A nanofiber liquid chromatography separation material and preparation method thereof

Abstract

The present invention provides a nanofiber liquid chromatography separation material and a preparation method thereof, the preparation method comprising the following steps: S1, hydrolyzing an inorganic oxide precursor in a solvent and mixing it with a porogen; S2, electrospinning the mixed solution into nanofiber filaments; S3, washing and sintering the nanofiber filaments, removing the porogen, and forming a porous nanofiber membrane; S4, crushing the nanofiber membrane into nanofiber powder; S5, modifying a chromatographic stationary phase on the surface of the nanofiber powder to obtain a nanofiber liquid chromatography separation material. The present invention prepares porous nanofibers by adding a porogen and using electrospinning technology, which can increase the specific surface area of ​​the material and reduce the fiber diameter, and crushes the porous nanofibers into fiber powder, and modifies the chromatographic stationary phase on the surface as a liquid chromatography separation material. Compared with conventional spherical liquid chromatography separation materials, the fiber powder separation material has lower fluid resistance, shorter mass transfer distance, and higher separation efficiency.

Description

Technical Field

[0001] The invention relates to the technical field of liquid chromatography separation materials, and in particular to a nanofiber liquid chromatography separation material and a preparation method thereof. Background Art

[0002] Liquid chromatography fillers are solid materials used to separate substances in liquid chromatography columns. They have a variety of forms, including irregular particles, porous particles, core-shell particles, fibrous materials, membrane materials, monolithic columns, etc., in addition to common microspheres. These different forms provide flexibility for specific separation needs and can meet the separation challenges of different samples. The choice of filler form usually depends on the nature of the analyte, the separation target, and the chromatographic technology used.

[0003] At present, the development of conventional chromatographic materials has encountered great challenges. Irregular particle fillers were once common in early chromatographic systems, but their separation efficiency was much lower than that of microsphere materials. The overall column material has good permeability, but it is difficult to prepare and has poor repeatability. Core-shell particles have a solid or non-porous core and a porous shell. Their design purpose is to provide a faster molecular diffusion path and reduce the bandwidth of molecular diffusion, but the synthesis of core-shell materials is extremely difficult and difficult to popularize. In short, for particulate materials, in order to reduce the mass transfer distance and improve the separation efficiency, the diameter of the microspheres needs to be further reduced, which will bring extremely high chromatographic separation pressure. At present, conventional 2μm chromatographic columns usually need to be operated at a column pressure of 100MPa; if the particle size of the microspheres is reduced to below 1μm, it needs to be operated at a column pressure of 200MPa, which brings great challenges to all components of the entire liquid chromatography system.

[0004] Compared with granular chromatographic separation materials, fiber materials have larger pores, which can significantly reduce fluid resistance. Prior art US20060201881A1 discloses a fiber-based liquid chromatography separation material, which uses high molecular polymer micron fibers with a fiber diameter of more than 10 μm, and is filled into a chromatographic column in the form of fiber bundles, resulting in low separation efficiency, and the fiber itself has a small specific surface area and a small sample capacity, resulting in an overall separation performance far inferior to that of traditional chromatographic microspheres. Summary of the invention

[0005] In view of the shortcomings of the prior art, the technical problem to be solved by the present invention is how to increase the specific surface area of ​​fiber-based liquid chromatography separation materials, reduce the fiber diameter, and improve the separation efficiency.

[0006] To achieve the above object, the present invention provides a method for preparing a nanofiber liquid chromatography separation material, comprising the following steps:

[0007] S1, hydrolyzing an inorganic oxide precursor in a solvent and mixing it with a porogen to form a uniform mixed solution;

[0008] S2, electrospinning the mixed solution into nanofiber filaments;

[0009] S3, washing and sintering the nanofiber filaments to remove the porogen and form a porous nanofiber membrane;

[0010] S4, crushing the nanofiber membrane into nanofiber powder;

[0011] S5. Screen out nanofiber powder of suitable specifications, and modify the chromatographic stationary phase on the surface of the nanofiber powder to obtain a nanofiber liquid chromatography separation material.

