CN108514864B - Chitin/graphene oxide composite sponge and preparation method and application thereof - Google Patents
Chitin/graphene oxide composite sponge and preparation method and application thereof Download PDFInfo
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- 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
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61M—DEVICES FOR INTRODUCING MEDIA INTO, OR ONTO, THE BODY; DEVICES FOR TRANSDUCING BODY MEDIA OR FOR TAKING MEDIA FROM THE BODY; DEVICES FOR PRODUCING OR ENDING SLEEP OR STUPOR
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- A61M1/36—Other treatment of blood in a by-pass of the natural circulatory system, e.g. temperature adaptation, irradiation ; Extra-corporeal blood circuits
- A61M1/3679—Other treatment of blood in a by-pass of the natural circulatory system, e.g. temperature adaptation, irradiation ; Extra-corporeal blood circuits by absorption
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- 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
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- 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
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Abstract
The invention belongs to the field of bioengineering separation, and particularly relates to chitin/graphene oxide composite sponge and a preparation method and application thereof. The preparation method comprises the following steps: preparing chitin/graphene oxide composite sponge: dissolving chitin and graphene oxide in a sodium hydroxide/urea system together at a low temperature, heating, and freezing and drying to obtain the chitin/graphene oxide composite sponge material. The method has the advantages of mild reaction conditions, low cost, environmental protection and the like. The prepared chitin/graphene oxide composite sponge for bilirubin adsorption has the advantages of large adsorption capacity, high adsorption efficiency and the like on bilirubin template molecules, and can be applied to adsorption of bilirubin in blood purification.
Description
Technical Field
The invention belongs to the field of bioengineering separation, and particularly relates to chitin/graphene oxide composite sponge and a preparation method and application thereof.
Background
The content of bilirubin in normal human blood is 0.2-1 mg/dL, and if bilirubin is excessively produced or metabolic pathways are blocked, a large amount of bilirubin is accumulated in a human body, and systemic toxicity is generated. In recent years, with the rapid development of biomaterials, hemoperfusion therapy has been rapidly developed and is gradually accepted by a wide range of patients, and is a "third therapy" following drugs and surgical therapies. The core content in the hemoperfusion therapy is the research and development of blood adsorbing materials, a plurality of adsorbing materials are prepared at present, and some products are applied to clinic. However, the existing adsorbing material has poor adsorption performance and poor biocompatibility on one hand, and has high cost on the other hand, so that the treatment burden of patients is increased. Therefore, the development of novel adsorption materials with good adsorption performance and blood compatibility and the cost reduction as far as possible have important scientific research significance and clinical practical value.
Bilirubin contains carboxyl and imino, and the adsorption material can adsorb bilirubin through nonpolar adsorption (hydrophobic adsorption), anion exchange adsorption (electrostatic interaction) or polar adsorption (hydrogen bond interaction). Currently, there are two main types of adsorption materials used for bilirubin blood perfusion: activated carbon and resin. The activated carbon is used as an adsorbing material, so that the activated carbon can seriously damage blood platelets, and tiny carbon granules can cause embolism in blood vessels. The granular activated carbon coating is later used for blood perfusion, so that the activated carbon blood perfusion enters a clinical practical stage. The core of the technology is the research and development of high-performance adsorption materials, some high-molecular resin adsorption materials are continuously researched and developed at present for adsorbing bilirubin, and foreign XAD series adsorption resins and domestic NK107, NK110 and other adsorption resin products are all used for clinic of hemoperfusion. The clinical effect of the used adsorbing materials cannot be completely satisfied up to now, and the main reasons are that the existing adsorbing materials have the problems of poor adsorption performance, poor blood compatibility, high material cost and the like.
In recent years, the development and utilization of environment-friendly renewable resources can alleviate the problems of exhaustion of limited resources on the earth and environmental pollution, and the like, and the development and utilization of environment-friendly renewable resources have attracted attention. Chitin is a renewable resource widely existing in nature, mainly exists in mail and crab shells, cell walls of fungi and algae and shells of arthropods, has the advantages of rich resources, environmental friendliness, low price, good biocompatibility, biodegradability and the like, and can be widely applied to the field of biomedicine. However, chitin has high crystallinity and is difficult to dissolve.
The graphene oxide has a large specific surface area, a rich pore structure and oxygen-containing functional groups (such as-OH, -COOH, C ═ O and the like), has a wide and efficient adsorption capacity, can adsorb substances such as metals, organic substances, small molecules and the like, is an excellent efficient adsorption material, can be used for removing water pollution, toxins and the like, uses bilirubin as a main toxin in blood, and has efficient adsorption on graphene oxide. Therefore, the graphene oxide is a blood perfusion adsorbing material with great potential, has excellent mechanical property and conductivity, is easy to functionalize on the surface, and can be combined with other materials. But due to poor biocompatibility and blood compatibility of graphene oxide, the application of graphene oxide in biomedicine is severely limited.
