Method for preparing oxirane in presence of catalyst as particles

FIELD: organic chemistry, chemical technology.

SUBSTANCE: invention describes a method for preparing oxirane in reactor comprising a liquid reaction medium. Method involves carrying out reaction between olefin and peroxide compound in liquid reaction medium in the presence of a solid catalyst and a solvent. Solid catalyst comprises zeolite as an active component and it is used in form of particles wherein at least part of particles present in reactor in the fluidized state. Invention provides increasing rate of the process that results to the enhanced output.

EFFECT: improved preparing method.

1 ex

 

The present invention concerns a method of obtaining oxirane by the reaction of an olefin with a peroxide compound in a liquid medium containing solid catalyst. It concerns, in particular, obtaining propylene oxide or epichlorohydrin by epoxidation of propylene or allylchloride using hydrogen peroxide.

A known method of producing propylene oxide by reaction between propylene and hydrogen peroxide in the presence of silicalite titanium as a catalyst. For example, according to patent application EP 0659473 this method is implemented in a reactor containing a fixed catalyst bed.

In addition, it is known that this method of obtaining the activity of catalysts of the type silicalite titanium after a certain period of time falls. Therefore it is necessary to separate the catalyst from the reaction medium for regeneration or replacement.

In the method described in patent application EP 0659473 present in the form of a stationary layer of the catalyst is difficult to remove from the reactor for regeneration or replacement.

The aim of the present invention is to eliminate this disadvantage by using a new method of obtaining oxirane, in which it becomes easy to separate the catalyst from the reaction medium. Another objective of the present invention is to offer a way when it is about Islena the application is easy to take away the reaction heat. This allows operation at a higher speed and, therefore, to provide improved performance.

In this regard, the present invention concerns a method of obtaining oxirane in a reactor containing a liquid reaction medium, according to which, in a liquid reaction medium olefin reacts with the peroxide compound in the presence of a solid catalyst and in the presence of a solvent; in accordance with the present invention, a solid catalyst is used in the form of particles and at least part of the particles is in the reactor in a fluidized state.

One of the essential features of the method in accordance with the present invention is the use of the catalyst in the form of particles in fluidized condition. It should be noted how unexpected the fact that in the epoxidation reaction in a liquid medium between the olefin and the peroxide compound in the presence of a solvent can be used free-flowing particle bed. Indeed, until now it was difficult to assume that the particles epoxidised catalyst can withstand fluidization, as due to their nature, these particles are fragile and can be crushed or broken under the influence of fluidization. The applicant has unexpectedly found that these particles maintain fluidization no significant p is Teri catalytic activity, while not collapsing and losing graininess. The fact that these particles can be used in a fluidized bed state, is compared with a stationary layer of advantage, since it becomes easy to extract the catalyst from the reactor for regeneration or replacement. In addition, the mode of reaction with the fluid layer provides good heat transfer and, consequently, facilitates control of the reaction temperature, and also provides a uniform dispersion of the catalyst in the liquid reaction medium.

The basic principles of operation fluid layer described in "Perry's Chemical Engineers' Handbook, Sixth edition, 1984, p.4-25, 4-26, 20-3 and 20-58 on 20-75.

In the framework of the present invention, the term "fluid state" means that the catalyst particles are in constant motion, which is not observed in the stationary layer, where the catalyst remains stationary throughout the reaction. However, the particle motion is limited, as they remain in the zone of the reactor, called the fluid layer and located between the zone of distribution of the fluid and the area of emission of solid particles. Therefore, in principle, the particles do not leave the zone of the fluid layer during the reaction, whereas in the floating layer of particles addicted to all parts of the reactor.

Area distribution of the fluid dispenser contains p is designated for to avoid preferential flow of fluid and, therefore, to provide a uniform flow of fluid. Typically, the dispenser is made in the form of the distribution plate or grid. Area particulate is designed to stop the movement of the solid catalyst particles.

Fluidized condition of the catalyst particles in mainly through the fluid medium moving in the reactor from the bottom up, creating an upward flow with the speed of ascent, at which fluidization of the catalyst particles. Preferably, this fluid is a liquid. It is preferably formed of a liquid reaction medium containing olefin, a peroxide compound, a solvent, usually water, a portion of oxirane and possibly formed during the reaction by-products.

Normal operation fluid layer depends on several factors. In particular, we can mention the choice of the distributor, the lifting speed of the fluid, the weight of the catalyst particles, the diameter of the catalyst particles, the size of the reactor and the height of the fluid layer. All these parameters depend on each other. Therefore, to ensure the good functioning of the fluid layer is necessary to determine the optimal combination of parameters which produce the p remains in a fluid state throughout the reaction.

In the method according to the present invention can be applied to any known appropriate type of distributor.

The lifting speed of the upward flow of fluid is usually greater than or equal to 0.01 m/min, in particular greater than or equal to 0.05 m/min speed, typically less than or equal to 10 m/min, in particular less than or equal to 5 m/min

The catalyst particles generally have apparent specific gravity, measured by free flow in the air greater than or equal to 0.1 g/cm3in particular greater than or equal to 0.5 g/cm3. Most often apparent specific gravity less than or equal to 2 g/cm3in particular less than or equal to 1 g/cm3.

The catalyst particles generally have a diameter greater than or equal to 100 μm, in particular greater than or equal to 200 μm. The average diameter is typically less than or equal to 5000 μm, in particular less than or equal to 2000 μm.

Preferably the catalyst contains a small part of the fine particles with diameter less than 100 μm, because these fine particles can easily move beyond the fluid layer and cause, thus, catalyst losses, contamination of the installation or the appearance of uncontrolled side reactions. As a rule, the proportion of fine particles less than or equal to 5 wt.% the weight of the catalyst, in particular less than or equal to 2 wt.%, for example, less than or equal to 0,ves.%.

Used in the method according to the present invention, the catalyst particles generally contain a binder and an active element. The amount of binder is typically greater than or equal to 1% by weight of the catalyst, in particular greater than or equal to 10%. Often the content of the binder is less than or equal to 90% by weight of the catalyst, in particular less than or equal to 60%.

The active element is typically a zeolite, preferably of titanium-containing zeolite. Under the titanium-containing zeolite understand solid substance containing silica with a microporous crystalline zeolite structure type, in which some of the silicon atoms are replaced by titanium atoms. Titanium-containing zeolite preferably has a crystalline structure of ZSM-5, ZSM-11, ZSM-12, MCM-41, ZSM-48. He may also have a crystalline structure of beta zeolite type, preferably not containing aluminum. For this method are well suited zeolites with a range of infrared absorption, about components 950-960 cm-1. The most preferred titanium-containing zeolites silicalite type. Preference is given to zeolites with formula xTiO2(1-x)SiO2where x is from 0.0001 to 0.5, preferably from 0.001 to 0.05. Materials of this type are known under the name of TS-1 are microporous crystalline zeolite is the structure, similar to the structure of zeolite ZSM-5.

The binder usually contains one or more derivatives of silicon.

The catalyst particles can be obtained by any known method, for example by extrusion, as described in patent application WO 99/28029 filed on behalf of the applicant, the contents of which are incorporated into the present patent application by reference, or by using spray technology, as described in patent application WO 99/241164 filed on behalf of the applicant, the contents of which are also included in the present patent application by reference.

In the first variant implementation of the method in accordance with the present invention, the reactor consists of several tubular reactors arranged in parallel in a heat exchanger, with each reactor contains a fluid layer of catalyst particles. Tubular reactors, as a rule, are fed in parallel from a single source reaction medium containing olefin, a peroxide compound and a solvent. This single source may also contain recycled remnants formed of oxirane and/or by-products. The heat exchanger preferably includes a chamber filled with a cooling liquid in which is immersed tubular reactors. Alternative technical solution may consist of forced circulation in the chamber of the coolant, which can be the t to be under pressure, enough not to change its state (and just heat), or may partially evaporate.

This embodiment is of particular interest, as it allows much easier to provide equivalent conditions (in particular, with regard to losses load), each tubular reactor than in the way in which used catalyst in the form of a stationary layer. In addition, it allows you to work with the reaction tubes of small size, even on an industrial scale. In smaller reactors easier to achieve homogeneous dispersion of the catalyst, as in a large reactor there is a much greater probability of formation of preferential flow in some parts of the reactor. The small size reactors also provide work at a higher reaction rate without the formation of by-products. Indeed, it was found that in the reaction epoxygenase environment formed oxiran can undergo side reactions of hydrolysis and alcoholysis (methanolysis, if the solvent used methanol) with the formation of side products. In the reactor a small amount of contact between the formed oxirane and water or solvent is minimized in comparison with a large reactor.

In the second variant implementation of the method in accordance with this from what Britanie reactor contains a single camera, containing reaction medium and a catalyst in a fluidized condition, that surrounds one or more tubes located next to each other, which circulates the coolant. Alternative technical solution may consist of forced circulation in the pipes of the coolant, which may be under sufficient pressure so as not to change its state (and just heat), or may partially evaporate.

These two implementation options provide easy removal of the reaction heat generated during epoxidation by heating and/or evaporation of the coolant.

Used in the method according to the present invention, the solvent may be selected from linear or branched saturated aliphatic alcohols. Typically, the alcohol solvent contains up to 10 carbon atoms, preferably from 1 to 6 carbon atoms. As examples can be mentioned methanol and ethanol. Methanol is preferred.

Most often the reaction epoxydiols environment also contains water.

The amount of solvent used in the method according to the present invention typically comprises at least 25 wt.% the weight of the reaction medium, in particular at least 40 wt.%, for example, at least 50 wt.%. Usually this number is not greater than 99 wt.%, in particular not greater than 95 wt.%.

The molar ratio of the olefin and the amount of peroxide compounds involved in the method in accordance with the present invention, generally at least equal to 0.1, in particular at least 0.2 and preferably at least 0.5 in. Most often, this molar ratio is not more than 100, in particular not more than 50 and preferably does not exceed 25.

The method in accordance with the present invention can be carried out in a continuous mode or intermittent mode. It can be implemented only in a single reactor or in multiple reactors installed in series. When implementing the method in several reactors preferably peroxy compound only in the first reactor, as described in the patent application filed by the applicant on the same day as the present patent application, and entitled "Method of obtaining oxirane using peroxide compounds" (the contents of which are incorporated by reference into the present patent application). In addition, each reactor can be installed distillation column for separating formed of oxirane from the liquid reaction medium before the introduction of the latter into the next reactor, as described in the patent application filed by the applicant on the same day as the present application, and Sagl the run "Method of obtaining oxirane, includes Department of oxirane from the reaction environment" (the contents of which are incorporated by reference).

When the method in accordance with the present invention is realized in the continuous mode, the peroxide compound, generally used in a quantity of at least 0,005 mol per hour and per gram of catalyst, in particular at least 0.01 mol per hour and per gram of catalyst. Typically, the amount of peroxide compounds is less than or equal to 25 mol per hour and per gram of catalyst, in particular less than or equal to 10 mol per hour and per gram of catalyst. The preferred amount of peroxide compounds greater than or equal to 0.03 mol per hour and per gram of catalyst and less than or equal to 2.5 mol per hour and per gram of Katalizator.

In the method according to the present invention, the peroxide compound is preferably used in aqueous solution. Typically, the aqueous solution contains at least 2 wt.% peroxide compounds, in particular at least 5 wt.%. Most often it contains not more than 50 wt.% peroxide compounds, in particular 70 wt.%.

The temperature of the reaction between the olefin and the peroxide compound can vary from 10 to 125°C. In the preferred embodiment, described in patent application EP 99/08703 on behalf of the applicant, it exceeds 35°to compensate for the gradual desak is evalu catalyst. The temperature can be less than or equal to 40°C, preferably be less than or equal to 45°C. a More preferred temperature is greater than or equal to 50°C. the reaction Temperature is preferably less than 100°C.

In the method according to the present invention, the reaction between the olefin and the peroxide compound can be carried out at atmospheric pressure. It can also take place under pressure. Typically, this pressure does not exceed 40 bar. In practice, the most suitable pressure 20 bar.

Peroxide compounds which may be used in the method according to the present invention are peroxide compounds containing one or more peroxide functional groups (-UN), which can release active oxygen and to carry out epoxidation. Good results were obtained when using inorganic peroxide compounds. Suitable hydrogen peroxide and peroxide compounds, which can produce hydrogen peroxide under the reaction conditions of the epoxidation. The most preferred hydrogen peroxide.

If you use hydrogen peroxide, it makes sense to apply the method according to the present invention an aqueous solution of hydrogen peroxide in cheese, that is untreated. For example, you can use the solution obtained by prostatectomie with almost pure water from the mixture, obtained by oxidation of at least one alkylanthraquinones (a method called "method JSC auto-oxidation"), without further processing by washing and/or cleaning. These crude solutions of hydrogen peroxide containing generally from 0.001 to 10 g/l of organic impurities, expressed as TOC (total organic carbon). They usually contain cations of metals such as alkali metals or alkaline-earth metals, for example sodium) and anions (such as phosphates, nitrates) in an amount of from 0.01 to 10 g/L.

In another embodiment, a method you can use the hydrogen peroxide solution obtained by synthesis from oxygen and hydrogen in the presence of methanol.

Obtained using the method in accordance with the present invention oxiran is an organic compound that meets the General formula

Typically, oxiran contains from 2 to 10 carbon atoms, preferably from 3 to 6 carbon atoms. Preferably obtained using the method in accordance with the present invention oxirane represent 1,2-epoxypropane and 1,2-epoxy-3-chloropropane. The preferred 1,2-epoxypropane.

Preferred for use in the method according to the present invention, the olefins contain from 2 to 10 carbon atoms and preferably from 3 to 6 carbon atoms. Well p is chodat propylene, butylene and allylchloride. Preference is given to propylene and allylchloride. The most preferred propylene.

In the method according to the present invention in the reactor can also be supplied with gas, do not have a negative effect on the epoxidation reaction. Indeed, in the patent application WO 99/48883 (the contents of which are incorporated by reference into the present patent application) the applicant found that by introducing a gaseous compound in the reaction medium with a flow rate sufficient to move produced oxirane and for removal from the reactor simultaneously with gaseous compound, thereby reducing the contact time between the received oxirane and reaction environment epoxidation. Thus additionally avoid the formation of by-products and increase the selectivity of the epoxidation. Another option is to separate the formed of oxirane from the liquid reaction medium by distillation in the distillation column.

In the method according to the present invention can be necessary to control the pH of the liquid phase. For example, it makes sense to maintain the pH of the liquid phase during the reaction between the olefin and the peroxide compound at the level of 4.8 to 6.5, for example, by adding a base (sodium hydroxide) in epoxydiols environment, as recommended in the patent States the e WO 99/48882 in the name of the applicant (the contents of which are incorporated by reference into the present patent application).

The reaction between the olefin and the peroxide compound can be carried out in the presence of salts such as sodium chloride, as described in patent application WO ER/08703, filed in the name of the applicant (the contents of which are incorporated by reference into the present patent application).

It may be preferable to introduce into the reactor in which the epoxidation reaction, the olefin dissolved in one or more alkanes. For example, you can type in epoxygenase reactor the fluid containing olefin and at least 10 vol.% (in particular 20 vol.%, for example, at least 30 vol.%) one or more alkanes. For example, in the case of propylene, the latter can be mixed with at least 10 vol.% propane, if the reactor is injected recycled unconverted propylene. Can also be used a source of propylene, not completely cleared from propane.

Example 1

In this example, the epoxidation of propylene (Re) used plant comprises a reactor with a fluidized bed with the recirculation circuit of the liquid. The reactor may contain a glass tube with a diameter of 1.5 cm with double casing. In the upper part and the lower part of the reactor is equipped with two gratings designed for the holding of the catalyst.

Pre-saturated D reaction medium under pressure and containing the th methanol (Meon)+H 2O+H2About2+Re+propylene oxide (EO), at a flow rate of 5 l/hour fed into the reactor containing the catalyst. Subsequently, the resulting EOS is removed in the gas phase by distillation. The resulting liquid phase is divided into the output stream (excess) and the recycle stream, to which is added N2About2and Meon and which is returned to the reactor after re-saturation Re.

The catalyst has the form of spheres with a size of 0.4-0.6 mm from silicalite Ti dispersed in a ratio of 1/3 by weight in a matrix of microporous silica. They were obtained by the method of "Sol-gel" in the liquid phase.

Given the diameter of the reactor, the flow passing through the reactor the reaction medium, adjusted to 5 l/h, corresponds to the rate of passage through the empty pipe, equal to 0.47 m/min, i.e. the value that is greater than the minimum velocity of fluidization of balls, which is close to the value of 0.1 m/min This is the minimum velocity of fluidization is observed due to caused by the expansion layer. The height of the catalytic layer varies, therefore, from 5 cm at rest up to 7 cm in test mode.

After 347 hours at 77°at a pressure of 8 bar pull 4,441 g of the catalyst used, the amount of 4,500 g, which is the average loss of only 0.17 mg/hour or 0,004 %/hour.

1. The method of obtaining oxiran is in the reactor, containing liquid reaction medium, according to which, in a liquid reaction medium carry out the reaction between the olefin and peroxide compound in the presence of a solid catalyst and a solvent, characterized in that the solid catalyst contains a zeolite as the active element, the fact that it is used in the form of particles, and the fact that at least part of the particles is in the reactor in a fluidized state.

2. The method according to claim 1, characterized in that the liquid reaction medium containing olefin, a peroxide compound, the solvent, the formed oxiran and possibly by-products, moves in the reactor from the bottom up, creating an upward flow with the speed of providing fluidization of the catalyst particles.

3. The method according to claim 1 or 2, characterized in that the catalyst particles have an apparent specific gravity measured at the free over the air, equal to from 0.1 to 2 g/cm3.

4. The method according to any one of claims 1 to 3, characterized in that the catalyst particles have a diameter of from 100 to 5000 μm.

5. The method according to any one of claims 1 to 4, characterized in that the lifting speed of the liquid reaction medium is from 0.01 to 10 m/min

6. The method according to any one of claims 1 to 5, characterized in that the reactor consists of several tubular reactors arranged in parallel in a heat exchanger, where they are fed from the only the i.i.d. source of the liquid reaction medium, containing olefin, a peroxide compound and a solvent.

7. The method according to claim 6, characterized in that the sole source also contains recycled remnants formed of oxirane and/or by-products.

8. The method according to claim 6 or 7, characterized in that evolved during the reaction heat away through the coolant surrounding the tubular reactor.

9. The method according to any one of claims 1 to 5, characterized in that the reactor consists of a single chamber containing liquid reaction medium and a catalyst in a fluidized condition in which shipped a few located next to each other with pipes that carry the coolant.

10. The method according to any one of claims 1 to 9, characterized in that oxiran is propylene oxide or epichlorohydrin, the olefin is propylene or allylchloride, the peroxide compound is hydrogen peroxide, the catalyst contains silicalite titanium, and the solvent is methanol.

11. The method according to any one of claims 1 to 10, in which the environment of the epoxidation reaction contains water.

12. The method according to any one of claims 1 to 11, in which the peroxy compound is inorganic.

13. The method according to any one of claims 1 to 12, in which the peroxide compound is used in the form of an aqueous solution.



 

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