Facility for production of readily polymerised compound and installation for fabricating readily polymerised compound

FIELD: petroleum chemistry.

SUBSTANCE: invention can be implemented in rectifying and evaporating towers. Condenser 20 consists of tubular panel 33, of a dividing chamber 31, into which from above there is supplied gas containing acrylic acid, also the condenser consists of chamber 32 wherein cooling medium is supplied. Cooling pipes 34 vertically pass through chamber 32. The first pipe for supply of polymerisation inhibitor 28 enters chamber 31 outside condenser 20, while sprayer 35 is connected with the end of the first pipe for supply of polymerisation inhibitor 28. The first pipe for supply of polymerisation inhibitor 28 is supported with holder 36 outside condenser 20.

EFFECT: stable continuous processing in condenser during long period of time due to eliminating polymerisation of readily polymerised compound in condenser of simple design wherein fumes of readily polymerised compound enter.

5 cl, 2 ex, 6 dwg

 

The technical field to which the invention relates.

The present invention relates to a device for the production of easily curable compounds used in the column equipment such as a distillation column and evaporative column for easily curable compound, and a device for producing easily curable compounds. The present invention particularly relates to a device for the production of easily curable compounds used in the column the equipment with a condenser for gas in the upper part of the column or condenser outlet gas, and the device for producing easily curable compounds.

Prior art

The equipment for manufacture of highly polymerized compounds such as (meth)acrylic acid or (meth)acrylate, column includes equipment such as a distillation column for crude (meth)acrylic acid or crude (meth)acrylate or distillation column for the products of the decomposition reaction with the extraction of (meth)acrylic acid or the like in the decomposition of high-boiling substances.

In this column the equipment part or all of the gas in the upper part of the column may be cooled and siren in the condenser for liquefying gas in the upper part of the column with education as a result of this phlegmy or is pistillata. In addition, gas (discharge gas)containing valuable substances, which were nscontainerframe in the condenser gas in the upper part of the column may be cooled in the condenser outlet gas extraction, thus, valuable substances.

When the condenser is condensed and liquefied gaseous easily curable substance is formed depleted inhibitor solution without inhibitor of polymerization. Thus, this capacitor to work with easily curable compound usually involves the use of method of spraying a solution containing a polymerization inhibitor, in a capacitor for suppressing the formation of polymerized product in the condensate, resulting in the condensate contains a polymerization inhibitor (see, for example, Japan patent 2000-344688).

When installed, a traditional sprayer for spraying the solution containing the polymerization inhibitor, and installed a pipeline for supply to the spray solution containing the polymerization inhibitor, with holder for suppression of vibrations from the pipe and working spray because of the amount of current flow, the mass of the pipeline or other

In the traditional, vertically installed capacitor type tubular panel 50, in which the top gas containing the easily polymerize the second connection, as shown in figure 5, for example, the supply pipe inhibitor of polymerization 53 along which the spray 52 is served inhibitor of polymerization, so that the polymerization inhibitor is sprayed on the entire upper surface of the tubular panel 51 which separates the gas passage and the passage of the cooling medium over the tubular panel 51 of the nozzle 52 is supported inside the capacitor 50 from the bottom of the bracket 54. In addition, as shown in Fig.6, for example, the supply pipe inhibitor of polymerization 53 is supported from above by a holder 55 inside the capacitor 50. The gas supplied to the capacitor 50, is condensed in a cooling pipe 56.

Condensation can easily form a polymerized product, because the condensate does not contain a polymerization inhibitor. Thus, containing the polymerization inhibitor liquid is sprayed onto the tubular panel 51 of the spray 52, which is supplied from a pipe for supplying the polymerization inhibitor 53, to suppress the polymerization reaction. Thus, it is possible to prevent the formation of a polymerized product of the tubular panel 51. In addition, containing the polymerization inhibitor fluid passes through the cooling pipe 56, thereby providing a supply of the polymerization inhibitor in the condensate formed inside the cooling pipe 56.

The above-mentioned conventional capacitor is usually inside nebgen refrigerator to avoid the impact of the transportation process or processes of disassembly and cleaning of the condenser. But easily curable compound may condense on the holder, which may form a polymerized product.

More specifically, the temperature of the fluid passing through the pipe for supplying the polymerization inhibitor 53 and in contact with the bracket 54 or 55, is usually lower than the temperature of the gas containing the easily curable compound fed to the condenser 50. Thus, the brackets 54 or 55 is cooled and the condensate without inhibitor of polymerization is formed on the bracket 54 or 55, and may be formed polymerized product.

Description beings inventions

The present invention is a device that allows a stable continuous process in the condenser for a long time by preventing polymerization of the easily curable compounds in the condenser with a simple design that receives a pair of easily curable compounds.

Conducted extensive research and found that the formation of the cured product can be avoided as follows. (1) on the Outside of the capacitor is set to the holder in a place where water is not condensed. (2) if the strength is insufficient, when the holder is installed outside of the condenser, you must install the holder to the inside of the capacitor. In case of installation of holder inside the condenser, the solution containing the polymerization inhibitor, also sprayed on the holder.

That is, the present invention includes: a loading and unloading device for use with an easily curable compound, in which are received a pair of easy polymersomes compounds containing: the region of condensation, which is easily curable compound may condense inside the handling device, the distributor for the condensation to distribute inhibitor of polymerization of the condensation area, the pipe for supplying the polymerization inhibitor in the dispenser area of condensation and support means for supporting the dispenser of the condensation area in a predetermined position inside the working device, and the support means is a means for maintaining a source of inhibitor of polymerization outside the working device and installation for the production of easily curable compounds containing a loading and unloading device.

Preferably, the device for producing easily curable compound is a distillation installation or evaporation plant for easily curable compounds, while distilling plant comprises a distillation column and a device for production is as easily curable compound, and the setup for evaporation contains the evaporator, the reboiler and device for the manufacture of highly polymerized compounds.

Brief description of drawings

Figure 1 shows a vertical view in section of the upper part of the capacitor according to one variant of implementation of the present invention.

Figure 2 shows a vertical view in section of the upper part of the capacitor according to another variant implementation of the present invention.

Figure 3 shows a vertical view in section of the upper part of the capacitor according to another variant implementation of the present invention.

Figure 4 shows a diagram of distillers as an example installations for the production according to the present invention.

Figure 5 shows a vertical view in section of the upper part of the explanatory example of the conventional capacitor.

Figure 6 shows a vertical view in section of the upper part of another example of the conventional capacitor.

The best option of carrying out the invention

Hereinafter the present invention will be described in more detail.

A loading and unloading device for use with an easily curable compound according to the present invention is a device for easily curable compound, in which are received a pair of easily curable compound and which is concludes: the circulation area, in which easily curable compound may condense inside the handling device, the dispenser of the condensation area for distribution of the polymerization inhibitor in the condensation area, the supply pipe of the polymerization inhibitor to the filing of the polymerization inhibitor in the dispenser area of condensation and support means for supporting the dispenser area of condensation in a predetermined position inside the handling device, with (1) support means is a means for maintaining the inlet pipe inhibitor of polymerization outside handling device or (2) support means is a means for maintaining the inlet pipe inhibitor of polymerization inside the handling device, and a loading and unloading the device further includes a means of distribution for the bearing means for the distribution of the polymerization inhibitor to the support tool.

