CN110158316B - Modified polylactic acid non-woven fabric for oil-water separation and preparation method and application thereof - Google Patents
Modified polylactic acid non-woven fabric for oil-water separation and preparation method and application thereof Download PDFInfo
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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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- B01J20/28038—Membranes or mats made from fibers or filaments
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- 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
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- 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
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Abstract
The invention provides a preparation method of a modified polylactic acid non-woven fabric for oil-water separation, which comprises the following steps: (1) dissolving PDLA in an organic solvent to prepare a PDLA solution with the weight of 0.1-5%, adding a poor solvent of polylactic acid with the volume of 1-4 times that of the PDLA solution, and stirring to obtain a mixed solution; (2) pouring the mixed solution in the step (1) into a container filled with PLLA non-woven fabrics; (3) standing at room temperature for a certain time, and drying. The micron-sized small particles are generated on the modified polylactic acid non-woven fabric prepared by the method, the surface roughness of the polylactic acid non-woven fabric is increased, the contact angle of the non-woven fabric to water in the air is 150 degrees at most, the contact angle to oil is 0 degree, the adsorption capacity is improved by more than 40 percent compared with that of the unmodified polylactic acid non-woven fabric, and the modified polylactic acid non-woven fabric still has better stability after being reused for 10 times. The preparation method is simple, completely biodegradable, and free from secondary pollution, and can be used for treating oily wastewater in a large range.
Description
Technical Field
The invention relates to an oil-water separation technology, in particular to a modified polylactic acid non-woven fabric for oil-water separation and a preparation method and application thereof.
Background
In recent years, as industrial pollution has been increased, the discharge of oily wastewater has been increased. Frequent petroleum spills and industrial discharges of organic solvents cause serious environmental pollution and ecological problems around the world. The traditional oil-water separation technology generally has the defects of low efficiency, long time consumption, high cost and the like. In order to solve these problems, new oil-water separation methods and materials are continuously researched and developed, and oil-absorbing materials are gradually growing into the main force of oil-water separation.
In recent decades, the research on oil-water separation materials by predecessors has been more and more important, and the traditional oil-water separation materials, such as sponge and other porous materials, have wide application. However, the material has the defects of low selectivity to oil, small adsorption quantity and the like, and the service life is short. On the basis, the artificially synthesized material is widely used as the oil-water separation material, but the material generally has the defects of unstable chemical property and low reuse rate, is mostly not biodegradable, and has the risk of causing secondary pollution.
Polylactic acid (PLA) is a synthetic route which is extensive, and the final degradation product is CO2And H2O, a completely biodegradable polymer material. The preparation method has the advantage of good biocompatibility, and has good application prospect and research value. The former simply utilizes a phase separation method to produce the super-hydrophobic polylactic acid film, but the film has poor mechanical property and is not suitable for the oil-water separation industry. It has also been reported that the adhesion layer is coated on the surface of the polylactic acid nonwoven fabric and then the nano SiO2 particles are adsorbed, but the experimental operation of the method is complicated, and the obtained oil-water separation material has poor wear resistance due to the addition of other particles.
Polylactic acids are reported to be classified into levorotatory polylactic acid (PLLA) and dextrorotatory polylactic acid (PDLA) according to the difference in optical rotation of the polymer molecular chain. When PLLA is blended with PDLA in a certain ratio, a Stereocomplex (SC) is formed. It differs from the respective homopolymers of PLLA and PDLA, mainly in the following 3 aspects: (1) PLA-sc has higher melting temperature which is about 50 ℃ higher than the melting points of the respective homopolymers of PLLA and PDLA; (2) the PLA-sc crystal is a triclinic crystal stacked in 31 helical conformation, and belongs to a beta crystal form; (3) it has superior impact and mechanical properties compared to the respective homopolymers of PLLA and PDLA.
