CN118637826B - Cerium-containing modified rare earth water-retaining glaze for ceramics and preparation method thereof - Google Patents
Cerium-containing modified rare earth water-retaining glaze for ceramics and preparation method thereof Download PDFInfo
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- CN118637826B CN118637826B CN202411110260.4A CN202411110260A CN118637826B CN 118637826 B CN118637826 B CN 118637826B CN 202411110260 A CN202411110260 A CN 202411110260A CN 118637826 B CN118637826 B CN 118637826B
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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
- 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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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
- C04B41/5022—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials with vitreous materials
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/85—Coating or impregnation with inorganic materials
- C04B41/86—Glazes; Cold glazes
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
- Y02P40/60—Production of ceramic materials or ceramic elements, e.g. substitution of clay or shale by alternative raw materials, e.g. ashes
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Abstract
The invention provides a preparation method of a cerium-containing modified rare earth water-retaining glaze for ceramics, which comprises the following steps of uniformly mixing cerium salt, polyvinyl alcohol and a dispersing agent, adding ammonia water into the mixture, stirring the mixture under a heating condition, cooling the mixture to room temperature after the reaction is completed to obtain a mixture, centrifuging the mixture to obtain an intermediate, drying, calcining and sanding the intermediate to obtain a modified additive, and adding the modified additive into the glaze, and uniformly mixing the modified additive to obtain the cerium-containing modified rare earth water-retaining glaze. According to the cerium-containing modified rare earth water-retaining glaze for ceramics, part of sulfonyl groups of sodium dodecyl benzene sulfonate are converted into phenolic hydroxyl groups under an alkaline condition, more cerium atoms are fixed, the dissolved oxygen in water is increased, a carbon skeleton formed by high-temperature calcination of a dodecyl long chain and polyvinyl alcohol is favorable for adsorbing impurity ions, the carbon skeleton is stabilized, and the conductivity is reduced, so that the water quality of drinking water is improved.
Description
Technical Field
The invention belongs to the field of ceramics, and particularly relates to a cerium-containing modified rare earth water-retaining glaze for ceramics and a preparation method thereof.
Background
Cerium is widely explored in the manufacture of nanocrystals for fuel cells and catalytic applications. Their range of applications is scalable in these disciplines, ce having been successfully used as host material for dopants or as dopants for substances with unique functional purposes in optoelectronics, high energy physics and electrochemistry. Cerium oxide has at least two stable chemical states, namely cerium oxide (CeO 2) and cerium oxide (Ce 2O3), commonly referred to as sesquioxide. Pure CeO 2 has a fluorite structure with a special Fm3m group, in particular in the range from room temperature to melting point temperature. The phase change of CeO2 2-Ce2O3 depends on the oxygen pressure and temperature in the system, and the transition of reduction can be attributed to the quantum process link of oxygen vacancy formation and migration and ionization/delocalization of the 4f electrons of cerium. The close thermodynamic stability of CeO 2 and Ce 2O3 facilitates easy and reversible transformations between these two compounds, resulting in a series of partially reduced CeO 2-x phases that act as oxygen reservoirs by creating or eliminating oxygen vacancies.
Water is the most vital compound on earth and drinking water is a major challenge facing the world in the 21 st century. Pure and uncontaminated water is a fundamental condition for the survival of all organisms. More than 71% of the earth's surface is covered with water, but according to international standards, less than 68.1% of the water is potable due to different pollution. 69 major sources of water pollution include industrial wastewater discharge, agricultural activities, municipal wastewater, environmental and global changes. The presence of heavy metals, dyes and microorganisms, even in trace amounts, is very dangerous to human health, aquatic systems and the environment. At present, glazes on the market are mainly used for beautifying the surface of ceramics and improving the luster and touch feeling of the ceramics, but do not have the function of water conservation and cannot achieve the safety of drinking water.
Disclosure of Invention
In view of the above, the invention aims to overcome the defects in the prior art, and provides a cerium-containing modified rare earth water-retaining glaze for ceramics and a preparation method thereof.
In order to achieve the above purpose, the technical scheme of the invention is realized as follows:
The preparation process of water-retaining glaze with cerium-containing modified RE for ceramic includes the following steps:
Step 1, uniformly mixing cerium salt, polyvinyl alcohol and a dispersing agent, adding ammonia water into the mixture, stirring the mixture under a heating condition, and cooling the mixture to room temperature after the reaction is completed to obtain a mixture;
Step2, centrifuging the mixture to obtain an intermediate;
Step 3, drying, calcining and sanding the intermediate to obtain a modified additive;
And step 4, adding the modified additive into the glaze, and uniformly mixing to obtain the cerium-containing modified rare earth water-retaining glaze.
