A method of obtaining a lower mono - and dialkylphenols

 

(57) Abstract:

Use: production of lower mono - and dialkylphenols. The inventive method of obtaining lower mono - and dialkylphenols (DUB) involves feeding benzene and lower olefin in the alkylation plant, equipped with a reactor unit for the interaction of benzene with a lower olefin in the presence of a catalyst complex on the basis of anhydrous aluminium chloride, a node separation of the catalyst complex from the alkylate, a node of a multi-stage rectification with the last stages of selection return benzene, lower alkyl benzene, the lower the DUB, partially refundable in the alkylation reactor, and partly allocated to the installation, and polyalkylbenzenes (PUB), while the lowest DUB before drainage installation is subjected to a clear rectification in three distillation columns, in the first of which emit light fraction stream which is returned to the node in the multi-stage distillation and reactor block, in the second column provide a complete separation of the light fraction, the flow of which return to the node in the multi-stage distillation and reactor unit, in the third column of the cubic product of the second column separates the lowest DUB from the PUB, which returns tdelay by rectification from the pitched product and return in the reactor block alkylation. 1 table, 1 Il.

The invention relates to the production technology of lower mono - and dialkylphenols and can be used in petrochemical plants.

A method of obtaining lower alkyl benzenes (AB) by the alkylation of benzene lower olefins in the presence of a catalyst complex on the basis of anhydrous aluminium chloride, in accordance with which the alkylate washed with water, neutralized and subjected to multi-stage distillation with the release of the reversionary benzene, lower alkyl benzenes and polyalkylbenzenes. The latter is mixed with fresh original benzene (mass ratio of benzene and polyalkylbenzenes 1:(0,41-0,72) and subjected to azeotropic dehydration. Drained the original benzene and polyalkylbenzene served on alkylation. This method makes it possible to obtain the lowest monoalkylbenzenes (selectivity 93,3-93,5 ), but lower dialkylphenol (DUB) it does not produce (1).

For the production of DUB (diethylbenzene) ethylbenzene subjected to disproportionation at elevated temperature in the presence of a catalyst complex on the basis of anhydrous aluminium chloride. The process is carried in the ideal mode of displacement when the concentration of the catalyst komata rectification allocate commodity diethylbenzene, meet quality brand AND (TU-6-030387-75), and side pitched a product used as a component of fuel oil (2).

Thus, for the production of AB and DUB, you must have two separate installations. At the same time, capital operating and other costs are significantly lower when combining on a single installation of production AB and DUB.

Also known industrial method of obtaining lower AB and DAB on a single installation, which consists in the following. Benzene and lower olefin is fed to the alkylation plant, equipped with a reactor unit for the interaction of benzene with a lower olefin in the presence of a catalyst complex on the basis of anhydrous aluminium chloride, a node separation of the catalyst complex from the alkylate, a node of a multi-stage rectification with the last stages of selection return benzene, lower alkyl benzene, lower dialkylphenol partially returned to the alkylation reactor, and partly allocated to the installation, and polyalkylbenzenes. Exhaust with installation flow DUB (mix diethylbenzene) are used as high-octane additives to motor fuels (gasoline) (3).

The disadvantages of this method is nevitta monomer, used in the synthesis ionoobmennyh resins). On the other hand, the drainage installation raw DUB and the PUB does not allow you to use contained polyalkylbenzene as the return of the commodity component, which leads to unnecessarily high unit costs source of ethylene and benzene (flow source, referred to the unit of product).

Thus, a review of the prior art shows the need for developing a method of obtaining a lower mono - and dialkylphenols, allowing installation with one reactor alkylation-parallelomania to get lower mono - and dialkylphenols, suitable for the production of monomers with lowest specific costs source of ethylene and benzene.

In accordance with the invention features a method of obtaining a lower mono - and dialkylphenols, including the filing of benzene and lower olefin in the alkylation plant, equipped with a reactor unit for the interaction of benzene with a lower olefin in the presence of a catalyst complex on the basis of anhydrous aluminium chloride, a node separation of the catalyst complex from the alkylate, a node of a multi-stage rectification with the last stages of selection return benzene, lower alkyl is, and polyalkylbenzenes; lower dialkylphenol before drainage installation is subjected to a clear rectification in three distillation columns, the first of which emit light fraction stream which returns the node multistage distillation and reactor block, in the second column provide a complete separation of the light fraction, the flow of which is returned to the reactor unit, in the third column of the cubic product of the second column separates the lower dialkylphenol from polyalkylbenzenes faction, which in return node multistage rectification on stage allocation polyalkylbenzene fraction in the reactor block.

The expression "reaction block" in this description means the ability to use a single reactor or in multiple reactors that perform the same function, but this expression expansion cannot be interpreted: installation containing multifunctional reactors, such as reactor alkylation and disproportionation reactor of this invention do not have a relationship.

The invention is illustrated in the figure "schematic diagram of obtaining mono - and dulcibella".

