POLYCONDENSATION STOICHIOMETRY CONTROL

• US 20190315922A1
• Filed: 04/12/2019
• Published: 10/17/2019
• Est. Priority Date: 04/17/2018
• Status: Abandoned Application

• Current Assignee: SHPP Global Technologies BV (Government of Saudi Arabia)
• Original Assignee: SABIC Global Technologies BV (Government of Saudi Arabia)
• Inventors: KLOPPENBURG, LIOBA MARIA, SULUB, YUSUF, GONZALEZ SERRANO, CESAR, ODLE, ROY RAY
• Application Number:
  US16/383,209
• Publication Number:
  US 20190315922A1
• Time in Patent Office: Days
• CPC Class Codes: C08G 73/1014 in the form of (mono)anhydrid
• CPC Class Codes: C08G 73/1032 characterised by the solvent(s) used
• CPC Class Codes: C08G 73/1042 Copolyimides derived from at least two different tetracarboxylic compounds or two different diamino compounds
• CPC Class Codes: C08G 73/1053 with oxygen only in the tetracarboxylic moiety
• CPC Class Codes: C08G 73/1071 Wholly aromatic polyimides containing oxygen in the form of ether bonds in the main chain
• CPC Class Codes: G01N 2021/8514 with immersed mirror
• CPC Class Codes: G01N 21/272 for following a reaction, e.g. for determining photometrically a reaction rate (photometric cinetic analysis)
• CPC Class Codes: G01N 21/359 using near infrared light

Abstract

A method of making a polyetherimide including: setting a target range for the anhydride-amine stoichiometry in a reaction mixture; combining a solvent, a diamine, a bis(ether anhydride), and an optional end capping agent to form the reaction mixture wherein the reaction mixture has a polyamic acid content; analyzing the amine and anhydride end group content of the reaction mixture using near infrared vibrational spectroscopy; calculating the anhydride-amine stoichiometry; comparing the calculated anhydride-amine stoichiometry to the target stoichiometry, and, when necessary, adjusting the concentration of bis(ether anhydride) or diamine based on the comparison of the calculated anhydride-amine stoichiometry to the target stoichiometry.

Claims

1. A method of making a polyetherimide comprising:

setting a target range for the anhydride-amine stoichiometry in a reaction mixture;

combining a solvent, a diamine, a bis(ether anhydride), and an optional end capping agent to form the reaction mixture wherein the reaction mixture has a polyamic acid content;

analyzing the amine and anhydride end group content of the reaction mixture using near infrared vibrational spectroscopy;

calculating the anhydride-amine stoichiometry;

comparing the calculated anhydride-amine stoichiometry to the target stoichiometry, and, when necessary, adjusting the concentration of bis(ether anhydride) or diamine based on the comparison of the calculated anhydride-amine stoichiometry to the target stoichiometry.

2. The method of claim 1, wherein the diamine is m-phenylene diamine, p-phenylene diamine or a combination thereof and the bis(ether anhydride) is bisphenol A dianhydride.

3. The method of claim 1, wherein the solvent is o-dichlorobenzene, dichlorotoluene, 1,2,4-trichlorobenzene, diphenyl sulfone, anisole, veratrole, diphenylether, or phenetole.

4. The method of claim 1, wherein the reaction mixture further comprises an end capping agent.

5. The method of claim 1, wherein the target range for anhydride-amine stoichiometry is −

25 to 25 mole %.

6. The method of claim 1, wherein analyzing the amine and anhydride end group content is performed inline.

7. The method of claim 1, wherein analyzing the amine and anhydride end group content is performed using a probe having a fixed path length of 2 to 8 mm.

8. The method of claim 1, wherein the reaction mixture has a solids content of 20 to 70 wt %.

9. The method of claim 8, wherein the reaction mixture is sampled under super-atmospheric pressure to provide a sample for analyzing the amine and anhydride end group content.

10. The method of claim 1, wherein the reaction mixture further comprises a catalyst.