CN111218731A - Sol for preparing alumina fiber and preparation method thereof - Google Patents
Sol for preparing alumina fiber and preparation method thereof Download PDFInfo
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- CN111218731A CN111218731A CN201911370757.9A CN201911370757A CN111218731A CN 111218731 A CN111218731 A CN 111218731A CN 201911370757 A CN201911370757 A CN 201911370757A CN 111218731 A CN111218731 A CN 111218731A
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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
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Abstract
The invention provides a preparation method of a sol for preparing alumina fibers, which comprises the following steps: and stirring and mixing the polyaluminium chloride solution, the silica sol, the spinning auxiliary agent and the defoaming agent, and distilling under reduced pressure to obtain the sol for preparing the alumina fiber. The invention selects powdery polyaluminium chloride as an aluminum source for preparing the sol of the alumina fiber. Compared with the method for preparing the sol by using aluminum chloride as the aluminum source, the method for preparing the spinning sol by using the low-cost and cheap inorganic aluminum source suitable for continuous industrial production has the advantages of higher spinnability, better spinning performance and rheological performance and no pollution to the environment. Compared with aluminum sources such as aluminum powder and hydrochloric acid, the method saves energy consumption in the process of producing the aluminum sol, does not need secondary treatment on hydrogen and volatile acid gas generated in the sol preparation process, and has simple and safe process and labor saving.
Description
Technical Field
The invention relates to the technical field of materials, in particular to a sol for preparing alumina fibers and a preparation method thereof.
Background
The alumina fiber is an inorganic fiber with the advantages of high temperature resistance, high mechanical strength, chemical erosion resistance, small thermal conductivity, insulation, noise reduction and the like. Because of its high-temperature heat-insulating property is obvious, it can be extensively used in the fields of various high-temperature furnace linings of metallurgical industry, automobile and spaceflight, etc. Al thereof2O3The content is more than 67 percent, or other oxides are doped. The preparation method is characterized in that an aluminum source and a silicon source are prepared into a spinning solution by a sol-gel method, and the spinning solution is subjected to a spinning process, a blowing process, a dry extrusion process, an electrostatic spinning process to form fibers, and then the fibers are subjected to high-temperature heat treatment to form a polycrystalline crystalline phase.
When the sol of alumina fiber is prepared by the sol-gel method, the used aluminum sources are classified into organic aluminum sources and inorganic aluminum sources. Organic aluminum sources are most commonly used: aluminum isopropoxide, aluminum acetylacetonate, aluminum acetate, and the like; the organic aluminum source aluminum sol has the main advantages of uniform chemical components, high purity, low temperature of the process, and the like, and has the defects of great influence on preparation conditions, active property of alkyl aluminum alkoxide, influence on spinnability of the sol by water addition, catalyst concentration, reaction time, temperature, and the like, and high price of the alkyl aluminum alkoxide serving as an aluminum source, and environmental pollution caused by organic matters generated in the reaction process. In a word, the cost of the industrial production of the alumina sol prepared by using the organic aluminum source is high, and the reaction process is not easy to control.
The spinnability of the aluminum sol prepared by utilizing inorganic aluminum sources such as aluminum powder, aluminum salt and the like is derived from Al13 colloidal particles contained in the aluminum sol, Al13 colloidal particles have 24 active-Al-OH bonds, have high positive charges and strong bridging capacity, and are beneficial to forming long-chain molecules with other additives containing hydroxyl groups such as acidic silica sol.
Disclosure of Invention
In view of the above, the technical problem to be solved by the present invention is to provide a method for preparing a sol for preparing alumina fibers, wherein the sol for preparing alumina fibers prepared by the present invention has characteristics of low cost, safety, no environmental protection problem, and good spinning performance and rheological performance.
The invention provides a preparation method of a sol for preparing alumina fibers, which comprises the following steps:
and stirring and mixing the polyaluminium chloride solution, the silica sol solution, the spinning auxiliary agent and the defoaming agent, and distilling under reduced pressure to obtain the sol for preparing the alumina fiber.
Preferably, the polyaluminium chloride solution is an aqueous solution prepared by dissolving polyaluminium chloride powder in water; the dissolving temperature is 60-120 ℃; the mass concentration of the polyaluminium chloride in the polyaluminium chloride solution is 30-50%.
