Novel high-temperature-resistant ceramic composite heat-insulating energy-saving material and preparation method thereof

By combining modified kaolin with rare earth elements, combined with modified fibers and composite adhesives, a porous structure is constructed, which solves the problems of uneven thermal expansion and weak thermal shock resistance of ceramic materials at high temperatures, and achieves excellent compression performance and thermal management effect at high temperatures.

CN120483761APending Publication Date: 2025-08-15DAQING ZHUOCHENGDA TECHNOLOGY CO LTD
View PDF 1 Cites 0 Cited by

Patent Information

Application Number
CN202510797857.9
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-06-16
Publication Date
2025-08-15

AI Technical Summary

Technical Problem

Existing ceramic materials are prone to uneven thermal expansion, structural collapse, weak thermal shock resistance, long thermal conduction paths, and insufficient infrared radiation mechanism at high temperatures, resulting in limited overall performance.

Method used

By combining modified kaolin with rare earth elements, a stable framework structure is formed, combined with modified fibers and composite adhesives, a silicone-modified silicon carbide microsphere foaming agent is introduced to build a porous structure and optimize the internal structure and thermal management performance of the material.

Benefits of technology

It significantly improves the high-temperature compression performance, thermal impact toughness and infrared radiation of the material, reduces the thermal conductivity, enhances the compressive strength and thermal management performance, and is suitable for high-temperature and high-strength industrial applications.

✦ Generated by Eureka AI based on patent content.

Smart Images

  • Figure SMS_1
    Figure SMS_1
Patent Text Reader

Abstract

The invention discloses a novel high-temperature-resistant ceramic composite heat-insulating energy-saving material and a preparation method thereof, belongs to the technical field of ceramic preparation, and aims to solve the technical problem that the high-temperature resistance and the energy-saving performance of a ceramic material in the prior art need to be further improved. The novel high-temperature-resistant ceramic composite heat-insulating energy-saving material comprises the following raw materials in parts by weight: 80-98 parts of a modified ceramic raw material, 5-8 parts of a modified foaming agent, 4-5 parts of a composite adhesive and 32-45 parts of an auxiliary material, generation of secondary mullite is promoted by preparing modified kaolin, the far infrared performance of a product is improved by introducing rare earth elements, the mechanical performance of the material is improved by utilizing modified fibers in a modified adhesive, meanwhile, the far infrared performance of the material is improved by rare earth components, a siloxane structure on the outer layer of a modified foaming agent, and the foaming performance is improved. The preparation method provides support for a porous structure generated by high-temperature foaming of silicon carbide, improves the compression resistance of the product, and provides synergistic cooperation of the three components, thereby obtaining a high-performance ceramic material.
Need to check novelty before this filing date? Find Prior Art

Description

Technical Field

[0001] The present invention relates to the technical field of ceramic preparation, and in particular to a high-temperature resistant ceramic composite heat-insulating energy-saving new material and a preparation method thereof. Background Art

[0002] The development of high-temperature resistant and energy-saving ceramic materials has undergone a transformation process from structural ceramics to functional ceramics. In the early days, traditional ceramics such as alumina and mullite were mostly used, focusing on solving the problems of high-temperature stability and mechanical strength. With the increase in energy-saving needs, research has gradually focused on thermal functional properties with low thermal conductivity and high infrared emissivity, prompting the material to develop from a dense structure to a porous composite system. In recent years, by introducing rare earth elements, infrared emission phases, multi-scale foaming structures and fiber reinforcement mechanisms, the coordinated optimization of multiple properties such as high-temperature resistance, thermal shock resistance, thermal insulation and radiation heat transfer has been achieved. Advanced preparation technologies such as low-temperature sintering, aerogel composites, interface regulation and intelligent design have promoted the widespread application of such ceramics in aerospace, high-temperature furnace linings, heat recovery and energy-saving buildings. The current research trend is deepening towards the integration of material structure and function, green and sustainable preparation and improvement of service stability.

[0003] Prior art CN116253578B discloses a high temperature resistant inorganic fiber ceramic thermal insulation material, the raw materials of which include: 25-40 parts by mass of pre-cured sodium silicate, 60-75 parts by mass of water, 0.60-1.25 parts by mass of surfactant, 0.3-0.6 parts by mass of bentonite, 3-5 parts by mass of glass fiber, 30-40 parts by mass of aluminum silicate fiber, 10-20 parts by mass of ceramic microspheres, 30-50 parts by mass of aluminum oxide, 10 -20 parts by mass of magnesium oxide, 1-1.5 parts by mass of foaming agent; a preparation method of high-temperature resistant inorganic fiber ceramic thermal insulation material is also provided; this thermal insulation material has the characteristics of light weight and high strength, flexibility and impact resistance, waterproofness, freeze-thaw resistance, and high temperature resistance. The operating temperature is -40℃-1200℃, the thermal conductivity coefficient is 0.03-0.15w / mk, and it reaches Class A fire protection. It can be widely used in civil buildings, equipment facilities, cold storage, industrial plants, thermal pipelines, storage tanks, etc.

[0004] However, the above invention obtains a high-temperature resistant thermal insulation ceramic material by foaming the ceramic material with a foaming agent and then sintering it. However, the pre-cured sodium silicate, glass fiber and aluminum silicate fiber are physically mixed to form a matrix, which lacks a strong chemical bonding mechanism. The interface between the particles and the fibers is loose, which easily causes crack expansion under compression load. The ceramic microbeads do not optimize the pore support and are prone to structural collapse. The components have insufficient thermal stability, the matrix is prone to uneven thermal expansion at high temperatures, the fibers do not form an effective stress buffer network, microcracks are prone to rapid temperature changes, and the ability to resist thermal shock is weak. The foaming agent relies on a simple network structure, the pore distribution is uneven, there is a lack of an efficient thermal barrier mechanism, the heat conduction path is long, the infrared radiation mechanism is insufficient, and the heat exchange efficiency is low, which limits the overall performance and restricts the performance optimization.

[0005] In view of the technical defects in this aspect, a solution is now proposed. Summary of the Invention

[0006] The purpose of the present invention is to provide a high-temperature resistant ceramic composite insulation energy-saving new material and a preparation method thereof, which are used to solve the technical problem that the high-temperature resistance and energy-saving performance of existing ceramic materials need to be further improved.

[0007] The purpose of the present invention can be achieved through the following technical solutions: A high-temperature resistant ceramic composite thermal insulation energy-saving new material, comprising the following raw materials in parts by weight: 80-98 parts of modified ceramic raw materials, 5-8 parts of modified foaming agents, 4-5 parts of composite adhesives, and 32-45 parts of auxiliary materials; Furthermore, the auxiliary material comprises the following raw materials in parts by weight: 1-2 parts of polyvinyl alcohol, 1-3 parts of silica sol and 20-30 parts of dispersant, wherein the dispersant is deionized water.

