CN102505351A - Method for preparing polysulfonamide separating films by aid of electrostatic spinning - Google Patents
Method for preparing polysulfonamide separating films by aid of electrostatic spinning Download PDFInfo
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- CN102505351A CN102505351A CN2011103615080A CN201110361508A CN102505351A CN 102505351 A CN102505351 A CN 102505351A CN 2011103615080 A CN2011103615080 A CN 2011103615080A CN 201110361508 A CN201110361508 A CN 201110361508A CN 102505351 A CN102505351 A CN 102505351A
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Abstract
The invention relates to a method for preparing polysulfonamide separating films by the aid of electrostatic spinning. The method includes steps that N-N dimethyl acetamide is used as solvent, an electrostatic spinning condition is optimized by an orthogonal test method, polysulfonamide spinning liquid with mass percent ranging from 10% to 15% is adopted at the room temperature, spinning voltage ranges from 20kV to 30kV, the receiving distance between a receiving device and a spinneret ranges from 12cm to 18cm, and under the best condition, the nanometer polysulfonamide separating films are prepared by the aid of electrostatic spinning. At the temperature ranging from 100 DEG C to 140 DEG C, the nanometer polysulfonamide separating films are treated in a vacuum drying box for 20 hours to 30 hours. Absorption performance test experiments show that polysulfonamide non-woven fabrics after being in electrostatic spinning have a high-absorption performance, the absorption performance of the polysulfonamide non-woven fabrics is higher than that of a film directly cast by spinning liquid by twice to four times, and accordingly electrostatic spinning is a potential method for preparing the high-absorption polysulfonamide separating films. The method expands the application field of polysulfonamide and electrostatic spinning, and has certain creativeness and practicality.
Description
Technical field
The present invention relates to a kind of macromolecule organic separation membrane and preparation method thereof, be specifically related to a kind of polysulfonamides diffusion barrier and utilize the method for electrostatic spinning its preparation.
Background technology
The strategy of sustainable development that China is implementing requires modern enterprise in the economic pursuit benefit, can not diminish environmental benefit, ecological benefits and social benefit, finally realizes low consumption, efficient, the free of contamination mode of production.Along with the mankind in the mine, activity in production such as smelting, electrolysis, plating, agricultural chemicals, medicine, paint, pigment increasing; No matter the heavy metal wastewater thereby that produces is all to increase greatly in quantity or on kind; Cause many heavy metals to get into the ecosystem, caused the serious environmental pollution and the wasting of resources.Therefore, the improvement of heavy metal wastewater thereby is the key subjects in environmental protection field, the world always.For realizing sustainable development, require on the one hand industrial wastewater is rationally handled, require that on the other hand the composition capable of using in the waste water is carried out recycling and handle energy savings when realizing sustainable development.
Filtering or adsorbing is one of main method of wastewater treatment, accounts for leading role in this membrane separation technique.It is the technology of 21 century that membrane separation technique is described as, and it will cause a revolution at separation field.Along with the aggravation of environmental pollution and the shortage of water resource, people to the cry of the recycle of waste water and advanced treating with require increasingly high.Eighties of last century sixties; Membrane separation technique with the form first Application that replaces second pond in wastewater treatment; And obtained fabulous effect; But be limited to the restriction of membrane preparation technology at that time; Fail to be applied [Smith C V. The Use of Ultra Filtration Membrane for Activated Sludge Separation [A]. Presented Paper of 24th Annual Purdue Industrial Waste Conference [C]. [sl.]: 1969,1300-1310.].Up to the eighties in 20th century, along with the development of membrane preparation technology and process and perfect.Membrane technology is used for wastewater treatment in a variety of forms.
