WO2016058111A1

WO2016058111A1 - Preparation method for porous nanofibres

Info

Publication number: WO2016058111A1
Application number: PCT/CN2014/000903
Authority: WO
Inventors: 袁振其
Original assignee: 太仓苏纶纺织化纤有限公司
Priority date: 2014-10-13
Filing date: 2014-10-13
Publication date: 2016-04-21

Abstract

A preparation method for porous nanofibres, the method comprising: dissolving spinning material in a solvent, adding polyvinylpyrrolidone, stirring evenly, and preparing a nanofibre polymer solution; adding SiO₂ nanoparticles to the nanofibre polymer solution, and magnetically stirring until even, the resulting solution acting as a spinning solution; pouring the spinning solution into a jetting device, spinning under the effect of an additional electric field, obtaining SiO₂ nanoparticle-containing nanofibres by controlling the spinning time and moving a receiving screen, and baking; soaking an SiO₂ nanoparticle-containing nanofibre solution with an HF solution and stirring slowly, washing and drying, and obtaining a porous nanofibre fabric. The present invention uses particle doping and removal means, achieves a hole-producing effect on the nanofibres, and is thereby used for the purposes of increasing the comparative area of the fabric, and improving dyeing properties.

Description

Method for preparing porous nanofiber

Technical field

The invention relates to a preparation method of porous nanofibers, in particular to a preparation method of porous nanofibers capable of improving dyeability.

Background technique

At present, with the improvement of people's living standards and the constant renewal of consumer concepts, consumers are increasingly demanding the quality, variety and color of fiber textiles, especially nanofiber textiles. The commonly used polyester is a kind of synthetic fiber. Because the molecular structure of polyester is relatively regular, its hydrophilicity and dyeability are poor. Traditional chemical modification consumes a lot of water and chemicals, which is not only complicated to operate but also pollutes the environment.

At the same time, the preparation of inorganic nanofibers by electrospinning combined with high-temperature calcination technology is a widely used method in recent years. The method is simple to operate, and the prepared inorganic fiber structure can realize morphology and structure through solution properties, spinning parameters and post-treatment. Controllable, showing excellent properties in the field of textile materials.

In summary, there is an urgent need for a method for preparing porous nanofibers capable of improving dyeability, which can improve the specific surface area of the fabric, controllability of the structure, enhance the surface roughness, and achieve the hole making of the nano material, thereby improving Its dyeability.

Summary of the invention

Hydrofluoric acid (HF) is a weak acid that can be specifically reacted with silica (SiO ₂ ) with a chemical reaction equation of SiO ₂ +6HF=H ₂ SIF ₆ +2H ₂ O. The SiO ₂ sacrificial layer is etched by HF. Due to the different reaction of nanofibers and SiO ₂ to HF, the effect of removing the nanofibers can be achieved by using the method of particle doping in the removal, thereby providing a comparative area of the fabric and improving the dyeability. purpose.

In order to achieve the above object, the technical solution provided by the present invention is:

A method for preparing porous nanofibers, comprising:

1) dissolving the spinning material in a solvent, adding polyvinylpyrrolidone, and stirring uniformly to prepare a nanofiber polymer solution;

2) adding SiO ₂ nanoparticles to the nanofiber polymer solution, magnetically stirring until uniform, as a spinning solution;

3) pouring the spinning solution into the ejector, spinning under the action of an additional electric field, obtaining nanofibers containing SiO ₂ nanoparticles by controlling the spinning time and moving the receiving screen, and baking;

4) The nanofibers containing SiO ₂ nanoparticles are soaked in an HF solution and slowly stirred, washed and dried to obtain a porous nanofiber fabric.

Further, the nanomaterial is one or a mixture of materials of polyester, polyacrylonitrile and its copolymer, cellulose and lignin, and the solution is N,N-dimethyldiamide.

Further, in the step 1), the mass ratio of the textile material to the solvent is 1:9 to 1:5, and the mass fraction of the polyvinylpyrrolidone is 10%; in the step 2), the SiO ₂ nanoparticles are added to the nanometer. 5-13% of the fiber polymer solution; in step 3), the additional electric field strength is 0.2kv/cm-2kv/cm, the receiving screen is 10-45cm from the spinneret, and the baking temperature is 400-650°C; In step 4), the HF solution has a mass fraction of 25-55%, and the soaking and slow agitation time is 8-16 h.

Further, in step 1), the mass ratio of the textile material to the solvent is 1:7; in step 2), the SiO ₂ nanoparticle is added as 8% of the nanofiber polymer solution; in step 3), The additional electric field strength is 1 kv/cm, the receiving screen is 35 cm from the spinning port, and the baking temperature is 550 ° C; in the step 4), the mass fraction of the HF solution is 45%, and the time of the soaking and slow stirring is 10h.

Further, the nanofibers have a diameter of 300 to 400 nm.

With the above technical solutions, the beneficial effects of the present invention are as follows:

1. In the present invention, HF is used to etch the sacrificial layer of SiO2. Since the reaction of nanofibers and SiO ₂ to HF is different, the effect of the nanofibers can be achieved by using the method of particle doping in the removal, mesoporous and microporous structure. coexist.

