High-temperature-resistant composite fiber paper and preparation method thereof

Abstract

The invention provides high-temperature-resistant composite fiber paper and a preparation method thereof.The preparation method comprises the steps that 1, basalt fibers and zirconium oxide fibers are defibered respectively, and basalt fiber slurry and zirconium oxide fiber slurry are obtained; (2) mixing the basalt fiber slurry and the zirconium oxide fiber slurry, and sequentially carrying out ultrasonic dispersion and ball milling treatment to obtain composite fiber slurry; and (3) carrying out wet molding on the composite fiber slurry, coating the surface of the molded composite fiber paper with a binder solution, and sequentially drying and curing to obtain the high-temperature-resistant composite fiber paper. According to the invention, the high-temperature-resistant composite fiber paper with the thickness of less than 1mm and higher strength can be continuously produced by a wet manufacturing process.

Description

Technical Field

[0001] The invention relates to the technical field of wet heat insulation protection, and in particular to a high temperature resistant composite fiber paper and a preparation method thereof. Background Art

[0002] The most representative high-temperature resistant fiber material at present is zirconia fiber. Zirconia fiber has the advantages of extremely high melting point (about 2700℃), excellent chemical stability, outstanding wear resistance, fatigue resistance and low thermal conductivity, and can maintain the stability of structure and performance under extremely high temperatures. Zirconia fiber has extremely important application value in the fields of aviation, aerospace and ultra-high temperature industrial furnace insulation, especially in the oxidizing atmosphere environment over 1600℃, it can be used for a long time.

[0003] Among the existing zirconia products, there are dry methods for preparing zirconia fiber felt and fiberboard, and wet methods for making zirconia fiber paper. For example, CN106996055A provides a method for preparing zirconia fiber paper, which includes adding water glass inorganic binder to zirconia slurry, forming wet paper sheets by copying on a net, and then compounding an aluminum foil layer and drying to obtain a zirconia fiber paper for low-temperature deep-cold insulation. However, in wet manufacturing, the thickness of zirconia fiber paper is too thick, usually more than 1 mm, and the strength of the finished paper is too low, making it difficult to produce continuously.

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

[0005] The embodiment of the present invention provides a high temperature resistant composite fiber paper and a preparation method thereof, which can solve the problem that the thickness of the zirconia fiber paper is too thick and the strength of the finished paper is low in the traditional wet forming process.

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

[0007] (1) respectively decomposing basalt fiber and zirconia fiber to obtain basalt fiber slurry and zirconia fiber slurry;

[0008] (2) After mixing the basalt fiber slurry and the zirconia fiber slurry, ultrasonic dispersion and ball milling are performed in sequence to obtain a composite fiber slurry;

[0009] (3) After wet forming the composite fiber slurry, a binder solution is coated on the surface of the formed composite fiber paper, and the paper is dried and cured to obtain the high temperature resistant composite fiber paper.

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

[0011] Preferably, in step (1), the concentration of the basalt fiber slurry and the zirconia fiber slurry is 0.5-1.5%; and the mass concentration of the auxiliary agent 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 mass content of zirconium oxide in the zirconium oxide fiber is ≥80%, and the length of the zirconium oxide fiber is 2.5-3.5 mm, and the diameter is 3.5-4.5 μm.

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

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

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

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

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

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

[0020] Preferably, in step (3), the drying is carried out by heating the temperature from 25°C to 120°C in a gradient manner; wherein the temperature is increased from 20°C to 90°C at a heating rate of 45-60°C / min, and the temperature is increased 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° C. and the curing time is 5-15 min.

[0022] In a second aspect, the present invention provides a high temperature resistant composite fiber paper, which is prepared by the method for preparing 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 the present invention, basalt fiber and zirconia fiber are firstly decomposed to obtain basalt fiber slurry and zirconia fiber slurry, and then the two slurries are mixed by ultrasonic dispersion and ball milling treatment to obtain composite fiber slurry, so as to improve the surface performance of basalt fiber and improve the dispersion performance of basalt fiber, so that basalt fiber and zirconia fiber are evenly dispersed in the composite fiber slurry; then the composite fiber slurry is wet-formed to prepare a wet paper web with basalt fiber as a reinforcing skeleton; finally, a binder solution is further coated on the surface of the wet paper web, so as to further improve the forming strength of the composite fiber paper. In this way, the present invention can continuously produce high-temperature resistant composite fiber paper with a thickness of less than 1 mm and high strength by a wet manufacturing process. BRIEF DESCRIPTION OF THE DRAWINGS

[0025] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative work.

