A kind of preparation method of electrospinning glue solution for preparing alumina ultrafine fiber

An electrospinning and ultra-fine fiber technology, applied in the chemical characteristics of fibers, rayon manufacturing, textiles and papermaking, etc., can solve the problems of poor flexibility, unfriendly environment, and reduced fiber strength, to ensure fiber-forming properties and Continuity, broad application prospects, stable performance

Inactive Publication Date: 2016-04-20
HENAN COAL CHEM IND GROUP INST +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The above-mentioned electrospinning systems for the preparation of alumina fibers all have some defects in varying degrees: the system using inorganic aluminum compounds and aluminum-containing compound nanoparticles as the aluminum source, in order to improve spinnability, the amount of polymer spinning aid added Large, it is easy to increase the number of defects in the fiber heat treatment process, and it is easy to cause the reduction of fiber strength and flexibility after calcination; the system using aluminum acetylacetonate as the aluminum source uses acetone or dimethylformamide as the solvent, which is not friendly to the environment; AlCl 3 In the system that is the aluminum source together with aluminum isopropoxide, the sol obtained by hydrolysis-polymerization of aluminum alkoxide is an unstable system that changes with temperature, and the viscosity changes greatly with aging time. The rheological properties of the sol are not easy to control. And it takes a long time to prepare a suitable electrospinning sol

Method used

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  • A kind of preparation method of electrospinning glue solution for preparing alumina ultrafine fiber
  • A kind of preparation method of electrospinning glue solution for preparing alumina ultrafine fiber
  • A kind of preparation method of electrospinning glue solution for preparing alumina ultrafine fiber

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] ⑴ Weigh the pseudo-boehmite powder (see the TEM photo figure 1(a)) 2.54g, measure 14mL of distilled water and stir the pseudo-boehmite powder to make slurry, the concentration of adding is 2.84mol L -1 7mL of nitric acid solution, heated and stirred to 80-85°C under condensing and reflux conditions, and then cooled to room temperature to obtain aluminum sol. Add 10mL of absolute ethanol to the prepared aluminum sol, stir well, then slowly add 0.28mL tetraethyl orthosilicate, continue to stir for 2 hours, then add 1.8g of PVP, stir and dissolve to obtain a translucent spinning dope (see attached figure 1 (b)).

[0033] (2) Inject the spinning glue prepared in step (1) into a 20mL plastic syringe, using a No. 16 stainless steel blunt needle, the feeding rate is 2.1mL / h, the voltage is 20kV, the receiving distance is 20cm, and the humidity in the spinning machine cavity 30%, electrospinning at a temperature of 52°C to prepare alumina precursor fibers.

[0034] (3) Pl...

Embodiment 2

[0037] Take 1.56g of pseudo-boehmite powder, measure 13mL of distilled water to stir the pseudo-boehmite powder, and add the concentration of 1.51mol L -1 13mL of nitric acid solution, heated and stirred to 80-85°C under the condition of condensing and reflux, and then cooled to room temperature to obtain aluminum sol. Add 1.34g of PVA to the prepared aluminum sol. After the PVA is fully swollen, raise the temperature of the system to about 80°C under slow mechanical stirring, stir until the PVA is completely dissolved, and cool to room temperature naturally, then slowly add 0.61mL of silica sol (SiO 2 The concentration is 1.0mol·L -1 ), and continue to stir for 1 hour to obtain a translucent spinning glue.

[0038] Step (2) is as described in Example 1, the difference is that the receiving distance is 13cm.

[0039] Step (3) is the same as in Example 1.

[0040] Gained Al 2 o 3 The diameter of the ceramic fiber is 200-500nm, Al 2 o 3 Content 97%, SiO 2 The content is...

Embodiment 3

[0042] ⑴Weigh 2.75g of pseudo-boehmite powder, measure 20mL of distilled water to stir the pseudo-boehmite powder into slurry, and add the concentration to 3.0mol L -1 6.0 mL of nitric acid solution, heated and stirred to 80-85°C under the condition of condensing and reflux, and then cooled to room temperature to obtain aluminum sol. Take 15mL of the prepared aluminum sol, add 9mL of absolute ethanol, stir well, then slowly add the concentration of 0.21mol L -1 ZrO(NO 3 ) 2 1.35mL, after continuous stirring for 2 hours, add 1.37g of PVP, stir until the PVP is completely dissolved, that is, the appearance of translucent spinning glue is obtained.

[0043] (2) Inject the spinning glue solution prepared in step (1) into a 20mL plastic syringe, using a No. 8 stainless steel blunt needle. Alumina precursor fibers were prepared by electrospinning under the conditions of a feeding rate of 2.4mL / h, a voltage of 20kV, a receiving distance of 13cm, a humidity of 30% in the spinning m...

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Abstract

The invention relates to a preparation method of an electrostatic spinning colloidal liquid for preparation of aluminum oxide ultrafine fibers, which comprises the following steps: peptizing pseudo-boehmite used as an aluminum source with nitric acid, thus obtaining aluminum-containing colloidal sol; and then, adding a spin finish aid and other additives to prepare the spinning colloidal liquid. According to the preparation method provided by the invention, the prepared spinning colloidal liquid can increase the aluminum content, ensures the smooth running of the electrostatic spinning process, has the characteristics of stable performance, favorable repetitiveness, preparation convenience, relative environment friendliness and the like, and has wide application prospects for preparation and production of ultrafine aluminum oxide fibers.

Description

technical field [0001] The invention belongs to the field of preparation of spinning glue for electrostatic spinning, and in particular relates to a preparation method of electrostatic spinning glue for preparing alumina superfine fibers. technical background [0002] Electrospinning is currently one of the most effective technologies for preparing ultrafine fibers. This technology was originally used to prepare polymer nanofibers (see: Compos. Sci. Technol. 2003, 63.2223), and then gradually developed into ceramic / metal oxide micro-nanostructured fibers, and has been increasingly valued. So far, many inorganic fibers with a diameter of tens of nanometers to hundreds of nanometers have been prepared by electrospinning technology (see: Synthetic Fibers, 2010, 39(3), 5 and Synthetic Fibers, 2012, 41(7), 8). [0003] The basic process of preparing alumina fiber by electrospinning technology includes: firstly, the spinning dope is prepared, which is generally composed of alumi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): D01F1/02C04B35/10C04B35/622
Inventor 李中军张建平申小清李壮陈风英曹国喜赵治华刘焦萍王吉超张秀全李宁李宗耀徐才华徐柳
Owner HENAN COAL CHEM IND GROUP INST
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