[0012] The present invention prepares porous nanofibers by adding porogens and electrospinning technology, which can increase the specific surface area of ​​the material, reduce the fiber diameter, and crush the porous nanofibers into fiber powders, modify the chromatographic stationary phase on the surface, and use them as liquid chromatography separation materials. Compared with conventional spherical liquid chromatography separation materials, the fiber powder separation material has lower fluid resistance, shorter mass transfer distance, and higher separation efficiency.

[0013] In a preferred or optional embodiment, in step S2, the diameter of the nanofiber filament is 50nm-2000nm, preferably 200nm-1000nm, and more preferably 300nm-800nm. Nanofibers have a small diameter and a short mass transfer distance, so rapid separation can be achieved.

[0014] In a preferred or optional embodiment, in step S3, the surface pore size of the nanofiber membrane is 2nm~100nm, preferably 5nm~30nm, and the specific surface area is 20m 2 / g~800m 2 / g, preferably 200m 2 / g~500m 2 / g. The porosity and pore size in the nanofibers can be adjusted to increase the specific surface area of ​​the material and improve the separation effect.

[0015] In a preferred or optional embodiment, in step S5, the length of the nanofiber powder obtained by sieving is 1 μm to 100 μm, preferably 5 μm to 20 μm. The nanofiber powder can be directly filled into a chromatographic column for use, increasing the number of separation plates and improving separation efficiency.

[0016] In a preferred or optional embodiment, in step S1, the inorganic oxide is selected from at least one of silicon dioxide, zirconium oxide, aluminum oxide, titanium oxide, magnesium oxide, cerium oxide, and zinc oxide. The nanofibers used in the present invention have a wide range of materials, extending to various inorganic oxide systems.

[0017] In a preferred or optional embodiment, in step S1, the porogen is selected from at least one of polyethylene oxide, polymethyl pyrrolidone, polyacrylonitrile, polymethyl methacrylate, and polyimide.

[0018] In a preferred or optional embodiment, in the step S3, the sintering temperature is lower than the melting point of the inorganic oxide, and the difference is above 100°C, preferably above 200°C.

[0019] By removing the porogen of the polymer material through sintering, the surface of the nanofiber can have a uniformly distributed porous structure, thereby increasing the specific surface area of ​​the material.

[0020] In a preferred or optional embodiment, in step S1, the solvent is selected from at least one of water, alcohol, ester, amide, sulfoxide, and nitrogen methyl pyrrolidone.

[0021] In a preferred or optional embodiment, in step S5, the chromatographic stationary phase is selected from at least one of a reverse phase chromatographic stationary phase, a hydrophilic chromatographic stationary phase, a chiral chromatographic stationary phase, and an ion pair chromatographic stationary phase. The chromatographic stationary phase is directly modified on the surface of the nanofiber to achieve selective adsorption and separation of specific substances.

[0022] The present invention also provides a nanofiber liquid chromatography separation material, which is prepared by the above preparation method. Compared with conventional microspherical chromatography separation materials, the nanofiber liquid chromatography separation material of the present invention has the advantages of high fiber filling porosity, low fluid back pressure, shorter mass transfer distance, and high separation efficiency.

[0023] Compared with the prior art, the present invention has the following beneficial effects:

[0024] (1) The mass transfer distance of the nanofiber liquid chromatography separation material of the present invention is short: as the diameter of the nanofiber decreases, the corresponding mass transfer distance shortens; if the diameter of the nanofiber is around 500 nm, the mass transfer distance is shortened by 10 times compared with conventional 5 μm microspheres, and by 2.5 times compared with 2.5 μm core-shell microspheres.

[0025] (2) The nanofiber liquid chromatography separation material of the present invention has a large specific surface area: by adding a porogen, uniform nanopores are formed on the surface of the nanofiber, thereby increasing the specific surface area of ​​the material.