Main melt spinning and the solvent spinning of adopting of traditional high polymer fibre spinning, the diameter of fiber is generally more than tens microns.Yet along with the high speed development of information, biotechnology, the energy, environment, advanced manufacturing technology and national defence, the miniaturization of element, intellectuality, high integrated, high density storage and ultrafast transmission etc. are more and more littler to the dimensional requirement of material.Therefore, the preparation of nano-fiber material plays crucial effects to the future development demand.Electrostatic spinning technique has obtained especially paying attention to because of producing diameter continuously at sub-micron even nano level high polymer fibre in recent years.Because fibre diameter reaches nanoscale, the draw ratio of fiber, the high several magnitude of the relative traditional fibre of specific area.It is big that the nonwoven fabric that electrostatic spinning is processed has specific area, and the characteristics that hole dimension is little are membrane materials, the good substitute of cell tissue supporter and other skin pharmaceutical treatment.
Virtue sulfone synthetic fibre is the new fiber as fire resistant filter material; Because the sulphur atom on the polyarylsulfone (PAS) molecular backbone is in highest oxidation state; Aromatic rings is difficult to oxidation again; Therefore, fragrant sulfone synthetic fibre have that good heat resistance, heat endurance, high temperature dimensional stability, thermal contraction are stable, anti-flammability, electrical insulating property, radiation resistance and chemical stability.Polysulfones is as a kind of functional material, and is cheap and easy to get, has excellent mechanical intensity, the close property of resistance to compression and chemical stability, and can degrade by antibiont, extensively applied to milipore filter and the compound porous support membrane of using.Usually film requires to have high permeation rate and selectivity, can resist chemistry, bacterium and mechanical force destruction and have long service life, low membrane material cost etc.The sustainable development policy that the present invention combines country to carry out; Character requirement around diffusion barrier; Characteristics such as it is big that comprehensive electrostatic spinning prepares the nonwoven fabric specific area, and hole dimension is little and polysulfonamides is high temperature resistant, high strength, characteristics such as corrosion-resistant propose to utilize the method for electrostatic spinning to prepare the imagination of the polysulfonamides diffusion barrier of high adsorption; For the range of application of expanding polysulfonamides fibre has proposed new approaches, there are certain theory researching value and application market to be worth.
Summary of the invention
Order of the present invention is to provide a kind of method of electrostatic spinning to prepare the method for polysulfonamides diffusion barrier.Its concrete preparation method:
A kind of preparation method of polysulfonamides diffusion barrier; The polysulfonamides diffusion barrier adopts the method for electrostatic spinning, and voltage is 20-30kV, and receiving range is 12-18cm; Polysulfonamides spinning solution mass percent is 10-15%, and polysulfonamides solvent that spinning solution adopts is N-N dimethylacetylamide DMAc.
Among the preparation method of above-mentioned polysulfonamides diffusion barrier; Polysulfonamides PSA spinning solution is joined in the syringe, guarantee that spinning head does not have obstruction, will obtain the polysulfonamides nonwoven and be distributed under the 100-140 ℃ of temperature; In vacuum drying chamber, handle 20-30h, obtain polysulfonamides PSA diffusion barrier.
Polysulfonamides diffusion barrier of the present invention is the polysulfonamides solution of 10-15% according to mass percent, processes through electrospinning process.
The present invention optimizes the electrostatic spinning condition through orthogonal test method, comprises the concentration of best spinning solution, best spinning voltage, optimum reception distance.
The present invention characterizes through the absorption property of absorption property test experiments to the polysulfonamides PSA diffusion barrier that makes.
The present invention utilizes electrostatic spinning apparatus to prepare nano level polysulfonamides nonwoven fabric; Has high-specific surface area; The hydrophilic radical of the empty network of internal crosslinking and high pore volume and the intrinsic existence of polysulfonamides, the high adsorption diffusion barrier character of facilitating polysulfonamides PSA has light weight and the intrinsic high strength of polysulfonamides PSA in addition; High temperature resistant, corrosion resistant excellent properties.The present invention has following advantage:
A) film-forming process is simple;
B) the polysulfonamides nonwoven fabric of electrostatic spinning preparation is the diffusion barrier of nanoscale polysulfonamides formation;
C) the diffusion barrier specific area of nanoscale polysulfonamides formation is bigger;
D) diffusion barrier of nanoscale polysulfonamides formation has littler hole dimension;
E) diffusion barrier of nanoscale polysulfonamides formation has higher absorption property;
F) diffusion barrier of nanoscale polysulfonamides formation has high strength, and is high temperature resistant, the resistance to chemical attack characteristic.
Description of drawings
The electrostatic spinning apparatus structural representation of Fig. 1 for using among the present invention.
Among the figure: 1-electrostatic spinning syringe, 2-spinning solution, 3-spinning syringe needle
4-high voltage source, 5-spinning fibre, 6-receiver, 7-nonwoven fabric.
The specific embodiment
The specific embodiment:
Polysulfonamides diffusion barrier of the present invention is 11% polysulfonamides solution according to mass percent, processes through electrospinning process, referring to figure one.Concrete steps are:
A. be solvent with dimethylacetylamide DMAc, the preparation mass percent concentration is the dimethylacetylamide DMAc solution of 11% polysulfonamides PSA, and through magnetic agitation polymer is fully dissolved;
B. polysulfonamides PSA spinning solution is joined in the syringe, guarantee that spinning head does not have obstruction, control spinning voltage 30kV; Receiving range between receiving system and the spinning head is 15cm; Obtain the polysulfonamides nonwoven fabric, and in 120 ℃ of following dry 24h, and obtain polysulfonamides PSA diffusion barrier.
The concrete steps of preparation casting film are: the spinning solution that configures is directly placed on the slide in 120 ℃ of following dry 24h of vacuum tank.
The concrete steps of the adsorptivity of test polysulfonamides diffusion barrier are:
(a) with a certain amount of CrCl of dissolved in distilled water
3, and constant volume obtains the solution of concentration 10mmol/L in the volumetric flask of 25ml;
(b) get polysulfonamides electrostatic spinning diffusion barrier and the casting film of equal in quality 0.1g, place the vial that contains 20mlCrCl3 solution respectively;
(c) vial in (b) being placed temperature is 25 ℃, and frequency is to vibrate 8h in the oscillator under the 80r/min;
(d) (Perkin Elmer, Waltmham USA) analyze Cr in the suspension through inductively coupled plasma emission spectrometer optima-7300DV
3+Concentration, and calculate adsorption capacity through equation.
wherein Qe (mmol/g) is adsorption capacity; Ion concentration when Co and Ce (mmol/L) represent the initial sum balance respectively; V (mL) is a liquor capacity, and m (g) is the quality of dry caudacoria.
1. contrast different adsorbents to Cr
3+Suction-operated
| Adsorbent | m(g) | V(mL) | Co(mmol/L) | Ce(mmol/L) | Qe(mmol/g) |
| Casting film | 0.10 | 20.00 | 10.00 | 9.98 | 4.84 |
| The quiet film that spins | 0.10 | 2000 | 10.00 | 9.95 | 13.06 |
(e) absorption property of contrast electrostatic spinning polysulfonamides diffusion barrier and casting film; As shown in table 1; The quiet polysulfonamides nonwoven fabric that spun improves 2.7 times than the adsorptivity that directly adopts the spinning solution casting film, shows through electrospinning process to prepare high adsorption polysulfonamides diffusion barrier.
Claims (2)
1. an electrostatic spinning prepares the method for polysulfonamides diffusion barrier; It is characterized in that; The polysulfonamides diffusion barrier adopts the method for electrostatic spinning, and voltage is 20-30kV, and receiving range is 12-18cm; Polysulfonamides spinning solution mass percent is 10-15%, and polysulfonamides solvent that spinning solution adopts is N-N dimethylacetylamide DMAc.
