CN116351402A - Preparation method and application of recyclable MXene/polyethersulfone composite microsphere - Google Patents
Preparation method and application of recyclable MXene/polyethersulfone composite microsphere Download PDFInfo
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- 239000004695 Polyether sulfone Substances 0.000 title claims abstract description 63
- 229920006393 polyether sulfone Polymers 0.000 title claims abstract description 63
- 239000004005 microsphere Substances 0.000 title claims abstract description 58
- 239000002131 composite material Substances 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 239000000243 solution Substances 0.000 claims abstract description 68
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims abstract description 29
- 239000000463 material Substances 0.000 claims abstract description 24
- 239000008280 blood Substances 0.000 claims abstract description 20
- 210000004369 blood Anatomy 0.000 claims abstract description 20
- 238000003756 stirring Methods 0.000 claims abstract description 10
- 238000000746 purification Methods 0.000 claims abstract description 9
- VDZOOKBUILJEDG-UHFFFAOYSA-M tetrabutylammonium hydroxide Chemical compound [OH-].CCCC[N+](CCCC)(CCCC)CCCC VDZOOKBUILJEDG-UHFFFAOYSA-M 0.000 claims abstract description 8
- 230000001112 coagulating effect Effects 0.000 claims abstract description 6
- 238000009830 intercalation Methods 0.000 claims abstract description 6
- 230000002687 intercalation Effects 0.000 claims abstract description 6
- 238000005530 etching Methods 0.000 claims abstract description 4
- 238000010041 electrostatic spinning Methods 0.000 claims abstract description 3
- 239000012456 homogeneous solution Substances 0.000 claims abstract description 3
- 239000007788 liquid Substances 0.000 claims description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 230000005686 electrostatic field Effects 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 5
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- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 238000002347 injection Methods 0.000 claims description 4
- 239000007924 injection Substances 0.000 claims description 4
- 238000004108 freeze drying Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 2
- 238000005345 coagulation Methods 0.000 claims description 2
- 230000015271 coagulation Effects 0.000 claims description 2
- 239000012046 mixed solvent Substances 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- 238000001291 vacuum drying Methods 0.000 claims description 2
- 238000004090 dissolution Methods 0.000 claims 1
- 235000019441 ethanol Nutrition 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 claims 1
- 238000000967 suction filtration Methods 0.000 claims 1
- BPYKTIZUTYGOLE-IFADSCNNSA-N Bilirubin Chemical compound N1C(=O)C(C)=C(C=C)\C1=C\C1=C(C)C(CCC(O)=O)=C(CC2=C(C(C)=C(\C=C/3C(=C(C=C)C(=O)N\3)C)N2)CCC(O)=O)N1 BPYKTIZUTYGOLE-IFADSCNNSA-N 0.000 abstract description 32
- LEHOTFFKMJEONL-UHFFFAOYSA-N Uric Acid Chemical compound N1C(=O)NC(=O)C2=C1NC(=O)N2 LEHOTFFKMJEONL-UHFFFAOYSA-N 0.000 abstract description 15
- TVWHNULVHGKJHS-UHFFFAOYSA-N Uric acid Natural products N1C(=O)NC(=O)C2NC(=O)NC21 TVWHNULVHGKJHS-UHFFFAOYSA-N 0.000 abstract description 15
- 229940116269 uric acid Drugs 0.000 abstract description 15
- 238000001179 sorption measurement Methods 0.000 abstract description 13
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 abstract description 9
- 238000005191 phase separation Methods 0.000 abstract description 4
- 239000012620 biological material Substances 0.000 abstract description 2
- PQXKHYXIUOZZFA-UHFFFAOYSA-M lithium fluoride Chemical compound [Li+].[F-] PQXKHYXIUOZZFA-UHFFFAOYSA-M 0.000 abstract 2
- 239000007864 aqueous solution Substances 0.000 abstract 1
- DDRJAANPRJIHGJ-UHFFFAOYSA-N creatinine Chemical compound CN1CC(=O)NC1=N DDRJAANPRJIHGJ-UHFFFAOYSA-N 0.000 description 28
- 239000010936 titanium Substances 0.000 description 17
- 229940109239 creatinine Drugs 0.000 description 14
- 239000002244 precipitate Substances 0.000 description 14
- 238000002835 absorbance Methods 0.000 description 6
- 239000003053 toxin Substances 0.000 description 6
- 231100000765 toxin Toxicity 0.000 description 6
- 108700012359 toxins Proteins 0.000 description 6
- 238000005119 centrifugation Methods 0.000 description 5
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- 230000002000 scavenging effect Effects 0.000 description 3
