Polyphenyl ether polymerization reaction device

Abstract

The invention belongs to the technical field of polyphenyl ether polymerization reaction, particularly relates to a polyphenyl ether polymerization reaction device, and provides the following scheme aiming at the problems that in the prior art, materials are easily stirred in a polymerization sleeve to generate explosion risk, and the materials and a catalyst are independently stirred to influence the working efficiency. The mixing device is used for mixing the catalyst; the raw material batching kettle is used for mixing raw materials, and stirrers are arranged in the catalyst batching kettle and the raw material batching kettle; and the polymerization sleeve reactor is used for carrying out mixed reaction on the raw materials and the catalyst. According to the polymerization sleeve reactor, no stirrer is arranged, in the rising section of the sleeve, along with introduction of oxygen, materials react in the sleeve and are fully mixed at the same time, the explosion risk of the materials caused by mechanical friction of the stirrer is eradicated, the raw materials and a catalyst can be mixed and stirred at the same time, and the working efficiency is improved.

Description

Technical Field

[0001] The invention relates to the technical field of polyphenylene ether polymerization reaction, in particular to a polyphenylene ether polymerization reaction device. Background Art

[0002] The synthesis of polyphenylene ether by precipitation polycondensation is that 2,6-dimethylphenol is catalyzed by copper-amine complex, and then oxidized, coupled, and polymerized in toluene solvent to obtain a crude product, and then extracted, precipitated, washed powder, dried, etc. to obtain a polypropyl ether product.

[0003] Oxidation, coupling and polymerization reactions are carried out in an intermittent reactor. The raw material 2,6-dimethylphenol is heated to become a liquid phase and then fully mixed with the toluene solution, and then slowly injected into the reactor with a metering pump. The catalyst copper chloride and complex amine are fully mixed with the toluene solution in the mixing tank and added to the reactor. At the same time, oxygen is bubbled into the bottom of the reactor, and stirring is turned on to allow the materials to fully react. After reacting for 3-4 hours, the materials are discharged. Since the oxidative coupling reaction is an exothermic reaction, in order to suppress side reactions, the polymerization reaction temperature is controlled to be maintained at about 25°C, and an external circulation heat extraction method is adopted, that is, part of the reaction mixture is extracted from the bottom of the kettle and returned from the top of the reactor after being heated with cold water. The extraction and separation of the reaction product is carried out in an extraction kettle, which is an intermittent operation equipment with a stirrer. The extractant and the reaction product are added to the extraction kettle respectively, stirred and then allowed to stand, and then the crude polyphenylene ether product without solvent is obtained by phase separation.

[0004] In the prior art, stirring of materials in a polymerization sleeve is prone to explosion risk, and stirring of materials and catalysts is performed separately, which affects work efficiency. Summary of the invention

[0005] The purpose of the present invention is to solve the shortcomings of the prior art that stirring of materials in a polymerization sleeve easily generates explosion risks, and stirring of materials and catalysts is performed separately, which affects work efficiency, and a polyphenylene ether polymerization reaction device is proposed.

[0006] In order to achieve the above object, the present invention adopts the following technical solutions:

[0007] A polyphenylene ether polymerization reaction device, comprising:

[0008] Catalyst batching kettle, used for mixing and batching the catalyst;

[0009] The raw material batching kettle is used to mix the raw materials. A stirrer is provided in both the catalyst batching kettle and the raw material batching kettle;

[0010] A polymerization sleeve reactor is used to mix raw materials and catalysts for reaction. A catalyst metering pump is connected between the catalyst batching kettle and the polymerization sleeve reactor. A raw material delivery pump is connected between the raw material batching kettle and the polymerization sleeve reactor.

[0011] A tail gas cooler is connected to the polymerization tube reactor and is used for cooling the tail gas;

[0012] A gas-liquid separation tank is connected to the bottom of the polymerization tube reactor and is used to separate gas and liquid;

[0013] The rotary disc extraction tower is used to extract the reaction materials, and an extraction tower feed pump is connected to the gas-liquid separation tank.

[0014] Preferably, the exhaust gas cooler is connected to a weapon processor.

[0015] Preferably, the top of the rotary disc extraction tower is connected to an auxiliary solution replenisher, and the reaction material is replenished with auxiliary solution through the auxiliary solution replenisher before entering the rotary disc extraction tower.

