CN104649283A - Preparation method for nano beta-calcium silicate/selenium biological active composite material - Google Patents
Preparation method for nano beta-calcium silicate/selenium biological active composite material Download PDFInfo
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Abstract
The invention discloses a preparation method for a nano beta-calcium silicate/selenium biological active composite material. The preparation method is characterized by comprising the following steps: (1) at a room temperature, adding sodium oleate and calcium chloride into a three-mouth flask containing deionized water, absolute ethyl alcohol and normal hexane, and after heating in water bath and refluxing for a certain time, performing post-treatment to prepare calcium oleate; (2) adding the prepared calcium oleate into the three-mouth flask containing alcohol and an oil-soluble solvent, sufficiently dissolving at 45 DEG C, then, adding an aqueous solution of sodium silicate, heating in water bath and refluxing for a certain time; (3) cooling a reaction system to 0 DEG C, adding an aqueous solution of sodium selenite, sufficiently stirring, adding an aqueous solution of ascorbic acid and completely reacting at a room temperature; (4) alternatively washing and drying the prepared sample with the deionized water and the alcohol, and then roasting the sample in a muffle furnace to obtain the nano beta-calcium silicate/selenium biological active composite material. According to the antibacterial experiment, the composite material has antibacterial rates of 92+/-4% and 95+/-4% on escherichia coli and staphylococcus aureus respectively. As an antibacterial biological active material, the nano beta-calcium silicate/selenium biological active composite material has a wide application prospect.
Description
Technical field
The invention belongs to the preparation field of nano material, particularly a kind of preparation method with the bioactive composite material of the nanometer β-Calucium Silicate powder/selenium of germ resistance.
Background technology
In recent years, Calucium Silicate powder is studied widely in field of biology.Experiment in vivo and vitro proves, Calucium Silicate powder has good induction osteoid apatite Forming ability and Bioactivity, and in simulated body fluid, osteoid apatite is greater than the speed formed at other biological glass and glass-ceramic surface in the speed that Calucium Silicate powder surface is formed.In vitro cell experiment shows, Calucium Silicate powder no cytotoxicity and there is good biological activity, the calcium of stripping, silicon ion have the effect promoting Oesteoblast growth, further research also shows that calcium-silica-base material is compared calcium-phosphorous-based materials and had better osteogenic activity, and is applied on osseous tissue and joint as filling and repair materials.
In addition, bacteriological infection is inevitable complication in Implant, although through strict sterilization and aseptic technique, the infection rate still having 0.5-3% exists.Selenium is the necessary trace element of human body, nanometer selenium also has very strong antibacterial, research shows that nanometer selenium effectively can suppress the growth of streptococcus aureus and treat a series of infection (Tran because streptococcus aureus causes, P.A.Webster, T.J.Int.J.Nanomed.2001,6,1553-1558); By all demonstrating the colibacillary growth that the probiotic bacterium of being rich in selenium can suppress pathogenic in body with experiment in vitro, experiment in vitro confirms after 96h, and the probiotic bacterium (every gram of probiotic bacterium is containing 0.509 microgram selenium) of being rich in selenium just can suppress colibacillary growth; Inoculated colibacillary mouse is injected a certain amount of probiotic bacterium of being rich in selenium, after 28 days, is injected the survival rate of the mouse of the probiotic bacterium containing selenium apparently higher than (the Yang J do not injected, Huang K, Qin S, Zhao Z, Chen F.DigDis Sci.2009; 54 (2): 246-254).Namely being conducive to regulating tissue and the interaction of storeroom if designed, there are again two effect biological active materials of germ resistance, treatment reparation and preventing infection are integrated, being worth having important medical use.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of preparation method with the bioactive composite material of germ resistance.
In order to solve the problem, the invention provides the preparation method of a kind of nanometer β-Calucium Silicate powder/selenium bioactive composite material, it is characterized in that, comprise the following steps:
Step 1): under room temperature, sodium oleate, calcium chloride are joined respectively in the there-necked flask containing dehydrated alcohol, normal hexane and deionized water, after heating in water bath backflow, obtain calcium oleate through aftertreatment;
Step 2): joined by obtained calcium oleate in the there-necked flask containing ethanol, oil-dissolving solvent, make it fully dissolve at 45 DEG C, add the aqueous solution of water glass subsequently, heating in water bath refluxes;
Step 3): reaction system is cooled to 0 DEG C, then adds the aqueous solution of Sodium Selenite, after fully stirring, add Vitamin C aqueous acid, react completely under room temperature;
Step 4): by obtained sample respectively with the alternately washing of deionized water, ethanol, after drying, sample is calcined and is obtained in retort furnace nanometer β-Calucium Silicate powder/selenium matrix material.
