CN104591779A - Nano-silver-particle-embedded porous ceramic sheet as well as preparation method and application thereof - Google Patents
Nano-silver-particle-embedded porous ceramic sheet as well as preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a nano-silver-particle-embedded porous ceramic sheet as well as a preparation method and an application thereof. The preparation method comprises the following steps of mixing sawdust and clay with mass percentage of 11-13% into a silver nitrate solution to obtain a mixture, firstly carrying out ultrasonic dispersion on the mixture for 1-2 hours, uniformly stirring, fixing the mixed system to a wafer, carrying out air-drying for 70-80 hours at room temperature, placing the wafer in a kiln, heating the wafer at a heating speed of 2.5 DEG C/min to 600 +/- 20 DEG C and at a heating speed of 5 DEG C/min to 900 +/- 20 DEG C and carrying out heat preservation for 3-4 hours. The nano-silver-particle-embedded porous ceramic sheet prepared by the preparation method has the advantages of larger surface area, good firmness with nano silver particles, the material has good and stable bacteria-killing capability, the removal rate of microorganisms in water can reach above 99% and the ceramic sheet can be used as an alternative technology and method of family water purification.
Description
Technical field
The present invention relates to Drinking Water Sanitization Technology and ceramic water-purification technical field, be specifically related to a kind of porous ceramics piece embedding nano-Ag particles and preparation method thereof and application.
Background technology
Tap water problem becomes global concern, and according to statistics, unsafe tap water disease relevant with water pollutions is died from per year over 1800000 people in the whole world, and about 7.8 hundred million people's drinking waters lack clean water source.The World Health Organization (WHO) suggestion adopts suitable on-site treatment method can effectively solve household drinking water problem.There are some researches show that family's drinking-water treatment in situ can improve drinking water safety effectively, compared to waterhead area process, but this depends on user's compliance.Therefore, practicality, the property born and stability become the key factor of exploitation treatment in situ technology.
Traditional treatment in situ technology has the technology such as membrane filtration, high-temperature sterilization and sunlight sterilization, but owing to there are some uncertain factors, makes its technology lack practicality.In addition, due to environmental health problem, these treatment technologies all easily produce secondary pollution.Therefore, the treatment in situ technology (material) effectively can remove pathogenic bacterium in water, meet that user requires, process is steady in a long-term, reduce secondary pollution, being convenient to transport and use becomes the focus of current concern.
Argent sterilization is considered to a kind of effective tap water treatment in situ technology and method, effectively can kill the bacterium in water, virus and protozoon, and the good colourity of water quality and smell can be kept, compared to the chemostefilant such as chlorine and iodine, some researchs show that argent disinfection technology can kill the bacterium in dewatering, and show good persistence.But, in some developing countries and regions, the consumption of metallic Silver material and its widespread use of restriction of production.In addition, argent nano particle is directly used in water sterilization, easily to generation secondary pollution, there is toxicity to organism, and uneconomical applicable.Therefore, a kind of carrier of fixing nano-Ag particles must be sought, maintain it and play its efficiency steadily in the long term.
Porous ceramics water filter can be used as the carrier of nanometer silver, and its peculiar larger specific surface area ensures silver-colored dispersity, and silver fully contacts with disease caused by infectious water pathogenic microorganism, and then can ensure decontamination effect improving.Silver-colored load on carrier, if simply elemental silver and carrier mixing, usually can not closely combine between the two.In patent disclosed at present, the process of nano-silver loaded pottery is that polystep reaction is formed, the method such as chemical reducing agent or uv irradiating that particularly applies is by silver ion reduction, such as patent " a kind of preparation method of porous diatomite-based AgO ceramic material ", publication number is CN102060561A, patent " method of Diatomite-based Porous Ceramics and loading Ag doped with nano TiO 2 thereof ", publication number is CN101891497A, and patent " a kind of silver-colored modified porous ceramic membrane and preparation method thereof and application ", publication number is CN104084055A.These methods or process easily cause secondary pollution, anionic current is become estranged nanometer silver is insecure etc., affects starting material utilising efficiency and water-purifying material functional efficiency.
Summary of the invention
Technical problem to be solved by this invention is to provide the porous ceramics piece of a kind of flexible and convenient operation, the embedding nano-Ag particles that with low cost, processing drinking water is effective.
