GB2598511A - Modified polylactic acid non-woven fabric for oil-water separation, preparation method therefor and application thereof - Google Patents

Modified polylactic acid non-woven fabric for oil-water separation, preparation method therefor and application thereof Download PDF

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Publication number
GB2598511A
GB2598511A GB2116986.7A GB202116986A GB2598511A GB 2598511 A GB2598511 A GB 2598511A GB 202116986 A GB202116986 A GB 202116986A GB 2598511 A GB2598511 A GB 2598511A
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polylactic acid
nonwoven fabric
oil
pdla
water separation
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GB202116986D0 (en
GB2598511B (en
Inventor
Jiang Wei
Zhu Chenxi
Hu Jinglei
Sun Ping
Li Aimin
Zhang Quanxing
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Nanjing University
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Nanjing University
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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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
    • B01D17/08—Thickening liquid suspensions by filtration
    • 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
    • B01J20/28038—Membranes or mats made from fibers or filaments
    • 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
    • C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/507—Polyesters
    • 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
    • C02F1/40—Devices for separating or removing fatty or oily substances or similar floating material
    • 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
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/08—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with halogenated hydrocarbons
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
    • D06M13/144—Alcohols; Metal alcoholates
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
    • D06M13/224—Esters of carboxylic acids; Esters of carbonic acid
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/16—Synthetic fibres, other than mineral fibres
    • D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M2101/32—Polyesters
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
    • D06M2200/10—Repellency against liquids
    • D06M2200/12—Hydrophobic properties

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Textile Engineering (AREA)
  • Analytical Chemistry (AREA)
  • Water Supply & Treatment (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Environmental & Geological Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Nonwoven Fabrics (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Polyesters Or Polycarbonates (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
  • Artificial Filaments (AREA)

Abstract

Provided in the present invention is a preparation method for a modified polylactic acid non-woven fabric for oil-water separation, comprising the following steps: (1) dissolving PDLA in an organic solvent to prepare a 0.1-5wt% PDLA solution, adding a poor solvent of polylactic acid having a volume 1-4 times that of the PDLA solution, and stirring to obtain a mixed solution; (2) pouring the mixed solution obtained in step (1) into a container containing a PLLA non-woven fabric; (3) allowing same to stand for a certain period of time at room temperature, and then drying. Micron-sized particles generated on the modified polylactic acid non-woven fabric prepared according to the present application increase the surface roughness of the polylactic acid non-woven fabric, the highest contact angle of the non-woven fabric in air to water is 150°, the contact angle of the non-woven fabric to oil is 0°, the adsorption capacity of the modified polylactic acid non-woven fabric is increased by more than 40% compared to the adsorption capacity of unmodified polylactic acid non-woven fabric, and the modified polylactic acid non-woven fabric still has good stability after being repeatedly used 10 times. The preparation method of the present invention is simple, and the prepared fabric is completely biodegradable, will not cause secondary pollution and is widely applicable to the treatment of oily wastewater.

Description

SPECIFICATION
MODIFIED POLYLACTIC ACID NONWOVEN FABRIC FOR OIL/WATER
SEPARATION AND PREPARATION METHOD AND APPLICATION THEREOF
TECHNICAL FIELD
The present invention relates to an oil/water separation technology, and more particularly, is a modified polylactic acid nonwoven fabric for oil/water separation and a preparation method and application thereof
BACKGROUND
In recent years, with the increasing industrial pollution, the discharge of oily wastewater is also increased gradually. Frequent oil leakage and industrial discharge of organic solvents have caused serious environmental pollution and ecological problems around the world. Traditional oillwater separation technologies generally have low efficiency, long time consumption, high costs, and other defects. In order to solve these problems, new oil/water separation methods and materials have been continuously researched and developed, and oil-absorbing materials have gradually grown into a main force of oil/water separation.
In recent decades, predecessors have paid more and more attention to the research of oil/water separation materials, and traditional oil/water separation materials, such as sponges and other porous materials, are widely used. However, the materials have low selectivity to oil, low adsorption capacity and other defects, and have a very short service life. On this basis, artificial synthetic materials have been widely used as a main force of the oil/water separation materials, but these materials generally have the defects of unstable chemical property and low reuse rate, and most of the materials are not biodegradable, with a risk of secondary pollution.
