CN108837708A - The preparation method of polymerization degree polyvinyl chloride hollow fiber ultrafiltration membrane - Google Patents
The preparation method of polymerization degree polyvinyl chloride hollow fiber ultrafiltration membrane Download PDFInfo
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- CN108837708A CN108837708A CN201810684666.1A CN201810684666A CN108837708A CN 108837708 A CN108837708 A CN 108837708A CN 201810684666 A CN201810684666 A CN 201810684666A CN 108837708 A CN108837708 A CN 108837708A
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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
-
- 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
- B01D67/0011—Casting solutions therefor
-
- 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
- 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
-
- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2323/00—Details relating to membrane preparation
- B01D2323/46—Impregnation
Abstract
The invention discloses the preparation methods of polymerization degree polyvinyl chloride hollow fiber ultrafiltration membrane, the present invention passes through using the polyvinyl chloride of high polymerization degree as main body, by the way that organic solvent is added during the preparation process, pore former, additive, and by casting solution and the common extrusion molding of gel media, obtained ultrafiltration membrane has preferable intensity and mechanical property, increase tensile resistance, and the flux of ultrafiltration membrane is big, hydrophilic polymer in ultrafiltration membrane can be gathered in the surface of film in forming process, in actual use, hydrophilic layer can be formed with water molecules, it avoids pollution object and directly contacts film surface, prevent spot from blocking fenestra, to have better resistance tocrocking.
Description
Technical field
The present invention relates to ultrafiltration membranes to research and develop processing technique field, specifically polymerization degree polyvinyl chloride hollow fiber ultrafiltration membrane
Preparation method.
Background technique
Ultrafiltration membrane is that a kind of aperture specification is consistent, and nominal pore range is 0.01 micron of micropore filtering film below.In film
Side impose appropriate pressure, the solute molecule less than aperture can be sifted out, to separate molecular weight greater than 500 dalton (atoms
Mass unit）, partial size be greater than 10 nanometers of particle.Ultrafiltration membrane is one of the polymeric membrane for separation developed earliest, the sixties just
Realize the industrialized production of ultrafiltration apparatus.Current ultrafiltration membrane haves the shortcomings that poor mechanical property, flux are low.
Summary of the invention
The purpose of the present invention is to provide the preparation methods of polymerization degree polyvinyl chloride hollow fiber ultrafiltration membrane, on solving
State the problem of proposing in background technique.
To achieve the above object, the present invention provides the following technical solutions：
The preparation method of polymerization degree polyvinyl chloride hollow fiber ultrafiltration membrane, including following preparation step：
S1, by the dehydrated alcohol of the N- dimethyl acetamide of 20-30 parts by weight and 130-150 parts by weight after mixing, Xiang Rong
Be added in liquid the polyglycerol monostearate of 4-9 parts by weight, the polyacrylic acid solution of 8-12 parts by weight, 20-30 parts by weight it is poly-
Ether sulfone, the tetramethyl divinyl disiloxane of 15-20 parts by weight, 1-3 parts by weight graphene, be heated to 30-40 DEG C, ultrasound
The pore former of 5-7 parts by weight and the additive of 10-20 parts by weight is added after reaction 3-5 hours in stirring, is again stirring for obtaining
Phase solution；
S2, homogeneous phase solution is placed in 70-90 DEG C of vacuum oven, 10-12 hours dry, the casting solution after obtaining deaeration；
S3, by casting solution and gel media with 1：1 ratio is poured on spinneret, and casting solution and gel media pass through spinneret
Afterwards, the liquid film for obtaining tubulose is dipped in deionized water and solidifies after liquid film to be passed through to 0-30 centimetres of airspace, impregnates 12-
After 15 hours, the membrane after solidifying is taken out, is washed 5-7 times, is placed into baking oven, under the conditions of 60-80 DEG C using dehydrated alcohol
Drying.
As a further solution of the present invention：The pore former in step S1 is polyvinylpyrrolidone and polyethylene glycol
Mixed solution, the additive are titania powder reagent.
