RU131378U1 - INSTALLING THE TREATMENT OF BUTYL ALCOHOL - Google Patents

Abstract

An apparatus for producing tertiary butyl alcohol by a liquid-phase reaction of an isobutylene-containing hydrocarbon mixture with water at an elevated temperature in the presence of tertiary butyl alcohol as a solvent, including a 4-shelf reactor filled with a sulfation-cation catalyst and a rectification unit of the resulting reaction mixture, characterized in that the installation consists of three reactors of which two parallel 4-shelf reactors with the same amount of sulfocationion catalyst loaded into them, and a separate 4-section reactor from them with the same loading of the same sulfocationite catalyst in sections, into which the reaction mixture from the previous two 4-shelf reactors flows in a common stream.

Description

This utility model relates to devices used in the field of petrochemistry, in particular, to the location and interconnection of devices for the synthesis of tertiary butyl alcohol (TBS), which is used as an intermediate in organic synthesis, for example, to produce isobutylene and isoprene used in the production of butyl rubber and isoprene rubber.

A known method of producing TBS by the liquid-phase reaction of isobutylene in the form of an isobutylene-containing hydrocarbon fraction with water at a temperature of 80-90 ° C with a countercurrent flow of feeds of the initial reagents into a column reactor filled with a sulfocationic catalyst. Water and the isobutylene-containing fraction is supplied at a volume ratio of (7-10): 1, which corresponds to a molar ratio of water: isobutylene (80-110): 1. The resulting TBS is removed from the reactor as part of two reaction streams, which are a dilute solution of TBS in hydrocarbons and a dilute solution of TBS in water. The performance of the process is 100 g of isobutylene per 1 liter of catalyst per hour. From the obtained TBS solutions are isolated by distillation [S.Yu. Pavlov. Isolation and purification of monomers for synthetic rubber, L., "Chemistry", 1987, S. 133-136].

The disadvantage of this method is the low rate of hydration reaction due to the mutual insolubility of the starting reagents, as well as the complexity of the technology and the increased energy costs associated with the allocation of TBS from two diluted solutions.

A known method of producing TBS by the liquid-phase reaction of isobutylene in the form of an isobutylene-containing hydrocarbon fraction with water at a temperature of 70-110 ° C with a direct-flow feed of a stream of starting reagents into a vertical reactor filled with a sulfocationic catalyst. Water and isobutylene are supplied at a molar ratio of (5-20): 1. To increase the mutual solubility of the reagents, the hydration reaction is carried out in the presence of a homogenizer - a polar solvent of ethyl cellosolve in an amount of 10-70% wt. to water and a nonionic emulsifier. The productivity of the isobutylene process is 150-170 g / l · h. TBS is isolated by distillation from the obtained reaction mixture [SU 512622, published 1/30/1983].

The disadvantage of this method is the formation of undesirable by-products from the solvent with the participation of TBS, the complexity of the technology and increased energy costs associated with the allocation of TBS from a dilute mixture with water and ethyl cellosolve.

A known method of producing TBS by a liquid-phase reaction of isobutylene or an isobutylene-containing hydrocarbon mixture with water at a temperature of 30-110 ° C, preferably 50-90 ° C, with a direct-flow feed of the starting reagents into a reactor filled with a sulfocationite catalyst. Preferably, 2-5 series reactors are used. Reactors with a fixed catalyst bed are used with uniform loading of the amount of catalyst in each reactor / bed. To increase the mutual solubility of the reactants, the hydration reaction is carried out in the presence of TBS as a solvent in an amount of 21.6-78% wt. in the reaction zone. The productivity of the isobutylene process is 160-200 g / l · h. From the obtained reaction mixture, TBS is isolated by distillation [US 4307257, published 22.12.1981].

The disadvantage of this method is the conversion of about 1% of isobutylene into by-products - isobutylene dimers and oligomers, which complicate the isolation of TBS and impair its quality. The activity of the catalyst in the process decreases, the productivity of isobutylene below 130 g / l · h after 6-8 thousand hours operation process. After this period, the entire catalyst is discharged from the reactor and replaced with a fresh batch, which complicates the technology and increases production costs.

Closest to the claimed is a known method for producing TBS by reaction from an isobutylene or isobutylene-containing hydrocarbon mixture with water using a reactor filled with four or five catalyst beds, in which the amount of catalyst is increased from layer to layer in the direction of feed of the starting reagents. As a catalyst, cation-exchange resins in the H-form are used, including macroporous sulfocationionites (KU-23, Duolite C26, Amberlyst 15, Lewatit K2629, Dowex 50, Purolite CT275 and others). The hydration reaction is carried out at a temperature of 50-100 ° C and a pressure of 14-25 at. in the presence of tertiary butyl alcohol as a solvent. TBS is isolated from the resulting reaction mixture by distillation. [RU 2453526, published 11/10/2011 prototype]. The conversion of isobutylene in the process is 82.0-88.2%, the yield of isobutylene dimers is 0.25-0.35%. Within 12-14 thousand hours continuous operation process indicators do not change.

In order to further reduce the yield of by-products while maintaining the performance of the process for the production of TBS, a facility is proposed that consists of three reactors, of which two parallel 4-shelf reactors with the same amount of sulfocationion catalyst loaded in them, and a 4-section reactor separately from them with the same loading of the same sulfocationite catalyst in sections, into which the reaction mixture from the previous two 4-shelf reactors flows in a common stream.

Installation works as follows.

To obtain the required amount of TBS, an isobutylene-containing fraction is fed to 4-shelf reactors with the same amount of sulfocationion catalyst loaded into them. In this case, the combined stream from the first two parallel reactors of TBS synthesis enters the third reactor of TBS synthesis.

From the latter along the reactor, the resulting reaction mixture is fed to distillation to recover unconverted hydrocarbons.

A significant distinguishing feature of the proposed installation from the prototype is that the synthesis of TBS is carried out in three reactors, of which two parallel four-shelf reactors with the same amount of sulfocationic catalyst loaded in them, and four separate section reactors separate from them with the same load of the same sulfocationic the catalyst in sections, into which the reaction mixture from the previous two four shelf reactors flows in a common stream.

The process at the proposed facility for the synthesis of TBS allows you to carry out the process with higher selectivity, the yield of isobutylene dimers from 0.18 to 0.25%. The selectivity of the installation for 14 thousand hours of continuous operation is not reduced.

Claims (1)

An apparatus for producing tertiary butyl alcohol by a liquid-phase reaction of an isobutylene-containing hydrocarbon mixture with water at an elevated temperature in the presence of tertiary butyl alcohol as a solvent, including a 4-shelf reactor filled with a sulfation-cation catalyst and a rectification unit of the resulting reaction mixture, characterized in that the installation consists of three reactors of which two parallel 4-shelf reactors with the same amount of sulfocationion catalyst loaded into them, and a separate 4-section reactor from them with the same loading of the same sulfocationite catalyst in sections, into which the reaction mixture from the previous two 4-shelf reactors flows in a common stream.