CN109092082A - A kind of high humility hollow fiber filter membrane silk casting method - Google Patents
A kind of high humility hollow fiber filter membrane silk casting method Download PDFInfo
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- CN109092082A CN109092082A CN201811171441.2A CN201811171441A CN109092082A CN 109092082 A CN109092082 A CN 109092082A CN 201811171441 A CN201811171441 A CN 201811171441A CN 109092082 A CN109092082 A CN 109092082A
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- filter membrane
- hollow fiber
- membrane silk
- high humility
- fiber filter
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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
- B01D69/08—Hollow fibre membranes
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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
- B01D67/0016—Coagulation
Abstract
The invention proposes a kind of high humility hollow fiber filter membrane silk casting methods, step includes configuring casting solution using macromolecule material of preparing and diluent, using solvent and water configuration solidification core liquid, using cellulose acetate and cosolvent configuration solidification atmosphere liquid, filter membrane silk is sprayed using triple channel spinneret, filter membrane silk table face is handled using atomization atmosphere liquid, ultimately form high humility hollow fiber filter membrane silk, there is good surface property and mechanical performance using filter membrane silk prepared by casting method of the invention, can be improved hydrophily and filter capacity.
Description
Technical field
The present invention relates to technical field of membrane separation more particularly to a kind of high humility hollow fiber filter membrane silk casting methods.
Background technique
It is many a little wide that hollow fiber filter membrane silk loads that density is big, is not required to backing material, simple production process etc. together
General is applied to separation technology field, main to be spun using the wet spinning of inversion of phases, dry method in the preparation of hollow-fibre membrane
Silk, dry-wet spinning and the methods of melt spinning-stretching, melt spinning-sintering, melt spinning-dissolution.These preparation sides
The hollow-fibre membrane that method obtains has been able to satisfy the requirements of the fields to film-strength such as general chemical separation, enrichment, purification.But for
Some higher occasions of peeling strength, doughnut film strength can't be satisfactory.
In recent years, enhancement type hollow fiber film receives attention, is the appearance in woven tube such as inner support hollow-fibre membrane
Face coats casting solution again through coagulation forming, which has single skin structure, can be used as external-compression type film or drawing-in type film uses, application
It is largely hollow fiber ultrafiltration membrane in the film of sewage treatment, because its film wire is very thin, the filling area in unit volume is big, water
Flux is big, at low cost, thus is widely used, but hollow fiber ultrafiltration membrane needs constantly to carry out clearly in use
It washes, cleaning easily leads to fracture of wire, and the appearance of fracture of wire can then be such that entire filtration system collapses.
Also because of the problem, the further genralrlization application of ultrafiltration membrane receives obstruction, therefore how to increase breaking for film wire
Power is urgent problem in current industry.
Summary of the invention
In view of this, the invention proposes a kind of high humility hollow fiber filter membrane silk casting methods.
The technical scheme of the present invention is realized as follows: the present invention provides a kind of high humility hollow fiber filter membrane silks to pour
Method includes the following steps:
Step 1: configuration casting solution: macromolecule material of preparing being mixed with diluent, wherein macromolecule material of preparing
Mass percent is 25%~40%, and the mass percent of diluent is 60%~75%, under the conditions of temperature is 40~80 DEG C
It uniformly mixed in spinning kettle, melt, obtain casting solution after deaeration；
Step 2: configuration solidification core liquid, is configured to solidification core liquid for solvent and water in mass ratio 10-20: 80-90；
Step 3: the casting solution in step 1 is passed through in the intermediate duct of triple channel spinneret, it will be solidifying in step 2
Gu the road Nei that core liquid is passed through triple channel spinneret sprays；
Step 4: configuration atmosphere liquid, be in mass ratio (40-60) by cellulose acetate and cosolvent: (60-40) is configured to
Atmosphere liquid；
Step 5: woven tube, casting solution, solidification core liquid are squeezed out through spinneret simultaneously, by certain length after extrusion
Air gap squeezes out spinneret and enters after being atomized atmosphere liquid using atmosphere liquid made from atomising device atomization steps four in air gap
Solidified in solidification liquid, then wound through washing, post-processing and wire drawing wheel, obtains high humility hollow fiber filter membrane silk.
On the basis of above technical scheme, it is preferred that the woven tube be by the fiber of 50-200dtex through twirl stock,
Machine compiles the woven tube to be formed.
On the basis of above technical scheme, it is preferred that the fiber be polyester fiber, Fypro, glass fibre,
One of polyethylene fibre or polypropylene fibre.
On the basis of above technical scheme, it is preferred that in step 1, the macromolecule material of preparing is polytetrafluoroethyl-ne
One of alkene, Kynoar, polypropylene, polyethylene, polyimides or polysulfones.
