Nanometer heat-insulating anticorrosion high-temperature-resistant material, preparation method and application thereof

Abstract

The application discloses a kind of nano heat insulation anticorrosion high-temperature-resistant materials and preparation method and application thereof, belong to coke oven production technical field.The material includes: 40-45 parts of skeleton coarse material, 30-35 parts of skeleton fine material, 1-5 parts of plasticizer, 0.1-2 parts of shrinkage inhibitor, 0.1-2 parts of preservative, 0.1-2 parts of coagulant, 0.1-1 parts of inhibitor, 5-15 parts of filler, 15-25 parts of binder by weight fraction;The material has multistage pore structure, including the intergranular macropore formed between skeleton coarse material, the nanopore formed between skeleton coarse material and skeleton fine material and the nanopore structure inside skeleton fine material;Nano heat insulation anticorrosion high-temperature-resistant material particle size D50 is 40-100nm.To overcome the technical problems such as poor adhesion of existing coking riser inner tube high-temperature-resistant paint, poor high-low temperature strain adhesion, poor corrosion resistance and complex structure leading to inconvenience in use.

Description

TECHNICAL FIELD

[0001] The present application belongs to the technical field of coke oven production, and particularly relates to a nano heat-insulating anticorrosion high-temperature-resistant material and a preparation method and application thereof. BACKGROUND

[0002] Coke oven raw gas is a high-calorific corrosive mixture rich in methane, hydrogen sulfide and other components. In the inner cylinder of the rising pipe, there is a narrow window for temperature control: below 450 DEG C, the tar condensation will cause blockage, and above 800 DEG C, the accumulated carbon will grow into graphite. At the same time, once water leaks into the carbonization chamber, it will cause irreversible damage to the oven body. Temperature fluctuation and excessive heat exchange efficiency can easily lead to rapid cooling of the raw gas, causing coking blockage, heat exchange efficiency reduction and black smoke emission, etc., which seriously affect the production stability. Therefore, it is urgent to develop a new material for the inner wall of the rising pipe. The material should have good heat insulation performance to slow down the heat exchange and maintain the temperature of the raw gas in a reasonable range; at the same time, it must be resistant to strong corrosion of hydrogen sulfide and ammonia and other media. Due to the large fluctuation of raw gas temperature and the high extreme temperature, it should have the characteristics of high temperature resistance and high and low temperature change resistance. The inner cylinder material determines the efficiency of the raw gas treatment of the rising pipe and the normal running time of the coke oven, and has industrial application value.

[0003] To address the aforementioned problems, Chinese invention patent application CN106122681A discloses a composite high-temperature and wear-resistant flue gas conveying pipeline. An insulation layer is filled inside an outer steel pipe. An outer fixing plate and an inner fixing plate are installed within the insulation layer. A reinforcing steel ring is placed between the outer and inner fixing plates. A reinforcing steel mesh is installed on the inner wall of the insulation layer, and a fire-resistant plastic is filled inside the reinforcing steel mesh. A silicon carbide ceramic layer is installed on the inner wall of the pipe through a ceramic fixing plate. However, this design requires fixation via the steel ring and reinforcing steel plate, resulting in weak adhesion. Furthermore, the use of the silicon carbide ceramic layer leads to high thermal conductivity and poor insulation performance. Chinese utility model patent CN210176735U provides a zirconium corundum wear-resistant plastic material, including a heat-insulating outer layer, a wear-resistant inner layer, a first skeleton reinforcement layer, a second skeleton reinforcement layer, a first outer layer embedded reinforcement block, a first outer layer embedded reinforcement slot, an inner layer embedded reinforcement block, an inner layer embedded reinforcement slot, reinforcing bars, a second outer layer embedded reinforcement block, and a second outer layer embedded reinforcement slot. The construction is complex, requires a lot of mechanical reinforcement, and is inconvenient to use. Another Chinese invention patent application with publication number CN105503142A discloses a lightweight plastic material for waste heat boilers that can be constructed under extremely cold conditions. This plastic material is made by mixing expanded vermiculite, silica powder, aluminum dihydrogen phosphate solution, and CA-60 aluminate cement into ceramsite. It has high strength, good thermal shock resistance and thermal insulation performance when used for waste heat boiler lining. Although it can be constructed under extremely cold conditions, it becomes loose due to expansion, adsorbs acidic gases from raw coal gas, produces a lot of corrosion, has a short service life, and cannot meet the high-temperature operating conditions of coking riser heat exchange equipment with temperature fluctuations.

[0004] In summary, existing high-temperature resistant coatings commonly used in coking riser pipe inner cylinders suffer from technical problems such as poor adhesion, poor adhesion under high and low temperature strain, poor corrosion resistance, and inconvenience in use due to complex structure. There is an urgent need to develop a new inner cylinder material that combines excellent heat insulation, strong corrosion resistance, high temperature resistance, and convenient construction. Summary of the Invention

[0005] In order to overcome the shortcomings of the prior art, the present invention aims to provide a nano-insulating, corrosion-resistant, and high-temperature resistant material, its preparation method, and its application, so as to overcome the technical problems of poor adhesion, poor adhesion to high and low temperature strain, poor corrosion resistance, and inconvenience in use caused by complex structure of the existing high-temperature resistant coatings commonly used in the inner cylinder of coking riser pipes.

[0006] To achieve the above objectives, the present invention employs the following technical solution:

[0007] This invention provides a nano-insulating, corrosion-resistant, and high-temperature resistant material, comprising, by weight:

[0008] 40-45 parts of coarse skeleton material, 30-35 parts of fine skeleton material, 1-5 parts of plasticizer, 0.1-2 parts of shrinkage inhibitor, 0.1-2 parts of preservative, 0.1-2 parts of coagulant, 0.1-1 parts of inhibitor, 5-15 parts of filler, and 15-25 parts of binder.

[0009] The alumina content of the coarse and fine skeleton materials is ≥85%;

[0010] The nano-insulating, corrosion-resistant, and high-temperature resistant material has a multi-level porous structure, including interparticle channels formed between coarse skeleton materials, nanopores formed between coarse and fine skeleton materials, and nanopore structures inside the fine skeleton materials; the particle size D50 of the nano-insulating, corrosion-resistant, and high-temperature resistant material is 40-100 nm.

[0011] More preferably, the nano-insulating, corrosion-resistant, and high-temperature resistant material comprises, by weight parts:

[0012] 40-45 parts of coarse skeleton material, 31-34 parts of fine skeleton material, 2-4 parts of plasticizer, 0.5-1.5 parts of anti-shrinkage agent, 0.5-1.5 parts of preservative, 0.5-0.9 parts of coagulant, 0.2-0.5 parts of inhibitor, 5-15 parts of filler, and 15-25 parts of binder.

[0013] More preferably, the nano-insulating, corrosion-resistant, and high-temperature resistant material comprises, by weight parts:

[0014] 41-44 parts of coarse skeleton material, 31-34 parts of fine skeleton material, 2-4 parts of plasticizer, 0.5-1.5 parts of anti-shrinkage agent, 0.5-1.5 parts of preservative, 0.5-0.9 parts of coagulant, 0.2-0.5 parts of inhibitor, 8-12 parts of filler, and 18-23 parts of binder.

[0015] In one embodiment, the coarse skeleton material is selected from one of bauxite, cordierite, brown corundum and mullite with an alumina content ≥85%; the fine skeleton material is selected from one of bauxite and white clay with an alumina content ≥85%; and the filler is selected from one of kaolin and bentonite.

