Process system for preparing olefin copolymer

Abstract

The utility model provides a process system for preparing an olefin copolymer. The process system comprises a polymerization device; the belt type drying device is communicated with the polymerization device, so that the copolymer slurry in the polymerization device is conveyed to the belt type drying device to be dried; and the recovery device is communicated with the belt type drying device so as to recover the solvent and the monomer generated by drying in the belt type drying device. The process system for preparing the olefin copolymer can be used for industrial continuous production of maleic anhydride and olefin, the problem of rapid heat release in the polymerization process is relieved by continuously adding fresh raw materials, and rapid solid-liquid separation and solvent and monomer recovery are simultaneously realized through the belt type drying device; the copolymer does not need to be washed again to remove impurities, the problems of low efficiency and difficult wet material conveying caused by filtering are avoided, the reaction process is short, the operation is simple, and the method is suitable for industrial production.

Description

Technical Field

[0001] The utility model relates to the field of continuous production of olefin-maleic anhydride copolymers, in particular to a process system for preparing olefin copolymers. Background Art

[0002] Olefin-maleic anhydride copolymer is an amphiphilic polymer prepared by copolymerization of maleic anhydride and olefin under the action of an initiator. The olefin segment in the structure has strong lipophilicity, and the maleic anhydride segment has good hydrophilicity, which can be used for amphiphilic interface materials. This polar copolymer has rich chemical derivative reactions. The anhydride group in the maleic anhydride copolymer can further undergo esterification, amidation, imidization and ionization reactions. It has a wide range of uses in adhesives, drilling fluids, crude oil depressants, adhesives, emulsion polymerization stabilizers, highly absorbent polymers, cement water reducers, scale inhibitors in pipelines, paper coating materials, plastic modifiers, etc. The non-polarity of polyolefins (polyethylene, polypropylene, etc.) limits their application in the field of composites involving polar interfaces and polar materials. Maleic anhydride olefin copolymer products can be used for the composite of polyolefins with polar materials such as ABS, polycarbonate, nylon, polyester, etc., expanding the application range of polyolefin materials.

[0003] Maleic anhydride is solid, and olefin is gas or liquid. Maleic anhydride needs to be dissolved in a suitable solvent in advance and contacted with olefin to cause polymerization reaction. Since unreacted maleic anhydride monomer will cause the polymerization product to be unstable, bring odor, produce color and other problems, it is necessary to select a suitable solvent (which can dissolve maleic anhydride monomer but cannot dissolve the polymerization product, such as ethyl acetate, acetone, etc.) to wash the polymerization product and then filter it.

[0004] At present, in the industrial production process of maleic anhydride olefin copolymer, solid-liquid separation often adopts methods such as vacuum cone filtration, centrifuge or plate-and-frame filtration, but due to the small particles, there is a problem of slow filtration efficiency. At the same time, the purification process still needs to be repeatedly separated from the solid, which aggravates the problem of low production efficiency and has a serious impact on normal production efficiency. Moreover, these filtering methods of the prior art have intermittent filtration or violent empty operation, which has a certain danger and needs to improve process continuity and safety. Utility Model Content

[0005] The main purpose of the utility model is to provide a process system for preparing olefin copolymers, so as to overcome the defects in the prior art that it is difficult to realize continuous production when copolymerizing maleic anhydride and olefins, and the solid-liquid separation efficiency is low.

[0006] In order to achieve the above object, the utility model provides a process system for preparing olefin copolymers, comprising:

[0007] Polymerization device;

[0008] A belt drying device, connected to the polymerization device, so that the copolymer slurry in the polymerization device is transported to the belt drying device for drying;

[0009] A recovery device is connected to the belt drying device to recover the solvent and monomer generated by drying in the belt drying device.

[0010] In one embodiment of the process system for preparing olefin copolymers described in the utility model, the polymerization device is further connected to a maleic anhydride storage tank, an olefin storage tank and an initiator storage tank.

