CN106178969A - The preparation method of a kind of high-performance complex reverse osmosis membrane and prepared reverse osmosis membrane thereof - Google Patents
The preparation method of a kind of high-performance complex reverse osmosis membrane and prepared reverse osmosis membrane thereof Download PDFInfo
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- CN106178969A CN106178969A CN201610634534.9A CN201610634534A CN106178969A CN 106178969 A CN106178969 A CN 106178969A CN 201610634534 A CN201610634534 A CN 201610634534A CN 106178969 A CN106178969 A CN 106178969A
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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
- B01D67/0081—After-treatment of organic or inorganic membranes
- B01D67/0093—Chemical modification
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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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- 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
Abstract
The present invention proposes the preparation method of a kind of high-performance complex reverse osmosis membrane, preparation including aqueous phase liquid, prepared by preparation and the product of oil-phase solution, its key technology is to control interpolation kind and the addition of phosphorus-containing compound in oil-phase solution, phosphorus-containing compound and the acid chloride groups of reaction monomers in oil phase are with the form effect of coordinate bond, thus change oil phase reaction monomers solubility parameter in oil solvent, during carrying out interface polymerization reaction, be conducive to oil phase monomer fast transferring to water phase and an oil phase interface, accelerate and the polyreaction of polyfunctional amine reaction monomers in aqueous phase solution, the polyamide functional layer making generation is thin and compact, water flux and salt rejection rate performance are the highest.The product prepared is in the NaCl solution of 1500ppm, and pH value is 7.5～8, temperature 25 DEG C, and under the conditions of test pressure 150psi, salt rejection rate is 94.52%～99.55%, and water flux is 40.8gfd～61.2gfd.
Description
Technical field
The present invention relates to reverse osmosis membrane technology field, particularly relate to a kind of high-performance complex reverse osmosis membrane preparation method and
Its reverse osmosis membrane prepared.
Background technology
Reverse osmosis technology is under certain pressure effect, by means of molten by solution of the selective retention effect of reverse osmosis membrane
Matter and the separate separation method of solvent, compared with other film kinds (nanofiltration, ultrafiltration, microfiltration etc.), have less membrane aperture, can have
Effect removes in water the impurity such as salt, Organic substance, colloid, antibacterial.Reverse osmosis membrane has been widely used for environment, pharmacy, chemical industry, work
Multiple industry such as industry and field.In order to improve the efficiency of reverse osmosis membrane, some companies and research institution have attempted many raising films
The method of aquifer yield, has plenty of and adds the additives such as amine salt, isopropanol, dimethyl sulfoxide in aqueous phase solution, but the water to film
Flux promotes little；Have adds polyreaction chain terminating agent, such as Benzenecarbonyl chloride., although this method is to carrying in oil-phase solution
High diaphragm flux has certain help, but reduces the crosslinking degree of reverse osmosis membrane two phase reaction monomer, makes the membrane structure pine of formation
Dissipate, be that these constrain the application of reverse osmosis membrane the most to a certain extent to lose diaphragm salt rejection rate as cost.Therefore, explore
The preparation method of a kind of new complex reverse osmosis membrane, is greatly improved diaphragm under ensureing the salt rejection rate premise that reverse osmosis membrane is excellent
Water-yielding capacity, has important practical significance and economic benefit.
Summary of the invention
In view of this, it is an object of the invention to propose the preparation method of a kind of high-performance complex reverse osmosis membrane and prepare
Reverse osmosis membrane, reverse osmosis membrane diaphragm water flux under low operating pressures is high, ensures diaphragm salt rejection rate simultaneously.