[0016] In one embodiment, the plasticizer is selected from red clay and yellow clay; the anti-shrinkage agent is selected from kyanite and wollastonite; the preservative is selected from oxalic acid, citric acid and tartaric acid; and the coagulant is selected from CA. Type 50 calcium aluminate, CA Type 60 calcium aluminate and CA One of type 70 calcium aluminate; the inhibitor is selected from one of chromium trioxide and ferric phosphate; the binder is selected from one of aluminum dihydrogen phosphate solution, aluminum sulfate solution and aluminum phosphate solution.

[0017] This invention also provides a method for preparing a nano-insulating, corrosion-resistant, and high-temperature resistant material, comprising the following steps:

[0018] The coarse skeleton material, fine skeleton material, plasticizer, shrinkage inhibitor, coagulant and filler are added in sequence and then subjected to high-energy ball milling to obtain nano powder.

[0019] A nano-binder was prepared by mixing a binder, a preservative, and an inhibitor and then emulsifying them under vacuum.

[0020] Nanoparticles and nano-binders are mixed and vacuum kneaded to obtain nano-insulated, corrosion-resistant, and high-temperature resistant materials.

[0021] In one embodiment, the nanoparticles have a particle size of 50-100 nm and a specific surface area greater than 800 m². 2 / g, with a pore size of 20-50nm.

[0022] In one embodiment, the particle size of the nano-binder is 50-100 nm.

[0023] In one embodiment, the high-energy ball mill has a revolution speed of 200-500 rpm, a rotation speed of 800-1500 rpm, a revolution-rotation speed ratio of 1:(2.3-2.5), and a high-energy ball milling time of 20-30 min.

[0024] In one embodiment, the vacuum emulsification rotation speed is 6000-8000 rpm, the vacuum degree is 0.05-0.08 MPa, and the emulsification time is 30-50 minutes.

[0025] In one embodiment, the vacuum degree of the vacuum kneading is 0.05-0.08 MPa, the rotation speed is 500-800 rpm, the feeding speed is 50-100 mL / min, and the kneading time is 40-60 minutes.

[0026] This invention also provides the application of a nano-insulating, corrosion-resistant, and high-temperature resistant material in the inner cylinder of a coking riser pipe.

[0027] Compared with the prior art, the present invention has the following beneficial effects:

[0028] This invention provides a nano-insulating, corrosion-resistant, and high-temperature resistant material. It utilizes coarse and fine skeleton materials with an alumina content ≥85%, ensuring high refractoriness and a theoretical temperature resistance exceeding 1700℃. This allows for direct contact with high-temperature raw coal gas, making it suitable for extreme high-temperature and fluctuating conditions within riser pipes, preventing cracking, pulverization, and detachment due to high temperatures. The material possesses a unique multi-level porous structure, including interparticle channels between the coarse skeleton materials, nanopores between the coarse and fine skeleton materials, and nanopores within the fine materials, combined with a particle size D50 of 40. The uniform 100nm nanostructure provides excellent synergistic effects in heat storage and insulation, effectively increasing the material's specific heat capacity, enhancing heat absorption and barrier capabilities, significantly reducing thermal conductivity, and slowing down the cooling rate of raw coal gas. This fundamentally avoids problems such as tar condensation, channel blockage, and black smoke emission, ensuring stable production. The binder uses an acidic system, compatible with acidic corrosive gases such as hydrogen sulfide and ammonia in coke oven raw gas, making it less prone to corrosion reactions. Simultaneously, the inhibitor can complex metal ions in the raw materials, further enhancing the material's corrosion resistance. The nanostructure ensures thorough bonding between the binder and powder, and the multi-level porous structure hinders the penetration of high-temperature oxygen and corrosive gases, resulting in no corrosion of the inner cylinder substrate of carbon steel and alloy steel risers, with an extremely low corrosion rate, thus solving the problem of easy corrosion of traditional materials. Plasticizers enhance material toughness, reduce high-temperature brittleness, and prevent cracking during temperature fluctuations. Anti-shrinkage agents compensate for volume changes in high-temperature ranges (300℃-400℃, 900℃-1000℃) that are prone to shrinkage and expansion, mitigating volume fluctuations in hierarchical porous structures and ensuring nanoscale stability and overall structural integrity. Preservatives extend the material's application period, facilitating on-site application. Accelerators ensure a high curing rate at low temperatures, adapting to various application conditions. Strong adhesion allows for firm adhesion even at thicknesses exceeding 10mm, eliminating the need for rivets, metal mesh, or other physical fixation, further enhancing application convenience.

[0029] In another aspect, this invention provides a method for preparing a nano-insulating, corrosion-resistant, and high-temperature resistant material. First, the heat-insulating powder, including coarse and fine skeleton materials, is nano-sized using a high-energy ball milling process. This process refines the powder to form nanoscale particles (the final material's D50 is concentrated between 40nm and 100nm, with a narrow particle size distribution). Simultaneously, a uniform multi-level porous structure is constructed, ensuring the material's nanoscale and structural uniformity. Next, a vacuum emulsification process is used to treat the binder, preservative, and inhibitor, ensuring uniform particle size and sufficient dispersion of the binder system, preventing agglomeration. Finally, a vacuum kneading process effectively removes air bubbles from the system, allowing the nano-powder to react more fully and bind more tightly with the emulsified binder system. This ensures uniform and concentrated pores within the material, guaranteeing the material's core properties such as heat insulation, high-temperature resistance, and corrosion resistance from a process perspective. To address the shortcomings of traditional thermal insulation materials, such as complex composition, inconvenient construction, poor adhesion, and weak adhesion under high and low temperature strain, this method utilizes nano-sizing to create a single-component system, simplifying construction. Simultaneously, the synergistic effect of nano-sizing, vacuum kneading, and emulsification significantly enhances material adhesion and resistance to alternating high and low temperatures, eliminating the need for auxiliary construction methods such as rivets and metal mesh, thus reducing construction difficulty and cost. The nanoscale particle size and hierarchical porous structure formed through high-energy ball milling more effectively absorb and block heat transfer, resulting in a significant reduction in thermal conductivity compared to traditional insulation materials, leading to a substantial improvement in insulation performance. Vacuum emulsification of the binder further ensures uniform particle size distribution, allowing for a more complete reaction between the binder and nanoparticles, improving the material's corrosion resistance and high-temperature resistance, ensuring it can meet the complex operating conditions of the riser pipe's inner cylinder, characterized by high temperature, strong corrosion, and large temperature fluctuations. The preparation process is simple and easy to control, enabling large-scale production. The materials prepared by this process can optimize the heat exchange efficiency of the inner cylinder of the coking riser, reduce the maintenance risks caused by tar adhesion and black smoke due to excessively low raw coal temperature, reduce maintenance costs, improve production efficiency, extend the service life of the inner cylinder of the riser, eliminate the risk of major overhaul, and have good economic applicability and broad prospects for large-scale application. Detailed Implementation

[0030] To enable those skilled in the art to understand the features and effects of the present invention, the terms and expressions mentioned in the specification are explained and defined in general below. Unless otherwise specified, all technical and scientific terms used herein have the ordinary meaning understood by those skilled in the art regarding the present invention, and in case of conflict, the definitions in this specification shall prevail.

[0031] In this document, all features defined by numerical ranges or percentage ranges, such as numerical values, quantities, contents, and concentrations, are for the sake of brevity and convenience only. Accordingly, descriptions of numerical ranges or percentage ranges should be considered as covering and specifically disclosing all possible sub-ranges and individual numerical values ​​(including integers and fractions) within those ranges.

[0032] In this article, unless otherwise specified, “contains,” “includes,” “containing,” “has,” or similar terms cover the meanings of “composed of” and “mainly composed of,” for example, “A contains a” covers the meanings of “A contains a and others” and “A contains only a.”