[0008] The preparation method of the modified ceramic raw material comprises the following steps: A1. Add kaolin and 10 wt% sulfuric acid aqueous solution into a stirred tank. After the temperature of the stirred tank is raised to 60-80° C., stir at this temperature for 1-2 hours, and perform post-treatment to obtain activated kaolin. A2. Add activated kaolin and modifying solution into a ball mill, ball mill at room temperature for 4-6 hours, and post-treat to obtain modified kaolin; The reaction principle for preparing modified kaolin is as follows: after kaolin is heated in a sulfuric acid solution, some hydroxyl groups in its crystal structure are removed, and aluminum ions are partially dissolved, forming structural defects and reaction sites. Subsequently, the lanthanum ions and cerium ions in the modification solution undergo coordination reactions with hydroxyl groups or oxygen bridge groups on the surface of the kaolin during ball milling, forming rare earth-oxygen-silicon / aluminum bonds. Some rare earth ions enter the interlayers of the kaolin or embed into defect positions, thereby preparing modified kaolin.

[0009] A3. Weigh 10-25 parts of corundum, 60-80 parts of mullite, and 5-8 parts of modified kaolin by weight, and mix them to obtain a modified ceramic raw material.

[0010] Furthermore, in step A1, the ratio of kaolin and 10 wt% aqueous sulfuric acid solution is 1 g: 5-6 mL, and the post-treatment includes: after the treatment is completed, the temperature of the reactor is lowered to room temperature, the reaction liquid is filtered to collect the filter cake, the filter cake is washed with anhydrous ethanol and deionized water 3-5 times, and the filter cake is transferred to a vacuum drying oven at a temperature of 60-80 ° C. and vacuum dried to constant weight to obtain activated kaolin; Furthermore, in step A2, the amount ratio of activated kaolin and modifying liquid is 1g:2-3mL, wherein the modifying liquid is obtained by mixing cerium nitrate, lanthanum nitrate and deionized water in a ratio of 1-2g:1-2g:100mL, the ball milling medium in the ball mill is zirconia balls with a particle size of 2-3mm, and the ball-to-material ratio is 5-8:1. The post-processing includes: after the ball milling is completed, taking out the material, using anhydrous ethanol and deionized water to filter the material cake 3-5 times, and then transferring the material to a vacuum drying oven at a temperature of 60-80°C, and vacuum drying to constant weight to obtain modified kaolin.

[0011] Furthermore, the preparation method of the modified foaming agent comprises the following steps: B1. Add silicon carbide microspheres and a mixed solvent into a reactor, adjust the pH of the reaction system to 3-4 with boric acid, and stir at room temperature for 10-12 minutes. Then, add methyl orthosilicate into the reactor, continue stirring for 3-4 hours, and let it stand for 21-24 hours. Post-process and obtain modified microspheres. B2. Add the modified microspheres, anhydrous ethanol and sodium hydroxide into the reactor, increase the temperature of the reactor to 40-60°C, add 3-(2,3-epoxypropoxy)propyltrimethoxysilane into the reactor, keep warm and stir for 2-3 hours, and then post-treat to obtain the modified foaming agent.

[0012] The reaction principle for preparing the modified foaming agent is as follows: methyl orthosilicate undergoes partial hydrolysis and polycondensation under acidic conditions to form a polysiloxane network on the surface of silicon carbide microspheres to achieve inorganic coating modification; under alkaline anhydrous conditions, the epoxy group in 3-(2,3-epoxypropoxy)propyltrimethoxysilane is ring-opened under base catalysis to generate an intermediate with nucleophilic activity, which undergoes a ring-opening grafting reaction with the hydroxyl groups on the surface of the microspheres to form a covalently bonded organic silicon layer, thereby preparing the modified foaming agent.

[0013] Furthermore, in step B1, the amount ratio of the silicon carbide microspheres, the mixed solvent and methyl orthosilicate is 4-5g:30-36mL:1-2g, wherein the mixed solvent is obtained by mixing deionized water and anhydrous ethanol in a volume ratio of 2-3:6-7. The post-treatment includes: after the treatment is completed, the temperature of the reactor is lowered to room temperature, the reaction liquid is filtered to collect the filter cake, and the filter cake is transferred to a muffle furnace at a temperature of 700-800°C and kept warm for 2h to obtain modified microspheres; Furthermore, in step B2, the modified microspheres, anhydrous ethanol, sodium hydroxide and 3-(2,3-epoxypropoxy)propyltrimethoxysilane are used in a ratio of 3-4 g:20-24 mL:0.3-0.4 g:1-2 g, and the post-treatment includes: after the treatment is completed, the temperature of the reactor is lowered to room temperature, the reaction liquid is filtered to collect the filter cake, and the filter cake is washed 3-5 times with anhydrous ethanol and deionized water. After that, the filter cake is transferred to a vacuum drying oven at a temperature of 60-80°C, and vacuum dried to constant weight to obtain a modified foaming agent.

[0014] Furthermore, the preparation method of the composite adhesive is as follows: adding ethyl orthosilicate and deionized water to a reactor, stirring at room temperature for 10-12 minutes, adding a 30-40wt% sulfuric acid aqueous solution to the reactor, adjusting the system pH to 3-4, standing for 3-4 hours, adding aluminum isopropylate and modified fiber to the reactor, and post-processing to obtain a composite adhesive.

[0015] The reaction principle for preparing the modified adhesive is as follows: ethyl orthosilicate undergoes hydrolysis and condensation reaction under acidic conditions to generate a silicon-oxygen network structure mainly composed of silicon-oxygen silicon; aluminum isopropoxide forms an aluminum hydroxyl intermediate during the hydrolysis process, which further undergoes condensation reaction with silanol to form an aluminum-oxygen-silicon bond; the hydroxyl groups on the fiber surface undergo condensation reaction with silanol or aluminum hydroxyl groups, causing them to be embedded in the silica structure to form an aluminum-containing composite silicate adhesive.

[0016] Furthermore, the usage ratio of ethyl orthosilicate, deionized water, aluminum isopropoxide and modified fiber is 8-10g:40-50mL:1-2g:1-2g, and the post-processing includes: after the reaction is completed, transferring the reaction liquid to a rotary evaporator with a salt bath temperature of 60-80°C, and distilling under reduced pressure until no liquid is extracted to obtain a composite adhesive.

[0017] Furthermore, the preparation method of the modified fiber comprises the following steps: C1. Add yttrium nitrate, ytterbium nitrate, europium nitrate, titanium chloride, polyvinyl pyrrolidone, deionized water and anhydrous ethanol into a stirred tank, and stir at room temperature for 10-15 minutes to obtain a spinning solution; C2. adding the spinning liquid into an electrospinning machine and electrospinning to obtain composite fibers; C3, transferring the composite fiber to a tubular furnace and calcining it to obtain a modified fiber precursor; C4. Add the modified fiber precursor and 4-5 wt% sodium hydroxide aqueous solution into a reactor, increase the temperature of the reactor to 40-50° C., keep warm and soak for 40-60 minutes, and post-treat to obtain the modified fiber.

