Method for epoxidation of olefins

FIELD: organic chemistry, chemical technology.

SUBSTANCE: invention relates to a method for catalytic epoxidation of (C2-C6)-olefins with hydrogen peroxide. Method is carried out in the flow-type reaction system of continuous effect wherein the reaction mixture is passed through a immobile catalytic layer inside of reactor fitted with a cooling device and in simultaneous maintaining the temperature profile into the reactor wherein the cooling medium temperature in the cooling agent is at least 40°C and the maximal temperature inside of the catalytic layer is 60°C, not above. Invention provides improving the conversion degree and selectivity of the product by using the conventional systems.

EFFECT: improved method of synthesis.

12 cl, 1 tbl, 7 ex

 

Description of the prior art

From EP-A 100119 known that using hydrogen peroxide propene can be converted into the oxide, propene, if the catalyst is to apply a titanium containing zeolite.

Unreacted hydrogen peroxide from the reaction mixture epoxidation cost-effectively recover impossible. In addition, the presence of unreacted hydrogen peroxide due to the additional effort and costs associated with the treatment of the reaction mixture. Thus, in a preferred embodiment, the process of epoxidation of propene is carried out with the use of an excess of propene, corresponding to the achievement of a high degree of conversion of hydrogen peroxide. In order to achieve a high degree of conversion of hydrogen peroxide is advisable to apply a flow reaction system of continuous action. This reaction system may include one or more tubular flow reactors, or installation with two or more sequentially interconnected reactors with mixed flow. Examples of reactors with mixed flow reactors are tank type mixer, reactor recirculation, the fluidized bed reactor and a reactor with a fixed layer and the recirculation of the liquid phase.

Moreover, like the greater is NSTU reactions oxidation reaction of epoxidation of olefins with hydroperoxides is vysokotekhnologicheskoi. Thus to control the course of the reaction to ensure allocation of sufficient quantity of heat released by an exothermic reaction, it is necessary to take precautions. This problem is especially pronounced in flowing systems with continuous action, employ reactors fixed bed. In addition, more than essential for effective temperature control, the influence of which in the course of the epoxidation reactions determines the degree of conversion and selectivity in the product.

In accordance with a significant number of patent publications, examples of which are ER-AND 230949, EP-A 568336, EP-A 712852, EP-A 757045, JP-A 4-59769, WO 97/47613 and US 5591875, reactions epoxidation of olefins with hydrogen peroxide is carried out in suspensions of titanium containing zeolites as catalyst. In the course of the reaction according to this method of temperature control is less difficult, resulting in these patent documents specified a wide range of acceptable reaction temperatures from -20 to 150°With, so the examples used a temperature in the range of 0 and 85°C.

In EP-A 100119 in addition to reactions in suspension of the catalyst described the use of a tubular flow reactor of continuous operation with a fixed catalytic layer, which is immersed in about ladusaw bath, controlled in the range from 15 to 20°C.

In example 8 of WO 97/47614 described the reaction of propene with hydrogen peroxide using a tubular reactor with a fixed bed, equipped with a cooling water jacket. With thermostat, the temperature of the cooling medium controlled by the interval between 0 and 5°C. the product Yield and selectivity against him for industrial purposes are still insufficient.

As far as applicants are aware, all documents related to the existing level of technology and is dedicated to epoxydecane of olefins with hydrogen peroxide in a tubular reactor with a fixed bed, equipped with cooling means, indicated only coolant temperature, and no information is provided regarding the actual temperature inside the reactor. As is known, for example, from the work of Walter Brötz and others, Technische Chemie I, Weinheim, 1982, s, in case of exothermic reactions, the temperature profile in the cross section of the tubular reactor is characterized by a parabolic shape with increasing temperature from the periphery to the center of the reactor. In addition, the temperature may vary along the axial line of the tubular reactor.

In EP-A 659473 described method of epoxidation, in which process peritonism the flow of the liquid mixture of hydrogen peroxide, solvent and propene passed through maintaining iwny a number of series connected reaction zones with a fixed layers. Inside the reactor temperature control means for heat dissipation, eye-catching individual reaction zones are absent. Thus, each reaction zone can be considered as independent adiabatic reactor. In each reaction zone the reaction is carried out to a partial conversion of each reaction zone liquid reaction mixture is removed, is directed through an external heat exchanger for removal of heat of reaction and then the main part of this liquid phase return in this reaction zone, and a small part of the liquid phase serves in the following area. Simultaneously, gaseous propene together with a mixture liquid of starting materials in parallel flow through the reaction zone with a fixed guide layers in the liquid phase and at the end of this reaction system is extracted, in addition to the liquid reaction mixture, in the form of oxygen-containing gas stream. Although the implementation of such a method, the reaction makes it possible to increase the yield of propene oxide in comparison with that achieved in conventional tubular reactors without temperature control, as described in EP-A 659473, it is, however, associated with considerable additional costs given the complexity of the reaction system is required to implement this method.

