CN106693720B - A kind of film-forming method improving liner microfiltration membranes surface flatness - Google Patents
A kind of film-forming method improving liner microfiltration membranes surface flatness Download PDFInfo
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- CN106693720B CN106693720B CN201611258789.6A CN201611258789A CN106693720B CN 106693720 B CN106693720 B CN 106693720B CN 201611258789 A CN201611258789 A CN 201611258789A CN 106693720 B CN106693720 B CN 106693720B
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- casting solution
- supporter
- film
- wire
- spinneret
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Classifications
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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
- B01D69/105—Support pretreatment
-
- 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
- B01D61/147—Microfiltration
-
- 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
- B01D69/02—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor characterised by their properties
-
- 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
- B01D69/08—Hollow fibre membranes
- B01D69/087—Details relating to the spinning process
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
- C02F1/444—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by ultrafiltration or microfiltration
Abstract
The present invention relates to a kind of film-forming method for improving liner microfiltration membranes surface flatness, specifically: resin, solvent, additive are put into stirred tank stirring and dissolving according to a certain percentage and form casting solution；Make to enter spinneret through spinning kettle, filter after the casting solution deaeration to be formed；Make supporter after atomising device is atomized enter spinneret and in die orifice exit with the casting solution in conjunction with so that casting solution be uniformly coated on supporting body surface formation film wire；So that film wire is tentatively formed after coagulation bath, after further the DMAC in casting solution is precipitated in aqueous solution by other gel slots, and water diffuses in fenestra, is finally formed in finished product film wire income receive silk machine by wrapping wire, post-processing.The present invention can reduce supporter cost by the atomization process to supporter while guaranteeing film surface smoothness, and preparation process is simple, controllable, increases an adjustable variable during casting solution is in conjunction with supporter, increases the wide in range property of product.
Description
Technical field
The present invention relates to a kind of film-forming methods for improving liner microfiltration membranes surface flatness, are widely used in water process
In field.
Background technique
Belt material microfiltration membranes refer to lining-reinforced hollow-fibre membrane, are to increase bundle-shaped support in traditional hollow
Body, to improve the intensity of film wire, tensile strength and compression strength are significantly larger than common hollow-fibre membrane, and pulling force is greater than
50KG, support body material are generally terylene material, and price is relatively inexpensive, at present the more braiding of water treatment field supporter
Form is high volume or crocheting method, belt material microfiltration membranes are equably to apply to spread separating layer in supporting body surface in simple terms, the two
In conjunction with needing to keep certain adhesive force, antistripping effect will be got well, and the film surface after smearing needs to reach certain smoothness,
It is theoretically more more smooth more uniform better, to improve the contamination resistance of film in operational process.
Existing liquid phase separation film method detailed process is resin, solvent, additive to be put into stir according to a certain percentage
Stirring and dissolving in kettle is mixed, enters coagulating bath split-phase, sizing through spinning kettle, filter, spinneret after casting solution deaeration, for belt material
Film, for supporter through spinneret and in die orifice exit in conjunction with casting solution, casting solution is uniformly coated on supporting body surface shape
At film wire, film wire is tentatively formed after coagulation bath, after by other gel slots further by the DMAC (dimethyl in casting solution
Acetamide) it is precipitated in aqueous solution, the principle of gel is the displacement of liquid liquid, and DMAC is diffused into water in feed liquid, and water diffuses to fenestra
In, finally pass through wrapping wire, post-treating and other steps, ultimately forms finished product film wire.
As market competition is more fierce, some enterprises for doing film can reduce film production cost, and with lining form it is main at
Originally it is supporter, when establishment density becomes smaller or mesh number reduces, the gap of supporting body surface be will increase, and casting solution was being smeared
Easily occur " bleed " (casting solution is flowed under incomplete gel state or infiltered in supporter) problem in journey, causes after molding
Film surface is rough, uneven, and needs to carry out formula some adjustment after there is this situation, but effect is often unobvious,
And while being formulated change, film properties will appear variation, be difficult to weigh.To reach same film surface smoothness, need
Using the higher supporter of mesh number or thicker separating layer is smeared, two methods will increase production cost, and supporter is worked out
After density is less than to a certain degree, the smooth effect of film surface is unable to reach by increasing smearing thickness.
