CN105233704A - Novel preparation method of high-performance composite film - Google Patents
Novel preparation method of high-performance composite film Download PDFInfo
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- CN105233704A CN105233704A CN201510621226.8A CN201510621226A CN105233704A CN 105233704 A CN105233704 A CN 105233704A CN 201510621226 A CN201510621226 A CN 201510621226A CN 105233704 A CN105233704 A CN 105233704A
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Abstract
The present invention provides a novel preparation method of a high-performance and high-strength composite film. The preparation method comprises: a) dissolving an organic polymer film preparing material in an organic solvent to obtain a homogeneous solution, adding a certain amount of an additive, uniformly mixing, and carrying out standing deaeration to obtain a film casting solution; and 2) placing the film casting solution in a constant pressure propeller, and spraying the film casting solution on a nonwoven fabric fixed on the surface of a rotation roller in a spray-coating manner by using a solution injection method while rotating the rotation roller, wherein the lower half portion of the rotation roller is immersed in the coagulation bath, and the constant pressure propeller speed, the injection distance, the rotation roller speed, the material feeding temperature, the atomizing pressure, and the air flow rate parameter are controlled to control the pore size and the distribution of the film so as to obtain the high-performance and high-strength fiber composite film. According to the present invention, the method has characteristics of simple preparation process, easy operation, low equipment requirements, energy saving and low cost, and is suitable for large-scale production.
Description
Technical field
The present invention relates to the preparation method of a kind of high-performance, high-strength composite film, be specifically related to a kind of that adopt solution gunite acquisition aperture adjustable, that there is spongelike structure high-strength composite tunica fibrosa.
Background technology
Membrane separation technique is as a kind of new and effective fluid separation element operating technology, owing to having separation, concentrated, purifying and refining function concurrently, there are again efficient, energy-saving and environmental protection, molecule level is filtered and filter process is simple, be easy to the features such as control, achieve the develop rapidly attracted people's attention in recent years, it is widely used in the industrial circle such as the manufacture of sterilized water, high-purity water or beverage, the purification of air.Further, in recent years, be also used widely in the field such as sanitary wastewater and industrial wastewater.Current filming technology mainly contains: the methods such as immersion precipitation phase inversion process, thermally induced phase separation, steam induction phase separation method.In the preparation process of composite membrane, membrane aperture and pore structure have vital impact to performance.A lot of to aperture and the isoparametric regulate and control method of pore structure, comprising the selection in solvent/non-solvent system, in casting solution, add perforating agent, add easy volatile solvent, the methods such as regulation and control membrance casting condition.By the regulation and control to aperture, the continuous transformation of fenestra most Zhongdao dense non-porous film from micro-meter scale to nanoscale can be realized.Being coated with and realizing polysulfones fenestra by the temperature of the content of non-solvent in regulation and control casting solution and kind, coagulating bath and environment and ambient humidity and the time of staying in triumphant patent of invention " a kind of polysulfones diffusion barrier and preparation method thereof " (CN104437138A) is spongy gradient-structure.Although this method controls the pore structure of film, complicated operation, and need a large amount of organic solvents.For most of membrane material, improving the concentration of casting solution is the main method reducing aperture, but when casting solution concentration is too high, its mobility is too poor and be difficult to scrape and paint mould.And along with the increase in aperture, the mechanical performance of membrane material will certainly reduce, and therefore its durability also can be affected.Therefore the regulation and control of membrane aperture and the guarantee of membrane material mechanical performance are seemed particularly important.
Solution gunite is adopted to be that carrier prepares composite membrane on its surface with non-weaving cloth, above method mesoporous can be solved and be difficult to regulation and control, mechanical strength is difficult to the problem ensured, this method can by the size reconciling air flow rate, the distance of injection, the rotating speed, feeding temperature etc. of live-rollers come controlling diaphragm aperture under lower casting solution concentration, the unnecessary environmental pollution that the use decreasing multiple organic solvent in above method brings, and this kind of method is simple to operation, be applicable to industrial production.Select non-weaving cloth to be that carrier works in coordination with the mechanical strength enhancing composite film material simultaneously, improve stability and the durability of composite membrane.
