CN107999039B - PLA-TPs nanofiber membrane and preparation method and application thereof - Google Patents

PLA-TPs nanofiber membrane and preparation method and application thereof Download PDF

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CN107999039B
CN107999039B CN201711274993.1A CN201711274993A CN107999039B CN 107999039 B CN107999039 B CN 107999039B CN 201711274993 A CN201711274993 A CN 201711274993A CN 107999039 B CN107999039 B CN 107999039B
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王亚茹
徐岚
何吉欢
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Suzhou University
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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
    • B01J20/28054—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 surface properties or porosity
    • B01J20/28057—Surface area, e.g. B.E.T specific surface area
    • 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
    • B01J20/262—Synthetic macromolecular compounds obtained otherwise than by reactions only involving carbon to carbon unsaturated bonds, e.g. obtained by polycondensation
    • 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
    • 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
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00—Formation of filaments, threads, or the like
    • D01D5/0007—Electro-spinning
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00—Formation of filaments, threads, or the like
    • D01D5/0007—Electro-spinning
    • D01D5/0015—Electro-spinning characterised by the initial state of the material
    • D01D5/003—Electro-spinning characterised by the initial state of the material the material being a polymer solution or dispersion
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/70—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres
    • D04H1/72—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged
    • D04H1/728—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged by electro-spinning
    • 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
    • C02F2101/10—Inorganic compounds
    • C02F2101/20—Heavy metals or heavy metal compounds

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  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Textile Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Analytical Chemistry (AREA)
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  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
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Abstract

The invention discloses a preparation method of a PLA-TPs nanofiber membrane, which is characterized by comprising the following steps: (1) dissolving polylactic acid in a mixed solution of DCM and DMF to obtain a polylactic acid solution with the concentration of 6wt% -8wt%, wherein the mass ratio of the mixed solution of DCM and DMF is 7:3-8: 2; (2) dissolving tea polyphenol in the polylactic acid solution, and uniformly stirring to obtain PLA-TPs mixed spinning solution, wherein the mass ratio of the tea polyphenol to the polylactic acid is (0.04-0.5): 1; (3) starting a spinning machine, and carrying out electrostatic spinning on the mixed spinning solution under the conditions that the temperature is 20-30 ℃ and the relative humidity is 45-65% to obtain the PLA-TPs nanofiber membrane. The invention also discloses the PLA-TPs nanofiber membrane and application thereof in the aspect of adsorbing heavy metal ions. The method can prepare the PLA-TPs nanofiber membrane with good uniformity, high specific surface area and strong adsorption capacity, has super strong adsorption capacity on silver ions in the wastewater, and can be used for purification treatment of the wastewater.

