CN104959046A - Reverse osmosis membrane and preparation method thereof - Google Patents
Reverse osmosis membrane and preparation method thereof Download PDFInfo
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- CN104959046A CN104959046A CN201510357025.1A CN201510357025A CN104959046A CN 104959046 A CN104959046 A CN 104959046A CN 201510357025 A CN201510357025 A CN 201510357025A CN 104959046 A CN104959046 A CN 104959046A
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- reverse osmosis
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Abstract
The invention provides a reverse osmosis membrane. The reverse osmosis membrane comprises, by weight, 96.5%-97.2% of non-woven fabrics, 0.04% of m-phenylenediamine, 2.45%-3.26% of triethylamine, 0.05% of phase transfer catalyst, 0.04%-0.27% of trimesoyl chloride and 0.06%-1% of polysulfone. A preparation method of the reverse osmosis membrane includes the steps that 1, the m-phenylenediamine, the triethylamine and the phase transfer catalyst are dissolved in water to be prepared into a water phase; 2, the trimesoyl chloride is dissolved in organic solvent to be prepared into an organic phase; 3, the non-woven fabrics and the polysulfone are made into a polysulfone base membrane, a polysulfone layer of the polysulfone base membrane is in contact with water to make the polysulfone layer wet, and the redundant water phase is removed; 4, after the wet polysulfone layer is in contact reaction with the organic phase, the redundant organic phase is removed, and accordingly a polyamide reverse osmosis membrane is obtained through oven treatment. The reverse osmosis membrane can increase the initial permeation flux, and meanwhile the excellent salt removing rate, antifouling property and durability are achieved.
Description
Technical field
The present invention relates to Material Field, particularly relate to a kind of reverse osmosis membrane and preparation method thereof.
Technical background
Infiltration is that solvent passes the semi permeability diffusion barrier of isolation two kinds of solution and has the phenomenon of the solution movement of high solute concentration from the solution with low solute concentration to another.In this case, moved by solvent and the pressure acted on the solution with high solute concentration is referred to as osmotic pressure.But when applying the external pressure than osmotic pressure higher level, solvent moves to the solution with low solute concentration, and this phenomenon is referred to as counter-infiltration.According to principle of reverse osmosis, barometric gradient can be used as driving force, by pellicle, various types of salt or organic substance are separated.Utilize the reverse osmosis membrane of counter-infiltration phenomenon oneself through being used to the material of isolated molecule level, from salt solution or seawater, remove salt, and provide can for the water of family, commercial and industrial.
But it is lower to there is initial permeate flux efficiency in polyamide-based reverse osmosis membrane prepared by conventional method
Deficiency, cause the deterioration of water purifying function.Further, when using reverse osmosis membrane to carry out water treatment, solute or ionic compound may be adsorbed to reverse osmosis membrane surface and pollute this reverse osmosis membrane, thus cause water permeation characteristic, and such as permeation flux and salt rejection rate decline in time.Therefore, seem particularly important by the polyamide seawater desalination reverse osmosis film that Controlling Technology condition processability is good.
Summary of the invention
The present invention, for overcoming the deficiencies in the prior art, provides a kind of reverse osmosis membrane, and this reverse osmosis has high water flux and salt rejection rate performance, and stable performance.
