CN104488966A - Antimicrobial agent for quartz-carried nano silver phosphate ceramic and preparation method thereof - Google Patents
Antimicrobial agent for quartz-carried nano silver phosphate ceramic and preparation method thereof Download PDFInfo
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- CN104488966A CN104488966A CN201410756792.5A CN201410756792A CN104488966A CN 104488966 A CN104488966 A CN 104488966A CN 201410756792 A CN201410756792 A CN 201410756792A CN 104488966 A CN104488966 A CN 104488966A
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Abstract
The invention discloses an antimicrobial agent for quartz-carried nano silver phosphate ceramic. The natural quartz mineral raw material, which is used as a carrier, carries 20-50nm silver phosphate particles, wherein the carrying amount of the silver phosphate particles is 0.03-0.1g/g. The invention also discloses a preparation method of the antimicrobial agent, which comprises the following steps: carrying out ball milling on the natural pure quartz mineral raw material, screening, drying, dispersing in a deionized water-ethanol mixed solution until the mass-volume solubility of the white powder is 1:25, adding an AgNO3 solution, magnetically stirring, adding a sodium phosphate solution, and continuing stirring to react for 1 hour; and sequentially cleaning with anhydrous ethanol and deionized water, drying, calcining and naturally cooling. The preparation method uses cheap and accessible raw materials, can implement industrial production, and is a green practical synthesis method. The preparation method has the advantages of no pollution, high synthesis efficiency and low energy consumption, and is simple to operate.
Description
Technical field
The invention belongs to ceramic technical field of function materials, be specifically related to a kind of quartzy loaded with nano silver orthophosphate pottery antibacterial agent, the invention still further relates to the preparation method of this antibacterial agent.
Background technology
Along with improving constantly of scientific and technological progress and living standards of the people, people improve living environment, improve life quality, to treasure healthy requirement growing, the development trend that development and production has the architectural pottery of antibacterial functions, domestic ceramics has become current ceramic industry.At present, be applied to ceramic antibacterial agent and be mostly based on silver orthophosphate, after mixing with glaze and burning till, make pottery have antibacterial functions.The preparation method of antibacterial agent is by liquor argenti nitratis ophthalmicus and sodium radio-phosphate,P-32 solution 3:1 hybrid reaction in molar ratio, generates silver orthophosphate precipitation.The prepared general particle of silver phosphate antibacterial agent is comparatively large, and mostly be micron order, reactivity is poor, and antibacterial effect is general, and can separate out elemental silver in ceramic glaze firing process, affects Ceramic glaze decoration.
Summary of the invention
The object of this invention is to provide a kind of quartzy loaded with nano silver orthophosphate pottery antibacterial agent, solve existing pottery silver phosphate antibacterial agent particle comparatively large, the problems such as reactivity is poor, and high-temperature stability is poor, improve the antibacterial effect of antibacterial agent.
Another object of the present invention is to provide a kind of preparation method of quartzy loaded with nano silver orthophosphate pottery antibacterial agent.
The technical solution adopted in the present invention is, a kind of quartzy loaded with nano silver orthophosphate pottery antibacterial agent, with natural quartz raw mineral materials carrier, supported on carriers has the silver orthophosphate particle of 20 ~ 50nm, and the load capacity of silver orthophosphate particle is 0.03 ~ 0.1g/g.
Another technical scheme of the present invention is, a kind of preparation method of quartzy loaded with nano silver orthophosphate pottery antibacterial agent, the quartzy loaded with nano silver orthophosphate pottery antibacterial agent prepared with natural quartz raw mineral materials for carrier, supported on carriers has the silver orthophosphate particle of 20 ~ 50nm, and the load capacity of silver orthophosphate particle is 0.03 ~ 0.1g/g;
Specifically implement according to following steps:
Step 1: natural pure quartz mineral raw material is joined ball milling in ball grinder and sieves, then puts into 150 DEG C of baking ovens by minus mesh slurry dry, obtains white powder for subsequent use;
Step 2: be scattered in the mixed solution of deionized water and ethanol by step 1 gained white powder, makes the quality of white powder-volume solubility be 1:25, adds the AgNO that concentration is 1g/100ml wherein
3solution magnetic agitation 12h; Then add phosphate sodium solution that concentration is 1g/100ml wherein and continue to stir, reaction 1h then; This solution centrifugal is also cleaned successively by absolute ethyl alcohol and deionized water, after drying, obtains yellow greenish powder;
Step 3: step 2 gained yellow greenish powder is placed in Muffle furnace in air atmosphere calcination processing, naturally cools to room temperature subsequently, can obtain quartzy loaded with nano silver orthophosphate pottery antibacterial powder.
Feature of the present invention is also,
In step 1, in ball grinder, the mass ratio of the material of ball milling, ball, water is 1:2.5:0.8.
