CN111235693A - Preparation method of melt-spun alumina fiber - Google Patents
Preparation method of melt-spun alumina fiber Download PDFInfo
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- CN111235693A CN111235693A CN202010036893.0A CN202010036893A CN111235693A CN 111235693 A CN111235693 A CN 111235693A CN 202010036893 A CN202010036893 A CN 202010036893A CN 111235693 A CN111235693 A CN 111235693A
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
Abstract
The invention provides a preparation method of a spinning alumina fiber, which comprises the following steps: a) mixing polyaluminium chloride sol and silica sol, adding a spinning auxiliary agent and a crystalline phase sintering auxiliary agent for reaction to obtain alumina sol to be spun into fibers; adding the emulsified paraffin solution to obtain a spinning solution; b) spinning and collecting cotton in turn on the spinning solution obtained in the step a) to obtain spinning fibers; c) carrying out heat treatment on the spun fibers obtained in the step b) to obtain spun alumina fibers. Compared with the prior art, the preparation method provided by the invention firstly adopts a specific formula to obtain the spinning solution suitable for the spinning process, and then combines specific process steps and conditions to realize better interaction, so that the obtained spinning alumina fiber has smooth surface, less doubling, long fiber and difficult fracture. Experimental results show that the fiber dispersion index of the spun alumina fiber obtained by the preparation method provided by the invention is more than 80mL/g, and the anti-vibration crushing rate of the fiber is less than 6%.
Description
Technical Field
The invention relates to the technical field of alumina fibers, in particular to a preparation method of a spinning alumina fiber.
Background
The industrial preparation of the alumina fiber mainly adopts a mode of combining a sol-gel method and a wire throwing process; however, fibers that are spun out through the openings tend to break and the fibers that are just spun out tend to stick together relatively thick.
Chinese patent publication No. CN109943896A discloses a colloid filamentation apparatus and method. It has solved prior art design technical problem such as reasonable inadequately. Including setting up the throwing motor on throwing the silk seat, the motor shaft of throwing the silk motor is hollow form just the motor shaft in wear to be equipped with the pay-off body, pay-off body and conveying pipeline be linked together, the conveying pipeline setting is in cooling device, the motor shaft lower extreme of throwing the silk motor be connected with the throwing silk disk body, the fixed hot air blast structure that links to each other with the motor shaft that is equipped with in throwing silk disk body upper end, be equipped with between throwing the silk motor and the hot air blast structure with the hot air blast structure corresponding hot air production device. The technical scheme can solve the problem that the wire throwing hole is blocked due to the fact that the alumina sol is easily and quickly solidified because of high temperature and the influence of a hot air system.
However, the fibers are further stretched by a hot air system and are rapidly dried, so that the problem that the fiber-forming fibers are fragile, easy to break and adhered to each other cannot be solved (the evaporation of water during fiber forming, which is an area where a large amount of water vapor is gathered, hot air is favorable for fiber forming, but the fibers are not dispersed in time because the rotating speed of a spinning disk is high during fiber forming, and the fibers still adhere due to moisture absorption).
Disclosure of Invention
In view of the above, the present invention provides a method for preparing a spun alumina fiber, which has a smooth surface, less fiber doubling, and a long fiber length and is not easy to break.
The invention provides a preparation method of a spinning alumina fiber, which comprises the following steps:
a) mixing polyaluminium chloride sol and silica sol, adding a spinning auxiliary agent and a crystalline phase sintering auxiliary agent for reaction to obtain alumina sol to be spun into fibers; adding the emulsified paraffin solution to obtain a spinning solution;
b) spinning and collecting cotton in turn on the spinning solution obtained in the step a) to obtain spinning fibers;
c) carrying out heat treatment on the spun fibers obtained in the step b) to obtain spun alumina fibers.
Preferably, Al of the polyaluminum chloride sol in step a)2O3The content is 25 wt% -35 wt%; SiO of the silica sol2The content is 20 wt% -30 wt%;
al in the polyaluminum chloride sol2O3And SiO in silica sol2The mass ratio of (70-100): (0 to 30).
Preferably, the spinning auxiliary in the step a) is prepared from the following components in percentage by mass (0.5-1): (5-8): (0.2-0.8): 100 of lactic acid, polyvinyl alcohol, alcohol and water.