[0033] For the sake of brevity, not all possible combinations of the technical features in each implementation scheme or embodiment are described herein. Therefore, as long as there is no contradiction in the combination of these technical features, the technical features in each implementation scheme or embodiment can be combined arbitrarily, and all possible combinations should be considered within the scope of this specification.

[0034] This invention provides a nano-insulating, corrosion-resistant, and high-temperature resistant material, its preparation method, and its application.

[0035] One aspect provides a nano-insulating, corrosion-resistant, and high-temperature resistant material, comprising, by weight:

[0036] 40-45 parts of coarse skeleton material, 30-35 parts of fine skeleton material, 1-5 parts of plasticizer, 0.1-2 parts of anti-shrinkage agent, 0.1-2 parts of preservative, 0.1-2 parts of coagulant, 0.1-1 parts of inhibitor, 5-15 parts of filler, and 15-25 parts of binder.

[0037] The alumina content of the coarse and fine skeleton materials is ≥85%;

[0038] The nano-insulating, corrosion-resistant, and high-temperature resistant material has a multi-level porous structure, including interparticle channels formed between coarse skeleton materials, nanopores formed between coarse and fine skeleton materials, and nanopore structures inside the fine skeleton materials; the particle size D50 of the nano-insulating, corrosion-resistant, and high-temperature resistant material is 40-100 nm.

[0039] The preferred weight percentage of the skeleton material is 40-45 parts, and the most preferred weight percentage is 41-44 parts. The skeleton material is one of bauxite, cordierite, brown corundum, and mullite with an alumina content ≥85%.

[0040] The embodiments of the present invention use skeleton rough material produced by Zibo Lingdong Abrasives Co., Ltd. The alumina content of the skeleton rough material is ≥85%, the particle size is 1-3 mm, of which 1-2 mm is ≥80%.

[0041] The preferred weight percentage of the skeleton fines is 31-34 parts. The skeleton fines are made from either bauxite or white clay with an alumina content of ≥85%.

[0042] The embodiments of the present invention use bauxite produced by Lingshou Yuer Environmental Protection Technology Co., Ltd., with an alumina content ≥85% and a particle size of 60-100 mesh.

[0043] The plasticizer is preferably present in 2-4 parts by weight. The plasticizer is one of commercially available red clay and yellow clay, with an alumina content of ≥40% and a particle size of 200-325 mesh.

[0044] The shrink-proof agent is preferably present in 0.5-1.5 parts by weight. The shrink-proof agent is selected from kyanite and wollastonite, with a particle size of 200-325 mesh.

[0045] The preservative is preferably present in an amount of 0.5-1.5 parts by weight. The preservative is selected from one of oxalic acid, citric acid, and tartaric acid.

[0046] The embodiments of the present invention use commercially available oxalic acid with a content of 99.6%.

[0047] The preferred weight percentage of the coagulant accelerator is 0.5-0.9 parts. The coagulant accelerator is selected from CA. Type 50 calcium aluminate, CA Type 60 calcium aluminate and CA One of the 70-type calcium aluminate, with an aluminum oxide content of ≥50%.

[0048] The inhibitor is preferably present in an amount of 0.2-0.5 parts by weight. The inhibitor is selected from chromium trioxide and ferric phosphate.

[0049] The filler is preferably selected from kaolin and bentonite, with a particle size of 200-325 mesh. The filler is preferably selected from kaolin and bentonite.

[0050] The binder is preferably 15-25 parts by weight, and most preferably 18-23 parts by weight. The binder is selected from one of aluminum dihydrogen phosphate solution, aluminum sulfate solution, and aluminum phosphate solution.

[0051] This invention provides a nano-insulating, corrosion-resistant, and high-temperature resistant material for the inner cylinder of a coking riser pipe. From the raw material perspective, the coarse skeleton material, represented by brown fused alumina, and the fine skeleton material, represented by bauxite, are ball-milled. This process creates intergranular channels between the coarse skeleton materials and nanoporous structures between the coarse and fine skeleton materials, while also containing nanoporous structures within the fine skeleton materials themselves. The high alumina content of the skeleton raw materials ensures the material possesses high refractoriness and excellent high-temperature resistance. Through nano-processing, the channel structure and the uniform, highly concentrated nanostructures can synergistically enhance heat storage, giving the material a higher specific heat capacity, allowing it to absorb more heat, and thus achieving excellent thermal insulation performance.

[0052] Plasticizers (such as red clay) possess strong plasticizing properties in the system, ensuring the material's toughness during use and reducing its brittleness at high temperatures. During high-temperature use, materials exhibit significant shrinkage in the 300-400℃ and 900-1000℃ ranges, followed by rapid expansion. Anti-shrinkage agents (such as kyanite), containing a large amount of silica, can expand rapidly, compensating for volume changes in the pore and nanopore structures, and ensuring the nanoscale stability of the material during use. Preservatives (such as oxalic acid) can extend the construction period and facilitate construction operations; setting accelerators (such as calcium aluminate) ensure the material's curing rate at low temperatures; and inhibitors (such as ferric phosphate) can complex iron ions in the raw materials, improving the material's corrosion resistance. The preferred binder is an aluminum dihydrogen phosphate system, which is an acidic system and has a good affinity for acidic gases in the raw coal gas in the coking riser pipe. It will not cause corrosion due to differences in the acidity or alkalinity of the system. After the binder is nano-sized, it is fully combined with the powder through vacuum kneading, which can further ensure the nano-size stability of the material and ensure the overall performance stability of the nano-insulation, corrosion-resistant and high-temperature resistant material used in the inner cylinder of the riser pipe.

[0053] On the other hand, a method for preparing a nano-insulating, corrosion-resistant, and high-temperature resistant material is provided, comprising the following steps:

[0054] S1. Preparation of nanoparticles: Using a CGN-1000 high-energy ball mill, with a revolution speed of 200-500 rpm and a rotation speed of 800-1500 rpm, and a revolution-rotation speed ratio of 1:(2.3-2.5), the coarse skeleton material, fine skeleton material, plasticizer, anti-shrinkage agent, coagulant, and filler were sequentially added to the ball mill jar for high-energy ball milling for 20-30 minutes. The resulting nanoparticles, with a particle size of 50-100 nm, were measured using a laser nanoparticle size analyzer. The specific surface area, pore volume, and pore size were then measured using a fully automated physical adsorption analyzer. The specific surface area was greater than 800 m² / s. 2 A product is considered qualified if its average pore size is between 20-50 nm per gram.

[0055] S2, Preparation of nano-binder: Add a predetermined amount of binder, preservative and inhibitor to a vacuum emulsifier, set the rotation speed to 6000-8000 rpm and the vacuum degree to 0.05-0.08 MPa, and perform vacuum emulsification for 30-50 minutes. The particle size is qualified by laser nanoparticle size analyzer, which shows a particle size of 50-100 nm. This achieves nano-scale binder, which has stronger adhesion, requires less material and has a lower cost.

[0056] S3, Preparation of nano-insulating, corrosion-resistant and high-temperature resistant materials: The nano powder prepared in S1 is placed in a vacuum kneader, the vacuum degree is 0.05-0.08MPa, the rotation speed is 500-800 rpm, and the nano binder prepared in S2 is slowly added through a liquid feed pump at a feeding rate of 50-100mL / min. After the nano binder is added, knead for 40-60 minutes to obtain nano-insulating, corrosion-resistant and high-temperature resistant materials.