- 238000009210 therapy by ultrasound Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical group N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- 238000011013 endotoxin removal Methods 0.000 description 2
- -1 polytetrafluoroethylene Polymers 0.000 description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 description 2
- 230000001376 precipitating effect Effects 0.000 description 2
- 239000006228 supernatant Substances 0.000 description 2
- 229910052723 transition metal Inorganic materials 0.000 description 2
- 150000003624 transition metals Chemical class 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000001523 electrospinning Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 210000003734 kidney Anatomy 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 230000004060 metabolic process Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 239000010955 niobium Substances 0.000 description 1
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 1
- 229910052757 nitrogen Chemical group 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 229940045136 urea Drugs 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
- B01J20/262—Synthetic macromolecular compounds obtained otherwise than by reactions only involving carbon to carbon unsaturated bonds, e.g. obtained by polycondensation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
- B01D15/10—Selective adsorption, e.g. chromatography characterised by constructional or operational features
- B01D15/20—Selective adsorption, e.g. chromatography characterised by constructional or operational features relating to the conditioning of the sorbent material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/223—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material containing metals, e.g. organo-metallic compounds, coordination complexes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28016—Particle form
- B01J20/28021—Hollow particles, e.g. hollow spheres, microspheres or cenospheres
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Abstract
The invention discloses a recyclable MXene/polyethersulfone composite microsphere and a preparation method thereof, belonging to the technical field of biological materials, wherein the microsphere consists of an organic solution of MXene and polyethersulfone, and the preparation method thereof is disclosed as follows: firstly, etching MAX material through lithium fluoride and hydrochloric acid, then, after intercalation is carried out in tetrabutylammonium hydroxide aqueous solution, ultrasonically dissolving the MAX material in N, N-dimethylacetamide solution; then adding polyether sulfone into the N, N-dimethylacetamide solution of the MXene, stirring, and carrying out phase separation on the homogeneous solution in a coagulating bath by an electrostatic spinning technology to form microspheres; the microsphere can be used for preparing blood purification treatment equipment, and has good adsorption capacity on uric acid and bilirubin in blood.
Description
Technical Field
The invention relates to the technical field of biological materials, and particularly discloses a preparation method and application of a recyclable MXene/polyethersulfone composite microsphere.
Background
MXenes is a family of two-dimensional transition metal carbonitrogens, and is generally represented by M n+1 X n T x M represents an early transition metal (e.g., titanium, vanadium, niobium, molybdenum), X is carbon and/or nitrogen, n=1-3, T x Represents surface end capping groups such as-OH, -O-and-F. Currently 20 different MXenes have been synthesized, predicting the existence of more MXenes. Their physical and chemical properties can be fine tuned by varying the structure and synthesis conditions. Ti (Ti) 3 C 2 The MXene is the most studied type at present because of the mild etching conditions and good biocompatibility. Polyethersulfone has good mechanical properties and acid and alkali resistance, and is a commercial polymer raw material widely applied to the technical field of blood purification.
Polyethersulfone materials are often used as a base material for blood purification materials because of their good mechanical properties and blood compatibility, but because of their poor adsorption of toxins in blood, it is necessary to modify polyethersulfone base materials. As a two-dimensional lamellar material, MXene has a large specific surface area, and in the etching process of HCl and LiF, the surface of MXene is easy to obtain oxygen-rich surface groups, which is favorable for adsorbing toxin molecules in blood, such as creatinine, uric acid, urea, bilirubin and the like.
