Porous antioxidant composite porcelain and preparation method thereof

Abstract

The invention relates to the technical field of porcelain, in particular to porous antioxidant composite porcelain and a preparation method thereof, and the preparation method comprises the following steps: weighing the following raw materials in parts by weight: 35-40 parts of clay, 10-15 parts of aluminum oxide, 6-10 parts of an aluminum nitride-doped modified homogenizing agent, 5-9 parts of kaolin and 5-8 parts of a sodium silicate blender. According to the porous anti-oxidation composite porcelain, clay is adopted as a matrix, aluminum oxide and kaolin are added to be matched with an aluminum nitride modified homogenizing agent and a sodium silicate blender, the raw materials are blended and synergized, compression molding is performed, and finally homogenizing sintering is performed, so that the porous anti-oxidation composite porcelain is obtained. The porous performance, the high-temperature oxidation resistance and the mechanical bending strength performance of the obtained composite porcelain are harmoniously improved, and meanwhile, the stability effect of the product is remarkable under different degrees of corrosion conditions.

Description

Technical Field

[0001] The present invention relates to the technical field of porcelain, and in particular to a porous anti-oxidation composite porcelain and a preparation method thereof. Background Art

[0002] Ceramic materials refer to a class of inorganic non-metallic materials made from natural or synthetic compounds through forming and high-temperature sintering. Porcelain products made of ceramics, in order to optimize the porous properties of the product, can easily lead to poor high-temperature oxidation resistance and mechanical bending strength of the product. At the same time, the product has poor stability under different degrees of corrosion conditions, which limits the product's efficiency. Summary of the Invention

[0003] In view of the defects of the prior art, the purpose of the present invention is to provide a porous anti-oxidation composite porcelain and a preparation method thereof to solve the problems raised in the above background technology.

[0004] The present invention solves the technical problem by adopting the following technical solutions:

[0005] The present invention provides a method for preparing a porous anti-oxidation composite porcelain, comprising the following steps:

[0006] Step 1: weigh the following raw materials by weight: 35-40 parts of clay, 10-15 parts of alumina, 6-10 parts of a leveling agent modified by doping with aluminum nitride, 5-9 parts of kaolin, and 5-8 parts of a sodium silicate blending agent;

[0007] Step 2: The raw materials are wet-milled thoroughly, and then pressed into a mold at a pressure of 10 MPa for 1 hour. Finally, the raw materials are homogenized and sintered to obtain a porous antioxidant composite porcelain.

[0008] Preferably, the preparation method of the aluminum nitride-doped modified leveling agent is:

[0009] S01: Preparation of modification solution;

[0010] S02: irradiating aluminum nitride in a proton irradiation box, obtaining irradiated aluminum nitride, and ultrasonically modifying the irradiated aluminum nitride and the modifying liquid in a weight ratio of 4:7, obtaining an aluminum nitride-doped modifying liquid after the ultrasonic modification is completed;

[0011] S03: adding 3-5 parts of aluminum borate whiskers and 2-4 parts of nano-attapulgite to 5-8 parts of sodium alginate solution, and then adding 3-5 parts of urea solution and blending thoroughly, and then filtering and drying to obtain a homogenizing agent;

[0012] S04: The modified liquid and the leveling agent mixed with aluminum nitride are mixed in a weight ratio of 5:3 and ball-milled at a ball-milling speed of 1000-1500 r / min for 2 h. After the ball-milling is completed, the mixture is filtered and dried to obtain the aluminum nitride-doped and modified leveling agent.

[0013] Preferably, the irradiation power of the irradiation treatment in the proton irradiation box is 400-500W, and the irradiation is 1 hour; the ultrasonic power of the ultrasonic modification treatment is 350-400W, and the ultrasonic treatment is 30-40 minutes.

[0014] Preferably, the mass fraction of the sodium alginate solution is 4-7%; the mass fraction of the urea solution is 3-5%.

[0015] Preferably, the preparation method of the modified liquid is:

[0016] S01a: Preheating the silicon carbide fiber to obtain preheated silicon carbide fiber, adding 1-3 parts of silane coupling agent and 3-5 parts of preheated silicon carbide fiber to 5-8 parts of 5% by mass dopamine hydrochloride solution, stirring evenly, to obtain a fiber solution;

[0017] S01b: uniformly blending 3-5 parts of lanthanum boride, 2-4 parts of nano-titanium dioxide, 1-3 parts of perlite, and 5-8 parts of a 5% by mass sodium lignin sulfonate solution to obtain an additive;

[0018] Add the additives to the fiber liquid in a weight ratio of 3:(5-7) and stir thoroughly to obtain a modified liquid.

