Method of producing organic hydroperoxide, industrial installation for said production and method where said organic hydroperoxide is used to produce alkylene oxide

FIELD: chemistry.

SUBSTANCE: disclosed is a method of producing organic hydroperoxide involving: a) oxidation of an organic compound to obtain an organic reaction product containing organic hydroperoxide; b) mixing at least a portion of the organic reaction product from step (a) with a basic aqueous solution to obtain a mixture of basic aqueous solution and an organic reaction product; c) separating the mixture from step (b) to obtain a separated organic phase containing organic hydroperoxide, and a separated aqueous phase; d) mixing at least a portion of the separated organic phase from step (c) with water to obtain a mixture of aqueous and organic phases; and e) separating the mixture from step (d) to obtain a separated organic phase containing organic hydroperoxide and a separated aqueous phase in separation of the organic phase and the aqueous phase at step (e) is carried out using a coagulator containing glass fibre. The invention also discloses a method of producing alkylene oxide where said organic hydroperoxide is used, as well as an industrial installation for realising said method.

EFFECT: improved removal of impurities of basic materials.

9 cl, 3 dwg, 2 tbl, 26 ex

 

Technical field of invention

The present invention relates to a method for producing an organic hydroperoxide, industrial setting for getting to the way in which the organic hydroperoxide to prepare accelerated.

Prior inventions

The U.S. patent And 5883268 describes a method of producing propylene oxide, which includes paraxylylene ethylbenzene. With the reaction mixture of reaction paraxylylene can interact with aqueous base in a quantity sufficient to neutralize acidic components. In the future, the final mixture can be divided into two phases: water and organic (hydrocarbon). The organic phase, which contains a number of grounds, can be rinsed with water in order to separate the core material. In the method of U.S. patent-And-5883268 water evaporated from the organic phase.

Patent WO-A-03/066584 describes a method of obtaining a product containing alcylaryl hydroperoxide. In this way the aqueous phase must be separated from the hydrocarbon phase. The division in the patent WO-A-03/066584 partially can be performed using the coagulator.

The presence of residual basic materials such as sodium salt, in an organic phase comprising an organic hydroperoxide, may gustavstrasse during subsequent processing of the organic hydroperoxide.

Improved removal of such basic materials, in addition, allows to use a higher amount of base to neutralize any acidic components in the reaction mixture, the reaction paraxylylene. So also may be the improvement of the efficiency of removal of the base material is improved removal of acid components.

Thus, it is desirable to provide an improved method for the preparation of organic hydroperoxide, which can be improved removal of basic materials.

The invention

It was found that the removal of basic materials can be improved by separation of the aqueous and organic phases by using a coagulant containing fiberglass. It has been unexpectedly found that fiberglass work well in the harsh environment of the method according to the invention, and while there is a slight corrosion. Accordingly, the present invention provides a method of obtaining organic hydroperoxide, which includes:

a) oxidation of organic compounds for organic reaction product containing organic hydroperoxide;

(b) mixing at least part of the organic reaction product from stage (a) with a basic aqueous solution to obtain a mixture of the basic aqueous solution and the organic reaction product;

(c) separating the mixture of stage (b) to obtain the separated organic phase containing organic hydroperoxide, and the separated aqueous phase;

(d) mixing at least part of the separated organic phase from step (c) with water to form a mixture of aqueous and organic phases; and

(e) separating the mixture of stage (d) to obtain the separated organic phase containing organic hydroperoxide, and the separated aqueous phase;

in which the separation of the separated organic and the separated aqueous phase at the stage (e) is performed using a coagulant containing glass fiber.

Fiberglass is mainly used in ways in which they are subjected to contact with a strongly basic or acidic compounds due to possible corrosion of the fibers. Therefore, it is very unexpected that fiberglass work well in this way.

In addition, the use of optical fibers allows to limit the time and space required for the separation of organic and aqueous phases. In the past, this separation of organic and aqueous phases required the installation, including individual sedimentary camera with subsequent separation vessel, including possible coagulating means. The present invention makes it possible to use only the separation vessel, including koaguliruut the e means and the area of deposition, so that didn't need any separate previous sedimentary camera before entering into the separation vessel.

Organic hydroperoxide obtained by the method according to the invention can preferably be used in the method of producing accelerated, which includes the preparation of the organic phase containing organic hydroperoxide according to the aforementioned method, and a further stage of contacting at least part of the obtained organic phase containing organic hydroperoxide, with alkene with getting accelerated and organic alcohol.

In addition to the above, the present invention further proposes an industrial installation for the removal of basic materials from the organic phase containing organic hydroperoxide, which (installation) includes a mixer for mixing the organic phase with water; and separating vessel, associated directly or indirectly with a mixer for separating the mixture obtained in purified organic phase containing organic hydroperoxide, and the aqueous phase; where the mixer is a static mixer, and the separation vessel includes one or more samples containing glass fiber.

Figures

The invention is illustrated by the following figures.

Figure 1: Industrial mustache is the time for the method according to the invention.

Figa: fiberglass before use according to the present invention (new glass).

Figw: fiberglass after use according to the present invention (used fiberglass).

Detailed description of the invention

The organic compound used in the method of the present invention, can, in principle, be any connection. Examples of suitable organic compounds include alcylaryl and tertiary alkyl compounds. Alcylaryl compounds that are most often used are benzene compounds containing at least 1 alkyl substituent, which contains from 1 to 10 carbon atoms, preferably from 2 to 8 carbon atoms. Preferably the compound of the benzene contains an average of from 1 to 2 parts. More preferred alcylaryl compounds are ethylbenzene, cumene and diisopropylbenzene. Tertiary alkyl compounds that can be used include tertiary butane (i.e. the 2-methylpropan). The most preferred organic compound is ethylbenzene. When ethylbenzene is used as the organic compounds, the method can be used for the preparation of ethylbenzene hydroperoxide.

Oxidation of organic compounds at the stage a) of the method according to the finding can be made in any suitable way, known in the prior art. The oxidation is preferably performed by contacting an organic compound with a gas containing oxygen, such as air. The oxidation can be performed in the liquid phase in the presence of a diluent. This diluent is preferably a compound which is in liquid state under the reaction conditions and does not react with the starting materials and the resulting product. However, the diluent may also be a connection, necessarily present during the reaction. For example, if alkylaryl represents ethylbenzene, the diluent may also be ethylbenzene. In a preferred embodiment, the method thus can be used to obtain a solution of ethylbenzene hydroperoxide in ethylbenzene. In a further preferred embodiment, the oxidation product is subsequently concentrated, for example, through instant distillation by boiling.

