CN108311119A - Styrene base resin micro nanometer fiber felt of adsorbable polycyclic aromatic hydrocarbon and preparation method thereof - Google Patents
Styrene base resin micro nanometer fiber felt of adsorbable polycyclic aromatic hydrocarbon and preparation method thereof Download PDFInfo
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- CN108311119A CN108311119A CN201810022706.6A CN201810022706A CN108311119A CN 108311119 A CN108311119 A CN 108311119A CN 201810022706 A CN201810022706 A CN 201810022706A CN 108311119 A CN108311119 A CN 108311119A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
- B01J20/261—Synthetic macromolecular compounds obtained by reactions only involving carbon to carbon unsaturated bonds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
- B01J20/264—Synthetic macromolecular compounds derived from different types of monomers, e.g. linear or branched copolymers, block copolymers, graft copolymers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28023—Fibres or filaments
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28033—Membrane, sheet, cloth, pad, lamellar or mat
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4806—Sorbents characterised by the starting material used for their preparation the starting material being of inorganic character
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/32—Hydrocarbons, e.g. oil
- C02F2101/327—Polyaromatic Hydrocarbons [PAH's]
Abstract
The invention belongs to technical field of polymer materials, styrene base resin micro nanometer fiber porous material of specially adsorbable polycyclic aromatic hydrocarbon and preparation method thereof.The present invention uses the micro-nano layer co-extrusion device being made of molds such as two extruders, two Melt Pumps, styrene base resin and interlayer fluoropolymer resin are subjected to melting extrusion by two extruders respectively and prepare two kinds of polymer resin alternating layer structure fiber, isolated polymer resin is removed again and obtains micron to nano grade styrene-based polymer fiber, and then deposition prepares the styrene base resin micro nanometer fiber felt with porous structure on filter membrane.Specific surface area, pore structure and the fibrofelt thickness of the micro nanometer fiber felt can be controlled by number, pulling speed, micro nanometer fiber dosage of layering superpositing unit in preparation process etc..The present invention is simple and easy to do, of low cost, can be mass-produced, and solvent-free pollution can be applied to the water pollutions process field such as polycyclic aromatic hydrocarbon in adsorbed water body.
Description
Technical field
The invention belongs to technical field of polymer materials, and in particular to a kind of styrene base resin of adsorbable polycyclic aromatic hydrocarbon
Micro nanometer fiber felt（Porous material）And preparation method thereof.
Background technology
Micro nanometer fiber by the flexibility of its high specific surface area, surface modification and other better than Traditional bulk material
Performance is widely applied in fields such as organizational project, biological medicine, environmental protections, and the technology of preparing of micro nanometer fiber
Also further exploitation and innovation have been obtained.Up to the present, the conventional method for preparing micro nanometer fiber includes mainly chemical method, phase
Partition method, self-assembly method and spinning processing method etc..And spinning processing method includes mainly method of electrostatic spinning, bi-component composite spinning
Method, meltblown and flash-spinning method etc..Wherein method of electrostatic spinning is the most commonly used method for preparing polymer micro-nanometer fiber
One of.However method of electrostatic spinning prepares micro nanometer fiber of high cost, low output, is difficult to mass produce, and experimentation needs
A large amount of organic solvents are used, environmental pollution is caused.And it is simple and feasible to prepare micro nanometer fiber using micro-nano layer coetrusion, spirit
It is living convenient, it is of low cost, can it is continuous, produce in enormous quantities, solvent-free pollution；And the micro nanometer fiber size uniform prepared can
Control, range are wide, and the fluoropolymer resin that micro nanometer fiber is prepared for can not find the methods of solvent progress electrostatic spinning is more to provide
A kind of simple and direct efficient method, and the mechanical property of micro nanometer fiber can also be significantly improved in conjunction with uniaxial stretch process
（J.F. Cheng, H.T. Pu, J. Du, A Processing Method with High Efficiency for Low
Density Polyethylene Nanofibers Reinforced by Aligned Carbon Nanotubes via
Nanolayer Coextrusion, Polymer, 2017, 111: 222-228）.
It is relied on by the porous material that polymer micro-nanometer fiber of the diameter in nanometer to sub-micrometer range is prepared
Compared to the clear superiority of traditional sorbing material, including big specific surface area, abundant pore structure and surface-functionalized spirit
Activity has wide practical use in terms of environmental protection（Huang Z.M., Zhang Y.Z., Kotaki M., et al.
Composites Science and Technology. 2003, 63(15): 2223–2253）.For example, micro nanometer fiber
Film successfully develops into fine air filter, can effectively remove（About 100% removal rate）Diameter 1 and 5 μm it
Between airborne particulate (Kattamuri N, Shin J H, Kang B, Lee C G, Lee J K, Sung C.
Development and surface characterization of positively charged filters[J].
Jourinal of Material Science, 2005, 40: 4531-4539).In addition it is made there are many different polymer
Micro nanometer fiber film be used to be effectively removed heavy metal ion and organic compound pollutant in water, such as phenolphthalein and oil.