As a further solution of the present invention：The polyglycerol monostearate in step S1 is 4 parts by weight, polypropylene
Acid solution is 8 parts by weight, and polyether sulfone is 20 parts by weight, and tetramethyl divinyl disiloxane is 15 parts by weight, and graphene is 1 weight
Part is measured, pore former is 5 parts by weight, and additive is 10 parts by weight.
As a further solution of the present invention：Heating temperature in step S1 is set as 30 DEG C, and it is small that the reaction time is set as 3
When, the temperature setting in vacuum oven in step S2 is 70 DEG C, and drying time is set as 10 hours, the air in step S3
It is set to 0 centimetre, soaking time is set as 12 hours, and drying time is set as 60 DEG C.
As a further solution of the present invention：The polyglycerol monostearate in step S1 is 7 parts by weight, polypropylene
Acid solution is 10 parts by weight, and polyether sulfone is 25 parts by weight, and tetramethyl divinyl disiloxane is 17 parts by weight, graphene 2
Parts by weight, pore former are 6 parts by weight, and additive is 15 parts by weight.
As a further solution of the present invention：Heating temperature in step S1 is set as 35 DEG C, and it is small that the reaction time is set as 4
When, the temperature setting in vacuum oven in step S2 is 80 DEG C, and drying time is set as 11 hours, the air in step S3
15 centimetres are set to, soaking time is set as 14 hours, and drying time is set as 70 DEG C.
As a further solution of the present invention：The polyglycerol monostearate in step S1 is 9 parts by weight, polypropylene
Acid solution is 12 parts by weight, and polyether sulfone is 30 parts by weight, and tetramethyl divinyl disiloxane is 20 parts by weight, graphene 3
Parts by weight, pore former are 7 parts by weight, and additive is 20 parts by weight.
As a further solution of the present invention：Heating temperature in step S1 is set as 40 DEG C, and it is small that the reaction time is set as 5
When, the temperature setting in vacuum oven in step S2 is 90 DEG C, and drying time is set as 12 hours, the air in step S3
30 centimetres are set to, soaking time is set as 15 hours, and drying time is set as 80 DEG C.
Compared with prior art, the beneficial effects of the invention are as follows：The present invention by using the polyvinyl chloride of high polymerization degree as
Main body squeezes out jointly by the way that organic solvent, pore former, additive are added during the preparation process, and by casting solution and gel media
Molding, obtained ultrafiltration membrane have preferable intensity and mechanical property, increase tensile resistance, and the flux of ultrafiltration membrane is big,
Hydrophilic polymer in ultrafiltration membrane can be gathered in the surface of film in forming process, in actual use, can be with hydrone
It in conjunction with hydrophilic layer is formed, avoids pollution object and directly contacts film surface, prevent spot from blocking fenestra, to have better anti-pollution
Metachromia.
Specific embodiment
The following is a clear and complete description of the technical scheme in the embodiments of the invention, it is clear that described embodiment
Only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, the common skill in this field
Art personnel every other embodiment obtained without making creative work belongs to the model that the present invention protects
It encloses.
Embodiment 1
The preparation method of polymerization degree polyvinyl chloride hollow fiber ultrafiltration membrane, including following preparation step：
S1, by the dehydrated alcohol of the N- dimethyl acetamide of 20-30 parts by weight and 130-150 parts by weight after mixing, Xiang Rong
Be added in liquid the polyglycerol monostearate of 4-9 parts by weight, the polyacrylic acid solution of 8-12 parts by weight, 20-30 parts by weight it is poly-
Ether sulfone, the tetramethyl divinyl disiloxane of 15-20 parts by weight, 1-3 parts by weight graphene, be heated to 30-40 DEG C, ultrasound
The pore former of 5-7 parts by weight and the additive of 10-20 parts by weight is added after reaction 3-5 hours in stirring, is again stirring for obtaining
Phase solution；
S2, homogeneous phase solution is placed in 70-90 DEG C of vacuum oven, 10-12 hours dry, the casting solution after obtaining deaeration；
S3, by casting solution and gel media with 1：1 ratio is poured on spinneret, and casting solution and gel media pass through spinneret
Afterwards, the liquid film for obtaining tubulose is dipped in deionized water and solidifies after liquid film to be passed through to 0-30 centimetres of airspace, impregnates 12-
After 15 hours, the membrane after solidifying is taken out, is washed 5-7 times, is placed into baking oven, under the conditions of 60-80 DEG C using dehydrated alcohol
Drying.