The technical problem that the present invention also will solve is to provide the preparation method of above-mentioned porous ceramics piece.
The technical problem that the present invention finally will solve is to provide the application of above-mentioned porous ceramics piece in drink water purifying is degerming.
For solving the problems of the technologies described above, the technical solution used in the present invention is as follows:
A kind of preparation method embedding the porous ceramics piece of nano-Ag particles, it is characterized in that, to join in silver nitrate aqueous solution after wood chip and clay 11 ~ 13% mixing by mass percentage, mixture is first with ultrasonic wave dispersion 1 ~ 2h, stir again, mixed system is fixed into disk, and air-dry 70 ~ 80h (preferred 72h) at normal temperatures, then this disk is placed in kiln and is warming up to 600 ± 20 DEG C with 2.5 DEG C/min, 900 ± 20 DEG C are warming up to again with 5 DEG C/min, then be incubated 3 ~ 4h (preferred 3h), obtain final product.
Wherein, described clay is purchased from Sigma-Aldrich, and its main component is kaolinite and Yi Laishi, and its size distribution situation is:
The particle of <2 μm accounts for 25-30wt%;
The particle of 2 ~ 20 μm accounts for 55-60wt%;
The particle of >20 μm accounts for and about respectively accounts for 10-20wt%.
Preferred size distribution situation is:
The particle of <2 μm accounts for 28wt%;
The particle of 2 ~ 20 μm accounts for 56wt%;
The particle of >20 μm accounts for and about respectively accounts for 16wt%.
Wherein, described wood chip was 20 mesh sieve gained.
Wherein, in mixed system, in mixed system, the ratio of the weight of Silver Nitrate and clay and wood chip gross weight is 1 ~ 5:62 ~ 63.
Wherein, use hand-operated hydraulic press that mixed system is fixed into disk, needed for fixing single disk, the quality of mixed system is 82.7 ~ 86.7g, and the diameter of the disk of formation is 60 ~ 90mm, and thickness is 20 ~ 40mm.。
The physico-chemical property of the porous ceramics piece of above-mentioned embedding nano-Ag particles can pass through the mixing quality ratio and the Silver Nitrate dosage that change clay and wood chip, and forming materials realizes.Such as, add by changing the content that Silver Nitrate amount changes silver in water-purifying material; By changing the mixing quality ratio of clay and wood chip, thus the porosity of water-purifying material can be changed; In forming materials process, change disk size, realize porosity and the specific surface area of material itself.
The porous ceramics piece of the embedding nano-Ag particles that above-mentioned preparation method prepares is also within protection scope of the present invention.
The application in direct drinking water purification is degerming of the porous ceramics piece of above-mentioned embedding nano-Ag particles is also within protection scope of the present invention.The porous ceramics piece embedding nano-Ag particles is placed in water, porous ceramics piece plays the effect of bactericidal purifying to water, the elemental silver of load on ceramic membrane and release silver ions directly kill the microorganism in water, be purified degerming after direct-drinking water, and the concentration of silver ions of release is lower than the relevant criterion of World Health Organization's defined.
Beneficial effect: the present invention and current material, compared with technology, have the following advantages:
How empty ceramic water-purification material prepared by the present invention draw materials convenient and simple, preparation process is easy to operate, be easy to carry, and without any need for chemical agent in nano-Ag particles generative process, only to be formed by clay-wood chip mixture roasting process.Meanwhile, the specific surface area that how empty the stupalith of preparation be concrete larger, impel the nano-Ag particles on mesoporous top layer fully to contact with disease caused by infectious water pathogenic microorganism, the nano-Ag particles particle diameter of formation is about 2.5nm, and difficult drop-off; The silver of nano-scale can significantly improve the purification bacteria-eliminating efficacy of silver.The silver ions that porous ceramics scavenging material discharges maintains low concentration (< 0.35mg/L) for a long time, meets the relevant drinking water standard of World Health Organization's defined.Ensureing effectively kills except while the bacterium in tap water, can saving silver consumption, the also stability of guarantee porous ceramics scavenging material.
Accompanying drawing explanation
Fig. 1 is water-purifying material transmission electron microscope picture (TEM) and the energy spectrometer figure (EDS) of embodiment 1 preparation.Wherein, A ceramic plate central interior, B ceramic topcoats, C are water-purifying material energy spectrometer figure (EDS).
