CN105749768A - Composite reverse osmosis membrane with high salt removing rate and controllable flux and method for preparing composite reverse osmosis membrane - Google Patents
Composite reverse osmosis membrane with high salt removing rate and controllable flux and method for preparing composite reverse osmosis membrane Download PDFInfo
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- CN105749768A CN105749768A CN201610250887.9A CN201610250887A CN105749768A CN 105749768 A CN105749768 A CN 105749768A CN 201610250887 A CN201610250887 A CN 201610250887A CN 105749768 A CN105749768 A CN 105749768A
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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
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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
- 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
- B01D69/12—Composite membranes; Ultra-thin membranes
- B01D69/125—In situ manufacturing by polymerisation, polycondensation, cross-linking or chemical reaction
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Abstract
The invention discloses a composite reverse osmosis membrane with a high salt removing rate and controllable flux and a method for preparing the composite reverse osmosis membrane.The method includes coating water-phase solution layers on a basement membrane with porous polysulfone support layers; coating oil-phase solution layers on the basement membrane; carrying out interfacial polymerization reaction on two phases to obtain polyamide ultrathin functional separation layers; cleaning and drying the basement membrane in follow-up procedures to obtain the composite reverse osmosis membrane.The composite reverse osmosis membrane and the method have the advantages that the composite reverse osmosis membrane produced by the aid of the method is detected by the aid of 1500ppm NaCl solution under the conditions of the pH (potential of hydrogen) of 7.5-8, the temperature of 25 DEG C and the test pressures of 150psi, the salt removing rate is 99.30%-99.75%, and the water flux is 33gfd-50gfd.
Description
Technical field
The present invention relates to a kind of reverse osmosis membrane, particularly to the compound reverse osmosis membrane that a kind of equipment with high desalinization and flux are controlled, the preparation method that the invention still further relates to above-mentioned reverse osmosis membrane.
Background technology
Reverse osmosis technology is under certain pressure effect, by means of the separation method that the solute in solution and solvent are separated by the selective retention effect of reverse osmosis membrane, compared with other film kinds (nanofiltration, ultrafiltration, microfiltration etc.), there is less membrane aperture, can effectively remove the impurity such as salt in water, Organic substance, colloid, antibacterial.Reverse osmosis membrane has been widely used for multiple industries and the fields such as environment, pharmacy, chemical industry, industry.Main two critical technical parameters of reverse osmosis membrane are salt rejection rate and water flux, and both are contradictory relations, shifting.With regard to domestic existing technology, pursuing the film product of equipment with high desalinization, its aquifer yield is not high；And produce the product that water is high, the operating pressure of its needs is higher, or its salt rejection rate is relatively low.It addition, in the processing procedure of reverse osmosis membrane, be difficult to reach to be accurately controlled to diaphragm salt rejection rate and flux, the product often produced does not reach intended performance requirement.So, the application of reverse osmosis membrane is constrained to a certain extent.
Summary of the invention
For problems of the prior art, first purpose of the present invention is in that to propose a kind of equipment with high desalinization and the controlled compound reverse osmosis membrane of flux.
Second purpose of the present invention is in that the preparation method proposing above-mentioned reverse osmosis membrane.
For solving above-mentioned technical problem, first purpose of the present invention is achieved by the following technical programs:
A kind of equipment with high desalinization and the controlled compound reverse osmosis membrane of flux, porous polysulfone supporting layer counterdie is coated with aqueous phase solution layer, it is coated with oil-phase solution layer, makes biphase to obtain polyamide ultrathin function stratum disjunctum by interface polymerization reaction, obtain after follow-up cleaning, drying；Wherein,
The surfactant of aqueous phase solution to be weight concentration be 0.5%～5% polyfunctional amine solution, weight concentration 0.5%～2% in aqueous phase solution layer, and the polar solvent of weight concentration 3%～10%, regulating pH value through sodium hydroxide after stirring to prepare to 7～9, described polyfunctional amine is aromatic series, aliphatic or alicyclic polyfunctional amine；
In oil-phase solution layer, oil-phase solution is add the multi-functional acyl halide that weight concentration is 0.05%～0.3% in the aliphatic hydrocarbon of 4～12 carbon atoms, cycloalphatic hydrocarbon or aromatic hydrocarbon; stirring and dissolving and get final product, described multi-functional acyl halide is aromatic series, aliphatic or alicyclic multi-functional acyl halide.