[0019] Preferably, the silane coupling agent is silane coupling agent KH550; the preheating temperature is 55-60° C., and the preheating time is 1 hour.

[0020] Preferably, the preparation method of the sodium silicate conditioning agent is:

[0021] S11: fully mixing sodium silicate, yttrium nitrate solution and nano-silica sol to obtain sodium silicate solution;

[0022] S12: treating the diatomaceous earth at 150-170° C. for 10 minutes, dispersing the diatomaceous earth in a 5% potassium permanganate solution at 25-30° C. for 1 hour at a dispersion speed of 100-150 r / min, then washing with water, filtering, and drying to obtain pretreated diatomaceous earth;

[0023] S13: Blend 4-7 parts of pretreated diatomaceous earth and 5-8 parts of sodium silicate solution, stir thoroughly, and finally filter and dry to obtain a sodium silicate blending agent.

[0024] Preferably, the mass ratio of the sodium silicate, yttrium nitrate solution and nano-silica sol is (4-6):(7-9):2; wherein the mass fraction of the yttrium nitrate solution is 3-5%.

[0025] Preferably, the specific operating steps of the homogenization sintering process are:

[0026] First, heat to 550-570℃ at a rate of 5-7℃ / min, keep warm for 1h, then heat to 1050-1100℃ at a rate of 4-6℃ / min, keep warm for 20-30min, then heat to 1220-1250℃ at a rate of 2-3℃ / min, keep warm for 2h, and finally air cool to room temperature.

[0027] The present invention also provides a method for preparing porous anti-oxidation composite porcelain and the porous anti-oxidation composite porcelain prepared by the method.

[0028] Compared with the prior art, the present invention has the following beneficial effects:

[0029] The porous anti-oxidation composite porcelain of the present invention uses clay as a matrix, and by adding alumina and kaolin, a leveling agent modified by aluminum nitride, and a sodium silicate blending agent, the raw materials are synergistically blended, followed by molding, and finally homogenization and sintering. The resulting composite porcelain has coordinated improvements in porous properties, high-temperature oxidation resistance, and mechanical bending strength. At the same time, the product has significant stability under different degrees of corrosion conditions.

[0030] The aluminum nitride-doped modified homogenizing agent is prepared by ball-milling the modified liquid mixed with aluminum nitride, wherein the modified liquid mixed with aluminum nitride is irradiated with protons to stimulate its active efficiency, and then ultrasonically modified by the modified liquid. The silicon carbide fiber in the modified liquid is preheated and activated, and then improved by blending with a silane coupling agent and a dopamine hydrochloride solution, and the added additives are used to coordinate the fiber liquid. The additives include lanthanum boride, nano-titanium dioxide and perlite, and a sodium lignin sulfonate solution with a mass fraction of 5%. The liquid is blended and coordinated. Through the improvement of the coordination between the raw materials, lanthanum boride, nano-titanium dioxide and perlite are used as the matrix materials and are blended into the system. The resulting aluminum nitride-doped modified liquid optimizes the performance coordination and performance stability of the product in the system. The leveling agent is improved by blending aluminum borate whiskers, nano-attapulgite, sodium alginate solution and urea solution. The whisker-like aluminum borate whiskers are combined with the lamellar nano-attapulgite to reinforce the system, further enhancing the performance of the product.

[0031] The sodium silicate blending agent is improved by mixing sodium silicate, yttrium nitrate solution and nano-silica sol, and then the pre-treated diatomaceous earth is optimized. The pre-treated diatomaceous earth is thermally improved and then activated and improved with potassium permanganate solution. The sodium silicate blending agent prepared by the co-coordination between the raw materials is further coordinated with the leveling agent modified by doping aluminum nitride in the system, so that the performance of the product is further improved; the homogenization sintering treatment adopts a step-by-step and segmented heat homogenization sintering treatment. Through the step-by-step sintering improvement, the performance coordination and performance stability of the composite porcelain can be further optimized. DETAILED DESCRIPTION

[0032] The following is a clear and complete description of the technical solutions in the embodiments of the present invention in conjunction with specific embodiments. Obviously, the described embodiments are only 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 creative efforts are within the scope of protection of the present invention.

