A high-temperature resistant composite fiber paper and its preparation method

Abstract

This invention provides a high-temperature resistant composite fiber paper and its preparation method. The preparation method includes: (1) slurrying basalt fiber and zirconium oxide fiber to obtain basalt fiber slurry and zirconium oxide fiber slurry respectively; (2) mixing the basalt fiber slurry and the zirconium oxide fiber slurry, and then subjecting them to ultrasonic dispersion and ball milling treatments in sequence to obtain a composite fiber slurry; (3) wet molding the composite fiber slurry, coating the surface of the molded composite fiber paper with an adhesive solution, and then drying and curing in sequence to obtain the high-temperature resistant composite fiber paper. This invention can continuously produce high-temperature resistant composite fiber paper with a thickness of less than 1 mm and high strength using a wet manufacturing process.

Description

Technical Field

[0001] This invention relates to the field of wet-process thermal insulation and protection technology, and in particular to a high-temperature resistant composite fiber paper and its preparation method. Background Technology

[0002] Currently, zirconia fiber is the most representative high-temperature resistant fiber material. Zirconia fiber possesses advantages such as an extremely high melting point (approximately 2700℃), excellent chemical stability, outstanding wear resistance, fatigue resistance, and low thermal conductivity, enabling it to maintain structural and performance stability at extreme high temperatures. Zirconia fiber has extremely important application value in aerospace, aviation, and ultra-high temperature industrial kiln insulation fields, especially in its ability to be used for extended periods in oxidizing atmospheres exceeding 1600℃.

[0003] Existing zirconia products include dry-process preparation of zirconia fiber felt and fiberboard, and wet-process manufacturing of zirconia fiber paper. For example, CN106996055A provides a method for preparing zirconia fiber paper, which involves adding water glass inorganic binder to zirconia slurry, forming a wet paper sheet by web forming, then laminating it with an aluminum foil layer and drying it to obtain a zirconia fiber paper for cryogenic insulation. However, in wet manufacturing, the zirconia fiber paper is too thick, usually exceeding 1 mm, and the paper strength is too low, making continuous production difficult.

[0004] Therefore, based on the above problems, there is an urgent need to provide a high-temperature resistant composite fiber paper and its preparation method. Summary of the Invention

[0005] This invention provides a high-temperature resistant composite fiber paper and its preparation method, which can solve the problems of excessive thickness and low paper strength of zirconia fiber paper in the traditional wet forming process.

[0006] In a first aspect, the present invention provides a method for preparing high-temperature resistant composite fiber paper, the method comprising the following steps:

[0007] (1) Basalt fiber and zirconium oxide fiber were decomposed to obtain basalt fiber slurry and zirconium oxide fiber slurry respectively;

[0008] (2) After mixing the basalt fiber slurry and the zirconium oxide fiber slurry, ultrasonic dispersion and ball milling are performed sequentially to obtain composite fiber slurry;

[0009] (3) After the composite fiber pulp is wet-formed, an adhesive solution is coated on the surface of the formed composite fiber paper, and the paper is dried and cured in sequence to obtain the high-temperature resistant composite fiber paper.

[0010] Preferably, in step (1), when the basalt fiber is decomposed, the step of adding an auxiliary agent to the water is further included; wherein the auxiliary agent is at least one of cationic polyacrylamide or polymethacryloyloxyethyltrimethylammonium chloride.

[0011] Preferably, in step (1), the concentrations of the basalt fiber slurry and the zirconium oxide fiber slurry are 0.5-1.5%; and the mass concentration of the additives is 0.4-1.3%.

[0012] Preferably, in step (1), the basalt fiber has a length of 6-18 mm and a diameter of 7.5-8.5 μm.

[0013] Preferably, in step (1), the zirconium oxide fiber has a zirconium oxide content of ≥80% by mass, and the zirconium oxide fiber has a length of 2.5-3.5 mm and a diameter of 3.5-4.5 μm.

[0014] Preferably, in step (2), the dry weight ratio of basalt fiber in the composite fiber slurry is 1-50%.

