Method of producing para-tert-butylphenol and apparatus for realising said method

FIELD: chemistry.

SUBSTANCE: invention relates to an improved method of producing para-tert-butylphenol by alkylation of phenol with isobutylene on a heterogeneous sulphocationite catalyst, separating the reaction mass containing phenol, para-tert-butylphenol, ortho-tert-butylphenol, 2,4-di-tert-butylphenol and high-boiling impurities by vacuum rectification in two columns with collection of phenol and ortho-tert-butylphenol in distillate form. The reaction mass is subjected to rotory-film evaporation to separate high-boiling impurities therefrom; the commercial product is separated in an additional rectification column in distillate form; absorption trapping of uncondensed para-tert-butylphenol vapour is carried out on a vacuum line; the bottom residue of the commercial product separating column, which contains 2,4-di-tert-butylphenol and para-tert-butylphenol, is recycled to the step for alkylating phenol with isobutylene. The invention also relates to an apparatus for realising the method of producing para-tert-butylphenol.

EFFECT: method enables to obtain a product with high purity and high output.

2 cl, 1 dwg

 

The present group of inventions relates to the field of petrochemical synthesis, in particular, to methods for para-tert-butylphenol high quality.

There are several analogues of the proposed group of inventions, including the methods of extraction of para-tert-butylphenol (hereinafter PTBF). For example, there is a method of allocating PTBF, in which, after carrying out the synthesis in the reactor alkylation of phenol with isobutylene, the reaction mixture consisting of phenol, ortho-tert-butylphenol (hereinafter ATBF), PTBF, 2.4-di-tert-butylphenol (hereinafter 2,4-dabf) and high-boiling impurities (hereinafter IP), separated by vacuum distillation into three columns with the selection in the first column of the phenol, the second remaining phenol and OTBF, and the third product in the form of distillate and the mixture EAP, 2,4-dabf and part PTBF in the form of VAT residue (U.S. patent N 3422157, N. class. 260-624, publ. 14.01.69 year). Purity para-tert-butylphenol obtained in this way, reaches up to 95-99%. The main disadvantage of this method is a significant loss of the target product, as it is lost together with substandard kubovy balance and with pairs that are crystallizing lead to clogging of the vacuum lines, causing a shutdown of the entire plant for cleaning.

A known method for separating para-tert-butylphenol, in which the reaction mass is alkyl which the formation of phenol with isobutylene, consisting of phenol, OTBF, PTBF, 2,4-dabf and high-boiling impurities are cleaned from the last one random evaporation and further divided in two sequential columns, with the release in the first part of phenol, OTBF and PTBF and the second PTBF in the form of distillate and 2,4-dabf in the form of the cubic residue (description to ed. St. USSR N 979319, MKI SS 39/06, SS 37/34, publ. 07.12.82,, bull. No. 45). The disadvantage of this method is that sulfonic acids, found in the EAP, in a single evaporation of the reaction mass under conditions of high temperature and long time act as a catalyst, accelerating the rate of adverse reactions, thereby reducing the quality and yield of marketable product.

The closest analogue to the proposed group of inventions is a method of separation of para-tert-butylphenol from the reaction mixture and the device for its implementation by vacuum distillation in two columns with a selection of phenol and ATBF in both columns in the form of a distillate and a commercial product derived from a cube, the second column, and also at the level of the plates 1-8 of the second column and from shlemovoy line reboiler of the second column (see, for example, the description of the patent RU №2176633, IPC 7/74, SS 39/06, B01D 3/16 published 10.12.2001).

A device for implementing the method comprises a reactor alkalinemanganese with isobutylene in heterogeneous sulfocationites catalyst, equipped with a pipeline of conclusion of the reaction mass, the first and second column vacuum distillation, connected by a pipeline, the second column supply piping side selection vapors PTBF level plates 1-8 casing string and vapor removal PTBF from the slurry line reboiler of the second column (see, for example, the description of the patent RU №2176633, MPK7 SS 37/74, SS 39/06, B01D 3/16 published 10.12.2001).