Preferably, described step 1) in the temperature of water-bath be 70 DEG C ~ 75 DEG C, return time is 2-4h.
Preferably, described step 1) in the concentration of sodium oleate be 3.0mol/L, its solvent temperature is 45 DEG C.
Preferably, described step 1) in the volumetric molar concentration of calcium chloride be 3.0mol/L.
Preferably, described step 2) in the volumetric molar concentration of calcium oleate be 0.25mol/L.
Preferably, described step 2) oil-soluble solvent is hexanaphthene, normal hexane or toluene.
Preferably, described step 2) concentration of mesosilicic acid sodium solution is 0.25mol/L.
Preferably, described step 2) in the temperature of water-bath be 70 DEG C ~ 75 DEG C, return time is 2-4h.
Preferably, described step 3) in the volumetric molar concentration of Sodium Selenite be 0.3-0.5mol/L.
Preferably, described step 3) in the volumetric molar concentration of xitix be 0.6-1.0mol/L.
Preferably, described step 3) reaction times be 2-4h.
Preferably, described step 4) in alternately washing be specially: first use absolute ethanol washing, then remove supernatant liquor at 8000rpm centrifugation 10min; With deionized water wash, then remove supernatant liquor at 8000rpm centrifugation 15min, so circulate dehydrated alcohol-deionized water wash 3 times; Finally use absolute ethanol washing, under 8000rpm, centrifugation 10min is precipitated.
Preferably, described step 4) in dry temperature be 60 DEG C.
Preferably, described step 4) in the calcining temperature of retort furnace be 460-800 DEG C, calcination time is 2h.
Benzene is invented to the sign of material and the evaluation of anti-microbial property that provide
One, In Vitro Bacteriostasis performance test
The test of nanometer β-Calucium Silicate powder/selenium matrix material anti-microbial property is adopted with the following method: experimental strain adopts intestinal bacteria and streptococcus aureus.Get a certain amount of strain inoculation in the LB liquid nutrient medium of 50mL, on the constant-temperature table of 37 DEG C, 160rpm cultivates 18 ~ 24h, in order to antibacterial test.Laboratory sample and equipment used in testing are through 121 DEG C of high-temperature sterilization 20min; Bacterium liquid after former cultivation is diluted 102 times; Get the bacterium liquid 1mL after dilution to be inoculated in and nanometer β-Calucium Silicate powder to be housed, in the vial of nanometer β-Calucium Silicate powder/selenium matrix material; Sample and bacterium liquid add the stroke-physiological saline solution of 10mL respectively, cover tightly bottle cap acts on 18 ~ 24h in the constant incubator of 37 DEG C after, with hand rolling 30s, are eluted by bacterium; Get 100 μ L after the multiple that bacterium liquid normal saline dilution after wash-out is suitable on LB solid medium, be coated with flat board, parallel painting three, count cultivate 18 ~ 24h in the constant incubator of 37 DEG C after and average, then carry out converting the bacteria living number obtained in vial.Be calculated as follows the bacteriostasis rate of antimicrobial sample:
In formula:
C
t-control sample is inoculated and the mean value of the bacterial count recorded after cultivating 18 ~ 24h;
T
t-experiment sample is inoculated and the mean value of the bacterial count recorded after cultivating 18 ~ 24h.
The present invention has following outstanding beneficial effect:
1) concise in technology of the present invention, simple to operate;
2) antimicrobial efficiency of the nanometer β prepared by the present invention-Calucium Silicate powder/selenium compound is high, to intestinal bacteria and streptococcus aureus bacteriostasis rate be respectively 92 ± 4% and 95 ± 4%.
