The method of gas-phase polymerization of alpha-olefins and a reactor for implementing the method

 

(57) Abstract:

Usage: in the chemical industry, in the way of gas-phase polymerization of alpha-aleinov in the reactor with a fluidized bed. The inventive method gas-phase polymerization of alpha-olefins in a reactor with a fluidized bed containing pseudoainhum lattice, in which the gas mixture out of the upper part of the reactor and returned to the bottom of the reactor, below pseudoviruses lattice, using a recirculating pipe connecting the upper part of the reactor with its lower part, below pseudoviruses lattice of the solid catalytic component, socialization, activator and inhibitor activity continuously or intermittently introduced into the reactor together with the carrier gas through the supply pipe, the outlet of which is located at the upper surface or slightly above the upper surface pseudoviruses lattice and is located towards the center of the cross section of the reactor. 2 S. and 6 C. p. F.-ly, 3 ill.

The invention relates to a method of gas-phase polymerization of alpha-olefins in a reactor with a fluidized bed.

It is known that the polymerization of al the liquefied layer.

The polymerization system includes an elongated reactor in which the particles of the resulting polymer are maintained in fluidized condition by moving up a fluidized bed of a gas stream containing the polymerization of alpha-olefins. In the lower part of the reactor includes / tube sheet or porous plate, known as pseudozyma lattice, which allows pseudoviruses gas stream entering the reactor from the bottom of named grids, distributed under fluidized layer, supporting polymer particles in fluidized condition over a specified grid. This system usually includes a pipe connecting the upper part of the reactor with its lower part, below pseudoviruses lattice. The named pipe is equipped with a compressor for circulating the gas mixture coming from the upper part of the reactor, and at least one heat exchanger for cooling the gas mixture in order to lower the reaction temperature before the gas mixture is returned to the bottom of the reactor. The reactor is equipped with means for the introduction of alpha-olefins (alpha-olefins), catalyst and other components of the reaction mass, and sredstvami for gas-phase polymerization of alpha-olefins in a fluidized bed reactor, well known in the art. Such catalysts are the catalytic system of the Ziegler-Natta comprising a solid catalyst containing a compound of a transition metal belonging to groups IV, V or VI of the Periodic system of elements, such as titanium or vanadium, and preferably a magnesium compound; and socialization containing ORGANOMETALLIC compound of a metal belonging to groups I, II or III of the Periodic system of elements.

Other suitable catalysts are catalysts based on chromium oxide supported on silica, and thermoactivation in novosstroitelnaya environment.

The solid catalyst or the solid component of the catalyst may be introduced into the reactor continuously or intermittently through the inlet in the wall of the reactor vessel. Such a device of the reactor may not be satisfactory for achieving high activity catalytic systems, as a solid component in this setup may not be distributed by a fluid layer well enough or fast enough, which can lead to the formation of places overheating and the formation of agglomerates.

In addition to the catalysts may the th layer.

The method of the present invention allows to overcome or at least partially solve the problems associated with adding in gas-phase reactor with a fluidized bed of solid catalytic components and other components that need to be quickly and uniformly dispersed in the fluidized bed.

The technical result is achieved due to the fact that in the method of gas-phase polymerization of alpha-olefins in a reactor with a fluidized bed containing pseudoainhum lattice, in which the gas mixture out of the upper part of the reactor and returned to the bottom of the reactor, below pseudoviruses lattice using a recirculating pipe connecting the upper part of the reactor with its lower part, below pseudoviruses lattice of the solid catalytic component, socialization, activator and inhibitor activity continuously or intermittently introduced into the reactor together with the carrier gas through the supply pipe, the outlet of which is located at the upper surface or slightly above the upper surface pseudoviruses lattice and is located towards the center of the cross section of the reactor.

in the liquid; inhibitor activity is dimethylformamide; specified pre-dimethylformamide is heated prior to introduction into the supply pipe; a carrier gas is passed through the supply pipe at a speed not less 20 m/s

The above process is carried out in a reactor for gas-phase polymerization of alpha-olefins in a fluidized bed containing a cylindrical housing with a lid and bottom perforated pseudoainhum grille in the lower part of the reactor, where the reaction layer, and is located in the bottom of the reactor feed gas pipeline-media connections for input of additives in accordance with the technology of the process, the outlet of the supply pipe is located in the direction of the vertical axis of the reactor at the upper surface or slightly above the perforated grid, and the supply pipe provided with a means for introducing separately or together solid catalytic component, socializaton, activator or inhibitor activity.