Have the result shows that, the polymer such as styrol copolymer, nylon 6 prepare micro nanometer fiber porous material can directly be extracted from water
The organic pollution of trace has the ability of significant enrichment organic pollution in water.In addition, with other powder or particle
Adsorbent is compared, and membranaceous and felted adsorbent can be used directly, and separation (the Qi D from solution system are easy after absorption
J, Kang X J, Chen L Q, Zhang Y Y, Wei H M, Gu Z Z. Electrospun polymer
nanofibers as a solid-phase extraction sorbent for the determination of trace
pollutants in environmental water[J]. Analytical and Bioanalytical Chemistry,
2008, 390: 929-938).However it is few at present more about using polymer micro-nanometer fiber porous material to handle water body
The research of cyclophane hydrocarbon pollutant is reported.
Polycyclic aromatic hydrocarbon（PAHs）By a kind of chemical combination being made of two or more fused aromatic phenyl ring with lipophilic property
Object has relatively high desorption activation energy.Chemical constitution due to its stabilization and low bioavailability, polycyclic aromatic hydrocarbon can be with
Long-term existence in the environment.It is mainly derived from forest fire, Grass fires and human activity（Such as military operation, vehicle row
It puts, agricultural production, house trash burning, combustion of fossil fuel, petroleum industry leakage, the life of carbon black, coal tar asphalt and pitch
Production, heat supply, power generation and engine exhaust etc.）.Polycyclic aromatic hydrocarbon is widely present in air, in soils and sediments and water body,
Although the solubility of PAHs in water is very low（Such as pyrene is 140 ppb）, but its toxicity is very high.Since it is with superpower
Carcinogenicity constitutes great threat to environment and human health.Therefore people be dedicated to research find effective method to
The polycyclic aromatic hydrocarbon in soil and water is handled, is endangered caused by environment and human health to reduce polycyclic aromatic hydrocarbon.Existing side
Method is mainly the following：Ozonation, photocatalytic method, biological degradation method and absorption method, wherein biological degradation method when
Between it is very long, oxidizing process causes secondary pollution carrying out the while of being largely chemically treated.Importantly, these methods all without
Method removes ppb grades of Determination of Trace Polycyclic Aromatic Hydrocarbons pollutant（Mahanty B., Pakshirajan K., Dasu V. V.,
Critical Reviews in Environmental Science and Technology 2011, 41 (19), 1697-
1746）.
It is that process that is a kind of fruitful and being widely used is simple, cost with sorbing material processing polycyclic aromatic hydrocarbon pollutant
Cheap method.Ideal adsorbent should have strong adsorption capacity and be easily separated.And when adsorbent cost is relatively low and can
When with mass production, rule more attractive is adsorbed.Current several primary sorbents include activated carbon, carbon nanomaterial and swelling
Soil etc..And these adsorbents are existed in the form of powder or particle mostly, it is difficult to cycling and reutilization and be possible to ring
Secondary pollution is caused in border, and manufacturing cost is higher, thus the reality for limiting absorption method processing water body polycyclic aromatic hydrocarbon pollution is answered
With (Lamichhane S, Bal Krishna K C, Ssrukkalige R. Polycyclic aromatic
hydrocarbons (PAHs) removal by sorption: A review[J]. Chemosphere, 2016, 148:
336-353).According to similar compatibility principle, the adsorbent with aromatic ring is suitable for the absorption of polycyclic aromatic hydrocarbon.Therefore pass through micro-nano layer
Coetrusion prepares styrene base resin micro nanometer fiber porous adsorbing material, the polycyclic aromatic hydrocarbon being expected to be used in adsorbed water body,
Not only cost is relatively low, can produce in enormous quantities, and micro nanometer fiber felt has the specific surface area of bigger compared to bulk material,
And be then easy to separate and recover from water body compared to powdered and granular material, the secondary pollution of water body will not be caused.
Invention content
The purpose of the present invention is to provide a kind of felt thickness uniform, controllable, large specific surface area can be adsorbed quickly and efficiently
Polycyclic aromatic hydrocarbon will not cause environment on styrene base resin micro nanometer fiber felt of secondary pollution and preparation method thereof.
The styrene base resin micro nanometer fiber felt of adsorbable polycyclic aromatic hydrocarbon proposed by the present invention（Porous material）Preparation
Method, the specific steps are：
（One）First, it is cut using by two extruders, two Melt Pumps, coextrusion junction station and layering superpositing unit, fiber
Micro-nano layer co-extrusion device (Pu letter spit of fland, An Peng, Wei Yanli, Du Jiang, a kind of preparation of polymer micro-nanometer fiber of mold composition
Method, Chinese invention patent on April 23rd, 2015101959284,2015), by styrene base resin with as the poly- of separate layer
Polymer resin carries out melting extrusion by two extruders respectively, prepares two kinds of polymer resin alternating layer structure fiber；
（Two）Then, the isolated polymer resin in alternating layer structure fiber is dissolved, the micron to nano grade of size uniform is obtained
Styrene-based polymer fiber；
（Three）Then, deposition prepares the styrene base resin micro nanometer fiber felt with porous structure on filter membrane；
Specific surface area, pore structure and the fibrofelt thickness of styrene base resin micro nanometer fiber felt can be by points in preparation process
The conditions such as number, pulling speed, micro nanometer fiber dosage of layer superpositing unit control.
Raw material components in the micro-nano layer coextrusion method are calculated as with mass number：
100 parts of styrene-based polymer resin,
50-200 parts of isolated polymer resin.