From US 5849937 known method of epoxidation of propene using the-W of hydroperoxides, in particular, organic hydroperoxides. The reaction mixture is sent to a cascade of series-connected reactors with a fixed layers with peritonism mode of operation of each individual reactor. Likewise described in EP-A 659473 in each reactor to carry out only a partial transformation and reactors are not equipped with heat exchange means. Likewise described in EP-A 659473 reaction heat assign transmission stream, the exhaust from each reactor through the heat exchanger, after which the reaction mixture is introduced into the next in this series reactor with a porous layer that adds to the complexity of this reaction system.

The disadvantages of reaction systems, which are discussed in EP-A 659473 and US 5849937, are the complexity and, consequently, increased the cost of investments.

Whereas the above-described modern art, the present invention is to develop a method for the epoxidation of olefins, in the exercise which improves the degree of conversion and selectivity in respect of the product in comparison with achievable by WO 97/476-14 and which can be realized with conventional reaction systems.

The object of the invention

This goal is reached by way catalytic epoxidation of olefins with hydrogen peroxide in a flow reaction system is Birmingham continuous action, in which the reaction mixture is passed through a fixed catalyst layer in the reactor equipped with cooling means, while maintaining the inside of the reactor of such a temperature profile in which the temperature of the cooling medium in the cooling means is at least 40°and the maximum temperature inside the catalytic layer does not exceed 60°C.

When creating the present invention, it was found that carrying out the epoxidation reaction in this way to meet the requirement provided according to the invention the temperature profile, optimized balance between degree of conversion and selectivity can be achieved with conventional reaction system. Thanks now available method of epoxidation of olefins with a high degree of conversion of hydrogen peroxide and selectivity in the product at low capital cost, which increases the efficiency of the method in General. Due to the relatively high activation temperature for the reaction of epoxidation in order to achieve economically acceptable degree of conversion process should be at a certain minimum temperature. But, on the other hand, the heat released by an exothermic reaction, the reactor must be effectively take on the Kolka at elevated temperatures occurring adverse reactions, which decreases the selectivity for the product. Maintaining the reactor temperature profile in accordance with the invention a narrow range would give the opportunity to achieve both goals simultaneously.

In EP-A 659473 said that in the conventional tubular reactors the temperature rise in the catalytic layer exceeds 15°whereas in accordance with the examples in EP-A 659473, the growth temperature is not more than 8°and in the preferred embodiment, is equal to 5.5°C. Thus, as described in EP-A 659473 to achieve high values of the yield of propylene oxide inside the catalytic layer, it is necessary to maintain the lowest possible temperature increase. This reduced temperature growth in accordance with EP-A 659473 could only be achieved by conducting the reaction in the individual reaction zone only to a partial transformation, resulting in a large part of the reaction mixture should be returned to the process, and intermediate cooling of the reaction mixture.

But contrary to this assumption superior total product yield in terms of hydrogen peroxide in comparison with the results of the implementation are presented in EP-A 659473 the most preferred options can be obtained, as shown in more detail below in the examples, despite the use of the group in accordance with the present invention a conventional reactor system without intermediate external cooling.

Detailed description of the invention

When performing the present invention can be applied to any reactor, equipped with a fixed catalyst layer and cooling means. In the preferred embodiment, tubular apply, Novotrubny or mnogotarifnye reactors. In the most preferred embodiment used a tubular reactor equipped with a cooling water jacket, because they are usually available at a relatively low cost. As the cooling medium, which is pumped through the cooling means, preferably through a cooling jacket can be used all conventional cooling media like oils, alcohols, liquid salts or water. Preferably the water.

In accordance with the present invention inside the reactor support such a temperature profile in which the temperature of the cooling medium in the cooling medium tubular reactor is at least 40°and the maximum temperature inside the catalytic layer does not exceed 60°C, preferably 55°C. In the preferred embodiment, the temperature of the cooling medium regulating thermostat.

The maximum temperature inside the catalytic layer is measured using a variety of suitable means for measuring temperature, such as thermocouples or sensors Pt-100 posted priblizitelen is along the centerline preferably a tubular reactor at an acceptable distance from each other. The ability to measure temperature in the catalytic layer inside the reactor as a whole with the precision that is needed to control the number of locations inside the reactor and distances between the means of the temperature measurement.

The maximum temperature of the catalytic layer can be adjusted by different means. Depending on the type of reactor maximum temperature of the catalytic layer can be adjusted by regulating the flow rate passing through the reactor the reaction mixture, the regulation of the flow rate of the cooling medium passing through the cooling means, or a loss of catalytic activity, for example by diluting the catalyst with an inert material.

