A high-temperature-resistant insulating ceramic product and a preparation method thereof
Patent Information
- Application Number
- CN202610967888.9
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2026-07-01
- Publication Date
- 2026-09-18
- Estimated Expiration
- 2046-07-01
AI Technical Summary
德化地区以生产高品质的日用陶瓷和工艺陶瓷闻名于世,随着日用陶瓷的不断发展,在对陶瓷的绝缘性提出更高的要求,为了提升陶瓷的绝缘性,容易降低产品的易洁、力学性能,同时产品的耐高温、耐不同腐蚀稳定性降低,产品的综合协调性差,限制了产品的使用效率
本发明绝缘陶瓷制品采用陶瓷基料配合改性碳化硅剂、二氧化硅填充剂进行协配调和,制成的陶瓷制品绝缘性、易洁、力学性能协调性增进,同时产品的耐高温、耐不同腐蚀稳定性优异,产品的综合协调性效果显著。
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Abstract
Description
Technical Field
[0001] This invention relates to the field of insulating ceramics technology, specifically to a high-temperature resistant insulating ceramic product and its preparation method. Background Technology
[0002] Ceramics are widely used in construction, daily life, and many other fields. Dehua region is world-renowned for producing high-quality daily-use ceramics and art ceramics. With the continuous development of daily-use ceramics, higher requirements are being placed on the insulation properties of ceramics. However, improving the insulation of ceramics can easily reduce the ease of cleaning and mechanical properties of the product. At the same time, the product's high-temperature resistance and resistance to various corrosions decrease, resulting in poor overall product coordination and limiting its efficiency. Based on this, the present invention provides further improvements. Summary of the Invention
[0003] In view of the deficiencies of the prior art, the purpose of this invention is to provide a high-temperature resistant insulating ceramic product and its preparation method, so as to solve the problems mentioned in the background art.
[0004] The present invention solves the technical problem by adopting the following technical solution: This invention provides a high-temperature resistant insulating ceramic product, comprising the following raw materials in parts by weight: 70-90 parts ceramic matrix, 5-12 parts modified silicon carbide agent, 6-10 parts silica filler, 1-3 parts dispersant, and 2-5 parts binder.
[0005] Preferably, the ceramic matrix comprises the following raw materials in parts by weight: 25-30 parts illite powder, 15-20 parts potassium feldspar powder, 10-15 parts quartz, and 5-8 parts microsilica powder; the dispersant is sodium hexametaphosphate; and the binder is carboxymethyl cellulose.
[0006] Preferably, the preparation method of the modified silicon carbide agent includes the following steps: S1, heat-treat silicon carbide at 110-120℃ for 1 hour, then air-cool to room temperature to obtain heat-treated silicon carbide; S2, heat-treated silicon carbide and the modification liquid are subjected to ultrasonic modification treatment at a weight ratio of 3:(5-7), ultrasonic power of 350-450W, ultrasonic treatment for 1 hour, and after ultrasonic treatment, the modified silicon carbide agent is obtained by filtration and drying.
[0007] Preferably, the modified liquid is prepared by: A 2-5% (w / w) solution of dopamine hydrochloride, silane coupling agent KH560, and a 75-85% (w / w) aqueous ethanol solution were prepared in a weight ratio of (3-5):2:(8-10) to obtain a dopamine hydrochloride solution. 2-4 parts by weight of yttrium oxide, 1-3 parts by weight of carbon nanotubes, 3-5 parts by weight of nano-alumina, and 4-7 parts by weight of the dopamine hydrochloride solution were thoroughly mixed to obtain a modified solution.
[0008] The modified silicon carbide agent is made by thermally modifying silicon carbide, followed by ultrasonic modification treatment with a modified liquid. The modified liquid contains hydrochloric acid dopamine solution, silane coupling agent KH560 and ethanol aqueous solution, which are blended and coordinated. At the same time, yttrium oxide, carbon nanotubes and nano alumina are added for further improvement. The resulting modified silicon carbide agent optimizes the product's coordination and performance stability in the system.
[0009] Preferably, the method for preparing the silica filler is as follows: S11, add silica to a sodium lignosulfonate solution with a mass fraction of 2-5% and 4-7 times the total weight of silica and stir until homogeneous to obtain a silica dispersion; S12, the silica dispersion and the filling liquid are mixed and ball-milled at a weight ratio of (8-11):5. After ball milling, the mixture is filtered and dried to obtain the silica filler.