Easily curable compound used in the present invention, easily causes a polymerization reaction under such conditions as heat. Typical easily curable compound of the present invention is at least one of the compounds selected from a number of compounds such as acrylic acid, methacrylic sour is a and their esters. Examples of acrylates include methyl acrylate, acrylate, butyl acrylate, isobutylamine, tert-butyl acrylate, 2-ethyl hexyl acrylate, 2-hydroxyethylacrylate, 2-hydroxypropylmethacrylate and methoxyethylamine. Examples of the methacrylates include compounds similar to the above-mentioned acrylates.

In a loading and unloading device serves pairs easily curable compounds. Substance, partially containing a pair of easily curable compound, or a pair of easily curable compounds can be supplied in a loading and unloading device. Examples of such a handling device includes a capacitor, ferry column, tank, pump and pipeline.

The condensation region is the part inside the handling device, where a pair of easily curable compounds can condense and where it can be liquid easily curable compound without inhibitor of polymerization. Such condensation region includes the region in which the temperature may be lower than the temperature of the vapor is easily curable compounds where the condensate is easily curable compounds. Examples of such areas of condensation include: tubular plate or the cooling pipe of the condenser; the upper part of the column or plate near her in distillation columns; the end part e of the bone and the cranked portion or valve, supplied with the pump or piping.

The present invention is more effectively applicable to the handling device, in which liquid, easily curable compound without inhibitor of polymerization is easily formed by condensation of vapors easily curable compounds. Examples of such loading and unloading devices include known condenser (heat exchanger)in which a passage for the flow of the cooling medium and a passage for gas, containing a pair of easily curable compounds separated heat transfer element.

Dispenser for the condensation is a device for the distribution of the polymerization inhibitor in the condenser. Examples of such distributors of capacitors include a water sprayer, such as a spray nozzle for water, and the sprayer as a spray nozzle. The sprinkler preferably used in the present invention from the point of view of a large area of distribution and prevent excessive distribution of the polymerization inhibitor.

The supply pipe of the polymerization inhibitor is a pipe for supplying the polymerization inhibitor in the dispenser for the condensation. Such a pipe for supplying the polymerization inhibitor may include the use of a well-known line is horseflies, selected depending on conditions such as the environment in handling the device and the amount of the polymerization inhibitor.

The polymerization inhibitor used in the present invention suppresses the formation of a polymerized product from easily curable compounds. Examples of such polymerization inhibitors include acrylate copper, dithiocarbamate copper, phenolic compounds, and phenothiazine compound.

Examples of dithiocarbamates copper include: dialkyldithiocarbamate copper, such as copper dimethyldithiocarbamate, copper diethyldithiocarbamate, dipropylthiocarbamate copper and dibutyldithiocarbamate copper; cycloalkylcarbonyl copper, such as atlantajournal copper, tetramethylthiuram copper, pentametilenditiokarbamata copper and hexamethylenediisocyanate copper; and cyclohexylcarbamate copper, such as occipitocervical copper.

Examples of phenolic compounds include hydroquinone, mackinon, pyragollole, catechin, resorcinol, phenol and cresol.

Examples of phenothiazine compounds include phenothiazines, bis-(α-methylbenzyl)phenothiazines, 3,7-dioctylphthalate and bis-(α-dimethylbenzyl)phenothiazines.

The polymerization inhibitor used in this invention is selected depending on conditions such as type is easily curable connection is in. The polymerization inhibitor may be used as such or in the form of a solution easily curable compounds, subject to technological operations, or as a solvent that does not affect the movement of easily curable compounds, such as other appropriate solvent, for distribution. Distributable polymerization inhibitor may contain a substance other than those described above, depending on the process, but the type or quantity can be selected with the proviso that the substance does not affect the transportation of easily curable compounds.

Supporting means is a means for maintaining the inlet pipe inhibitor of polymerization, so that the dispenser in the condensation area is held in a predetermined position inside the handling device. Such means may include the use of known means for maintaining pipes, such as a bracket, the bracket or strap. The phrase "predetermined position inside the handling device" refers to the position in which the dispenser area of condensation may distribute the inhibitor of polymerization on the entire area of condensation.

Distribution means for the supporting means is a means for distribution inhibito is and polymerization around the supporting means, installed inside the handling device. Such a distribution means for the supporting means may consist of the above distributor or spray and hose him inhibitor of polymerization.

The present invention relates to the production unit for production of easily curable compounds, including loading and unloading device. Production unit includes a loading and unloading device and is capable of producing easily curable compound. This production plant may involve the use of devices commonly used in the production of easily curable compounds.

Easily curable compound can be obtained in a known manner to obtain. Examples of methods of obtaining acrylic acid and acrylate include the following methods (1) to (3).

(1) the Method comprises: a stage of oxidation to obtain acrylic acid through vapor-phase catalytic oxidation of propane, propylene and/or acrolein; stage collection to collect acrylic acid as an aqueous solution of acrylic acid obtaining a gas containing acrylic acid, formed at the stage of oxidation, and the implementation of its contact with water; phase extraction for the extraction of acrylic acid with the relevant solvent for extraction of the aqueous solution of acrylic acid, received during the collection phase; phase separation for the separation of acrylic acid and solvent extracted from the received fluid; purification step for purifying the separated acrylic acid by distillation or the like; phase extraction for recovery of valuable substances serving as starting material liquid with a high boiling point containing adducts of acrylic acid Michael and polymerization inhibitor used at each stage, selected from the above-mentioned stages, the column for the decomposition reaction; and the stage prior to submission of the learned valuable substances at any stage after the stage of collection.

(2) the Method comprises: a stage of oxidation to obtain acrylic acid vapor-phase catalytic oxidation of propane, propylene and/or acrolein; stage collection for collecting the acrylic acid in the aqueous solution of acrylic acid-implementation contact gas containing acrylic acid, formed at the stage of oxidation with water; stage azeotropic separation for removal of crude acrylic acid from the bottom of the column for azeotropic separation distillation of an aqueous solution of acrylic acid obtained during the collection phase in the column for azeotropic separation in the presence of an azeotropic solvent; phase separation of acetic acid to remove acetic acid from the allotted is krylovii acid; purification step to remove high boiling impurities; phase extraction for recovery of valuable substances by filing in the source material, high-boiling liquids containing adducts of acrylic acid Michael and the polymerization inhibitor used at each stage, selected from the above-mentioned stages, the column for the decomposition reaction; and the stage prior to the filing of valuable substances at any stage after the stage of collection.

(3) the Method comprises: a stage of oxidation to obtain acrylic acid vapor-phase catalytic oxidation of propane, propylene and/or acrolein; stage collection/separation for collecting the acrylic acid in the form of an organic solution of acrylic acid, obtained as a result of the implementation of the contact gas containing acrylic acid obtained at the stage of oxidation with an organic solvent, and the simultaneous removal of water, acetic acid and the like; a stage of separation for separation of acrylic acid from the organic solution of acrylic acid; phase extraction for recovery of valuable substances by filing in the source material, high-boiling liquid containing a polymerization inhibitor and organic the solvent used at each of the stages, and adducts of acrylic acid Michael, obtained from the above-mentioned stages and to columns reaction is izlozheniya; stage prior to the filing of valuable substances at any stage after collection stage and the stage of cleaning solvent to clean the part or all of the extracted organic solvent.