Polylactic acid (PLA) is a completely biodegradable polymer material with a wide range of synthetic routes and final degradation products of CO2 and H20. The polylactic acid has the advantage of good biocompatibility, and very good application prospect and research value. Predecessors simply used a phase separation method to produce a super-hydrophobic polylactic acid film, but the film has a very poor mechanical property so as to be unsuitable for oil/water separation industry. It has been reported that the adsorption of nano-SiO2 particles by coating an adhesive layer on a surface of a polylactic acid nonwoven fabric is researched, but this method has a complicated experimental operation, and the obtained
SPECIFICATION
oil/water separation material has poor wear-resisting property due to the addition of other particles.
It has been reported that the polylactic acid may be divided into poly L lactic acid (PLLA) and poly D lactic acid (PDLA) according to different optical activities of a polymer molecular chain of the polylactic acid. When the PLLA and the PDLA are blended in a certain proportion, a stereocomplex (SC) may be formed. The stereocomplex is mainly different from homopolymers of the PLLA and the PDLA in the following three aspects: (1) the PLA-SC has a high melting temperature, which is nearly 50°C higher than that of the homopolymers of the PLLA and the PDLA; (2) a PLA-SC crystal is a triclinic crystal stacked in 31 helical conformation, which belongs to a 13 crystal form; (3) and compared with the homopolymers of the PLLA and the PDLA, the PLA-SC has excellent impact and mechanical properties.
SUMMARY
Object of the present invention: aiming at the technical problems in the prior art above, the present application provides a modified polylactic acid nonwoven fabric for oil/water separation and a preparation method thereof, and an application thereof in treating oily wastewater.
Technical solutions: the preparation method of the modified polylactic acid nonwoven fabric for oil/water separation according to the present application includes the following steps of: (I) dissolving PDLA into an organic solvent to obtain a PDLA solution, and adding a nonsolvent of polylactic acid; (2) taking a PLLA nonwoven fabric, and dropwise adding the mixed solution obtained in step (1) to soak the nonwoven fabric in the mixed solution; and (3) after step (2), standing for 12 hours to 36 hours, and then drying.
In step (1), a molecular weight of the PDLA ranges from 20,000 to 200,000; the organic solvent is dichloromethane or chloroform; and the nonsolvent of polylactic acid is at least one of ethanol, n-butanol and butyl acetate.
In step (1), a concentration of the PDLA solution is 0.1%wt to 511Owt; and a volume ratio of the PDLA solution to the nonsolvent of polylactic acid is 1: Ito 5.
In step (2), a molecular weight of the PLLA ranges from 40,000 to 200,000.
In step (3), the standing is carried out at room temperature, and the drying refers to drying in an oven at 20°C to 80°C for 4 hours to 24 hours.
SPECIFICATION
A modified polylactic acid nonwoven fabric for oil/water separation obtained by the preparation method above also falls within the scope of protection of the present application. A contact angle of the modified polylactic acid nonwoven fabric to water is about 150 degrees, and a contact angle of the modified polylactic acid nonwoven fabric to oil is about 0 degree. Moreover, an oil absorption volume of the nonwoven fabric prepared is increased by more than 40%, and the nonwoven fabric may be recycled for more than 10 times An application of the modified polylactic acid nonwoven fabric for oil/water separation in treating oily wastewater also falls within the scope of protection of the present application.
According to the present invention, a dichloromethane solution containing a nonsolyent of PDLA is dripped on the PLLA nonwoven fabric, so that a slightly soluble surface containing PLLA is formed on the PLLA nonwoven fabric. The PDLA contained in the PDLA solution is blended with the above PLLA dissolved in the solution, phase separation occurs during volatilization of the solvent and the nonsolvent, and a stereocomplex of the polylactic acid is formed on a surface of the nonwoven fabric The stereocomplex is formed on the surface of the nonwoven fabric for oil/water separation prepared according to the present invention due to self-assembly, and the stereocomplex is directly connected with the nonwoven fabric through a strong chemical bond, so that the prepared nonwoven fabric for oil/water separation has good stability and wear-resisting property.
In the present application, the PDLA refers to poly D lactic acid and the PLLA refers to poly L lactic acid.
