Method of extraction of phenol, pyrocatechin and hydrochinone, mixtures thereof with water and a resinous products

 

(57) Abstract:

Usage: chemical technology of pirotehnika and hydroquinone, phenol extraction and dioxygenases from aqueous solutions. The inventive mixture of phenol, pyrocatechol, hydroquinone and resin with water treated with extractant: simple or complex ether or mixtures thereof, or a higher alcohol, in the presence of the additive salt-bis(5-nitrosulfonic)-methane, taken in an amount of 15 to 50% by weight of a resinous products. Then the aqueous layer was separated, and the organic layer by distillation produce the final products. table 1.

The invention relates to chemical technology and can be used in the production of pyrocatechin and hydroquinone, which are widely used as intermediates for the production of antioxidants, pharmaceuticals, dyes, etc.

A well-known way of separating organic substances and in particular phenol and dioxygenases from their resinous products from aqueous solutions by rectification (1,2).

When you do this consistently distilled water-phenol azeotrope, phenol or water depending on the concentration of the original solution, dioxygenase. The main disadvantage of semi products and low degree of extraction of dioxygenases for preserving transportability bottom mass. In addition, there is a large amount of dilute water-phenol solution, which requires the solution of the question of disposal.

Also known a method of separation of phenols from aqueous solutions by extraction with organic solvents (3). The closest technical solution is a way of separating phenols from their aqueous solutions by extraction of such solvents as high molecular weight alcohols, benzene, coal oil, complex, and ethers, in particular diisopropyl ether and butyl acetate (4).

The advantage of this method is that the process is carried out, usually in mild temperature conditions (t 20-50aboutC). The resin is removed with the aqueous phase, and phenols can be easily separated from the organic solvent by distillation.

With all the advantages of this method, its implementation in some cases may be limited. In particular, an attempt separation of phenol, pyrocatechin and hydroquinone from resin from the aqueous reaction mixture obtained in the hydroxylation of phenol by hydrogen peroxide, by their extraction was Neue the centering and coagulation resinous products.

The aim of the invention is to increase the efficiency of extraction and improvement of the technological process.

This task is solved by the claimed method, including the process of extraction of the aqueous layer with an organic solvent, selected from a number of simple ether, ester, higher alcohol, or their mixture, followed by distillation of the organic layer, the distinctive feature of which is that the extraction in the initial mixture is injected sodium salt dentalinsurance.com formula

in the amount of 15-20 wt.% from the contained resinous impurities.

Sodium salt dentalinsurance - solid crystalline substance, soluble in water and poor in organic solvents. Technical product according to GOST 6848-79, trade name dispersant "NF" represents a 30% aqueous solution or a dry powder with a basic substance content of 52%, which makes it easy to solve the question of its dosage. The product is produced in a large volume and is not a deficiency.

In the process of testing did not identify any characteristics that limit the use of this substance as in the individual form and in the form of technical pneu column with a nozzle in the form of Raschig rings 3x5 mm The height of the column of 3 m, diameter 20 mm

In the original reaction mass obtained in the process of hydroxylation of phenol by hydrogen peroxide in the amount of 400 g is made of 3.4 g of sodium salt dentalinsurance.com at the rate of 30% of the contained resins. The resulting solution was fed to the top of the extraction column. In the bottom of the column serves diisopropyl ether in the amount of 158, the extract Obtained is displayed on top of the column, and an aqueous solution of resinous products below.

The results of this and subsequent experiments were carried out in a similar way as presented in the table. As extractant was used as diisopropyl ether, and other solvents. Aqueous solution and the extractant solvent are fed into the counter top and bottom of the column depending on their density. The component with lower density serves in the bottom of the column. Extract and an aqueous solution of resins derived from opposite sides, and the extract is directed to the selection of target products. Extraction can also be carried out in the three-volume extractor periodic action.

As can be seen from the table, the proposed method allows for the extraction of phenol, pyrocatechin and hydroquinone from their aqueous Rast is edely stated parameters leads to deterioration of these indicators. Thus, a reduction in the content made dentalinsurance.com (see experiments 10 and 11) leads to the partial loss of resinous impurities and reduce the degree of extraction of phenols. The increase in the content dentalinsurance.com leads to his waste.

Thus, implementation of the proposed method provides efficient separation of phenols from resinous products in the process of their extraction from aqueous solutions. However, due to the more progressive the form of commodities produced dibutylethanolamine - disperser "NF" in comparison with the prototype, improves the manufacturability of the process. In addition, the additive dibutylethanolamine is more efficient and can be used in lower concentrations, this product is less scarce.

METHOD of extraction of PHENOL, PYROCATECHIN AND HYDROCHINONE, MIXTURES thereof WITH WATER AND a RESINOUS PRODUCTS, including extraction of the aqueous layer with an organic solvent, selected from a number of simple ether, ester, higher alcohol, or their mixture, followed by distillation of the organic layer, characterized in that the extraction in the initial mixture is injected sodium salt form dentalinsurance.com

 

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