Description

PLA-TPs nanofiber membrane and preparation method and application thereof
Technical Field
The invention relates to the field of nano materials, in particular to a preparation method of a PLA-TPs nanofiber membrane, the PLA-TPs nanofiber membrane prepared by the method and application of the PLA-TPs nanofiber membrane.
Background
One of the major problems in this century is environmental pollution caused by industrial activities, and the introduction of a large amount of chemicals into the environment for the purposes of industrialization, chemical engineering, textiles, mining, agriculture, cosmetics, paper making, leather, and the like. Water contaminants in the form of dyes or metal ions pose a serious threat to human health. Drinking heavy metal water destroys the nervous system, may cause skin irritation, renal insufficiency, and may increase the risk of cancer. The removal of heavy metals has attracted a great deal of researcher's attention in view of the high toxicity of these materials. Conventional methods for removing heavy metals from water include chemical precipitation, ion exchange, electrochemical methods, membrane filtration and adsorption. Among these methods, adsorption is the most efficient, economical, and it is flexible to operate, highly efficient, and has a rich source of adsorbent. Among the available adsorbents, nanofiber membranes have attracted considerable interest to researchers due to their high specific surface area and porous structure.
The nanofiber membrane prepared by electrostatic spinning has the outstanding advantages of high specific surface area, high porosity, an internally communicated open pore structure and the like, so that the nanofiber membrane has good adsorption performance and recycling performance in the aspect of adsorption and separation of heavy metal ions. However, the general nanofiber membrane can only be used for adsorbing heavy metal solution with relatively low concentration. Therefore, in order to solve the problem of adsorption of the aqueous solution with relatively high concentration of heavy metal ions, it is necessary to develop a super adsorption-reduction nanofiber membrane.
Tea polyphenol can be used as a reducing agent and a surface protective agent to adsorb heavy metal ions so as to reduce the heavy metal ions into nano particles, and other reagents are not needed. Polylactic acid Poly (lactic acid) (PLA) with biocompatibility and biodegradation performance and controllable degradation speed and Tea Polyphenol (TPs) with good water solubility, no toxicity and no harm are mixed to be used as solute, and Dichloromethane (DCM) and N-N Dimethylformamide (DMF) are used as solvents to prepare the PLA/TPs nanofiber membrane. Realizing the super-adsorption reduction of silver ions in the wastewater.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method of a PLA-TPs nanofiber membrane, the PLA-TPs nanofiber membrane which has good uniformity, high specific surface area and strong adsorption capacity can be prepared by the method, and the nanofiber membrane has super-strong adsorption capacity on silver ions in wastewater and can be used for purification treatment of the wastewater.
In order to solve the technical problems, the invention provides a preparation method of a PLA-TPs nanofiber membrane, which comprises the following steps:
(1) dissolving polylactic acid in a mixed solution of DCM and DMF to obtain a polylactic acid solution with the concentration of 6wt% -8wt%, wherein the mass ratio of the mixed solution of DCM and DMF is 7:3-8: 2;
(2) dissolving tea polyphenol in the polylactic acid solution prepared in the step (1), and uniformly stirring to obtain PLA-TPs mixed spinning solution, wherein the mass ratio of the tea polyphenol to the polylactic acid is (0.04-0.5) to 1;
(3) starting a spinning machine, and carrying out electrostatic spinning on the PLA-TPs mixed spinning solution under the conditions that the temperature is 20-30 ℃ and the relative humidity is 45-65% to obtain the PLA-TPs nano fiber membrane.
In a preferred embodiment of the invention, the distance between the receiving plate and the spinneret is 10-20 cm.
In a preferred embodiment of the invention, the voltage is in the range of 10-20 KV.
In a preferred embodiment of the present invention, the flow rate of the mixed spinning dope is 0.6 to 1.5 ml/h.
The invention also discloses the PLA-TPs nanofiber membrane prepared by the preparation method.
The invention also discloses application of the PLA-TPs nanofiber membrane in the aspect of adsorbing heavy metal ions, in particular application in the aspect of adsorbing silver ions in wastewater.
The preparation method of the PLA-TPs nanofiber membrane is simple to operate and short in process flow, the PLA-TPs nanofiber membrane with good surface uniformity, high specific surface area and strong adsorption capacity can be obtained, and the PLA-TPs nanofiber membrane has super strong adsorption capacity on heavy metal ions in wastewater and can be used for purification treatment of the wastewater.
The tea polyphenol has strong binding performance to inorganic ions, so the tea polyphenol is very suitable for the adsorption treatment of heavy metal ions in wastewater. However, the method of adding tea polyphenol to wastewater has not been effective. According to the invention, the characteristic of high specific surface area of the electrostatic spinning nanofiber is utilized, the tea polyphenol and the polylactic acid are subjected to mixed electrospinning to obtain the PLA-TPs composite nanofiber membrane, and due to the characteristic of high specific surface area, the contact area of the tea polyphenol and the wastewater is increased, so that the adsorption capacity of heavy metal ions is enhanced.
Drawings
FIGS. 1-5 are scanning electron micrographs of PLA-TPs nanofiber film samples prepared in examples 1-5, respectively.
Detailed Description
The present invention is further described below in conjunction with the following figures and specific examples so that those skilled in the art may better understand the present invention and practice it, but the examples are not intended to limit the present invention.
Example 1
A preparation method of PLA-TPs nanofiber membrane comprises the following steps:
(1) adding a DCM/DMF mixed solution with a mass ratio of 8:2 into a brown ground bottle, then weighing a certain mass of polylactic acid, adding the polylactic acid into the mixed solution, then placing the brown ground bottle on a magnetic stirrer, and stirring at a constant speed for 2-4h until a solute is completely dissolved, wherein the solution is clear and transparent, and a polylactic acid solution with a concentration of 6-8 wt% is obtained;
(2) weighing tea polyphenol with a certain mass according to the mass ratio of the tea polyphenol to the polylactic acid of 0.04:1, adding the tea polyphenol into the polylactic acid solution, and then placing the prepared mixed solution on a magnetic stirrer to stir at a constant speed for 24 hours to obtain a uniform spinning solution;
(3) starting a spinning machine, controlling the experimental environment temperature to be 20-30 ℃ and the relative humidity to be 45-65%, and obtaining the PLA-TPs nanofiber membrane by adopting an electrostatic spinning technology.
In the step (3), the specific steps of electrospinning include:
pouring the prepared spinning solution into a syringe with the inner diameter of a jet orifice of 0.7mm and the capacity of 10ml, fixing the syringe on a syringe pump, and respectively connecting the jet orifice and a receiving plate of the syringe to the positive electrode and the negative electrode of a direct-current high-voltage power supply, wherein the receiving plate is a metal plate. And after the experimental device checks that the solution does not exist, the injection pump is started to adjust the flow, and after the solution slowly flows out, the high-voltage power supply is started and the voltage is adjusted to start the spinning experiment. The distance between the receiving plate and the spinneret is 10-20cm, the voltage range is 10-20KV, and the flow rate of the spinning solution is 0.6-1.5 ml/h.
Example 2
A preparation method of PLA-TPs nanofiber membrane, which is different from example 1 only in that the mass ratio of solvent is DCM: DMF ═ 7: 3.
Example 3
A preparation method of PLA-TPs nanofiber membrane, which is different from example 1 only in that the mass ratio of tea polyphenol to polylactic acid is 0.125: 1.
Example 4
A preparation method of PLA-TPs nanofiber membrane, which is different from example 1 only in that the mass ratio of tea polyphenol to polylactic acid is 0.25: 1.
Example 5
A preparation method of PLA-TPs nanofiber membrane, which is different from example 1 only in that the mass ratio of tea polyphenol to polylactic acid is 0.5: 1.
Examples of the experiments
PLA-TPs nanofiber membrane samples prepared in examples 1 to 5 were cut into a size of 4cm × 4cm, placed in a constant temperature incubator shaker at 37 ℃ and 60rmp for 2 hours, and the nanofiber membrane was removed and filtered through filter paper, and the content of silver ions remaining in the solution was measured by an atomic absorption spectrometer, and the results are shown in Table 1.
TABLE 1 samples of examples 1-5 vs. Ag+Adsorption result of (2)
Figure BDA0001496352820000041
As can be seen from FIG. 1, through electrospinning, PLA-TPs nanofiber membranes with fiber diameter of about 400-800nm and good fiber apparent structure uniformity were obtained, and the nanofiber membranes had extremely high specific surface area. In example 1, because the content of highly volatile DCM in the solvent is relatively high, DCM on the fiber surface is rapidly volatilized during spinning, so that micropores are generated on the nanofiber surface, and the specific surface area of the fiber membrane is further increased. In examples 3 to 5, the physical properties of the spinning solution were affected due to the higher content of tea polyphenol, and the surface of the obtained fiber had no more micropores.
As can be seen from Table 1, in the adsorption test, the nanofiber membrane was aligned to Ag as the content of tea polyphenols in the fibers increased+The stronger the adsorption capacity, when the mass ratio of tea polyphenol to polylactic acid in the fiber is 0.5:1, the adsorption capacity to Ag is higher+The adsorption rate of (D) is up to 82%. It should be noted that in example 1, the obtained nanofibers have micropores distributed on the surface, and the specific surface area of the fiber membrane is increased, so that the nanofiber membrane has the function of resisting Ag+The adsorption rate of (a) is higher than that of the fiber membrane of example 3.
The PLA-TPs nanofiber membrane prepared by the method has the advantages of good uniformity, high specific surface area, strong adsorption capacity and the like, has super strong adsorption capacity on heavy metal ions in wastewater, and can be used for purification treatment of wastewater.
The above-mentioned embodiments are merely preferred embodiments for fully illustrating the present invention, and the scope of the present invention is not limited thereto. The equivalent substitution or change made by the technical personnel in the technical field on the basis of the invention is all within the protection scope of the invention. The protection scope of the invention is subject to the claims.

