Method of extraction of phenol from phenol resin production of phenol and acetone kukolnik method

 

(57) Abstract:

Usage: in a co-production of phenol and acetone, extraction of phenol from a phenol resin. The inventive resin twice treated with 3 - 5 wt.% an aqueous solution of ammonia in water at a mass ratio of resin solution 1:(1.5 to 4) and mixing. The aqueous layer was separated from the organic layer and vyderjivat at boiling point for 2 - 4 hours eye-Catching when heated, ammonia is directed to the saturation of the source of ammonia solution, comprising 50 to 95 wt.%, recirculating in the system of the aqueous layer from the extraction step of the phenol with the addition of fresh water to 100 %. The resulting phenol is extracted from aqueous solution with an organic solvent, separated the layers and regenerate the extractant by distillation of the organic layer. table 1.

The invention relates to petrochemical technology, namely the production of phenol and acetone Kukolnik method.

In the process of producing phenol and acetone from cumene (IPA) form high-boiling by-products, generally referred to as phenolic resin. The composition of the phenolic resin includes a large number of components: phenol, acetophenone, dimethylphenylcarbinol (DMPC), Dimov>2SO4. Phenolic resin has the following average composition, wt. phenol 10,11; acetophenone 16,35; DMPC 8,23; dimers --methylstyrene 31,99; cumylphenol 24,13); the amount of unidentified 8,11; salt 1,08.

To date phenolic resin is not found qualified in full and mostly burned as boiler fuel. However, in connection with the aggravation of the environmental situation in some regions of the country using phenolic resin as a boiler fuel is difficult, and, as a consequence, the waste does not find sales. Difficulty burning phenolic resin to a large extent due to the presence of phenol. In addition, in accordance with THE 38.10286-87 phenolic resin contains up to 8 wt. phenol, resulting in losses of phenol and accordingly to an increase in specific consumption of IPA. Deeper depletion of phenol from phenol resin by using the rectification is not possible to obtain sufficiently pure phenol. Thus, removing the phenol from the phenol resin is a major technical challenge.

There is a method of phenol recovery of light oil fractions of the products of the destructive distillation of coal extraction with an aqueous solution of methanol or water (method Metasolv). The number n is the atur 160aboutWith the pressure of 20 ATM and in addition, the inability of the phenol recovery of high purity.

A known way of separating phenols from organic mixtures by sequential treatment with solutions of alkali, and then the acid, followed by separation of phenols by settling. Among the disadvantages of this method are mainly the large number of chemically contaminated wastewater, corrosion of equipment, and so on isolation of pure phenol from phenol resin rectification method (with a relatively small content of phenol compared with acetophenone) is hampered by the presence of an azeotrope with a maximum boiling point in the system phenol-acetophenone.

A known method of separation of phenols, in particular of parameningeal of phenolic resin by treating it with an aqueous solution of alkali with further processing of the aqueous layer with a solution of a strong mineral acid to neutral reaction and separation layers (prototype). Among the disadvantages of this method include the presence of a large number of chemically contaminated wastewater, corrosion of equipment, etc.

The aim of the invention is the extraction of pure phenol, getting obstinately phenolic resin, liquidizer> The proposed method for the processing of phenolic resins involves reacting a phenolic resin with an aqueous solution of ammonia with the formation of phenolate ammonium allocation of phenol by thermal decomposition of phenolate, extraction of phenol from aqueous solution and subsequent separation of the phenol from the extractant.

The first stage of the process is carried out by treating phenol resin 2-5% aqueous solution of ammonia. The resulting ammonium phenolate transferred to the aqueous phase. Treated in this way from phenol, phenol resin may be further directed to the isolation of pure acetophenone or catalytic decomposition or burning.

In the second stage of the process the resulting phenolate ammonium undergoes thermal decomposition. The resulting ammonia is sent to recycling, and an aqueous solution of phenol is sent to the extraction carried out in the usual way. As extractant can be used ethers, hydrocarbons, etc. After extraction 50-95% aqueous solution saturated with ammonia and sent to recycling in contact with the resin.

A distinctive feature of the proposed method is that as the alkaline agent is ammonia when aspect] is at ammonium and recycling 50-95% water after extraction of the phenol to the machining stage phenolic resin.

In the implementation of the proposed method use aqueous ammonia with a concentration of 2-5% Decrease in ammonia concentrations below 2% leads to the increase of the reaction volume, and the increase in concentrations above 5% worsens partition between aqueous and organic phases. When increasing the recycling of water in excess of 95% reduces the degree of extraction of salts of the phenolic resin. At lower recycle less than 50% increases the amount of water involved in the process.

The advantages of the proposed method achieved by differences from known, are as follows:

the proposed method requires virtually no consumption of reagents (the minimum flow is determined only by technological losses);

in the process, carried out according to the proposed method reduced the amount of wastewater;

due to the lack of acid, corrosion of equipment is insignificant.

P R I m e R 1. 30 g of phenolic resin is mixed with 3% aqueous ammonia solution at a mass ratio of 1 to 1.5, respectively. The mixture is stirred for 60 minutes After the 45-minute sedimentation separating the oil layer from the aqueous layer, containing the ammonium phenolate and salt. The oil layer obtained after extraction smachivaetsya above. After separating the oil layer from the water of the latter is connected to the first water layer. The resulting oil layer is again mixed with 3% aqueous ammonia solution at a mass ratio of 1 to 1.5, respectively. Next, repeat all the operations described above. The aqueous layer was combined with the aqueous layer obtained after a 2-h extraction. The combined aqueous layers boiled for 4 h for the destruction of the ammonium phenolate on phenol and ammonia. Released gaseous ammonia is used to prepare a 3% ammonia solution.

