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Continuous cyclopentylmethyl ether production process and production system

A technology of cyclopentyl methyl ether and production method, which is applied in the directions of ether preparation, organic chemistry, preparation of ether by addition of unsaturated compounds, etc., can solve the problem of low degree of continuity of cyclopentyl methyl ether production equipment and the like

Active Publication Date: 2016-04-13
ZHEJIANG ALPHARM CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The invention solves the technical problem that the continuous degree of the existing cyclopentyl methyl ether production device is not high, and the purpose is to improve the conversion rate of materials and improve production efficiency

Method used

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  • Continuous cyclopentylmethyl ether production process and production system
  • Continuous cyclopentylmethyl ether production process and production system
  • Continuous cyclopentylmethyl ether production process and production system

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0073] The above system is used for continuous production, the pressure of the vaporized CPE flowing through the adsorption column is 2MPa, 100°C; the particle diameter of amberlyst15 filled in the fixed bed reactor is 1.2-1.8mm; the particle diameter of amberlyst-35 is 0.5-1.2 mm; the specific surface area of ​​amberlyst15 is 30-40m 2 / g, the average pore diameter is 30-40nm, and the total heat exchange capacity is 4.8-5.3eq / L-R. The molar ratio of cyclopentene to methanol is 1.6:1, the temperature of the fixed bed reactor is 100-105°C, and the liquid hourly space velocity is 0.35hr - 1 , the gas hourly space velocity is 110hr -1 ; The pressure is 0.1Mpa. After the continuous production is finished, the conversion rate of methanol is 96%, and the GC purity of the product in the reaction solution is greater than 90% (the purity of the GC area normalization method; sampling every 30min); the purity of the cyclopentyl methyl ether prepared by refining is greater than 99.5%, ...

Embodiment 2

[0075] The above system is used for continuous production, the pressure of the vaporized CPE flowing through the adsorption column is 2MPa, 100°C; the particle diameter of amberlyst15 filled in the fixed bed reactor is 1.2-1.5mm; the particle diameter of amberlyst-35 is 0.5-0.8 mm, the specific surface area of ​​amberlyst15 is 30-40m 2 / g, the average pore diameter is 30-40nm, and the total heat exchange capacity is 4.8-5.3eq / L-R. The molar ratio of cyclopentene to methanol is 1.6:1, the temperature of the fixed bed reactor is 100-105°C, and the liquid hourly space velocity is 0.35hr - 1 , the gas hourly space velocity is 116hr -1 ; The pressure is 0.12Mpa. After the continuous production is finished, the conversion rate of methanol is 97%, and the GC purity of the product in the reaction solution is greater than 93% (the purity of the GC area normalization method; sampling every 30min); the purity of the cyclopentyl methyl ether prepared by refining is greater than 99.5%, ...

Embodiment 3

[0081] Compared with Example 1, the difference is that the vaporized CPE flows through the adsorption column at a pressure of 5 MPa and 90°C. After the continuous production is finished, the conversion rate of methanol is 95%, and the GC purity of the product in the reaction solution is greater than 90% (the purity of the GC area normalization method; sampling every 30min); the purity of the cyclopentyl methyl ether prepared by refining is greater than 99.5%, The overall yield of cyclopentyl methyl ether is greater than 88%.

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Abstract

The present invention discloses a continuous cyclopentylmethyl ether production process and production system, the production process comprises vaporization of cyclopentene, filteration through an adsorption column, mixing with methanol and vaporization in a raw material vaporizer, catalytic addition reaction of the cyclopentene by entering a fixed bed reactor, distillation of the reaction solution by a light component removal tower, recovery and reuse of CPE and the methanol from light components, and rectification of a light component removal tower kettle liquid by a CPME rectification device to obtain cyclopentylmethyl ether, wherein the temperature of the catalytic addition reaction is 100-105 DEG C, the liquid hourly space velocity is 0.35-0.55hr<-1>, the gas hourly space velocity is 110-125hr<-1>, the pressure is 0.1-0.12Mpa. The conversion rate of the methanol is greater than 95%, the gas chromatography (GC) purity of a product in the reaction solution is greater than 90%, the purity of the cyclopentylmethyl ether prepared by refining is greater than 99.5% (the purity is detected by GC area normalization method), and the total yield of the cyclopentylmethyl ether is more than 80%.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a continuous production system and synthesis method of cyclopentyl methyl ether. Background technique [0002] Cyclopentyl methyl ether is a new type of environmentally friendly high-performance hydrophobic ether solvent, referred to as CPME, developed by a Japanese company and launched in October 2006. It is a new type of environmentally friendly high-performance hydrophobic ether solvent, which can replace tetrahydrofuran, formazan Ether solvents such as tetrahydrofuran, methyl tert-butyl ether and dioxane. As a reaction solvent, it can be used in reactions such as Grignard reaction, coupling reaction, coupling amination reaction, metal reduction reaction, Lewis acid reaction and Friedel-Crafts reaction. It is also used in extraction, crystallization, surface treatment and polymerization processes. [0003] There are many methods for synthesizing cyclopentyl methyl ...

Claims

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Application Information

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IPC IPC(8): C07C41/06C07C43/184
CPCC07C41/06C07C43/184
Inventor 翁高翔沈纪达张俊
Owner ZHEJIANG ALPHARM CHEM TECH
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