Antibacterial and environmentally friendly ceramic and preparation method thereof

Abstract

The invention discloses an antibacterial and environmentally friendly ceramic and a preparation method thereof, belonging to the technical field of ceramics. The method comprises: dissolving aluminum chloride, barium nitrate and ferric nitrate in a solvent and stirring and mixing them to prepare a first mixed liquid; adding kaolin and carbon powder to the first mixed liquid and stirring and mixing them to obtain a second mixed liquid; dispersing boron, carbon, aluminum, boron oxide, zirconium dioxide and barium carbonate in a dispersant and mixing them to prepare a third mixed liquid; adding boron oxide, aluminum hydroxide, titanium boride, zirconium, silicon, sodium zirconate, sodium carbonate, calcium tungstate and zirconium dioxide to the second mixed liquid and stirring and mixing them to prepare a mixed slurry; using the mixed slurry to prepare an embryo body, placing the embryo body in a sintering furnace and performing sintering treatment at different temperature stages and sintering environments. The prepared ceramic has high strength, is not prone to cracking in an environment with rapid temperature changes, and has good corrosion resistance.

Description

Technical Field

[0001] The present invention belongs to the technical field of ceramics, and in particular relates to an antibacterial and environmentally friendly ceramic and a preparation method thereof. Background Art

[0002] Ceramics have a long history of development. In the early days, they were mainly used as daily necessities and works of art. With the development of ceramic preparation technology, the performance of ceramics has become better and better, making fired ceramics suitable for more and more scenarios. Ceramics are also increasingly used in industry, and their use in life is becoming wider and wider. Different usage scenarios have different performance requirements for ceramics. For example, some require ceramics to have high mechanical strength, some require ceramics to have high antibacterial properties, and some require ceramics to have good corrosion resistance when used in harsh environments such as acidic or saline environments. Although some ceramics can meet the use requirements in terms of performance, there are still some shortcomings. For example, ceramics are prone to cracking when the temperature changes rapidly, which affects the use of ceramics. Summary of the Invention

[0003] The purpose of the embodiments of the present invention is to provide an antibacterial and environmentally friendly ceramic and a preparation method thereof, so as to solve the problem that ceramics are prone to cracking when the temperature changes rapidly.

[0004] In a first aspect, an embodiment of the present invention provides a method for preparing an antibacterial and environmentally friendly ceramic, comprising:

[0005] Dissolving aluminum chloride, barium nitrate, and ferric nitrate in a solvent and stirring and mixing the mixture to prepare a first mixed solution;

[0006] Adding kaolin and carbon powder to the first mixed solution and stirring and mixing to obtain a second mixed solution;

[0007] dispersing boron, carbon powder, aluminum, boron oxide, zirconium dioxide, and barium carbonate in a dispersant and mixing them to prepare a third mixed solution;

[0008] Adding boron oxide, aluminum hydroxide, titanium boride, zirconium, silicon, sodium zirconate, sodium carbonate, calcium tungstate, and zirconium dioxide to the second mixed solution and stirring and mixing to prepare a mixed slurry;

[0009] preparing an embryo body using the mixed slurry;

[0010] Place the embryo in a sintering furnace and heat it to 380-520°C and treat it in vacuum for 0.5-2 hours;

[0011] Then heat to 850-970℃ and treat in the first environment for 1-2.5h;

[0012] After cooling the embryos, immerse them in the third mixed solution;

[0013] Then place the embryo in a sintering furnace and heat it to 350-480℃ and treat it in vacuum for 10-40 minutes;

[0014] Continue to heat up to 930-1120℃ and treat in the second environment for 1-3 hours;

[0015] Then the temperature is raised to 1250-1520℃ and treated in the third environment for 2-6h;

[0016] The first environment is a vacuum or argon environment, the second environment is a vacuum or argon environment, and the third environment is a vacuum or inert environment.

[0017] Optionally, in the mixed slurry, the content of the components in the raw materials is:

[0018] Kaolin 20-43 parts by mass;

[0019] 2.6-4.5 parts by mass of carbon powder;

[0020] Aluminum chloride 0.3-0.7 parts by mass;

[0021] 0.4-1.1 parts by mass of barium nitrate;

[0022] 0.3-0.8 parts by mass of ferric nitrate;

[0023] 1.8-3.5 parts by mass of boron oxide;

[0024] 1.5-3 parts by mass of aluminum hydroxide;

[0025] 0.5-1 parts by mass of titanium boride;

[0026] Silicon 0.5-1.2 parts by mass;

[0027] Zirconium 0.3-0.8 parts by mass;

[0028] 0.6-1.8 parts by mass of sodium zirconate;

[0029] 0.4-0.8 parts by mass of sodium carbonate;

[0030] 0.3-1.2 parts by mass of calcium tungstate;

[0031] 0.5-1.5 parts by mass of zirconium dioxide.

[0032] Optionally, in the third mixed solution, the content of the components in the raw materials is:

[0033] Boron 0.5-1 parts by mass;

[0034] Carbon powder 1.5-2.7 parts by mass;

[0035] Aluminum 0.7-1.8 parts by mass;

[0036] Zirconium 0.3-0.6 parts by mass;

[0037] 0.5-1.2 parts by mass of boron oxide;

[0038] 0.2-0.5 parts by mass of zirconium dioxide;

[0039] 0.2-0.5 parts by mass of barium carbonate.

[0040] Optionally, the step of heating to 1250-1520° C. and treating in a third environment for 2-6 hours comprises:

[0041] First, heat to 1250-1320℃ and treat in vacuum environment for 0.5-2h;

[0042] After cooling the embryo, the embryo is placed in an acidic solution for 0.5-1 hour, and then placed in an alkaline solution for 0.5-1 hour; then the embryo is placed in a sintering furnace, heated to 1350-1520° C., and treated in nitrogen for 0.5-2 hours.

[0043] Optionally, after placing the embryonic body in a sintering furnace and heating it to 1350-1520° C. and treating it in nitrogen for 0.5-2 hours, the method further comprises:

[0044] The embryo body is placed in an oxidizing atmosphere at 820-900°C for 10-30 minutes.