[0011] In one embodiment of the process system for preparing olefin copolymers described in the utility model, the maleic anhydride storage tank and the initiator storage tank are respectively connected to the solvent storage tank; and stirring units are respectively provided in the maleic anhydride storage tank and the initiator storage tank.

[0012] In one embodiment of the process system for preparing olefin copolymers described in the utility model, the polymerization device includes a prepolymerization reactor and a loop reactor connected to each other, the prepolymerization reactor is connected to the maleic anhydride storage tank, the olefin storage tank and the initiator storage tank respectively, and the loop reactor is connected to the belt drying device.

[0013] In one embodiment of the process system for preparing olefin copolymers of the utility model, the prepolymerization reactor and the loop reactor are respectively provided with temperature control units.

[0014] In one embodiment of the process system for preparing olefin copolymers described in the utility model, the loop tube reactor includes a circulation tube and a partition, the partition is arranged in the circulation tube to divide the circulation tube into a plurality of rooms, each room is provided with an inlet and an outlet.

[0015] In one embodiment of the process system for preparing olefin copolymers described in the utility model, the recovery device is a separator, and the solvent and monomers produced by the drying enter the separator for separation to obtain recovered solvent and recovered monomers.

[0016] In one embodiment of the process system for preparing olefin copolymers described in the utility model, the separator is connected to the olefin storage tank to transport the recovered monomer to the olefin storage tank.

[0017] In one embodiment of the process system for preparing olefin copolymers described in the utility model, the maleic anhydride storage tank and the initiator storage tank are respectively connected to the solvent storage tank; the separator is also connected to the solvent storage tank to transport the recovered solvent to the solvent storage tank.

[0018] In one embodiment of the process system for preparing olefin copolymers described in the utility model, the belt drying device is a single-stage belt dryer, a multi-stage belt dryer or a multi-layer belt dryer.

[0019] Beneficial effects of the utility model:

[0020] The process system for preparing olefin copolymers of the utility model can be used for industrial continuous polymerization of maleic anhydride and olefins, and the problem of rapid heat release in the polymerization process is alleviated by continuously adding fresh raw materials. The belt drying device is used to simultaneously realize rapid separation of solid and liquid and recovery of solvent and monomer. The copolymer does not need to be washed and impurities removed again, and the problems of low efficiency caused by filtration and difficulty in conveying wet materials are avoided. The reaction process is short, the operation is simple, and the utility model is suitable for industrial production. BRIEF DESCRIPTION OF THE DRAWINGS

[0021] Figure 1 This is a schematic diagram of a process system for preparing olefin copolymers in one embodiment of the utility model;

[0022] Figure 2 The present invention is a flow chart of a method for preparing olefin copolymers in one embodiment of the present invention.

[0023] Wherein, the reference numerals are:

[0024] V11 Solvent Tank

[0025] V12 Maleic Anhydride Storage Tank

[0026] V13 Initiator Tank

[0027] V14 Olefin Storage Tank

[0028] R11 Prepolymerization Reactor

[0029] R12 loop reactor

[0030] V21 Copolymer Slurry Tank

[0031] G31 Belt Dryer

[0032] T51 Recovery Unit DETAILED DESCRIPTION

[0033] The technical scheme of the utility model is described in detail below. The following implementation methods are implemented on the premise of the technical scheme of the utility model, and a detailed implementation process is given. However, the protection scope of the utility model is not limited to the following implementation methods. The structures or experimental methods in the following implementation methods that do not specify specific conditions are usually based on conventional conditions.

[0034] The utility model provides a process system for preparing olefin copolymers, see Figure 1 , including a polymerization device, a belt drying device G31 and a recovery device T51.