Summary of the invention
In order to overcome drawbacks described above present in existing film-forming method, the invention proposes a kind of raising liner micro-filtration film surfaces
The method of smoothness, this method are to be optimized by spinning technique, on the basis of not feed change, formula in supporter
Atomization process, appropriate quickening casting solution and the feed liquid gelation rate for supporting contact level are carried out to supporter before smearing casting solution,
Bleed is avoided the occurrence of, to achieve the purpose that the smoothness of film surface after raising molding.Particular technique side of the invention
Case is as follows:
A kind of film-forming method improving liner microfiltration membranes surface flatness, this method comprises the following steps:
(1) resin, solvent, additive are put into stirring and dissolving in stirred tank according to a certain percentage and form casting solution；
(2) make to enter spinneret through spinning kettle, filter after the casting solution deaeration to be formed；
(3) make supporter through spinneret and in die orifice exit in conjunction with the casting solution so that casting solution equably applies
It overlays on supporting body surface and forms film wire；
(4) so that film wire is tentatively formed after coagulation bath, after by other gel slots further by the DMAC in casting solution
It is precipitated in aqueous solution, and water diffuses in fenestra, finally forms finished product film wire by wrapping wire, post-processing；
It is characterized by:
This method further includes the steps that carrying out atomization process to supporter before supporter enters spinneret.
Atomising device needed for above-mentioned atomization process is a sleeve, and sleeve is equipped with multiple atomizers, can pass through tune
Seamless power and/or replacement different model atomizer change water flow, reach different degrees of atomizing effect, general same rule
The atomizer of lattice, pressure more high flow capacity is bigger, and the effect of atomization is stronger, in addition can be opened or closed according to atomizing effect individually
Atomizer.According to the difference of fogging degree, casting solution can reach different degrees of gel effect after contacting with supporter, generally
For, when select cost is relatively low, mesh number lower supporter when, need to atomization process degree to supporter it is deeper, principle is
Solvent is exchanged with the mass transfer of non-solvent in homogeneous polymer solution ambient enviroment, and phase point occurs from homogeneous polymer solution
From, it is transformed into the gel structure of a three-dimensional macromolecular network type, final film-forming, and to the atomization process of supporter, it can
Change split-phase speed and film formation time, control the combination speed of casting solution and supporter, reach not only smooth but also there is certain bonding
The purpose of power, the film surface after fundamentally solving the problems, such as film forming is uneven, reaches certain smoothness.
Feature of the present invention is due to being provided with the step of carrying out atomization process to supporter, so can be by reducing supporter
Mesh number or casting solution smearing thickness achieve the purpose that reduce cost, while can keep the smoothness of film surface again, and atomization process
Controllably, it can arbitrarily be adjusted according to the characteristics of supporter and formula, cost is relatively low for atomization process, need to only increase the mist machine and corresponding made
Atomizer, water consumption are less.
Detailed description of the invention
In order to be easier to understand technical solution of the present invention and beneficial technical effect, by referring to what is be shown in the accompanying drawings
A specific embodiment of the invention is described in detail the present invention.These attached drawings depict only typical implementation of the invention
Mode does not constitute the limitation to protection scope of the present invention, in which:
Fig. 1 is the stream of the film-forming method of raising liner microfiltration membranes surface flatness according to embodiment of the present invention
Cheng Tu.
Fig. 2 is used in the film-forming method of the raising liner microfiltration membranes surface flatness of above embodiment according to the present invention
Atomising device perspective view.
Fig. 3-6 be respectively atomization quantity be 12cc/min, 20cc/min, 35cc/min and 47cc/min when bleed degree it is micro-
Photo.