[0045] Optionally, the kaolin is pretreated kaolin, and the treatment method of the pretreated kaolin is:

[0046] The kaolin is acid-washed with an acidic solution, then alkali-washed with an alkaline solution, washed with water, and then dried;

[0047] Mixing the dried kaolin with boron and titanium to prepare a first mixed powder;

[0048] The first mixed powder is placed in silane gas and treated at 800-950° C. for 0.5-1.5 hours;

[0049] Then, the first mixed material powder is placed in the first mixed gas and treated at 870-1020° C. for 0.5-1 h;

[0050] The first mixed gas includes argon, methane and nitrogen.

[0051] Optionally, the mass of boron in the first mixed powder is 1.2-3% of the mass of kaolin, and the mass of titanium in the first mixed powder is 0.6-1.5% of the mass of kaolin;

[0052] The volume of methane in the first mixed gas accounts for 12-25%, and the volume of nitrogen in the first mixed gas accounts for 15-30%.

[0053] Optionally, the kaolin is pretreated kaolin, and the treatment method of the pretreated kaolin is:

[0054] The kaolin is acid-washed with an acidic solution, then alkali-washed with an alkaline solution, washed with water, and then dried;

[0055] The dried kaolin is mixed with boron, titanium and silicon diimide to prepare a second mixed powder;

[0056] The second mixed powder is placed in ammonia and treated at 780-900°C for 0.5-2h;

[0057] The kaolin is then placed in methane gas and treated at 820-950°C for 0.5-1.5h;

[0058] Finally, the kaolin is placed in nitrogen and treated at 1460-1550° C. for 10-40 minutes.

[0059] Optionally, the mass of boron in the second mixed powder is 1-2.5% of the mass of kaolin, the mass of titanium in the second mixed powder is 0.4-1.2% of the mass of kaolin, and the mass of diimino silicon in the second mixed powder is 0.8-3% of the mass of kaolin.

[0060] The embodiment of the present invention further provides an antibacterial and environmentally friendly ceramic, which is prepared using the above-mentioned preparation method.

[0061] In the preparation method of the antibacterial and environmentally friendly ceramics of the embodiment of the present invention, aluminum chloride, barium nitrate, and ferric nitrate are dissolved in a solvent and stirred and mixed to prepare a first mixed liquid, kaolin and carbon powder are added to the first mixed liquid and stirred and mixed to obtain a second mixed liquid, boron, carbon powder, aluminum, boron oxide, zirconium dioxide, and barium carbonate are dispersed in a dispersant and mixed to prepare a third mixed liquid, boron oxide, aluminum hydroxide, titanium boride, zirconium, silicon, sodium zirconate, sodium carbonate, calcium tungstate, and zirconium dioxide are added to the second mixed liquid and stirred and mixed to prepare a mixed slurry, the mixed slurry is used to prepare a blank, and the blank is placed in a sintering furnace for sintering treatment at different temperature stages and sintering environments. The prepared ceramic has high strength, is not prone to cracks in an environment with rapidly changing temperature, has good high and low temperature resistance, good corrosion resistance, good antibacterial properties, and can be applied to a variety of usage environments. DETAILED DESCRIPTION

[0062] The following will be combined with the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the embodiments described are part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making any creative efforts shall fall within the scope of protection of the present invention.

[0063] The method for preparing the antibacterial and environmentally friendly ceramic of the present invention comprises:

[0064] Dissolving aluminum chloride, barium nitrate, and ferric nitrate in a solvent and stirring and mixing the mixture to prepare a first mixed solution;

[0065] Adding kaolin and carbon powder to the first mixed solution and stirring and mixing to obtain a second mixed solution;

[0066] dispersing boron, carbon powder, aluminum, boron oxide, zirconium dioxide, and barium carbonate in a dispersant and mixing them to prepare a third mixed solution;

[0067] Adding boron oxide, aluminum hydroxide, titanium boride, zirconium, silicon, sodium zirconate, sodium carbonate, calcium tungstate, and zirconium dioxide to the second mixed solution and stirring and mixing to prepare a mixed slurry;

[0068] preparing an embryo body using the mixed slurry;

[0069] Place the embryo in a sintering furnace and heat it to 380-520°C and treat it in vacuum for 0.5-2 hours;

[0070] Then heat to 850-970℃ and treat in the first environment for 1-2.5h;

[0071] After cooling the embryo, immerse it in the third mixed solution. The immersion can be performed under ultrasonic conditions so that the third mixed solution can penetrate into the pores. The ultrasonic immersion can be performed at 20-60 kHz and the ultrasonic immersion time can be 0.5-2 hours.

[0072] Then place the embryo in a sintering furnace and heat it to 350-480℃ and treat it in vacuum for 10-40 minutes;

[0073] Continue to heat up to 930-1120℃ and treat in the second environment for 1-3 hours;

[0074] Then the temperature is raised to 1250-1520℃ and treated in the third environment for 2-6h;

[0075] The first environment is a vacuum or argon environment, the second environment is a vacuum or argon environment, and the third environment is a vacuum or inert environment.

[0076] In the preparation method of the antibacterial and environmentally friendly ceramics of the embodiment of the present invention, aluminum chloride, barium nitrate, and ferric nitrate are dissolved in a solvent and stirred and mixed to prepare a first mixed liquid, kaolin and carbon powder are added to the first mixed liquid and stirred and mixed to obtain a second mixed liquid, boron, carbon powder, aluminum, boron oxide, zirconium dioxide, and barium carbonate are dispersed in a dispersant and mixed to prepare a third mixed liquid, boron oxide, aluminum hydroxide, titanium boride, zirconium, silicon, sodium zirconate, sodium carbonate, calcium tungstate, and zirconium dioxide are added to the second mixed liquid and stirred and mixed to prepare a mixed slurry, the mixed slurry is used to prepare a blank, and the blank is placed in a sintering furnace for sintering treatment at different temperature stages and sintering environments. The prepared ceramic has high strength, is not prone to cracks in an environment with rapidly changing temperature, has good high and low temperature resistance, good corrosion resistance, good antibacterial properties, and can be applied to a variety of usage environments.