In a preferred embodiment, the flow rate of the cooling medium adjusted so as to maintain the temperature difference between the cooling medium inlet in the cooling means and at the output is less than 5°S, preferably less than 3°S, most preferably less than 2°C.

In accordance with another preferred variant, the reaction mixture was passed through the catalyst layer at a flow rate per unit cross section of the flow from 1 to 100 m/h, preferably from 5 to 50 m/h, most preferably from 5 to 30 m/h Flow rate per cross sectional area of flow is defined as the ratio of the flow rate on the Oka/cross section of the catalytic layer. Therefore, the flow rate per cross sectional area of flow in this tubular reactor can be varied by regulating the speed of flow of the reaction mixture.

In addition, in the preferred embodiment, the reaction mixture is passed through a catalytic layer with an average hourly velocity of the fluid (SCSI) from 1 to 20 h-1preferably from 1.3 to 15 h-1.

The method according to the present invention can be peritonea variant or variant with upward flow, resulting in a more preferred option peritonism thread. In a preferred embodiment of the present invention the process is carried out with maintaining the catalytic layer mode "dripping a thin stream".

In contrast, described in EP-A 659473 the process of transformation in the individual reactor or reaction zone to a limited extent not required and in accordance with the present invention is not preferred. However, in order to be able to carry out the process continuously, when the catalyst for the epoxidation replace and/or regenerate, you can also, if necessary, to use two or more reactors, placed in parallel or in series according to the above.

For implementing the method of epoxidation in accordance with the invention in ka is este catalysts suitable for use crystalline titanium containing zeolites, in particular, the zeolite composition (TiO2)x(SiO2)1-xwhere x represents a number from 0.001 to 0.05, which is characterized by the crystal structure of the MFI or MEL, known as titanosilicate-1 and titanosilicate-2. Such catalysts can be obtained, for example, in accordance with the method described in US 4410501. Titanosilicates the catalyst can be applied in the form of a molded catalyst in the form of granules, extrudates, or other molded apply For opportunities molding process, the catalyst may include from 1 to 99% of the binder or of the material of the carrier, and all acceptable binders and materials carriers in the reaction conditions created for epoxidation, do not interact with hydrogen peroxide or an epoxide. In the preferred embodiment, as catalysts for stationary use layer extrudates with a diameter of from 1 to 5 mm

When performing the present invention in a preferred embodiment, entering the reactor, the total stream comprises an aqueous solution of hydrogen peroxide, olefin and an organic solvent. Thus, these components can be introduced into the reactor in the form of an independent source materials or prior to introduction into the reactor several of these source materials are mixed. In a preferred embodiment, the temperature entering the reactor flow (flow) R is guiraut thus, so it was different from the temperature of the cooling medium is less than X°preferably adjusted to a level that is approximately equal to its temperature.

The application of the method in accordance with the invention allows to epoxidizing any olefins, particularly olefins containing from 2 to 6 carbon atoms each. The method in accordance with the invention is most suitable for the epoxidation of propene to propene oxide. Economic reasons for carrying out the process on an industrial scale, preferably using propene not in pure form and in the form of technical mixtures with propane, which typically contains from 1 to 15 vol.% propane. Propene can be introduced in the reaction system in liquid and in gaseous form.

When implementing the method in accordance with the invention, hydrogen peroxide is used in the form of an aqueous solution containing hydrogen peroxide is from 1 to 90 wt.%, preferably from 10 to 70 wt.%, and particularly preferably from 30 to 50 wt.%. Hydrogen peroxide can be applied in the form of technically available stable solutions. Acceptable non-stabilized aqueous solutions of hydrogen peroxide, such as generated during the implementation antrahinonovye method for producing hydrogen peroxide.

In order to increase the solubility of the olefin, preferably propene, the Jew is th phase, in a preferred embodiment, the reaction is carried out in the presence of a solvent. For use as a solvent suit all solvents that are in the selected reaction conditions, hydrogen peroxide is not oxidized or oxidized only to a low degree and are dissolved in water in amounts greater than 10 wt.%. Preferred solvents are completely mixed with water. Acceptable solvents include alcohols, such as methanol, ethanol and tert-butanol; glycols, such as ethylene glycol, 1,2-propandiol or 1,3-propandiol; cyclic ethers, such as tetrahydrofuran, dioxane or propylene oxide; glycol ethers, such as, for example, etilenglikolevye ether, etilenglikolevye ether, etilenglikolevye ether or propilenglikolmonostearata ether; and ketones, such as acetone or 2-butanone. Especially preferred for use as the solvent methanol.

The pressure inside the reactor is generally maintained at a level of from 5 to 50 bar, preferably from 15 to 25 bar.