Further, the dispersing agent in the step 1 is sodium dodecyl benzene sulfonate, the cerium salt is cerium halide, and the cerium halide is at least one of CeF 4•3H2O、CeCl3•6H2O、CeBr2•7H2 O or CeI 3•9H2 O.
Further, the solid-to-liquid ratio of cerium salt, polyvinyl alcohol, dispersing agent and ammonia water in the step 1 is 6-15g:1-3g:0.5-1g:5-12mL, and the mass concentration of the ammonia water is 2-28%.
Further, the temperature of the heating step in the step 1 is 70-100 ℃, and the stirring step in the step 1 is 4-8 hours.
Further, the temperature of the centrifugation step in the step 2 is 15-30 ℃, the rotating speed is 6000-12000rpm, and the time is 0.5-2 hours.
Further, the temperature of the drying step in the step 3 is 70-100 ℃ for 1-4 hours, the temperature of the calcining step in the step 3 is 600-800 ℃ for 1-4 hours, the temperature rising rate is 5-10 ℃ per minute, the concentration of the sand grinding step in the step 3 is 20-35%, the temperature is 20-30 ℃, the time is 4-6 hours, the rotating speed is 2500-3300rpm, the mass concentration of the sand grinding step in the step 3 is 20-35%, the temperature is 20-30 ℃, the time is 4-6 hours, and the rotating speed is 2500-3300rpm.
Further, the mass ratio of the modifying additive to the glaze in the step 4 is 1-10:100.
Further, the glaze in the step4 comprises, by weight, 10-35 parts of quartz, 5-25 parts of mica, 15-25 parts of dolomite, 15-25 parts of feldspar, 5-15 parts of talcum and 5-15 parts of barium carbonate.
The cerium-containing modified rare earth water-retaining glaze for ceramics prepared by the preparation method.
The application of the cerium-containing modified rare earth water-retaining glaze for ceramics is that the cerium-containing modified rare earth water-retaining glaze is applied to the preparation of ceramic products.
The sodium dodecyl benzene sulfonate reacts under alkaline condition to generate sodium dodecyl phenol, the sodium dodecyl phenol combines with cerium ions to have stronger electrostatic adsorption force, after high-temperature calcination, the carbon skeleton combined by polyvinyl alcohol and cerium ions is broken by a dodecyl long chain, and part of cerium ions are fixed on the dodecyl, so that the specific surface area and active sites of the carbon skeleton are increased, and the water-retaining effect is improved.
Compared with the prior art, the invention has the following advantages:
In the cerium-containing modified rare earth water-retaining glaze for ceramics, part of sulfonyl groups of sodium dodecyl benzene sulfonate are converted into phenolic hydroxyl groups under alkaline conditions, more cerium atoms are fixed, and the dissolved oxygen in water is increased.
Drawings
FIG. 1 is a bar graph of dissolved oxygen according to an embodiment of the present invention;
Fig. 2 is a bar graph of electrical conductivity according to an embodiment of the present invention.
Detailed Description
Unless defined otherwise, technical terms used in the following examples have the same meaning as commonly understood by one of ordinary skill in the art to which the present invention pertains. The test reagents used in the following examples are all conventional biochemical reagents unless otherwise specified, and the test methods are all conventional methods unless otherwise specified.
Sodium dodecyl benzene sulfonate, hereinafter referred to as SDBS.
Polyvinyl alcohol, sodium dodecylbenzenesulfonate and aqueous ammonia (NH 3•H2 O), potassium iodide, manganese sulfate tetrahydrate, sodium thiosulfate pentahydrate, sodium carbonate, concentrated sulfuric acid were purchased from beijing solebao technologies, cerous nitrate hexahydrate, cerous chloride hexahydrate, cerous sulfate tetrahydrate, cerous oxalate were purchased from Shanghai milin Biochemical technologies, inc., all chemicals were used without further treatment, and distilled water (ρ=18.2M Ω.cm, 25 ℃) was from Millipore milli-Q water purification system.
The present invention will be described in detail with reference to examples.
Example 1
The preparation process of water-retaining glaze with cerium-containing modified RE for ceramic includes the following steps:
(1) Uniformly mixing 10g of cerium chloride hexahydrate, 2g of polyvinyl alcohol and 1g of sodium dodecyl benzene sulfonate, adding 10mL of ammonia water (20%) into the mixture, stirring the mixture for 6 hours under the heating condition of 80 ℃, and cooling the mixture to room temperature after the reaction is completed to obtain a mixture;
(2) Centrifuging the mixture at 10000rpm for 0.5 hour to obtain an intermediate;
(3) The intermediate is dried for 4 hours at 80 ℃, then calcined for 3 hours at 700 ℃, the calcining temperature rising speed is 5 ℃ per minute, after the muffle furnace is cooled to room temperature, the calcined powder is added into water, the concentration of the powder is controlled to be 25%, the powder is added into a sand mill, the sand milling temperature is 25 ℃, the sand milling rotating speed is 3200rpm, and the sand milling time is 5 hours to the modified additive;
(4) Adding 20 parts of quartz, 20 parts of mica, 20 parts of dolomite, 20 parts of feldspar, 10 parts of talcum, 5 parts of barium carbonate and 5 parts of modifying additive into 100 parts of water, stirring, uniformly coating on a ceramic blank, adding a ceramic cup coated with glaze into a calciner, calcining at 1200 ℃ for 11 hours, controlling the calcining heating rate at 10 ℃ per minute, and cooling to room temperature to obtain a cerium-containing rare earth glaze modified water-retaining ceramic Cup (CLL).