[0018] The reaction principle for preparing modified fibers is as follows: yttrium nitrate, ytterbium nitrate and europium nitrate dissociate in the solution to form rare earth ions, titanium chloride hydrolyzes to form titanium oxide intermediates, polyvinyl pyrrolidone forms a stable complex solution by coordination with metal ions, and is solidified by electrospinning to form a uniformly distributed metal-organic composite fiber. During the calcination process, the organic components decompose, and the metal ions form corresponding oxides and are evenly distributed in the fiber. Under alkaline conditions, the fiber surface undergoes hydroxylation or passivation treatment, which promotes surface structure reorganization and functional group exposure, forming a rare earth-titanium composite modified fiber with good surface activity.

[0019] Furthermore, in step C1, the ratio of yttrium nitrate, ytterbium nitrate, europium nitrate, titanium chloride, polyvinyl pyrrolidone, deionized water and anhydrous ethanol is 3.8g:2.3g:4.4g:1.9g:18-20g:90-95g:90-95g; Furthermore, in step C2, the parameters of the electrospinning machine are: voltage 18-20 kV, electrode distance 12-15 cm, and air humidity 35-40%; Furthermore, in step C3, the calcination operation is as follows: transferring the composite fiber to a muffle furnace, heating the temperature from room temperature to 600-700°C at a rate of 8-10°C / min in an air atmosphere, and keeping the temperature for 2 hours to obtain a modified fiber precursor; Furthermore, in step C4, the usage ratio of the modified fiber precursor and the 4-5wt% sodium hydroxide aqueous solution is 1-2g:4-5mL, and the post-treatment includes: after the treatment is completed, the temperature of the reactor is lowered to room temperature, the reaction liquid is filtered to collect the filter cake, the filter cake is washed 3-5 times with anhydrous ethanol and deionized water, and the filter cake is transferred to a vacuum drying oven at a temperature of 60-80°C, and vacuum dried to constant weight to obtain modified fiber.

[0020] The present invention also discloses a method for preparing a high-temperature resistant ceramic composite thermal insulation energy-saving new material, comprising the following steps: S1. Add the modified ceramic raw material, composite adhesive and dispersant to a stirring tank, stir at room temperature for 10-15 minutes, then continue to add polyvinyl alcohol and silica sol, continue to stir for 20-25 minutes, then add the modified foaming agent and stir for 10-20 minutes to obtain a ceramic slurry; S2. Pour the ceramic slurry into a mold, vacuum degas, transfer the mold to a calcining furnace, calcine in stages, and demold to obtain a high-temperature resistant ceramic.

[0021] Furthermore, in step S2, the operation of the staged calcination is as follows: the calcining furnace is heated to 80-100°C at a heating rate of 8-10°C / min, and the temperature is kept at this temperature for 2-4 hours. The temperature is then increased to 300-400°C at a heating rate of 5-6°C / min, and the temperature is kept at this temperature for 1 hour. The temperature is then increased to 950-1050°C at a heating rate of 10°C / min, and the temperature is kept at this temperature for 30-40 minutes. Finally, the temperature is increased to 1250-1350°C at a heating rate of 5-8°C / min, and the temperature is kept at this temperature for 1.5-2.5 hours.

[0022] The present invention has the following beneficial effects: 1. The present invention enhances the density and thermal stability of the ceramic matrix by compounding modified kaolin and rare earth elements under high temperature conditions, forms a stable skeleton structure, effectively improves its compressive strength, and utilizes the modified fiber and composite adhesive to work together to effectively disperse stress under compressive load, slow down crack propagation, prevent local stress concentration, and significantly improve the toughness and compressive resistance of the material. Secondly, by introducing a foaming agent and modifying the siloxane layer on its surface, a supporting effect is provided to ensure that the porous structure formed by the silicon carbide microspheres does not suffer a decrease in strength due to excessive pores under compressive load. At the same time, the modification of the silane coupling agent enhances the compatibility between the components and optimizes the inherent structure of the material. Through the synergistic cooperation between these materials, the high-temperature resistant ceramics finally obtained retain the lightweight advantage of the porous structure under compressive load, and significantly improve its compressive strength, showing excellent high-temperature compression performance, and are suitable for high-temperature and high-strength industrial applications.

[0023] 2. The high-temperature resistant ceramics prepared by the present invention form a highly dense and stable ceramic skeleton structure through the synergistic effect of modified kaolin, rare earth elements and composite adhesives, effectively suppressing the non-uniformity of thermal expansion and significantly reducing the overall thermal expansion coefficient. In an environment where thermal stress changes drastically, the modified fibers in the structure act as a stress buffer network, which can effectively release the internal stress caused by thermal gradients and prevent rapid crack expansion, thereby improving the thermal shock toughness of the material; in addition, the siloxane-modified microsphere foaming agent provides a uniform and stable porous structure, so that the material has good thermal strain buffering capacity during rapid heating or sudden cooling. The coordinated combination of the porous structure and the dense skeleton maintains structural integrity under high-temperature cycles, ensuring that the ceramic does not peel or break; ultimately, through the synergistic effect between the various components of the material, the dimensional stability and thermal shock resistance of the ceramic at high temperatures are significantly enhanced, making it suitable for insulation and structural applications in harsh high-temperature alternating environments.

[0024] 3. The present invention improves the far-infrared radiation capacity of the ceramic skeleton by synergistically doping modified kaolin with rare earth elements. At the same time, the rare earth modified fibers introduced into the composite adhesive further enhance the emission response of the material to the mid- and far-infrared bands, forming a multi-scale, multi-point synergistic emission system in the overall structure of the material, significantly improving the infrared emissivity; further, the siloxane-modified silicon carbide microsphere foaming agent constructs a highly uniform closed-cell structure in the material, which not only reduces the effective heat conduction path in the material and significantly reduces the thermal conductivity, but also works together with the rare earth reinforced skeleton to form scattering and multiple reflections in the infrared band, thereby improving radiation efficiency and enhancing the thermal barrier effect. The rare earth fibers themselves have good thermal stability and radiation activity. Their position in the structure enables them to participate in thermal radiation and regulate the thermal field distribution on a microscopic scale, thereby improving the overall thermal management performance of the material. Ultimately, through the organic combination and functional synergy between multiple components, the material effectively reduces heat conduction loss while enhancing the radiation heat exchange efficiency, thereby significantly improving its energy-saving effect. DETAILED DESCRIPTION

[0025] The technical solutions of the present invention will be clearly and completely described below in conjunction with the embodiments. Obviously, the embodiments described are only some embodiments of the present invention, not all 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.

[0026] The kaolin used in the present invention was purchased from Shanghai McLean Biochemical Technology Co., Ltd. with the item number K812211; the corundum used in the present invention was purchased from Shanghai Aladdin Biochemical Technology Co., Ltd. with the item number A119598; the polyvinyl alcohol used in the present invention was purchased from Shanghai Aladdin Biochemical Technology Co., Ltd. with the item number P139537; the mullite used in the present invention was purchased from Shanghai McLean Biochemical Technology Co., Ltd. with the item number M970145; the polyvinyl pyrrolidone used in the present invention was purchased from Shanghai Aladdin Biochemical Technology Co., Ltd. with the item number R615356; the silica sol used in the present invention was purchased from Guangdong Wengjiang Chemical Reagent Co., Ltd., PA88497-500g; the silicon carbide microspheres used in the present invention were purchased from Zhejiang Yamei Nano Technology Co., Ltd. with the item number AM-SiC-051-3.