In addition to the desired organic hydroperoxide during the oxidation of organic compounds produces a wide range of pollutants. Although most organic compounds are present in small quantities, the presence of organic acids, it has been found that sometimes causes problems when further use of organic hydroperoxides. As described in the patent US-A-5883268, the way to reduce contaminants is the contacting of the reaction product containing an organic hydroperoxide with an aqueous solution of an alkali metal (i.e. water based). However, contact with an aqueous solution of an alkali metal introduces some amount of alkali metal in the reaction product containing organic hydroperoxide. Although the amount of organic acids can be reduced by washing, alkali metal, the amount of pollutants alkali metal will increase.

At the stage (b) of the method of the present invention, at least part of the organic reaction product, which contains an organic hydroperoxide, mixed with a basic aqueous solution to obtain a mixture. The result can be neutralized, at least part of the organic acid by-products.

Preferably, essentially all the organic reaction product is mixed with a basic aqueous solution.

Under the blending understand what organic reaction product and a basic aqueous solution in contact with each other in such a way that it turns out their mixture. When mixing can be obtained a large area of the boundary surface between the organic reaction product and an aqueous solution, which provides mass transfer. The mixing stage (b) can the be performed by any means which well-known experts in this area as suitable for this method, including, for example, mixing by means of a static mixer, a mixing tank or by means of fiber in contact with the device.

Preferably used is basically an aqueous solution containing one or more compounds of an alkali metal. Suitable alkaline sources for use in an aqueous solution of the alkali metal include hydroxides, carbonates and bicarbonates of the alkali metal. Examples of these compounds are NaOH, KOH, Na2CO3To2CO3, Panso3and KHCO3. Because of their easy availability, preferably using NaOH and/or Na2CO3. The amount of alkali metal present in an aqueous solution of an alkali metal, can be widely changed. Preferably used in the concentration of the alkali metal from 0.01 to 25% wt./mass., and more preferably the concentration of the alkaline metal from 0.1 to 10% wt./mass. in the calculation on the entire aqueous solution.

In a preferred embodiment, stage (b) comprises dispersing a basic aqueous solution in at least part of the organic reaction product so that the mixture was a dispersion of droplets of the basic aqueous solution into the organic phase.

At the stage (c) the mixture obtained in stage b), separated into an organic phase containing organic hydroperoxide, and the aqueous phase. The separation may be performed by any means known to specialists in this field of technology. Preferably the separation is performed by separation of the phases, for example, using sediment chambers.

At stage (d), at least part of the separated organic phase from the previous phase is washed with water. More preferably, essentially all of the organic phase obtained in the previous phase is washed with water. Water may be clean, but preferably it is at least partially from the wastewater. Washing, mainly will be using a combination of fresh water, recycled water and, optionally, additional wastewater obtained in other stages of this method.

This washing is performed by mixing at least part of the organic phase with water to obtain a mixture of aqueous and organic phases in stage (d).

Under the blending understand what organic phase stage (c) and water contact with each other in such a way that it turns out their mix.

In a preferred embodiment, stage (d) comprises a dispersion of water, at least part of the organic phase obtained in stage (c) so that the mixture is produced in the form of a dispersion of water droplets in organic the tion phase.

After that, the mixture of organic and aqueous phase obtained in stage (d), again divided into stages (e).

Depending on the amount of contaminants present in the organic phase containing the organic peroxide, the combination of stages (d) and (e) of the method may be performed either once or repeatedly. In a preferred embodiment, the sequence of stages (d) and (e) are repeated one or more times. By repeating steps (d) and (e) are preferably repeated once or twice, which generally gives a two or three stage washing (d) and phase separation (e).

According to the invention, at least one of the stages (e) is performed using a coagulant containing fiberglass. Preferably all stages (e)present in the method are performed using a coagulant containing glass fiber.

Preferably, stage (d), the preceding stage (e), which uses the coagulator, containing fiberglass, is performed at a specific volume ratio. When stage (e) is performed using a coagulant containing glass fiber, the volume ratio of aqueous phase to organic phase by stage (d) is preferably in the range of from 1:100 to 1:2. More preferably the volume ratio in the stage (d) is in the range from 1:10 to 1:3, most preferably in the range of 18 to 1:4.

The mixing stage (d) may be performed by any means known to the specialists in this area as suitable for this method, including, for example, mixing by means of a static mixer, a mixing tank or by means of fiber in contact with the device. In the preferred embodiment, however, the organic and aqueous phase are mixed in a controlled manner with sufficient turbulence. Preferably therefore, the organic phase contacts the water at the stage (d) through a static mixer.

The mechanism of mixing in the static mixer is different from the mechanisms in other types of mixers, such as, for example, the mixing VAT. Static mixers provide a longer time of contact between the two phases at high turbulence, and as a result, their help can be obtained a more uniform distribution of droplet size than, for example, by using a mixing VAT. That is, the use of a static mixer leads to a better handling of the mixture and drop size. A static mixer may be any static mixer, well-known experts in this field. Examples of suitable static mixers are described, for example, in the article "Mixing in the process industries" N. Harnby, etc. In a preferred embodiment, assistantance mixer is used in this way, to get the pressure drop across the static mixer, exceeding 0.05, preferably greater than 0.1 bar.

Preferably a static mixer contains in the range of 1 to 30 of the mixing elements, more preferably from 2 to 20 and most preferably from 3 to 12 elements. As shown N. Harnby, and others, the mixing element is essentially a pipe that includes obstacles like walls, which cause intermittent or continuous changes in direction of flow. Obstacles cause intense turbulence. For practical purposes, the elements preferably are placed sequentially, so that the direction was changed from element to element.

The diameter of the static mixer can vary widely. For practical purposes, the diameter of the static mixer varies from 2 mm to 2 m

If it is preceded by a stage (e), which is used coagulator, containing fiberglass, step (d) preferably includes mixing the organic phase and water in such a way and to such an extent that you get a certain amount of drops. More preferably at this stage (d) preparing a dispersion comprising droplets that have Swarovski average droplet size in the range from 30 to 300 micrometers. More preferably, the droplets have Swarovski cf is dni droplet size in the range from 50 to 250 micrometers. Swarovski average droplet size may be determined by the method as described in the article Streiff and other "New Fundamentals for Liquid-Liquid Dispersion Using Static Mixers", MIXING IX, 1997. Then measure the properties of the mixture, such as viscosity, surface tension, density and flow rate, can then be calculated droplet size, for example, by the equation (9), mentioned in this article.

The droplets are preferably water drops dispersed in the organic phase.

Drops with the above average size of the droplets can be mostly obtained using a static mixer.

In a preferred embodiment, stage (e) includes providing the possibility that the organic and aqueous phases were combined, for example, with the formation of large drops in the coagulator, and then providing the phases opportunities into the area of deposition. When using coagulator separation is accelerated. In this case, stage (e) preferably includes:

(1) processing the mixture obtained in stage d) in the coagulator containing glass fiber, to obtain a mixture containing droplets with a larger drop size;

(2) providing a mixture comprising drops with increased size of the droplets obtained in stage (1), the ability to layer in the zone of deposition of obtaining the separated organic phase and separated the Oh aqueous phase;

(3) the removal of organic and aqueous phase from the zone of deposition.