[0010] Preferably, the filling liquid is prepared by: S121, add 1-3 parts by weight of lanthanum nitrate solution with a mass fraction of 4% and 1-2 parts by weight of silane coupling agent KH550 to 3-5 parts by weight of chitosan solution with a mass fraction of 2-5%, and mix evenly to obtain modified chitosan solution. S122, 2-5 parts by weight of kaolin, 1-3 parts by weight of aluminum borate whiskers and 5-8 parts by weight of modified chitosan liquid are thoroughly mixed to obtain the first filler liquid; 2-5 parts by weight of basalt fiber, 1-3 parts by weight of calcined talc powder and 3-5 parts by weight of zirconium silicate are thoroughly mixed to obtain the second filler. S123, the first filling liquid and the second filling agent are mixed and ball-milled at a weight ratio of (5-8):3 to obtain the filling liquid.
[0011] The silica filler is made by dispersing silica in a sodium lignosulfonate solution, then blending and ball milling the filler solution. Kaolin and aluminum borate whiskers in the filler solution are used as the matrix, and then blended with modified chitosan solution. The modified chitosan solution is made by blending and optimizing chitosan solution, lanthanum nitrate solution and silane coupling agent. Basalt fiber, calcined talc powder and zirconium silicate are added to further combine and make a second filler. The filler solution obtained by the synergistic optimization of the first filler solution and the second filler solution further improves the functionality of the product system, thereby further optimizing the performance of the product.
[0012] Preferably, the ceramic product further includes 3-6 parts of modified cerium dioxide agent, and the modified cerium dioxide agent is prepared by: Mix 2-3 parts by weight of silane coupling agent KH550, 3-5 parts by weight of 75-85% aqueous ethanol solution and 0.5-1 parts by weight of deionized water, and stir at 300-500 r / min at 45-48℃ for 30 min to pre-hydrolyze and obtain silane hydrolysate. Mix 4-5 parts by weight of cerium dioxide, 3-4 parts by weight of titanium dioxide, 2-3 parts by weight of lutetium oxide, 8-10 parts by weight of silane hydrolysate, and 10-15 parts by weight of anhydrous ethanol, and stir the mixture at 65-67°C and 400-500 r / min for 2 h to obtain a blend. Add 20-30 parts by weight of Tris buffer to the blending agent to adjust the pH of the system to 8.0-8.5, then add 0.8-1 parts by weight of dopamine hydrochloride, and stir the mixture at 350-370 r / min at 28-30℃ for 4-5 h. After the reaction is completed, filter the mixture, wash it three times with anhydrous ethanol, and air dry it to obtain the modified cerium dioxide agent.
[0013] The modified cerium dioxide agent is prepared by mixing cerium dioxide, titanium dioxide, and lutetium oxide with silane hydrolysate, and further optimizing the mixture with Tris buffer and dopamine hydrochloride. Through the synergistic improvement of the raw materials, the modified cerium dioxide agent further enhances the functionality of the product in the system, thereby further improving and optimizing the product's performance.
[0014] Preferably, the pH of the Tris buffer solution is 8.5-8.7 and the mass concentration is 0.05-0.07 mol / L.
[0015] The present invention also provides a method for preparing high-temperature resistant insulating ceramic products, comprising the following steps: weighing raw materials according to the weight parts, wet ball milling the raw materials thoroughly, then molding them in a mold, and then sintering them to obtain high-temperature resistant insulating ceramic products.
[0016] Preferably, the specific steps of the sintering process are as follows: For S11a, first heat to 300℃ at a rate of 2-3℃ / min, hold for 10-15min, then heat to 850-900℃ at a rate of 3-4℃ / min, hold for 35-45min. S11b, then raise the temperature to 1100-1200℃ at a rate of 1.5-2.5℃ / min, hold for 1 hour, then raise the temperature to 1300℃ at a rate of 0.5-1.5℃ / min, hold for 2-3 hours; S11c, then naturally cooled to 800℃, and finally cooled to room temperature at 3-5℃ / min.
[0017] By employing multiple heating and cooling processes and adjusting the sintering step by step, homogenized sintering is achieved, resulting in ceramic products with superior density and further improved product performance.
[0018] Compared with the prior art, the present invention has the following beneficial effects: The insulating ceramic products of this invention are formulated and blended with ceramic base material, modified silicon carbide agent, and silicon dioxide filler. The resulting ceramic products have improved insulation, easy cleaning, and mechanical properties. At the same time, the products have excellent high temperature resistance and resistance to different corrosions, and the overall coordination effect of the products is significant. Detailed Implementation
[0019] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to specific examples. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.
[0020] This embodiment of a high-temperature resistant insulating ceramic product comprises the following raw materials in parts by weight: 70-90 parts ceramic matrix, 5-12 parts modified silicon carbide agent, 6-10 parts silica filler, 1-3 parts dispersant, and 2-5 parts binder.
[0021] Preferably, the ceramic matrix comprises the following raw materials in parts by weight: 25-30 parts illite powder, 15-20 parts potassium feldspar powder, 10-15 parts quartz, and 5-8 parts microsilica powder; the dispersant is sodium hexametaphosphate; and the binder is carboxymethyl cellulose.