Claims (4)

  1. The application of the PLA-TPs nanofiber membrane in the aspect of adsorbing heavy metal ions is characterized in that the preparation method of the PLA-TPs nanofiber membrane comprises the following steps:
    (1) dissolving polylactic acid in a mixed solution of DCM and DMF to obtain a polylactic acid solution with the concentration of 6wt% -8wt%, wherein the mass ratio of DCM to DMF in the polylactic acid solution is 8: 2;
    (2) dissolving tea polyphenol in the polylactic acid solution prepared in the step (1), and uniformly stirring to obtain PLA-TPs mixed spinning solution, wherein the mass ratio of the tea polyphenol to the polylactic acid is (0.04-0.5) to 1;
    (3) starting a spinning machine, and carrying out electrostatic spinning on the PLA-TPs mixed spinning solution under the conditions that the temperature is 20-30 ℃ and the relative humidity is 45-65% to obtain the PLA-TPs nano fiber membrane.
  2. 2. The use according to claim 1, wherein in step (3), the distance between the receiving plate and the spinneret is 10-20 cm.
  3. 3. Use according to claim 1, wherein in step (3) the voltage is in the range of 10-20 kV.
  4. 4. The use according to claim 1, wherein in step (3), the flow rate of the mixed spinning solution is 0.6 to 1.5 mL/h.
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CN108660614B (en) * 2018-05-22 2020-04-03 西南交通大学 Polylactic acid porous film and preparation method thereof
CN111513395A (en) * 2020-05-18 2020-08-11 武汉大学 Novel antimicrobial environment-friendly mask and manufacturing method thereof
CN112481833A (en) * 2020-12-31 2021-03-12 华南农业大学 Environment-friendly micro-nano fiber film material, preparation method thereof and application thereof in water lead pollution treatment
CN113413923A (en) * 2021-06-24 2021-09-21 昆明理工大学 Method for preparing acid-base difunctional nanofiber material by electrostatic spinning
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