CN112337895A - Cross-linked electrostatic spinning fiber membrane and preparation method and application thereof - Google Patents

Abstract

The invention belongs to the technical field of material manufacturing. The invention provides a preparation method of a cross-linked electrostatic spinning fibrous membrane, which comprises the steps of mixing polyvinylpyrrolidone, a polymer and a solvent to obtain a spinning solution; spinning the spinning solution by a specific electrostatic spinning process to obtain an electrostatic spinning fiber membrane; and mixing the obtained electrostatic spinning fiber membrane, an initiator, a cross-linking agent and a solvent, and then carrying out cross-linking reaction to obtain the cross-linked electrostatic spinning fiber membrane. The invention also provides the cross-linked electrostatic spinning fiber membrane, which has excellent oil-water separation performance and can be applied to oil-water separation to separate oil-water mixtures or oil-in-water emulsions.

Description

Cross-linked electrostatic spinning fiber membrane and preparation method and application thereof

Technical Field

The invention relates to the technical field of material manufacturing, in particular to a cross-linked electrostatic spinning fibrous membrane and a preparation method and application thereof.

Background

The water resource is the foundation of human survival and development, along with the development of society, the demand of people on energy is increased rapidly, the exploitation of petroleum resources is increased day by day, and oil contamination accidents frequently occur and a great amount of oily sewage is generated due to natural or artificial factors in the processes of processing, transportation and use. The oil pollutants in the water body can isolate air, so that the ecological environment of the water body is greatly changed, and the environment is fatally damaged.

Common oil-water separation methods include incineration, gravity settling, adsorption, air flotation, membrane separation, and the like. The incineration method causes secondary pollution to the environment and also causes waste of resources. The gravity settling method requires long separation time and low efficiency, and cannot meet actual requirements. The adsorption method has poor selectivity, and the adsorbed oil contains a large amount of water and has poor separation effect. The air floatation separation method is to inject a large amount of inert gas into sewage to generate bubbles. And then the densely distributed bubbles are used as carriers to be combined with oil drops, so that the floating rate of the oil drops is accelerated, and the oil-water separation is rapidly realized. The air floatation method can treat oily sewage on a large scale, but can only effectively separate oil drops with larger particle sizes in the oily sewage, and cannot treat emulsified oil and dissolved oil in the oily sewage.

Disclosure of Invention

The invention aims to overcome the defects in the prior art and provides a crosslinked electrospun fiber membrane as well as a preparation method and application thereof.

In order to achieve the above object, the present invention provides the following technical solutions:

the invention provides a preparation method of a cross-linked electrostatic spinning fiber membrane, which comprises the following steps:

(1) mixing a polymer A, a polymer B and a solvent to obtain a spinning solution;

(2) carrying out electrostatic spinning on the spinning solution to obtain an electrostatic spinning fiber membrane;

(3) mixing the electrostatic spinning fiber membrane, an initiator, a cross-linking agent and a solvent, and then carrying out a cross-linking reaction to obtain a cross-linked electrostatic spinning fiber membrane;

the polymer A is polyvinylpyrrolidone;

the polymer B is polyacrylonitrile, polyether sulfone, polyurethane, polyvinylidene fluoride, polystyrene, polymethyl methacrylate, polyaniline, polyarylene ether nitrile, cellulose, polylactic acid or cellulose acetate.

Preferably, the mass ratio of the polymer B to the polymer A in the step (1) is 1: 0.05 to 0.2;

the mass ratio of the sum of the mass of the polymer B and the mass of the polymer A to the mass of the solvent is 0.08-0.12: 1;

the solvent is N, N-dimethylformamide, dimethyl sulfoxide, dimethylacetamide, chlorobenzene, chloroform, acetone, dichloromethane or trichloromethane.

Preferably, the mixing in step (1) is stirring and ultrasound carried out sequentially;

the stirring speed is 300-800 rpm, the stirring time is 12-24 hours, and the stirring temperature is 18-60 ℃;

the power of the ultrasound is 35-45 kHz, the time of the ultrasound is 0.5-2 h, and the temperature of the ultrasound is 18-60 ℃.

Preferably, the device used in the electrospinning in the step (2) is a syringe, the syringe has a specification of 5-20 mL, the inner diameter of a needle in the syringe is 0.39-0.43 mm, and the outer diameter of the needle in the syringe is 0.69-0.73 mm.

Preferably, the voltage of the electrostatic spinning in the step (2) is 8-20 KV, the injection speed of the electrostatic spinning is 0.2-0.4 mm/min, the translation speed of a needle of the electrostatic spinning is 280-320 mm/min, the translation stroke of the electrostatic spinning is 480-520 mm, the distance between the needle of the electrostatic spinning and a receiving roller is 8-20 cm, and the rotating speed of the receiving roller is 80-120 rpm.

Preferably, the mass ratio of the cross-linking agent to the solvent in the step (3) is 0.01-0.05: 1; the mass ratio of the electrostatic spinning fiber membrane to the cross-linking agent is 1: 0.01 to 0.05; the mass ratio of the mass sum of the electrostatic spinning fiber membrane and the cross-linking agent to the mass sum of the initiator is 1: 0.01 to 0.05;

the crosslinking agent is persulfate, 1, 7-octadiene, alkylene bisacrylamide or a divinylaromatic compound;

the persulfate is ammonium persulfate, potassium persulfate or sodium persulfate;

the divinylaromatic compound is divinylbenzene or divinylethylbenzene;

the initiator is peroxide or azobisisobutyronitrile;

the peroxide is dibenzoyl peroxide or ditert-butyl peroxide.

Preferably, the temperature of the crosslinking reaction in the step (3) is 15-90 ℃, and the time of the crosslinking reaction is 0.5-9 h.

The application also provides the crosslinked electrostatic spinning fiber membrane obtained by the preparation method.

The application also provides the application of the crosslinked electrostatic spinning fiber membrane in separating oil and water.

Preferably, the oil-water mixture is an oil-water mixture or an oil-in-water emulsion;

the diameter of the oil-in-water emulsion is 100-500 nm;

the type of the oil in the separated oil water is one or more of gasoline, kerosene, diesel oil, engine oil, normal hexane, cyclohexane, petroleum ether, trichloromethane, toluene, isooctane, carbon tetrachloride and chloroform.

The invention provides a preparation method of a cross-linked electrostatic spinning fibrous membrane, which comprises the steps of mixing polyvinylpyrrolidone, a polymer and a solvent to obtain a spinning solution; spinning the spinning solution by a specific electrostatic spinning process to obtain an electrostatic spinning fiber membrane; and mixing the obtained electrostatic spinning fiber membrane, an initiator, a cross-linking agent and a solvent, and then carrying out cross-linking reaction to obtain the cross-linked electrostatic spinning fiber membrane. The invention also provides the cross-linked electrostatic spinning fiber membrane, which has excellent oil-water separation performance and can be applied to oil-water separation to separate oil-water mixtures or oil-in-water emulsions.

