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Method for detecting azoisobutyronitrile residue in acrylonitrile polymerization solution

A technology of azobisisobutyronitrile and detection method, which is applied in the field of detection of azobisisobutyronitrile residue in acrylonitrile polymerization liquid

Inactive Publication Date: 2010-12-15
CHINA NAT BLUESTAR GRP CO LTD
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  • Application Information

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Yet existing patent and document also do not have the report about AIBN residual detection method in acrylonitrile polymerization liquid

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  • Method for detecting azoisobutyronitrile residue in acrylonitrile polymerization solution
  • Method for detecting azoisobutyronitrile residue in acrylonitrile polymerization solution
  • Method for detecting azoisobutyronitrile residue in acrylonitrile polymerization solution

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Embodiment 1

[0018] A series of AIBN standard solutions with concentrations of 2ppm, 10ppm, 50ppm, 100ppm and 200ppm were prepared, and the solvent was dimethyl sulfoxide (DMSO). These standard solutions were tested with a Waters ACQUITY UPLCTM high performance liquid chromatograph. Column (BEH C 18 1.7μm, 2.1×50mm), the column temperature is 30°C, the volume ratio of the mobile phase acetonitrile and water is 1:1 mixed solution, the flow rate of the mobile phase is 0.5mL / min, the detector is an ultraviolet detector, and the detection wavelength is 346 nm, the sample injection volume was 10 μL. After above-mentioned solution is analyzed by high performance liquid chromatography, obtain as follows: figure 1 The HPLC spectrum shown. According to the relationship between AIBN peak integral area and concentration, draw a standard curve, such as figure 2 shown.

Embodiment 2

[0020] Take 1g of acrylonitrile polymer solution, add 3g of DMSO to dilute, precipitate in dichloromethane, filter, and concentrate the filtrate to 4g at room temperature to obtain an AIBN solution without polyacrylonitrile. Use HPLC to test the AIBN solution. The reaction procedure of HPLC With embodiment 1. The integral area that obtains AIBN peak is 589 ( image 3 ),Depend on figure 1 The concentration of AIBN was found to be 6.5ppm. Therefore, the residual amount of AIBN in this acrylonitrile polymerization solution is 6.5×4=26 ppm.

Embodiment 3

[0022] Take 1g of acrylonitrile polymer solution, add 3g of DMSO to dilute, precipitate in ethanol, filter, and concentrate the filtrate to 4g at room temperature to obtain an AIBN solution without polyacrylonitrile, test the AIBN solution by HPLC, and the reaction procedure of HPLC is the same as in the example 1, the integrated area of ​​AIBN peak is 573, by figure 1 The concentration of AIBN was found to be 6.3ppm. Therefore, the residual amount of AIBN in this acrylonitrile polymerization solution is 6.3×4=25.2 ppm.

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Abstract

The invention relates to a method for detecting azoisobutyronitrile (AIBN) residue in acrylonitrile polymerization solution. The method is characterized by being implemented through a high performance liquid chromatograph (HPLC) and comprising the following steps of: 1, preparing AIBN series of standard solution with different concentrations, testing the AIBN standard solution by using the HPLC, and establishing a standard curve between an AIBN peak area and the concentration thereof; and 2, precipitating the acrylonitrile polymerization solution in a precipitator, filtering to remove polyacrylonitrile, concentrating the filter liquor to obtain AIBN solution which does not contain the polyacrylonitrile, using the AIBN solution which does not contain the polyacrylonitrile for HPLC test, measuring the integral area of the AIBN peak, and substituting the integral area into the standard curve so as to calculate the residue of the AIBN. The method for detecting the azoisobutyronitrile (AIBN) residue in the acrylonitrile polymerization solution has the advantages of accuracy, sensitivity, high efficiency and simple operation.

Description

technical field [0001] The invention relates to a detection method for azobisisobutyronitrile residues in an acrylonitrile polymerization liquid, more particularly to a detection method for azobisisobutyronitrile in an acrylonitrile polymerization liquid used for preparing carbon fiber precursors. Background technique [0002] Polyacrylonitrile-based carbon fiber has excellent properties such as high specific strength, high specific modulus, high temperature resistance, corrosion resistance, fatigue resistance, creep resistance, and good electrical conductivity and thermal conductivity. It is used in aerospace, mechanical electronics, chemical building materials and Advanced sporting goods and other aspects have an irreplaceable role. The polymerization process is a prerequisite for the preparation of carbon fibers with excellent performance, and each polymerization parameter must be strictly controlled. There are many polymerization methods of acrylonitrile, mainly includi...

Claims

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Application Information

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IPC IPC(8): G01N30/02
Inventor 鲁代仁张雪芹卢培栋朱栋栋李瑞亢胡衍平
Owner CHINA NAT BLUESTAR GRP CO LTD
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