In step 2, the volume ratio of deionized water and ethanol is 1:1 ~ 1:10.
AgNO in step 2
3the volume ratio of solution and white powder, water, alcohol mixed solution is 1:7 ~ 1:2.
Sodium ascorbyl phosphate and AgNO in step 2
3mol ratio be 1:3.
In step 2, sodium ascorbyl phosphate can be one or more in sodium phosphate, sodium hydrogen phosphate, sodium dihydrogen phosphate.
In step 3, light grass green powder calcination processing in Muffle furnace is incubated 2h after temperature is warming up to 500 DEG C with 1 DEG C/min.
The invention has the beneficial effects as follows, the present invention's quartz loaded with nano silver orthophosphate pottery antibacterial agent, improve the dispersiveness of silver orthophosphate pottery antibacterial agent, and the cheaper starting materials used is easy to get, can suitability for industrialized production, is the synthetic method of one " green " practicality.Have pollution-free, simple to operate, combined coefficient is high, the advantage that energy consumption is low.Has the condition of suitability for industrialized production.
Accompanying drawing explanation
Fig. 1 is the SEM figure of quartzy loaded with nano silver orthophosphate pottery antibacterial agent prepared by the embodiment of the present invention 3.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in detail.
A kind of quartzy loaded with nano silver orthophosphate pottery antibacterial agent, with natural quartz raw mineral materials carrier, supported on carriers has the silver orthophosphate particle of 20 ~ 50nm, and the load capacity of silver orthophosphate particle is 0.03 ~ 0.1g/g.
Another technical scheme of the present invention is, a kind of quartzy loaded with nano silver orthophosphate pottery preparation method of antibacterial pulvis, specifically implements according to following steps:
Step 1: natural pure quartz mineral raw material is joined ball milling in ball grinder with the mass ratio of material, ball, water for 1:2.5:0.8 and sieves, then puts into 150 DEG C of baking ovens by minus mesh slurry dry, obtains white powder for subsequent use;
Step 2: step 1 gained white powder is scattered in the mixed solution of deionized water and ethanol, the volume ratio of deionized water and ethanol is 1:1 ~ 1:10, make the quality of white powder-volume solubility be 1:25, add the AgNO that concentration is 1g/100ml wherein
3solution magnetic agitation 12h, AgNO
3the volume ratio of solution and white powder, water, alcohol mixed solution is 1:7 ~ 1:2.Then add phosphate sodium solution that concentration is 1g/100ml wherein and continue to stir, reaction 1h, sodium ascorbyl phosphate and AgNO then,
3mol ratio be 1:3.This solution centrifugal is also cleaned successively by absolute ethyl alcohol and deionized water, after drying, obtains yellow greenish powder.
Step 3: step 2 gained yellow greenish powder is placed in Muffle furnace in air atmosphere calcination processing, is incubated 2h after temperature is warming up to 500 DEG C with 1 DEG C/min, naturally cools to room temperature subsequently, can obtain quartzy loaded with nano silver orthophosphate pottery antibacterial agent.
Embodiment 1
By natural for 100g pure quartz mineral raw material, the ratio being 1:2.5:0.8 according to the mass ratio of material, ball, water joins ball milling 1h in ball grinder, crosses 80 order porous and sieves.Then minus mesh slurry is put into 150 DEG C of baking ovens dry, obtain white powder for subsequent use.Above-mentioned white powder being taken 2g is scattered in the mixed solution of 50ml deionization hydrate alcohol, and wherein the volume ratio of deionization hydrate alcohol is 1:1, adds the AgNO that 7.3ml concentration is 1g/100ml wherein
3solution magnetic agitation 12h.Then, then add sodium radio-phosphate,P-32 solution that 2.4ml concentration is 1g/100ml wherein and continue to stir, reaction 1h, this solution centrifugal being cleaned successively by absolute ethyl alcohol and deionized water, after drying, obtains yellow greenish powder.Gained yellow green powder is placed in Muffle furnace in air atmosphere calcination processing.Its temperature increasing schedule is 1 DEG C/min, in 500 DEG C of insulation 2h.Naturally cool to room temperature subsequently, quartzy loaded with nano silver orthophosphate pottery antibacterial agent can be obtained.
