阅读说明：本技术 一种气相沉积聚苯胺复合导电纱线的制备方法 (Preparation method of vapor deposition polyaniline composite conductive yarn ) 是由 洪剑寒 韩潇 胡铖烨 于 2019-10-15 设计创作，主要内容包括：本发明属于导电纤维领域,具体涉及一种气相沉积聚苯胺复合导电纱线的制备方法,包括如下步骤：步骤1,将纱线基材进行等离子体处理,得到前处理纱线；步骤2,将前处理纱线浸泡至反应液,待纱线吸附完成后压辊挤压得到带液纱线；步骤3,将带液纱线放入苯胺蒸汽室内吸附反应,取出后储存于容器内静置反应,形成聚苯胺导电层,得到复合导电纱线。本发明解决了废液排放多和原材料利用率低的问题,通过浸泡吸附与蒸汽吸附的方式实现表面导电层的原位聚合,大大提升了导电效率,也杜绝了废液的排放。(The invention belongs to the field of conductive fibers, and particularly relates to a preparation method of vapor deposition polyaniline composite conductive yarns, which comprises the following steps: step 1, carrying out plasma treatment on a yarn base material to obtain a pre-treated yarn; step 2, soaking the pretreated yarn into a reaction solution, and extruding by a compression roller after the yarn is adsorbed to obtain yarn with liquid; and 3, putting the yarn with the liquid into an aniline steam chamber for adsorption reaction, taking out the yarn and storing the yarn in a container for standing reaction to form a polyaniline conductive layer, thus obtaining the composite conductive yarn. The invention solves the problems of much waste liquid discharge and low utilization rate of raw materials, realizes in-situ polymerization of the surface conducting layer by soaking adsorption and steam adsorption, greatly improves the conducting efficiency, and also avoids the discharge of waste liquid.)

1. A preparation method of vapor deposition polyaniline composite conductive yarn is characterized by comprising the following steps: the method comprises the following steps:

Step 1, carrying out plasma treatment on a yarn base material to obtain a pre-treated yarn;

Step 2, soaking the pretreated yarn into a reaction solution, and extruding by a compression roller after the yarn is adsorbed to obtain yarn with liquid;

And 3, putting the yarn with the liquid into an aniline steam chamber for adsorption reaction, taking out the yarn and storing the yarn in a container for standing reaction to form a polyaniline conductive layer, thus obtaining the composite conductive yarn.

2. The method for preparing vapor-deposited polyaniline composite conductive yarn as claimed in claim 1, wherein: the parameters of the plasma treatment of the step 1 are as follows: the yarn processing length is 4m, the reaction gas is oxygen, the electrode plate interval is 4mm, and the yarn running speed is 2 m/min.

3. The method for preparing vapor-deposited polyaniline composite conductive yarn as claimed in claim 1, wherein: and 2, adopting a mixed solution of an oxidant and doping acid as the reaction solution in the step 2, wherein the concentration of the oxidant is 80-200g/L, and the concentration of the doping acid is 0.4-3.0 mol/L.

4. The method for preparing the vapor-deposited polyaniline composite conductive yarn as claimed in claim 3, wherein: the oxidant is one of ammonium persulfate, ferric trichloride and vanadium pentoxide.

5. The method for preparing the vapor-deposited polyaniline composite conductive yarn as claimed in claim 3, wherein: the doping acid is one of sulfuric acid, hydrochloric acid, phosphoric acid, perchloric acid and p-toluenesulfonic acid.

6. The method for preparing vapor-deposited polyaniline composite conductive yarn as claimed in claim 1, wherein: the liquid carrying rate of the liquid carrying yarn in the step 2 is 12-15%.

7. the method for preparing vapor-deposited polyaniline composite conductive yarn as claimed in claim 1, wherein: the concentration of the phthalic anhydride steam in the step 3 is 0-0.02 g/L.

8. The method for preparing vapor-deposited polyaniline composite conductive yarn as claimed in claim 1, wherein: the time of the adsorption reaction in the step 3 is 10-25 min.