Therefore, a technology for preparing a novel bilirubin adsorption material with high adsorption capacity, high mechanical properties and good blood compatibility by combining chitin and graphene oxide is urgently needed in the medical field at present.
Disclosure of Invention
In order to overcome the defects and shortcomings in the prior art, the invention mainly aims to provide a preparation method of chitin/graphene oxide composite sponge.
The invention also aims to provide the chitin/graphene oxide composite sponge.
The invention further aims to provide application of the chitin/graphene oxide composite sponge.
The invention relates to the fields of chemistry, biology, medicine and the like, and has the characteristic of interdisciplinary research.
The purpose of the invention is realized by the following technical scheme:
a preparation method of chitin/graphene oxide composite sponge comprises the following steps:
dissolving chitin and graphene oxide in a sodium hydroxide/urea system by adopting a low-temperature freezing-melting method to obtain a solution containing the chitin and the graphene oxide;
heating the solution containing chitin and graphene oxide in a sealed manner at the temperature of 60-90 ℃ for 5-12 h to obtain chitin/graphene oxide hydrogel;
washing the hydrogel to be neutral, and freezing and drying to obtain the chitin/graphene oxide composite sponge material;
the mass ratio of the chitin to the graphene oxide in the chitin/graphene oxide hydrogel is 100: 5 to 30.
Preferably, the mass percentage of the chitin in the solution is 1-4 wt%.
Preferably, the solution containing chitin and graphene oxide is prepared by the following method: dissolving chitin and graphene oxide into a sodium hydroxide/urea solution together at-80 to-40 ℃, and centrifuging to obtain a solution containing the chitin and the graphene oxide.
More preferably, the mass percent of the sodium hydroxide is 8-11wt%, and the mass percent of the urea is 4-6 wt%.
More preferably, the centrifugation speed is 3000-.
A chitin/graphene oxide composite sponge is prepared by the preparation method of the chitin/graphene oxide composite sponge.
The chitin/graphene oxide composite sponge is applied to the adsorption of bilirubin, and particularly aims at the adsorption of bilirubin in blood of a patient with high bilirubinemia clinically (the concentration of bilirubin in blood is higher than 20 mg/dL).
According to the invention, the graphene oxide is modified by the chitin with good biocompatibility and blood compatibility, so that the biocompatibility and blood compatibility of the graphene oxide can be greatly improved, and the composite material with excellent comprehensive performance is prepared, so that the graphene oxide can be widely applied to blood perfusion.
Compared with the prior art, the invention has the following advantages and effects:
1. the chitin/graphene oxide composite sponge with high porosity, high mechanical property and good blood compatibility can be prepared by combining the chitin and the graphene oxide with low cost by using a simple heating method, so that the high-performance adsorption of bilirubin is realized;
2. in the preparation technology, a green and environment-friendly sodium hydroxide/urea system is selected to be dissolved to obtain a mixed solution of chitin and graphene oxide, and then the mixed solution is heated, frozen and dried to obtain the composite material, so that the reaction condition is mild, and the operation is simple and convenient.
3. The chitin/graphene oxide composite sponge material prepared by the invention has a good adsorption effect on target molecule bilirubin, and can quickly remove bilirubin.
Drawings
Fig. 1 is a Scanning Electron Microscope (SEM) image of chitin sponge obtained in comparative example 1.
Fig. 2 is a Scanning Electron Microscope (SEM) image of the chitin/graphene oxide composite sponge obtained in example 2.
FIG. 3 is a chart showing evaluation of blood compatibility in comparative example 1 and examples 1 to 3.
FIG. 4 is a graph showing mechanical properties of comparative example 1 and examples 1 to 3.
FIG. 5 is a graph of porosity for comparative example 1 and examples 1-3.
FIG. 6 is a graph showing the dynamic adsorption curves of bilirubin by the products obtained in comparative example 1 and examples 1 to 3.
FIG. 7 is a graph showing the adsorption curves of the products obtained in comparative example 1 and example 3 at different bilirubin concentrations.
FIG. 8 is a dynamic adsorption curve of products obtained in comparative example 1 and examples 1 to 3 under simulated blood perfusion conditions.
Detailed Description
The present invention will be described in further detail with reference to examples, but the embodiments of the present invention are not limited thereto.
The reagents in the following examples are commercially available.