[0016] Preferably, the outside of the polymerization sleeve reactor is connected to an outer ring pipe and an inner ring pipe, the outer ring pipe is connected to a raw material delivery pump, the inner ring pipe is connected to a catalyst metering pump, the outer ring pipe and the inner ring pipe are both connected to oxygen ports, and cooling jackets are provided on the outside of the outer ring pipe and the inner ring pipe, and the cooling jackets are connected to a coolant.

[0017] Preferably, a catalyst kettle cover is provided on the top of the catalyst batching kettle, and a batching kettle cover is provided on the top of the raw material batching kettle. The same rectangular connecting box is installed on the top of the catalyst kettle cover and the batching kettle cover, and the two agitators are rotatably connected to the catalyst kettle cover and the batching kettle cover through bearings.

[0018] Preferably, the two agitators include two stirring rods, which are rotatably connected to the catalyst kettle cover and the ingredient kettle cover, stirring blades are installed on the outer sides of the two stirring rods, and scraper plates are installed on the bottom ends of the two stirring rods, and the two scraper plates are in contact with the inner walls of the catalyst ingredient kettle and the raw material ingredient kettle.

[0019] Preferably, a servo motor is installed at the bottom of the rectangular connecting box, and a rotating rod is rotatably installed in the rectangular connecting box through a bearing, first bevel gears are fixedly installed at both ends of the rotating rod, and second bevel gears are fixedly installed at the tops of the two stirring rods, the two first bevel gears are meshed with the two second bevel gears, a worm is installed on the output shaft of the servo motor, and a worm wheel is sleeved on the outer side of the rotating rod, and the worm is meshed with the worm wheel.

[0020] Preferably, linear motors are installed on the outer sides of the catalyst batching kettle and the raw material batching kettle, and the output shafts of the two linear motors are fixedly installed on the bottom of the rectangular connection box.

[0021] Preferably, the tops of the catalyst batching kettle and the raw material batching kettle are both provided with sealing rings, and the bottoms of the catalyst kettle cover and the batching kettle cover are both provided with sealing grooves, and the sealing rings cooperate with the corresponding sealing grooves.

[0022] In the present invention, the beneficial effects of the polyphenylene ether polymerization reaction device are:

[0023] The present invention adds 2-6-dimethylphenol and toluene into a raw material batching kettle, adds different types of catalysts into the catalyst batching kettle, starts a servo motor to drive a worm to rotate, the worm drives a rotating rod to rotate through a worm gear, the rotating rod drives two stirring rods to rotate through two first bevel gears and two second bevel gears, the two stirring rods drive a plurality of stirring blades to rotate, and respectively mix and stir with the raw material and the catalyst, the two stirring rods drive two scraping plates to make circular motion, the two scraping plates respectively clean the inner walls of the catalyst batching kettle and the raw material batching kettle, avoid materials adhering to the inner walls of the catalyst batching kettle and the raw material batching kettle, can mix and stir the raw material and the catalyst at the same time, and improve work efficiency;

[0024] The two linear motors provided in the present invention drive the catalyst kettle cover and the ingredient kettle cover to move upward by pushing the rectangular connection box upward, so that the agitator moves upward, which is convenient for cleaning;

[0025] There is no agitator in the polymerization sleeve reactor of the present invention. In the rising section of the sleeve, as oxygen is introduced, the materials are fully mixed while reacting in the sleeve, eliminating the risk of explosion of the materials due to mechanical friction of the agitator. The reaction product is finally deposited at the bottom of the reactor and flows to the gas-liquid separation tank by gravity, and oxygen is separated by standing, eliminating the transportation of oxygen-containing materials and reducing the explosion risk of the process. There is no need to set up a reaction product circulation pump and cooler, which simplifies the production process. The adopted sleeve heat exchange process can accurately control the reaction temperature, prevent the reactor from overheating, and effectively inhibit the occurrence of side reactions;

[0026] The reaction products of the present invention are initially separated inside the reactor, and the unreacted materials circulate between the outer loop pipe of the reactor and the reactor, thereby improving the conversion rate of the reaction, greatly reducing the catalyst and unreacted materials carried by the reaction products entering the gas-liquid separator, and reducing the load of subsequent treatment procedures.