Summary of the invention
The invention provides a kind of preparation method of novel high-performance composite membrane, adopt the method that solution sprays, by the angle of rake speed of adjustment constant voltage, jet length, live-rollers rotating speed, feeding temperature, atomization pressure, air flow rate, obtain the controlled composite separating film in aperture at nonwoven fabric surface.
The present invention prepares high-performance, high-strength composite diffusion barrier, and concrete preparation process is as follows:
(1) by mass content be 1 ~ 30% the organic polymer material of preparing of abundant drying join in organic solvent, stirring and dissolving 1 ~ 5h under 50 ~ 100 DEG C of conditions, obtain homogeneous phase solution, appropriate additive is added after thing to be polymerized dissolves completely, continue to be stirred to and dissolve completely, by solution left standstill or in vacuum drying chamber deaeration 1 ~ 24h obtain casting solution, stand-by;
(2) solution after deaeration step (1) obtained is placed in constant voltage propeller, adopt the method that solution sprays, by adjustment jet length, live-rollers rotating speed, feeding temperature parameter, casting solution is sprayed at and is fixed on the non-weaving cloth of roll surface by the parameter such as atomizing pressure and air flow rate, transfer roller is rotated while solution sprays, transfer roller Lower Half is immersed in 0.5 ~ 24h in coagulating bath, then rinsing 48h in pure water is transferred to, in rinse cycle, every 2 ~ 5h changes a water, and the composite membrane prepared at room temperature is placed 24h and dried in the shade.The pore-size distribution of composite membrane is between 50nm ~ 100 μm, and porosity is between 30 ~ 90%, and film thickness is between 30 ~ 1000 μm.
Described organic polymer material of preparing refers to Kynoar, dimethyl silicone polymer, poly-trimethyl silicane propine, polyacrylonitrile, Vingon, polyvinyl alcohol, polyvinyl chloride, polypropylene, polyethylene, Merlon, polyimide, polyamide-based, polysulfones, cellulose derivative class etc.Different polymer can be selected according to different demands.
Described organic solvent refers to the mixed solvent of acetone, dimethyl formamide, dimethylacetylamide, oxolane, dimethyl sulfoxide (DMSO), 1-METHYLPYRROLIDONE, MEK or above-mentioned solvent.
The mass content of described organic solvent is 70 ~ 95%.
Described additive refers to polymeric additive or low molecular weight additives, and polymeric additive has polyvinylpyrrolidone, polyethylene glycol etc.; Low molecular weight additives has anhydrous Lithium chloride, calcium chloride, calcium nitrate, acetic acid, triethyl phosphate, ethanol, acetone, glycerine, ethylene glycol, water etc.
The consumption of described additive is 1 ~ 10%.
The material of described non-weaving cloth is natural fiber or the synthetic fibers such as cotton, fiber crops, wool, silk, asbestos fibre, glass fibre, terylene, polyamide fibre, polypropylene fibre.
The angle of rake speed of parameter constant voltage that described solution sprays is 1mL ~ 100L/h, jet length is 1 ~ 20cm, live-rollers rotating speed is 1 ~ 1000r/min, feeding temperature is 0 ~ 100 DEG C, atomizing pressure is 0.1 ~ 10MPa, air flow rate is 10mL/h ~ 100L/h.
Described coagulating bath refers to distilled water, methyl alcohol, ethanol, propyl alcohol or both above mixed solvents above-mentioned.
The method that the present invention utilizes solution to spray prepares high-performance, high-strength composite film, avoid the use of a large amount of organic solvent in the methods such as the induction of immersion precipitation phase inversion process, thermally induced phase separation and steam is separated, reduce the discharge of organic solvent, decrease the harm to environment.Simultaneously to have efficiency high for solution gunite, and the advantages such as equipment is simple, easy to operate, are conducive to large-scale industrial production.The more important thing is that this method can regulate and control the aperture of composite membrane, there is very large potential using value.
Accompanying drawing explanation
Fig. 1 is the electromicroscopic photograph of the composite membrane prepared by embodiment 1.
Fig. 2 is the cross-section photographs of the composite membrane prepared by embodiment 1.
Detailed description of the invention
Below by way of the method that specific embodiment describes for further illustrating the present invention, but be not intended that the invention be limited to these embodiments.