Disclosure of Invention
The purpose of the invention is as follows: aiming at the technical problems in the prior art, the application provides a modified polylactic acid non-woven fabric for oil-water separation, a preparation method thereof and application thereof in treating oily wastewater.
The technical scheme is as follows: the application discloses a preparation method of modified polylactic acid non-woven fabric for oil-water separation, which comprises the following steps:
(1) dissolving PDLA in an organic solvent to obtain a PDLA solution, and adding a poor solvent of polylactic acid;
(2) taking a PLLA non-woven fabric, dropwise adding the mixed solution obtained in the step (1) to soak the non-woven fabric in the mixed solution;
(3) and (3) after the operation of the step (2), standing for 12-36h, and then drying.
In the step (1), the molecular weight of the PDLA is 20000-200000; the organic solvent is dichloromethane or trichloromethane; the poor solvent of the polylactic acid is at least one of ethanol, n-butyl alcohol and butyl acetate.
In the step (1), the concentration of the PDLA solution is 0.1-5 wt%; the volume ratio of the PDLA solution to the poor solvent of the polylactic acid is 1: 1-5.
In the step (2), the molecular weight of the PLLA is 40000-200000.
And (3) standing in a room temperature environment, wherein the drying refers to drying in an oven at the temperature of 20-80 ℃ for 4-24 h.
The modified polylactic acid non-woven fabric for oil-water separation prepared according to the method is also within the protection scope of the application. The contact angle of the modified polylactic acid non-woven fabric for oil-water separation to water is about 150 degrees, and the contact angle to oil is about 0 degrees. And the oil absorption of the prepared non-woven fabric is improved by more than 40 percent, and the non-woven fabric can be recycled for more than 10 times.
The application of the modified polylactic acid non-woven fabric for oil-water separation in treating oil-containing wastewater is also within the protection scope of the application.
In the invention, a methylene dichloride solution of PDLA containing poor solvent is dripped on a PLLA non-woven fabric, so that a slightly soluble surface containing PLLA is formed on the PLLA non-woven fabric. PDLA contained in the PDLA solution is mixed with PLLA dissolved in the solution, phase separation occurs in the volatilization process of the solvent and poor solvent, and a stereocomplex of polylactic acid is formed on the surface of the non-woven fabric. The surface of the oil-water separation non-woven fabric prepared by the invention forms a stereo compound due to self-assembly, and the stereo compound is directly connected with the non-woven fabric through a strong chemical bond, so that the prepared oil-water separation non-woven fabric has good stability and wear resistance.
In the present application, PDLA means poly-D-lactic acid and PLLA means poly-L-lactic acid.
Has the advantages that: the contact angle of the polylactic acid oil-water separation non-woven fabric to water in the air is near 150 degrees; the contact angle to oil is around 0 °; the oil-water separator can be used in the field of oil-water separation, the oil absorption is improved by more than 40%, the oil-water separator can be recycled for more than 10 times, and the durability is good. Experiments prove that the prepared oil-water separation non-woven fabric has the characteristics of stability, wear resistance and high-efficiency separation; after being used and abandoned, the material can be degraded in natural environment, and secondary pollution can not be generated; can be used for oil-water separation of oily sewage, such as oil-water separation of oily sewage containing edible oil, gasoline and the like, and has wide application prospect.
Drawings
FIG. 1 is an enlarged scanning electron micrograph of the surface morphology of the prepared oil-water separation nonwoven fabric;
FIG. 2 is a photograph showing the shape of a water drop (3. mu.l) measured in the air on the surface of a prepared oil-water separation nonwoven fabric;
fig. 3 is a photograph showing the shape of oil droplets (3 μ l) measured in the air on the surface of the prepared oil-water separation nonwoven fabric;
FIG. 4 is a photograph showing the effect of the oil-water separating nonwoven fabric prepared in example on absorbing oily substances;
FIG. 5 is a graph showing the data of water contact angle change after 10 repetitions of the nonwoven fabric for oil-water separation prepared in example.