[0057] To address the shortcomings of traditional thermal insulation materials, such as poor adhesion of high-temperature resistant materials, poor adhesion under high and low temperature strain, poor corrosion resistance, and inconvenience caused by complex composition, as well as the problems of large temperature fluctuations in the inner cylinder of coking riser pipes, complex raw coal gas composition, many types and high content of corrosive gases, and the need for physical auxiliary construction methods such as rivets and metal mesh for traditional thermal insulation materials, this invention provides a method for preparing a nano-insulating, corrosion-resistant, and high-temperature resistant thermal insulation material.

[0058] This method utilizes nano-sizing of the insulating powder and binder to produce a single-component, high-temperature resistant, corrosion-resistant rising pipe inner cylinder insulation material. This facilitates construction, enhances the adhesion of the high-temperature resistant material, and improves adhesion under high and low temperature strain. High-energy ball milling of the insulating powder creates nano-sized particles and a multi-level porous structure, allowing heat flow to be absorbed during conduction, effectively blocking heat transfer and giving the material excellent insulation performance. Simultaneously, it improves the high-temperature resistance and corrosion resistance of the rising pipe inner cylinder insulation material, meeting the requirements of various complex operating conditions, increasing the heat exchange efficiency of the coking rising pipe inner cylinder, reducing maintenance risks caused by black smoke emissions due to excessively low raw coal temperatures, reducing maintenance costs, increasing production efficiency, and demonstrating the feasibility of large-scale production.

[0059] The binder was emulsified to further ensure the uniform distribution of particle size. The resulting material was tested and found that the D50 was concentrated between 40-100nm and uniformly distributed. The thermal conductivity was reduced by orders of magnitude compared with traditional thermal insulation materials, resulting in excellent thermal insulation performance. The excellent thermal insulation performance of the material is the result of the combined effect of component ratio, hierarchical pore structure design and nano-sizing.

[0060] The corrosion resistance test of the nano-insulating, corrosion-resistant, and high-temperature resistant material prepared by this invention on carbon steel surfaces shows that its corrosion rate is very low, with virtually no corrosion. This is because the binder has a more uniform particle size during the nano-sizing process, resulting in a more complete reaction with the nano-powder; the nano-powder has a high specific surface area, leading to a more complete reaction with the nano-binder, reducing corrosion to substrates such as carbon steel and alloy steel, and ensuring that the material does not corrode the metal matrix—an advantage not possessed by ordinary insulation materials. Simultaneously, the material's unique inter-particle pore structure and intra-particle nanopore structure can hinder the conduction of high-temperature oxygen, adsorbing it and preventing it from contacting the inner cylinder of the riser pipe, thus avoiding corrosion of the metal material by high-temperature oxygen.

[0061] The material prepared by this invention undergoes high-energy ball milling of powder and vacuum emulsification treatment with binder, resulting in a more complete and uniform reaction. The material has uniform and concentrated internal pores and a narrow particle size range. This particle size distribution ensures uniform heat conduction and absorption within the insulation layer, thereby providing higher temperature resistance. Theoretically, it can directly contact high-temperature raw coal gas and withstand temperatures exceeding 1700℃, ensuring the safety of the inner cylinder of the riser pipe and making its service life consistent with that of the riser pipe body, thus eliminating the risk of major overhauls.

[0062] Finally, the material prepared by this invention is simple and easy to construct, and still has strong adhesion when the construction thickness exceeds 10mm, which is significantly different from traditional thermal insulation materials.

[0063] The present invention will be further illustrated below with reference to specific embodiments. It should be understood that these embodiments are for illustrative purposes only and are not intended to limit the scope of the invention. Furthermore, it should be understood that after reading the teachings of this invention, those skilled in the art can make various alterations or modifications to the invention, and these equivalent forms also fall within the scope defined in this application.

[0064] The following examples use instruments and equipment conventional in the art. Experimental methods in the following examples, unless otherwise specified, are generally performed under conventional conditions or as recommended by the manufacturer. All raw materials used in the following examples are conventional commercially available products with specifications conventional in the art. In this specification and the following examples, unless otherwise specified, "%" refers to weight percentage, "parts" refers to parts by weight, and "ratio" refers to weight proportion.

[0065] Example 1:

[0066] This embodiment provides a nano-insulating, corrosion-resistant, and high-temperature resistant material, comprising the following components by weight: 42.0 parts brown corundum, 32.0 parts bauxite, 3 parts red clay, 1.2 parts wollastonite, 0.9 parts oxalic acid, and 0.6 parts CA. Calcium aluminate type 50, 0.3 parts ferric phosphate, 10 parts kaolin, and 20 parts of a substance with a density of 1.47 g / cm³ 3 Aluminum dihydrogen phosphate solution.

[0067] This embodiment presents a method for preparing a nano-insulating, corrosion-resistant, and high-temperature resistant material, comprising the following steps:

[0068] S1001, Preparation of Nanoparticles: A CGN-1000 high-energy ball mill was used with a revolution speed of 400 rpm, a rotation speed of 1000 rpm, and a revolution-rotation speed ratio of 1:2.5 to grind 1-3 mm brown corundum, 80 mesh bauxite, 300 mesh red clay, 300 mesh wollastonite, and CA... Type 50 calcium aluminate and 300-mesh kaolin were sequentially added to a ball mill jar and subjected to high-energy ball milling for 25 minutes. The resulting nanoparticle size was measured using a laser nanoparticle size analyzer, yielding nanoparticles with an average particle size of 75 nm. The specific surface area and pore size were further analyzed using a fully automated physical adsorption analyzer, with a specific surface area greater than 893 m². 2 / g, with an average pore size of 32nm.

[0069] S1002, Preparation of nano-binder: A predetermined amount of aluminum dihydrogen phosphate solution, oxalic acid and ferric phosphate were added to a vacuum emulsifier. The rotation speed was set to 7000 rpm and the vacuum degree to 0.06 MPa. Vacuum emulsification was carried out for 40 minutes. The average particle size was measured by a laser nanoparticle size analyzer and was found to be 67.7 nm, which is qualified. The preparation of nano-binder was completed.

[0070] S1003, Preparation of nano-insulating, corrosion-resistant and high-temperature resistant material: The nano powder prepared in S1001 is placed in a vacuum kneader, the vacuum degree is 0.06MPa, the rotation speed is 600 rpm, and the nano binder prepared in S1002 is slowly added through a liquid feed pump at a feed rate of 75mL / min. After the nano binder is added, knead for 50 minutes to obtain the nano-insulating, corrosion-resistant and high-temperature resistant material for the inner cylinder of the coking riser pipe.

[0071] Example 2:

[0072] This embodiment provides a nano-insulating, corrosion-resistant, and high-temperature resistant material, comprising the following components by weight: 42.0 parts mullite, 32.0 parts bauxite, 3 parts red clay, 1.2 parts wollastonite, 0.9 parts oxalic acid, and 0.6 parts CA. Calcium aluminate type 50, 0.3 parts ferric phosphate, 10 parts kaolin, and 20 parts of a substance with a density of 1.47 g / cm³ 3 Aluminum dihydrogen phosphate solution.

[0073] This embodiment presents a method for preparing a nano-insulating, corrosion-resistant, and high-temperature resistant material, comprising the following steps:

[0074] S2001, Preparation of Nanoparticles: A CGN-1000 high-energy ball mill was used with a revolution speed of 400 rpm, a rotation speed of 1000 rpm, and a revolution-rotation speed ratio of 1:2.5 to grind 1-3 mm mullite, 80 mesh bauxite, 300 mesh red clay, 300 mesh wollastonite, and CA... Type 50 calcium aluminate and 300-mesh kaolin were sequentially added to a ball mill jar and subjected to high-energy ball milling for 25 minutes. The resulting nanoparticle size was measured using a laser nanoparticle size analyzer, yielding nanoparticles with an average particle size of 70.2 nm. The specific surface area and pore size were further analyzed using a fully automated physical adsorption analyzer, showing a specific surface area greater than 867 m². 2 / g, with an average pore size of 22nm.

