CN107051216A - A kind of method for preparing inner support reinforced type polyvinylidene fluoride hollow fiber film - Google Patents
A kind of method for preparing inner support reinforced type polyvinylidene fluoride hollow fiber film Download PDFInfo
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- CN107051216A CN107051216A CN201710163629.1A CN201710163629A CN107051216A CN 107051216 A CN107051216 A CN 107051216A CN 201710163629 A CN201710163629 A CN 201710163629A CN 107051216 A CN107051216 A CN 107051216A
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- Prior art keywords
- braided rope
- hollow
- polyvinylidene fluoride
- method described
- hollow braided
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Classifications
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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
-
- 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
-
- 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
- B01D71/30—Polyalkenyl halides
- B01D71/32—Polyalkenyl halides containing fluorine atoms
- B01D71/34—Polyvinylidene fluoride
Abstract
The invention discloses a kind of method for preparing inner support reinforced type polyvinylidene fluoride hollow fiber film, it is to be prepared using phase separation method, alkali decrement treatment first is carried out to polyester hollow braided rope, the hollow braided rope is immersed in high temperature Kynoar casting solution again, take out, the hollow braided rope for coating casting solution is passed through from the clasp with buttonhole, final set, washes, dry and be made.Using terylene alkali weight reduction accelerant coordinate naoh treatment polyester hollow braided rope, polyester fiber can be effectively facilitated multiphase hydrolysis occurs in treatment fluid, so that fiber surface produces the digging erosion phenomenon of uneven hole, so as to improve the adhesion on polyester hollow braided rope surface so that polyvinylidene fluoride layer is difficult to open from its sur-face peeling;Inner support reinforced type polyvinylidene fluoride hollow fiber film prepared by the present invention, the membrane flux is big, it is easy to accomplish industrialized production.
Description
Technical field
The invention belongs to hollow-fibre membrane field, more particularly to a kind of inner support reinforced type polyvinylidene fluoride hollow fiber
The preparation method of film.
Background technology
Hollow-fibre membrane as film a kind of form, it have compressive property it is good, without supporter, have in membrane module
The advantages of density is high, unit volume membrane area is big, flux is big is loaded, has been widely used in municipal wastewater processing, reclaimed water
In the field such as reuse and medication chemistry.However, the pollution of the flux and less film in order to maintain film, in engineering operation frequently with
The measure such as turbulent flow aeration interval water outlet and empty exposure so that hollow-fibre membrane is constantly swung during use, in this process
In, hollow-fibre membrane is easy to because intensity is not high and occurs to be broken and then influence the quality of water outlet.
In order to improve doughnut film strength, closely during the last ten years, many colleges and universities and scientific research institutions are all enhanced in development
The research of hollow-fibre membrane, this method is:Hollow braided rope is woven with high-speed knitter, the inclined fluorine of a strata is coated in its outer surface
Ethene casting solution, is solidified, and washing is post-processed and is made.This membrane flux is big, and intensity is high, not easily broken in MBR module
Silk.But for reinforced type polyvinylidene fluoride hollow fiber film on the market, the polyvinylidene fluoride layer of its filtration and increasing
The bonding force between layers of the hollow braided rope of strong intensity effect is poor, is easily peeled off and then influences to use.
Done a lot of work both at home and abroad between raising hollow braided rope and polyvinylidene fluoride layer in terms of adhesive property, such as
Hollow braided rope is woven into using superfine fibre;Applied in two coats casting solution, first applies weak solution, then apply highly concentrated solution;Thermic phase
Method prepares Kynoar film layer;Heat hollow braided rope;Corona treatment hollow braided rope improves the adhesive property of rope
Etc., theoretically analyze, these methods in enhancement type hollow fiber film between hollow braided rope and polyvinylidene fluoride layer to gluing
Connecing performance has certain improvement, but from the point of view of commercially available enhancement type hollow fiber film, its polyvinylidene fluoride layer is still easily from hollow
Peeled away on kernmantle.
The content of the invention
, should it is an object of the invention to provide a kind of preparation method of inner support reinforced type polyvinylidene fluoride hollow fiber film
Method is simple, it is easy to accomplish industrialized production, the inner support reinforced type polyvinylidene fluoride hollow fiber film of preparation, its polyvinylidene fluoride
Alkene cortex is difficult to peel away from hollow braided rope, and membrane flux is big.
