CN117263237A - Preparation method of aluminum titanate nanofiber - Google Patents

Preparation method of aluminum titanate nanofiber Download PDF

Info

Publication number
CN117263237A
CN117263237A CN202311200166.3A CN202311200166A CN117263237A CN 117263237 A CN117263237 A CN 117263237A CN 202311200166 A CN202311200166 A CN 202311200166A CN 117263237 A CN117263237 A CN 117263237A
Authority
CN
China
Prior art keywords
aluminum titanate
aluminum
stirring
nanofiber
needle
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN202311200166.3A
Other languages
Chinese (zh)
Inventor
张尚权
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Anhui Keang New Material Technology Co ltd
Original Assignee
Anhui Keang New Material Technology Co ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Anhui Keang New Material Technology Co ltd filed Critical Anhui Keang New Material Technology Co ltd
Priority to CN202311200166.3A priority Critical patent/CN117263237A/en
Publication of CN117263237A publication Critical patent/CN117263237A/en
Pending legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G23/00Compounds of titanium
    • C01G23/003Titanates
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/01Particle morphology depicted by an image
    • C01P2004/03Particle morphology depicted by an image obtained by SEM
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/10Particle morphology extending in one dimension, e.g. needle-like
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/32Thermal properties

Abstract

The invention discloses a preparation method of aluminum titanate nanofiber, and belongs to the technical field of aluminum titanate. Adding spinning auxiliary agent into N, N-dimethylformamide solution, stirring strongly, adding organic acid for acidification, selecting aluminum isopropoxide as an aluminum source, adding the aluminum source into the acidified solution, dissolving aluminum isopropoxide into a titanium source, stirring fully, spinning by electrostatic spinning, and calcining the spun fiber in a muffle furnace to obtain the aluminum titanate nanofiber. The method has the advantages of simple process, low equipment requirement, mild reaction condition and low preparation cost; the prepared aluminum titanate has a nanofiber structure, the diameter of the calcined aluminum titanate is 200-500nm, the thermal expansion coefficient is low, compared with common aluminum titanate, the aluminum titanate has the advantages of lower sintering temperature, better thermal shock resistance and obviously improved mechanical strength, and the improved properties enable the aluminum titanate nanofiber to be widely applied in manufacturing and have important application significance.

