RU2711295C2 - Process line and method of producing polymerisation products thereon - Google Patents

Abstract

FIELD: physics.

SUBSTANCE: invention relates to equipment for performance of technological cycle for production of anti-turbulence additives. Technological line for production of anti-turbulence additive includes devices: capacity of loading of carrier fluid - perfluorinated compound, loading capacity of monomer - high alpha-olefin, a polymerisation reactor, a separation device, a filter, a mixing apparatus, a disperser, a condensate collector connected to the heat exchanger, as well as a container with a dispersion medium. Devices form the first circular contour and the second circular contour. Process line comprises container with dispersion medium, which is connected to mixing device, mixing device has input from filter, which is technologically connected to separation device, and mixing device is connected to finished anti-turbulence additive dispersant. Also described is a method of producing an anti-turbulence additive on the disclosed process line.

EFFECT: use of the process line with a polymerisation reactor enables to create streams of a solvent and a monomer with repeated use of components, efficient separation of components in the reactor, wherein efficiency of using the equipment increases with high quality of the obtained polymerisation products.

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Description

The invention relates to equipment for conducting continuous chemical processes, namely, the technological cycle for producing anti-turbulent additives, can be used to carry out polymerization processes with the formation of polymer particles on the surface of a solid catalyst or to carry out other catalytic and heterogeneous chemical reactions or mass transfer processes, including number, with the formation of particles of the solid phase and (or) with a change in the density of the solid phase.

A chemical process is known for producing a suspension antiturbulent additive using equipment including a polymerization reactor, a precipitation reactor, a mixing tank, a polymer purification column, a flow dispersant in which hexene-1 is polymerized in a batch reactor R-1 with an anchor mixer. The scheme of this process is described in the dissertation of Stankevich B.C. - Section 5 - “The process of obtaining a suspension of antiturbulent additives based on polyhexene for the transportation of hydrocarbon liquids”, Nat. researched Tom. Polytechnic un-t - Tomsk, 2013 .-- 153 p.: Ill. RSL OD, 13 13-5 / 837.

Also known is a production line for producing an anti-turbulent additive based on polyolefins, which is the closest analogue and described in the utility model patent of the Russian Federation No. 142733, (published on June 27, 2014, bull. No. 18). The line consists of a capacitive polymerizer, which is connected in series with a screw pump, and that, in turn, is connected in series with a capacitive degasser-disperser, to which a decanter-type centrifugal apparatus and a finished product homogenizer are connected in series with the pipe. Moreover, the degasser-dispersant at the inlet is equipped with a flat-slot nozzle with a slit width of 1-4 mm, and is also equipped with a vapor condenser.

The disadvantages of the known production lines are the low efficiency of using the volume of the production lines due to the high viscosity of the solutions of high molecular weight polyalphaolefins, as well as the complexity and laboriousness of separating polyalphaolefins from the solution, due to the low resistance of high molecular weight polyalphaolefins in solution to hydrodynamic effects.

The objective of the invention is to increase the efficiency of using the production line for the production of polymerization products by isolating the polymer from the solution in the form of solid particles during the polymerization process, as well as to reduce the complexity and achieve a stable state of a highly concentrated suspension of high molecular weight polyalphaolefins without their destruction and preliminary grinding.

The technical result is the creation of circular contours for technological cycles:

- the first circular loop is formed by sequentially placed and technologically interconnected loading capacity of the monomer - the highest alpha olefin, a polymerization reactor containing a carrier fluid to form a reaction medium, a separation device, a heat exchanger and a condensate collector connected to the loading capacity of the monomer - higher alpha an olefin;

- the second circular circuit is formed by sequentially placed and technologically interconnected capacity of the carrier fluid, a polymerization reactor in which the carrier fluid is used to form a reaction medium, a separation device connected to the carrier fluid; and

- the production line contains a container with a dispersion medium, which is connected to the mixing apparatus, the mixing apparatus has an input from a filter, which is technologically connected to the separation device, and the mixing apparatus is connected to the dispersant of the finished anti-turbulent additive.

The task is achieved in that the polymerization products are obtained using a production line on which the carrier fluid and the higher alpha-olefin are fed into the polymerization reactor, in which the polymerization reaction proceeds in the presence of a titanium-magnesium catalyst. The polymerization process is carried out in a carrier liquid medium to form a reaction process medium, followed by separation, and then the resulting product is fed through a filter to a mixing apparatus in which it is connected to a dispersion medium until a stable homogeneous suspension is formed, which then goes to the packing operation. Perfluorinated compounds are used as the carrier fluid of the reaction process.

The polymerization process is carried out until the formation of polymer particles of not more than 1 mm, and complete when the conversion of the higher poly-alpha-olefin reaches at least 40 and not more than 70%.

At the separation stage, the polymerization products are separated into streams, the product of higher density returns to the polymerization stage, and the lower density through the heat exchanger and condensate collector enters the polymerization reactor for reuse.

