Norbornene production method

A technology for norbornene and a production method, applied in the field of preparing norbornene, can solve the problems of reaction temperature and pressure safety traps, harshness, etc., and achieve the effects of avoiding explosion danger, improving selectivity, and improving yield

Active Publication Date: 2016-04-13
SHANGHAI PEARLK CHEM
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Problems solved by technology

[0007] In the prior art, the conditions for the diene synthesis reaction between CPD and ethylene are still relatively harsh, and the high reaction temperature and pressure bring great safety hazards to the production process, and the endothermic depolymerization of DCPD and the synthesis of diene are not fully utilized. Exothermic heat balance, there is a risk of CPD forming DCPD oligomers and oligomers continue to polymerize to form DCPD polymers

Method used

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Embodiment 1～6

[0031]The reaction was carried out in two tank reactors connected in series with a volume capacity of 2 liters and 1 liter respectively. The reactor was equipped with a stirring device, a cooling coil, and an electric heating system was installed outside. The prepared dicyclopentadiene (DCPD), solvent methyl isobutyl ketone (MIBK) and polymerization inhibitor (TBC) solution are continuously sent into the first tank reactor from the bottom of the first tank reactor with a pump , After starting the stirring, feed the required part of ethylene gas, and raise the temperature to the required temperature, and then use the constant pressure valve to adjust the pressure of the reactor to the set pressure, and the reaction liquid of the first tank reactor passes through the reactor The discharge port on the upper side is continuously discharged into the second tank reactor through the bottom of the second tank reactor, and the reaction continues under the set conditions, and the reactio...

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Abstract

A norbornene production method uses two tank reactors in series, so that dicyclopentadiene (DCPD) depolymerizes into cyclopentadiene (CPD), and cyclopentadiene and ethylene are subjected to a Diels-Alder reaction to convert into norbornene (NB). The method is as below: 1) continuously feeding the prepared dicyclopentadiene, a solvent methyl isobutyl ketone (MIBK) and a polymerization inhibitor p-tert-butyl catechol (TBC) solution by a pump from the bottom of a first tank reactor to a reactor, stirring, introducing ethylene gas, reacting at the temperature of 170-190 DEG C and under the pressure of 7-11 MPa, maintaining the materials in the reactor for 10-120 min; 2) maintaining the materials in a second tank reactor for 10-80 min at the reaction temperature of 200-220 DEG C and under the pressure of 7-10 MPa; sending the discharged reaction solution into a refining system to obtain refined norbornene with content of higher than 99.9 wt.%. The method increase the yield of NB and effectively prevents the generation of CPD polymer and polymer.

Description

technical field [0001] The present invention relates to a kind of method that takes dicyclopentadiene (DCPD) and ethylene as raw material to prepare norbornene (NB), particularly relate to using methyl isobutyl ketone (MIBK) as solvent, in two tank reaction in series In the device, dicyclopentadiene (DCPD) is depolymerized into cyclopentadiene (CPD), and cyclopentadiene (CPD) undergoes a Diels-Alder reaction with ethylene to convert into norbornene. Background technique [0002] Norbornene (NB), chemical name bicyclo[2.2.1]-2-heptene, molecular formula C 7 h 10 , relative molecular mass 94.16, boiling point 96°C, melting point 44-46°C, flash point -15°C, density 0.950g / cm 3 , Refractive index 1.4475, it is white translucent crystal at room temperature, easy to sublimate. Norbornene (NB) is mainly used in the synthesis of cycloolefin copolymers (COC). COC has the advantages of low density, low hygroscopicity, high transparency, high heat resistance, high refractive index ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C2/50C07C13/42
CPCC07C2/50C07C4/22C07C13/42C07C13/15
Inventor 石康明
Owner SHANGHAI PEARLK CHEM
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