The method of producing acrylate includes, for example, the stage of the esterification reaction involving the reaction of acrylic acid and an alcohol with an organic acid, a cationic ion exchange resin or the like as a catalyst; the stage of concentration, including extraction, evaporation and distillation as a single operation for the concentration of a solution of the crude acrylate obtained by the reaction of esterification; purification step for purification in a purification column, acrylate in the concentrated liquid obtained at the stage of concentration; and the stage of extraction for recovery of valuable substances fed into the column of the decomposition reaction or return to the process fluid with a high boiling point containing acrylates and Michael adducts, such as β-aryloxyphenoxy, β-alkoxyamine and β-hydroxypropionate, as main components in the liquid of the bottom of the purification column, and the polymerization inhibitors used in the above-mentioned stages. Each of the unit operations in the stage of concentration is chosen arbitrarily, depending on the ratio of acrylic acid and alcohol in the source material for the esterification reaction, ka is alistore, used in the esterification reaction, physical properties of the source material, by-products of the reaction and acrylates, etc.

A liquid with a high boiling point may contain acrylic acid, a dimer of acrylic acid (hereinafter referred to as dimer), trimmer acrylic acid (hereinafter referred to as a trimmer), β-alkoxyamino acid and β-alkoxyamine as main components, obtained at any stage, except fluid bottom of the purification column acrylate products; and polymerization inhibitors used in the production stages, depending on the type used alcohol. Valuable substances can be extracted from such a liquid with a high boiling point of a liquid with a high boiling point containing adducts of Michael, in the decomposition reactor. Then extract valuable substances can be submitted to the appropriate stage, such as stage of the esterification reaction, and the stage of concentration.

The above-mentioned adduct Michael on the basis of acrylic acid or acrylate refers to the product obtained by the condensation reaction of Michael acrylic acid and raw materials acrylate. Examples of such Michael adduct obtained in the production of acrylic acid include: dimer of acrylic acid (hereinafter referred to as dime is); trimmer acrylic acid (hereinafter referred to as a trimmer) and a tetramer of acrylic acid (hereinafter referred to as a tetramer). In addition, examples of the Michael adduct obtained in the production of the acrylate include: the Michael adducts of acrylic acid with the above-mentioned acrylates, such as complex alkilany ether containing from 2 to 8 carbon atoms, or a complex cycloalkenyl ether, such as β-acrilchimproject; adducts Michael alcohol-based, such as β-alkoxyphenyl; dimers; trimers; tetramer; esters of trimers; esters tetramers; β-hydroxypropionic acid and β-hydroxypropionate.

Production installation according to the present invention may involve the use of devices or apparatus commonly used in the production of easily curable compounds, such as distillation apparatus or evaporative apparatus for easily curable compounds.

Can be used distillation column, commonly used in chemical production. Within the distillation columns are plates or nozzles. Specific examples of dishes include nozzle plates, each having a drain tube, plate type, perforated plates, valve plates, plates SUPERFRAC, plates MAX-FRAC and plates with dual flow without videospussy tubes.

p> Examples of structured packings include: SULZER PACKING, available from the firm Sulzer Brothers Ltd.; SUNITOMO-SULZER PACKING, available from the company Sumitomo Heavy Industries, Ltd.; MELLAPAK, available from the company Sumitomo Heavy Industries, Ltd.; GEM-PAK, available from the firm of Koch-Glitsch, LP; MONTZ-PAK, available from the firm Julius Montz GmbH; GOOD ROLL PACKING, available from the firm's Tokyo Tokushu Kanaami K.K.; HONEYCOME PACK, available from the company NGK Industries, Ltd.; IMPULSE PACKING, available from the company Nagaoka International Corporation; and MS PACK, available from Mitsubishi Chemical Engineering Corporation.

Examples of statistical nozzles include: INTALOX SADDLES, available from the company Saint-Gobain NorPro; TELLERETT available from the company Nittetsu Chemical Engineering Ltd.; PALL RINGS, available from BASF Aktiengesellsghaft; CASCADE MINI-RING, available from the firm Mass Transfer Ltd.; FLEXI RINGS, available from the company JGK Corporation.

The type of plates and nozzles is not limited in the present invention may be used one type of plates and nozzles or two or more types may be used in combination with each other, as usual. In the production of easily curable compounds, the reaction can be performed in a distillation column, and the reaction distillation column corresponds to a distillation column in the present invention.

Can also be used setting for evaporation, commonly used in chemical plants. That is the setting for evaporation is supplied by the evaporator and a reboiler and may not necessarily include the con is ensator (refrigerator) for condensing the evaporated gas, storage capacity condensate pump for transporting condensate and fridge for gas outlet for additional cooling neskondensirovannyh gas. Installation for evaporation includes the above-mentioned handling device.

The condenser is a heat exchanger for cooling the gas in the top of the column and the condenser is a heat exchanger for cooling gas outlet, each attached to a distillation column in the distillation installation or evaporative installation. The capacitor is normally classified as a capacitor mounted inside the column, and a condenser mounted outside the column, but the present invention is generally applicable to the condenser installed outside of the column. The type of capacitor is not particularly limited, and specific examples of the capacitor includes a vertically mounted tubular panel, horizontally mounted tubular panel, pipe U-shaped type, capacitor type double pipe, type a square block and plate type.

The materials handling device, production system and its peripheral devices in the present invention is not particularly limited and is preferably selected depending on easily curable compounds intended for the transport of the s operations, and temperature conditions. Stainless steels are often used as materials in the manufacture of, for example, (meth)acrylic acid and (meth)acrylates, which are typical easily polymerized substances, but the materials are not limited to stainless steels. Examples of such stainless steels include SUS 304, SUS 304L, SUS 316, SUS 316L, SUS 317, SUS 317L, SUS 327 and hastelloy. The materials selected physical properties of each fluid from the standpoint of corrosion resistance or the like

In the present invention the amount of the polymerization inhibitor, distributed on an area of condensation from the distributor inhibitor of polymerization may be determined arbitrarily depending on various conditions such as the amount of feed in the handling device can be easily polymerized connection type easily curable compound and the size of the area of condensation.

Further distillation device for acrylic acid will be described in embodiments implementing the present invention with reference to the drawings.

The first option exercise

As shown in figure 4, the distillation device for acrylic acid includes a housing 1 column (distillation column) for the distillation of crude acrylic acid; a condenser 20 for cooling the vapors containing acrylic acid to condensation; the capacity for FLEG is s 21, which receives the condensate formed in the condenser 20; fridge to gas outlet 25 for additional cooling of the gas cooled in the condenser 20, with extraction as a result of this valuable substances; and vacuum equipment 26 to reduce the pressure in the distillation system.

The outlet 2 to drain the lower part of the column is installed in the lower part of the housing 1 columns. The inlet 3 and the pipe 11, through which is fed a portion of the released fluid to the bottom of the column is connected to outlet port 2.