Detailed Description
The present invention is illustrated by the following specific examples.
The PLLA nonwoven fabric was purchased from bridge industries, Inc. of Jiangxi nations.
Example 1
A preparation method of a modified polylactic acid non-woven fabric for oil-water separation comprises the following specific steps:
(1) preparing a PDLA solution with the concentration of 0.1 wt%, adding an isometric poor solvent into the PDLA solution, and magnetically stirring for 30 min; wherein the poor solvent is prepared by magnetic stirring of ethanol, n-butanol and butyl acetate with equal volume, the molecular weight of PDLA is 20000, and the organic solvent is dichloromethane;
(2) dripping 15ml of the mixed solution obtained in the step (1) into a culture dish filled with a round PLLA non-woven fabric (Mw 40000) with the diameter of 6cm, wherein the molecular weight of PLLA is 40000;
(3) and (3) standing the non-woven fabric in the culture dish in the step (2) for 24 hours at normal temperature, and then drying the non-woven fabric in an oven at 40 ℃ for 6 hours to obtain the oil-water separation non-woven fabric.
Example 2
A preparation method of a modified polylactic acid non-woven fabric for oil-water separation comprises the following specific steps:
(1) a PDLA solution with a concentration of 0.1% wt was prepared using an organic solvent, and then 4 times the volume of a poor solvent was added to the PDLA solution, followed by magnetic stirring for 30 min. Wherein the poor solvent is prepared by magnetic stirring of ethanol, n-butanol and butyl acetate with equal volume for 30min, wherein the molecular weight of PDLA is 20000, and the organic solvent is dichloromethane;
(2) dripping 15ml of the mixed solution obtained in the step (1) into a culture dish filled with a round PLLA non-woven fabric (Mw 40000) with the diameter of 6cm, wherein the molecular weight of PLLA is 40000;
(3) and (3) standing the non-woven fabric in the culture dish in the step (2) for 24 hours at normal temperature, and then drying the non-woven fabric in an oven at 40 ℃ for 6 hours to obtain the oil-water separation non-woven fabric.
Example 3
A preparation method of a modified polylactic acid non-woven fabric for oil-water separation comprises the following specific steps:
(1) preparing a PDLA solution with the concentration of 5% by weight by using an organic solvent, adding an equal volume of a poor solvent into the PDLA solution, and magnetically stirring for 30 min. Wherein the poor solvent is prepared by magnetic stirring of ethanol, n-butanol and butyl acetate with equal volume, the molecular weight of PDLA is 20000, and the organic solvent is dichloromethane;
(2) dripping 15ml of the mixed solution obtained in the step (1) into a culture dish filled with a round PLLA non-woven fabric (Mw 40000) with the diameter of 6cm, wherein the molecular weight of PLLA is 40000;
(3) and (3) standing the non-woven fabric in the culture dish in the step (2) for 24 hours at normal temperature, and then drying the non-woven fabric in an oven at 40 ℃ for 6 hours to obtain the oil-water separation non-woven fabric.
Example 4
A preparation method of a modified polylactic acid non-woven fabric for oil-water separation comprises the following specific steps:
(1) a PDLA solution having a concentration of 5% by weight was prepared using an organic solvent, and then 4 times the volume of a poor solvent was added to the PDLA solution, followed by magnetic stirring for 30 min. Wherein the poor solvent is prepared by magnetic stirring of ethanol, n-butanol and butyl acetate with equal volume, the molecular weight of PDLA is 20000, and the organic solvent is dichloromethane;
(2) dripping 15ml of the mixed solution obtained in the step (1) into a culture dish filled with a round PLLA non-woven fabric (Mw 40000) with the diameter of 6cm, wherein the molecular weight of PLLA is 40000;
(3) and (3) standing the non-woven fabric in the culture dish in the step (2) for 24 hours at normal temperature, and then drying the non-woven fabric in an oven at 40 ℃ for 6 hours to obtain the oil-water separation non-woven fabric.