[0026] (3) The nanofiber liquid chromatography separation material of the present invention has high separation efficiency: the material's specific surface area is greatly increased and the mass transfer distance is shortened, both of which are conducive to improving the separation efficiency. The number of chromatographic separation plates of the nanofiber can reach 1 million per meter.

[0027] (4) The fluid resistance of the nanofiber liquid chromatography separation material of the present invention is small: the interfiber pores of the nanofibers are large, and the fluid resistance is significantly reduced compared with nanomicrospheres. BRIEF DESCRIPTION OF THE DRAWINGS

[0028] Figure 1 This is an electron microscope image of the silicon dioxide nanofiber powder in Example 1.

[0029] Figure 2 This is the nitrogen adsorption curve of the silicon dioxide nanofiber powder in Example 1.

[0030] Figure 3 This is the chromatogram of the separation of alkylbenzenes by the nanofiber liquid chromatography column in Example 1. DETAILED DESCRIPTION

[0031] In order to make the above-mentioned purposes, features and advantages of the present invention more obvious and easy to understand, the specific embodiments of the present invention are described in detail below in conjunction with the accompanying drawings. It should be noted that the following embodiments are only used to illustrate the implementation method and typical parameters of the present invention, and are not used to limit the parameter range described in the present invention. Reasonable changes derived therefrom are still within the scope of protection of the claims of the present invention.

[0032] It should be noted that the endpoints and any values ​​of the ranges disclosed in this article are not limited to the precise ranges or values, and these ranges or values ​​should be understood to include values ​​close to these ranges or values. For numerical ranges, the endpoint values ​​of each range, the endpoint values ​​of each range and the individual point values, and the individual point values ​​can be combined with each other to obtain one or more new numerical ranges, and these numerical ranges should be regarded as specifically disclosed in this article.

[0033] The specific embodiment of the present invention provides a nanofiber liquid chromatography separation material and a preparation method thereof, comprising the following steps:

[0034] S1. The inorganic oxide precursor is hydrolyzed in a solvent and mixed with a porogen to form a uniform mixed solution.

[0035] In a specific embodiment, the inorganic oxide may be selected from silicon dioxide, zirconium oxide, aluminum oxide, titanium oxide, magnesium oxide, cerium oxide, zinc oxide, etc., preferably silicon oxide, zirconium oxide, and aluminum oxide. The precursor of silicon oxide is selected from methyl orthosilicate, ethyl orthosilicate, organosilane, etc., preferably methyl orthosilicate and ethyl orthosilicate; the precursor of zirconium oxide is selected from zirconate, preferably n-butyl zirconate; the precursor of aluminum oxide is selected from alkyl aluminum, alkoxy aluminum, preferably isopropyl aluminate.

[0036] In a specific embodiment, the solvent is selected from water, alcohol, ester, amide, sulfoxide, nitrogen methyl pyrrolidone, etc., preferably dimethylformamide and nitrogen methyl pyrrolidone.

[0037] In a specific embodiment, the porogen is selected from high molecular polymers, such as polyethylene oxide, polymethyl pyrrolidone, polyacrylonitrile, polymethyl methacrylate, polyimide, and the like.

[0038] S2. Weaving the mixed solution into nanofibers by electrospinning technology. The diameter of the nanofibers obtained by electrospinning is 50 nm to 2000 nm, preferably 200 nm to 1000 nm, and more preferably 300 nm to 800 nm.

[0039] In a specific embodiment, the atmosphere for electrospinning can be selected from air, nitrogen, humidified air, etc., preferably humidified air.

[0040] S3. Cleaning and sintering the nanofiber filaments to remove the porogen and form a stable porous nanofiber membrane.

[0041] In a specific embodiment, the sintering temperature is adjusted according to the melting point of the inorganic oxide, and needs to be lower than the melting point of the inorganic oxide, generally the difference is above 100°C, preferably the difference is above 200°C.