[0075] S2002, Preparation of nano-binder: A predetermined amount of aluminum dihydrogen phosphate solution, oxalic acid and ferric phosphate were added to a vacuum emulsifier. The rotation speed was set to 7000 rpm and the vacuum degree to 0.06 MPa. Vacuum emulsification was carried out for 40 minutes. The average particle size was measured by a laser nanoparticle size analyzer and was found to be 67.7 nm, which is qualified. The preparation of nano-binder was completed.

[0076] S2003, Preparation of nano-insulating, corrosion-resistant and high-temperature resistant material: The nano powder prepared in S2001 is placed in a vacuum kneader, the vacuum degree is 0.06MPa, the rotation speed is 600 rpm, and the nano binder prepared in S2002 is slowly added through a liquid feed pump at a feed rate of 75mL / min. After the nano binder is added, knead for 50 minutes to obtain the nano-insulating, corrosion-resistant and high-temperature resistant material for the inner cylinder of the coking riser pipe.

[0077] Example 3:

[0078] This embodiment provides a nano-insulating, corrosion-resistant, and high-temperature resistant material, comprising the following components by weight: 42.0 parts of bauxite, 32.0 parts of white clay, 3 parts of red clay, 1.2 parts of wollastonite, 0.9 parts of oxalic acid, and 0.6 parts of CA. Calcium aluminate type 50, 0.3 parts ferric phosphate, 10 parts kaolin, and 20 parts of a substance with a density of 1.47 g / cm³ 3 Aluminum dihydrogen phosphate solution.

[0079] This embodiment presents a method for preparing a nano-insulating, corrosion-resistant, and high-temperature resistant material, comprising the following steps:

[0080] S3001, Preparation of Nanoparticles: A CGN-1000 high-energy ball mill was used with a revolution speed of 400 rpm, a rotation speed of 1000 rpm, and a revolution-rotation speed ratio of 1:2.5 to mix bauxite, 80-mesh white clay, 300-mesh red clay, 300-mesh wollastonite, and CA... Type 50 calcium aluminate and 300-mesh kaolin were sequentially added to a ball mill jar and subjected to high-energy ball milling for 25 minutes. The resulting nanoparticle size was measured using a laser nanoparticle size analyzer, yielding nanoparticles with an average particle size of 75 nm. The specific surface area and pore size were further analyzed using a fully automated physical adsorption analyzer, with a specific surface area greater than 893 m². 2 / g, with an average pore size of 32nm.

[0081] S3002, Preparation of nano-binder: A predetermined amount of aluminum dihydrogen phosphate solution, oxalic acid and ferric phosphate were added to a vacuum emulsifier. The rotation speed was set to 7000 rpm and the vacuum degree to 0.06 MPa. Vacuum emulsification was carried out for 40 minutes. The average particle size was measured by a laser nanoparticle size analyzer and was found to be 67.7 nm, which is qualified. The preparation of nano-binder was completed.

[0082] S3003, Preparation of nano-insulating, corrosion-resistant and high-temperature resistant material: The nano powder prepared in S3001 is placed in a vacuum kneader, the vacuum degree is 0.06MPa, the rotation speed is 600 rpm, and the nano binder prepared in S3002 is slowly added through a liquid feed pump at a feed rate of 75mL / min. After the nano binder is added, knead for 50 minutes to obtain the nano-insulating, corrosion-resistant and high-temperature resistant material for the inner cylinder of the coking riser pipe.

[0083] Example 4:

[0084] This embodiment provides a nano-insulating, corrosion-resistant, and high-temperature resistant material, comprising the following components by weight: 42.0 parts brown corundum, 32.0 parts bauxite, 3 parts yellow clay, 1.2 parts kyanite, 0.9 parts oxalic acid, and 0.6 parts CA. Calcium aluminate type 60, 0.3 parts ferric phosphate, 10 parts kaolin, and 20 parts of a substance with a density of 1.47 g / cm³ 3 Aluminum dihydrogen phosphate solution.

[0085] This embodiment presents a method for preparing a nano-insulating, corrosion-resistant, and high-temperature resistant material, comprising the following steps:

[0086] S4001, Preparation of Nanopowder: A CGN-1000 high-energy ball mill was used with a revolution speed of 400 rpm, a rotation speed of 1000 rpm, and a revolution-to-rotation speed ratio of 1:2.5. Brown corundum (1-3 mm particle size), 80-mesh bauxite, 300-mesh yellow clay, 300-mesh kyanite, CA-60 calcium aluminate, and 300-mesh kaolin were sequentially added to the mill jar and ball-milled for 25 minutes. The average particle size was measured to be 75 nm using a laser nanoparticle size analyzer. The specific surface area and pore size were further analyzed using a fully automated physical adsorption analyzer; the specific surface area was greater than 814 m². 2 / g, with an average pore size of 39.4nm.

[0087] S4002, Preparation of nano-binder: Add a predetermined amount of aluminum dihydrogen phosphate solution, oxalic acid and ferric phosphate to a vacuum emulsifier, set the rotation speed to 7000 rpm and the vacuum degree to 0.06 MPa, and perform vacuum emulsification for 40 minutes. The average particle size was measured by a laser nanoparticle size analyzer and was found to be 67.7 nm, which is qualified. The preparation of nano-binder is complete.

[0088] S4003, Preparation of nano-insulating, corrosion-resistant and high-temperature resistant material: The nano powder prepared in S4001 is placed in a vacuum kneader, the vacuum degree is 0.06MPa, the rotation speed is 600 rpm, and the nano binder prepared in S4002 is slowly added through a liquid feed pump at a feed rate of 75mL / min. After the nano binder is added, knead for 50 minutes to obtain nano-insulating, corrosion-resistant and high-temperature resistant material for the inner cylinder of the coking riser pipe.

[0089] Example 5:

[0090] This embodiment provides a nano-insulating, corrosion-resistant, and high-temperature resistant material, comprising the following components by weight: 42.0 parts brown corundum, 32.0 parts bauxite, 3 parts red clay, 1.2 parts kyanite, 0.9 parts citric acid, and 0.6 parts CA. Calcium aluminate type 50, 0.3 parts ferric phosphate, 10 parts kaolin, and 20 parts of a substance with a density of 1.47 g / cm³ 3 Aluminum dihydrogen phosphate solution.

[0091] This embodiment presents a method for preparing a nano-insulating, corrosion-resistant, and high-temperature resistant material, comprising the following steps:

[0092] S5001, Preparation of Nanoparticles: A CGN-1000 high-energy ball mill was used with a revolution speed of 400 rpm, a rotation speed of 1000 rpm, and a revolution-rotation speed ratio of 1:2.5 to grind 1-3 mm brown corundum, 80 mesh bauxite, 300 mesh red clay, 300 mesh kyanite, and CA... Type 50 calcium aluminate and 300-mesh kaolin were sequentially added to a ball mill jar and subjected to high-energy ball milling for 25 minutes. The resulting nanoparticle size was measured using a laser nanoparticle size analyzer, yielding nanoparticles with an average particle size of 75 nm. The specific surface area and pore size were further analyzed using a fully automated physical adsorption analyzer, showing a specific surface area greater than 824.5 m². 2 / g, with an average pore size of 36.9nm.