[0022] The preparation method of the modified silicon carbide agent in this embodiment includes the following steps: S1, heat-treat silicon carbide at 110-120℃ for 1 hour, then air-cool to room temperature to obtain heat-treated silicon carbide; S2, heat-treated silicon carbide and the modification liquid are subjected to ultrasonic modification treatment at a weight ratio of 3:(5-7), ultrasonic power of 350-450W, ultrasonic treatment for 1 hour, and after ultrasonic treatment, the modified silicon carbide agent is obtained by filtration and drying.
[0023] The preparation method of the modified liquid in this embodiment is as follows: A 2-5% (w / w) solution of dopamine hydrochloride, silane coupling agent KH560, and a 75-85% (w / w) aqueous ethanol solution were prepared in a weight ratio of (3-5):2:(8-10) to obtain a dopamine hydrochloride solution. 2-4 parts by weight of yttrium oxide, 1-3 parts by weight of carbon nanotubes, 3-5 parts by weight of nano-alumina, and 4-7 parts by weight of the dopamine hydrochloride solution were thoroughly mixed to obtain a modified solution.
[0024] The method for preparing the silica filler in this embodiment is as follows: S11, add silica to a sodium lignosulfonate solution with a mass fraction of 2-5% and 4-7 times the total weight of silica and stir until homogeneous to obtain a silica dispersion; S12, the silica dispersion and the filling liquid are mixed and ball-milled at a weight ratio of (8-11):5. After ball milling, the mixture is filtered and dried to obtain the silica filler.
[0025] The preparation method of the filling liquid in this embodiment is as follows: S121, add 1-3 parts by weight of lanthanum nitrate solution with a mass fraction of 4% and 1-2 parts by weight of silane coupling agent KH550 to 3-5 parts by weight of chitosan solution with a mass fraction of 2-5%, and mix evenly to obtain modified chitosan solution. S122, 2-5 parts by weight of kaolin, 1-3 parts by weight of aluminum borate whiskers and 5-8 parts by weight of modified chitosan liquid are thoroughly mixed to obtain the first filler liquid; 2-5 parts by weight of basalt fiber, 1-3 parts by weight of calcined talc powder and 3-5 parts by weight of zirconium silicate are thoroughly mixed to obtain the second filler. S123, the first filling liquid and the second filling agent are mixed and ball-milled at a weight ratio of (5-8):3 to obtain the filling liquid.
[0026] The ceramic product of this embodiment also includes 3-6 parts of modified cerium dioxide agent, and the preparation method of the modified cerium dioxide agent is as follows: Mix 2-3 parts by weight of silane coupling agent KH550, 3-5 parts by weight of 75-85% aqueous ethanol solution and 0.5-1 parts by weight of deionized water, and stir at 300-500 r / min at 45-48℃ for 30 min to pre-hydrolyze and obtain silane hydrolysate. Mix 4-5 parts by weight of cerium dioxide, 3-4 parts by weight of titanium dioxide, 2-3 parts by weight of lutetium oxide, 8-10 parts by weight of silane hydrolysate, and 10-15 parts by weight of anhydrous ethanol, and stir the mixture at 65-67°C and 400-500 r / min for 2 h to obtain a blend. Add 20-30 parts by weight of Tris buffer to the blending agent to adjust the pH of the system to 8.0-8.5, then add 0.8-1 parts by weight of dopamine hydrochloride. Stir the mixture at 350-370 rpm for 4-5 hours at 28-30℃. After the reaction is complete, filter the mixture, wash it three times with anhydrous ethanol, and air dry it to obtain the modified cerium dioxide agent. The pH of the Tris buffer is 8.5-8.7, and the mass concentration is 0.05-0.07 mol / L.
[0027] The preparation method of a high-temperature resistant insulating ceramic product according to this embodiment includes the following steps: weighing the raw materials according to the weight parts, wet ball milling the raw materials thoroughly, then molding them in a mold, and then sintering them to obtain the high-temperature resistant insulating ceramic product.
[0028] The specific steps of the sintering process in this embodiment are as follows: For S11a, first heat to 300℃ at a rate of 2-3℃ / min, hold for 10-15min, then heat to 850-900℃ at a rate of 3-4℃ / min, hold for 35-45min. S11b, then raise the temperature to 1100-1200℃ at a rate of 1.5-2.5℃ / min, hold for 1 hour, then raise the temperature to 1300℃ at a rate of 0.5-1.5℃ / min, hold for 2-3 hours; S11c, then naturally cooled to 800℃, and finally cooled to room temperature at 3-5℃ / min.