Embodiment 2
By natural for 100g pure quartz mineral raw material, the ratio being 1:2.5:0.8 according to the mass ratio of material, ball, water joins ball milling 1h in ball grinder, crosses 325 order porous and sieves.Then minus mesh slurry is put into 150 DEG C of baking ovens dry, obtain white powder for subsequent use.Above-mentioned white powder being taken 2g is scattered in the mixed solution of 50ml deionization hydrate alcohol, and wherein the volume ratio of deionization hydrate alcohol is 1:1, adds the AgNO that 24.4ml concentration is 1g/100ml wherein
3solution magnetic agitation 12h.Then, then add sodium radio-phosphate,P-32 solution that 7.8ml concentration is 1g/100ml wherein and continue to stir, reaction 1h, this solution centrifugal being cleaned successively by absolute ethyl alcohol and deionized water, after drying, obtains yellow greenish powder.Gained yellow green powder is placed in Muffle furnace in air atmosphere calcination processing.Its temperature increasing schedule is 1 DEG C/min, in 500 DEG C of insulation 2h.Naturally cool to room temperature subsequently, quartzy loaded with nano silver orthophosphate pottery antibacterial agent can be obtained.
Embodiment 3
By natural for 100g pure quartz mineral raw material, the ratio being 1:2.5:0.8 according to the mass ratio of material, ball, water joins ball milling 1h in ball grinder, crosses 160 order porous and sieves.Then minus mesh slurry is put into 150 DEG C of baking ovens dry, obtain white powder for subsequent use.Above-mentioned white powder being taken 2g is scattered in the mixed solution of 50ml deionization hydrate alcohol, and wherein the volume ratio of deionization hydrate alcohol is 1:5, adds the AgNO that 14.6ml concentration is 1g/100ml wherein
3solution magnetic agitation 12h.Then, then add sodium radio-phosphate,P-32 solution that 4.7ml concentration is 1g/100ml wherein and continue to stir, reaction 1h, this solution centrifugal being cleaned successively by absolute ethyl alcohol and deionized water, after drying, obtains yellow greenish powder.Gained yellow green powder is placed in Muffle furnace in air atmosphere calcination processing.Its temperature increasing schedule is 1 DEG C/min, in 500 DEG C of insulation 2h.Naturally cool to room temperature subsequently, quartzy loaded with nano silver orthophosphate pottery antibacterial agent can be obtained.
Embodiment 4
By natural for 100g pure quartz mineral raw material, the ratio being 1:2.5:0.8 according to the mass ratio of material, ball, water joins ball milling 1h in ball grinder, crosses 160 order porous and sieves.Then minus mesh slurry is put into 150 DEG C of baking ovens dry, obtain white powder for subsequent use.Above-mentioned white powder being taken 2g is scattered in the mixed solution of 50ml deionization hydrate alcohol, and wherein the volume ratio of deionization hydrate alcohol is 1:10, adds the AgNO that 14.6ml concentration is 1g/100ml wherein
3solution magnetic agitation 12h.Then, then add sodium radio-phosphate,P-32 solution that 4.7ml concentration is 1g/100ml wherein and continue to stir, reaction 1h, this solution centrifugal being cleaned successively by absolute ethyl alcohol and deionized water, after drying, obtains yellow greenish powder.Gained yellow green powder is placed in Muffle furnace in air atmosphere calcination processing.Its temperature increasing schedule is 1 DEG C/min, in 500 DEG C of insulation 2h.Naturally cool to room temperature subsequently, quartzy loaded with nano silver orthophosphate pottery antibacterial agent can be obtained.
Embodiment 5
By natural for 100g pure quartz mineral raw material, the ratio being 1:2.5:0.8 according to the mass ratio of material, ball, water joins ball milling 1h in ball grinder, crosses 160 order porous and sieves.Then minus mesh slurry is put into 150 DEG C of baking ovens dry, obtain white powder for subsequent use.Above-mentioned white powder being taken 2g is scattered in the mixed solution of 50ml deionization hydrate alcohol, and wherein the volume ratio of deionization hydrate alcohol is 1:5, adds the AgNO that 14.6ml concentration is 1g/100ml wherein
3solution magnetic agitation 12h.Then, then add sodium dihydrogen phosphate that 3.5ml concentration is 1g/100ml wherein and continue to stir, reaction 1h, this solution centrifugal being cleaned successively by absolute ethyl alcohol and deionized water, after drying, obtains yellow greenish powder.Gained yellow green powder is placed in Muffle furnace in air atmosphere calcination processing.Its temperature increasing schedule is 1 DEG C/min, in 500 DEG C of insulation 2h.Naturally cool to room temperature subsequently, quartzy loaded with nano silver orthophosphate pottery antibacterial agent can be obtained.