Drawings

FIG. 1 is a scanning electron microscope image of a crosslinked polyvinylpyrrolidone/polyacrylonitrile electrospun fiber membrane of example 1 of the present application;

FIG. 2 is a digital photograph of a crosslinked polyvinylpyrrolidone/polyacrylonitrile electrospun fiber membrane of example 1 of the present application;

FIG. 3 is a graph showing the effect of separating petroleum ether and water mixtures by using a crosslinked polyvinylpyrrolidone/polyacrylonitrile electrospun fiber membrane according to example 1 of the present application;

FIG. 4 is a graph showing the effect of an oil-in-water emulsion of crosslinked polyvinylpyrrolidone/polyacrylonitrile electrospun fiber membrane on the separation of petroleum ether and water in example 1 of the present application.

Detailed Description

The invention provides a preparation method of a cross-linked electrostatic spinning fiber membrane, which comprises the following steps:

(1) mixing a polymer A, a polymer B and a solvent to obtain a spinning solution;

(2) carrying out electrostatic spinning on the spinning solution to obtain an electrostatic spinning fiber membrane;

(3) mixing the electrostatic spinning fiber membrane, an initiator, a cross-linking agent and a solvent, and then carrying out a cross-linking reaction to obtain a cross-linked electrostatic spinning fiber membrane;

the polymer A is polyvinylpyrrolidone;

the polymer B is preferably polyacrylonitrile, polyethersulfone, polyurethane, polyvinylidene fluoride, polystyrene, polymethyl methacrylate, polyaniline, polyarylene ether nitrile, cellulose, polylactic acid, or cellulose acetate.

In the present invention, the mass ratio of the polymer B to the polymer a in the step (1) is preferably 1: 0.05 to 0.2, and more preferably 1: 0.08 to 0.17, more preferably 1: 0.11 to 0.14.

In the present invention, the mass ratio of the sum of the masses of the polymer B and the polymer a to the solvent is preferably 0.08 to 0.12: 1, more preferably 0.09 to 0.11: 1.

in the present invention, the solvent is preferably N, N-dimethylformamide, dimethyl sulfoxide, dimethylacetamide, chlorobenzene, chloroform, acetone, dichloromethane or chloroform.

In the present invention, the mixing in the step (1) is preferably stirring and sonication performed sequentially.

In the invention, the stirring speed is preferably 300-800 rpm, more preferably 400-700 rpm, and more preferably 500-600 rpm; the stirring time is preferably 12-24 hours, more preferably 14-22 hours, and even more preferably 16-20 hours; the stirring temperature is preferably 18-60 ℃, more preferably 30-50 ℃, and even more preferably 35-45 ℃.

In the invention, the power of the ultrasonic wave is preferably 35-45 kHz, more preferably 36-44 kHz, and even more preferably 38-42 kHz; the ultrasonic time is preferably 0.5-2 h, more preferably 1-1.5 h, and even more preferably 1.2-1.3 h; the temperature of the ultrasonic wave is preferably 18-60 ℃, more preferably 30-50 ℃, and even more preferably 35-45 ℃.

In the invention, the device used for electrostatic spinning in the step (2) is preferably an injector, and the specification of the injector is preferably 5-20 mL, and more preferably 10-15 mL; the inner diameter of a needle head in the injector is preferably 0.39-0.43 mm, and more preferably 0.40-0.42 mm; the outer diameter of the needle head in the injector is preferably 0.69-0.73 mm, and more preferably 0.70-0.72 mm.

In the invention, the voltage of electrostatic spinning in the step (2) is preferably 8-20 KV, more preferably 10-18 KV, and more preferably 12-16 KV; the injection speed of the electrostatic spinning is preferably 0.2-0.4 mm/min, and more preferably 0.25-0.35 mm/min; the translation speed of the needle head of the electrostatic spinning is preferably 280-320 mm/min, and more preferably 290-310 mm/min; the translation stroke of the electrostatic spinning is preferably 480-520 mm, and more preferably 490-510 mm; the distance between the needle head of the electrostatic spinning and the receiving roller is preferably 8-20 cm, more preferably 10-18 cm, and even more preferably 12-16 cm; the rotation speed of the receiving roller is preferably 80-120 rpm, more preferably 90-110 rpm, and even more preferably 95-105 rpm.

In the invention, the temperature of electrostatic spinning in the step (2) is preferably 20-30 ℃, more preferably 22-28 ℃, and more preferably 24-26 ℃; the relative humidity of the electrostatic spinning is preferably 30-40%, more preferably 32-38 ℃, and even more preferably 34-36 ℃.

In the invention, the electrostatic spinning technology is adopted to combine polyvinylpyrrolidone and high molecular polymer to obtain the electrostatic spinning fiber membrane.

In the invention, the mass ratio of the cross-linking agent to the solvent in the step (3) is preferably 0.01-0.05: 1, more preferably 0.02 to 0.04: 1, more preferably 0.025 to 0.035: 1; the mass ratio of the electrospun fiber membrane to the crosslinking agent is preferably 1: 0.01 to 0.05, more preferably 1: 0.02 to 0.04; the mass ratio of the mass sum of the electrostatic spinning fiber membrane and the cross-linking agent to the mass sum of the initiator is 1: 0.01 to 0.05, more preferably 1: 0.02 to 0.04.

In the present invention, the solvent in the step (3) is preferably water.

In the present invention, the crosslinking agent is preferably a persulfate, 1, 7-octadiene, alkylene bisacrylamide, or a divinylaromatic compound.

In the present invention, the persulfate is preferably ammonium persulfate, potassium persulfate, or sodium persulfate.

In the present invention, the divinylaromatic compound is preferably divinylbenzene or divinylethylbenzene.

In the present invention, the initiator is preferably a peroxide or azobisisobutyronitrile.

In the present invention, the peroxide is preferably dibenzoyl peroxide or ditert-butyl peroxide.

In the invention, the temperature of the crosslinking reaction in the step (3) is preferably 15-90 ℃, more preferably 30-75 ℃, and more preferably 45-60 ℃; the time of the crosslinking reaction is preferably 0.5-9 h, more preferably 1-8 h, and even more preferably 3-6 h.

In the present invention, the electrospun fiber membrane, the initiator and the crosslinking agent are subjected to a chemical crosslinking reaction in a solvent. The initiator causes the cross-linking reaction to proceed, and the polyvinylpyrrolidone and the high molecular polymer in the electrostatic spinning fiber membrane are linked between macromolecular chains under the action of the cross-linking agent to obtain the three-dimensional polymer.

The invention also provides the cross-linked electrostatic spinning fiber membrane obtained by the preparation method.

The invention also provides application of the crosslinked electrostatic spinning fiber membrane in oil-water separation.

In the present invention, the oil-water is preferably an oil-water mixture or an oil-in-water emulsion.

In the invention, the diameter of the oil-in-water emulsion is preferably 100-500 nm, more preferably 200-400 nm, and even more preferably 230-370 nm.

In the invention, the type of the oil in the separated oil-water is preferably one or more of gasoline, kerosene, diesel oil, engine oil, normal hexane, cyclohexane, petroleum ether, chloroform, toluene, isooctane, carbon tetrachloride and chloroform.

