CN109126489A - A kind of preparation method of small molecular cut off polysulfone ultrafiltration membrane - Google Patents
A kind of preparation method of small molecular cut off polysulfone ultrafiltration membrane Download PDFInfo
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- CN109126489A CN109126489A CN201811155951.0A CN201811155951A CN109126489A CN 109126489 A CN109126489 A CN 109126489A CN 201811155951 A CN201811155951 A CN 201811155951A CN 109126489 A CN109126489 A CN 109126489A
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- ultrafiltration membrane
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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
- B01D71/66—Polymers having sulfur in the main chain, with or without nitrogen, oxygen or carbon only
- B01D71/68—Polysulfones; Polyethersulfones
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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
- B01D61/14—Ultrafiltration; Microfiltration
- B01D61/145—Ultrafiltration
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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
- B01D67/0009—Organic membrane manufacture by phase separation, sol-gel transition, evaporation or solvent quenching
- B01D67/0013—Casting processes
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- Dispersion Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention discloses a kind of preparation method of small molecular cut off polysulfone ultrafiltration membrane, 1) polysulfones and additive are dissolved into solvent and obtain casting solution；2) casting solution is subjected to vacuum defoamation, and it is prepared to polysulfone ultrafiltration membrane basement membrane on industrial equipment；3) polyvinyl alcohol (PVA) aqueous solution is prepared；4) PVA aqueous solution is added after a certain amount of concentrated sulfuric acid to the ultrafiltration membrane surface for being coated in preparation, then puts it into baking oven and is reacted；5) ultrafiltration membrane after reacting, which impregnates, to be cleaned in pure water to get required ultrafiltration membrane.The present invention prepares composite membrane by react with PVA in polysulfones membrane surface, changes reaction condition in preparing film engineering and film surface cortex and micropore are adjusted with this, obtain the polysulfone ultrafiltration membrane of different molecular weight cut off.
Description
Technical field
The present invention is a kind of method for preparing small molecular cut off polysulfone ultrafiltration membrane, belongs to ultrafiltration membrane preparation technical field.
Background technique
Ultrafiltration membrane is one of one total kind of novel chemical unit operation, and main effect is to be separated by filtration, be concentrated, purifying biological system
In product, medicine and food industry；It is also used in the devices such as the preparation of blood, waste water and ultrapure water, application is very extensive.Ultrafiltration
UF membrane may replace the natural subsidence in traditional handicraft, plate-frame filtering, and vacuum drum is centrifugated, and solvent extraction, resin mentions
It is pure, the technical process such as active carbon decoloring.The process is normal-temperature operation, and no phase-state change does not generate secondary pollution.With very good
The advantages of.
Scientific research personnel is very deeply comprehensive to the research of ultrafiltration membrane at present, and various types of ultrafiltration membranes all have, respectively
The ultrafiltration membrane of kind trapped molecular weight is also to have, but the ultrafiltration membrane (retention molecule is less than 5000) of low retention molecule compares in the market
It is less, and flux is all relatively low.Therefore the ultrafiltration membrane for studying lower retention molecule is needed.Research has low retention molecule
Ultrafiltration membrane can substitute part nanofiltration membrane to a certain extent, so that ultrafiltration membrane has wider application range.This is specially
Benefit has invented a kind of method for preparing different trapped molecular weight ultrafiltration membranes.
Summary of the invention
The object of the present invention is to provide a kind of methods for preparing different molecular weight cut off ultrafiltration membrane.
For this purpose, the technical scheme is that a kind of preparation method of small molecular cut off polysulfone ultrafiltration membrane, feature exist
In: include the following steps:
1) polysulfones and additive are dissolved into solvent and obtain casting solution；
2) casting solution is subjected to vacuum defoamation, and prepares polysulfone ultrafiltration membrane basement membrane；
3) polyethylene glycol (PVA) aqueous solution that preparation concentration is 0.02-0.2wt%；
4) PVA aqueous solution is added after a certain amount of concentrated sulfuric acid to the ultrafiltration membrane surface for being coated in preparation, then puts it into baking
It is reacted in case；
5) ultrafiltration membrane after reacting, which impregnates, to be cleaned in pure water to get required ultrafiltration membrane.