For solving above-mentioned technical problem, the present invention is achieved by the following technical solutions:
The preparation method of a kind of high-performance complex reverse osmosis membrane, comprises the steps:
(1) preparation of aqueous phase liquid: aromatic series polyfunctional amine and surfactant are successively dissolved in the water, stir
After, in obtained aqueous solution, add sodium hydrate regulator solution pH value i.e. obtain aqueous phase liquid, wherein, the many officials of described aromatic series to 7～9
It is 3% that energy amine accounts for the mass concentration of aqueous solution, and it is 0.5% that surfactant accounts for the mass concentration of aqueous solution；
(2) preparation of oil-phase solution: multi-functional for aromatic series acyl halide and phosphorus-containing compound are successively dissolved in stone
In cerebrol, obtaining oil phase liquid after stirring, wherein, the multi-functional acyl halide of aromatic series accounts for the mass concentration of oil solution and is
0.12%, it is 0.12%～0.36% that phosphorus-containing compound accounts for the mass concentration of oil solution；
(3) prepared by product: first the non-woven fabrics counterdie scribbling polysulfones is immersed aqueous phase solution and keeps 30 seconds, uses surface finish
Stainless steel rider remove the aqueous phase liquid of non-woven fabrics counterdie excess surface after, then this counterdie is immersed oil phase liquid keeping 40 seconds, removes
After removing surface residual oil phase liquid, subsequently enter in 80 DEG C of baking ovens and keep 5 minutes, the most cleaned drying, obtain high-performance and be combined
Type reverse osmosis membrane.
As preferably, in described step (1), described aromatic series polyfunctional amine is m-diaminobenzene., described surfactant
Selected from dodecylbenzene sodium sulfonate or dodecyl sodium sulfate.
As preferably, in described step (2), the multi-functional acyl halide of described aromatic series is pyromellitic trimethylsilyl chloride,
Described phosphorus-containing compound is the one in trimethyl phosphate, triethyl phosphate, triphenyl phosphate, triphenyl phosphorus.
The invention allows for a kind of reverse osmosis membrane prepared according to above-mentioned preparation method, it is molten at the NaCl of 1500ppm
Liquid, pH value is 7.5～8, temperature 25 DEG C, and under the conditions of test pressure 150psi, salt rejection rate is 94.52%～99.55%, water flux
For 40.8gfd～61.2gfd.
The present invention compared with prior art has the beneficial effect that the preparation method of the present invention, due to phosphorus-containing compound
Addition, with the acid chloride groups of reaction monomers in oil phase with the form effect of coordinate bond, thus oil phase reaction monomers can be changed and exists
Solubility parameter in oil solvent, during carrying out interface polymerization reaction, beneficially oil phase monomer fast transferring is to water oil two
Intersection interface, accelerates and the polyreaction of polyfunctional amine reaction monomers in aqueous phase solution, the polyamide functional layer making generation thin and
Densification, water flux and salt rejection rate performance are the highest.The NaCl solution of the product 1500ppm that the present invention prepares, pH value is 7.5
～8, temperature 25 DEG C, test pressure 150psi under the conditions of, salt rejection rate is 94.52%～99.55%, water flux be 40.8gfd～
61.2gfd。
Detailed description of the invention
Get information about the present invention for allowing those skilled in the art become apparent from, the present invention will be made further below
Explanation.
The present invention uses homemade porous polysulfone supporting layer counterdie, and first soak phase liquid by it, then soaks oil-phase solution, and two communicate
Cross interface polymerization reaction and obtain polyamide ultrathin function stratum disjunctum, more post-treated cleaning finally gives compound reverse osmosis membrane
Sheet.In order to obtain higher water flux under driving at ultralow pressure and ensure that diaphragm salt rejection rate is controlled, key technology of the present invention is control
The interpolation kind of phosphorus-containing compound and addition in oil-phase solution processed.Describe in detail below in conjunction with being embodied as case.
Comparative example:
Reverse osmosis membrane preparation method is as follows:
1, the preparation of aqueous phase liquid: the m-diaminobenzene. of mass concentration 3% will be accounted for and account for the detergent alkylate of mass concentration 0.5%
Sodium sulfonate is successively dissolved in the water, and the back end hydrogenation sodium oxide that stirs regulation solution ph, between 7～9, i.e. obtains aqueous phase liquid；
2, the preparation of oil-phase solution: the pyromellitic trimethylsilyl chloride accounting for mass concentration 0.12% is dissolved in alkane mixed solution stone
In cerebrol, after stirring and get final product；
3, first the non-woven fabrics counterdie scribbling polysulfones is immersed aqueous phase solution to keep 30 seconds, with the stainless steel rider of surface finish
After removing the aqueous phase solution of excess surface, then this counterdie immersed oil-phase solution and keeps 40 seconds, removing surface residual oil phase molten
After liquid, subsequently enter in 80 DEG C of baking ovens and keep 5 minutes, then after follow-up cleaning, drying, finally give high-performance compound reverse osmosis
Permeable membrane.