In the present invention, the styrene-based polymer resin uses the thermoplastic styrene base of any suitable melt-processed
Polymer, specific optional self-polystyrene, styrene-acrylonitrile copolymer, acrylonitrile-butadiene-styrene copolymer and poly-
Styrene（Fe3O4）It is any in compound resin, but it is not limited only to this.
In the present invention, the separation resin is the thermoplastic, polymeric materials of any suitable melt-processed, and with benzene second
Alkenyl polymer resin is compared, in water or organic solvent have entirely different dissolubility, specifically can be selected from polyethylene glycol oxide,
It is any in polymethyl methacrylate, polyethylene glycol and polyvinyl alcohol.
In the present invention, the extruder melting extrusion styrene-based polymer resin and each section of processing temperature for separating resin
Degree is arranged according to the conventional extrusion processing temperature of each section condition of corresponding resin.
In the present invention, the coextrusion junction station is a kind of dual channel mold, connects two extruders and can collect folded
It adds into layering superpositing unit, which carries heating device.
In the present invention, the layering superpositing unit is a kind of double torsion runner molds, and with heating device, using a system
Row delaminating units connect to adjust thickness in monolayer in fiber, to obtain 2n+1The structure of alternating layer, cuts using fiber die
Alternating layer structure fiber is obtained, and by the stretching of roller wrap-up, prepares the controllable fiber of size uniform.Delaminating units
Number can theoretically increase always, in practical operation, take 2-12.
In the present invention, the coextrusion junction station and the temperature setting for being layered superpositing unit use styrene-based polymer
Resin and separates the higher person of resin extruded machine die temperature or float according to this temperature or float downward 10-20 DEG C.
In the present invention, the alternating layer structure fiber can realize that fiber microlayer thickness is distributed by adjusting screw rod rotating speed,
To volume ratio of the two kinds of materials of control in alternating layer structure.
In the present invention, the alternating layer structure fiber can stretch fiber by adjusting the rotating speed of roller collection device
Adjust the size of fiber.
In the present invention, the method that the isolated polymer resin by alternating layer structure is separated is to utilize benzene
Isolated polymer is dissolved and is protected by vinylite and isolated polymer the resin deliquescent difference in water or organic solvent
Styrene base resin is stayed, fiber shape is obtained.
In the present invention, the styrene-based polymer resin micro nanometer fiber size is 50nm-50 μm.
In the present invention, the thickness adjustable extent of the styrene-based polymer resin micro nanometer fiber felt is
1mm-3mm。
In the present invention, the filter membrane for preparing styrene base resin micro nanometer fiber felt is copper filter membrane or stainless steel
Matter filter membrane.
A kind of preparation method of the styrene base resin micro nanometer fiber felt of adsorbable polycyclic aromatic hydrocarbon proposed by the present invention, tool
Body operating procedure is：
The first step：Prepare two kinds of polymer resin alternating layer structure fiber operating process be：
Styrene base resin and isolated polymer resin are subjected to melting extrusion by two extruders respectively, then by fused materials
It is delivered to junction station, and is converged herein, by being overlapped the principle of cutting with layering superpositing unit, in delaminating process middle level
The vertical cutting of structure experience is divided into two streams, expands horizontally and reconsolidate, to make the quantity of layer double, it is evident that pass through n
A layering superpositing unit will form 2n+1Coextruded layer, and obtain thickness in monolayer micro-nano by fiber die cutting and wrap-up
The styrene base resin and isolated polymer resin alternating layer structure fiber of meter level；Wherein, can be turned by adjusting extruder screw
Speed come obtain different volumes than alternating layer fiber.
Second step：The operating process of isolated polymer resin in fiber spin-off alternating layer structure fiber is：
There are two types of methods for stripping：
（1）Obtained fluoropolymer resin alternating structure fiber is subjected to high-speed stirred, rotating speed 800-1000r/min, and ultrasound
Dispersion for 24 hours, to which water-insoluble separation resin is carried out selective dissolution separation with organic solvent, or is divided water solubility with water
Separated and dissolved is carried out every resin, obtains the controllable micro/nano level styrene base resin fiber of size uniform.
（2）Obtained fluoropolymer resin alternating structure fiber is rinsed with giant, pressure 5-10MPa, the time
20-40min obtains the controllable micro/nano level styrene base resin fiber of size uniform to detach water-soluble resin.
Third walks：Deposition prepares the operation stream of the styrene base resin micro nanometer fiber felt with porous structure on filter membrane
Cheng Wei：
The styrene base resin fiber obtained after separation process removes separate layer resin is sunk by mass range 0.5g-20g
Product is different from 40-80 DEG C of dry 24-48h on filter membrane, by solvent for use when separation, obtains thickness range as 1mm-3mm's
Styrene base resin micro nanometer fiber felt.
Fibrofelt obtained by the present invention, polycyclic aromatic hydrocarbon pollutant in can be used for removing water, specifically obtained fibre
It ties up felt to immerse in the aqueous solution containing polycyclic aromatic hydrocarbon, you can remove polycyclic aromatic hydrocarbon pollutant in water removal.
In the present invention, the concentration range of the polycyclic aromatic hydrocarbon aqueous solution is 30ppb-130ppb.
In the present invention, the polycyclic aromatic hydrocarbon be it is water-soluble in 2-5 ring polycyclic aromatic hydrocarbons, specific fluorenes, phenanthrene, anthracene, pyrene, benzene
And it is any in anthracene or BaP etc., but it is not limited only to this.