Technical Field

The invention belongs to the field of conductive fibers, and particularly relates to a preparation method of vapor deposition polyaniline composite conductive yarns.

Background

With the development of science and technology and the pursuit of people for good life, the application of functional fiber materials with antistatic property, electromagnetic radiation resistance, electric signal transmission and the like in various fields is wider and wider, and the market space of conductive fibers which are light, soft, highly conductive and easy to weave is continuously expanded. At present, the conductive components of the commonly used conductive fibers mainly comprise inorganic materials such as metal, metal oxide, carbon black and the like. With the continuous and deep basic research and application research, the application prospect of the polymer conductive material in the conductive fiber is widely concerned.

Compared with other polymer conductive materials, Polyaniline (PANI) has the advantages of low price, simple synthesis, high conductivity and stable performance, and is considered as a polymer conductive material with the most application prospect. Conductive fibers are one of the research hotspots of PANI. The method for preparing the conductive fiber by using the PANI as the conductive component and adopting the blending spinning method is a simple and easy method, but the application prospect of the method is very poor because of the difficult solubility and the difficult meltability of the PANI and the adverse effect of the blending spinning method on the mechanical property of the fiber. The conductive fiber can also be obtained by performing surface treatment on the fiber by PANI, the conductive PANI is dissolved and then continuously coated on the surface of the yarn by adopting a padding mode, so that continuous conductive treatment is realized, but the PANI can only be dissolved in a few solvents such as concentrated sulfuric acid, N-methyl-2-pyrrolidone and the like, so that the cost is high, the preparation is difficult, and the practical significance is low.

The PANI conductive layer is formed by directly polymerizing the aniline monomer on the surface of the fiber, and the phenomenon of aniline in-situ polymerization discovered at the end of the last 80 th century provides a new idea for preparing the PANI conductive fiber. The in-situ polymerization method comprises the steps of placing the fiber in a solution of aniline monomer, doping acid and oxidant step by step, and enabling aniline to perform oxidative polymerization and doping reaction on the surface of the fiber to generate the PANI conducting layer, so that the PANI composite conducting fiber with the skin-core structure is formed. Researchers at home and abroad use a plurality of common fibers as base materials to conduct electric conduction treatment.

The conductivity of the conductive fiber prepared by the in-situ polymerization method is far higher than that of a blend spinning method, the spinnability is better than that of a metal fiber, and the physical and mechanical properties of a matrix fiber are basically not influenced, so that the preparation method of the PANI conductive fiber which is considered as the most commercial prospect since the coming of the world is provided. However, when the conductive fiber is prepared by the in-situ polymerization method, the adsorption and polymerization reaction of aniline are completed in the solution step by step, and the continuous conductive treatment of the yarn cannot be realized, so that the fiber is generally immersed in aniline for more than 2 hours and then placed in a solution doped with acid and an oxidant to generate the PANI through the oxidative polymerization reaction in order to ensure the sufficient adsorption of aniline. Therefore, the efficiency of preparing the conductive fiber by the traditional in-situ polymerization method is extremely low, and meanwhile, the problems of low raw material utilization rate, high waste liquid discharge and the like exist, so that the in-situ polymerization phenomenon is still in the laboratory stage for nearly 30 years.

Disclosure of Invention

Aiming at the problems in the prior art, the invention provides a preparation method of vapor deposition polyaniline composite conductive yarn, which solves the problems of more waste liquid discharge and low raw material utilization rate, realizes in-situ polymerization of a surface conductive layer by means of soaking adsorption and steam adsorption, greatly improves the conductive efficiency, and also avoids the discharge of waste liquid.

In order to achieve the technical purpose, the technical scheme of the invention is as follows:

A preparation method of vapor deposition polyaniline composite conductive yarn comprises the following steps:

Step 1, carrying out plasma treatment on a yarn base material to obtain a pre-treated yarn;

Step 2, soaking the pretreated yarn into a reaction solution, and extruding by a compression roller after the yarn is adsorbed to obtain yarn with liquid;

and 3, putting the yarn with the liquid into an aniline steam chamber for adsorption reaction, taking out the yarn and storing the yarn in a container for standing reaction to form a polyaniline conductive layer, thus obtaining the composite conductive yarn.