In the reactor feed the pipeline passes vertically through the bottom of the reactor vessel in the direction of pseudoviruses lattice; the supply pipeline is located along the axis of the reactor in the direction is to be used any catalyst, which is usually used in gas-phase reactor with a fluidized bed, such as a catalyst or catalytic system, which were mentioned above, the solid particles of the prepolymer obtained by reacting one or more alpha-olefins with a catalyst or catalytic system, and solid particles of alpha-olefin polymer or copolymer, even with catalytic polymerization activity, such as a polymer transferred from one polymerization reactor to another (between stages in a multistage polymerization process).

So, for example, as a solid catalytic component can be used to highly active catalyst of the Ziegler-Natta in the form of solid particles containing magnesium, halogen and at least one transition metal of group IV, V or VI of the Periodic system of elements, such as titanium, vanadium or zirconium. Optionally, the catalyst may be deposited on a suitable carrier, such as silicon dioxide, aluminum oxide or magnesium compound such as magnesium chloride or magnesium alkoxide.

Another example of a highly active catalyst, which can be used in the proposed image is such as silicon dioxide, aluminum oxide or aluminum silicate.

The specified catalyst may be used directly or in the form of a prepolymer. The transformation in the prepolymer is typically performed using the interaction of the catalyst with one or more alpha olefine in such quantity that the prepolymer contained 0,002-10 mm transition metal 1, the components Usually interact in the presence of socializaton containing ORGANOMETALLIC compound in which the metal belongs to group I, II or III of the Periodic system of elements, in an amount such that the molar ratio of metal in the ORGANOMETALLIC compound to the amount of the transition metal was 0.1-50, preferably 0.5 to 20. Acetalization used to obtain the fluoropolymer may be the same or different from socializaton used in gas-phase polymerization reactor with pseudouridine layer.

The prepolymer can be produced continuously and directly into the reactor.

In accordance with one embodiments of the present invention, the catalyst is subjected to continuous pre-polymerization in the reactor prior to polymerization, previtali piping in the reactor.

The solid catalytic component may be solid particles, even with catalytic polymerization activity. However, in the method of the present invention mainly provides for the introduction of relatively small quantities of the catalytic component in the gas-phase fluidized bed.

The solid catalytic component is normally introduced into the reactor in the form of a dry powder or in the form of a suspension or dispersion in an appropriate solvent.

Socialization introduced into gas-phase polymerization reactor with a fluidized bed, may be ORGANOMETALLIC compound containing a metal of group I, II or III of the Periodic system of elements, such as aluminum, zinc or magnesium. Acetalization can be introduced into the polymerization reactor together with the catalyst and/or separately from the catalyst. According to the invention, socialization entered separately from the catalyst may be introduced through the supply pipeline. Sometimes, however, it is preferable that socialization and inhibitor activity, interacting with each other, was not introduced both through the same supply pipeline.

According to the method proposed invented the wide range of materials, of which preferred are gases and liquids, with volatility in the conditions of polymerization and is able to reduce the rate of polymerization of alpha-olefins in the presence of a catalyst. Appropriate activity inhibitors are inhibitors such as carbon monoxide, carbon disulphide, oxysulfide carbon, oxides and peroxides of nitrogen, oxygen, alcohols, aldehydes, ketones, thiols, water and electron-donating compounds are capable of forming complexes with the catalyst and to reduce the rate of polymerization.

Inhibitor activity may be introduced into the reactor in the form of a solution in an appropriate solvent. If the specified inhibitor is a liquid or capable of dissolving in the liquid before introduction into the reactor, it is preferable to heat. And more preferably, if the liquid prior to its introduction into the reactor to heat up until it turns into steam.