Description

Preparation method of aluminum titanate nanofiber
Technical Field
The invention belongs to the technical field of aluminum titanate, and particularly relates to a preparation method of aluminum titanate nanofiber.
Background
Along with the rapid development of modern industry and high-temperature technology, the demand for fiber materials with high-temperature resistance, good thermal shock resistance and other comprehensive properties is more and more urgent, and the traditional aluminum silicate and other materials cannot meet the requirements of severe environments with high temperatures above 1350 ℃. Aluminum titanate (Al) 2 TiO 5 ) The material not only has high melting point (1860+/-10 ℃), but also has low thermal expansion coefficient (alpha is less than 1.5X10) -6 Low thermal conductivity (1.5W/(mK)), and hasHas the characteristics of excellent thermal shock resistance, strong acid and alkali corrosion resistance and the like, and is widely applied to the fields of military industry, metallurgy, kiln, environmental protection, automobile manufacturing, glass manufacturing and the like. The products which can be manufactured are as follows: a temperature thermocouple protective sleeve, a metallurgical industry pipeline, an automobile engine exhaust pipe, a high-grade refractory material and the like. However, aluminum titanate has poor mechanical properties, microcracks occur in the cooling process, and aluminum titanate is easy to decompose at low temperature and has poor thermal stability, which limit the application field of aluminum titanate.
In this regard, the chinese patent application of related art publication No. CN101172851a discloses a method for preparing a spinnable sol of aluminum titanate fiber, but the sol preparation process related to the present invention involves acid corrosion and vacuum treatment, which has high requirements on equipment and high preparation cost, and if the aluminum titanate nanofiber needs to be prepared, the spinnability of the sol needs to be further improved. The invention discloses an aluminum titanate nanofiber and a preparation method thereof, wherein the invention adopts a hydrothermal method, the hydrothermal reaction temperature is difficult to control, the technical difficulty is high, and the safety performance is poor.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a preparation method of aluminum titanate nanofiber.
The aim of the invention can be achieved by the following technical scheme:
the preparation method of the aluminum titanate nanofiber comprises the following steps:
s1, dissolving a spinning aid (PVP or PVB) in N, N-Dimethylformamide (DMF) in a three-neck flask with a stirring device, and stirring and uniformly mixing to obtain a mixed solution; the dosage ratio of polyvinylpyrrolidone to N, N-dimethylformamide is 5g to 100mL;
s2, adding organic acid (one or more of formic acid, acetic acid and propionic acid) into a three-neck flask provided with a stirring device, mixing with the mixed solution, stirring fully, then adding Aluminum Isopropoxide (AIP), stirring rapidly, then slowly adding a titanium source (tetrabutyl titanate or isopropyl titanate), and stirring fully for 8 hours until the mixture is completely dissolved to obtain spinning solution; the ratio of the dosage of the mixed solution, the organic acid, the aluminum isopropoxide and the titanium source is 100mL to 20-40g to 10-20g;
s3, transferring the spinning solution into a needle tube, mounting a flat-mouth needle, loading on a propelling device, loading 10kV-30kV positive pressure on the needle, loading 10kV-30kV negative pressure on a collecting roller, carrying out electrostatic spinning, setting the humidity to be 30% -70%, controlling the temperature to be 10 ℃ -30 ℃, pushing the needle at the speed of 2mL/h, and collecting on a collector to obtain a fibrous membrane;
and S4, placing the fiber membrane into a muffle furnace, heating to 800-1000 ℃ at a heating speed of 5 ℃/min for 1-3 h, and removing organic matters to obtain the aluminum titanate nanofiber.
The invention has the beneficial effects that:
the aluminum titanate nanofiber obtained by the invention has the advantages of simple process, lower equipment requirement, mild reaction condition, low preparation cost, low energy consumption and no harmful emission, is particularly suitable for large-scale production, has a nanofiber structure, has the diameter of 200-500nm after calcination, has the advantage of low thermal expansion coefficient of aluminum titanate, has lower sintering temperature and better thermal shock resistance compared with common aluminum titanate, and has better mechanical strength, particularly obviously improved flexural strength, and the improved properties can lead the prepared aluminum titanate nanofiber to be widely applied in the fields of nonferrous metallurgy with high requirements on high temperature resistance and thermal shock resistance, the manufacturing of products such as high-performance ceramic nozzles, ceramic pipes, ceramic molds and the like, and have important application significance.
Drawings
The invention is further described below with reference to the accompanying drawings.
FIG. 1 is a scanning electron microscope image of an aluminum titanate nanofiber prepared in example 3 of the present invention.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