[0029] Example 1: A high-temperature resistant insulating ceramic product, comprising the following raw materials in parts by weight: 70 parts ceramic matrix, 5 parts modified silicon carbide agent, 6 parts silica filler, 1 part dispersant, and 2 parts binder.
[0030] The ceramic matrix comprises the following raw materials in parts by weight: 25 parts illite powder, 15 parts potassium feldspar powder, 10 parts quartz, and 5 parts microsilica powder; the dispersant is sodium hexametaphosphate; and the binder is carboxymethyl cellulose.
[0031] The preparation method of the modified silicon carbide agent in this embodiment includes the following steps: S1, silicon carbide is heat-treated at 110°C for 1 hour and then air-cooled to room temperature to obtain heat-treated silicon carbide; S2, heat-treated silicon carbide and the modifying liquid are subjected to ultrasonic modification treatment at a weight ratio of 3:5, ultrasonic power of 350W, ultrasonic treatment for 1 hour, and after ultrasonic treatment, the modified silicon carbide agent is obtained by filtration and drying.
[0032] The preparation method of the modified liquid in this embodiment is as follows: A 2% (w / w) dopamine hydrochloride solution, silane coupling agent KH560, and a 75% (w / w) aqueous ethanol solution were prepared in a weight ratio of 3:2:8 to obtain a dopamine hydrochloride solution. 2 parts by weight of yttrium oxide, 1 part by weight of carbon nanotubes, 3 parts by weight of nano-alumina, and 4 parts by weight of dopamine hydrochloride solution were thoroughly mixed to obtain a modified solution.
[0033] The method for preparing the silica filler in this embodiment is as follows: S11, Add silica to a 2% sodium lignosulfonate solution (4 times the total weight of silica) and stir until homogeneous to obtain a silica dispersion; S12, the silica dispersion and the filling liquid are mixed and ball-milled at a weight ratio of 8:5. After ball milling, the mixture is filtered and dried to obtain the silica filler.
[0034] The preparation method of the filling liquid in this embodiment is as follows: S121, add 1 part by weight of lanthanum nitrate solution with a mass fraction of 4% and 1 part by weight of silane coupling agent KH550 to 3 parts by weight of chitosan solution with a mass fraction of 2%, and mix evenly to obtain modified chitosan solution. S122, 2 parts by weight of kaolin, 1 part by weight of aluminum borate whiskers and 5 parts by weight of modified chitosan liquid are thoroughly mixed to obtain the first filling liquid; 2 parts by weight of basalt fiber, 1 part by weight of calcined talc powder and 3 parts by weight of zirconium silicate are thoroughly mixed to obtain the second filler. S123, the first filling liquid and the second filling agent are mixed and ball-milled at a weight ratio of 5:3 to obtain the filling liquid.
[0035] The ceramic product of this embodiment also includes 3 parts of modified cerium dioxide agent, and the preparation method of the modified cerium dioxide agent is as follows: Two parts by weight of silane coupling agent KH550, three parts by weight of 75% ethanol aqueous solution and 0.5 parts by weight of deionized water were mixed and pre-hydrolyzed at 300 r / min at 45℃ for 30 min to obtain silane hydrolysate. Four parts by weight of cerium dioxide, three parts by weight of titanium dioxide, two parts by weight of lutetium oxide, eight parts by weight of silane hydrolysate, and ten parts by weight of anhydrous ethanol were mixed and stirred at 400 r / min for 2 h at 65 °C to obtain a blend. Add 20 parts by weight of Tris buffer to the blending agent to adjust the pH of the system to 8.0, then add 0.8 parts by weight of dopamine hydrochloride. Stir the mixture at 350 rpm for 4 hours at 28°C. After the reaction is complete, filter the mixture, wash it three times with anhydrous ethanol, and air dry it to obtain the modified cerium dioxide agent. The pH of the Tris buffer was 8.5, and the mass concentration was 0.05 mol / L.
[0036] The preparation method of a high-temperature resistant insulating ceramic product according to this embodiment includes the following steps: weighing the raw materials according to the weight parts, wet ball milling the raw materials thoroughly, then molding them in a mold, and then sintering them to obtain the high-temperature resistant insulating ceramic product.
[0037] The specific steps of the sintering process in this embodiment are as follows: S11a, first heat to 300℃ at a rate of 2℃ / min, hold for 10min, then heat to 850℃ at a rate of 3℃ / min, hold for 35min; S11b, then heat to 1100℃ at a rate of 1.5℃ / min and hold for 1 hour, then heat to 1300℃ at a rate of 0.5℃ / min and hold for 2 hours; S11c, then naturally cooled to 800℃, and finally cooled to room temperature at 3℃ / min.
[0038] Example 2: A high-temperature resistant insulating ceramic product, comprising the following raw materials in parts by weight: 90 parts ceramic matrix, 12 parts modified silicon carbide agent, 10 parts silica filler, 3 parts dispersant, and 5 parts binder.