Beneficial effects: the polylactic acid nonwoven fabric for oil/water separation according to the present application has the contact angle to water in air of about 150 degrees and the contact angle to oil of about 0 degree; and may be used in the field of oil/water separation, the oil absorption volume of the polylactic acid nonwoven fabric for oil/water separation is increased by more than 40%, and the polylactic acid nonwoven fabric for oil/water separation may be recycled for more than 10 times, with a good durability. In the present invention, experiments prove that the prepared nonwoven fabric of oil/water separation has the characteristics of stability wear-resisting property and high-efficiency separation; may be degraded in a natural environment without secondary pollution after being used and discarded; and may be used for oil/water separation of oily wastewater, such as oil/water separation of oily wastewater containing edible oil, gasoline, and the like, with a broad application prospect -3 -
SPECIFICATION
BRIEF DESCRIPTION OF THE DRAWINGS
FIG 1 is an enlarged scanning electron microscope photograph of a surface morphology of a prepared nonwoven fabric for oil/water separation; FIG 2 is a photograph of a shape of a water droplet (3 microliters) measured in air on a surface of the prepared nonwoven fabric for oil/water separation; FIG 3 is a photograph of a shape of an oil droplet (3 microliters) measured in air on the surface of the prepared nonwoven fabric for oil/water separation; FIG 4 is a photograph of an effect of the prepared nonwoven fabric for oil/water separation in the embodiment for absorbing an oily substance; and FIG. 5 is a graph of change data of a contact angle to water of the prepared nonwoven fabric for oil/water separation in the embodiment after repeatedly using for 10 times.
DETAILED DESCRIPTION
The present invention is described hereinafter through the specific embodiments. PLLA nonwoven fabric was purchased from Jiangxi Guoctiao Industrial Co., Ltd. Embodiment I A preparation method of a modified polylactic acid nonwoven fabric for oil/water separation included the following specific steps.
(1) A PDLA solution with a preparation concentration of 0.1%wt was prepared with an organic solvent, and then an equal volume of nonsolvent was added into the above PDLA solution, and magnetically stirred for 30 minutes. The nonsolvent was prepared by magnetically stirring equal volumes of ethanol, n-butanol and butyl acetate, a molecular weight of the PDLA was 20,000, and the organic solvent was dichloromethane.
(2) 15 ml of the mixed solution obtained in step (1) was dropwi se added into a circular PLLA nonwoven fabric (Mw=40,000) culture dish with a diameter of 6 cm, wherein a molecular weight of the PLLA was 40,000.
(3) The nonwoven fabric was stood in the culture dish in step (2) at a normal temperature for 24 hours, and then dried in an oven at 40°C for 6 hours to obtain the nonwoven fabric for oil/water separation.
Embodiment 2
SPECIFICATION
A preparation method of a modified polylactic acid nonwoven fabric for oil/water separation included the following specific steps.
(1) A PDLA solution with a preparation concentration of 0.1%m was prepared with an organic solvent, and then 4 times volume of nonsolvent was added into the above PDLA solution, and magnetically stirred for 30 minutes. The nonsolvent was prepared by magnetically stirring equal volumes of ethanol, n-butanol and butyl acetate for 30 minutes, a molecular weight of the PDLA was 20,000, and the organic solvent was di chl oromethane.
(2) 15 ml of the mixed solution obtained in step (1) was dropwi se added into a circular PLLA nonwoven fabric (Mw=40,000) culture dish with a diameter of 6 cm, wherein a molecular weight of the PLLA was 40,000.
(3) The nonwoven fabric was stood in the culture dish in step (2) at a normal temperature for 24 hours, and then dried in an oven at 40°C for 6 hours to obtain the nonwoven fabric for oil/water separation.
Embodiment 3 A preparation method of a modified polylactic acid nonwoven fabric for oil/water separation included the following specific steps.
(1) A PDLA solution with a preparation concentration of 5%wt was prepared with an organic solvent, and then an equal volume of nonsolvent was added into the above PDLA solution, and magnetically stirred for 30 minutes. The nonsolvent was prepared by magnetically stirring equal volumes of ethanol, n-butanol and butyl acetate, a molecular weight of the PDLA was 20,000, and the organic solvent was dichloromethane.
(2) 15 ml of the mixed solution obtained in step (1) was dropwi se added into a circular PLLA nonwoven fabric (Mw=40,000) culture dish with a diameter of 6 cm, wherein a molecular weight of the PLLA was 40,000.
