Reaction system and method for synthesizing olefin maleic anhydride polymer microspheres
By designing a system including a thermostat, a mixing device and a reactor, the problem of temperature control and mixing of reactants in the polymerization reaction of olefins and maleic anhydride is solved, and the efficient and stable polymerization reaction is achieved, which is suitable for large-scale Industrialized production.
Patent Information
- Application Number
- CN202310965698.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2023-08-02
- Publication Date
- 2025-02-14
AI Technical Summary
The prior art is difficult to achieve constant temperature control and rapid mixing of reactants in the polymerization of olefins and maleic anhydride, resulting in low reaction efficiency and uneven product products.
A system including a thermostat, a mixing device and a reactor is designed. The reactor inlet temperature is regulated by the thermostat, and the mixing device realizes rapid mixing of reactants, and the continuous design of the reactor and the ring of the temperature-controlled medium area is carried out. Assume that the temperature and pressure are stable.
The temperature stable control of the olefin maleic anhydride polymerization reaction and the rapid and uniform mixing of reactants are achieved, the reaction efficiency and quality stability of the product are improved, and it is suitable for large-scale industrial production.
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Figure CN119425602A_ABST
Abstract
Description
Technical Field
[0001] The invention belongs to the field of solution precipitation polymerization, and more specifically, relates to a reaction system and method for synthesizing olefin maleic anhydride polymer microspheres. Background Art
[0002] After olefins and maleic anhydride are mixed in a solvent, polymerization is carried out under the action of an initiator to obtain an emulsion polymer suspension. Based on the reasonable interaction between the polymer and the solvent, no additional surfactant or stabilizer is required, and the polymer obtained by the reaction can be stably suspended in the solvent for a long time. C4-C9 olefins can react with maleic anhydride under certain reaction conditions to form polymer microspheres by self-stabilizing precipitation polymerization. The size and particle size distribution of the polymer microspheres are related to the monomer concentration, initiator concentration, crosslinking agent concentration and reaction residence time.
[0003] The polymerization reaction of olefins and maleic anhydride is an exothermic reaction, and the heat release is uneven throughout the reaction process. Too high a temperature will lead to inactivation of the reaction and denaturation of the product, while too low a temperature will cause the reaction to stop and the microspheres to stop growing. Therefore, controlling the constant temperature of the reactor is the biggest difficulty.
[0004] In addition, the microspheres of the polymerization product of olefin and maleic anhydride are easily affected by shear force, resulting in changes in the morphology and particle size distribution of the microspheres, so it is impossible to use the stirring method to achieve convective heat transfer and heat removal.
[0005] CN113968927A uses a tubular reactor to synthesize low molecular weight styrene (a kind of olefin) and maleic anhydride resin. The method uses an initiator to pre-mix with a monomer and a solvent and then enter the reactor to heat the reaction; since the initiator needs to be stored at low temperature, the storage temperature of each monomer mixture is about 10 ° C, and the low temperature cold consumption is large, and the reaction needs to be carried out at more than 70 ° C, so the tubular reactor has a long section for the warming of the monomer mixture, which significantly extends the length of the reactor; in addition, the entire tubular reactor needs to be immersed in heat transfer oil, because the thermal conductivity of the heat transfer oil is low, and its temperature control will become very difficult after the capacity is expanded. On the other hand, the residence time of the tubular reactor is only 700s, and the reaction time of the olefin and maleic anhydride polymerization system is mostly several hours. If this configuration is adopted, the tubular reactor will be very long and difficult to carry out industrial production. Finally, the tubular reactor is horizontal, which will cause the microspheres to precipitate and hang on the wall of the reaction liquid at the end of the reaction, blocking the tube, and the reaction efficiency decreases. Moreover, the system has no mixing and temperature control device, and it is impossible to achieve industrial large-scale uniform mixing.
[0006] CN111085154AB adopts baffle design, which is only used for olefin and maleic anhydride polymerization of C2-C4, and cannot be applied to olefin and maleic anhydride polymerization of C5-C9. The method adds monomer and initiator etc. at different positions of the reactor to realize the reaction, and the heat is removed by cooling medium outside. The shortcoming of the method is that the local production of monomer addition is relatively large flow rate. It takes a long time for different materials to mix evenly, and only a small-scale reaction can be realized. If the production capacity is improved, the material is not easy to mix evenly, and the reaction residence time needs a large reactor volume, and the equipment occupies a large area. At the same time, the baffle after amplification is easy to appear wall hanging phenomenon, which is difficult to clean, and there is a local flow rate too fast at the baffle, which destroys the reaction microsphere, and easily causes the reaction product to be uneven. In addition, the method does not propose an effective reaction temperature control scheme, and the stable control of the reaction temperature of polymer microspheres is the key to the reaction system.
