CN105983350A - Preparation method of hydrophobic polypropylene-polyethylene glycol terephthalate blended micropore membrane - Google Patents
Preparation method of hydrophobic polypropylene-polyethylene glycol terephthalate blended micropore membrane Download PDFInfo
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- CN105983350A CN105983350A CN201510039160.1A CN201510039160A CN105983350A CN 105983350 A CN105983350 A CN 105983350A CN 201510039160 A CN201510039160 A CN 201510039160A CN 105983350 A CN105983350 A CN 105983350A
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Abstract
The invention discloses a preparation method of a hydrophobic polypropylene-polyethylene glycol terephthalate blended micropore membrane. The micropore membrane includes, by mass, 10-50 parts of a polypropylene-polyethylene glycol terephthalate blended material and 50-90 parts of an ester diluent. The polypropylene-polyethylene glycol terephthalate blended material includes polypropylene, a compatibilizer, polyethylene glycol terephthalate and a nucleating agent according to the mass ratio of 90-50:1-10:5-40:0-1. Through quantitative addition of the compatibilizer for compatibly modifying the polypropylene and polyethylene glycol terephthalate, the hydrophobic polypropylene-polyethylene glycol terephthalate blended micropore membrane is prepared. The polypropylene-polyethylene glycol terephthalate blended membrane, compared with a pure polypropylene micropore membrane, is improved greatly in hydrophobicity and mechanical performance. The pore size of the membrane is 0.1-10 [mu]m and is easy to control.
Description
Technical field
The present invention relates to membrane separation technique, particularly relate to a kind of thermally induced phase separation preparation and hydrophobic microporous membrane preparation method is blended.
Background technology
Membrane separation technique because its efficiency is high, equipment is simple, energy-conserving and environment-protective, the feature such as easy and simple to handle, there are great commercial Application potentiality.Wherein Membrane Materials (membrane distillation, MD) technology is a kind of membrance concentration process with dewatering microporous film both sides steam pressure reduction as mass transfer force.MD technology can operate under negative pressure and lower temperature compared with other membrane separating process, and the cheap energy such as available industrial waste heat, the rejection of component non-volatile to macromole, inorganic salt etc. close to 100%, one of study hotspot having become as membrane separation technique at present.The technology of preparing of high separability energy dewatering microporous film is restriction film distillation technology application and the key of industrialization thereof, membrane material for MD should meet hydrophobicity and two basic demands of porous, secondly also to have enough mechanical strengths, excellent heat stability, chemical stability.The maximum obstruction of MD technology heavy industrialization application is that membrane material easily occurs hydrophiling to pollute, and membrane material mechanical strength is unable to maintain that MD process is run steadily in the long term simultaneously.The membrane material of single formula is less due to controlled condition, constrain the development of film distillation technology equally, polymer is blended also known as polymeric material alloy, and polymeric material alloying is to realize improving the hydrophobic performance of film, mechanical strength and membrane distillation properties, widening membrane material kind and the regulation and control extremely effective method of membrane structure.
1981, the roundup preparing microporous membrane about thermally induced phase separation is that the patent delivered by Castro proposes the earliest, thermally induced phase separation (thermally induced phase separation, TIPS) is a kind of method that, low temperature split-phase principle compatible based on macromolecular solution high temperature prepares porous membranes.TIPS method is prepared the maximum advantage of microporous membrane and is to can be applicable under room temperature the polymer without suitable solvent.But prepared by blended membrane material for tradition TIPS method, it is desirable to two kinds of intermingling materials have the compatibility, as poor in the bi-material compatibility, cannot be blended.This patent proposes a kind of method that the TIPS of use method uses two kinds of poor materials of the compatibility to prepare dewatering microporous film, i.e. by adding bulking agent
Polyethylene terephthalate is the engineering plastics of a kind of excellent performance, because it is cheap and has the performances such as excellent thermostability, chemical proofing, obdurability, electrical insulating property and safety, it is widely used in the fields such as fiber, thin film, engineering plastics, polyester bottles, is one of most widely used functional polymer polymer；Polypropylene is cheap, has extensive chemical stability and heat stability, but the material impact strength prepared by virgin pp is low, and fragility is big and toughness is not enough.Polyethylene terephthalate is the engineering plastics of a kind of excellent performance, because of its excellent thermostability, chemical proofing, obdurability.Adding in the film with polypropylene as matrix of polyethylene terephthalate be can further improve the hydrophobicity of film and improve film shock resistance and toughness.But polypropylene is blended with polyethylene terephthalate and belongs to the poor system of the compatibility, thermally induced phase separation simple blend film forming cannot be used, originally research and propose and improve Miscibility by addition bulking agent, prepare high-performance polypropylene-polyethylene terephthalate and dewatering microporous film is blended.
