Method of separation of cyclohexanone from reaction mixture of water - acetonitrile - cyclohexene - cyclohexanone

FIELD: chemistry.

SUBSTANCE: method involves the preparation of cyclohexanone by cyclohexene oxidation, the isolation of cyclohexanone from a mixture of water-acetonitrile-cyclohexene-cyclohexanone of any composition by combining in the process scheme an autoclaving rectification with a medium-volatile separation agent acetonitrile and three-phase delamination in a Florentine vessel followed by feeding each layer to the rectification columns. The process scheme preferably comprises four distillation columns and a Florentine vessel.

EFFECT: separation of a reaction mixture of any composition into practically pure components that meet the quality requirements of marketable products.

2 cl, 2 dwg, 4 ex



Same patents:

FIELD: chemistry.

SUBSTANCE: invention relates to a method of hydrogenating phenol on a palladium catalyst (0.5 wt % Pd on super-crosslinked polystyrene) in excess hydrogen with molar ratio of hydrogen to phenol of 4-5:1 at atmospheric pressure. The method includes diluting the catalyst with an inert diluent (ceramic spheres with diameter of 1-2 mm) and the process is carried out in the temperature range of 120-220C with volume rate of feeding the raw material of 0.4-2.0 h-1. The method enables to obtain cyclohexanone with selectivity of 87.1-100% with phenol conversion of 84.0-99.8%.

EFFECT: improved method.

1 ex

FIELD: chemistry.

SUBSTANCE: invention relates to a method of dehydration of cyclohexanol into cyclohexanone. The claimed method of dehydration of cyclohexanol into cyclohexanone is realised in a gas phase at an increased temperature in the presence of a catalyst, which contains active components, consisting for 5688 wt % of zinc oxide and for 8.039.0 wt % of calcium carbonate. The applied catalyst is used in the form of a catalytic system with alternation in the gas course of three layers of different height, filled with different ratio of the catalyst and ceramics. The first, protective-distributing, layer consists of ceramics 1020 cm high. The second layer of the main reaction ignition zone consists of the catalyst and ceramics in a ratio of 1:1 with the layer as high as a diameter of a flue duct of smoke gases. The third layer of the main reaction zone consists of the catalyst and ceramics in a ratio of 3:1 with the layer height, equal to the height of the apparatus before the first input of the flue duct.

EFFECT: claimed method makes it possible to avoid an undesirable course of side reactions, prevent the catalyst coking and increase its service term.

3 cl, 1 tbl, 5 ex

FIELD: chemistry.

SUBSTANCE: described is a method of purification of cyclohexanone, obtained by oxidation of cyclohexane with air oxygen or dehydrogenation of cyclohexanol, in which the process of rectification is performed in a split vacuum rectification column (2 columns), where distillate of the first column feeds the second column; from the bottom of the first column a mixture of cyclohexanol and highly boiling admixtures is removed for further separation, and the bottom of the second column is a condensate for the first, an alkali (KOH) solution in cyclohexanol, equivalent to the content of ethers, is introduced into it.

EFFECT: obtaining highly pure cyclohexanone.

1 dwg, 2 tbl, 1 ex

FIELD: chemistry.

SUBSTANCE: invention relates to method of obtaining methyl ether of (3aR, 4S, 7aR)-4-hydroxy-4-m-tolylethynyloctahydroindole-1-carboxylic acid of formula (I), with application of novel intermediate compounds of formulas (II) and (III).

EFFECT: improvement of method.

10 cl, 30 ex

FIELD: power industry.

SUBSTANCE: cyclohexane oxidation reactor includes device for supply and distribution of air or inert medium - nitrogen with supply channels and transverse partition walls with openings. Partition walls cover the whole reactor cross section without a gap, and openings have any shape and location, but mutual arrangement of air or nitrogen supply and distribution devices with supply channels and openings in transverse partition walls is such that in emergency conditions, when nitrogen is supplied via the channels, there created by means of nitrogen jets distributed in reaction volume are gas partitions conditionally closing the openings, which together with transverse partition walls provide quasi-stationary separation of reaction volume into compartments.

EFFECT: proposed reactor design implements the main principle of fire and explosion safety by means of quasi-stationary separation of inner reactor volume with fire and explosion hazardous product by means of inert medium (nitrogen) jets into smaller volumes - compartments.

4 cl, 5 dwg

FIELD: process engineering.