Suitable activators are activators, such as ORGANOMETALLIC compounds of metals belonging to groups I, II or III of the Periodic system of elements, in particular alumoorganic, tsinkorganicheskie or magyarkanizsa connection. The preferred means is to tri-n-butylamine and triisobutylaluminum. The activator may be the same as acetalization.

Activator, as well as the inhibitor activity may be introduced directly into the reactor or it can be introduced in the form of a solution in an appropriate solvent or as a dispersion in a liquid, which, before their introduction into the reactor is preferably heated, and more preferably is converted into steam.

The supply pipe has an opening at the surface or slightly above the upper surface pseudoviruses lattice. There is a turbulent fluidized bed region where bubbles and there is a strong mixing.

The outlet of the supply pipe is directed toward the center of the cross section of the reactor. The mixing layer is below where it adjoins the walls of the reactor. Preferably, the supply pipeline was in the center of the cross section of the reactor.

Avoid large gaps of flow within the fluidized bed preferably, the supply pipeline was included in the reactor in place below pseudoviruses lattice, passed through the bars and went just a little maslichnye supply piping can be used for the introduction of various components. For example, if the activator and inhibitor activity must be injected continuously and at the same time, if these two components can interact with each other, it is preferable to introducing them to use separate pipelines. If these two components do not react with each other, they can be introduced through the same pipeline.

For introducing into the reactor a solid catalytic component, socializaton, activator or inhibitor activity using a carrier gas. This gas can be fresh monomer or other gas supplied to the reactor or recycle gas. The velocity of the gas in the supply pipe that supplies the solid catalytic component, socialization, activator or inhibitor activity in General is at least 1 m/s, preferably at least 3 m/s, more preferably at least 20 m/s and most preferably at least 30 m/s, the Upper limit of the gas velocity, which can be used depends on such factors as the density of the feed material, the conditions within the fluidized bed and the length of the jet, which it would be desirable to create for introducing gas into the layer. In fact, the upper limit may be, for example, 100 MgO invention is intended for the polymerization of one or more alpha-aleinov, containing from 2 to 12 carbon atoms, in particular for the polymerization of ethylene or propylene. The method of the present invention can be, in particular, used to homopolymerization of ethylene or copolymerization of ethylene with at least one alpha-olefin containing from 3 to 12 carbon atoms.

It was found that if the method of the present invention is injected inhibitor activity (such as dimethylformamide), this inhibitor has an almost immediate effect. If, however, this inhibitor is introduced below pseudoviruses lattice, then its effect can appear only after several hours.

The present invention also relates to a device intended for the implementation of the proposed method. This device encompasses gas-phase polymerization reactor with a fluidized bed containing in its lower part a lattice, providing a fluidized state, and the supply pipeline, which enters the reactor in place, located below the grating, passes through the grating and has an outlet at its upper surface or slightly above the upper surface of the specified grid. The outlet pipe directed but together or solid catalytic component, socializaton, activator, or an active inhibitor; a carrier gas.

Preferably, the pipeline is mainly vertically through the bottom of the reactor to pseudoviruses lattice.

In Fig. 1 schematically depicts a gas-phase polymerization reactor with a fluidized bed of Fig. 2 schematically depicts a bottom of the reactor shown in Fig. 1; Fig. 3 schematically shows a second variant of the bottom of the reactor depicted in Fig. 1, in combination with the reactor prior to polymerization, connected with the supply pipe.

