Cyclopentaol preparing and refining method

A technology for cyclopentanol and cyclopentene is applied in the field of preparation and purification of cyclopentanol, and can solve the problems of large circulation amount of raw material cyclopentene, low reaction conversion rate and the like

Active Publication Date: 2005-10-05

SINOPEC SHANGHAI PETROCHEMICAL CO LTD

1 Cites 6 Cited by

AI-Extracted Technical Summary

Problems solved by technology

But the deficiency of this method is that the reaction conversion rate is still relat...

Abstract

This invention is cyclopentanol making and refining method, including the procedure: 1) in the existence of catalyst cyclopentene pass hydration reaction in solvent phenylic acid. the mole ratio of cyclopentene and water is 0.8-5.0, reaction temperature 130-180deg.C, reaction pressure 1.0-3.0MPa and reaction time 1-5 hours, the catalyst comprises the main catalyst and activator, the catalyst is strong acid cation exchange resin with sulfo group anchored on the surface, and the activating solvent is trialkylamine. The dosage of catalysts are: cyclopentene/ main catalyst=(10-30)/1; activator/ main catalyst=(0.1-5)/100. The reacted materials cool to house temperature and demix into oil phase and aqueous phase, the oil phase materials through continuous distilling to cut 38-55deg.C cuts to cool and get cyclopentene, and cut 135-165deg.C cuts to cooling collect refined cyclepentanol, the residue is material full of phenylic acid.

Application Domain

Organic compound preparationPreparation by hydroxy group addition

Technology Topic

SolventPhenylic acid +11

Image

Examples

Experimental program(2)

Example

[0022] [Examples 1 to 6]

[0023] The hydration reaction is carried out in a 500ml autoclave, which is equipped with a stirring device and a heating device. Put 30 grams of spherical, strongly acidic cation exchange resin (main catalyst) with sulfonic acid groups anchored on the surface into a hanging basket, and then fix the hanging basket above the stirring blade. Trialkylamine (co-catalyst), cyclopentene, water and solvent phenol are pumped into the kettle with a peristaltic pump according to the required ratio. After replacing the air in the autoclave with nitrogen three times, the pressure was increased to an absolute pressure of 1.0-3.0 MPa with nitrogen. Start the stirring device and heat to increase the temperature, control the reaction temperature to be 130-180°C, and maintain the required reaction time.

[0024] After the reaction is over, cool to room temperature, discharge, and stand for stratification. The oil phase material is heated and distilled under normal pressure, cuts the 38-55°C fraction, condenses and collects unreacted cyclopentene. Cut the fraction at 140-150°C, condense and collect the refined cyclopentanol. The bottom liquid is a material rich in phenol, and the bottom liquid materials, unreacted cyclopentene and water phase materials are returned to the reaction system.

Example

[0025] [Comparative Examples 1~2]

[0026] The co-catalyst trialkylamine and solvent phenol were not added during feeding, and the reaction products were cooled to room temperature and left to stand for separation and then separated by distillation. The rest were the same as in Examples 1-6.

[0027] The reaction conditions not described in the above examples and comparative examples are shown in Table 1, and the reaction results are shown in Table 2. Since the method provided by the present invention is a batch reaction, the conversion rate of cyclopentene in the reaction result is usually higher than the single-pass conversion rate of the continuous reaction. However, it can be seen from the data of the examples and comparative examples that under the same reaction conditions, There is a significant difference in the conversion rate of cyclopentene in the reaction system with or without cocatalyst and solvent phenol.

[0028] Promoter

[0029] Cyclopentene single pass conversion rate

PUM

Description & Claims & Application Information

We can also present the details of the Description, Claims and Application information to help users get a comprehensive understanding of the technical details of the patent, such as background art, summary of invention, brief description of drawings, description of embodiments, and other original content. On the other hand, users can also determine the specific scope of protection of the technology through the list of claims; as well as understand the changes in the life cycle of the technology with the presentation of the patent timeline. Login to view more.