Preferably, the addition amount of the spinning aid in the step a) is Al2O312 to 18 weight percent of solid content.
Preferably, the crystalline phase sintering aid in step a) is selected from one or more of magnesium chloride solution, boric acid solution, zirconium acetate solution and calcium chloride aqueous solution.
Preferably, the reaction temperature in the step a) is 80-120 ℃, and the reaction time is 2-5 h.
Preferably, the preparation process of the emulsified paraffin solution in the step a) specifically comprises the following steps:
diluting the emulsified paraffin with water, slightly shaking or slightly stirring the diluted emulsified paraffin in hot water at the temperature of between 60 and 80 ℃ to naturally form uniform fluid, and preparing the uniform fluid to obtain an emulsified paraffin solution with the concentration of between 50 and 60 weight percent.
Preferably, the addition amount of the emulsified paraffin solution in the step a) is 0.1-2% of the mass of the alumina sol to be spun into fibers.
Preferably, the spinning process in the step b) adopts spinning and cotton collecting equipment, which specifically comprises the following steps: the primary upward blowing wind pressure is 0.2MPa to 0.4MPa, an included angle of 50 degrees to 70 degrees is formed between the primary upward blowing wind pressure and the tangential direction of the throwing disc, the secondary upward blowing wind pressure is 0.06MPa to 0.2MPa, an included angle of 70 degrees to 90 degrees is formed between the primary upward blowing wind pressure and the tangential direction of the throwing disc, the primary downward induced wind pressure is 0.3MPa to 0.5MPa, the primary downward induced wind pressure is 1m to 2m above the cotton collecting net, the secondary downward induced wind pressure is 0.1MPa to 0.3MPa, the curing distance is 3m to 7m, the wind temperature is 120 ℃ to 145 ℃, and the rotating speed of the throwing disc is 20Hz to 40 Hz.
Preferably, the heat treatment process in step c) is specifically:
removing the absorbed water contained in the fiber from the spun fiber at 105-150 ℃; then heating to 450-550 ℃ according to the heating rate of 5-10 ℃/min, and then preserving heat for 2-3 h; and then heating to 1200-1400 ℃ according to the heating rate of 10-20 ℃/min, and then preserving the heat for 30-60 min to obtain the spinning alumina fiber.
The invention provides a preparation method of a spinning alumina fiber, which comprises the following steps: a) mixing polyaluminium chloride sol and silica sol, adding a spinning auxiliary agent and a crystalline phase sintering auxiliary agent for reaction to obtain alumina sol to be spun into fibers; adding the emulsified paraffin solution to obtain a spinning solution; b) spinning and collecting cotton in turn on the spinning solution obtained in the step a) to obtain spinning fibers; c) carrying out heat treatment on the spun fibers obtained in the step b) to obtain spun alumina fibers. Compared with the prior art, the preparation method provided by the invention firstly adopts a specific formula to obtain the spinning solution suitable for the spinning process, and then combines specific process steps and conditions to realize better interaction, so that the obtained spinning alumina fiber has smooth surface, less doubling, long fiber and difficult fracture. Experimental results show that the fiber dispersion index of the spun alumina fiber obtained by the preparation method provided by the invention is more than 80mL/g, and the anti-vibration crushing rate of the fiber is less than 6%.
Meanwhile, the preparation method of the wire throwing alumina fiber provided by the invention solves the technical problems that the fiber formed by throwing out the wire throwing hole is easy to break and the just thrown fiber is thick and easy to adhere to each other, and has important significance in the field of alumina fiber synthesis.
Drawings
FIG. 1 is a scanning electron microscope image of a spun-spun alumina fiber provided in example 1 of the present invention;
FIG. 2 is a scanning electron micrograph of a spun-spun alumina fiber according to comparative example 1 of the present invention;
FIG. 3 is a scanning electron micrograph of a spun alumina fiber according to comparative example 2 of the present invention.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a preparation method of a spinning alumina fiber, which comprises the following steps:
a) mixing polyaluminium chloride sol and silica sol, adding a spinning auxiliary agent and a crystalline phase sintering auxiliary agent for reaction to obtain alumina sol to be spun into fibers; adding the emulsified paraffin solution to obtain a spinning solution;
b) spinning and collecting cotton in turn on the spinning solution obtained in the step a) to obtain spinning fibers;
c) carrying out heat treatment on the spun fibers obtained in the step b) to obtain spun alumina fibers.