The polymerization system is shown in Fig. 1, includes a reactor 1 with a fluidized bed comprising a vertical cylinder 2 at its upper part with a camera 3 for a released product, and in its lower part with pseudoainhum the grating 4. Camera 3 for eye-catching product are connected by a pipe 5 with cyclone 6, in which particles carried by the gas mixture leaving the reactor 1, are separated from the gas. The pipe 7 connects the lower end of the cyclone 6 to the mixing chamber ejector compressor 8 through the pipe 9 enters the carrier gas. The pipeline 10 for re-introduction of solid particles behold the first heat exchanger 12, which in turn through the pipeline 13 is connected to the compressor 14, from which the gas through the pipeline 15 is supplied to the second heat exchanger 16. Then recycle gas is introduced into the reactor 1 below pseudoviruses lattice through the pipeline 17. A pipe 18 connects the pipe 17 with the pipe 9, which enables the use of recycle gas as a carrier gas for the ejector compressor 8. The pipe 19 is designed to feed the catalyst into the reactor 1. The removal of the polymer product is in the pipeline 20. Fresh monomer and other ingredients necessary to maintain the composition and pressure of the reaction gas can be introduced through the pipeline 21. Line 22 is used for the introduction of solid catalytic component, socializaton or inhibitor activity in the pipe 23 for supplying raw materials. This supply pipe 23 provided with a valve 24.

In Fig. 2 presents a view of the lower part of the reactor with a fluidized bed, suitable for use in the method of the present invention. Elements similar to those used in Fig. 1 are denoted by similar numerals.

Psevdoeroziya grating 4 consists of three truncated conical sec the hat is the internal radius of the reactor and the base radius of the truncated cone TS. R2 represents the common ground of the two truncated cones TS and TS, and R1 represents the common ground of the two truncated cones TC1 and TC. Can also be used and other forms pseudoviruses lattice, for example flat or convex lattice.

The supply pipe 23 enters the reactor through the bottom of the reactor and passes vertically up pseudoviruses grating 4. The outlet 25 of the pipe 23 is located at the level of the upper surface of the specified grid and is directed towards the center of the cross section of the reactor. The supply pipe has a radius r. Within the specified supply pipe can be inserted liners to change the effective radius of the pipeline, which allows to vary the velocity of the gas at the same time the volumetric flow rate. Basically the internal diameter of the supply pipe is from about 0.05 to 0.10 m

The solid catalytic component, acetalization or inhibitor activity are served together with the carrier gas through the pipeline 22. The carrier gas may also be supplied via a supply pipe 23 from the bottom through a valve 24.

The device shown in Fig. 2, can also be used to remove the polymer from the bottom of the reactor.

the deposits in the method of the present invention. Elements similar to those described in Fig. 1 and 2 are denoted by similar numerals. This option includes the reactor 26 for pre-polymerization, connected with the supply pipe 23.

The reactor 26 for pre-polymerization includes a straight cylinder, in which the pipe 27 enters ethylene; pipe 28 enters socialization; pipeline 29 hydrogen, and the catalyst conduit 30. The catalyst is stored mainly in an inert atmosphere, for example under nitrogen atmosphere in the tank 31 from which he through the ball valve 32 is fed into the pipeline 30. Inert gas, such as nitrogen, may be introduced through the pipe 33, intended to make solid catalyst particles in the reactor 26 for the preliminary polymerization.

The amount of catalyst, socializaton, hydrogen and ethylene fed to the reactor prior to polymerization, and the size of the direct cylinder reactor is preferably chosen in such a way as to ensure the velocity of the gas in the specified cylinder is more than about 1 m/s and the residence time sufficient to perform a preliminary polymerization catalyst to a relatively low polymer lane is accounted from 1 to 5 g of polymer.

In the variant shown in Fig. 3, the carrier gas flows through the pipe 23 through the valve 24. Line 22 is provided with a nozzle 34, which provides the dispersion of the prepolymer in the carrier gas. The end of the supply pipe 23 is located slightly above pseudoviruses grating 4, it is provided with a valve 35, which provides the dispersion of the mixture in the fluidized bed. The diameter of the supply pipe 23, the diameters of the holes of the distributor 35 and total gas flow rate is chosen so that the speed of injection ranged from 1 to 90 m/s, preferably from 20 to 90 m/s, and most preferably from about 30 to 90 m/s This speed provides good penetration into the fluidized bed, and better dispersion of the prepolymer.

The above description only illustrates the invention and in no way should be construed as a limitation of the proposed variants of the preferred device for implementing the method of the invention and the accompanying drawings.

In addition, the proposed invention is illustrated below by examples.

P R I m e R 1. A copolymer of ethylene and butene-1 was obtained with isponsor. 1 and 2.