The disadvantage of such a method and device for its implementation is the selection of the fed to the second column of a mixture of phenol, OTBF, PTBF, 2,4-dabf, EAP, only 5-30 % of the amount of para-tert-butylphenol with a purity of more than 99 % of the mass. The rest of PTBF emit from the cube column. The presence of this product contains 2,4-dabf and VP negative impact on the concentration of the basic substance, its temperature of crystallization and the color, which prevents its use in the pharmaceutical industry, in the production of various polymers and plasticizers. The presence of the EAP also makes it impossible to supply substandard PTBF back on stage alkylation.

The technical result of the proposed method and device for its implementation is expressed in obtaining para-tert-butylphenol high quality with a purity of more than 99 % of the mass and increasing the yield of the target product.

The essence of the method is Holocene para-tert-butylphenol is its implementation by alkylation of phenol with isobutylene in heterogeneous sulfocationites catalyst, separation of the reaction mixture containing phenol, para-tert-butylphenol, ortho-tert-butylphenol, 2,4-di-tert-butylphenol, high-boiling impurities by vacuum distillation in two columns with a selection of phenol and ortho-tert-butylphenol as a distillate, and differs from the closest analogue of the fact that the reaction mass is subjected to a rotary film evaporation to separate from her high-boiling impurities, the selection of products is carried out in the additional distillation column as distillate, vacuum line perform absorption capture neskondensirovannyh vapor para-tert-butylphenol, VAT residue columns selection of products containing 2,4-di-tert-butylphenol and para-tert-butylphenol, recycle on stage alkylation of phenol with isobutylene.

The essence of the device for implementing the method of producing para-tert-butylphenol is that contains the reactor alkylation of phenol with isobutylene in heterogeneous sulfocationites catalyst, supplied by piping the output of the reaction mass, the first and second vacuum columns rectification connected by piping, piping the output of the distillate of the first and second columns are connected to the alkylation reactor, and differs from the closest analogue of the fact that the alkylation reactor piping o Rea the traditional mass is connected with a rotary film evaporator, equipped vessels receiving VAT residue and distillate connected to a rotary film evaporator, additional pipelines, distillate receiver of a rotary film evaporator is connected to an additional pipeline from the absorber, the other pipe is connected to the first distillation column, the second distillation column pipe connected to a third distillation column, the bottom of which is equipped with a pipeline output recirculating flow, connected to the alkylation reactor, and the upper part is equipped with a pipeline output vapor product connected with a reflux condenser, which is connected by piping to the separator, the separator is connected by a pipeline with a capacity of reception of commodity para-tert-butylphenol, and additional pipeline absorber, the bottom of which is connected by a pipeline with a capacity of reception of distillate rotary film evaporator.

The method of obtaining para-tert-butylphenol and device for its implementation is illustrated in the diagram on the drawing.

The proposed method of producing para-tert-butylphenol high quality involves the alkylation of phenol with isobutylene in heterogeneous sulfocationites the catalyst, separating the high-boiling impurities from the reaction mass consisting of f is Nola, para-tert-butylphenol, OTBF, 2,4-di-tert-butylphenol and high-boiling impurities by rotary film evaporation, separation of the reaction mass by vacuum distillation in three columns with the selection in the first column of part of the phenol, the second - phenol and ortho-tert-butylphenol, which recycle the stage alkylation, in the third - para-tert-butylphenol in the form of a distillate and a mixture of 2,4-di-tert-butylphenol and residual para-tert-butylphenol in the form of VAT residue, which is recycled to the stage of alkylation of phenol with isobutylene. To prevent para-tert-butylphenol in the vacuum equipment and the subsequent driving of the equipment during its crystallization in vacuum line perform absorption capture neskondensirovannyh vapor para-tert-butylphenol (see drawing).