Due to the increase of the drop size due to coalescence first (partial) separation of phases can be obtained at stage (1), allowing for improved separation stage (2). The area of deposition may represent a separate sediment chamber or zone of deposition, built in the same vessel as the coagulator. Preferably use one of the separation vessel, including the coagulator and the area of deposition.

In case of large amount of the flocculating agent may preferably be preceded by an additional area of deposition. In this case, stage e) comprises the additional step of separation (0), at which the mixture is allowed the opportunity to settle in this area for organic and aqueous phase, after which the two phases are separated. Preferably the separated organic phase, still containing dispersed therein a water droplet, then process using coagulant containing glass fibre, at the stage (1).

The use of such additional stages of separation is particularly advantageous when using a higher volume ratio of aqueous phase to organic. Especially advantageous when the volume ratio of aqueous phase to organic phase (d) is in the range from 1:8 to 1:4.

Fiberglass, CA is nimue in the present invention, can be any fiber. It is preferable, however, that the fiber was free from containing phosphorus and/or sulfur additives. It was found that in some cases these additives can lead to increased decomposition of organic hydroperoxide. The preferred glass fiber are fibers made from glass containing less than 1000 mass. hours/million of elemental sulfur based on the total amount of glass. The amount of elemental phosphorus based on the total amount of glass is preferably not more than 1000 mass. hours/million Most preferably the amount of elemental sulfur is not more than 290 mass. hours/million, while, additionally, the number of elementary phosphorus is not more than 250 mass. hours/million

Can be used with any type of optical fibers, known to specialists in this field. Examples of suitable types of glass include glass A-type (i.e. soda-lime silicate glass), glass C-type (i.e. calcium borosilicate glass), glass D-type (i.e. borosilicate glass with a low dielectric constant), glass E-type (i.e. alumosilicate-borosilicate glass with a maximum alkali content of 2% wt./mass.), ECRGLASS ® (i.e. calcium aluminosilicate glass), glass AR-type (i.e. resistant to alkali glass, consisting of shelo the different silicates of zirconium), glass R-type (i.e. calcium aluminosilicate glass and glass S-2-type (i.e. magnesium aluminosilicate glass). Of them prefer glass C-type, ECRGLASS ® and glass R-type because of their resistance to acid corrosion, and particularly preferred AR glass because of its resistance to alkali. In other advantageous embodiments, the implementation used glass E-type. It was found that the advantage that when using glass E-type there is surprisingly little corrosion of the glass.

This is shown in the figures and in the examples.

The thickness of the fibers can vary widely. It is preferable, however, that the diameter of the fibers was in the range of from 0.1 to 50 micrometers. More preferably, the diameter of the fibers was in the range of from 1 to 20 micrometers and more preferably in the range from 5 to 15 micrometers.

In a preferred embodiment, the optical fiber can be woven together with other materials, such as, for example, stainless steel or Teflon fibers. The use of such joint ligaments with, for example, stainless steel or Teflon material is advantageous because of Teflon or stainless steel supports fiber and prevents the seal under the pressure of the flow. Especially preferred is a combination of fine optical fibers, nab the emer having a diameter in the range from 1 to 20 microns, in combination with the more coarse Teflon fibers, for example having a diameter in the range from 20 to 40 microns, or stainless steel fibers, for example having a diameter in the range from 250 to 300 microns.

Optionally, you can also use combinations of layers of different materials. For example, one or more layers consisting of glass fibers, can be connected with one or more layers of another material, or related materials.

Under the coagulator imply a means of facilitating the coalescence of one phase, mixed with another phase. More specifically, under the coagulator can mean funds in which the dispersion is passed through coalescers the environment used for coalescence and separation melkodispersionnyh drops. Under cholesterola environment can be understood environment, which operates by maintaining drops in dispergirovannom condition for quite a long time that they form droplets that are large enough to stratification. In the method according to the invention, the optical fiber can be understood as fiber, which are such cholesterola environment.

The coagulator may, for example, be present in the form coagulating cartridge, that is the container that holds the fibers in certain positions. In another example, the coagulator may prisutstvovatb form coagulating layer, that is knitted, woven or laminated fabrics or fibers, which are installed in the separation vessel, sometimes also called "coagulatory grid.

Coagulator for use in the present invention can be any known coagulator, suitable from the point of view of experts in this field of technology.

The coagulator is often placed in a separation vessel, i.e. a vessel in which can be accomplished by separation of the aqueous and organic phases. Separating vessels, which can be used coagulator include vertical or horizontal vessels. Preferably, a horizontal separator vessel.

One separation vessel may include one or more samples. Preferably one separation vessel contains from 1 to 10, more preferably from 1 to 5 samples.

Such samples can be placed in such a separation vessel by any method known to specialists in this field. For example, such samples can be placed in the separation vessel horizontally, diagonally or vertically. In one preferred embodiment, the samples are arranged essentially vertically, whereas a mixture of organic and aqueous phase flows through the coalescers essentially in a horizontal direction across the essentially horizontal separation vessel. In another preferred embodiment, the samples are essentially horizontally, whereas a mixture of organic and aqueous phase flows through the coalescers essentially in a vertical direction through an essentially vertical separation vessel.

Coalescers can be located anywhere within the separation vessel, for example in the part upstream horizontal separation vessels, along the entire length of the horizontal separator vessel or in part, downstream of a horizontal separator vessel. In a preferred embodiment, at least one coagulator placed essentially vertically throughout the length of the essentially horizontal separation vessel. In a particularly preferred embodiment, the separation vessel is an essentially horizontal separation vessel comprising one or two coagulator over the whole cross section of the separation vessel located essentially vertically above the flow in the separation vessel; and further comprising one or two coagulator on the part of the cross-section of the separation vessel located essentially vertically below the flow in the separation vessel. Coalescers, located downstream in the separation vessel, preferably Animat space from the top of the separation vessel to less than 9/10, preferably less than 4/5 and more preferably less than 2/3 of the height of the separation vessel, leaving an open passage at the bottom of the separation vessel.

The separation vessel may contain a coagulant, for example, in the form coagulatory grid or coagulating cartridge. The cartridges can be advantageous, if the desired large area of contact. The large contact area provides a low flow rate.

Examples of suitable samples are described, for example, in "Liquid-Liquid coalescer Design Manual” ACS Industries, LP, Houston, Texas, USA.

In the separation vessel can be used one or more coagulating grids or cartridges. For example, the separation vessel can include a combination of the first and second coagulating nets associated with each other in the front part of the separation vessel, and the combination of the third and fourth coagulatory nets associated with each other in the second position downstream in the vessel. As stated above, coagulatory mesh and/or cartridges can be used horizontally or vertically.