A kind of method for preparing inner support reinforced type polyvinylidene fluoride hollow fiber film of the present invention, is caused using non-solvent
Prepared by phase separation method, alkali decrement treatment is first carried out to polyester hollow braided rope, then coat high temperature in the hollow braided rope outer surface
Polyvinylidene fluoride film liquid, solidification, washing, post processing and be made.
A kind of method for preparing inner support reinforced type polyvinylidene fluoride hollow fiber film, this method comprises the following steps:
1) at 70~100 DEG C, polyester is handled with sodium hydroxide and the mixed aqueous solution of terylene alkali weight reduction accelerant hollow
5~30min of kernmantle, take out washing, dry it is stand-by;
2) Kynoar casting solution is prepared:At 50~90 DEG C, by Kynoar, pore former, solvent according to quality
Than 12~25: 2~10: 65~86 mixing, stirring, dissolving, Kynoar casting solution is made in filtering after deaeration;
3) coagulation bath is prepared:Solvent and water are configured to coagulation bath according to mass percent 0~45: 55~100;
4) by step 1) hollow braided rope for preparing be immersed in 100~130 DEG C through step 2) prepare it is poly-
2~15min in vinylidene casting solution, takes out, and the hollow braided rope for coating casting solution is passed through from the clasp with buttonhole, directly
Connect and be placed on step 3) made from solidification forming in coagulation bath, the inner support washed, dried and the present invention is made is enhanced poly-
Vinylidene hollow-fibre membrane.
The step 1) the aqueous solution in sodium hydroxide mass percent be 10~30%;
The step 1) the aqueous solution in terylene alkali weight reduction accelerant be non-ionic base reduction promoter or cationic
Base reduction promoter;
The step 1) the aqueous solution in terylene alkali weight reduction accelerant mass percent be 1~5%;
The internal diameter of the polyester hollow braided rope is 0.5~2.2mm, and external diameter is 1.2~3.2mm;
The step 2) in Kynoar weight average molecular weight be 40~700,000;
The step 2) in pore former be polyvinylpyrrolidone, polyethylene glycol in one or two kinds of mixture,
Polyvinylpyrrolidone model is selected from K12, K17, K25, K30, K60, K90, and molecular weight polyethylene glycol is 200-20000;
The step 2) or step 3) in solvent be dimethylformamide, dimethyl acetamide, dimethyl sulfoxide (DMSO), N- methyl
The mixture of one or both of pyrrolidones;
The step 3) in buttonhole a diameter of 1.3~3.5mm;
The step 3) in solidification forming temperature be 20~80 DEG C, the time be 2~20min.
The present invention compared with prior art, with following advantage:
1) using terylene alkali weight reduction accelerant coordinate naoh treatment polyester hollow braided rope, can effectively promote
Enter polyester fiber and multiphase hydrolysis occurs in treatment fluid, its hydrolysis is opened from amorphous area surface macromolecular end of the chain ester bond
Begin, be since fiber surface, gradually to develop to nexine so that fiber surface produces the digging erosion phenomenon of uneven hole,
So as to improve the adhesion on polyester hollow braided rope surface so that polyvinylidene fluoride layer is difficult to open from its sur-face peeling;
2) present invention is by the hollow of normal temperature state during hollow braided rope is coated with Kynoar casting solution
Kernmantle is immersed in 100~130 DEG C of polyvinylidene fluoride film liquid, using both hollow braided rope and polyvinylidene fluoride film liquid it
Between the temperature difference it is big so that the adhesive property between Kynoar film layer and hollow braided rope is more preferable;
3) hollow braided rope for being coated with polyvinylidene fluoride film liquid is scraped using the clasp with buttonhole, may be such that poly- inclined
PVF film liquid is uniformly coated on hollow braided rope, and the thickness of easily controllable Kynoar film layer;
4) a kind of method for preparing inner support reinforced type polyvinylidene fluoride hollow fiber film of the invention, its Kynoar
Cortex is difficult to peel away from hollow braided rope, and the membrane flux is big, it is easy to accomplish industrialized production.