[0077] In some embodiments, in the mixed slurry, the component contents in the raw materials may be:

[0078] Kaolin 20-43 parts by mass;

[0079] 2.6-4.5 parts by mass of carbon powder;

[0080] Aluminum chloride 0.3-0.7 parts by mass;

[0081] 0.4-1.1 parts by mass of barium nitrate;

[0082] 0.3-0.8 parts by mass of ferric nitrate;

[0083] 1.8-3.5 parts by mass of boron oxide;

[0084] 1.5-3 parts by mass of aluminum hydroxide;

[0085] 0.5-1 parts by mass of titanium boride;

[0086] Silicon 0.5-1.2 parts by mass;

[0087] Zirconium 0.3-0.8 parts by mass;

[0088] 0.6-1.8 parts by mass of sodium zirconate;

[0089] 0.4-0.8 parts by mass of sodium carbonate;

[0090] 0.3-1.2 parts by mass of calcium tungstate;

[0091] 0.5-1.5 parts by mass of zirconium dioxide.

[0092] In an embodiment of the present invention, in the third mixed solution, the component contents in the raw materials are:

[0093] Boron 0.5-1 parts by mass;

[0094] Carbon powder 1.5-2.7 parts by mass;

[0095] Aluminum 0.7-1.8 parts by mass;

[0096] Zirconium 0.3-0.6 parts by mass;

[0097] 0.5-1.2 parts by mass of boron oxide;

[0098] 0.2-0.5 parts by mass of zirconium dioxide;

[0099] 0.2-0.5 parts by mass of barium carbonate.

[0100] In some specific embodiments, the step of heating to 1250-1520° C. and treating in a third environment for 2-6 hours may include:

[0101] First, heat to 1250-1320℃ and treat in vacuum environment for 0.5-2h;

[0102] After cooling the embryo, the embryo is placed in an acidic solution for 0.5-1 hour, and then placed in an alkaline solution for 0.5-1 hour; then the embryo is placed in a sintering furnace, heated to 1350-1520° C., and treated in nitrogen for 0.5-2 hours.

[0103] Optionally, after placing the embryonic body in a sintering furnace and heating it to 1350-1520° C. and treating it in nitrogen for 0.5-2 hours, the following steps may be further included:

[0104] The embryo body is placed in an oxidizing atmosphere at 820-900°C for 10-30 minutes.

[0105] In some embodiments of the present invention, the kaolin is pretreated kaolin, and the treatment method of the pretreated kaolin may be:

[0106] The kaolin is acid-washed with an acidic solution, then alkaline-washed with an alkaline solution, washed with water, and then dried; the acidic solution may be a sulfuric acid solution with a concentration of 0.5-2 mol / L, a hydrochloric acid solution with a concentration of 0.5-2 mol / L, or a nitric acid solution with a concentration of 0.5-2 mol / L; the alkaline solution may be a sodium hydroxide solution with a concentration of 0.5-2 mol / L;

[0107] Mixing the dried kaolin with boron and titanium to prepare a first mixed powder;

[0108] The first mixed powder is placed in silane gas and treated at 800-950° C. for 0.5-1.5 hours;

[0109] Then, the first mixed material powder is placed in the first mixed gas and treated at 870-1020° C. for 0.5-1 h;

[0110] The first mixed gas includes argon, methane and nitrogen.

[0111] Optionally, the mass of boron in the first mixed powder is 1.2-3% of the mass of kaolin, and the mass of titanium in the first mixed powder is 0.6-1.5% of the mass of kaolin;

[0112] The volume of methane in the first mixed gas accounts for 12-25%, and the volume of nitrogen in the first mixed gas accounts for 15-30%.

[0113] In some other embodiments of the present invention, the kaolin is pretreated kaolin, and the treatment method of the pretreated kaolin is:

[0114] The kaolin is acid-washed with an acidic solution, then alkali-washed with an alkaline solution, washed with water, and then dried; the acidic solution can be a sulfuric acid solution with a concentration of 0.5-2 mol / L, a hydrochloric acid solution with a concentration of 0.5-2 mol / L, or a nitric acid solution with a concentration of 0.5-2 mol / L; the alkaline solution can be a sodium hydroxide solution with a concentration of 0.1-2 mol / L; the alkaline solution can also be ammonia water, sodium carbonate solution, sodium bicarbonate solution, calcium hydroxide solution, potassium hydroxide solution, etc.;

[0115] The dried kaolin is mixed with boron, titanium and silicon diimide to prepare a second mixed powder;

[0116] The second mixed powder is placed in ammonia and treated at 780-900°C for 0.5-2h;

[0117] The kaolin is then placed in methane gas and treated at 820-950°C for 0.5-1.5h;

[0118] Finally, the kaolin is placed in nitrogen and treated at 1460-1550° C. for 10-40 minutes.

[0119] Optionally, the mass of boron in the second mixed powder is 1-2.5% of the mass of kaolin, the mass of titanium in the second mixed powder is 0.4-1.2% of the mass of kaolin, and the mass of diimino silicon in the second mixed powder is 0.8-3% of the mass of kaolin.

[0120] The antibacterial and environmentally friendly ceramics according to the embodiments of the present invention are prepared using the above-described preparation method of the present invention.

[0121] The present invention will be further described below through some embodiments. Example 1

[0122] The preparation method of antibacterial environmentally friendly ceramics comprises the following steps:

[0123] Dissolving aluminum chloride, barium nitrate, and ferric nitrate in a solvent and stirring and mixing the mixture to prepare a first mixed solution;

[0124] Adding kaolin and carbon powder to the first mixed solution and stirring and mixing to obtain a second mixed solution;

[0125] dispersing boron, carbon powder, aluminum, boron oxide, zirconium dioxide, and barium carbonate in a dispersant and mixing them to prepare a third mixed solution;

[0126] Adding boron oxide, aluminum hydroxide, titanium boride, zirconium, silicon, sodium zirconate, sodium carbonate, calcium tungstate, and zirconium dioxide to the second mixed solution and stirring and mixing to prepare a mixed slurry;

[0127] preparing an embryo body using the mixed slurry;

[0128] The embryo was placed in a sintering furnace and heated to 380°C and treated in vacuum for 2 hours;

[0129] Then the temperature was raised to 970°C and treated in the first environment for 1 hour;

[0130] After cooling the embryos, immerse them in the third mixed solution;

[0131] Then, the embryo body was placed in a sintering furnace and heated to 480°C and treated in vacuum for 10 minutes;

[0132] Continue heating to 930℃ and treat in the second environment for 3h;

[0133] Then the temperature was raised to 1520°C and treated in the third environment for 2 hours;

[0134] The first environment is a vacuum, the second environment is a vacuum, and the third environment is an inert environment.