Preferably, the polyaluminium chloride parameters are specifically as follows: al (Al)2O3The content of (A) is as follows: 29 to 31 wt%; basicity: 40-65 wt%; insoluble matter is less than or equal to 0.1 wt%; fe2O3The content of (B) is less than or equal to 0.1 wt%.
Preferably, the mass ratio of the alumina in the polyaluminium chloride solution to the silica in the silica sol is 1: (0.1-0.5).
Preferably, the spinning auxiliary agent is selected from one or more of polyvinyl alcohol, polyvinylpyrrolidone, polyethylene glycol and polyvinyl acetate;
the molecular weight of the spinning auxiliary agent is 70000-120000; the alcoholysis degree is more than or equal to 80 percent;
the mass concentration of the spinning auxiliary agent is 5-10%; the solid content of the spinning auxiliary agent is 3-9 wt% of the sum of the solid contents of alumina in the polyaluminium chloride solution and silica in the silica sol solution.
Preferably, the reduced pressure distillation temperature is 120-190 ℃; the reduced pressure distillation pressure is-0.080-0.090 MPa; the time of the reduced pressure distillation is 1-5 h.
Preferably, the viscosity of the sol for preparing alumina fiber is: 800-1500 mpa.s, and the granularity is 50-100 nm; solid content: 30 to 45 wt%.
Preferably, the defoaming agent is polydimethylsiloxane; the addition amount of the defoaming agent is one thousandth of the weight of the polyaluminium chloride solution.
The invention provides a sol for preparing alumina fibers, which is prepared by the preparation method of any one of the technical schemes.
The invention provides an alumina fiber which is prepared from the sol for preparing the alumina fiber.
Compared with the prior art, the invention provides a preparation method of sol for preparing alumina fiber, which comprises the following steps: and stirring and mixing the polyaluminium chloride solution, the silica sol, the spinning auxiliary agent and the defoaming agent, and distilling under reduced pressure to obtain the sol for preparing the alumina fiber. The invention selects powdery polyaluminium chloride as an aluminum source for preparing the sol of the alumina fiber. Compared with the method for preparing the sol by using aluminum chloride as the aluminum source, the method for preparing the spinning sol by using the low-cost and cheap inorganic aluminum source suitable for continuous industrial production has the advantages of higher spinnability, better spinning performance and rheological performance and no pollution to the environment. Compared with aluminum sources such as aluminum powder and hydrochloric acid, the method saves energy consumption in the process of producing the aluminum sol, does not need secondary treatment on hydrogen and volatile acid gas generated in the sol preparation process, and has simple and safe process and labor saving.
Drawings
FIG. 1 is a diagram of a sol prepared by the method described in example 1 of the present invention;
FIG. 2 is a graph of the rheological properties of the colloid prepared in example 3 of the present invention;
FIG. 3 is a graph of the rheological properties of the colloid prepared in comparative example 1 of the present invention.
Detailed Description
The invention provides a sol for preparing alumina fiber and a preparation method thereof, and a person skilled in the art can use the content for reference and appropriately improve the process parameters to realize the preparation. It is expressly intended that all such similar substitutes and modifications apparent to those skilled in the art are deemed to be within the scope of the invention. While the methods and applications of this invention have been described in terms of preferred embodiments, it will be apparent to those of ordinary skill in the art that variations and modifications in the methods and applications described herein, as well as other suitable variations and combinations, may be made to implement and use the techniques of this invention without departing from the spirit and scope of the invention.
The invention provides a preparation method of a sol for preparing alumina fibers, which comprises the following steps:
and stirring and mixing the polyaluminium chloride solution, the silica sol, the spinning auxiliary agent and the defoaming agent, and distilling under reduced pressure to obtain the sol for preparing the alumina fiber.
The invention relates to a method for preparing sol for preparing alumina fiber, which firstly prepares polyaluminium chloride solution.
Weighing a polyaluminum chloride solution, dissolving the polyaluminum chloride solution in deionized water, heating and stirring to prepare a solution with the mass fraction of 30-50%.