The present invention adopts water-oil interface method to synthesize the bioactive composite material of nanometer β-Calucium Silicate powder/selenium.Water-oil interface method, refers to that chemical reaction occurs in the interface of two-phase, is generally the reaction that two mutual exclusive water-oil interface occur.Utilize two phases in reaction, reactant can be dispersed in respectively in upper and lower two liquid, make Product formation in the interface of two-phase.Therefore the present invention mainly by the matrix material of water-oil interface synthesis of nano β-Calucium Silicate powder and nanometer selenium in conjunction with the excellent biological activity of Calucium Silicate powder and the effective germ resistance of nanometer selenium, play its each leisure advantage biologically, better application prospect will be had.
Accompanying drawing explanation
Fig. 1 is process flow sheet of the present invention;
The mixture X ray diffracting spectrum of the nanometer β of Fig. 2 obtained by the present invention-Calucium Silicate powder/selenium;
The mixture EDS collection of illustrative plates of the nanometer β of Fig. 3 obtained by the present invention-Calucium Silicate powder/selenium;
The mixture TEM of the nanometer β of Fig. 4 obtained by the present invention-Calucium Silicate powder/selenium schemes;
The antibacterial experiment design sketch of the mixture of the nanometer β of Fig. 5 obtained by the present invention-Calucium Silicate powder/selenium;
The mixture of the nanometer β of Fig. 6 obtained by the present invention-Calucium Silicate powder/selenium is to the experimental result statistical graph of intestinal bacteria and streptococcus aureus.
Embodiment
For making the present invention become apparent, hereby with preferred embodiment, and accompanying drawing is coordinated to be described in detail below.
Embodiment 1
(1) take 9.1g sodium oleate, 45 DEG C are dissolved in the deionized water of 10.0mL.After sodium oleate dissolves completely, add the calcium chloride water of 3.0mol/L.35.0mL normal hexane is added in system, and 20.0mL dehydrated alcohol.Heating in water bath is backflow extremely, magnetic agitation 2h.
(2) after question response completes, be cooled to 0 DEG C, the solid of adularescent is separated out, and vacuum filtration, calcium oleate is prepared in drying.
(3) 2.3g calcium oleate is taken, in the dehydrated alcohol of 45 DEG C of hexanaphthenes being dissolved in 15.0mL, 10.0mL.After calcium oleate dissolves completely, add the sodium silicate aqueous solution of 0.25mol/L.Heating in water bath is backflow extremely, magnetic agitation 2h.
(4) after above-mentioned reaction completes, be cooled to 0 DEG C, add the sodium selenite aqueous solution of 0.3mol/L, after fully stirring, add the aqueous ascorbic acid of 0.6mol/L, reaction 2h.
(5), after reaction terminates, absolute ethanol washing, then removes supernatant liquor at 8000rpm centrifugation 10min; Deionized water wash, removes supernatant liquor at 8000rpm centrifugation 15min, and so circulate dehydrated alcohol-deionized water wash 3 times; Finally use absolute ethanol washing, under 8000rpm, centrifugation 10min is precipitated.60 DEG C of dryings in air dry oven, are finally placed in the matrix material that namely retort furnace 460 DEG C calcining 2h obtains nanometer β-Calucium Silicate powder/selenium; When calcining temperature is 800 DEG C, the product of acquisition is β-Calucium Silicate powder.
(6) nanometer β-Calucium Silicate powder/selenium matrix material is used for the antibacterial experiment of intestinal bacteria and streptococcus aureus.
Embodiment 2
(1) take 9.1g sodium oleate, 45 DEG C are dissolved in the deionized water of 10.0mL.After sodium oleate dissolves completely, add the calcium chloride water of 3.0mol/L.35.0mL normal hexane is added in system, and 20.0mL dehydrated alcohol.Heating in water bath is backflow extremely, magnetic agitation 3h.
(2) after question response completes, be cooled to 0 DEG C, the solid of adularescent is separated out, and vacuum filtration, calcium oleate is prepared in drying.
(3) 2.3g calcium oleate is taken, in the dehydrated alcohol of 45 DEG C of normal hexanes being dissolved in 15.0mL, 10.0mL.After calcium oleate dissolves completely, add the sodium silicate aqueous solution of 0.25mol/L.Heating in water bath is backflow extremely, magnetic agitation 3h.
(4) after above-mentioned reaction completes, be cooled to 0 DEG C, add the sodium selenite aqueous solution of 0.4mol/L, after fully stirring, add the aqueous ascorbic acid of 0.8mol/L, reaction 3h.