Comparative example 1
The preparation process of water-retaining glaze with cerium-containing modified RE for ceramic includes the following steps:
(1) Uniformly mixing 10g of cerium chloride hexahydrate, 2g of polyvinyl alcohol and 1g of cetyltrimethylammonium bromide, adding 10mL of ammonia water (20%) into the mixture, stirring the mixture for 6 hours under the heating condition of 80 ℃, and cooling the mixture to room temperature after the reaction is completed to obtain a mixture;
(2) Centrifuging the mixture at 10000rpm for 0.5 hour to obtain an intermediate;
(3) The intermediate is dried for 4 hours at 80 ℃, then calcined for 3 hours at 700 ℃, the calcining temperature rising speed is 5 ℃ per minute, after the muffle furnace is cooled to room temperature, the calcined powder is added into water, the concentration of the powder is controlled to be 25%, the powder is added into a sand mill, the sand milling temperature is 25 ℃, the sand milling rotating speed is 3200rpm, and the sand milling time is 5 hours to the modified additive;
(4) Adding 20 parts of quartz, 20 parts of mica, 20 parts of dolomite, 20 parts of feldspar, 10 parts of talcum, 5 parts of barium carbonate and 5 parts of modifying additive into 100 parts of water, stirring, uniformly coating on a ceramic blank, adding a ceramic cup coated with glaze into a calciner, calcining at 1200 ℃ for 11 hours, controlling the calcining heating rate at 10 ℃ per minute, and cooling to room temperature to obtain the cerium-containing rare earth glaze modified water-retaining ceramic cup.
Comparative example 2
The preparation process of water-retaining glaze with cerium-containing modified RE for ceramic includes the following steps:
(1) Uniformly mixing 10g of cerium chloride hexahydrate, 2g of polyvinyl alcohol and 1g of sodium dodecyl benzene sulfonate, stirring for 6 hours under the heating condition of 80 ℃, and cooling to room temperature after the reaction is completed to obtain a mixture;
(2) Centrifuging the mixture at 10000rpm for 0.5 hour to obtain an intermediate;
(3) The intermediate is dried for 4 hours at 80 ℃, then calcined for 3 hours at 700 ℃, the calcining temperature rising speed is 5 ℃ per minute, after the muffle furnace is cooled to room temperature, the calcined powder is added into water, the concentration of the powder is controlled to be 25%, the powder is added into a sand mill, the sand milling temperature is 25 ℃, the sand milling rotating speed is 3200rpm, and the sand milling time is 5 hours to the modified additive;
(4) Adding 20 parts of quartz, 20 parts of mica, 20 parts of dolomite, 20 parts of feldspar, 10 parts of talcum, 5 parts of barium carbonate and 5 parts of modifying additive into 100 parts of water, stirring, uniformly coating on a ceramic blank, adding a ceramic cup coated with glaze into a calciner, calcining at 1200 ℃ for 11 hours, controlling the calcining heating rate at 10 ℃ per minute, and cooling to room temperature to obtain the cerium-containing rare earth glaze modified water-retaining ceramic cup.
Comparative example 3
The preparation process of water-retaining glaze with cerium-containing modified RE for ceramic includes the following steps:
(1) 10gCe (NO 3)3•6H2 O, 2g of polyvinyl alcohol and 1g of sodium dodecyl benzene sulfonate are uniformly mixed, 10mL of ammonia water (20%) is added into the mixture, the mixture is stirred for 6 hours under the heating condition of 80 ℃, and the mixture is cooled to room temperature after the reaction is completed;
(2) Centrifuging the mixture at 10000rpm for 0.5 hour to obtain an intermediate;
(3) The intermediate is dried for 4 hours at 80 ℃, then calcined for 3 hours at 700 ℃, the calcining temperature rising speed is 5 ℃ per minute, after the muffle furnace is cooled to room temperature, the calcined powder is added into water, the concentration of the powder is controlled to be 25%, the powder is added into a sand mill, the sand milling temperature is 25 ℃, the sand milling rotating speed is 3200rpm, and the sand milling time is 5 hours to the modified additive;
(4) Adding 20 parts of quartz, 20 parts of mica, 20 parts of dolomite, 20 parts of feldspar, 10 parts of talcum, 5 parts of barium carbonate and 5 parts of modifying additive into 100 parts of water, stirring, uniformly coating on a ceramic blank, adding a ceramic cup coated with glaze into a calciner, calcining at 1200 ℃ for 11 hours, controlling the calcining heating rate at 10 ℃ per minute, and cooling to room temperature to obtain the cerium-containing rare earth glaze modified water-retaining ceramic cup.