[0033] The method for preparing a porous anti-oxidation composite porcelain of this embodiment comprises the following steps:

[0034] Step 1: weigh the following raw materials by weight: 35-40 parts of clay, 10-15 parts of alumina, 6-10 parts of a leveling agent modified by doping with aluminum nitride, 5-9 parts of kaolin, and 5-8 parts of a sodium silicate blending agent;

[0035] Step 2: The raw materials are wet-milled thoroughly, and then pressed into a mold at a pressure of 10 MPa for 1 hour. Finally, the raw materials are homogenized and sintered to obtain a porous antioxidant composite porcelain.

[0036] The preparation method of the aluminum nitride-doped leveling agent of this embodiment is as follows:

[0037] S01: Preparation of modification solution;

[0038] S02: irradiating aluminum nitride in a proton irradiation box, obtaining irradiated aluminum nitride, and ultrasonically modifying the irradiated aluminum nitride and the modifying liquid in a weight ratio of 4:7, obtaining an aluminum nitride-doped modifying liquid after the ultrasonic modification is completed;

[0039] S03: adding 3-5 parts of aluminum borate whiskers and 2-4 parts of nano-attapulgite to 5-8 parts of sodium alginate solution, and then adding 3-5 parts of urea solution and blending thoroughly, and then filtering and drying to obtain a homogenizing agent;

[0040] S04: The modified liquid and the leveling agent mixed with aluminum nitride are mixed in a weight ratio of 5:3 and ball-milled at a ball-milling speed of 1000-1500 r / min for 2 h. After the ball-milling is completed, the mixture is filtered and dried to obtain the aluminum nitride-doped and modified leveling agent.

[0041] In the proton irradiation box of this embodiment, the irradiation power of the irradiation treatment is 400-500W, and the irradiation time is 1 hour; the ultrasonic power of the ultrasonic modification treatment is 350-400W, and the ultrasonic treatment time is 30-40 minutes.

[0042] The mass fraction of the sodium alginate solution in this embodiment is 4-7%; the mass fraction of the urea solution is 3-5%.

[0043] The preparation method of the modified liquid of this embodiment is:

[0044] S01a: Preheating the silicon carbide fiber to obtain preheated silicon carbide fiber, adding 1-3 parts of silane coupling agent and 3-5 parts of preheated silicon carbide fiber to 5-8 parts of 5% by mass dopamine hydrochloride solution, stirring evenly, to obtain a fiber solution;

[0045] S01b: uniformly blending 3-5 parts of lanthanum boride, 2-4 parts of nano-titanium dioxide, 1-3 parts of perlite, and 5-8 parts of a 5% by mass sodium lignin sulfonate solution to obtain an additive;

[0046] Add the additives to the fiber liquid in a weight ratio of 3:(5-7) and stir thoroughly to obtain a modified liquid.

[0047] The silane coupling agent in this embodiment is silane coupling agent KH550; the preheating temperature is 55-60° C., and the preheating time is 1 hour.

[0048] The preparation method of the sodium silicate blending agent of the present embodiment is:

[0049] S11: fully mixing sodium silicate, yttrium nitrate solution and nano-silica sol to obtain sodium silicate solution;

[0050] S12: treating the diatomaceous earth at 150-170° C. for 10 minutes, dispersing the diatomaceous earth in a 5% potassium permanganate solution at 25-30° C. for 1 hour at a dispersion speed of 100-150 r / min, then washing with water, filtering, and drying to obtain pretreated diatomaceous earth;

[0051] S13: Blend 4-7 parts of pretreated diatomaceous earth and 5-8 parts of sodium silicate solution, stir thoroughly, and finally filter and dry to obtain a sodium silicate blending agent.

[0052] The mass ratio of sodium silicate, yttrium nitrate solution and nano-silica sol in this embodiment is (4-6):(7-9):2; the mass fraction of yttrium nitrate solution is 3-5%.

[0053] The specific steps of the homogenization sintering process in this embodiment are:

[0054] First, heat to 550-570℃ at a rate of 5-7℃ / min, keep warm for 1h, then heat to 1050-1100℃ at a rate of 4-6℃ / min, keep warm for 20-30min, then heat to 1220-1250℃ at a rate of 2-3℃ / min, keep warm for 2h, and finally air cool to room temperature.

[0055] The porous anti-oxidation composite porcelain prepared by the method for preparing the porous anti-oxidation composite porcelain of this embodiment.

[0056] Example 1.

[0057] The method for preparing a porous anti-oxidation composite porcelain of this embodiment comprises the following steps:

[0058] Step 1: weigh the following raw materials by weight: 35 parts of clay, 10 parts of alumina, 6 parts of a leveling agent modified by doping with aluminum nitride, 5 parts of kaolin, and 5 parts of a sodium silicate blending agent;

[0059] Step 2: The raw materials are wet-milled thoroughly, and then pressed into a mold at a pressure of 10 MPa for 1 hour. Finally, the raw materials are homogenized and sintered to obtain a porous antioxidant composite porcelain.