The MXene material is applied in a powder form, has poor mechanical properties and is not easy to recycle, and greatly limits the application of the MXene material in blood purification, so that the MXene material and a polymer material are compounded to be applied in a microsphere mode, and the MXene material is a simple solution. In electrospinning, polyether sulfone is usually required to be dissolved in an organic solvent, but the solubility of an MXene material in the organic solvent is poor and the compatibility of the MXene material with a high polymer material is poor. So that the comprehensive application of MXene is limited.
Disclosure of Invention
One of the purposes of the invention is to solve the problem of poor compatibility of the existing MXene material and polymer materials such as polyethersulfone dissolved in organic solvents, and provide a feasible improvement method for the further application of the MXene material, and the invention is realized by the following technical means:
the invention discloses a recyclable MXene/polyethersulfone composite microsphere, which comprises the following components:
the mass ratio of MXene to polyethersulfone is 1: (50-200);
mixing an N, N-dimethylacetamide solution of MXene with polyethersulfone to form a homogeneous solution, wherein the mass ratio of the sum of the mass of MXene and the mass of polyethersulfone in the solution to the mass ratio of the solvent N, N-dimethylacetamide solution is (14-16): (84-86).
Further, the MAX phase material is Ti 3 AlC 2 The method comprises the steps of carrying out a first treatment on the surface of the The MXene material is Ti 3 C 2 。
Further, the Ti is 3 C 2 The N, N-dimethylacetamide solution of (2) is prepared by the following method:
1) 1-1.6g LiF is weighed quantitatively, dissolved in 20mL of 9mol/L hydrochloric acid and stirred in a polytetrafluoroethylene beaker until the LiF is completely dissolved; weigh 1g Ti 3 AlC 2 Adding a small amount of powder into the solution for multiple times, and stirring at 35 ℃ for 24-48 hours to obtain a first solution;
2) Transferring the first solution into a centrifuge tube, centrifuging at 4000rpm, taking a precipitate, washing the precipitate twice by using 1mol/L dilute hydrochloric acid, washing the precipitate by using deionized water until the pH value of supernatant fluid after centrifugation is more than or equal to 6, obviously expanding the precipitate, and freeze-drying the precipitate for 24 hours to obtain a freeze-dried precipitate;
3) Taking 1g of freeze-dried precipitate, putting the precipitate into a beaker, adding 15ml of a 25%wt tetrabutylammonium hydroxide solution into the solution, and stirring the solution at a constant temperature of 30 ℃ for more than 8 hours to perform intercalation reaction;
4) After intercalation is finished, the system is placed into a centrifuge tube for centrifugation, ethanol is used for washing and precipitating twice, then N, N-dimethylacetamide solution is added, after shaking evenly, ultrasonic treatment is carried out for 30min, and the Ti is obtained by centrifugation 3 C 2 N, N-dimethylacetamide solution of (a);
5) Ti in solution 3 C 2 The content of (2) is determined by: by mixing 1mL of the Ti 3 C 2 Filtering the N, N-dimethylacetamide solution, vacuum drying, and then weighing to determine the concentration in units: mg/mL.
The invention also discloses a preparation method of any one of the MXene/polyethersulfone composite microspheres, which comprises the following steps:
1) Preparing an MXene/polyethersulfone composite microsphere balling liquid:
adding polyethersulfone into N, N-dimethylacetamide solution, stirring at room temperature for 2-8h to obtain polyethersulfone solution, adding Ti into the polyethersulfone solution 3 C 2 Stirring the N, N-dimethylacetamide solution for 20 to 30 minutes to obtain a balling liquid;
2) Preparation of MXene/polyethersulfone composite microspheres:
extracting the prepared balling liquid into an injector, pushing the injector in an electrostatic field to enable the balling liquid to form liquid drops to fall into a coagulation bath for phase conversion, and obtaining the MXene/polyethersulfone composite microspheres.
Further, the electrostatic field in the step 2) is formed by an electrostatic spinning machine, and the diameter of the microsphere is controlled by adjusting electrostatic voltage and the injection speed of a syringe needle or a pushing injection.
Further, the coagulating bath in the step 2) is a mixed solvent of deionized water and ethanol.
The invention also discloses the MXene/polyethersulfone composite microsphere prepared by any one of the preparation methods.
The invention also discloses an application of the MXene/polyethersulfone composite microsphere in preparing blood purifying equipment.