Pipe 4 for supplying the liquid to the bottom of the column from the inlet 3 is connected with the inlet 3 and the reboiler 5, for heating the liquid, the lower part of the column from pipe 4 is connected to the pipe 4. Pipe 6 for supplying heated fluid bottom of the column is connected to a reboiler 5, and the inlet pipe 7 for supplying the liquid to the bottom of the column in case 1 columns of the pipe 6 is connected with the pipe 6.

The pump 12 for supplying the liquid to the bottom of the column of pipe 11 is connected with the pipe 11 and pipe 13 is connected to the pump 12.

On the other hand, the pipe 19 for supplying gas containing acrylic acid, is connected with the upper part of the column body 1 columns. The capacitor 20 is connected with the pipe 19, and the capacity to phlegmy 21 is connected to the condenser 20. Condenser gas outlet 25 and a pump 22 for supplying condensate in the technology for phlegmy 21 is connected with the capacity to phlegmy 21. Vacuum equipment 26 is connected to the condenser outlet gas 25.

The pipe 23 to return part of the condensate in the housing 1 of the column is connected to the pump 22. The pipe 23 is divided into a pipe 24 for supplying part of the condensate in the form of purified acrylic acid and a pipe 27 for supplying part of the condensate in the condenser 20 and the condenser outlet gas 25.

The supply pipe inhibitor of polymerization of 30 to introduction of the polymerization inhibitor in the condensate part is connected to a pipe 27. The pipe 27 is divided into the first pipe for supplying the polymerization inhibitor 28 for feeding the condensate containing the entered polymerization inhibitor, a capacitor 20 and a second pipe for supplying the polymerization inhibitor 29 for introducing the condensate containing the entered polymerization inhibitor, a condenser for gas outlet 25.

As shown in figure 1, the capacitor 20 is a vertically positioned heat exchanger tube panel, in which the gas passes through the tubes and the cooling medium passes through the shirt. The capacitor 20 includes the following elements: a tubular pad 33, the separating chamber 31, in which the top gas containing acrylic acid, and the camera 32, which serves a cooling medium; and a cooling pipe 34 opening into the chamber 31 and passing through the chamber 32 vertically. Figure 1 shows only one of ohlord the operating pipe 34, but it really has plenty of cooling pipes 34.

The first pipe for supplying the polymerization inhibitor 28 enters the chamber 31 from the outside of the capacitor 20 and the spray 35 is connected to the end of the first pipe for supplying the polymerization inhibitor 28. The first pipe for supplying the polymerization inhibitor 28 is supported by a holder 36 on the outside of the condenser 20. Thus, the spray 35 is supported in position for spraying inhibitor of polymerization on the entire upper surface of the tubular pad 33. Condenser gas outlet 25 has the same structure as the capacitor 20.

The crude acrylic acid is fed into the housing 1 column for distillation. Part of the liquid bottom of the column circulates in the direction from the inlet 2 to the intake pipe 3, the pipe 4, the reboiler 5, pipe 6 and the pipe 7 and is returned into the housing 1 of the column. Another part of the liquid bottom of the column is displayed as the rest through the outlet 2, the pipe 11, the pump 112 and the pipe 13. The distilled substance from the upper part of the column is introduced into the container to phlegmy 21 through the pipe 19 and through the condenser 20. The temperature of the lower part of the column is preferably from 60 to 120°C., particularly preferably from 70 to 100°C., and the pressure in the upper part of the column is preferably from 1 to 50 kPa, particularly preferably from 2 to 20 kPa.

The hour is ü acrylic acid in the tank for phlegmy 21 is returned to the upper part of the column through the pump 22 and the pipe 23. Another part of acrylic acid is supplied through the pipe 27 and is mixed with a polymerization inhibitor, coming through the pipe 30 for supplying the polymerization inhibitor. The mixture passes into the spray 35 mounted within each of the capacitor 20 and the condenser from the gas outlet 25, the first pipe 28 for supplying the polymerization inhibitor and the second pipe 29 for supplying the polymerization inhibitor.

A mixed solution of acrylic acid and a polymerization inhibitor is sprayed on the entire upper surface of the tubular pad 33 of the spray 35. The tubular pad 33 is cooled by a cooling medium in the chamber 32. Thus, when the gas supplied into the chamber 31, comes into contact with the tubular pad 33, acrylic acid in the gas easily condenses, and the liquid acrylic acid without inhibitor of polymerization is formed on the tubular pad 33. That is, the upper surface of the tubular pad 33 serves as a region of condensation.

However, acrylic acid containing a polymerization inhibitor, is sprayed on the tubular pad 33, and the polymerization inhibitor is supplied in liquid acrylic acid in the tubular pad 33, thus preventing the formation of a polymerized product of acrylic acid on the tubular pad 33. In the condenser for gas outlet 25 also prevents the formation of a polymerized product and is easily curable compound, such as acrylic acid.

In addition, the inhibitor of polymerization passes through the cooling pipes 34 and a polymerization inhibitor enters the condensate of acrylic acid, formed inside the cooling pipes 34. Thus, the formation of a polymerized product of acrylic acid is prevented in the cooling pipes 34 and capacity to phlegmy 21 that, in turn, prevents clogging of the cooling pipes 34, etc.

The rest of acrylic acid from the tank 21 to phlegmy is taken in the form of purified acrylic acid through a pipe 24 extending from the pipe 23. The gas in the tank for phlegmy 21 again cooled in the condenser to the gas outlet 25 and condensed acrylic acid is returned to the tank phlegmy 21. The gas component is discharged in the form of outlet gas after passing through the vacuum equipment 26.

In the present embodiment, with the simple construction of providing the holder 36 on the outside of the capacitor 20 of the first pipe for supplying the polymerization inhibitor 28 can be held without contact holder 36 with a gas containing acrylic acid, and thus keep the spray 35 in position. Thus, condensation or polymerized product of acrylic acid on the holder 36 can be prevented, thereby ensuring a stable continuous operation ol the production plants for the production of acrylic acid over a long period of time.

The second option of carrying out the invention

As shown in figure 2, the plant for production of acrylic acid according to the present invention has the same design that the installation of the first variant implementation, except that: the holder 37 to maintain the first pipe 28 for supplying the polymerization inhibitor inside the capacitor 20 from the top used instead of the holder 36; and further established the third pipe 38 for supplying the polymerization inhibitor into the chamber 31 from the outside of the condenser 20 and the spray device 39 connected to the top of the third pipe for supplying the polymerization inhibitor 38 for spraying inhibitor of polymerization around the holder 37. The spray device 39 is supported in position when the polymerization inhibitor may be supplied to the entire surface of the holder 37 to the third pipe 38 for supplying the polymerization inhibitor. The third pipe 38 for supplying the polymerization inhibitor may be: pipe branched from the first pipe 28 for supplying the polymerization inhibitor; pipe branched from the pipe 27 downstream from the connection of the pipe 30 for supplying the polymerization inhibitor, or a pipe for supply of the polymerization inhibitor in a completely different line.

In the present embodiment of the invention, a gas containing acrylic acid, in contact with the holder 37 can the t to condense on the surface of the holder 37. That is, the region of condensation in this embodiment of the invention includes the surface of the holder 37. However, the polymerization inhibitor is sprayed on the surface of the holder 37, thus preventing the formation of a polymerized product of acrylic acid on the surface of the holder 37.