[0027] Example 1 This embodiment provides a method for preparing a composite adhesive for preparing a high-temperature resistant ceramic composite thermal insulation energy-saving new material, comprising the following steps: Step 1: Preparation of composite fibers Weigh 19.0 g of yttrium nitrate, 11.5 g of ytterbium nitrate, 22.0 g of europium nitrate, 9.5 g of titanium chloride, 90.0 g of polyvinyl pyrrolidone, 450.0 g of deionized water and 450.0 g of anhydrous ethanol into a stirred tank, stir at room temperature for 10 min to obtain a textile solution, and add the textile solution to an electrospinning machine. The parameters of the electrospinning machine are: voltage of 18 kV, electrode distance of 12 cm, air humidity of 35%, and spinning to obtain composite fibers.

[0028] Step ②, preparation of modified fiber Weigh: 40.0g of composite fiber is transferred to a muffle furnace, and in an air atmosphere, the temperature is raised from room temperature to 600℃ at a rate of 8℃ / min, and kept warm for 2h to obtain a modified fiber precursor. Then, 20.0g of the modified fiber precursor and 80.0mL of 4wt% sodium hydroxide aqueous solution are added to the reactor, the reactor temperature is raised to 40℃, and the mixture is kept warm and soaked for 40min. After the treatment is completed, the reactor temperature is lowered to room temperature, the reaction liquid is filtered, and the filter cake is collected. After washing the filter cake 3 times with anhydrous ethanol and deionized water, the filter cake is transferred to a vacuum drying oven at 60℃ and vacuum dried to constant weight to obtain modified fiber.

[0029] Step ③: Preparation of composite adhesive Weigh: 80.0g of ethyl orthosilicate and 400.0mL of deionized water were added to the reactor, stirred at room temperature for 10 minutes, and then a 30wt% aqueous sulfuric acid solution was added to the reactor. After adjusting the pH of the system to 4, the mixture was allowed to stand for 3 hours, and then 10.0g of aluminum isopropoxide and 10.0g of modified fiber were added to the reactor. After the reaction was completed, the reaction solution was transferred to a rotary evaporator with a salt bath temperature of 60°C, and distilled under reduced pressure until no liquid was extracted to obtain a composite adhesive.

[0030] Example 2 This embodiment provides a method for preparing a composite adhesive for preparing a high-temperature resistant ceramic composite thermal insulation energy-saving new material, comprising the following steps: Step 1: Preparation of composite fibers Weigh 19.0 g of yttrium nitrate, 11.5 g of ytterbium nitrate, 22.0 g of europium nitrate, 9.5 g of titanium chloride, 18-20 g of polyvinyl pyrrolidone, 90-95 g of deionized water, and 90-95 g of anhydrous ethanol into a stirred tank, stir at room temperature for 10-15 minutes to obtain a textile solution, and add the textile solution to an electrospinning machine. The parameters of the electrospinning machine are: voltage of 18-20 kV, electrode distance of 12-15 cm, and air humidity of 35-40%, and spin to obtain composite fibers.

[0031] Step ②, preparation of modified fiber Weigh: 40.0g of composite fiber is transferred to a muffle furnace, and in an air atmosphere, the temperature is raised from room temperature to 600℃ at a rate of 10℃ / min, and kept warm for 2h to obtain a modified fiber precursor. Then, 20.0g of the modified fiber precursor and 100.0mL of 5wt% sodium hydroxide aqueous solution are added to the reactor, the reactor temperature is raised to 50℃, and the mixture is kept warm and soaked for 40min. After the treatment is completed, the reactor temperature is lowered to room temperature, the reaction liquid is filtered, and the filter cake is collected. After washing the filter cake 3 times with anhydrous ethanol and deionized water, the filter cake is transferred to a vacuum drying oven at 80℃ and vacuum dried to constant weight to obtain modified fiber.

[0032] Step ③: Preparation of composite adhesive Weigh: 100.0g of ethyl orthosilicate and 500.0mL of deionized water were added to the reactor, stirred at room temperature for 12 minutes, and then a 40wt% aqueous sulfuric acid solution was added to the reactor. After adjusting the pH of the system to 4, the reactor was allowed to stand for 4 hours, and then 20.0g of aluminum isopropoxide and 20.0g of modified fiber were added to the reactor. After the reaction was completed, the reaction solution was transferred to a rotary evaporator with a salt bath temperature of 80°C, and distilled under reduced pressure until no liquid was extracted to obtain a composite adhesive.

[0033] Example 3 This embodiment provides a method for preparing a composite adhesive for preparing a high-temperature resistant ceramic composite thermal insulation energy-saving new material, comprising the following steps: Step 1: Preparation of composite fibers Weigh 19.0 g of yttrium nitrate, 11.5 g of ytterbium nitrate, 22.0 g of europium nitrate, 9.5 g of titanium chloride, 100.0 g of polyvinyl pyrrolidone, 475 g of deionized water and 475 g of anhydrous ethanol into a stirred tank, stir at room temperature for 12 minutes to obtain a textile solution, and add the textile solution to an electrospinning machine. The parameters of the electrospinning machine are: voltage of 20 kV, electrode distance of 15 cm, air humidity of 36%, and spinning to obtain composite fibers.

[0034] Step ②, preparation of modified fiber Weigh: 40.0g of composite fiber is transferred to a muffle furnace, and in an air atmosphere, the temperature is raised from room temperature to 640°C at a rate of 9°C / min, and kept warm for 2h to obtain a modified fiber precursor. Then, 20.0g of the modified fiber precursor and 96.0mL of 5wt% sodium hydroxide aqueous solution are added to the reactor, the reactor temperature is raised to 45°C, and the mixture is kept warm and soaked for 50min. After the treatment is completed, the reactor temperature is lowered to room temperature, the reaction liquid is filtered, and the filter cake is collected. After washing the filter cake 4 times with anhydrous ethanol and deionized water, the filter cake is transferred to a vacuum drying oven at a temperature of 70°C, and vacuum dried to constant weight to obtain modified fiber.

[0035] Step ③: Preparation of composite adhesive Weigh: 96.0g of ethyl orthosilicate and 450.0mL of deionized water were added to the reactor, stirred at room temperature for 12 minutes, and then a 36wt% aqueous sulfuric acid solution was added to the reactor. After adjusting the pH of the system to 3, the reactor was allowed to stand for 4 hours, and then 16.0g of aluminum isopropoxide and 16.0g of modified fiber were added to the reactor. After the reaction was completed, the reaction solution was transferred to a rotary evaporator with a salt bath temperature of 70°C, and distilled under reduced pressure until no liquid was extracted to obtain a composite adhesive.