[0035] In one embodiment, the process system for preparing olefin copolymers of the utility model can be used for copolymerization of olefin and maleic anhydride. Wherein, the olefin can be a gaseous olefin or a liquid olefin. In another embodiment, the polymerization device of the utility model is connected with the maleic anhydride storage tank V12, the olefin storage tank V14 and the initiator storage tank V13 to transport maleic anhydride, olefin and initiator to the polymerization device for polymerization reaction. The utility model does not specifically limit the type of olefin, for example, isobutylene, styrene, etc. The utility model does not specifically limit the type of initiator, and any initiator commonly used in the art can be used.

[0036] In one embodiment, the polymerization device of the utility model comprises a prepolymerization reactor R11 and a loop reactor R12 connected to each other, olefin and maleic anhydride are prepolymerized in the prepolymerization reactor R11, and continuous feeding can take away a large amount of polymerization heat generated in the initial stage. Then, the prepolymerization product is transported to the loop reactor R12, and controlled final polymerization is achieved by adjusting the flow rate and reaction time.

[0037] In one embodiment, the prepolymerization reactor R11 of the utility model is connected to the maleic anhydride storage tank V12, the olefin storage tank V14 and the initiator storage tank V13 respectively, and the loop reactor R12 is connected to the belt drying device G31. The prepolymerization reactor R11, the maleic anhydride storage tank V12, the olefin storage tank V14 and the initiator storage tank V13 are provided with flow meters, for example, to control the flow rate. In another embodiment, the maleic anhydride storage tank V12 and the initiator storage tank V13 of the utility model are respectively connected to the solvent storage tank V11 to transport the solvent in the solvent storage tank V11 to the maleic anhydride storage tank V12 and the initiator storage tank V13; in another embodiment, the maleic anhydride storage tank V12 and the initiator storage tank V13 of the utility model are respectively provided with stirring units to stir the materials in the storage tanks to make them evenly mixed.

[0038] In one embodiment, a temperature control unit and a stirring unit are provided in the prepolymerization reactor R11 to control the temperature of the polymerization process and to stir the polymer material. The present invention does not specifically limit the temperature control unit, for example, it is a heat medium jacket layer design, and the temperature of the polymerization process is adjusted by the heat medium flow rate.

[0039] The utility model does not specifically limit the loop reactor R12, and any conventional loop reactor in the art can be used. In one embodiment, the loop reactor R12 includes a circulation pipe and a partition, which is arranged in the circulation pipe to divide the circulation pipe into a plurality of rooms, each of which is provided with an inlet and an outlet.

[0040] The belt drying device G31 of the utility model is connected to the polymerization device, specifically, the belt drying device G31 is connected to the loop reactor R12, so that the copolymer slurry in the loop reactor R12 is transported to the belt drying device G31 for drying. The utility model realizes the rapid separation of solid and liquid and the recovery of solvent and monomer at the same time through the belt drying device. Compared with the prior art in which the copolymer slurry is first filtered and centrifuged and then subjected to ordinary drying, the utility model has the advantages of high processing efficiency, no need for washing, and easy material transportation.

[0041] The utility model does not specifically limit the belt drying device, and any belt drying machine commonly used in the art can be used. The belt drying device of the utility model can be a single-stage belt drying machine, a multi-stage belt drying machine or a multi-layer belt drying machine, which can be selected according to the needs.

[0042] In one embodiment, a copolymer slurry tank V21 is further provided between the belt drying device G31 and the loop reactor R12 for storing the copolymer slurry obtained by polymerization in the loop reactor R12.

[0043] The utility model does not particularly limit the drying temperature and drying pressure of the belt drying device G31, which can be selected as needed. Through drying, the solvent and unreacted monomers in the copolymer slurry are converted into gaseous state and discharged from the belt drying device G31, and the dried copolymer product is discharged from the system.