Diaphragm uses following condition to detect: the NaCl solution of 1500ppm, and pH is 7.5～8, temperature 25 DEG C, test pressure
Power 150psi, acquired results is shown in Table 1.
Embodiment 1:
Reverse osmosis membrane production method is as follows:
1, the preparation of aqueous phase liquid: same to comparative example；
2, the preparation of oil-phase solution: the pyromellitic trimethylsilyl chloride of mass concentration 0.12% will be accounted for and account for mass concentration 0.12%
Trimethyl phosphate is dissolved in alkane mixed solution Petroleum；
3, the same comparative example of film-forming method.
The same comparative example of diaphragm detection method, the results are shown in Table 1.
Embodiment 2:
Reverse osmosis membrane production method is as follows:
1, the preparation of aqueous phase liquid: same to comparative example；
2, the preparation of oil-phase solution: the pyromellitic trimethylsilyl chloride of mass concentration 0.12% will be accounted for and account for mass concentration 0.24%
Trimethyl phosphate is dissolved in alkane mixed solution Petroleum；
3, the same comparative example of film-forming method.
The same comparative example of diaphragm detection method, the results are shown in Table 1.
Embodiment 3:
Reverse osmosis membrane production method is as follows:
1, the preparation of aqueous phase liquid: same to comparative example；
2, the preparation of oil-phase solution: the pyromellitic trimethylsilyl chloride of mass concentration 0.12% will be accounted for and account for mass concentration 0.36%
Trimethyl phosphate is dissolved in alkane mixed solution Petroleum；
3, the same comparative example of film-forming method.
The same comparative example of diaphragm detection method, the results are shown in Table 1.
Embodiment 4:
Reverse osmosis membrane production method is as follows:
1, the preparation of aqueous phase liquid: same to comparative example；
2, the preparation of oil-phase solution: the pyromellitic trimethylsilyl chloride of mass concentration 0.12% will be accounted for and account for mass concentration 0.12%
Triethyl phosphate is dissolved in alkane mixed solution Petroleum；
3, the same comparative example of film-forming method.
The same comparative example of diaphragm detection method, the results are shown in Table 1.
Embodiment 5:
Reverse osmosis membrane production method is as follows:
1, the preparation of aqueous phase liquid: same to comparative example；
2, the preparation of oil-phase solution: the pyromellitic trimethylsilyl chloride of mass concentration 0.12% will be accounted for and account for mass concentration 0.24%
Triethyl phosphate is dissolved in alkane mixed solution Petroleum；
3, the same comparative example of film-forming method.
The same comparative example of diaphragm detection method, the results are shown in Table 1.
Embodiment 6:
Reverse osmosis membrane production method is as follows:
1, the preparation of aqueous phase liquid: same to comparative example；
2, the preparation of oil-phase solution: the pyromellitic trimethylsilyl chloride of mass concentration 0.12% will be accounted for and account for mass concentration 0.36%
Triethyl phosphate is dissolved in alkane mixed solution Petroleum；
3, the same comparative example of film-forming method.
The same comparative example of diaphragm detection method, the results are shown in Table 1.
Embodiment 7:
Reverse osmosis membrane production method is as follows:
1, the preparation of aqueous phase liquid: same to comparative example；
2, the preparation of oil-phase solution: the pyromellitic trimethylsilyl chloride of mass concentration 0.12% will be accounted for and account for mass concentration 0.12%
Triphenyl phosphate is dissolved in alkane mixed solution Petroleum；
3, the same comparative example of film-forming method.
The same comparative example of diaphragm detection method, the results are shown in Table 1.