Still more preferably, in step 1, the diluent is one of dimethylformamide, dimethyl acetamide
Or two kinds of mixture.
On the basis of above technical scheme, it is preferred that in step 2, the solvent is dimethyl sulfoxide, N- methyl pyrrole
The mixture of one or both of pyrrolidone.
On the basis of above technical scheme, it is preferred that in step 4, the cosolvent is gaultherolin, salicylic acid
At least one of ethyl ester, methyl benzoate, ethyl benzoate, benzyl alcohol, dimethyphthalate.
On the basis of above technical scheme, it is preferred that in step 4, the temperature of the atmosphere liquid is 40~80 DEG C.
On the basis of above technical scheme, it is preferred that in step 5, the length of the air gap is 15~30cm.
On the basis of above technical scheme, it is preferred that in step 5, the temperature of atomization is 20~50 DEG C.
A kind of high humility hollow fiber filter membrane silk casting method of the invention has below compared with the existing technology beneficial to effect
Fruit:
The present invention provides a kind of casting methods of high humility hollow fiber filter membrane silk, by during pouring extrusion
The surface of film wire is handled using atomization atmosphere liquid, the intensity of film wire, and the surface parent of film wire not only can be enhanced
Outlet capacity is stronger, and the resistance to worry performance of film wire can also get a promotion, while using cellulose acetate as the material of atomization atmosphere, moreover it is possible to
One layer of very thin macromolecule membranous layer is formed on the surface of film wire, cellulose acetate has the ability of certain retention molecule, while can
To improve the strainability and mechanical performance of filter membrane silk.
Specific embodiment
Below in conjunction with embodiment of the present invention, the technical solution in embodiment of the present invention is carried out clearly and completely
Description, it is clear that described embodiment is only some embodiments of the invention, rather than whole embodiments.Base
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts all
Other embodiments shall fall within the protection scope of the present invention.
A kind of high humility hollow fiber filter membrane silk casting method of the present invention sequentially includes the following steps:
Embodiment 1
25g polytetrafluoroethylene (PTFE) is mixed with 75g dimethylformamide, is put into three-necked flask, 40 DEG C of water-bath stirrings are melted
Melt, melting finishes stopping stirring, keeps the temperature standing and defoaming；10g dimethyl sulfoxide and 90g water are uniformly mixed and obtain solidification core liquid；
40g cellulose acetate is mixed with 60g gaultherolin, 40 DEG C is heated to, obtains atmosphere liquid；The polyester fiber of 50dtex is led to
It crosses twirl stock and machine is compiled to form woven tube；Each led into inner duct, intermediate duct and the outer duct in triple channel spinneret or
Person pours woven tube, casting solution and solidification core liquid, squeezes out, and the film wire of extrusion passes through the air gap of 15cm, is full of mist in the air gap
The atmosphere liquid of change, the atmosphere liquid temperature of atomization are 20 DEG C, and film wire is again introduced into solidification core liquid after air gap, again pass by water
It washes, post-process and winding obtains high humility hollow fiber filter membrane silk.
Embodiment 2
30g polypropylene is mixed with 70g dimethyl acetamide, is put into three-necked flask, 50 DEG C of water-bath stirrings, melting,
Melting finishes stopping stirring, keeps the temperature standing and defoaming；13gN- methyl pyrrolidone and 87g water are uniformly mixed and obtain solidification core liquid；
50g cellulose acetate is mixed with 50g gaultherolin, 50 DEG C is heated to, obtains atmosphere liquid；The polyamide of 100dtex is fine
Dimension is compiled by twisting stock and machine and to form woven tube；Lead to respectively in inner duct, intermediate duct and the outer duct in triple channel spinneret
Enter or pour woven tube, casting solution and solidification core liquid, squeeze out, the film wire of extrusion passes through the air gap of 20cm, fills in the air gap
The atmosphere liquid being completely atomized, the atmosphere liquid temperature of atomization are 30 DEG C, and film wire is again introduced into solidification core liquid after air gap, are again passed by
Washing, post-processing and winding obtain high humility hollow fiber filter membrane silk.