Further, the blood purification apparatus includes: blood purification of bilirubin, creatinine and uric acid clearance disorders occurs.
The final object of the invention is to apply the MXene/polyethersulfone composite microsphere to the adsorption of toxins in blood. Therefore, testing the adsorption capacity of the adsorbed toxin in blood should be the blood purification of patients with abnormal kidney metabolism. The MXene is uniformly distributed in the porous matrix of the polyethersulfone, so that good adsorption performance is provided for the microsphere, and simultaneously, the MXene and the polyethersulfone have good blood compatibility, and the adsorption performance is based on the adsorption characteristic brought by the large specific surface area and rich surface active sites of the MXene.
Compared with the prior art, the invention has the advantages that:
1. inventors use Ti 3 C 2 The polyether sulfone composite microsphere is used for removing three blood toxins of creatinine, uric acid and bilirubin, and the microsphere is found to be used for removing the three blood toxinsAll blood toxins can be effectively removed.
2. The invention provides a method for preparing Ti 3 C 2 In the method for practical application of MXene in the field of blood purification, after the MXene and polyethersulfone are compounded, compared with MXene powder, the MXene-like compound has better mechanical properties and is easier to apply and recycle.
3. The invention and the traditional method adopt the ultrasonic treatment to carry out Ti 3 C 2 Compared with the method of dispersing in organic solvent, the Ti formed by the method 3 C 2 Better compatibility with polyethersulfone, ti 3 C 2 The MXene/polyethersulfone composite microsphere is more uniformly dispersed in polyethersulfone, and has better scavenging ability for creatinine, uric acid and bilirubin through tests.
Drawings
FIG. 1 is a scanning electron microscope image of an intercalated MXene according to an embodiment of the invention;
FIG. 2 is a cross-sectional scanning electron microscope image of the MXene/polyethersulfone composite microspheres prepared in the example of the present invention;
FIG. 3 shows the creatinine scavenging ability of microspheres in examples;
FIG. 4 shows the uric acid scavenging ability of microspheres in examples;
the ability of the microspheres to scavenge bilirubin in the example of FIG. 5.
Detailed Description
The invention will be further described with reference to the accompanying drawings.
The adsorption performance test method of the microsphere prepared in the embodiment 1-3 comprises the following steps:
(1) Creatinine adsorption performance test:
a concentration-absorbance standard curve is established by using 10mg/L, 5mg/L, 2.5mg/L and 1.25mg/mL of creatinine solution; placing microspheres with wet weight of 20mg into 20ml of creatinine solution (50 mg/L), placing in a shaking table, shaking at 37 ℃ in a dark place for 6 hours, measuring absorbance of the absorbed solution at 232nm by an ultraviolet spectrophotometer, and calculating the adsorption capacity of the microspheres according to the lambert beer law, wherein the result is shown in figure 3;
(2) Uric acid adsorption performance test:
a standard curve of concentration-absorbance was established using 50. Mu. Mol/L, 25. Mu. Mol/L, 12.5. Mu. Mol/L, 6.25. Mu. Mol/L uric acid solution; placing microspheres with wet weight of 20mg into 20mL uric acid solution (250 mu mol/L), placing in a shaking table, shaking at 37 ℃ in a dark place for 6 hours, measuring absorbance of the absorbed solution at 293nm by an ultraviolet spectrophotometer, and calculating the adsorption capacity of the microspheres according to the lambert beer law, wherein the result is shown in figure 4;
(3) Bilirubin adsorption performance test:
a standard curve of concentration-absorbance was established using bilirubin solutions of 15mg/L, 7.5mg/L, 3.75mg/L, and 1.875 mg/L; the microspheres with the wet weight of 20mg are placed into 20mL of bilirubin solution (150 mg/L), the bilirubin solution is vibrated for 6 hours at the constant temperature of 37 ℃ in a dark place, then the absorbance of the absorbed solution at 438nm is measured by an ultraviolet spectrophotometer, and the absorption capacity of the microspheres is calculated according to the lambert beer law, and the result is shown in figure 5.
