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Amidoximated polyacrylonitrile spinning solution and nanoscale ion exchange fiber prepared from solution

A technology of polyacrylonitrile spinning and ion exchange fiber, applied in cation exchange materials, ion exchange water/sewage treatment, rayon manufacturing, etc., can solve the problems of easy breakage, complicated process, difficult spinning, etc., and achieve excellent adsorption performance effect

Inactive Publication Date: 2016-05-11
JILIN UNIV
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  • Abstract
  • Description
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Problems solved by technology

After the study, it was found that although the above-mentioned fiber membrane has good adsorption performance, when the polyacrylonitrile electrospun fiber membrane reacts with hydroxylamine hydrochloride, the strength of the fiber membrane decreases greatly with the increase of the amount of hydroxylamine hydrochloride introduced, and the flexibility becomes very poor. It is brittle, easily broken, and cannot be used. At the same time, in mass production, there are also problems such as cumbersome process and inconvenient operation caused by the reaction of large pieces of fiber cloth; theoretically, polyacrylonitrile and hydroxylamine hydrochloride undergo amidoximation Nanofibers can also be obtained by spinning, which can not only form a flexible fiber film, but also realize the continuous operation of acrylonitrile polymerization → amidoximation → electrospinning, avoiding the inconvenience of large fiber cloth for amidoximation reaction. It is beneficial to the batch industrial production of this type of fiber. The literature (Liu Bin, Preparation and Performance Research of Amidoximated Nanomaterials [Master's Thesis], 2015) reacts polyacrylonitrile with hydroxylamine hydrochloride to prepare amidoximated polyacrylonitrile solution , and then prepared nanofibers capable of adsorbing copper ions and lead ions by electrospinning
However, the amidoximated polyacrylonitrile solution obtained by this method has a high viscosity and is difficult to spin, and as time goes on, the viscosity gradually increases, resulting in a gradual increase in fiber diameter, and the formation of insoluble crosslinks in more than ten hours. Gel, in industrial continuous production, will inevitably block nozzles, pipelines, and cause danger. How to solve the problem of viscosity increase and gel formation in amidoximated polyacrylonitrile spinning solution is the key to its industrial application

Method used

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  • Amidoximated polyacrylonitrile spinning solution and nanoscale ion exchange fiber prepared from solution
  • Amidoximated polyacrylonitrile spinning solution and nanoscale ion exchange fiber prepared from solution
  • Amidoximated polyacrylonitrile spinning solution and nanoscale ion exchange fiber prepared from solution

Examples

Experimental program
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Effect test

Embodiment 1

[0032] (1) Preparation of amidoximated polyacrylonitrile solution: adding 2.9g hydroxylamine hydrochloride and 6.9g potassium carbonate to the DMF solution of 40g polyacrylonitrile (Jilin Petrochemical Company) with a mass percent concentration of 10.0%, heating and stirring at 80°C, After reacting for 3.5 hours, stop heating and cool to room temperature, and filter to obtain an amidoximated polyacrylonitrile solution.

[0033](2) Viscosity change: Use a rotary viscometer to measure the viscosity of the amidoximated polyacrylonitrile solution obtained in step (1). During the measurement, it is found that with the rotation of the viscometer rotor, the pointer on the reading dial begins to shake significantly, and the viscosity increases in a short time. Movement in the general direction, beyond the range of the viscometer. After rotating for a few minutes, the amidoximated polyacrylonitrile solution has been cross-linked, and the formed cross-linked product adheres to the surfa...

Embodiment 2-4

[0036] Add 2.9g of hydroxylamine hydrochloride and 6.9g of potassium carbonate to a DMF solution of 40g of polyacrylonitrile with a concentration of 10.0% by mass, heat and stir at 80°C, react for 3.5h, stop heating and cool to room temperature, and filter to obtain amidoximated polypropylene Nitrile solution.

