CN106975100A - A kind of nano composite material of cerium oxide/mesoporous silicon and its preparation method and application - Google Patents
A kind of nano composite material of cerium oxide/mesoporous silicon and its preparation method and application Download PDFInfo
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- A61L26/00—Chemical aspects of, or use of materials for, wound dressings or bandages in liquid, gel or powder form
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- A61L26/00—Chemical aspects of, or use of materials for, wound dressings or bandages in liquid, gel or powder form
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Abstract
The present invention relates to a kind of nano composite material of cerium oxide/mesoporous silicon, the cerium oxide nanocrystal and amido modified nanometer particle changed comprising part, the cerium oxide nanocrystal of part conversion are modified in the surface of amido modified nanometer particle；The mass ratio of cerium oxide nanocrystal that part is changed and amido modified nanometer particle is 1~20；The cerium oxide nanocrystal of part conversion carries out part conversion using 2- bromo acids.The invention further relates to the preparation method of the nano composite material of cerium oxide/mesoporous silicon and its application in wound healing or tissue repair.The composite can balance the active oxygen radical level of the surface of a wound, reduce level of inflammation, and adhesive effect is played using nanometer bridge effect；And preparing reaction system gently, condition is controllable, and prepared material is respectively provided with good biocompatibility, with good clinical conversion possibility.
Description
Technical field
The present invention relates to cerium oxide/mesoporous silicon field of composite material preparation, and in particular to a kind of nano composite material of cerium oxide/mesoporous silicon and its preparation method and application.
Background technology
Chronic refractory skin trauma brings pain to patient, while bringing white elephant to health system.Because chronic refractory sexual trauma is with very high disability rate and fatal rate, needs badly and develop the deficiency that new treatment means make up existing therapies means.According to statistics, only in the chronic refractory trauma patient in the U.S. just about 6,500,000, the cost for chronic refractory sexual trauma every year just more than 25,000,000,000 dollars, and it is contemplated that, with obesity, the incidence of disease more and more higher of diabetes, this numeral will also continue to increase.
To the afunction of various molecular cell signals necessary to normal wound healing process or to be interfered be the basic reason to form chronic refractory sexual trauma.In addition, the microorganisms intrusion surface of a wound in external environment also results in chronic inflammatory reaction, more it is unfavorable for the healing of the surface of a wound.There is certain correlation in existing document report, the generation of chronic inflammatory reaction and tumour.In addition to chronic refractory sexual trauma, promote by liver, kidney, lung, the healing of wound and recoverys of organ dysfunction that the internal organ operation such as heart is caused are also to work as the intractable difficult medical problem of previous comparison.For by liver, kidney, lung, the wound that the internal organ operation such as heart is caused, operation stitching and polymer bonding agent are conventional at present and effective treatment means.But for liver, for Fei Deng soft connective tissues, operation stitching can cause certain organ injury.Polymer bonding agent is also because the condition of the polymerization or cross-linking reaction in control volume is excessively complicated and the reason such as limited is acted in the vivo environment of moistening limit its application.
The characteristics of being moistened for some internal organs softness and cause many external internal factors of chronic refractory sexual trauma, some nearest basic research and preclinical study show that nano-particle has huge potentiality in terms of the wound healing for promoting a variety of causes to cause.Ludwik Leibler et al. achievement in research finds that a drop silicon nano solution can produce quick strong adhesive effect between two blocks of single hydrogels at ambient temperature.The Ludwik Leibler et al.'s test result indicates that consistent with the result on hydrogel in animal skin wound and internal organ operation wound model, nano-particle solution can accelerate the healing of wound by a kind of so-called nanometer bridge effect.
But existing result of study shows, due to shortage glutathione, the endogenic antioxidant such as vitamin E so that one of the reason for elevated reactive oxygen species of site of injury is the chronic refractory sexual trauma of formation such as diabetes and age ageing can not be neutralized.Therefore, only accelerate the healing of wound by nanometer bridge effect in the prior art, the reactive oxygen species of site of injury, the DeGrain of accelerating wound healing are not balanced with antioxidant.
The content of the invention
The purpose of the present invention is to overcome defect of the prior art there is provided a kind of nano composite material of cerium oxide/mesoporous silicon and its preparation method and application.
The technical scheme that the present invention is provided is as follows：
A kind of nano composite material of cerium oxide/mesoporous silicon, the cerium oxide nanocrystal and amido modified nanometer particle changed comprising part, the cerium oxide nanocrystal of described part conversion is modified in the surface of amido modified nanometer particle；The mass ratio of cerium oxide nanocrystal that part is changed and amido modified nanometer particle is 1~20；The cerium oxide nanocrystal of described part conversion carries out part conversion using 2- bromo acids.