(5) after reaction terminates, with absolute ethanol washing, then supernatant liquor is removed at 8000rpm centrifugation 10min; With deionized water wash, then remove supernatant liquor at 8000rpm centrifugation 15min, so circulate dehydrated alcohol-deionized water wash 3 times; Finally use absolute ethanol washing, under 8000rpm, centrifugation 10min is precipitated.60 DEG C of dryings in air dry oven, are finally placed in the matrix material that namely retort furnace 460 DEG C calcining 2h obtains nanometer β-Calucium Silicate powder/selenium.
Embodiment 3
(1) take 9.1g sodium oleate, 45 DEG C are dissolved in the deionized water of 10.0mL.After sodium oleate dissolves completely, add the calcium chloride water of 3.0mol/L.35.0mL normal hexane is added in system, and 20.0mL dehydrated alcohol.Heating in water bath is backflow extremely, magnetic agitation 4h.
(2) after question response completes, be cooled to 0 DEG C, the solid of adularescent is separated out, and vacuum filtration, calcium oleate is prepared in drying.
(3) 2.3g calcium oleate is taken, in the dehydrated alcohol of 45 DEG C of toluene being dissolved in 15.0mL, 10.0mL.After calcium oleate dissolves completely, add the sodium silicate aqueous solution of 0.25mol/L.Heating in water bath is backflow extremely, magnetic agitation 4h.
(4) after above-mentioned reaction completes, be cooled to 0 DEG C, add the sodium selenite aqueous solution of 0.5mol/L, after fully stirring, add the aqueous ascorbic acid of 1.0mol/L, reaction 4h.
(5) after reaction terminates, first use absolute ethanol washing, then remove supernatant liquor at 8000rpm centrifugation 10min; With deionized water wash, then remove supernatant liquor at 8000rpm centrifugation 15min, so circulate dehydrated alcohol-deionized water wash 3 times; Finally use absolute ethanol washing, under 8000rpm, centrifugation 10min is precipitated.60 DEG C of dryings in air dry oven, are finally placed in the matrix material that namely retort furnace 460 DEG C calcining 2h obtains nanometer β-Calucium Silicate powder/selenium.
As shown in Figure 1, be the mixture reacting flow chart of nanometer β-Calucium Silicate powder/selenium.
Fig. 2 is the mixture XRD figure spectrum of nanometer β-Calucium Silicate powder/selenium that embodiment 1-3 obtains, and wherein, (a) is under 460 DEG C of calcination conditions; B () is under 800 DEG C of calcination conditions.
Fig. 3 is the EDS collection of illustrative plates of the mixture of nanometer β-Calucium Silicate powder/selenium that embodiment 1-3 obtains.
Fig. 4 is the TEM figure of the matrix material of nanometer β-Calucium Silicate powder/selenium that embodiment 1 obtains.
Fig. 5 is the antibacterial effect figure of nanometer β-Calucium Silicate powder/selenium matrix material that embodiment 1 obtains, and is respectively the experiment of intestinal bacteria blank (a1), β-Calucium Silicate powder (b1), β-Calucium Silicate powder/selenium (c1); The experiment of staphylococcus aureus blank (a2), β-Calucium Silicate powder (b2), β-Calucium Silicate powder/selenium (c2).
Fig. 6 is that the surface adhesion colony number after the obtained intestinal bacteria of embodiment 1 and streptococcus aureus and two groups of sample contacts cultivate 24h adds up that (* represents sample β-CaSiO
3/ and blank between variant) (mean value ± standard deviation, n=5, * * P < 0.01).
Claims (14)
1. a preparation method for nanometer β-Calucium Silicate powder/selenium bioactive composite material, is characterized in that, comprise the following steps:
Step 1): under room temperature, sodium oleate, calcium chloride are joined respectively in the there-necked flask containing dehydrated alcohol, normal hexane and deionized water, after heating in water bath backflow, obtain calcium oleate through aftertreatment;
Step 2): joined by obtained calcium oleate in the there-necked flask containing ethanol, oil-dissolving solvent, make it fully dissolve at 45 DEG C, add the aqueous solution of water glass subsequently, heating in water bath refluxes;
Step 3): reaction system is cooled to 0 DEG C, then adds the aqueous solution of Sodium Selenite, after fully stirring, add Vitamin C aqueous acid, react completely under room temperature;
Step 4): by obtained sample respectively with the alternately washing of deionized water, ethanol, after drying, sample is calcined and is obtained in retort furnace nanometer β-Calucium Silicate powder/selenium matrix material.