This variant of the invention allows to maintain the first pipe 28 for supplying the polymerization inhibitor, to maintain the spray 35 in the proper position and to prevent the formation of a polymerized product of acrylic acid within the condenser 20, even when the first pipe 28 for supplying the polymerization inhibitor is rigidly attached on the outside of the capacitor 20 due to various problems, such as preventing vibrations or strength of the pipe.

In this embodiment of the invention using a pipe branched from the pipe 28 for supplying the polymerization inhibitor in the form of a third pipe 38 for supplying the polymerization inhibitor, is more effective from the point of view of simplicity of the scheme and the submission of polymerization inhibitor in the condenser 20 or capacitor 25 to the gas outlet.

The third variant embodiment of the invention

As shown in figure 3, the production device for producing acrylic acid according to this variant embodiment of the invention has the same schema, is the second variant of the invention, with the exception of the following:

the holder 40 to maintain the first pipe 28 for supplying the polymerization inhibitor inside the capacitor 20 from the bottom is used instead of the holder 37 and the sprinkler 39 is supported by the third pipe 38 for supplying the polymerization inhibitor in the position in which the polymerization inhibitor can be sprayed around the holder 40. The same effects as in the second embodiment, can be implemented in this embodiment of the invention.

In the present invention the position of the holder is defined as a supporting tool, can be defined generally carried out calculations of mechanical strength. However, the holder typically install: outside condenser 20, when the body 1 of the column has a diameter of at least 1 m, and the inside of the capacitor 20 when the housing 1 of the column has a diameter of 1 m or more.

In addition, in each of the embodiments of the present invention is used, the holder having a design brackets, but the holder used in the present invention is not limited to such construction. It is only necessary that the holder had "form", "dimensions" and "thickness", as a result usually carried out calculations of mechanical strength.

Examples

Hereinafter the present invention will be described in more detail based on examples and compare the selected examples but the present invention is not limited to them.

Example 1

Distillation of the crude acrylic acid was carried out in the distillation setup, shown in figure 4, requires the use of a distillation column made of stainless steel SUS 316 having an inner diameter 1100 mm, length 20000 mm, with 21 perforated plates (plates with dual stream)located inside the body 1 of the column. The capacitor 20 stainless steel SUS 316L had a diameter of 890 mm and length 3050 mm Condenser for gas drainage stainless steel SUS 316L had a diameter of 480 mm and a length 2440 mm Condensate is passed through the cooling tubes in each capacitor 20 and the condenser for gas drainage 25.

Within each of the capacitor 20 and the condenser for gas drainage 25 was installed spray 35, and the holder inside them was not installed, as shown in figure 1.

In distillation setup, shown in figure 4, the mixture of 98.5 wt.% of acrylic acid, 0.3 wt.% maleic acid and 0.3 wt.% dimer of acrylic acid, in the form of a crude acrylic acid was applied to the housing 1 of the column at 90°C at the rate of 1300 kg/h

The liquid obtained by dissolving 8 wt.% methanone and 1 wt.% fenotiazina in acrylic acid was given in the upper part of the column body 1 column with a speed of 34 kg/h and the crude liquid acrylic monomer is fed into the housing 1 of the column with speed is 31 kg/HR not shown on the figure of the reservoir for the liquid, containing a polymerization inhibitor. The process is conducted at a pressure in the upper part of the column of 2.8 kPa, the pressure in the lower part of the column of 7.9 kPa, the temperature in the upper part of the column 53°C and the temperature in the lower part of the column 75°C and result in the lower part of the column was obtained acrylic acid of high purity, having a purity 99.8 wt.% or more.

Part of acrylic acid of high purity, obtained from the upper part of the column, regulated, bringing the concentration of methanone up to 200 hours per million by mixing with a liquid containing a polymerization inhibitor (metochion) from the pipe 30 for supplying the polymerization inhibitor, through the condenser 20, a pipe for phlegmy 20, pump 22 and the pipe 27. Regulated acrylic acid of high purity was applied to the capacitor 20 with the speed of 1020 kg/h and the condenser for gas outlet 25 with a speed of 995 kg/h

After continuous operation for 6 months in the above conditions, the operation was stopped to assess the capacitor 20 and the housing 1 of the column. The survey results confirmed that there was no accumulation of substances and no clogging of the condenser 20 in the process.

Comparative example 1

Repeating the same operations as in example 1, except that the condenser 20 and condenser gas outlet 25, as shown in figure 1, was replaced by a capacitor 50, pokazannym 5.

After working for 3 months the temperature of the liquid in the lower part of the column is gradually increased and increased the difference between the pressure capacity for phlegmy 21 and the pressure of the upper part of the column in the housing 1 of the column. Thus, exclude the supply of steam to the reboiler 5.

Work stopped and examined the interior of the installation. The results of the survey confirmed the formation of loose granular polymerized product on the upper surface of the tubular panel 51 in the condenser 50.

Example 2

Distillation of the crude acrylate was performed in a distillation setup, shown in figure 4, using a distillation column made of stainless steel (SUS 316)having an inner diameter of 1500 mm, length 14700 mm and 20 plates with double thread, installed inside. The capacitor 20 stainless steel SUS 316L had a diameter of 1020 mm and length 3050 mm Condenser gas outlet 25 of the steel SUS 316L had a diameter of 303 mm and length 2440 mm Condensate is passed through the cooling tubes in each capacitor 20 and the condenser for the gas outlet 25.

Spray 35 was installed inside each of the capacitors of the capacitor 20 and the condenser for gas outlet 25, and as shown in figure 1, the holder within not been set.

In distillation setup, shown in figure 4, the mixture of 99.3 wt.% ethyl acrylate, and 0.04 wt.% ethyl acetate, and 0.04 wt.% e is ylpropionic, of 0.52 wt.% acrylic acid and 0.1 wt.% hydroquinone, as crude acrylate, filed in the housing 1 of the column at 90°C at the rate of 4500 kg/h

The liquid obtained by dissolving 1.5 wt.% methanone in the acrylate was applied to the upper part of the housing 1 of the column at a rate of 30 kg/h of capacity for liquids, containing the polymerization inhibitor (not shown). The work was carried out at the pressure of the upper part of the column of 21.3 kPa, the pressure bottom of the column to 26.7 kPa, the temperature of the upper part of the column 56°C and the temperature of the lower part of the column 71°C, with getting acrylate of high purity, having a purity of 99.9 wt.% or more, leaving the upper part of the column.

Part of the acrylate of high purity obtained in the upper part of the column was mixed with 11 kg/s liquid containing the polymerization inhibitor from the inlet pipe inhibitor of polymerization 30, through the condenser 20, a pipe for phlegmy 21, pump 22 and the pipe 27. The mixture was applied to the capacitor 20 with a speed of 1750 kg/h and condenser gas outlet 25 at the rate of 1,000 kg/h

After continuous operation for 6 months in such conditions, the work stopped for examination of the capacitor 20 and the housing 1 of the column. The results showed that no accumulation of sediments and there is no blockage of the capacitor 20 during operation.

Comparative example 2

Repeated the same process, Thu and in example 2, except that the condenser 20 and condenser gas outlet 25, as shown in figure 1, was replaced by a capacitor 50, is shown in Fig.6.