In above-mentioned preparation method:
Step 1) the additive is trimesic acid (TMA), and polysulfones and trimesic acid (TMA) are dissolved into solvent
Obtain casting solution.
Total mass percentage of step 1) the additive trimesic acid is 2%.
In the step 4), the content of the concentrated sulfuric acid is 0.01% (volume ratio) in the PVA aqueous solution.
PVA mixed solution is coated uniformly on polysulfones membrane surface in the step 4), and about 1 minute or so.
The step 4) by coating after film be put into baking oven, the time be 10 minutes, temperature be respectively 60 DEG C, 80 DEG C and
90℃。
Ultrafiltration membrane obtained impregnates 12 hours in pure water in the step 5).
The beneficial effects of the present invention are: preparation method of the present invention is simple, raw material sources are cheap extensively；By film surface into
Row is modified, and controls the process conditions of preparation film forming, is regulated and controled with this to ultrafiltration film properties and structure, suitable for film point
From field.Can be observed according to the SEM figure to membrane plane, film in temperature 60 C have biggish hole, 80 DEG C and 90 DEG C
When have lesser aperture；The composite membrane trapped molecular weight prepared in the case of 60 DEG C is both greater than 10000, at 90 DEG C, PVA concentration
0.02wt% can retain lesser molecule (800)；Temperature can influence the reaction of film surface generation, to change film surface knot
Structure influences film properties.The ultrafiltration composite membrane of temperature collective effect preparation, can retain different molecular matter when PVA content and reaction
Amount.
Detailed description of the invention
It is described in further detail below in conjunction with attached drawing and embodiments of the present invention
Fig. 1 is the rejection of polysulfones composite hyperfiltration membrane (PVA0.02wt%) at different temperatures, and S1 is 60 DEG C, S2 80
DEG C, S3 is 90 DEG C；
Fig. 2 is the rejection of polysulfones composite hyperfiltration membrane (PVA0.03wt%) at different temperatures, and S4 is 60 DEG C, S5 80
DEG C, S6 is 90 DEG C；
Fig. 3 is the rejection of polysulfones composite hyperfiltration membrane (PVA0.05wt%) at different temperatures, and S7 is 60 DEG C, S8 80
DEG C, S9 is 90 DEG C；
Fig. 4 is the rejection of polysulfones composite hyperfiltration membrane (PVA0.1wt%) at different temperatures, and S10 is 60 DEG C, S11 80
DEG C, S12 is 90 DEG C；
Fig. 5 is the rejection of polysulfones composite hyperfiltration membrane (PVA0.2wt%) at different temperatures, and S13 is 60 DEG C, S14 80
DEG C, S15 is 90 DEG C.
Specific embodiment
The present invention is done below with reference to example and is further explained.The following example is merely to illustrate the present invention, but simultaneously
It is not used to limit practical range of the invention.
Embodiment 1 prepares polyvinyl alcohol water solution
(1) preparation of PVA aqueous solution: weighing 485g pure water and heated with heating stirrer, temperature control 30 DEG C with
Under, it weighs 15g polyvinyl alcohol (PVA) and is added in weighed pure water, being stirred a hour makes PVA be evenly distributed on pure water
In, heating stirring is then carried out to it, temperature is controlled at 95 DEG C, so that its solution is become colorless and transparent and particle, as institute is not present
Needing content is the PVA aqueous solution of 3%wt, spare.
(2) whether titration test solution is pure, and discovery solution does not go out after iodine solution is added dropwise is carried out to PVA aqueous solution with iodine solution
Existing floccule, solution is available, and no person re-starts preparation.
Embodiment 2 prepares polysulfones ultrafiltration composite membrane
(1) the PVA aqueous solution prepared in example 1 is diluted to 0.02wt% with pure water, the solution after weighing 75g dilution,
The 0.02ml concentrated sulfuric acid is added wherein, it is spare.