[0007] In summary, since the storage temperatures of the monomers, initiators and cross-linking agents in the olefin maleic anhydride polymerization reaction are different, the above-mentioned prior art cannot meet the requirements of rapid mixing of reaction raw materials, temperature adjustment and reaction heat removal during large-scale production. Therefore, it is necessary to develop a new reaction system or reactor to meet the special reaction conditions of the above-mentioned olefin maleic anhydride precipitation polymerization. Summary of the invention
[0008] The purpose of the present invention is to provide a reaction system and method for synthesizing olefin maleic anhydride polymer microspheres in view of the defects of the prior art. The present invention regulates the inlet temperature of the reactor by setting a thermostat, achieves efficient and rapid mixing by setting a mixing device, and proposes a new type of reactor, which can continuously and massively produce olefin maleic anhydride polymer microspheres.
[0009] In order to achieve the above-mentioned object, the present invention provides a synthetic olefin maleic anhydride polymer microsphere reaction system on the one hand, the system comprises a reactor, a thermostat, a flow control unit, a temperature control unit and a pressure control unit, and also comprises a mixing device and / or a feed distribution device;
[0010] The reactor comprises a reactor inlet, a reaction area, a reactor outlet and a temperature control medium area; the reactor inlet, the reaction area and the reactor outlet are connected in sequence, or, when a feed distribution device is present, the reactor inlet, the feed distribution device, the reaction area and the reactor outlet are connected in sequence; the temperature control medium area is arranged around the outer wall of the reaction area;
[0011] The thermostat comprises a thermostat medium side and a mixing monomer side;
[0012] The inlet on the mixed monomer side is connected to an olefin feed line, a maleic anhydride feed line and a solvent feed line, and is optionally connected to a cross-linking agent feed line;
[0013] The outlet of the mixed monomer side is connected to a mixed monomer outlet pipeline; the mixed monomer outlet pipeline and the initiator solution feed pipeline are both directly connected to the reactor inlet, or, when the mixing device exists, the mixed monomer outlet pipeline and the initiator solution feed pipeline are both connected to the reactor inlet through the mixing device;
[0014] The flow control unit is used to control the feed flow of the initiator solution, olefin, maleic anhydride, solvent and optionally the cross-linking agent;
[0015] The temperature control unit is used to control the flow rate of the temperature control medium entering the temperature control medium side and the flow rate of the temperature control medium entering the temperature control medium area;
[0016] The pressure control unit is used to control the reaction pressure of the reactor.
[0017] In the present invention, if Figure 1 , 2 As shown, the reactor inlet, the reaction zone and the reactor outlet are connected in sequence from bottom to top, or, when the feed distribution device is present, the reactor inlet, the feed distribution device, the reaction zone and the reactor outlet are connected in sequence from bottom to top; or, as Figure 3 As shown, the reactor inlet, the reaction zone and the reactor outlet are connected in sequence from top to bottom, or, when a feed distribution device is present, the reactor inlet, the feed distribution device, the reaction zone and the reactor outlet are connected in sequence from top to bottom.
[0018] According to the present invention, preferably, the reaction area includes at least one reaction chamber, and each reaction chamber is distributed along the axial direction of the reaction area; the inlets of each reaction chamber are interconnected; and the outlets of each reaction chamber are interconnected.
[0019] According to the present invention, preferably, the temperature control medium area includes at least one temperature control medium cavity, and the temperature control medium cavities are interconnected or not interconnected.
[0020] According to the present invention, preferably, the reactor outlet is also connected to a reaction polymer discharge pipeline, and the reaction polymer discharge pipeline is connected to a downstream separation device.
[0021] According to the present invention, preferably, the feed distribution device is a distribution plate and / or a distribution pipe.
[0022] According to the present invention, preferably, the outer wall of the distribution plate is tightly connected to the inner wall of the shell at the inlet of the reactor;
[0023] The distribution plate is of bubble cap type, orifice plate type or water cap type.