The parameters of the polyaluminium chloride provided by the invention are as follows: high purity Al2O3The content of (A) is as follows: 29 to 31 wt%; basicity: 40-65 wt%; insoluble matter is less than or equal to 0.1 wt%; fe2O3The content of (B) is less than or equal to 0.1 wt%.
According to the invention, the polyaluminium chloride solution is an aqueous solution prepared by heating and dissolving polyaluminium chloride powder in water; the preferable dissolving temperature is 60-120 ℃; more preferably 80 to 110 ℃. In the present invention, the heating and dissolving method is not limited, but it is preferable to heat and continuously stir until the solution is dissolved to be a transparent solution. The present invention is not limited to the specific operation of the stirring, and those skilled in the art will be familiar with the operation.
The mass concentration of the obtained polyaluminium chloride solution is preferably 30-48%; more preferably 35 to 45%.
The presence of hydrogen and acid gas was not detected in the process.
The parameters of the silica sol are as follows: PH is 2-4, and granularity: 10 to 20nm of SiO2wt％：15～30％。
The spinning auxiliary agent is prepared into a solution with the mass concentration of 5-10%.
The spinning auxiliary agent is preferably selected from one or more of polyvinyl alcohol, polyvinylpyrrolidone, polyethylene glycol and polyvinyl acetate; more preferably polyvinyl alcohol or polyvinyl pyrrolidone.
The molecular weight of the spinning auxiliary agent is 70000-120000; the alcoholysis degree is more than or equal to 80 percent.
The mass concentration of the spinning auxiliary in the spinning auxiliary aqueous solution is preferably 5-10%; more preferably 6% to 8%.
After the polyaluminium chloride solution, the silica sol and the spinning auxiliary agent are prepared, the polyaluminium chloride solution, the silica sol, the spinning auxiliary agent and the defoaming agent are stirred and mixed. The present invention is not limited to the specific operation of the stirring, and those skilled in the art will be familiar with the operation. In the present invention, the source of the raw material is not limited and may be commercially available.
The adding sequence of the polyaluminium chloride solution, the silica sol, the spinning auxiliary agent and the defoaming agent is not limited, and the materials can be added together, or the weighed acidic silica sol, the prepared polyvinyl alcohol solution and the defoaming agent are added into the polyaluminium chloride solution and stirred uniformly.
According to the invention, the mass ratio of alumina in the polyaluminium chloride solution to silica in the silica sol is preferably 1: (0.1 to 0.5); more preferably 1 (0.1 to 0.4).
The solid content of the spinning auxiliary agent is 3-9 wt% of the sum of the solid contents of alumina in the polyaluminium chloride solution and silica in the silica sol; more preferably from 4 to 8 wt%.
The defoaming agent is polydimethylsiloxane; the addition amount of the defoaming agent is one thousandth to five thousandth of the weight of the polyaluminium chloride solution.
After stirring and mixing, the mixture was distilled under reduced pressure to obtain a sol for preparing alumina fibers.
The preferable concrete is as follows: after stirring and mixing, carrying out reduced pressure distillation, concentrating and reacting for a period of time until the sol reaches a certain viscosity and granularity, stopping reaction, taking out and pouring into a container, sealing, cooling, aging and storing. The viscosity of the sol for preparing alumina fiber according to the present invention: 800-1500 mpa.s, and the granularity is 50-100 nm; solid content: 30-45 percent. The sol has a two-dimensional linear structure, good rheological property and an irrelevant siphonage phenomenon.
The preferable reduced pressure distillation temperature is 120-190 ℃; more preferably 130-180 ℃; the reduced pressure distillation pressure is-0.080-0.090 MPa; the time of the reduced pressure distillation is 1-5 h.
The apparatus and operation of the vacuum distillation are not limited in the present invention, and those skilled in the art will be familiar with the apparatus and operation.
The invention provides a sol for preparing alumina fibers, which is prepared by the preparation method of any one of the technical schemes.
The preparation method of the sol for preparing alumina fiber according to the present invention has been described above clearly, and is not described herein again.
The invention provides an alumina fiber which is prepared from the sol for preparing the alumina fiber.
The specific method for preparing the alumina fiber is not limited in the invention, and the alumina fiber can be formed by a spinning process, a blowing process, a dry extrusion process or an electrostatic spinning process, which are well known to those skilled in the art, and then subjected to high-temperature heat treatment to form a polycrystalline crystalline phase, wherein the raw material adopts the sol for preparing the alumina fiber or the sol prepared by the preparation method, and the protection scope of the invention is defined.
The invention provides a preparation method of a sol for preparing alumina fibers, which comprises the following steps: and stirring and mixing the polyaluminium chloride solution, the silica sol solution, the spinning auxiliary agent and the defoaming agent, and distilling under reduced pressure to obtain the sol for preparing the alumina fiber. The invention selects powdery polyaluminium chloride as an aluminum source for preparing the sol of the alumina fiber. Compared with the method for preparing the sol by using aluminum chloride as the aluminum source, the method for preparing the spinning sol by using the low-cost and cheap inorganic aluminum source suitable for continuous industrial production has the advantages of higher spinnability, better spinning performance and rheological performance and no pollution to the environment. Compared with aluminum sources such as aluminum powder and hydrochloric acid, the method saves energy consumption in the process of producing the aluminum sol, does not need secondary treatment on hydrogen and volatile acid gas generated in the sol preparation process, and has simple and safe process and labor saving.
The method for detecting the escape of hydrogen and acid gas preferably comprises the following steps:
when the polyaluminium chloride is dissolved, the burning matches are close to the kettle mouth of the reaction kettle, whether the matches are burnt is more vigorous or not is observed, and as a result, the matches are extinguished quickly, and the re-burning phenomenon is not generated. After the pH test paper is wetted by ammonia water, the pH test paper is quickly close to the upper part of the liquid level of the polyaluminum chloride solution in the stirring and dissolving process, and the test paper does not discolor (the change from alkalinity to neutrality is not shown).
In order to further illustrate the present invention, a sol for preparing alumina fiber and a preparation method thereof according to the present invention will be described in detail with reference to the following examples.
Example 1
(1) 200kg of polyaluminium chloride powder (the solid content of alumina is 30%) and 400kg of deionized water are weighed, and the polyaluminium chloride powder is slowly added into the deionized water, heated at 95 ℃ and continuously stirred until the polyaluminium chloride powder is dissolved into a transparent solution. The presence of hydrogen and acid gas was not detected in the process.
(2) Weighing 78kg of acidic silica sol (the solid content of the silica is 30%); 2.55kg of polyvinyl alcohol is weighed and dissolved into a solution with the mass fraction of 8% at the temperature of 90 ℃ for later use.
(3) Adding the weighed acidic silica sol, the prepared polyvinyl alcohol solution and 0.2kg of defoaming agent into a polyaluminium chloride solution, uniformly stirring, carrying out concentration distillation at 150 ℃, keeping the vacuum degree at 0.085Mpa, and reacting for 3 hours to prepare the sol for the alumina fiber, wherein the formula is shown in figure 1.
(4) The colloid is taken out to detect that the temperature is 50 ℃, the average particle size is 60 nm-80 nm, the rheological property is detected to be non-Newtonian fluid, the colloid has a two-dimensional linear structure, is aged for 3 days at constant temperature, has the viscosity of 1900mpa.s, can be spun, and has less slag balls. Can be suitable for preparing alumina fiber. The fiber forming rate is 95.7%.
Example 2
(1) 200kg of polyaluminium chloride powder (the solid content of alumina is 30%) and 400g of deionized water are weighed, and the polyaluminium chloride powder is slowly added into the deionized water, heated at 95 ℃ and continuously stirred until the polyaluminium chloride powder is dissolved into a transparent solution. The presence of hydrogen and acid gas was not detected in the process.
(2) Weighing 50kg of acidic silica sol (the solid content of the silica is 30%); 5.25kg of polyvinyl alcohol is weighed and dissolved into a solution with the mass fraction of 8% at the temperature of 90 ℃ for later use.
(3) Adding the weighed acidic silica sol and the prepared polyvinyl alcohol solution into a polyaluminium chloride solution, uniformly stirring, carrying out concentration distillation at 150 ℃, keeping the vacuum degree at 0.085Mpa, and reacting for 3 hours to prepare the sol for the alumina fiber.
