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A detection method for ammonia ion replacement rate of polyacrylonitrile spinning solution

A technology of polyacrylonitrile spinning and ion replacement, which is applied in the direction of chemical analysis by titration method, can solve problems such as difficulty in controlling the degree of ammoniation, and achieve the effect of accurate control of dosage and residence time.

Active Publication Date: 2021-11-02
ZHONGFU SHENYING CARBON FIBER
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, it is difficult to control the degree of ammoniation in the actual production process. At present, there is only a detection method for dissolved ammonia in the polymerization liquid, and there is no report on the detection of the replacement rate of ammonium itaconate ion in the polymer.

Method used

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  • A detection method for ammonia ion replacement rate of polyacrylonitrile spinning solution
  • A detection method for ammonia ion replacement rate of polyacrylonitrile spinning solution

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Step 1. Take the spinning solution to be tested in a weighing bottle, weigh 1-2g of the spinning solution on a multi-position balance by the subtraction method, and put it on one end of the glass rod, accurate to 0.0001g, and record it as m=1.1258g.

[0043] Step 2. The end of the glass rod stained with the sample takes the center of the glass plate as the center, and rotates slowly against the glass plate to evenly spread it into a thin layer;

[0044] Step 3. Measure the hydrochloric acid standard solution of quantitative V = 25ml to rinse the samples on the glass plate and glass rod, completely collect the rinse water in the iodine bottle, and be careful not to leak out. The sample contacts the rinse water to solidify into a film, and use tweezers Gently remove the film into the iodine bottle, wash the surface of the glass plate with the remaining hydrochloric acid solution, and completely collect the cleaning water into the iodine bottle of rinsing water. Cover the ...

Embodiment 2

[0053] Step 1. Take the spinning solution to be tested in a weighing bottle, weigh 1-2 g of the spinning solution on a multi-position balance by the subtraction method, and put it on one end of the glass rod, accurate to 0.0001 g, and record it as m=1.5116 g.

[0054] Step 2. The end of the glass rod stained with the sample takes the center of the glass plate as the center, and rotates slowly against the glass plate to evenly spread it into a thin layer;

[0055] Step 3. Measure the hydrochloric acid standard solution of quantitative V = 25ml to rinse the samples on the glass plate and glass rod, completely collect the rinse water in the iodine bottle, and be careful not to leak out. The sample contacts the rinse water to solidify into a film, and use tweezers Gently remove the film into the iodine bottle, wash the surface of the glass plate with the remaining hydrochloric acid solution, and completely collect the cleaning water into the iodine bottle of rinsing water. Cover t...

Embodiment 3

[0064] Step 1. Take the spinning solution to be tested in a weighing bottle, weigh 1-2 g of the spinning solution on a multi-position balance by the subtraction method, and place it on one end of the glass rod, accurate to 0.0001 g, and record it as m=1.8718 g.

[0065] Step 2. The end of the glass rod stained with the sample takes the center of the glass plate as the center, and rotates slowly against the glass plate to evenly spread it into a thin layer;

[0066] Step 3. Measure the hydrochloric acid standard solution of quantitative V = 25ml to rinse the samples on the glass plate and glass rod, completely collect the rinse water in the iodine bottle, and be careful not to leak out. The sample contacts the rinse water to solidify into a film, and use tweezers Gently remove the film into the iodine bottle, wash the surface of the glass plate with the remaining hydrochloric acid solution, and completely collect the cleaning water into the iodine bottle of rinsing water. Cover...

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Abstract

The invention belongs to the field of organic matter detection, in particular to a detection method for ammonia ion replacement rate of polyacrylonitrile spinning solution. According to the method, a quantitative spinning solution is weighed to the center of the dry glass surface, smeared with a glass rod to form a film, rinsed and soaked with a quantitative hydrochloric acid solution and water respectively, and the rinse water is titrated with a sodium hydroxide standard solution , to calculate the ammonia ion replacement rate in the spinning solution. The method provided by the invention realizes accurate control of the amount and the residence time of the polymerization solution in the amination modification through the titration of the standard solution.

Description

technical field [0001] The invention belongs to the field of organic matter detection, in particular to a method for detecting the ammonia ion replacement rate of polyacrylonitrile spinning liquid. Background technique [0002] Due to its excellent mechanical properties, polyacrylonitrile carbon fiber has been widely used in many fields as a high-performance reinforcing material. It is an important strategic basic material and a typical new military-civilian dual-use material. At present, the preparation and control technology of high-quality raw silk has become one of the main reasons restricting the performance improvement of carbon fiber. [0003] Polyacrylonitrile carbon fiber is obtained by preparing polyacrylonitrile and comonomer through a series of processes such as free radical reaction polymerization, spinning and carbonization. Among them, itaconic acid, as the most common comonomer at present, has a higher increase in polyacrylonitrile Cyclization reaction effic...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N31/16
CPCG01N31/16
Inventor 丁正南连峰李果王芬张克勤
Owner ZHONGFU SHENYING CARBON FIBER
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