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Method for quickly detecting concentration of polyacrylonitrile-based free radical coagulation bath

A polyacrylonitrile-based, detection method technology, applied in measuring devices, specific gravity measurement, instruments, etc., can solve the problems of long cycle, long time-consuming titration, unable to guide process production in time, etc., and achieve the effect of saving time

Inactive Publication Date: 2011-07-27
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

The classic method for detecting the concentration of dimethyl sulfoxide uses the iodometric method. The iodometric method takes a long time to titrate, and the cycle for obtaining the results is long. It cannot guide the process production in time, and has a certain effect on the control of the long-term stability of the original silk. limitations

Method used

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  • Method for quickly detecting concentration of polyacrylonitrile-based free radical coagulation bath
  • Method for quickly detecting concentration of polyacrylonitrile-based free radical coagulation bath

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Embodiment 1, the rapid detection of dimethyl sulfoxide concentration in the coagulation bath

[0020] 1. Obtain the standard curve of the relationship between dimethyl sulfoxide concentration and density

[0021] 1.1 Prepare the standard solution of dimethyl sulfoxide: use the same raw material dimethyl sulfoxide in the production of polyacrylonitrile-based carbon fiber spinning coagulation bath to prepare standard solutions with different concentrations (dimethyl sulfoxide is a superior reagent) . Assuming that the integer of the mass concentration value of the coagulation bath to be tested is α%, then the number of prepared concentration standard solutions is at least 6, and the mass concentrations used in this experiment are α%, α±1%, α±2%, α±2%. 3% selected 7 experimental points in total, with X 0 express. See Table 1 for details.

[0022] 1.2 Test the density value of the standard solution: place the prepared standard solution in a constant temperature water b...

Embodiment 2

[0038] Embodiment 2: This embodiment 2 is a measurement comparison embodiment of rapid measurement and iodometric method measurement concentration.

[0039] 1. Prepare the standard solution of dimethyl sulfoxide: use dimethyl sulfoxide of the same raw material in the production of polyacrylonitrile-based raw silk spinning coagulation bath to prepare standard solutions of different concentrations (dimethyl sulfoxide is a superior reagent ). Assuming that the integer of the mass concentration value of the coagulation bath to be tested is α%, then the number of prepared concentration standard solutions is at least 6, and the mass concentrations used in this experiment are α%, α±1%, α±2%, α A total of 7 experimental points were selected for ±3%, see Table 4 below for details.

[0040] 2. Use the iodometric method to titrate the prepared solution. The titration method is as follows: Take about 1g of dimethyl sulfoxide standard solution in a 100mL volumetric flask, weigh it accurat...

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Abstract

The invention provides a method for quickly detecting concentration of a polyacrylonitrile-based free radical coagulation bath, comprising the following steps: firstly obtaining a standard curve equation y is equal to ax plus b on the relationship of concentration and density of dimethyl sulfoxide; validating the standard deviation and correlation of the standard curve equation; if the standard deviation is not more than 1 and simultaneously the correlation is more than 0.9950, the linear equation can be used directly; the density of the coagulation bath can be measured by a portable densimeter; the measured density is converted into concentration by the standard linear equation, thus obtaining the concentration of coagulation bath dimethyl sulfoxide. The method has the advantages of quickly detecting the coagulation bath dimethyl sulfoxide during the polyacrylonitrile-based free radical spinning process, and improving the exactness and timeliness on the concentration control of the coagulation bath during the spinning process.

Description

technical field [0001] The invention belongs to a detection method, and relates to a rapid detection method for the concentration of a coagulation bath in the spinning process of polyacrylonitrile-based carbon fibers. Background technique [0002] As a new type of material, polyacrylonitrile-based carbon fiber has high specific strength, high specific modulus, light weight, high temperature resistance, corrosion resistance, excellent electrical properties, small heat transfer and thermal expansion coefficient, With the characteristics of good chemical stability, it is widely used as a functional material in various fields such as aerospace, aviation, national defense and military industry, machinery industry, civil construction, sporting goods, medical equipment, chemical building materials, energy and transportation. (Zhang Yue, Chen Yingbin, etc., Research Progress of Polyacrylonitrile-based Carbon Fiber, Fiber Composite Materials, 2009, 1) Polyacrylonitrile-based carbon f...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N9/36
Inventor 吕春祥张颖新李新莲李永红王颖妍李燕生
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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