The parameters of the plasma treatment of the step 1 are as follows: the yarn processing length is 4m, the reaction gas is oxygen, the electrode plate interval is 4mm, and the yarn running speed is 2 m/min.

and 2, adopting a mixed solution of an oxidant and doping acid as the reaction solution in the step 2, wherein the concentration of the oxidant is 80-200g/L, and the concentration of the doping acid is 0.4-3.0 mol/L.

The oxidant is one of ammonium persulfate, ferric trichloride and vanadium pentoxide.

The doping acid is one of sulfuric acid, hydrochloric acid, phosphoric acid, perchloric acid and p-toluenesulfonic acid.

the liquid carrying rate of the liquid carrying yarn in the step 2 is 12-15%.

The concentration of the phthalic anhydride steam in the step 3 is 0-0.02 g/L.

The time of the adsorption reaction in the step 3 is 10-25 min.

Aiming at the problems of low-efficiency preparation of the traditional in-situ polymerization method and low utilization rate of raw materials of the existing yarn continuous preparation method based on the in-situ polymerization method, the mixed solution of oxidant and doped acid is pre-impregnated into the yarn, then the yarn is exposed in an aniline steam environment, so that aniline steam is adsorbed on the surface of the yarn and reacts with the oxidant and the doped acid to generate conductive PANI, the continuous preparation of the PANI conductive yarn is realized, and the utilization rate of the raw materials is greatly improved.

The invention has the following advantages:

1. the invention solves the problems of much waste liquid discharge and low utilization rate of raw materials, realizes in-situ polymerization of the surface conducting layer by soaking adsorption and steam adsorption, greatly improves the conducting efficiency, and also avoids the discharge of waste liquid.

2. According to the invention, aniline steam is adsorbed on the surface of the yarn and reacts with an oxidant and a doping acid to generate the conductive PANI, so that the continuous preparation of the PANI conductive yarn is realized, and meanwhile, the utilization rate of raw materials is greatly improved.

Drawings

FIG. 1 is a comparison of the surface topography before and after the conductive treatment of the polyester filament yarn of example 1 of the present invention;

Fig. 2 is a comparison of the surface morphology of the p-aramid fiber before and after the conductive treatment in example 2 of the present invention.

Detailed Description

A specific embodiment of the present invention will be described in detail with reference to fig. 1 and 2, but the present invention is not limited thereto.

A preparation method of vapor deposition polyaniline composite conductive yarn comprises the following steps:

Step 1, carrying out plasma treatment on a yarn base material to obtain a pre-treated yarn;

Step 2, soaking the pretreated yarn into a reaction solution, and extruding by a compression roller after the yarn is adsorbed to obtain yarn with liquid;

And 3, putting the yarn with the liquid into an aniline steam chamber for adsorption reaction, taking out the yarn and storing the yarn in a container for standing reaction to form a polyaniline conductive layer, thus obtaining the composite conductive yarn.

The parameters of the plasma treatment of the step 1 are as follows: the yarn processing length is 4m, the reaction gas is oxygen, the electrode plate interval is 4mm, and the yarn running speed is 2 m/min.

And 2, adopting a mixed solution of an oxidant and doping acid as the reaction solution in the step 2, wherein the concentration of the oxidant is 80-200g/L, and the concentration of the doping acid is 0.4-3.0 mol/L.

The oxidant is one of ammonium persulfate, ferric trichloride and vanadium pentoxide.

the doping acid is one of sulfuric acid, hydrochloric acid, phosphoric acid, perchloric acid and p-toluenesulfonic acid.

the liquid carrying rate of the liquid carrying yarn in the step 2 is 12-15%.

The concentration of the phthalic anhydride steam in the step 3 is 0-0.02 g/L.

The time of the adsorption reaction in the step 3 is 10-25 min.