Embodiment
Embodiment 1
1) 60g sodium hydroxides, 2g cationic base reduction promoter FN and 138g water is weighed respectively to be positioned in beaker, will
They are mixed, dissolving;20cm polyester hollow braided rope (internal diameter is 0.5mm, and external diameter is 1.2mm) is intercepted, is placed it in
State processing 5min in the aqueous solution (temperature be 100 DEG C) of beaker, take out washing, dry it is stand-by;
2) at 90 DEG C, by 25g Kynoar (molecular weight is 400,000), 10g polyvinylpyrrolidones (K30) and 65g bis-
It is 25% Kynoar casting solution that mass concentration is made after NMF mixing, dissolving, filtering, deaeration;
3) by step 1) hollow braided rope for preparing be immersed in 130 DEG C through step 2) polyvinylidene fluoride for preparing
2min in alkene casting solution, is taken out, and the hollow braided rope for coating casting solution is worn from the clasp with buttonhole (a diameter of 1.3mm)
Cross, 20min is solidified in the water for being directly placed at 20 DEG C, wash, dry and be made the inner support enhancement type polyvinylidene fluorine second of the present invention
Alkene hollow-fibre membrane.The water flux of the hollow-fibre membrane is 633L/m2H, and the film is under dry state or hygrometric state, Kynoar
Cortex can not all be peeled away from hollow braided rope.
Embodiment 2
1) weigh 20g sodium hydroxides, 10g base reduction promoter TF-106 and 170g water respectively to be positioned in beaker, by it
Mix, dissolve;20cm polyester hollow braided rope (internal diameter is 2.2mm, and external diameter is 3.2mm) is intercepted, is placed it in above-mentioned
Processing 30min in the aqueous solution (temperature be 70 DEG C) of beaker, take out washing, dry it is stand-by;
2) at 80 DEG C, by 20g Kynoar (molecular weight is 600,000), 7g polyethylene glycol (molecular weight 1000) and 73g bis-
It is 20% Kynoar casting solution that mass concentration is made after methylacetamide mixing, dissolving, filtering, deaeration;
3) coagulation bath is prepared:30g dimethyl acetamides and 270g water are well mixed and are positioned in culture dish as solidifying
Gu body lotion;
4) by step 1) hollow braided rope for preparing be immersed in 120 DEG C through step 2) polyvinylidene fluoride for preparing
5min in alkene casting solution, is taken out, and the hollow braided rope for coating casting solution is worn from the clasp with buttonhole (a diameter of 3.5mm)
Cross, be directly placed at 80 DEG C through step 3) solidify 2min in the coagulation bath for preparing, wash, dry and the present invention is made
Inner support reinforced type polyvinylidene fluoride hollow fiber film.The water flux of the hollow-fibre membrane is 776L/m2H, and the film exists
Under dry state or hygrometric state, Kynoar cortex can not all be peeled away from hollow braided rope.
Embodiment 3
1) the non-ionic base reduction promoter of 40g sodium hydroxides, 5g is weighed respectively and 155g water is positioned in beaker, by it
Mix, dissolve;20cm polyester hollow braided rope (internal diameter is 1.8mm, and external diameter is 3.0mm) is intercepted, is placed it in above-mentioned
Processing 10min in the aqueous solution (temperature be 90 DEG C) of beaker, take out washing, dry it is stand-by;
2) at 50 DEG C, by 12g Kynoar (molecular weight is 700,000), 1g polyethylene glycol (molecular weight 600), 1g polyethylene
It is 12% poly- inclined that mass concentration is made after pyrrolidones (K90) and the mixing of 87g 1-METHYLPYRROLIDONEs, dissolving, filtering, deaeration
PVF casting solution;
3) coagulation bath is prepared:Well mixed be positioned in culture dish of 135g 1-METHYLPYRROLIDONEs and 165g water is made
For coagulation bath;
4) by step 1) hollow braided rope for preparing be immersed in 100 DEG C through step 2) polyvinylidene fluoride for preparing
15min in alkene casting solution, is taken out, and the hollow braided rope for coating casting solution is worn from the clasp with buttonhole (a diameter of 3.2mm)
Cross, be directly placed at 45 DEG C through step 3) solidify 10min in the coagulation bath for preparing, wash, dry and this hair is made
Bright inner support reinforced type polyvinylidene fluoride hollow fiber film.The water flux of the hollow-fibre membrane is 957L/m2H, and the film
Under dry state or hygrometric state, Kynoar cortex can not all be peeled away from hollow braided rope.