Object of the present invention is achieved by the following technical programs:
A kind of reverse osmosis membrane, raw material comprises following component parts by weights and counts: non-woven fabrics 96.5 ~ 97.2%, m-phenylene diamine (MPD) 0.04%, triethylamine 2.45 ~ 3.26%, phase transfer catalyst 0.05%, pyromellitic trimethylsilyl chloride 0.04 ~ 0.27%, polysulfones 0.06 ~ 1%;
Further, the main component of above-mentioned non-woven fabrics is PET;
Further, above-mentioned phase transfer catalyst is the one in benzyltriethylammoinium chloride, triethylamine hydrochloride, tetrabutylammonium chloride;
Further, the preparation method of above-mentioned reverse osmosis membrane, comprises the steps:
(1) aqueous phase is mixed with by soluble in water to m-phenylene diamine (MPD), triethylamine and phase transfer catalyst;
(2) pyromellitic trimethylsilyl chloride is dissolved in organic solvent is mixed with organic phase;
(3) non-woven fabrics and polysulfones are made polysulfones counterdie, the polysulfones layer of polysulfones counterdie contact with aqueous phase cause its soak, remove unnecessary aqueous phase;
(4) by after wetting polysulfones layer and organic phase haptoreaction, remove after unnecessary organic phase through baking oven place
Reason obtains polyamide reverse osmose membrane;
Further, in above-mentioned steps (2), organic solvent is the one in Isopar G, cyclohexane, n-decane, normal heptane;
Further, the polysulfones layer of above-mentioned steps (3) polysulfones counterdie contacts with aqueous phase and causes its wetting time is 10 ~ 20min;
Further, above-mentioned steps (4) polysulfones layer and organic phase haptoreaction time 20s ~ 90s;
Further, the temperature of above-mentioned baking oven is 40 ~ 60 DEG C.
beneficial effect of the present invention:
A kind of reverse osmosis membrane of the present invention, according to the embodiment of the present invention's design, reverse osmosis membrane comprises polysulfones layer, described polysulfones layer has the hole formed in its surface, described hole have the distribution of preset range, average diameter and hole area than etc., therefore, compared with existing reverse osmosis membrane, reverse osmosis membrane of the present invention can realize the initial permeate flux improved, and has excellent salt rejection rate, antifouling property and durability simultaneously.
Accompanying drawing explanation
Fig. 1 is a kind of reverse osmosis membrane seawater reverse osmosis membrane of the present invention evaluating apparatus;
In figure, 1, former pond, 2, pure water pond, 3, high-pressure pump, 4, film testboard, 5, control valve, 6, flowmeter, 7, ball valve 1,8, ball valve 2,9, ball valve 3,10, ball valve 4,11, ball valve 5, A, produce water;
Fig. 2 is water flux under a kind of reverse osmosis membrane of the present invention different haptoreaction time and salt rejection rate.
Detailed description of the invention
Below in conjunction with accompanying drawing, the technical scheme of a kind of reverse osmosis membrane of the present invention is further illustrated.
Embodiment
The invention provides a kind of preparation method of reverse osmosis membrane, raw material comprises following component parts by weights and counts: non-woven fabrics 96.5 ~ 97.2%, m-phenylene diamine (MPD) 0.04%, triethylamine 2.45 ~ 3.26%, phase transfer catalyst 0.05%, pyromellitic trimethylsilyl chloride 0.04 ~ 0.27%, polysulfones 0.06 ~ 1%, and the main component of non-woven fabrics is PET; Transfer catalyst is the one in benzyltriethylammoinium chloride, triethylamine hydrochloride, tetrabutylammonium chloride; The preparation method of reverse osmosis membrane, specifically comprises the steps:
(1) aqueous phase is mixed with by soluble in water to m-phenylene diamine (MPD), triethylamine and phase transfer catalyst;
(2) pyromellitic trimethylsilyl chloride is dissolved in organic solvent is mixed with organic phase;
(3) non-woven fabrics and polysulfones are made polysulfones counterdie, the polysulfones layer of polysulfones counterdie removes unnecessary aqueous phase after contacting with aqueous phase and causing its wetting 10 ~ 20min;
(4) by after wetting polysulfones layer and organic phase haptoreaction 20s ~ 90s, after removing unnecessary organic phase, after 40 ~ 60 DEG C of oven for drying, polyamide reverse osmose membrane is obtained.
In step (2), organic solvent is the one in Isopar G, cyclohexane, n-decane, normal heptane.