Comparative example 1
Dissolving 2g of chitin (Ch) in 98g of sodium hydroxide/Urea (NaOH/Urea) system by adopting a low-temperature freezing-melting method at the temperature of minus 80 ℃, and centrifuging at 6000rpm for 15min to obtain pure chitin solution, wherein the mass fraction of the sodium hydroxide (NaOH) is 11wt%, and the mass fraction of the Urea (Urea) is 4 wt%. Then adding 3mL of the chitin solution into a 10mL sealed glass bottle by a sealed heating method, heating at 90 ℃ for 12h to obtain hydrogel, washing to be neutral, and freeze-drying the hydrogel by a freeze-drying method to obtain chitin sponge, wherein an SEM image of the chitin sponge is shown in figure 1.
Example 1
Dissolving chitin and graphene oxide in a sodium hydroxide/Urea (NaOH/Urea) system by adopting a low-temperature freezing-melting method at the temperature of-80 ℃, centrifuging at 6000rpm for 15min to obtain a mixed solution containing the chitin and the graphene oxide, wherein the mass fraction of the sodium hydroxide (NaOH) is 11wt%, the mass fraction of the Urea (Urea) is 4wt%, the mass fraction of the chitin (Ch) is 2 wt%, the mass fraction of the Graphene Oxide (GO) is 0.1 wt%, and the ratio of the chitin to the graphene oxide is 100: 5. and then adding 3mL of the chitin and graphene oxide mixed solution into a 10mL sealed glass bottle by adopting a sealed heating method, heating for 12h at 90 ℃ to obtain hydrogel, washing to be neutral, and freeze-drying the hydrogel by adopting a freezing-drying method to obtain the chitin/graphene oxide composite sponge (Ch/GO-5).
Example 2
Experimental conditions and procedures reference example 1, except that the ratio of chitin to graphene oxide is 100: 10. finally obtaining chitin/graphene oxide composite sponge (Ch/GO-10), wherein the SEM atlas of the chitin/graphene oxide composite sponge is shown in figure 2.
Example 3
Experimental conditions and procedures reference example 1, except that the ratio of chitin to graphene oxide is 100: 20. finally obtaining the chitin/graphene oxide composite sponge (Ch/GO-20).
FIG. 3 shows a blood compatibility evaluation chart for partial thromboplastin activity time (APTT) and Prothrombin Time (PT) of comparative example 1 and examples 1 to 3. As can be seen from fig. 3, after a proper amount of graphene oxide is added, the blood compatibility of the material is not decreased, but is slightly improved. When the ratio of the chitin to the graphene oxide is 100:10, the anticoagulant performance is best, and the corresponding biocompatibility is also best; when the amount of the graphene oxide is increased, the blood compatibility of the material is reduced, and it is expected that when the proportion of the graphene oxide exceeds the limit range of the invention, the blood compatibility of the material is too low, thereby limiting the application of the material in the aspect of biomedicine.
FIGS. 4 and 5 show the mechanical property diagram and porosity diagram of comparative example 1 and examples 1 to 3. As can be seen from fig. 4 and 5, the mechanical properties and porosity of the composite sponge increase with the increase of the content of graphene oxide, and are improved compared with pure chitin sponge.
Fig. 6 shows a dynamic adsorption curve diagram of bilirubin by the chitin sponge obtained in the comparative example 1 and the chitin/graphene oxide composite sponge materials obtained in examples 1 to 3, wherein 10mg of the chitin/graphene oxide composite sponge materials prepared in the comparative example 1 and examples 1 to 3 are respectively weighed and added into 30mL of bilirubin solution with the concentration of 20mg/dL, the bilirubin solution is vibrated away from light at room temperature, after a certain time of adsorption, the absorbance of the solution at 438nm is detected by an ultraviolet spectrophotometer, and the adsorption quantity Q (mg/g) of the chitin sponge and the chitin/graphene oxide composite sponge materials is calculated by using the formula 1. As can be seen from fig. 6, the adsorption capacity of the chitin/graphene oxide composite sponge starts to be significantly increased after about 1.5 hours compared with that of the chitin sponge, and the adsorption capacity of the chitin/graphene oxide composite sponge material after 4 hours of adsorption is 30-100 mg/g higher than that of the chitin sponge according to the difference of the amount of graphene oxide.
Fig. 7 shows adsorption curves of the chitin sponge obtained in comparative example 1 and the chitin/graphene oxide composite sponge material obtained in example 3 at different bilirubin concentrations, wherein 10mg of the chitin sponge and the chitin/graphene oxide composite sponge material prepared in comparative example 1 and example 3 are respectively weighed and added into 30mL of bilirubin solutions with concentrations of 10mg/mL, 20mg/mL, 30mg/mL, 40mg/mL, 50mg/mL and 60mg/mL, and are subjected to light-shielding oscillation at room temperature for 4 hours, and after adsorption, the absorbance of the solution at 438nm is detected by using an ultraviolet spectrophotometer, and the adsorption quantity Q (mg/g) of the chitin sponge and the chitin/graphene oxide composite sponge material is calculated by using formula 1. As can be seen from FIG. 7, with the increase of bilirubin concentration, the difference between the adsorption amounts of Ch/GO-20 and Ch further increases, and the difference reaches about 150mg/g at most; in addition, Ch reaches a saturation state when the bilirubin concentration is 40mg/mL, and Ch/GO-20 reaches the saturation state when the bilirubin concentration is 50mg/mL, so that the Ch/GO-20 has a faster adsorption rate and a wider applicable concentration range compared with Ch.