[0135] In the mixed slurry, the content of the components in the raw materials is:

[0136] 20 parts by mass of kaolin; 2.6 parts by mass of carbon powder; 0.7 parts by mass of aluminum chloride;

[0137] 0.4 parts by mass of barium nitrate; 0.8 parts by mass of ferric nitrate; 1.8 parts by mass of boron oxide;

[0138] 1.5 parts by mass of aluminum hydroxide; 1 part by mass of titanium boride; 0.5 parts by mass of silicon;

[0139] 0.3 parts by mass of zirconium; 1.8 parts by mass of sodium zirconate; 0.4 parts by mass of sodium carbonate;

[0140] 0.3 parts by mass of calcium tungstate; 0.5 parts by mass of zirconium dioxide.

[0141] In the third mixed solution, the content of the components in the raw materials is:

[0142] 0.5 parts by mass of boron; 1.5 parts by mass of carbon powder; 1.8 parts by mass of aluminum;

[0143] 0.3 parts by mass of zirconium; 0.5 parts by mass of boron oxide;

[0144] 0.5 parts by mass of zirconium dioxide; 0.2 parts by mass of barium carbonate. Example 2

[0145] The preparation method of antibacterial environmentally friendly ceramics comprises the following steps:

[0146] Dissolving aluminum chloride, barium nitrate, and ferric nitrate in a solvent and stirring and mixing the mixture to prepare a first mixed solution;

[0147] Adding kaolin and carbon powder to the first mixed solution and stirring and mixing to obtain a second mixed solution;

[0148] dispersing boron, carbon powder, aluminum, boron oxide, zirconium dioxide, and barium carbonate in a dispersant and mixing them to prepare a third mixed solution;

[0149] Adding boron oxide, aluminum hydroxide, titanium boride, zirconium, silicon, sodium zirconate, sodium carbonate, calcium tungstate, and zirconium dioxide to the second mixed solution and stirring and mixing to prepare a mixed slurry;

[0150] preparing an embryo body using the mixed slurry;

[0151] The embryo was placed in a sintering furnace and heated to 520°C and treated in vacuum for 0.5 h;

[0152] Then the temperature was raised to 850°C and treated in the first environment for 2.5h;

[0153] After cooling the embryos, immerse them in the third mixed solution;

[0154] The embryonic body is then placed in a sintering furnace and heated to 350°C and treated in vacuum for 40 minutes;

[0155] Continue heating to 1120℃ and treat in the second environment for 1 hour;

[0156] Then the temperature was raised to 1250°C and treated in the third environment for 6 hours;

[0157] The first environment is a vacuum environment, the second environment is a vacuum environment, and the third environment is an inert environment.

[0158] In the mixed slurry, the content of the components in the raw materials is:

[0159] Kaolin 43 parts by mass; carbon powder 4.5 parts by mass; aluminum chloride 0.3 parts by mass;

[0160] 1.1 parts by mass of barium nitrate; 0.3 parts by mass of ferric nitrate; 3.5 parts by mass of boron oxide;

[0161] 3 parts by mass of aluminum hydroxide; 0.5 parts by mass of titanium boride; 1.2 parts by mass of silicon;

[0162] 0.8 parts by mass of zirconium; 0.6 parts by mass of sodium zirconate; 0.8 parts by mass of sodium carbonate;

[0163] 1.2 parts by mass of calcium tungstate; 1.5 parts by mass of zirconium dioxide.

[0164] In the third mixed solution, the content of the components in the raw materials is:

[0165] Boron 1 part by mass; Carbon powder 2.7 parts by mass; Aluminum 0.7 parts by mass;

[0166] 0.6 parts by mass of zirconium; 1.2 parts by mass of boron oxide;

[0167] 0.2 parts by mass of zirconium dioxide; 0.5 parts by mass of barium carbonate. Example 3

[0168] The preparation method of antibacterial environmentally friendly ceramics comprises the following steps:

[0169] Dissolving aluminum chloride, barium nitrate, and ferric nitrate in a solvent and stirring and mixing the mixture to prepare a first mixed solution;

[0170] Adding kaolin and carbon powder to the first mixed solution and stirring and mixing to obtain a second mixed solution;

[0171] dispersing boron, carbon powder, aluminum, boron oxide, zirconium dioxide, and barium carbonate in a dispersant and mixing them to prepare a third mixed solution;

[0172] Adding boron oxide, aluminum hydroxide, titanium boride, zirconium, silicon, sodium zirconate, sodium carbonate, calcium tungstate, and zirconium dioxide to the second mixed solution and stirring and mixing to prepare a mixed slurry;

[0173] preparing an embryo body using the mixed slurry;

[0174] The embryo was placed in a sintering furnace and heated to 450°C and treated in vacuum for 1 hour;

[0175] Then the temperature was raised to 920°C and treated in the first environment for 1.5h;

[0176] After cooling the embryos, immerse them in the third mixed solution;

[0177] Then, the embryo body is placed in a sintering furnace and heated to 400°C and treated in vacuum for 20 minutes;

[0178] Continue heating to 1050℃ and treat in the second environment for 2h;

[0179] Then the temperature was raised to 1370°C and treated in the third environment for 4 hours;

[0180] The first environment is a vacuum environment, the second environment is a vacuum environment, and the third environment is an inert environment.