Example 5
A preparation method of a modified polylactic acid non-woven fabric for oil-water separation comprises the following specific steps:
(1) PDLA solution with concentration of 0.1% wt is prepared by organic solvent, then equal volume of poor solvent is added into the PDLA solution, and magnetic stirring is carried out for 30 min. Wherein the poor solvent is prepared by magnetic stirring of ethanol, n-butanol and butyl acetate with equal volume, the molecular weight of PDLA is 200000, and the organic solvent is chloroform;
(2) dripping 15ml of the mixed solution obtained in the step (1) into a culture dish filled with a round PLLA non-woven fabric (Mw 40000) with the diameter of 6cm, wherein the molecular weight of PLLA is 40000;
(3) and (3) standing the non-woven fabric in the culture dish in the step (2) for 24 hours at normal temperature, and then drying the non-woven fabric in an oven at 40 ℃ for 6 hours to obtain the oil-water separation non-woven fabric.
Example 6
A preparation method of a modified polylactic acid non-woven fabric for oil-water separation comprises the following specific steps:
(1) a PDLA solution with a concentration of 0.1% wt was prepared using an organic solvent, and then 4 times the volume of a poor solvent was added to the PDLA solution, followed by magnetic stirring for 30 min. Wherein the poor solvent is prepared by magnetic stirring of ethanol, n-butanol and butyl acetate with equal volume, the molecular weight of PDLA is 200000, and the organic solvent is chloroform;
(2) dripping 15ml of the mixed solution obtained in the step (1) into a culture dish filled with a round PLLA non-woven fabric (Mw 40000) with the diameter of 6cm, wherein the molecular weight of PLLA is 40000;
(3) and (3) standing the non-woven fabric in the culture dish in the step (2) for 24 hours at normal temperature, and then drying the non-woven fabric in an oven at 40 ℃ for 6 hours to obtain the oil-water separation non-woven fabric.
Example 7
A preparation method of a modified polylactic acid non-woven fabric for oil-water separation comprises the following specific steps:
(1) preparing a PDLA solution with the concentration of 5% by weight by using an organic solvent, adding a poor solvent with the same volume as the PDLA solution, and magnetically stirring for 30 min. Wherein the poor solvent is prepared by magnetic stirring of ethanol, n-butanol and butyl acetate with equal volume, the molecular weight of PDLA is 200000, and the organic solvent is chloroform;
(2) dripping 15ml of the mixed solution obtained in the step (1) into a culture dish filled with a round PLLA non-woven fabric (Mw 40000) with the diameter of 6cm, wherein the molecular weight of PLLA is 40000;
(3) and (3) standing the non-woven fabric in the culture dish in the step (2) for 24 hours at normal temperature, and then drying the non-woven fabric in an oven at 40 ℃ for 6 hours to obtain the oil-water separation non-woven fabric.
Example 8
A preparation method of a modified polylactic acid non-woven fabric for oil-water separation comprises the following specific steps:
(1) a PDLA solution having a concentration of 5% by weight was prepared using an organic solvent, and then 4 times the volume of a poor solvent was added to the PDLA solution, followed by magnetic stirring for 30 min. Wherein the poor solvent is prepared by magnetic stirring of ethanol, n-butanol and butyl acetate with equal volume, the molecular weight of PDLA is 200000, and the organic solvent is chloroform;
(2) dripping 15ml of the mixed solution obtained in the step (1) into a culture dish filled with a round PLLA non-woven fabric (Mw 40000) with the diameter of 6cm, wherein the molecular weight of PLLA is 40000;
(3) and (3) standing the non-woven fabric in the culture dish in the step (2) for 24 hours at normal temperature, and then drying the non-woven fabric in an oven at 40 ℃ for 6 hours to obtain the oil-water separation non-woven fabric.