[0044] The recovery device T51 of the utility model is connected to the belt drying device G31 to recover the solvent and monomer produced by drying in the belt drying device. In one embodiment, the recovery device T51 is a separator, and the solvent and monomer produced by drying enter the separator for separation to obtain recovered solvent and recovered monomer. The utility model does not particularly limit the structure of the separator, for example, it is a distillation device, and the solvent and monomer are separated by distillation. In one embodiment, the recovery device T51 is connected to the olefin storage tank V14 to transport the recovered monomer to the olefin storage tank V14. In another embodiment, the recovery device T51 is connected to the prepolymer reactor (polymerization device) to transport the recovered monomer to the prepolymer reactor (polymerization device). In another embodiment, the recovered monomer is circulated back to the recovery device T51 through a pipeline.

[0045] In one embodiment, the recovery device T51 is connected to the solvent storage tank V11 to transport the recovered solvent to the solvent storage tank V11. In another embodiment, the recovered solvent is circulated back to the recovery device T51 through a pipeline.

[0046] The process system for preparing olefin copolymers of the utility model can realize continuous production of olefin-maleic anhydride copolymers, including continuous solid-liquid separation and purification of copolymer slurry, thereby solving the problems of low efficiency of filtering, centrifugation and other methods and difficulty in conveying wet materials.

[0047] The process flow of this utility model is as follows Figure 2 As shown, maleic anhydride and olefin are first prepolymerized in the prepolymerization reactor R11, and then final polymerization is carried out in the loop reactor R12, and the flow rate and reaction time are adjusted as needed. After the polymerization process is completed, the copolymer slurry is directly transported to the belt drying device G31 to achieve the separation of solid and liquid. The belt drying device G31 can be dried under reduced pressure or vacuum. The solvent and unreacted monomers produced by drying are transported to the recovery device T51 for further separation and recovery, and the copolymer product obtained by drying is discharged from the system. The polymer product produced by the utility model does not undergo stirring, extrusion and other operations during the drying process, retains the original morphology of the polymerization form, is loose and easy to flow, and avoids the problem of agglomeration in the prior art.

[0048] The technical solution of the present application will be further described in detail below with specific embodiments.

[0049] Example 1

[0050] A certain amount of maleic anhydride is added to the maleic anhydride storage tank V12, and then butyl acetate in the solvent storage tank V11 is passed into the maleic anhydride storage tank V12 for dissolution, and then the completely dissolved maleic anhydride solution is added to the prepolymerization reactor R11, the prepolymerization reactor R11 is evacuated, and the liquid isobutylene in the olefin storage tank V14 is added to the prepolymerization reactor R11. Azobisisobutyronitrile is added to the initiator storage tank V13, and then butyl acetate is added for dissolution. After the material in the prepolymerization reactor R11 reaches the reaction temperature, the initiator solution is added to the prepolymerization reactor R11, and the reaction is carried out at 70°C for 0.2h. The mixed solution enters the loop reactor R12 at a fixed flow rate, and continues to polymerize in the loop reactor. After the polymerization is complete, it is transported to the copolymer slurry tank V21. The mixed solution in the copolymer slurry tank V21 is pumped into the belt drying device G31 for drying. The drying temperature is 120°C and the pressure is -0.08MPa. The product after drying is isobutylene-maleic anhydride copolymer. The solvent and excess isobutylene are transported to the recovery device T51 for separation of the solvent and olefins. The top temperature is 35°C, the bottom temperature is 75°C, the reflux ratio is 0.5, and the pressure is -0.1MPa. At the same time, the flow rate of the maleic anhydride storage tank V12, the flow rate of the olefin storage tank, and the flow rate of the initiator storage tank can realize the continuous feeding and discharging of the raw materials and realize the continuous production of maleic anhydride polar polymers.