[0026] Figure 1 The present invention provides a flow chart of a method for preparing high temperature resistant composite fiber paper according to an embodiment of the present invention. DETAILED DESCRIPTION

[0027] In order to make the purpose, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the drawings in the embodiments of the present invention. Obviously, the described embodiments are part of the embodiments of the present invention, rather than all the embodiments. Based on the embodiments in the present invention, all other embodiments obtained by ordinary technicians in this field without making creative work are within the scope of protection of the present invention.

[0028] like Figure 1 As shown, the embodiment of the present invention first provides a method for preparing high temperature resistant composite fiber paper, and the preparation method comprises the following steps:

[0029] (1) respectively decomposing basalt fiber and zirconia fiber to obtain basalt fiber slurry and zirconia fiber slurry;

[0030] (2) After mixing the basalt fiber slurry and the zirconia fiber slurry, ultrasonic dispersion and ball milling are performed in sequence to obtain a composite fiber slurry;

[0031] (3) After wet forming the composite fiber slurry, a binder solution is coated on the surface of the formed composite fiber paper, and the paper is dried and cured to obtain the high temperature resistant composite fiber paper.

[0032] Considering that basalt fiber has excellent high temperature resistance and has good mechanical properties and stability at temperatures as high as 1000°C or above, basalt fiber is used as a skeleton to be composited with zirconia fiber in the embodiment of the present invention, so as to improve the strength of the finished paper. At the same time, considering that the surface of basalt fiber is relatively smooth and the surface energy is relatively low, when it is directly mixed with zirconia fiber for decomposition, the dispersion of basalt fiber in the slurry will be poor. In the embodiment of the present invention, basalt fiber and zirconia fiber are first decompressed respectively to obtain basalt fiber slurry and zirconia fiber slurry, and then the two slurries are mixed in turn by ultrasonic dispersion and ball milling to obtain composite fiber slurry, so as to improve the surface properties of basalt fiber and improve the dispersion performance of basalt fiber, so that basalt fiber and zirconia fiber are evenly dispersed in the composite fiber slurry; then the composite fiber slurry is wet-formed to prepare a wet paper web with basalt fiber as a reinforcing skeleton; finally, a binder solution is further coated on the surface of the wet paper web to further improve the forming strength of the composite fiber paper. In this way, the present invention can continuously produce high-temperature resistant composite fiber paper with a thickness of less than 1 mm and high strength by a wet manufacturing process.

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

[0034] In the embodiment of the present invention, when basalt fibers are added to water for decomposition, the above-mentioned types of additives are added to the decomposition system, which not only can further reduce the surface energy of the basalt fibers to form a stable suspension system, but also can make the basalt fibers evenly dispersed in the composite fiber slurry after mixing with the zirconia fiber slurry. At the same time, the composite fiber slurry will not cluster again during the wet forming process, which is convenient for papermaking.

[0035] It should be noted that, in the embodiment of the present invention, when cationic polyacrylamide and polymethacryloyloxyethyl trimethyl ammonium chloride are mixed with basalt fibers for delamination, a synergistic effect can occur between the two, which is further beneficial to ensure the uniformity of the dispersion of basalt fibers in the fiber slurry.

[0036] According to some preferred embodiments, in step (1), the concentration of the basalt fiber slurry and the zirconia 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 auxiliary agent 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 the embodiment of the present invention, during the decomposition process, the additive of the above mass concentration is added and mixed with the basalt fiber, so that the surface energy of the basalt fiber can be improved well, so that the basalt fiber has good dispersion in the slurry, thereby forming a stably dispersed composite fiber slurry. The experiment of the present invention confirms that if the mass concentration of the additive is too low, it is not conducive to improving the dispersion of the basalt fiber in the slurry. If the mass concentration of the additive is too high, the basalt fiber will cluster in the slurry, which is not conducive to forming a stably dispersed composite fiber slurry.

[0038] Furthermore, during deflaking, in order to ensure better deflaking performance, the speed of the deflaker in the embodiment of the present invention is preferably 1000-8000 r / min, and the deflaking time is preferably 1-3 min.

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

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

[0041] It should be noted that the basalt fiber in the embodiment of the present invention is preferably prepared by full electric melting method, and the zirconia fiber is preferably prepared by solution electrospinning method, which is further beneficial to the comprehensive performance of the final high temperature resistant composite fiber paper.

