade at room temperature after removal excess surface solution；The polyamine aqueous phase solution by m-phenylene diamine (MPD), dodecyl sodium sulfate,
Camphorsulfonic acid, triethylamine mixing is soluble in water configures, and the mass fraction of the m-phenylene diamine (MPD) is 1.0-3.0%, and described ten
The mass fraction of dialkyl sulfonates is 0.15%, and the mass fraction of the camphorsulfonic acid is 4%, the quality point of the triethylamine
Number is 2%；
(3) HBPAC prepared by step (1) is dissolved in mixed organic solvents and obtains mixed liquor, then handle step (3)
Resulting support membrane is soaked in the mixed liquor, is reacted 5-20 seconds, and the support membrane removal film surface after impregnating is then taken out
Redundant solution is simultaneously dried in the shade at room temperature；The mixed organic solvents are mixed by primary solvent and polar organic solvent, institute
The primary solvent stated is one kind or two kinds any of n-hexane, normal heptane or IsoParG, the volume fraction of the polar solvent
For 5-40%；In the mixed liquor, the mass fraction of HBPAC is 0.001%-0.01% (preferably 0.005%)；
(4) step (3) resulting support membrane is soaked in the hexane solution of pyromellitic trimethylsilyl chloride, is reacted 30-60 seconds,
It dries in the shade at room temperature after taking out the support membrane removal film surface redundant solution after impregnating；The n-hexane of the pyromellitic trimethylsilyl chloride
In solution, pyromellitic trimethylsilyl chloride liquid quality fraction is 0.05-0.30%；
(5) support membrane obtained step (4) is placed in 40-80 DEG C of baking oven, is heat-treated 5-10 minutes, then using go from
Sub- water is washed to obtain the high-throughput equipment with high desalinization mixed-matrix reverse osmosis membrane.
Further, by preferred, in step (1), the additional amount of the thionyl chloride shown in the formula (I) to surpass
Branched polymer is that the quality of carboxy blocking dissaving polymer is calculated as 40ml/g.
Further, by preferred, in step (2), in the polyamine aqueous phase solution, m-phenylene diamine (MPD) mass fraction is preferably
2%.
Further, by preferred, in step (3), the polar solvent is acetone, chloroform, chloroform, two chloroethenes
Alkane, trichloroethanes, tetrahydrofuran, ethyl acetate.
Further, in step (3), in the mixed organic solvents, the polar solvent volume fraction is preferably
15%.
Further, by preferred, in step (4), the pyromellitic trimethylsilyl chloride liquid quality fraction is 0.15%.
Further, by preferred, in step (5), the heat treatment temperature is 60 DEG C, and heat treatment time is 5 minutes.
Carboxy blocking dissaving polymer HBP bibliography of the present invention [Li Tianliang, it is amphipathic end carboxyl super branched
Synthesis, characterization and its multiple response self assembly research of polyester, Shanghai Institute Of Technology, 2015] it is prepared.
Compared with prior art, the beneficial effects of the present invention are:
The present invention uses simple and easy treatment process, has chosen a kind of dissaving polymer (Hyperbranched
Polymer), by allowing to its functionalization to participate in interfacial polymerization, it is used for preparing mixed-matrix reverse osmosis membrane, benefits
In the structure of dissaving polymer height cladodification itself, the netted hole number of the aramid layer of mixed-matrix reverse osmosis membrane increases,
The resistance to mass tranfer of water is reduced, so that prepared mixed-matrix reverse osmosis membrane mentions on the basis of keeping higher salt rejection rate
High water flux.
(4) Detailed description of the invention
Fig. 1 is No. 1 film front SEM figure；
Fig. 2 is No. 3 film front SEM figures；
Fig. 3 is No. 11 film front SEM figures；
Fig. 4 is No. 13 film front SEM figures.
(5) specific embodiment
Below by example, the invention will be further described, but protection scope of the present invention is not limited only to this.
Polysulfones support membrane of the present invention purchase is oozed gloomy environmentally friendly High Seience Technology Co., Ltd. from Hunan.
Raw material HBP in embodiment of the present invention is prepared in accordance with the following steps:
30g (about 0.1mol) PEG600,1g (about 0.006mol) p-methyl benzenesulfonic acid is added in 250 milliliters of three-necked flasks.