[0051] Example 2

[0052] A certain amount of maleic anhydride is added to the maleic anhydride storage tank V12, and then the dimethyl carbonate in the solvent storage tank V11 is passed into the maleic anhydride storage tank V12 for dissolution, and then the completely dissolved maleic anhydride solution is added to the prepolymerization reactor R11, and the prepolymerization reactor R11 is evacuated, and the liquid styrene in the olefin storage tank V14 is added to the prepolymerization reactor R11. Benzoyl peroxide is added to the initiator storage tank V13, and then dimethyl carbonate is added to dissolve. After the material in the prepolymerization reactor R11 reaches the reaction temperature, the initiator solution is added to the prepolymerization reactor R11, and the reaction is carried out at 70°C for 0.4h. The mixed solution enters the loop reactor R12 at a fixed flow rate, and continues to polymerize in the loop reactor. After the polymerization is complete, it is transported to the copolymer slurry tank V21. The mixed solution in the copolymer slurry tank V21 is pumped into the belt drying device G31 for drying. The drying temperature is 140°C and the pressure is -0.09MPa. The product is styrene-maleic anhydride copolymer. The solvent and excess styrene are transported to the recovery device T51 for separation of solvent and olefin, with a tower top temperature of 90°C, a tower bottom temperature of 120°C, a reflux ratio of 0.5, and a pressure of -0.1MPa. At the same time, the flow rate of the maleic anhydride storage tank V12, the flow rate of the olefin storage tank, and the flow rate of the initiator storage tank can be set to achieve continuous feeding and discharging of raw materials and realize continuous production of maleic anhydride polar polymers.

[0053] Of course, the present invention may have many other embodiments. Without departing from the spirit and essence of the present invention, technicians familiar with the field may make various corresponding changes and deformations based on the present invention, but these corresponding changes and deformations should all fall within the scope of protection of the claims of the present invention.

Claims

1. A process system for preparing olefin copolymers, characterized in that: include: Polymerization devices; A belt drying device, connected to the polymerization device, so that the copolymer slurry in the polymerization device is transported to the belt drying device for drying; A recovery device is connected to the belt drying device to recover the solvent and monomer generated by drying in the belt drying device.

2. The process system for preparing olefin copolymers according to claim 1, characterized in that: The polymerization device is also connected to a maleic anhydride storage tank, an olefin storage tank and an initiator storage tank.

3. The process system for preparing olefin copolymers according to claim 2, characterized in that: The maleic anhydride storage tank and the initiator storage tank are respectively connected to the solvent storage tank; and stirring units are respectively arranged in the maleic anhydride storage tank and the initiator storage tank.

4. The process system for preparing olefin copolymers according to claim 2, characterized in that: The polymerization device comprises a prepolymerization reactor and a loop reactor which are connected. The prepolymerization reactor is connected to the maleic anhydride storage tank, the olefin storage tank and the initiator storage tank respectively, and the loop reactor is connected to the belt drying device.

5. The process system for preparing olefin copolymers according to claim 4, characterized in that: The prepolymerization reactor and the loop reactor are respectively provided with temperature control units.

6. The process system for preparing olefin copolymers according to claim 4, characterized in that: The loop reactor comprises a circulation tube and a partition, wherein the partition is arranged in the circulation tube to divide the circulation tube into a plurality of chambers, each of which is provided with an inlet and an outlet.

7. The process system for preparing olefin copolymers according to claim 2, characterized in that: The recovery device is a separator, and the solvent and monomer generated by the drying enter the separator for separation to obtain a recovered solvent and a recovered monomer.

8. The process system for preparing olefin copolymers according to claim 7, characterized in that: The separator is communicated with the olefin storage tank to transport the recovered monomer to the olefin storage tank.

9. The process system for preparing olefin copolymers according to claim 7, characterized in that: The maleic anhydride storage tank and the initiator storage tank are respectively connected to the solvent storage tank; the separator is also connected to the solvent storage tank to transport the recovered solvent to the solvent storage tank.

10. The process system for preparing olefin copolymers according to claim 1, characterized in that: The belt drying device is a single-stage belt drying machine, a multi-stage belt drying machine or a multi-layer belt drying machine.

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