[0024] According to the present invention, preferably, the annular tube or the branch-shaped tube;
[0025] The distribution pipe is provided with at least one opening, and the diameter of the opening is 1-25 mm.
[0026] According to the present invention, preferably, the number of the mixing devices is 1-2.
[0027] According to the present invention, preferably, the mixing device is a static mixer, a dynamic mixer or a microinterface mixer.
[0028] According to the present invention, preferably, the flow control unit includes an olefin feed flow control subunit, a maleic anhydride feed flow control subunit, a solvent feed flow control subunit and an initiator solution feed flow control subunit, and optionally includes a crosslinking agent feed flow control subunit.
[0029] According to the present invention, preferably, the temperature control unit comprises a reactor temperature control subunit and a mixed monomer temperature control subunit; preferably, the reactor temperature control subunit is at least one group.
[0030] According to the present invention, preferably, the pressure control unit comprises a reactor pressure control subunit.
[0031] According to the present invention, preferably, the outlet of the temperature control medium side is connected to the inlet of the temperature control medium in the temperature control medium area, and the outlet of the temperature control medium in the temperature control medium area is connected to the inlet of the temperature control medium side, forming a closed loop.
[0032] Another aspect of the present invention provides a method for synthesizing olefin maleic anhydride polymer microspheres, wherein the method uses the system and comprises the following steps:
[0033] The olefin, maleic anhydride, solvent and optional cross-linking agent are fed into the thermostat respectively through flow control to obtain a mixed monomer at a target temperature;
[0034] The mixed monomers at the target temperature are fed into the reactor inlet together with the initiator solution, or the mixed monomers at the target temperature and the initiator solution are mixed uniformly by the mixing device and then fed into the reactor inlet; a reaction is carried out in the reaction area to obtain a reaction product, which is discharged from the system through the reactor outlet.
[0035] According to the present invention, preferably, the reaction product discharged from the system enters the downstream separation device for separation.
[0036] According to the present invention, preferably, the olefin is a C4-C9 olefin and / or a hydrocarbon mixture having a C4-C9 olefin content of greater than 20% by mass.
[0037] According to the present invention, preferably, the solvent is at least one organic solvent selected from the group consisting of alcohols, esters, ketones, alkanes and ethers.
[0038] According to the present invention, preferably, the cross-linking agent is divinylbenzene and / or styrene.
[0039] According to the present invention, preferably, the initiator solution is a solution formed by dissolving the initiator in the solvent; the initiator is at least one of azobisisobutyronitrile, azobisisoheptanenitrile and dibenzoyl peroxide.
[0040] According to the present invention, preferably, the operating temperature of the reaction zone is 40-130°C, the residence time is 0.5-12 hours, and the operating pressure is 0.5-2.5 MPaG; the temperature difference between the temperature control medium and the operating temperature of the reaction zone is within 20°C.
[0041] According to the present invention, preferably, the temperature of the outlet of the thermostat on the mixing monomer side is 40-100°C.
[0042] According to the present invention, preferably, the temperature range of the temperature regulating medium is 30-200°C.
[0043] According to the present invention, preferably, the temperature range of the temperature control medium is 30-90°C.
[0044] According to the present invention, preferably, the molar ratio of the olefin to maleic anhydride is (0.5-1):(1-3);
[0045] The content of maleic anhydride is 3%-15% based on the total weight of the mixed monomers at the target temperature;
[0046] The content of the crosslinking agent is 0.05%-2% based on the total weight of the maleic anhydride;
[0047] The content of the initiator is 0.05%-5% based on the total weight of the maleic anhydride.
[0048] In the present invention, the dosage ratio of the above-mentioned olefins, maleic anhydride, cross-linking agent, initiator, etc. adjusts the residence time of the reactor, determines the conversion rate of the monomer and the size of the product, and the reactor temperature control subunit controls the flow rate of the temperature control medium so that the mixed monomer reaches the target temperature, and then the mixed monomer at the target temperature is mixed with the initiator solution and enters the mixing device for rapid mixing. After being mixed evenly, it enters the reactor inlet and enters the reaction area after being distributed by the feed distribution device. The mixed monomer temperature control subunit controls the flow rate of the temperature control medium and the pressure control unit controls the reaction pressure of the reactor, thereby ensuring the stability of the system reaction temperature and pressure. The reaction product arrives at the reactor outlet after coming out of the reaction area, and then enters the downstream separation device for separation.