[0093] S5002, Preparation of nano-binder: Add a predetermined amount of aluminum dihydrogen phosphate solution, citric acid and ferric phosphate to a vacuum emulsifier, set the rotation speed to 7000 rpm and the vacuum degree to 0.06 MPa, and perform vacuum emulsification for 40 minutes. The average particle size was measured by a laser nanoparticle size analyzer and was found to be 67.7 nm, which is qualified. The preparation of nano-binder is complete.

[0094] S5003, Preparation of nano-insulating, corrosion-resistant and high-temperature resistant material: The nano powder prepared in S5001 is placed in a vacuum kneader, the vacuum degree is 0.06MPa, the rotation speed is 600 rpm, and the nano binder prepared in S5002 is slowly added through a liquid feed pump at a feed rate of 75mL / min. After the nano binder is added, knead for 50 minutes to obtain nano-insulating, corrosion-resistant and high-temperature resistant material for the inner cylinder of the coking riser pipe.

[0095] Example 6:

[0096] This embodiment provides a nano-insulating, corrosion-resistant, and high-temperature resistant material, comprising the following components by weight: 42.0 parts brown corundum, 32.0 parts bauxite, 3 parts red clay, 1.2 parts wollastonite, 0.9 parts oxalic acid, and 0.6 parts CA. 70 type calcium aluminate, 0.3 parts ferric phosphate, 10 parts kaolin, and 20 parts aluminum sulfate solution.

[0097] This embodiment presents a method for preparing a nano-insulating, corrosion-resistant, and high-temperature resistant material, comprising the following steps:

[0098] S6001, Preparation of Nanoparticles: A CGN-1000 high-energy ball mill was used with a revolution speed of 400 rpm, a rotation speed of 1000 rpm, and a revolution-to-rotation speed ratio of 1:2.5 to grind 1-3 mm brown corundum, 80 mesh bauxite, 300 mesh red clay, 300 mesh wollastonite, and CA... Type 70 calcium aluminate and 300-mesh kaolin were sequentially added to a ball mill jar and subjected to high-energy ball milling for 25 minutes. The resulting nanoparticle size was measured using a laser nanoparticle size analyzer, yielding nanoparticles with an average particle size of 75 nm. The specific surface area and pore size were further analyzed using a fully automated physical adsorption analyzer, with a specific surface area greater than 893 m². 2 / g, with an average pore size of 32nm.

[0099] S6002, Preparation of nano-binder: Add a predetermined amount of aluminum sulfate solution, oxalic acid and ferric phosphate to a vacuum emulsifier, set the rotation speed to 7000 rpm and the vacuum degree to 0.06 MPa, and perform vacuum emulsification for 40 minutes. The average particle size was measured by a laser nanoparticle size analyzer and was found to be 72.4 nm, which is qualified. The preparation of nano-binder is complete.

[0100] S6003, Preparation of nano-insulating, corrosion-resistant and high-temperature resistant material: The nano powder prepared in S6001 is placed in a vacuum kneader, the vacuum degree is 0.06MPa, the rotation speed is 600 rpm, and the nano binder prepared in S6002 is slowly added through a liquid feed pump at a feed rate of 75mL / min. After the nano binder is added, knead for 50 minutes to obtain the nano-insulating, corrosion-resistant and high-temperature resistant material for the inner cylinder of the coking riser pipe.

[0101] Example 7

[0102] This embodiment provides a nano-insulating, corrosion-resistant, and high-temperature resistant material, comprising the following components by weight: 42.0 parts brown corundum, 32.0 parts bauxite, 3 parts yellow clay, 1.2 parts wollastonite, 0.9 parts tartaric acid, and 0.6 parts CA. Calcium aluminate type 50, 0.3 parts ferric phosphate, 10 parts bentonite, and 20 parts of a substance with a density of 1.47 g / cm³ 3 Aluminum dihydrogen phosphate solution.

[0103] This embodiment presents a method for preparing a nano-insulating, corrosion-resistant, and high-temperature resistant material, comprising the following steps:

[0104] S7001, Preparation of Nanoparticles: A CGN-1000 high-energy ball mill was used with a revolution speed of 400 rpm, a rotation speed of 1000 rpm, and a revolution-to-rotation speed ratio of 1:2.5 to grind 1-3 mm brown corundum, 80 mesh bauxite, 300 mesh yellow clay, 300 mesh wollastonite, and CA... Type 50 calcium aluminate and 300-mesh bentonite were sequentially added to a ball mill jar and subjected to high-energy ball milling for 25 minutes. The resulting nanoparticle size was measured using a laser nanoparticle size analyzer, yielding nanoparticles with an average particle size of 69.5 nm. The specific surface area and pore size were further analyzed using a fully automated physical adsorption analyzer, with a specific surface area greater than 872.5 m². 2 / g, with an average pore size of 29.8nm.

[0105] S7002, Preparation of nano-binder: A predetermined amount of aluminum dihydrogen phosphate solution, tartaric acid and ferric phosphate were added to a vacuum emulsifier. The rotation speed was set to 7000 rpm and the vacuum degree to 0.06 MPa. Vacuum emulsification was carried out for 40 minutes. The average particle size was measured by a laser nanoparticle size analyzer and was found to be 67.7 nm, which is qualified. The preparation of nano-binder was completed.

[0106] S7003, Preparation of nano-insulating, corrosion-resistant and high-temperature resistant material: The nano powder prepared in S7001 above is placed in a vacuum kneader, the vacuum degree is 0.06MPa, the rotation speed is 600 rpm, and the nano binder prepared in S7002 is slowly added through a liquid feed pump at a feed rate of 75mL / min. After the nano binder is added, knead for 50 minutes to obtain nano-insulating, corrosion-resistant and high-temperature resistant material for the inner cylinder of the coking riser pipe.

[0107] Example 8:

[0108] This embodiment provides a nano-insulating, corrosion-resistant, and high-temperature resistant material, comprising the following components by weight: 40.0 parts brown corundum, 30.0 parts bauxite, 1 part red clay, 0.1 parts wollastonite, 0.1 parts oxalic acid, and 0.1 parts CA. Calcium aluminate type 50, 0.1 parts ferric phosphate, 5 parts kaolin, and 25 parts of a substance with a density of 1.47 g / cm³ 3 Aluminum dihydrogen phosphate solution.

[0109] The preparation method used in this embodiment is exactly the same as that in Example 1. The difference is that the revolution speed of the high-energy ball mill is 200 rpm, the rotation speed is 800 rpm, the revolution speed-rotation speed ratio is 1:2.3, and the high-energy ball milling time is 20 minutes; the vacuum emulsification speed is 6000 rpm, the vacuum degree is 0.05 MPa, and the time is 30 minutes; the conditions for adding the nano powder to the nano binder and kneading are as follows: vacuum degree is 0.05 MPa, rotation speed is 500 rpm, feed rate is 50 mL / min, and kneading time is 40 minutes.

[0110] Example 9:

[0111] This embodiment provides a nano-insulating, corrosion-resistant, and high-temperature resistant material, comprising the following components by weight: 45.0 parts cordierite, 35.0 parts bauxite, 5 parts red clay, 0.1 parts wollastonite, 2 parts oxalic acid, and 2 parts CA. 50-type calcium aluminate, 1 part ferric phosphate, 15 parts kaolin, 15 parts of a material with a density of 1.47 g / cm³ 3 Aluminum dihydrogen phosphate solution.

[0112] The preparation method used in this embodiment is exactly the same as that in Example 1. The difference is that the high-energy ball milling speed is 500 rpm, the rotation speed is 1500 rpm, the ratio of the rotation speed to the rotation speed is 1:2.3, and the high-energy ball milling time is 30 minutes; the vacuum emulsification speed is 8000 rpm, the vacuum degree is 0.08 MPa, and the time is 50 minutes; the conditions for adding the nano powder to the nano binder and kneading are as follows: vacuum degree is 0.08 MPa, rotation speed is 800 rpm, feed rate is 100 mL / min, and kneading time is 60 minutes.