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

[0043] In the embodiment of the present invention, a composite fiber slurry is prepared by mixing a certain amount of basalt fiber and zirconia fiber by ultrasonic dispersion and ball milling. During the mixing process, the zirconia fiber and the basalt fiber can be dispersed with each other. After wet molding, a composite fiber paper with basalt fiber as the skeleton and a thickness of less than 1 mm can be formed, and the molding strength of the fiber paper can be significantly improved, which is convenient for continuous production.

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

[0045] In the process of mixing the two fiber slurries, although adding a dispersant can improve the dispersion performance of the fiber and make the composite fiber slurry dispersed more evenly, the dispersant will decompose at about 300-400°C, and thus cannot meet the requirements of using the zirconium oxide fiber in an environment above 1000°C. Therefore, in the embodiment of the present invention, the two fibers are mixed and dispersed by physical dispersion, that is, firstly, the mixed slurry is ultrasonically dispersed, and the ultrasonic frequency, temperature and time of the ultrasonic dispersion are controlled, so that the entangled fiber filaments are evenly dispersed by the cavitation effect of the ultrasonic wave; then, the mixed slurry is further ball-milled at a certain temperature, and the fibers are rubbed against each other during the ball milling process, so that the entanglement points between the fiber clusters and the chopped fibers can be further dispersed. At the same time, during the ball milling process, the inorganic components on the fiber surface can produce an activation effect under the action of mechanical force, thereby further enhancing the dispersibility of the fiber slurry. By strictly controlling the parameters such as the rotation speed and time of the ball milling process, this is not only conducive to further improving the dispersibility of the fiber, but also can 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 the step of adjusting the pH of the composite fiber slurry to 2.0-3.0 using a pH adjusting agent; wherein the pH adjusting agent is a sulfuric acid solution.

[0047] In an embodiment of the present invention, before wet forming, a dilute sulfuric acid solution (mass concentration is less than or equal to 70%) is used to adjust the pH value of the composite fiber slurry to 2.0-3.0, which is beneficial to further improve the dispersion performance of the fibers in the composite fiber slurry. Then, water is added to carry out wet forming at a papermaking concentration of 0.15-0.25wt%, and then the composite fiber paper is obtained after natural dehydration, vacuum dehumidification and drying in sequence. It should be noted that, in an embodiment of the present invention, the vacuum degree of vacuum dehumidification is 0.03-0.05Mpa, the forced vacuum degree is 0.04-0.06Mpa, and the drying temperature is 180-205°C.

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

[0049] In an embodiment of the present invention, after the composite fiber paper is obtained after wet forming, a coating method is adopted to coat a certain concentration of the above-mentioned binder solution on both sides of the composite fiber paper, thereby enhancing the bonding between the basalt fiber and the zirconia 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 in a gradient heating manner for drying; wherein the temperature is increased from 20°C to 90°C at a heating rate of 45-60°C / min (for example, 45°C / min, 50°C / min or 60°C / min), and the temperature is increased from 90°C to 120°C at a heating rate of 5-15°C / min (for example, 5°C / min, 10°C / min or 15°C / min); the curing temperature is 155-175°C (for example, 155°C, 160°C, 170°C or 175°C), and the curing time is 5-15min (for example, 5min, 8min, 10min, 12min or 15min).

[0051] In an embodiment of the present 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 zirconia fiber, thereby further ensuring the good strength and toughness of the high-temperature resistant composite fiber paper.

[0052] The embodiment of the present invention further provides a high temperature resistant composite fiber paper, which is prepared by any of the preparation methods described above.

[0053] In the embodiment of the present invention, a continuously produced high temperature resistant composite fiber paper is prepared by a wet manufacturing process. The composite fiber paper has a thickness of less than 1 mm, high strength, good flexibility, ultra-high temperature resistance (800-1400°C), and good conductivity. The gram weight of the composite fiber paper in the embodiment of the present invention is 35±5g / m 2 , thickness is 0.05±0.02mm.

[0054] In order to more clearly illustrate the technical solution and advantages of the present invention, a high temperature resistant composite fiber paper and a preparation method thereof are described in detail below through several embodiments.