[0042] The surface pore size of the sintered nanofiber membrane is 2nm~100nm, preferably 5nm~30nm, and the specific surface area is 20m 2 / g~800m 2 / g, preferably 200m 2 / g~500m 2 / g.

[0043] S4, crushing the nanofiber membrane into nanofiber powder.

[0044] In a specific embodiment, the length of the nanofiber powder is 1 μm to 100 μm, preferably 5 μm to 20 μm.

[0045] S5. Screen out nanofiber powder of suitable specifications, and modify the chromatographic stationary phase on the surface of the nanofiber powder to obtain a nanofiber liquid chromatography separation material.

[0046] In a specific embodiment, the chromatographic stationary phase is selected according to the substance to be separated, and a reverse phase chromatographic stationary phase, a hydrophilic chromatographic stationary phase, a chiral chromatographic stationary phase, an ion pair chromatographic stationary phase, etc. can be selected.

[0047] The prepared nanofiber liquid chromatography separation material is filled into a chromatographic column and connected to the outside world, and its performance can be evaluated. In a specific embodiment, the nanofiber powder is pressed into a chromatographic column tube by a homogenization method, and the connection of the sieve plate and the end of the column tube is similar to that of a traditional liquid chromatography column: a sieve plate is put on the end of the column tube, and the external thread at the end of the column tube and the internal thread of the end are used to tighten the matching. After the mobile phase cleans the chromatographic column, the back pressure and separation efficiency of the chromatographic column can be tested.

[0048] The above method uses electrospinning technology to prepare porous nanofibers and crush them into fiber powder. As liquid chromatography separation materials, compared with conventional microsphere chromatography separation materials, nanofiber liquid chromatography separation materials have the following advantages: nanofibers have a wider material range and can be extended to various inorganic oxide systems; nanofibers have a shorter mass transfer distance and can be separated quickly; nanofibers have a large specific surface area and a higher separation efficiency; the inter-fiber pores of irregularly filled nanofibers are larger, and the fluid resistance is significantly reduced.

[0049] The technical solutions and effects of the present invention are described below through specific embodiments.

[0050] Example 1

[0051] The process of preparing silica nanofiber liquid chromatography separation material is as follows:

[0052] (1) Add 4.5 g of tetraethyl orthosilicate, 10 g of dimethylformamide, and 1.18 g of polyacrylonitrile into a reagent bottle, stir magnetically at room temperature for 2 h, add 0.5 g of hydrochloric acid (2 M), and stir magnetically at room temperature for 2 days to obtain an electrospinning precursor solution.

[0053] (2) Using aluminum foil as a collector, the rotating receiving drum speed was 110 rpm, the receiving distance was 10 cm, the spinning voltage was 20 kV, and the feed rate was 3 mL / min. Electrospinning was performed to obtain nanofibers with a diameter of about 400 nm.

[0054] (3) The temperature of the nanofiber filaments was raised to 150°C at a rate of 5°C / min and kept at this temperature for 2 h; the temperature was raised to 350°C at a rate of 5°C / min and kept at this temperature for 2 h; the temperature was raised to 750°C at a rate of 5°C / min and kept at this temperature for 6 h; and the temperature was lowered to obtain a sintered nanofiber membrane.

[0055] (4) Cut the sintered nanofiber membrane into pieces, put it into a grinder, grind it at 20,000 rpm for 10 min, and sieve it through a 20 μm sieve for 3 times to obtain silica nanofiber powder. The morphology of the silica nanofiber powder is as follows: Figure 1 Its nitrogen adsorption curve is shown as Figure 2 As shown, its specific surface area is 330m 2 / g, and the average pore size is 12nm.

[0056] (5) Take 5 g of silica nanofiber powder, rinse it with 6 M hydrochloric acid, pure water, and ethanol for 2 hours, and then dry it in a vacuum oven at 80°C overnight.