19.2g (0.1mol) 1,2,4-tricarboxylic anhydride is dissolved in 50 milliliters of tetrahydrofurans, under 60 DEG C of condition of heating and stirring, passes through 100 milliliters
It is slowly dropped into three-necked flask in constant pressure funnel 2h, continues to stir 6h after being added dropwise to complete.Three-necked flask connects mechanical agitator,
It is passed through nitrogen using water segregator, is warming up to 100 DEG C, reacts 1h, is warming up to 120 DEG C, reacts 1h, 30 millis are added in this backward there-necked flask
It rises DMF and is warming up to 140 DEG C of reaction 4h, obtain head product.After head product is cooling, the bag filter for the use of molecular cut off being 3500,
It dialyses 2 days in acetone, obtains HBP after dialysis product drying.
Example 1:
It will be soaked in having a size of 20cm × 10cm polysulfones support membrane in 50 milliliters of polyamine aqueous phase solutions 2 minutes, it is described
Contain 2wt% m-phenylene diamine (MPD), 0.15wt% dodecyl sodium sulfate, 4wt% camphorsulfonic acid, 2wt% in polyamine aqueous phase solution
Triethylamine, after removing redundant solution, dry in the shade film surface at room temperature.After film surface dries, above-mentioned polysulfones support membrane is soaked in 50
In the hexane solution of milliliter 0.15wt% pyromellitic trimethylsilyl chloride, it is made to carry out interfacial polymerization, soaking time is 40 seconds, is then gone
Except redundant solution, after drying in the shade at room temperature, it is placed in 60 DEG C of baking ovens and is heat-treated 5 minutes, obtain No. 1 film.No. 1 film is traditional handicraft preparation
Control group, according to Fig. 1 it is known that its film surface of reverse osmosis membrane of traditional handicraft preparation has typical nodositas structure, and
And roughness is larger.
Example 2:
30g (about 0.1mol) PEG600,1g (about 0.006mol) p-methyl benzenesulfonic acid is added in 250 milliliters of three-necked flasks.
19.2g (0.1mol) 1,2,4-tricarboxylic anhydride is dissolved in 50 milliliters of tetrahydrofurans, under 60 DEG C of stirring conditions, passes through 100 milliliters of constant pressures
It is slowly dropped into three-necked flask in dropping funel 2h, continues to stir 6h after being added dropwise to complete.Three-necked flask connects mechanical agitator, uses
Water segregator is passed through nitrogen, is warming up to 100 DEG C, reacts 1h, is warming up to 120 DEG C, reacts 1h, this backward there-necked flask is added 30 milliliters
DMF is warming up to 140 DEG C of reaction 4h, obtains head product, after head product is cooling, the bag filter for the use of molecular cut off being 3500, in
It dialyses 2 days in acetone, obtains HBP after dialysis product drying.HBP is mixed with thionyl chloride, is heated to 80 DEG C, is condensed back anti-
10h is answered, reaction solution revolving removal thionyl chloride is obtained, HBPAC can be obtained；
It will be soaked in having a size of 20cm × 10cm polysulfones support membrane in 50 milliliters of polyamine aqueous phase solutions 2 minutes, the solution
In contain 2wt% m-phenylene diamine (MPD), 0.15wt% dodecyl sodium sulfate, 4wt% camphorsulfonic acid, 2wt% triethylamine.It is extra to remove
After solution, dry in the shade film surface at room temperature.After film surface dries, above-mentioned polysulfones support membrane is soaked in 50 milliliters and contains 0.01wt%
HBPAC, 15v/v% chloroform, 0.15wt% pyromellitic trimethylsilyl chloride hexane solution in, make its carry out interfacial polymerization, leaching
Steeping the time is 40 seconds, then removes redundant solution, after drying in the shade at room temperature, is placed in 60 DEG C of baking ovens and is heat-treated 5 minutes, obtain No. 2 films.
Example 3:
HBPAC preparation process is consistent with example 2.