Firstly, mixing polyaluminium chloride sol and silica sol, adding a spinning auxiliary agent and a crystalline phase sintering auxiliary agent for reaction to obtain the alumina sol to be spun into fibers. In the invention, the polyaluminum chloride sol is an aluminum source; al of the polyaluminum chloride sol2O3The content is preferably 25 to 35 wt%, more preferably 25 wt%. In the present invention, the preparation process of the polyaluminum chloride sol preferably comprises:
mixing aluminum powder, hydrochloric acid and distilled water, heating and refluxing at 60-110 ℃ to obtain polyaluminum chloride sol, and cooling to room temperature for later use;
more preferably:
mixing aluminum powder, hydrochloric acid and distilled water, heating and refluxing at 70-90 ℃ to obtain polyaluminum chloride sol, and cooling to room temperature for later use. The sources of the aluminum powder and hydrochloric acid are not particularly limited in the present invention, and commercially available products known to those skilled in the art may be used. In the present invention, the purity of the powdery aluminum is preferably 99% or more, WFe2O3% preferably 0.01%; the above-mentionedThe particle size of the aluminum powder is preferably 200 to 600 mesh.
In the invention, the molar ratio of the aluminum powder, the hydrochloric acid (calculated as HCl) and the distilled water is preferably (1.6-2): 1: (10-30), more preferably 1.6: 1: 22.75.
in the invention, the silica sol is a silicon source; the silica sol is preferably prepared from tetraethoxysilane, the pH is preferably 2-4, and the granularity is preferably 10-20 nm; SiO of the silica sol2The content is preferably 20 wt% to 30 wt%. The source of the tetraethoxysilane is not particularly limited in the present invention, and commercially available products known to those skilled in the art may be used.
In the present invention, Al in the polyaluminum chloride sol2O3And SiO in silica sol2The mass ratio of (1) to (100): (0-30), more preferably (70-90): (10-30), more preferably 80: 20.
the mixing process is not particularly limited, and the technical scheme of manual stirring or mechanical stirring which is well known to those skilled in the art can be adopted, so that the raw materials are uniformly mixed.
In the invention, the spinning auxiliary agent is preferably prepared from the following components in a mass ratio of (0.5-1): (5-8): (0.2-0.8): 100 of lactic acid, polyvinyl alcohol, alcohol and water, more preferably from the group consisting of 0.75: 6: 0.5: 100 of lactic acid, polyvinyl alcohol, alcohol and water. The sources of the lactic acid, polyvinyl alcohol and alcohol are not particularly limited in the present invention, and commercially available products well known to those skilled in the art may be used; wherein the average molecular weight of the polyvinyl alcohol is preferably 103～107The alkalization degree is preferably 75-95.
In the present invention, the addition amount of the spinning aid is preferably Al2O312 to 18 wt% of solid content, more preferably Al2O315% by weight of the solids content.
In the present invention, the crystalline phase firing aid is preferably one or more selected from a magnesium chloride solution, a boric acid solution, a zirconium acetate solution, and a calcium chloride aqueous solution, and more preferably a calcium chloride aqueous solution. The invention is used for preparing the crystal phase sintering aidThe source is not particularly limited, and commercially available products of the above magnesium chloride solution (concentration of 25 wt% to 35 wt%), boric acid solution (concentration of 3 wt%), zirconium acetate solution (concentration of 15 wt% to 16 wt% in terms of Zr), and calcium chloride aqueous solution (concentration of 30 wt% to 40 wt%) known to those skilled in the art may be used. In the present invention, the amount of the crystal phase sintering aid added (measured as solute in the solution) is preferably Al2O30.5 to 5 wt% of the solid content, more preferably Al2O32% by weight of the solids content.
In the present invention, the temperature of the reaction is preferably 80 to 120 ℃, more preferably 100 ℃; the reaction time is preferably 2 to 5 hours, more preferably 3 hours.
The present invention preferably further comprises, after the reaction:
and cooling and aging the alumina sol obtained by the reaction to obtain the alumina sol to be spun into fibers.
After the alumina sol for spinning is obtained, the emulsified paraffin solution is added into the alumina sol to obtain the spinning solution. In the invention, the pH value of the emulsified paraffin solution is preferably 6-7, the solid active ingredient is preferably more than 99%, and the solid content of the emulsion is preferably 1-50%.