[0039] The ceramic matrix comprises the following raw materials in parts by weight: 30 parts illite powder, 20 parts potassium feldspar powder, 15 parts quartz, and 8 parts microsilica powder; the dispersant is sodium hexametaphosphate; and the binder is carboxymethyl cellulose.
[0040] The preparation method of the modified silicon carbide agent in this embodiment includes the following steps: S1, silicon carbide is heat-treated at 120°C for 1 hour and then air-cooled to room temperature to obtain heat-treated silicon carbide; S2, heat-treated silicon carbide and the modifying liquid are subjected to ultrasonic modification treatment at a weight ratio of 3:7, ultrasonic power of 450W, ultrasonic treatment for 1 hour, and after ultrasonic treatment, the modified silicon carbide agent is obtained by filtration and drying.
[0041] The preparation method of the modified liquid in this embodiment is as follows: A 5% (w / w) solution of dopamine hydrochloride, silane coupling agent KH560, and an 85% (w / w) aqueous ethanol solution were prepared in a weight ratio of 5:2:10 to obtain a dopamine hydrochloride solution. 4 parts by weight of yttrium oxide, 3 parts by weight of carbon nanotubes, 5 parts by weight of nano-alumina, and 7 parts by weight of dopamine hydrochloride solution were thoroughly mixed to obtain a modified solution.
[0042] The method for preparing the silica filler in this embodiment is as follows: S11, Add silica to a 5% sodium lignosulfonate solution (7 times the total weight of silica) and stir until homogeneous to obtain a silica dispersion; S12, the silica dispersion and the filling liquid are mixed and ball-milled at a weight ratio of 11:5. After ball milling, the mixture is filtered and dried to obtain the silica filler.
[0043] The preparation method of the filling liquid in this embodiment is as follows: S121, add 3 parts by weight of 4% lanthanum nitrate solution and 2 parts by weight of silane coupling agent KH550 to 5 parts by weight of chitosan solution with a mass fraction of 5%, and mix evenly to obtain modified chitosan solution. S122, 5 parts by weight of kaolin, 3 parts by weight of aluminum borate whiskers and 8 parts by weight of modified chitosan liquid are thoroughly mixed to obtain the first filling liquid; 5 parts by weight of basalt fiber, 3 parts by weight of calcined talc powder and 5 parts by weight of zirconium silicate are thoroughly mixed to obtain the second filler. S123, the first filling liquid and the second filling agent are mixed and ball-milled at a weight ratio of 8:3 to obtain the filling liquid.
[0044] The ceramic product of this embodiment also includes 6 parts of modified cerium dioxide agent, and the preparation method of the modified cerium dioxide agent is as follows: Mix 3 parts by weight of silane coupling agent KH550, 5 parts by weight of 85% ethanol aqueous solution and 1 part by weight of deionized water, and stir at 500 r / min at 48℃ for 30 min to pre-hydrolyze to obtain silane hydrolysate. 5 parts by weight of cerium dioxide, 4 parts by weight of titanium dioxide, 3 parts by weight of lutetium oxide, 10 parts by weight of silane hydrolysate, and 15 parts by weight of anhydrous ethanol were mixed and stirred at 500 r / min for 2 h at 67 °C to obtain a blend. Add 30 parts by weight of Tris buffer to the blending agent to adjust the pH of the system to 8.5, then add 1 part by weight of dopamine hydrochloride. Stir the mixture at 370 r / min for 5 h at 30 °C. After the reaction is complete, filter the mixture, wash it three times with anhydrous ethanol, and air dry it to obtain the modified cerium dioxide agent. The pH of the Tris buffer was 8.7 and the mass concentration was 0.07 mol / L.
[0045] The preparation method of a high-temperature resistant insulating ceramic product according to this embodiment includes the following steps: weighing the raw materials according to the weight parts, wet ball milling the raw materials thoroughly, then molding them in a mold, and then sintering them to obtain the high-temperature resistant insulating ceramic product.
[0046] The specific steps of the sintering process in this embodiment are as follows: S11a, first heat to 300℃ at a rate of 3℃ / min, hold for 15min, then heat to 900℃ at a rate of 4℃ / min, hold for 45min; S11b, then heat to 1200℃ at a rate of 2.5℃ / min, hold for 1 hour, then heat to 1300℃ at a rate of 1.5℃ / min, hold for 3 hours; S11c, then naturally cooled to 800℃, and finally cooled to room temperature at 5℃ / min.
[0047] Example 3: A high-temperature resistant insulating ceramic product, comprising the following raw materials in parts by weight: The composition consists of 80 parts ceramic matrix, 7.5 parts modified silicon carbide, 8 parts silica filler, 2 parts dispersant, and 3.5 parts binder.