It will be soaked in having a size of 20cm × 10cm polysulfones support membrane in 50 milliliters of polyamine aqueous phase solutions 2 minutes, the solution
In contain 2wt% m-phenylene diamine (MPD), 0.15wt% dodecyl sodium sulfate, 4wt% camphorsulfonic acid, 2wt% triethylamine.It is extra to remove
After solution, dry in the shade film surface at room temperature.After film surface dries, above-mentioned polysulfones support membrane is soaked in 50 milliliters of 0.005wt%
In the hexane solution of HBPAC, 10v/v% chloroform, first time interfacial polymerization is carried out, soaking time is 10 seconds, is removed more
After remaining solution, dry in the shade at room temperature.After film surface dries, above-mentioned polysulfones support membrane is soaked in the equal benzene three of 50 milliliters of 0.15wt%
In the hexane solution of formyl chloride, it is made to carry out second of interfacial polymerization, soaking time is 40 seconds, redundant solution is then removed,
After drying in the shade at room temperature, it is placed in 60 DEG C of baking ovens and is heat-treated 5 minutes, obtain No. 3 films.No. 3 films are the novel mixed base of new process preparation
Plasma membrane, surface topography are as shown in Figure 2, it can be seen that and its membrane superficial tissue still keeps typical polyamide nodositas structure, but
Its nodositas structure size is significantly reduced with quantity.
Using the sodium-chloride water solution of 2000ppm, under the pressure of 1.6Mpa, film properties are tested.It is as follows to obtain result:
Example 4-6:
Except polar solvent is changed to dichloroethanes, tetrahydrofuran, ethyl acetate by chloroform respectively in mixed organic solvents
Outside, remaining operating condition is consistent with example 3, respectively obtains 4-6 film.
Using the sodium-chloride water solution of 2000ppm, under the pressure of 1.6Mpa, film properties are tested.It is as follows to obtain result:
Example 7-9:
When except first time interfacial polymerization, the polar solvent concentration is respectively outside 5v/v%, 10v/v%, 20v/v%,
Remaining operating condition is consistent with example 3, respectively obtains 7-9 film.
Using the sodium-chloride water solution of 2000ppm, under the pressure of 1.6Mpa, film properties are tested.It is as follows to obtain result:
Example 10-13:
When except first time interfacial polymerization, HBPAC concentration be respectively 0.001w/w%, 0.002w/w%, 0.008w/w%,
Outside 0.01w/w%, remaining operating condition is consistent with example 3, respectively obtains 10-13 film.Fig. 3 is No. 11 film surface SEM
Figure, Fig. 4 are No. 13 film surface SEM figures, it can be seen that with the increase of HBPAC additive amount, No. 11 films and No. 13 film surface tubercles
Shape number of structures and size taper off trend.It further looks at it can be seen that discontinuity zone occur in two kinds of film surfaces, and are somebody's turn to do
Discontinuity zone area is positively correlated with HBPAC additive amount.In conjunction with membrane separating property result it is found that film surface occur it is discontinuous
Region can be conducive to promote membrane flux to a certain extent, but should be noted that the discontinuity zone will lead to film salt rejection rate
It reduces.
Using the sodium-chloride water solution of 2000ppm, under the pressure of 1.6Mpa, film properties are tested.It is as follows to obtain result:
Example 14-16:
When except first time interfacial polymerization, time of contact is respectively 5 seconds, 15 seconds, 20 seconds outer, remaining operating condition and examples 3
It is consistent, respectively obtains 14-16 film.
Using the sodium-chloride water solution of 2000ppm, under the pressure of 1.6Mpa, film properties are tested.It is as follows to obtain result:
Claims (9)
1. a kind of high throughput equipment with high desalinization mixed-matrix reverse osmosis membrane, it is characterised in that: the high-throughput equipment with high desalinization mixing
Matrix reverse osmosis membrane is prepared as follows:
(1) carboxy blocking dissaving polymer HBP shown in formula (I) is mixed with thionyl chloride, is heated to 80 DEG C, be condensed back
10h is reacted, reaction solution revolving removal thionyl chloride is obtained, the hyperbranched poly of the sealing end of acid chloride groups shown in formula (II) can be obtained
Close object HBPAC；
In formula (I) or formula (II), the R are as follows: HO (CH2CH2)nOH, average molecular weight 600；
(2) polysulfones support membrane is soaked in polyamine aqueous phase solution 1-10 minutes, takes out the polysulfones support membrane removal after impregnating
It dries in the shade at room temperature after excess surface solution；The polyamine aqueous phase solution is by m-phenylene diamine (MPD), dodecyl sodium sulfate, camphor
Sulfonic acid, triethylamine mixing is soluble in water configures, and the mass fraction of the m-phenylene diamine (MPD) is 1.0-3.0%, the dodecane
The mass fraction of base sodium sulfonate is 0.15%, and the mass fraction of the camphorsulfonic acid is 4%, and the mass fraction of the triethylamine is
2%；
(3) HBPAC prepared by step (1) is dissolved in mixed organic solvents and obtains mixed liquor, step (3) are then handled into gained
Support membrane be soaked in the mixed liquor, react 5-20 second, then taking out the support membrane after impregnating, to remove film surface extra
Solution simultaneously dries in the shade at room temperature；The mixed organic solvents are mixed by primary solvent and polar organic solvent, described
Primary solvent is one kind or two kinds any of n-hexane, normal heptane or IsoParG, and the volume fraction of the polar solvent is 5-
40%；In the mixed liquor, the mass fraction of HBPAC is 0.001%-0.01%；
(4) step (3) resulting support membrane is soaked in the hexane solution of pyromellitic trimethylsilyl chloride, is reacted 30-60 seconds, taken out
It dries in the shade at room temperature after support membrane removal film surface redundant solution after immersion；The hexane solution of the pyromellitic trimethylsilyl chloride
In, pyromellitic trimethylsilyl chloride liquid quality fraction is 0.05-0.30%；
(5) support membrane for obtaining step (4) is placed in 40-80 DEG C of baking oven, is heat-treated 5-10 minutes, is then used deionized water
Washing obtains the high-throughput equipment with high desalinization mixed-matrix reverse osmosis membrane.