The specified method is implemented on the production line of polymerization products, including a polymerization reactor, a heat exchanger and a dispersant of the finished product, which additionally introduced the container loading components (carrier fluid, higher alpha-olefin), a special tank, separation device, heat exchanger, filter, and mixing apparatus which form closed loops.

The first circular circuit is formed by a higher alpha-olefin — higher alpha-olefin loading capacitor sequentially placed and technologically interconnected, a polymerization reactor containing a carrier fluid to form a reaction medium, a separation device, a heat exchanger and a condensate collector connected to the higher alpha loading capacitance -olefin - a higher alpha olefin.

The second circular contour is formed by sequentially placed and technologically interconnected storage capacity of the carrier fluid, a polymerization reactor in which the carrier fluid is used to form a reaction medium, a separation device connected to the capacity of the carrier fluid.

The production line contains a container with a dispersion medium, which is connected to the mixing apparatus, the mixing apparatus has an input from a filter, which is technologically connected to the separation device, and the mixing apparatus is connected to the dispersant of the finished anti-turbulent additive.

A special container is connected to the mixing apparatus and the dispersant of the finished product.

The polymerization reactor of the technological line consists of a housing, inside which there is a mixing device consisting of a shaft with blades made in the form of external and internal tapes twisted in opposite directions, while the blades of the lower part of the inner tapes are mounted on the shaft and located below the blades of the outer tapes and made in pairs, and the length of the blades selected with the ability to capture solid and suspended components of the reaction mass from the surface of the liquid.

The invention is illustrated in the image, where in FIG. 1 schematically shows a production line for producing polymerization products, FIG. 2 - polymerization reactor.

The production line consists of tanks 1 and 2 - loading of input components in an amount of at least two, and a special loading tank 3. Tanks 1, 2 of the loading of input components are connected to the polymerization reactor 4, and to the separation device 5. The separation device 5 through the heat exchanger 6 and the condensate collector 7 is connected to the input tank 1. The separation device 5 is connected through a filter 8 to the mixing apparatus 9 and to the dispersant 10 of the finished product. A special loading capacity 3 is connected to the mixing apparatus 9.

The polymerization reactor 4 consists of a housing 11 provided with a thermostatic jacket 12. Inside the housing there is a shaft 13, on which 14 - external tapes are fixed; 15 - inner tapes; 16 - magnetic clutch; 17 - gear motor; a - supply of reagents; b - removal of reaction products; c, d - removal and supply of coolant; d - drain; e - viewing window.

The technological line for the production of polymerization products works as follows.

From the feed tank 1 of the input components, a higher alpha olefin, for example, hexene 1, enters the polymerization reactor 4, at the same time from the feed tank 2 of the input components, a carrier fluid, for example, perfluorodimethylcyclohexane. The volume ratio of the input components should correspond from 2: 1 to 1: 2.

The polymerization takes place in the polymerization reactor 4, but does not allow isolation of the higher alpha olefin, which is a solvent for the resulting poly alpha olefin, in the form of a liquid phase. At the same time, a catalytic system consisting of a catalyst, for example, titanium-magnesium and organoaluminum cocatalyst, is loaded into the polymerization reactor 4, while the polymerization process of the hexene-1 component in the medium of perfluorinated compounds proceeds in the polymerization reactor 4.

As a result of this process, a polymer is formed in the polymerisation reactor 4 in the form of particles that are rounded in shape and have a porous structure, and the process continues until a particle size of not more than 1 mm is obtained. The process ends when the conversion of the hexene 1 component is at least 40%, but not more than 70%.

Let us consider in more detail the design of the polymerization reactor 4, in which the main operation takes place - the production of poly-alpha-olefin, which is the main active ingredient of the anti-turbulent additive.

The reactor 4 operates as follows. The input components enter through the nozzle into the housing 11 for supplying reagents a.

The solid particles of the catalyst and the polymer particles forming around them are maintained in suspension using the outer and inner stirrer belts 14 and 15 mounted on a common shaft 13.

The heat generated by the polymerization is removed from the reaction mass through the wall of the jacket 12. The cooled reaction mass moves down along the wall of the jacket 12 in a downward flow formed by the outer pair of tapes 14.

An upward flow is formed in the central part of the reactor by an inner pair of belts 15. The coolant enters the shirt through the fitting g, heating up, rises and is removed from the shirt 12 through the fitting in.