In the present invention, the preparation process of the emulsified paraffin solution is preferably specifically:
diluting the emulsified paraffin with water, slightly shaking or slightly stirring the emulsified paraffin in hot water at the temperature of between 60 and 80 ℃ to naturally form uniform fluid, and preparing the uniform fluid to obtain an emulsified paraffin solution with the concentration of between 50 and 60 weight percent;
more preferably:
diluting the emulsified paraffin with water, slightly shaking or slightly stirring in hot water of 80 ℃ to naturally form uniform fluid, and preparing to obtain an emulsified paraffin solution with the concentration of 55 wt%. In the invention, the emulsified paraffin is preferably water-soluble solid self-emulsified water-soluble paraffin which is solid at normal temperature and can be directly used after being diluted to the required concentration; the source of the emulsified paraffin is not particularly limited in the present invention, and commercially available products well known to those skilled in the art may be used.
In the invention, the addition amount of the emulsified paraffin solution is preferably 0.1-2% of the mass of the alumina sol to be subjected to spinning and fiber forming, and more preferably 0.5% of the mass of the alumina sol to be subjected to spinning and fiber forming. In the invention, the emulsified paraffin solution is added to play a fiber forming lubricating role, isolate the fiber from a high-humidity environment, greatly reduce the influence of the high-temperature high-humidity fiber forming environment on the fiber, and avoid the fiber defect caused by adhesion after the fiber is touched as much as possible; however, the excessive concentration can cause more burning-off of organic matters during heat treatment, which is not beneficial to energy conservation and environmental protection; and the concentration is too low, the lubrication and isolation effect is not obvious, and the fiber lubrication and isolation are incomplete.
After the spinning solution is obtained, the spinning solution is sequentially subjected to spinning and cotton collection to obtain the spinning fibers. In the invention, the spinning process preferably adopts spinning and cotton collecting equipment; the spinning process preferably comprises the following steps:
the primary upward blowing wind pressure is 0.2MPa to 0.4MPa, an included angle of 50 degrees to 70 degrees is formed between the primary upward blowing wind pressure and the tangential direction of the throwing disc, the secondary upward blowing wind pressure is 0.06MPa to 0.2MPa, an included angle of 70 degrees to 90 degrees is formed between the primary upward blowing wind pressure and the tangential direction of the throwing disc, the primary downward induced wind pressure is 0.3MPa to 0.5MPa, the primary downward induced wind pressure is 1m to 2m above the cotton collecting net, the secondary downward induced wind pressure is 0.1MPa to 0.3MPa, the curing distance is 3m to 7m, the wind temperature is 120 ℃ to 145 ℃, and the rotating speed of the throwing disc is 20Hz to 40 Hz;
more preferably:
the primary upward blowing air pressure is 0.25MPa, an included angle of 50 degrees is formed between the primary upward blowing air pressure and the tangential direction of the silk throwing disc, the secondary upward blowing air pressure is 0.1MPa, an included angle of 70 degrees is formed between the primary upward blowing air pressure and the tangential direction of the silk throwing disc, the primary downward induced air pressure is 0.3MPa, the primary upward blowing air pressure is 1-2 m above the cotton collecting net, the secondary downward induced air pressure is 0.15MPa, the curing distance is 7m, the air temperature is 145 ℃, and the rotating speed of the silk throwing disc is 40 Hz.
The invention adopts the spinning process with the specific steps, conditions and parameters, wherein primary up-blowing is a fiber forming effect, secondary up-blowing is a blowing-off effect, and lower induced air is used for matching air flow; wind pressure is adjusted, namely wind power is adjusted, the fibers are blown away by the wind power within a certain range, and the force acting on the fibers can be effectively exerted only by matching with the fiber forming direction when the wind power is applied; meanwhile, the air flow stability in the cotton collecting chamber is ensured by the coordination of air induction and upward blowing. The matching adjustment of the spinning (fiber forming) process can ensure that the quality and the length of the fiber can be controlled within a required range.
The invention has no special limitation on the cotton collection, and the technical scheme of cotton collection well known to those skilled in the art is adopted, so that the dry and fluffy throwing fiber is obtained.