SUBSTANCE: proposed installation comprises, at least, two reactors equipped with, at least, one bypass tube connected with union of discharge from the first or previous reactor to second or next reactor from internal: wall cavity or tank secured to down-take pipe. Note here that internal wall cavity or tank is used as intermediate collector for heat-control additional feed of mix of volume equal to that of mix maximum portion added simultaneously into second and next reactor for heat control. Besides, every bypass tube incorporates flow rate control valve.

EFFECT: higher safety, reduced metal input.

4 cl, 3 dwg

FIELD: chemistry.

SUBSTANCE: present invention relates to a method of producing cyclohexanone and cyclohexanol, as well as an apparatus for realising said method. The disclosed method involves processing a reaction liquid containing cyclohexane, cyclohexanone, cyclohexanol, cyclohexyl hydroperoxide and organic acids from a cyclohexane oxidation step, and involving cooling the reaction liquid, neutralisation thereof with an alkali, separation into a first aqueous-alkaline layer and a first organic layer, decomposition of the cyclohexyl hydroperoxide in the presence of a catalyst and an alkali, and separation of a second aqueous-alkaline layer, return thereof into the cyclohexyl hydroperoxide decomposition unit and for neutralisation, and separation of a second organic layer for distillation of cyclohexane with extraction of cyclohexanone and cyclohexanol and returning cyclohexane to its oxidation step. After cooling, the reaction liquid is washed from organic acids by feeding water into its stream followed by separation of the aqueous-acidic layer and cleaning thereof via extraction with cyclohexane and returning the extract into the stream of the reaction liquid, and distillation of the raffinate with separation of the aqueous-acidic runoff and distillate which is fed into the stream of the reaction liquid, and the prepared organic layer is fed to the neutralisation step in form of a mixture of the washed reaction liquid and extract containing cyclohexyl hydroperoxide.

EFFECT: invention enables to obtain the end products using a simple and cheap method.

8 cl, 1 ex, 2 dwg

FIELD: process engineering.

SUBSTANCE: invention relates to catalyst for dehydration of cyclohexanol to cyclohexane and to method of its production. Proposed catalyst comprises the following components in wt %: calcium carbonate - 16.4-37.0, graphite - 1.0-3.0, and zinc oxide making the rest. Proposed method comprises preparing reaction mix of previously mentioned composition containing sources of zinc oxide and calcium carbonate, moulding, drying, and calcinating. Note here that said mix comprises the following components in wt %: calcium carbonate - 12.4-29.8, carboxymethylcellulose or methylcellulose - 0.1-1.0, and base zinc carbonate making the rest, while graphite is added into amounts sufficient for production of said catalyst.

EFFECT: higher strength, lower costs, simplified production, reduced harmful effects.

3 cl, 2 tbl, 2 ex

FIELD: chemistry.

SUBSTANCE: method involves a step for oxidising cyclohexane to obtain cyclohexyl hydroperoxide, a step for catalytic decomposition of cyclohexyl hydroperoxide on a heterogeneous catalyst to obtain a mixture of cyclohexanol and cyclohexanone and a step for distilling cyclohexane, carried out at high temperature and pressure. Said steps form a single circulation loop in which the reaction mixture is circulated through transfer of cyclohexane vapour from the boiler of the distillation apparatus into an oxidation reactor, as well as due to subsequent spontaneous overflow under gravitational forces of the liquid reaction mixture from the oxidation reactor to a decomposition reactor and then into the boiler of the distillation apparatus. The cyclohexane oxidation reactor lies over the cyclohexyl hydroperoxide decomposition reactor which is on the same level as or below the level of the boiler of the distillation apparatus. Conversion of cyclohexane in the oxidation zone is not more than 1.0 mol % and conversion of cyclohexyl hydroperoxide in the decomposition zone is not less than 90.0 mol %.

EFFECT: high selectivity of the cyclohexane oxidation process.

8 cl, 1 tbl, 1 dwg, 15 ex

FIELD: chemistry.

SUBSTANCE: invention relates to a method of preparing a mixture of cyclohexanol and cyclohexanone which are intermediate products in production of polyamides nylon-6 and nylon-6.6. The method is realised at high temperature and high pressure and involves the following successive cycles: oxidation of cyclohexane - decomposition of cyclohexylhydroperoxide, wherein oxidation of cyclohexane and decomposition of cyclohexylhydroperoxide are carried out in separate series-connected reactors without intermediate separation of the aqueous phase, whereby in each separate cycle, cyclohexane is oxidised with air or an oxygen-containing gas in liquid phase in the absence of a catalyst until conversion of cyclohexane of not more than 1.5 mol %, and the cyclohexylhydroperoxide formed during oxidation of cyclohexane is decomposed on a heterogeneous catalyst in a separate reactor until conversion of not less than 90 mol %.