(4) The colloid is taken out to detect that the temperature is 50 ℃, the viscosity is 1100mpa.s, the average particle size is 70 nm-90 nm, the detected rheological property is non-Newtonian fluid, the colloid has a two-dimensional linear structure, is aged for 3 days at constant temperature, has the viscosity of 1900mpa.s, can be spun, and has less slag balls. Can be suitable for preparing alumina fiber. The fiber forming rate is 96.2%.
Example 3
(1) 200kg of polyaluminium chloride powder (the solid content of alumina is 30%) and 400g of deionized water are weighed, and the polyaluminium chloride powder is slowly added into the deionized water, heated at 95 ℃ and continuously stirred until the polyaluminium chloride powder is dissolved into a transparent solution. The presence of hydrogen and acid gas was not detected in the process.
(2) Weighing 50kg of acidic silica sol (the solid content of the silica is 30%); 5.25kg of polyvinyl alcohol is weighed and dissolved into a solution with the mass fraction of 8% at the temperature of 90 ℃ for later use.
(3) And adding the weighed acidic silica sol and the prepared polyvinyl alcohol solution into a polyaluminium chloride solution, uniformly stirring, carrying out concentration distillation at 180 ℃, keeping the vacuum degree at 0.085Mpa, and reacting for 3.5 hours to prepare the sol for the alumina fiber.
(4) The colloid is taken out to detect that the temperature is 50 ℃, the viscosity is 2150mpa.s, the average particle size is 90 nm-100 nm, the detected rheological property is non-Newtonian fluid, the colloid has a two-dimensional linear structure, is aged for 3 days at constant temperature, has the viscosity of 3000mpa.s, can be spun into fibers, and has fewer slag balls. Can be suitable for preparing alumina fiber. The fiber forming rate is 95.4%. FIG. 2 is a graph of the rheological properties of the colloid prepared in example 3 of the present invention;
comparative example 1
(1) 200kg of anhydrous aluminum chloride powder (the solid content of alumina is 30%) and 400g of deionized water are weighed, and the anhydrous aluminum chloride powder is slowly added into the deionized water, heated at 95 ℃ and continuously stirred until the anhydrous aluminum chloride powder is dissolved into a transparent solution. The presence of hydrogen and acid gas was not detected in the process.
(2) Weighing 50kg of acidic silica sol (the solid content of the silica is 30%); 5.25kg of polyvinyl alcohol is weighed and dissolved into a solution with the mass fraction of 8% at the temperature of 90 ℃ for later use.
(3) And adding the weighed acidic silica sol and the prepared polyvinyl alcohol solution into a polyaluminium chloride solution, uniformly stirring, carrying out concentration distillation at 180 ℃, keeping the vacuum degree at 0.085Mpa, and reacting for 3.5 hours to prepare the sol for the alumina fiber.
(4) The colloid is taken out to detect that the temperature is 50 ℃, the viscosity is 1350mpa.s, the average particle size is 40 nm-50 nm, the detected rheological property is non-Newtonian fluid, the two-dimensional linear structure is not obvious, the constant-temperature aging is carried out for 3 days, the viscosity is 1600mpa.s, and the spinning effect is poor. Is not suitable for preparing alumina fiber. The fiber forming rate is 70.3%. FIG. 3 is a graph of the rheological properties of the colloid prepared in comparative example 1 of the present invention. It can be seen from fig. 2 and 3 that the alumina sol with suitable viscosity is more easily prepared by adopting the polyaluminium chloride powder, has obvious shear thinning phenomenon when being subjected to shearing force, has a viscosity reduction ratio of about 46 percent, and is easy to spin into fibers, while the alumina sol prepared by adopting the anhydrous aluminium chloride powder under the same process has smaller viscosity, the raw materials are not beneficial to the generation of a two-dimensional linear structure, the viscosity reduction ratio is 27 percent, and the fibers are not easy to spin into fibers, so the fiber forming rate is lower.