In the present invention, the styrene base resin micro nanometer fiber felt removes the Longer absorption times of polycyclic aromatic hydrocarbon in water removal
For 24 hours for 0.1-.It is preferred that 1-24 hours.
It is initial that the styrene base resin micro nanometer fiber felt that specific desirable mass range is 0mg-240mg is added to 100mL
In the polycyclic aromatic hydrocarbon aqueous solution of a concentration of 30ppb-130ppb, magnetic agitation 0-24h, timing sampling detection.
This kind of styrene base resin micro nanometer fiber felt thickness uniform, controllable prepared by the present invention has larger specific surface
Product, has stronger adsorption capacity to polyaromatic hydrocarbon pollutant, is easily recycled, will not cause secondary pollution to environment,
Water process sorbing material is can be used as, has good application prospect in environmental area.The present invention is simple and practicable, cost is relatively low, can
Continuously and produce in enormous quantities, to realize industrialization.
Description of the drawings
Fig. 1 is that micro-nano layer coetrusion prepares polystyrene micro nanometer fiber schematic diagram.
Fig. 2 is the infrared spectrogram of polystyrene micro nanometer fiber.
Fig. 3 is the stereoscan photograph of polystyrene micro nanometer fiber（A, the layering superpositing unit number of c, e, g are respectively
2、5、7、9）With size distribution plot.
Fig. 4 is the digital photograph of polystyrene micro nanometer fiber felt.
Fig. 5 be the layering superpositing unit number that mass concentration is 1g/L be 9 polystyrene micro nanometer fiber felt to initial dense
Degree is the adsorption dynamics adsorption kinetics line chart of the aqueous solution of the pyrene of 130ppb.
Fig. 6 is eliminating rate of absorption-adsorbate of the pyrene after different quality concentration polystyrene micro nanometer fiber felt adsorbs for 24 hours
Mass concentration line chart.
Fig. 7 is the polystyrene micro nanometer fiber that the layering superpositing unit number that mass concentration is 1g/L is respectively 2,5,7,9
Adsorption dynamics adsorption kinetics line chart of the felt to the aqueous solution for the pyrene that initial concentration is 130ppb.
Fig. 8 be the layering superpositing unit number that mass concentration is 1g/L be 9 polystyrene micro nanometer fiber felt to initial dense
Degree is respectively the adsorption dynamics adsorption kinetics line chart of the aqueous solution of the pyrene of 35,50,70,100,130ppb.
Specific implementation mode
Following embodiment, which is merely, further illustrates the present invention, under the purport for not violating the present invention, the present invention
It should be not limited to the content that following experimental example is specifically expressed.
It is raw materials used as follows：
PS（PG-33）, Zhenjiang Qi Mei Chemical Co., Ltd.s
PEO（1500000 molecular weight）Shanghai Chemical Co., Ltd. of federation, DOW Chemical（POLYOX WSR N80）
Fe3O4（98%）, ALADDIN
ABS（PA-707K）, Zhenjiang Qi Mei Chemical Co., Ltd.s
SAN（PN-118）, Zhenjiang Qi Mei Chemical Co., Ltd.s
Pyrene（98%）, ACROS.
Embodiment 1
The micro-nano layer co-extrusion equipment shown in Fig. 1 prepares polystyrene micro nanometer fiber.By polystyrene resin PS and separate poly-
Polymer resin PEO is added separately in two extruders, for be added PS extruder, each area's temperature be followed successively by 130 DEG C,
160 DEG C, 190 DEG C, screw speed 10r/min；For be added PEO extruder, each area's temperature be followed successively by 60 DEG C, 120 DEG C,
180 DEG C, screw speed 10r/min；Junction station and layering superpositing unit cutting module are 200 DEG C, die temperature 190-200
DEG C, setting cutting module has 2,5,7,9 superpositing units, to obtain 24,26,28,210 alternating layer structure.And
It is wound with wrap-up, to obtain 8 layers, 64 layers, 256 layers, 1024 layers of alternating structure fiber.
Obtained PS and PEO alternating structures fiber are subjected to high-speed stirred in water and ultrasonic disperse or use giant
It rinses, to detach PEO resins, obtains the controllable micron to nano grade PS fibers of size uniform, PS obtained is micro-nano
Fiber carries out infrared analysis by EQUINOXSS/HYPERION2000 spectrometer, and Fig. 2 infrared detections show to make
The PS micro nanometer fibers obtained do not have absorption peak near 1100cm-1, and the PEO in composite fibre has been completely removed.
Obtained PS micro nanometer fibers are subjected to morphology observation and dimension analysis, Fig. 3 by 250 FEG SEM of QUANTA
(a) (b) the result shows that when superpositing unit number is 2, the fiber size that micro-nano layer coextrusion technology obtains is evenly distributed, average
Size is 55 μm.Fig. 3 (c) (d) is the result shows that when superpositing unit number is 5, fiber ruler that micro-nano layer coextrusion technology obtains
Very little to be evenly distributed, average-size is 6 μm.For Fig. 3 (e) (f) the result shows that when superpositing unit number is 7, micro-nano layer is coextruded skill
The fiber size that art obtains is evenly distributed, and average-size is 2 μm.Fig. 3 (g) (h) scanning electron microscope testing result shows single in superposition
When first number is 9, the fiber size that micro-nano layer coextrusion technology obtains is evenly distributed, average-size 200nm.