A device for implementing this method includes a reactor 1 alkylation of phenol with isobutylene in heterogeneous sulfocationites catalyst, supplied by a pipe 12 of the conclusion of the reaction mass, the first and second column vacuum distillation 5,6 connected by a pipe 24, pipelines 25,26 output recirculating flow of distillate connected to the alkylation reactor 1, and differs from the closest analogue of the fact that the alkylation reactor 1 pipeline 12 conclusion the reaction mass is coupled to a rotary film evaporator 2, equipped vessels receiving VAT residue 3 and 4 distillate connected to a rotary film evaporator 2 extra pipes 13 and 14, the receiver 4 distillate rotary film evaporator 2 is connected to additional tubing 16 with the absorber 10, another pipe 15 is connected to the first distillation column 5, the second distillation column 6 is connected by a pipe 17 with an additional third distillation column 7, the bottom of which is equipped with a pipe 19 o re-circulating flow, connected to the alkylation reactor 1, and the upper part is equipped with a pipeline 18 o vapor product United reflux condenser 8, which is connected by a pipe 20 to the separator 9, the separator is connected by a pipe 22 with a capacity of 11 receiving commodity para-tert-butylphenol, and additional pipeline s absorber 10, the bottom of which is connected by a pipe 23 with a capacity of 4 admission distillate rotary film evaporator (see drawing).

The implementation of the method of producing para-tert-butylphenol is illustrated in the example below using the device for its implementation.

In the alkylation reactor 1 download isobutylene and phenol, return phenol and OTBF pipeline 25 and 26, allocated in rectification columns 5 and 6 in the form of distillate, TRU is aprovado 19 - VAT residue of the distillation column 7. Reaction mass consisting of phenol, PTBF, OTBF, 2,4-dabf and EP in the pipeline 12 is served in the FIR, which separates the EAP from other products. The PG output pipe 13 into the container receiving VAT residue 3 and the distillate EPI - pipeline 14 into the container 4. Using a rotary film evaporation to prevent the EAP on stage vacuum distillation, the presence of which leads to lower quality commodity product, allows to carry out the alkylation reaction with a smaller excess of phenol with respect to isobutylene, because in these conditions, there is a greater output of commodity PTBF than in the nearest analogue, and there is no need to limit the formation of by-product of 2,4-dabf, who returned as recycle to the alkylation reactor 1 (see drawing).

Separating vessel 4 of the reaction mass into two parts, one serves for irrigation absorber 10 through the pipeline 16, and the greater is directed through the pipe 15 to the rectification in three sequential distillation columns 5, 6 and 7. The distillate columns 5,6 consisting of phenol and OTBF, the pipes 25 and 26 serves back to the alkylation reactor. Due to the fact that the VAT residue column 7, which is a mixture of 2,4-dabf and PTBF, does not contain the EAP, it is sent back to the article the Dios alkylation pipeline 19 to increase the yield of the target product. The distillate of the column 7, containing PTBF high quality, condensed in the reflux condenser 8 connected with the column pipe 18, then it is sent through the pipeline 20 to the separator 9, where the separation of the liquid portion and neskondensirovannyh vapors. From the separator by line 22 and the liquid part is served in the capacity of 11 receiving commodity PTBF, and pipeline 21 neskondensirovannyh pair PTBF enter the absorber 10, where they capture. Thereby it is possible to avoid loss of marketable product and to ensure the stable operation of vacuum equipment. Cubic part of the absorber output on line 23 into the container 4 (see drawing).

The proposed group of the invention allows to obtain a marketable product, free of impurities, reducing its main characteristics, such as concentration of the basic substance, the temperature of crystallization and color that can be used in the pharmaceutical industry and the production of various polymers and plasticizers, and to increase the yield of the target product.

