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Method for preparing cyclopentadiene by thermaldepolymerization of dicyclopentadiene

A technology for producing cyclopentadiene and dicyclopentadiene from dicyclopentadiene, which is applied in the field of organic matter preparation to achieve the effects of increasing CPD yield, reducing energy consumption, and reducing the chance of collision and dimerization

Active Publication Date: 2009-12-30
SHANDONG NHU PHARMA +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method improves the cracking device, but the added preheating and vaporization steps make DCPD partially polymerized or coked before cracking

Method used

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  • Method for preparing cyclopentadiene by thermaldepolymerization of dicyclopentadiene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026]160.5 g of dicyclopentadiene (content 97%) was put into a 250 ml three-neck flask equipped with a thermometer and a stirring rotor. A rectification tower is used to separate the products, the material is stainless steel, and the top of the tower is condensed with ethanol at -10°C. The flask and the bottom of the tower are connected by a volatilization tube, and a micro water pump outlet is located at the bottom of the tower. An oil-water separator is added at the bottom of the tower, and the flask is heated by an electric heating mantle. When the temperature of the kettle is about 170°C, water is sprayed to the bottom of the tower through a micro-water pump. 45°C, the flow rate of the water pump is adjusted according to the value displayed by the thermometer at the bottom of the tower. The temperature at the top of the tower is 41-42°C and remains stable. Receive the distillate, observe the stratification of the oil-water separator, and separate the water layer at regul...

Embodiment 2

[0028] 167.6 g of dicyclopentadiene (content 97%) was put into a 250 ml three-neck flask equipped with a thermometer and a stirring rotor. A rectification tower is used to separate the products, the material is stainless steel, and the top of the tower is condensed with ethanol at -10°C. The flask and the bottom of the tower are connected by a volatilization tube, and a micropump outlet is located at the bottom of the tower. The pump feed tube was inserted into the 99% cyclopentane (boiling point 46°C, temperature 17°C at this time) container. The flask is heated by an electric heating jacket. When the temperature of the kettle is about 170°C, spray cyclopentane liquid to the bottom of the tower through a micro-metering pump. The temperature displayed by the bottom thermometer is always lower than 60°C and higher than 50°C. The flow rate of the metering pump is based on the value displayed by the bottom thermometer. Adjustment. The temperature at the top of the tower is 41-4...

Embodiment 3

[0030] 169.6 g of dicyclopentadiene (content 97%) was put into a 250 ml three-neck flask equipped with a thermometer and a stirring rotor. A rectification tower is used to separate the products, the material is stainless steel, and the top of the tower is condensed with ethanol at -10°C. The flask and the bottom of the tower are connected by a volatilization tube, and a micropump outlet is located at the bottom of the tower. The feed pipe of the pump was inserted into the container of chloroform (boiling point 61° C. under normal pressure). The flask is heated by an electric heating jacket. When the temperature of the kettle is about 170°C, the chloroform liquid is sprayed to the bottom of the tower through a micrometering pump. The temperature displayed by the bottom thermometer is always lower than 60°C and higher than 45°C. The flow rate of the metering pump is based on the value displayed by the bottom thermometer. Adjustment. The temperature at the top of the tower is 4...

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Abstract

The invention discloses a method for preparing cyclopentadiene by decomposing dicyclopentadiene through a liquid-phase depolymerization method. The existing liquid-phase depolymerization method has the defects that the energy consumption is high, the speed is low, the dicyclopentadiene is easy to polymerize into tripolymer or larger polymer when staying at the high temperature for a long time, etc. The method is characterized in that 1) the dicyclopentadiene is taken as raw material and is heated to be 150-240 DEG C in a reactor, so that the dicyclopentadiene is vaporized, and part of the dicyclopentadiene is decomposed to be the cyclopentadiene; 2) a volatilization tube is arranged between the top of the reactor and the bottom of a rectifying tower, the high temperature mixed gas of the dicyclopentadiene and the cyclopentadiene enters into the volatilization tube for reducing the temperature, cooling diluent is injected towards the end of the volatilization tube by the bottom of the rectifying tower, and the gas flow flowing out of the end of the volatilization tube is mixed with the cooling diluent. The method ensures the dicyclopentadiene to be fully depolymerized, reduces the polymerization phenomenon of the cyclopentadiene, improves the production efficiency, reduces the energy consumption of liquid-phase depolymerization, and remarkably increases the yield of the cyclopentadiene.

Description

technical field [0001] The invention relates to a method for preparing organic matter, in particular to a method for decomposing dicyclopentadiene to obtain high-purity cyclopentadiene by using a liquid phase depolymerization method. Background technique [0002] Cyclopentadiene (CPD for short) has a wide range of uses, such as pharmaceutical intermediates, synthetic plastics, resins, pesticides, rubber, etc. Among them, cyclopentene, cyclopentane and their subsequent derivatives are especially popular in the synthesis of pharmaceutical and chemical intermediates. focus on. At present, there are many manufacturers of CPD in China, generally using dicyclopentadiene (DCPD for short) as the raw material, adopting the method of direct heating distillation decomposition (liquid phase depolymerization method) or the method of vaporization high temperature instant depolymerization (gas phase depolymerization method) ) to prepare CPD. [0003] At present, most domestic manufacture...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C13/15C07C4/22
Inventor 季根忠陈江张谦吕文庆梁强盛胡鑫鹦冯仪红
Owner SHANDONG NHU PHARMA
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