After working for 4 months of the liquid temperature of the lower part of the column is gradually increased and increased the difference between the pressure in the vessel to phlegmy 21 and the pressure of the upper housing 1 columns. Thus, excluded the admission of steam to the reboiler 5.

Work stopped and examined the inner part of the installation. The results of the survey showed the presence of polymerized product on the upper surface of the tubular panel 51 in the condenser 50.

Industrial application

According to the present invention the formation of a polymerized product support tool set for spray polymerization inhibitor, suppressed in the loading and unloading device for transporting easily polymerized compounds, such as a capacitor or condenser outlet gas, and thereby prevents clogging. Thus, the production device for producing easily polymerized compounds, such as distillation column, comprising a loading and unloading device for easily curable compounds can stably and continuously work for a long period of time.

The present invented the e is more effective for spraying inhibitor of polymerization widely and effectively, when the distributor for distribution of the polymerization inhibitor is a spray.

In particular, the present invention is more effectively applicable to the transportation or receipt of easily curable compounds, such as (meth)acrylic acid or (meth)acrylate.

1. Device for the production of lignopolimering connection, which serves pairs lignopolimering compounds containing:
the region of condensation, in which lignopolimering connection is condensed inside the unit,
dispenser for the condensation to distribute inhibitor of polymerization of the condensation area,
a pipe for supplying the polymerization inhibitor for the filing of the polymerization inhibitor in the dispenser in the condensation area and
support means for maintaining the dispenser in the condensation area in a predetermined position inside the device, and
the supporting means is a means for maintaining the pipe for supplying the polymerization inhibitor from the outside of the device.

2. Device for the production of lignopolimering connection, which serves pairs lignopolimering compounds containing:
the region of condensation, which is easily curable compound is condensed inside the unit,
the distributor for the area of the condensation for distribution inhibitor of polymerization of the condensation area,
the supply pipe of the polymerization inhibitor to the filing of the polymerization inhibitor in the dispenser for the condensation and
support means for maintaining the dispenser in the condensation area in a predetermined position inside the device, and the supporting means is a means for maintaining the inlet pipe inhibitor of polymerization within the device, and the device further includes a means of distribution for the supporting means for the distribution of the polymerization inhibitor into the support tool.

3. Device for the production of lignopolimering compound according to claim 1 or 2, which is a capacitor.

4. Device for the production of lignopolimering compound according to claim 1 or 2, in which the dispenser is a spray.

5. Device for the production of lignopolimering compound according to claim 1 or 2, in which leggopoker.com compound is at least one of the compounds selected from (meth)acrylic acid and (meth)acrylate.

6. For lignopolimering connection, which is a distillation installation or evaporation plant for lignopolimering connection, while distilling plant comprises a distillation column and a device for the production of leggopoker the constituent compounds according to any one of claims 1 to 5 and the evaporator includes an evaporator, the reboiler and device for the production of lignopolimering compound according to any one of claims 1 to 5.

7. For lignopolimering connection according to claim 6, in which lignopolimering connection includes at least one compound selected from (meth)acrylic acid and (meth)acrylate.



 

Same patents:

FIELD: chemistry.

SUBSTANCE: invention concerns regeneration of monomer complex ethers of substituted or non-substituted acrylic acid or styrene-containing monomers, particularly device for regeneration of monomer complex ethers of substituted or non-substituted acrylic acid or styrene-containing monomers from polymer material containing respective structural units. Device includes: heated reactor for monomer-containing gas generation from polymer material, and shifting device for propulsion of relocated product, combined with reactor or being a part of reactor. To enhance output and purity of generated monomer, heat carrier comprised by multiple spherical units with diametre within 0.075 to 0.25 mm is preferred.

EFFECT: relocated material containing polymer material and heat carrier.

2 cl, 5 dwg, 3 ex

FIELD: chemistry.

SUBSTANCE: invention concerns organic compound synthesis, particularly method of obtaining 4-biphenylmetacrylate of the formula . Obtained compound is applied in production of heat and weather resistant polymer materials. Claimed method involves dissolution of 4-phenylphenol in 10 wt % aqueous solution of caustic soda, further dosage of acylating agent in the form of metacrylic acid anhydride agent in reaction mix preliminarily cooled to 0-(+5°)C at such rate so as to keep the mix temperature below +10°C at molar ratio of 4-phenylphenol and metacrylic acid anhydride of 1:(1.1-1.5), reaction mix maturing at room temperature with stirring, organic layer extraction, flushing by alkali solution, and drying.

EFFECT: enhanced output of 4-biphenylmetacrylate, admixture content of non-reacted 4-phenylphenol reduced to 0,003-0,005 wt %.

3 cl, 1 tbl, 10 ex

FIELD: chemistry.

SUBSTANCE: invention refers to advanced method of production of (meth)acrylic acid ester including (meth)acrylic acid purification by contacting raw (meth)acrylic acid containing manganese as an impurity manganese, and cation-exchange resin to remove manganese. To ensure contacting raw (meth)acrylic acid and cation-exchange resin, water is pre-added to (meth)acrylic acid. Besides, the method involves reaction of purified (meth)acrylic acid and alcohol with acid catalyst added.

EFFECT: method allows preventing effectively deactivation of the acid catalyst used in etherification reaction, equipment plugging and can ensure stable ester manufacturing.

3 cl, 5 tbl, 5 ex

FIELD: chemistry.

SUBSTANCE: invention relates to improved method of obtaining (meth)acrylic ester including stage of etherification of (meth)acrylic acid with C1-C4alcohol in presence of catalyst from highly acidic cation-exchange resin in form of immovable layer for obtaining (meth)acrylic ester; addition of polymerisation inhibitor into reactor or into distillation column for isolation; stage of isolation, at which (meth)acrylic acid that did not react is separated from reaction solution, obtained at reaction stage, where temperature in distillation column still is in the range from 60 to 100°C, and pressure at the top of distillation column is in the range from 1.33 to 26.7 kPa; and recirculation stage in order to return thus obtained (meth)acrylic acid, that did not react, to reaction stage, where solid substances, contained in isolated (meth)acrylic acid that did not react and is returned to reaction stage, are isolated from it. In industry used method of obtaining (meth)acrylic esters is improved in such way as to prolong service life of used in it catalyst from highly acidic cation-exchange resin.

EFFECT: elaboration of improved method of obtaining (meth)acrylic ester.

5 cl, 2 ex, 1 dwg

FIELD: chemistry.

SUBSTANCE: present invention pertains to improvement of the method of producing (met)acrylic acid and complex (met)acrylic esters, involving the following stages: (A) reacting propane, propylene or isobutylene and/or (met)acrolein with molecular oxygen or with a gas, containing molecular oxygen through gas-phase catalytic oxidation, obtaining crude (met)acrylic acid; (B) purification of the obtained crude (met)acrylic acid, obtaining a (met)acrylic acid product; and (C) reacting raw (met)acrylic acid with alcohol, obtaining complex (met)acrylic esters, in the event that the installation used in any of the stages (B) and (C), taking place concurrently, stops. The obtained excess crude (met)acrylic acid is temporarily stored in a tank. After restoring operation of the stopped installation, the crude (met)acrylic acid, stored in the tank, is fed into the installation, used in stage (B), and/or into the installation used in stage (C). (Met)acrylic acid output of the installation used in stage (A) should be less than total consumption of (met)acrylic acid by installations used in stages (B) and (C).