2. the preparation method of nanometer β-Calucium Silicate powder/selenium bioactive composite material as claimed in claim 1, is characterized in that, described step 1) in the temperature of water-bath be 70 DEG C ~ 75 DEG C, return time is 2-4h.
3. the preparation method of the bioactive composite material of nanometer β-Calucium Silicate powder/selenium as claimed in claim 1, is characterized in that, described step 1) in the concentration of sodium oleate be 3.0mol/L, its solvent temperature is 45 DEG C.
4. the preparation method of the bioactive composite material of nanometer β-Calucium Silicate powder/selenium as claimed in claim 1, is characterized in that, described step 1) in the volumetric molar concentration of calcium chloride be 3.0mol/L.
5. the preparation method of the bioactive composite material of nanometer β-Calucium Silicate powder/selenium as claimed in claim 1, is characterized in that, described step 2) in the volumetric molar concentration of calcium oleate be 0.25mol/L.
6. the preparation method of the bioactive composite material of nanometer β-Calucium Silicate powder/selenium as claimed in claim 1, is characterized in that, described step 2) oil-soluble solvent is hexanaphthene, normal hexane or toluene.
7. the preparation method of the bioactive composite material of nanometer β-Calucium Silicate powder/selenium as claimed in claim 1, is characterized in that, described step 2) concentration of mesosilicic acid sodium solution is 0.25mol/L.
8. the preparation method of the bioactive composite material of nanometer β-Calucium Silicate powder/selenium as claimed in claim 1, is characterized in that, described step 2) in the temperature of water-bath be 70 DEG C ~ 75 DEG C, return time is 2-4h.
9. the preparation method of the bioactive composite material of nanometer β-Calucium Silicate powder/selenium as claimed in claim 1, is characterized in that, described step 3) in the volumetric molar concentration of Sodium Selenite be 0.3-0.5mol/L.
10. the preparation method of the bioactive composite material of nanometer β-Calucium Silicate powder/selenium as claimed in claim 1, is characterized in that, described step 3) in the volumetric molar concentration of xitix be 0.6-1.0mol/L.
The preparation method of the bioactive composite material of 11. nanometer β-Calucium Silicate powder/selenium as claimed in claim 1, is characterized in that, described step 3) reaction times be 2-4h.
The preparation method of the bioactive composite material of 12. nanometer β-Calucium Silicate powder/selenium as claimed in claim 1, it is characterized in that, described step 4) in alternately washing be specially: first use absolute ethanol washing, then remove supernatant liquor at 8000rpm centrifugation 10min; With deionized water wash, then remove supernatant liquor at 8000rpm centrifugation 15min, so circulate dehydrated alcohol-deionized water wash 3 times; Finally use absolute ethanol washing, under 8000rpm, centrifugation 10min is precipitated.
The preparation method of the bioactive composite material of 13. nanometer β-Calucium Silicate powder/selenium as claimed in claim 1, is characterized in that, described step 4) in dry temperature be 60 DEG C.
The preparation method of the bioactive composite material of 14. β-Calucium Silicate powder/selenium as claimed in claim 1, is characterized in that, described step 4) in the calcining temperature of retort furnace be 460-800 DEG C, calcination time is 2h.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105217681A (en) * | 2015-10-29 | 2016-01-06 | 东华大学 | A kind of method by regulating temperature of reaction to prepare different crystal forms nanometer titanium dioxide hafnium particle |
| CN105256354A (en) * | 2015-10-29 | 2016-01-20 | 东华大学 | Preparing method of 316 L stainless steel with surface containing nanometer Se particles |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105217681A (en) * | 2015-10-29 | 2016-01-06 | 东华大学 | A kind of method by regulating temperature of reaction to prepare different crystal forms nanometer titanium dioxide hafnium particle |
| CN105256354A (en) * | 2015-10-29 | 2016-01-20 | 东华大学 | Preparing method of 316 L stainless steel with surface containing nanometer Se particles |
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