Optionally, the mixture of organic and aqueous phase may be filtered through a filter before contact with the optical fibers. Such filters generally have openings not more than 20 micrometers, preferably not more than 10 micrometers.

Coagulator for use in the present invention MoE is should be used in the usual way, as is well known to specialists in this field of technology. Common to control the differential pressure across the coagulator during operation. If the differential pressure becomes acceptable, the flocculating agent can be purified, for example, by reverse flushing.

Separation of organic and aqueous phases in stage (e) is preferably performed in a continuous way. Preferably the mixture obtained in stage (d)is fed to the vessel separation stage (e) at a speed in the range from 0.01 to 10.0 cm/s, more preferably in the range of from 0.1 to 3.0 cm/s

The pressure used during the separation, can vary widely. The separation is preferably performed in the liquid phase, preferably at a pressure in the range from 0.01 to 80 bar, more preferably in the range of from 0.1 to 17 bar. Preferably the separation of organic and aqueous phases in stage (e) is performed at a temperature of from 0 to 150°C, more preferably at a temperature in the range from 20 to 100°C and even more preferably in the range from 40 to 8°C. In an advantageous embodiment, the heat can be dissipated from the earlier stages of the process, for example, the heat output of the stages of a) or b), which can be used in stage e).

In a particularly preferred embodiment, cooling is used in stage b) washing with alkali by means of heat exchange with the stage e).

From lannou the organic phase, comprising organic hydroperoxide obtained in stage (e), can be advantageously used in the method of producing accelerated according to the invention.

Alkene used in this method is a preferred alkene containing from 2 to 10 carbon atoms, and more preferably alkene containing from 2 to 4 carbon atoms. The corresponding cooked accelerated preferably contains from 2 to 10 carbon atoms and more preferably from 2 to 4 carbon atoms, respectively. Examples of alkenes that can be used include ethylene, propylene, 1-butylene and 2-butylene, which can be prepared the corresponding ethylene oxide, propylene oxide and builtoutside.

The method according to the invention is particularly advantageous for obtaining propylene oxide. Therefore, the most preferred alkene is propylene, which can be obtained the corresponding propylene oxide.

In the advanced stage (f) of the method, at least part of the organic phase containing organic hydroperoxide obtained by the method described above in the present invention may be contacted with the alkene to obtain accelerated. The organic hydroperoxide is converted to the corresponding alcohol. Preferably this reaction is performed in the presence of a catalyst. P is impactfully the catalyst for such a method comprises titanium on silica and/or silicate. In addition, the preferred catalysts are described in EP-A-345856. The reaction occurs mainly at moderate temperatures and pressures, in particular at temperatures in the range from 25 to 200°C, preferably in the range from 40 to 135°C. the Exact value of the pressure is not critical as long as it satisfies the order to maintain the reaction mixture in liquid form or in the form of a mixture of vapor and liquid. Basically, the pressure can be in the range from 1 to 100 bar, preferably in the range of from 20 to 80 bar.

Accelerated can be separated from the reaction product by any means that is known as the suitable skilled in this technical field. For example, the liquid reaction product can be treated by fractional distillation and/or selective extraction. The solvent, the catalyst and any unreacted alkene or hydroperoxide can be recycled for further use.

Preferably the organic compound for use in the present invention is ethylbenzene, which turns on the stage (f) 1-phenylethanol. If the organic compound is a benzene, such a method is generally further includes: (g) allocation of at least part 1-phenylethanol from the reaction mixture obtained in stage (f), and (h) the conversion of 1-phenylethanol obtained on a hundred is AI (g), in styrene.

Methods that can be used for this step is described in WO 99/42425 and WO 99/42426. However, in principle, can be used by any suitable method known to specialists in this field of technology.

The present invention is further illustrated by the following examples.

Examples 1-13

In the reactor blew air through ethylbenzene. The resulting product was concentrated to obtain a mixture containing approximately 26% of the mass./mass. of ethylbenzene hydroperoxide (EBHP)dissolved in ethylbenzene. Additionally, this mixture was attended by organic acid by-products, containing approximately 66 mass. hours/million formic and acetic acid, 72 mass. hours/million propionic acid and 2843 masses. hours/million benzoic acid.

A mixture containing EBHP neutralized aqueous solution of about 0.5% by weight of sodium hydroxide. Subsequently, the organic and aqueous phases were separated.

The organic phase is brought into contact with the water flow in the installation, as shown in figure 1. Organic phase (containing EBHP dissolved in ethylbenzene) (101) in contact with the water flow (102) and mixed in a static mixer (103). The mixture from the mixer (103), was filed in the horizontal separator vessel (104), including coagulatory layer (105), located vertically in the vessel separation, each coagulatory layer contained fiberglass E-type with a diameter of 10 microns. In the separation vessel and the mixture was separated into a purified stream of the organic phase (106) and an aqueous stream containing a basic residue (107). Part of the water flow processed (108), and the part was removed from the unit through outlet (109). The feed mixture was supplied pure water stream (110). The removal efficiency was determined by measuring the amount (mass. hours/million calculated on the whole mixture) sodium (CNain mixtures lines (101) and (106), respectively, by atomic-absorption spectroscopy and computation efficiency according to the formula below:

[CNa (101)-CNa (106)]/CNa (101)*100 (I)

For each example in table 1 is given the input concentration (mass. h/m) Na and speed of the mixture in line (101). The removal efficiency is also indicated in the table. In addition, table 1 shows the mass ratio of the organic phase (OR), aqueous phase (AQ) and clean water flow for processing (CCC)used in each example; the mass ratio of the organic phase (OR) and aqueous phase (AQ); and type of coagulant. The aqueous phase was dispersible in the organic phase. The average size of the droplets in the aqueous phase was determined by the method described in Streiff and other "New Fundamentals for Liquid-Liquid Dispersion Using Static" Mixers, MIXING IX, 1997. The results are listed in table 1.

Examples 14-25

We used the same set is ka and conditions of the way, as defined in examples 1-13. In this case, however, used several different types of materials coagulator. The results are shown in table 2. Fiberglass E-type had a diameter of approximately 10 microns, whereas that of Teflon fibers had a diameter of approximately 21 microns.

Example 26

In the continuous process according to the present invention performed the following steps.

In the first stage alkaline processing a stream of ethylbenzene hydroperoxide, 26% of the mass./mass., dissolved in ethylbenzene (EBHP solution)containing 0.02 mEq/g of acid was contacted with an aqueous solution of about 0.5% wt./mass. NaOH at a temperature of 60-65°C.

Then the organic and aqueous phases were allowed to settle within 14 minutes of the time of separation in the empty horizontal vessel. The mass ratio of EBHP solution to aqueous solution was 0,22 during contact, the pH of the aqueous phase, leaving an empty horizontal vessel was about 8.