[0048] The ceramic matrix comprises the following raw materials in parts by weight: 27.5 parts illite powder, 17.5 parts potassium feldspar powder, 12.5 parts quartz, and 6.5 parts microsilica powder; the dispersant is sodium hexametaphosphate; and the binder is carboxymethyl cellulose.
[0049] The preparation method of the modified silicon carbide agent in this embodiment includes the following steps: S1, silicon carbide is heat-treated at 115°C for 1 hour and then air-cooled to room temperature to obtain heat-treated silicon carbide; S2, heat-treated silicon carbide and the modifying liquid are subjected to ultrasonic modification treatment at a weight ratio of 3:6, ultrasonic power of 400W, ultrasonic treatment for 1 hour, and after ultrasonic treatment, the modified silicon carbide agent is obtained by filtration and drying.
[0050] The preparation method of the modified liquid in this embodiment is as follows: A 3.5% (w / w) dopamine hydrochloride solution, silane coupling agent KH560, and an 80% (w / w) aqueous ethanol solution were prepared in a weight ratio of 4:2:9 to obtain a dopamine hydrochloride solution. 3 parts by weight of yttrium oxide, 2 parts by weight of carbon nanotubes, 4 parts by weight of nano-alumina, and 5.5 parts by weight of dopamine hydrochloride solution were thoroughly mixed to obtain a modified solution.
[0051] The method for preparing the silica filler in this embodiment is as follows: S11, Add silica to a sodium lignosulfonate solution with a mass fraction of 3.5% (5.5 times the total weight of silica) and stir until homogeneous to obtain a silica dispersion; S12, the silica dispersion and the filling liquid are mixed and ball-milled at a weight ratio of 9:5. After ball milling, the mixture is filtered and dried to obtain the silica filler.
[0052] The preparation method of the filling liquid in this embodiment is as follows: S121, add 2 parts by weight of 4% lanthanum nitrate solution and 1.5 parts by weight of silane coupling agent KH550 to 4 parts by weight of chitosan solution with a mass fraction of 3.5%, and mix evenly to obtain modified chitosan solution. S122, 3.5 parts by weight of kaolin, 2 parts by weight of aluminum borate whiskers and 6.5 parts by weight of modified chitosan liquid are thoroughly mixed to obtain the first filler liquid; 3.5 parts by weight of basalt fiber, 2 parts by weight of calcined talc powder and 4 parts by weight of zirconium silicate are thoroughly mixed to obtain the second filler. S123, the first filling liquid and the second filling agent are mixed and ball-milled at a weight ratio of 6.5:3 to obtain the filling liquid.
[0053] The ceramic product of this embodiment also includes 4.5 parts of modified cerium dioxide agent, and the preparation method of the modified cerium dioxide agent is as follows: 2.5 parts by weight of silane coupling agent KH550, 4 parts by weight of 80% ethanol aqueous solution and 0.75 parts by weight of deionized water were mixed and pre-hydrolyzed at 400 r / min at 46℃ for 30 min to obtain silane hydrolysate. 4.5 parts by weight of cerium dioxide, 3.5 parts by weight of titanium dioxide, 2.5 parts by weight of lutetium oxide, 9 parts by weight of silane hydrolysate, and 12.5 parts by weight of anhydrous ethanol were mixed and stirred at 450 r / min for 2 h at 66 °C to obtain a blend. Add 25 parts by weight of Tris buffer to the blending agent to adjust the pH of the system to 8.2, then add 0.9 parts by weight of dopamine hydrochloride. Stir the mixture at 360 r / min for 4.5 h at 29 °C. After the reaction is complete, filter the mixture, wash it three times with anhydrous ethanol, and air dry it to obtain the modified cerium dioxide agent. The pH of the Tris buffer was 8.6, and the mass concentration was 0.06 mol / L.
[0054] The preparation method of a high-temperature resistant insulating ceramic product according to this embodiment includes the following steps: weighing the raw materials according to the weight parts, wet ball milling the raw materials thoroughly, then molding them in a mold, and then sintering them to obtain the high-temperature resistant insulating ceramic product.
[0055] The specific steps of the sintering process in this embodiment are as follows: S11a, first heat to 300℃ at a rate of 2.5℃ / min, hold for 12.5min, then heat to 880℃ at a rate of 3.5℃ / min, hold for 40min; S11b, then heat to 1150℃ at a rate of 2.0℃ / min, hold for 1h, then heat to 1300℃ at a rate of 1℃ / min, hold for 2.5h; S11c, then naturally cooled to 800℃, and finally cooled to room temperature at 4℃ / min.
[0056] Comparative Example 1: Unlike Example 3, no modified silicon carbide agent was added.