1. The method of obtaining para-tert-butylphenol by alkylation of phenol with isobutylene in heterogeneous sulfocationites the catalyst, separation of the reaction mixture containing phenol, para-tert-butylphenol, ortho-tert-butylphenol, 2,4-di-tert-butylphenol, high-boiling impurities by vacuum the rectification in two columns with a selection of phenol and ortho-tert-butylphenol in the form of distillate, characterized in that the reaction mass is subjected to a rotary film evaporation to separate from her high-boiling impurities, the selection of products is carried out in the additional distillation column as distillate, vacuum line perform absorption capture neskondensirovannyh vapor para-tert-butylphenol, VAT residue column selection commercial product containing 2,4-di-tert-butylphenol and para-tert-butylphenol, recycle on stage alkylation of phenol with isobutylene.

2. Apparatus for implementing a method of producing para-tert-butylphenol according to claim 1, containing the reactor alkylation of phenol with isobutylene in heterogeneous sulfocationites catalyst, supplied by piping the output of the reaction mass, the first and second column vacuum distillation, United piping, piping the output of the distillate of the first and second columns are connected to the alkylation reactor, characterized in that the alkylation reactor piping output of the reaction mass is connected with a rotary film evaporator equipped with tanks taking the cubic residue and distillate connected to a rotary film evaporator, additional pipelines, distillate receiver of a rotary film evaporator is connected to an additional pipeline from the absorber, and the other is their pipe is connected to the first distillation column, which is connected by pipeline with the second, the second distillation column pipe connected to a third distillation column, the bottom of which is equipped with a pipeline output recirculating flow, connected to the alkylation reactor, and the upper part is equipped with a pipeline output vapor product connected with a reflux condenser, which is connected by piping to the separator, the separator is connected by a pipeline with a capacity of reception of commodity para-tert-butylphenol, and additional pipeline absorber, the bottom of which is connected by a pipeline with a capacity of reception of distillate rotary film evaporator.



 

Same patents:

FIELD: medicine, pharmaceutics.

SUBSTANCE: present invention refers to a new (-)-stereoisomer of formula (I) wherein X is H, or its pharmaceutically acceptable salt which agonise GABA receptor, to a pharmaceutical composition on the basis of the presented compound, to a method for preparing the (-)-stereoisomer of formula (I) or its pharmaceutically acceptable salt, to a method for inducing or maintaining general anaesthesia, to a method for promoting pain management and to a method for promoting pain management and to a method for prototyping antiemetic activity with the use of the presented (-)-stereoisomer or its pharmaceutically acceptable salt, as well as to a new diastereoisomer (-)-2,6-di-fluoro-butylphenyl ester of carbamic acid of formula (II) wherein R1 represents a chiral amino group, and X is H, or to its pharmaceutically acceptable salt.

EFFECT: preparing the pharmaceutically acceptable salt which agonise GABA receptor.

14 cl, 15 ex, 8 tbl, 3 dwg

FIELD: medicine, pharmaceutics.

SUBSTANCE: present invention refers to a new (-)-stereoisomer of formula (I) wherein X is H, or its pharmaceutically acceptable salt which agonise GABA receptor, to a pharmaceutical composition on the basis of the presented compound, to a method for preparing the (-)-stereoisomer of formula (I) or its pharmaceutically acceptable salt, to a method for inducing or maintaining general anaesthesia, to a method for promoting pain management and to a method for promoting pain management and to a method for prototyping antiemetic activity with the use of the presented (-)-stereoisomer or its pharmaceutically acceptable salt, as well as to a new diastereoisomer (-)-2-fluoro-butyl-6-isopropylphenyl ester of carbamic acid of formula (II) wherein R1 represents a chiral amino group, and X is H.

EFFECT: preparing the pharmaceutically acceptable salt which agonise GABA receptor.

16 cl, 12 ex, 6 tbl, 4 dwg

FIELD: chemistry.

SUBSTANCE: present invention relates to a method for desalination of phenol resin and apparatus to that end. The disclosed method involves mixing starting components - phenol resin, diisopropyl ether, water and concentrated sulphuric acid at temperature 20-60°C, phase separation of the mixture into a top organic layer, which is a mixture of desalinated phenol resin and ether, and a bottom aqueous layer with subsequent removal of the aqueous layer and distillation of ether from the organic layer and obtaining desalinated phenol resin, wherein the obtained ether is fed to the step for mixing components. The starting components are used in the following weight ratio: resin : ether : water : sulphuric acid = 1 : (0.2-0.6) : (0.7-1.0) : (0.007-0.018), wherein mixing is carried out in turbulent conditions.