Isolated PS micro nanometer fibers are dried into 1- on filter membrane according to the difference of separation solvent used at 40-80 DEG C
It is uniform to obtain thickness by 48h（1mm）Polystyrene micro nanometer fiber felt, as shown in Figure 4.
Embodiment 2
By polystyrene resin and magnetic iron oxide（Fe3O4）It is blended by different ratio with mixer, obtains compound resin.With micro-
A layer co-extrusion equipment of receiving prepares compound resin micro nanometer fiber.By compound resin PS（Fe3O4）With isolated polymer resin PEO points
It is not added in two extruders, for PS is added（Fe3O4）Extruder, each area's temperature be followed successively by 120 DEG C, 170 DEG C, 200
DEG C, screw speed 10r/min；For the extruder of PEO is added, each area's temperature is followed successively by 60 DEG C, 120 DEG C, 180 DEG C, spiral shell
Bar rotating speed is 10r/min；Junction station and layering superpositing unit cutting module are 200 DEG C, and die temperature is 190-200 DEG C, setting
Cutting module has 2,5,7,9 superpositing units, to obtain 24,26,28,210 alternating layer structure.It is used in combination winding to fill
It sets and is wound, to obtain 8 layers, 64 layers, 256 layers, 1024 layers of alternating structure fiber.The PS that will be obtained（Fe3O4）It is handed over PEO
It rinses for structural fibers progress high-speed stirred and ultrasonic disperse or with giant, to be detached to PEO resins, obtains
The controllable micron to nano grade PS of size uniform（Fe3O4）Fiber.By isolated PS（Fe3O4）Micro nanometer fiber is used in
The difference of separation solvent dry 1-48h at 40-80 DEG C on filter membrane, it is uniform to obtain thickness（1mm）Polystyrene-four aoxidize
Three ferromagnetism micro nanometer fiber felts.
Characterizing method and result are similar to Example 1.
Embodiment 3
Styrene terpolymer resin is prepared with micro-nano layer co-extrusion equipment（ABS）Micro nanometer fiber.Styryl is polymerize
Resin ABS and isolated polymer resin PEO are added separately in two extruders, for the extruder of ABS, Qi Gequ is added
Temperature is followed successively by 150 DEG C, 180 DEG C, 220 DEG C, screw speed 10r/min；For the extruder of PEO, each area's temperature is added
60 DEG C, 120 DEG C, 180 DEG C are followed successively by, screw speed 10r/min；Junction station and layering superpositing unit cutting module are 220 DEG C,
Die temperature is 210-220 DEG C, and setting cutting module has 2,5,7,9 superpositing units, to obtain 24,26,28,
210 alternating layer structure.It is used in combination wrap-up to be wound, to obtain 8 layers, 64 layers, 256 layers, 1024 layers of alternating structure fibre
Dimension.It is rinsed by obtained ABS and PEO alternating structure fibers progress high-speed stirred and ultrasonic disperse or with giant, to
PEO resins are detached, the controllable micron to nano grade ABS fibers of size uniform are obtained.By the micro-nano fibres of isolated ABS
Dimension dry 1-48h at 40-80 DEG C on filter membrane according to the difference of separation solvent used, it is uniform to obtain thickness（1mm）Benzene second
Alkene terpolymer micro nanometer fiber felt.
Characterizing method and result are similar to Example 1.
Embodiment 4
Styrene binary copolymer resin is prepared with micro-nano layer coextrusion technology（SAN）Micro nanometer fiber.Styryl is polymerize
Resin SAM and isolated polymer resin PEO are added separately in two extruders, for the extruder of SAN, Qi Gequ is added
Temperature is followed successively by 150 DEG C, 180 DEG C, 220 DEG C, screw speed 10r/min；For the extruder of PEO, each area's temperature is added
60 DEG C, 120 DEG C, 180 DEG C are followed successively by, screw speed 10r/min；Junction station and layering superpositing unit cutting module are 220 DEG C,
Die temperature is 210-220 DEG C, and setting cutting module has 2,5,7,9 superpositing units, to obtain 24,26,28,
210 alternating layer structure.It is used in combination wrap-up to be wound, to obtain 8 layers, 64 layers, 256 layers, 1024 layers of alternating structure fibre
Dimension.It is rinsed by obtained SAN and PEO alternating structure fibers progress high-speed stirred and ultrasonic disperse or with giant, to
PEO resins are detached, the controllable micron to nano grade SAN fibers of size uniform are obtained.By the micro-nano fibres of isolated SAN
Dimension dry 1-48h at 40-80 DEG C on filter membrane according to the difference of separation solvent used, it is uniform to obtain thickness（1mm）Benzene second
Alkene bipolymer micro nanometer fiber felt.
Characterizing method and result are similar to Example 1.