Embodiment 3
35g polyimides, 35g dimethylformamide and 30g dimethyl acetamide are mixed, put into three-necked flask,
60 DEG C of water-bath stirrings, melting, melting finish stopping stirring, keep the temperature standing and defoaming；16g dimethyl sulfoxide and 84g water are mixed equal
It is even to obtain solidification core liquid；55g cellulose acetate is mixed with 45g gaultherolin, 60 DEG C is heated to, obtains atmosphere liquid；It will
The glass fibre of 150dtex is compiled by twisting stock and machine and to form woven tube；Inner duct in triple channel spinneret, intermediate duct and
Woven tube, casting solution and solidification core liquid are each led into or poured in outer duct, is squeezed out, and the film wire of extrusion passes through the gas of 25cm
Gap, the atmosphere liquid full of atomization in the air gap, the atmosphere liquid temperature of atomization are 40 DEG C, and film wire is again introduced into solidifying after air gap
Gu core liquid again passes by washing, post-processing and winding and obtains high humility hollow fiber filter membrane silk.
Embodiment 4
40g polysulfones is mixed with 60g dimethyl acetamide, is put into three-necked flask, 80 DEG C of water-bath stirrings, melting are melted
Melt and finish stopping stirring, keeps the temperature standing and defoaming；19g dimethyl sulfoxide and 81g water are uniformly mixed and obtain solidification core liquid；By 60g
Cellulose acetate is mixed with 40g gaultherolin, is heated to 80 DEG C, obtains atmosphere liquid；The polyethylene fibre of 200dtex is passed through
It twists stock and machine is compiled to form woven tube；Each led into inner duct, intermediate duct and the outer duct in triple channel spinneret or
Woven tube, casting solution and solidification core liquid are poured, is squeezed out, the film wire of extrusion passes through the air gap of 30cm, is full of atomization in the air gap
Atmosphere liquid, the atmosphere liquid temperature of atomization is 50 DEG C, and film wire is again introduced into solidification core liquid after air gap, again pass by washing,
Post-processing and winding obtain high humility hollow fiber filter membrane silk.
Comparative example 1
25g polytetrafluoroethylene (PTFE) is mixed with 75g dimethylformamide, is put into three-necked flask, 40 DEG C of water-bath stirrings are melted
Melt, melting finishes stopping stirring, keeps the temperature standing and defoaming；20g dimethyl sulfoxide and 80g water are uniformly mixed and obtain solidification core liquid；
The polyester fiber of 50dtex is compiled by twisting stock and machine and to form woven tube；Inner duct, intermediate duct in triple channel spinneret
With each lead into or pour woven tube, casting solution and solidification core liquid in outer duct, squeeze out, the film wire of extrusion passes through the gas of 15cm
Gap, film wire is again introduced into solidification core liquid after air gap, again passes by washing, post-processing and winding and obtains high humility doughnut
Filter membrane silk.
Comparative example 2
30g polypropylene is mixed with 70g dimethyl acetamide, is put into three-necked flask, 50 DEG C of water-bath stirrings, melting,
Melting finishes stopping stirring, keeps the temperature standing and defoaming；13gN- methyl pyrrolidone and 87g water are uniformly mixed and obtain solidification core liquid；
The Fypro of 100dtex is compiled by twisting stock and machine and to form woven tube；Inner duct, interstitial hole in triple channel spinneret
Woven tube, casting solution and solidification core liquid are each led into or poured in road and outer duct, is squeezed out, and the film wire of extrusion is by 20cm's
Air gap, film wire is again introduced into solidification core liquid after air gap, again passes by washing, post-processing and winding and obtains the hollow fibre of high humility
Tie up filter membrane silk.The performance test results:
The foregoing is merely better embodiments of the invention, are not intended to limit the invention, all of the invention
Within spirit and principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of high humility hollow fiber filter membrane silk casting method, which comprises the steps of:
Step 1: configuration casting solution: macromolecule material of preparing being mixed with diluent, wherein the quality of macromolecule material of preparing
Percentage is 25%~40%, and the mass percent of diluent is 60%~75%, is being spun under the conditions of temperature is 40~80 DEG C
It is uniformly mixed in silk kettle, melts, obtains casting solution after deaeration；
Step 2: configuration solidification core liquid, is configured to solidification core liquid for solvent and water in mass ratio 10-20: 80-90；
Step 3: the casting solution in step 1 is passed through in the intermediate duct of triple channel spinneret, by the solidification core in step 2
The road Nei that liquid is passed through triple channel spinneret sprays；
Step 4: configuration atmosphere liquid, be in mass ratio (40-60) by cellulose acetate and cosolvent: (60-40) is configured to atmosphere
Liquid；
Step 5: woven tube, casting solution, solidification core liquid are squeezed out through spinneret simultaneously, by the air gap of certain length after extrusion,
Using atmosphere liquid made from atomising device atomization steps four in air gap, squeezes out spinneret and enter solidification liquid after being atomized atmosphere liquid
In solidified, then through washing, post-processing and wire drawing wheel wind, obtain high humility hollow fiber filter membrane silk.