[0060] The preparation method of the aluminum nitride-doped leveling agent of this embodiment is as follows:

[0061] S01: Preparation of modification solution;

[0062] S02: irradiating aluminum nitride in a proton irradiation box, obtaining irradiated aluminum nitride, and ultrasonically modifying the irradiated aluminum nitride and the modifying liquid in a weight ratio of 4:7, obtaining an aluminum nitride-doped modifying liquid after the ultrasonic modification is completed;

[0063] S03: adding 3-5 parts of aluminum borate whiskers and 2 parts of nano-attapulgite to 5 parts of sodium alginate solution, and then adding 3 parts of urea solution and blending thoroughly, and then filtering and drying to obtain a homogenizing agent;

[0064] S04: The modified liquid and the leveling agent mixed with aluminum nitride are mixed in a weight ratio of 5:3 and ball-milled at a speed of 1000 r / min for 2 h. After the ball milling is completed, the mixture is filtered and dried to obtain the aluminum nitride-doped and modified leveling agent.

[0065] In the proton irradiation box of this embodiment, the irradiation power of the irradiation treatment is 400W, and the irradiation time is 1 hour; the ultrasonic power of the ultrasonic modification treatment is 350W, and the ultrasonic treatment time is 30 minutes.

[0066] The mass fraction of the sodium alginate solution in this embodiment is 4%; the mass fraction of the urea solution is 3%.

[0067] The preparation method of the modified liquid of this embodiment is:

[0068] S01a: Preheating the silicon carbide fiber to obtain preheated silicon carbide fiber, adding 1 part of silane coupling agent and 3 parts of preheated silicon carbide fiber to 5 parts of 5% by mass dopamine hydrochloride solution, stirring evenly, to obtain a fiber solution;

[0069] S01b: 3 parts of lanthanum boride, 2 parts of nano-titanium dioxide, 1 part of perlite, and 5 parts of 5% by mass sodium lignin sulfonate solution are uniformly blended to obtain an additive;

[0070] Add the additives to the fiber liquid at a weight ratio of 3:5 and stir thoroughly to obtain a modified liquid.

[0071] The silane coupling agent used in this embodiment is silane coupling agent KH550; the preheating temperature is 55° C., and the preheating time is 1 hour.

[0072] The preparation method of the sodium silicate blending agent of the present embodiment is:

[0073] S11: fully mixing sodium silicate, yttrium nitrate solution and nano-silica sol to obtain sodium silicate solution;

[0074] S12: treating the diatomaceous earth at 150° C. for 10 minutes, dispersing the diatomaceous earth in a 5% potassium permanganate solution at 25° C. for 1 hour at a dispersion speed of 100 r / min, then washing with water, filtering, and drying to obtain pretreated diatomaceous earth;

[0075] S13: Blend 4 parts of pretreated diatomaceous earth and 5 parts of sodium silicate solution, stir thoroughly, and finally filter and dry to obtain a sodium silicate blending agent.

[0076] In this embodiment, the mass ratio of sodium silicate, yttrium nitrate solution and nano-silica sol is 4:7:2; the mass fraction of yttrium nitrate solution is 3%.

[0077] The specific steps of the homogenization sintering process in this embodiment are:

[0078] First, heat to 550℃ at a rate of 5℃ / min, keep warm for 1h, then heat to 1050℃ at a rate of 4℃ / min, keep warm for 20min, then heat to 1220℃ at a rate of 2℃ / min, keep warm for 2h, and finally air cool to room temperature.

[0079] The porous anti-oxidation composite porcelain prepared by the method for preparing the porous anti-oxidation composite porcelain of this embodiment.

[0080] Example 2.

[0081] The method for preparing a porous anti-oxidation composite porcelain of this embodiment comprises the following steps:

[0082] Step 1: weigh the following raw materials according to weight: 40 parts of clay, 15 parts of alumina, 10 parts of a leveling agent modified by doping with aluminum nitride, 9 parts of kaolin, and 8 parts of a sodium silicate blending agent;

[0083] Step 2: The raw materials are wet-milled thoroughly, and then pressed into a mold at a pressure of 10 MPa for 1 hour. Finally, the raw materials are homogenized and sintered to obtain a porous antioxidant composite porcelain.