80% wt./mass. the separated aqueous phase comprising an aqueous solution of NaOH was reworked again to communicate with the new EBHP solution. The remaining 20% wt./mass. were merged as wastewater and replaced through the water with the subsequent washing stage and a new alkaline solution comprising 20 wt. -%/mass. NaOH dissolved in water. The organic phase, including the maintenance solution EBHP, coming out of the vessel, contained 59 mass. hours/million of sodium and acid content decreased to 0.003 mEq/g

In the second stage, which is the first stage of leaching, the stream comprising the organic phase from the first stage, mixed with the flow of flush water in the first static mixer, creating a thread, comprising a dispersion of water in the organic phase with a mean droplet size of 150 μm. The dispersion was brought to the first horizontal dividing the vessel. The mixture evenly divided on coagulatory grids, consisting of two layers, one of which was associated with stainless steel wire and fiberglass, and the other was associated with stainless steel wire and Teflon. Each layer had a thickness of 12 inches (30.5 cm), and together these two layers was formed by 24 inches (61 cm) thick coagulating grid.

The organic and aqueous phases were separated. The organic phase is conducted through the second coagulating grid, consisting of two layers, one of which was associated with stainless steel wire and fiberglass, and the other was associated with stainless steel wire and Teflon. Each layer had a thickness of 12 inches (30.5 cm), and together these two layers was formed by 24 inches (61 cm) thick coagulating grid.

90% of the mass./mass. the separated aqueous phase was recycled into the circulation flow to it again precontractual with novoiolchanskai phase in the first static mixer. The remaining 10% wt./mass. the water supplied to the first static mixer compensated for due to the flow of wash water leaving the second horizontal separation vessel. The flow of the organic phase leaving the first horizontal dividing the vessel, contained 3.5 wt. hours/million of sodium.

At the third stage, which is the second washing stage, the flow of the organic phase from the previous washing stage was mixed with an incremental flow of flush water in the second static mixer, creating a thread, comprising a dispersion of water in the organic phase with a mean droplet size of 150 μm. The dispersion was introduced in the second horizontal separation vessel. Dispersed flow is evenly distributed on coagulatory grid, consisting of two layers connected together by stainless steel wire and fiberglass. Each layer had a thickness of 12 inches (30.5 cm), and together these two layers was formed by 24 inches (61 cm) thick coagulating grid.

Organic and aqueous phase were separated. The organic phase is conducted through the second coagulating grid, consisting of two layers connected together by stainless steel wire and fiberglass. Each layer had a thickness of 12 inches (30.5 cm), and together these two layers was formed by 24 inches (61 cm) thick coagulating grid.

90% of the mass./mass. the separated aqueous phase recircula is whether in the circulation flow, so again he precontractual with the new organic phase in the second static mixer and a flow of 10% wt./mass. recycled into the first static mixer in the second stage. The remaining 10% wt./mass. water in the second static mixer was filled with the flow of new wash water. Mass phase ratio of organic phase to fresh water was 25.3:1.

The flow of the organic phase leaving the second horizontal separation vessel, contained 0.02 mass. hours/million of sodium.

Complete the effective removal of acids in these subsequent stages were 85%and a removal efficiency of sodium in the United stages of water washing was of 99.97%.

Table 1
Examples 1-13
Etc.Whodont. Na (mass. hours/million)Linear velocity (cm/s)OR:AQ:CCCThe ratio of AQ:or SIGThe droplet sizeThe type of coagulantRemoval efficiency (%)
123,60,86400:50:151:1043 glass96,2
224,20,86400:50:151:1095glassto 97.1
324,90,86400:50:151:10200glass93,6
4to 19.90,61280:33:01:10305glass88,6
518,80,47220:30:01:10406glass85,1
6160,48220:30:151:887glassto 91.1
726,20,48220:30:151:8191glass94,4
819,80,60280:38:191:8305glass91,4
9210,48220:30:151:8405glass85,4
1017,70,73320:67:01:556glass96,9
1119,60,73320:67:121:5122glass98,0
1219,60,75 320:80:121:5255glass97,9
1323,30,65280:63:121:5300glass94,8

Table 2
Examples 14-25
Etc.Whodont. Na (mass. hours/million)Linear velocity (cm/s)OR:AQ:CCCThe ratio of AQ:or SIGThe droplet sizeThe type of coagulantEfficiencies of removal (%)
14a 21.50,71400:50:151:10200glass93,6
1528,10,86330:40:151:10 251glass92,4
1618,90,86400:501:10200SS/glass93,9
1718,90,71330:401:10251SS/glass92,6
1819,70,86400:501:10200Teflon/glass93,9
1918,480,71330:401:10251Teflon/glass92,2
20*of 21.20,69320:421:8260Teflon 85,8
2119,40,69320:421:8260glassfor 91.3
22*19,30,68320: 351: 10124Teflon89,4
2322,40,68320: 351: 10124glass91,8
24*20,40,68320: 351: 1056Teflon90,1
2518,80,68320: 351: 1056glass93,5
* Against the positive examples

Example 27, corrosion of glass fibers

In order to determine the extent of corrosion of glass fibers, in the first horizontal dividing the vessel was used fiberglass E-type on the first wash stage, as shown in example 26, in 4 months.

Figa shows fiberglass to their use (fresh fiberglass), and figv shows the glass after use (used fiberglass).

As you can see, essentially, no corrosion was not observed.

1. The method of obtaining alcylaryl hydroperoxide, which includes:
(a) oxidation alcylaryl connection with obtaining organic reaction product containing alcylaryl hydroperoxide;
(b) mixing at least part of the organic reaction product from stage (a) with a basic aqueous solution to obtain a mixture of a basic aqueous solution and the organic reaction product;
(c) separating the mixture from step (b) to obtain the separated organic phase containing alcylaryl hydroperoxide, and the separated aqueous phase;
(d) mixing at least part of the separated organic phase from step (C) with water to form a mixture of aqueous and organic phases; and
(e) separating the mixture from step (d) to obtain the separated organic phase containing alcylaryl hydro is eroxide, and the separated aqueous phase;
in which the mixture obtained in stage (d)is a dispersion comprising droplets having Swarovski the average droplet size in the range from 30 to 300 μm, where the drops are water droplets dispersed in the organic phase; and
the separation of the separated organic phase and the separated aqueous phase at the stage (e) is carried out by means of a coagulant containing glass fiber.

2. The method according to claim 1, in which the sequence of stages (d) and (e) repeating one or more times.

3. The method according to claim 1 or 2, in which the volume ratio of aqueous phase to organic phase by stage (d) is in the range from 1:100 to 1:2.

4. The method according to claim 1 or 2, in which the glass are glass fiber, having a diameter in the range from 1 to 20 microns.

