Method for measuring polymer modification ratio

Patent metadata

Field	Value
Publication number	US-2018328901-A1
Application number	US-201715739504-A
Country	US
Kind code	A1
Filing date	Jul 14, 2017
Priority date	Jul 26, 2016
Publication date	Nov 15, 2018
Grant date	—

Abstract

The present invention relates to a method for measuring a polymer modification ratio, and more particularly, to a method for measuring a polymer modification ratio, which includes preparing a first solution by dissolving a polymer mixture containing a modified polymer and an unmodified polymer in a first solvent, injecting the first solution into a column filled with an adsorbent, adsorbing the modified polymer onto the adsorbent, and eluting the first solution in which the unmodified copolymer is dissolved, transferring the eluted first solution to a detector, injecting a second solvent into the column to elute the second solution in which the adsorbed modified polymer is dissolved, and transferring the eluted second solution to the detector.

First claim

1 . A method for measuring a polymer modification ratio, comprising:
preparing a first solution by dissolving a polymer mixture containing a modified polymer and an unmodified polymer in a first solvent; injecting the first solution into a column filled with an adsorbent; adsorbing the modified polymer onto the adsorbent, and eluting the first solution in which the unmodified copolymer is dissolved; transferring the eluted first solution to a detector; injecting a second solvent into the column to elute a second solution in which the adsorbed modified polymer is dissolved; and transferring the eluted second solution to the detector.

2 . The method according to claim 1 , wherein the polymer is a conjugated diene-based polymer.

3 . The method according to claim 1 , wherein the adsorbent is a silica-based adsorbent.

4 . The method according to claim 1 , wherein the first solvent is a polar solvent or a nonpolar solvent,
the second solvent is a polar solvent or a nonpolar solvent, the second solvent is a nonpolar solvent when the first solvent is a polar solvent, and the second solvent is a polar solvent when the first solvent is a nonpolar solvent.

5 . The method according to claim 4 , wherein the polar solvent is at least one selected from the group consisting of water, methanol, ethanol, n-propanol, n-butanol, isopropanol, formic acid, acetic acid, acetone, nitromethane, propylene carbonate, 1,2-dioxane, 1,3-dioxane, 1,4-dioxane, tetrahydrofuran (THF), acetonitrile (MeCN), dimethylformamide (DMF), dimethylsulfoxide (DMSO), methyl ethyl ketone, benzonitrile, pyridine, nitroethane, benzyl alcohol, methoxy ethanol, and formamide.

6 . The method according to claim 4 , wherein the nonpolar solvent is at least one selected from the group consisting of hexane, benzene, toluene, diethyl ether, chloroform, ethylacetate, dichloromethane, cyclohexane, tetrachloromethane, iso-octane, xylene, butyl ether, isopropyl ether, and ethylene chloride.

7 . The method according to claim 1 , wherein the first solution is injected at a flow rate of 0.001 to 30 ml/min.

8 . The method according to claim 1 , wherein the second solvent is injected at a flow rate of 0.001 to 30 ml/min.

9 . The method according to claim 1 , wherein the second solvent is injected after the entire amount of the unmodified polymer is eluted.

10 . The method for claim 9 , wherein the second solvent is continuously injected into the column into which the first solution is injected according to gradient elution.

11 . The method according to claim 1 , wherein the modification ratio is calculated by Equation 2 below from a chromatogram according to the method for measuring a polymer modification ratio;

Modification



ratio




(
%
)

=

Peak



area



of



modified



polymer

Peak



area



of



unmodified



polymer

+

Peak



area



of



modified



polymer

×
100

[

Equation



2

]

where the peak area of the unmodified polymer is a peak area of the chromatogram for the first solution transferred to the detector, and the peak area of the modified polymer is a peak area of the chromatogram for the second solution transferred to the detector.

Assignees

• Lg Chemical Ltd

Inventors

• Choi Heung Yeal
• Kim No Ma
• Kim Yu Jin

Classifications

• G01N30/8606

  Integration · CPC title

• G01N30/74

  Optical detectors {(measurement of intensity, velocity, spectral content, polarisation, or phase of infrared, visible or ultraviolet light G01J)} · CPC title

• G01N30/34

  of fluid composition, e.g. gradient (G01N30/36 takes precedence) · CPC title

• G01N30/16

  Injection (G01N30/24 takes precedence) · CPC title

• B01J20/3257

  the functional group or the linking, spacer or anchoring group as a whole comprising at least one of the heteroatoms nitrogen, oxygen or sulfur together with at least one silicon atom, these atoms not being part of the carrier as such · CPC title