Method for synthesizing ε-caprolactone

A technology of caprolactone and cyclohexanone, which is applied in the continuous process field of synthesizing ε-caprolactone, can solve the problems of difficulty in large-scale production, high separation cost, and long process flow, so as to avoid the decline of product yield and high Conversion rate, high selectivity effect

Active Publication Date: 2021-12-28
CHINA PETROLEUM & CHEM CORP +1
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  • Abstract
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Problems solved by technology

[0004] Chinese patent CN 103539770 A discloses a microchannel reaction technology for preparing ε-caprolactone based on the oxidation of cyclohexanone with peracetic acid, and Chinese patent CN 106279093 A discloses a method for preparing ε-caprolactone based on the oxidation of cyclohexanone with m-chloroperoxybenzoic acid. For the microchannel reaction technology of ε-caprolactone, the above two processes need to prepare peroxyacid first and then use peroxyacid to oxidize cyclohexanone. The process is relatively long, and the organic acid after the reaction must be separated and recovered. For the re-preparation of peroxyacid, the separation cost is relatively high, and it is difficult in large-scale production

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  • Method for synthesizing ε-caprolactone

Examples

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Embodiment 1

[0014] Use a metering pump to transport the aqueous phase raw material containing oxidant and catalyst, wherein the mass fraction of hydrogen peroxide is 40%, the mass fraction of catalyst is 1.5%, and the molar ratio of oxalic acid and sodium tungstate in the catalyst is 1.0; The oil phase raw material, wherein the water-carrying agent toluene mass fraction is 50%. The molar ratio of the oxidant in the water phase raw material to the cyclohexanone in the oil phase raw material is 3.5, and the two streams of materials are respectively preheated by a preheater and fully mixed in a micro mixer at 50°C. The liquid at the outlet of the micro-mixer enters the micro-reactor as a liquid-phase raw material through the connecting pipeline, enters the micro-reactor through the liquid-phase raw material inlet, and contacts with the air entering from the lower gas-phase inlet in countercurrent to carry out the cyclohexanone oxidation reaction. The heating medium in the tube wall provides ...

Embodiment 2

[0016] Use a metering pump to transport the aqueous phase raw material containing oxidant and catalyst, wherein the mass fraction of hydrogen peroxide is 30%, the mass fraction of catalyst is 1.5%, and the molar ratio of oxalic acid to sodium tungstate in the catalyst is 1.0; The oil phase raw material, wherein the water-carrying agent toluene mass fraction is 50%. The molar ratio of the oxidizing agent in the water phase raw material to the cyclohexanone in the oil phase raw material is 3.5, and the two streams of materials are respectively preheated by a preheater and fully mixed in a micro mixer at 50°C. The liquid at the outlet of the micro-mixer enters the micro-reactor as a liquid-phase raw material through the connecting pipeline, enters the micro-reactor through the liquid-phase raw material inlet, and contacts with the air entering from the lower gas-phase inlet in countercurrent to carry out the cyclohexanone oxidation reaction. The heating medium in the tube wall pr...

Embodiment 3

[0018]Use a metering pump to transport the aqueous phase raw material containing oxidant and catalyst, wherein the mass fraction of peracetic acid is 15%, the mass fraction of catalyst is 1.5%, and the molar ratio of oxalic acid and sodium tungstate in the catalyst is 1.0; The oil phase raw material of the water agent, wherein the toluene mass fraction of the water agent is 50%. The molar ratio of the oxidizing agent in the water phase raw material to the cyclohexanone in the oil phase raw material is 3.5, and the two streams of materials are respectively preheated by a preheater and fully mixed in a micro mixer at 50°C. The liquid at the outlet of the micro-mixer enters the micro-reactor as a liquid-phase raw material through the connecting pipeline, enters the micro-reactor through the liquid-phase raw material inlet, and contacts with the air entering from the lower gas-phase inlet in countercurrent to carry out the cyclohexanone oxidation reaction. The heating medium in th...

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Abstract

The invention discloses a method for synthesizing ε-caprolactone, which comprises making the water-phase raw material containing a homogeneous catalyst of sodium tungstate and an oxidant and the oil-phase raw material containing cyclohexanone and a water-carrying agent, in a micro-mixer In the mixing process, the obtained liquid-phase raw materials and gas-phase raw materials continue to undergo the reaction separation coupling process in the microreactor to obtain the step of ε-caprolactone, and use a low-concentration oxidant to oxidize cyclohexanone in one step, without the technical scheme of preparing peroxyacid , which better solves the problem of the safety of the reaction process in the prior art, and can be used in the field of strengthening the coupling process of mixed reactions by microchannel technology.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis technology, and in particular relates to a continuous process for synthesizing ε-caprolactone in a micro-reaction device using cyclohexanone and hydrogen peroxide as raw materials. Background technique [0002] ε-caprolactone is an environmentally friendly polyester monomer, mainly used for the synthesis of polycaprolactone, a polymer material with unique biocompatibility, biodegradability and good permeability, and can also be used as a modified material Copolymerization with other polymer monomers or blending with polymer materials to improve its gloss, transparency, biodegradability and anti-adhesive properties, etc., is a fine chemical with a very broad market application prospect in recent years. [0003] At present, the production method of ε-caprolactone in the world is mainly peroxyacid oxidation method, that is, using peroxyacid as an oxidant to oxidize cyclohexanone to synthesi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D313/04B01J19/00
CPCC07D313/04B01J19/0093B01J2219/00873
Inventor 储博钊钟思青何乐路马俊
Owner CHINA PETROLEUM & CHEM CORP
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