[0057] (6) Add 50 mL of a 5% toluene solution of octadecyldimethylsilyl chloride and 20 mL of pyridine to the obtained powder, place in an oven at 100 °C, and react for 12 hours.

[0058] (7) Repeat step (6) twice, wash, and vacuum dry to obtain a porous silica nanofiber powder modified with a reverse phase chromatography stationary phase.

[0059] (8) The obtained powder was dispersed in methanol, homogenized at 80 MPa, and filled into a stainless steel column tube with an inner diameter of 4.6 mm and a length of 250 mm to obtain a silica nanofiber liquid chromatography column.

[0060] The silica nanofiber liquid chromatography column was connected to the liquid chromatograph and flushed with 100% methanol for 30 minutes. The methanol flow rate was adjusted to 1, 2, 3, and 4 mL / min, and the measured back pressures were 2.3, 4.3, 6.4, and 8.7 MPa, respectively.

[0061] The silica nanofiber liquid chromatography column prepared in this example was used to separate five alkylbenzenes under the following separation conditions: acetonitrile / water (65:35), flow rate 1.0 mL / min, and detection wavelength 210 nm. Figure 3 As shown in the figure, the five compounds are toluene (1), ethylbenzene (2), propylbenzene (3), butylbenzene (4), and pentylbenzene (5). The chromatographic dead time is about 5.5 minutes, and these alkylbenzene small molecules are effectively separated on the silica nanofiber liquid chromatography column.

[0062] Example 2

[0063] The process of preparing zirconium oxide nanofiber liquid chromatography separation material is as follows:

[0064] (1) Add 4.5 g of n-butyl zirconate, 10 g of dimethylformamide, and 1.5 g of polymethylpyrrolidone into a reagent bottle, stir magnetically at room temperature for 2 h, add 0.5 g of hydrochloric acid (2 M), and stir magnetically at room temperature for 2 days to obtain an electrospinning precursor solution.

[0065] (2) Using aluminum foil as a collector, the rotating receiving cylinder speed was 110 rpm, the receiving distance was 10 cm, the spinning voltage was 20 kV, and the feed rate was 3 mL / min. Electrospinning was performed to obtain nanofibers with a diameter of about 500 nm.

[0066] (3) The temperature of the nanofiber filaments was raised to 150°C at a rate of 5°C / min and kept at this temperature for 2 h; the temperature was raised to 500°C at a rate of 5°C / min and kept at this temperature for 2 h; the temperature was raised to 1000°C at a rate of 5°C / min and kept at this temperature for 6 h; after cooling, a sintered nanofiber membrane was obtained.

[0067] (4) The sintered nanofiber membrane was cut into pieces and put into a grinder at 20,000 rpm for 10 min. The powder was sieved through a 10 μm sieve three times to obtain a zirconium oxide nanofiber powder with a specific surface area of ​​450 m 2 / g, and the average pore size is 18nm.

[0068] (5) Take 5 g of zirconium oxide nanofiber powder, rinse it with 6M hydrochloric acid, pure water, and ethanol for 2 hours, and then dry it in a vacuum oven at 80°C overnight.

[0069] (6) Add 50 mL of a 5% toluene solution of octadecyldimethylsilyl chloride and 20 mL of pyridine to the obtained powder, place in an oven at 100 °C, and react for 12 hours.

[0070] (7) Repeat step (6) twice, wash, and vacuum dry to obtain a porous zirconia nanofiber powder modified with a reverse phase chromatography stationary phase.

[0071] (8) The obtained powder was dispersed in methanol, homogenized at 80 MPa, and filled into a stainless steel column tube with an inner diameter of 4.6 mm and a length of 250 mm to obtain a zirconia nanofiber liquid chromatography column.

[0072] The zirconia nanofiber liquid chromatography column was connected to the liquid chromatograph and flushed with 100% methanol for 30 minutes. The methanol flow rate was adjusted to 1, 2, 3, and 4 mL / min, and the measured back pressures were 1.9, 3.3, 4.8, and 6.5 MPa, respectively.