After obtaining the spun fiber, the invention carries out heat treatment on the obtained spun fiber to obtain the spun alumina fiber. In the present invention, the heat treatment process is preferably specifically:
removing the absorbed water contained in the fiber from the spun fiber at 105-150 ℃; then heating to 450-550 ℃ according to the heating rate of 5-10 ℃/min, and then preserving heat for 2-3 h; heating to 1200-1400 ℃ according to the heating rate of 10-20 ℃/min, and then preserving the heat for 30-60 min to obtain the spinning alumina fiber;
more preferably:
removing the absorbed water contained in the fiber from the spun fiber at 105 ℃; then heating to 450 ℃ according to the heating rate of 5 ℃/min, and then preserving the heat for 2-3 h; and heating to 1300 ℃ according to the heating rate of 20 ℃/min, and then preserving the heat for 50min to obtain the spinning alumina fiber.
In the invention, the process of heating to 450-550 ℃ can remove the thermal decomposition product of the organic group and part of the coordinated water.
The preparation method provided by the invention firstly adopts a specific formula to obtain the spinning solution suitable for the spinning process, and then combines specific process steps and conditions to realize better interaction, so that the obtained spinning alumina fiber has smooth surface and less doubling, and meanwhile, the fiber is long and is not easy to break. The invention provides a preparation method of a spinning alumina fiber, which comprises the following steps: a) mixing polyaluminium chloride sol and silica sol, adding a spinning auxiliary agent and a crystalline phase sintering auxiliary agent for reaction to obtain alumina sol to be spun into fibers; adding the emulsified paraffin solution to obtain a spinning solution; b) spinning and collecting cotton in turn on the spinning solution obtained in the step a) to obtain spinning fibers; c) carrying out heat treatment on the spun fibers obtained in the step b) to obtain spun alumina fibers. Compared with the prior art, the preparation method provided by the invention firstly adopts a specific formula to obtain the spinning solution suitable for the spinning process, and then combines specific process steps and conditions to realize better interaction, so that the obtained spinning alumina fiber has smooth surface, less doubling, long fiber and difficult fracture. Experimental results show that the fiber dispersion index of the spun alumina fiber obtained by the preparation method provided by the invention is more than 80mL/g, and the anti-vibration crushing rate of the fiber is less than 6%.
Meanwhile, the preparation method of the wire throwing alumina fiber provided by the invention solves the technical problems that the fiber formed by throwing out the wire throwing hole is easy to break and the just thrown fiber is thick and easy to adhere to each other, and has important significance in the field of alumina fiber synthesis.
To further illustrate the present invention, the following examples are provided for illustration. The raw materials used in the following examples of the present invention are all commercially available; wherein the purity of the aluminum powder is more than 99 percent, WFe2O3Less than or equal to 0.01 percent and 200-600 meshes; hydrochloric acid (HCl, 36.5%), analytically pure; lactic acid, technical grade; polyvinyl alcohol having an average molecular weight of 103～107The alkalization degree is 75-95; alcohol, technical grade; the silica sol is prepared from tetraethoxysilane (analytically pure), the pH value is 2-4, the granularity is 10 nm-20 nm, and the WSiO is2% is 20% -30%; the concentration of the calcium chloride aqueous solution is 30-40 wt%; emulsified paraffin, water-soluble solid self-emulsified water-soluble wax, diluting to the required concentration and then directly using, the liquid is neutral, the pH is 6-7, the solid active ingredient is more than 99%, the solid content of the emulsion is 1% -50%, the appearance is light yellow or milky white solid plate-shaped, the phenomena of layering, filling and obvious impurity mixing are avoided, the active ingredient is more than 98%, and the product is specifically provided by Shizhuang Jiatuo chemical technology Limited and has the specification of No. 60; the spinning process adopts a spinning and cotton collecting device (conventional, mobile cotton collecting mesh belt).