On tropopause composition, wt. Al C1327; C6H633; monoalkylphenol 18; polyalkylbenzene 22. The catalyst complex is prepared in a separate apparatus (not shown in the figure, because the catalyst complex and a method of its preparation are not the object of the present invention). The catalyst complex can be fed continuously or intermittently, as known from the prior art) is preferable. The catalyst complex is prepared by any well-known from the prior art method.

Line 2 on the installation serves the original benzene, line 3 of the lower olefin (ethylene or propylene). In practice it is possible to use pure olefins or hydrocarbon fraction containing, for example ethane-ethylene or propane-propylene fraction. On line 4 by alkylation return serves raw DUB, and on line 5 return benzene. All of these flows in the alkylation reactor 6. (The installation may contain one or more alkylation reactors, as noted above). The alkylation reactor may be any of those known in the prior art. In particular, it is possible to use the reactor column type, known from (3) or any other reactor for liquid-phase alkylation of benzene nlnoy capacity of about 30 tons From the top of the column 19 assign boiling impurities that on line 20 back to the alkylation reactor, and the other part (from 1 to 99.) in the distillation column 13. When receiving mono - and diethylbenzene in the upper part of the column 19 maintain a temperature of about 153oAnd at the bottom about 190oC. Extending from the lower part of the distillation column product line 2 serves in a distillation column 22, the separation capacity of about 50 tons In the upper part of the column 22 maintain a temperature of about 180oWith, and in the lower 200o(When receiving mono - and diethylbenzene). In the column 22 is a comprehensive removal of low-boiling products. Suitable rectification of the conditions under which loss of distillate DUB together with low-boiling products is minimal, for which the distillation should be carried out at reflux of the order of 10-20. The distillation column 22 through line 23 is mixed with the distillate of the column 19 and returned to the alkylation reactor and distillation column 13, line 31. CBM product of the column 22 through line 24 serves in a distillation column 25, the separation capacity of about 30 tons, operated at reflux numbers from 1.5 to 5. As distillate from the top of the column through line 20 assign DUB, the quality of the receiving mono - and diethylbenzene keep the temperature at the top and at the bottom of the column 183 and 193oS, respectively. As the cubic product from the bottom of the column through line 27 to divert the flow of high-boiling impurities (PUB and resin). Part of this flow on the return line 28 to column 16, and the other part on line 29 back to the alkylation reactor 6. The relationship between these flows is in the range from 2:1 to 1:95. The specific value of this ratio is determined depending on how much catalyst poisons contained in the product stream 27. With the increasing content of catalytic poisons in the product stream 27 should be an increase in flow directed to the column 13. On the contrary, when the decrease of catalytic poisons in the product stream 27 should be an increase in flow directed into the reactor 6. Column 19, 22, 25, it is advisable to operate at a pressure close to atmospheric. In the case of using propylene as the starting olefin is advisable to maintain the temperature of the top and bottom of the columns 19, 22, 25: 165/195oWITH, 180/205oWITH, 193/205oS, respectively. The catalyst complex is selected in the node 8 may be fully or partially returned to the reactor 6 through line 30, indicated in the figure by the dotted line.

Expert it is clear that the figure shows the principal is as columns, pumps, intermediate capacity, automation and control, etc., not shown.

Examples 1 and 2. Industrial plant collected under the scheme in accordance with the figure, conduct pilot runs with the aim of obtaining the ethyl - and diethylbenzene (example 1), and isopropyl - and diisopropylbenzene (example 2).

The process conditions described above in the description of process flow diagram, consumption of basic raw material and product flows in the table.

In accordance with example 1 are as ethylbenzene, meets the requirements of the production of styrene, diethylbenzene, which fully complies with the receipt of ion-exchange resins, and stream PUB+resin (POS. 17), which can be used as raw material for the production of surface-active substances (surfactants) or component fuel stove.

In accordance with example 2, get isopropylbenzene, meets the requirements of the synthesis of phenol, acetone and/or alpha-methylstyrene, diisopropylbenzene that meets the requirements of obtaining ion-exchange resins, and stream PUB+resin (POS. 17), which can be used as Sinie new technical result, specified in the preamble of the description of the present invention. These examples illustrate some possible embodiments of the invention, but not limit its scope defined by the patent claims.

A method of obtaining a lower mono - and dialkylphenols, including the filing of benzene and lower olefin in the alkylation plant, equipped with a reactor unit for the interaction of benzene with a lower olefin in the presence of a catalyst complex on the basis of anhydrous aluminium chloride, a node separation of the catalyst complex from the alkylate, a node of a multi-stage rectification with the last stages of selection return benzene, lower alibendol, lower dialkylphenol partially returned in the reactor block, and partially withdrawn from the installation, and polyalkylbenzenes, characterized in that the lower dialkyl before drainage installation is subjected to a clear rectification in three distillation columns, in the first of which emit light fraction stream which is returned to the node in the multi-stage distillation and reactor block, in the second column provide a complete separation of the light fraction, the flow of which return to the node in the multi-stage distillation and reactor bknai faction, you return to the site multistage rectification on stage allocation polyalkylbenzene fraction in the reactor block.

 

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