The cooled aqueous solution containing phenol and salt, mixed with diethyl ether in a volume ratio of 1 to 1.5, respectively, stirred for 30 minutes After settling the mixture to separate the aqueous layer from the organic containing phenol. The aqueous layer was further used for preparation of solution of ammonia. The ether is distilled off from phenol, which is then purified in a known manner.

The obtained data on the excretion of phenol in the table.

P R I m m e R 2. 30 g of phenolic resin is mixed with 3% aqueous ammonia solution, prepared with water that contains 95% recycled and 5% fresh water, at mass ratio of 1 to 4, respectively. Then hold SS="ptx2">

P R I m e R 3. 30 g of phenolic resin is mixed with a 5% aqueous solution of ammonia, prepared with water containing 50% recycled and 50% fresh water, in a mass ratio of 1 to 3, respectively. Further, the experience carried out as described in example 1.

The obtained data on the excretion of phenol in the table.

P R I m e R 4. 30 g of phenolic resin is mixed with 3% aqueous ammonia solution, prepared with water that contains 95% recycled and 5% fresh water, at mass ratio of 1 to 4, respectively. Stir the mixture for 30 minutes Then the experience carried out as described in example 1, the difference lies in the fact that the water layer to decompose the ammonium phenolate boiled for 2 h and extraction of phenol from aqueous layer is carried out at a volume ratio of water and ether 1 1, respectively, the mixture mix 20 minutes

The obtained data on the excretion of phenol in the table.

METHOD of extraction of PHENOL FROM PHENOL RESIN PRODUCTION of PHENOL AND ACETONE KUKOLNIK METHOD of treatment of the resin with an aqueous solution of the base with obtaining phenoxide salt dissolved in the water layer, with subsequent decomposition of the salt to none and starting with the release of phenol extraction of dissolved organic is mesheanii and the mass ratio of resin: the solution equal to 1:(1,5-4,0), after which the resulting aqueous layer was separated and kept at boiling temperature for 2-4 h, and released when gaseous ammonia is directed to the preparation of the source of ammonia solution comprising 50-95 wt. recirculating system water layer from the stage of extraction of phenol from aqueous solution and fresh water to 100%

 

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13 cl, 4 ex

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25 cl, 1 dwg, 2 ex

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2 ex, 1 tbl

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10 cl, 4 ex

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13 cl, 2 tbl, 2 ex

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5 cl, 3 dwg, 6 tbl, 4 ex

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11 cl, 1 dwg, 9 ex

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5 cl, 4 ex, 8 tbl

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3 cl, 1 dwg, 1 tbl

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9 cl, 1 ex, 1 dwg, 1 tbl

FIELD: chemical industry; methods of production of the phenols by the catalytic decomposition of the cumene hydroperoxide into phenol and acetone.

SUBSTANCE: the invention is pertaining to production of phenols by the catalytic decomposition of the cumene hydroperoxide into phenol and acetone. The method provides for oxidization of the cumene into the cumene hydroperoxide, catalyzed by the acid decomposition of the cumene hydroperoxide, neutralization of the produced product of the decomposition, maintaining the product in the homogeneous phase before neutralization, which is conducted by means of the aqueous base. The phenol is separated by fractionation of the neutralized product. The aqueous base represents the water solution of the sodium hydroxide or phenoxide. In particular use the regenerated phenoxide, at least, on one phase of the treatment at production of the phenol. It is preferential to add the sodium hydroxide water solution to the reaction product in such a concentration and such amount, that to receive the concentration of sodium phenolate in the homogeneous phase from 0.2 up to 2.5 mass %. The temperature of the homogeneous phase after the add-on of the aqueous base is set within the range of 20°С-150°С, the preferable temperature is within the range of 60°С-120°С. It is preferential, that the reaction product is saturated with the oxygen-containing gas. The technical result of the invention is the decreased quantity of the undesirable impurities in the products of the acid decomposition of the cumene hydroperoxide.

EFFECT: the invention ensures the decreased quantity of the undesirable impurities in the products of the acid decomposition of the cumene hydroperoxide.

13 cl, 4 ex

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SUBSTANCE: invention relates to a method for purifying phenolic flow prepared after distillation of raw acetone in separating decomposition products of cumene hydroperoxide from hydroxyacetone by rectification method. For removal of hydroxyacetone from phenolic flow methods of azeotropic-extractive rectification is used with using a combined separating agent wherein hydrocarbon (cumene and/or α-methylstyrene) is used as one components, and water is used as another component. Method involves feeding a separating agent in common with feeding a column, maintaining the mass ratio of hydrocarbon and water that equal or above the mass ratio of concentrations of hydrocarbon and water in the corresponding azeotropic mixtures, removing hydroxyacetone from column with distillate aqueous flow and feeding organic phase to phlegm wherein this organic phase is depleted with hydroxyacetone. Use of this method provides enhancing selectivity and complete distillation of hydroxyacetone.

EFFECT: improved purifying method.

17 cl, 2 dwg, 13 ex

FIELD: chemistry.

SUBSTANCE: invention relates to the method of obtaining phenol and acetone by acid-catalysable decomposition of hydro-peroxide of cumene in the environment of the reaction products at elevated temperatures in one stage. In this case the process is carried out in the presence of a catalyst, prepared immediately before its introduction into the reactor for the decomposition of hydro-peroxide of cumene by mixing sulfuric acid with phenol at the ratio of from 2:1 till 1:1000 and the waiting time from mixing till putting into the reactor for the decomposition of hydro-peroxide of cumene from 1 to 600 minutes at a temperature from 20 to 80°C. As a rule, sulfuric acid has a concentration of higher than 75% or oleum is used.

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2 cl, 4 tbl, 4 ex

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