The nano composite material for above-mentioned cerium oxide/mesoporous silicon that the present invention is provided can balance the active oxygen radical level of the surface of a wound, reduce level of inflammation, and play adhesive effect using nanometer bridge effect.First, nanometer particle has nanometer bridge effect, can promote wound healing；Secondly, cerium oxide nanocrystal can balance the elevated reactive oxygen species of site of injury, and then oxidative damage effect of the reactive oxygen species to the cell membrane and protein of periwound environment is reduced, the cerium oxide nanocrystal of energy neutralization activity oxygen cluster is used for wound repair, the deficiency of endogenous antioxidant can be made up.In order to which cerium oxide nanocrystal is connected into nanometer particle surface in the form of stable covalent bond, part conversion is carried out to cerium oxide nanocrystal first with 2- bromo acids, nanometer particle surface is carried out again amido modified, be conducive between the two compound, finally make it that performance is further lifted after two kinds of Material claddings.
Preferably, the particle diameter for the cerium oxide nanocrystal that described part is changed is 1~10nm, the particle diameter of described amido modified nanometer particle is 5~500nm.Cerium oxide nanocrystal and the affiliated particle size range of nanometer particle, are easy to the uniform composite that must be modified in the surface of nanometer particle, obtain pattern and excellent performance of cerium oxide nanocrystal.
The present invention also provides a kind of preparation method of the nano composite material of cerium oxide/mesoporous silicon, comprises the following steps：
1) cerous acetate hydrate and oleyl amine are added in dimethylbenzene, 3~6h are reacted at 85 DEG C~95 DEG C, aging, precipitation obtain cerium oxide nanocrystal；
2) to step 1) in obtained cerium oxide nanocrystal, carry out part conversion using 2- bromo acids, obtain the cerium oxide nanocrystal of part conversion；
3) and then by hexadecyltrimethylammonium chloride and triethanolamine it is dissolved in water, 0.5~5h is reacted at 90 DEG C~100 DEG C, tetraethyl orthosilicate is continuously added and 3- aminopropyl triethoxysilanes reacts 0.5~5h, centrifugation, washing, obtains amido modified mesoporous silicon dioxide nano particle；
4) cerium oxide nanocrystal and amido modified nanometer particle changed part are added in ethanol, and 8~15h is reacted at 45 DEG C~55 DEG C, the nano composite material of cerium oxide/mesoporous silicon is obtained.
Using above-mentioned preparation method, the nano composite material of cerium oxide/mesoporous silicon can be prepared, the composite can balance the active oxygen radical level of the surface of a wound by cerium oxide nanocrystal, reduce level of inflammation, adhesive effect can be played using the nanometer bridge effect of nanometer particle again, therefore, the advantage of two kinds of materials is mutually aided in so that the performance of the nano composite material of cerium oxide/mesoporous silicon further gets a promotion.
Preferably, described step 1) in cerous acetate hydrate and oleyl amine mass ratio be 1:7~9.
Preferably, described step 3) in hexadecyltrimethylammonium chloride, triethanolamine, the rate of charge of tetraethyl orthosilicate and 3- aminopropyl triethoxysilanes be：1.5~2.5g：0.03~0.05g：1.4~1.6ml：0.14~0.16ml.
Preferably, described step 4) in the cerium oxide nanocrystal changed of part and amido modified nanometer particle mass ratio into 1~20.Pass through the mass ratio of regulation and control between the two, control the content of the cerium oxide nanocrystal that part is changed in the nano composite material of cerium oxide/mesoporous silicon, so that the cerium oxide nanocrystal of part conversion is easy to modify in amido modified nanometer particle surface, it is easy to the regulation and control of pattern and the modification of cerium oxide nanocrystal.
Preferably, described step 2) in part conversion refer to, by step 1) in obtained cerium oxide nanocrystal, 2- bromo acids and citric acid be added sequentially to chloroform and the in the mixed solvent of N-N dimethylformamides stirs 20~30h.Part conversion is in order to cerium oxide nanocrystal is connected into nanometer particle surface in the form of stable covalent bond.
Preferably, described 2- bromo acids and the mass ratio of cerium oxide nanocrystal are：20~60.
The present invention also provides a kind of application of nano composite material of cerium oxide/mesoporous silicon in wound healing.