[0036] Example 4 This embodiment provides a method for preparing a modified foaming agent for preparing a high-temperature resistant ceramic composite thermal insulation energy-saving new material, comprising the following steps: Step I: Preparation of modified microspheres Weigh 100.0 mL of deionized water and 350.0 mL of anhydrous ethanol to obtain a mixed solvent; Weigh: 40.0g of silicon carbide microspheres and 300.0mL of mixed solvent were added to the reactor, the pH of the reaction system was adjusted to 3 with boric acid and stirred at room temperature for 10 minutes, then 10.0g of methyl orthosilicate was added to the reactor, and the stirring was continued for 3 hours, and then allowed to stand for 21 hours. After the treatment was completed, the temperature of the reactor was lowered to room temperature, the reaction liquid was filtered to collect the filter cake, and the filter cake was transferred to a muffle furnace at a temperature of 700°C and kept warm for 2 hours to obtain modified microspheres.

[0037] Step II: Preparation of modified foaming agent Weigh: 30.0 g of modified microspheres, 200.0 mL of anhydrous ethanol and 3.0 g of sodium hydroxide are added to the reactor, the temperature of the reactor is raised to 40°C, 10.0 g of 3-(2,3-epoxypropoxy)propyltrimethoxysilane is added to the reactor, and the mixture is stirred for 2 hours. After the treatment is completed, the temperature of the reactor is lowered to room temperature, the reaction liquid is filtered to collect the filter cake, and the filter cake is washed 3 times with anhydrous ethanol and deionized water. The filter cake is transferred to a vacuum drying oven at a temperature of 60°C and vacuum dried to constant weight to obtain a modified foaming agent.

[0038] Example 5 This embodiment provides a method for preparing a modified foaming agent for preparing a high-temperature resistant ceramic composite thermal insulation energy-saving new material, comprising the following steps: Step I: Preparation of modified microspheres Weigh 150.0 mL of deionized water and 300.0 mL of anhydrous ethanol to obtain a mixed solvent; Weigh: 50.0g of silicon carbide microspheres and 360.0mL of mixed solvent were added to the reactor, the pH of the reaction system was adjusted to 3 with boric acid and stirred at room temperature for 12 minutes, then 20.0g of methyl orthosilicate was added to the reactor, and the stirring was continued for 4 hours, and then the mixture was allowed to stand for 24 hours. After the treatment was completed, the temperature of the reactor was lowered to room temperature, the reaction liquid was filtered to collect the filter cake, and the filter cake was transferred to a muffle furnace at a temperature of 800°C and kept warm for 2 hours to obtain modified microspheres.

[0039] Step II: Preparation of modified foaming agent Weigh: 40.0 g of modified microspheres, 240.0 mL of anhydrous ethanol and 4.0 g of sodium hydroxide are added to the reactor, the temperature of the reactor is raised to 60°C, 20.0 g of 3-(2,3-epoxypropoxy)propyltrimethoxysilane is added to the reactor, and the mixture is stirred for 3 hours. After the treatment is completed, the temperature of the reactor is lowered to room temperature, the reaction liquid is filtered to collect the filter cake, and the filter cake is washed 5 times with anhydrous ethanol and deionized water. The filter cake is transferred to a vacuum drying oven at a temperature of 80°C and vacuum dried to constant weight to obtain a modified foaming agent.

[0040] Example 6 This embodiment provides a method for preparing a modified foaming agent for preparing a high-temperature resistant ceramic composite thermal insulation energy-saving new material, comprising the following steps: Step I: Preparation of modified microspheres Weigh 120.0 mL of deionized water and 300.0 mL of anhydrous ethanol to obtain a mixed solvent; Weigh: 42.0g of silicon carbide microspheres and 320.0mL of mixed solvent were added to the reactor, the pH of the reaction system was adjusted to 3 with boric acid and stirred at room temperature for 12 minutes, then 15.0g of methyl orthosilicate was added to the reactor, and the stirring was continued for 4 hours, and then the mixture was allowed to stand for 24 hours. After the treatment was completed, the temperature of the reactor was lowered to room temperature, the reaction liquid was filtered to collect the filter cake, and the filter cake was transferred to a muffle furnace at a temperature of 750°C and kept warm for 2 hours to obtain modified microspheres.

[0041] Step II: Preparation of modified foaming agent Weigh: 36.0 g of modified microspheres, 210.0 mL of anhydrous ethanol and 3.6 g of sodium hydroxide were added to the reactor, the temperature of the reactor was raised to 50 ° C, 16.0 g of 3-(2,3-epoxypropoxy)propyltrimethoxysilane was added to the reactor, and the mixture was stirred for 3 hours. After the treatment was completed, the temperature of the reactor was lowered to room temperature, the reaction liquid was filtered to collect the filter cake, and the filter cake was washed 4 times with anhydrous ethanol and deionized water. The filter cake was transferred to a vacuum drying oven at a temperature of 70 ° C and vacuum dried to constant weight to obtain a modified foaming agent.

[0042] Example 7 This embodiment provides a method for preparing a modified ceramic raw material for preparing a high-temperature resistant ceramic composite thermal insulation energy-saving new material, comprising the following steps: Step (i) Preparation of activated kaolin Weigh: 100.0 g of kaolin and 500.0 mL of 10 wt% aqueous sulfuric acid solution are added to a stirring tank. After the temperature of the stirring tank is raised to 60°C, it is kept warm and stirred for 1 hour. After the treatment is completed, the temperature of the reaction tank is lowered to room temperature, the reaction liquid is filtered to collect the filter cake, and the filter cake is washed 3 times with anhydrous ethanol and deionized water. The filter cake is transferred to a vacuum drying oven at a temperature of 60°C and vacuum dried to constant weight to obtain activated kaolin.

[0043] Step (ii): Preparation of modified kaolin Weigh 1.0 g of cerium nitrate, 1.0 g of lanthanum nitrate, and 100.0 mL of deionized water and mix to obtain a modified solution. Weigh: 10.0 g activated kaolin and 20.0 mL modified liquid are added to a ball mill. The ball milling medium in the ball mill is zirconia balls with a particle size of 2 mm, the ball-to-material ratio is 5:1, and the ball milling is carried out at room temperature for 4 hours. After the ball milling is completed, the material is taken out and the filter cake is filtered three times with anhydrous ethanol and deionized water. The material is then transferred to a vacuum drying oven at a temperature of 60°C and vacuum dried to constant weight to obtain modified kaolin.

[0044] Step (iii) Preparation of modified ceramic raw materials Weigh 10 parts of corundum, 60 parts of mullite and 5 parts of modified kaolin in parts by weight, and mix them to obtain a modified ceramic raw material.