[0057] Comparative Example 2: Unlike Example 3, no modifying liquid was added during the preparation of the modified silicon carbide agent.
[0058] Comparative Example 3: Unlike Example 3, yttrium oxide and carbon nanotubes were not used in the preparation of the modified liquid.
[0059] Comparative Example 4: Unlike Example 3, no silica filler was added.
[0060] Comparative Example 5: Unlike Example 3, no filling liquid was added during the preparation of the silica filler.
[0061] Comparative Example 6: Unlike Example 3, no first filling liquid was added during the preparation of the filling liquid.
[0062] Comparative Example 7: Unlike Example 3, kaolin and aluminum borate whiskers were not added in the preparation of the first filling liquid.
[0063] Comparative Example 8: Unlike Example 3, the modified chitosan solution was replaced with a chitosan solution with a mass fraction of 3.5%.
[0064] Comparative Example 9: Unlike Example 3, no second filler was added during the preparation of the filling solution.
[0065] Comparative Example 10: Unlike Example 3, calcined talc and zirconium silicate were not added in the preparation of the second filler.
[0066] Comparative Example 11: Unlike Example 3, no modified cerium dioxide agent was added.
[0067] Comparative Example 12: Unlike Example 3, titanium dioxide and lutetium oxide were not added in the preparation of the modified cerium dioxide agent.
[0068] Comparative Example 13: Unlike Example 3, Tris buffer and dopamine hydrochloride were not added during the preparation of the modified cerium dioxide agent.
[0069] The products of Examples 1-3 and Comparative Examples 1-13 were tested for insulation, ease of cleaning, and mechanical properties. Simultaneously, the products' high-temperature resistance and resistance to different corrosion types were tested (the product was placed at 70°C for 12 hours, then placed under 5% hydrochloric acid mist for 12 hours; this constituted one cycle, and was repeated 10 times; the product was placed at 100°C for 12 hours, then placed under 8% hydrochloric acid mist for 12 hours; this constituted one cycle, and was repeated 10 times). The test results are shown in Table 1. Table 1 Performance test results:
[0070] As can be seen from Comparative Examples 1-13 and Examples 1-3, the product of Example 3 has excellent mechanical strength, insulation and easy-to-clean properties, and the product has significant high temperature resistance and corrosion stability to different degrees. Without the addition of modified silicon carbide, silica filler, and modified cerium dioxide, the performance of the product tends to deteriorate to varying degrees. By using modified silicon carbide, silica filler, and modified cerium dioxide in combination for synergistic effect, the product's performance is the best. In the preparation of modified silicon carbide agent, no modifying liquid was added; in the preparation of modifying liquid, yttrium oxide and carbon nanotubes were not used for treatment; and in the preparation of silica filler, no filling liquid was added. The performance of the products all showed varying degrees of deterioration. Furthermore, in the preparation of the filling liquid, no first filling liquid was added; in the preparation of the first filling liquid, kaolin and aluminum borate whiskers were not added; the modified chitosan liquid was replaced with a 3.5% chitosan solution by mass; and in the preparation of the filling liquid, no second filler was added; and in the preparation of the second filler, calcined talc and zirconium silicate were not added. The performance of the products also showed varying degrees of deterioration. Only the filling liquid prepared by the specific method of this invention, in combination with the second filler and optimized through mutual coordination, resulted in the most significant performance improvement. The preparation of the filling liquid of this invention is unique, and the specific raw materials prepared using the technical solution of this invention exhibit the most outstanding performance. The modified cerium dioxide agent was not prepared without the addition of titanium dioxide and lutetium oxide, Tris buffer and dopamine hydrochloride, and the performance of the product tended to deteriorate. Only the modified cerium dioxide agent prepared by the method of this invention showed the most significant performance effect.
[0071] 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 implemented 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 exemplary and non-limiting, and the scope of the invention is defined by the appended claims rather than the foregoing description. Thus, it is intended that all variations falling within the meaning and scope of equivalents of the claims be included within the present invention.
[0072] Furthermore, it should be understood that although this specification describes embodiments, not every embodiment contains only one independent technical solution. This narrative style is merely for clarity. Those skilled in the art should consider the specification as a whole, and the technical solutions in each embodiment can also be appropriately combined to form other embodiments that can be understood by those skilled in the art.