EFFECT: present invention enables to obtain desalinated resin with high degree of purity while reducing the cost of the process and the obtained product.

13 cl, 24 ex, 6 tbl, 2 dwg

FIELD: chemistry.

SUBSTANCE: said compound is a clear phenol antioxidant from 2,6-di-tert-butyl-phenol through successive aminomethylation, hydrogenolysis and extraction of the desired product. The process is carried out in the presence of 2,6-di-tert-butyl-phenol and 2,4-di-tert-butyl-phenol in amount of 0.015-0.04 wt % and 0.1-0.2 wt % respectively, to the initial 2,6-di-tert-butyl-phenol.

EFFECT: method enables to obtain a compound having guaranteed colour index for a long storage period.

1 tbl, 7 ex

FIELD: chemistry.

SUBSTANCE: invention refers to method of reaction of alkene(s) contained in hydrocarbon stream, and in a reaction-rectifying system provided with rectifying sections and in between reaction zones with subnatant catalyst. The fluid is poured from the top of each overlying zone to the bottom of underlying zone. It is followed with partial disperse passing of vapour flow from underlying zone through each reaction zone. Thus residual vapour flow from each underlying zone is backflow to the top of overlying reaction zone through overflow space to poured fluid. As a rule, higher-boiling reagent is nontertiary alcohol, carboxylic acid or benzene, while essential reaction product is ether, ester or alkylbenzene.

EFFECT: improved method.

7 cl, 3 dwg, 6 ex

FIELD: organic chemistry, chemical technology.

SUBSTANCE: invention relates to a method for preparing hydroxyaromatic compounds by oxidation of aromatic compounds with nitrous oxide in gaseous phase in the presence of zeolites. Method is realized by interaction of aromatic compounds of the formula (I): Ar-Rn wherein Ar means benzene or naphthalene; R means bromine, chlorine, fluorine atom, -NO2, -CN, -NH2, hydroxy-group, alkyl with 1-6 carbon atoms or phenyl; n = 0, 1 or 2 with nitrous oxide in gaseous phase in the presence of zeolites taken among the following order: pentasil, ferrierite and zeolite-β. Zeolite crystallites size is less 100 nm that is calcined before using at temperature from 500°C to 1350°C for 0.5-18 h. Before the calcination process zeolite is modified preferably by precipitation of silane or borane. Method provides realization of the process for a single step with high yield of the end compound and minimal formation of by-side substances.

EFFECT: improved preparing method.

11 cl, 3 tbl, 13 ex

FIELD: organic chemistry, chemical technology.

SUBSTANCE: invention relates to phenolic compounds, derivatives of dialkoxyethanals that are intermediate substances in organic synthesis and can be used as cross-linking agents of phenolic type no evolving formaldehyde also. Phenolic compounds are described of the general formula (I):

wherein: R means (C3-C17)-dialkoxymethyl, 1,3-dioxolan-2-yl substituted possibly at positions 4 and/or 5 with one or some (C1-C8)-alkyls, or 1,3-dioxane-2-yl substituted possibly at positions 4 and/or 5, and/or 6 with one or some (C1-C8)-alkyls; n = 1, 2 or 3, and group or groups of the formula: -CH(OH)-R are at ortho-position and/or at para-position with respect to OH in the cycle group; m = from 0 to 4-n; X means the functional group, such as OH or Hal, or (C1-C8)-alkyl, or (C1-C8)-alkoxyl, or (C5-C12)-aryl comprising in the known cases 1 or 2 heteroatoms, such as nitrogen or oxygen, or carboxy-group, or the group -CO-Y wherein Y means (C1-C8)-alkyl or (C1-C8)-alkoxyl, or amido-group, or amino-group, or thiol-group under condition that at least on of ortho- or para-positions in phenol cycle must be substituted with hydrogen atom, and their salts with alkaline metals, earth-alkaline metals and amines also. Method for preparing indicated phenolic compounds involves interaction of the corresponding substituted phenol wherein at least one ortho- or para-position in phenol cycle must be substituted with hydrogen atom with substituted aldehyde in the presence of a base. Invention provides preparing new compounds that can be used as cross-linking agents no evolving formaldehyde and as intermediate compounds used in organic synthesis.

