Process for preparing high purity epichlorohydrin

• US 5,169,964 A
• Filed: 04/04/1989
• Issued: 12/08/1992
• Est. Priority Date: 04/06/1988
• Status: Expired due to Fees

• Current Assignee: Deutsche Solvay-Werke GmbH Langhansstrasse
• Original Assignee: Deutsche Solvay-Werke GmbH
• Inventors: Jakobson, Gerald, Siemanowski, Werner
• Primary Examiner(s): Ivy, C. Warren
• Assistant Examiner(s): Trinh, Ba K.
• Application Number:
  US07/333,008
• Time in Patent Office: 1,344 Days
• Field of Search: 549/541
• US Class Current: 549/541
• CPC Class Codes: C07D 301/32 Separation; Purification

Abstract

The present invention relates to a process for preparing ultrapure epichlorohydrin from epichlorohydrin containing technical impurities, by fractional distillation under particular conditions, preferably with continuous operation, that yield a product of very high purity and very low content of halogenated hydrocarbons. Epoxy resins made with such ultrapure epichlorohydrin are especially well suited for use in fabricating electrical components and microchips.

Claims

1. A process for preparing high-purity epichlorohydrin from epichlorohydrin containing technical impurities, which comprises the steps of:

preheating technical epichlorohydrin to a temperature below its boiling point; and

fractionally distilling said preheated technical epichlorohydrin at a pressure of 0.2 to 1.05 bar in a column having at least 15 theoretical plates and which is provided with heating or evaporating means located at or near the sump of the column, inlet means for introducing technical epichlorohydrin at an intermediate point in said column, and outlet means for withdrawing high-purity epichlorohydrin at a point above said inlet means,

wherein said preheated technical epichlorohydrin is introduced into said column at a distance from said evaporation or heating means which is greater than one-tenth of the total length of the column, and the high-purity epichlorohydrin is withdrawn at a distance from said evaporation or heating means which is greater than one-third of the total length of the column,

and wherein the temperature difference between said preheated technical epichlorohydrin introduced into the column and the operational epichlorohydrin introduced into the column and the operational temperature in the column is 50°

C. or less.

2. The process of claim 1, wherein said column has at least 20 theoretical plates.

3. The process of claim 2, wherein said column has at least 25 theoretical plates.

4. The process of claim 1, wherein the technical epichlorohydrin is introduced into said column at a distance from said evaporation or heating means which is greater than one-quarter of the total length of the column.

5. The process of claim 1, wherein the high-purity epichlorohydrin is withdrawn at a distance from said evaporation or heating means which is greater than one-half of the total length of the column.

6. The process of claim 1, wherein said temperature difference is 10°

C. or less.

7. The process of claim 1, wherein the preheated technical epichlorohydrin is continuously introduced into the column.

8. The process of claim 7, wherein low-boiling impurities or low-boiling azeotropic mixtures with epichlorohydrin are continuously withdrawn at the head of the column and high-boiling impurities or high-boiling azeotropic mixtures containing epichlorohydrin are continuously withdrawn at the foot of the column.

9. The process of claim 1, wherein the rate of introduction of the technical epichlorohydrin is regulated in such a manner that the amount introduced is substantially equal to the sum of the amounts discharged or withdrawn.

10. The process of claim 1, wherein the heating of the epichlorohydrin in the column is carried out by using a circulation evaporator.

11. The process of claim 1, wherein the distance between the position on the column of said inlet means and the position on the column of said outlet means is greater than one-fifth of the length of the column.

12. The process of claim 11, wherein said distance between said inlet means and said outlet means is greater than one-quarter of the length of the column.

13. The process of claim 1, wherein said pressure is 0.5 to 1 bar.

14. The process of claim 1, wherein said column is a perforated-plate column, a bubble-cap plate column or a packed column.