[0049] The beneficial effects of the technical solution of the present invention are as follows:
[0050] 1) The reactor in the reaction system of the present invention is a continuous reactor. The reaction system of the present invention eliminates the use of a stirred tank reactor, thereby simplifying the reactor design; the temperature control of the reaction system of the present invention is more accurate and stable; the present invention simplifies the production operation process, and the reaction capacity of the reactor in the reaction system of the present invention is increased by more than 10 times compared with that of a batch reactor, thereby realizing large-scale industrial continuous production of olefin maleic anhydride polymerization reaction in different solvent systems.
[0051] 2) The present invention uses a thermostat to achieve the initial reaction temperature requirements of olefins, maleic anhydride, solvents, cross-linking agents and initiators with different storage temperature requirements and source temperatures, thereby creating conditions for continuous reaction, solving the problems of difficulty in heat removal or local overcooling to stop the reaction due to different monomer storage temperatures, uneven mixing of continuous reactions, low flow requirements for polymerization reactions, and reduced heat transfer coefficient due to complex internal components and reaction wall hangings in the reactor, thereby achieving stable control of the polymerization reaction temperature and producing copolymer microsphere products with stable and uniform quality, laying a foundation for large-scale production.
[0052] 3) The present invention realizes rapid mixing of the mixed monomer and initiator solution through a mixing device.
[0053] 4) The system of the present invention has strong applicability and is suitable for the self-stabilized precipitation polymerization of C4-C9 olefins and maleic anhydride in various solvent systems to produce copolymer microspheres.
[0054] Other features and advantages of the present invention will be described in detail in the following detailed description. BRIEF DESCRIPTION OF THE DRAWINGS
[0055] The above and other objects, features and advantages of the present invention will become more apparent through a more detailed description of exemplary embodiments of the present invention in conjunction with the accompanying drawings, wherein like reference numerals generally represent like components throughout the exemplary embodiments of the present invention.
[0056] Figure 1 A schematic diagram of a reaction system for synthesizing olefin maleic anhydride polymer microspheres provided by the present invention is shown.
[0057] Figure 2 A schematic diagram of a reaction system for synthesizing olefin maleic anhydride polymer microspheres provided by the present invention is shown.
[0058] Figure 3 A schematic diagram of a reaction system for synthesizing olefin maleic anhydride polymer microspheres provided by the present invention is shown.
[0059] The following are the descriptions of the reference numerals:
[0060] Thermostat 1, mixing device 2, reaction area 3, feed distribution device 4, temperature control medium area 5, reactor inlet 6, reactor outlet 7, temperature control medium side 8;
[0061] Olefin feed pipeline 9, maleic anhydride feed pipeline 10, solvent feed pipeline 11, initiator solution feed pipeline 12, crosslinking agent feed pipeline 13, mixed monomer outlet pipeline 14, mixing device outlet 15; reaction polymer outlet pipeline 16, temperature regulating medium 17, temperature control medium 18;
[0062] Olefin feed flow control subunit F1, maleic anhydride feed flow control subunit F2, solvent feed flow control subunit F3, initiator solution feed flow control subunit F4, crosslinking agent feed flow control subunit F5, reactor temperature control subunit T1, mixed monomer temperature control subunit T2, reactor pressure control subunit P1. DETAILED DESCRIPTION
[0063] The preferred embodiments of the present invention will be described in more detail below. Although the preferred embodiments of the present invention are described below, it should be understood that the present invention can be implemented in various forms and should not be limited by the embodiments set forth herein. On the contrary, these embodiments are provided to make the present invention more thorough and complete, and to fully convey the scope of the present invention to those skilled in the art.
[0064] Example 1
[0065] This embodiment provides a reaction system for synthesizing olefin maleic anhydride polymer microspheres, such as Figure 1 As shown, the system includes a reactor, a thermostat 1, a flow control unit, a temperature control unit, a pressure control unit, a mixing device 2, and a feed distribution device 4;
[0066] The reactor inlet 6, the feed distribution device 4, the reaction area 3 and the reactor outlet 7 are connected in sequence from bottom to top; the temperature control medium area 5 is arranged around the outer wall of the reaction area 3; the reactor outlet 7 is also connected to a reaction polymer discharge pipeline 16, and the reaction polymer discharge pipeline 16 is connected to a downstream separation device; the feed distribution device 4 is a distribution plate, the outer wall of which is tightly connected to the inner wall of the shell of the reactor inlet 6, and the distribution plate is a bubble cap type; the mixing device 2 is a dynamic mixing kettle.
