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Detection method of free chlorine ions in polyisobutylene

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

Active Publication Date: 2013-12-11
SHANDONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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) Dissolving of polyisobutylene: take by weighing 0.328g polyisobutylene (sample 1, weight average molecular weight M w =100,000) was dissolved in 50mL tetrahydrofuran to make a homogeneous solution;

[0033] (2) Extraction of chloride ions in polyisobutene: under stirring conditions, slowly drop the homogeneous solution prepared in step (1) into 100 mL of ultrapure water, and after the polyisobutene is precipitated from the water, the solution is subjected to high-speed Centrifuge for 15 minutes at a speed of 4500 rpm; pour off the supernatant liquid; wash the precipitated polyisobutene twice with 10 mL ultrapure water, combine the supernatant liquid and the washing solution; distill off the tetrahydrofuran and water in the extraction solution; add 10 mL ultrapure water Soak in 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 obtain an absorption sol...

Embodiment 2

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

[0041] (2) Extraction of chloride ions in polyisobutene: under stirring conditions, slowly drop the homogeneous solution prepared in step (1) into 100 mL of ultrapure water, and after the polyisobutene is precipitated from the water, the solution is subjected to high-speed Centrifuge for 20 minutes at a speed of 4600 rpm; pour off the supernatant liquid; wash the precipitated polyisobutene twice with 10 mL ultrapure water, combine the supernatant liquid and the washing solution; distill off tetrahydrofuran and water in the extraction solution; add 10 mL ultrapure water Soak in 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 obtain an absorption solution...

Embodiment 3

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

[0049] (2) Extraction of chloride ions in polyisobutene: under stirring conditions, slowly drop the homogeneous solution prepared in step (1) into 100 mL of ultrapure water, and after the polyisobutene is precipitated from the water, the solution is subjected to high-speed Centrifuge for 20 minutes at a speed of 4600rpm; pour out the supernatant liquid; wash the precipitated polyisobutene twice with 10 mL ultrapure water, combine the supernatant liquid and the washing solution; distill off the tetrahydrofuran and water in the extraction solution; add 10 mL ultrapure water Soak in 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 obtain an absorption solu...

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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 insulation materials, sealing materials, gasoline detergents and chewing gum base glue and many other aspects. Polyisobutylene is prepared by cationic polymerization of monomer isobutylene, generally using Lewis acid (Lewis) as cationic polymerization initiator, such as AlCl 3 , SnCl 4 、TiCl 4 and BF 3 Wait. The catalyst in the polymerization product is removed by alkali washing and water washing. In order not to affect the dielectric constant, electrical insulation, and thermal stability of polyisobutylene products, especially medical grade and foo...

Claims

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Application Information

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