Example 9
A preparation method of a modified polylactic acid non-woven fabric for oil-water separation comprises the following specific steps:
(1) a PDLA solution having a concentration of 0.5% wt was prepared using an organic solvent, and then a poor solvent was added to the PDLA solution in an amount of 1.5 times the volume of the solution, followed by magnetic stirring for 30 min. Wherein the poor solvent is prepared by magnetic stirring of ethanol, n-butanol and butyl acetate with equal volume, the molecular weight of PDLA is 100000, and the organic solvent is dichloromethane;
(2) dropping 15ml of the mixed solution obtained in the step (1) into a culture dish filled with a round PLLA non-woven fabric (Mw is 100000) with the diameter of 6cm, wherein the molecular weight of PLLA is 100000;
(3) and (3) standing the non-woven fabric in the culture dish in the step (2) for 24 hours at normal temperature, and then drying the non-woven fabric in an oven at 40 ℃ for 6 hours to obtain the oil-water separation non-woven fabric.
Example 10
A preparation method of a modified polylactic acid non-woven fabric for oil-water separation comprises the following specific steps:
(1) a1% wt PDLA solution was prepared with an organic solvent, and then 1.5 times the volume of a poor solvent was added to the PDLA solution, followed by magnetic stirring for 30 min. Wherein the poor solvent is prepared by magnetic stirring of ethanol, n-butanol and butyl acetate with equal volume, the molecular weight of PDLA is 60000, and the organic solvent is chloroform;
(2) dropping 15ml of the mixed solution obtained in the step (1) into a culture dish filled with a circular PLLA non-woven fabric (Mw 60000) with the diameter of 6cm, wherein the molecular weight of PLLA is 60000;
(3) and (3) standing the non-woven fabric in the culture dish in the step (2) for 24 hours at normal temperature, and then drying the non-woven fabric in an oven at 40 ℃ for 6 hours to obtain the oil-water separation non-woven fabric.
Example 11
A preparation method of a modified polylactic acid non-woven fabric for oil-water separation comprises the following specific steps:
(1) a PDLA solution having a concentration of 2% wt was prepared using an organic solvent, and then a poor solvent was added to the PDLA solution in an amount of 1.5 times the volume of the solution, followed by magnetic stirring for 30 min. Wherein the poor solvent is prepared by magnetic stirring of ethanol, n-butanol and butyl acetate with equal volume, the molecular weight of PDLA is 100000, and the organic solvent is dichloromethane;
(2) dropping 15ml of the mixed solution obtained in the step (1) into a culture dish filled with a round PLLA non-woven fabric (Mw is 100000) with the diameter of 6cm, wherein the molecular weight of PLLA is 100000;
(3) and (3) standing the non-woven fabric in the culture dish in the step (2) for 24 hours at normal temperature, and then drying the non-woven fabric in an oven at 40 ℃ for 6 hours to obtain the oil-water separation non-woven fabric.
Example 12
A preparation method of a modified polylactic acid non-woven fabric for oil-water separation comprises the following specific steps:
(1) a PDLA solution having a concentration of 0.5% wt was prepared using an organic solvent, and then 2 times the volume of a poor solvent was added to the PDLA solution, followed by magnetic stirring for 30 min. Wherein the poor solvent is prepared by magnetic stirring of ethanol, n-butanol and butyl acetate with equal volume, the molecular weight of PDLA is 100000, and the organic solvent is chloroform;
(2) dropping 15ml of the mixed solution obtained in the step (1) into a culture dish filled with a round PLLA non-woven fabric (Mw is 100000) with the diameter of 6cm, wherein the molecular weight of PLLA is 100000;
(3) and (3) standing the non-woven fabric in the culture dish in the step (2) for 24 hours at normal temperature, and then drying the non-woven fabric in an oven at 40 ℃ for 6 hours to obtain the oil-water separation non-woven fabric.