EFFECT: improved method for preparing.

13 cl, 1 dwg, 10 ex

FIELD: organic chemistry, chemical technology.

SUBSTANCE: invention relates to a method for synthesis of phenols alkylated at ortho-position as parent substances used in preparing organic compounds. Method for preparing o-alkylphenols is carried out by interaction of phenol with alkanol at increased temperature in gaseous phase in the presence of metal oxide as a catalyst. Process is carried out for at least two stages in the molar ratio alkanol : phenol about ≤0.4, preferably, from 0.2 to 0.4 at each stage. Methanol is used as alkanol usually using aluminum gamma-oxide as a catalyst and process is carried out at temperature 300-400°C. Reaction products are separated by distillation. Invention provides increasing yield the end product due to enhancing selectivity with respect to o-alkylphenol.

EFFECT: improved method for preparing.

9 cl, 4 tbl, 2 ex

FIELD: chemical technology.

SUBSTANCE: invention relates to preparing antioxidants of phenolic type. Method involves using alkylation products of mixture of para- and ortho-isomers of isononylphenol with isobutylene as an antioxidant. Alkylation reaction is carried out at 40-120°C and 0.02-0.4 MPa in the presence of acid catalyst in batch and continuous feeding isobutylene to reactor unit providing maintaining isobutylene concentration in reaction mass 0.8 mole/l, not above, and the total amount of isobutylene feeding to alkylation 1.82-2.0 mole per 1 mole parent alkylphenols. Method provides preparing antioxidant showing good technological properties and high effectiveness of protective effect for rubbers of emulsion polymerization and rubbers based on thereof, and simple method for its synthesis also.

EFFECT: improved method for preparing.

6 cl, 3 tbl, 7 ex

The invention relates to a method of selective oxidation of aromatic compounds (e.g. benzene and its derivatives) in gidroksilirovanii aromatic compounds (for example, into the corresponding phenols)

FIELD: chemistry.

SUBSTANCE: invention relates to a method of producing purified hydroquinone and moulding said hydroquinone into flakes from crude hydroquinone essentially containing hydroquinone and small amounts of impurities, including at least resorcinol, pyrogallol and trace amounts of pyrocatechol. The method is characterised by that it involves the following steps: a step for purifying crude hydroquinone by distillation, involving (A) distillation with removal of low-boiling substances from the top part of the column, wherein crude hydroquinone HQ° is fed into the distillation column and wherein resorcinol is removed from the top part of the distillation column, optionally together with all or some of the other light impurities, as a result of which a crude mixture M is extracted from the bottom part of the column, containing hydroquinone and heavy impurities; and (B) distillation with removal of high-boiling substances from the bottom part of the column, wherein the crude mixture M, obtained at step (A), is fed into the distillation column and wherein pyrogallol is removed from the bottom part of the column, optionally together with all or some of the other heavy impurities, as a result of which hydroquinone in purified form (HQ) is extracted from the top part of the column. Further, the method involves a step for moulding the purified hydroquinone obtained from distillation, via deposition thereof in form of a film onto a substrate made from heat-conducting material or coated with heat-conducting material, followed by solidification thereof by bringing the substrate to a suitable temperature, and then extracting the solidified hydroquinone in form of flakes using any suitable means. The time for holding the hydroquinone in the distillation column at step (A) and step (B) is less than one hour. The invention also relates to hydroquinone flakes obtained using the described method and apparatus for realising said method.

