CN103536625A - Nanometer cerium oxide composite and preparation method thereof as well as antioxidant - Google Patents
Nanometer cerium oxide composite and preparation method thereof as well as antioxidant Download PDFInfo
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Abstract
The invention relates to a nanometer cerium oxide composite and a preparation method thereof as well as an antioxidant. The nanometer cerium oxide composite is formed by beta-cyclodextrin grafted cambiform porous structure nanometer cerium oxide, has uniform particle diameter, good activity and very superior anti-oxidation capacity and is small in size and stable in water. The preparation method has the advantages of high yield, low cost and short production process.
Description
Technical field:
The present invention relates to technical field of nano material, be specifically related to a kind of nano-cerium oxide composite and preparation method thereof, antioxidant.
Technical background:
Oxidation reaction is the critical process of life continuation, but it is also that the mankind produce one of arch-criminal of disease simultaneously.Free radical or oxidant can decompose cell and tissue, affect metabolic function, and can cause different health problems.Under normal circumstances, cell can be resisted the injury that these free radicals bring, but because diet is unhealthy, the appearance of the problems such as Exposure to Sunlight, pressure, environmental pollution, it is very limited that the protection of cell self seems.If can eliminate too much oxyradical, for many free radicals, cause and aging-related disease can both prevent.Such as common cancer, arteriosclerosis, diabetes, cataract, cardiovascular diseases, senile dementia, arthritis etc., it is relevant to free radical that these diseases are all considered to.So it need to absorb some extra antioxidants, prevent the quick aging of cell or be killed.Studies have shown that, the antioxidant system of human body be one can be comparable with immune system, have and improve and the system of sophisticated functions, body antioxidative ability is stronger, just more healthy, life is also longer.In the last few years, along with people more and more pay attention to health, the research and development of antioxidant had also more and more caused interest widely.
The research of antioxidant at present mainly concentrates on organic or natural product, along with nano science is flourish, inorganic nano material is also little by little applied to the fields such as biological and medical treatment, and the unique features that for example cerium oxide nanostructure coexists due to its trivalent and tetravalence is used as antioxidant and is studied fast.But these materials are widely applied to and in medical treatment, remain a huge challenge, because inorganic matter is difficult to be dispersed in biological solvent, or when it is synthetic, with some toxic components, can not be applied to active somatic cell, therefore the synthetic nano-anti-oxidation inorganic matter that can combine with Biomedia becomes particularly important.Have researcher to utilize dextran, polymer etc. are grafted on the surface of nano-cerium oxide to help it to improve dispersibility and the stability in solvent, expand its application in antioxidation.But these method steps are more numerous and diverse, building-up process is difficult to control, and conditional request is harsh, is difficult to realize industrialization; And due to the combination of later-stage utilization molecule, reduced to a great extent the oxidation resistance of material itself.
Summary of the invention
For the deficiencies in the prior art, the invention provides a kind of nano-cerium oxide composite and preparation method thereof, antioxidant, nano-cerium oxide composite of the present invention consists of the spindle shape loose structure nano-cerium oxide of grafted by beta cyclodextrin, particle diameter is even, yardstick is little, activity is good, stable in water, there is very superior oxidation resistance, preparation method productive rate is high, cost is low, and production procedure is short.
The technical solution used in the present invention is:
A composite, consists of the spindle shape loose structure nano-cerium oxide of grafted by beta cyclodextrin; The length of described spindle shape loose structure nano-cerium oxide is 50～90nm, wide 20～50nm.
A preparation method for nano-cerium oxide composite, step comprises:
A, by beta-schardinger dextrin-and the water-soluble mixed solution that makes of cerous salt, in mixed solution, the ratio of the amount of substance of beta-schardinger dextrin-and cerous salt is 0.1～2:1, described beta-schardinger dextrin-concentration is 0.00125mol/L～0.4mol/L, and the concentration of cerous salt is 0.0125mol/L～0.2mol/L; Described cerous salt is selected from cerium chloride, one or more in cerous nitrate and cerous sulfate;
In B, the mixed solution that makes to steps A, add alkali and fully stir, making mixed solution produce cotton-shaped mixture; Described alkali is 3.75～30:1 with the ratio of the amount of substance of cerous salt; Described alkali is selected from sodium hydroxide and/or potassium hydroxide;
C, the mixed liquor that step B is made are heated to 100-200 ℃, and reaction 0.5-36 hour, is precipitated thing, and precipitate is filtered and washes clean, and dry, the spindle shape loose structure nano-cerium oxide that makes grafted by beta cyclodextrin is nano-cerium oxide composite;
, by nano-cerium oxide composite, made.
Nano-cerium oxide composite particle diameter prepared by the present invention is even, yardstick is little, active good, stable in water, there is very superior oxidation resistance; Preparation method productive rate is high, and cost is low, and production procedure is short, and method is simply controlled, and equipment requirements is not high, is applicable to suitability for industrialized production.