Compared with the existing technology, beneficial effects of the present invention are embodied in：
(1) cerium oxide/mesoporous silicon novel nanocomposite materials can balance the active oxygen radical level of the surface of a wound, reduce level of inflammation, and playing the mechanism such as adhesive effect using nanometer bridge effect promotes acute and chronic wound healing and tissue repair.
(2) gentle the present invention relates to reaction system, condition is controllable, and prepared material is respectively provided with good biocompatibility, with good clinical conversion possibility.
Brief description of the drawings
The X-ray diffractogram for the cerium oxide nanocrystal that Fig. 1 changes for the part in embodiment 1；
The transmission electron microscope photo for the cerium oxide nanocrystal that Fig. 2 changes for the part in embodiment 1；
Fig. 3 be embodiment 1 in amido modified nanometer particle transmission electron microscope photo；
Fig. 4 be embodiment 1 in cerium oxide/mesoporous silicon nano composite material transmission electron microscope photo；
Fig. 5 be embodiment 1 in cerium oxide/mesoporous silicon nano composite material scanning transmission electron microscope photo；
Fig. 6 be embodiment 1 in cerium oxide/mesoporous silicon nano composite material distribution diagram of element；
Fig. 7 be application examples in cerium oxide/mesoporous silicon nano composite material MTS cytoactive quantitative analysis results figures；
Fig. 8 is the different materials processing SD rat trauma model Healing Rates in the present invention, and wherein MSN-ceria is the nano composite material of cerium oxide/mesoporous silicon, and MSN is nanometer particle, and Control is blank test；
Fig. 9 is the picture of the processing SD rat trauma models of the different materials in the present invention, and wherein MSN-ceria is the nano composite material of cerium oxide/mesoporous silicon, and MSN is nanometer particle, and Control is blank test.
Embodiment
The preparation and its application in wound healing is promoted of cerium oxide of the present invention/nanometer composite are elaborated with reference to specific embodiment and accompanying drawing.
Embodiment 1
(1) synthesis of cerium oxide nanocrystal and part conversion：0.4g cerous acetates hydrate and 3.2g oleyl amines are added in 15ml dimethylbenzene, are stirred at room temperature 4 hours, hastens to rise to 90 degrees Celsius with the heating of 2 centigrade per minutes；1ml deionized waters are expelled in reaction system, aging three hours, acetone precipitation, centrifugation obtains cerium oxide nanocrystal.Cerium oxide nanocrystal, 0.5g 2- bromo acids and the 0.05g citric acids that synthesis is obtained are added sequentially to 7.5ml chloroforms and the in the mixed solvent stirring of 7.5ml N,N-dimethylformamides is produced for 24 hours.
The cerium oxide nanocrystal of part conversion to obtaining carries out X-ray diffraction, as shown in Figure 1；And the cerium oxide nanocrystal changed to part carries out morphology characterization with transmission electron microscope, as shown in Figure 2.
(2) synthesis of amido modified mesoporous silicon dioxide nano particle：2g hexadecyltrimethylammonium chlorides and 0.02g triethanolamines are added in 20ml deionized waters, stirring is warming up to 95 degrees Celsius, add tetraethyl orthosilicate 1.5ml and 150 0.5~1h of μ L 3- aminopropyl triethoxysilane stirring reactions.Template is washed away by centrifugation and 1wt% sodium chloride methanol solutions and can obtain amido modified mesoporous silicon dioxide nano particle.
Transmission electron microscope morphology characterization is carried out to the amido modified nanometer particle prepared, as shown in Figure 3.
(3) synthesis of the nano composite material of cerium oxide/mesoporous silicon：The concentration that 5ml parts are changed reacts the nano composite material that can obtain cerium oxide/mesoporous silicon for 12 hours into the ethanol solution of the ethanol solution of 0.6mM cerium oxide nanocrystals and amido modified mesoporous silicon dioxide nano particle of 1ml 0.5mg/ml at 45 degrees Celsius.Carry out transmission electron microscope and scanning transmission electron microscope to the nano composite material for obtaining cerium oxide/mesoporous silicon, acquired results as shown in Figures 4 and 5, a diameter of 50~60nm of the nano composite material of cerium oxide/mesoporous silicon；Elementary analysis is also carried out in addition, as shown in Figure 6, it is known that the ball of grey refers to mesoporous silicon, white point refers to cerium oxide.