(2) solution prepared by (1) in embodiment 2 is coated uniformly on membrane surface by the polysulfones basement membrane for choosing certain size,
It is put into baking oven after about 1 minute or so, temperature control is 60 DEG C, and the time is 10 minutes.
(3) composite membrane prepared immerses 12h in pure water, as required ultrafiltration membrane.Contact angle is 69.64 ± 3, and pure water is logical
Amount is 74.096 ± 10, molecular weight 10000 (rejection 76.71%).
Embodiment 3
By for PVA concentration dilution to 0.03wt%, other steps are constant in step (1) in embodiment 2.Contact angle be 73,7 ±
3, pure water flux is 66.421 ± 10, molecular weight 10000 (rejection 65.02%).
Embodiment 4
By for PVA concentration dilution to 0.05wt%, other steps are constant in step (1) in embodiment 3.Contact angle is 70.68
± 3, pure water flux is 39.69 ± 10, molecular weight 10000 (rejection 85.33%).
Embodiment 5
By for PVA concentration dilution to 0.1wt%, other steps are constant in step (1) in embodiment 4.Contact angle be 71,76 ±
4, pure water flux is 26.81 ± 5, molecular weight 10000 (rejection 87.87%).
Embodiment 6
By for PVA concentration dilution to 0.2wt%, other steps are constant in step (1) in embodiment 5.Contact angle be 67.74 ±
5, pure water flux is 17.977 ± 5, molecular weight 10000 (rejection 72.7%).
Embodiment 7
It is 80 DEG C by temperature controls in step (2) in embodiment 2, other steps are constant.Contact angle is 60.52 ± 5, pure water
Flux is 47.81 ± 5, molecular weight 10000 (rejection 87.14%).
Embodiment 8
By for PVA concentration dilution to 0.03wt%, other steps are constant in step (1) in embodiment 7.Contact angle is 61.06
± 5, pure water flux is 33.818 ± 5, molecular weight 6000 (rejection 89.58%).
Embodiment 9
By for PVA concentration dilution to 0.05wt%, other steps are constant in step (1) in embodiment 8.Contact angle is 66.78
± 5, pure water flux is 21.241 ± 5, molecular weight 6000 (rejection 94.95%).
Embodiment 10
By for PVA concentration dilution to 0.1wt%, other steps are constant in step (1) in embodiment 9.Contact angle be 59.76 ±
5, pure water flux is 5.65 ± 3, molecular weight 1000 (rejection 95.04%).
Embodiment 11
By for PVA concentration dilution to 0.2wt%, other steps are constant in step (1) in embodiment 3.Contact angle be 72.08 ±
4, pure water flux is 7.368 ± 4, molecular weight 1000 (rejection 94.24%).
Embodiment 12
It is 90 DEG C by temperature controls in step (2) in embodiment 2, other steps are constant.Contact angle is 58.14 ± 3, pure water
Flux is 43.634 ± 10, molecular weight 6000 (rejection 93.26%).
Embodiment 13
By for PVA concentration dilution to 0.03wt%, other steps are constant in step (1) in embodiment 12.Contact angle is 72.62
± 5, pure water flux is 41.477 ± 10, molecular weight 10000 (rejection 96.25%).
Embodiment 14
By for PVA concentration dilution to 0.05wt%, other steps are constant in step (1) in embodiment 13.Contact angle is 75.76
± 3, pure water flux is 25.341 ± 5, molecular weight 6000 (rejection 94.75%).
Embodiment 15
By for PVA concentration dilution to 0.1wt%, other steps are constant in step (1) in embodiment 14.Contact angle is 65.88
± 3, pure water flux is 8.17 ± 5, molecular weight 800 (rejection 92.29%).
Embodiment 16
By for PVA concentration dilution to 0.2wt%, other steps are constant in step (1) in embodiment 15.Contact angle be 77.5 ±
5, pure water flux is 3.537 ± 3, molecular weight 1000 (rejection 89.5%).