(3) The nonwoven fabric was stood in the culture dish in step (2) at a normal temperature for 24 hours, and then dried in an oven at 40°C for 6 hours to obtain the nonwoven fabric for oil/water separation.
Embodiment 4 A preparation method of a modified polylactic acid nonwoven fabric for oil/water
SPECIFICATION
separation included the following specific steps.
(1) A PDLA solution with a preparation concentration of 5%wt was prepared with an organic solvent, and then 4 times volume of nonsolvent was added into the above PDLA solution, and magnetically stirred for 30 minutes. The nonsolvent was prepared by magnetically stirring equal volumes of ethanol, n-butanol and butyl acetate, a molecular weight of the PDLA was 20,000, and the organic solvent was dichloromethane.
(2) 15 ml of the mixed solution obtained in step (1) was dropwi se added into a circular PLLA nonwoven fabric (Mw=40,000) culture dish with a diameter of 6 cm, wherein a molecular weight of the PLLA was 40,000.
(3) The nonwoven fabric was stood in the culture dish in step (2) at a normal temperature for 24 hours, and then dried in an oven at 40°C for 6 hours to obtain the nonwoven fabric for oil/water separation.
Embodiment 5 A preparation method of a modified polylactic acid nonwoven fabric for oil/water separation included the following specific steps.
(1) A PDLA solution with a preparation concentration of 0.1%wt was prepared with an organic solvent, and then an equal volume of nonsolvent was added into the above PDLA solution, and magnetically stirred for 30 minutes. The nonsolvent was prepared by magnetically stirring equal volumes of ethanol, n-butanol and butyl acetate, a molecular weight of the PDLA was 200,000, and the organic solvent was trichloromethane.
(2) 15 ml of the mixed solution obtained in step (1) was dropwi se added into a circular PLLA nonwoven fabric (Mw=40,000) culture dish with a diameter of 6 cm, wherein a molecular weight of the PLLA was 40,000.
(3) The nonwoven fabric was stood in the culture dish in step (2) at a normal temperature for 24 hours, and then dried in an oven at 40°C for 6 hours to obtain the nonwoven fabric for oil/water separation.
Embodiment 6 A preparation method of a modified polylactic acid nonwoven fabric for oil/water separation included the following specific steps.
SPECIFICATION
(I) A PDLA solution with a preparation concentration of 0.1%wt was prepared with an organic solvent, and then 4 times volume of nonsolvent was added into the above PDLA solution, and magnetically stirred for 30 minutes The nonsolvent was prepared by magnetically stirring equal volumes of ethanol, n-butanol and butyl acetate, a molecular weight of the PDLA was 200,000, and the organic solvent was trichloromethane.
(2) 15 ml of the mixed solution obtained in step (1) was dropwi se added into a circular PLLA nonwoven fabric (Mw=40,000) culture dish with a diameter of 6 cm, wherein a molecular weight of the PLLA was 40,000.
(3) The nonwoven fabric was stood in the culture dish in step (2) at a normal temperature for 24 hours, and then dried in an oven at 40°C for 6 hours to obtain the nonwoven fabric for oil/water separation.
Embodiment 7 A preparation method of a modified polylactic acid nonwoven fabric for oil/water separation included the following specific steps.
(1) A PDLA solution with a preparation concentration of 5%wt was prepared with an organic solvent, and then an equal volume of nonsolvent was added into the above PDLA solution, and magnetically stirred for 30 minutes. The nonsolvent was prepared by magnetically stirring equal volumes of ethanol, n-butanol and butyl acetate, a molecular weight of the PDLA was 200,000, and the organic solvent was trichloromethane (2) 15 ml of the mixed solution obtained in step (1) was dropwi se added into a circular PLLA nonwoven fabric (Mw=40,000) culture dish with a diameter of 6 cm, wherein a molecular weight of the PLLA was 40,000.
(3) The nonwoven fabric was stood in the culture dish in step (2) at a normal temperature for 24 hours, and then dried in an oven at 40°C for 6 hours to obtain the nonwoven fabric for oil/water separation.
Embodiment 8 A preparation method of a modified polylactic acid nonwoven fabric for oil/water separation included the following specific steps.