Fig. 2 is embodiment 1 sterilization experiment design sketch, and wherein A is material sterilization effect trend map, and B is the concentration of silver ions that material discharges in sterilization process.
Fig. 3 be three kinds of scavenging materials to colibacillary test result, wherein A is material sterilization effect trend map, and B is the concentration of silver ions that material discharges in sterilization process.
Embodiment
According to following embodiment, the present invention may be better understood.But those skilled in the art will readily understand, the content described by embodiment only for illustration of the present invention, and should can not limit the present invention described in detail in claims yet.
Embodiment 1:
Prepared by porous ceramics water-purifying material: with its mixture 62.5g with the ratio of mixture 9:1 of clay and wood chip, used clay is characterized as: clay is purchased from Sigma-Aldrich, its main component is kaolinite and Yi Laishi, and the size distribution situation of clay is < 2 μm, 2-20 μm, the particle of > 20 μm about respectively accounts for 28wt%, 56wt%, 16wt%; In addition, wood chip was that 20 mesh sieves obtained.Clay and wood chip mixture are joined in the concentration 1.3mol/L silver nitrate solution of 19.2ml, mixture first disperses 1-2h by ultrasonic wave, stir again, with hand-operated hydraulic press, mixture is fixedly become the disk of diameter 80mm and thickness 30mm, and air-dry 72 hours at normal temperatures.Then this disk is placed in kiln and is warming up to 600 DEG C with 2.5 DEG C/min, then be warming up to 900 DEG C with 5 DEG C/min, be then incubated 3h, obtained material 1.
By the step and method of above-mentioned preparation, just change concentration 1.3mol/L silver nitrate solution into do not add Silver Nitrate deionized water, prepare the porous ceramic film material (material 2) not having silver.
The nanometer silver porous ceramics water-purifying material (material 1) of above-mentioned preparation, porous ceramic film material (material 2) and nano-Ag particles are used for sterilization test, wherein nano-Ag particles is the medicine bought, and size is 20 ~ 40nm; In sterilization test, the nano-Ag particles added is consistent with silver content in nanometer silver porous ceramics water-purifying material.The phenogram of nanometer silver porous ceramics water-purifying material (material 1) is shown in Fig. 1 and Fig. 2.
Sterilization is tested: above-mentioned preparation two kinds of porous ceramics water-purifying materials and 2.7g nano-Ag particles are used for killing the middle intestinal bacteria that dewater.Be added to respectively by above-mentioned materials and fill in the colibacillary phosphate buffer soln of 200mL, wherein phosphate buffered agent concentration is 10mmol/L, and e. coli concentration is 10
7cfu/L.The colibacillary phosphoric acid salt mixed solution not adding any reagent and medicine is designated as blank.Sample respectively according to the time of setting, measure coliform count and concentration of silver ions, dependence test the results are shown in Figure 3.Result shows: nanometer silver porous ceramics water-purifying material shows good sterilization effect, and compared to nano-Ag particles, nanometer silver porous ceramics water-purifying material sterilizing ability is suitable with it, and the silver ions of release is less, can maintain the stability of its performance.
Embodiment 2:
Substantially the same manner as Example 1, difference is: the quality adding the Silver Nitrate of mixture is 1g, and the material prepared is designated as material 3.
Substantially the same manner as Example 1, difference is: the disk with hand-operated hydraulic press, mixture fixedly being become diameter 80mm and thickness 20mm, and the material prepared is designated as material 4.
Sterilization is tested: by above-mentioned preparation three kinds of porous ceramics water-purifying materials (material 1, material 3 and material 4) for killing the middle intestinal bacteria that dewater.Being added to respectively by three different porous ceramics water-purifying materials fills in the colibacillary phosphate buffer soln of 200mL, and wherein phosphate buffered agent concentration is 10mmol/L, and e. coli concentration is 10
7cfu/L.Sample respectively according to the time of setting, measure coliform count and concentration of silver ions, dependence test the results are shown in Figure 3.Result shows: in material, the content of silver and the porosity of material have impact on the sterilizing ability of material, and porosity is higher, add the contact area of silver and bacterium; Therefore by changing dosage and the forming materials size of silver, the performance of its sterilization can be changed.