In the appended drawing reference indicated in Fig. 1-2:
1: stirred tank；2: spinning kettle；3: nitrogen gas tank；4: supporter；5: atomising device；6: spinneret；7: coagulating bath；8: receiving
Silk machine；9: sleeve；10: atomizer.
Specific embodiment
Referring to Fig.1, the film of a kind of raising liner microfiltration membranes surface flatness according to embodiment of the present invention
Method is specially that resin, solvent, additive are put into stirring and dissolving in stirred tank 1 according to a certain percentage to form casting solution；Make shape
At casting solution deaeration after through spinning kettle 2, filter enter spinneret 6.Selectively, spinning kettle 2 is connected with nitrogen gas tank 3, past
Nitrogen is passed through in spinning kettle 2 for pushing casting solution spinning, nitrogen is advantageous in that stabilization, and casting solution is not easy to be oxidized.Support
Body 4 through atomising device 5 atomization after enter spinneret 6 and in 6 exit of spinneret in conjunction with the casting solution so that casting solution is equal
It is coated in 4 surface of supporter evenly and forms film wire；Film wire is tentatively formed after coagulation bath 7, after by other gel slots into one
DMAC in casting solution is precipitated in aqueous solution step, and water diffuses in fenestra, finally forms finished product by wrapping wire, post-processing
Film wire is taken in receive silk machine 8.
Atomising device 5 needed for above-mentioned atomization process is a sleeve 9, and sleeve is equipped with atomizer 10.In the implementation
In mode, the internal diameter of sleeve 9 is 90mm, outer diameter 100mm, and two groups of atomizers, every group of atomizer number are equipped on sleeve 9
Amount is four, and four nozzles 10 in every group of atomizer are uniformly distributed along the circumferencial direction of sleeve, two groups of atomizers it
Between distance be 120mm, be that 40mm (can calculate the length of sleeve at a distance from every group of atomizer sleeve ends nearest with its
Degree is 200mm).By adjusting pressure and the atomizer 10 of different model can be replaced change water flow, reach different degrees of
Atomizing effect, general same specification atomizer 10, pressure more high flow capacity is bigger, and the effect of atomization is stronger, in addition can root
Individual atomizers 10 are opened or closed according to atomizing effect.According to the difference of fogging degree, casting solution can after contacting with supporter 4
Reach different degrees of gel effect, in general, when select cost is relatively low, mesh number lower supporter 4 when, need to be to supporter
4 atomization process degree is deeper, and principle is that solvent is exchanged with the mass transfer of non-solvent in homogeneous polymer solution ambient enviroment, from
Occur mutually to separate in homogeneous polymer solution, is transformed into the gel structure of a three-dimensional macromolecular network type, is finally solidified into
Film, and to the atomization process of supporter 4, split-phase speed and film formation time can be changed, control the combination speed of casting solution and supporter 4
Degree achievees the purpose that not only smooth but also has certain cohesive force, and the film surface after fundamentally solving the problems, such as film forming is uneven, reaches
To certain smoothness.
The diameter of general supporter 4 is 1.5-2.0mm, and is according to the volume that above-mentioned size can calculate sleeve 9
1271.7cm3If the residence time in sleeve 9 of supporter 4 is 1 second, for the atomization process of supporter 4, atomizer
10 sizes should be at 100-150 μm, and atomization quantity is adjustable in 10-50cc/min, thus realize different atomization process effects, it is appropriate to add
The feed liquid gelation rate of fast casting solution and 4 contact surface of supporter, avoids the occurrence of bleed, to improve film surface after molding
Smoothness.Bleed degree that Fig. 3-6 is respectively atomization quantity when being 12cc/min, 20cc/min, 35cc/min and 47cc/min is aobvious
Micro- photo.From, it can be seen that film surface smoothness effects are related to bleed degree, bleed is more serious, and film surface is more not in Fig. 3-6
Smooth, as shown in figure 3, bleed is lighter, film surface is more flat and smooth, no concave-convex injustice phenomenon, as shown in Figure 6.