Embodiment 2
(1) synthesis of cerium oxide nanocrystal and part conversion：0.4g cerous acetates hydrate and 3.6g oleyl amines are added in dimethylbenzene, are stirred at room temperature 6 hours, hastens to rise to 95 degrees Celsius with the heating of 2 centigrade per minutes；1ml deionized waters are expelled in the reaction system of inert gas shielding, aging three hours, acetone precipitation, centrifugation obtains cerium oxide nanocrystal.The oxidation that synthesis is obtained is nanocrystalline, 0.5g 2- bromo acids and 0.05g citric acids are added sequentially to 7.5ml chloroforms and the in the mixed solvent stirring of 7.5ml N,N-dimethylformamides is produced for 24 hours.
(2) synthesis of amido modified mesoporous silicon dioxide nano particle：2.4g hexadecyltrimethylammonium chlorides and 0.05g triethanolamines are added in 20ml deionized waters, stirring is warming up to 95 degrees Celsius, add tetraethyl orthosilicate 1.4ml and 160 μ L 3- aminopropyl triethoxysilane stirring reactions.Template is washed away by centrifugation and 1wt% sodium chloride methanol solutions and can obtain amido modified mesoporous silicon dioxide nano particle.
(3) synthesis of the nano composite material of cerium oxide/mesoporous silicon：The concentration that 8ml parts are changed can obtain the nano composite material of cerium oxide/mesoporous silicon for 12 hours into the ethanol solution of 0.6mM cerium oxide nanocrystals and the sub 50 degrees Celsius of reactions in ethanol system of the amido modified mesoporous silicon dioxide nano particles of 1ml 0.5mg/ml.
Embodiment 3
(1) synthesis of cerium oxide nanocrystal and part conversion：0.4g cerous acetates hydrate and 2.8g oleyl amines are added in dimethylbenzene, are stirred at room temperature 3 hours, hastens to rise to 88 degrees Celsius with the heating of 2 centigrade per minutes；1ml deionized waters are expelled in the reaction system of inert gas shielding, aging three hours, acetone precipitation, centrifugation obtains cerium oxide nanocrystal.The oxidation that synthesis is obtained is nanocrystalline, 0.5g 2- bromo acids and 0.05g citric acids are added sequentially to 7.5ml chloroforms and the in the mixed solvent stirring of 7.5ml N,N-dimethylformamides is produced for 24 hours.
(2) synthesis of amido modified mesoporous silicon dioxide nano particle：2g hexadecyltrimethylammonium chlorides and 0.04g triethanolamines are added in 20ml deionized waters, stirring is warming up to 95 degrees Celsius, add tetraethyl orthosilicate 1.4ml and 160 μ L 3- aminopropyl triethoxysilane stirring reactions.Template is washed away by centrifugation and 1wt% sodium chloride methanol solutions and can obtain amido modified mesoporous silicon dioxide nano particle.
(3) synthesis of the nano composite material of cerium oxide/mesoporous silicon：The concentration that 4ml parts are changed can obtain the nano composite material of cerium oxide/mesoporous silicon for 12 hours into the ethanol solution of 0.6mM cerium oxide nanocrystals and the sub 60 degrees Celsius of reactions in ethanol system of the amido modified mesoporous silicon dioxide nano particles of 1ml 0.5mg/ml.
Application examples
The nano composite material of cerium oxide/mesoporous silicon is used for SD rats and promotes skin wound healing
Biocompatibility in vitro is evaluated：Human skin fibroblasts strain (HSF) is selected to investigate the biocompatibility in vitro of the nano composite material of various concentrations nanometer material and cerium oxide/mesoporous silicon.MTS cytoactive quantitative analysis results are as shown in Figure 7, various concentrations group cell survival rate shows that the nano composite material (MSN-ceria) of nanometer material (MSN) and cerium oxide/mesoporous silicon is respectively provided with good biocompatibility in vitro more than 80%.
The foundation and interpretation of result of skin trauma model：10wt% chloraldurates are anaesthetized to SD rats by intraperitoneal injection according to 4ml/kg dosage, back hair is rejected, the wound of the full skin thickness of standardized 2 centimeter lengths at back.Rat is randomly divided into 3 groups, every group 5.3 groups of rat back site of injurys give blank (control), 50 μ L 10mg/ml nanometer particle water dispersion solutions (MSN), the nano composite material water dispersion solution (MSN-ceria) of 50 μ L 10mg/ml cerium oxide/mesoporous silicon respectively.At the appointed time point records each group wound length recovery situation.The reparation speed of wound is as shown in figure 8, Fig. 9 is rat back wound first day and the photo of the 9th day.