EFFECT: use of the present invention enables to avoid problems associated with use of hydroquinone powder.

39 cl, 6 dwg

FIELD: chemistry.

SUBSTANCE: invention relates to a novel form of hydroquinone, characterised by that it has the form of flakes - dense particles, having the shape of plates, characterised by that the flakes have length which varies from 0.5 to 6 cm and width which varies from 0.5 to 3 cm. The invention also relates to use of said flakes as an intermediate product for producing hydroquinone in form of isotropic particles, as well as a method of producing said flakes. The method involves the following steps: if necessary, spraying hydroquinone powder, depositing hydroquinone in liquid state in form of a film onto a substrate made from material or coated with a material which conducts heat, solidifying the hydroquinone by bringing the substrate to a suitable temperature and collecting the solidified product in form of flakes using any suitable means.

EFFECT: use of the novel form of hydroquinone enables to solve dust and cleaning problems arising during production of hydroquinone.

24 cl, 5 ex, 1 tbl, 4 dwg

FIELD: chemistry.

SUBSTANCE: present invention relates to a continuous method of removing methylbenzofuran and hydroxyacetone from a stream of crude phenol containing methylbenzofuran and hydroxyacetone. The method involves passing the stream of crude phenol through at least two successive reactors containing an acidic ion-exchange resin, where temperature in the successive reactors drops in the direction of flow of phenol such that temperature in the first reactor in the direction of flow phenol ranges from 100 to 200°C, and temperature in the next reactor in the direction of flow of phenol ranges from 50 to 90°C, without a step for thermal separation between the two successive reactors. The invention also relates to a method of producing phenol used in said phenol purification method.

EFFECT: group of inventions is an efficient and cheap method of purifying phenol to obtain highly pure phenol.

15 cl, 3 ex, 3 dwg

FIELD: chemistry.

SUBSTANCE: invention relates to a method of purifying crude hydroquinone HQ0, essentially containing hydroquinone and small amounts of impurities, containing both: (i) impurities having a lower evaporation temperature than that of hydroquinone, referred to as light impurities, including resorcinol; and (ii) impurities having a higher evaporation temperature than that of hydroquinone, referred to as heavy impurities, including pyrogallol. Said method is characterised by that is includes the following steps: (A) distillation in the top part of the column, in which the crude hydroquinone HQ0 is injected into a distillation column, having reflux ratio from 300 to 2000, and where the resorcinol is removed in the top part of the column, optionally in conjunction with all or part of the other light impurities, whereby a crude mixture M, containing hydroquinone and heavy impurities, is recovered in the bottom part of the column; and (B) distillation in the bottom part of the column, in which the crude mixture M obtained in step (A) is injected into the distillation column and where pyrogallol is removed in the bottom part of the column, optionally in conjunction with all or part of the other heavy impurities, whereby hydroquinone in purified form (HQ), having impurity content less than 4000 ppm, is recovered in the top part of the column.

EFFECT: invention is a cost-effective method for purifying hydroquinone.

18 cl, 1 ex, 2 dwg

FIELD: chemistry.

SUBSTANCE: invention relates to a method for continuous extraction of phenol from a partial stream formed during production of bisphenol A, where said partial stream contains 40-90 wt % phenol, 5-40 wt % bisphenol A, as well as 5-40 wt % by-products of the reaction of phenol and acetone to bisphenol A, in which a) a partial stream is fed into a vacuum distillation column containing at least 5 theoretical separation steps, b) in the vacuum distillation column phenol is distilled through the head part, c) a first portion of the stream from the base of the column is released from the process, and d) a second portion of the stream from the base of the column is continuously fed into the reactor in which there is isomerisation and splitting of bisphenol A and by-products contained in the stream from the base of the column to form phenol at temperature higher than 190°C and hydrodynamic holding for at least 120 minutes in the presence of an acid catalyst and then returned to the vacuum distillation column. Mass flow of the portion of the stream from the base of the column fed into the reactor is more than 30% of the mass flow of the partial stream at step a) fed into the vacuum distillation column.