Embodiment 5
Polystyrene micro nanometer fiber felt is tested with Fluorescence Spectrometer（It is 9 to be layered superpositing unit number）Absorption to polycyclic aromatic hydrocarbon pyrene
Performance measures equilibrium adsorption time and the rate of adsorption.First configuration concentration be respectively 130,65,32.5,16.25,8.125ppb
Pyrene each 10ml of aqueous solution, with Fluorescence Spectrometer measure 372nm at fluorescence intensity, drawing curve.Then it configures dense
Degree is the aqueous solution 100ml of the pyrene of 130ppb, takes 0.1g polystyrene micro nanometer fiber felts, immerses the aqueous solution of the pyrene configured
In, magnetic agitation takes the supernatant liquor 3mL of the aqueous solution of pyrene to be detected with Fluorescence Spectrometer glimmering at 372nm at regular intervals
Luminous intensity obtains the polystyrene micro nanometer fiber felt that layering superpositing unit number that mass concentration as shown in Figure 5 is 1g/L is 9
To the adsorption dynamics adsorption kinetics line chart of the aqueous solution for the pyrene that initial concentration is 130ppb.As shown in figure 5, prolonging with adsorption time
Long, the absorption of polystyrene micro nanometer fiber felt can be divided into three phases：It it is the quick adsorption stage from 0 to 40min, pyrene is through micro-
Residual concentration after nanofiber mats absorption accounts for the 52% of original concentration.；40min-90min, the rate of adsorption is slack-off, when 90min,
Residual concentration of the pyrene after the absorption of micro nanometer fiber felt accounts for the 35% of original concentration；After 90min, absorption tends to balance.
Embodiment 6
Different quality concentration polystyrene micro nanometer fiber felt is tested with Fluorescence Spectrometer（It is 9 to be layered superpositing unit number）To polycyclic
The absorption property of aromatic hydrocarbons pyrene probes into adsorbate equilibrium adsorption mass concentration and equilibrium adsorption removal rate.Configuration concentration is distinguished first
For each 10ml of aqueous solution of the pyrene of 130,65,32.5,16.25,8.125ppb, the fluorescence at 372nm is measured with Fluorescence Spectrometer
Intensity, drawing curve.Then configuration concentration is the aqueous solution 1000mL of the pyrene of 130ppb, and the unique variable of contrived experiment is
The quality of polystyrene micro nanometer fiber felt, weigh quality be respectively 20,40,60,80,100,120,140,160,180,
The polystyrene micro nanometer fiber felt of 220mg immerses the aqueous solution of the pyrene of 10 parts 100mL/ parts of the 130ppb configured respectively
In；Magnetic agitation for 24 hours, takes the supernatant liquor 3mL of the aqueous solution of 10 parts of pyrenes to carry out fluorescence spectrum detection, obtains as shown in FIG. 6
Eliminating rate of absorption-adsorbate mass concentration broken line of pyrene after the absorption for 24 hours of different quality concentration polystyrene micro nanometer fiber felt
Figure.As shown in fig. 6, with the increase of polystyrene micro nanometer fiber felt mass concentration, the eliminating rate of absorption of pyrene rises therewith；When
After the quality of adsorbate reaches 1.4g/L, the trend of rising slows down, and absorption has basically reached balance, so equilibrium adsorption matter quality
A concentration of 1.4g/L.It, can be with to the absorption of pyrene as shown in fig. 6, with the increase of polystyrene micro nanometer fiber felt mass concentration
It is divided into three phases：Quickly improve the stage, when the mass concentration of adsorbate increases to 0.6g/L from 0.2g/L, adsorption effect with
The raising of mass concentration and quickly improve；It tends towards stability the stage, during quality rises to 1.4g/L from 0.6g/L, absorption
The trend that effect improves slows down relatively；It tends to balance the stage, after the quality of adsorbate reaches 1.4g/L, eliminating rate of absorption is basic
Maintain an equal level, absorption reaches equilibrium stage, and it is 95.70% to be balanced eliminating rate of absorption.
Embodiment 7
Suction of the polystyrene micro nanometer fiber felt of different layering superpositing unit numbers to polycyclic aromatic hydrocarbon pyrene is tested with Fluorescence Spectrometer
Attached performance probes into influence of the fibre diameter to absorption property.First configuration concentration be respectively 130,65,32.5,16.25,
Each 10ml of aqueous solution of the pyrene of 8.125ppb measures the fluorescence intensity at 372nm, drawing curve with Fluorescence Spectrometer.So
Configuration concentration is the aqueous solution 400mL of the pyrene of 130ppb afterwards, and the unique variable of contrived experiment is to prepare the micro-nano fibre of polystyrene
The layering superpositing unit number used is tieed up, the different coextrusion numbers of plies are weighed（8 layers, 64 layers, 256 layers, 1024 layers）Polystyrene is micro-
Each 100mg of nanofiber mats, immerses the aqueous solution of the pyrene of the 130ppb of 100mL configured respectively, magnetic agitation for 24 hours, every
The aqueous solution supernatant liquor that a period of time takes out each number of plies 3mL pyrenes carries out Fluorescence Spectrometer detection, obtains as shown in Figure 7
The polystyrene micro nanometer fiber felt that the layering superpositing unit number that mass concentration is 1g/L is respectively 2,5,7,9 is to initial concentration
The adsorption dynamics adsorption kinetics line chart of the aqueous solution of the pyrene of 130ppb.As shown in Figure 7, as layering superpositing unit number increases, fiber
The number of plies increases, and polystyrene micro nanometer fiber felt improves the adsorption effect of pyrene in aqueous solution；When the fiber number of plies is 1024 layers,
Tunica fibrosa is best to the adsorption effect of pyrene in water, this is because the fiber number of plies is big, fibre diameter is small, micro nanometer fiber felt specific surface
Product is big, and adsorption effect is good.