Embodiment 4
1) the non-ionic base reduction promoter of 30g sodium hydroxides, 8g is weighed respectively and 162g water is positioned in beaker, by it
Mix, dissolve;20cm polyester hollow braided rope (internal diameter is 1.5mm, and external diameter is 2.5mm) is intercepted, is placed it in above-mentioned
Processing 15min in the aqueous solution (temperature be 80 DEG C) of beaker, take out washing, dry it is stand-by;
2) at 80 DEG C, by 16g Kynoar (molecular weight is 600,000), 5g polyethylene glycol (molecular weight 2000), 39g diformazans
Mass concentration is made after base formamide and the mixing of 40g dimethyl acetamides, dissolving, filtering, deaeration to cast for 16% Kynoar
Film liquid;
3) coagulation bath is prepared:90g dimethylformamides and 210g water are well mixed and are positioned in culture dish as solidifying
Gu body lotion;
4) by step 1) hollow braided rope for preparing be immersed in 110 DEG C through step 2) polyvinylidene fluoride for preparing
10min in alkene casting solution, is taken out, and the hollow braided rope for coating casting solution is worn from the clasp with buttonhole (a diameter of 2.7mm)
Cross, be directly placed at 60 DEG C through step 3) solidify 5min in the coagulation bath for preparing, wash, dry and the present invention is made
Inner support reinforced type polyvinylidene fluoride hollow fiber film.The water flux of the hollow-fibre membrane is 812L/m2H, and the film exists
Under dry state or hygrometric state, Kynoar cortex can not all be peeled away from hollow braided rope.
Claims (10)
1. a kind of method for preparing inner support reinforced type polyvinylidene fluoride hollow fiber film, it is characterised in that this method include with
Lower step:
1) at 70~100 DEG C, with the aqueous solution of sodium hydroxide, terylene alkali weight reduction accelerant handle polyester hollow braided rope 5~
30min, take out washing, dry it is stand-by;
2) Kynoar casting solution is prepared:At 50~90 DEG C, by Kynoar, pore former, solvent according to mass ratio 12
Kynoar casting solution is made in~25: 2~10: 65~86 mixing, stirring, dissolving, filtering after deaeration;
3) coagulation bath is prepared:Solvent and water are configured to coagulation bath according to mass percent 0~45: 55~100;
4) by step 1) hollow braided rope for preparing be immersed in 100~130 DEG C through step 2) the poly- inclined fluorine for preparing
2~15min in ethene casting solution, is taken out, and the hollow braided rope for coating casting solution is passed through from the clasp with buttonhole, directly put
Put in step 3) made from solidification forming in coagulation bath, wash, dry and be made the inner support enhancement type polyvinylidene fluorine of the present invention
Ethene hollow-fibre membrane.
2. terylene alkali weight reduction accelerant in the aqueous solution according to the method described in claim 1, it is characterised in that the step 1)
For non-ionic base reduction promoter or cationic base reduction promoter.
3. the quality hundred of sodium hydroxide in the aqueous solution according to the method described in claim 1, it is characterised in that the step 1)
Divide than being 10~30%.
4. terylene alkali weight reduction accelerant in the aqueous solution according to the method described in claim 1, it is characterised in that the step 1)
Mass percent be 1~5%.
5. according to the method described in claim 1, it is characterised in that the internal diameter of the hollow braided rope is 0.5~2.2mm, outside
Footpath is 1.2~3.2mm.
6. the weight average molecular weight of Kynoar is according to the method described in claim 1, it is characterised in that the step 2)
40~700,000.
7. according to the method described in claim 1, it is characterised in that the step 2) pore former be polyvinylpyrrolidone,
The mixture of one or two kinds of in polyethylene glycol, polyvinylpyrrolidone model be selected from K12, K17, K25, K30, K60,
K90, molecular weight polyethylene glycol is 200-20000.
8. according to the method described in claim 1, it is characterised in that the step 2) or step 3) in solvent be dimethyl formyl
The mixture of one or both of amine, dimethyl acetamide, dimethyl sulfoxide (DMSO), 1-METHYLPYRROLIDONE.
9. a diameter of 1.3~3.5mm of buttonhole according to the method described in claim 1, it is characterised in that the step 3).
10. solidification forming temperature is 20~80 DEG C according to the method described in claim 1, it is characterised in that the step 3),
Time is 2~20min.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US10906006B2 (en) | 2017-10-12 | 2021-02-02 | Tianjin Polytechnic University | Homogeneous fiber reinforced PVDF hollow fiber membrane and preparation method thereof |
CN114053883A (en) * | 2021-09-10 | 2022-02-18 | 北京赛诺膜技术有限公司 | Polyvinylidene fluoride hollow fiber membrane and preparation method thereof |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US10906006B2 (en) | 2017-10-12 | 2021-02-02 | Tianjin Polytechnic University | Homogeneous fiber reinforced PVDF hollow fiber membrane and preparation method thereof |
CN114053883A (en) * | 2021-09-10 | 2022-02-18 | 北京赛诺膜技术有限公司 | Polyvinylidene fluoride hollow fiber membrane and preparation method thereof |
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