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Detection method of free chlorine ions in polyisobutylene

A technology of polyisobutylene and detection method, which is applied in the chemical industry to achieve the effects of simple operation, low cost and high detection accuracy

Active Publication Date: 2012-07-11
SHANDONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Separation and extraction of free chloride ions in polyisobutylene by dissolution and precipitation method, detection by ion chromatography technology conductivity detector, determination of chloride ion content by calculating the peak area of ​​the chloride ion chromatogram, this method has not been reported

Method used

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  • Detection method of free chlorine ions in polyisobutylene
  • Detection method of free chlorine ions in polyisobutylene
  • Detection method of free chlorine ions in polyisobutylene

Examples

Experimental program
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Effect test

Embodiment 1

[0032] (1) Dissolution of polyisobutylene: Weigh 0.328 g of polyisobutylene (sample 1, weight average molecular weight M w = 100,000) was dissolved in 50 mL of tetrahydrofuran to make a homogeneous solution;

[0033] (2) Extraction of chloride ions in polyisobutylene: under stirring conditions, the homogeneous solution prepared in step (1) was slowly added dropwise to 100 mL of ultrapure water, and after the polyisobutylene was precipitated from the water, the solution was subjected to high-speed Centrifugal separation, time 15min, rotating speed 4500rpm; pour out the supernatant liquid; wash the precipitated polyisobutene with 10mL ultrapure water twice, combine the supernatant liquid and washing solution; evaporate the tetrahydrofuran and water in the extraction solution; add 10mL ultrapure water; Wash with pure water to extract chloride ions, shake repeatedly, so that the chloride ions on the inner wall of the container are completely dissolved in the aqueous solution to ob...

Embodiment 2

[0040] (1) Dissolution of polyisobutylene: Weigh 0.791 g of polyisobutylene (sample 2, weight average molecular weight M w = 67,000) was dissolved in 50 mL of tetrahydrofuran to make a homogeneous solution;

[0041] (2) Extraction of chloride ions in polyisobutylene: under stirring conditions, the homogeneous solution prepared in step (1) was slowly added dropwise to 100 mL of ultrapure water, and after the polyisobutylene was precipitated from the water, the solution was subjected to high-speed Centrifugal separation, time 20min, rotating speed 4600rpm; pour out the supernatant liquid; wash the precipitated polyisobutene with 10mL ultrapure water twice, combine the supernatant liquid and washing solution; evaporate the tetrahydrofuran and water in the extraction solution; add 10mL ultrapure water; Wash with pure water to extract chloride ions, shake repeatedly, so that the chloride ions on the inner wall of the container are completely dissolved in the aqueous solution to obt...

Embodiment 3

[0048] (1) Dissolution of polyisobutylene: Weigh 0.324 g of polyisobutylene (sample 3, weight average molecular weight M w = 149,000) was dissolved in 50 mL of tetrahydrofuran to make a homogeneous solution;

[0049] (2) Extraction of chloride ions in polyisobutylene: under stirring conditions, the homogeneous solution prepared in step (1) was slowly added dropwise to 100 mL of ultrapure water, and after the polyisobutylene was precipitated from the water, the solution was subjected to high-speed Centrifugal separation, time 20min, rotating speed 4600rpm; pour out the supernatant liquid; wash the precipitated polyisobutene with 10mL ultrapure water twice, combine the supernatant liquid and washing solution; evaporate the tetrahydrofuran and water in the extraction solution; add 10mL ultrapure water; Wash with pure water to extract chloride ions, shake repeatedly, so that the chloride ions on the inner wall of the container are completely dissolved in the aqueous solution to ob...

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Abstract

The invention discloses a detection method of free chlorine ions in polyisobutylene, which is also applicable to the detection of other polyolefin free chlorine ions, and adopts a dissolution-precipitation method to separate and extract the free chlorine ions in the polyisobutylene and measures the chlorine ion content in the absorption liquid though the chlorine ion quantitative analysis method as the ion chromatography. The technical scheme is simple and reliable to operate, requires no special device, is particularly applicable to the detection of the free chlorine ions in the polyisobutylene, and has high detection accuracy. The detection method of the free chlorine ions in the polyisobutylene adopting the ion chromatography with the detection lower limit being ppb level is convenient and reliable.

Description

technical field [0001] The invention relates to a method for detecting free chloride ions in high molecular polymers, in particular to a method for detecting free chloride ions in polyisobutylene, and belongs to the technical field of chemical industry. Background technique [0002] Polyisobutylene is a class of industrialized polyolefins, widely used in lubricating oil, rubber, adhesives, plasticizers, softeners, electrical insulating materials, sealing materials, gasoline detergents and gum base glue and many other aspects. Polyisobutene is obtained by cationic polymerization of monomer isobutene, generally using Lewis acid (Lewis) as a cationic polymerization initiator, such as AlCl 3 , SnCl 4 , TiCl 4 and BF 3 Wait. The catalyst in the polymerized product was removed by alkaline washing and water elution. In order not to affect the dielectric constant, electrical insulation and thermal stability of polyisobutylene products, especially medical grade and food grade po...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
Inventor 朱庆增李春晓主沉浮
Owner SHANDONG UNIV
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