Continuous preparation method of tricyclopentadiene

A technology of tricyclopentadiene and dicyclopentadiene, which is applied in the field of continuous preparation of tricyclopentadiene, can solve the problems of labor cost, equipment cost and production cost increase, complicated operation, long polymerization time, etc. Polymerization time, high volumetric efficiency, and small back-mixing effects

Inactive Publication Date: 2017-04-05
TIANJIN UNIV +1
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Problems solved by technology

[0004] In the preparation process of the high-density liquid jet fuel tetrahydrotricyclopentadiene prepared by the above-mentioned U.S. patent and the Chinese patent, there are the following disadvantages: firstly, the polymerization reaction process described above is operated in a batch reactor, and the polymerization time is longer, and both more than 5 hours;
Each batch of batch reactor polymerization to obtain tricyclopentadiene needs to go through links such as feeding, discharging, temperature rise, long-term constant temperature reaction, and discharging. The operation is more complicated, resulting in labor costs, equipment costs and production costs in the entire production process. cost multiplied

Method used

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  • Continuous preparation method of tricyclopentadiene

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Effect test

Embodiment 1

[0020] The dicyclopentadiene raw material with a purity of 95wt% is transported and injected from the lower port of the tubular reactor with a high-pressure constant-flow pump at a flow rate of 3ml / s. The reactor volume is 60ml, the aspect ratio is 50, and the reaction volume space velocity is 3h -1 , the heating temperature of the reaction tube is 180°C, and the reaction pressure is 2MPa. After the reaction is stable, the product is collected at the outlet, and there is no loss of material during the entire reaction process. The composition of the product was analyzed by gas chromatography, and the content of dicyclopentadiene in the mixture was 67.6wt%, the mass content of tricyclopentadiene was 31.3wt%, and the content of by-product high polymer was 1.1wt%.

Embodiment 2

[0022] The dicyclopentadiene raw material with a purity of 95wt% is transported and injected from the lower port of the tubular reactor with a high-pressure constant-flow pump at a flow rate of 5ml / s. The reactor volume is 150ml, the aspect ratio is 40, and the reaction volume space velocity is 2h -1 , the heating temperature of the reaction tube is 200°C, and the reaction pressure is 3MPa. After the reaction is stable, the product is collected at the outlet, and there is no loss of material during the entire reaction process. The composition of the product was analyzed by gas chromatography, and the content of dicyclopentadiene in the mixture was 60.3wt%, the mass content of tricyclopentadiene was 36.3wt%, and the content of by-product high polymer was 3.4wt%.

Embodiment 3-9

[0024] The polymerization reaction process of each embodiment is the same as that of Examples 1 and 2, except that the adjustment of reaction conditions includes: reactor aspect ratio, reactor volume space velocity, reaction temperature, and reaction pressure. Finally, mixed products containing tricyclopentadiene with different mass contents were obtained.

[0025]

[0026] Using dicyclopentadiene as raw material and using continuous polymerization in a tubular reactor instead of intermittent polymerization in a reactor to prepare tricyclopentadiene can effectively improve the polymerization efficiency, simplify the reaction process, greatly reduce manual operations, save production costs, and are more conducive to large-scale production.

[0027] The height-to-diameter ratio range of the tubular reactor is selected between 10 and 200. Under the condition of a certain reactor volume, too small a height-to-diameter ratio may cause insufficient heating of the material in the m...

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Abstract

The invention discloses a continuous preparation method of tricyclopentadiene. The method includes the steps of: taking dicyclopentadiene as the raw material, injecting the raw material into a tubular reactor with a height-diameter ratio of 10-200 at a uniform volume space velocity of 0.5-3h<-1>, and carrying out polymerization reaction at a gauge pressure of 0.5-5MPa and a reaction temperature of 160-250DEG C, thus obtaining a product containing tricyclopentadiene at the exit. The preparation method provided by the invention realizes continuous feeding and discharging, improves the product yield and reduces the production cost.

Description

technical field [0001] The invention belongs to the field of organic synthesis, and in particular relates to a continuous preparation method of tricyclopentadiene. Background technique [0002] Liquid jet fuel is the guarantee to provide power for supersonic fighter jets, strategic and tactical missiles, rockets and other aircraft. High-density liquid jet fuel has higher volumetric energy than conventional aviation kerosene, which can provide more propulsion energy for aircraft and significantly improve the performance of aircraft. speed, load and range. Tetrahydrotricyclopentadiene is a high-density hydrocarbon that has been extensively studied and used as a cutting-edge high-performance liquid aviation fuel. Its synthesis process is as follows: using dicyclopentadiene as raw material, through polymerization, hydrogenation, isomerization, It is synthesized by cutting and purifying fractions. Tricyclopentadiene, as a product of thermal polymerization of dicyclopentadiene, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C2/50C07C13/64
CPCC07C2/50C07C13/64
Inventor 张香文邹吉军王庆法肖伟彭浩胡贤贤刘林林崔艳斌裴慧霞崔丽梅
Owner TIANJIN UNIV
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