The technical solutions provided by the present invention are described in detail below with reference to examples, but they should not be construed as limiting the scope of the present invention.

Example 1

Weighing 10g of polyvinylpyrrolidone, 200g of polyacrylonitrile and 2200g of N, N-dimethylformamide, mixing, stirring at the speed of 400rpm at 25 ℃ for 18 hours, and performing ultrasonic treatment at the power of 40kHz at 25 ℃ for 1 hour after stirring to obtain a spinning solution;

using a 15mL injector, wherein the inner diameter of a syringe needle is 0.41mm, the outer diameter of the syringe needle is 0.71mm, extracting a spinning solution, controlling the voltage of electrostatic spinning to be 12KV, the injection speed to be 0.04mm/min, coating an aluminum foil on a receiving roller by a receiving device, controlling the distance between the spinning needle and the receiving roller to be 10cm, the rotating speed of the receiving roller to be 100r/min, the translation speed of the electrostatic spinning needle to be 300mm/min, the translation stroke of the electrostatic spinning to be 500mm, the spinning temperature to be 25 ℃, and the relative humidity to be 35%, and obtaining the polyvinylpyrrolidone/polyacrylonitrile electrostatic spinning fiber membrane by electrostatic spinning;

and mixing the obtained polyvinylpyrrolidone/polyacrylonitrile electrospun fiber membrane, 2.1g of ammonium persulfate, 210g of water and 2.121g of azobisisobutyronitrile, and crosslinking at 90 ℃ for 9 hours to obtain the crosslinked polyvinylpyrrolidone/polyacrylonitrile electrospun fiber membrane.

The crosslinked polyvinylpyrrolidone/polyacrylonitrile electrospun fiber membrane obtained in this example was subjected to electron microscopic scanning, and the scanning result is shown in fig. 1.

The crosslinked polyvinylpyrrolidone/polyacrylonitrile electrospun fiber membrane obtained in this example was photographed, and a digital photograph is shown in fig. 2.

The crosslinked polyvinylpyrrolidone/polyacrylonitrile electrospun fiber membrane prepared in this example was used to separate a mixture of petroleum ether and water, and the separation effect is shown in fig. 3.

The crosslinked polyvinylpyrrolidone/polyacrylonitrile electrospun fiber membrane prepared in this example was used to separate oil-in-water emulsions of petroleum ether and water, and the separation effect is shown in fig. 4.

The crosslinked polyvinylpyrrolidone/polyacrylonitrile electrospun fiber membrane obtained in the embodiment is used for separating the mixture of petroleum ether and water, and the separation efficiency is more than 98%.

Example 2

Weighing 30g of polyvinylpyrrolidone, 300g of polyacrylonitrile and 3300g of N, N-dimethylformamide, mixing, stirring at the speed of 500pm for 24 hours at 25 ℃, and performing ultrasonic treatment at the power of 35kHz for 0.5 hour at 25 ℃ after stirring to obtain a spinning solution;

using a 15mL injector, wherein the inner diameter of a syringe needle is 0.41mm, the outer diameter of the syringe needle is 0.71mm, extracting a spinning solution, controlling the voltage of electrostatic spinning to be 18KV, the injection speed to be 0.03mm/min, coating an aluminum foil on a receiving roller by using a receiving device, controlling the distance between the spinning needle and the receiving roller to be 16cm, the rotating speed of the receiving roller to be 100r/min, the translation speed of the electrostatic spinning needle to be 280mm/min, the translation stroke of the electrostatic spinning to be 490mm, the spinning temperature to be 25 ℃, and the relative humidity to be 35%, and carrying out electrostatic spinning to obtain a polyvinylpyrrolidone/polyacrylonitrile electrostatic spinning fiber membrane;

the obtained polyvinylpyrrolidone/polyacrylonitrile electrospun fiber membrane, 6.6g of sodium persulfate, 330g of water and 6.732g of dibenzoyl peroxide were mixed and crosslinked at 90 ℃ for 9 hours to obtain a crosslinked polyvinylpyrrolidone/polyacrylonitrile electrospun fiber membrane.

The crosslinked polyvinylpyrrolidone/polyacrylonitrile electrostatic spinning fiber membrane obtained in the embodiment is used for separating the mixture of gasoline and water, and the separation efficiency is more than 97%.

Example 3

Weighing 15g of polyvinylpyrrolidone, 75g of polyacrylonitrile and 900g of N, N-dimethylformamide, mixing, stirring at the speed of 600pm for 12 hours at 30 ℃, and performing ultrasonic treatment at the power of 45kHz for 0.5 hour at 30 ℃ after stirring is finished to obtain a spinning solution;

using a 15mL injector, wherein the inner diameter of a syringe needle is 0.41mm, the outer diameter of the syringe needle is 0.71mm, extracting a spinning solution, controlling the voltage of electrostatic spinning to be 16KV, the injection speed to be 0.02mm/min, coating an aluminum foil on a receiving roller by using a receiving device, controlling the distance between the spinning needle and the receiving roller to be 12cm, the rotating speed of the receiving roller to be 100r/min, the translation speed of the electrostatic spinning needle to be 310mm/min, the translation stroke of the electrostatic spinning to be 510mm, the spinning temperature to be 25 ℃, and the relative humidity to be 35%, and obtaining the polyvinylpyrrolidone/polyacrylonitrile electrostatic spinning fiber membrane by electrostatic spinning;

and mixing the obtained polyvinylpyrrolidone/polyacrylonitrile electrospun fiber membrane, 2.7g of potassium persulfate, 90g of water and 2.781g of ditert-butyl peroxide, and crosslinking at 90 ℃ for 9 hours to obtain the crosslinked polyvinylpyrrolidone/polyacrylonitrile electrospun fiber membrane.

The crosslinked polyvinylpyrrolidone/polyacrylonitrile electrospun fiber membrane obtained in the embodiment is used for separating a mixture of n-hexane and water, and the separation efficiency is over 98%.

Example 4

Weighing 50g of polyvinylpyrrolidone, 500g of polyethersulfone and 5500g of dimethylacetamide, mixing, stirring at the speed of 600pm for 24 hours at 25 ℃, and carrying out ultrasonic treatment at the power of 40kHz for 1 hour at 25 ℃ after stirring is finished to obtain a spinning solution;

using a 15mL injector, wherein the inner diameter of a syringe needle is 0.41mm, the outer diameter of the syringe needle is 0.71mm, extracting a spinning solution, controlling the voltage of electrostatic spinning to be 15KV, the injection speed to be 0.02mm/min, coating an aluminum foil on a receiving roller by a receiving device, controlling the distance between the spinning needle and the receiving roller to be 15cm, the rotating speed of the receiving roller to be 100r/min, the translation speed of the electrostatic spinning needle to be 290mm/min, the translation stroke of the electrostatic spinning to be 500mm, the spinning temperature to be 25 ℃, and the relative humidity to be 35%, and obtaining the polyvinylpyrrolidone/polyethersulfone electrostatic spinning fiber membrane by electrostatic spinning;

and mixing the obtained polyvinylpyrrolidone/polyether sulfone electrospun fiber membrane, 22g of 1, 7-octadiene, 550g of water and 22.88g of dibenzoyl peroxide, and crosslinking at 25 ℃ for 1h to obtain the crosslinked polyvinylpyrrolidone/polyether sulfone electrospun fiber membrane.