The above is only the preferred embodiment of the present invention; be noted that for those skilled in the art; under the premise without departing from the principles of the invention, can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (8)
1. one kind embeds the preparation method of the porous ceramics piece of nano-Ag particles, it is characterized in that, to join in silver nitrate aqueous solution after wood chip and clay 11 ~ 13% mixing by mass percentage, mixture first with ultrasonic wave dispersion 1 ~ 2h, then stirs, mixed system is fixed into disk, and air-dry 70 ~ 80h at normal temperatures, then this disk is placed in kiln and is warming up to 600 ± 20 DEG C with 2.5 DEG C/min, then be warming up to 900 ± 20 DEG C with 5 DEG C/min, then be incubated 3 ~ 4h, obtain final product.
2. preparation method according to claim 1, is characterized in that, described clay, and its main component is kaolinite and Yi Laishi, and its size distribution situation is:
The particle of <2 μm accounts for 25-30wt%;
The particle of 2 ~ 20 μm accounts for 55-60wt%;
The particle of >20 μm accounts for and about respectively accounts for 10-20wt%.
3. preparation method according to claim 1, is characterized in that, described wood chip, is 20 mesh sieve gained.
4. preparation method according to claim 1, is characterized in that, in mixed system, the ratio of the weight of Silver Nitrate and clay and wood chip gross weight is 1 ~ 5:62 ~ 63.
5. preparation method according to claim 1, is characterized in that, uses hand-operated hydraulic press that mixed system is fixed into disk.
6. preparation method according to claim 1, is characterized in that, needed for fixing single disk, the quality of mixed system is 82.7 ~ 86.7g, and the disk diameter of formation is 60 ~ 90mm, and thickness is 20 ~ 40mm.
7. the porous ceramics piece of the embedding nano-Ag particles that the preparation method in claim 1 ~ 6 described in any one prepares.
8. the application of porous ceramics piece in direct drinking water purification is degerming of embedding nano-Ag particles according to claim 7.
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Cited By (6)
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| CN104996464A (en) * | 2015-07-24 | 2015-10-28 | 中山市瑞佳厨房电器有限公司 | Preparing method of nano-silver sheet for sterilization of water and nano-silver sheet |
| CN107043242A (en) * | 2017-02-28 | 2017-08-15 | 沈阳理工大学 | One kind prepares porous ceramic composite and foam solution method using sludge and cow dung |
| CN108002861A (en) * | 2018-01-11 | 2018-05-08 | 厦门理工学院 | A kind of degerming water purification clay filtering material and its preparation method and application |
| CN108178612A (en) * | 2018-01-19 | 2018-06-19 | 大田县源生竹业有限公司 | A kind of preparation process of the antibacterial bamboo charcoal ceramic tile of damping |
| CN111116168A (en) * | 2018-11-01 | 2020-05-08 | 王双彬 | Mesoporous clay filter material and preparation method thereof |
| CN112357984A (en) * | 2020-10-26 | 2021-02-12 | 杭州电子科技大学 | Silver-doped clay particle, preparation method thereof and biological sand filtering system |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104996464A (en) * | 2015-07-24 | 2015-10-28 | 中山市瑞佳厨房电器有限公司 | Preparing method of nano-silver sheet for sterilization of water and nano-silver sheet |
| CN107043242A (en) * | 2017-02-28 | 2017-08-15 | 沈阳理工大学 | One kind prepares porous ceramic composite and foam solution method using sludge and cow dung |
| CN107043242B (en) * | 2017-02-28 | 2021-03-16 | 沈阳理工大学 | Method for preparing porous ceramic composite material and foam liquid by using sludge and cow dung |
| CN108002861A (en) * | 2018-01-11 | 2018-05-08 | 厦门理工学院 | A kind of degerming water purification clay filtering material and its preparation method and application |
| CN108178612A (en) * | 2018-01-19 | 2018-06-19 | 大田县源生竹业有限公司 | A kind of preparation process of the antibacterial bamboo charcoal ceramic tile of damping |
| CN111116168A (en) * | 2018-11-01 | 2020-05-08 | 王双彬 | Mesoporous clay filter material and preparation method thereof |
| CN112357984A (en) * | 2020-10-26 | 2021-02-12 | 杭州电子科技大学 | Silver-doped clay particle, preparation method thereof and biological sand filtering system |
| CN112357984B (en) * | 2020-10-26 | 2023-09-01 | 杭州电子科技大学 | Silver-doped clay particles, preparation method thereof and biological sand filtering system |
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Application publication date: 20150506 |