Example 13
Characteristic and function identification of oil-water separation modified polylactic acid non-woven fabric
1. Scanning observation of electron microscope
Scanning the oil-water separation non-woven fabric obtained in the example by an electron microscope, and observing the surface morphology by magnifying 3000 times, wherein the result is shown in figure 1, and a blocky structure is generated on the surface of the fiber, so that the surface roughness of the non-woven fabric is increased.
2. Oil absorption and hydrophobicity study of oil-water separation mesh membrane
When 3. mu.l of water was dropped on the oil-water separation nonwoven fabric obtained in example 1 in the air and measured by a contact angle meter, the contact angle with water in the air was 150 °, as shown in FIG. 2. In the air, 3 μ l of n-hexane was dropped on the oil-water separation nonwoven fabric obtained in example 1, and the contact angle with oil in the air was 0 ° as shown in fig. 3.
3. Oil-water separation non-woven fabric separation oil-water mixture
The oil-water separating nonwoven fabric prepared in the above example has a good absorption ability for oily substances, as shown in FIG. 4.
4. Stability determination
After the oil-water separation nonwoven fabric prepared in example 1 is reused for 10 times, as shown in fig. 5, the oil-water separation nonwoven fabric still has a strong hydrophobic effect, which indicates that the oil-water separation nonwoven fabric has good stability.
Claims (4)
1. A preparation method of a modified polylactic acid non-woven fabric for oil-water separation is characterized by comprising the following steps:
(1) dissolving PDLA in an organic solvent to obtain a PDLA solution, adding a poor solvent of polylactic acid, and uniformly stirring to obtain a mixed solution;
(2) taking a PLLA non-woven fabric, dropwise adding the mixed solution obtained in the step (1) to soak the non-woven fabric in the mixed solution;
(3) after the operation of the step (2), standing for 12-36h, and then drying;
in the step (1), the molecular weight of the PDLA is 20000-200000; the organic solvent is dichloromethane or trichloromethane; the poor solvent of the polylactic acid is at least one of ethanol, n-butyl alcohol and butyl acetate;
in the step (1), the concentration of the PDLA solution is 0.1-5 wt%; the volume ratio of the PDLA solution to the poor solvent of the polylactic acid is 1: 1-5;
in the step (2), the molecular weight of the PLLA is 40000-200000.
2. The preparation method according to claim 1, wherein in the step (3), the mixture is allowed to stand in a room temperature environment, and the drying is performed in an oven at 20-80 ℃ for 4-24 h.
3. The modified polylactic acid nonwoven fabric for oil-water separation prepared by the preparation method according to claim 1 or 2.
4. The use of the modified polylactic acid nonwoven fabric for oil-water separation prepared by the preparation method according to claim 1 or 2 for treating oil-containing wastewater.
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| CN201910456896.7A CN110158316B (en) | 2019-05-29 | 2019-05-29 | Modified polylactic acid non-woven fabric for oil-water separation and preparation method and application thereof |
| PCT/CN2020/073447 WO2020238270A1 (en) | 2019-05-29 | 2020-01-21 | Modified polylactic acid non-woven fabric for oil-water separation, preparation method therefor and application thereof |
| GB2116986.7A GB2598511B (en) | 2019-05-29 | 2020-01-21 | Modified polylactic acid nonwoven fabric for oil/water separation and preparation method and application thereof |
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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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| JP2007039954A (en) * | 2005-08-02 | 2007-02-15 | Asenthy:Kk | Oil absorber using oil decomposing microorganism and biodegradation nonwoven fabric |
| JP5038920B2 (en) * | 2008-01-22 | 2012-10-03 | 帝人ファイバー株式会社 | Method for producing water-absorbing polylactic acid fiber structure, water-absorbing polylactic acid fiber structure, and fiber product |
| CN102698471B (en) * | 2012-05-16 | 2014-10-22 | 清华大学 | Oil-water separating mesh film and preparation method thereof |
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