The following examples 1-3 were prepared from solutions of MXene in N, N-dimethylacetamide:
1) 1.6g LiF is weighed quantitatively, dissolved in 20ml of 9mol/L hydrochloric acid and stirred in a polytetrafluoroethylene beaker until the LiF is completely dissolved; weigh 1g Ti 3 AlC 2 Adding the powder into the solution for a plurality of times in a small amount, and stirring for 36 hours at 35 ℃;
2) Transferring the solution after the reaction into a centrifuge tube, centrifuging at 4000rpm, taking a precipitate, then using 1mol/L dilute hydrochloric acid to perform twice cleaning and shaking, centrifuging, taking the process of the precipitate, then using deionized water to clean the precipitate, wherein the pH value of the supernatant is more than or equal to 6, and after the precipitate is obviously swelled, freeze-drying the material for 24 hours;
3) Taking 1g of the freeze-dried precipitate, putting the precipitate into a beaker, adding 15ml of a 25% wt tetrabutylammonium hydroxide solution into the beaker, and stirring the solution at a constant temperature of 30 ℃ for 8 hours to perform intercalation reaction;
4) After intercalation is finished, the system is placed into a centrifuge tube for centrifugation, ethanol is used for washing and precipitating twice, then 10mLN, N-dimethylacetamide solution is added, after shaking, ultrasonic treatment is carried out for 30min, and Ti is obtained by centrifugation 3 C 2 N, N-dimethylacetamide solution of (a);
the above-mentioned intercalated MXene has a plate-like structure of a larger size as shown in fig. 1.
Example 1
In the embodiment, the mass ratio of MXene to polyethersulfone is 1:150, 1950mg of polyethersulfone is dissolved in 11087mg of N, N-dimethylacetamide solution, stirred for 4 hours at room temperature to form a homogeneous polyethersulfone solution, then 1mLMXene of N, N-dimethylacetamide solution is added into the homogeneous polyethersulfone solution, and the mixture is stirred for 30 minutes at room temperature to be uniformly mixed to obtain a balling liquid; the balling liquid is filled into a syringe, and is sprayed by electricity under an electrostatic field to form liquid drops, and phase separation rapidly occurs in a coagulating bath of water and ethanol (volume ratio is 1:3), so as to form microspheres with uniform size. The microspheres were soaked in PBS buffer for use. The scanning electron microscope image of the inside of the dried microsphere is shown in fig. 2, and as can be seen from fig. 2, the inside of the microsphere has a porous structure, and the pore canal wall has MXene sheet folds.
The creatinine clearance, uric acid clearance and bilirubin clearance were tested as described above, and the results are shown in FIGS. 3-5, which show that the microspheres of this example have clearance ability for creatinine, uric acid and bilirubin.
Example 2
The present example is intended to illustrate the effect of the content of MXene on the endotoxin removal effect of MXene/polyethersulfone composite microspheres, and the mass ratio of MXene to polyethersulfone in the present example is 1:100.
1300mg of polyethersulfone is dissolved in 7094mg of N, N-dimethylacetamide solution, stirred for 4 hours at room temperature to form homogeneous polyethersulfone solution, then 1 mM XeneN, N-dimethylacetamide solution is added into the homogeneous polyethersulfone solution, and stirred for 30 minutes at room temperature to be uniformly mixed to obtain a balling solution; the balling liquid is filled into a syringe, and is sprayed by electricity under an electrostatic field to form liquid drops, and phase separation rapidly occurs in a coagulating bath of water and ethanol (volume ratio is 1:3), so as to form microspheres with uniform size. The microspheres were soaked in PBS buffer for use. The microsphere has a porous structure inside, and the pore walls are provided with MXene sheet folds.
The results of the creatinine clearance, uric acid clearance and bilirubin clearance tests performed as described above are shown in FIGS. 3-5, and it can be seen from the figures that the microspheres of this example have clearance ability for creatinine, uric acid and bilirubin, and the clearance performance is increased as compared with example 1.
Example 3
The present example is intended to illustrate the effect of the content of MXene on the endotoxin removal effect of MXene/polyethersulfone composite microspheres, and the mass ratio of MXene to polyethersulfone in the present example is 1:75.