EFFECT: method increases overall selectivity of converting cyclohexane to cyclohexanone and cyclohexanol and also considerably reduces formation of by-products.

9 cl, 19 ex, 2 tbl, 1 dwg

FIELD: chemistry.

SUBSTANCE: claimed invention relates to a method of obtaining saturated aliphatic ketone, represented by the general formula (2), (where n stands for an integer number from 1 to 3; R represents a hydroxyl group, a cyclohexyl group, an alkyl group, which has from 1 to 4 carbon atoms, or an acyl group, which has from 1 to 4 carbon atoms), applied as an initial material for the production of medications, agrochemical preparations, optic functional materials and functional materials for electronics. The method consists in hydrogenation of a nucleus of an aromatic ketone, represented by the general formula (1), (where n stands for an integer number from 1 to 3; R represents a hydroxyl group, a phenyl group, an alkyl group, which has from 1 to 4 carbon atoms, or an acyl group, which has from 1 to 4 carbon atoms), with hydrogen under pressure in the presence of a solvent at a temperature from 20 to 120C and in the presence of a catalyst, which carries from 0.1 to 20 wt % of the ruthenium atom on a carrier.

EFFECT: method makes it possible to obtain the target product with high selectivity.

6 cl, 24 ex

FIELD: chemistry.

SUBSTANCE: invention concerns method of cyclic alkane oxidation by oxidation agent for obtaining a product, where oxidation is performed in cracking fractionator including vat zone at bottom end, head zone at top end, and reaction zone between vat and head zones. Reaction mix is kept boiling in reaction zone, and oxidation agent is added into reaction zone in at least two split flows. Non-reacted raw material leaving reaction zone is recycled into reaction zone. Gas containing molecular oxygen is used as oxidation agent, and reaction mix containing target product is collected below reaction zone.

EFFECT: simple and cost-effective method of obtaining the product, enhanced conversion of source material and selectivity of target product generation.

6 cl, 1 dwg, 3 ex

FIELD: industrial organic synthesis.

SUBSTANCE: invention relates to production of cyclohexanol or cyclohexanone via hydrogenation of phenol or benzene with hydrogen in presence of catalyst and diluent followed by hydration in case of using benzene as starting material. Process is characterized by that hydrogen and benzene or hydrogen and phenol preheated in heat exchanger, provided with condensate intake control circuit, and circulation gas are supplied to vaporizer and preheater, provided with heating steam consumption control circuits, through supply lines provided with shutoff valves. Phenol or benzene and circulation gas, as well as heating steam and condensate consumptions are specified and adjusted. Preheated mix is then fed into separator to separate gas from liquid phase, which is removed, while remaining gas mixture is sent to hydrogenation reactors comprising temperature control zones and heat-extracting tube-type condensers and provided with phenol or benzene, hydrogen and condensate control circuits, temperature sensors connected to controllers to adjust consumptions of phenol or benzene, hydrogen and condensate, and wherein diluent volume level compared to that of catalyst is controlled and hydration temperature is measured. Resulting product enters cooler and then separation column provided with cyclohexanol or cyclohexanone recovery level control and adjusting, wherefrom it is directed to gas circulation line comprising cooler, separator, and compressor equipped with pipelines with circulation gas consumption control circuits.

EFFECT: increased productivity with regard to cyclohexanol or cyclohexanone.

2 dwg

The invention relates to an improved method of decomposition of the hydroperoxide with the formation of a mixture containing the corresponding alcohol and ketone, comprising the stage of: a) adding water in the amount of 0.5-20% in the mixture containing the hydroperoxide; (b) the deletion of specified volume of water in such a way that together with water removes water-soluble impurities; C) removing the remaining water in such a way that the reaction mixture is not more than 2% of water; and (d) decomposition of the specified hydroperoxide by contacting the reaction mixture with a catalytic amount of a heterogeneous catalyst containing gold, supported on a carrier

FIELD: chemistry.