[0045] Example 8 This embodiment provides a method for preparing a modified ceramic raw material for preparing a high-temperature resistant ceramic composite thermal insulation energy-saving new material, comprising the following steps: Step (i) Preparation of activated kaolin Weigh: 100.0 g of kaolin and 600.0 mL of 10 wt% aqueous sulfuric acid solution are added to a stirring tank. After the temperature of the stirring tank is raised to 80°C, it is kept warm and stirred for 2 hours. After the treatment is completed, the temperature of the reaction tank is lowered to room temperature, the reaction liquid is filtered to collect the filter cake, and the filter cake is washed 5 times with anhydrous ethanol and deionized water. The filter cake is transferred to a vacuum drying oven at a temperature of 80°C and vacuum dried to constant weight to obtain activated kaolin.

[0046] Step (ii): Preparation of modified kaolin Weigh 2.0 g of cerium nitrate, 2.0 g of lanthanum nitrate, and 100.0 mL of deionized water and mix to obtain a modified solution. Weigh: 10.0 g activated kaolin and 30.0 mL modified liquid are added to a ball mill. The ball milling medium in the ball mill is zirconia balls with a particle size of 3 mm, the ball-to-material ratio is 8:1, and the ball milling is carried out at room temperature for 6 hours. After the ball milling is completed, the material is taken out and the filter cake is filtered 5 times with anhydrous ethanol and deionized water. The material is transferred to a vacuum drying oven at a temperature of 80°C and vacuum dried to constant weight to obtain modified kaolin.

[0047] Step (iii) Preparation of modified ceramic raw materials Weigh 25 parts of corundum, 75 parts of mullite and 6 parts of modified kaolin in parts by weight, and mix them to obtain a modified ceramic raw material.

[0048] Example 9 This embodiment provides a method for preparing a modified ceramic raw material for preparing a high-temperature resistant ceramic composite thermal insulation energy-saving new material, comprising the following steps: Step (i) Preparation of activated kaolin Weigh: 10.0 g of kaolin and 56.0 mL of 10 wt% sulfuric acid aqueous solution are added to a stirring tank. After the temperature of the stirring tank is raised to 70 ° C, it is kept warm and stirred for 2 hours. After the treatment is completed, the temperature of the reaction tank is lowered to room temperature, the reaction liquid is filtered to collect the filter cake, and the filter cake is washed 4 times with anhydrous ethanol and deionized water. After that, the filter cake is transferred to a vacuum drying oven at a temperature of 70 ° C, and vacuum dried to constant weight to obtain activated kaolin.

[0049] Step (ii): Preparation of modified kaolin Weigh 1.6 g of cerium nitrate, 1.6 g of lanthanum nitrate, and 100.0 mL of deionized water and mix to obtain a modified solution. Weigh: 10.0 g activated kaolin and 25.0 mL modified liquid are added to a ball mill. The ball milling medium in the ball mill is zirconia balls with a particle size of 2 mm, the ball-to-material ratio is 6:1, and the ball milling is carried out at room temperature for 5 hours. After the ball milling is completed, the material is taken out and the filter cake is filtered 4 times with anhydrous ethanol and deionized water. The material is then transferred to a vacuum drying oven at a temperature of 70°C and vacuum dried to constant weight to obtain modified kaolin.

[0050] Step (iii) Preparation of modified ceramic raw materials 16 parts of corundum, 72 parts of mullite and 6 parts of modified kaolin were weighed and mixed to obtain a modified ceramic raw material.

[0051] Example 10 This embodiment provides a method for preparing a high-temperature resistant ceramic composite thermal insulation energy-saving new material, comprising the following steps: Step 1: Prepare ceramic slurry 80 parts of the modified ceramic raw material prepared in Example 7, 4 parts of the composite adhesive prepared in Example 1, and 20 parts of deionized water were weighed and added to a stirring kettle. After stirring at room temperature for 10-15 minutes, 1 part of polyvinyl alcohol and 1 part of silica sol were added. After stirring for 20 minutes, 5 parts of the modified foaming agent prepared in Example 4 were added and stirred for 10 minutes to obtain a ceramic slurry.

[0052] Step 2: Preparation of high temperature resistant ceramics The ceramic slurry is poured into the mold. After vacuum degassing, the mold is transferred to a calcining furnace. The calcining furnace is heated to 80°C at a heating rate of 8°C / min, kept warm for 2 hours, and then heated to 300°C at a heating rate of 5°C / min. After keeping warm for 1 hour, the temperature is continued to be heated to 950°C at a heating rate of 10°C / min, kept warm for 30 minutes, and finally heated to 1250°C at a heating rate of 5°C / min, kept warm for 1.5 hours, and demolded to obtain high-temperature resistant ceramics.

[0053] Example 11 This embodiment provides a method for preparing a high-temperature resistant ceramic composite thermal insulation energy-saving new material, comprising the following steps: Step 1: Prepare ceramic slurry 88 parts of the modified ceramic raw material prepared in Example 8, 5 parts of the composite adhesive prepared in Example 2, and 30 parts of deionized water were weighed and added to a stirring kettle. After stirring at room temperature for 15 minutes, 2 parts of polyvinyl alcohol and 3 parts of silica sol were added. After stirring for 25 minutes, 8 parts of the modified foaming agent prepared in Example 5 were added and stirred for 20 minutes to obtain a ceramic slurry.

[0054] Step 2: Preparation of high temperature resistant ceramics The ceramic slurry is poured into the mold. After vacuum degassing, the mold is transferred to a calcining furnace. The calcining furnace is heated to 100°C at a heating rate of 10°C / min, and kept warm for 4 hours. Then, the temperature is increased to 400°C at a heating rate of 6°C / min. After keeping warm for 1 hour, the temperature is continued to be increased to 1050°C at a heating rate of 10°C / min, and kept warm for 40 minutes. Finally, the temperature is increased to 1350°C at a heating rate of 8°C / min, and kept warm for 2.5 hours. The mold is then demolded to obtain high-temperature resistant ceramics.

[0055] Example 12 This embodiment provides a method for preparing a high-temperature resistant ceramic composite thermal insulation energy-saving new material, comprising the following steps: Step 1: Prepare ceramic slurry 81 parts of the modified ceramic raw material prepared in Example 9, 5 parts of the composite adhesive prepared in Example 3, and 25 parts of deionized water were weighed and added to a stirring kettle. After stirring at room temperature for 12 minutes, 2 parts of polyvinyl alcohol and 2 parts of silica sol were added. After stirring for 24 minutes, 6 parts of the modified foaming agent prepared in Example 6 were added and stirred for 16 minutes to obtain a ceramic slurry.

[0056] Step 2: Preparation of high temperature resistant ceramics The ceramic slurry is poured into the mold. After vacuum degassing, the mold is transferred to a calcining furnace. The calcining furnace is heated to 100°C at a heating rate of 9°C / min, and kept warm for 3 hours. Then, the temperature is increased to 400°C at a heating rate of 5°C / min, and kept warm for 1 hour. Then, the temperature is continued to be increased to 1000°C at a heating rate of 10°C / min, and kept warm for 35 minutes. Finally, the temperature is increased to 1325°C at a heating rate of 6°C / min, and kept warm for 2 hours. The high-temperature resistant ceramic is demolded.

[0057] Comparative Example 1 The difference between this comparative example and Example 12 is that in the modified ceramic raw material used in step 1, an equal amount of kaolin is used to replace the modified kaolin.