EFFECT: the method allows for processing (met)acrylic acid, temporarily stored in a tank, when stage (B) or (C) stops, without considerable change in workload in stage (A).

2 ex

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

FIELD: chemistry.

SUBSTANCE: catalytic composition contains the catalyst of olefin metathesis as one component, and phenol derivatives as another component, at proportion: 1 mol equivalent of catalyst to 200-1500 mol equivalents of phenol derivatives. In another modification, the catalytic composition contains as the second component the alcohol derivates which do not contain the C-H fragments at α-position to hydroxyl function, at proportion: 1 mol equivalent of catalyst to 200-1500 mol equivalents of alcohol derivatives. Another one modification of the invention has quinine or its derivatives as the second component of the catalytic composition. Particularly, the ruthenium complex with formula can be used as a catalyst of olefin metathesis.

EFFECT: number of catalyst turnover and life-time of catalyst in metathesis reaction of dialkylmaleate with ethylene are increased.

10 cl, 12 ex, 6 tbl

FIELD: organic chemistry, chemical technology, polymers.

SUBSTANCE: invention relates to novel polyalkoxylated trimethylolpropane (meth)acrylic esters. Invention proposes polyesters of the following formulas (Ib) and (Ic) wherein EO means O-CH2-CH2-; PO means independently of one another O-CH2-CH(CH3)- or O-CH(CH3)-CH2-; n1 + n2 + n3 = 28, 29, 30, 31, 32, 33, 34, 35, 36, 37, 38, 39, 40, 41, 42, 43, 44, 45, 46, 47, 48, 49, 50, 51, 52, 54, 55, 56, 57, 58, 59 or 60; m1 + m2 + m3 = 4, 5, 6, 7, 8, 9, 10, 11, 12 or 13; R1, R2 and R3 mean independently of one another hydrogen atom (H) or -CH3. Proposed esters can be used in preparing polymers absorbing aqueous liquids and forming hydrogel. Invention provides development of compounds that can be used as radical cross-linking agent, in particular, for superabsorbers.

EFFECT: valuable properties of esters.

12 cl, 2 tbl, 7 ex

FIELD: organic synthesis.

SUBSTANCE: claimed method includes reaction of maleic acid C1-C4-alcohol esters with ethylene in presence of metathesis catalyst at 20-140°C ethylene pressure of 101325-506625 Pa.

EFFECT: method of high selectivity, mild conditions without uses of toxic reagents.

7 cl, 28 ex, 8 tbl

FIELD: industrial production of methacrylic acids at reduced amount of industrial wastes.

SUBSTANCE: proposed method is performed by catalytic oxidation of propane, propylene or isobutylene in vapor phase at separation of final product and forming of high-boiling mixture as by-product which contains (according to Michaels addition) water, alcohol or methacrylic acid added to methacrylic group. By-product is decomposed in thermal decomposition reactor at simultaneous distillation of decomposition products in distilling column from which methacrylic acid is taken in form of distillate. Flow of liquid decomposition residue is forced for peripheral direction by means of mixing blades before withdrawal from reactor. Peripheral direction is obtained with the aid of liquid fed from the outside of decomposition reactor; to this end use is made of initial high-boiling material or flow of liquid discharged from decomposition reactor. If necessary, etherification stage is performed through interaction with alcohol for obtaining methecrylic ester. Decomposition of by-product formed at obtaining methacrylic acid by oxidation of propylene or isobutylene or at obtaining methacrylic acid by interaction of acid with alcohol by alcohol through introduction of by-product into thermal decomposition reactor provided with distilling column which has plates made in form of disks and toroids for simultaneous decomposition and distillation. Plant proposed for realization of this method includes thermal decomposition reactor and distilling column, level meters and lines for discharge of liquid containing easily polymerized compounds. Level indicator mounted at area of accumulation of liquid shows pressure differential. Line for detecting the side of high pressure of this level meter is connected with accumulated liquid discharge line.

EFFECT: updated technology; increased yield of target products.

38 cl, 14 dwg, 2 tbl, ex

FIELD: chemistry.

SUBSTANCE: method includes supply of initial mixture and dimethylsulfoxide (DMSO) as separating agent, taken in ratio 7-7.5:1 to initial mixture, into extraction rectification column (1) efficiency 50 t.t., initial mixture being supplied on 30 t.t., separating agent on 10 t.t. of column (plate numeration from top of column), phlegm number in column constitutes 1.5-2, taking of benzol in distillate and mixture benzol-perfluorobenzol (PFB) - tertiary amyl alcohol (TAA)-DMSO from column (1) cube , supply of mixture PFB-TA-DMSO on 25 t.t. of column of separating agent regeneration (2) with efficiency 50 t.t., phlegm number in column being 1-3, removal separating agent from column cube and its supply to column (1), supply of column (2) distillate, representing aseotropic mixture PFB-TAA, for separation into complex of two columns (3) and (4) with efficiency 35 t.t., with removal from column cubes of TAA and PFB, respectively, aesotropic mixture being supplied on 18 t.t. of column (3), phlegm numbers of columns (3) and (4) being equal 0.5-1.5 and 1-2 respectively, re-cycle of aseotrope PFB-TAA, which is separated in distillate of column (4) into column(3) feeding, ratio of re-cycle of column (4) and feeding of column (3) being (1-1.1):0.66, pressure in columns (1)-(3) is 300 mm of mercury, pressure in column (4) - 760 mm of mercury.

EFFECT: simplification of technology, increase of ecological compatibility of process and quality of obtained products.

1 tbl, 1 dwg, 1 ex

FIELD: physicochemical techniques.

SUBSTANCE: sublimation of nonvolatile organic compounds comprises heating thereof on conducting grid, through which electric current is passed. Organic substance layer is deposited on grid of current conducting material, in particular metal, and obtained layer is mechanically pressed to grid.

EFFECT: accelerated sublimation and increased purity of sublimed product.

2 cl, 1 dwg, 1 tbl, 12 ex

FIELD: natural substances, chemical technology.

SUBSTANCE: invention relates to a method for preparing chitosan and purification from components of the reaction mixture - low-molecular products of deacetylation and alkali excess. Invention relates to a method for purifying chitosan prepared by solid-state method involving treatment of reaction mass with extractant consisting of 3.3-20.0% of water, 32.2-57.1% of ethyl acetate and 24.6-64.5% of ethanol at the extractant boiling point. Also, invention relates to a method for purifying chitosan prepared by suspension method and involving treatment of the reaction mass with ethyl acetate and the following treatment with extractant consisting of 6.2-25.0% of water, 12.5-62.5% of ethyl acetate and 31.3-62.5% of ethanol at the extractant boiling point.

EFFECT: improved isolating and preparing method.

3 cl, 2 tbl, 1 dwg

FIELD: chemical technology.

SUBSTANCE: invention relates to a method for treatment of aluminum alcoholates. Method involves passing aluminum alcoholates through a column filled with extrudates of aluminum oxide in γ-form with pore volume from 0.4 to 0.8 cm3/g prepared by preliminary hydrolysis of aluminum alcoholates, molding the prepared aluminum oxide to extrudates with diameter from 1.6 to 3 mm and length 3-4 mm and their following purification by calcinations at temperature 400-500°C. As a rule, the treatment of alcoholates is carried out at temperature 20-150°C in column for 1-5 h. Method provides the development of simple and available technology for treatment of aluminum alcoholates with hydrocarbon chain length from C3 to C6 and above from impurities up to the level 10-3-10-4 wt.-%.

