阅读说明：本技术 一种琼胶纳米纤维的制备方法 (Preparation method of agar nanofiber ) 是由 张兴光 王威 徐正东 景晓辉 于 2020-04-01 设计创作，主要内容包括：本发明提供了一种琼胶纳米纤维的制备方法,采用喷射纺丝法制备得到纤维,采用喷射纺丝法所得纤维直径较小,纤维形貌良好,表面平滑且不会产生空洞,纤维力学性能能够满足应用需求。(The invention provides a preparation method of agar nanofiber, which is characterized in that the fiber is prepared by adopting a jet spinning method, the diameter of the fiber obtained by adopting the jet spinning method is small, the appearance of the fiber is good, the surface is smooth, no cavity is generated, and the mechanical property of the fiber can meet the application requirement.)

1. A preparation method of agar nanofibers is characterized by comprising the following steps:

(1) adding agar into DMSO, stirring at 50-90 ℃ to obtain an agar solution with the concentration of 25-30 wt%, and then filtering and defoaming to obtain an agar spinning solution;

(2) feeding the spinning solution obtained in the step (1) into a spinning box body through a metering pump at the speed of 8-12mL/h by using an injection pump, forming a trickle when the spinning solution is extruded from a spinning nozzle, simultaneously introducing compressed gas into the spinning box body, wherein the pressure of the compressed gas is 0.30MPa, enabling the obtained spinning trickle to enter the spinning box body, volatilizing the solvent to form fibers under the combined action of high-pressure gas flow and the spinning box body, and collecting the fibers on a receiving plate by using the air suction action generated by a fan to obtain agar nanofibers;

(3) and (3) repeatedly washing the nano-fibers obtained in the step (2) with ethanol/water solution for three times, and then drying in an oven to obtain the finished product.

2. The method for preparing agar nano-fiber according to claim 1, wherein the temperature of the spinning manifold is 50-80 ℃, the mass concentration of ethanol/water solution is 60 wt%, the drying temperature is 60-80 ℃, and the drying time is 0.5-4 h.

Technical Field

The invention belongs to the field of nanofibers, and particularly relates to a preparation method of agar nanofibers.

Background

Agar is the main economic component of marine red algae, is used as a seaweed gel product with a wide application range, is widely applied to a plurality of fields of food, medicine, health care, cosmetics, printing and dyeing and the like, and has wide application and market prospect. The red algae species which can be applied to the agar processing comprise more than thirty species such as gelidium amansii, asparagus, gracilaria crispatus, gracilaria taro and the like, and the species which can realize the industrialized cultivation up to now comprise the asparagus, the gracilaria crispatus and the gracilaria taro.

The jet spinning technology is a novel nano fiber preparation technology capable of obtaining spun fibers with small diameters, takes polymer solution as an object, takes high-speed airflow as a driving force, forms polymer jet flow under the action of the high-speed airflow after the spinning solution is extruded through a spinneret orifice, and further drafts and refines the jet flow in a receiving device.

In the prior art, a wet spinning process is usually adopted to prepare agar fibers, wherein in the wet spinning process, after a high polymer is prepared into a spinning solution, the spinning solution is directly sprayed into a coagulating bath through a spinning nozzle to be coagulated into filaments, cavities are often generated during coagulation, so that the mechanical strength of the fibers is low, and the mechanical properties of the agar fibers prepared by the wet spinning method cannot meet the requirements.

Disclosure of Invention

The technical problem to be solved by the invention is to provide a method for preparing agar nanofibers, wherein the fibers are prepared by a jet spinning method, the fibers obtained by the jet spinning method have small diameter, good appearance, smooth surface and no cavity, and the mechanical properties of the fibers can meet the application requirements.