Prior art use thermally induced phase separation prepare hydrophobic polypropylene microporous membrane, as disclosed No. CN01144479.7, No. CN200510041012.X, the preparation of microporous polypropylene membrane described by CN201010191837.0 Chinese patent, use Thermal inactive method by changing proportioning regulation and control product microporous polypropylene membrane pore-size distribution and the porosity of polymer and diluent.But due to shortcomings such as the toughness of polypropylene material own are not enough, frangible, it is applied to during Membrane Materials easily to occur hydrophiling and the problem such as ruptures, limiting the application of microporous polypropylene membrane.Simultaneously because the hydrophobicity of polypropylene is relatively strong, poor with other polymer-polymer miscibilities, it is difficult to be modified with other polymer blended preparation hydrophobic membrane.Prior art uses polypropene blended film, as No. CN201410211836.6 described, previously prepared polypropylene-nylon blending material, uses intermingling material to re-use thermic phase method masking, and polypropylene carries out hydrophilic modifying acquisition hydrophilic film for ultra-filtration process.At present both at home and abroad patent and document are prepared polypropylene-polyethylene terephthalate the relevant report of dewatering microporous film are blended without directly utilizing thermally induced phase separation temporarily.
Summary of the invention
For the problem such as the existing easy hydrophiling of MD membrane material and mechanical strength be low, the purpose of the present invention is to propose to a kind of polypropylene-polyethylene terephthalate and the preparation method of dewatering microporous film is blended, this microporous membrane, with polypropylene, polyethylene terephthalate, bulking agent, nucleator and diluent as raw material, uses thermally induced phase separation to prepare polypropylene-polyethylene terephthalate and dewatering microporous film is blended.Polypropylene-polyethylene terephthalate prepared in accordance with the present invention is blended dewatering microporous film, section structure is uniform alveolate texture, micropore size 0.01 μm～10 μm, membrane porosity is 30%-85%, contact angle is more than 120 °, hot strength 9MPa-24MPa, elongation at break 12%-16%.Products obtained therefrom film relatively virgin pp microporous membrane all has a distinct increment at hydrophobicity and mechanical strength.It is applied to 0.5mol L-1NaCl solution vacuum membrane distillation process, when feed rate is 30L h-1, during feeding temperature 80 DEG C, membrane flux can reach 14.38kg m-2·h-1, rejection is higher than 99.99%.
Polypropylene-the polyethylene terephthalate of the present invention is blended the preparation method of dewatering microporous film and carries out in accordance with the following steps:
(1) material is prepared: 50-90 part esters diluent, 10-50 part polypropylene-polyethylene terephthalate intermingling material (polypropylene, bulking agent, polyethylene terephthalate and nucleator, the mass ratio of each component is 90-50: 1-10: 5-40: 0-1)；
(2) mixture in step (1) is placed in high score stirred autoclave, constant temperature 180 DEG C-250 DEG C, under nitrogen protective condition, stirs 2h-6h, obtain uniform solution；Stop stirring and stand solution 1h-5h with deaeration, obtaining homogeneous casting solution；
(3) the homogeneous casting solution that step (2) obtains is coated in template or is coated on non-woven fabrics supporting layer via flat membrane casting equipment and obtains Flat Membrane, or casting solution is sent into double screw extruder, extrusion temperature is 180 DEG C-250 DEG C, spins hollow-fibre membrane by spinning head；The Flat Membrane of molding or hollow-fibre membrane enter 0-50 DEG C of coagulating bath and occur to be separated；
(4) the film extractant of purity more than 90% step (3) prepared stands or ultrasonic extraction 8h-30h, finally air-dries or is placed in baking oven drying in air and obtain polypropylene-polyethylene terephthalate dewatering microporous film is blended.
Above-mentioned bulking agent is polypropylene grafted maleic anhydride, polypropylene grafted methacrylic acid.
Above-mentioned diluent is one or several in dimethyl phthalate, diethyl phthalate, dibutyl phthalate, dioctyl phthalate, SA dibutyl ester.