[0015] Preferably, in step (2), the ultrasonic dispersion frequency is 60-120Hz, the time is 5-10min, and the temperature is 0-25℃;

[0016] Preferably, the ball milling process is performed at a rotation speed of 280-320 r / min, a time of 3-7 min, and a temperature of 20-30℃.

[0017] Preferably, step (2) further includes adjusting the pH of the composite fiber pulp to 2.0-3.0 using a pH adjuster; wherein the pH adjuster is a sulfuric acid solution.

[0018] Preferably, in step (3), the adhesive solution is at least one of sodium silicate solution, aluminum silicate solution, potassium silicate solution or magnesium silicate solution.

[0019] More preferably, the mass concentration of the adhesive solution is 5-20%.

[0020] Preferably, in step (3), the temperature is increased from 25°C to 120°C using a gradient heating method for drying; wherein the temperature is increased from 25°C to 90°C at a heating rate of 45-60°C / min, and from 90°C to 120°C at a heating rate of 5-15°C / min.

[0021] Preferably, in step (3), the curing temperature is 155-175℃ and the time is 5-15min.

[0022] In a second aspect, the present invention provides a high-temperature resistant composite fiber paper, which is prepared by the preparation method of the high-temperature resistant composite fiber paper described in any one of the first aspects above.

[0023] Compared with the prior art, the present invention has at least the following beneficial effects:

[0024] In this invention, basalt fibers and zirconium oxide fibers are first decomposed to obtain basalt fiber slurry and zirconium oxide fiber slurry, respectively. Then, the two slurries are mixed by sequentially subjecting them to ultrasonic dispersion and ball milling to obtain a composite fiber slurry. This improves the surface properties and dispersion performance of the basalt fibers, ensuring uniform dispersion of both basalt and zirconium oxide fibers in the composite fiber slurry. Subsequently, this composite fiber slurry is used to prepare a wet paper web with basalt fibers as the reinforcing skeleton through a wet forming process. Finally, by further coating the surface of the wet paper web with an adhesive solution, the forming strength of the composite fiber paper is further improved. Thus, this invention enables the continuous production of high-temperature resistant composite fiber paper with a thickness of less than 1 mm and high strength using a wet manufacturing process. Attached Figure Description

[0025] To more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0026] Figure 1 This is a flowchart of a method for preparing a high-temperature resistant composite fiber paper according to an embodiment of the present invention. Detailed Implementation

[0027] To make the objectives, technical solutions, and advantages of the embodiments of the present invention clearer, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments obtained by those skilled in the art based on the embodiments of the present invention without creative effort are within the scope of protection of the present invention.

[0028] like Figure 1 As shown, this embodiment of the invention first provides a method for preparing high-temperature resistant composite fiber paper, which includes the following steps:

[0029] (1) Basalt fiber and zirconium oxide fiber were decomposed to obtain basalt fiber slurry and zirconium oxide fiber slurry respectively;

[0030] (2) After mixing the basalt fiber slurry and the zirconium oxide fiber slurry, ultrasonic dispersion and ball milling are performed sequentially to obtain composite fiber slurry;

[0031] (3) After the composite fiber pulp is wet-formed, an adhesive solution is coated on the surface of the formed composite fiber paper, and the paper is dried and cured in sequence to obtain the high-temperature resistant composite fiber paper.

[0032] Considering the excellent high-temperature resistance of basalt fiber, which exhibits good mechanical properties and stability at temperatures exceeding 1000℃, this invention employs basalt fiber as a skeleton combined with zirconia fiber to enhance paper strength. However, given the smooth surface and low surface energy of basalt fiber, direct mixing with zirconia fiber would result in poor dispersion of the basalt fiber in the pulp. Therefore, this invention first separately decomposes the basalt fiber and zirconia fiber to obtain basalt fiber pulp and zirconia fiber pulp, respectively. Then, the two pulps are sequentially mixed through ultrasonic dispersion and ball milling to obtain a composite fiber pulp. This improves the surface properties and dispersion performance of the basalt fiber, ensuring uniform dispersion of both fibers in the composite fiber pulp. The composite fiber pulp is then used to prepare a wet paper web with basalt fiber as the reinforcing skeleton through a wet forming process. Finally, a binder solution is coated onto the surface of the wet paper web to further enhance the forming strength of the composite fiber paper. Thus, the present invention can continuously produce high-temperature resistant composite fiber paper with a thickness of less than 1 mm and high strength using a wet manufacturing process.