The crosslinked polyvinylpyrrolidone/polyethersulfone electrospun fiber membrane obtained in the example is used for separating the mixture of kerosene and water, and the separation efficiency is more than 98%.

Example 5

Weighing 10g of polyvinylpyrrolidone, 100g of polyurethane and 1100g of N, N-dimethylformamide, mixing, stirring at the speed of 450rpm for 24 hours at 25 ℃, and carrying out ultrasonic treatment at the power of 42kHz for 0.5 hour at 25 ℃ after stirring is finished to obtain a spinning solution;

using a 15mL injector, wherein the inner diameter of a syringe needle is 0.41mm, the outer diameter of the syringe needle is 0.71mm, extracting a spinning solution, controlling the voltage of electrostatic spinning to be 16KV, the injection speed to be 0.02mm/min, coating an aluminum foil on a receiving roller by using a receiving device, controlling the distance between the spinning needle and the receiving roller to be 15cm, the rotating speed of the receiving roller to be 100r/min, the translation speed of the electrostatic spinning needle to be 310mm/min, the translation stroke of the electrostatic spinning to be 480mm, the spinning temperature to be 25 ℃, and the relative humidity to be 35%, and obtaining the polyvinylpyrrolidone/polyurethane electrostatic spinning fiber membrane by electrostatic spinning;

the obtained polyvinylpyrrolidone/polyurethane electrospun fiber membrane, 5.5g of 1, 7-octadiene, 110g of water, and 5.775g of ditert-butyl peroxide were mixed and crosslinked at 25 ℃ for 0.5h to obtain a crosslinked polyvinylpyrrolidone/polyurethane electrospun fiber membrane.

The crosslinked polyvinylpyrrolidone/polyurethane electrospun fiber membrane obtained in this example was used to separate a mixture of cyclohexane and water with a separation efficiency of 98% or more.

Example 6

Weighing 18g of polyvinylpyrrolidone, 180g of polyvinylidene fluoride and 1980g of dimethyl sulfoxide, mixing, stirring at the speed of 320rpm at 60 ℃ for 12 hours, and carrying out ultrasonic treatment at the power of 38kHz at 60 ℃ for 1 hour after stirring is finished to obtain a spinning solution;

using a 15mL injector, wherein the inner diameter of a needle of the injector is 0.41mm, the outer diameter of the needle is 0.71mm, extracting a spinning solution, controlling the voltage of electrostatic spinning to be 15KV, the injection speed to be 0.02mm/min, coating an aluminum foil on a receiving roller by a receiving device, controlling the distance between the spinning needle and the receiving roller to be 15cm, the rotating speed of the receiving roller to be 100r/min, the translation speed of the needle of the electrostatic spinning to be 300mm/min, the translation stroke of the electrostatic spinning to be 520mm, the spinning temperature to be 25 ℃, and the relative humidity to be 35%, and obtaining the polyvinylpyrrolidone/polyvinylidene fluoride electrostatic spinning fiber membrane by electrostatic spinning;

and mixing the obtained polyvinylpyrrolidone/polyvinylidene fluoride electrostatic spinning fiber membrane, 1.98g of 1, 7-octadiene, 198g of water and 1.9998g of dibenzoyl peroxide, and crosslinking at 25 ℃ for 1h to obtain the crosslinked polyvinylpyrrolidone/polyvinylidene fluoride electrostatic spinning fiber membrane.

The crosslinked polyvinylpyrrolidone/polyvinylidene fluoride electrospun fiber membrane obtained in the example is used for separating a mixture of n-hexane and water, and the separation efficiency is more than 98%.

Example 7

Weighing 8g of polyvinylpyrrolidone, 160g of polymethyl methacrylate and 1680g of N, N-dimethylformamide, mixing, stirring at the speed of 600rpm at 60 ℃ for 12 hours, and performing ultrasonic treatment at the power of 40kHz at 60 ℃ for 1 hour after stirring to obtain a spinning solution;

using a 15mL injector, wherein the inner diameter of a syringe needle is 0.41mm, the outer diameter of the syringe needle is 0.71mm, extracting a spinning solution, controlling the voltage of electrostatic spinning to be 20KV, the injection speed to be 0.03mm/min, coating an aluminum foil on a receiving roller by using a receiving device, controlling the distance between the spinning needle and the receiving roller to be 15cm, the rotating speed of the receiving roller to be 100r/min, the translation speed of the electrostatic spinning needle to be 280mm/min, the translation stroke of the electrostatic spinning to be 510mm, the spinning temperature to be 25 ℃, and the relative humidity to be 35%, and obtaining the polyvinylpyrrolidone/polymethyl methacrylate electrostatic spinning fiber membrane by electrostatic spinning;

the obtained polyvinylpyrrolidone/polymethyl methacrylate electrospun fiber membrane, 3.36g of alkylene bisacrylamide, 168g of water, and 3.4272g of azobisisobutyronitrile were mixed and crosslinked at 25 ℃ for 1 hour to obtain a crosslinked polyvinylpyrrolidone/polymethyl methacrylate electrospun fiber membrane.

The crosslinked polyvinylpyrrolidone/polymethyl methacrylate electrospun fiber membrane obtained in the example is used for separating the mixture of the engine oil and the water, and the separation efficiency is more than 98%.

Example 8

Weighing 23g of polyvinylpyrrolidone, 115g of polystyrene and 1380g of dimethyl sulfoxide, mixing, stirring at 550rpm for 18 hours at 40 ℃, and carrying out ultrasonic treatment at 38kHz for 1 hour at 40 ℃ after stirring is finished to obtain a spinning solution;

using a 15mL injector, wherein the inner diameter of a syringe needle is 0.41mm, the outer diameter of the syringe needle is 0.71mm, extracting a spinning solution, controlling the voltage of electrostatic spinning to be 12KV, the injection speed to be 0.02mm/min, coating an aluminum foil on a receiving roller by a receiving device, controlling the distance between the spinning needle and the receiving roller to be 10cm, the rotating speed of the receiving roller to be 100r/min, the translation speed of the electrostatic spinning needle to be 320mm/min, the translation stroke of the electrostatic spinning to be 480mm, the spinning temperature to be 25 ℃, and the relative humidity to be 35%, and obtaining the polyvinylpyrrolidone/polystyrene electrostatic spinning fiber membrane by electrostatic spinning;

the obtained polyvinylpyrrolidone/polystyrene electrospun fiber membrane, 4.14g of divinylbenzene, 138g of water, and 4.2642g of azobisisobutyronitrile were mixed and crosslinked at 30 ℃ for 1 hour to obtain a crosslinked polyvinylpyrrolidone/polystyrene electrospun fiber membrane.