This reactor comprises a vertical cylinder, with a height of 10 m and the radius R3 of 1.5 m, and at its upper part contains the camera to eye-catching product.

In the lower part of the cylindrical reactor has a grid to ensure pseudoviruses effect and the Central feeding pipe, as shown in Fig. 2.

Psevdoeroziya lattice consists of three coaxial truncated conical sections (TC1, TC and TS). These tapered surfaces are contoured A1, A2 and A3 corners 6about, 12aboutand 20aboutrespectively; the total basis of two cones TC1 and TC has a radius R1 of 0.7 m, and the total basis of two cones TS and TS has a radius R2 1.2m

The supply pipe has a radius r of 0.05 m, and its outlet is located in the centre pseudoviruses lattice. This supply pipe is vertically downwards from pseudoviruses lattice through the bottom of the reactor. Full flow is provided by a rapidly opening valve type spherical casing, acting through pneumatic regulation, which provides its full opening for 0.5 sec Via the inlet hole located between the valve and the bottom of the reactor, flows rastsenivaya lattice is a fluidized bed, the height of which is maintained at about 8 PM the Specified layer contains 15 t linear polyethylene copolymer of ethylene and butene-1 low density. The temperature of the fluidized bed was maintained at about 75aboutC.

Pseudoviruses gas contained ethylene, butene-1, hydrogen and nitrogen, with the full pressure of about 2.0 MPa and had a speed of about 0.5 m/s

The catalyst was periodically introduced into the reactor through an outlet in the side wall of the reactor. The catalyst containing titanium, chlorine and magnesium, was previously converted into a prepolymer containing 40 g of polyethylene per 1 millimoles of titanium; and tri-n-octylamine in an amount such that the molar ratio Al/Ti was about 0,8-0,85.

Tri-n-octylamine also introduced into the reactor to obtain a molar ratio of Al/Ti in the reactor equal to 1.6.

A solution of dimethylformamide (DMF) in isopentane containing 0,004 M DMF) for 1 l, is continuously fed into the reactor through the inlet opening and the supply pipeline. The DMF solution pre-heated to 80aboutUsing a heat exchanger located behind the pump, the feed solution in DMF inlet. The carrier gas, which represents a process gas at a temperature of 5

It was noted that during the copolymerization introduction DMF had an almost instant effect on the reactive ability of hydrogen and activity.

P R I m m e R 2. A copolymer of ethylene and butene-1 was obtained with the use of the system containing the gas-phase reactor with a fluidized bed, in accordance with the description given in example 1, except that the temperature of the fluidized bed in the main, supported at 74aboutAnd the supply pipeline used for the introduction of a pre-polymerized catalyst together with DMF.

The catalyst, which was similar to the catalyst used in example 1 was injected in the form of dry solid particles in the base of the reactor prior to polymerization (diameter 0.5 m, the length of the cylinder 3 m). The catalyst was injected through the ball valve under nitrogen pressure and at a flow rate of 750 g/h of Ethylene were introduced into the reactor prior to polymerization with the consumption of 870 g/h tri-n-octylamine continuously fed into the reactor prior to polymerization so that the molar ratio Al/Ti with /PM

The catalyst was subjected to preliminary polymerization in the reactor prior to polymerization to the level where the catalyst 1 millimoles of titanium had 5 g of polymer.

Slightly pre-polymerized catalyst with reaction gases coming from the reactor prior to polymerization in the supply pipeline, where it was transferred to a polymerization reactor with a carrier gas, which was a process gas at a temperature of 55aboutWith and held by the feeding pipeline at a speed of about 20 m/s Temperature specified process gas above the temperature of the cooled recycle gas fed into the lower part of the reactor for fluidized polymer particles.

1. The method of gas-phase polymerization of alpha-olefins in a reactor with a fluidized bed containing pseudoainhum lattice, in which the gas mixture out of the upper part of the reactor and returned to the bottom of the reactor, below pseudoviruses lattice, using a recirculating pipe connecting the upper part of the reactor with its lower part, below pseudoviruses lattice, characterized in the legally introduced into the reactor together with the gas carrier through the supply pipeline, the outlet of which is located at the upper surface or slightly above the upper surface pseudoviruses lattice and is located towards the center of the cross section of the reactor.