Example 1
(1) Aluminum powder, hydrochloric acid (as HCl) and distilled water are mixed according to a molar ratio of 1.6: 1: 22.75, heating and refluxing at 70-90 ℃ to obtain Al2O3Polyaluminium chloride sol with a content of 25 wt%, coolingCooling to room temperature for later use;
mixing lactic acid, polyvinyl alcohol, alcohol and water according to a mass ratio of 0.75: 6: 0.5: mixing and dissolving at normal temperature in a proportion of 100 to obtain a spinning auxiliary agent;
according to the mass ratio of aluminum oxide in an aluminum source to silicon oxide in silica sol of 80: 20, respectively weighing an aluminum source and silica sol, and uniformly mixing the aluminum source and the silica sol to obtain mixed silica-alumina sol; then adding a spinning auxiliary agent into the mixed silicon-aluminum sol according to the spinning auxiliary agent accounting for 15 wt% of the solid content of the aluminum oxide, adding a calcium chloride aqueous solution according to the calcium chloride accounting for 2 wt% of the solid content of the aluminum oxide, and polymerizing for 3 hours at 100 ℃ to obtain aluminum oxide sol; cooling and aging to obtain alumina sol to be spun into fibers;
diluting the emulsified paraffin with deionized water, slightly shaking or slightly stirring in hot water at 80 ℃ to naturally form uniform fluid, and preparing into emulsified paraffin solution with the concentration of 55 wt% to form milky white emulsion;
according to the mass ratio of 0.5: and (3) adding the emulsified paraffin wax solution into alumina sol to be spun into fibers according to the proportion of 100 to obtain spinning solution.
(2) The spinning process comprises the following steps: the primary upward blowing pressure is 0.25MPa, an included angle of 50 degrees is formed between the primary upward blowing pressure and the tangential direction of the silk throwing disc, the secondary upward blowing pressure is 0.1MPa, an included angle of 70 degrees is formed between the secondary upward blowing pressure and the tangential direction of the silk throwing disc, the primary downward induced air pressure is 0.3MPa (1-2 m above the cotton collecting net), the secondary downward induced air pressure at the bottom of the cotton collecting net is 0.15MPa, the curing distance is 7m, the air temperature is 145 ℃, and the rotating speed of the silk throwing disc is 40 Hz; obtaining precursor fiber; and collecting cotton to obtain dry and fluffy throwing fibers.
(3) Removing the absorbed water contained in the fiber from the spun fiber at 105 ℃; heating to 450 ℃ according to the heating rate of 5 ℃/min, removing the thermal decomposition product of the organic group and part of the coordination water, and preserving the heat for 2-3 h at the temperature; and heating to 1300 ℃ according to the heating rate of 20 ℃/min, and preserving the heat for 50min to obtain the spinning alumina fiber.
The scanning electron microscope image of the spun alumina fiber obtained by the preparation method provided by the embodiment 1 of the invention is shown in fig. 1, and as can be seen from fig. 1, the spun alumina fiber has a smooth surface, less yarn doubling and long fiber length. Through detection, the fiber dispersion index of the spun alumina fiber obtained by the preparation method provided by the embodiment 1 of the invention is 87mL/g, and the anti-vibration and crushing rate of the fiber is 5.2%.
Comparative example 1 (without emulsified paraffin solution)
(1) Aluminum powder, hydrochloric acid (as HCl) and distilled water are mixed according to a molar ratio of 1.6: 1: 22.75, heating and refluxing at 70-90 ℃ to obtain Al2O3Cooling the polyaluminium chloride sol with the content of 25 wt% to room temperature for later use;
mixing lactic acid, polyvinyl alcohol, alcohol and water according to a mass ratio of 0.75: 6: 0.5: mixing and dissolving at normal temperature in a proportion of 100 to obtain a spinning auxiliary agent;
according to the mass ratio of aluminum oxide in an aluminum source to silicon oxide in silica sol of 80: 20, respectively weighing an aluminum source and silica sol, and uniformly mixing the aluminum source and the silica sol to obtain mixed silica-alumina sol; then adding a spinning auxiliary agent into the mixed silicon-aluminum sol according to the spinning auxiliary agent accounting for 15 wt% of the solid content of the aluminum oxide, adding a calcium chloride aqueous solution according to the calcium chloride accounting for 2 wt% of the solid content of the aluminum oxide, and polymerizing for 3 hours at 100 ℃ to obtain aluminum oxide sol; cooling and aging to obtain alumina sol to be spun into fiber, and taking the alumina sol as spinning solution.