974mg of polyethersulfone is dissolved in 5092mg of N, N-dimethylacetamide solution, stirred for 4 hours at room temperature to form homogeneous polyethersulfone solution, then 1ml of MXeneN, N-dimethylacetamide solution is added into the homogeneous polyethersulfone solution, and stirred for 30 minutes at room temperature to be uniformly mixed to obtain a balling solution; the balling liquid is filled into a syringe, and is sprayed by electricity under an electrostatic field to form liquid drops, and phase separation rapidly occurs in a coagulating bath of water and ethanol (volume ratio is 1:3), so as to form microspheres with uniform size. The microspheres were soaked in PBS buffer for use. The microsphere has a porous structure inside, and the pore walls are provided with MXene sheet folds.
The results of the creatinine clearance, uric acid clearance and bilirubin clearance tests performed as described above are shown in FIGS. 3-5, and it can be seen from the figures that the microspheres of this example have clearance ability for creatinine, uric acid and bilirubin, and the clearance performance is increased as compared with examples 1 and 2.
Claims (9)
1. A recyclable MXene/polyethersulfone composite microsphere comprising:
the mass ratio of MXene to polyethersulfone is 1: (50-200);
mixing an N, N-dimethylacetamide solution of MXene with polyethersulfone to form a homogeneous solution, wherein the mass ratio of the sum of the mass of MXene and the mass of polyethersulfone in the solution to the mass ratio of the solvent N, N-dimethylacetamide solution is (14-16): (84-86).
2. The MXene/polyethersulfone composite microsphere according to claim 1, wherein:
the MAX phase material is Ti 3 AlC 2 ；
The MXene material is Ti 3 C 2 。
3. The MXene/polyethersulfone composite microsphere according to claim 1, wherein:
the N, N-dimethylacetamide solution of MXene is prepared by the following method:
1) Etching MAX raw materials in a solution of HCl and LiF, cleaning for multiple times by using deionized water, and freeze-drying a multi-layer MXene material for later use;
2) Adding the multi-layer MXene material into tetrabutylammonium hydroxide solution, stirring for more than 8 hours, after intercalation, centrifuging, and washing twice by absolute ethyl alcohol to obtain a washed multi-layer MXene material;
3) And adding 20mLN, N-dimethylacetamide solution into the cleaned multilayer MXene material, and performing ultrasonic dissolution to obtain the N, N-dimethylacetamide solution of MXene.
4. The MXene/polyethersulfone composite microsphere according to claim 3, wherein:
step 3) the content of MXene in the N, N-dimethylacetamide solution of MXene is determined by the following method:
taking 1mLMXene N, N-dimethylacetamide solution for suction filtration, and determining the concentration of the MXene in the N, N-dimethylacetamide solution after vacuum drying, wherein the unit is: mg/mL.
5. A method of preparing an MXene/polyethersulfone composite microsphere according to any one of claims 1-4, comprising:
1) Preparing an MXene/polyethersulfone composite microsphere balling liquid:
adding polyethersulfone into N, N-dimethylacetamide solution, stirring at room temperature for 2-8h to obtain polyethersulfone solution, adding N, N-dimethylacetamide solution of MXene into polyethersulfone solution, stirring for 20-30min to obtain balling liquid;
2) Preparation of MXene/polyethersulfone composite microspheres:
extracting the prepared balling liquid into an injector, pushing the injector in an electrostatic field to enable the balling liquid to form liquid drops to fall into a coagulation bath for phase conversion, and obtaining the MXene/polyethersulfone composite microspheres.
6. The method of manufacturing according to claim 5, wherein:
the electrostatic field in the step 2) is formed by an electrostatic spinning machine, and the diameter of the microsphere is controlled by adjusting electrostatic voltage and the injection speed of a syringe needle or a pushing injection speed.
7. The method according to claim 5, wherein:
the coagulating bath in the step 2) is a mixed solvent of deionized water and ethanol.
8. An MXene/polyethersulfone composite microsphere made in accordance with the method of any one of claims 5-7.
9. Use of an MXene/polyethersulfone composite microsphere according to any one of claims 1-4, 8 for the preparation of a blood purification device.
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