Preparation of aluminum titanate nanofibers
S1, dissolving 5g of PVP in 100mL of N, N-dimethylformamide in a three-neck flask with a stirring device, and uniformly stirring and mixing to obtain a mixed solution;
s2, adding 20mL of acetic acid and 100mL of mixed solution into a three-neck flask with a stirring device, fully stirring, then adding 20g of aluminum isopropoxide, rapidly stirring, slowly adding 10g of tetrabutyl titanate, and fully stirring for 8 hours until the mixture is completely dissolved to obtain spinning solution;
s3, transferring the spinning solution into a needle tube, installing a flat-mouth needle, loading on a propelling device, loading 10kV positive pressure on the needle, loading 10kV negative pressure on a collecting roller, setting the humidity to be 30%, controlling the temperature to be 10 ℃, pushing the needle at the speed of 2mL/h, and collecting on a collector to obtain a fibrous membrane;
and S4, placing the fiber membrane into a muffle furnace, heating to 800 ℃ for 1h, and removing organic matters to obtain the aluminum titanate nanofiber.
Example 2
Preparation of aluminum titanate nanofibers
S1, dissolving 5g of PVP in 100mL of N, N-dimethylformamide in a three-neck flask with a stirring device, and uniformly stirring and mixing to obtain a mixed solution;
s2, adding 20mL of acetic acid into a three-neck flask with a stirring device, mixing with 100mL of mixed solution, fully stirring, then adding 30g of aluminum isopropoxide, rapidly stirring, slowly adding 15g of tetrabutyl titanate, and fully stirring for 8 hours until the mixture is completely dissolved to obtain spinning solution;
s3, transferring the spinning solution into a needle tube, installing a flat-mouth needle, loading on a propelling device, loading 10kV positive pressure on the needle, loading 10kV negative pressure on a collecting roller, setting the humidity to be 30%, controlling the temperature to be 10 ℃, pushing the needle at the speed of 2mL/h, and collecting on a collector to obtain a fibrous membrane;
and S4, placing the fiber membrane into a muffle furnace, heating to 800 ℃ for 1h, and removing organic matters to obtain the aluminum titanate nanofiber.
Example 3
Preparation of aluminum titanate nanofibers
S1, dissolving 5g of PVP in 100mL of N, N-dimethylformamide in a three-neck flask with a stirring device, and uniformly stirring and mixing to obtain a mixed solution;
s2, adding 20mL of acetic acid into a three-neck flask with a stirring device, mixing with 100mL of the mixed solution, fully stirring, then adding 40g of aluminum isopropoxide, rapidly stirring, slowly adding 20g of tetrabutyl titanate, and fully stirring for 8 hours until the mixture is completely dissolved to obtain spinning solution;
s3, transferring the spinning solution into a needle tube, installing a flat-mouth needle, loading on a propelling device, loading 10kV positive pressure on the needle, loading 10kV negative pressure on a collecting roller, setting the humidity to be 30%, controlling the temperature to be 10 ℃, pushing the needle at the speed of 2mL/h, and collecting on a collector to obtain a fibrous membrane;
and S4, placing the fiber membrane into a muffle furnace, heating to 800 ℃ for 1h, and removing organic matters to obtain the aluminum titanate nanofiber.
As shown in FIG. 1, a scanning electron microscope image of the aluminum titanate nanofiber prepared in example 3 was obtained.
Example 4
Preparation of aluminum titanate nanofibers
S1, dissolving 5g of PVB in 100mL of N, N-dimethylformamide in a three-neck flask with a stirring device, and stirring and mixing uniformly to obtain a mixed solution;
s2, adding 20mL of acetic acid into a three-neck flask with a stirring device, mixing with 100mL of the mixed solution, fully stirring, then adding 40g of aluminum isopropoxide, rapidly stirring, slowly adding 20g of tetrabutyl titanate, and fully stirring for 8 hours until the mixture is completely dissolved to obtain spinning solution;
s3, transferring the spinning solution into a needle tube, installing a flat-mouth needle, loading on a propelling device, loading 10kV positive pressure on the needle, loading 10kV negative pressure on a collecting roller, setting the humidity to be 30%, controlling the temperature to be 10 ℃, pushing the needle at the speed of 2mL/h, and collecting on a collector to obtain a fibrous membrane;
and S4, placing the fiber membrane into a muffle furnace, heating to 800 ℃ for 1h, and removing organic matters to obtain the aluminum titanate nanofiber.
Example 5
Preparation of aluminum titanate nanofibers
S1, dissolving 5g of PVP in 100mL of N, N-dimethylformamide in a three-neck flask with a stirring device, and uniformly stirring and mixing to obtain a mixed solution;
s2, adding 20mL of acetic acid and 100mL of mixed solution into a three-neck flask with a stirring device, fully stirring, then adding 40g of aluminum isopropoxide, rapidly stirring, slowly adding 20g of isopropyl titanate, and fully stirring for 8 hours until the mixture is completely dissolved to obtain spinning solution;
s3, transferring the spinning solution into a needle tube, installing a flat-mouth needle, loading on a propelling device, loading 10kV positive pressure on the needle, loading 10kV negative pressure on a collecting roller, setting the humidity to be 30%, controlling the temperature to be 10 ℃, pushing the needle at the speed of 2mL/h, and collecting on a collector to obtain a fibrous membrane;