[0055] Embodiment 1:

[0056] (1) 10 g of basalt fiber with a length of 18±0.5 mm and 6±0.5 mm and a diameter of 8±0.5 μm was added to water, and an additive with a mass concentration of 1.2% (cationic polyacrylamide and polymethacryloyloxyethyl trimethyl ammonium chloride in a mass ratio of 1:1) was added thereto, and then the fiber was deflaked in a deflaking machine at a speed of 6000 r / min for 1 min to obtain a basalt fiber slurry with a slurry concentration of 1.0%;

[0057] 10 g of zirconia fiber with a length of 3±0.5 mm and a diameter of 4±0.5 μm was deflaked in a deflaking machine at a speed of 6000 r / min for 1 min to obtain a zirconia fiber slurry with a slurry concentration of 1.0%;

[0058] (2) The basalt fiber slurry and the zirconia fiber slurry were stirred and mixed at room temperature (25°C) at a speed of 500 r / min for 10 min, and then ultrasonicated at 0°C at an ultrasonic frequency of 60 Hz for 10 min, and then placed in a ball mill and ball milled at 25°C at a speed of 300 r / min for 7 min to obtain a composite fiber slurry;

[0059] (3) The pH value of the composite fiber slurry is adjusted to 2.5 with dilute sulfuric acid, and then water is added. The slurry is formed by wet papermaking at a papermaking concentration of 0.2 wt%, and the composite fiber paper is obtained after natural dehydration, vacuum dehumidification and drying. Finally, a binder solution (a magnesium silicate solution with a mass concentration of 10%) is coated on the upper and lower surfaces of the fiber composite paper by curtain coating, and the paper is dried at 120°C until the substrate has a constant weight, and then cured to obtain a high-temperature resistant composite fiber paper. During the drying process, the paper is dried from room temperature (25°C) to 120°C in a gradient heating method, and the gradient heating method is as follows: the heating rate from room temperature to 90°C is 50°C / min, and the heating rate from 90°C to 120°C is 10°C / min; the curing condition is to cure at 160°C for 10 min.

[0060] Embodiment 2:

[0061] (1) 8 g of basalt fiber with a length of 16±0.5 mm and 6±0.5 mm and a diameter of 8±0.5 μm was added to water, and an additive with a mass concentration of 1.2% (cationic polyacrylamide and polymethacryloyloxyethyl trimethyl ammonium chloride in a mass ratio of 1:1) was added thereto, and then the fiber was deflaked in a deflaking machine at a speed of 6000 r / min for 1 min to obtain a basalt fiber slurry with a slurry concentration of 1.0%;

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

[0063] (2) The basalt fiber slurry and the zirconia fiber slurry were stirred and mixed at room temperature (25°C) at a speed of 500 r / min for 10 min, and then ultrasonicated at 80 Hz for 10 min at 0°C, and then placed in a ball mill and ball milled at 280 r / min for 7 min at 25°C to obtain a composite fiber slurry;

[0064] (3) The pH value of the composite fiber slurry is adjusted to 2.5 with dilute sulfuric acid, and then water is added. The slurry is formed by wet papermaking at a papermaking concentration of 0.2 wt%, and the composite fiber paper is obtained after natural dehydration, vacuum dehumidification and drying. Finally, a binder solution (a magnesium silicate solution with a mass concentration of 10%) is coated on the upper and lower surfaces of the fiber composite paper by curtain coating, and the paper is dried at 120°C until the substrate has a constant weight, and then cured to obtain a high-temperature resistant composite fiber paper. During the drying process, the paper is dried from room temperature (25°C) to 120°C in a gradient heating method, and the gradient heating method is as follows: the heating rate from room temperature to 90°C is 50°C / min, and the heating rate from 90°C to 120°C is 10°C / min; the curing condition is to cure at 160°C for 10 min.

[0065] Embodiment 3:

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

[0067] Embodiment 4:

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

[0069] Embodiment 5:

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

[0071] Embodiment 6:

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

[0073] Embodiment 7:

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

[0075] Embodiment 8:

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

[0077] Embodiment 9:

[0078] Example 9 is basically the same as Example 1, except that: in step (1), 8 g of basalt fiber with a length of 16±0.5 mm and 6±0.5 mm and a diameter of 8±0.5 μm is added to water, and the fiber is deflaked in a deflaking machine at a speed of 6000 r / min for 1 min to obtain a basalt fiber slurry with a slurry concentration of 1.0%.