5. The method according to claim 1 or 2, in which the mixing stage (d) is performed by means of a static mixer.

6. The method of producing accelerated, which includes the preparation of the organic phase containing alcylaryl hydroperoxide, according to the method according to any one of claims 1 to 5; and the subsequent stage (f) to contact at least part of the obtained organic phase containing alcylaryl hydroperoxide, with alkene with getting accelerated and organic alcohol.

7. The method according to claim 6, in which the contact organic f is PS, containing alcylaryl hydroperoxide, with the alkene in the presence of a catalyst of titanium on silica and/or silicate.

8. The method according to claim 6 or 7, in which alcylaryl connection is an ethylbenzene, and alcylaryl hydroperoxide ethylbenzol hydroperoxide, and which further includes:
(g) separating at least part 1-phenylethanol from the reaction mixture obtained in stage (f), and
(h) the conversion of 1-phenylethanol obtained in stage (g), styrene.

9. Industrial unit for the removal of basic substances from the organic phase containing alcylaryl hydroperoxide, which includes a mixer for mixing the organic phase with water; and separating vessel, associated directly or indirectly with a mixer, to separate the mixture to clean the organic phase containing alcylaryl hydroperoxide, and the aqueous phase; where the mixer is a static mixer, and the separation vessel includes one or more samples containing fiberglass.



 

Same patents:

FIELD: chemistry.

SUBSTANCE: invention relates to a method of recycling wastes from catalytic epoxidation of olefins using organic hydroperoxides, which involves extraction and treatment of the heavy epoxidate fraction with an alkali solution and treatment of the resultant spent alkaline stream with an extractant. The invention proposes addition of a ligand which forms a molybdenum organometallic complex to the spent alkaline stream and extraction from the spent alkaline stream of a fraction containing propylene glycol, acetophenone, ethylbenzene, phenol, methyl phenyl carbinol and the molybdenum organometallic complex formed, treatment with an extractant at T≥Tcr and P≥Pcr with subsequent splitting of the extract into fractions through stepped reduction of pressure from Pextr to P<Pcr with number of pressure reduction steps equal to the number of fractions of the components which should be obtained, taking into account the molybdenum organometallic complex, where Tcr, Pcr are critical temperature and pressure values of the extractant and Pextr is extraction pressure.

EFFECT: maintaining high degree of extracting molybdenum from the spent alkaline stream regardless of its composition and possibility of extracting fractions of components contained in the spent alkaline stream.

1 dwg, 3 tbl, 8 ex

FIELD: chemistry.

SUBSTANCE: invention is related to combined method, which combines olefin epoxidation with preparation of cyclohexanone and cyclohexanol, which are intermediate for production of adipic acid or caprolactam - nylon precursors. Usually cyclohexanone and cyclohexanol are produced by oxidation of cyclohexane with production of cyclohexylhydroperoxide, which is then removed or decomposed. However, in this invention intermediate compound, cyclohexylhydroperoxide is used as oxidant for olefin epoxidation with valuable product making in this process. In process of epoxidation catalyst is used, which contains transition metal and amorphous porous inorganic oxide, which has disorderly interconnected mesopores. The specified mesopores account for at least around 97 volume percents from total volume of mesopores and micropores. Specified porous inorganic oxide has specific area surface from 400 to 1100 m2/g.

EFFECT: porous inorganic oxide is characterised by X-ray picture, having peak from 0,5 to 3,0 degrees 2θ.

13 cl, 5 dwg, 11 ex

FIELD: chemistry.

SUBSTANCE: invention refers to method of alkylen oxide production as involving (i) mixing the original raw stock containing organic hydroperoxide and alken with and recycled flow to prepare the reaction mixture containing alcohol 5 to 80 wt % per total amount of the reaction mixture; (ii) contacting the reaction mix and the heterogeneous epoxidation catalyst to make the flow containing alkylen oxide and alcohol; and (iii) recycling the flow 30 to 95 wt % from the stage (ii) to the stage (i).

EFFECT: method improvement.

9 cl, 1 ex

FIELD: chemistry.

SUBSTANCE: method involves treatment of heavy olefin fraction by an alkali solution, processing of obtained discharge alkali flow by extragent, and further precipitation of molybdenum trisulfide by precipitator. According to invention, sodium hydrosulfide is applied as molybdenum trisulfide precipitator. The method allows regulation of molybdenum trisulfide precipitator feed, reduction of precipitation reactor dimensions and energy consumption of heating and stirring, significant reduction waste and hydrogen sulfide discharge at high molybdenum extraction degree of 90.5-97.6%.

EFFECT: improved method of molybdenum extraction from products of catalytic olefin epoxidation by organic hydroperoxides.

6 ex

FIELD: organic chemistry, chemical technology.

SUBSTANCE: invention relates to a method for synthesis of alkylene oxides. Method involves contacting organic hydroperoxide and alkene with a heterogeneous epoxidation catalyst and removal of products flow containing alkylene oxide and alcohol. Fresh catalyst contacts with a feeding mixture taken in the mole ratio of alkene to organic hydroperoxide by at least 1.2-fold more as compared with their the mole ratio in the usual regimen of work. Invention allows enhancing the catalytic activity of catalyst and conversion of hydroperoxide.

EFFECT: improved method of synthesis.

5 cl, 2 ex

FIELD: organic chemistry, chemical technology.

SUBSTANCE: invention relates to a method for synthesis of styrene. At the first step the method involves interaction of ethylbenzene hydroperoxide with propene in the presence of catalyst to yield propylene oxide and 1-phenylethanol followed by separate treatment of reaction flow and removing propylene oxide. At the second step the method involves interaction of 1-phenylethanol-containing distillate with a heterogenous dehydration catalyst at temperature 150-320°C to obtain styrene. Distillate contains 0.30 wt.-%, not above, compounds of molecular mass at least 195 Da. Invention provides decreasing the content of by-side compounds in styrene and to enhance it's the conversion degree.

EFFECT: improved method of synthesis.

3 cl, 3 tbl

FIELD: organic chemistry, chemical technology.

SUBSTANCE: invention relates to method for synthesis of alkylaryl peroxide-containing compound. Method involves the following steps: (a) oxidation of alkylaryl compound to yield the alkylaryl hydroperoxide-containing reaction substance; (b) treatment of at least part of the reaction substance containing alkylaryl hydroperoxide synthesized at the step (a) wherein this the reaction product comprises less 0.05% of sodium (by mass); (c) separation of product synthesized at the step (b) for hydrocarbon phase containing alkylaryl hydroperoxide and an aqueous phase; (d) repeating steps (b) and (c) by one or some time being optionally. Also, synthesis of alkylaryl hydroxide involves the additional treatment step (e) of at least part of hydrocarbon phase containing alkylaryl hydroperoxide synthesized at steps (c) or (d), olefin and a catalyst to yield alkylaryl hydroxide and oxirane compounds, and (f) separation of at least part of oxirane compound from alkylaryl hydroxide. Synthesis of alkenylaryl involves the additional step (g) of dehydration of at least part of alkylaryl hydroxide synthesized at step (f). Invention provides simplifying the technological process resulting to synthesis of improved substance containing alkylaryl hydroperoxide from which alkylaryl hydroxide is prepared followed by preparing alkenylaryl.