[0073] The nanofiber liquid chromatography column prepared in this example was used to separate five alkylbenzenes, and the separation conditions were: acetonitrile / water (65:35), flow rate 1.0 mL / min, and detection wavelength 210 nm. The chromatographic dead time was about 8 minutes, and the alkylbenzene small molecules were effectively separated on the zirconium oxide nanofiber liquid chromatography column.

[0074] Example 3

[0075] The process of preparing alumina nanofiber liquid chromatography separation material is as follows:

[0076] (1) Add 5 g of isopropyl aluminate, 10 g of dimethylformamide, and 3 g of polyethylene oxide into a reagent bottle, stir magnetically at room temperature for 2 h, add 0.5 g of hydrochloric acid (2 M), and stir magnetically at room temperature for 2 days to obtain an electrospinning precursor solution.

[0077] (2) Using aluminum foil as a collector, the rotating receiving drum speed was 110 rpm, the receiving distance was 10 cm, the spinning voltage was 20 kV, and the feed rate was 3 mL / min. Electrospinning was performed to obtain nanofibers with a diameter of 300 nm.

[0078] (3) The temperature of the nanofiber filaments was raised to 150°C at a rate of 5°C / min and kept at this temperature for 2 h; the temperature was raised to 500°C at a rate of 5°C / min and kept at this temperature for 2 h; the temperature was raised to 900°C at a rate of 5°C / min and kept at this temperature for 6 h; after cooling, a sintered nanofiber membrane was obtained.

[0079] (4) The sintered nanofiber membrane was cut into pieces and put into a grinder at 20,000 rpm for 10 min. The powder was sieved through a 15 μm sieve three times to obtain an alumina nanofiber powder with a specific surface area of ​​500 m 2 / g, and the average pore size is 25nm.

[0080] (5) Take 5 g of alumina nanofiber powder, rinse it with 6 M hydrochloric acid, pure water, and ethanol for 2 hours, and then dry it in a vacuum oven at 80°C overnight.

[0081] (6) Add 50 mL of a 5% toluene solution of octadecyldimethylsilyl chloride and 20 mL of pyridine to the obtained powder, place in an oven at 100 °C, and react for 12 hours.

[0082] (7) Repeat step (6) twice, wash, and vacuum dry to obtain a porous alumina nanofiber powder modified with a reverse phase chromatography stationary phase.

[0083] (8) The obtained powder was dispersed in methanol, homogenized at 80 MPa, and filled into a stainless steel column tube with an inner diameter of 4.6 mm and a length of 250 mm to obtain an alumina nanofiber liquid chromatography column.

[0084] The alumina nanofiber liquid chromatography column was connected to the liquid chromatograph and flushed with 100% methanol for 30 minutes. The methanol flow rate was adjusted to 1, 2, 3, and 4 mL / min, and the measured back pressures were 2.8, 5.3, 7.8, and 10.3 MPa, respectively.

[0085] The aluminum oxide nanofiber liquid chromatography column prepared in this example was used to separate five alkylbenzenes, and the separation conditions were: acetonitrile / water (65:35), flow rate 1.0 mL / min, and detection wavelength 210 nm. The chromatographic dead time was about 5 minutes, and the alkylbenzene small molecules were effectively separated on the zirconium oxide nanofiber liquid chromatography column.

[0086] Comparative Example 1

[0087] 3 μm mesoporous silica microspheres (pore size 10 nm, specific surface area 350 m 2 / g) was filled into a stainless steel column tube with an inner diameter of 4.6 mm and a length of 250 mm to obtain a microsphere liquid chromatography column.

[0088] The microsphere liquid chromatography column was connected to the liquid chromatograph and flushed with 100% methanol for 30 minutes. The methanol flow rate was adjusted to 1, 2, 3, and 4 mL / min, and the measured back pressures were 25.5, 52.4, 73.6, and 100.3 MPa, respectively.