The crosslinked polyvinylpyrrolidone/polystyrene electrospun fiber membrane obtained in the example is used for separating the mixture of trichloromethane and water, and the separation efficiency is more than 98%.

Example 9

Weighing 5g of polyvinylpyrrolidone, 100g of poly (arylene ether nitrile) and 1050g of N, N-dimethylformamide, mixing, stirring at the speed of 400rpm at 25 ℃ for 18 hours, and performing ultrasonic treatment at the power of 42kHz at 25 ℃ for 1 hour after stirring to obtain a spinning solution;

using a 15mL injector, wherein the inner diameter of a syringe needle is 0.41mm, the outer diameter of the syringe needle is 0.71mm, extracting a spinning solution, controlling the voltage of electrostatic spinning to be 14KV, the injection speed to be 0.03mm/min, coating an aluminum foil on a receiving roller by using a receiving device, controlling the distance between the spinning needle and the receiving roller to be 12cm, the rotating speed of the receiving roller to be 100r/min, the translation speed of the electrostatic spinning needle to be 290mm/min, the translation stroke of the electrostatic spinning to be 515mm, the spinning temperature to be 25 ℃, and the relative humidity to be 35%, and carrying out electrostatic spinning to obtain the polyvinylpyrrolidone/polyarylene ether nitrile electrostatic spinning fiber membrane;

the resulting polyvinylpyrrolidone/polyarylene ether nitrile electrospun fiber membrane, 4.2g of divinylbenzene, 105g of water and 4.368g of dibenzoyl peroxide were mixed and crosslinked at 30 ℃ for 0.5h to obtain a crosslinked polyvinylpyrrolidone/polyarylene ether nitrile electrospun fiber membrane.

The crosslinked polyvinylpyrrolidone/polyarylene ether nitrile electrospun fiber membrane obtained in this example was used to separate a mixture of toluene and water with a separation efficiency of 96% or more.

Example 10

Weighing 14g of polyvinylpyrrolidone, 70g of cellulose and 840g of dimethylacetamide, mixing, stirring at 550rpm for 18 hours at 40 ℃, and performing ultrasonic treatment at 40 ℃ for 1 hour at 40kHz to obtain a spinning solution;

using a 15mL injector, wherein the inner diameter of a syringe needle is 0.41mm, the outer diameter of the syringe needle is 0.71mm, extracting a spinning solution, controlling the voltage of electrostatic spinning to be 17KV, the injection speed to be 0.03mm/min, coating an aluminum foil on a receiving roller by using a receiving device, controlling the distance between the spinning needle and the receiving roller to be 13cm, the rotating speed of the receiving roller to be 100r/min, the translation speed of the electrostatic spinning needle to be 310mm/min, the translation stroke of the electrostatic spinning to be 490mm, the spinning temperature to be 25 ℃, and the relative humidity to be 35%, and obtaining the polyvinylpyrrolidone/cellulose electrostatic spinning fiber membrane by electrostatic spinning;

the obtained polyvinylpyrrolidone/cellulose electrospun fiber membrane, 4.2g of 1, 7-octadiene, 84g of water and 4.41g of ditert-butyl peroxide were mixed and crosslinked at 35 ℃ for 0.5h to obtain a crosslinked polyvinylpyrrolidone/cellulose electrospun fiber membrane.

The crosslinked polyvinylpyrrolidone/cellulose electrospun fiber membrane obtained in the example is used for separating a mixture of isooctane and water, and the separation efficiency is more than 98%.

Example 11

Weighing 5g of polyvinylpyrrolidone, 50g of polylactic acid and 550g of dimethyl sulfoxide, mixing, stirring at the speed of 620rpm at 45 ℃ for 24 hours, and carrying out ultrasonic treatment at the power of 38kHz at 45 ℃ for 0.5 hour after stirring is finished to obtain a spinning solution;

using a 15mL injector, wherein the inner diameter of a syringe needle is 0.41mm, the outer diameter of the syringe needle is 0.71mm, extracting a spinning solution, controlling the voltage of electrostatic spinning to be 16KV, the injection speed to be 0.02mm/min, coating an aluminum foil on a receiving roller by using a receiving device, controlling the distance between the spinning needle and the receiving roller to be 10cm, the rotating speed of the receiving roller to be 100r/min, the translation speed of the electrostatic spinning needle to be 285mm/min, the translation stroke of the electrostatic spinning to be 510mm, the spinning temperature to be 25 ℃, and the relative humidity to be 35%, and obtaining the polyvinylpyrrolidone/polylactic acid electrostatic spinning fiber membrane by electrostatic spinning;

the obtained polyvinylpyrrolidone/polylactic acid electrospun fiber membrane, 0.55g of alkylene bisacrylamide, 55g of water, and 0.5555g of azobisisobutyronitrile were mixed and crosslinked at 35 ℃ for 1 hour to obtain a crosslinked polyvinylpyrrolidone/polylactic acid electrospun fiber membrane.

The crosslinked polyvinylpyrrolidone/polylactic acid electrospun fiber membrane obtained in the example is used for separating the mixture of carbon tetrachloride and water, and the separation efficiency is more than 98%.

Example 12

Weighing 23g of polyvinylpyrrolidone, 230g of cellulose acetate and 2530g of dimethylacetamide, mixing, stirring at the speed of 450rpm for 18 hours at 50 ℃, and performing ultrasonic treatment at the power of 35kHz for 1 hour at 50 ℃ after stirring to obtain a spinning solution;

using a 15mL injector, wherein the inner diameter of a syringe needle is 0.41mm, the outer diameter of the syringe needle is 0.71mm, extracting a spinning solution, controlling the voltage of electrostatic spinning to be 18KV, the injection speed to be 0.02mm/min, coating an aluminum foil on a receiving roller by using a receiving device, controlling the distance between the spinning needle and the receiving roller to be 14cm, the rotating speed of the receiving roller to be 100r/min, the translation speed of the electrostatic spinning needle to be 320mm/min, the translation stroke of the electrostatic spinning to be 480mm, the spinning temperature to be 25 ℃, and the relative humidity to be 35%, and obtaining the polyvinylpyrrolidone/cellulose acetate electrostatic spinning fiber membrane by electrostatic spinning;

the obtained polyvinylpyrrolidone/cellulose acetate electrospun fiber membrane, 5.06g of potassium persulfate, 253g of water and 5.1612g of ditert-butyl peroxide were mixed and crosslinked at 90 ℃ for 8 hours to obtain a crosslinked polyvinylpyrrolidone/cellulose acetate electrospun fiber membrane.

The crosslinked polyvinylpyrrolidone/cellulose acetate electrospun fiber membrane obtained in this example was used to separate a mixture of chloroform and water with a separation efficiency of 98% or more.