Comparative example 2
Aluminum powder, hydrochloric acid and distilled water are mixed according to a molar ratio of 1.8: 1: 14 to meter the material. Hydrochloric acid and distilled water were mixed and heated to 60 ℃. And (3) manually adding aluminum powder, wherein the adding rate is 20-30% per hour of the adding amount. After the addition is finished, the temperature is raised to 105 ℃ for continuous reaction for 3h, and the polyaluminium chloride sol is obtained. Avoid machinery to add the aluminite powder and cause and add the mouth and block up because of receiving the vapor, adopt artifical feeding mode, and the reinforced time is longer, increases the amount of labour. The process generates a large amount of hydrogen and volatilized acid gas, and needs to be recycled in a centralized manner so as to avoid pollution and potential safety hazards. And the open system has a large amount of water volatilization. The polyaluminium chloride powder is directly dissolved into solution, the process is simple, safe and environment-friendly, and the waste of materials and energy consumption in industrial production is reduced.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A method for preparing a sol for preparing alumina fibers, comprising:
and stirring and mixing the polyaluminium chloride solution, the silica sol, the spinning auxiliary agent and the defoaming agent, and distilling under reduced pressure to obtain the sol for preparing the alumina fiber.
2. The method according to claim 1, wherein the polyaluminum chloride solution is an aqueous solution prepared by dissolving polyaluminum chloride powder in water; the dissolving temperature is 60-120 ℃; the mass concentration of the polyaluminium chloride in the polyaluminium chloride solution is 30-50%.
3. The preparation method according to claim 1, wherein the polyaluminium chloride parameters are in particular: al (Al)2O3The content of (A) is as follows: 29 to 31 wt%; basicity: 40-65 wt%; insoluble matter is less than or equal to 0.1 wt%; fe2O3The content of (B) is less than or equal to 0.1 wt%.
4. The preparation method according to claim 1, wherein the mass ratio of the alumina in the polyaluminum chloride solution to the silica in the silica sol is 1: (0.1-0.5).
5. The preparation method according to claim 4, wherein the spinning auxiliary is one or more selected from polyvinyl alcohol, polyvinylpyrrolidone, polyethylene glycol and polyvinyl acetate;
the molecular weight of the spinning auxiliary agent is 70000-120000; the alcoholysis degree is more than or equal to 80 percent;
the mass concentration of the spinning auxiliary agent is 5-10%; the solid content of the spinning auxiliary agent is 3-9 wt% of the sum of the solid contents of alumina in the polyaluminium chloride solution and silica in the silica sol.
6. The preparation method according to claim 1, wherein the reduced pressure distillation temperature is 120 to 190 ℃; the reduced pressure distillation pressure is-0.080-0.090 MPa; the time of the reduced pressure distillation is 1-5 h.
7. The production method according to claim 1, wherein the viscosity of the sol for producing alumina fibers is: 800-1500 mpa.s, and the granularity is 50-100 nm; solid content: 30 to 45 wt%.
8. The method of claim 1, wherein the defoaming agent is polydimethylsiloxane; the addition amount of the defoaming agent is one thousandth of the weight of the polyaluminium chloride solution.
9. A sol for producing alumina fibers, characterized by being produced by the production method according to any one of claims 1 to 8.
10. An alumina fiber produced from the sol for producing alumina fiber according to claim 9.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103496724A (en) * | 2013-08-30 | 2014-01-08 | 航天特种材料及工艺技术研究所 | Preparation method of nano alumina sol and gel |
| 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 |
| CN106757523A (en) * | 2016-11-29 | 2017-05-31 | 陕西盛迈石油有限公司 | The preparation method of polycrystalline mullite fibre |
| CN107778016A (en) * | 2017-11-06 | 2018-03-09 | 陕西盛迈石油有限公司 | The method that alumina sol infusion process prepares alumina fibre |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103496724A (en) * | 2013-08-30 | 2014-01-08 | 航天特种材料及工艺技术研究所 | Preparation method of nano alumina sol and gel |
| 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 |
| CN106757523A (en) * | 2016-11-29 | 2017-05-31 | 陕西盛迈石油有限公司 | The preparation method of polycrystalline mullite fibre |
| CN107778016A (en) * | 2017-11-06 | 2018-03-09 | 陕西盛迈石油有限公司 | The method that alumina sol infusion process prepares alumina fibre |
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