Embodiment 1
(1) Kynoar that 3g is fully dry is joined in 92g dimethylacetylamide, stirring and dissolving 2h under 50 DEG C of conditions, the 5g anhydrous Lithium chloride added after thing to be polymerized dissolves completely, continue to be stirred to and dissolve completely, obtain homogeneous phase solution, standing and defoaming 30min, stand-by;
(2) solution after deaeration step (1) obtained is placed in constant voltage propeller, fltting speed is set to 100mL/h, adopt the method that solution sprays, adjustment jet length is 5cm, live-rollers rotating speed is 10r/min, feeding temperature is 25 DEG C, be 1.5MPa at atomizing pressure, air flow rate is that casting solution is sprayed at and is fixed on the terylene non-weaving cloth of roll surface by 160mL/h, transfer roller is rotated while solution sprays, transfer roller Lower Half is immersed in 10h in coagulating bath running water, then rinsing 48h in pure water is transferred to, in rinse cycle, every 2 ~ 5h changes a water, the composite membrane prepared at room temperature is placed 24h and is dried in the shade.
The high-performance prepared by above-mentioned steps, high-strength composite film, as shown in Figure 1, can find out the even aperture distribution of composite membrane, aperture size is distributed between 200 ~ 500nm.Fig. 2 is the scanning electron microscope diagram of composite membrane section, as seen from Figure 2, composite membrane is uniform spongy hole, drawn strength test, the hot strength of this composite membrane is 81.1MPa, and the hot strength 79.6MPa comparing terylene non-weaving cloth improves 1.9%.
Embodiment 2
(1) Kynoar that 10g is fully dry is joined in 85g dimethylacetylamide, stirring and dissolving 3h under 80 DEG C of conditions, the 5g anhydrous Lithium chloride added after thing to be polymerized dissolves completely, continue to be stirred to and dissolve completely, obtain homogeneous phase solution, standing and defoaming 5h, stand-by;
(2) solution after deaeration step (1) obtained is placed in constant voltage propeller, fltting speed is set to 400mL/h, adopt the method that solution sprays, adjustment jet length is 10cm, live-rollers rotating speed is 15r/min, feeding temperature is 50 DEG C, be 2.5MPa at atomizing pressure, air flow rate is that casting solution is sprayed at and is fixed on the polypropylene non-woven fabric of roll surface by 200mL/h, transfer roller is rotated while solution sprays, transfer roller Lower Half is immersed in coagulating bath running water, to be sprayed complete after take off non-weaving cloth, immersed 10h in the right running water of coagulating bath, after be transferred to rinsing 48h in pure water, in rinse cycle, every 2 ~ 5h changes a water, the composite membrane prepared at room temperature is placed 24h and is dried in the shade.
The high-performance prepared by above-mentioned steps, high-strength composite film, its aperture size is distributed between 100 ~ 300nm.Drawn strength test, the hot strength of this composite membrane is 83.1MPa, and the hot strength 81.2MPa comparing polypropylene non-woven fabric improves 2.3%.
Embodiment 3
(1) 10g bisphenol-a polysulfone is joined in 85g nitrogen methyl pyrrolidone, stirring and dissolving 3h under 80 DEG C of conditions, the 5g calcium chloride added after thing to be polymerized dissolves completely, continue to be stirred to and dissolve completely, obtain homogeneous phase solution, in vacuum drying chamber, deaeration 1h, stand-by;
(2) solution after deaeration step (1) obtained is placed in constant voltage propeller, fltting speed is set to 300mL/h, adopt the method that solution sprays, adjustment jet length is 15cm, live-rollers rotating speed is 30r/min, feeding temperature is 50 DEG C, be 1.5MPa at atomizing pressure, air flow rate is that casting solution is sprayed at and is fixed on the terylene non-weaving cloth of roll surface by 140mL/h, transfer roller is rotated while solution sprays, transfer roller Lower Half immerses in coagulating bath absolute ethyl alcohol, to be sprayed complete after take off non-weaving cloth, immersed 10h in coagulating bath absolute ethyl alcohol, then rinsing 48h in pure water is transferred to, in rinse cycle, every 2 ~ 5h changes a water, the composite membrane prepared at room temperature is placed 24h and is dried in the shade.