Accompanying drawing explanation
Fig. 1 is X-ray diffraction (XRD) figure of the nano-cerium oxide composite that makes of embodiment 1;
Fig. 2 is scanning electron microscopy (SEM) photo of the nano-cerium oxide composite that makes of embodiment 1;
Fig. 3 is transmission electron microscopy (TEM) photo of the nano-cerium oxide composite that makes of embodiment 1;
Fig. 4 is the ultraviolet light transmittance test pattern of the anti-hydrogen peroxide oxidation of nano-cerium oxide composite that makes of embodiment 1,
In figure, a is the light transmittance curve of the mixed liquor of nano-cerium oxide composite and water; B is that the mixed liquor of nano-cerium oxide composite and water adds the light transmittance curve immediately recording after hydrogen peroxide; C is that the mixed liquor of nano-cerium oxide composite and water adds the light transmittance curve that hydrogen peroxide placement recorded after 5 days; D is that the mixed liquor of nano-cerium oxide composite and water adds the light transmittance curve that hydrogen peroxide placement recorded after 20 days;
Fig. 5 is scanning electron microscopy (SEM) photo of the nano-cerium oxide composite that makes of embodiment 2;
Fig. 6 is scanning electron microscopy (SEM) photo of the nano-cerium oxide composite that makes of embodiment 3;
Fig. 7 is scanning electron microscopy (SEM) photo of the nano-cerium oxide composite that makes of embodiment 4;
Fig. 8 is scanning electron microscopy (SEM) photo of the nano-cerium oxide composite that makes of embodiment 5.
The specific embodiment
Embodiment 1
A composite, consists of the spindle shape loose structure nano-cerium oxide of grafted by beta cyclodextrin; The length of described spindle shape loose structure nano-cerium oxide is 60-80nm, wide 20-30nm.
A preparation method for nano-cerium oxide composite, step comprises:
A, by beta-schardinger dextrin-and the water-soluble mixed solution that makes of cerous nitrate, in mixed solution, the ratio of the amount of substance of beta-schardinger dextrin-and cerous nitrate is 1:1, described beta-schardinger dextrin-concentration is 0.1mol/L, the concentration of cerous nitrate is 0.1mol/L;
In B, the mixed solution that makes to steps A, add sodium hydroxide and fully stir; Described sodium hydroxide is 15:1 with the ratio of the amount of substance of cerous nitrate;
C, the mixed liquor that step B is made are heated to 120 ℃, react 3 hours, are precipitated thing, precipitate is cooling, filter, be washed to neutrality, and 60 ℃ of vacuum drying 12h obtain light yellow product, make nano-cerium oxide composite.
, by nano-cerium oxide composite, made.
The nano-cerium oxide composite making is dispersed in water by the concentration of 10g/L, under room temperature, after standing one month, observes, nano-cerium oxide composite is still dispersed in water uniformly, illustrates that the mixed liquor stability of itself and water is very good, has good water solublity.
The composite of preparation is carried out to oxidation resistance test: composite is dispersed in water by the concentration of 10g/L, gets the mixed liquor of 4 parts of each 3mL composites and water, with the light transmittance of ultraviolet-visible spectrophotometer test a copy of it mixed liquor; Then to all the other 3 portions of mixed liquors, respectively add one of 30% hydrogen peroxide, the light transmittance of test a copy of it mixed liquor; Then will remain 2 portions of mixed liquors places respectively after 5 days, 20 days and tests transmittance, test result is shown in Fig. 4, and as can be seen from Figure, nano-cerium oxide composite has good oxidation resistance in aqueous solution, in figure, a overlaps substantially with d, illustrates that cyclicity is very good.
Embodiment 2
A composite, consists of the spindle shape loose structure nano-cerium oxide of grafted by beta cyclodextrin; The length of described spindle shape loose structure nano-cerium oxide is 70-80nm, wide 20-30nm.
A preparation method for nano-cerium oxide composite, step comprises:
A, by beta-schardinger dextrin-and the water-soluble mixed solution that makes of cerium chloride, in mixed solution, the ratio of the amount of substance of beta-schardinger dextrin-and cerium chloride is 0.5:1, described beta-schardinger dextrin-concentration is 0.1mol/L, the concentration of cerium chloride is 0.2mol/L;
In B, the mixed solution that makes to steps A, add potassium hydroxide and fully stir, making mixed solution produce cotton-shaped mixture; Described potassium hydroxide is 5:1 with the ratio of the amount of substance of cerium chloride;
C, the mixed liquor that step B is made are heated to 180 ℃, react 0.5 hour, be precipitated thing, precipitate is filtered and washes clean, 60 ℃ of vacuum drying 12h, the spindle shape loose structure nano-cerium oxide that makes grafted by beta cyclodextrin is nano-cerium oxide composite;
, by nano-cerium oxide composite, made.
Embodiment 3
A composite, consists of the spindle shape loose structure nano-cerium oxide of grafted by beta cyclodextrin; The length of described spindle shape loose structure nano-cerium oxide is 70-90nm, wide 30-50nm.