[0181] In the mixed slurry, the content of the components in the raw materials is:

[0182] 30 parts by mass of kaolin; 3.5 parts by mass of carbon powder; 0.5 parts by mass of aluminum chloride;

[0183] 0.8 parts by mass of barium nitrate; 0.5 parts by mass of ferric nitrate; 2.5 parts by mass of boron oxide;

[0184] 2.3 parts by mass of aluminum hydroxide; 0.7 parts by mass of titanium boride; 0.8 parts by mass of silicon;

[0185] 0.5 parts by mass of zirconium; 1.2 parts by mass of sodium zirconate; 0.6 parts by mass of sodium carbonate;

[0186] 0.8 parts by mass of calcium tungstate; 1 part by mass of zirconium dioxide.

[0187] In the third mixed solution, the content of the components in the raw materials is:

[0188] 0.7 parts by mass of boron; 2 parts by mass of carbon powder; 1.2 parts by mass of aluminum;

[0189] 0.5 parts by mass of zirconium; 0.9 parts by mass of boron oxide;

[0190] 0.4 parts by mass of zirconium dioxide; 0.4 parts by mass of barium carbonate. Example 4

[0191] The difference between Example 4 and Example 3 is:

[0192] The step "then heating to 1370°C and treating in a third environment for 4 hours" in Example 3 is changed to "first heating to 1250°C and treating in a vacuum environment for 2 hours; cooling the embryo body and then treating in an acidic solution for 0.5 hours, then in an alkaline solution for 0.5 hours; then placing the embryo body in a sintering furnace, heating to 1350°C, and treating in a nitrogen atmosphere for 2 hours." The acidic solution is a 0.5 mol / L nitric acid solution, and the alkaline solution can be a 0.5 mol / L sodium hydroxide solution. Example 5

[0193] The difference between Example 5 and Example 3 is:

[0194] The step "then heating to 1370°C and treating in a third environment for 4 hours" in Example 3 is changed to "first heating to 1320°C and treating in a vacuum environment for 0.5 hours; cooling the embryo body and treating in an acidic solution for 1 hour, then in an alkaline solution for 1 hour; then heating the embryo body in a sintering furnace, heating to 1520°C, and treating in a nitrogen atmosphere for 0.5 hours." The acidic solution can be a 0.5 mol / L nitric acid solution, and the alkaline solution can be a 0.5 mol / L sodium hydroxide solution. Example 6

[0195] The difference between Example 6 and Example 3 is:

[0196] The kaolin is pretreated kaolin, and the processing method of the pretreated kaolin is:

[0197] The kaolin is acid-washed with an acidic solution, then alkaline-washed with an alkaline solution, washed with water, and then dried; the acidic solution may be a 0.5 mol / L nitric acid solution, and the alkaline solution may be a calcium hydroxide solution;

[0198] Mixing the dried kaolin with boron and titanium to prepare a first mixed powder;

[0199] The first mixed powder is placed in silane gas and treated at 800° C. for 1.5 hours;

[0200] Then, the first mixed material powder is placed in the first mixed gas and treated at 1020° C. for 0.5 h;

[0201] The first mixed gas includes argon, methane and nitrogen;

[0202] The mass of boron in the first mixed powder is 1.2% of the mass of kaolin, and the mass of titanium in the first mixed powder is 1.5% of the mass of kaolin;

[0203] The volume of methane in the first mixed gas accounts for 12%, and the volume of nitrogen in the first mixed gas accounts for 30%. Example 7

[0204] The difference between Example 7 and Example 3 is:

[0205] The kaolin is pretreated kaolin, and the processing method of the pretreated kaolin is:

[0206] The kaolin is acid-washed with an acidic solution, then alkaline-washed with an alkaline solution, washed with water, and then dried; the acidic solution may be a 0.5 mol / L nitric acid solution, and the alkaline solution may be a calcium hydroxide solution;

[0207] Mixing the dried kaolin with boron and titanium to prepare a first mixed powder;

[0208] The first mixed powder is placed in silane gas and treated at 950° C. for 0.5 h;

[0209] Then, the first mixed material powder is placed in the first mixed gas and treated at 870° C. for 1 hour;

[0210] The first mixed gas includes argon, methane and nitrogen;

[0211] The mass of boron in the first mixed powder is 3% of the mass of kaolin, and the mass of titanium in the first mixed powder is 0.6% of the mass of kaolin;

[0212] The volume of methane in the first mixed gas accounts for 25%, and the volume of nitrogen in the first mixed gas accounts for 15%. Example 8

[0213] The difference between Example 8 and Example 5 is:

[0214] The kaolin is pretreated kaolin, and the processing method of the pretreated kaolin is:

[0215] The kaolin is acid-washed with an acidic solution, then alkaline-washed with an alkaline solution, washed with water, and then dried; the acidic solution may be a 0.5 mol / L nitric acid solution, and the alkaline solution may be a calcium hydroxide solution;

[0216] Mixing the dried kaolin with boron and titanium to prepare a first mixed powder;

[0217] The first mixed powder is placed in silane gas and treated at 800° C. for 1.5 hours;

[0218] Then, the first mixed material powder is placed in the first mixed gas and treated at 1020° C. for 0.5 h;

[0219] The first mixed gas includes argon, methane and nitrogen;

[0220] The mass of boron in the first mixed powder is 1.2% of the mass of kaolin, and the mass of titanium in the first mixed powder is 1.5% of the mass of kaolin;

[0221] The volume of methane in the first mixed gas accounts for 12%, and the volume of nitrogen in the first mixed gas accounts for 30%. Example 9

[0222] The difference between Example 9 and Example 5 is:

[0223] The kaolin is pretreated kaolin, and the processing method of the pretreated kaolin is:

[0224] The kaolin is acid-washed with an acidic solution, then alkaline-washed with an alkaline solution, washed with water, and then dried; the acidic solution may be a 0.5 mol / L nitric acid solution, and the alkaline solution may be a calcium hydroxide solution;

[0225] Mixing the dried kaolin with boron and titanium to prepare a first mixed powder;

[0226] The first mixed powder is placed in silane gas and treated at 950° C. for 0.5 h;

[0227] Then, the first mixed material powder is placed in the first mixed gas and treated at 870° C. for 1 hour;

[0228] The first mixed gas includes argon, methane and nitrogen;

[0229] The mass of boron in the first mixed powder is 3% of the mass of kaolin, and the mass of titanium in the first mixed powder is 0.6% of the mass of kaolin;