Fig. 8 shows a kinetic adsorption curve diagram of the chitin sponge obtained in comparative example 1 and the chitin/graphene oxide composite sponge material obtained in examples 1-3 under a simulated blood perfusion condition, wherein 10mg of the chitin sponge and the chitin/graphene oxide composite sponge material prepared in comparative example 1 and examples 1-3 are respectively weighed, 30mL of bilirubin solution with a concentration of 20mg/mL is respectively passed through the chitin/graphene oxide composite sponge material by using the pressure of a pump, the flow rate of the pump is 1mL/min, after circulation is performed for 8 times at room temperature, the absorbance of the solution at 438nm is detected by using an ultraviolet spectrophotometer, and the adsorption Q (mg/g) of the chitin sponge and the chitin/graphene oxide composite sponge material is calculated by using formula 1. As can be seen from fig. 8, although the advantages of the chitin/graphene oxide composite sponge are not so obvious at the beginning under the condition of simulating blood perfusion, after about 3.5 hours of adsorption, the adsorption capacity of the chitin/graphene oxide composite sponge is about 50-150 mg/g higher than that of the chitin sponge according to the difference of graphene oxide content, which means that in practical medical applications, the adsorption performance of the chitin/graphene oxide composite sponge is also greatly improved.
The formula for calculating the adsorption quantity Q (mg/g) of the chitin/graphene oxide composite sponge material is as follows:
wherein, C0Is the initial concentration (mg/L) of the bilirubin solution, CtIs the concentration (mg/L) of the bilirubin solution after a certain period of adsorption, V is the volume (L) of the bilirubin solution, and m is the mass (g) of the sponge material used for the adsorption of bilirubin.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (7)
1. The preparation method of the chitin/graphene oxide composite sponge is characterized by comprising the following steps:
dissolving chitin and graphene oxide in a sodium hydroxide/urea system by adopting a low-temperature freezing-melting method to obtain a solution containing the chitin and the graphene oxide;
heating the solution containing chitin and graphene oxide in a sealed manner at the temperature of 60-90 ℃ for 5-12 h to obtain chitin/graphene oxide hydrogel;
washing the hydrogel to be neutral, and freezing and drying to obtain the chitin/graphene oxide composite sponge material;
the mass ratio of the chitin to the graphene oxide in the chitin/graphene oxide hydrogel is 100: 20 to 30.
2. The method for preparing the chitin/graphene oxide composite sponge as claimed in claim 1, wherein the chitin is 1-4wt% in the solution.
3. The method for preparing chitin/graphene oxide composite sponge according to claim 1, wherein the solution containing chitin and graphene oxide is prepared by the following method: dissolving chitin and graphene oxide in a sodium hydroxide/urea solution at-80 to-40 ℃, and centrifuging to obtain a solution containing the chitin and the graphene oxide.
4. The method for preparing chitin/graphene oxide composite sponge according to claim 3, wherein the mass percent of sodium hydroxide is 8-11wt%, and the mass percent of urea is 4-6 wt%.
5. The method of claim 3, wherein the centrifugation speed is 3000-6000rpm and the centrifugation time is 5-30 min.
6. A chitin/graphene oxide composite sponge, which is prepared by the preparation method of the chitin/graphene oxide composite sponge of any one of claims 1-5.
7. The use of a chitin/graphene oxide composite sponge according to claim 6 for the preparation of a non-therapeutic bilirubin-adsorbing material.
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| CN109897235A (en) * | 2019-01-31 | 2019-06-18 | 华南理工大学 | A kind of chitin/graphene composite sponge and preparation method and application |
| CN110550693A (en) * | 2019-08-30 | 2019-12-10 | 大连理工大学 | Preparation method and application of ZnO-GO/chitin aerogel composite material |
| CN113061271B (en) * | 2021-04-08 | 2022-09-27 | 中国科学院深圳先进技术研究院 | Phosphorus-based graphene chitin gel photo-thermal film and preparation method and application thereof |
| CN113697796B (en) * | 2021-07-09 | 2023-01-20 | 中山大学 | Three-dimensionally communicated carbon nanosheet with ultrahigh specific surface area, and preparation method and application thereof |
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