Method of extraction of phenol and acetophenone from the high-boiling bottoms production of phenol method kukolnik

 

(57) Abstract:

Usage: the technology of production of phenol and acetone Kukolnik method, the selection of acetophenone from the bottoms of the distillation of the reaction products. The inventive source rectification distillation residues containing phenol, acetophenone, cumylphenol, diameter = methylstyrene and the high-boiling residue fed to the first distillation column for separation of phenol from which the concentrated distillation residues with significantly reduced phenol content is served to the second distillation column concentration bottoms. The stream enriched compounds boiling between the boiling point of phenol and balance, in particular cumylphenol, is removed from the second column from a point below the point of supply and return at least part of the specified thread in the first column at a point above the point of supply. The upper shoulder straps from the first distillation column containing at least 95 wt.% phenol, and enriched with acetophenone top shoulder straps from the second column, containing not less than 70 wt.% of acetophenone, subjected to repeated distillation for separation of phenol and acetophenone. 1 S. and 4 C.p. f-crystals, 2 ill., table 2.

The invention relates to SP ptx2">

The phenol obtained acid-catalyzed decomposition of gidroperekisi cumene, traditionally cleaned through a series of distillations in which all of the heavier components of the mixture decomposition are separated as the upper shoulder strap.

The product of decomposition usually neutralized in an alkaline ion exchanger before cracking products of phenol and acetone, by-products and unreacted cumene for recycle.

Decaying material sequentially divided into acetone, cumene, methylsterol (AMC), phenol and high-boiling residues. Phenol, acetone and AMS are also treated in the final products. Selected cumene is washed with caustic to correct its acidity before a repeat cycle for oxidation. Separation of raw decaying mass is the number of columns of fractional distillation of industrial manufacturing.

Purification of phenol is performed in vacuum distillation columns, usually equipped with 30 - 40 vapor-liquid counterflow contact plates or mass transfer indurated layers of equivalent height.

A significant amount of phenol stay with high-boiling at the bottom of the final column distillation, in which OpenAL in the upper chase usually more than 15% of the phenol remains as residue such the rectification column of phenol in parallel with heavy impurities, such as acetophenone, cumylphenol, the dimer - methylstyrene (AMS-dimers) and other high boiling (the residue). Although an attempt is made to allocate more phenol residue subsequent columns, although of lower quality in order to reduce the amount of phenol lost with high boiling in a VAT residue columns, the phenol is at least 5% of the total number of the high-boiling residue. He usually burned with regenerierung only heat.

In addition, the upper shoulder straps so the remainder of the subsequent columns mainly phenol contain too much of acetophenone to be acceptable as a product, so they are recyclorama flow in the method for reprocessing.

U.S. patent N 4.415.409 (Zukewich and others) consider the method of extractive distillation of phenol and acetophenone using cumylphenol as the extraction solvent. However, this patent does not consider and does not offer the combination of distillation stages and additional advantages of the method claimed here.

In the method of separation of phenol, obtained by the decomposition of gidroperekisi cumene from the high-boiling impurities, the improvement includes:

a) feeding phenol distillation distillation is stillation column A selection phenol;

b) feeding the concentrated still bottoms with a significantly reduced content of phenol from A column into a second distillation column B concentration residue;

c) removing a stream rich in compounds boiling between the boiling point of phenol and balance, in particular cumylphenol from the specified column B from a point below the point of feed and return at least part of the specified stream in A given column at a point above the point of feed;

d) regeneration of the upper straps of the columns of A, containing at least 95 wt. % phenol; and

(e) regeneration enriched with acetophenone upper straps from column B that contains at least 75 wt.% of acetophenone.

In Fig. 1 presents a diagram similar, representing a comparative example 1; Fig.2 - scheme of the method according to the invention shown in example 2.

Developed improvement, by means of which an additional amount of phenol with good purity can be extracted from conventional phenol distillation bottoms; acetophenone can be selected in a relatively concentrated form, which is of industrial importance, enriched cumylphenol thread can be dedicated to regenerating cumylphenol, and the amount of phenol, Ter the remnants of the phenol distillation column, containing recycled amount of phenol, acetophenone and cumylphenol with AMS-dimers and high-boiling residue, served by line 4 into an intermediate point of the distillation column A phenol recovery of continuous operation. Column A preferably is 15 to 30 plates and operates at a ratio of reflux distilled from 1.5 : 1 to 2.5 : 1 and reduced pressure, preferably below 50 mm RT.art., measured at the top with minimized thermal decomposition. As is known in the technique, referred to here plates can be replaced gasket. Column A is in condition for receiving the concentrated still bottoms with a significantly reduced content of phenol.