EFFECT: improved method of synthesis.

11 cl, 1 tbl, 6 ex

FIELD: industrial organic synthesis.

SUBSTANCE: invention relates to production of alkylaryl hydroperoxides useful as starting material in production of propylene oxide and alkenylaryl. Process of invention comprises following stages: oxidation of alkylaryl compound to form reaction product containing alkylaryl hydroperoxide; contacting at least part of reaction product with basic aqueous solution; separation of hydrocarbon phase containing alkylaryl hydroperoxide from aqueous phase; containing at least part of above hydrocarbon phase with aqueous solution containing waste water, said aqueous solution containing less than 0.2% alkali metal and/or salt (determined as ratio of metal component to total amount of solution); and separation of hydrocarbon phase from aqueous phase. By bringing at least part of above hydrocarbon phase containing alkylaryl hydroperoxide into interaction with propylene and catalyst, alkylaryl hydroxide and propylene oxide are obtained. At least part of propylene oxide is then separated from alkylaryl hydroxide. Dehydration of at least part of alkylaryl hydroxide results in formation of alkenylaryl.

EFFECT: reduced amount of contaminating by-products in alkylaryl hydroperoxide preparation stage.

8 cl, 4 ex

FIELD: organic chemistry, chemical technology.

SUBSTANCE: invention relates to a method for interaction of an organic compound with hydroperoxide. Invention describes a continuous method of interaction of organic compound comprising at least one C-C-double bond with hydroperoxide in the presence of a catalyst. Method involves interaction of organic compound at the reaction step (R1) under the range of the own pressure below 100 bars, temperature in the range 0-120°C and in the molar ratio of reacting organic compound to hydroperoxide in the range 0.7-20 with hydroperoxide in the presence of a zeolite-containing catalyst to yield at least one flow of the product (P1). Then at least one flow of the product (P1) is fed to intermediate treatment (Z1) wherein (Z1) forms at least one the hydroperoxide-containing product flow (PZ1) and wherein the intermediate treatment represents distillation separation of hydroperoxide from at least one the product flow (P1) or addition of a base to at least one the product flow (P1) and at least one the product flow is fed to at least in the reaction step (R2) wherein under pressure in the own pressure up to 100 bars, temperature in the range 0-120°C and in the molar ratio of the reacting organic compound to hydroperoxide in the range 0.7-20 hydroperoxide is subjected for interaction with an organic compound in the presence of a zeolite-containing catalyst to yield at least one the product flow (P2) wherein at least one of reaction steps (R1) and (R2) the method involves using the reactors system comprising at least two reactors joined in parallel. Also, invention describes a device for carrying out the interaction of an organic compound with hydroperoxide.

EFFECT: improved method for interaction.

9 cl

FIELD: organic chemistry, chemical technology.

SUBSTANCE: invention proposes a method for synthesis of oxirane compounds comprising the following steps: (i) oxidation of alkylaryl wherein alkyl substitute comprises from 2 to 10 carbon atoms to yield alkylaryl hydroperoxide; (ii) contacting at least part of alkylaryl hydroperoxide prepared at the step (i) with olefin at the temperature range 0-200°C and under pressure in the range 1-100 x 105 H/m2 in the presence of a catalyst comprising titanium on silicon dioxide and/or silicate to yield oxirane compound and alkylaryl hydroxyl; (iii) optional interaction of at least part of alkylaryl hydroperoxide prepared at the step (i) to yield phenol and ketone; (iv) separation of oxirane compound from the reaction product from the step (ii0, and (v) contacting at least part of the reaction product no containing oxirane with hydrogen at temperature 100-330°C and under pressure 0.1-50 x 105 H/m2 in the presence of the hydrogenation catalyst to yield alkylaryl and at least part of the latter is re-circulated to the step (i) wherein the hydrogenation catalyst represents catalyst comprising copper compound, zinc compound and at least one compound chosen from the group consisting of aluminum, zirconium, magnesium rare-earth metals and their mixtures. Invention provides the possibility for synthesis of oxirane compounds without necessity for simultaneous synthesis of other compounds.

EFFECT: improved method of synthesis.

5 cl, 7 ex

FIELD: chemistry.

SUBSTANCE: invention relates to a method of producing cyclic geminal bis-hydroperoxides from ketones with ring size C12-C15 used to produce 1,2,4,5-tetraoxanes having high anti-parasitic activity. Cyclic geminal bis-hydroperoxides can also be used as radical polymerisation initiators. The disclosed method of producing C12-C15 cyclic geminal bis-hydroperoxides involves reaction of corresponding C12-C15 cycloalkanones with hydrogen peroxide in the presence of boron trifluoride in an ether medium in molar ratio C12-C15 cycloalkanone:boron trifluoride:hydrogen peroxide equal to 1:0.8-1.2:7-12.

EFFECT: method enables to obtain C12-C15 cyclic geminal bis-hydroperoxides in a single step and simplifies and lowers the cost of the process, cuts reaction time, as well as labour, material- and power consumption when producing bis-hydroperoxides; method enables to obtain desired products with high output and high selectivity.

1 cl, 1 tbl, 8 ex

FIELD: chemistry.

SUBSTANCE: invention relates to the technology of producing peroxyacids which can be used in delignification and bleaching cellulose materials in the textile industry. The method of preparing a peroxyacid solution for delignification and bleaching involves reaction of acetic acid and hydrogen peroxide in equimolar amounts in the presence of an acid catalyst - sulphuric acid and organophosphonate-nitriletrimethylene phosphonic acid with ozonation, with ozone consumption of 1-4 g/h.

EFFECT: high output of peroxyacid and high efficiency during delignification and bleaching.

1 cl, 2 tbl

FIELD: chemistry.

SUBSTANCE: invention relates to synthesis of hydroperoxides of alkylaromatic hydrocarbons which can serve as a source of oxygen-containing organic compounds (phenol, methylphenols, acetone, cyclohexanone etc) and as an initiator of emulsion polymerisation of unsaturated hydrocarbons. The invention discloses a method for synthesis of hydroperoxides of alkylaromatic hydrocarbons through liquid-phase oxidation of these hydrocarbons with atmospheric oxygen at atmospheric pressure, process temperature of 110-130°C, for 1-3 hours in the presence of a 4-methyl-N-hydroxyphthalimide catalyst in amount of 1.0-2.0 wt %.

EFFECT: catalyst prevents use of an initiator and alkaline additives, which considerably simplifies the process, higher conversion of initial alkylaromatic hydrocarbons while preserving high selectivity of the process.