[0033] According to some preferred embodiments, in step (1), when the basalt fiber is decomposed, the step of adding an auxiliary agent to the water is also included; wherein the auxiliary agent is at least one of cationic polyacrylamide or polymethacryloyloxyethyltrimethylammonium chloride.

[0034] In this embodiment of the invention, when basalt fibers are added to water for dissolution, the above-mentioned additives are added to the dissolution system. This not only further reduces the surface energy of the basalt fibers, making them form a stable suspension system, but also allows the basalt fibers to be evenly dispersed in the composite fiber slurry after being mixed with zirconium oxide fiber slurry. At the same time, the composite fiber slurry will not agglomerate again during the wet forming process, which is convenient for papermaking.

[0035] It should be noted that in the embodiments of the present invention, when cationic polyacrylamide and polymethacryloyloxyethyltrimethylammonium chloride are mixed with basalt fibers for descaling, the two can have a synergistic effect, which further helps to ensure the uniformity of basalt fibers in fiber slurry dispersion.

[0036] According to some preferred embodiments, in step (1), the concentration of the basalt fiber slurry and the zirconium oxide fiber slurry is 0.5-1.5% (for example, it can be 0.5%, 0.8%, 1%, 1.2% or 1.5%); the mass concentration of the additive is 0.4-1.3% (for example, it can be 0.4%, 0.5%, 0.8%, 1.0%, 1.1%, 1.2% or 1.3%).

[0037] In this embodiment of the invention, during the dispersing process, the basalt fibers are mixed with an additive of the aforementioned mass concentration. This effectively improves the surface energy of the basalt fibers, resulting in better dispersibility of the basalt fibers in the slurry and thus forming a stable and dispersed composite fiber slurry. Experiments of this invention have confirmed that if the mass concentration of the additive is too low, it is detrimental to improving the dispersibility of the basalt fibers in the slurry; if the mass concentration of the additive is too high, it will cause the basalt fibers to agglomerate in the slurry, which is not conducive to forming a stable and dispersed composite fiber slurry.

[0038] Furthermore, during the dredging process, in order to ensure better dredging performance, the preferred rotation speed of the dredging machine in this embodiment of the invention is 1000-8000 r / min, and the preferred dredging time is 1-3 min.

[0039] According to some preferred embodiments, in step (1), the basalt fiber has a length of 6-18 mm (e.g., 6 mm, 8 mm, 10 mm, 12 mm, 16 mm or 18 mm) and a diameter of 7.5-8.5 μm (e.g., 7.5 μm, 7.8 μm, 8 μm, 8.2 μm or 8.5 μm); the zirconium oxide fiber has a zirconium oxide content ≥80% by mass, and the zirconium oxide fiber has a length of 2.5-3.5 mm (e.g., 2.5 mm, 2.8 mm, 3 mm, 3.2 mm or 3.5 mm) and a diameter of 3.5-4.5 μm (e.g., 3.5 μm, 3.8 μm, 4 μm, 4.2 μm or 4.5 μm).

[0040] In this embodiment of the invention, by controlling the diameter and length of basalt fiber and zirconium oxide fiber, it is beneficial to prepare a high-temperature resistant fiber composite paper with low thickness and good strength. Furthermore, in this embodiment of the invention, the basalt fiber is preferably a mixture of long fiber (12-18 mm) and short fiber (6-12 mm), which can further enhance the final paper strength.

[0041] It should be noted that the basalt fiber in the embodiments of the present invention is preferably prepared by the full electrofusion method, and the zirconia fiber is preferably prepared by the solution electrospinning method. This further improves the overall performance of the final high-temperature resistant composite fiber paper.

[0042] According to some preferred embodiments, in step (2), the dry weight ratio of basalt fiber in the composite fiber slurry is 1-50% (for example, 1%, 5%, 10%, 20%, 30%, 40% or 50%).