[0079] Embodiment 10:

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

[0081] Embodiment 11:

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

[0083] Embodiment 12:

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

[0085] Embodiment 13:

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

[0087] Comparative Example 1:

[0088] Comparative Example 1 is substantially the same as Example 1, except that in step (3), the binder 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 slurry is adjusted to 2.5 with dilute sulfuric acid, and then water is added to form it according to the wet papermaking method with a papermaking concentration of 0.2wt%, and the composite fiber paper is obtained after natural dehydration, vacuum dehumidification and drying.

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

[0092] Performance testing method:

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

[0094] Thermal conductivity at room temperature: The thermal conductivity of composite fiber paper at room temperature is tested according to the method in GB / T 10295 "Determination of steady-state thermal resistance and related properties of thermal insulation materials - Heat flow meter method";

[0095] Short-term heat resistance and heat shrinkage rate: The heat resistance temperature and heat shrinkage rate of composite fiber paper in long-term (4h) and short-term (1h) heat resistance are measured according to the methods in GB / T9914.2-2001 "Determination of combustible content of glass fiber" and GB / T5988-2022 "Test method for permanent linear change of refractory materials after heating".

[0096] Tensile strength: The tensile strength of composite fiber paper is measured according to the method in GB / T1447-2005 “Test method for tensile properties of fiber reinforced plastics”.

[0097] Table 1

[0098]

[0099] It can be seen from the results in Table 1 that in the embodiment of the present invention, the basalt fiber and the zirconia fiber are separately dispersed and then mixed, the composite fiber is evenly dispersed by ultrasonic dispersion and ball milling, the basalt fiber is used as a skeleton to improve the strength, the zirconia fiber is used as a filler to maintain the heat resistance, and a silicate binder is added to prepare a high-temperature resistant composite fiber material. The basalt fiber effectively enhances the strength of the material, so that the zirconia fiber can be continuously produced, and when silicate is selected as the binder, the molding strength can be further improved, and a composite fiber paper resistant to a high temperature of 1600°C is prepared, which effectively solves the problem of insufficient strength and excessive thickness of the 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, rather than to limit it. Although the present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that they can still modify the technical solutions described in the aforementioned embodiments, or make equivalent replacements for some of the technical features therein. However, these modifications or replacements do not deviate the essence of the corresponding technical solutions from the spirit and scope of the technical solutions of the embodiments of the present invention.

Claims

1. A method for preparing high temperature resistant composite fiber paper, characterized in that: The preparation method comprises the following steps: (1) respectively decomposing basalt fiber and zirconia fiber to obtain basalt fiber slurry and zirconia fiber slurry; (2) After mixing the basalt fiber slurry and the zirconia fiber slurry, ultrasonic dispersion and ball milling are performed in sequence to obtain a composite fiber slurry; (3) After wet forming the composite fiber slurry, a binder solution is coated on the surface of the formed composite fiber paper, and the paper is dried and cured to obtain the high temperature resistant composite fiber paper.

2. The preparation method according to claim 1, characterized in that: In step (1), when the basalt fiber is decomposed, the step also includes adding an auxiliary agent to water; wherein the auxiliary agent is at least one of cationic polyacrylamide or polymethacryloyloxyethyltrimethylammonium chloride.

3. The preparation method according to claim 2, characterized in that: In step (1), 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%.

4. The preparation method according to claim 1, characterized in that: In step (1), the basalt fiber has a length of 6-18 mm and a diameter of 7.5-8.5 μm; and / or The mass content of zirconium oxide in the zirconium oxide fiber is ≥80%, and the length of the zirconium oxide fiber is 2.5-3.5 mm, and the diameter is 3.5-4.5 μm.

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

6. The preparation method according to claim 1, characterized in that: In step (2), the frequency of the ultrasonic dispersion is 60-120 Hz, the time is 5-10 min, and the temperature is 0-25° C.; and / or 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°C.

7. The preparation method according to claim 1, characterized in that: Step (2) also includes the step of using a pH adjuster to adjust the pH of the composite fiber slurry to 2.0-3.0; wherein the pH adjuster is a sulfuric acid solution.

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

9. The preparation method according to claim 1, characterized in that: In step (3), drying is performed by heating from 25°C to 120°C in a gradient heating manner; wherein the heating rate is 45-60°C / min from 20°C to 90°C, and the heating rate is 5-15°C / min from 90°C to 120°C; and / or The curing temperature is 155-175° C. and the curing time is 5-15 minutes.

10. A high temperature resistant composite fiber paper, characterized in that: The preparation method is described in any one of claims 1 to 9.

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