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Process for removal of 1,2-epoxy-5-hexene from epichlorohydrin

An epichlorohydrin, epoxy-based technology applied to remove 1 from epichlorohydrin, which can solve problems such as pollution, increased complexity and cost

Inactive Publication Date: 2016-02-24
HEXION INC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Therefore, there is a potential contamination problem with the process
This will again add complexity and cost

Method used

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  • Process for removal of 1,2-epoxy-5-hexene from epichlorohydrin

Examples

Experimental program
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Embodiment

[0044] Experimental setup. The simulation experiments were carried out in a jacketed glass reactor with a reaction volume of about 250 ml equipped with temperature control, reflux condenser, overhead stirrer and UV-VIS probe. Here is the addition of 1,2-epoxy-5-hexene to a solution containing a fixed amount of dissolved Cl 2 of pure ECH instead of first preparing epichlorohydrin and dosing Cl based on the 1,2-epoxy-5-hexene contained therein 2 . This has the advantage of reproducibility and facilitates comparison of results.

[0045] By using Hastelloy (Hastelloy) autoclave, the Cl 2 Dissolve in epichlorohydrin and transfer to a glass reactor. During the transfer from the autoclave to the glass reactor, the Cl in epichlorohydrin 2 Concentration is stable. Cl 2 Concentrations were measured by UV-VIS spectrophotometer at a wavelength of 360 nm. The concentrations of 1,2-epoxy-5-hexene and epichlorohydrin were measured by gas chromatography. In a typical example, dissolv...

Embodiment 2-7

[0049] using different temperatures and Cl 2 / 1,2-epoxy-5-hexene ratio, the results of the corresponding reactions are listed in Table 1 (entries 2-7). The reaction time for the exhaustion of the halogen was the same as that of Comparative Example C1, which was less than 5 seconds.

[0050] Table 1. Chlorination of 1,2-epoxy-5-hexene in epichlorohydrin

[0051]

[0052] (*) Calculated based on 1,2-epoxy-5-hexene and other ethylenically unsaturated components in epichlorohydrin

[0053] The reaction proceeds well when the temperature is higher than 30°C, because the Cl 2 It reacts with 1,2-epoxy-5-hexene with high selectivity. Using excess Cl 2 Can result in complete removal of 1,2-epoxy-5-hexene, but also result in excess chlorine present in the product. Comparing Examples 1 (Comparative), 2 and 3 shows that a substantial amount of 1,2-epoxy-5-hexene can be removed using substoichiometric amounts of chlorine. Embodiments 5 to 7 show that high temperatures can be used....

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Abstract

The invention relates to a process for purification of epichlorohydrin containing 1,2-epoxy-5-hexene impurity, by (a) epoxidizing allyl chloride contaminated with 1,5-hexadiene into epichlorohydrin, (b) removing any unreacted allyl chloride, (c) adding a halogen to the crude epichlorohydrin obtained after the removal of unreacted allyl chloride and allowing the halogen to react with 1,2-epoxy-5-hexene and other olefinically unsaturated components, if any, in the crude epichlorohydrin, and (d) rectifying the product of step (c) to obtain epichlorohydrin, wherein the amount of halogen added in step (c) is at a molar ratio of at least 0.5:1 to less than 1:1 calculated on the amount of said 1,2-epoxy-5-hexene and said other olefinically unsaturated components in the crude epichlorohydrin, and allowing the halogen to react until it is fully converted.

Description

technical field [0001] The present invention relates to a process for the removal of 1,2-epoxy-5-hexene from epichlorohydrin during the preparation of epichlorohydrin by epoxidation of allyl chloride. Background technique [0002] Epichlorohydrin is usually prepared by epoxidation of allyl chloride. Unfortunately, there is an impurity in the allyl chloride starting material: 1,5-hexadiene. This impurity participates in the epoxidation reaction and produces a by-product, 1,2-epoxy-5-hexene, which causes problems in the further use of epichlorohydrin. [0003] Rectification is the separation of components of a liquid mixture by successive distillations (partial evaporation and condensation) and obtaining products by using integral or differential processes. Effective separation of pure components can be obtained by this process (Perry's Chemical Engineers' Handbook, 6 th edition, 18-3). Unfortunately, 1,2-epoxy-5-hexene has a boiling point of 118-121°C, so it cannot be sep...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D303/08
CPCC07D301/32C07D303/08
Inventor P·黑萨克尔斯M·卡佩伦J·林克S·伦斯-范德李J·A·范赖恩
Owner HEXION INC
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