Claims (6)
1. a kind of preparation method of small molecular cut off polysulfone ultrafiltration membrane, it is characterised in that:
Include the following steps:
1) polysulfones and additive are dissolved into solvent and obtain casting solution；
2) casting solution is subjected to vacuum defoamation, and prepares polysulfone ultrafiltration membrane basement membrane；
3) polyethylene glycol (PVA) aqueous solution that preparation concentration is 0.02-0.2wt%；
4) PVA aqueous solution is added after a certain amount of concentrated sulfuric acid to the ultrafiltration membrane surface for being coated in preparation, is then put it into baking oven
It is reacted；
5) ultrafiltration membrane after reacting, which impregnates, to be cleaned in pure water to get required ultrafiltration membrane.
2. preparation method according to claim 1, it is characterised in that: the additive is trimesic acid (TMA).
3. preparation method according to claim 2, it is characterised in that: in the casting solution, the trimesic acid it is total
Mass percentage be 2%.
4. preparation method according to claim 1, it is characterised in that: in step 4), the concentrated sulfuric acid contains in the PVA aqueous solution
Amount is 0.01% (volume ratio).
5. preparation method according to claim 1, it is characterised in that: in step 4), the film after the coating is put into baking oven,
Time is 10 minutes, and temperature is respectively 60 DEG C, 80 DEG C and 90 DEG C.
6. preparation method according to claim 1, it is characterised in that: in step 5), the time impregnated in pure water is
12h。
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| CN201811155951.0A CN109126489B (en) | 2018-09-30 | 2018-09-30 | Preparation method of small-interception-molecular-weight polysulfone ultrafiltration membrane |
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| CN201811155951.0A CN109126489B (en) | 2018-09-30 | 2018-09-30 | Preparation method of small-interception-molecular-weight polysulfone ultrafiltration membrane |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112808034A (en) * | 2020-12-22 | 2021-05-18 | 浙江迪萧环保科技有限公司 | Preparation method of novel composite loose nanofiltration membrane |
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| CN1509804A (en) * | 2002-12-26 | 2004-07-07 | 天津工业大学膜科学与技术研究所 | Method for preparing composite hollow fibre membrane |
| CN101073750A (en) * | 2007-03-30 | 2007-11-21 | 浙江大学 | Method for producing density and gradient sectional porous ultrafiltration membrane |
| CN102091538A (en) * | 2011-01-10 | 2011-06-15 | 杭州水处理技术研究开发中心有限公司 | Method for preparing polyvinyl alcohol nanofiltration membrane with high rejection coefficient |
| JP5397772B2 (en) * | 2010-01-13 | 2014-01-22 | 独立行政法人物質・材料研究機構 | Polymer self-supporting membrane and separation membrane using the same |
| CN106914156A (en) * | 2017-04-10 | 2017-07-04 | 浙江工业大学 | A kind of preparation method of Novel polyvinyl alcohol NF membrane |
| CN108159894A (en) * | 2018-01-17 | 2018-06-15 | 浙江工业大学 | A kind of preparation method of polyvinyl alcohol composite nanometer filtering film |
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2018
- 2018-09-30 CN CN201811155951.0A patent/CN109126489B/en active Active
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| CN1509804A (en) * | 2002-12-26 | 2004-07-07 | 天津工业大学膜科学与技术研究所 | Method for preparing composite hollow fibre membrane |
| CN101073750A (en) * | 2007-03-30 | 2007-11-21 | 浙江大学 | Method for producing density and gradient sectional porous ultrafiltration membrane |
| JP5397772B2 (en) * | 2010-01-13 | 2014-01-22 | 独立行政法人物質・材料研究機構 | Polymer self-supporting membrane and separation membrane using the same |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112808034A (en) * | 2020-12-22 | 2021-05-18 | 浙江迪萧环保科技有限公司 | Preparation method of novel composite loose nanofiltration membrane |
| CN112808034B (en) * | 2020-12-22 | 2022-07-29 | 浙江迪萧科技有限公司 | Preparation method of composite loose nanofiltration membrane |
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