[0037] Add formic acid to the prepared amidoximated polyacrylonitrile solution as a cross-linking inhibitor, stir at room temperature for 3.5 hours to obtain amidoximated polyacrylonitrile spinning solution, measure the solution after standing at room temperature for 0h, 12h, 24h, 36h, and 72h viscosity.

[0038] Using the above-mentioned amidoximated polyacrylonitrile spinning solution as raw material, using electrospinning technology (Zhao Yiyang, high-voltage electrospinning technology to construct one-dimensional micro-nano structure materials [Ph. Under the condition of 20%, the spinning voltage is adjusted to 18KV, the receiving distance is 15cm, the advancing s...

Embodiment 5-7

[0040] Add 2.9g of hydroxylamine hydrochloride and 6.9g of potassium carbonate to a DMF solution of 40g of polyacrylonitrile with a concentration of 10.0% by mass, heat and stir at 80°C, react for 3.5h, stop heating and cool to room temperature, and filter to obtain amidoximated polypropylene Nitrile solution.

[0041] Add quantitative acetic acid to the prepared amidoximated polyacrylonitrile solution as a cross-linking inhibitor, stir at room temperature for 3-4 hours to obtain amidoximated polyacrylonitrile spinning solution, and place them at room temperature for 0h, 12h, 24h, 36h, and 72h respectively Measure the solution viscosity.

[0042] According to the method in Example 2, amidoximated polyacrylonitrile nanofibers were prepared, and their adsorption capacity for copper ions and lead ions was determined.

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Abstract

The invention provides an amidoximated polyacrylonitrile spinning solution and a nanoscale ion exchange fiber prepared from the solution, and belongs to the technical field of nanoscale ion exchange fiber preparation. A preparation method comprises the steps that hydroxylamine hydrochloride (or organic polyamine) and a catalyst are added into a polyacrylonitrile solution, reacting under stirring is performed for 2-5 h at the temperature of 60 DEG C-120 DEG C, the temperature is lowered to room temperature, and filtering is performed to obtain an amidoximated polyacrylonitrile solution; a crosslink inhibitor is added into the amidoximated polyacrylonitrile solution, the mixture is stirred to be uniform to obtain the amidoximated polyacrylonitrile spinning solution, the amidoximated polyacrylonitrile spinning solution is prepared into a nanofiber membrane by adopting an electrospinning technique, and the nanofiber membrane is subjected to aftertreatment to obtain the nanoscale ion exchange fiber which can be used for adsorbing harmful substances in water. The method is simple and effective, the spinning solution which is stable in viscosity and cannot generate gel is obtained, and the nanoscale ion exchange fiber which has the good adsorption capacity on heavy metal ions is prepared by taking the spinning solution as the raw material.

Description

technical field [0001] The invention belongs to the technical field of preparing nanoscale ion exchange fibers, in particular to an amidoximated polyacrylonitrile spinning solution with stable viscosity and no gel formation and nanoscale ion exchange fibers prepared by using the solution. Background technique [0002] Metal mines, non-ferrous smelting, iron and steel, electrolysis, electroplating, petrochemicals, batteries, leather, pesticides, paints, medicines, pigments, circuit boards, aviation equipment, etc. are key industries that have an important impact on the national economy. In the production of these industries A large amount of heavy metal-containing wastewater will inevitably be produced. Once it is discharged into rivers and other water bodies, whether it is directly drunk or eaten after being enriched in the food chain, many serious diseases will occur. It is of great significance to treat the wastewater from the source to meet the discharge standards. [000...

Claims

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Application Information

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IPC IPC(8): D01F6/54D01F1/10D04H1/43D04H1/728B01J39/20C02F1/42C02F1/62
CPCB01J39/20C02F1/42C02F1/62C02F2001/425C02F2101/20D01F1/10D01F6/54D04H1/43D04H1/728
Inventor 杨清彪闫春秋宋岩鲁冠秀任晶李耀先
Owner JILIN UNIV
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