EFFECT: improved treatment method.

2 cl, 5 ex

FIELD: processes catalyzed by metal-phosphoro-organic ligand complexes when target product may be selectively extracted and separated from liquid product.

SUBSTANCE: Specification gives description of methods of separation of one or several products of decomposition of phosphoro-organic ligand, one or several reaction byproducts and one or several products from liquid reaction product synthesized continuously and containing one or several non-consumed reagents, catalyst in form of complex of metal-phosphoro-organic ligands, not obligatory free phosphoro-organic ligand, one or several said decomposition products of phosphoro-organic ligand, one or several said reaction byproducts, one or several said products, one or several non-polar solvents and one or several polar solvents by separation of phases where (i) is selectivity of non-polar phase for phosphoro-organic ligand relative to one or several products expressed by ratio of distribution coefficient Ef1 whose magnitudes exceeds about 2.5; (ii)is selectivity of non-polar phase for phosphoro-organic ligand relative to one or several decomposition products expressed by ratio of distribution coefficients Ef2 whose magnitude exceeds proximately 2.5; and (iii) is selectivity of non-polar phase for phosphoro-organic ligand relative to one or several reaction byproducts expressed by ratio of distribution coefficients Ef3 whose magnitude exceeds approximately 2.5 (versions). Description is also given of continuous methods of obtaining one or several products (versions) and reaction mixture containing one or several aldehyde products.

EFFECT: increased conversion of initial materials and selectivity by product; avoidance or exclusion of deactivation of catalyst.

20 cl, 2 tbl

FIELD: improved processes catalyzed by complexes of a metal- organophosphorous ligand.

SUBSTANCE: the invention presents the improved processes catalyzed by complexes of metal-organophosphorous ligand. The method of extraction includes: feeding of the indicated liquid reactionary product in the zone of separation, stirring of the indicated liquid reactionary product with production by separation of phases of a polar phase containing one or several unreacted reactants, a complex catalyst metal- organophosphorous ligand, not obligatory free organophosphorous ligand and one or several polar dissolvents; and a nonpolar phase containing one or several products of decomposition of the organophosphorous ligand, one or several by-products of the reaction and one or several products. Further the method provides for the stages of withdrawal from the zone of separation and feeding into the reaction zone and-or into the zone of separation. In the given method selectivity of the polar phase for the organophosphorous ligand concerning one or several products is expressed by a ratio of distribution coefficients Efl, which has a value more than approximately 2.5; (ii) the selectivity of the polar phase for the organophosphorous ligand concerning one or several decomposition products of the organophosphorous ligand is expressed by a ratio of distribution coefficients Ef2, which has a value more than approximately 2.5; and (iii)the selectivity of the polar phase for the organophosphorous ligand concerning one or several by-products of reaction is expressed by a ratio of distribution coefficients Ef3, which value is more, than approximately 2.5. The method allows to reduce a negative effect on the process, for example, on prevention of a decrease of efficiency of the catalyst, conversion of the initial material and selectivity by a product.

EFFECT: the invention ensures reduction of a negative effect on the process, on efficiency of the catalyst, on conversion of the initial material and selectivity by a product.

20 cl, 2 tbl

The invention relates to the chemical industry for the production of chlorobenzene method of chlorination of benzene, and can be used in the production of phenyltrichlorosilane (FTHS), where on the one hand, the chlorobenzene is used as a raw material, and on the other hand in the production FTHS as a by-product is formed benzene, chlorine - and organochlorosilane

The invention relates to an improved method of separating one or more products from the liquid reaction product containing the catalyst in the form of complex compounds of a metal with an organophosphorus ligand, optionally free organophosphorus ligand, a non-polar solvent, the polar solvent is selected from the group comprising NITRILES, lactones, pyrrolidone, formamide and sulfoxidov, and named one or more products, the method comprises (1) mixing named liquid reaction product to obtain phase separation a nonpolar phase containing the above catalyst, optionally free organophosphorus ligand and called nonpolar solvent and a polar phase, contains named one or more products and a polar solvent, and (2) the Department called the polar phase from the named non-polar phase, and named the organophosphorus ligand has a distribution coefficient between the nonpolar solvent and the polar solvent of greater than about 5, and named one or more products is the distribution coefficient between the polar solvent and the nonpolar rastvorimo of the reaction product, containing the catalyst in the form of complex compounds with metal-phosphorus metal, optionally free organophosphorus ligand, a non-polar solvent and one or more products, the method comprises (1) mixing named liquid reaction product with a polar solvent selected from the group comprising NITRILES, lactones, pyrrolidone, formamide and sulfoxidov, to obtain phase separation a nonpolar phase containing the above-mentioned catalyst, optionally free organophosphorus ligand and called nonpolar solvent and a polar phase containing named one or more products and a polar solvent, and (2) the Department called the polar phase from the named non-polar phase, and named the organophosphorus ligand and named one or more products have the distribution coefficient between the nonpolar solvent and the polar solvent of greater than about 5, and named one or more products is the distribution coefficient between the polar solvent and the nonpolar solvent of greater than about 0.5
The invention relates to a method of producing crystallization dicarboxylic acids from a solution containing not less than one organic dicarboxylic acid, by adding to the solution until crystallization or during crystallization, at least one anionic polyelectrolyte with a molecular weight of at least 2,000, preferably from 100000 to 500000, in the amount of from 0.01 to 200 h

FIELD: improved processes catalyzed by complexes of a metal- organophosphorous ligand.

SUBSTANCE: the invention presents the improved processes catalyzed by complexes of metal-organophosphorous ligand. The method of extraction includes: feeding of the indicated liquid reactionary product in the zone of separation, stirring of the indicated liquid reactionary product with production by separation of phases of a polar phase containing one or several unreacted reactants, a complex catalyst metal- organophosphorous ligand, not obligatory free organophosphorous ligand and one or several polar dissolvents; and a nonpolar phase containing one or several products of decomposition of the organophosphorous ligand, one or several by-products of the reaction and one or several products. Further the method provides for the stages of withdrawal from the zone of separation and feeding into the reaction zone and-or into the zone of separation. In the given method selectivity of the polar phase for the organophosphorous ligand concerning one or several products is expressed by a ratio of distribution coefficients Efl, which has a value more than approximately 2.5; (ii) the selectivity of the polar phase for the organophosphorous ligand concerning one or several decomposition products of the organophosphorous ligand is expressed by a ratio of distribution coefficients Ef2, which has a value more than approximately 2.5; and (iii)the selectivity of the polar phase for the organophosphorous ligand concerning one or several by-products of reaction is expressed by a ratio of distribution coefficients Ef3, which value is more, than approximately 2.5. The method allows to reduce a negative effect on the process, for example, on prevention of a decrease of efficiency of the catalyst, conversion of the initial material and selectivity by a product.

EFFECT: the invention ensures reduction of a negative effect on the process, on efficiency of the catalyst, on conversion of the initial material and selectivity by a product.

20 cl, 2 tbl

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