Technical scheme and beneficial effect are described in detail embodiment described above; it should be understood that the foregoing is only the specific embodiment of the present invention; it is not intended to limit the invention; all any modifications made in the spirit of the present invention; supplement and equivalent substitution etc., should be included in the scope of the protection.
Claims (9)
1. a kind of nano composite material of cerium oxide/mesoporous silicon, it is characterised in that the oxygen changed comprising part
Change the nanocrystalline and amido modified nanometer particle of cerium, the cerium oxide nanocrystal that described part is changed
Modify in the surface of amido modified nanometer particle；The cerium oxide nanocrystal and amino of part conversion
The mass ratio of the nanometer particle of modification is 1~20；The cerium oxide nanocrystal profit of described part conversion
Part conversion is carried out with 2- bromo acids.
2. the nano composite material of cerium oxide/mesoporous silicon according to claim 1, it is characterised in that
The particle diameter for the cerium oxide nanocrystal that described part is changed is 1~10nm, described amido modified mesoporous silicon
The particle diameter of nano-particle is 5~500nm.
3. a kind of preparation side of the nano composite material of cerium oxide/mesoporous silicon as claimed in claim 1 or 2
Method, it is characterised in that comprise the following steps：
1) cerous acetate hydrate and oleyl amine are added in dimethylbenzene, 3~6h are reacted at 85 DEG C~95 DEG C,
Aging, precipitation, obtain cerium oxide nanocrystal；
2) to step 1) in obtained cerium oxide nanocrystal, carry out part conversion using 2- bromo acids,
Obtain the cerium oxide nanocrystal of part conversion；
3) water and then by hexadecyltrimethylammonium chloride and triethanolamine is dissolved in, it is anti-at 90 DEG C~100 DEG C
0.5~5h is answered, tetraethyl orthosilicate is continuously added and 3- aminopropyl triethoxysilanes reacts 0.5~5h, centrifuge,
Washing, obtains amido modified mesoporous silicon dioxide nano particle；
4) cerium oxide nanocrystal and amido modified nanometer particle changed part are added to ethanol
In, 8~15h is reacted at 45 DEG C~55 DEG C, the nano composite material of cerium oxide/mesoporous silicon is obtained.
4. the preparation method of the nano composite material of cerium oxide/mesoporous silicon according to claim 3, its
Be characterised by, described step 1) in cerous acetate hydrate and oleyl amine mass ratio be 1:7~9.
5. the preparation method of the nano composite material of cerium oxide/mesoporous silicon according to claim 3, its
Be characterised by, described step 3) in hexadecyltrimethylammonium chloride, triethanolamine, tetraethyl orthosilicate
Rate of charge with 3- aminopropyl triethoxysilanes is：1.5~2.5g：0.03~0.05g：1.4~1.6ml：
0.14~0.16ml.
6. the preparation method of the nano composite material of cerium oxide/mesoporous silicon according to claim 3, its
Be characterised by, described step 4) in part change cerium oxide nanocrystal received with amido modified mesoporous silicon
The mass ratio of rice corpuscles is 1~20.
7. the preparation method of the nano composite material of cerium oxide/mesoporous silicon according to claim 3, its
Be characterised by, described step 2) in part conversion refer to, by step 1) in obtained cerium oxide nano
Brilliant, 2- bromo acids and citric acid are added sequentially to the mixed solvent of chloroform and N-N dimethylformamides
20~30h of middle stirring.
8. the preparation method of the nano composite material of cerium oxide/mesoporous silicon according to claim 7, its
It is characterised by, described 2- bromo acids and the mass ratio of cerium oxide nanocrystal are：20~60.
9. a kind of nano composite material of cerium oxide/mesoporous silicon as claimed in claim 1 or 2 is in wound healing
Application in conjunction.
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| CN114949205A (en) * | 2021-11-18 | 2022-08-30 | 昆明理工大学 | Preparation method and application of mesoporous nano material |
| CN114949205B (en) * | 2021-11-18 | 2023-12-19 | 昆明理工大学 | Preparation method and application of mesoporous nano material |
| RU2777167C1 (en) * | 2021-11-29 | 2022-08-01 | ОБЩЕСТВО С ОГРАНИЧЕННОЙ ОТВЕТСТВЕННОСТЬЮ "НОВАСКИН" (ООО "Новаскин") | Method for obtaining a remedy for eliminating skin defects and treating wounds in the form of a gel |
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