Above-mentioned nucleator is the one in adipic acid, suberic acid, dibenzylidene sorbitol.
Above-mentioned extractant is that the one in methanol, ethanol, propanol, n-butyl alcohol, isobutanol, isopropanol lives several mixture.
Compared with prior art, the present invention carries out capacity increasing modifying by suitable bulking agent to polypropylene and polyethylene terephthalate, the blend film of preparation has the characteristic of the advantages such as good chemical performance and the rigidity of polypropylene material, is provided simultaneously with the characteristics such as the good hydrophobicity of pet material and pliability；Blend film has the premium properties of two kinds of polymer concurrently.Preparation process is simply efficient, and membrane material is with low cost, and membrane pore structure is prone to regulation and control, uniform narrow pore-size distribution；Polypropylene-the polyethylene terephthalate of preparation is blended hydrophobic microporous membrane flux height, contamination resistance is strong, mechanical strength is high, rejection is high, it is adaptable to MD, film absorb and Membrane Extraction.
Accompanying drawing explanation
For different polypropylene/polyethylene terephthalate quality, than blend film cross section SEM figure, (polypropylene/polyethylene terephthalate mass ratio a, b, c and d is respectively 4: 1,6: 1,8: 1 and 10: 1 to Fig. 1；Blend film solid content is all 30%), note: the region adding frame in figure is solid-liquid phase fractional crystallization region.
Fig. 2 is that polypropylene-polyethylene terephthalate is blended dewatering microporous film contact angle determination result.
Fig. 3 is that (a is hot strength to product film of the present invention with virgin pp dewatering microporous film measuring mechanical property comparison diagram；B is elongation at break).
Fig. 4 is polypropylene-polyethylene terephthalate dewatering microporous film and virgin pp microporous membrane vacuum membrane distillation performance comparison figure.
Detailed description of the invention
Example 1
(1) film preparation material: weighing mass ratio is 70 parts of esters diluent dibutyl phthalates, 30 parts of polypropylene-polyethylene terephthalate intermingling materials (isotactic polypropylene, polyethylene terephthalate, bulking agent polypropylene grafted maleic anhydride, nucleator dibenzylidene sorbitol, the mass ratio of each component is 85.9: 8.6: 5: 0.5)；
(2) being placed in high-temperature stirring reactor by the mixture in step (1), 250 DEG C of constant temperature, stir speed (S.S.) is 250rpm and stirs 4h under conditions of nitrogen protection, obtains uniform solution；Stop stirring and stand solution 2h with deaeration, obtaining homogeneous casting solution；
(3) homogeneous casting solution step (2) obtained is coated on non-woven fabrics supporting layer via flat membrane casting equipment and obtains Flat Membrane, and scraping film temperature is 180 DEG C, and the Flat Membrane of molding immerses in 25 DEG C of solidification water-baths and completes to be separated；
(4) the film ethanol extractant ultrasonic extraction 24h of purity 95% step (3) prepared, finally dries 2h in 60 DEG C, obtains product polypropylene-polyethylene terephthalate and dewatering microporous film is blended.
It is 70.57% that product is blended hydrophobic microporous membrane porosity, and contact angle is 116.81 °, and hot strength is 22.17MPa, and elongation at break is 14.67%.It is applied to 0.5mol L-1NaCl solution vacuum membrane distillation process, when feed rate is 30L h-1, vacuum is 0.095MPa, when feeding temperature is 80 DEG C, and membrane flux 11.08kg m-2·h-1。
Example 2
(1) film preparation material: weighing mass ratio is 60 parts of esters diluent dibutyl phthalates, 40 parts of polypropylene-polyethylene terephthalate intermingling materials (isotactic polypropylene, polyethylene terephthalate, bulking agent polypropylene grafted maleic anhydride, nucleator dibenzylidene sorbitol, the mass ratio of each component is 85.9: 8.6: 5: 0.5)；
(2) being placed in high-temperature stirring reactor by the mixture in step (1), 250 DEG C of constant temperature, stir speed (S.S.) is 250rpm and stirs 4h under conditions of nitrogen protection, obtains uniform solution；Stop stirring and stand solution 2h with deaeration, obtaining homogeneous casting solution；
(3) homogeneous casting solution step (2) obtained is coated on non-woven fabrics supporting layer via flat membrane casting equipment and obtains Flat Membrane, and scraping film temperature is 180 DEG C, and the Flat Membrane of molding immerses 25 DEG C of solidification water-baths and completes to be separated；
(4) the film ethanol extractant ultrasonic extraction 24h of purity 95% step (3) prepared, finally dries 2h in 60 DEG C, obtains product polypropylene-polyethylene terephthalate and dewatering microporous film is blended.