The ceramic cups obtained in example 1 and comparative examples 1 to 3 were subjected to a dissolved oxygen amount test of water quality, and a blank control was a ceramic cup using a glaze to which no modifying additive was added, and the test method was performed by an iodometry method, and the test method was as follows:
The drinking water switch is regulated to slowly flow, and the ceramic cup to be measured is connected to about one half to one third of the overflow container, so that bubbles in water cannot be generated, the ceramic cup after drinking water is added is kept stand, and oxygen is prevented from entering the ceramic cup. 1mL of MnSO 4 solution (36 g of manganese sulfate tetrahydrate is fixed to 100mL by water) is sucked by a suction pipe, the solution is stretched into the bottom of a ceramic cup and added into drinking water, 2mL of alkaline potassium iodide solution (500 g of sodium hydroxide is dissolved in 300mL of water, 150g of potassium iodide is dissolved in 200mL of water, the two solutions are mixed and fixed to 1L of water), when the precipitate sinks to the bottom, 2mL of concentrated sulfuric acid (98%) is stretched into the lowest layer of the solution by the suction pipe and added, 100mL of the liquid is sucked by a suction pipe, the solution is added into a 250mL conical flask, sodium thiosulfate solution (6.2 g of sodium thiosulfate pentahydrate) is added into 1L of boiling water, then 0.2g of sodium carbonate is added for titration until the solution turns light yellow, 1mL of 1% starch solution is added, the sodium thiosulfate solution is continuously titrated, and the blue just returns to the calculated amount. Calculated by the amount of sodium thiosulfate used.
As shown in FIG. 1, compared with cetyl trimethyl ammonium bromide, no ammonia water, other cerium salts and blank ceramic cups, CCL ceramic cups show the highest dissolved oxygen, and the fact that enamel contained in the CCL ceramic cups has a very strong oxygen evolution effect is proved, meanwhile, sodium dodecyl benzene sulfonate promotes the increase of active sites of Ce under alkaline conditions, trivalent cerium and tetravalent cerium are mutually converted in ceramic glaze containing Ce, and the dissolved oxygen of the ceramic cups is improved.
The ceramic cups obtained in example 1 and comparative examples 1 to 3 were subjected to conductivity test of water quality, and a blank control was a ceramic cup using a glaze without addition of a modifying additive, and the test method was carried out using a MIK-TDS210-B conductivity detector of rice:
the ceramic cup to be measured is connected with purified water to two thirds, then the ceramic cup to be measured is placed for 2 hours, and the probe is placed into the water of the ceramic cup to be measured, kept for 30 seconds, read and recorded.
As shown in fig. 2, CCL has the lowest conductivity, which also proves that sodium dodecyl benzene sulfonate can better fix Ce atoms and polyvinyl alcohol, reduce ion concentration in water, adsorb other impurity ions, and improve quality of drinking water.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, alternatives, and improvements that fall within the spirit and scope of the invention.
Claims (9)
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| CN1426963A (en) * | 2001-12-17 | 2003-07-02 | 暨南大学 | Manufacturing method of nano cerium oxide powder |
| CN113149440A (en) * | 2021-03-16 | 2021-07-23 | 箭牌家居集团股份有限公司 | Environment-friendly negative ion opaque glaze and preparation method of sanitary ceramic using same |
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| CN206308273U (en) * | 2016-12-12 | 2017-07-07 | 广东芬芳陶瓷有限公司 | A kind of anion ecological ceramic structure |
| CN207122077U (en) * | 2017-08-25 | 2018-03-20 | 佛山市高明贝斯特陶瓷有限公司 | Anion ceramic thin plate |
| CN108017081B (en) * | 2017-12-19 | 2020-03-24 | 清华大学 | Preparation method of nano cerium oxide particles |
| CN118291043A (en) * | 2024-03-22 | 2024-07-05 | 包头市利晨科技有限公司 | Preparation method of nano cerium oxide polishing slurry |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1426963A (en) * | 2001-12-17 | 2003-07-02 | 暨南大学 | Manufacturing method of nano cerium oxide powder |
| CN113149440A (en) * | 2021-03-16 | 2021-07-23 | 箭牌家居集团股份有限公司 | Environment-friendly negative ion opaque glaze and preparation method of sanitary ceramic using same |
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