Concentrated distillation residues from the column with A significantly reduced content of phenol is served by line 6 at an intermediate point of the second distillation column concentration of residue of continuous action B. Column B is preferably 10 to 20 plates and operates at a ratio of reflux distilled and reduced pressure, the same as for column A.

The stream enriched compounds boiling between the boiling point of phenol and residue removed from column B, line 7 below the supply line 6 and is returned to the column A at the point it is pure phenolic distillate. In particular, the acetophenone is present in much lower concentrations. The upper straps of the columns of A contain at least 95 wt.% phenol, preferably at least 99 wt.% of phenol. Part of the flow, the output on line 7 can be withdrawn through line 8 and may be further purified for the regeneration of cumylphenol. Alternative part of the output line 8, can be burned for heat recovery. The upper shoulder straps that are output from the column B, line 9, consists predominantly of acetophenone, for example, not less than 70%, and industrial significance. Distillation residues from the column B, the output line 10, can be incinerated with heat recovery. The implementation of this method, there is a significant reduction in the number of phenol, lose the rest.

Example 1 (comparative). Distillation residues of phenol distillation column having the composition 1', presented in table.1, served by line I to the II-th plate 20 is a plate distillation column continuous action C, operating at a pressure of 35 mm RT.article and the ratio of distillation 3 (Fig.1). The flows of the upper shoulder straps and bottoms are displayed on lines 3 and 2, having a composition of 8' and 9', respectively. As you can see from the table.1, the phenol in the upper shoulder straps contains about XI part 1' (PL.2), the same as being submitted in comparative example 1, is supplied via line 4 at 12 plate 20 is a plate distillation column continuous action A, operating at a pressure of 35 mm RT.article and distillation ratio of 2 (Fig.2). Distillation residues from the column output line 6, have the composition 4' and is served by line 6 on the 10-th plate 15 is a plate column B. the Flow part 2' enriched compounds boiling between the boiling point of phenol and the balance, shown on line 7 with the 5-th column plate B and is returned on the 15th plate column A, line 7. The result of adding the upper shoulder straps from the column A, the output on lines 5, are much more pure phenolic distillate - (3', PL. 2). In particular, the acetophenone is present in much lower concentrations (0,5% compared to 18.5%). Part thread part 2' is shown on line 8 (part 7', PL.2) and may be further purified, if required, for the regeneration of cumylphenol. Alternative part of the output line 8, can be burned for heat recovery. The upper shoulder straps that are output from the column B, line 9, have the structure 5 and consists predominantly of acetophenone. Distillation residues from the column B, the output line 10, have the 6' and may the example 1 (0,2 versus 3.9 parts).

The examples are for purposes of illustration, and the method of the invention can be performed in conditions similar to but not identical to the conditions specified in example 2. For example, the number of plates in the column may be different, the point of feeding and excretion can be changed under the condition that the line 7 is always fed at a higher plate than line 4 column A, line 7 always comes from the column B is lower than the line 6 is in column B.

The amount of material withdrawn from column B, line 7, may vary between 100 and 200% of the amount applied to the column A. the Total number of cumylphenol supplied to the column A, line 7, should be not less than 4 times greater than the total number of acetophenone supplied in column A.

1. Method of extraction of phenol and acetophenone from the high-boiling bottoms production of phenol Kukolnik method containing phenol, acetophenone, cumylphenol, dimers of alpha-methylstyrene and high-boiling impurities by fractional distillation in distillation columns continuous operating at reduced pressure and the supply of high-boiling aromatic hydrocarbon to the top of the column, characterized in that the raw material is sent to the first distillation column, utrirovanny VAT residue with a lower content of phenol, which is sent to the second distillation column, from the top of which is distilled enriched with acetophenone fraction containing at least 75 wt.% of acetophenone, and also from the intermediate section of the second column from a point below the point of supply, placing a side stream enriched compounds boiling between the boiling point of phenol and distillation residue, in particular enriched cumylphenol, and a side stream is used as supplied in the column aromatic hydrocarbon, for which part of the flow back into the first column at a point above the point of input power in the first column.

2. The method according to p. 1, characterized in that the remaining part of the side stream from the second column, enriched compounds boiling between the boiling point of phenol and distillation residue, in particular enriched cumylphenol, is removed from the system.

3. The method according to p. 2, characterized in that the second column select side stream that contains at least 60 wt.% cumylphenol.

4. The method according to PP.1 and 2, characterized in that the first column serves cumylphenol, total weight of which at least 4 times the total weight of acetophenone, the entries in the first column.


 

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