It is 50.33% that product is blended hydrophobic microporous membrane porosity, and contact angle is 117.43 °, and hot strength is 24.34MPa, and elongation at break is 16.04%.It is applied to 0.5mol L-1NaCl solution vacuum membrane distillation process, when feed rate is 30L h-1, vacuum is 0.095MPa, when feeding temperature is 80 DEG C, and membrane flux 7.03kg m-2·h-1。
Example 3
(1) film preparation material: weighing mass ratio is 70 parts of esters diluent dibutyl phthalates, 30 parts of polypropylene-polyethylene terephthalate intermingling materials (isotactic polypropylene, polyethylene terephthalate, bulking agent polypropylene grafted maleic anhydride, nucleator dibenzylidene sorbitol, the mass ratio of each component is 81: 13.5: 5: 0.5)；
(2) being placed in high-temperature stirring reactor by the mixture in step (1), 250 DEG C of constant temperature, stir speed (S.S.) is 250rpm and stirs 4h under conditions of nitrogen protection, obtains uniform solution；Stop stirring and stand solution 2h with deaeration, obtaining homogeneous casting solution；
(3) homogeneous casting solution step (2) obtained is coated on non-woven fabrics supporting layer via flat membrane casting equipment and obtains Flat Membrane, and scraping film temperature is 180 DEG C, and the Flat Membrane of molding immerses 25 DEG C of solidification water-baths and completes to be separated；
(4) the film ethanol extractant ultrasonic extraction 24h of purity 95% step (3) prepared, finally dries 2h in 60 DEG C, obtains product polypropylene-polyethylene terephthalate and dewatering microporous film is blended.
It is 62.43% that product is blended hydrophobic microporous membrane porosity, and contact angle is 118.62 °, and hot strength is 27.23MPa, and elongation at break is 17.53%.It is applied to 0.5mol L-1NaCl solution vacuum membrane distillation process, when feed rate is 30L h-1, vacuum is 0.095MPa, and when feeding temperature is 80 DEG C, membrane flux is 10.03kg m-2·h-1。
Comparative example 1
(1) film preparation material: weighing mass ratio is 70 parts of esters diluent dibutyl phthalates, 29.95 parts of isotactic polypropylene, 0.05 part of nucleator dibenzylidene sorbitol；
(2) being placed in high-temperature stirring reactor by the mixture in step (1), 180 DEG C of constant temperature, stir speed (S.S.) is 250rpm and stirs 4h under conditions of nitrogen protection, obtains uniform solution；Stop stirring and stand solution 2h with deaeration, obtaining homogeneous casting solution；
(3) homogeneous casting solution step (2) obtained is coated on non-woven fabrics supporting layer via flat membrane casting equipment and obtains Flat Membrane, and scraping film temperature is 180 DEG C, and the Flat Membrane of molding immerses 25 DEG C of solidification water-baths and completes to be separated；
(4) the film ethanol extractant ultrasonic extraction 24h of purity 95% step (3) prepared, finally dries 2h in 60 DEG C, obtains product polypropylene-polyethylene terephthalate and dewatering microporous film is blended.
It is 65.43% that the virgin pp prepared is blended hydrophobic microporous membrane porosity, and contact angle is 98.11 °, and hot strength is 16.32MPa, and elongation at break is 11.74%.It is applied to 0.5mol L-1NaCl solution vacuum membrane distillation process, when feed rate is 30L h-1, vacuum is 0.095MPa, and during feeding temperature 80 DEG C, membrane flux is 13.01kg m-2·h-1。
Obtained by comparing embodiment analysis: prepared by comparative example raw material is not blended to use polyethylene terephthalate, only use isotactic polypropylene, take same thermally induced phase separation to prepare hydrophobic polypropylene microporous membrane.From test result, product hydrophobic polypropylene microporous membrane porosity, water contact angle, hot strength and elongation at break relatively equivalent polymers content polypropylene-polyethylene terephthalate are blended dewatering microporous film and substantially reduce.Proof utilizes the inventive method preparation that dewatering microporous film its membrane property is blended and is significantly better than single hydrophobic polypropylene microporous membrane, improves including hydrophobicity, and porosity increase and mechanical strength and survivability are strengthened.
