Reciprocating-plate column reactor for epoxidation of epoxy resins

Patent metadata

Field	Value
Publication number	US-9527950-B2
Application number	US-201213600461-A
Country	US
Kind code	B2
Filing date	Aug 31, 2012
Priority date	Sep 27, 2011
Publication date	Dec 27, 2016
Grant date	Dec 27, 2016

Abstract

A process comprising: a) contacting a polyhydric phenol and an epihalohydrin in the presence of a catalyst under reaction conditions to form an organic feed comprising a bishalohydrin ether and a solvent; b) contacting the organic feed and an aqueous feed comprising an inorganic hydroxide in a reciprocating-plate column reactor under reaction conditions to form a dispersed aqueous phase and an organic product; and c) collecting the organic product comprising an epoxy resin, is disclosed.

First claim

What is claimed is:

1. A process comprising:
a) contacting a polyhydric phenol and an epihalohydrin in the presence of a catalyst under reaction conditions to form an organic feed comprising a bishalohydrin ether and at least 10 weight percent of a solvent, wherein the molar ratio of said epihalohydrin to said polyhydric phenol is in the range of from 1:1 to 50:1;
b) contacting said organic feed comprising a bishalohydrin ether and at least 10 weight percent of a solvent and an aqueous feed comprising an inorganic hydroxide in a reciprocating-plate column reactor under reaction conditions to form a dispersed aqueous phase and an organic product, wherein said reaction conditions comprise a reaction temperature of from 15° C. to 50° C.; and
c) collecting said organic product comprising an epoxy resin, wherein the epihalohydrin yield loss ranges from 2.5% to 6.6% used to make the epoxy resin.

2. A process in accordance with claim 1 wherein said phenol is selected from the group consisting of bisphenol-A, bisphenol-F, phenol-formaldehyde novolacs, cresol-formaldehyde novolacs, bisphenol-A-formaldehyde novolacs, trisphenols, biphenols, diphenols, hydroquinone and combinations thereof and said epihalohydrin is selected from the group consisting of epichlorohydrin, epibromohydrin, methylepichlorohydrin and combinations thereof.

3. A process in accordance with claim 1 wherein said catalyst of step a) is selected from the group consisting of sodium hydroxide, potassium hydroxide, calcium hydroxide, and combinations thereof.

4. A process in accordance with claim 1 wherein excess epihalohydrin is used in step (a).

5. A process in accordance with claim 1 wherein said inorganic hydroxide of step b) is selected from the group consisting of sodium hydroxide, potassium hydroxide, calcium hydroxide, and combinations thereof.

6. A process in accordance with claim 1 wherein step a) is conducted in the presence of a cosolvent selected from the group consisting of isopropanol, 1-methoxy-2-propanol, and combinations thereof.

7. A process in accordance with claim 1 wherein step a) is conducted in the presence of a dilution solvent selected from the group consisting of toluene, xylenes, methyl ethyl ketone, methyl isobutyl ketone, and combinations thereof.

8. A process in accordance with claim 1 wherein step b) is conducted in the presence of a dilution solvent selected from the group consisting of toluene, xylenes, methyl ethyl ketone, methyl isobutyl ketone, and combinations thereof.

9. A process in accordance with claim 1 wherein said solvent further comprises a group comprising epihalohydrin, a cosolvent, a dilution solvent, and combinations thereof.

10. A process in accordance with claim 1 wherein step b) is conducted in the presence of a cosolvent selected from the group consisting of isopropanol, 1-methoxy-2-propanol, and combinations thereof.

11. A process in accordance with claim 1 wherein step b) is conducted in the presence of a phase transfer agent.

12. A process in accordance with claim 11 wherein said phase transfer agent is a quaternary amine.

13. A process in accordance with claim 1 wherein said collecting in step c) comprises:
i. washing said organic product with water; and
ii. devolatilizing said organic product to form said epoxy resin.

14. A process in accordance with claim 1 wherein said reaction conditions in step a) comprise a first reaction temperature in the range of from 10° C. to 100° C. and said reaction conditions in step b) comprise a second reaction temperature in the range of from 0° C. to 100° C.

15. A process in accordance with claim 1 wherein said reciprocating column reactor has a stroke length in the range of from 0.2 cm to 10 cm, an agitation frequency in the range of from about 0.1 Hz to about 10 Hz, and a plate spacing in the range of from about 0.3 cm to about 30 cm.

16. A process in accordance with claim 9 wherein said solvent is removed and replaced with a different solvent before said contacting of step b).

17. A process in accordance with claim 1 wherein 80% or more of the polyhydric phenolic OH groups are etherified.

Assignees

• Young Thomas C
• Worley William G
• Drake Robert M
• Blue Cube Ip Llc

Inventors

• Young Thomas C
• Worley William G
• Drake Robert M

Classifications

• C08G59/063

  with epihalohydrins · CPC title

• C08G59/022 Primary

  characterised by the preparation process or apparatus used · CPC title