The high-performance prepared by above-mentioned steps, high-strength composite film, its aperture size is distributed between 200 ~ 500nm.Drawn strength test, the hot strength of this composite membrane is 84.5MPa, and the hot strength 79.6MPa comparing terylene non-weaving cloth improves 6.2%.
Embodiment 4
(1) 10g polyacrylonitrile is joined 85g solvent volume ratio be 3: 1 dimethyl formamide and oxolane mixed solution in, 4h is stirred at 80 DEG C, the 5g polyvinylpyrrolidone added after thing to be polymerized dissolves completely, continue to be stirred to and dissolve completely, obtain homogeneous phase solution, in vacuum drying chamber, deaeration 1h, stand-by;
(2) solution after deaeration step (1) obtained is placed in constant voltage propeller, fltting speed is set to 500mL/h, adopt the method that solution sprays, adjustment jet length is 15cm, live-rollers rotating speed is 20r/min, feeding temperature is 80 DEG C, be 2MPa at atomizing pressure, air flow rate is that casting solution is sprayed at and is fixed on the terylene non-weaving cloth of roll surface by 200mL/h, transfer roller is rotated while solution sprays, transfer roller Lower Half immerses in coagulating bath absolute ethyl alcohol, to be sprayed complete after take off non-weaving cloth, immersed 10h in coagulating bath running water, then rinsing 48h in pure water is transferred to, in rinse cycle, every 2 ~ 5h changes a water, the composite membrane prepared at room temperature is placed 24h and is dried in the shade.
The high-performance prepared by above-mentioned steps, high-strength composite film, its aperture size is distributed between 100 ~ 600nm.Drawn strength test, the hot strength of this composite membrane is 83.7MPa, and the hot strength 79.6MPa comparing terylene non-weaving cloth improves 5.2%.
Claims (9)
1. a novel processing step for high performance composite membrane, specifically comprises the steps:
(1) by mass content be 1 ~ 30% the organic polymer material of preparing of abundant drying join in organic solvent, stirring and dissolving 1 ~ 5h under 50 ~ 100 DEG C of conditions, appropriate additive is added after thing to be polymerized dissolves completely, continue to be stirred to and dissolve completely, by solution left standstill or in vacuum drying chamber deaeration 1 ~ 24h obtain casting solution, stand-by;
(2) casting solution that step (1) obtains is placed in constant voltage propeller, adopt the method that solution sprays, by the angle of rake speed of adjustment constant voltage, jet length, live-rollers rotating speed, feeding temperature, atomization pressure, casting solution is sprayed at and is fixed on the non-weaving cloth of roll surface by air flow rate parameter, transfer roller is rotated while solution sprays, transfer roller Lower Half is immersed in coagulating bath, to be sprayedly to complete, non-weaving cloth is immersed 0.5 ~ 24h in coagulating bath, then rinsing 48h in pure water is transferred to, in rinse cycle, every 2 ~ 5h changes a water, the ambient temperatare that is compounded in prepared is put 24h and is dried in the shade.
2. preparation method as claimed in claim 1, is characterized in that: described organic polymer material of preparing refers to Kynoar, dimethyl silicone polymer, poly-trimethyl silicane propine, polyacrylonitrile, Vingon, polyvinyl alcohol, polyvinyl chloride, polypropylene, polyethylene, Merlon, polyimide, polyamide-based, polysulfones, cellulose derivative class etc.
3. preparation method as claimed in claim 1, is characterized in that: described organic solvent refers to the mixed solvent of acetone, dimethyl formamide, dimethylacetylamide, oxolane, dimethyl sulfoxide (DMSO), 1-METHYLPYRROLIDONE, MEK or above-mentioned solvent.
4. preparation method as claimed in claim 1, is characterized in that: the mass content of described organic solvent is 70 ~ 95%.
5. preparation method as claimed in claim 1, is characterized in that: described additive refers to polymeric additive or low molecular weight additives, and polymeric additive has polyvinylpyrrolidone, polyethylene glycol etc.; Low molecular weight additives has anhydrous Lithium chloride, calcium chloride, calcium nitrate, acetic acid, triethyl phosphate, ethanol, acetone, glycerine, ethylene glycol, water etc.