[0058] Comparative Example 2 The difference between this comparative example and Example 12 is that the modified fiber is not used in the composite adhesive used in step 1.

[0059] Comparative Example 3 The difference between this comparative example and Example 12 is that the modified foaming agent is omitted in step 1 and replaced with an equal amount of silicon carbide microspheres.

[0060] Performance testing: The compressive strength, thermal expansion coefficient, and thermal shock temperature of the high-temperature resistant ceramics prepared in Examples 10-12 and Comparative Examples 1-3 were measured with reference to the standard JC / T 2135-2012 "Honeycomb Ceramic Thermal Storage Body"; The infrared emissivity and thermal conductivity of the high-temperature resistant ceramics prepared in Examples 10-12 and Comparative Examples 1-3 were measured with reference to the standard JC / T 2137-2012 "Honeycomb Ceramic Thermal Storage Body"; specific data are shown in Table 1.

[0061] Table 1 - Performance test data of each sample

[0062] Data Analysis: After comparing and analyzing the data in Table 1, it can be found that the C-axis compressive strength of the high-temperature resistant ceramics prepared by the present invention is 26 MPa, the thermal expansion coefficient is 4.0×10 -7 ℃-1 , thermal shock resistance temperature is 518℃, infrared radiation rate is 92% and thermal conductivity is 0.07W·(m·K) -1 , all data are better than those of the comparative example; By comparing the data in Table 1, it can be found that the compression resistance of the high-temperature resistant ceramics prepared in Comparative Examples 1-3 is significantly lower than that of the high-temperature resistant ceramics prepared in Example 12, indicating that: The kaolin used in Comparative Example 1 was not activated with sulfuric acid and coordinated with rare earths, lacking rare earth-oxygen-silicon / aluminum bonds, resulting in fewer defect sites, low secondary mullite formation efficiency, insufficient skeleton density, weak inter-particle bonding, decreased compressive strength, and low surface hydroxyl activity, resulting in poor bonding with the adhesive aluminum-oxygen-silicon bonds, easy formation of microcracks at the interface, increased stress concentration under compressive loads, and easy fracture of the material, resulting in lower compressive strength than that of the embodiment; The composite adhesive used in Comparative Example 2 does not contain modified fibers and relies solely on a silicon-aluminum network for bonding. This lacks crack deflection and bridging mechanisms, resulting in failure to disperse stress, rapid crack propagation, severe stress concentration, and decreased compressive strength and toughness. Furthermore, the lack of chemical bonding between the fiber hydroxyl groups and the adhesive results in low interfacial strength and insufficient cohesion, leading to easy fracture under compressive loads and lower compressive performance than in the examples. In Comparative Example 3, the porous silicon structure produced after silicon carbide foaming has no polysiloxane coating protection, the pores are easy to collapse under compressive load, the compressive strength is reduced, and there is no covalent bond modification of silane coupling agent, the compatibility with the matrix interface is poor, the bonding is weak, and it is easy to slip or micro-crack under compressive load, resulting in the overall compressive resistance being lower than that of the embodiment.

[0063] By comparing the data in Table 1, it can be found that the high temperature resistance of the high temperature resistant ceramics prepared in Comparative Examples 1-3 is significantly lower than that of the high temperature resistant ceramics prepared in Example 12, indicating that: The kaolin used in Comparative Example 1 lacks rare earth stabilization, has limited secondary mullite formation, poor skeleton thermal stability, a high thermal expansion coefficient of the decomposition product, increased overall thermal expansion, and lacks crystal structure stability. It is prone to phase change or microcracks under thermal stress, has reduced thermal shock resistance, and is easily peeled off during rapid heating / sudden cooling, resulting in poorer high-temperature resistance than that of the embodiment. Comparative Example 2 has no fiber stress buffer net. Thermal stress concentration leads to crack propagation, thermal shock toughness decreases, and it is easy to peel off during rapid heating / sudden cooling. The fiber hydroxyl group and aluminum oxide silicon bond are missing, the interface stability is poor, and the thermal expansion non-uniformity increases, resulting in poor high temperature resistance compared with the embodiment. In comparative example 3, the porous silicon structure has no silicon structure coating, the pores are easy to collapse under thermal stress, the thermal strain buffering capacity is reduced, the thermal shock resistance is weakened, cracks are easy to appear during rapid heating / sudden cooling, and there is no silane coupling agent modification, the interface bonding is poor, and the thermal expansion non-uniformity is increased, resulting in high temperature resistance lower than that of the embodiment.

[0064] By comparing the data in Table 1, it can be found that the energy-saving performance of the high-temperature resistant ceramics prepared in Comparative Examples 1-3 is significantly lower than that of the high-temperature resistant ceramics prepared in Example 12, indicating that: The kaolin used in Comparative Example 1 contains no rare earth oxides and has low far-infrared emissivity, resulting in a decrease in radiation heat exchange efficiency. Furthermore, the kaolin has poor interfacial compatibility with the porous silicon structure, uneven porosity, increased heat conduction paths, and increased thermal conductivity. Furthermore, the kaolin has no rare earth radiation sites, weak infrared scattering ability, and large heat conduction losses, resulting in energy-saving effects far lower than those of the examples. The fibrous rare earth oxide of Comparative Example 2 is missing, the radiation active sites are reduced, the infrared emissivity is reduced, and the radiation heat exchange efficiency is reduced. In addition, the lack of fiber hydroxyl groups reduces the compatibility of the material with the porous silicon structure, the porosity is uneven, the heat conduction path is increased, and the thermal conductivity is increased. At the same time, there is no fiber thermal field regulation, the heat distribution is uneven, and the conduction loss is large, resulting in an energy saving effect lower than that of the embodiment; The porous silicon structure of Comparative Example 3 is not coated with silicon material, has a long heat conduction path, and has a higher thermal conductivity than the closed-cell structure of the embodiment. It is not modified with a silane coupling agent, has an uneven pore distribution, weak infrared scattering ability, and reduced radiation efficiency, which increases heat conduction losses, resulting in energy-saving effects significantly lower than the low thermal conductivity porous structure of the embodiment.

[0065] Finally, the present invention explains that the synergistic effect of modified kaolin, foaming agent, fiber and composite adhesive is used to construct a high-temperature resistant ceramic composite material. The modified kaolin is activated by sulfuric acid and coordinated with rare earth to form rare earth-oxygen-silicon / aluminum bonds. High-temperature sintering promotes the formation of secondary mullite, laying the foundation for a dense skeleton, providing high compressive strength and low thermal expansion coefficient. The polysiloxane of the modified foaming agent coats the porous silicon structure, and the silane coupling agent optimizes compatibility, maintaining low thermal conductivity and infrared scattering. The rare earth-titanium oxide of the modified fiber enhances toughness and resistance to thermal shock temperature by crack deflection, supplementing radiation sites. The aluminum-oxygen-silicon bonds of the composite adhesive connect the various components and strengthen interface stability. Segmented calcination integrates chemical bonding and structural functions, balancing the dense skeleton and porous structure to ensure high infrared emissivity. Each step forms a unified system through chemical coupling, structural synergy and functional integration. The absence of any component will destroy the interface continuity, structural balance or radiation efficiency, resulting in a decrease in compression resistance, high temperature resistance and energy saving performance.