The pore former in step S1 is polyvinylpyrrolidone and polyethylene glycol mixed solution, and the additive is two
Titanium dioxide powder reagent.
The polyglycerol monostearate in step S1 is 4 parts by weight, and polyacrylic acid solution is 8 parts by weight, polyether sulfone
For 20 parts by weight, tetramethyl divinyl disiloxane is 15 parts by weight, and graphene is 1 parts by weight, and pore former is 5 parts by weight,
Additive is 10 parts by weight.
Heating temperature in step S1 is set as 30 DEG C, and the reaction time is set as 3 hours, the vacuum oven in step S2
In temperature setting be 70 DEG C, drying time is set as 10 hours, and the airspace in step S3 is set as 0 centimetre, when immersion
Between be set as 12 hours, drying time is set as 60 DEG C.
Embodiment 2
The preparation method of polymerization degree polyvinyl chloride hollow fiber ultrafiltration membrane, including following preparation step：
S1, by the dehydrated alcohol of the N- dimethyl acetamide of 20-30 parts by weight and 130-150 parts by weight after mixing, Xiang Rong
Be added in liquid the polyglycerol monostearate of 4-9 parts by weight, the polyacrylic acid solution of 8-12 parts by weight, 20-30 parts by weight it is poly-
Ether sulfone, the tetramethyl divinyl disiloxane of 15-20 parts by weight, 1-3 parts by weight graphene, be heated to 30-40 DEG C, ultrasound
The pore former of 5-7 parts by weight and the additive of 10-20 parts by weight is added after reaction 3-5 hours in stirring, is again stirring for obtaining
Phase solution；
S2, homogeneous phase solution is placed in 70-90 DEG C of vacuum oven, 10-12 hours dry, the casting solution after obtaining deaeration；
S3, by casting solution and gel media with 1：1 ratio is poured on spinneret, and casting solution and gel media pass through spinneret
Afterwards, the liquid film for obtaining tubulose is dipped in deionized water and solidifies after liquid film to be passed through to 0-30 centimetres of airspace, impregnates 12-
After 15 hours, the membrane after solidifying is taken out, is washed 5-7 times, is placed into baking oven, under the conditions of 60-80 DEG C using dehydrated alcohol
Drying.
The pore former in step S1 is polyvinylpyrrolidone and polyethylene glycol mixed solution, and the additive is two
Titanium dioxide powder reagent.
The polyglycerol monostearate in step S1 is 7 parts by weight, and polyacrylic acid solution is 10 parts by weight, polyether sulfone
For 25 parts by weight, tetramethyl divinyl disiloxane is 17 parts by weight, and graphene is 2 parts by weight, and pore former is 6 parts by weight,
Additive is 15 parts by weight.
Heating temperature in step S1 is set as 35 DEG C, and the reaction time is set as 4 hours, the vacuum oven in step S2
In temperature setting be 80 DEG C, drying time is set as 11 hours, and the airspace in step S3 is set as 15 centimetres, when immersion
Between be set as 14 hours, drying time is set as 70 DEG C.
Embodiment 3
The preparation method of polymerization degree polyvinyl chloride hollow fiber ultrafiltration membrane, including following preparation step：
S1, by the dehydrated alcohol of the N- dimethyl acetamide of 20-30 parts by weight and 130-150 parts by weight after mixing, Xiang Rong
Be added in liquid the polyglycerol monostearate of 4-9 parts by weight, the polyacrylic acid solution of 8-12 parts by weight, 20-30 parts by weight it is poly-
Ether sulfone, the tetramethyl divinyl disiloxane of 15-20 parts by weight, 1-3 parts by weight graphene, be heated to 30-40 DEG C, ultrasound
The pore former of 5-7 parts by weight and the additive of 10-20 parts by weight is added after reaction 3-5 hours in stirring, is again stirring for obtaining
Phase solution；
S2, homogeneous phase solution is placed in 70-90 DEG C of vacuum oven, 10-12 hours dry, the casting solution after obtaining deaeration；
S3, by casting solution and gel media with 1：1 ratio is poured on spinneret, and casting solution and gel media pass through spinneret
Afterwards, the liquid film for obtaining tubulose is dipped in deionized water and solidifies after liquid film to be passed through to 0-30 centimetres of airspace, impregnates 12-
After 15 hours, the membrane after solidifying is taken out, is washed 5-7 times, is placed into baking oven, under the conditions of 60-80 DEG C using dehydrated alcohol
Drying.