Embodiment 6
By natural for 100g pure quartz mineral raw material, the ratio being 1:2.5:0.8 according to the mass ratio of material, ball, water joins ball milling 1h in ball grinder, crosses 160 order porous and sieves.Then minus mesh slurry is put into 150 DEG C of baking ovens dry, obtain white powder for subsequent use.Above-mentioned white powder being taken 2g is scattered in the mixed solution of 50ml deionization hydrate alcohol, and wherein the volume ratio of deionization hydrate alcohol is 1:5, adds the AgNO that 14.6ml concentration is 1g/100ml wherein
3solution magnetic agitation 12h.Then, then add sodium dihydrogen phosphate that 4.1ml concentration is 1g/100ml wherein and continue to stir, reaction 1h, this solution centrifugal being cleaned successively by absolute ethyl alcohol and deionized water, after drying, obtains yellow greenish powder.Gained yellow green powder is placed in Muffle furnace in air atmosphere calcination processing.Its temperature increasing schedule is 1 DEG C/min, in 500 DEG C of insulation 2h.Naturally cool to room temperature subsequently, quartzy loaded with nano silver orthophosphate pottery antibacterial agent can be obtained.
Fig. 1 is the SEM figure of quartzy loaded with nano silver orthophosphate pottery antibacterial agent prepared by the embodiment of the present invention 3.As can be seen from Figure 1, antibacterial agent of the present invention is made up of quartz and nano silver particle, and silver orthophosphate particle size is 20-50nm, and it is evenly dispersed in Silica grain surface.So antibacterial agent of the present invention improves the dispersiveness of antibacterial substance silver orthophosphate, there is good antibacterial functions.
Claims (8)
1. a quartzy loaded with nano silver orthophosphate pottery antibacterial agent, with natural quartz raw mineral materials carrier, supported on carriers has the silver orthophosphate particle of 20 ~ 50nm, and the load capacity of silver orthophosphate particle is 0.03 ~ 0.1g/g.
2. the preparation method of a quartzy loaded with nano silver orthophosphate pottery antibacterial agent, it is characterized in that, the quartzy loaded with nano silver orthophosphate pottery antibacterial agent prepared with natural quartz raw mineral materials for carrier, supported on carriers has the silver orthophosphate particle of 20 ~ 50nm, and the load capacity of silver orthophosphate particle is 0.03 ~ 0.1g/g;
Specifically implement according to following steps:
Step 1: natural pure quartz mineral raw material is joined ball milling in ball grinder and sieves, then puts into 150 DEG C of baking ovens by minus mesh slurry dry, obtains white powder for subsequent use;
Step 2: be scattered in the mixed solution of deionized water and ethanol by step 1 gained white powder, makes the quality of white powder-volume solubility be 1:25, adds the AgNO that concentration is 1g/100ml wherein
3solution magnetic agitation 12h; Then add phosphate sodium solution that concentration is 1g/100ml wherein and continue to stir, reaction 1h then; This solution centrifugal is also cleaned successively by absolute ethyl alcohol and deionized water, after drying, obtains yellow greenish powder;
Step 3: step 2 gained yellow greenish powder is placed in Muffle furnace in air atmosphere calcination processing, naturally cools to room temperature subsequently, can obtain quartzy loaded with nano silver orthophosphate pottery antibacterial powder.
3. the preparation method of quartzy loaded with nano silver orthophosphate pottery antibacterial agent according to claim 2, is characterized in that, in step 1, in ball grinder, the mass ratio of the material of ball milling, ball, water is 1:2.5:0.8.
4. the preparation method of quartzy loaded with nano silver orthophosphate pottery antibacterial agent according to claim 2, it is characterized in that, in step 2, the volume ratio of deionized water and ethanol is 1:1 ~ 1:10.
5. the preparation method of the quartzy loaded with nano silver orthophosphate pottery antibacterial agent according to claim 2 or 4, is characterized in that, AgNO in step 2
3the volume ratio of solution and white powder, water, alcohol mixed solution is 1:7 ~ 1:2.
6. the preparation method of the quartzy loaded with nano silver orthophosphate pottery antibacterial agent according to claim 2 or 4, is characterized in that, sodium ascorbyl phosphate and AgNO in step 2
3mol ratio be 1:3.
7. the preparation method of the quartzy loaded with nano silver orthophosphate pottery antibacterial agent according to claim 2 or 4, is characterized in that, the sodium ascorbyl phosphate in step 2 can be one or more in sodium phosphate, sodium hydrogen phosphate, sodium dihydrogen phosphate.
8. the preparation method of quartzy loaded with nano silver orthophosphate pottery antibacterial agent according to claim 2, is characterized in that, in step 3, yellow greenish powder calcination processing in Muffle furnace is incubated 2h after temperature is warming up to 500 DEG C with 1 DEG C/min.
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| CN113070082A (en) * | 2021-03-31 | 2021-07-06 | 陕西科技大学 | Bismuth vanadate @ silver phosphate/graphene oxide composite photocatalyst and preparation method and application thereof |
| CN114018913A (en) * | 2021-11-09 | 2022-02-08 | 河南省奥瑞环保科技股份有限公司 | Rapid gas detection tube carrier pretreatment method |
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