[0084] The preparation method of the aluminum nitride-doped leveling agent of this embodiment is as follows:

[0085] S01: Preparation of modification solution;

[0086] S02: irradiating aluminum nitride in a proton irradiation box, obtaining irradiated aluminum nitride, and ultrasonically modifying the irradiated aluminum nitride and the modifying liquid in a weight ratio of 4:7, obtaining an aluminum nitride-doped modifying liquid after the ultrasonic modification is completed;

[0087] S03: adding 5 parts of aluminum borate whiskers and 4 parts of nano-attapulgite to 8 parts of sodium alginate solution, and then adding 5 parts of urea solution and blending thoroughly, and then filtering and drying to obtain a homogenizing agent;

[0088] S04: The modified liquid and the leveling agent mixed with aluminum nitride are mixed in a weight ratio of 5:3 and ball-milled at a ball-milling speed of 1500 r / min for 2 h. After the ball-milling is completed, the mixture is filtered and dried to obtain the leveling agent modified by aluminum nitride.

[0089] In the proton irradiation box of this embodiment, the irradiation power of the irradiation treatment is 500W, and the irradiation time is 1 hour; the ultrasonic power of the ultrasonic modification treatment is 400W, and the ultrasonic treatment time is 40 minutes.

[0090] The mass fraction of the sodium alginate solution in this embodiment is 7%; the mass fraction of the urea solution is 5%.

[0091] The preparation method of the modified liquid of this embodiment is:

[0092] S01a: Preheating the silicon carbide fiber to obtain preheated silicon carbide fiber, adding 3 parts of silane coupling agent and 5 parts of preheated silicon carbide fiber to 8 parts of 5% by mass dopamine hydrochloride solution, stirring evenly, to obtain fiber liquid;

[0093] S01b: 5 parts of lanthanum boride, 4 parts of nano-titanium dioxide, 3 parts of perlite, and 8 parts of 5% by mass sodium lignin sulfonate solution are uniformly blended to obtain an additive;

[0094] Add the additives to the fiber liquid in a weight ratio of 3:7 and stir thoroughly to obtain a modified liquid.

[0095] The silane coupling agent in this embodiment is silane coupling agent KH550; the preheating temperature is 60° C., and the preheating is performed for 1 hour.

[0096] The preparation method of the sodium silicate blending agent of the present embodiment is:

[0097] S11: fully mixing sodium silicate, yttrium nitrate solution and nano-silica sol to obtain sodium silicate solution;

[0098] S12: treating the diatomaceous earth at 170° C. for 10 minutes, dispersing the diatomaceous earth in a 5% potassium permanganate solution at 30° C. for 1 hour at a dispersion speed of 150 r / min, then washing with water, filtering, and drying to obtain pretreated diatomaceous earth;

[0099] S13: 7 parts of pretreated diatomaceous earth and 8 parts of sodium silicate solution are mixed and stirred thoroughly, and finally filtered and dried to obtain a sodium silicate blending agent.

[0100] In this embodiment, the mass ratio of sodium silicate, yttrium nitrate solution and nano-silica sol is 6:9:2; the mass fraction of yttrium nitrate solution is 5%.

[0101] The specific steps of the homogenization sintering process in this embodiment are:

[0102] First, heat to 570℃ at a rate of 7℃ / min, keep warm for 1h, then heat to 1100℃ at a rate of 6℃ / min, keep warm for 30min, then heat to 1250℃ at a rate of 3℃ / min, keep warm for 2h, and finally air cool to room temperature.

[0103] The porous anti-oxidation composite porcelain prepared by the method for preparing the porous anti-oxidation composite porcelain of this embodiment.

[0104] Example 3.

[0105] The method for preparing a porous anti-oxidation composite porcelain of this embodiment comprises the following steps:

[0106] Step 1: weigh the following raw materials according to weight: 37.5 parts of clay, 12.5 parts of alumina, 8 parts of a leveling agent modified by doping with aluminum nitride, 7 parts of kaolin, and 6.5 parts of a sodium silicate blending agent;

[0107] Step 2: The raw materials are wet-milled thoroughly, and then pressed into a mold at a pressure of 10 MPa for 1 hour. Finally, the raw materials are homogenized and sintered to obtain a porous antioxidant composite porcelain.