[0089] The five alkylbenzenes were separated using the microsphere liquid chromatography column prepared in this comparative example. The separation conditions were: acetonitrile / water (65:35), a flow rate of 1.0 mL / min, a detection wavelength of 210 nm, and a chromatographic dead time of about 10 minutes. The alkylbenzene small molecules were effectively separated on the microsphere liquid chromatography column.

[0090] Comparative Example 2

[0091] A polypropylene hollow fiber with a diameter of 250 μm (length 250 mm, specific surface area 10 m 2 / g), and then flattened in the form of fiber bundles and filled into a stainless steel column tube with an inner diameter of 4.6 mm and a length of 250 mm to obtain a micron fiber liquid chromatography column.

[0092] The microfiber liquid chromatography column was connected to the liquid chromatograph and flushed with 100% methanol for 30 minutes. The methanol flow rate was adjusted to 1, 2, 3, and 4 mL / min, and the measured back pressures were 0.5, 0.8, 1.1, and 1.5 MPa, respectively.

[0093] The five alkylbenzenes were separated using the micron fiber liquid chromatography column prepared in this comparative example. The separation conditions were: acetonitrile / water (65:35), a flow rate of 1.0 mL / min, and a detection wavelength of 210 nm. The small molecules of alkylbenzenes could not be effectively separated on the micron fiber liquid chromatography column.

[0094] Although the present invention is disclosed as above, the present invention is not limited thereto. Any person skilled in the art can make various changes and modifications without departing from the spirit and scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the scope defined by the claims.

Claims

1. A method for preparing a nanofiber liquid chromatography separation material, characterized in that: The following steps are involved: S1, hydrolyzing an inorganic oxide precursor in a solvent and mixing it with a porogen to form a uniform mixed solution, wherein the porogen is selected from at least one of polyethylene oxide, polymethyl pyrrolidone, polyacrylonitrile, polymethyl methacrylate, and polyimide; S2, electrospinning the mixed solution into nanofiber filaments, wherein the diameter of the nanofiber filaments is 50nm~2000nm; S3, cleaning and sintering the nanofibers to remove the porogen, forming a porous nanofiber membrane, wherein the surface pore size of the nanofiber membrane is 2nm~100nm and the specific surface area is 20m 2 / g~800m 2 / g; S4, crushing the nanofiber membrane into nanofiber powder; S5. Screen out nanofiber powder of suitable specifications, wherein the length of the screened nanofiber powder is 1 μm to 100 μm, and modify the chromatographic stationary phase on the surface of the nanofiber powder to obtain a nanofiber liquid chromatography separation material.

2. The method for preparing the nanofiber liquid chromatography separation material according to claim 1, characterized in that: In the step S1, the inorganic oxide is selected from at least one of silicon dioxide, zirconium oxide, aluminum oxide, titanium oxide, magnesium oxide, cerium oxide, and zinc oxide.

3. The method for preparing the nanofiber liquid chromatography separation material according to claim 1, characterized in that: In the step S3, the sintering temperature is lower than the melting point of the inorganic oxide, and the difference is more than 100°C.

4. The method for preparing the nanofiber liquid chromatography separation material according to claim 1, characterized in that: In the step S1, the solvent is selected from at least one of water, alcohol, ester, amide, sulfoxide, and nitrogen methyl pyrrolidone.

5. The method for preparing the nanofiber liquid chromatography separation material according to claim 1, characterized in that: In step S5, the chromatographic stationary phase is selected from at least one of a reverse phase chromatographic stationary phase, a hydrophilic chromatographic stationary phase, a chiral chromatographic stationary phase, and an ion pair chromatographic stationary phase.

6. A nanofiber liquid chromatography separation material, characterized in that: Prepared by the preparation method according to any one of claims 1 to 5.

Images