The foregoing is only present pre-ferred embodiments, not in order to limit the present invention, all within the spirit and principles in the present invention, any modification, equivalent substitution and improvement etc. made, should be included within the scope of the present invention.
Claims (5)
1. polypropylene-polyethylene terephthalate is blended a dewatering microporous film, and it is prepared raw material and comprises material of main part, it is characterised in that: press
Mass fraction calculates, including 10-50 part polypropylene-polyethylene terephthalate intermingling material, 50-90 part esters diluent；Described poly-third
Alkene-polyethylene terephthalate intermingling material composition includes polypropylene, bulking agent, polyethylene terephthalate and nucleator, each component
Mass ratio is 90-50: 1-10: 5-40: 0-1.
Polypropylene-polyethylene terephthalate the most according to claim 1 is blended dewatering microporous film, it is characterised in that: described increase-volume
Agent is polypropylene grafted maleic anhydride, polypropylene grafted methacrylic acid.
Polypropylene-polyethylene terephthalate the most according to claim 1 is blended dewatering microporous film, it is characterised in that: described dilution
Agent is in dimethyl phthalate, diethyl phthalate, dibutyl phthalate, dioctyl phthalate, SA dibutyl ester
One or several；Described nucleator one in adipic acid, suberic acid, dibenzylidene sorbitol.
4. polypropylene-polyethylene terephthalate as claimed in claim 1 is blended the preparation method of dewatering microporous film, it is characterised in that
Comprise the steps:
(1) material is prepared: 50-90 part esters diluent, 10-50 part polypropylene-polyethylene terephthalate intermingling material (polypropylene, increasing
Holding agent, polyethylene terephthalate and nucleator, the mass ratio of each component is 90-50: 1-10: 5-40: 0-1)；
(2) mixture in step (1) is placed in high score stirred autoclave, constant temperature 180 DEG C-250 DEG C, under nitrogen protective condition, stirs 2h-6h,
Obtain uniform solution；Stop stirring and stand solution 1h-5h with deaeration, obtaining homogeneous casting solution；
(3) the homogeneous casting solution that step (2) obtains is coated in template or is coated on non-woven fabrics supporting layer via flat membrane casting equipment and obtains Flat Membrane,
Or casting solution is sent into double screw extruder, extrusion temperature is 180 DEG C-250 DEG C, spins hollow-fibre membrane by spinning head；The Flat Membrane of molding or
Person's hollow-fibre membrane enters 0-50 DEG C of coagulating bath and occurs to be separated；
(4) extractant of the film purity more than 90% step (3) prepared stands or ultrasonic extraction 8h-30h, finally air-dries in air or puts
Dry in baking oven and obtain polypropylene-polyethylene terephthalate dewatering microporous film is blended.
5. require that described polypropylene-polyethylene terephthalate is blended dewatering microporous film according to claim 1, it is characterised in that: described
Extractant one or several mixture in methanol, ethanol, propanol, n-butyl alcohol, isobutanol, isopropanol.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US11376553B2 (en) * | 2020-02-24 | 2022-07-05 | Tianjin University Of Science And Technology | Superhydrophobic polypropylene porous film, preparation method therefor, and method for improving hydrophobicity of polypropylene porous film |
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| CN103272484A (en) * | 2013-05-27 | 2013-09-04 | 河北工业大学 | Method for preparing high-hydrophobicity microporous membrane |
| CN103785303A (en) * | 2012-11-02 | 2014-05-14 | 中国石油化工股份有限公司 | Preparation method and application of polypropylene hollow fiber hydrophobic membrane |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103785303A (en) * | 2012-11-02 | 2014-05-14 | 中国石油化工股份有限公司 | Preparation method and application of polypropylene hollow fiber hydrophobic membrane |
| CN103272484A (en) * | 2013-05-27 | 2013-09-04 | 河北工业大学 | Method for preparing high-hydrophobicity microporous membrane |
Non-Patent Citations (1)
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| 柳峰等: ""PET/PP共混改性研究进展"", 《材料科技》 * |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US11376553B2 (en) * | 2020-02-24 | 2022-07-05 | Tianjin University Of Science And Technology | Superhydrophobic polypropylene porous film, preparation method therefor, and method for improving hydrophobicity of polypropylene porous film |
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Application publication date: 20161005 |