The pore former in step S1 is polyvinylpyrrolidone and polyethylene glycol mixed solution, and the additive is two
Titanium dioxide powder reagent.
The polyglycerol monostearate in step S1 is 9 parts by weight, and polyacrylic acid solution is 12 parts by weight, polyether sulfone
For 30 parts by weight, tetramethyl divinyl disiloxane is 20 parts by weight, and graphene is 3 parts by weight, and pore former is 7 parts by weight,
Additive is 20 parts by weight.
Heating temperature in step S1 is set as 40 DEG C, and the reaction time is set as 5 hours, the vacuum oven in step S2
In temperature setting be 90 DEG C, drying time is set as 12 hours, and the airspace in step S3 is set as 30 centimetres, when immersion
Between be set as 15 hours, drying time is set as 80 DEG C.
It is obvious to a person skilled in the art that invention is not limited to the details of the above exemplary embodiments, Er Qie
In the case where without departing substantially from spirit or essential attributes of the invention, the present invention can be realized in other specific forms.Therefore, no matter
From the point of view of which point, the present embodiments are to be considered as illustrative and not restrictive, and the scope of the present invention is by appended power
Benefit requires rather than above description limits, it is intended that all by what is fallen within the meaning and scope of the equivalent elements of the claims
Variation is included within the present invention.
Claims (8)
1. the preparation method of polymerization degree polyvinyl chloride hollow fiber ultrafiltration membrane, which is characterized in that including following preparation step：
S1, by the dehydrated alcohol of the N- dimethyl acetamide of 20-30 parts by weight and 130-150 parts by weight after mixing, Xiang Rong
Be added in liquid the polyglycerol monostearate of 4-9 parts by weight, the polyacrylic acid solution of 8-12 parts by weight, 20-30 parts by weight it is poly-
Ether sulfone, the tetramethyl divinyl disiloxane of 15-20 parts by weight, 1-3 parts by weight graphene, be heated to 30-40 DEG C, ultrasound
The pore former of 5-7 parts by weight and the additive of 10-20 parts by weight is added after reaction 3-5 hours in stirring, is again stirring for obtaining
Phase solution；
S2, homogeneous phase solution is placed in 70-90 DEG C of vacuum oven, 10-12 hours dry, the casting solution after obtaining deaeration；
S3, by casting solution and gel media with 1：1 ratio is poured on spinneret, and casting solution and gel media pass through spinneret
Afterwards, the liquid film for obtaining tubulose is dipped in deionized water and solidifies after liquid film to be passed through to 0-30 centimetres of airspace, impregnates 12-
After 15 hours, the membrane after solidifying is taken out, is washed 5-7 times, is placed into baking oven, under the conditions of 60-80 DEG C using dehydrated alcohol
Drying.
2. the preparation method of polymerization degree polyvinyl chloride hollow fiber ultrafiltration membrane according to claim 1, which is characterized in that
The pore former in step S1 is polyvinylpyrrolidone and polyethylene glycol mixed solution, and the additive is titanium dioxide powder
Last reagent.
3. the preparation method of polymerization degree polyvinyl chloride hollow fiber ultrafiltration membrane according to claim 1, which is characterized in that
The polyglycerol monostearate in step S1 is 4 parts by weight, and polyacrylic acid solution is 8 parts by weight, and polyether sulfone is 20 weight
Part, tetramethyl divinyl disiloxane is 15 parts by weight, and graphene is 1 parts by weight, and pore former is 5 parts by weight, and additive is
10 parts by weight.
4. the preparation method of polymerization degree polyvinyl chloride hollow fiber ultrafiltration membrane according to claim 3, which is characterized in that
Heating temperature in step S1 is set as 30 DEG C, and the reaction time is set as 3 hours, the temperature in vacuum oven in step S2
70 DEG C are set as, drying time is set as 10 hours, and the airspace in step S3 is set as 0 centimetre, and soaking time is set as
12 hours, drying time was set as 60 DEG C.