Film properties is tested:
The N aCl aqueous solution of 32 g/L of 15L is prepared in the former pond of seawater reverse osmosis membrane evaluating apparatus (see figure 1), seawater reverse osmosis membrane being cut into fixed dimension loads in testboard, the mass concentration 32 g/L NaCI aqueous solution is switched to after first rinsing 15min with pure water under the pressure of 3.45 MPa, at 25 DEG C, under the pressure of 5.52MPa, test the performance of seawater reverse osmosis membrane.
As can be seen from Figure 2, the haptoreaction time is time of PA membrane film forming, and be condition of crucial importance, along with the increase of haptoreaction time, salt rejection rate presents the trend first increasing and subtract afterwards, and water flux presents downward trend always.The haptoreaction time, when being 60s, the salt rejection rate of poly-phthalein amine film peaked 99.6%, then along with the increase salt rejection rate of haptoreaction time declines to some extent.
The present invention contacts instead at polysulfones layer with organic phase, and add phase transfer catalyst (PTC) in answering, PTC is generally used for the reaction between two-phase, can fast reaction speed and reduction reaction temperature.As shown in Table 1, the performance of selected PTC to poly-phthalein amine film all improves a lot.
salt rejection rate when table 1 adds different PTC and water flux
When the mass fraction of triethylamine hydrochloride is 3% time, water flux reaches maximum 34 L/(m
2h).
The present invention have chosen 4 kinds of organic phase solvent, and the salt rejection rate under four kinds of solvents and water flux are in table 2.
salt rejection rate under table 2 four kinds of solvents and water flux
As can be seen from Table 2, IsoparG and n-decane can make the poly-phthalein amine film obtained have good performance, and these 2 kinds of solvents are all belong to Long carbon chain alkane, and the carbon chain lengths of Isopar G is 9 ~ 10, and the carbon chain lengths of n-decane is 10.
It should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention, can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.The all available prior art of each part not clear and definite in the present embodiment is realized.
Claims (8)
1. a reverse osmosis membrane, raw material comprises following component parts by weights and counts: non-woven fabrics 96.5 ~ 97.2%, m-phenylene diamine (MPD) 0.04%, triethylamine 2.45 ~ 3.26%, phase transfer catalyst 0.05%, pyromellitic trimethylsilyl chloride 0.04 ~ 0.27%, polysulfones 0.06 ~ 1%.
2. reverse osmosis membrane as claimed in claim 1, it is characterized in that, the main component of non-woven fabrics is PET.
3. reverse osmosis membrane as claimed in claim 1 or 2, it is characterized in that, phase transfer catalyst is the one in benzyltriethylammoinium chloride, triethylamine hydrochloride, tetrabutylammonium chloride.
4. the preparation method of reverse osmosis membrane as claimed in claim 1, comprises the steps:
(1) aqueous phase is mixed with by soluble in water to m-phenylene diamine (MPD), triethylamine and phase transfer catalyst;
(2) pyromellitic trimethylsilyl chloride is dissolved in organic solvent is mixed with organic phase;
(3) non-woven fabrics and polysulfones are made polysulfones counterdie, the polysulfones layer of polysulfones counterdie contact with aqueous phase cause its soak, remove unnecessary aqueous phase;
(4) by after wetting polysulfones layer and organic phase haptoreaction, remove after unnecessary organic phase through baking oven place
Reason obtains polyamide reverse osmose membrane.
5. the preparation method of reverse osmosis membrane as claimed in claim 4, is characterized in that: in step (2), organic solvent is the one in Isopar G, cyclohexane, n-decane, normal heptane.
6. the preparation method of reverse osmosis membrane as claimed in claim 4, is characterized in that: the polysulfones layer of step (3) polysulfones counterdie contacts with aqueous phase and causes its wetting time is 10 ~ 20min.
7. the preparation method of reverse osmosis membrane as claimed in claim 4, is characterized in that: step (4) polysulfones layer and organic phase haptoreaction time 20s ~ 90s.