Embodiment 8:
Reverse osmosis membrane production method is as follows:
1, the preparation of aqueous phase liquid: same to comparative example；
2, the preparation of oil-phase solution: the pyromellitic trimethylsilyl chloride of mass concentration 0.12% will be accounted for and account for mass concentration 0.24%
Triphenyl phosphate is dissolved in alkane mixed solution Petroleum；
3, the same comparative example of film-forming method.
The same comparative example of diaphragm detection method, the results are shown in Table 1.
Embodiment 9:
Reverse osmosis membrane production method is as follows:
1, the preparation of aqueous phase liquid: same to comparative example；
2, the preparation of oil-phase solution: the pyromellitic trimethylsilyl chloride of mass concentration 0.12% will be accounted for and account for mass concentration 0.36%
Triphenyl phosphate is dissolved in alkane mixed solution Petroleum；
3, the same comparative example of film-forming method.
The same comparative example of diaphragm detection method, the results are shown in Table 1.
Embodiment 10:
Reverse osmosis membrane production method is as follows:
1, the preparation of aqueous phase liquid: same to comparative example；
2, the preparation of oil-phase solution: the pyromellitic trimethylsilyl chloride of mass concentration 0.12% will be accounted for and account for mass concentration 0.12%
Triphenyl phosphorus is dissolved in alkane mixed solution Petroleum；
3, the same comparative example of film-forming method.
The same comparative example of diaphragm detection method, the results are shown in Table 1.
Embodiment 11:
Reverse osmosis membrane production method is as follows:
1, the preparation of aqueous phase liquid: same to comparative example；
2, the preparation of oil-phase solution: the pyromellitic trimethylsilyl chloride of mass concentration 0.12% will be accounted for and account for mass concentration 0.24%
Triphenyl phosphorus is dissolved in alkane mixed solution Petroleum；
3, the same comparative example of film-forming method.
The same comparative example of diaphragm detection method, the results are shown in Table 1.
Embodiment 12:
Reverse osmosis membrane production method is as follows:
1, the preparation of aqueous phase liquid: same to comparative example；
2, the preparation of oil-phase solution: the pyromellitic trimethylsilyl chloride of mass concentration 0.12% will be accounted for and account for mass concentration 0.36%
Triphenyl phosphorus is dissolved in alkane mixed solution Petroleum；
3, the same comparative example of film-forming method.
The same comparative example of diaphragm detection method, the results are shown in Table 1.
Table 1
| Phosphorus-containing compound kind | Phosphorus-containing compound content (%) | Water flux (GFD) | Salt rejection rate (%) | |
| Comparative example | / | / | 36.0 | 99.56 |
| Embodiment 1 | Trimethyl phosphate | 0.12 | 47.4 | 99.09 |
| Embodiment 2 | Trimethyl phosphate | 0.24 | 52.8 | 97.93 |
| Embodiment 3 | Trimethyl phosphate | 0.36 | 53.4 | 95.49 |
| Embodiment 4 | Triethyl phosphate | 0.12 | 43.2 | 99.32 |
| Embodiment 5 | Triethyl phosphate | 0.24 | 48.6 | 98.93 |
| Embodiment 6 | Triethyl phosphate | 0.36 | 50.4 | 97.27 |
| Embodiment 7 | Triphenyl phosphate | 0.12 | 57.0 | 98.17 |
| Embodiment 8 | Triphenyl phosphate | 0.24 | 60.6 | 96.33 |
| Embodiment 9 | Triphenyl phosphate | 0.36 | 61.2 | 94.52 |
| Embodiment 10 | Triphenyl phosphorus | 0.12 | 40.8 | 99.55 |
| Embodiment 11 | Triphenyl phosphorus | 0.24 | 43.8 | 99.47 |
| Embodiment 12 | Triphenyl phosphorus | 0.36 | 45.0 | 99.4 |
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all essences in the present invention
Within god and principle, any modification, equivalent substitution and improvement etc. made, should be included within the scope of the present invention.