5. the preparation method of polymerization degree polyvinyl chloride hollow fiber ultrafiltration membrane according to claim 1, which is characterized in that
The polyglycerol monostearate in step S1 is 7 parts by weight, and polyacrylic acid solution is 10 parts by weight, and polyether sulfone is 25 weight
Part, tetramethyl divinyl disiloxane is 17 parts by weight, and graphene is 2 parts by weight, and pore former is 6 parts by weight, and additive is
15 parts by weight.
6. the preparation method of polymerization degree polyvinyl chloride hollow fiber ultrafiltration membrane according to claim 5, which is characterized in that
Heating temperature in step S1 is set as 35 DEG C, and the reaction time is set as 4 hours, the temperature in vacuum oven in step S2
80 DEG C are set as, drying time is set as 11 hours, and the airspace in step S3 is set as 15 centimetres, and soaking time is set as
14 hours, drying time was set as 70 DEG C.
7. the preparation method of polymerization degree polyvinyl chloride hollow fiber ultrafiltration membrane according to claim 1, which is characterized in that
The polyglycerol monostearate in step S1 is 9 parts by weight, and polyacrylic acid solution is 12 parts by weight, and polyether sulfone is 30 weight
Part, tetramethyl divinyl disiloxane is 20 parts by weight, and graphene is 3 parts by weight, and pore former is 7 parts by weight, and additive is
20 parts by weight.
8. the preparation method of polymerization degree polyvinyl chloride hollow fiber ultrafiltration membrane according to claim 7, which is characterized in that
Heating temperature in step S1 is set as 40 DEG C, and the reaction time is set as 5 hours, the temperature in vacuum oven in step S2
90 DEG C are set as, drying time is set as 12 hours, and the airspace in step S3 is set as 30 centimetres, and soaking time is set as
15 hours, drying time was set as 80 DEG C.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101837250A (en) * | 2010-06-22 | 2010-09-22 | 苏州绿膜科技有限公司 | Modified polrvinyl chloride hollow fiber ultrafiltration membrane, preparation method and application thereof |
| CN101837249A (en) * | 2010-06-13 | 2010-09-22 | 苏州绿膜科技有限公司 | Composite polrvinyl chloride hollow fiber ultrafiltration membrane and preparation method thereof |
| CN102861519A (en) * | 2011-07-05 | 2013-01-09 | 北京金通量科技有限公司 | Preparation method of long-acting hydrophilic polyvinyl chloride hollow fiber ultrafiltration membrane |
| CN105709620A (en) * | 2016-04-28 | 2016-06-29 | 安阳华森纸业有限责任公司 | Preparation method of hollow fiber oxygen permeable membrane |
| CN107096402A (en) * | 2016-02-19 | 2017-08-29 | 中国科学院苏州纳米技术与纳米仿生研究所 | Oil resistant absorption and adhesion material, film, coating and preparation method and application in water |
-
2018
- 2018-06-28 CN CN201810684666.1A patent/CN108837708A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101837249A (en) * | 2010-06-13 | 2010-09-22 | 苏州绿膜科技有限公司 | Composite polrvinyl chloride hollow fiber ultrafiltration membrane and preparation method thereof |
| CN101837250A (en) * | 2010-06-22 | 2010-09-22 | 苏州绿膜科技有限公司 | Modified polrvinyl chloride hollow fiber ultrafiltration membrane, preparation method and application thereof |
| CN102861519A (en) * | 2011-07-05 | 2013-01-09 | 北京金通量科技有限公司 | Preparation method of long-acting hydrophilic polyvinyl chloride hollow fiber ultrafiltration membrane |
| CN107096402A (en) * | 2016-02-19 | 2017-08-29 | 中国科学院苏州纳米技术与纳米仿生研究所 | Oil resistant absorption and adhesion material, film, coating and preparation method and application in water |
| CN105709620A (en) * | 2016-04-28 | 2016-06-29 | 安阳华森纸业有限责任公司 | Preparation method of hollow fiber oxygen permeable membrane |
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