and S4, placing the fiber membrane into a muffle furnace, heating to 800 ℃ for 1h, and removing organic matters to obtain the aluminum titanate nanofiber.
Example 6
Preparation of aluminum titanate nanofibers
S1, dissolving 5g of PVP in 100mL of N, N-dimethylformamide in a three-neck flask with a stirring device, and uniformly stirring and mixing to obtain a mixed solution;
s2, adding 20mL of acetic acid into a three-neck flask with a stirring device, mixing with 100mL of the mixed solution, fully stirring, then adding 40g of aluminum isopropoxide, rapidly stirring, slowly adding 20g of tetrabutyl titanate, and fully stirring for 8 hours until the mixture is completely dissolved to obtain spinning solution;
s3, transferring the spinning solution into a needle tube, installing a flat-mouth needle, loading on a propelling device, loading 30kV positive pressure on the needle, loading 30kV negative pressure on a collecting roller, setting the humidity to be 30%, controlling the temperature to be 10 ℃, pushing the needle at the speed of 2mL/h, and collecting on a collector to obtain a fibrous membrane;
and S4, placing the fiber membrane into a muffle furnace, heating to 800 ℃ for 1h, and removing organic matters to obtain the aluminum titanate nanofiber.
Example 7
Preparation of aluminum titanate nanofibers
S1, dissolving 5g of PVP in 100mL of N, N-dimethylformamide in a three-neck flask with a stirring device, and uniformly stirring and mixing to obtain a mixed solution;
s2, adding 20mL of acetic acid into a three-neck flask with a stirring device, mixing with 100mL of the mixed solution, fully stirring, then adding 40g of aluminum isopropoxide, rapidly stirring, slowly adding 20g of tetrabutyl titanate, and fully stirring for 8 hours until the mixture is completely dissolved to obtain spinning solution;
s3, transferring the spinning solution into a needle tube, installing a flat-mouth needle, loading on a propelling device, loading 10kV positive pressure on the needle, loading 10kV negative pressure on a collecting roller, setting the humidity to 70%, controlling the temperature to 30 ℃, pushing the needle at the speed of 2mL/h, and collecting on a collector to obtain a fibrous membrane;
and S4, placing the fiber membrane into a muffle furnace, heating to 800 ℃ for 1h, and removing organic matters to obtain the aluminum titanate nanofiber.
Example 8
Preparation of aluminum titanate nanofibers
S1, dissolving 5g of PVP in 100mL of N, N-dimethylformamide in a three-neck flask with a stirring device, and uniformly stirring and mixing to obtain a mixed solution;
s2, adding 20mL of acetic acid into a three-neck flask with a stirring device, mixing with 100mL of the mixed solution, fully stirring, then adding 40g of aluminum isopropoxide, rapidly stirring, slowly adding 20g of tetrabutyl titanate, and fully stirring for 8 hours until the mixture is completely dissolved to obtain spinning solution;
s3, transferring the spinning solution into a needle tube, installing a flat-mouth needle, loading on a propelling device, loading 10kV positive pressure on the needle, loading 10kV negative pressure on a collecting roller, setting the humidity to be 30%, controlling the temperature to be 10 ℃, pushing the needle at the speed of 2mL/h, and collecting on a collector to obtain a fibrous membrane;
and S4, placing the fiber membrane into a muffle furnace, heating to 1000 ℃ for 1h, and removing organic matters to obtain the aluminum titanate nanofiber.
Comparative example
The shape to be measured is made according to different standards using common aluminum titanate.
Examples 1-8, comparative examples, were prepared into corresponding shapes to be tested according to different criteria, and performance tests were performed to obtain the results shown in the following table:
as can be seen from the table, the prepared aluminum titanate has a nanofiber structure, the diameter of the nanofiber is 50-100 nm, the aluminum titanate has the advantage of low thermal expansion coefficient of aluminum titanate, and compared with common aluminum titanate, the aluminum titanate has the advantages of lower sintering temperature, better thermal shock resistance, obviously improved mechanical strength and particularly breaking strength, and the improved properties can lead the prepared aluminum titanate nanofiber to be widely applied in the fields of nonferrous metallurgy with high requirements on high temperature resistance and thermal shock resistance, mechanical manufacturing, and the manufacturing of products such as high-performance ceramic nozzles, ceramic pipe fittings, ceramic molds and the like, and have important application significance.
In the description of the present specification, the descriptions of the terms "one embodiment," "example," "specific example," and the like, mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms do not necessarily refer to the same embodiments or examples. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is merely illustrative and explanatory of the invention, as various modifications and additions may be made to the particular embodiments described, or in a similar manner, by those skilled in the art, without departing from the scope of the invention or exceeding the scope of the invention as defined in the claims.