Certainly, those skilled in the art can according to actual needs the size to sleeve 9 and the number of atomizer 10 and
Distribution is adjusted, naturally it is also possible to the size of atomizer 10 and the numerical value of atomization quantity is adjusted according to atomizing effect, this is simultaneously
It is not detached from protection scope of the present invention.
The present invention by the atomization process to supporter, can be reduced while guaranteeing film surface smoothness supporter at
This, preparation process is simple, controllable, increases an adjustable variable during casting solution is in conjunction with supporter, increases
The wide in range property of product.
The present invention can embody in the form of other are specific, but this is without departing from protection scope of the present invention, originally
The protection scope of invention is defined only by the following claims.
Claims (1)
1. a kind of film-forming method for improving liner microfiltration membranes surface flatness, this method comprises the following steps:
(1) resin, solvent, additive are put into stirring and dissolving in stirred tank according to a certain percentage and form casting solution；
(2) make to enter spinneret through spinning kettle, filter after the casting solution deaeration to be formed；
(3) make supporter through spinneret and in die orifice exit in conjunction with the casting solution so that casting solution is uniformly coated on
Supporting body surface forms film wire；
(4) so that film wire is tentatively formed after coagulation bath, after by other gel slots further by casting solution DMAC be precipitated
In aqueous solution, and water diffuses in fenestra, finally by wrapping wire, post-processing form finished product film wire；
It is characterized by:
This method further includes the steps that carrying out atomization process, the atomization process institute to supporter before supporter enters spinneret
Atomising device is a sleeve, and multiple atomizers are equipped on the sleeve；
This method further includes adjustment pressure and/or replacement different model atomizer to change water flow to reach different degrees of
The step of atomizing effect；
This method further includes the steps that opening or closing individual atomizers according to atomizing effect.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611258789.6A CN106693720B (en) | 2016-12-30 | 2016-12-30 | A kind of film-forming method improving liner microfiltration membranes surface flatness |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611258789.6A CN106693720B (en) | 2016-12-30 | 2016-12-30 | A kind of film-forming method improving liner microfiltration membranes surface flatness |
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| Publication Number | Publication Date |
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| CN106693720A CN106693720A (en) | 2017-05-24 |
| CN106693720B true CN106693720B (en) | 2019-10-18 |
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| CN109433018B (en) * | 2018-11-28 | 2021-03-23 | 常州大学 | Preparation method of ultrathin silicon-based alcohol-water separation membrane with thickness less than 50nm |
| CN114797484B (en) * | 2021-01-19 | 2023-02-28 | 中国石油化工股份有限公司 | Porous separation membrane with adsorption performance and preparation method and application thereof |
| CN115245758B (en) * | 2021-04-28 | 2023-07-21 | 中国石油化工股份有限公司 | Composite forward osmosis membrane and preparation method and application thereof |
| CN115245757B (en) * | 2021-04-28 | 2023-07-21 | 中国石油化工股份有限公司 | Composite nanofiltration membrane and preparation method and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103111194A (en) * | 2013-03-05 | 2013-05-22 | 天津工业大学 | Preparation method of homogeneous reinforced hollow fiber membrane |
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| KR960014337B1 (en) * | 1993-12-20 | 1996-10-15 | 제일합섬 주식회사 | Manufacturing method of composite membrane |
| CN102430346A (en) * | 2011-10-26 | 2012-05-02 | 天津市宝钜净化设备工程有限公司 | Preparation method of non-woven fabric or weaving cotton cloth supporting ultra-filtration/micro-filtration composite membrane |
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| CN103111194A (en) * | 2013-03-05 | 2013-05-22 | 天津工业大学 | Preparation method of homogeneous reinforced hollow fiber membrane |
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Address after: 301800 No.10, Fuli Road, plastic products industrial zone, Baodi District, Tianjin Patentee after: Oseco membrane technology (Tianjin) Co.,Ltd. Address before: 301800 No.10, Fuli Road, plastic products industrial zone, Baodi District, Tianjin Patentee before: TIANJIN BISHUIYUAN MEMBRANE MATERIAL Co.,Ltd. |
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