Method for purifying recycle alcohol solvent of olefin epoxidation process and olefin epoxidation method

A technology for epoxidation reaction and alcohol recovery, which is applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of reducing equipment investment and operating costs, large volume of hydrogenation reaction devices, and high operating costs. Achieve the effects of reducing equipment investment and operating costs, good hydrogenation effect, and increasing hydrogenation reaction rate

Active Publication Date: 2015-09-23
HUNAN CHANGLING PETROCHEM SCI & TECH DEV CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to overcome the recovery of alcohol solvents in the existing olefin epoxidation reaction process, when the catalytic hydrogenation process is used for purification, circulating hydrogen and its corresponding circulation system are required, so that the volume of the hydrogenation reaction device is relatively large, and the equipment investment is relatively large. For the technical problems of high operating cost and low space velocity, a method for purifying the recovered alcohol solvent is provided. This method uses a small amount of hydrogen and does not need to circulate hydrogen, thereby omitting the need for a hydrogen circulation system and simplifying the hydrogenation reaction device. , reducing equipment investment and operating costs, and being able to operate at higher airspeeds

Method used

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  • Method for purifying recycle alcohol solvent of olefin epoxidation process and olefin epoxidation method
  • Method for purifying recycle alcohol solvent of olefin epoxidation process and olefin epoxidation method
  • Method for purifying recycle alcohol solvent of olefin epoxidation process and olefin epoxidation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0081] (1) Install 50g of titanium-silicon catalyst TS-1 in the constant temperature reaction zone of the fixed-bed tubular reactor. The catalyst is equipped with ceramic ring packing on the upper and lower sides, and the airtightness of the entire reaction system is kept intact. The propylene and liquid streams enter the reaction zone in an upflow manner to carry out the epoxidation reaction to obtain an epoxidation reaction mixture. Wherein, in the liquid stream, the molar ratio of methanol:propylene:hydrogen peroxide is 6:2:1, ammonia water is added into the liquid stream, so that the pH of the liquid stream is 5.3. Control the reaction temperature to 40°C, the reaction pressure to 2.5MPa, and the liquid hourly space velocity to 1.5h -1 .

[0082] (2) The epoxidation reaction mixture obtained in step (1) is subjected to rectification under the condition of a pressure of 0.15 MPa to separate the propylene oxide and obtain recovered alcohol solvent at the same time.

[0083...

Embodiment 2

[0098] (1) The same method as in Example 1 was used to carry out the epoxidation reaction.

[0099] (2) The recovered alcohol solvent was obtained by the same method as in Example 1.

[0100] (3) Inject hydrogen gas into the recovered alcohol solvent obtained in step (2) by the same method as in Example 1, except that the temperature in the liquid channel is 150° C. and the pressure is 1.5 MPa. The amount of hydrogen injected into the recovered alcohol solvent was 1.0 times the saturated amount of hydrogen dissolved in the recovered alcohol solvent (0.05 g / 100 g at 150° C. and 1.5 MPa).

[0101] The obtained hydrogen-containing circulating alcohol solvent is sent into a tubular reactor for hydrotreating, wherein the difference between hydrotreating and Example 1 is:

[0102] Al 2 o 3 As a carrier, Co is used as an active component, and Ti is used as an auxiliary agent, wherein, based on the total amount of the catalyst and in terms of elements, the content of Co is 5% by we...

Embodiment 3

[0106] (1) The same method as in Example 1 was used to carry out the epoxidation reaction.

[0107] (2) The recovered alcohol solvent was obtained by the same method as in Example 1.

[0108] (3) Inject hydrogen gas into the recovered alcohol solvent obtained in step (2) using the same method as in Example 1, except that the temperature in the liquid channel is 140°C and the pressure is 3.5MPa. The amount of hydrogen gas injected into the recovered alcohol solvent was 1.0 times the saturated dissolved amount of hydrogen gas in the recovered alcohol solvent (0.07 g / 100 g at 140° C. and 3.5 MPa).

[0109] The obtained hydrogen-containing circulating alcohol solvent is sent into a tubular reactor for hydrogenation, wherein the difference between the hydrogenation and Example 1 is that the catalyst with catalytic hydrogenation is made of SiO 2As a carrier, Ni is used as an active component, and Ti is used as an auxiliary agent, wherein, based on the total amount of the catalyst a...

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Abstract

The present invention provides a method for purifying a recycle alcohol solvent of olefin epoxidation process, and the method is as follows: hydrogen is sent into the recycle alcohol solvent by holes with the average pore size in nanoscale to obtain a hydrogen-containing recycle alcohol solvent; and the hydrogen-containing recycle alcohol solvent is sent into a tubular fixed bed reactor in the upward flowing manner for contact with a catalytic hydrogenation catalyst under the condition of liquid phase hydrogenation processing. The present invention also provides an olefin epoxidation method using the method for purifying. The method for purifying can effectively reduce the dosage of hydrogen without maintaining of recycle hydrogen in the reactor, the demand for a hydrogen recycle device is eliminated, the hydrogenation reaction process is simplified, the equipment investment and operation cost can be greatly reduced, and the operation can be performed under high space velocity. By adoption of the method for purifying of the recycle alcohol solvent, the method has good hydrogenation effect on a variety of impurities in the recycle alcohol solvent, and a high purity recycle alcohol solvent can be obtained.

Description

technical field [0001] The present invention relates to a method for purifying recovered alcohol solvent from an olefin epoxidation reaction process, and also relates to a method for olefin epoxidation. Background technique [0002] With the development of petrochemical and fine chemical industry, oxygen-containing organic compounds have become very important intermediates. Using hydrogen peroxide as oxidant, low-carbon alcohol as solvent, and titanium-silicon molecular sieve as catalyst to catalyze the epoxidation of olefins to prepare oxygen-containing organic compounds meet the requirements of green chemistry and atomic economy development concepts, and are a very promising prospect. Green new technology. In this process, the solvent is generally recycled. [0003] However, the olefin epoxidation process not only produces impurities such as carbonyl compounds, acetal (ketone) compounds, and nitrogen-containing compounds in the reaction and separation stages, but also pr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C29/90C07C31/04C07D301/12C07D303/04
Inventor 李华佘喜春王伟李庆华易娇
Owner HUNAN CHANGLING PETROCHEM SCI & TECH DEV CO LTD
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