[0067] The thermostat 1 comprises a thermostat medium side 8 and a mixing monomer side;
[0068] The inlet on the mixed monomer side is connected with an olefin feed pipeline 9, a maleic anhydride feed pipeline 10, a solvent feed pipeline 11, and a cross-linking agent feed pipeline 13;
[0069] The outlet of the mixed monomer side is connected to a mixed monomer outlet pipeline 14; the mixed monomer outlet pipeline 14 and the initiator solution feed pipeline 12 are both connected to the reactor inlet 6 through the mixing device 2;
[0070] The flow control unit is used to control the feed flow of initiator solution, olefin, maleic anhydride, solvent and crosslinking agent, including olefin feed flow control subunit F1, maleic anhydride feed flow control subunit F2, solvent feed flow control subunit F3, initiator solution feed flow control subunit F4, crosslinking agent feed flow control subunit F5;
[0071] The temperature control unit is used to control the flow rate of the temperature control medium entering the temperature control medium side and the flow rate of the temperature control medium entering the temperature control medium area, and includes a reactor temperature control subunit T1 and a mixed monomer temperature control subunit T2;
[0072] The pressure control unit is used to control the reaction pressure of the reactor, and includes a reactor pressure control subunit P1.
[0073] This embodiment also provides a method for synthesizing olefin maleic anhydride polymer microspheres, using the above system, comprising the following steps:
[0074] 1) Isobutylene (normal temperature), maleic anhydride (65°C), solvent isoamyl acetate (45°C) and cross-linking agent divinylbenzene (6°C) are added to the thermostat 1 at 150kg / h, 160kg / h, 1200kg / h and 2.5kg / h respectively through respective flow control, the temperature of the outlet of the mixed monomer side of the thermostat 1 is set to 75°C, that is, the temperature of the mixed monomer is 75°C, the thermostat 1 is passed through the thermostat 1 for temperature adjustment, and the temperature of the inlet of the thermostat medium side is 100°C;
[0075] 2) After the mixed monomer comes out from the outlet on the mixed monomer side of the thermostat, it is mixed with 50 kg / h of a 7.5% concentration of initiator isoamyl azobisisobutyronitrile acetate solution (45° C.) and then enters the dynamic mixer. After passing through the dynamic mixer, it enters the reactor inlet 6 from the lower part of the reactor and enters the reaction zone 3 through the feed distribution device 4.
[0076] 3) The reaction temperature of the reaction zone 3 is set to 72°C, the residence time of the reactor is about 4.1h, the reaction temperature is controlled by controlling the flow rate of the temperature control medium, the temperature of the temperature control medium inlet is 60°C, the reaction pressure of the reactor outlet 7 is set to 0.8MPaG, and polymer microspheres are obtained at the reactor outlet 7. The polymer microspheres enter the downstream separation device through the reaction polymer discharge pipeline 16 for product separation. The yield of the polymer microspheres after separation is 75% (calculated as maleic anhydride).
[0077] Example 2
[0078] This embodiment provides a reaction system for synthesizing olefin maleic anhydride polymer microspheres. The difference between this embodiment and embodiment 1 is that: the mixing device is a static mixer;
[0079] This embodiment also provides a method for synthesizing olefin maleic anhydride polymer microspheres, using the above system, comprising the following steps:
[0080] 1) an isobutylene-containing C4 mixture (normal temperature, isobutylene content 39%wt), maleic anhydride (65°C), a solvent isoamyl acetate (45°C) and a cross-linking agent divinylbenzene (6°C) are added to a thermostat 1 at 262kg / h, 120kg / h, 900kg / h and 2kg / h respectively through respective flow control, the temperature of the outlet of the mixed monomer side of the thermostat 1 is set to 72°C, that is, the temperature of the mixed monomer is 72°C, a temperature regulating medium is introduced into the thermostat 1 for temperature adjustment, and the temperature of the inlet of the temperature regulating medium side is 100°C;
[0081] 2) After the mixed monomer comes out from the outlet on the mixed monomer side of the thermostat, it is mixed with 40 kg / h of a 7.5% initiator isoamyl azobisisobutyronitrile acetate solution (45° C.) and then enters the static mixer. After passing through the static mixer, it enters the reactor inlet 6 from the lower part of the reactor and enters the reaction zone 3 through the feed distribution device 4.
