Method for determining the compositional distribution of a crystalline copolymer

• US 5,008,204 A
• Filed: 02/02/1988
• Issued: 04/16/1991
• Est. Priority Date: 02/02/1988
• Status: Expired due to Fees

• Current Assignee: Exxon Chemical Patents Inc. (Exxon Mobil Corporation)
• Original Assignee: Exxon Chemical Patents Inc. (Exxon Mobil Corporation)
• Inventors: Stehling, Ferdinand C.
• Primary Examiner(s): Hill, Jr., Robert J.
• Application Number:
  US07/151,350
• Time in Patent Office: 1,169 Days
• Field of Search: 436/85, 436/161, 73/53, 73/61.1 C, 210/-35, 210/656, 210/774, 210/198.2, 210/662, 528/481, 422/70
• US Class Current: 436/85
• CPC Class Codes: B01D 9/0013 by indirect heat exchange
• CPC Class Codes: B01D 9/004 Fractional crystallisation; Fractionating or rectifying columns
• CPC Class Codes: B01D 9/0063 Control or regulation control per se G05
• CPC Class Codes: G01N 2030/008 Thermal desorption
• CPC Class Codes: G01N 25/147 by cristallisation
• CPC Class Codes: G01N 33/44 Resins; rubber; leather

Abstract

A method for fractionating crystalline copolymers to determine solubility distribution as a function of temperature. Fractionation is conducted by passing a solvent through a column containing the crystallized copolymer at an increasing temperature from 6° C. to about 120° C. The polymer solution exiting the column is analyzed by infrared spectroscopy or NMR to determine the composition distribution of the copolymer.

Claims

1. A method for determining the solubility distribution of a crystalline copolymer, comprising the steps of:

dissolving the copolymer in a solvent at elevated temperature;

filling a column with the solvent containing the dissolved copolymer;

crystallizing the copolymer within the column by reducing the temperature of the column to below ambient temperature;

passing pure solvent through the column at an increasing column temperature to gradually dissolve the copolymer; and

continuously measuring the concentration of the copolymer in the solvent exiting the column.

2. The method of claim 1, wherein the solvent is tetrachloroethylene.

3. The method of claim 1, wherein the pure solvent is passed through the column below ambient temperature to substantially remove uncrystallized polymer prior to increasing the column temperature.

4. The method of claim 1, wherein the column temperature is increased from about 6°

C to about 150°

C.

5. The method of claim 1, further comprising the steps of:

collecting the solvent exiting the column in fractions; and

analyzing the solvent fractions for molecular weight and monomer composition.

6. A method for determining the solubility distribution and composition distribution of a crystalline copolymer, comprising the steps of:

dissolving the copolymer in a solvent at elevated temperature;

filling a packed column with the solvent containing the dissolved copolymer;

crystallizing the copolymer within the column by reducing the temperature of the column to below or about 6°

C,

passing pure solvent through the column at an increasing column temperature to gradually dissolve the copolymer;

continuously measuring the concentration of the copolymer in the solvent exiting the column;

collecting the solvent exiting the column in fractions; and

analyzing the solvent fractions for molecular weight and monomer composition.

7. The method of claim 6, wherein the solvent is tetrachloroethylene.

8. The method of claim 6, wherein the pure solvent is passed through the column at or below about 6°

C for at least one hour to remove uncrystallized polymer prior to increasing the column temperature.

9. The method of claim 6, wherein he column temperature is increased from about 6°

C. to about 150°

C.

10. A method for determining the solubility distribution and composition distribution of a crystalline copolymer, comprising the steps of:

dissolving the copolymer in a solvent at elevated temperatures;

filling a column with the solvent containing the dissolved copolymer;

crystallizing the copolymer within the column by reducing the temperature of the column to about 0°

C.,

passing pure solvent through the column at 0°

C for at least an hour to remove uncrystallized polymer;

passing pure solvent through the column at an increasing column temperature of from about 0°

C. to about 150°

C. to gradually dissolve the crystallized copolymer.

continuously measuring the concentration of the copolymer in the solvent exiting the column;

collecting the solvent exiting the column in fractions; and

analyzing the solvent fractions for molecular weight and composition.

11. The method of claim 10, wherein the solvent is tetrachloroethylene.