2. a kind of high humility hollow fiber filter membrane silk casting method as described in claim 1, which is characterized in that the woven tube
It is that the fiber of 50-200dtex is compiled into the woven tube to be formed by twirl stock, machine.
3. a kind of high humility hollow fiber filter membrane silk casting method as claimed in claim 2, which is characterized in that the fiber is
One of polyester fiber, Fypro, glass fibre, polyethylene fibre or polypropylene fibre.
4. a kind of high humility hollow fiber filter membrane silk casting method as described in claim 1, which is characterized in that in step 1,
The macromolecule material of preparing is one in polytetrafluoroethylene (PTFE), Kynoar, polypropylene, polyethylene, polyimides or polysulfones
Kind.
5. a kind of high humility hollow fiber filter membrane silk casting method as described in claim 1, which is characterized in that in step 1,
The diluent is the mixture of one or both of dimethylformamide, dimethyl acetamide.
6. a kind of high humility hollow fiber filter membrane silk casting method as described in claim 1, which is characterized in that in step 2,
The solvent is the mixture of one or both of dimethyl sulfoxide, N-Methyl pyrrolidone.
7. a kind of high humility hollow fiber filter membrane silk casting method as described in claim 1, which is characterized in that in step 4,
The cosolvent is gaultherolin, salethyl, methyl benzoate, ethyl benzoate, benzyl alcohol, neck phthalic acid diformazan
At least one of ester.
8. a kind of high humility hollow fiber filter membrane silk casting method as described in claim 1, which is characterized in that in step 4,
The temperature of the atmosphere liquid is 40~80 DEG C.
9. a kind of high humility hollow fiber filter membrane silk casting method as described in claim 1, which is characterized in that in step 5,
The length of the air gap is 15~30cm.
10. a kind of high humility hollow fiber filter membrane silk casting method as described in claim 1, which is characterized in that in step 5,
The temperature of atomization is 20~50 DEG C.
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| CN201811171441.2A CN109092082B (en) | 2018-10-08 | 2018-10-08 | High-humidity hollow fiber filter membrane silk pouring method |
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| CN201811171441.2A CN109092082B (en) | 2018-10-08 | 2018-10-08 | High-humidity hollow fiber filter membrane silk pouring method |
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| CN109092082A true CN109092082A (en) | 2018-12-28 |
| CN109092082B CN109092082B (en) | 2020-06-12 |
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| JPS594164B2 (en) * | 1975-12-30 | 1984-01-28 | 旭化成株式会社 | Macro Kagatachi Yukusen Inoseizouhouhou |
| CN101988217A (en) * | 2009-08-04 | 2011-03-23 | 上海太平洋纺织机械成套设备有限公司 | Vertical atomized chemical fiber molding method |
| CN102068918A (en) * | 2010-12-09 | 2011-05-25 | 苏州汇龙膜技术发展有限公司 | Hydrophilic polyethylene hollow fiber membrane and preparation method thereof |
| CN102205208A (en) * | 2011-04-20 | 2011-10-05 | 天津工业大学 | Device for preparing fiber-reinforced hollow fiber film |
| CN103285743A (en) * | 2013-06-28 | 2013-09-11 | 厦门建霖工业有限公司 | Hydrophilization modification method for polyvinyl chloride alloy ultrafiltration membrane |
| CN103949166A (en) * | 2014-04-30 | 2014-07-30 | 刘必前 | Internal pressure type fiber-reinforced filter membrane and preparation method thereof |
-
2018
- 2018-10-08 CN CN201811171441.2A patent/CN109092082B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS594164B2 (en) * | 1975-12-30 | 1984-01-28 | 旭化成株式会社 | Macro Kagatachi Yukusen Inoseizouhouhou |
| CN101988217A (en) * | 2009-08-04 | 2011-03-23 | 上海太平洋纺织机械成套设备有限公司 | Vertical atomized chemical fiber molding method |
| CN102068918A (en) * | 2010-12-09 | 2011-05-25 | 苏州汇龙膜技术发展有限公司 | Hydrophilic polyethylene hollow fiber membrane and preparation method thereof |
| CN102205208A (en) * | 2011-04-20 | 2011-10-05 | 天津工业大学 | Device for preparing fiber-reinforced hollow fiber film |
| CN103285743A (en) * | 2013-06-28 | 2013-09-11 | 厦门建霖工业有限公司 | Hydrophilization modification method for polyvinyl chloride alloy ultrafiltration membrane |
| CN103949166A (en) * | 2014-04-30 | 2014-07-30 | 刘必前 | Internal pressure type fiber-reinforced filter membrane and preparation method thereof |
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| CN109092082B (en) | 2020-06-12 |
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