Embodiment 8
Absorption with Fluorescence Spectrometer test polystyrene micro nanometer fiber felt to the aqueous solution of the pyrene of different initial concentrations, is probed into
Influence of the initial concentration of the aqueous solution of pyrene to absorption property.First configuration concentration be respectively 130,65,32.5,16.25,
Each 10ml of aqueous solution of the pyrene of 8.125ppb measures the fluorescence intensity at 372nm, drawing curve with Fluorescence Spectrometer.So
Configuration concentration is respectively each 100mL of aqueous solution of the pyrene of 130,100,70,50,35ppb afterwards, and it is 1024 layers to weigh the coextrusion number of plies
Polystyrene micro nanometer fiber felt 100mg x 4, immerse the aqueous solution of the pyrene of 100mL configured, magnetic agitation respectively
For 24 hours, the aqueous solution supernatant liquor for taking out 3mL pyrenes at regular intervals carries out Fluorescence Spectrometer detection, obtains matter as shown in Figure 8
The polystyrene micro nanometer fiber felt that the layering superpositing unit number for measuring a concentration of 1g/L is 9 is respectively 35 to initial concentration, 50,
70, the adsorption dynamics adsorption kinetics line chart of the aqueous solution of the pyrene of 100,130ppb.As shown in Figure 8, polystyrene micro nanometer fiber felt pair
The aqueous solution of the pyrene of different initial concentrations has preferable absorption property, the suction to the aqueous solution for the pyrene that initial concentration is 50ppb
Attached effect is best.
Claims (19)
1. a kind of preparation method of the styrene base resin micro nanometer fiber felt of adsorbable polycyclic aromatic hydrocarbon, which is characterized in that specific
Steps are as follows：
（One）First, it is cut using by two extruders, two Melt Pumps, coextrusion junction station and layering superpositing unit, fiber
Styrene base resin and the fluoropolymer resin as separate layer are passed through two by the micro-nano layer co-extrusion device of mold composition respectively
Extruder carries out melting extrusion, prepares two kinds of polymer resin alternating layer structure fiber；
（Two）Then, the isolated polymer resin in alternating layer structure fiber is removed, the micron to nano grade of size uniform is obtained
Styrene-based polymer fiber；
（Three）Then, deposition prepares the styrene base resin micro nanometer fiber felt with porous structure on filter membrane；
Specific surface area, pore structure and the fibrofelt thickness of styrene base resin micro nanometer fiber felt can be by points in preparation process
The conditions such as number, pulling speed, micro nanometer fiber dosage of layer superpositing unit control；
Wherein, raw material components are calculated as with mass number：
100 parts of styrene-based polymer resin,
50-200 parts of isolated polymer resin.
2. preparation method according to claim 1, which is characterized in that the styrene-based polymer resin is using any
It is suitble to the thermoplastic styrene based polyalcohol of melt-processed, the separation resin is the thermoplastic poly of any suitable melt-processed
Object material is closed, and compared with styrene-based polymer resin, there is entirely different dissolubility in water or organic solvent.
3. preparation method according to claim 2, which is characterized in that the styrene-based polymer resin is selected from polyphenyl
It is any in ethylene, styrene-acrylonitrile copolymer, acrylonitrile-butadiene-styrene copolymer and polystyrene compound resin
Kind；The separation resin is any in polyethylene oxide, polymethyl methacrylate, polyethylene glycol and polyvinyl alcohol.
4. preparation method according to claim 1, which is characterized in that the extruder melting extrusion styryl polymerization
Resin and each section of processing temperature for separating resin are arranged according to the conventional extrusion processing temperature of each section condition of corresponding resin.
5. preparation method according to claim 1, which is characterized in that the coextrusion junction station is a kind of dual channel mould
Tool connects two extruders and can collect superposition into layering superpositing unit, which carries heating device.
6. preparation method according to claim 1, which is characterized in that the layering superpositing unit is a kind of double torsional flows
Road mold, and with heating device, connected using a series of delaminating units to adjust thickness in monolayer in fiber, to obtain 2n+1It hands over
For the structure of layer, cut to obtain alternating layer structure fiber using fiber die, and by the stretching of roller wrap-up, prepare
The controllable fiber of size uniform.
7. preparation method according to claim 1, which is characterized in that the coextrusion junction station and layering superpositing unit
Temperature setting using styrene-based polymer resin and separate the higher person of resin extruded machine die temperature or contrast this temperature
It floats or floats downward 10-20 DEG C.
8. preparation method according to claim 1, which is characterized in that the alternating layer structure fiber can pass through adjusting screw rod
Rotating speed realizes that fiber microlayer thickness is distributed, to volume ratio of the two kinds of materials of control in alternating layer structure.
9. preparation method according to claim 6, which is characterized in that the alternating layer structure fiber is received by adjusting roller
The rotating speed of acquisition means carries out fiber to stretch the size for adjusting fiber.
10. preparation method according to claim 1, which is characterized in that the isolated polymer by alternating layer structure
The method that resin is separated is to utilize styrene base resin and isolated polymer the resin dissolubility in water or organic solvent
Difference, by isolated polymer dissolve and retain styrene base resin, obtain fiber shape.