[0230] The volume of methane in the first mixed gas accounts for 25%, and the volume of nitrogen in the first mixed gas accounts for 15%. Example 10

[0231] The difference between Example 10 and Example 3 is that:

[0232] The kaolin is pretreated kaolin, and the processing method of the pretreated kaolin is:

[0233] The kaolin is acid-washed with an acidic solution, then alkaline-washed with an alkaline solution, washed with water, and then dried; the acidic solution may be a 0.5 mol / L nitric acid solution, and the alkaline solution may be a calcium hydroxide solution;

[0234] The dried kaolin is mixed with boron, titanium and silicon diimide to prepare a second mixed powder;

[0235] The second mixed powder was placed in ammonia and treated at 780°C for 2 hours;

[0236] The kaolin was then treated in methane gas at 950 °C for 0.5 h;

[0237] Finally, the kaolin was treated in nitrogen at 1460 °C for 40 min;

[0238] The mass of boron in the second mixed powder is 1% of the mass of kaolin, the mass of titanium in the second mixed powder is 1.2% of the mass of kaolin, and the mass of diimino silicon in the second mixed powder is 0.8% of the mass of kaolin. Example 11

[0239] The difference between Example 11 and Example 3 is that:

[0240] The kaolin is pretreated kaolin, and the processing method of the pretreated kaolin is:

[0241] The kaolin is acid-washed with an acidic solution, then alkaline-washed with an alkaline solution, washed with water, and then dried; the acidic solution may be a 0.5 mol / L nitric acid solution, and the alkaline solution may be a calcium hydroxide solution;

[0242] The dried kaolin is mixed with boron, titanium and silicon diimide to prepare a second mixed powder;

[0243] The second mixed powder was placed in ammonia and treated at 900°C for 0.5h;

[0244] The kaolin was then treated in methane gas at 820 °C for 1.5 h;

[0245] Finally, the kaolin was treated in nitrogen at 1550 °C for 10 min;

[0246] The mass of boron in the second mixed powder is 2.5% of the mass of kaolin, the mass of titanium in the second mixed powder is 0.4% of the mass of kaolin, and the mass of diimino silicon in the second mixed powder is 3% of the mass of kaolin. Example 12

[0247] The difference between Example 12 and Example 5 is that:

[0248] The kaolin is pretreated kaolin, and the processing method of the pretreated kaolin is:

[0249] The kaolin is acid-washed with an acidic solution, then alkaline-washed with an alkaline solution, washed with water, and then dried; the acidic solution may be a 0.5 mol / L nitric acid solution, and the alkaline solution may be a calcium hydroxide solution;

[0250] The dried kaolin is mixed with boron, titanium and silicon diimide to prepare a second mixed powder;

[0251] The second mixed powder was placed in ammonia and treated at 780°C for 2 hours;

[0252] The kaolin was then treated in methane gas at 950 °C for 0.5 h;

[0253] Finally, the kaolin was treated in nitrogen at 1460 °C for 40 min;

[0254] The mass of boron in the second mixed powder is 1% of the mass of kaolin, the mass of titanium in the second mixed powder is 1.2% of the mass of kaolin, and the mass of diimino silicon in the second mixed powder is 0.8% of the mass of kaolin. Example 13

[0255] The difference between Example 13 and Example 5 is that:

[0256] The kaolin is pretreated kaolin, and the processing method of the pretreated kaolin is:

[0257] The kaolin is acid-washed with an acidic solution, then alkaline-washed with an alkaline solution, washed with water, and then dried; the acidic solution may be a 0.5 mol / L nitric acid solution, and the alkaline solution may be a calcium hydroxide solution;

[0258] The dried kaolin is mixed with boron, titanium and silicon diimide to prepare a second mixed powder;

[0259] The second mixed powder was placed in ammonia and treated at 900°C for 0.5h;

[0260] The kaolin was then treated in methane gas at 820 °C for 1.5 h;

[0261] Finally, the kaolin was treated in nitrogen at 1550 °C for 10 min;

[0262] The mass of boron in the second mixed powder is 2.5% of the mass of kaolin, the mass of titanium in the second mixed powder is 0.4% of the mass of kaolin, and the mass of diimino silicon in the second mixed powder is 3% of the mass of kaolin.

[0263] The ceramics prepared by the preparation method in the above embodiment were subjected to performance tests, and the specific performance test results are shown in Table 1.

[0264] Low temperature resistance test: The ceramics prepared in the above examples were placed at -40°C for 30 days, and the surface of the ceramics was observed after removal.

[0265] Temperature change resistance test: The ceramic prepared in the above embodiment was placed at -40°C for 3 days, taken out and quickly placed in boiling water for 2 hours, and then the surface of the ceramic was taken out and observed.

[0266] Oxidation resistance test: The ceramics prepared in the above examples were placed in an air environment at 60°C for 10 days, and then the surface of the ceramics was taken out and observed.

[0267] Table 1 Performance test results of the ceramics prepared in the above examples

[0268] name Low temperature resistance test results Temperature change resistance test results Oxidation resistance test results Example 1 No cracks or changes on the surface No cracks or changes on the surface No cracks or changes on the surface Example 2 No cracks or changes on the surface No cracks or changes on the surface No cracks or changes on the surface Example 3 No cracks or changes on the surface No cracks or changes on the surface No cracks or changes on the surface Example 4 No cracks or changes on the surface No cracks or changes on the surface No cracks or changes on the surface Example 5 No cracks or changes on the surface No cracks or changes on the surface No cracks or changes on the surface Example 6 No cracks or changes on the surface No cracks or changes on the surface No cracks or changes on the surface Example 7 No cracks or changes on the surface No cracks or changes on the surface No cracks or changes on the surface Example 8 No cracks or changes on the surface No cracks or changes on the surface No cracks or changes on the surface Example 9 No cracks or changes on the surface No cracks or changes on the surface No cracks or changes on the surface Example 10 No cracks or changes on the surface No cracks or changes on the surface No cracks or changes on the surface Example 11 No cracks or changes on the surface No cracks or changes on the surface No cracks or changes on the surface Example 12 No cracks or changes on the surface No cracks or changes on the surface No cracks or changes on the surface Example 13 No cracks or changes on the surface No cracks or changes on the surface No cracks or changes on the surface

[0269] As can be seen from Table 1, the ceramics prepared in the above embodiment have good low-temperature resistance, are not prone to cracks or damage when the temperature changes rapidly, and no spots or damage are produced. The surface does not change after being placed in high-temperature air. The performance of the ceramics prepared by this method is stable.