2 tbl, 2 ex

FIELD: chemistry.

SUBSTANCE: invention relates to a method of producing isopropyl benzene hydroperoxide (IPB HP) which is then used to produce phenol and acetone using what is known as industrial cumol method. According to the invention, isopropyl benzene hydroperoxide is obtained by oxidising isopropyl benzene with molecular oxygen. The catalyst used is iron nanopowder with specific surface area of 6.9 m2/g, obtained through electrical explosion of a conductor in a nitrogen atomsphere. The process is carried out at 50-60°C.

EFFECT: increased output of isopropyl benzene hydroperoxide.

1 cl, 3 ex

FIELD: chemistry.

SUBSTANCE: invention relates to petrochemical industry and can be used in combined production of styrene and propylene oxide. Ethylbenzene hydroperoxide is obtained in accordance with the invention by oxidising ethylbenzene with atmospheric oxygen in a continuous reactor at atmospheric pressure in the presence of N-hydroxyphthalimide as a catalyst in amount of 0.5-3 wt % and temperature of the process of 125-130°C until achieving content of ethylbenzene hydroperoxide of 19.2%.

EFFECT: increased conversion of ethylbenzene and selectivity of the process.

1 cl, 1 ex

FIELD: chemistry.

SUBSTANCE: present invention relates to a method of continuous oxidation of saturated cyclic hydrocarbons using oxygen, into a mixture of hydroperoxide, alcohol and ketones. The method involves feeding into the lower part of a column and in parallel flow, a stream of oxidisable liquid hydrocarbon and a gas stream containing oxygen, and degassing the liquid phase in the upper part of the column by forming a gas dome and extraction of the degassed liquid phase. The gas containing oxygen is let into different compartments of the column, and into the dome and/or liquid phase at the level of the degassing zone, or directly above. A stream of non-oxidising gas with output sufficient for maintaining concentration of oxygen in the gas layer at the level of volume concentration, less than or equal to the upper limiting concentration of oxygen is supplied.

EFFECT: possibility of implementing a method with high selectivity on an explosion safe level.

9 cl, 1 dwg, 1 ex

FIELD: chemistry.

SUBSTANCE: invention concerns method of isopropylbenzene hydroperoxide (IPBHP) concentration, applied in phenol and acetone production by isopropylbenzene method. The claimed method involves feed of oxidate for rectification into a vessel with gas phase separation in top part or into condensers of rectification columns.

EFFECT: reduced load on columns, enhanced column efficiency, reduced loss of IPBHP with distillate, power saving.

3 cl, 2 dwg, 3 tbl, 3 ex

FIELD: organic chemistry, chemical technology.

SUBSTANCE: invention relates to method for synthesis of alkylaryl peroxide-containing compound. Method involves the following steps: (a) oxidation of alkylaryl compound to yield the alkylaryl hydroperoxide-containing reaction substance; (b) treatment of at least part of the reaction substance containing alkylaryl hydroperoxide synthesized at the step (a) wherein this the reaction product comprises less 0.05% of sodium (by mass); (c) separation of product synthesized at the step (b) for hydrocarbon phase containing alkylaryl hydroperoxide and an aqueous phase; (d) repeating steps (b) and (c) by one or some time being optionally. Also, synthesis of alkylaryl hydroxide involves the additional treatment step (e) of at least part of hydrocarbon phase containing alkylaryl hydroperoxide synthesized at steps (c) or (d), olefin and a catalyst to yield alkylaryl hydroxide and oxirane compounds, and (f) separation of at least part of oxirane compound from alkylaryl hydroxide. Synthesis of alkenylaryl involves the additional step (g) of dehydration of at least part of alkylaryl hydroxide synthesized at step (f). Invention provides simplifying the technological process resulting to synthesis of improved substance containing alkylaryl hydroperoxide from which alkylaryl hydroxide is prepared followed by preparing alkenylaryl.

EFFECT: improved method of synthesis.

11 cl, 1 tbl, 6 ex

FIELD: industrial organic synthesis.

SUBSTANCE: invention relates to production of alkylaryl hydroperoxides useful as starting material in production of propylene oxide and alkenylaryl. Process of invention comprises following stages: oxidation of alkylaryl compound to form reaction product containing alkylaryl hydroperoxide; contacting at least part of reaction product with basic aqueous solution; separation of hydrocarbon phase containing alkylaryl hydroperoxide from aqueous phase; containing at least part of above hydrocarbon phase with aqueous solution containing waste water, said aqueous solution containing less than 0.2% alkali metal and/or salt (determined as ratio of metal component to total amount of solution); and separation of hydrocarbon phase from aqueous phase. By bringing at least part of above hydrocarbon phase containing alkylaryl hydroperoxide into interaction with propylene and catalyst, alkylaryl hydroxide and propylene oxide are obtained. At least part of propylene oxide is then separated from alkylaryl hydroxide. Dehydration of at least part of alkylaryl hydroxide results in formation of alkenylaryl.

EFFECT: reduced amount of contaminating by-products in alkylaryl hydroperoxide preparation stage.

8 cl, 4 ex

FIELD: organic chemistry, chemical technology.

SUBSTANCE: invention proposes a method for synthesis of organic hydroperoxide comprising the reduced amount of impurities. Method involves the following steps: (a) oxidation of organic compound to yield the reaction product comprising organic hydroperoxide; (b) contacting at least part of the reaction product comprising organic hydroperoxide with the basic aqueous solution; (c) separation of hydrocarbon phase containing organic hydroperoxide from an aqueous phase; (d) washing out at least part of the separated hydrocarbon phase containing organic hydroperoxide, and (e) contacting at least part of hydrocarbon phase containing organic hydroperoxide with a protective layer comprising a solid adsorbent wherein a solid adsorbent shows porosity 50-98% by volume. Except for, invention proposes a method for preparing oxirane compound from hydrocarbon phase obtained at the step (e) by the method described above and containing alkylaryl hydroperoxide. The presence of the protective layer reduces the pressure increment in the catalyst layer that is caused by the declined content of impurities in the raw comprising alkylaryl hydroperoxide.

EFFECT: improved preparing method.

7 cl, 2 ex

Oil desalting unit // 2427410

FIELD: process engineering.

SUBSTANCE: invention relates to petroleum industry, in particular, to additional separation of oil from chlorine salts by forcing fresh water there through. Desalting unit is made up of oil pipeline section with flange joints. Unit body central section is equipped with L-shaped branch pipe to force water therein. Branch pipe end face represents hemisphere provided with wear resistant nozzles. Said L-like branch pipe is directed toward oil flow. Stationary vane grids are arranged ahead and behind of said branch pipe to divide water into ultimate particles and swirl oil along pipeline axis in carious directions.

EFFECT: production of commercial oil with stably low content of chlorine salts.

2 cl, 2 dwg

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