2. The method according to p. 1, characterized in that the activator or inhibitor activity is a liquid or can be soluble or dispersed in the liquid.

3. The method according to p. 2, characterized in that said inhibitor activity is dimethylformamide.

4. The method according to p. 3, characterized in that the pre-dimethylformamide is heated prior to its introduction in the supply pipeline.

5. The method according to PP.1 to 5, characterized in that the carrier gas is passed through the supply pipe at a speed not less 20 m/s

6. Reactor for gas-phase polymerization of alpha-olefins in a fluidized bed containing a cylindrical housing with a lid and bottom perforated pseudoainhum grille in the lower part of the reactor, where the reaction layer, and is located in the bottom of the reactor feed gas pipeline-media connections for input of additives in accordance with the technology of the process, characterized in that the outlet of the supply Tr is vannoy lattice, moreover, the supply pipe provided with a means for introducing separately or together solid catalytic component, socializaton, activator or inhibitor activity.

7. The reactor under item 6, characterized in that the supply pipe passes vertically through the bottom of the reactor vessel in the direction of pseudoviruses lattice.

8. Reactor PP. 6 and 7, characterized in that the supply pipeline is located along the axis of the reactor toward the center of the cross section of the reactor.

 

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FIELD: chemical industry; production of alkylchlorosilanes.

SUBSTANCE: the invention is dealt with chemical industry and is used for realization of processes of synthesis in a fluidized layer. The reactor for direct synthesis of alkylchlorosilanes operating in a mode of fluidization of finely dispersed silicon and catalyst with promoters in the form of gaseous products consists of: a cylindrical body, a gas-distributive device and a heat-exchange device, an inlet and an outlet connection pipes. The cylindrical body of the reactor is made in the form of two coaxial cylinders forming a ring-type reaction zone, in the lower part of which is located a ring-type gas-distributing device, and on the external in relation to the reaction zone cylindrical surfaces there are jackets for delivery and withdrawal of heat. The given engineering solution provides a high selectivity of the process of production of alkylchlorosilanes.

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3cl, 2 dwg

FIELD: luminescent materials.

SUBSTANCE: nitride coating precursor, in particular aluminum-, gallium-, or tin-containing metalloorganic nitride, is charged into reaction vessel 10a filled with electroluminescent phosphor, e.g. ZuS-Cu, and surrounded by heating means 30a using nitrogen as inert gas carrier. Precursor is passed through pipeline 32 open all over its length. Co-reagent, e.g. anhydrous ammonia is fed into lower part of vessel 12a through porous glass disk 12a. When vessel 10a is heated to 150-225°C, nitride coating precipitates on phosphor particles being in fluidized state. Phosphor bearing nonoxide coating is characterized by high brightness after 100 h use at high humidity.

EFFECT: enabled large-scale manufacture of phosphors.

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FIELD: heat exchange apparatus.

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EFFECT: enhanced efficiency and simplified structure of the reactor.

1 dwg

FIELD: chemical or physical processes.

SUBSTANCE: reactor comprises cylindrical housing provided with an external heat exchanger and separator arranged at tits top part, units for charging contact mass and discharging exhaust contact mass, supplying gas component and discharging finished product, gas distributor, and built-in heat exchanger. The reactor is provided with outer circulation loop which has heat exchanger, pump, and ejector connected with the unit for supplying gas component. The separator is provided with a branch pipe for recirculation circuit. The built-in heat exchanger can be made at least of one heat pipe whose evaporation zone is located in the housing of the reactor and condensation zone is provided with a heat exchanging cooling chamber arranged out of the reactor above the top part of its housing. The built-in heat exchanger can be also made of two or more heat pipes interconnected through horizontal bridges.

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EFFECT: the invention ensures upgrade of the method and the apparatus for realization of the heterogeneous gaseous reactions in a pseudo-fluidized layer.

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