8. the preparation method of reverse osmosis membrane as claimed in claim 4, is characterized in that: the temperature of described baking oven is 40 ~ 60 DEG C.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108452684A (en) * | 2018-03-20 | 2018-08-28 | 时代沃顿科技有限公司 | A kind of metal organic frame reverse osmosis membrane and preparation method thereof |
| CN108697991A (en) * | 2015-12-23 | 2018-10-23 | 索尔维特殊聚合物意大利有限公司 | Include the apertured polymeric film of silicate |
| CN109692579A (en) * | 2017-10-20 | 2019-04-30 | 中国石油化工股份有限公司 | Reverse osmosis membrane and its preparation method and application |
| US10688449B2 (en) | 2016-05-18 | 2020-06-23 | Lg Chem, Ltd. | Method for manufacturing water treatment separator, water treatment separator manufactured using same, and water treatment module comprising water treatment separator |
| CN115140899A (en) * | 2022-07-15 | 2022-10-04 | 浙江红狮环保股份有限公司 | Treatment technology of high organic matter and high salt wastewater |
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| CN102500244A (en) * | 2011-11-30 | 2012-06-20 | 杭州水处理技术研究开发中心有限公司 | Preparation method of reverse osmosis composite membrane for sea water desalinization |
| CN102716681A (en) * | 2012-06-01 | 2012-10-10 | 森泰环保（湖南）科技有限公司 | Reverse osmosis membrane and manufacturing method for reverse osmosis membrane |
| KR101250310B1 (en) * | 2012-08-30 | 2013-04-03 | 한국수자원공사 | Polyamide reverse osmosis membrane using polysulfone supporting material containing carbon nanotube and manufacturing method thereof |
| CN103240009A (en) * | 2013-05-22 | 2013-08-14 | 杭州北斗星膜制品有限公司 | Preparation method of polyamide reverse-osmosis membrane for sea water desalination |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102500244A (en) * | 2011-11-30 | 2012-06-20 | 杭州水处理技术研究开发中心有限公司 | Preparation method of reverse osmosis composite membrane for sea water desalinization |
| CN102716681A (en) * | 2012-06-01 | 2012-10-10 | 森泰环保（湖南）科技有限公司 | Reverse osmosis membrane and manufacturing method for reverse osmosis membrane |
| KR101250310B1 (en) * | 2012-08-30 | 2013-04-03 | 한국수자원공사 | Polyamide reverse osmosis membrane using polysulfone supporting material containing carbon nanotube and manufacturing method thereof |
| CN103240009A (en) * | 2013-05-22 | 2013-08-14 | 杭州北斗星膜制品有限公司 | Preparation method of polyamide reverse-osmosis membrane for sea water desalination |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108697991A (en) * | 2015-12-23 | 2018-10-23 | 索尔维特殊聚合物意大利有限公司 | Include the apertured polymeric film of silicate |
| US10688449B2 (en) | 2016-05-18 | 2020-06-23 | Lg Chem, Ltd. | Method for manufacturing water treatment separator, water treatment separator manufactured using same, and water treatment module comprising water treatment separator |
| CN109692579A (en) * | 2017-10-20 | 2019-04-30 | 中国石油化工股份有限公司 | Reverse osmosis membrane and its preparation method and application |
| CN108452684A (en) * | 2018-03-20 | 2018-08-28 | 时代沃顿科技有限公司 | A kind of metal organic frame reverse osmosis membrane and preparation method thereof |
| WO2019179082A1 (en) * | 2018-03-20 | 2019-09-26 | 时代沃顿科技有限公司 | Metal organic frame reverse osmosis membrane and preparation method therefor |
| CN108452684B (en) * | 2018-03-20 | 2020-04-24 | 时代沃顿科技有限公司 | Metal organic framework reverse osmosis membrane and preparation method thereof |
| CN115140899A (en) * | 2022-07-15 | 2022-10-04 | 浙江红狮环保股份有限公司 | Treatment technology of high organic matter and high salt wastewater |
| CN115140899B (en) * | 2022-07-15 | 2024-02-23 | 浙江红狮环保股份有限公司 | Treatment method of high-organic matter and high-salt wastewater |
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Application publication date: 20151007 |