As preferably, described polyfunctional amine is m-diaminobenzene., and its weight concentration accounting for aqueous phase solution is 3%.
As preferably, described multi-functional acyl halide is pyromellitic trimethylsilyl chloride, and its weight concentration accounting for oil-phase solution is 0.099%～0.169%.
As preferably, described surfactant is dodecylbenzene sodium sulfonate, and its weight concentration accounting for aqueous phase solution is 0.5%.
As preferably, described polar solvent is dimethyl sulphoxide solution or N-Methyl pyrrolidone solution or both mixed solutions, and its weight concentration accounting for aqueous phase solution is 4%～7%.
The preparation method of a kind of equipment with high desalinization and the controlled compound reverse osmosis membrane of flux, comprises the steps:
(1) preparation of aqueous phase solution: select the one of aromatic series, aliphatic or alicyclic polyfunctional amine to be dissolved in the water, its weight concentration in aqueous is 0.5%～5%, after it is completely dissolved, the surfactant accounting for this aqueous solution weight 0.5%～2% is added again in this aqueous solution, and account for the polar solvent of this aqueous solution weight 3%～10%, the back end hydrogenation sodium oxide that stirs regulates solution ph between 7～9, namely obtains aqueous phase solution；
(2) preparation of oil-phase solution: select the one of aromatic series, aliphatic or alicyclic multi-functional acyl halide; it is dissolved in selected from containing the one in the aliphatic hydrocarbon of 4～12 carbon atoms, cycloalphatic hydrocarbon and aromatic hydrocarbon, obtaining oil-phase solution after stirring and dissolving according to the ratio accounting for total solution weight 0.05%～0.3%；
(3) on polysulfone supporting layer counterdie, aqueous phase solution it is coated with, remove the aqueous phase solution of excess surface, allow the polysulfone supporting layer counterdie having adsorbed aqueous phase solution through the closing space with heat supply and exhausting system again, control its internal temperature 20 DEG C～30 DEG C, relative humidity 50%～80%, allows the moisture of face volatilize further；Afterwards, it is coated with oil-phase solution in the above, removes excess surface oil-phase solution, enter in 30 DEG C～120 DEG C baking ovens and dry, form polyamide ultrathin stratum disjunctum；After follow-up cleaning, drying, finally give compound reverse osmosis membrane.
As preferably, described polyfunctional amine is m-diaminobenzene., and its weight concentration accounting for aqueous phase solution is 3%.
As preferably, described multi-functional acyl halide is pyromellitic trimethylsilyl chloride, and its weight concentration accounting for oil-phase solution is 0.099%～0.169%.
As preferably, described surfactant is dodecylbenzene sodium sulfonate, and its weight concentration accounting for aqueous phase solution is 0.5%.
As preferably, described polar solvent is dimethyl sulphoxide solution or N-Methyl pyrrolidone solution or both mixed solutions, and its weight concentration accounting for aqueous phase solution is 4%～7%.
The present invention compared with prior art has the beneficial effect that the NaCl solution of the compound reverse osmosis diaphragm 1500ppm that the technology of the present invention produces, pH is 7.5～8, temperature 25 DEG C, detection when test pressure 150psi, salt rejection rate 99.30%～99.75%, water flux 33gfd～50gfd.
Detailed description of the invention
Get information about the present invention for allowing those skilled in the art become apparent from, below the present invention is further illustrated.