(I) A PDLA solution with a preparation concentration of 5%wt was prepared with an
SPECIFICATION
organic solvent, and then 4 times volume of nonsolvent was added into the above PDLA solution, and magnetically stirred for 30 minutes. The nonsolvent was prepared by magnetically stirring equal volumes of ethanol, n-butanol and butyl acetate, a molecular weight of the PDLA was 200,000, and the organic solvent was trichloromethane.
(2) 15 ml of the mixed solution obtained in step (1) was dropwi se added into a circular PLLA nonwoven fabric (Mw=40,000) culture dish with a diameter of 6 cm, wherein a molecular weight of the PLLA was 40,000.
(3) The nonwoven fabric was stood in the culture dish in step (2) at a normal temperature for 24 hours, and then dried in an oven at 40°C for 6 hours to obtain the nonwoven fabric for oil/water separation.
Embodiment 9 A preparation method of a modified polylactic acid nonwoven fabric for oil/water separation included the following specific steps.
(1) A PDLA solution with a preparation concentration of 0.5%wt was prepared with an organic solvent, and then 1.5 times volume of nonsolvent was added into the above PDLA solution, and magnetically stirred for 30 minutes. The nonsolvent was prepared by magnetically stirring equal volumes of ethanol, n-butanol and butyl acetate, a molecular weight of the PDLA was 100,000, and the organic solvent was dichloromethane.
(2) 15 ml of the mixed solution obtained in step (1) was dropwi se added into a circular PLLA nonwoven fabric (Mw=100,000) culture dish with a diameter of 6 cm, wherein a molecular weight of the PLLA was 100,000.
(3) The nonwoven fabric was stood in the culture dish in step (2) at a normal temperature for 24 hours, and then dried in an oven at 40°C for 6 hours to obtain the nonwoven fabric for oil/water separation.
Embodiment 10 A preparation method of a modified polylactic acid nonwoven fabric for oil/water separation included the following specific steps.
(1) A PDLA solution with a preparation concentration of 1%wt was prepared with an organic solvent, and then 1.5 times volume of nonsolvent was added into the above PDLA
SPECIFICATION
solution, and magnetically stirred for 30 minutes. The nonsolvent was prepared by magnetically stirring equal volumes of ethanol, n-butanol and butyl acetate, a molecular weight of the PDLA was 60,000, and the organic solvent was trichloromethane.
(2) 15 ml of the mixed solution obtained in step (1) was dropwi se added into a circular PLLA nonwoven fabric (Mw=60,000) culture dish with a diameter of 6 cm, wherein a molecular weight of the PLLA was 60,000.
(3) The nonwoven fabric was stood in the culture dish in step (2) at a normal temperature for 24 hours, and then dried in an oven at 40°C for 6 hours to obtain the nonwoven fabric for oil/water separation.
Embodiment 11 A preparation method of a modified polylactic acid nonwoven fabric for oil/water separation included the following specific steps.
(1) A PDLA solution with a preparation concentration of 2(1-owt was prepared with an organic solvent, and then 1.5 times volume of nonsolvent was added into the above PDLA solution, and magnetically stirred for 30 minutes. The nonsolvent was prepared by magnetically stirring equal volumes of ethanol, n-butanol and butyl acetate, a molecular weight of the PDLA was 100,000, and the organic solvent was dichloromethane.
(2) 15 ml of the mixed solution obtained in step (1) was dropwi se added into a circular PLLA nonwoven fabric (Mw=100,000) culture dish with a diameter of 6 cm, wherein a molecular weight of the PLLA was 100,000.
(3) The nonwoven fabric was stood in the culture dish in step (2) at a normal temperature for 24 hours, and then dried in an oven at 40°C for 6 hours to obtain the nonwoven fabric for oil/water separation.
Embodiment 12 A preparation method of a modified polylactic acid nonwoven fabric for oil/water separation included the following specific steps.
(1) A PDLA solution with a preparation concentration of 0.5%wt was prepared with an organic solvent, and then 2 times volume of nonsolvent was added into the above PDLA solution, and magnetically stirred for 30 minutes. The nonsolvent was prepared by
SPECIFICATION
magnetically stirring equal volumes of ethanol, n-butanol and butyl acetate, a molecular weight of the PDLAwas 100,000, and the organic solvent was trichloromethane.
(2) 15 ml of the mixed solution obtained in step (1) was dropwise added into a circular PLLA nonwoven fabric (Mw=100,000) culture dish with a diameter of 6 cm, wherein a molecular weight of the PLLA was 100,000.