[0108] The preparation method of the aluminum nitride-doped leveling agent of this embodiment is as follows:

[0109] S01: Preparation of modification solution;

[0110] S02: irradiating aluminum nitride in a proton irradiation box, obtaining irradiated aluminum nitride, and ultrasonically modifying the irradiated aluminum nitride and the modifying liquid in a weight ratio of 4:7, obtaining an aluminum nitride-doped modifying liquid after the ultrasonic modification is completed;

[0111] S03: adding 4 parts of aluminum borate whiskers and 3 parts of nano-attapulgite to 6.5 parts of sodium alginate solution, and then adding 4 parts of urea solution and blending thoroughly, and then filtering and drying to obtain a homogenizing agent;

[0112] S04: The modified liquid and the leveling agent mixed with aluminum nitride are mixed in a weight ratio of 5:3, and the mixture is ball-milled at a speed of 1250 r / min for 2 h. After the ball milling is completed, the mixture is filtered and dried to obtain the leveling agent modified by doping with aluminum nitride.

[0113] In the proton irradiation box of this embodiment, the irradiation power of the irradiation treatment is 450W, and the irradiation time is 1 hour; the ultrasonic power of the ultrasonic modification treatment is 370W, and the ultrasonic treatment time is 35 minutes.

[0114] The mass fraction of the sodium alginate solution in this embodiment is 5.5%; the mass fraction of the urea solution is 4%.

[0115] The preparation method of the modified liquid of this embodiment is:

[0116] S01a: Preheating the silicon carbide fiber to obtain preheated silicon carbide fiber, adding 2 parts of silane coupling agent and 4 parts of preheated silicon carbide fiber to 6.5 parts of 5% by mass dopamine hydrochloride solution, stirring evenly, to obtain fiber liquid;

[0117] S01b: 4 parts of lanthanum boride, 3 parts of nano-titanium dioxide, 2 parts of perlite, and 6.5 parts of 5% by mass sodium lignin sulfonate solution are uniformly blended to obtain an additive;

[0118] Add the additives to the fiber liquid in a weight ratio of 3:6 and stir thoroughly to obtain a modified liquid.

[0119] The silane coupling agent used in this embodiment is silane coupling agent KH550; the preheating temperature is 57.5° C., and the preheating time is 1 hour.

[0120] The preparation method of the sodium silicate blending agent of the present embodiment is:

[0121] S11: fully mixing sodium silicate, yttrium nitrate solution and nano-silica sol to obtain sodium silicate solution;

[0122] S12: The diatomaceous earth is first treated at 160° C. for 10 minutes. After the treatment, the diatomaceous earth is dispersed in a 5% potassium permanganate solution at 27.5° C. for 1 hour at a dispersion speed of 125 r / min, and then washed with water, filtered, and dried to obtain pretreated diatomaceous earth;

[0123] S13: 5.5 parts of pretreated diatomaceous earth and 6.5 parts of sodium silicate solution are mixed and stirred thoroughly, and finally filtered and dried to obtain a sodium silicate blending agent.

[0124] In this embodiment, the mass ratio of sodium silicate, yttrium nitrate solution and nano-silica sol is 5:8:2; the mass fraction of yttrium nitrate solution is 4%.

[0125] The specific steps of the homogenization sintering process in this embodiment are:

[0126] First, heat to 560℃ at a rate of 6℃ / min, keep warm for 1h, then heat to 1075℃ at a rate of 5℃ / min, keep warm for 25min, then heat to 1235℃ at a rate of 2.5℃ / min, keep warm for 2h, and finally air cool to room temperature.

[0127] The porous anti-oxidation composite porcelain prepared by the method for preparing the porous anti-oxidation composite porcelain of this embodiment.

[0128] Comparative Example 1.

[0129] The difference from Example 3 is that no leveling agent modified by doped aluminum nitride is added.

[0130] Comparative Example 2.

[0131] The difference from Example 3 is that no modified liquid doped with aluminum nitride is added in the preparation of the aluminum nitride-doped modified leveling agent.

[0132] Comparative Example 3.

[0133] The difference from Example 3 is that no irradiated aluminum nitride is added in the preparation of the modified solution blended with aluminum nitride.

[0134] Comparative Example 4.

[0135] The difference from Example 3 is that no modifying liquid is added in the preparation of the modifying liquid mixed with aluminum nitride.

[0136] Comparative Example 5.

[0137] The difference from Example 3 is that no additives are added to the modified liquid.

[0138] Comparative Example 6.

[0139] The difference from Example 3 is that no lanthanum boride or nano-titanium dioxide is added to the additives.

[0140] Comparative Example 7.

[0141] The difference from Example 3 is that no fiber liquid is added to the modified liquid.

[0142] Comparative Example 8.

[0143] The difference from Example 3 is that no preheated silicon carbide fiber is added to the fiber liquid.

[0144] Comparative Example 9.

[0145] The difference from Example 3 is that no leveling agent is added during the preparation of the leveling agent modified by doping aluminum nitride.