SUBSTANCE: invention relates to a method of conducting a process of absorbing a volatile substance, which is water, ammonia or carbon dioxide, from a gas phase with a liquid absorbent which contains an ionic liquid and a wetting additive, by bringing the gas phase into contact with a film of the absorbent. The wetting additive is selected from a group comprising nonionic surfactants, amphoteric surfactants and cationic surfactants. The invention also relates to an absorption refrigerating machine, having an absorber, a desorber, an evaporator, a condenser and a working body made from an absorbent and a volatile substance, wherein the absorber has a device for bringing the gas phase containing the volatile substance into contact with the absorbent film. The invention also relates to use a mixture of an absorbent containing a wetting additive and an ionic liquid, and a volatile substance as a working body in an absorption refrigerating machine.

EFFECT: method speeds up mass transfer and increases stability thereof over time during absorption, and also enables continuous absorption in small-size equipment.

14 cl, 2 tbl, 8 ex

FIELD: process engineering.

SUBSTANCE: this invention relates to semi-continuous deodorant for refining of food fats and/or oils. Proposed semi-continuous deodorant comprises at least one desorption section and differs in that said section includes buffer feed tray 1 for collection of fats and/or oils, means 2 for control of fat or oil flows from said tray 1, means 3 for distribution of said flows over structured packing 4 to make said flows get in contact with desorption agent in countercurrent and intake tray 5 for collection of fat and/or oil flows from structured packing 4. Deodorant includes one or more internal channels or one or more external channels, or combination thereof for desorption agent and volatile substances. Note here that said channels can collect desorption agent flows from one or more trays and are communicated with inlet of gas for desorption sections for reuse of desorption agent in countercurrent. Invention covers also the method of refining of fats and/or oils including the stage whereat the flow of fats and/or oils in fed in semi-continuous deodorant. Proposed method incorporates the stages whereat: i) fats and/or oils are collected at aforesaid buffer feed tray 1 in desorption section, ii) means 2 for control of fat or oil flows from said tray 1 controls said flows, iii) said flow is distributed over structured packing (4) for intensification of surface contact with desorption agent in countercurrent conditions, iv) flows of fats and/or oils from structured packing 4 is collected in intake tray 5 before discharge from desorption section for further treatment including contacts with desorption agent to be preferably collected for reuse in desorption section. Besides, it covers the method of intensification of contact between desorption agent and product in above described semi-continuous deodorant. Note that said method comprises the stages whereat the flows of desorption gas or desorption vapor are collected from one or more trays or sections via internal or external channels 9, 10 to direct collected one-shot flows of desorption agent via feed channel 11 in one or more desorption sections to bring said collected one-shot flows of desorption agent in contact with product flow in countercurrent before discharge of used flows of desorption agent for additional treatment. Besides, it covers the application of above described semi-continuous deodorant for refining of food fats and/or oils, for example, palm oil, vegetable oil and peanut oil, particularly, those containing volatile components in notable concentrations such as free fat acids to be desorbed, such as oils to physically refined.

EFFECT: higher efficiency of desorption, decreased consumption of steam, accelerated process.

10 cl, 5 dwg

FIELD: chemistry.

SUBSTANCE: invention concerns improved method for obtaining (meth)acrylic acid involving steam phase catalytic oxidation of propylene, propane or isobutylene for production of reaction mix, absorption of oxidised reaction product in water to obtain water solution containing (meth)acrylic acid, concentration of water solution in the presence of azeotropic agent and distillation of obtained (meth)acrylic acid in distillation column to obtaining purified (meth)acrylic acid. During operation of distillation column, including operation interruption and resumption, the column is washed with water, and afterwards azeotropic distillation is performed in the presence of azeotropic agent.

EFFECT: efficient and fast cleaning of distillation column with extraction of valuable substance.

5 cl, 5 dwg, 3 ex

The invention relates to the field of disposal of liquid radioactive waste

The invention relates to an improved method of separation of polyols, such as neopentyl glycol or atrial, and sodium formate or calcium, comprising adding to the mixture of the partial organic solvent, in which the polyhydric alcohol is dissolved, the crystallization of sodium formate or calcium, Department of formate sodium or calcium from the solution of a polyhydric alcohol in an organic solvent, for example, by filtration, recycling of organic solvent, cooling the solution and crystallization of a polyhydric alcohol, and as the organic solvent used solvent aromatic series such as toluene, after adding to the mixture of the partial substances organic solvent, the resulting mixture is heated to boiling point and produce at this temperature simultaneously: dehydration of the mixture by distillation with water recirculation separated from water, organic solvent, crystallization dissolved in an organic solvent, sodium formate or calcium and dissolution in an organic solvent, a polyhydric alcohol

The invention relates to apparatus and method for improving the flexibility of the way the process of reactive distillation