6. preparation method as claimed in claim 1, is characterized in that: the consumption of described additive is 1 ~ 10%.
7. preparation method as claimed in claim 1, is characterized in that: the material of described non-weaving cloth is natural fiber or the synthetic fibers such as cotton, fiber crops, wool, silk, asbestos fibre, glass fibre, terylene, polyamide fibre, polypropylene fibre.
8. preparation method as claimed in claim 1, is characterized in that: the angle of rake speed of parameter constant voltage that described solution sprays is 1mL ~ 100L/h, jet length is 1 ~ 20cm, live-rollers rotating speed is 1 ~ 1000r/min, feeding temperature is 0 ~ 100 DEG C, atomization pressure 0.1 ~ 10MPa, air flow rate scope are 10mL/h ~ 100L/h.
9. preparation method as claimed in claim 1, is characterized in that: described coagulating bath refers to distilled water, methyl alcohol, ethanol, propyl alcohol or both above mixed solvents above-mentioned.
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Cited By (6)
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CN105854748A (en) * | 2016-06-02 | 2016-08-17 | 天津工业大学 | Method for preparing cellulose acetate capsule with concave surface structure |
CN108451240A (en) * | 2018-01-31 | 2018-08-28 | 成都乐享智家科技有限责任公司 | A kind of Chinese medicine mattress and preparation method thereof and preparation system |
CN108554190A (en) * | 2018-03-05 | 2018-09-21 | 北京清源洁华膜技术有限公司 | A kind of seperation film and preparation method thereof for detaching bavin gasoline gas and air |
CN109115795A (en) * | 2018-09-06 | 2019-01-01 | 赵玮 | Atomization system, detection device and working method using the atomization system |
CN109321297A (en) * | 2018-11-15 | 2019-02-12 | 杭州勃扬能源设备有限公司 | A kind of oil field gas treatment process |
CN113699692A (en) * | 2020-05-21 | 2021-11-26 | 株式会社东芝 | Method for producing fiber sheet and apparatus for producing fiber sheet |
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CN203170229U (en) * | 2013-04-17 | 2013-09-04 | 中国科学院长春应用化学研究所 | Coating film scraping machine |
CN104815563A (en) * | 2015-04-20 | 2015-08-05 | 天津工业大学 | Reinforced hollow fibrous membrane and preparation method thereof |
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Cited By (11)
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CN105854748A (en) * | 2016-06-02 | 2016-08-17 | 天津工业大学 | Method for preparing cellulose acetate capsule with concave surface structure |
CN105854748B (en) * | 2016-06-02 | 2018-07-31 | 天津工业大学 | A kind of preparation method of surface concave structure acetate fiber cellulose capsule |
CN108451240A (en) * | 2018-01-31 | 2018-08-28 | 成都乐享智家科技有限责任公司 | A kind of Chinese medicine mattress and preparation method thereof and preparation system |
CN108554190A (en) * | 2018-03-05 | 2018-09-21 | 北京清源洁华膜技术有限公司 | A kind of seperation film and preparation method thereof for detaching bavin gasoline gas and air |
CN108554190B (en) * | 2018-03-05 | 2021-03-02 | 北京清源洁华膜技术有限公司 | Separation membrane for separating diesel and gasoline gas and air and preparation method thereof |
CN109115795A (en) * | 2018-09-06 | 2019-01-01 | 赵玮 | Atomization system, detection device and working method using the atomization system |
CN109115795B (en) * | 2018-09-06 | 2020-11-13 | 嘉兴鼎尚信息科技有限公司 | Atomization system, detection device using atomization system and working method |
CN109321297A (en) * | 2018-11-15 | 2019-02-12 | 杭州勃扬能源设备有限公司 | A kind of oil field gas treatment process |
CN109321297B (en) * | 2018-11-15 | 2020-06-30 | 杭州勃扬能源设备有限公司 | Treatment process of petroleum associated gas |
CN113699692A (en) * | 2020-05-21 | 2021-11-26 | 株式会社东芝 | Method for producing fiber sheet and apparatus for producing fiber sheet |
CN113699692B (en) * | 2020-05-21 | 2023-09-12 | 株式会社东芝 | Method and apparatus for producing fiber sheet |
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