The present invention adopts homemade porous polysulfone supporting layer counterdie, is first coated with aqueous phase solution thereon, is coated with oil-phase solution, biphase obtains polyamide ultrathin function stratum disjunctum by interface polymerization reaction, finally gives compound reverse osmosis diaphragm then through post processing.In order to obtain equipment with high desalinization and the controlled reverse osmosis membrane of flux, key technology of the present invention is in that to control the content of multi-functional acyl halide in aqueous phase solution Semi-polarity solvent and oil-phase solution and proportion relation realizes water flux control.It is described in detail below in conjunction with being embodied as embodiment.
Embodiment 1
Reverse osmosis membrane production method is as follows:
1, the preparation of aqueous phase solution: add 3kg m-diaminobenzene., 0.5kg dodecylbenzene sodium sulfonate, 4kgN-methyl pyrrolidone in 92.5kg water, obtains aqueous phase solution after stirring；
2, the preparation of oil-phase solution: be dissolved in the Petroleum of 100kg by pyromellitic trimethylsilyl chloride 0.1kg, obtains oil-phase solution after stirring；
3, first on polysulfone supporting layer counterdie, it is coated with aqueous phase solution, remove the solution of excess surface with low pressure air knife after, allow the counterdie having adsorbed aqueous phase solution through the closing space with heat supply and exhausting system again, control its internal temperature 26 DEG C, relative humidity 60%, time 1min, the moisture allowing counterdie face volatilizees further, afterwards, it is coated with oil-phase solution in the above, after removing a part of oil-phase solution in surface with low pressure air knife, subsequently enter maintenance 5min in 90 DEG C of baking ovens, dry oil phase liquid and form polyamide ultrathin stratum disjunctum, after follow-up cleaning, drying, finally give compound reverse osmosis membrane.
Membrane products adopts following condition to detect: the NaCl solution of 1500ppm, and pH is 7.5～8, temperature 25 DEG C, tests pressure 150psi, and acquired results is in Table 1.
Embodiment 2:
Reverse osmosis membrane production method is as follows:
1, the preparation of aqueous phase solution: add 3kg m-diaminobenzene., 0.5kg dodecylbenzene sodium sulfonate, 4kg dimethyl sulfoxide in 92.5kg water, obtains aqueous phase solution after stirring；
2, the preparation of oil-phase solution: with embodiment 1；
3, film-forming method is with embodiment 1.
Diaphragm detection method is with embodiment 1, and result is in Table 1.
Embodiment 3:
Reverse osmosis membrane production method is as follows:
1, the preparation of aqueous phase solution: add 3kg m-diaminobenzene., 0.5kg dodecylbenzene sodium sulfonate, 3kgN-methyl pyrrolidone, 1kg dimethyl sulfoxide in 92.5kg water, obtains aqueous phase solution after stirring；
2, the preparation of oil-phase solution: with embodiment 1；
3, film-forming method is with embodiment 1.
Diaphragm detection method is with embodiment 1, and result is in Table 1.
Embodiment 4:
Reverse osmosis membrane production method is as follows:
1, the preparation of aqueous phase solution: add 3kg m-diaminobenzene., 0.5kg dodecylbenzene sodium sulfonate, 2.5kgN-methyl pyrrolidone, 1.5kg dimethyl sulfoxide in 92.5kg water, obtains aqueous phase solution after stirring；
2, the preparation of oil-phase solution: with embodiment 1；
3, film-forming method is with embodiment 1.
Diaphragm detection method is with embodiment 1, and result is in Table 1.
Embodiment 5:
Reverse osmosis membrane production method is as follows:
1, the preparation of aqueous phase solution: with embodiment 4；
2, the preparation of oil-phase solution: be dissolved in the Petroleum of 100kg by pyromellitic trimethylsilyl chloride 0.15kg, obtains oil-phase solution after stirring；
3, film-forming method is with embodiment 1.
Diaphragm detection method is with embodiment 1, and result is in Table 1.
Embodiment 6:
Reverse osmosis membrane production method is as follows:
1, the preparation of aqueous phase solution: with embodiment 4；
2, the preparation of oil-phase solution: be dissolved in the Petroleum of 100kg by pyromellitic trimethylsilyl chloride 0.17kg, obtains oil-phase solution after stirring；
3, film-forming method is with embodiment 1.