2. the method for preparing the polysulfonamides diffusion barrier by the described electrostatic spinning of claim 1; It is characterized in that; Polysulfonamides PSA spinning solution is joined in the syringe, guarantee that spinning head does not have obstruction, will obtain the polysulfonamides nonwoven and be distributed under the 100-140 ℃ of temperature; In vacuum drying chamber, handle 20-30h, obtain polysulfonamides PSA diffusion barrier.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103184581A (en) * | 2013-03-21 | 2013-07-03 | 上海工程技术大学 | Method for preparing polysulfonamide/nanometer TiO2 composition fiber by electrostatic spinning method |
| CN107354589A (en) * | 2017-09-13 | 2017-11-17 | 哈尔滨工业大学 | A kind of wear-resisting, high temperature resistant porous fiber film preparation method |
| CN107675361A (en) * | 2017-10-12 | 2018-02-09 | 上海工程技术大学 | A kind of Static Spinning nano-composite fiber felt and its preparation method and application |
| CN109355803A (en) * | 2018-11-30 | 2019-02-19 | 中科院广州化学有限公司 | A kind of preparation method coating polysulfide Electrospun nano-fibers film and its application in the case where aoxidizing stimuli responsive in adsorbing metal ions |
| CN111249926A (en) * | 2020-02-24 | 2020-06-09 | 上海工程技术大学 | Meta-aramid/polysulfonamide nano composite air filter membrane and preparation method thereof |
Citations (3)
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| CN1063425A (en) * | 1992-01-17 | 1992-08-12 | 厦门大学 | The facture of high-efficient diffusion barrier |
| CN1935340A (en) * | 2006-09-04 | 2007-03-28 | 哈尔滨工业大学 | Polysulfone amide separating membrane and its modifying method utilizing nanotitanium dioxide |
| CN101390814A (en) * | 2008-10-29 | 2009-03-25 | 东南大学 | Beauty mask based on electro spinning nano fiber |
-
2011
- 2011-11-16 CN CN2011103615080A patent/CN102505351A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1063425A (en) * | 1992-01-17 | 1992-08-12 | 厦门大学 | The facture of high-efficient diffusion barrier |
| CN1935340A (en) * | 2006-09-04 | 2007-03-28 | 哈尔滨工业大学 | Polysulfone amide separating membrane and its modifying method utilizing nanotitanium dioxide |
| CN101390814A (en) * | 2008-10-29 | 2009-03-25 | 东南大学 | Beauty mask based on electro spinning nano fiber |
Non-Patent Citations (1)
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| 李开霞等: "聚苯砜对苯二甲酰胺_苝系荧光材料复合静电纺膜的制备与表征", 《合成技术及应用》, vol. 25, no. 4, 31 December 2010 (2010-12-31), pages 5 - 9 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103184581A (en) * | 2013-03-21 | 2013-07-03 | 上海工程技术大学 | Method for preparing polysulfonamide/nanometer TiO2 composition fiber by electrostatic spinning method |
| CN107354589A (en) * | 2017-09-13 | 2017-11-17 | 哈尔滨工业大学 | A kind of wear-resisting, high temperature resistant porous fiber film preparation method |
| CN107675361A (en) * | 2017-10-12 | 2018-02-09 | 上海工程技术大学 | A kind of Static Spinning nano-composite fiber felt and its preparation method and application |
| CN107675361B (en) * | 2017-10-12 | 2019-05-10 | 上海工程技术大学 | A kind of Static Spinning nano-composite fiber felt and its preparation method and application |
| CN109355803A (en) * | 2018-11-30 | 2019-02-19 | 中科院广州化学有限公司 | A kind of preparation method coating polysulfide Electrospun nano-fibers film and its application in the case where aoxidizing stimuli responsive in adsorbing metal ions |
| CN111249926A (en) * | 2020-02-24 | 2020-06-09 | 上海工程技术大学 | Meta-aramid/polysulfonamide nano composite air filter membrane and preparation method thereof |
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Application publication date: 20120620 |