(2) The spinning process comprises the following steps: the primary upward blowing pressure is 0.25MPa, an included angle of 50 degrees is formed between the primary upward blowing pressure and the tangential direction of the silk throwing disc, the secondary upward blowing pressure is 0.1MPa, an included angle of 70 degrees is formed between the secondary upward blowing pressure and the tangential direction of the silk throwing disc, the primary downward induced air pressure is 0.3MPa (1-2 m above the cotton collecting net), the secondary downward induced air pressure at the bottom of the cotton collecting net is 0.15MPa, the curing distance is 7m, the air temperature is 145 ℃, and the rotating speed of the silk throwing disc is 40 Hz; obtaining precursor fiber; and obtaining the spinning fiber after cotton collection.
(3) Removing the absorbed water contained in the fiber from the spun fiber at 105 ℃; heating to 450 ℃ according to the heating rate of 5 ℃/min, removing the thermal decomposition product of the organic group and part of the coordination water, and preserving the heat for 2-3 h at the temperature; and heating to 1300 ℃ according to the heating rate of 20 ℃/min, and preserving the heat for 50min to obtain the spinning alumina fiber.
The scanning electron microscope image of the spun alumina fiber obtained by the preparation method provided by comparative example 1 of the invention is shown in fig. 2. Through detection, the fiber dispersion index of the spun alumina fiber obtained by the preparation method provided by the comparative example 1 is 43mL/g, and the anti-vibration crushing rate of the fiber is 8%.
COMPARATIVE EXAMPLE 2 (wind temperature and wind pressure too low)
(1) Aluminum powder, hydrochloric acid (as HCl) and distilled water are mixed according to a molar ratio of 1.6: 1: 22.75, heating and refluxing at 70-90 ℃ to obtain Al2O3Cooling the polyaluminium chloride sol with the content of 25 wt% to room temperature for later use;
mixing lactic acid, polyvinyl alcohol, alcohol and water according to a mass ratio of 0.75: 6: 0.5: mixing and dissolving at normal temperature in a proportion of 100 to obtain a spinning auxiliary agent;
according to the mass ratio of aluminum oxide in an aluminum source to silicon oxide in silica sol of 80: 20, respectively weighing an aluminum source and silica sol, and uniformly mixing the aluminum source and the silica sol to obtain mixed silica-alumina sol; then adding a spinning auxiliary agent into the mixed silicon-aluminum sol according to the spinning auxiliary agent accounting for 15 wt% of the solid content of the aluminum oxide, adding a calcium chloride aqueous solution according to the calcium chloride accounting for 2 wt% of the solid content of the aluminum oxide, and polymerizing for 3 hours at 100 ℃ to obtain aluminum oxide sol; cooling and aging to obtain alumina sol to be spun into fibers;
diluting the emulsified paraffin with deionized water, slightly shaking or slightly stirring in hot water at 80 ℃ to naturally form uniform fluid, and preparing into emulsified paraffin solution with the concentration of 55 wt% to form milky white emulsion;
according to the mass ratio of 0.5: and (3) adding the emulsified paraffin wax solution into alumina sol to be spun into fibers according to the proportion of 100 to obtain spinning solution.
(2) The spinning process comprises the following steps: the primary upward blowing pressure is 0.15MPa, an included angle of 50 degrees is formed between the primary upward blowing pressure and the tangential direction of the silk throwing disc, the secondary upward blowing pressure is 0.05MPa, an included angle of 70 degrees is formed between the secondary upward blowing pressure and the tangential direction of the silk throwing disc, the primary downward induced air pressure is 0.3MPa (1-2 m above the cotton collecting net), the secondary downward induced air pressure at the bottom of the cotton collecting net is 0.15MPa, the curing distance is 7m, the air temperature is 100 ℃, and the rotating speed of the silk throwing disc is 40 Hz; obtaining precursor fiber; and obtaining the spinning fiber after cotton collection.
(3) Removing the absorbed water contained in the fiber from the spun fiber at 105 ℃; heating to 450 ℃ according to the heating rate of 5 ℃/min, removing the thermal decomposition product of the organic group and part of the coordination water, and preserving the heat for 2-3 h at the temperature; and heating to 1300 ℃ according to the heating rate of 20 ℃/min, and preserving the heat for 50min to obtain the spinning alumina fiber.
