阅读说明：本技术 一种琼胶纤维的制备方法 (Preparation method of agar fibers ) 是由 张兴光 王威 徐正东 景晓辉 鄢军 于 2020-04-01 设计创作，主要内容包括：本发明提供了一种琼胶纤维的制备方法,采用喷射纺丝法制备得到纤维,所述凝固浴中由底部搅拌装置产生液体漩涡,所述喷射细流由漩涡中心进入凝固浴,如此以避免单纯湿法纺丝过程中于纤维表面产生的空洞结构,所述凝固浴中加入乙二醛交联剂,使得琼脂纤维发生充分交联,纤维强度得到有效提升。(The invention provides a preparation method of agar fibers, which is characterized in that fibers are prepared by adopting a jet spinning method, a liquid vortex is generated in a coagulation bath by a bottom stirring device, a jet trickle enters the coagulation bath from the center of the vortex, so that a cavity structure generated on the surfaces of the fibers in a pure wet spinning process is avoided, and a glyoxal crosslinking agent is added into the coagulation bath, so that the agar fibers are fully crosslinked, and the fiber strength is effectively improved.)

1. The preparation method of the agar fiber is characterized by comprising the following steps:

(1) adding agar into DMF, stirring at 50-90 deg.C to obtain 25-30 wt% agar solution, filtering, and defoaming to obtain 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 0.10MPa, enabling the obtained spinning trickle to enter the spinning box body, enabling the spinning trickle to pass through a section of air section, then enabling the spinning trickle to enter a coagulating bath at the bottom of the spinning box body for coagulation forming, and leading out and collecting the formed fibers through a fiber turning guide roller and a finished product guide roller in a fiber coagulating bath;

(3) and (3) repeatedly washing the 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 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.

3. The method for preparing agar fiber according to claim 1, wherein the length of the air section is 5-7 cm.

4. The method for preparing agar fiber according to claim 1, wherein the coagulating bath is a calcium chloride water solution with the mass concentration of 20%, glyoxal is added as a cross-linking agent, and the mass concentration of glyoxal is 6-8%; the temperature of the coagulating bath is 20-30 ℃.

Technical Field

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

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 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 fibers, wherein the fibers are prepared by adopting a jet spinning method, a liquid vortex is generated in a coagulation bath by a bottom stirring device, and jet trickle enters the coagulation bath from the center of the vortex, so that a cavity structure generated on the surface of the fibers in a pure wet spinning process is avoided, and a glyoxal crosslinking agent is added into the coagulation bath, so that the agar fibers are fully crosslinked, and the fiber strength is effectively improved.

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

(1) adding agar into DMF, stirring at 50-90 deg.C to obtain 25-30 wt% agar solution, filtering, and defoaming to obtain 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 0.10MPa, the obtained spinning trickle enters the spinning box body, a coagulation bath is arranged at the lower part of the box body, a liquid vortex is generated in the coagulation bath by a bottom stirring device, the sprayed trickle enters the coagulation bath from the center of the vortex, and the obtained formed fiber is guided out and collected through a fiber steering guide roller and a finished product guide roller in the fiber coagulation bath;

(3) and (3) repeatedly washing the 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 coagulating bath is a calcium chloride water solution with the mass concentration of 20%, glyoxal is added as a cross-linking agent, and the mass concentration of the glyoxal is 6-8%; the temperature of the coagulating bath is 20-30 ℃.

The dry breaking strength of the obtained agar fiber reaches 7.0-9.0 CN/dtex.

The invention has the beneficial effects that:

(1) according to the invention, the agar fiber is prepared by adopting a jet spinning method, the fiber is prepared by adopting the jet spinning method, a liquid vortex is generated in the coagulation bath by a bottom stirring device, and the jet trickle enters the coagulation bath from the center of the vortex, so that a cavity structure generated on the surface of the fiber in the pure wet spinning process is avoided.

(2) And a glyoxal crosslinking agent is added into the coagulating bath, so that the agar fibers are fully crosslinked, and the fiber strength is effectively improved.

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:

the preparation method of the agar fiber comprises the following steps

(1) Adding agar into DMF, 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 11mL/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 0.10MPa, enabling the obtained spinning trickle to enter the spinning box body, configuring a coagulation bath at the lower part of the box body, generating a liquid vortex in the coagulation bath by using a bottom stirring device, enabling the sprayed trickle to enter the coagulation bath from the center of the vortex, and leading out and collecting the obtained formed fiber through a fiber turning guide roller and a finished product guide roller in the fiber coagulation bath;

(3) and (3) repeatedly washing the 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 coagulating bath is a calcium chloride aqueous solution with the mass concentration of 20%, glyoxal is added as a cross-linking agent, and the mass concentration of the glyoxal is 8%; the temperature of the coagulating bath is 20-30 ℃.

The dry breaking strength of the obtained agar fiber reaches 8.7 CN/dtex.

Example 2:

example 1:

the preparation method of the agar fiber comprises the following steps

(1) Adding agar into DMF, 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 11mL/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 0.10MPa, enabling the obtained spinning trickle to enter the spinning box body, configuring a coagulation bath at the lower part of the box body, generating a liquid vortex in the coagulation bath by using a bottom stirring device, enabling the sprayed trickle to enter the coagulation bath from the center of the vortex, and leading out and collecting the obtained formed fiber through a fiber turning guide roller and a finished product guide roller in the fiber coagulation bath;

(3) and (3) repeatedly washing the 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 coagulating bath is a calcium chloride aqueous solution with the mass concentration of 20%, glyoxal is added as a cross-linking agent, and the mass concentration of the glyoxal is 8%; the temperature of the coagulating bath is 20-30 ℃.

The dry breaking strength of the obtained agar fiber reaches 7.2 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.