The preparation method of the agar nanofiber provided by the invention comprises the following steps:

(1) adding agar into DMSO, stirring at 50-90 ℃ to obtain an agar solution with the concentration of 25-30 wt%, and then filtering and defoaming to obtain an agar spinning solution;

(2) feeding the spinning solution obtained in the step (1) into a spinning box body through a metering pump at the speed of 8-12mL/h by using an injection pump, forming a trickle when the spinning solution is extruded from a spinning nozzle, simultaneously introducing compressed gas into the spinning box body, wherein the pressure of the compressed gas is 0.30MPa, enabling the obtained spinning trickle to enter the spinning box body, volatilizing the solvent to form fibers under the combined action of high-pressure gas flow and the spinning box body, and collecting the fibers on a receiving plate by using the air suction action generated by a fan to obtain agar nanofibers;

(3) and (3) repeatedly washing the nano-fibers obtained in the step (2) with ethanol/water solution for three times, and then drying in an oven to obtain the finished product.

The temperature of the spinning manifold is 50-80 ℃, the mass concentration of the ethanol/water solution is 60 wt%, the drying temperature is 60-80 ℃, and the drying time is 0.5-4 h.

The diameter of the obtained nano fiber is 800-1000nm, and the dry fracture strength of the agar fiber reaches 3.0-5.0 CN/dtex.

The invention has the beneficial effects that:

the agar nanofiber prepared by the jet spinning method has the advantages of small diameter, good fiber appearance, smooth surface, no cavity and greatly improved mechanical property.

Detailed Description

The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.

Example 1:

(1) adding agar into DMSO, stirring at 80 ℃ to obtain an agar solution with the concentration of 25 wt%, and then filtering and defoaming to obtain an agar spinning solution;

(2) feeding the spinning solution obtained in the step (1) into a spinning box body through a metering pump at the speed of 8mL/h by using an injection pump, forming a trickle when the spinning solution is extruded from a spinning nozzle, introducing compressed gas into the spinning box body at the same time, wherein the pressure of the compressed gas is 0.30MPa, enabling the obtained spinning trickle to enter the spinning box body, volatilizing the solvent to form fibers under the combined action of high-pressure air flow and the spinning box body, and collecting the fibers on a receiving plate by using the air suction action generated by a fan to obtain the agar nanofiber;

(3) and (3) repeatedly washing the nano-fibers obtained in the step (2) with ethanol/water solution for three times, and then drying in an oven to obtain the finished product.

The temperature of the spinning manifold is 50-80 ℃, the mass concentration of the ethanol/water solution is 60 wt%, the drying temperature is 60-80 ℃, and the drying time is 0.5-4 h.

The diameter of the obtained nano fiber is 800nm, and the dry fracture strength of the agar fiber reaches 3.6 CN/dtex.

Example 2:

(1) adding agar into DMSO, stirring at 80 ℃ to obtain an agar solution with the concentration of 30 wt%, and then filtering and defoaming to obtain an agar spinning solution;

(2) feeding the spinning solution obtained in the step (1) into a spinning box body through a metering pump at the speed of 8mL/h by using an injection pump, forming a trickle when the spinning solution is extruded from a spinning nozzle, introducing compressed gas into the spinning box body at the same time, wherein the pressure of the compressed gas is 0.30MPa, enabling the obtained spinning trickle to enter the spinning box body, volatilizing the solvent to form fibers under the combined action of high-pressure air flow and the spinning box body, and collecting the fibers on a receiving plate by using the air suction action generated by a fan to obtain the agar nanofiber;

(3) and (3) repeatedly washing the nano-fibers obtained in the step (2) with ethanol/water solution for three times, and then drying in an oven to obtain the finished product.

The temperature of the spinning manifold is 50-80 ℃, the mass concentration of the ethanol/water solution is 60 wt%, the drying temperature is 60-80 ℃, and the drying time is 0.5-4 h.

The diameter of the obtained nano fiber is 900nm, and the dry fracture strength of the agar fiber reaches 4.7 CN/dtex.

The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes, which are made by the present specification, or directly or indirectly applied to other related technical fields, are included in the scope of the present invention.