2. By the preparation method of the invention, the specific surface area of the fabric can be effectively improved, the dye can be better dispersed therein, the dye uptake rate of the dye can be increased, and the dyeing of the color flower and the color stripe can be avoided. The increase of fabric pores allows the dye to diffuse to the internal volume and the amount of fixation increases. Therefore, the dyeing rate and color of the fabric are improved, and the pilling phenomenon of the fabric is improved. And the manufacturing process is simple, the environment is protected, the cost is low, and it is suitable for large-scale industrial production.

detailed description

Example 1

The spinning material is dissolved in a solvent, 10% polyvinylpyrrolidone is added, and the mixture is uniformly stirred to prepare a nanofiber spinning solution; the mass ratio of the textile material to the solvent is 1:9, and the nano material is polyester, polyacrylonitrile and One or a mixture of materials of copolymer and lignin, the solution being N,N-dimethyldiamide.

5% of the SiO ₂ nanoparticles were added to the nanofiber polymer solution, and magnetically stirred until homogeneous as a spin solution.

The spinning solution is added to an electrospinning machine for electrospinning, the additional electric field strength is 0.2 kV/cm, the screen is 10 cm from the spinneret, and the baking temperature is 400 ° C to obtain fibers containing SiO ₂ nanoparticles. .

The nanofibers containing SiO ₂ nanoparticles were soaked in a 25% HF solution and slowly stirred for 8 hours, and washed and dried to obtain a porous nanofiber fabric.

The surface roughness of the fabric is increased, the dyeing rate is increased, and the color fastness of the finished product is shown in Table 1.

Example 2

The spinning material is dissolved in a solvent, 10% polyvinylpyrrolidone is added, and the mixture is uniformly stirred to prepare a nanofiber spinning solution; the mass ratio of the textile material to the solvent is 1:5, and the nano material is polyester, polyacrylonitrile and One or a mixture of materials of copolymer and lignin, the solution being N,N-dimethyldiamide.

13% of the SiO ₂ nanoparticles were added to the nanofiber polymer solution, and magnetically stirred until homogeneous as a spin solution.

The spinning solution was added to an electrospinning machine for electrospinning, an additional electric field strength of 2 kV/cm, a screen distance of 45 cm from the spinneret, and a baking temperature of 650 ° C to obtain fibers containing SiO ₂ nanoparticles.

The nanofibers containing SiO ₂ nanoparticles were soaked in a 55% HF solution and slowly stirred for 16 hours, and washed and dried to obtain a porous nanofiber fabric.

Example 3

The spinning material is dissolved in a solvent, 10% polyvinylpyrrolidone is added, and the mixture is uniformly stirred to prepare a nanofiber spinning solution; the mass ratio of the textile material to the solvent is 1:7, and the nano material is polyester, polyacrylonitrile and One or a mixture of materials of copolymer and lignin, the solution being N,N-dimethyldiamide.

8% of SiO ₂ nanoparticles were added to the nanofiber polymer solution and magnetically stirred until homogeneous as a spin solution.

The spinning solution was added to an electrospinning machine for electrospinning, an additional electric field strength of 1 kV/cm, a screen distance of 35 cm from the spinneret, and a baking temperature of 550 ° C to obtain fibers containing SiO ₂ nanoparticles.

The nanofibers containing SiO ₂ nanoparticles were soaked in a 45% HF solution and slowly stirred for 10 hours, and washed and dried to obtain a porous nanofiber fabric.

Table 1 shows the color fastness of the finished products in Examples 1, 2, and 3:

The above-mentioned embodiments are merely illustrative of the embodiments of the present invention, and the description thereof is not to be construed as limiting the scope of the invention. It should be noted that a number of variations and modifications may be made by those skilled in the art without departing from the spirit and scope of the invention.

Claims

A method for preparing porous nanofibers, comprising:

1) dissolving the spinning material in a solvent, adding polyvinylpyrrolidone, and stirring uniformly to prepare a nanofiber polymer solution;

2) adding SiO 2 nanoparticles to the nanofiber polymer solution, magnetically stirring until uniform, as a spinning solution;

3) pouring the spinning solution into the ejector, spinning under the action of an additional electric field, obtaining nanofibers containing SiO 2 nanoparticles by controlling the spinning time and moving the receiving screen, and baking;

4) The nanofibers containing SiO 2 nanoparticles are soaked in an HF solution and slowly stirred, washed and dried to obtain a porous nanofiber fabric.
The method for preparing a porous nanofiber according to claim 1, wherein the nano material is one or a mixture of materials of polyester, polyacrylonitrile and a copolymer thereof and lignin, and the solution is N,N-dimethyldiamide.
The method for preparing a porous nanofiber according to claim 1, wherein in the step 1), the mass ratio of the textile material to the solvent is 1:9 to 1:5, and the mass fraction of the polyvinylpyrrolidone is 10%; In step 2), the SiO 2 nanoparticles are added to be 5-13% of the nanofiber polymer solution; in step 3), the additional electric field strength is 0.2 kv/cm-2 kv/cm, and the screen distance is accepted. The spinneret is 10-45 cm, the baking temperature is 400-650 ° C; in step 4), the HF solution mass fraction is 25-55%, and the soaking and slow stirring time is 8-16 h.
The method for preparing a porous nanofiber according to claim 3, wherein in the step 1), the mass ratio of the textile material to the solvent is 1:7; in the step 2), the SiO 2 nanoparticle is added as 8% of the nanofiber polymer solution; in step 3), the additional electric field strength is 1 kv/cm, the screen is 35 cm from the spinneret, and the baking temperature is 550 ° C; in step 4), the HF solution The mass fraction was 45% and the soaking and slow agitation time was 10 h.
The method for producing a porous nanofiber according to any one of claims 1 to 5, wherein the nanofiber has a diameter of 300 to 400 nm.