Continuous Preparation Method of High-Purity Quadricyclane

摘要

The invention discloses a continuous process for producing high-pure quadricyclane, in which “a reaction-rectification integral process” or “a reaction followed by rectification process” may be employed. The two processes both use a novel composite catalyst which is obtained by loading an organic photo-sensitizer on a solid photocatalyst, and the composite catalyst has a high activity and a good stability. In the reaction-rectification integral process, the composite catalyst is used by being blended with rectification fillers or covering the rectification fillers, so as to achieve the integration of the reaction and the rectification. In the reaction followed by rectification process, the composite catalyst and the rectification fillers are placed separately from each other. The two processes achieve a relatively short residence time of reactants, produce highly-pure quadricyclane, and reduce the formation of cokes.

主权项

1. A continuous process for producing highly-pure quadricyclane, comprising the following steps:
(a) a norbornadiene reactant is introduced into a reaction-rectification integral reactor; the reactor comprises a stainless steel cylinder in the outside, and a quartz tube is arranged inside of the reactor; an ultraviolet light source is arranged in the quartz tube, and rectification fillers and a composite catalyst are filled between the quartz tube and the stainless steel cylinder, wherein the rectification fillers are disorderly mixed with the composite catalyst in the particulate form, or the surface of the rectification fillers is covered with a layer of the composite catalyst; the introduced norbornadiene in a form of a liquid film or a gas-liquid mixture flows through the surface and inner channels of the composite catalyst so that a reaction is conducted to produce a reaction product comprising quadricyclane and cokes; and simultaneously, (b) under the rectification action provided by the reaction-rectification integral reactor, the norbornadiene gradually moves toward the top of the reaction-rectification integral reactor and the reaction continues; unreacted norbornadiene leaves from the top and after being condensed, it returns the reaction-rectification integral reactor as the circulating reactant; the product quadricyclane and cokes can move toward the bottom of the reaction-rectification integral reactor under the action of rectification and are discharged from the bottom to a distiller in which the distillation is conducted; at last, the quadricyclane in the purity of more than 99.5% is produced on the top of the distiller, and the cokes are remained in the bottom of the distiller.