The scanning electron microscope image of the spun alumina fiber obtained by the preparation method provided by the comparative example 2 of the invention is shown in fig. 3. Through detection, the fiber dispersion index of the spun alumina fiber obtained by the preparation method provided by the comparative example 2 is 46mL/g, and the anti-vibration crushing rate of the fiber is 7.4%.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (10)
1. A preparation method of a spinning alumina fiber comprises the following steps:
a) mixing polyaluminium chloride sol and silica sol, adding a spinning auxiliary agent and a crystalline phase sintering auxiliary agent for reaction to obtain alumina sol to be spun into fibers; adding the emulsified paraffin solution to obtain a spinning solution;
b) spinning and collecting cotton in turn on the spinning solution obtained in the step a) to obtain spinning fibers;
c) carrying out heat treatment on the spun fibers obtained in the step b) to obtain spun alumina fibers.
2. The method according to claim 1, wherein Al of the polyaluminum chloride sol in step a)2O3The content is 25 wt% -35 wt%; SiO of the silica sol2The content is 20 wt% -30 wt%;
al in the polyaluminum chloride sol2O3And SiO in silica sol2The mass ratio of (70-100): (0 to 30).
3. The preparation method of claim 1, wherein the spinning aid in the step a) is prepared from the following components in a mass ratio of (0.5-1): (5-8): (0.2-0.8): 100 of lactic acid, polyvinyl alcohol, alcohol and water.
4. The method according to claim 1, wherein the spinning aid is added in the amount of Al in step a)2O312 to 18 weight percent of solid content.
5. The method for preparing the ceramic tile as claimed in claim 1, wherein the crystalline phase sintering aid in the step a) is one or more selected from a magnesium chloride solution, a boric acid solution, a zirconium acetate solution and a calcium chloride aqueous solution.
6. The method according to claim 1, wherein the reaction in step a) is carried out at a temperature of 80 ℃ to 120 ℃ for 2h to 5 h.
7. The method according to claim 1, wherein the emulsified paraffin solution in step a) is prepared by the following steps:
diluting the emulsified paraffin with water, slightly shaking or slightly stirring the diluted emulsified paraffin in hot water at the temperature of between 60 and 80 ℃ to naturally form uniform fluid, and preparing the uniform fluid to obtain an emulsified paraffin solution with the concentration of between 50 and 60 weight percent.
8. The preparation method according to claim 1, wherein the addition amount of the emulsified paraffin solution in the step a) is 0.1-2% of the mass of the alumina sol to be spun into fiber.
9. The preparation method according to claim 1, wherein the spinning process in step b) adopts a spinning and cotton collecting device, which specifically comprises: the primary upward blowing wind pressure is 0.2MPa to 0.4MPa, an included angle of 50 degrees to 70 degrees is formed between the primary upward blowing wind pressure and the tangential direction of the throwing disc, the secondary upward blowing wind pressure is 0.06MPa to 0.2MPa, an included angle of 70 degrees to 90 degrees is formed between the primary upward blowing wind pressure and the tangential direction of the throwing disc, the primary downward induced wind pressure is 0.3MPa to 0.5MPa, the primary downward induced wind pressure is 1m to 2m above the cotton collecting net, the secondary downward induced wind pressure is 0.1MPa to 0.3MPa, the curing distance is 3m to 7m, the wind temperature is 120 ℃ to 145 ℃, and the rotating speed of the throwing disc is 20Hz to 40 Hz.
10. The method according to claim 1, wherein the heat treatment in step c) is carried out by:
removing the absorbed water contained in the fiber from the spun fiber at 105-150 ℃; then heating to 450-550 ℃ according to the heating rate of 5-10 ℃/min, and then preserving heat for 2-3 h; and then heating to 1200-1400 ℃ according to the heating rate of 10-20 ℃/min, and then preserving the heat for 30-60 min to obtain the spinning alumina fiber.
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| CN102070326A (en) * | 2010-11-30 | 2011-05-25 | 西安交通大学 | Preparation process of multi-element composite alumina-based continuous fibers |
| CN103408292A (en) * | 2013-07-26 | 2013-11-27 | 山东大学 | Preparation method for alumina-zirconia ceramic fiber |
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| CN102070326A (en) * | 2010-11-30 | 2011-05-25 | 西安交通大学 | Preparation process of multi-element composite alumina-based continuous fibers |
| CN103408292A (en) * | 2013-07-26 | 2013-11-27 | 山东大学 | Preparation method for alumina-zirconia ceramic fiber |
| CN106544757A (en) * | 2016-11-25 | 2017-03-29 | 陕西聚洁瀚化工有限公司 | Get rid of the method that a method prepares polycrystalline alumina fiber |
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