Example 13

Weighing 10g of polyvinylpyrrolidone, 50g of polyacrylonitrile and 600g of N, N-dimethylformamide, mixing, stirring at the speed of 750rpm for 24 hours at the temperature of 30 ℃, and carrying out ultrasonic treatment at the power of 42kHz for 0.5 hour at the temperature of 30 ℃ after stirring is finished to obtain a spinning solution;

using a 15mL injector, wherein the inner diameter of a syringe needle is 0.41mm, the outer diameter of the syringe needle is 0.71mm, extracting a spinning solution, controlling the voltage of electrostatic spinning to be 18KV, the injection speed to be 0.02mm/min, coating an aluminum foil on a receiving roller by using a receiving device, controlling the distance between the spinning needle and the receiving roller to be 14cm, the rotating speed of the receiving roller to be 100r/min, the translation speed of the electrostatic spinning needle to be 320mm/min, the translation stroke of the electrostatic spinning to be 480mm, the spinning temperature to be 25 ℃, and the relative humidity to be 35%, and obtaining the polyvinylpyrrolidone/polyacrylonitrile electrostatic spinning fiber membrane by electrostatic spinning;

the obtained polyvinylpyrrolidone/polyacrylonitrile electrospun fiber membrane, 1.8g of divinylbenzene, 60g of water, and 1.854g of ditert-butyl peroxide were mixed and crosslinked at 30 ℃ for 2 hours to obtain a crosslinked polyvinylpyrrolidone/polyacrylonitrile electrospun fiber membrane.

The crosslinked polyvinylpyrrolidone/polyacrylonitrile electrospun fiber membrane obtained in the embodiment is used for separating the mixture of isooctane and water, and the separation efficiency is more than 98%.

Example 14

Weighing 15g of polyvinylpyrrolidone, 150g of polyethersulfone and 1650g of dimethylacetamide, mixing, stirring at the speed of 600rpm at 25 ℃ for 24 hours, and carrying out ultrasonic treatment at the power of 38kHz at 25 ℃ for 1 hour after stirring to obtain a spinning solution;

using a 15mL injector, wherein the inner diameter of a syringe needle is 0.41mm, the outer diameter of the syringe needle is 0.71mm, extracting a spinning solution, controlling the voltage of electrostatic spinning to be 15KV, the injection speed to be 0.02mm/min, coating an aluminum foil on a receiving roller by a receiving device, controlling the distance between the spinning needle and the receiving roller to be 15cm, the rotating speed of the receiving roller to be 100r/min, the translation speed of the electrostatic spinning needle to be 285mm/min, the translation stroke of the electrostatic spinning to be 500mm, the spinning temperature to be 25 ℃, and the relative humidity to be 35%, and obtaining the polyvinylpyrrolidone/polyethersulfone electrostatic spinning fiber membrane by electrostatic spinning;

and mixing the obtained polyvinylpyrrolidone/polyether sulfone electrospun fiber membrane, 6.6g of ammonium persulfate, 165g of water and 6.864g of azobisisobutyronitrile, and crosslinking at 90 ℃ for 6 hours to obtain the crosslinked polyvinylpyrrolidone/polyether sulfone electrospun fiber membrane.

The crosslinked polyvinylpyrrolidone/polyethersulfone electrospun fiber membrane obtained in the example is used for separating the mixture of toluene and water, and the separation efficiency is more than 98%.

Example 15

Weighing 5g of polyvinylpyrrolidone, 50g of polyurethane and 550g of N, N-dimethylformamide, mixing, stirring at 480rpm for 24 hours at 25 ℃, and performing ultrasonic treatment at 42kHz for 2 hours at 25 ℃ to obtain a spinning solution;

using a 15mL injector, wherein the inner diameter of a syringe needle is 0.41mm, the outer diameter of the syringe needle is 0.71mm, extracting a spinning solution, controlling the voltage of electrostatic spinning to be 18KV, the injection speed to be 0.02mm/min, coating an aluminum foil on a receiving roller by using a receiving device, controlling the distance between the spinning needle and the receiving roller to be 14cm, the rotating speed of the receiving roller to be 100r/min, the translation speed of the electrostatic spinning needle to be 295mm/min, the translation stroke of the electrostatic spinning to be 505mm, the spinning temperature to be 25 ℃, and the relative humidity to be 35%, and obtaining the polyvinylpyrrolidone/polyurethane electrostatic spinning fiber membrane by electrostatic spinning;

the obtained polyvinylpyrrolidone/polyurethane electrospun fiber membrane, 2.75g of sodium persulfate, 55g of water, and 2.8875g of azobisisobutyronitrile were mixed and crosslinked at 75 ℃ for 5 hours to obtain a crosslinked polyvinylpyrrolidone/polyurethane electrospun fiber membrane.

The crosslinked polyvinylpyrrolidone/polyurethane electrospun fiber membrane obtained in the example is used for separating the mixture of trichloromethane and water, and the separation efficiency is more than 98%.

Example 16

Weighing 8g of polyvinylpyrrolidone, 40g of polyvinylidene fluoride and 480g of dimethyl sulfoxide, mixing, stirring at the speed of 400rpm at 60 ℃ for 12 hours, and carrying out ultrasonic treatment at the power of 35kHz at 60 ℃ for 1 hour after stirring to obtain a spinning solution;

using a 15mL injector, wherein the inner diameter of a syringe needle is 0.41mm, the outer diameter of the syringe needle is 0.71mm, extracting a spinning solution, controlling the voltage of electrostatic spinning to be 15KV, the injection speed to be 0.03mm/min, coating an aluminum foil on a receiving roller by using a receiving device, controlling the distance between the spinning needle and the receiving roller to be 10cm, the rotating speed of the receiving roller to be 100r/min, the translation speed of the electrostatic spinning needle to be 290mm/min, the translation stroke of the electrostatic spinning to be 510mm, the spinning temperature to be 25 ℃, and the relative humidity to be 35%, and obtaining the polyvinylpyrrolidone/polyvinylidene fluoride electrostatic spinning fiber membrane by electrostatic spinning;

the obtained polyvinylpyrrolidone/polyvinylidene fluoride electrospun fiber membrane, 0.48g of sodium persulfate, 48g of water and 0.4848g of ditert-butyl peroxide were mixed and crosslinked at 90 ℃ for 6 hours to obtain a crosslinked polyvinylpyrrolidone/polyvinylidene fluoride electrospun fiber membrane.

The crosslinked polyvinylpyrrolidone/polyvinylidene fluoride electrostatic spinning fiber membrane obtained in the embodiment is used for separating the mixture of petroleum ether and water, and the separation efficiency is more than 98%.

Example 17

Weighing 10g of polyvinylpyrrolidone, 100g of polymethyl methacrylate and 1100g of N, N-dimethylformamide, mixing, stirring at 680rpm for 12 hours at 60 ℃, and performing ultrasonic treatment at 44kHz for 1 hour at 60 ℃ after stirring to obtain a spinning solution;

using a 15mL injector, wherein the inner diameter of a syringe needle is 0.41mm, the outer diameter of the syringe needle is 0.71mm, extracting a spinning solution, controlling the voltage of electrostatic spinning to be 18KV, the injection speed to be 0.03mm/min, coating an aluminum foil on a receiving roller by using a receiving device, controlling the distance between the spinning needle and the receiving roller to be 15cm, the rotating speed of the receiving roller to be 100r/min, the translation speed of the electrostatic spinning needle to be 320mm/min, the translation stroke of the electrostatic spinning to be 500mm, the spinning temperature to be 25 ℃, and the relative humidity to be 35%, and obtaining the polyvinylpyrrolidone/polymethyl methacrylate electrostatic spinning fiber membrane by electrostatic spinning;

the obtained polyvinylpyrrolidone/polymethyl methacrylate electrospun fiber membrane, 2.2g of alkylene bisacrylamide, 110g of water, and 2.244g of azobisisobutyronitrile were mixed and crosslinked at 25 ℃ for 1 hour to obtain a crosslinked polyvinylpyrrolidone/polymethyl methacrylate electrospun fiber membrane.

The crosslinked polyvinylpyrrolidone/polymethyl methacrylate electrospun fiber membrane obtained in this example was used to separate a mixture of cyclohexane and water with a separation efficiency of 98% or more.

Example 18

Weighing 12g of polyvinylpyrrolidone, 240g of polystyrene and 2520g of dimethyl sulfoxide, mixing, stirring at the speed of 600rpm at 40 ℃ for 18 hours, and carrying out ultrasonic treatment at the temperature of 40 ℃ for 1 hour at the power of 35kHz to obtain a spinning solution;

using a 15mL injector, wherein the inner diameter of a syringe needle is 0.41mm, the outer diameter of the syringe needle is 0.71mm, extracting a spinning solution, controlling the voltage of electrostatic spinning to be 15KV, the injection speed to be 0.02mm/min, coating an aluminum foil on a receiving roller by a receiving device, controlling the distance between the spinning needle and the receiving roller to be 11cm, the rotating speed of the receiving roller to be 100r/min, the translation speed of the electrostatic spinning needle to be 300mm/min, the translation stroke of the electrostatic spinning to be 500mm, the spinning temperature to be 25 ℃, and the relative humidity to be 35%, and obtaining the polyvinylpyrrolidone/polystyrene electrostatic spinning fiber membrane by electrostatic spinning;

the obtained polyvinylpyrrolidone/polystyrene electrospun fiber membrane, 7.56g of divinylbenzene, 252g of water, and 7.7868g of azobisisobutyronitrile were mixed and crosslinked at 30 ℃ for 1 hour to obtain a crosslinked polyvinylpyrrolidone/polystyrene electrospun fiber membrane.

The crosslinked polyvinylpyrrolidone/polystyrene electrospun fiber membrane obtained in the example is used for separating a mixture of n-hexane and water, and the separation efficiency is more than 98%.

Example 19

Weighing 2g of polyvinylpyrrolidone, 20g of poly (arylene ether nitrile) and 220g of N, N-dimethylformamide, mixing, stirring at the speed of 700rpm at 25 ℃ for 18 hours, and performing ultrasonic treatment at the power of 45kHz at 25 ℃ for 1 hour after stirring to obtain a spinning solution;

using a 15mL injector, wherein the inner diameter of a syringe needle is 0.41mm, the outer diameter of the syringe needle is 0.71mm, extracting a spinning solution, controlling the voltage of electrostatic spinning to be 17KV, the injection speed to be 0.03mm/min, coating an aluminum foil on a receiving roller by using a receiving device, controlling the distance between the spinning needle and the receiving roller to be 13cm, the rotating speed of the receiving roller to be 100r/min, the translation speed of the electrostatic spinning needle to be 315mm/min, the translation stroke of the electrostatic spinning to be 505mm, the spinning temperature to be 25 ℃, and the relative humidity to be 35%, and carrying out electrostatic spinning to obtain the polyvinylpyrrolidone/polyarylene ether nitrile electrostatic spinning fiber membrane;

the resulting polyvinylpyrrolidone/polyarylene ether nitrile electrospun fiber membrane, 0.88g of divinylbenzene, 22g of water and 0.9152g of dibenzoyl peroxide were mixed and crosslinked at 30 ℃ for 0.5h to yield a crosslinked polyvinylpyrrolidone/polyarylene ether nitrile electrospun fiber membrane.

The crosslinked polyvinylpyrrolidone/polyarylene ether nitrile electrospun fiber membrane obtained in the example was used to separate a mixture of engine oil and water with a separation efficiency of 96% or more.

Example 20

Weighing 15g of polyvinylpyrrolidone, 300g of cellulose and 3150g of dimethylacetamide, mixing, stirring at the speed of 450rpm for 18 hours at 40 ℃, and carrying out ultrasonic treatment at the power of 35kHz for 1 hour at 40 ℃ after stirring is finished to obtain a spinning solution;

using a 15mL injector, wherein the inner diameter of a syringe needle is 0.41mm, the outer diameter of the syringe needle is 0.71mm, extracting a spinning solution, controlling the voltage of electrostatic spinning to be 18KV, the injection speed to be 0.03mm/min, coating an aluminum foil on a receiving roller by using a receiving device, controlling the distance between the spinning needle and the receiving roller to be 13cm, the rotating speed of the receiving roller to be 100r/min, the translation speed of the electrostatic spinning needle to be 280mm/min, the translation stroke of the electrostatic spinning to be 510mm, the spinning temperature to be 25 ℃, and the relative humidity to be 35%, and obtaining the polyvinylpyrrolidone/cellulose electrostatic spinning fiber membrane by electrostatic spinning;

the obtained polyvinylpyrrolidone/cellulose electrospun fiber membrane, 15.75g of sodium persulfate, 315g of water, and 16.5375g of di-tert-butyl peroxide were mixed and crosslinked at 90 ℃ for 4 hours to obtain a crosslinked polyvinylpyrrolidone/cellulose electrospun fiber membrane.

The crosslinked polyvinylpyrrolidone/cellulose electrospun fiber membrane obtained in the embodiment is used for separating the mixture of diesel oil and water, and the separation efficiency is more than 98%.

Example 21

Weighing 8g of polyvinylpyrrolidone, 40g of polylactic acid and 480g of dimethyl sulfoxide, mixing, stirring at the speed of 300rpm at 45 ℃ for 24 hours, and carrying out ultrasonic treatment at the power of 45kHz at 45 ℃ for 0.5 hour after stirring to obtain a spinning solution;

using a 15mL injector, wherein the inner diameter of a syringe needle is 0.41mm, the outer diameter of the syringe needle is 0.71mm, extracting a spinning solution, controlling the voltage of electrostatic spinning to be 14KV, the injection speed to be 0.02mm/min, coating an aluminum foil on a receiving roller by using a receiving device, controlling the distance between the spinning needle and the receiving roller to be 10cm, the rotating speed of the receiving roller to be 100r/min, the translation speed of the electrostatic spinning needle to be 300mm/min, the translation stroke of the electrostatic spinning to be 500mm, the spinning temperature to be 25 ℃, and the relative humidity to be 35%, and obtaining the polyvinylpyrrolidone/polylactic acid electrostatic spinning fiber membrane by electrostatic spinning;

the obtained polyvinylpyrrolidone/polylactic acid electrospun fiber membrane, 0.48g of alkylene bisacrylamide, 48g of water, and 0.4848g of azobisisobutyronitrile were mixed and crosslinked at 35 ℃ for 1 hour to obtain a crosslinked polyvinylpyrrolidone/polylactic acid electrospun fiber membrane.