[0043] In this embodiment of the invention, a composite fiber slurry is prepared by mixing a certain amount of basalt fiber and zirconium oxide fiber through ultrasonic dispersion and ball milling. During the mixing process, the zirconium oxide fiber can be dispersed with the basalt fiber. After wet molding, a composite fiber paper with basalt fiber as the skeleton and a thickness of less than 1 mm can be formed, which can significantly improve the molding strength of the fiber paper and facilitate continuous production.

[0044] According to some preferred embodiments, in step (2), the frequency of ultrasonic dispersion is 60-120Hz (e.g., 60Hz, 80Hz, 100Hz or 120Hz), the time is 5-10min (e.g., 5min, 6min, 7min, 8min, 9min or 10min), and the temperature is 0-25℃ (e.g., 0℃, 5℃, 10℃, 15℃, 20℃ or 25℃); the rotation speed of ball milling is 280-320r / min (e.g., 280r / min, 290r / min, 300r / min, 310r / min or 320r / min), the time is 3-7min (e.g., 3min, 4min, 5min, 6min or 7min), and the temperature is 20-30℃ (e.g., 20℃, 22℃, 25℃, 28℃ or 30℃).

[0045] While adding a dispersant during the mixing of two fiber pulps can improve fiber dispersion and make the composite fiber pulp more uniformly dispersed, the dispersant decomposes at around 300-400℃, thus failing to meet the requirements for zirconium oxide fiber use in environments above 1000℃. Therefore, in this embodiment of the invention, a physical dispersion method is used to mix and disperse the two fibers. First, the mixed pulp is ultrasonically dispersed, and the ultrasonic frequency, temperature, and time are controlled to utilize the cavitation effect of ultrasound to uniformly disperse the entangled fiber filaments. Then, the mixed pulp is further ball-milled at a certain temperature. During ball milling, the fibers rub against each other, which further disperses the entanglement points between fiber clusters and chopped fibers. At the same time, the inorganic components on the fiber surface can generate an activation effect under mechanical force during ball milling, thereby further enhancing the dispersibility of the fiber pulp. By strictly controlling the parameters such as the rotation speed and time of the ball milling, it is not only beneficial to further improve the dispersibility of the fibers, but also to avoid fiber breakage and prevent adverse effects on the strength of the final composite fiber paper.

[0046] According to some preferred embodiments, step (2) further includes adjusting the pH of the composite fiber pulp to 2.0-3.0 using a pH adjuster; wherein the pH adjuster is a sulfuric acid solution.

[0047] In this embodiment of the invention, before wet forming, the pH value of the composite fiber pulp is adjusted to 2.0-3.0 using a dilute sulfuric acid solution (mass concentration less than or equal to 70%). This is beneficial to further improve the dispersion performance of the fibers in the composite fiber pulp. Then, water is added to a papermaking concentration of 0.15-0.25 wt% for wet forming. After natural dehydration, vacuum dehumidification, and drying, the composite fiber paper is obtained. It should be noted that in this embodiment of the invention, the vacuum degree of vacuum dehumidification is 0.03-0.05 MPa, the forced vacuum degree is 0.04-0.06 MPa, and the drying temperature is 180-205℃.

[0048] According to some preferred embodiments, in step (3), the adhesive solution is at least one of sodium silicate solution, aluminum silicate solution, potassium silicate solution or magnesium silicate solution; preferably, the mass concentration of the adhesive solution is 5-20% (for example, it can be 5%, 8%, 10%, 12%, 15%, 18% or 20%).

[0049] In this embodiment of the invention, after obtaining the composite fiber paper through wet forming, a coating method is used to coat both sides of the composite fiber paper with the above-mentioned binder solution of a certain concentration, thereby enhancing the adhesion between basalt fiber and zirconium oxide fiber. At the same time, the binder has a certain strength, thereby further significantly improving the toughness of the composite fiber paper.

[0050] According to some preferred embodiments, in step (3), the temperature is increased from 25°C to 120°C using a gradient heating method for drying; wherein, the temperature is increased from 25°C to 90°C at a heating rate of 45-60°C / min (e.g., 45°C / min, 50°C / min or 60°C / min), and from 90°C to 120°C at a heating rate of 5-15°C / min (e.g., 5°C / min, 10°C / min or 15°C / min); the curing temperature is 155-175°C (e.g., 155°C, 160°C, 170°C or 175°C), and the time is 5-15 min (e.g., 5 min, 8 min, 10 min, 12 min or 15 min).

[0051] In this embodiment of the invention, a gradient heating method is adopted during the drying process, and the heating rate in each gradient heating process is controlled. This is beneficial for the binder solution on the surface of the composite fiber paper to combine with the basalt fiber and zirconium oxide fiber, thereby further ensuring the good strength and toughness of the high-temperature resistant composite fiber paper.

[0052] This invention also provides a high-temperature resistant composite fiber paper, which is prepared using any of the preparation methods described above.

[0053] In this embodiment of the invention, a continuously producible high-temperature resistant composite fiber paper is prepared using a wet manufacturing process. The composite fiber paper has a thickness of less than 1 mm, high strength, good flexibility, resistance to ultra-high temperatures (800-1400℃), and good electrical conductivity. The basis weight of the composite fiber paper in this embodiment of the invention is 35±5 g / m³. 2 The thickness is 0.05±0.02mm.

[0054] To more clearly illustrate the technical solution and advantages of the present invention, the following detailed description of a high-temperature resistant composite fiber paper and its preparation method is provided through several embodiments.

[0055] Example 1:

[0056] (1) 10g of basalt fibers with lengths of 18±0.5mm and 6±0.5mm and diameters of 8±0.5μm were added to water, and 1.2% of an auxiliary agent (cationic polyacrylamide and polymethacryloyloxyethyltrimethylammonium chloride in a mass ratio of 1:1) was added to the water. Then, the fibers were delaminated for 1 minute using a delaminator with a rotation speed of 6000r / min to obtain basalt fiber slurry with a slurry concentration of 1.0%.

[0057] 10g of zirconia fibers with a length of 3±0.5mm and a diameter of 4±0.5μm were delaminated in a delaminator at a speed of 6000r / min for 1min to obtain a zirconia fiber slurry with a slurry concentration of 1.0%.

[0058] (2) Basalt fiber slurry and zirconium oxide fiber slurry were stirred and mixed at 500 r / min for 10 min at room temperature (25℃), and then ultrasonicated at 60 Hz for 10 min at 0℃. The mixture was then placed in a ball mill and ball-milled at 300 r / min for 7 min at 25℃ to obtain composite fiber slurry.

[0059] (3) After adjusting the pH value of the composite fiber pulp to 2.5 with dilute sulfuric acid, water is added and the paper is formed according to the wet papermaking method with a papermaking concentration of 0.2wt%. After natural dehydration, vacuum dehumidification and drying, composite fiber paper is obtained. Finally, the adhesive solution (magnesium silicate solution with a mass concentration of 10%) is coated on the upper and lower surfaces of the fiber composite paper by the curtain coating method, and it is dried at 120℃ to constant weight of the substrate, and then cured to obtain high temperature resistant composite fiber paper. During drying, the temperature is raised from room temperature (25℃) to 120℃ by gradient heating. The temperature rise rate from room temperature to 90℃ is 50℃ / min, and the temperature rise rate from 90℃ to 120℃ is 10℃ / min. The curing condition is to cure at 160℃ for 10min.

[0060] Example 2:

[0061] (1) Add 8g of basalt fibers with lengths of 16±0.5mm and 6±0.5mm and diameters of 8±0.5μm to water, and add 1.2% of an auxiliary agent (cationic polyacrylamide and polymethacryloyloxyethyltrimethylammonium chloride in a mass ratio of 1:1) to the water. Then, decompose the fibers in a decomposition machine with a speed of 6000r / min for 1min to obtain a basalt fiber slurry with a slurry concentration of 1.0%.

[0062] 12g of zirconia fibers with a length of 3±0.5mm and a diameter of 4±0.5μm were delaminated in a delaminator at a speed of 6000r / min for 1min to obtain a zirconia fiber slurry with a slurry concentration of 1.0%.

[0063] (2) Basalt fiber slurry and zirconium oxide fiber slurry were stirred and mixed at 500 r / min for 10 min at room temperature (25℃), and then ultrasonicated at 80 Hz for 10 min at 0℃. The mixture was then placed in a ball mill and ball-milled at 280 r / min for 7 min at 25℃ to obtain composite fiber slurry.

[0064] (3) After adjusting the pH value of the composite fiber pulp to 2.5 with dilute sulfuric acid, water is added and the paper is formed according to the wet papermaking method with a papermaking concentration of 0.2wt%. After natural dehydration, vacuum dehumidification and drying, composite fiber paper is obtained. Finally, the adhesive solution (magnesium silicate solution with a mass concentration of 10%) is coated on the upper and lower surfaces of the fiber composite paper by the curtain coating method, and it is dried at 120℃ to constant weight of the substrate, and then cured to obtain high temperature resistant composite fiber paper. During drying, the temperature is raised from room temperature (25℃) to 120℃ by gradient heating. The temperature rise rate from room temperature to 90℃ is 50℃ / min, and the temperature rise rate from 90℃ to 120℃ is 10℃ / min. The curing condition is to cure at 160℃ for 10min.

[0065] Example 3:

[0066] Example 3 is basically the same as Example 1, except that in step (1), the mass of basalt fiber is 6g and the mass of zirconium oxide fiber is 14g.

[0067] Example 4:

[0068] Example 4 is basically the same as Example 1, except that in step (1), the mass of basalt fiber is 4g and the mass of zirconium oxide fiber is 16g.

[0069] Example 5:

[0070] Example 5 is basically the same as Example 1, except that in step (1), the mass of basalt fiber is 2g and the mass of zirconium oxide fiber is 18g.

[0071] Example 6:

[0072] Example 4 is basically the same as Example 1, except that in step (3), the adhesive solution is a sodium silicate solution with a mass concentration of 10%.

[0073] Example 7:

[0074] Example 7 is basically the same as Example 1, except that in step (3), the adhesive solution is an aluminum silicate solution with a mass concentration of 10%.

[0075] Example 8:

[0076] Example 8 is basically the same as Example 1, except that in step (3), the adhesive solution is a potassium silicate solution with a mass concentration of 10%.

[0077] Example 9:

[0078] Example 9 is basically the same as Example 2, except that in step (1), 8g of basalt fibers with lengths of 16±0.5mm and 6±0.5mm and diameter of 8±0.5μm are added to water and decomposed for 1min using a decomposition machine with a rotation speed of 6000r / min to obtain basalt fiber slurry with a slurry concentration of 1.0%.

[0079] Example 10:

[0080] Example 10 is basically the same as Example 1, except that in step (1), the additive is an additive (cationic polyacrylamide) with a mass concentration of 1.2%.

[0081] Example 11:

[0082] Example 11 is basically the same as Example 1, except that in step (1), the additive is an additive (polymethacryloyloxyethyltrimethylammonium chloride) with a mass concentration of 1.2%.

[0083] Example 12:

[0084] Example 12 is basically the same as Example 1, except that in step (1), the mass concentration of the additive is 1.8%.

[0085] Example 13:

[0086] Example 13 is basically the same as Example 1, except that in step (1), the additive is an additive with a mass concentration of 0.3%.

[0087] Comparative Example 1:

[0088] Comparative Example 1 is basically the same as Example 1, except that in step (3), the adhesive solution is a sodium phosphate solution with a mass concentration of 10%.

[0089] Comparative Example 2:

[0090] Comparative Example 2 is basically the same as Example 1, except that in step (3), the pH value of the composite fiber pulp is adjusted to 2.5 by dilute sulfuric acid and then water is added. The pulp is formed by wet papermaking with a papermaking concentration of 0.2wt%. After natural dehydration, vacuum dehumidification and drying, composite fiber paper is obtained.

[0091] The composite fiber paper prepared in the above embodiments and comparative examples was subjected to performance tests, and the test results are shown in Table 1.

[0092] Performance testing methods:

[0093] Thickness: The thickness of the composite fiber paper was determined according to the method in GB / T 3820-1997 "Determination of thickness of textiles and textile products";

[0094] Room temperature thermal conductivity: The room temperature thermal conductivity of composite fiber paper was tested according to the method in GB / T 10295 "Determination of steady-state thermal resistance and related properties of thermal insulation materials by heat flow meter method".

[0095] Short-term temperature resistance and temperature shrinkage rate: The temperature resistance and temperature shrinkage rate of composite fiber paper under long-term (4h) and short-term (1h) conditions were determined according to the methods in GB / T 9914.2-2001 "Determination of combustible content in glass fiber" and GB / T 5988-2022 "Test method for permanent linear change of refractory materials under heating".

[0096] Tensile strength: The tensile strength of the composite fiber paper was determined according to the method in GB / T 1447-2005 "Test Method for Tensile Properties of Fiber Reinforced Plastics".

[0097] Table 1

[0098]

[0099] As can be seen from the results in Table 1, in this embodiment of the invention, by separately dispersing and then mixing basalt fiber and zirconia fiber, and then dispersing the composite fiber evenly by ultrasonic dispersion and ball milling, using basalt fiber as a skeleton to improve strength, and zirconia fiber as a filler to maintain temperature resistance, and adding silicate binder, a high-temperature resistant composite fiber material was prepared. Basalt fiber effectively enhances the strength of the material, enabling continuous production of zirconia fiber. Furthermore, when silicate is selected as a binder, the molding strength can be further improved, and a composite fiber paper resistant to 1600℃ can be prepared, effectively solving the problems of insufficient strength and excessive thickness of zirconia fiber paper.

[0100] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, and not to limit them; although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some of the technical features; and these modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the spirit and scope of the technical solutions of the embodiments of the present invention.

Claims

1. A method for producing a high-temperature resistant composite fiber paper, characterized by, The preparation method includes the following steps: (1) Basalt fiber and zirconia fiber are respectively decomposed to obtain basalt fiber slurry and zirconia fiber slurry; the decomposition of basalt fiber further includes the step of adding an auxiliary agent to water; wherein the auxiliary agent is at least one of cationic polyacrylamide or polymethacryloyloxyethyltrimethylammonium chloride; the concentration of the basalt fiber slurry and the zirconia fiber slurry is 0.5-1.5%; the mass concentration of the auxiliary agent is 0.4-1.3%; (2) After mixing the basalt fiber slurry and the zirconium oxide fiber slurry, ultrasonic dispersion and ball milling are performed sequentially to obtain composite fiber slurry; the ultrasonic dispersion frequency is 60-120Hz, the time is 5-10min, and the temperature is 0-25℃; the ball milling speed is 280-320r / min, the time is 3-7min, and the temperature is 20-30℃; (3) After the composite fiber pulp is wet-formed, an adhesive solution is coated on the surface of the formed composite fiber paper, and the paper is dried and cured in sequence to obtain the high-temperature resistant composite fiber paper.

2. The production method according to claim 1, characterized by, In step (1), the basalt fibers have a length of 6-18 mm and a diameter of 7.5-8.5 μm; and / or The zirconium oxide fiber has a zirconium oxide content of ≥80% by mass, and the zirconium oxide fiber has a length of 2.5-3.5 mm and a diameter of 3.5-4.5 μm.

3. The preparation method according to claim 1, characterized in that, In step (2), the dry weight ratio of basalt fiber in the composite fiber slurry is 1-50%.

4. The preparation method according to claim 1, characterized in that, Step (2) further includes adjusting the pH of the composite fiber pulp to 2.0-3.0 using a pH adjuster; wherein the pH adjuster is a sulfuric acid solution.

5. The preparation method according to claim 1, characterized in that, In step (3), the adhesive solution is at least one of sodium silicate solution, aluminum silicate solution, potassium silicate solution or magnesium silicate solution; The mass concentration of the adhesive solution is 5-20%.

6. The preparation method according to claim 1, characterized in that, In step (3), the temperature is gradually increased from 25°C to 120°C for drying; specifically, the temperature is increased from 25°C to 90°C at a rate of 45-60°C / min, and from 90°C to 120°C at a rate of 5-15°C / min; and / or The curing temperature is 155-175℃, and the time is 5-15 minutes.

7. A high-temperature resistant composite fiber paper, characterized in that, It is prepared by any one of the preparation methods according to claims 1 to 6.

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