[0270] The ceramics prepared by the preparation method in the above embodiment were subjected to corrosion resistance tests, and the specific test results are shown in Table 2.

[0271] Acid resistance test: The ceramic prepared in the above example was placed in a 1 mol / L sulfuric acid solution at 30°C for 10 days, then taken out, rinsed with water, and dried, and the surface of the ceramic was observed.

[0272] Alkali resistance test: The ceramic prepared in the above embodiment was placed in a 1 mol / L sodium hydroxide solution at 30°C for 10 days, then taken out, rinsed with water and dried, and the surface of the ceramic was observed.

[0273] Salt resistance test: Sodium chloride was added to water to prepare a sodium chloride salt solution with a mass concentration of 8%. The ceramic prepared in the above example was placed in the salt solution at 30°C for 10 days. After removal, it was rinsed with water and dried, and the surface of the ceramic was observed.

[0274] Table 2 Performance test results of the ceramics prepared in the above examples

[0275] name Acid resistance test results Alkali resistance test results Salt tolerance test results Example 1 There are tiny spots on the surface, but the quality remains unchanged. No change in surface, no change in quality No change in surface, no change in quality Example 2 No change in surface, no change in quality There are tiny spots on the surface, but the quality remains unchanged. No change in surface, no change in quality Example 3 No change in surface, no change in quality No change in surface, no change in quality No change in surface, no change in quality Example 4 No change in surface, no change in quality No change in surface, no change in quality No change in surface, no change in quality Example 5 No change in surface, no change in quality No change in surface, no change in quality No change in surface, no change in quality Example 6 No change in surface, no change in quality No change in surface, no change in quality No change in surface, no change in quality Example 7 No change in surface, no change in quality No change in surface, no change in quality No change in surface, no change in quality Example 8 No change in surface, no change in quality No change in surface, no change in quality No change in surface, no change in quality Example 9 No change in surface, no change in quality No change in surface, no change in quality No change in surface, no change in quality Example 10 No change in surface, no change in quality No change in surface, no change in quality No change in surface, no change in quality Example 11 No change in surface, no change in quality No change in surface, no change in quality No change in surface, no change in quality Example 12 No change in surface, no change in quality No change in surface, no change in quality No change in surface, no change in quality Example 13 No change in surface, no change in quality No change in surface, no change in quality No change in surface, no change in quality

[0276] As can be seen from Table 2, the ceramics prepared in the above examples have good acid resistance, good alkali resistance, good salt resistance, and strong corrosion resistance.

[0277] The ceramics prepared by the preparation method in the above embodiment were tested for antibacterial properties. The test method was: Antibacterial Properties of Antibacterial Ceramic Products (JC / T897-2014), and the test bacteria was Escherichia coli.

[0278] Antibacterial test of ceramics after high-temperature air treatment: The ceramics prepared in the above embodiment were placed in an air environment at 60°C for 10 days and then taken out for antibacterial testing.

[0279] Antibacterial test of the ceramics after acid solution treatment: The ceramics prepared in the above examples were placed in a 1 mol / L sulfuric acid solution at 30°C for 10 days, then rinsed with water and dried, and tested for antibacterial properties.

[0280] Antibacterial test of the ceramics after alkaline solution treatment: The ceramics prepared in the above examples were placed in a 1 mol / L sodium hydroxide solution at 30°C for 10 days, then rinsed with water and dried, and tested for antibacterial properties.

[0281] The antibacterial properties of the ceramics treated with a saline solution were tested: sodium chloride was added to water to prepare an 8% sodium chloride salt solution. The ceramics prepared in the above example were placed in the saline solution at 30°C for 10 days, then rinsed with water and dried, and tested for antibacterial properties.

[0282] The antibacterial properties of the untreated ceramics and the ceramics after the above treatment were tested, and the specific test results are shown in Table 3.

[0283] Table 3 Antibacterial test results of the ceramics prepared in the above examples

[0284] name Antibacterial rate of untreated ceramics Antibacterial rate after oxidation resistance test Antibacterial rate after acid resistance test Antibacterial rate after alkali resistance test Antibacterial rate after salt tolerance test Example 1 96.62 96.63 96.67 96.58 96.61 Example 2 97.37 97.22 97.25 97.31 97.34 Example 3 97.79 97.68 97.71 97.82 97.81 Example 4 98.36 98.26 98.30 98.35 98.33 Example 5 98.42 98.41 98.50 98.44 98.40 Example 6 98.89 98.76 98.74 98.85 98.86 Example 7 98.76 98.69 98.80 98.73 98.77 Example 8 98.92 98.94 98.86 98.95 98.95 Example 9 98.87 98.86 98.89 98.91 98.88 Example 10 98.83 98.85 98.81 98.86 98.85 Example 11 98.77 98.61 98.71 98.81 98.80 Example 12 98.90 98.94 98.95 98.85 98.89 Example 13 98.96 98.87 98.90 98.92 98.93

[0285] As can be seen from Table 3, the ceramics prepared in the above embodiments have good antibacterial properties. After being treated with high-temperature air, acidic solution, alkaline solution and salt solution, the antibacterial properties of the ceramics are still good. Therefore, the ceramics have good antibacterial properties after being treated in different environments.

[0286] The ceramics prepared by the preparation method in the above embodiment were subjected to strength tests, and the specific test results are shown in Table 4.

[0287] Table 4 Tensile strength test results of the ceramics prepared in the above examples

[0288] name Untreated ceramic tensile strength / MPa Example 1 376 Example 2 385 Example 3 382 Example 4 408 Example 5 417 Example 6 421 Example 7 428 Example 8 439 Example 9 446 Example 10 429 Example 11 432 Example 12 457 Example 13 463

[0289] As shown in Table 4, the ceramics prepared in the above examples have high tensile strength, and the ceramic prepared using pretreated kaolin has an even higher tensile strength. The ceramics maintain good tensile strength even after treatment with high-temperature air, acidic solution, alkaline solution, and salt solution. Therefore, the ceramics have excellent corrosion resistance and tensile strength.