The crosslinked polyvinylpyrrolidone/polylactic acid electrospun fiber membrane obtained in the example is used for separating the mixture of kerosene and water, and the separation efficiency is more than 98%.

Example 22

Weighing 10g of polyvinylpyrrolidone, 50g of cellulose acetate and 600g of dimethylacetamide, mixing, stirring at the speed of 600rpm at 40 ℃ for 24 hours, and performing ultrasonic treatment at 40 ℃ for 1.5 hours at the power of 40kHz to obtain a spinning solution after stirring;

using a 15mL injector, wherein the inner diameter of a syringe needle is 0.41mm, the outer diameter of the syringe needle is 0.71mm, extracting a spinning solution, controlling the voltage of electrostatic spinning to be 18KV, the injection speed to be 0.03mm/min, coating an aluminum foil on a receiving roller by using a receiving device, controlling the distance between the spinning needle and the receiving roller to be 16cm, the rotating speed of the receiving roller to be 100r/min, the translation speed of the electrostatic spinning needle to be 300mm/min, the translation stroke of the electrostatic spinning to be 500mm, the spinning temperature to be 25 ℃, and the relative humidity to be 35%, and obtaining the polyvinylpyrrolidone/cellulose acetate electrostatic spinning fiber membrane by electrostatic spinning;

the obtained polyvinylpyrrolidone/cellulose acetate electrospun fiber membrane, 0.96g of alkylene bisacrylamide, 48g of water, and 0.9792g of azobisisobutyronitrile were mixed and crosslinked at 90 ℃ for 8 hours to obtain a crosslinked polyvinylpyrrolidone/cellulose acetate electrospun fiber membrane.

The crosslinked polyvinylpyrrolidone/cellulose acetate electrostatic spinning fiber membrane obtained in the embodiment is used for separating the mixture of gasoline and water, and the separation efficiency is more than 98%.

According to the embodiments, the invention provides a crosslinked electrospun fiber membrane, which is prepared by combining hydrophilic polyvinylpyrrolidone with a high molecular polymer by using an electrospinning technology, and then stabilizing the combination through chemical crosslinking, wherein the crosslinked polyvinylpyrrolidone/high molecular polymer fiber membrane with excellent oil-water separation performance is obtained by regulating and controlling the ratio of polyvinylpyrrolidone to high molecular polymer, the spinning conditions and the crosslinking conditions. The cross-linked electrostatic spinning fiber membrane provided by the invention can effectively separate an oil-water mixture and an oil-in-water emulsion, and brings a new direction for the purification of water environment and the sustainable development of water resources.

The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.

Claims (10)

1. A preparation method of a cross-linked electrostatic spinning fiber membrane is characterized by comprising the following steps:

(1) mixing a polymer A, a polymer B and a solvent to obtain a spinning solution;

(2) carrying out electrostatic spinning on the spinning solution to obtain an electrostatic spinning fiber membrane;

(3) mixing the electrostatic spinning fiber membrane, an initiator, a cross-linking agent and a solvent, and then carrying out a cross-linking reaction to obtain a cross-linked electrostatic spinning fiber membrane;

the polymer A is polyvinylpyrrolidone;

the polymer B is polyacrylonitrile, polyether sulfone, polyurethane, polyvinylidene fluoride, polystyrene, polymethyl methacrylate, polyaniline, polyarylene ether nitrile, cellulose, polylactic acid or cellulose acetate.

2. The production method according to claim 1, wherein the mass ratio of the polymer B to the polymer a in the step (1) is 1: 0.05 to 0.2;

the mass ratio of the sum of the mass of the polymer B and the mass of the polymer A to the mass of the solvent is 0.08-0.12: 1;

the solvent is N, N-dimethylformamide, dimethyl sulfoxide, dimethylacetamide, chlorobenzene, chloroform, acetone, dichloromethane or trichloromethane.

3. The production method according to claim 2, wherein the mixing in the step (1) is stirring and sonication performed in sequence;

the stirring speed is 300-800 rpm, the stirring time is 12-24 hours, and the stirring temperature is 18-60 ℃;

the power of the ultrasound is 35-45 kHz, the time of the ultrasound is 0.5-2 h, and the temperature of the ultrasound is 18-60 ℃.

4. The preparation method according to any one of claims 1 to 3, wherein the device used in the electrospinning in the step (2) is a syringe, the syringe has a size of 5 to 20mL, the inner diameter of the needle of the syringe is 0.39 to 0.43mm, and the outer diameter of the needle of the syringe is 0.69 to 0.73 mm.

5. The preparation method according to claim 4, wherein the voltage of the electrospinning in the step (2) is 8-20 KV, the bolus velocity of the electrospinning is 0.2-0.4 mm/min, the needle translation velocity of the electrospinning is 280-320 mm/min, the translation stroke of the electrospinning is 480-520 mm, the distance between the needle of the electrospinning and the receiving roller is 8-20 cm, and the rotation speed of the receiving roller is 80-120 rpm.

6. The preparation method according to claim 1, wherein the mass ratio of the crosslinking agent to the solvent in the step (3) is 0.01 to 0.05: 1; the mass ratio of the electrostatic spinning fiber membrane to the cross-linking agent is 1: 0.01 to 0.05; the mass ratio of the mass sum of the electrostatic spinning fiber membrane and the cross-linking agent to the mass sum of the initiator is 1: 0.01 to 0.05;

the crosslinking agent is persulfate, 1, 7-octadiene, alkylene bisacrylamide or a divinylaromatic compound;

the persulfate is ammonium persulfate, potassium persulfate or sodium persulfate;

the divinylaromatic compound is divinylbenzene or divinylethylbenzene;

the initiator is peroxide or azobisisobutyronitrile;

the peroxide is dibenzoyl peroxide or ditert-butyl peroxide.

7. The method according to claim 1, 2, 3, 5 or 6, wherein the temperature of the crosslinking reaction in the step (3) is 15 to 90 ℃ and the time of the crosslinking reaction is 0.5 to 9 hours.

8. The crosslinked electrospun fiber membrane obtained by the preparation method of any one of claims 1 to 7.

9. Use of the cross-linked electrospun fiber membrane of claim 8 for separating oil from water.

10. The use of claim 9, wherein the oil-water is an oil-water mixture or an oil-in-water emulsion;

the diameter of the oil-in-water emulsion is 100-500 nm;

the type of the oil in the separated oil water is one or more of gasoline, kerosene, diesel oil, engine oil, normal hexane, cyclohexane, petroleum ether, trichloromethane, toluene, isooctane, carbon tetrachloride and chloroform.

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