Diaphragm detection method is with embodiment 1, and result is in Table 1.
Embodiment 7:
Reverse osmosis membrane production method is as follows:
1, the preparation of aqueous phase solution: add 3kg m-diaminobenzene., 0.5kg dodecylbenzene sodium sulfonate, 2kgN-methyl pyrrolidone, 4.5kg dimethyl sulfoxide in 90kg water, obtains aqueous phase solution after stirring；
2, the preparation of oil-phase solution: be dissolved in the Petroleum of 100kg by pyromellitic trimethylsilyl chloride 0.13kg, obtains oil-phase solution after stirring；
3, film-forming method is with embodiment 1.
Diaphragm detection method is with embodiment 1, and result is in Table 1.
Embodiment 8:
Reverse osmosis membrane production method is as follows:
1, the preparation of aqueous phase solution: add 3kg m-diaminobenzene., 0.5kg dodecylbenzene sodium sulfonate, 2.5kgN-methyl pyrrolidone, 4.5kg dimethyl sulfoxide in 89.5kg water, obtains aqueous phase solution after stirring；
2, the preparation of oil-phase solution: with embodiment 1；
3, film-forming method is with embodiment 1.
Diaphragm detection method is with embodiment 1, and result is in Table 1.
Table 1
As it can be seen from table 1 in aqueous phase solution dimethyl sulfoxide mix with N-Methyl pyrrolidone use effect more effective than single solvent.Along with dimethyl sulfoxide content increases, water flux promotes rapidly, but salt rejection rate also declines substantially；The effectiveness comparison adding N-Methyl pyrrolidone comparatively speaking is mild.Along with the raising of pyromellitic trimethylsilyl chloride concentration in oil-phase solution, diaphragm salt rejection rate is obviously improved, and water flux declines therewith, but after reaching finite concentration, salt rejection rate tends towards stability, but water flux continues to reduce.
The diaphragm that Example 4, embodiment 5 and embodiment 8 produce rolls growth 40 inches with full-automatic wound membrane machine, the membrane module of diameter 4 inch gage is tested, test condition is as follows: the NaCl solution of 1500ppm, pH is 7.5～8, temperature 25 DEG C, test pressure 150/100psi, the response rate is 15%, and gained test result is in Table 2.
Table 2
| Component numerals | Embodiment 4 | Embodiment 5 | Embodiment 8 |
| Test pressure/psi | 150 | 150 | 100 |
| Salt rejection rate/% | 99.0～99.4 | 99.5～99.6 | 98.5～99.0 |
| Aquifer yield/gpd | 2400～2800 | 2000～2300 | 2100～2400 |
As can be seen from Table 2, can realize film product salt rejection rate and aquifer yield are well regulated and controled by the technology of the present invention, accomplishing equipment with high desalinization product on the one hand, on the other hand under the lower pressure of pole, assembly still embodies moderate aquifer yield and of a relatively high salt rejection rate.
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all within the spirit and principles in the present invention, any amendment of making, equivalent replacement, improvement etc., should be included within protection scope of the present invention.
Claims (10)
1. an equipment with high desalinization and the controlled compound reverse osmosis membrane of flux, it is characterized in that, porous polysulfone supporting layer counterdie is coated with aqueous phase solution layer, is coated with oil-phase solution layer, make biphase to obtain polyamide ultrathin function stratum disjunctum by interface polymerization reaction, obtain after follow-up cleaning, drying；Wherein,
The surfactant of aqueous phase solution to be weight concentration be 0.5%～5% polyfunctional amine solution, weight concentration 0.5%～2% in aqueous phase solution layer, and the polar solvent of weight concentration 3%～10%, regulating pH value through sodium hydroxide after stirring to prepare to 7～9, described polyfunctional amine is aromatic series, aliphatic or alicyclic polyfunctional amine；
In oil-phase solution layer, oil-phase solution is add the multi-functional acyl halide that weight concentration is 0.05%～0.3% in the aliphatic hydrocarbon of 4～12 carbon atoms, cycloalphatic hydrocarbon or aromatic hydrocarbon; stirring and dissolving and get final product, described multi-functional acyl halide is aromatic series, aliphatic or alicyclic multi-functional acyl halide.