11. preparation method according to claim 1, which is characterized in that the styrene-based polymer of the preparation is micro-nano
Fiber size is 50nm-50 μm.
12. preparation method according to claim 1, which is characterized in that the styrene base resin micro nanometer fiber felt
Thickness adjustable extent be 1mm-3mm.
13. preparation method according to claim 1, which is characterized in that described prepares the micro-nano fibre of styrene base resin
The filter membrane for tieing up felt is copper filter membrane or stainless steel filter membrane.
14. preparation method according to claim 1, which is characterized in that concrete operation step is：
The first step：Prepare two kinds of polymer resin alternating layer structure fiber operating process be：
Styrene base resin and isolated polymer resin are subjected to melting extrusion by two extruders respectively, then by fused materials
It is delivered to junction station, and is converged herein, by being overlapped the principle of cutting with layering superpositing unit, in delaminating process middle level
The vertical cutting of structure experience is divided into two streams, expands horizontally and reconsolidate, and to make the quantity of layer double, is layered by n
Superpositing unit will form 2n+1Coextruded layer, and obtain thickness in monolayer micro/nano level by fiber die cutting and wrap-up
Styrene base resin and isolated polymer resin alternating layer structure fiber；Wherein, it is obtained by adjusting extruder screw rotating speed
Different volumes than alternating layer fiber；
Second step：The operating process of isolated polymer resin in fiber spin-off alternating layer structure fiber is：
Two methods：
（1）Obtained fluoropolymer resin alternating structure fiber is subjected to high-speed stirred, rotating speed 800-1000r/min, and ultrasound
Disperse 20-24h, water-insoluble separation resin is subjected to selective dissolution separation with organic solvent, or divided water solubility with water
Separated and dissolved is carried out every resin, obtains the controllable micro/nano level styrene base resin fiber of size uniform；
（2）Obtained fluoropolymer resin alternating structure fiber is rinsed with giant, pressure 5-10MPa, time 20-
40min obtains the controllable micro/nano level styrene base resin fiber of size uniform to detach water-soluble resin；
Third walks：Deposition prepares the operating process of the styrene base resin micro nanometer fiber felt with porous structure on filter membrane
For：
The styrene base resin fiber obtained after separation process removes separate layer resin is sunk by mass range 0.5g-20g
Product is different from 40-80 DEG C of dry 24-48h on filter membrane, by solvent for use when separation, obtains thickness range as 1mm-3mm's
Styrene base resin micro nanometer fiber felt.
15. by the styrene base resin for the adsorbable polycyclic aromatic hydrocarbon that the preparation method according to one of claim 1-14 obtains
Micro nanometer fiber felt.
16. such as styrene base resin micro nanometer fiber felt according to claim 15 polycyclic aromatic hydrocarbon pollutant in going water removal
In application, specifically obtained fibrofelt is immersed in the aqueous solution containing polycyclic aromatic hydrocarbon, you can remove polycyclic aromatic hydrocarbon in water removal
Pollutant.
17. application according to claim 15, which is characterized in that the concentration range of the polycyclic aromatic hydrocarbon aqueous solution is
30ppb-130ppb。
18. application according to claim 15, which is characterized in that the polycyclic aromatic hydrocarbon be it is water-soluble in 2-5 rings
Polycyclic aromatic hydrocarbon, it is any in specific fluorenes, phenanthrene, anthracene, pyrene, benzanthracene or BaP etc..
19. application according to claim 15, which is characterized in that the styrene base resin micro nanometer fiber felt is gone
The Longer absorption times of polycyclic aromatic hydrocarbon are 0.1-24h in water removal.
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| CN103342766A (en) * | 2013-07-18 | 2013-10-09 | 南京工业大学 | Synthesis and preparation of novel hydrophobic polystyrene resin |
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| CN104629151A (en) * | 2015-02-16 | 2015-05-20 | 同济大学 | Porous vinyl resin film with controllable structure and preparation method thereof |
| CN104975375A (en) * | 2015-04-23 | 2015-10-14 | 同济大学 | Polymer micro-nano-fiber preparation method |
| CN105330780A (en) * | 2015-11-20 | 2016-02-17 | 同济大学 | Styrene base resin porous material capable of adsorbing polycyclic aromatic hydrocarbon and preparation method of styrene base resin porous material |
| US20170320040A1 (en) * | 2016-05-05 | 2017-11-09 | Trustees Of Tufts College | Methods and kits for removing organic pollutants from a contaminated sample |
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| CN103342766A (en) * | 2013-07-18 | 2013-10-09 | 南京工业大学 | Synthesis and preparation of novel hydrophobic polystyrene resin |
| CN104264235A (en) * | 2014-09-09 | 2015-01-07 | 天津工业大学 | Micro-nano sodium polyacrylate fiber mat production method |
| CN104629151A (en) * | 2015-02-16 | 2015-05-20 | 同济大学 | Porous vinyl resin film with controllable structure and preparation method thereof |
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| CN105330780A (en) * | 2015-11-20 | 2016-02-17 | 同济大学 | Styrene base resin porous material capable of adsorbing polycyclic aromatic hydrocarbon and preparation method of styrene base resin porous material |
| US20170320040A1 (en) * | 2016-05-05 | 2017-11-09 | Trustees Of Tufts College | Methods and kits for removing organic pollutants from a contaminated sample |
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