[0290] The above description is made in conjunction with the embodiments of the present invention, but the present invention is not limited to the above-mentioned specific implementation methods. The above-mentioned specific implementation methods are merely illustrative and not restrictive. Under the guidance of the present invention, ordinary technicians in this field can also make many forms without departing from the scope of protection of the purpose of the present invention and the claims, all of which are protected by the present invention.

Claims

1. A method for preparing antibacterial and environmentally friendly ceramics, characterized in that: include: Dissolving aluminum chloride, barium nitrate, and ferric nitrate in a solvent and stirring and mixing the mixture to prepare a first mixed solution; Adding kaolin and carbon powder to the first mixed solution and stirring and mixing to obtain a second mixed solution; dispersing boron, carbon powder, aluminum, boron oxide, zirconium dioxide, and barium carbonate in a dispersant and mixing them to prepare a third mixed solution; Adding boron oxide, aluminum hydroxide, titanium boride, zirconium, silicon, sodium zirconate, sodium carbonate, calcium tungstate, and zirconium dioxide to the second mixed solution and stirring and mixing to prepare a mixed slurry; preparing an embryo body using the mixed slurry; Place the embryo in a sintering furnace and heat it to 380-520°C and treat it in vacuum for 0.5-2 hours; Then heat to 850-970℃ and treat in the first environment for 1-2.5h; After cooling the embryos, immerse them in the third mixed solution; Then place the embryo in a sintering furnace and heat it to 350-480℃ and treat it in vacuum for 10-40 minutes; Continue to heat up to 930-1120℃ and treat in the second environment for 1-3 hours; Then the temperature is raised to 1250-1520℃ and treated in the third environment for 2-6h; The first environment is a vacuum or argon environment, the second environment is a vacuum or argon environment, and the third environment is a vacuum or inert environment; The steps of heating to 1250-1520°C and treating in the third environment for 2-6 hours include: First, heat to 1250-1320℃ and treat in vacuum environment for 0.5-2h; After cooling the embryo, the embryo is placed in an acidic solution for 0.5-1 hour, and then placed in an alkaline solution for 0.5-1 hour; then the embryo is placed in a sintering furnace, heated to 1350-1520° C., and treated in nitrogen for 0.5-2 hours.

2. The preparation method according to claim 1, characterized in that In the mixed slurry, the content of the components in the raw materials is: 20-43 parts by mass of kaolin; 2.6-4.5 parts by mass of carbon powder; Aluminum chloride 0.3-0.7 parts by mass; 0.4-1.1 parts by mass of barium nitrate; 0.3-0.8 parts by mass of ferric nitrate; 1.8-3.5 parts by mass of boron oxide; 1.5-3 parts by mass of aluminum hydroxide; 0.5-1 parts by mass of titanium boride; Silicon 0.5-1.2 parts by mass; Zirconium 0.3-0.8 parts by mass; 0.6-1.8 parts by mass of sodium zirconate; 0.4-0.8 parts by mass of sodium carbonate; 0.3-1.2 parts by mass of calcium tungstate; 0.5-1.5 parts by mass of zirconium dioxide.

3. The preparation method according to claim 1 or 2, characterized in that In the third mixed solution, the content of the components in the raw materials is: Boron 0.5-1 parts by mass; Carbon powder 1.5-2.7 parts by mass; Aluminum 0.7-1.8 parts by mass; Zirconium 0.3-0.6 parts by mass; 0.5-1.2 parts by mass of boron oxide; 0.2-0.5 parts by mass of zirconium dioxide; 0.2-0.5 parts by mass of barium carbonate.

4. The preparation method according to claim 1, characterized in that After placing the green body in a sintering furnace and heating it to 1350-1520° C. and treating it in nitrogen for 0.5-2 hours, the method further includes: The embryo body is placed in an oxidizing atmosphere at 820-900°C for 10-30 minutes.

5. The preparation method according to claim 1, characterized in that The kaolin is pretreated kaolin, and the processing method of the pretreated kaolin is: The kaolin is acid-washed with an acidic solution, then alkali-washed with an alkaline solution, washed with water, and then dried; Mixing the dried kaolin with boron and titanium to prepare a first mixed powder; The first mixed powder is placed in silane gas and treated at 800-950° C. for 0.5-1.5 hours; Then, the first mixed material powder is placed in the first mixed gas and treated at 870-1020° C. for 0.5-1 h; The first mixed gas includes argon, methane and nitrogen.

6. The preparation method according to claim 5, characterized in that The mass of boron in the first mixed powder is 1.2-3% of the mass of kaolin, and the mass of titanium in the first mixed powder is 0.6-1.5% of the mass of kaolin; The volume of methane in the first mixed gas accounts for 12-25%, and the volume of nitrogen in the first mixed gas accounts for 15-30%.

7. The preparation method according to claim 1, characterized in that The kaolin is pretreated kaolin, and the processing method of the pretreated kaolin is: The kaolin is acid-washed with an acidic solution, then alkali-washed with an alkaline solution, washed with water, and then dried; The dried kaolin is mixed with boron, titanium and silicon diimide to prepare a second mixed powder; The second mixed powder is placed in ammonia and treated at 780-900°C for 0.5-2h; The kaolin is then placed in methane gas and treated at 820-950°C for 0.5-1.5h; Finally, the kaolin is placed in nitrogen and treated at 1460-1550° C. for 10-40 minutes.

8. The preparation method according to claim 7, characterized in that The mass of boron in the second mixed powder is 1-2.5% of the mass of kaolin, the mass of titanium in the second mixed powder is 0.4-1.2% of the mass of kaolin, and the mass of diimino silicon in the second mixed powder is 0.8-3% of the mass of kaolin.

9. An antibacterial and environmentally friendly ceramic, characterized in that: Prepared by the preparation method according to any one of claims 1 to 8.