Claims (9)

1. The preparation method of the aluminum titanate nanofiber is characterized by comprising the following steps of:
s1, dissolving a spinning aid in N, N-dimethylformamide, and uniformly stirring and mixing to obtain a mixed solution;
s2, mixing the organic acid with the mixed solution, fully stirring, then adding aluminum isopropoxide, rapidly stirring, then adding a titanium source, fully stirring until the solution is completely clarified, and obtaining spinning solution;
s3, transferring the spinning solution into a needle tube, mounting a flat-mouth needle, loading on a pushing device, loading positive pressure on the needle, loading negative pressure on a collecting roller, pushing the needle under a certain temperature and humidity, and collecting on a collector to obtain a fiber film;
and S4, placing the fiber membrane into a muffle furnace, and heating to remove organic matters to obtain the aluminum titanate nanofiber.
2. The method for preparing aluminum titanate nanofibers according to claim 1, wherein the dosage ratio of polyvinylpyrrolidone and N, N-dimethylformamide in step S1 is 5 g/100 ml.
3. The method of claim 1, wherein the spinning aid in step S1 is PVP or PVB.
4. The method for preparing aluminum titanate nanofibers according to claim 1, wherein the ratio of the amounts of the mixed solution, the organic acid, aluminum isopropoxide and the titanium source in step S2 is 100 ml:20-40g:10-20g.
5. The method for preparing aluminum titanate nanofibers according to claim 1, wherein the organic acid in step S2 is one or more of formic acid, acetic acid or propionic acid.
6. The method for preparing aluminum titanate nanofibers according to claim 1, wherein in step S2, the titanium source is tetrabutyl titanate or isopropyl titanate.
7. The method of claim 1, wherein the sufficient stirring time in step S2 is greater than 8 hours.
8. The method for preparing aluminum titanate nanofibers according to claim 1, wherein in step S3, the voltage is 10kV-30kV, the humidity is 30% -70%, and the temperature is 10 ℃ to 30 ℃.
9. The method for preparing aluminum titanate nanofibers according to claim 1, wherein the heating temperature in step S4 is 800 ℃ to 1000 ℃ and the heating time is 1h to 3h.
CN202311200166.3A 2023-09-18 2023-09-18 Preparation method of aluminum titanate nanofiber Pending CN117263237A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202311200166.3A CN117263237A (en) 2023-09-18 2023-09-18 Preparation method of aluminum titanate nanofiber

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202311200166.3A CN117263237A (en) 2023-09-18 2023-09-18 Preparation method of aluminum titanate nanofiber

Publications (1)

Publication Number Publication Date
CN117263237A true CN117263237A (en) 2023-12-22

Family

ID=89205527

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202311200166.3A Pending CN117263237A (en) 2023-09-18 2023-09-18 Preparation method of aluminum titanate nanofiber

Country Status (1)

Country Link
CN (1) CN117263237A (en)

Similar Documents

Publication Publication Date Title
CN101982581B (en) Method for preparing aluminum oxide nanofiber by electrostatic spinning
CN107653518B (en) High-orientation-degree continuous superfine/nano alumina-based ceramic fiber bundle material and preparation method thereof
CN102731104B (en) Preparation process for composite continuous ceramic fiber
CN108929049A (en) A method of Basalt fiber high-temperature resisting performance is promoted by surface modification
WO2019019365A1 (en) Method for preparing alumina-zirconia composite continuous ceramic fiber
CN104451957B (en) Low density SiC nanofiber and its preparation method
CN106145687A (en) A kind of high strength glass fiber
CN106192078B (en) A method of the preparation of low oxygen content continuous SiC fiber is carried out using air curing
CN110424068B (en) SiC fiber prepared by doping ultrahigh-temperature ceramic composite material and method and application thereof
CN115124363B (en) High-temperature-resistant ultra-light ceramic fiber porous elastomer material and preparation method and application thereof
CN111807810A (en) Preparation method of nanowire/silicon-aluminum aerogel composite material
CN113668139A (en) Flexible high-temperature-resistant SiO2Preparation method of ceramic nanofiber membrane
CN113149615A (en) Super-elastic flexible three-dimensional composite ceramic nanofiber block and preparation method and application thereof
CN114806300A (en) Metal surface composite SiO 2 Aerogel coating and preparation method thereof
CN117263237A (en) Preparation method of aluminum titanate nanofiber
CN111021155B (en) Enhanced nano heat-insulating felt and preparation method and application thereof
CN113816729A (en) Electrostatic spinning nanofiber toughened alumina ceramic and preparation method thereof
CN102180656B (en) Technology for preparing alumina-based continuous fibers by using inorganic aluminum salts
CN114736028B (en) Magnesia ceramic composite carbon fiber and preparation method thereof
CN115652479B (en) Method for preparing silicon carbide hollow microspheres by electrostatic spinning method
CN111501132B (en) Method for preparing nano zirconium boride ceramic fiber by using organic zirconium source, ceramic fiber and application
CN108914554A (en) A kind of novel environment friendly fire resisting basalt fiber cloth
CN115262032A (en) Alumina flexible fiber and preparation method thereof
CN100551824C (en) The preparation method of modified Nano boron oxide
CN115417683A (en) Preparation method of oxide continuous filament reinforced oxide ceramic matrix composite

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination