CN108585474A - A kind of preparation method of anti-bacteria ceramic glaze filling nano-calcium carbonate - Google Patents
A kind of preparation method of anti-bacteria ceramic glaze filling nano-calcium carbonate Download PDFInfo
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- CN108585474A CN108585474A CN201810572605.6A CN201810572605A CN108585474A CN 108585474 A CN108585474 A CN 108585474A CN 201810572605 A CN201810572605 A CN 201810572605A CN 108585474 A CN108585474 A CN 108585474A
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
- C03C1/02—Pretreated ingredients
- C03C1/026—Pelletisation or prereacting of powdered raw materials
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2204/00—Glasses, glazes or enamels with special properties
- C03C2204/02—Antibacterial glass, glaze or enamel
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Abstract
The invention discloses a kind of preparation methods of anti-bacteria ceramic glaze filling nano-calcium carbonate：A, it is slowly stirred down, it is passed through kiln gas into the calcium hydroxide slurry after ageing and carries out carburizing reagent, until the pH value of reaction system is reduced to 9.0 8.0, then particular surface inorganic agent complex is added into reaction system, the reaction was continued under fast stirring is down to 6.5 7.0 to the pH value of reaction system, stops reaction；B, sodium molybdate and zinc nitrate are added into the slurry system obtained by step A, continues stirring to the complete mixing of system, then gained nano-calcium carbonate slurry is dehydrated, is dried, is crushed, dispense to get.Thus obtained nano-calcium carbonate calcium product has good antibacterial and uvioresistant, antioxygenic property and higher fatigue strength, to overcome the disadvantage that existing anti-bacteria ceramic glaze product uvioresistant is poor, antioxygenic property is poor, anti-microbial property is undesirable at present.
Description
Technical field
The present invention relates to the nano-calcium carbonate of field of material technology and its preparation method more particularly to a kind of anti-bacteria ceramics
Glaze filling nano-calcium carbonate and preparation method thereof.
Background technology
Calcium carbonate is a kind of important inorganic material, since price is low, raw material is wide, non-toxic and be widely used in making pottery
The fields such as porcelain, papermaking, ceramic glaze.Calcium carbonate product is increasingly sent out to the direction of fining, specialization, functionalization in recent years
Exhibition, nano-calcium carbonate is a kind of new type functional material to grow up the 1980s, is filled in ceramics and ceramic glaze
In, the properties of raising ceramics and ceramic glaze that can be fabulous improve the smoothness of glaze.Promote the drying of glaze but is easy production
Raw the shortcomings that being generated because of degassing, the coefficient of expansion and viscosity can be increased.But it there is that inoxidizability is poor, fatigue strength is lower
Disadvantage.
A kind of system of the white activated Calcium carbonate of the ceramics applied to water paint is disclosed in Chinese patent CN 106366697A
Preparation Method belongs to mineral processing and nonmetallic mineral material field.Including following technique, tcrude ore is cleaned, air-dried, is broken
Broken, grinding, finished product are collected, are packed, and the ore for being crushed to 25mm or less grain sizes is added to after evenly mixing with composite modifier
Grinding in grinder, in process of lapping, grader sorts fine powder, by dust-precipitator by fineness in 800-3000 purposes
Product collects, and coarse powder, which returns again to grinder, to be continued to grind；Composite modifier includes that mass percent is 0.4%-2%
The fluorescent whitening agent of 5040 type dispersants, 0.03%-0.2%.
A kind of resistance to oxidation pearl filler is disclosed in Chinese patent CN 104292707A, by the raw material of following parts by weight
It is made：Ammonium polyphosphate 1-2, ASA1-2, cyclohexanone 1-2, epoxidized soybean oil 0.4-0.8, zinc ricinate 0.8-1.1, maleic acid
Dimethyl ester 1.5-1.8, bimaleimide resin 1.5-1.8, lauric acid polyoxyethylene ester 0.1-0.2, dibutyl hydroxy toluene
2.6-2.9, ethyl alcohol 3-5, modified wood powder 20-30, precipitated calcium carbonate 180-200, water 60-80；Filler of the present invention has excellent
Oxidation resistent susceptibility is capable of the resistance to oxidation and weather resistance of reinforced plastics.
It is disclosed in Chinese patent CN 107524032A a kind of using modified calcium carbonate as the paper preparation side of filler
Method includes the following steps：(1) paper pulp raw material is put into after impregnating 1.5~3h in 90~95 DEG C of water, coupling agent is added and is kowtowed
Solution；(2) precipitated calcium carbonate is configured to a concentration of 40~55% calcium carbonate suspension；(3) cationic starch is configured to dense
Degree is the starch suspension of 50-65%, is then gelatinized 20~30min；(4) the starch solution pH value after gelatinization is adjusted to 8~10,
A concentration of 10~15% sodium stearate solution is added, forms compound；(5) compound is added to calcium carbonate suspension, and
Dispersant is added, obtains sediment, 40~50min is mixed in sediment at 75~85 DEG C, 250~300r/min.It adopts
The intensity of paper can be improved with the method for the present invention, increases paper smoothness, improve paper printing characteristic.
A kind of coating modified calcium carbonate and its system that dispersed effect is good is disclosed in Chinese patent CN 107446386A
Preparation Method, the coating modified calcium carbonate, including following raw material：Calcium carbonate, fatty alcohol polyoxyethylene ether ammonium sulfate, peroxidating
Lauroyl, trimethylolpropane tris (3- aziridinyls propionic ester), stannous chloride, vanadic anhydride, diethylenetriamine pentacarboxylic acid
Potassium, conditioning agent, diisooctyl phthalate, hexenyl bis-stearamides, 2- (bis- tertiary phenyl of 2'- hydroxyls -3', 5'-) -5- chlorine
Change benzotriazole, N- ethyl -5- methyl -2- (1- Methylethyls) hexamethylene formamide, stabilizer, the coating modified calcium carbonate
It is by made of surface modification, property regulation, crushing, drying and other steps.The activation rate of modified calcium carbonate of the invention is high,
The low and compatibility with high molecular polymer of oil factor is good.
In the known prior art and the above-mentioned several patents about nanon calcium carbonatefilled in high molecular material,
It is not directed to be filled in the relevant technologies of anti-bacteria ceramic glaze material.
Invention content
The technical problem to be solved in the present invention is to provide a kind of preparation sides of anti-bacteria ceramic glaze filling nano-calcium carbonate
Method, thus obtained nano-calcium carbonate calcium product have good antibacterial and antioxygenic property and higher fatigue strength, with gram
The clothes disadvantage that existing anti-bacteria ceramic glaze product antioxygenic property is poor at present, anti-microbial property is undesirable.
In order to solve the above technical problems, the technical solution used in the present invention is as follows.
A kind of preparation method of anti-bacteria ceramic glaze filling nano-calcium carbonate, this method comprises the following steps：
A, it is slowly stirred down, kiln gas is passed through into the calcium hydroxide slurry after ageing and carries out carburizing reagent, until reaction system
PH value is reduced to 9.0-8.0, particular surface inorganic agent complex is then added into reaction system, the reaction was continued under fast stirring
PH value to reaction system is down to 6.5-7.0, stops reaction；
B, sodium molybdate and zinc nitrate are added into the slurry system obtained by step A, continues stirring to the complete mixing of system, then will
Gained nano-calcium carbonate slurry is dehydrated, is dried, is crushed, is dispensed, and anti-bacteria ceramic glaze filling nano-calcium carbonate is obtained.
As a preferred technical solution of the present invention, in step A, the particular surface inorganic agent complex is using poly-
Ethylene glycol-calgon complex.
As a preferred technical solution of the present invention, in step A, the polyethylene glycol-calgon surface treatment
The volume ratio of polyethylene glycol and calgon is in agent complex（2-20）:（60-120）；Also, according to weight part ratio meter
It calculates, the ratio between the total weight of calcium carbonate in the total weight and system of the polyethylene glycol-calgon surface conditioning agent complex
For（1-15）:100.
As a preferred technical solution of the present invention, in step A, the polyethylene glycol-calgon surface treatment
The volume ratio of polyethylene glycol and calgon is in agent complex（4-16）:（80-100）；Also, according to weight part ratio meter
It calculates, the ratio between the total weight of calcium carbonate in the total weight and system of the polyethylene glycol-calgon surface conditioning agent complex
For（1-10）:100.
As a preferred technical solution of the present invention, in step A, the polyethylene glycol-calgon surface treatment
The volume ratio of polyethylene glycol and calgon is in agent complex（5-10）:（90-95）；Also, according to weight part ratio meter
It calculates, the ratio between the total weight of calcium carbonate in the total weight and system of the polyethylene glycol-calgon surface conditioning agent complex
For（2-5）:100.
As a preferred technical solution of the present invention, in step A, the digestion time of the calcium hydroxide slurry is 7-
10h。
As a preferred technical solution of the present invention, in step B, the dosage weight ratio of the sodium molybdate and zinc nitrate is
1:（0.5-5）；Also, it is calculated according to weight part ratio, calcium carbonate in the total weight and system of the sodium molybdate and zinc nitrate
The ratio between total weight is（5-8）:100.
As a preferred technical solution of the present invention, in step B, the dosage weight ratio of the sodium molybdate and zinc nitrate is
1:（1-3）；Also, it is calculated according to weight part ratio, calcium carbonate is total in the total weight and system of the sodium molybdate and zinc nitrate
Weight ratio is（6-7）:100.
As a preferred technical solution of the present invention, in step B, continue to be stirred to react after sodium molybdate and zinc nitrate is added
1h-3h。
It is using advantageous effect caused by above-mentioned technical proposal：
The present invention is added by the improvement to preparation method by adding specific surface conditioning agent complex and specific reaction
Material so that prepared nano-calcium carbonate calcium product has good antibacterial and antioxygenic property and higher fatigue strength, energy
It is enough effectively to overcome the shortcomings of existing anti-bacteria ceramic glaze product antioxygenic property is poor, anti-microbial property is undesirable at present, have
Extremely good practical value.
In performance indicator, anti-bacteria ceramic glaze filling nano-calcium carbonate prepared by the present invention has following advantages：
1. the nano-calcium carbonate product cut size being prepared is 80-100nm, whiteness reaches 90 or more, and soilless sticking phenomenon；2. the present invention
Nano-calcium carbonate made from method, due to the activation process by surfactant, on the basis of good anti-microbial property, especially
It shows excellent antioxygenic property, this be existing antibacterial glaze filling calcium carbonate it is incomparable.
With the first patent of inventor《Polyethersulfone resin the filling anti-oxidant nano-calcium carbonate of toughening uvioresistant and its system
Preparation Method and purposes》201710009309.0 comparing, the outstanding advantage of this patent is：1. at the composite surface that the present invention uses
Manage agent compared with the surface conditioning agent of first patent, it is advantageous that polar oligomer can orient be adsorbed on nano-calcium carbonate
Surface, make it have charge characteristic and form adsorption layer, prevent agglomeration, to significantly improve its dispersibility；②
The use of sodium molybdate and zinc nitrate in the present invention makes product surface generate zinc molybdate clad, uses as filler and is applied in ceramics
There is good anti-microbial property when material.
Specific implementation mode
The present invention is described in detail in following embodiment.Various raw materials used in the present invention and items of equipment are conventional city
Product is sold, can be bought and be directly obtained by market.
Embodiment 1
The preparation process of nano-calcium carbonate includes in the present embodiment：
A, under slow stirring, it is passed through kiln gas into the calcium hydroxide slurry after ageing 8h and carries out carburizing reagent, control reactant
The pH value of system is 8.0, and surface conditioning agent polyethylene glycol-calgon is added（v：v=5：95）, under fast stirring, continue anti-
It should be down to 6.8 to the pH value of reaction system, stop reaction, obtain nano-calcium carbonate slurry；
B, sodium molybdate and zinc nitrate is added, continues to stir 1h, nano-calcium carbonate slurry is dehydrated, dry, crush, is dispensed,
Obtain anti-bacteria ceramic glaze filling nano-calcium carbonate.
Embodiment 2
The preparation process of nano-calcium carbonate includes in the present embodiment：
A, under slow stirring, it is passed through kiln gas into the calcium hydroxide slurry after ageing 8h and carries out carburizing reagent, control reactant
The pH value of system is 8.0, and the surface conditioning agent polyethylene glycol-hexa metaphosphoric acid for the total weight 4% for being equivalent to calcium carbonate in system is added
Sodium（v：v=8：92）, under fast stirring, the reaction was continued is down to 6.8 to the pH value of reaction system, stops reaction, obtains nano-calcium carbonate
Calcium slurry.
B, sodium molybdate and zinc nitrate is added（w：w=1：2）, continue to stir 1h, nano-calcium carbonate slurry be dehydrated, is done
Dry, crushing, packing, obtain anti-bacteria ceramic glaze filling nano-calcium carbonate.
Embodiment 3
The preparation process of nano-calcium carbonate includes in the present embodiment：
A, under slow stirring, it is passed through kiln gas into the calcium hydroxide slurry after ageing 8h and carries out carburizing reagent, control reactant
The pH value of system is 8.0, and the surface conditioning agent polyethylene glycol-hexa metaphosphoric acid for the total weight 3% for being equivalent to calcium carbonate in system is added
Sodium（v：v=5：95）, under fast stirring, the reaction was continued is down to 6.8 to the pH value of reaction system, stops reaction, obtains nano-calcium carbonate
Calcium slurry；
B, sodium molybdate and zinc nitrate is added（w：w=1：2）, continue to stir 2h, nano-calcium carbonate slurry be dehydrated, is dried, powder
Broken, packing, obtains anti-bacteria ceramic glaze filling nano-calcium carbonate.
Embodiment 4
The preparation process of nano-calcium carbonate includes in the present embodiment：
A, under slow stirring, it is passed through kiln gas into the calcium hydroxide slurry after ageing 8h and carries out carburizing reagent, control reactant
The pH value of system is 9.0, and the surface conditioning agent polyethylene glycol-hexa metaphosphoric acid for the total weight 3% for being equivalent to calcium carbonate in system is added
Sodium（v：v=5：95）, under fast stirring, the reaction was continued is down to 7.0 to the pH value of reaction system, stops reaction, obtains nano-calcium carbonate
Calcium slurry；
B, sodium molybdate and zinc nitrate is added（w：w=1：2）, continue to stir 2h, nano-calcium carbonate slurry be dehydrated, is dried, powder
Broken, packing, obtains anti-bacteria ceramic glaze filling nano-calcium carbonate.
Embodiment 5
The preparation process of nano-calcium carbonate includes in the present embodiment：
A, under slow stirring, it is passed through kiln gas into the calcium hydroxide slurry after ageing 10h and carries out carburizing reagent, control reactant
The pH value of system is 9.0, and the surface conditioning agent polyethylene glycol-hexa metaphosphoric acid for the total weight 3% for being equivalent to calcium carbonate in system is added
Sodium（v：v=10：90）, under fast stirring, the reaction was continued is down to 6.8 to the pH value of reaction system, stops reaction, obtains nano-sized carbon
Sour calcium slurry；
B, sodium molybdate and zinc nitrate is added（w：w=1：2）, continue to stir 2h, nano-calcium carbonate slurry be dehydrated, is dried, powder
Broken, packing, obtains anti-bacteria ceramic glaze filling nano-calcium carbonate.
Embodiment 6
The preparation process of nano-calcium carbonate includes in the present embodiment：
A, under slow stirring, it is passed through kiln gas into the calcium hydroxide slurry after ageing 7h and carries out carburizing reagent, control reactant
The pH value of system is 8.5, and the surface conditioning agent polyethylene glycol-hexa metaphosphoric acid for the total weight 4% for being equivalent to calcium carbonate in system is added
Sodium（v：v=10：90）, under fast stirring, the reaction was continued is down to 7.2 to the pH value of reaction system, stops reaction, obtains nano-sized carbon
Sour calcium slurry；
B, sodium molybdate and zinc nitrate is added（w：w=1：2）, continue to stir 3h, nano-calcium carbonate slurry be dehydrated, is dried, powder
Broken, packing, obtains anti-bacteria ceramic glaze filling nano-calcium carbonate.
Embodiment 7, Anti-microbial Performance Tests
Anti-microbial property detection investigates the anti-of sample 6-24h with reference to People's Republic of China (PRC) building material industry standard JC/T897-2014
Bacterium rate, total plate count carry out count plate according to the method for GB4789.2.Each embodiment and comparative example are subjected to antibiotic property respectively
It can test, the calculation formula of antibacterium rate is：R=(B-C)/B*100%, wherein R is antibacterium rate, and B is blank control sample culture
The numerical value of average colony count after for 24 hours, unit is clump count（CFU）, C is average colony meter after anti-bacteria ceramic sample culture for 24 hours
Several numerical value, unit are clump count（CFU）, anti-microbial property test result such as following table：
Meanwhile in order to investigate the antibacterial effect after long term wear, the ceramic model for adding anti-bacteria ceramic glaze is subjected to simulation mill
Damage is tested, and still tests antibacterial effect according to the method described above after wear testing, test result is as follows for sterilization rate：
Embodiment 8, antioxygenic property experiment
The size of sample is 2mm × 4mm × 10mm, and sample need to first pass through corase grinding, polishing, cleaning, drying, record sample mass,
It will heat up into 1000 DEG C, 1100 DEG C and 1200 DEG C Muffle furnaces and keep the temperature to take out from stove after 5 h respectively and cool down in air, remember
The weight of sample after record oxidation.The weightening of front and back unit area is aoxidized according to sample（mg）To weigh the antioxygenic property of material.
Test result is as shown above, it is seen that the product of the invention existing product on antioxygenic property, which has, significantly to be carried
It rises.
Foregoing description is only proposed as the enforceable technical solution of the present invention, not as to the single of its technical solution itself
Restrictive condition.
Claims (9)
1. a kind of preparation method of anti-bacteria ceramic glaze filling nano-calcium carbonate, it is characterised in that：This method includes following step
Suddenly：
A, it is slowly stirred down, kiln gas is passed through into the calcium hydroxide slurry after ageing and carries out carburizing reagent, until reaction system
PH value is reduced to 9.0-8.0, particular surface inorganic agent complex is then added into reaction system, the reaction was continued under fast stirring
PH value to reaction system is down to 6.5-7.0, stops reaction；
B, sodium molybdate and zinc nitrate are added into the slurry system obtained by step A, continues stirring to the complete mixing of system, then will
Gained nano-calcium carbonate slurry is dehydrated, is dried, is crushed, is dispensed, and anti-bacteria ceramic glaze filling nano-calcium carbonate is obtained.
2. the preparation method of anti-bacteria ceramic glaze filling nano-calcium carbonate according to claim 1, it is characterised in that：Step
In rapid A, the particular surface inorganic agent complex uses polyethylene glycol-calgon complex.
3. the preparation method of anti-bacteria ceramic glaze filling nano-calcium carbonate according to claim 2, it is characterised in that：Step
In rapid A, the volume ratio of polyethylene glycol and calgon is in the polyethylene glycol-calgon surface conditioning agent complex
（2-20）:（60-120）；Also, it is calculated according to weight part ratio, the polyethylene glycol-calgon surface conditioning agent is compound
The ratio between the total weight of calcium carbonate is in the total weight and system of body（1-15）:100.
4. the preparation method of anti-bacteria ceramic glaze filling nano-calcium carbonate according to claim 3, it is characterised in that：Step
In rapid A, the volume ratio of polyethylene glycol and calgon is in the polyethylene glycol-calgon surface conditioning agent complex
（4-16）:（80-100）；Also, it is calculated according to weight part ratio, the polyethylene glycol-calgon surface conditioning agent is compound
The ratio between the total weight of calcium carbonate is in the total weight and system of body（1-10）:100.
5. the preparation method of anti-bacteria ceramic glaze filling nano-calcium carbonate according to claim 4, it is characterised in that：Step
In rapid A, the volume ratio of polyethylene glycol and calgon is in the polyethylene glycol-calgon surface conditioning agent complex
（5-10）:（90-95）；Also, it is calculated according to weight part ratio, the polyethylene glycol-calgon surface conditioning agent is compound
The ratio between the total weight of calcium carbonate is in the total weight and system of body（2-5）:100.
6. the preparation method of anti-bacteria ceramic glaze filling nano-calcium carbonate according to claim 1, it is characterised in that：Step
In rapid A, the digestion time of the calcium hydroxide slurry is 7-10h.
7. the preparation method of anti-bacteria ceramic glaze filling nano-calcium carbonate according to claim 1, it is characterised in that：Step
In rapid B, the dosage weight ratio of the sodium molybdate and zinc nitrate is 1:（0.5-5）；Also, it is calculated according to weight part ratio, it is described
The ratio between the total weight of calcium carbonate is in the total weight and system of sodium molybdate and zinc nitrate（5-8）:100.
8. the preparation method of anti-bacteria ceramic glaze filling nano-calcium carbonate according to claim 7, it is characterised in that：Step
In rapid B, the dosage weight ratio of the sodium molybdate and zinc nitrate is 1:（1-3）；Also, it is calculated according to weight part ratio, the molybdenum
The ratio between the total weight of calcium carbonate is in the total weight and system of sour sodium and zinc nitrate（6-7）:100.
9. the preparation method of anti-bacteria ceramic glaze filling nano-calcium carbonate according to claim 1, it is characterised in that：Step
In rapid B, continue to be stirred to react 1h-3h after sodium molybdate and zinc nitrate is added.
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| CN111423121A (en) * | 2020-04-29 | 2020-07-17 | 佛山科学技术学院 | Antibacterial ceramic glaze and preparation method thereof |
| CN113939475A (en) * | 2019-05-30 | 2022-01-14 | 白石工业株式会社 | Surface-treated calcium carbonate, process for producing the same, vinyl chloride resin composition, and molded article thereof |
| CN114736070A (en) * | 2022-04-25 | 2022-07-12 | 四川省农业科学院农业资源与环境研究所 | Coated controlled-release fertilizer and preparation method thereof |
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