[0146] Comparative Example 10.

[0147] The difference from Example 3 is that no aluminum borate whiskers or nano-attapulgite are added to the leveling agent.

[0148] Comparative Example 11.

[0149] The difference from Example 3 is that no sodium silicate blending agent is added.

[0150] Comparative Example 12.

[0151] The difference from Example 3 is that no pretreated diatomaceous earth is added in the preparation of the sodium silicate conditioning agent.

[0152] Comparative Example 13.

[0153] The difference from Example 3 is that no sodium silicate solution is added during the preparation of the sodium silicate conditioning agent.

[0154] Comparative Example 14.

[0155] The difference from Example 3 is that in the homogenization sintering treatment, the temperature was not raised to 1075°C at a rate of 5°C / min and kept at that temperature for 25 minutes. Instead, the temperature was directly raised from 560°C to 1235°C at a rate of 2.5°C / min, while other conditions remained unchanged.

[0156] The products of Examples 1 to 3 and Comparative Examples 1 to 14 were subjected to conventional performance tests to test the porous properties, high-temperature oxidation resistance, and mechanical flexural strength of the products. At the same time, the products were tested under different degrees of corrosion conditions (placed under 2% hydrochloric acid mist for 24 hours and placed under 8% hydrochloric acid mist for 24 hours). The test results are as follows:

[0157]

[0158]

[0159]

[0160]

[0161] It can be seen from Comparative Examples 1 to 14 and Examples 1 to 3 that;

[0162] The product of Example 3 has excellent porosity, and at the same time, the product has excellent high-temperature oxidation resistance and mechanical bending strength performance, and the three can be improved in a coordinated manner. In addition, the product has excellent performance stability under different degrees of corrosion conditions;

[0163] From Comparative Examples 1 to 14 and Example 3, it can be seen that the performance of the products without adding either the leveling agent modified by doped aluminum nitride or the sodium silicate blending agent showed a significant deterioration trend. The synergistic effect of the two was the most obvious.

[0164] The performance of the products showed varying degrees of deterioration when no aluminum nitride-doped modifying liquid was added to the preparation of the aluminum nitride-doped modifying liquid, no irradiated aluminum nitride was added to the preparation of the aluminum nitride-doped modifying liquid, no modifying liquid was added to the preparation of the aluminum nitride-doped modifying liquid, no additives were added to the modifying liquid, no lanthanum boride or nano-titanium dioxide was added to the additives, no fiber liquid was added to the modifying liquid, no preheated silicon carbide fiber was added to the fiber liquid, no leveling agent was added to the preparation of the aluminum nitride-doped modifying leveling agent, and no aluminum borate whiskers or nano-attapulgite were added to the leveling agent.

[0165] The modified liquid prepared by combining the fiber liquid obtained by the specific method of the present invention with the additive, and the modified liquid prepared by combining the modified liquid with the irradiated aluminum nitride and the aluminum nitride-doped modified leveling agent with the leveling agent, have the most significant performance effects. The effects of other methods are not as obvious as those of the present invention.

[0166] When no pretreated diatomaceous earth or sodium silicate liquid was added in the preparation of the sodium silicate conditioning agent, the performance of the product showed a trend of deterioration. At the same time, during the homogenization sintering treatment, the temperature was not raised to 1075°C at a rate of 5°C / min and kept warm for 25 minutes. The performance of the product also showed a trend of deterioration. The sodium silicate conditioning agent obtained by the specific method of the present invention and the specific homogenization sintering treatment of the present invention had the most significant product performance effect.

[0167] It will be apparent to those skilled in the art that the present invention is not limited to the details of the exemplary embodiments described above and that the invention can be embodied in other specific forms without departing from the spirit or essential characteristics of the invention. Therefore, the embodiments should be considered in all respects as illustrative and non-restrictive, and the scope of the invention is defined by the appended claims rather than the foregoing description, and it is intended that all variations that come within the meaning and range of equivalents of the claims be embraced therein.

[0168] In addition, it should be understood that although this specification is described in terms of implementation methods, not every implementation method contains only one independent technical solution. This narrative method of the specification is only for the sake of clarity. Those skilled in the art should regard the specification as a whole. The technical solutions in each embodiment can also be appropriately combined to form other implementation methods that can be understood by those skilled in the art.