A preparation method for nano-cerium oxide composite, step comprises:
A, by beta-schardinger dextrin-and the water-soluble mixed solution that makes of cerous nitrate, in mixed solution, the ratio of the amount of substance of beta-schardinger dextrin-and cerous nitrate is 2:1, described beta-schardinger dextrin-concentration is 0.025mol/L, the concentration of cerous nitrate is 0.0125mol/L;
In B, the mixed solution that makes to steps A, add sodium hydroxide and fully stir, making mixed solution produce cotton-shaped mixture; Described sodium hydroxide is 3.75:1 with the ratio of the amount of substance of cerous nitrate;
C, the mixed liquor that step B is made are heated to 150 ℃, react 20 hours, be precipitated thing, precipitate is filtered and washes clean, 60 ℃ of vacuum drying 12h, the spindle shape loose structure nano-cerium oxide that makes grafted by beta cyclodextrin is nano-cerium oxide composite;
, by nano-cerium oxide composite, made.
Embodiment 4
A composite, consists of the spindle shape loose structure nano-cerium oxide of grafted by beta cyclodextrin; The length of described spindle shape loose structure nano-cerium oxide is 60-90nm, wide 20-30nm.
A preparation method for nano-cerium oxide composite, step comprises:
A, by beta-schardinger dextrin-and the water-soluble mixed solution that makes of cerous sulfate, in mixed solution, the ratio of the amount of substance of beta-schardinger dextrin-and cerous sulfate is 0.1:1, described beta-schardinger dextrin-concentration is 0.002mol/L, the concentration of cerous sulfate is 0.02mol/L;
In B, the mixed solution that makes to steps A, add sodium hydroxide and fully stir, making mixed solution produce cotton-shaped mixture; Described sodium hydroxide is 30:1 with the ratio of the amount of substance of cerous sulfate;
C, the mixed liquor that step B is made are heated to 100 ℃, react 36 hours, be precipitated thing, precipitate is filtered and washes clean, 60 ℃ of vacuum drying 12h, the spindle shape loose structure nano-cerium oxide that makes grafted by beta cyclodextrin is nano-cerium oxide composite;
, by nano-cerium oxide composite, made.
Embodiment 5
A composite, consists of the spindle shape loose structure nano-cerium oxide of grafted by beta cyclodextrin; The length of described spindle shape loose structure nano-cerium oxide is 60-80nm, wide 30-50nm.
A preparation method for nano-cerium oxide composite, step comprises:
A, by beta-schardinger dextrin-and the water-soluble mixed solution that makes of cerous nitrate, in mixed solution, the ratio of the amount of substance of beta-schardinger dextrin-and cerous nitrate is 2:1, described beta-schardinger dextrin-concentration is 0.4mol/L, the concentration of cerous nitrate is 0.2mol/L;
In B, the mixed solution that makes to steps A, add sodium hydroxide and fully stir, making mixed solution produce cotton-shaped mixture; Described sodium hydroxide is 10:1 with the ratio of the amount of substance of cerous nitrate;
C, the mixed liquor that step B is made are heated to 200 ℃, react 12 hours, be precipitated thing, precipitate is filtered and washes clean, 60 ℃ of vacuum drying 12h, the spindle shape loose structure nano-cerium oxide that makes grafted by beta cyclodextrin is nano-cerium oxide composite;
, by nano-cerium oxide composite, made.
Claims (8)
1. a nano-cerium oxide composite, consists of the spindle shape loose structure nano-cerium oxide of grafted by beta cyclodextrin.
2. composite as claimed in claim 1, is characterized in that: the length of described spindle shape loose structure nano-cerium oxide is 50～90nm, wide 20～50nm.
3. a preparation method for nano-cerium oxide composite, step comprises:
A, by beta-schardinger dextrin-and the water-soluble mixed solution that makes of cerous salt, in mixed solution, the ratio of the amount of substance of beta-schardinger dextrin-and cerous salt is 0.1～2:1;
In B, the mixed solution that makes to steps A, add alkali and fully stir, making mixed solution produce cotton-shaped mixture;
C, the mixed liquor that step B is made are heated to 100-200 ℃, and reaction 0.5-36 hour, is precipitated thing, and precipitate is filtered and washes clean, and dry, the spindle shape loose structure nano-cerium oxide that makes grafted by beta cyclodextrin is nano-cerium oxide composite.
4. preparation method as claimed in claim 3, in described steps A, beta-schardinger dextrin-concentration is 0.00125mol/L～0.4mol/L, the concentration of cerous salt is 0.0125mol/L～0.2mol/L.
5. preparation method as claimed in claim 3, in described steps A, cerous salt is selected from cerium chloride, one or more in cerous nitrate and cerous sulfate.
6. preparation method as claimed in claim 3, in described step B, alkali is 3.75～30:1 with the ratio of the amount of substance of cerous salt.
7. preparation method as claimed in claim 3, in described step B, alkali is selected from sodium hydroxide and/or potassium hydroxide.
8. an antioxidant, is made by nano-cerium oxide composite.
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| CN106860427A (en) * | 2017-01-19 | 2017-06-20 | 浙江大学 | A kind of cerium oxide/iron oxide/nanometer composite and its preparation method and application |
| CN106975100A (en) * | 2016-01-15 | 2017-07-25 | 浙江大学 | A kind of nano composite material of cerium oxide/mesoporous silicon and its preparation method and application |
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