Claims
1. A high-temperature resistant insulating ceramic product, characterized in that, Including the following parts by weight of raw materials: 70-90 parts ceramic matrix, 5-12 parts modified silicon carbide agent, 6-10 parts silica filler, 1-3 parts dispersant, and 2-5 parts binder; The ceramic matrix comprises the following raw materials in parts by weight: 25-30 parts illite powder, 15-20 parts potassium feldspar powder, 10-15 parts quartz, and 5-8 parts microsilica powder; the dispersant is sodium hexametaphosphate; and the binder is carboxymethyl cellulose. The preparation method of the modified silicon carbide agent includes the following steps: S1, heat-treat silicon carbide at 110-120℃ for 1 hour, then air-cool to room temperature to obtain heat-treated silicon carbide; S2, heat-treated silicon carbide and the modification liquid are subjected to ultrasonic modification treatment at a weight ratio of 3:(5-7), ultrasonic power of 350-450W, ultrasonic treatment for 1 hour, and after ultrasonic treatment, the modified silicon carbide agent is obtained by filtration and drying. The modified liquid is prepared by: A 2-5% (w / w) dopamine hydrochloride solution, silane coupling agent KH560, and a 75-85% (w / w) aqueous ethanol solution were prepared in a weight ratio of (3-5):2:(8-10) to obtain a dopamine hydrochloride solution; 2-4 parts by weight of yttrium oxide, 1-3 parts by weight of carbon nanotubes, 3-5 parts by weight of nano-alumina, and 4-7 parts by weight of the dopamine hydrochloride solution were thoroughly mixed to obtain a modified solution; The preparation method of the silica filler is as follows: S11, add silica to a sodium lignosulfonate solution with a mass fraction of 2-5% and 4-7 times the total weight of silica and stir until homogeneous to obtain a silica dispersion; S12, the silica dispersion and the filling liquid are mixed and ball-milled at a weight ratio of (8-11):
5. After ball milling, the mixture is filtered and dried to obtain the silica filler. The method for preparing the filling liquid is as follows: S121, add 1-3 parts by weight of lanthanum nitrate solution with a mass fraction of 4% and 1-2 parts by weight of silane coupling agent KH550 to 3-5 parts by weight of chitosan solution with a mass fraction of 2-5%, and mix evenly to obtain modified chitosan solution. S122, 2-5 parts by weight of kaolin, 1-3 parts by weight of aluminum borate whiskers and 5-8 parts by weight of modified chitosan liquid are thoroughly mixed to obtain the first filler liquid; 2-5 parts by weight of basalt fiber, 1-3 parts by weight of calcined talc powder and 3-5 parts by weight of zirconium silicate are thoroughly mixed to obtain the second filler. S123, the first filling liquid and the second filling agent are mixed and ball-milled at a weight ratio of (5-8):3 to obtain the filling liquid; The ceramic product further includes 3-6 parts of modified cerium dioxide agent, and the preparation method of the modified cerium dioxide agent is as follows: Mix 2-3 parts by weight of silane coupling agent KH550, 3-5 parts by weight of 75-85% aqueous ethanol solution and 0.5-1 parts by weight of deionized water, and stir at 300-500 r / min at 45-48℃ for 30 min to pre-hydrolyze and obtain silane hydrolysate. Mix 4-5 parts by weight of cerium dioxide, 3-4 parts by weight of titanium dioxide, 2-3 parts by weight of lutetium oxide, 8-10 parts by weight of silane hydrolysate, and 10-15 parts by weight of anhydrous ethanol, and stir the mixture at 65-67°C and 400-500 r / min for 2 h to obtain a blend. Add 20-30 parts by weight of Tris buffer to the blending agent to adjust the pH of the system to 8.0-8.5, then add 0.8-1 parts by weight of dopamine hydrochloride, and stir the mixture at 350-370 r / min at 28-30℃ for 4-5 h. After the reaction is completed, filter the mixture, wash it three times with anhydrous ethanol, and air dry it to obtain the modified cerium dioxide agent.
2. The high-temperature resistant insulating ceramic product according to claim 1, characterized in that, The Tris buffer solution has a pH of 8.5-8.7 and a mass concentration of 0.05-0.07 mol / L.
3. A method for preparing a high-temperature resistant insulating ceramic product, used to prepare a high-temperature resistant insulating ceramic product as described in any one of claims 1-2, characterized in that, The process includes the following steps: weighing the raw materials according to their weight proportions, wet ball milling the raw materials thoroughly, then molding them in a mold, and finally sintering them to obtain high-temperature resistant insulating ceramic products.
4. The method for preparing a high-temperature resistant insulating ceramic product according to claim 3, characterized in that, The specific steps of the sintering process are as follows: For S11a, first heat to 300℃ at a rate of 2-3℃ / min, hold for 10-15min, then heat to 850-900℃ at a rate of 3-4℃ / min, hold for 35-45min. S11b, then raise the temperature to 1100-1200℃ at a rate of 1.5-2.5℃ / min, hold for 1 hour, then raise the temperature to 1300℃ at a rate of 0.5-1.5℃ / min, hold for 2-3 hours; S11c, then naturally cooled to 800℃, and finally cooled to room temperature at 3-5℃ / min.
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