Claims

1. A method for preparing porous antioxidant composite porcelain, characterized in that: The following steps are involved: Step 1: weigh the following raw materials by weight: 35-40 parts of clay, 10-15 parts of alumina, 6-10 parts of a leveling agent modified by doping with aluminum nitride, 5-9 parts of kaolin, and 5-8 parts of a sodium silicate blending agent; Step 2: The raw materials are wet-milled thoroughly, and then pressed into a mold at a pressure of 10 MPa for 1 hour. Finally, the mold is homogenized and sintered to obtain a porous antioxidant composite porcelain.

2. The method for preparing a porous anti-oxidation composite porcelain according to claim 1, characterized in that: The preparation method of the aluminum nitride-doped modified leveling agent is as follows: S01: Preparation of modification solution; S02: irradiating aluminum nitride in a proton irradiation box, obtaining irradiated aluminum nitride, and ultrasonically modifying the irradiated aluminum nitride and the modifying liquid in a weight ratio of 4:7, obtaining an aluminum nitride-doped modifying liquid after the ultrasonic modification is completed; S03: adding 3-5 parts of aluminum borate whiskers and 2-4 parts of nano-attapulgite to 5-8 parts of sodium alginate solution, and then adding 3-5 parts of urea solution and blending thoroughly, and then filtering and drying to obtain a homogenizing agent; S04: The modified liquid and the leveling agent mixed with aluminum nitride are mixed in a weight ratio of 5:3 and ball-milled at a ball-milling speed of 1000-1500 r / min for 2 h. After the ball-milling is completed, the mixture is filtered and dried to obtain the aluminum nitride-doped and modified leveling agent.

3. The method for preparing a porous anti-oxidation composite porcelain according to claim 2, characterized in that: The irradiation power of the proton irradiation box is 400-500W, and the irradiation time is 1 hour; the ultrasonic power of the ultrasonic modification treatment is 350-400W, and the ultrasonic treatment time is 30-40 minutes.

4. The method for preparing a porous anti-oxidation composite porcelain according to claim 2, characterized in that: The mass fraction of the sodium alginate solution is 4-7%; the mass fraction of the urea solution is 3-5%.

5. The method for preparing a porous anti-oxidation composite porcelain according to claim 2, characterized in that: The preparation method of the modified liquid is: S01a: Preheating the silicon carbide fiber to obtain preheated silicon carbide fiber, adding 1-3 parts of silane coupling agent and 3-5 parts of preheated silicon carbide fiber to 5-8 parts of 5% by mass dopamine hydrochloride solution, stirring evenly, to obtain a fiber solution; S01b: uniformly blending 3-5 parts of lanthanum boride, 2-4 parts of nano-titanium dioxide, 1-3 parts of perlite, and 5-8 parts of a 5% by mass sodium lignin sulfonate solution to obtain an additive; Add the additives to the fiber liquid in a weight ratio of 3:(5-7) and stir thoroughly to obtain a modified liquid.

6. The method for preparing a porous anti-oxidation composite porcelain according to claim 5, characterized in that: The silane coupling agent is silane coupling agent KH550; the preheating temperature is 55-60° C., and the preheating time is 1 hour.

7. The method for preparing a porous anti-oxidation composite porcelain according to claim 1, characterized in that: The preparation method of the sodium silicate conditioning agent is: S11: fully mixing sodium silicate, yttrium nitrate solution and nano-silica sol to obtain sodium silicate solution; S12: treating the diatomaceous earth at 150-170° C. for 10 minutes, dispersing the diatomaceous earth in a 5% potassium permanganate solution at 25-30° C. for 1 hour at a dispersion speed of 100-150 r / min, then washing with water, filtering, and drying to obtain pretreated diatomaceous earth; S13: Blend 4-7 parts of pretreated diatomaceous earth and 5-8 parts of sodium silicate solution, stir thoroughly, and finally filter and dry to obtain a sodium silicate blending agent.

8. The method for preparing a porous anti-oxidation composite porcelain according to claim 7, characterized in that: The mass ratio of the sodium silicate, yttrium nitrate solution and nano-silica sol is (4-6):(7-9):2; wherein the mass fraction of the yttrium nitrate solution is 5-8%.

9. The method for preparing a porous anti-oxidation composite porcelain according to claim 1, characterized in that: The specific operating steps of the homogenization sintering process are: First, heat to 550-570℃ at a rate of 5-7℃ / min, keep warm for 1h, then heat to 1050-1100℃ at a rate of 4-6℃ / min, keep warm for 20-30min, then heat to 1220-1250℃ at a rate of 2-3℃ / min, keep warm for 2h, and finally air cool to room temperature.

10. A porous antioxidant composite porcelain prepared by the method for preparing a porous antioxidant composite porcelain according to any one of claims 1 to 9.

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