EFFECT: method enables efficient processing of streams coming from production of bisphnol A to obtain highly pure phenol with high output.

5 cl, 1 tbl, 7 ex, 1 dwg

FIELD: chemistry.

SUBSTANCE: method involves the following stages: a) reaction of phenol and acetone in the presence of acid catalyst to obtain reaction mix containing bisphenol A. Further, b) water is removed from reaction mix by distillation, with distillation column operated at 100°C to 150°C in the bottom column part and at 20°C to 80°C in the top column part, 50 mbar to 300 mbar absolute pressure in the top column part and 100 mbar to 300 mbar absolute pressure in the bottom column part. Bisphenol A adduct with phenol is removed from reaction mix before distillation at b) stage by crystallisation and filtration.

EFFECT: maximum retention of unreacted residual acetone in reaction solution.

9 cl, 1 ex

FIELD: chemistry.

SUBSTANCE: present invention relates to production of phenol, method of extracting phenol from products of splitting cumene hydroperoxide and to a device for extracting phenol from products of splitting cumene. The method of producing phenol involves the following stages: i) oxidation of cumene, obtaining a reaction mixture containing cumene hydroperoxide and unreacted cumene; ii) splitting products obtained from stage i), obtaining a mixture of splitting products containing at least phenol, acetone, hydroxyacetone, unreacted cumene and water; iii) treatment of the mixture of splitting products obtained on stage ii) through distillation, which involves separation of the mixture of splitting products into at least three fractions using a single fractional distillation stage through: putting the mixture of splitting products into a distillation column, removal of the first fraction, containing acetone, from the upper part of the distillation column, removal of the second fraction, containing phenol, from the lower part of the distillation column, and removal of the third fraction, containing at least unreacted cumene, hydroxyacetone and water, in form of an off-stream. The outlet opening of the off-stream is higher the area for putting in the mixture of splitting products into the distillation column, characterised by removal of heat from the distillation column. The section for removing heat is higher than the outlet opening of the off-stream of the third fraction.

EFFECT: increased energy efficiency of methods using old technology, while maintaining quality standards and total output of end products.

25 cl, 6 dwg, 1 ex

FIELD: organic chemistry, chemical technology.

SUBSTANCE: invention relates to technology for producing phenol and acetone by cumene method, in particular, to a stage for separating cleavage products of alkylaryl hydroperoxide. Method involves separating a mixture of cleavage products for at least three fractions in a single distillation step by charging the mixture of cleavage products into lateral section of fractionating column, removal the first ketone-containing fraction through the upper part of fractionating column, removal of the second fraction containing substituted or unsubstituted phenol through the bottom part of column, and removal of the third fraction containing unreacted mono-, di- and/or trialkyl-substituted benzene and hydroxyketone as a side flow. The side outlet channel of the flow is located above the site for charging the mixture of cleavage products in fractionating column. The first fraction contains at least 75 wt.-% of ketone containing in the cleavage product before carrying out the distillation stage. Invention provides improvement of economy indices of the process due to reducing material and energetic consumptions and enhancing purity degree of final products.

EFFECT: improved method for treatment.

21 cl, 2 dwg

The invention relates to petrochemistry and can be used in the production of phenol and acetone Kukolnik method
The invention relates to a method for producing light-colored bisphenol a with slight residual content of oxygen and phenol

FIELD: process engineering.

SUBSTANCE: invention relates to mass-and-heat exchange hardware, particularly, to rectifiers and absorbers and may be used in petrochemical and chemical, oil and gas industries. Proposed rectifier tower comprises body with process unions, trays with vapor and overflow branch pipes, and height-adjustable bubble-cap trays. Horizontal edges of cap cutouts are equipped with vanes arranged radially outside in horizontal plane.

EFFECT: higher efficiency of mass exchange.

3 dwg

Up!