Catalyst particles with a density higher than the density of the initial charge are picked up by the upward flow in the central part of the reactor and rise up. The location of the lower edges of the inner pair of tapes 15 avoids the formation of a stagnant zone in the lower part of the reactor. The polymer particles formed on the surface of the catalyst with a density lower than the density of the initial charge are picked up by a downward flow near the wall of the shirt and fall down. The capture of light particles of the solid phase from the surface of the reaction mass is due to the fact that the blades of the outer tapes 16 protrude above the free surface of the reaction mass. The ascending and descending flows resulting from the rotation of the tapes 14, 15 ensure that the particles of the solid phase are kept in suspension throughout the synthesis process. The rotation of the mixer is carried out through the use of a gear motor 17 connected by a shaft 13 of the mixer through a magnetic coupling 16.

The end of the synthesis is judged by the reduction in thermal power diverted from the reactor. After the synthesis is completed, the reaction mass with the accumulated polymer is discharged from the reactor through the nozzle b.

To ensure the possibility of technological processes in an oxygen-free environment, as well as to prevent leakage of volatile process media from the reactor and the ingress of substances from the environment into the reactor, the stirrer is driven through a magnetic coupling.

Next, the resulting reaction mass is fed into the separation device 5, where it is divided into the following 2 streams. The first stream - perfluorodimethylcyclohexane settles in the lower part of the device and returns to the loading capacity of 2 input components. The second stream, hexene-1, evaporates as a result of heat supply to the jacket of the separator 5 and enters the heat exchanger 6, then it condenses and enters the load tank 1 of the input components for reuse through the condensate collector 7.

The third stream, namely, the polymer obtained as a result of synthesis, from the separation device 5 is fed through a filter 8 to the mixing and preparation apparatus 9 of an anti-turbulent additive (PTP).

In the polymerization process in the reactor 4, agglomerates are formed from polymer particles — the formation of several adhering particles, which must be destroyed to obtain a uniform fluid stable suspension.

For this, dispersion medium is preliminarily added from a special container 3 to the mixing and preparation unit 9 of the anti-turbulent additive (PTP) preparation unit, and then the contents are mixed in the mixing and preparation unit 9 (PTP), which is structurally connected to the flow dispersant 10, and through the dispersant 10, a circular flow of motion is formed.

In the dispersant 10, under the hydrodynamic influence, the agglomerates of the polymer particles break up and a stable homogeneous suspension is obtained.

The process ends if at least one, but not more than four volumes of the dispersion pass through the dispersant 10, counting on the mixing apparatus 9. Under the dispersion volume is meant the volume obtained in the process of preparing the finished form of PTP dispersion, that is, if we received 500 l of dispersion, then it must go through the dispersant from 1 to 4 times. Upon completion of the process, the finished product goes to the packaging operation.

The use of the proposed production line with a polymerization reactor allows one to obtain an anti-turbulent additive with the creation of carrier fluid and monomer flows — a higher alpha olefin with reuse of components, to efficiently separate the components in the reactor, while increasing the efficiency of using equipment with high quality of the obtained polymerization products.

Claims (10)

1. A technological line for producing an anti-turbulent additive, characterized in that it includes the following devices: loading capacity of a carrier fluid — perfluorinated compound, loading capacity of a monomer — higher alpha olefin, polymerization reactor, separation device, filter, mixing apparatus, dispersant, collector condensate connected to a heat exchanger, as well as a container with a dispersion medium, forming the following circular contours: - the first circular circuit is formed by sequentially placed and technologically interconnected loading capacity of the monomer - higher alpha-olefin, a polymerization reactor containing a carrier fluid to form a reaction medium, a separation device, a heat exchanger and a condensate collector connected to the loading capacity of the monomer - higher alpha an olefin; - the second circular circuit is formed by sequentially placed and technologically interconnected capacity of the carrier fluid, a polymerization reactor in which the carrier fluid is used to form a reaction medium, a separation device connected to the carrier fluid; and the processing line contains a container with a dispersion medium, which is connected to the mixing apparatus, the mixing apparatus has an input from a filter, which is technologically connected to the separation device, and the mixing apparatus is connected to the dispersant of the finished anti-turbulent additive. 2. A method of producing an anti-turbulent additive on a production line according to claim 1, including - supply of a carrier fluid and a monomer — a higher alpha olefin — to a polymerization reactor in which a polymerization reaction takes place in the presence of a titanium-magnesium catalyst in a medium of a carrier fluid — perfluorinated compounds, The polymerization process is carried out in a carrier fluid to form a reaction medium until the formation of polymer particles of not more than 1 mm and is completed when the conversion of the monomer is not less than 40 and not more than 70%, followed by separation, during which the resulting products are separated into streams: - the first stream containing a product of higher density, mainly perfluorinated compounds, returns to the polymerization stage through a second circular loop of the processing line; - a second stream containing a product of lower density, mainly monomer, through the vapor phase and condensation is returned to the polymerization stage through the first circular loop of the production line; After separation, the obtained polymer product is filtered off and fed to the mixing apparatus, in which it is connected with the dispersion medium until a stable homogeneous suspension is formed, then dispersion is carried out, after which the finished anti-turbulent additive is fed to the packing operation.

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