[0082] 3) The reaction temperature of the reaction zone 3 is set to 73°C, the residence time of the reactor is about 4.6 hours, the reaction temperature is controlled by controlling the flow rate of the temperature control medium, the temperature of the temperature control medium inlet is 64°C, the reaction pressure of the reactor outlet 7 is set to 0.8MPaG, and polymer microspheres are obtained at the reactor outlet 7. The polymer microspheres enter the downstream separation device through the reaction polymer discharge pipeline 16 for product separation. The yield of the polymer microspheres after separation is 79% (calculated as maleic anhydride).
[0083] Example 3
[0084] This embodiment provides a reaction system for synthesizing olefin maleic anhydride polymer microspheres, such as Figure 2 As shown, the difference between this embodiment and embodiment 1 is only that:
[0085] The inlet on the mixed monomer side is not connected to the cross-linking agent feeding pipeline 13 .
[0086] This embodiment also provides a method for synthesizing olefin maleic anhydride polymer microspheres, using the above system, comprising the following steps:
[0087] 1) 2-methyl-1-butene (normal temperature), maleic anhydride (65°C), and solvent (a mixture of isoamyl acetate and hexane, molar ratio 3:1, 45°C) are added to the thermostat 1 at 123 kg / h, 150 kg / h, and 1140 kg / h respectively through respective flow control, and the temperature of the outlet of the mixed monomer side of the thermostat 1 is set to 72°C, that is, the temperature of the mixed monomer is 72°C, and the thermostat 1 is passed through the thermostat 1 for temperature adjustment, and the temperature of the inlet of the thermostat medium side is 110°C;
[0088] 2) After the mixed monomer comes out from the outlet on the mixed monomer side of the thermostat, it is mixed with 53 kg / h of 7.5% initiator ethylene diisobutyronitrile (45° C.) and then enters the dynamic mixing kettle. After passing through the dynamic mixing kettle, it enters the reactor inlet 6 from the lower part of the reactor and enters the reaction zone 3 through the feed distribution device 4.
[0089] 3) The reaction temperature of the reaction zone 3 is set to 75°C, the residence time of the reactor is about 4.3h, the reaction temperature is controlled by controlling the flow rate of the temperature control medium, the temperature of the temperature control medium inlet is 70°C, the reaction pressure of the reactor outlet 7 is set to 0.65MPaG, and polymer microspheres are obtained at the reactor outlet 7. The polymer microspheres enter the downstream separation device through the reaction polymer discharge pipeline 16 for product separation. The yield of the polymer microspheres after separation is 65% (calculated as maleic anhydride).
[0090] The embodiments of the present invention have been described above, and the above description is exemplary, not exhaustive, and is not limited to the disclosed embodiments. Many modifications and changes will be apparent to those skilled in the art without departing from the scope and spirit of the described embodiments.
Claims
1. A reaction system for synthesizing olefin maleic anhydride polymer microspheres, characterized in that: The system comprises a reactor, a thermostat, a flow control unit, a temperature control unit and a pressure control unit, and also comprises a mixing device and / or a feed distribution device; The reactor comprises a reactor inlet, a reaction area, a reactor outlet and a temperature control medium area; the reactor inlet, the reaction area and the reactor outlet are connected in sequence, or, when a feed distribution device is present, the reactor inlet, the feed distribution device, the reaction area and the reactor outlet are connected in sequence; the temperature control medium area is arranged around the outer wall of the reaction area; The thermostat comprises a thermostat medium side and a mixing monomer side; The inlet on the mixed monomer side is connected to an olefin feed line, a maleic anhydride feed line and a solvent feed line, and is optionally connected to a cross-linking agent feed line; The outlet of the mixed monomer side is connected to a mixed monomer outlet pipeline; the mixed monomer outlet pipeline and the initiator solution feed pipeline are both directly connected to the reactor inlet, or, when the mixing device exists, the mixed monomer outlet pipeline and the initiator solution feed pipeline are both connected to the reactor inlet through the mixing device; The flow control unit is used to control the feed flow of the initiator solution, olefin, maleic anhydride, solvent and optionally the cross-linking agent; The temperature control unit is used to control the flow rate of the temperature control medium entering the temperature control medium side and the flow rate of the temperature control medium entering the temperature control medium area; The pressure control unit is used to control the reaction pressure of the reactor.