2. high throughput equipment with high desalinization mixed-matrix reverse osmosis membrane as described in claim 1, it is characterised in that: in step (1), institute
The additional amount for the thionyl chloride stated is using dissaving polymer shown in the formula (I) as the matter of carboxy blocking dissaving polymer
Amount is calculated as 40ml/g.
3. high throughput equipment with high desalinization mixed-matrix reverse osmosis membrane as described in claim 1, it is characterised in that: in step (2), institute
It states in polyamine aqueous phase solution, m-phenylene diamine (MPD) mass fraction is preferably 2%.
4. high throughput equipment with high desalinization mixed-matrix reverse osmosis membrane as described in claim 1, it is characterised in that: in step (3), institute
The polar solvent stated is acetone, chloroform, chloroform, dichloroethanes, trichloroethanes, tetrahydrofuran, ethyl acetate.
5. high throughput equipment with high desalinization mixed-matrix reverse osmosis membrane as described in claim 1, it is characterised in that: in step (3), institute
In the mixed organic solvents stated, polar solvent volume fraction is preferably 15%.
6. high throughput equipment with high desalinization mixed-matrix reverse osmosis membrane as described in claim 1, it is characterised in that: the mixed liquor
In, the mass fraction of HBPAC is 0.005%.
7. high throughput equipment with high desalinization mixed-matrix reverse osmosis membrane as described in claim 1, it is characterised in that: in step (4), institute
Stating pyromellitic trimethylsilyl chloride liquid quality fraction is 0.15%.
8. high throughput equipment with high desalinization mixed-matrix reverse osmosis membrane as described in claim 1, it is characterised in that: in step (5), institute
Stating heat treatment temperature is 60 DEG C, and heat treatment time is 5 minutes.
9. it is salty that a kind of high-throughput high desalination mixed-matrix reverse osmosis membrane as described in claim 1 is applied to drink water purifying, hardship
Water desalination or sea water desalination.
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| CN111001317B (en) * | 2019-12-05 | 2022-02-11 | 浙江工业大学 | High-flux high-selectivity composite nanofiltration membrane and preparation method thereof |
| CN111151137A (en) * | 2020-01-03 | 2020-05-15 | 浙江工业大学 | High-flux high-salt-rejection reverse osmosis composite membrane and preparation method thereof |
| CN111151137B (en) * | 2020-01-03 | 2022-03-15 | 浙江工业大学 | High-flux high-salt-rejection reverse osmosis composite membrane and preparation method thereof |
| CN113634141A (en) * | 2020-04-27 | 2021-11-12 | 万华化学集团股份有限公司 | Preparation method of polyamide composite reverse osmosis membrane, reverse osmosis membrane and application of reverse osmosis membrane |
| CN117547974A (en) * | 2024-01-12 | 2024-02-13 | 河南师范大学 | Polyaiperazine amide nanofiltration membrane with high acid-base stability and preparation method thereof |
| CN117547974B (en) * | 2024-01-12 | 2024-04-12 | 河南师范大学 | Polyaiperazine amide nanofiltration membrane with high acid-base stability and preparation method thereof |
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