In the preferred embodiment, to ensure that significant consumption of hydrogen peroxide olefin is used in excess relative to the hydrogen peroxide, and in the preferred embodiment, the value of the molar ratio of olefin, preferably the e-propene, and hydrogen peroxide is chosen in the range of from 1.1 to 10. When you add a solvent, in the preferred embodiment, the amount of solvent is chosen so that the reaction mixture was attended by only the liquid phase. In a preferred embodiment, the solvent is added to the value of mass attitudes towards the use of hydrogen peroxide solution from 0.5 to 20. The amount of catalyst can be varied within a wide range, and in the preferred embodiment, it is chosen so that the generated reaction conditions during the period from 1 min to 5 h, the consumption of hydrogen peroxide exceeded 90%, preferably more than 95%.

Further, the essence of the present invention are described in more detail with reference to the following examples.

Examples 1 and 2 and comparative examples 1 to 6

All of the examples used titanosilicate catalyst. From titanosilicates powder using a colloidal solution of silicic acid as a binder in accordance with example 5 in EP 00106671.1 was molded 2 mm extrudates. Used H2About2prepared in accordance with antrahinonovye method in aqueous solution with a concentration of 40 wt.%.

Epoxidation was performed continuously in a reaction tube with a volume of 300 ml, with a diameter of 10 mm and a length of 4 Mbale, the equipment included three containers for liquids and associated pumps, as well as the vessel for separating liquid. Three containers for liquids contained methanol, 40%N2About2and propene. The pH value of 40%N2About2ammonia was brought to 4.5. The reaction temperature regulated water coolant, which is circulated in the cooling jacket, so with a thermostat regulating the temperature of the coolant. The absolute pressure in the reactor was 25 bar. The mass flow rate of the supply pump was controlled so that the concentration of the original propene represented 21.5 wt.%, the initial concentration of methanol was 57 wt.%, and the initial concentration of H2About2was equal to 9.4 wt.%. The reactor worked in peritoneum version.

In the experiments of these examples and comparative examples, as shown in the table varied the temperature in the cooling jacket (Tohlord) and the total mass flow and the measured maximum temperature (Tmax). The flow rate was controlled in order to achieve comparable values transformation. The product yield was determined by gas chromatography, and the degree of transformation - N2About2-titration. According to the results of gas chromatographic analysis of hydrocarbons expected selek is Yunosti. It was determined by the amount of the formed oxide propene relative to the number of all the formed oxygen-containing hydrocarbons.

Table
No.Tohlord(°)Tmax(°)Flow rate (kg/h)The degree of transformation of H2O2(%)Selectivity for propene oxide (%)
SP130400.357198
SP30350,74599
P141590,359696

No.Tohlord(°)Tmax(°)Flow rate (kg/h)The degree of transformation of H2O2(%)Selectivity for propene oxide (%)
P241510,77998
SP349780,79091
SP44967 1,48093
SP561812,87491

Data presented in table show that in the narrow temperature range of the cooling medium and the maximum temperature in the catalytic layer is reached, as indicated in the description of the present invention, an optimized balance between the degree of conversion and selectivity in the product.

1. Way catalytic epoxidation With3-C6-olefins with hydrogen peroxide in a flow reaction system of continuous action, in which the reaction mixture is passed through a fixed catalyst layer in the reactor equipped with cooling means, while maintaining the inside of the reactor of such a temperature profile in which the temperature of the cooling medium in the cooling means is at least 40°and the maximum temperature inside the catalytic layer is not more than 60°C.

2. The method according to claim 1, in which the inside of the reactor support such a temperature profile in which the maximum temperature inside the catalytic layer is not more than 55°C.

3. The method according to any of the preceding paragraphs, in which the reactor is a tubular reactor, and a cooling means is om serves as a cooling jacket.

4. The method according to any of the preceding paragraphs, in which the reaction mixture is passed through a catalytic layer on peritonea option.

5. The method according to any of the preceding paragraphs, in which a fixed catalytic layer support Oceania a thin stream.

6. The method according to any of the preceding paragraphs, in which the reaction mixture is passed through a catalytic layer with a flow rate per unit cross section of the flow from 1 to 100 m/h, preferably from 5 to 50 m/h, most preferably from 5 to 30 m/h

7. The method according to any of the preceding paragraphs, in which the reaction mixture is passed through a catalytic layer with an average hourly velocity of the fluid (SCSI) from 1 to 20 h-1preferably from 1.3 to 15 h-1.

8. The method according to any of the preceding paragraphs, in which the pressure inside the reactor is maintained at a level of from 5 to 50 bar, preferably from 15 to 25 bar.

9. The method according to any of the preceding paragraphs, in which the catalyst used titanium containing zeolite.

10. The method according to any of the preceding paragraphs, in which entering the reactor, the total flow of raw material includes an aqueous solution of hydrogen peroxide, With2-C6-olefin and an organic solvent.

11. The method according to claim 10, in which the organic solvent is a methanol.

12. The method according to any of the previous points is, in which the olefin is a propene.



 

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