2. The synthetic olefin maleic anhydride polymer microsphere reaction system according to claim 1, wherein: The reaction area includes at least one reaction chamber, each reaction chamber is distributed along the axial direction of the reaction area; the inlets of each reaction chamber are interconnected; and the outlets of each reaction chamber are interconnected; The temperature control medium area includes at least one temperature control medium cavity, and each temperature control medium cavity is interconnected or disconnected with each other; The reactor outlet is also connected to a reaction polymer discharge pipeline, and the reaction polymer discharge pipeline is connected to a downstream separation device; The feed distribution device is a distribution plate and / or a distribution pipe.
3. The synthetic olefin maleic anhydride polymer microsphere reaction system according to claim 2, wherein: The outer wall of the distribution plate is tightly connected to the inner wall of the shell at the inlet of the reactor; The distribution plate is of bubble cap type, orifice plate type or water cap type.
4. The synthetic olefin maleic anhydride polymer microsphere reaction system according to claim 2, wherein: The distribution pipe is a ring-shaped pipe or a tree-shaped pipe; The distribution pipe is provided with at least one opening, and the diameter of the opening is 1-25 mm.
5. The synthetic olefin maleic anhydride polymer microsphere reaction system according to claim 1, wherein: The number of the mixing devices is 1-2; The mixing device is a static mixer, a dynamic mixing kettle or a micro-interface mixer.
6. The synthetic olefin maleic anhydride polymer microsphere reaction system according to claim 1, wherein: The flow control unit includes an olefin feed flow control subunit, a maleic anhydride feed flow control subunit, a solvent feed flow control subunit and an initiator solution feed flow control subunit, and optionally includes a cross-linking agent feed flow control subunit; The temperature control unit includes a reactor temperature control subunit and a mixed monomer temperature control subunit; preferably, the reactor temperature control subunit is at least one group; The pressure control unit includes a reactor pressure control subunit.
7. The synthetic olefin maleic anhydride polymer microsphere reaction system according to claim 1, wherein: The outlet of the temperature control medium side is connected to the inlet of the temperature control medium in the temperature control medium area, and the outlet of the temperature control medium in the temperature control medium area is connected to the inlet of the temperature control medium side, forming a closed loop.
8. A reaction method for synthesizing olefin maleic anhydride polymer microspheres, characterized in that: The method adopts the system according to any one of claims 1 to 7, comprising the following steps: The olefin, maleic anhydride, solvent and optional cross-linking agent are fed into the thermostat respectively through flow control to obtain a mixed monomer at a target temperature; The mixed monomers at the target temperature are fed into the reactor inlet together with the initiator solution, or the mixed monomers at the target temperature and the initiator solution are mixed uniformly by the mixing device and then fed into the reactor inlet; a reaction is carried out in the reaction area to obtain a reaction product, which is discharged from the system through the reactor outlet.
9. The method for synthesizing olefin maleic anhydride polymer microspheres according to claim 8, wherein: The reaction products discharged from the system enter the downstream separation device for separation; The olefin is a C4-C9 olefin and / or a hydrocarbon mixture having a C4-C9 olefin content of greater than 20% by mass; The solvent is at least one organic solvent selected from alcohols, esters, ketones, alkanes and ethers; The cross-linking agent is divinylbenzene and / or styrene; The initiator solution is a solution formed by dissolving the initiator in the solvent; the initiator is at least one of azobisisobutyronitrile, azobisisoheptanenitrile and dibenzoyl peroxide; The operating temperature of the reaction zone is 40-130°C, the residence time is 0.5-12 hours, and the operating pressure is 0.5-2.5MPaG; the temperature difference between the temperature control medium and the operating temperature of the reaction zone is within 20°C; The temperature of the outlet of the mixed monomer side of the thermostat is 40-100°C; The temperature range of the temperature regulating medium is 30-200°C.
10. The method for synthesizing olefin maleic anhydride polymer microspheres according to claim 9, wherein: The molar ratio of the olefin to maleic anhydride is (0.5-1):(1-3); The content of maleic anhydride is 3%-15% based on the total weight of the mixed monomers at the target temperature; The content of the crosslinking agent is 0.05%-2% based on the total weight of the maleic anhydride; The content of the initiator is 0.05%-5% based on the total weight of the maleic anhydride; The temperature range of the temperature control medium is 30-90°C.
Citation Information
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