(3) The nonwoven fabric was stood in the culture dish in step (2) at a normal temperature for 24 hours, and then dried in an oven at 40°C for 6 hours to obtain the nonwoven fabric for oil/water separation.
Embodiment 13 Characteristics and functional identification of modified polylactic acid nonwoven fabric for oil/water separation 1. Electron microscope scanning observation The nonwoven fabric for oil/water separation obtained in the above embodiment was scanned with an electron microscope, and a surface morphology of the nonwoven fabric for oil/water separation was observed at a magnification of 3,000 times. Results are shown in FIG. 1, and it can be seen that a blocky structure is formed on a fiber surface, which increases a surface roughness of the nonwoven fabric.
2. Research on oil absorption and hydrophobicity of mesh membrane for oil/water separation 3 microliters of water droplets were dropped on the nonwoven fabric for oil/water separation obtained in Embodiment 1 in air, and measured with a contact angle measuring instrument. Results are shown in FIG. 2, and a contact angle to water in air is 150 degrees. 3 microliters of n-hexane was dropped on the nonwoven fabric for oil/water separation obtained in Embodiment 1 in air, and measured with a contact angle measuring instrument. Results are shown in FIG. 3, and a contact angle to oil in air is 0 degree.
3. Separation of oil/water mixture with nonwoven fabric for oil/water separation The nonwoven fabric for oil/water separation obtained in the above embodiment has a good absorption capacity for an oily substance, as shown in FIG 4.
4. Stability measurement -10 -
SPECIFICATION
After being repeatedly used for 10 times, as shown in FIG. 5, the nonwoven fabric for oil/water separation obtained in Embodiment 1 still has a strong hydrophobic effect, which shows that the nonwoven fabric has a good stability

Claims (8)

  1. CLAIMS1. A preparation method of a modified polylactic acid nonwoven fabric for oil/water separation, comprising the following steps of (1) dissolving PDLA into an organic solvent to obtain a PDLA solution, adding a nonsolvent of polylactic acid, and stirring the mixture evenly to obtain a mixed solution; (2) taking a PLLA nonwoven fabric, and dropwise adding the mixed solution obtained in step (1) to soak the nonwoven fabric in the mixed solution; and (3) after step (2), standing for 12 hours to 36 hours, and then drying.
  2. 2. The preparation method according to claim 1, wherein in step (1), a molecular weight of the PDLA is 20,000 to 200,000; the organic solvent is dichloromethane or chloroform; the nonsolvent of polylactic acid is at least one of ethanol, n-butanol and butyl acetate.
  3. 3. The preparation method according to claim 1, wherein in step (1), a concentration of the PDLA solution ranges from 0.1%wt to 5%wt; and a volume ratio of the PDLA solution to the nonsolvent of polylactic acid is 1: Ito 5.
  4. 4. The preparation method according to claim 1, wherein in step (2), a molecular weight of the PLLA ranges from 40,000 to 200,000
  5. 5. The preparation method according to claim 1, wherein in step (3), the standing is carried out at room temperature, and the drying refers to drying in an oven at 20°C to 80°C for 4 hours to 24 hours
  6. 6. A modified polylactic acid nonwoven fabric for oil/water separation obtained by the preparation method according to any one of claims 1 to 5.
  7. 7. The modified polylactic acid nonwoven fabric for oil/water separation according to claim 6, wherein a contact angle of the modified polylactic acid nonwoven fabric to water is about 150 degrees, and a contact angle of the modified polylactic acid nonwoven fabric to oil is about 0 degree.
  8. 8. An application of a modified polylactic acid nonwoven fabric for oil/water separation obtained by the preparation method according to any one of claims 1 to 5 in treating oily wastewater.
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CN110841108A (en) * 2019-12-27 2020-02-28 南京思元医疗技术有限公司 Preparation method of polylactic acid microparticles and injectable soft tissue filler
CN113461995B (en) * 2021-07-22 2022-07-22 郑州大学 Preparation method of polylactic acid material with anti-adhesion sterilization function
CN115382516A (en) * 2022-08-23 2022-11-25 和远潜江电子特种气体有限公司 Preparation method of modified organic adsorption resin and application of modified organic adsorption resin in preparation of hydrogen bromide
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