[0113] Example 10:

[0114] This embodiment provides a nano-insulating, corrosion-resistant, and high-temperature resistant material, comprising the following components by weight: 41.0 parts brown corundum, 31.0 parts bauxite, 2 parts red clay, 2 parts wollastonite, 0.5 parts oxalic acid, and 0.5 parts CA. Calcium aluminate type 50, 0.2 parts chromium trioxide, 12 parts kaolin, and 23 parts with a density of 1.47 g / cm³ 3 Aluminum dihydrogen phosphate solution.

[0115] The preparation method used in this embodiment is exactly the same as that in Example 1.

[0116] Example 11:

[0117] This embodiment provides a nano-insulating, corrosion-resistant, and high-temperature resistant material, comprising the following components by weight: 44.0 parts brown corundum, 34.0 parts bauxite, 4 parts red clay, 1.5 parts wollastonite, 1.5 parts oxalic acid, and 0.9 parts CA. 50-type calcium aluminate, 0.5 parts ferric phosphate, 8 parts kaolin, and 18 parts aluminum phosphate solution.

[0118] The preparation method used in this embodiment is exactly the same as that in Example 1.

[0119] Comparative Example 1:

[0120] This comparative example provides a nano-insulating, corrosion-resistant, and high-temperature resistant material, comprising the following components by weight: 42.0 parts brown corundum, 32.0 parts bauxite, 3 parts red clay, 1.2 parts wollastonite, 0.9 parts oxalic acid, and 0.6 parts CA. Calcium aluminate type 50, 0.3 parts ferric phosphate, 10 parts kaolin, and 20 parts of a substance with a density of 1.47 g / cm³ 3 Aluminum dihydrogen phosphate solution.

[0121] The preparation method of the nano-insulating, corrosion-resistant, and high-temperature resistant material proposed in this comparative example includes the following steps:

[0122] S10001, Preparation of mixed powder: Using a mixer at 600 rpm, mix 1-3mm brown corundum, 80-mesh bauxite, 300-mesh red clay, 300-mesh wollastonite, and CA. Type 50 calcium aluminate and 300 mesh kaolin were added to a mixer and stirred for 25 minutes to obtain a mixed powder.

[0123] S10002, Preparation of modified binder: Add a predetermined amount of aluminum dihydrogen phosphate solution, oxalic acid and ferric phosphate to a homogenizer, set the speed to 7000 rpm, and the binder preparation is completed after 20 minutes.

[0124] S10003: Preparation of plastic: The mixed powder prepared in S10001 above is placed in a vacuum kneader at a speed of 600 rpm. The modified binder prepared in S10002 is added through a liquid pump. After the binder is added, the mixture is kneaded for 50 minutes to obtain the plastic.

[0125] Comparative Example 2:

[0126] This comparative example provides a nano-insulating, corrosion-resistant, and high-temperature resistant material, comprising the following components by weight: 42.0 parts brown corundum, 32.0 parts bauxite, 3 parts red clay, 1.2 parts wollastonite, 0.9 parts oxalic acid, and 0.6 parts CA. Calcium aluminate type 50, 0.3 parts ferric phosphate, 10 parts kaolin, and 20 parts of a substance with a density of 1.47 g / cm³ 3 Aluminum dihydrogen phosphate solution.

[0127] The preparation method of the nano-insulating, corrosion-resistant, and high-temperature resistant material proposed in this comparative example includes the following steps:

[0128] S20001, Preparation of mixed powder: Using a mixer at 600 rpm, mix 1-3mm brown corundum, 80-mesh bauxite, 300-mesh red clay, 300-mesh wollastonite, and CA. Type 50 calcium aluminate and 300 mesh kaolin were added to a mixer and stirred for 25 minutes to obtain a mixed powder.

[0129] S20002, Preparation of modified binder: Add a predetermined amount of aluminum dihydrogen phosphate solution, oxalic acid and ferric phosphate to a homogenizer, set the speed to 7000 rpm, and the modified binder is prepared after 20 minutes.

[0130] S20003: Preparation of plastic: The mixed powder prepared in S20001 and the modified binder prepared in S20002 are packaged separately to obtain plastic. When using, it is prepared on-site at a ratio of 4:1.

[0131] This invention provides a nano-insulating, corrosion-resistant, and high-temperature resistant material. It is easy to apply directly to the surface of ordinary carbon steel sheets, bars, and alloy substrates without the need for additional adhesives; simply ensuring the substrate is clean and dust-free is sufficient. After application, it dries at room temperature with relatively fast curing. To ensure optimal performance or meet testing requirements, curing for at least 48 hours is recommended. While high-temperature drying can accelerate the drying rate and shorten the drying time, it may not guarantee complete drying and should be used with caution.

[0132] The materials obtained in the examples and comparative examples were subjected to the following performance tests. The specific test methods and standards are as follows: (1) Thermal conductivity test

[0133] The thermal conductivity was measured using a thermal conductivity meter, with reference to GB / T 10295 "Steady-state heat flow meter method". The thermal conductivity of the materials in the comparative examples and control examples was used to evaluate their thermal insulation performance.

[0134] (2) Bond strength test

[0135] The plastics prepared in the examples and comparative examples were coated onto the surface of ordinary carbon steel sheets. After drying for 48 hours, the adhesion strength of the coating was measured using an adhesion strength tester to evaluate the bonding ability between the material and the substrate.

[0136] (3) High temperature resistance test

[0137] The actual working conditions of the inner cylinder of the coke oven raw gas riser pipe were simulated. The normal operating temperature of this inner cylinder is 800℃, which can exceed 1000℃ under dry burning conditions, and can reach 1500℃ under extreme conditions. The materials prepared in the examples and comparative examples were coated onto the surface of alloy steel sheets, and after high-temperature sintering, the coating surface was observed for phenomena such as cracking, peeling, flaking, and blistering to evaluate its high-temperature resistance.

[0138] (4) High and low temperature fastness test

[0139] To simulate the temperature fluctuations experienced during actual use of the riser pipe's inner cylinder, carbon steel specimens coated with the materials prepared in the examples and comparative examples were placed inside the riser pipe for calcination tests, with the temperature cycling over a wide range. After 17 days of continuous calcination, the specimens were removed, and the residual bond strength of the coating was measured using an adhesive strength tester to evaluate the coating bond strength of the material under alternating temperature conditions.

[0140] (5) Acid and alkali corrosion resistance test

[0141] The materials prepared in the examples and comparative examples were coated onto the surface of ordinary carbon steel sheets and dried for 72 hours before corrosion testing. Each steel sheet was first immersed in a 10% sulfuric acid solution for 24 hours, then removed and immersed in a 10% sodium hydroxide solution for 24 hours. After the test, the appearance of the coating was checked to observe for blistering, peeling, flaking, corrosion, or rust on the substrate.

[0142] (6) Particle size distribution test

[0143] The particle size of the materials prepared in the examples and comparative examples was tested using a laser nanoparticle size analyzer. The D50 (median particle size) was used as the evaluation index to compare and analyze the differences in the microstructure of the materials.

[0144] The materials prepared in the examples and comparative examples were tested for performance according to the above test methods, and the results are shown in Tables 1, 2 and 3.

[0145] Table 1

[0146] Material property test results of Examples 1-6

[0147]

[0148] Table 2

[0149] Material property test results of Examples 7-11

[0150]

[0151] Table 3

[0152] Comparative material performance test results

[0153]

[0154] Example 1 is an optimized solution that conforms to the technical solution of the present invention. Comparative Example 1 and Comparative Example 2 are traditional thermal insulation material preparation solutions. The core differences between the two are reflected in the formulation system, key preparation process, material microstructure and construction method: Example 1 adopts a single-component premixed system. The powder is nano-sized by high-energy ball milling, and the binder is dispersed at the nanoscale by vacuum emulsification process. Then, the composite is completed by vacuum kneading. The process parameters are precisely controlled throughout the process, and finally a dense material with nano-sized particles and multi-level pore structure is formed. The powder and binder react fully and no auxiliary fixation is required during construction. The thickness is more than 10 mm and still has strong adhesion.

[0155] Comparative Example 1 was a single component without nano-processing, while Comparative Example 2 was a two-component mixture (powder and binder packaged separately, mixed on-site in a 4:1 ratio). Both were prepared using ordinary mixing and stirring to produce powder, and the binder was prepared using conventional homogenizing. There were no processes such as vacuum emulsification or precise vacuum kneading. The final material had a particle size in the millimeter range, forming only a single coarse-pore structure. The particles were severely agglomerated, the components were unevenly mixed, the bond was loose, and there were a large number of interfacial voids. During construction, physical fixation with rivets, metal mesh, etc. was required, resulting in weak adhesion and cumbersome on-site operation.

[0156] The nano-hierarchical pores in Example 1 can effectively reflect scattered heat flow, with a thermal conductivity as low as 0.139 W / (m²). k) Excellent thermal insulation; the nanoparticles have a large specific surface area, ensuring sufficient contact with the binder, achieving a bonding strength of 92MPa and good resistance to high and low temperatures; the nano-binder uniformly covers the powder, and the multi-level pores can adsorb and block corrosive gases and high-temperature oxygen, achieving corrosion-free operation; the dense nanostructure can buffer high-temperature expansion stress, withstanding temperatures up to 1700℃, and the single-component premixed system has strong adhesion, requiring no auxiliary fixing and facilitating construction. In contrast, Comparative Examples 1 and 2 have coarse-porous structures with weak heat flow barrier and poor thermal insulation; the components are loosely bonded with many gaps, resulting in weak bonding strength and resistance to temperature changes, making them prone to cracking; the binder is unevenly dispersed, leading to a high corrosion rate; the loose structure causes easy particle detachment and localized overheating at high temperatures, resulting in insufficient temperature resistance, requiring physical auxiliary fixing or on-site two-component mixing, making construction cumbersome, and none of their performance characteristics are suitable for the complex working conditions of the coking riser inner cylinder.

[0157] Based on the equipment design and usage requirements of the coke oven rising pipe inner cylinder, and combined with the test results of this invention, the following conclusions can be drawn: The thermal conductivity of the material provided in the embodiments is significantly lower than that in the comparative examples, indicating that the thermal insulation performance of the material provided by this invention is superior. The bonding strength of the material provided in the embodiments is significantly higher than that of the material provided in the comparative examples, and its high-temperature resistance and high-low temperature fastness are also significantly better than those of the traditional thermal insulation material in the comparative examples, indicating that the material provided in the embodiments of this invention has good adaptability under high-temperature conditions. Comparative tests of acid and alkali corrosion resistance show that the corrosion resistance of the material provided in the embodiments of this invention is significantly better than that of the material in the comparative examples. Furthermore, particle size distribution tests show that the material provided in the embodiments of this invention is all nanoscale, while the particle size of the material in the comparative examples is millimeter-scale, which not only limits its thermal insulation and high-temperature resistance effects but also makes it inconvenient to use. In summary, the material provided in the embodiments of this invention is significantly superior to existing market products, possessing superior comprehensive performance in terms of thermal insulation, corrosion resistance, and high-temperature resistance, and can fully meet the operating requirements of the coke oven rising pipe inner cylinder.

[0158] The above content is only for illustrating the technical concept of the present invention and should not be construed as limiting the scope of protection of the present invention. Any modifications made to the technical solution based on the technical concept proposed in this invention shall fall within the scope of protection of this invention.

Claims

1. A nano-insulating, corrosion-resistant, and high-temperature resistant material, characterized in that, By weight, it includes: 40-45 parts of coarse skeleton material, 30-35 parts of fine skeleton material, 1-5 parts of plasticizer, 0.1-2 parts of shrinkage inhibitor, 0.1-2 parts of preservative, 0.1-2 parts of coagulant, 0.1-1 parts of inhibitor, 5-15 parts of filler, and 15-25 parts of binder. The alumina content of the coarse and fine skeleton materials is ≥85%; the nano heat-insulating, corrosion-resistant and high-temperature resistant material has a multi-level porous structure, including interparticle channels formed between coarse skeleton materials, nanopores formed between coarse and fine skeleton materials, and nanopore structure inside the fine skeleton materials; the particle size D50 of the nano heat-insulating, corrosion-resistant and high-temperature resistant material is 40-100nm. The binder is selected from one of aluminum dihydrogen phosphate solution, aluminum sulfate solution, and aluminum phosphate solution; The aforementioned nano-insulating, corrosion-resistant, and high-temperature resistant material is prepared by the following method: The coarse skeleton material, fine skeleton material, plasticizer, shrinkage inhibitor, coagulant and filler are added in sequence and then subjected to high-energy ball milling to obtain nano powder. A nano-binder was prepared by mixing a binder, a preservative, and an inhibitor and then emulsifying them under vacuum. Nanoparticles and nano-binders are mixed and vacuum kneaded to obtain nano-insulated, corrosion-resistant, and high-temperature resistant materials. The high-energy ball mill has a revolution speed of 200-500 rpm, a rotation speed of 800-1500 rpm, a revolution-rotation speed ratio of 1:(2.3-2.5), and a high-energy ball milling time of 20-30 min. The vacuum emulsification speed is 6000-8000 rpm, the vacuum degree is 0.05-0.08 MPa, and the emulsification time is 30-50 minutes; The vacuum degree of the vacuum kneading is 0.05-0.08 MPa, the rotation speed is 500-800 rpm, the feeding speed is 50-100 mL / min, and the kneading time is 40-60 minutes.

2. The nano-insulating, corrosion-resistant, and high-temperature resistant material according to claim 1, characterized in that, The coarse skeleton material is selected from bauxite and brown corundum; the fine skeleton material is selected from bauxite; and the filler is selected from kaolin and bentonite.

3. The nano-insulating, corrosion-resistant, and high-temperature resistant material according to claim 1, characterized in that, The plasticizer is selected from red clay and yellow clay; the anti-shrinkage agent is selected from kyanite and wollastonite; the preservative is selected from oxalic acid, citric acid and tartaric acid; the coagulant is selected from CA-50 calcium aluminate, CA-60 calcium aluminate and CA-70 calcium aluminate; and the inhibitor is selected from chromium trioxide and ferric phosphate.

4. The nano-insulating, corrosion-resistant, and high-temperature resistant material according to claim 1, characterized in that, The nanoparticles have a particle size of 50-100 nm and a specific surface area greater than 800 m². 2 / g, with a pore size of 20-50nm.

5. The nano-insulating, corrosion-resistant, and high-temperature resistant material according to claim 1, characterized in that, The particle size of the nano-binder is 50-100 nm.

6. The application of a nano-insulating, corrosion-resistant, and high-temperature resistant material in the inner cylinder of a coking riser pipe, characterized in that, The material is a nano-insulating, corrosion-resistant, and high-temperature resistant material as described in any one of claims 1 to 3.

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