Integrated high-throughput methods to characterize multi-component polymers

Patent metadata

Field	Value
Publication number	US-10732158-B2
Application number	US-201715658904-A
Country	US
Kind code	B2
Filing date	Jul 25, 2017
Priority date	Aug 31, 2016
Publication date	Aug 4, 2020
Grant date	Aug 4, 2020

Abstract

A method of analyzing a multi-component polymer comprising: (a) dissolving an multi-component polymer having a primary monomer and primary comonomer to form a first volume (soluble portion of multi-component polymer); (b) injecting a portion of the first volume into a chromatographic column to get elution first slices, leaving a second volume behind; (c) filtering the second volume to isolate multi-component polymer solids; (d) dissolving solids to form solution third solution (insoluble portion of multi-component polymer); (e) injecting a portion of third solution into the chromatographic column to get elution second slices; (f) obtain infra-red spectra at wavelengths suitable for the primary monomer and the primary comonomer of first and second elution slices, separately; and (g) for each elution slice, separately calculate: (i) the different polymer components (soluble and insoluble); and (ii) the comonomer content of each component (soluble and insoluble).

First claim

The invention claimed is:

1. A method of analyzing a multi-component polymer, MCP comprising:
a) dissolving a MCP having a primary monomer and primary comonomer in a vial to form a parent sample having a volume V 1 comprising soluble polymer;
b) injecting a portion of the V 1 into a chromatographic column to get elution slices E 1 , leaving a volume V 2 behind in the vial;
c) filtering V 2 to isolate MCP solids Mp;
d) dissolving solids Mp to form solution V 3 ;
e) injecting a portion of V 3 into the chromatographic column to get elution slices E 3 ;
f) obtaining IR spectra at wavelengths suitable for the primary monomer and the primary comonomer of E 1 and E 3 , separately; and
g) for each elution slice E 1 and E 3 , separately determine:
i) the different polymer components; and
ii) the comonomer content of each component.

2. The method of claim 1 , calculating the concentration of the soluble polymer in the solution of parent sample with the following formulae:
1) calculate the apparent concentration of soluble phase (C GPC ) of V 1 with the its mass recovery (MR Solu ) and assumed concentration (M 0 /V 0 ) where M 0 is the assumed polymer mass in solution and V 0 is the volume amount of solvent into the vial:

C
GPC

=

M
0

V
0

⁢

MR
Solu

2) prorate the apparent concentration to the actual concentration:

C
Solu

=

V

Sample
⁢

⁢
2

+

V
0

V

Sample
⁢

⁢
2

⁢

C
GPC

=

(

1
+

DV
0

M
Solu

)

⁢

M
0

V
0

⁢

MR
Solu

;

3) calculate the mass ratio of soluble phase (EP+aPP) in the MCP, where the MCP has a concentration C MCP ;

R
Solu

=

C
Solu

C
MCP

=

(

1
+

DV
0

M
Solu

)

⁢

M
0

V
0

⁢

MR
Solu

C
MCP

;

where “D” is solvent density and the MCP is assumed to be fully dissolved; or alternatively the C MCP can be determined with the similar procedure as C Solu ;

C
MCP

=

(

1
+

D
1

⁢

V
0

M
MCP

1

)

⁢

M
0

1

V
0

1

⁢

MR
MCP

1

,

where the 1 M 0 , 1 V 0 , 1 M MCP , 1 MR MCP in the first test are

Assignees

• Exxonmobil Chemical Patents Inc

Inventors

• Kang Shuhui

Classifications

• G01N2030/065

  using different phases to separate parts of sample · CPC title

• G01N2030/885

  involving polymers · CPC title

• B01J20/291

  Gel sorbents · CPC title

• B01J2220/54

  Sorbents specially adapted for analytical or investigative chromatography · CPC title

• G01N30/88

  Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 · CPC title