[0066] The above embodiments are intended only to illustrate the technical solutions of the present application and are not intended to limit them. The present application is not limited to the precise structures described above, and the specific implementation of the present application cannot be considered to be limited to these descriptions. For those skilled in the art to which the present application belongs, any changes and modifications made without departing from the concept of the present application should be deemed to fall within the scope of protection of the present application.

Claims

1. A high temperature resistant ceramic composite thermal insulation energy-saving new material, characterized in that: The raw material composition includes the following parts by weight: 80-98 parts of modified ceramic raw materials, 5-8 parts of modified foaming agents, 4-5 parts of composite adhesives and 32-45 parts of auxiliary materials; The preparation method of the modified ceramic raw material comprises the following steps: A1. Add kaolin and 10 wt% sulfuric acid aqueous solution into a stirred tank. After the temperature of the stirred tank is raised to 60-80° C., stir at this temperature for 1-2 hours, and perform post-treatment to obtain activated kaolin. A2. Add activated kaolin and modifying solution into a ball mill, ball mill at room temperature for 4-6 hours, and post-treat to obtain modified kaolin; A3. Weigh 10-25 parts of corundum, 60-80 parts of mullite, and 5-8 parts of modified kaolin by weight, and mix them to obtain a modified ceramic raw material.

2. A high temperature resistant ceramic composite thermal insulation energy-saving new material according to claim 1, characterized in that: The auxiliary materials include the following raw materials in parts by weight: 1-2 parts of polyvinyl alcohol, 1-3 parts of silica sol, and 20-30 parts of a dispersant. In the process of preparing the modified ceramic raw material, in step A1, the amount ratio of kaolin and 10wt% sulfuric acid aqueous solution is 1g:5-6mL; in step A2, the amount ratio of activated kaolin and modifying liquid is 1g:2-3mL, wherein the modifying liquid is obtained by mixing cerium nitrate, lanthanum nitrate, and deionized water in a ratio of 1-2g:1-2g:100mL, and the ball milling medium in the ball mill is zirconia balls with a particle size of 2-3mm, and the ball-to-material ratio is 5-8:

1.

3. The high temperature resistant ceramic composite thermal insulation energy-saving new material according to claim 1, characterized in that: The preparation method of the modified foaming agent comprises the following steps: B1. Add silicon carbide microspheres and a mixed solvent into a reactor, adjust the pH of the reaction system to 3-4 with boric acid, and stir at room temperature for 10-12 minutes. Then, add methyl orthosilicate into the reactor, continue stirring for 3-4 hours, and let it stand for 21-24 hours. Post-process and obtain modified microspheres. B2. Add the modified microspheres, anhydrous ethanol and sodium hydroxide into the reactor, increase the temperature of the reactor to 40-60°C, add 3-(2,3-epoxypropoxy)propyltrimethoxysilane into the reactor, keep warm and stir for 2-3 hours, and then post-treat to obtain the modified foaming agent.

4. The high temperature resistant ceramic composite thermal insulation energy-saving new material according to claim 3, characterized in that: In step B1, the amount ratio of the silicon carbide microspheres, the mixed solvent and methyl orthosilicate is 4-5g:30-36mL:1-2g, wherein the mixed solvent is obtained by mixing deionized water and anhydrous ethanol in a volume ratio of 2-3:6-7; in step B2, the amount ratio of the modified microspheres, anhydrous ethanol, sodium hydroxide and 3-(2,3-epoxypropoxy)propyltrimethoxysilane is 3-4g:20-24mL:0.3-0.4g:1-2g.

5. The high temperature resistant ceramic composite thermal insulation energy-saving new material according to claim 1, characterized in that: The preparation method of the composite adhesive comprises the following steps: adding ethyl orthosilicate and deionized water into a reactor, stirring at room temperature for 10-12 minutes, adding a 30-40 wt% aqueous sulfuric acid solution into the reactor, adjusting the pH value of the system to 3-4, standing for 3-4 hours, adding aluminum isopropylate and modified fiber into the reactor, and performing post-processing to obtain the composite adhesive.

6. The high temperature resistant ceramic composite thermal insulation energy-saving new material according to claim 5, characterized in that: The preparation method of the modified fiber comprises the following steps: C1. Add yttrium nitrate, ytterbium nitrate, europium nitrate, titanium chloride, polyvinyl pyrrolidone, deionized water and anhydrous ethanol into a stirred tank, and stir at room temperature for 10-15 minutes to obtain a spinning solution; C2. adding the spinning liquid into an electrospinning machine and electrospinning to obtain composite fibers; C3, transferring the composite fiber to a tubular furnace and calcining it to obtain a modified fiber precursor; C4. Add the modified fiber precursor and 4-5 wt% sodium hydroxide aqueous solution into a reactor, increase the temperature of the reactor to 40-50° C., keep warm and soak for 40-60 minutes, and post-treat to obtain the modified fiber.

7. The high temperature resistant ceramic composite thermal insulation energy-saving new material according to claim 6, characterized in that: In step C1, the usage ratio of yttrium nitrate, ytterbium nitrate, europium nitrate, titanium chloride, polyvinyl pyrrolidone, deionized water and anhydrous ethanol is 3.8g:2.3g:4.4g:1.9g:18-20g:90-95g:90-95g; in step C2, the parameters of the electrospinning machine are: voltage of 18-20kV, electrode distance of 12-15cm, and air humidity of 35-40%.

8. The high temperature resistant ceramic composite thermal insulation energy-saving new material according to claim 6, characterized in that: In step C3, the calcination operation is as follows: the composite fiber is transferred to a muffle furnace, and in an air atmosphere, the temperature is raised from room temperature to 600-700°C at a rate of 8-10°C / min, and kept warm for 2 hours to obtain a modified fiber precursor; in step C4, the amount ratio of the modified fiber precursor and 4-5wt% sodium hydroxide aqueous solution is 1-2g:4-5mL.

9. The method for preparing a high-temperature resistant ceramic composite thermal insulation energy-saving new material according to any one of claims 1 to 8, characterized in that: The preparation method of the high temperature resistant ceramic composite thermal insulation energy-saving new material comprises the following steps: S1. Add the modified ceramic raw material, composite adhesive and dispersant to a stirring tank, stir at room temperature for 10-15 minutes, then continue to add polyvinyl alcohol and silica sol, continue to stir for 20-25 minutes, then add the modified foaming agent and stir for 10-20 minutes to obtain a ceramic slurry; S2. Pour the ceramic slurry into a mold, vacuum degas, transfer the mold to a calcining furnace, calcine in stages, and demold to obtain high-temperature resistant ceramics.

Citation Information

Patent Citations

  • A high temperature resistant inorganic fiber ceramic thermal insulation material and preparation method thereof

    CN116253578B