2. equipment with high desalinization according to claim 1 and the controlled compound reverse osmosis membrane of flux, it is characterised in that described polyfunctional amine is m-diaminobenzene., and its weight concentration accounting for aqueous phase solution is 3%.
3. equipment with high desalinization according to claim 1 and the controlled compound reverse osmosis membrane of flux, it is characterised in that described multi-functional acyl halide is pyromellitic trimethylsilyl chloride, and its weight concentration accounting for oil-phase solution is 0.099%～0.169%.
4. equipment with high desalinization according to claim 1 and the controlled compound reverse osmosis membrane of flux, it is characterised in that described surfactant is dodecylbenzene sodium sulfonate, and its weight concentration accounting for aqueous phase solution is 0.5%.
5. equipment with high desalinization according to claim 1 and the controlled compound reverse osmosis membrane of flux, it is characterized in that, described polar solvent is dimethyl sulphoxide solution or N-Methyl pyrrolidone solution or both mixed solutions, and its weight concentration accounting for aqueous phase solution is 4%～7%.
6. the preparation method of equipment with high desalinization according to any one of claim 1-5 and the controlled compound reverse osmosis membrane of flux, it is characterised in that comprise the steps:
(1) preparation of aqueous phase solution: select the one of aromatic series, aliphatic or alicyclic polyfunctional amine to be dissolved in the water, its weight concentration in aqueous is 0.5%～5%, after it is completely dissolved, the surfactant accounting for this aqueous solution weight 0.5%～2% is added again in this aqueous solution, and account for the polar solvent of this aqueous solution weight 3%～10%, the back end hydrogenation sodium oxide that stirs regulates solution ph between 7～9, namely obtains aqueous phase solution；
(2) preparation of oil-phase solution: select the one of aromatic series, aliphatic or alicyclic multi-functional acyl halide; it is dissolved in selected from containing the one in the aliphatic hydrocarbon of 4～12 carbon atoms, cycloalphatic hydrocarbon and aromatic hydrocarbon, obtaining oil-phase solution after stirring and dissolving according to the ratio accounting for total solution weight 0.05%～0.3%；
(3) on polysulfone supporting layer counterdie, aqueous phase solution it is coated with, remove the aqueous phase solution of excess surface, allow the polysulfone supporting layer counterdie having adsorbed aqueous phase solution through the closing space with heat supply and exhausting system again, control its internal temperature 20 DEG C～30 DEG C, relative humidity 50%～80%, allows the moisture of face volatilize further；Afterwards, it is coated with oil-phase solution in the above, removes excess surface oil-phase solution, enter in 30 DEG C～120 DEG C baking ovens and dry, form polyamide ultrathin stratum disjunctum；After follow-up cleaning, drying, finally give compound reverse osmosis membrane.
7. the preparation method of equipment with high desalinization according to claim 6 and the controlled compound reverse osmosis membrane of flux, it is characterised in that described polyfunctional amine is m-diaminobenzene., and its weight concentration accounting for aqueous phase solution is 3%.
8. the preparation method of equipment with high desalinization according to claim 6 and the controlled compound reverse osmosis membrane of flux, it is characterised in that described multi-functional acyl halide is pyromellitic trimethylsilyl chloride, and its weight concentration accounting for oil-phase solution is 0.099%～0.169%.
9. the preparation method of equipment with high desalinization according to claim 6 and the controlled compound reverse osmosis membrane of flux, it is characterised in that described surfactant is dodecylbenzene sodium sulfonate, and its weight concentration accounting for aqueous phase solution is 0.5%.
10. the preparation method of equipment with high desalinization according to claim 6 and the controlled compound reverse osmosis membrane of flux, it is characterized in that, described polar solvent is dimethyl sulphoxide solution or N-Methyl pyrrolidone solution or both mixed solutions, and its weight concentration accounting for aqueous phase solution is 4%～7%.
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