Claims (4)
1. the preparation method of a high-performance complex reverse osmosis membrane, it is characterised in that comprise the steps:
(1) preparation of aqueous phase liquid: aromatic series polyfunctional amine and surfactant are successively dissolved in the water, after stirring, to
Obtained aqueous solution adds sodium hydrate regulator solution pH value and i.e. obtains aqueous phase liquid, wherein, described aromatic series polyfunctional amine to 7～9
The mass concentration accounting for aqueous solution is 3%, and it is 0.5% that surfactant accounts for the mass concentration of aqueous solution；
(2) preparation of oil-phase solution: multi-functional for aromatic series acyl halide and phosphorus-containing compound are successively dissolved in Petroleum
In, obtain oil phase liquid after stirring, wherein, the multi-functional acyl halide of aromatic series accounts for the mass concentration of oil solution and is
0.12%, it is 0.12%～0.36% that phosphorus-containing compound accounts for the mass concentration of oil solution；
(3) prepared by product: first the non-woven fabrics counterdie scribbling polysulfones is immersed aqueous phase solution holding 30 seconds, with surface finish not
After rust steel rider removes the aqueous phase liquid of non-woven fabrics counterdie excess surface, then this counterdie immersed oil phase liquid and keeps 40 seconds, removing table
After the remnants oil phase liquid of face, subsequently enter in 80 DEG C of baking ovens and keep 5 minutes, the most cleaned drying, obtain high-performance compound anti-
Permeable membrane.
Preparation method the most according to claim 1, it is characterised in that in described step (1), described aromatic series polyfunctional amine
For m-diaminobenzene., described surfactant is selected from dodecylbenzene sodium sulfonate or dodecyl sodium sulfate.
Preparation method the most according to claim 1, it is characterised in that in described step (2), described aromatic series is multi-functional
Acyl halide is pyromellitic trimethylsilyl chloride, described phosphorus-containing compound be trimethyl phosphate, triethyl phosphate, triphenyl phosphate, three
One in phenyl phosphorus.
4. the reverse osmosis membrane prepared according to the preparation method described in any one of claims 1 to 3, it is characterised in that at 1500ppm
NaCl solution, pH value is 7.5～8, temperature 25 DEG C, test pressure 150psi under the conditions of, salt rejection rate be 94.52%～
99.55%, water flux is 40.8gfd～61.2gfd.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107596930A (en) * | 2017-08-24 | 2018-01-19 | 江苏亚峰科技集团有限公司 | A kind of reverse osmosis film |
| CN107617346A (en) * | 2017-09-08 | 2018-01-23 | 宁波日新恒力科技有限公司 | A kind of polyamide reverse osmosis composite film and preparation method thereof |
| CN110756061A (en) * | 2019-10-12 | 2020-02-07 | 万华化学集团股份有限公司 | Oxidation-resistant high-flux reverse osmosis membrane and preparation method and application thereof |
| CN110813107A (en) * | 2019-11-08 | 2020-02-21 | 恩泰环保科技（常州）有限公司 | High-flux low-pressure composite reverse osmosis membrane and preparation method thereof |
| CN110975621A (en) * | 2019-12-25 | 2020-04-10 | 恩泰环保科技（常州）有限公司 | Reverse osmosis membrane based on weak base-weak acid buffer system and preparation method thereof |
| CN111408281A (en) * | 2019-01-07 | 2020-07-14 | 中国石油化工股份有限公司 | Composite forward osmosis membrane and preparation method thereof |
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| CN110813107A (en) * | 2019-11-08 | 2020-02-21 | 恩泰环保科技（常州）有限公司 | High-flux low-pressure composite reverse osmosis membrane and preparation method thereof |
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Effective date of registration: 20190401 Address after: 410205 6 Lu Tian Lu, high tech Development Zone, Changsha, Hunan Applicant after: Hunan Qinsen High-tech New Material Co.,Ltd. Address before: 410000 6 Lu Tian Lu, high tech Development Zone, Changsha, Hunan Applicant before: HUNAN KEENSEN TECHNOLOGY CO.,LTD. |
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Application publication date: 20161207 |