[0027] The reaction product of the present invention flows from the bottom of the polymerization sleeve reactor to the gas-liquid separation tank, stands in the gas-liquid separation tank, and after the dissolved oxygen is separated, the reaction product is pumped to the upper part of the rotary disc extraction tower through the extraction tower feed pump, and before entering the rotary disc extraction tower, the inhibitor solution is injected through the auxiliary solution supplementer, and the extractant is injected into the lower part of the rotary disc extraction tower. The extractant dissolved with toluene is discharged from the top of the rotary disc extraction tower, and the final product PPE is discharged from the bottom of the rotary disc extraction tower. BRIEF DESCRIPTION OF THE DRAWINGS

[0028] Figure 1 This is a schematic structural diagram of a polyphenylene ether polymerization reaction device proposed by the present invention;

[0029] Figure 2 It is a cross-sectional structural schematic diagram of the catalyst batching kettle, raw material batching kettle, two agitators and related parts proposed in the present invention;

[0030] Figure 3 The present invention proposes Figure 2 Schematic diagram of the structure of part A;

[0031] Figure 4 This is a schematic diagram of the three-dimensional structure of the raw material batching kettle proposed by the present invention;

[0032] Figure 5 This is a schematic diagram of the bottom view of the batching kettle cover proposed by the present invention.

[0033] In the figure: 1. catalyst batching kettle; 2. catalyst metering pump; 3. raw material batching kettle; 4. raw material delivery pump; 5. polymerization sleeve reactor; 6. tail gas cooler; 7. gas-liquid separation tank; 8. extraction tower feed pump; 9. turntable extraction tower; 11. catalyst kettle cover; 12. oxygen inlet; 14. tail gas recovery device; 15. auxiliary solution replenisher; 18. agitator; 181. stirring rod; 182. stirring blade; 183. scraper plate; 19. outer ring pipe; 20. inner ring pipe; 21. linear motor; 22. rectangular connecting box; 23. bearing; 24. rotating rod; 25. first bevel gear; 26. second bevel gear; 27. servo motor; 28. worm; 29. ​​worm wheel; 31. batching kettle cover; 32. sealing ring; 33. sealing groove. DETAILED DESCRIPTION

[0034] The technical solution of this embodiment will be clearly and completely described below in conjunction with the drawings in this embodiment. Obviously, the described embodiment is only a part of this embodiment, rather than all of the embodiments.

[0035] Embodiment 1

[0036] Reference Figure 1-Figure 5 , a polyphenylene ether polymerization reaction device, comprising:

[0037] Catalyst batching kettle 1, used for mixing and batching the catalyst;

[0038] The raw material batching kettle 3 is used to mix the raw materials. The catalyst batching kettle 1 and the raw material batching kettle 3 are both provided with a stirrer 18;

[0039] The polymerization sleeve reactor 5 is used for mixing the raw materials and the catalyst for reaction. A catalyst metering pump 2 is connected between the catalyst batching kettle 1 and the polymerization sleeve reactor 5. A raw material delivery pump 4 is connected between the raw material batching kettle 3 and the polymerization sleeve reactor 5.

[0040] The tail gas cooler 6 is connected to the polymerization tube reactor 5 and is used for cooling the tail gas;

[0041] A gas-liquid separation tank 7 is connected to the bottom of the polymerization tube reactor 5 and is used to separate gas and liquid;

[0042] The rotary disc extraction tower 9 is used for extracting the reaction materials, and an extraction tower feed pump 8 is connected to the gas-liquid separation tank 7 .

[0043] In this embodiment, the exhaust gas cooler 6 is connected to a weapon processor 14 .

[0044] In this embodiment, the top of the rotary disc extraction tower 9 is connected to an auxiliary solution replenisher 15 , and the reaction material is replenished with auxiliary solution through the auxiliary solution replenisher 15 before entering the rotary disc extraction tower 9 .

[0045] In this embodiment, the outer side of the polymerization sleeve reactor 5 is connected to an outer ring pipe 19 and an inner ring pipe 20, the outer ring pipe 19 is connected to the raw material delivery pump 4, the inner ring pipe 20 is connected to the catalyst metering pump 2, the outer ring pipe 19 and the inner ring pipe 20 are both connected to the oxygen port 12, and the outer side of the outer ring pipe 19 and the inner ring pipe 20 are provided with cooling jackets, and the cooling jackets are connected to the coolant.

[0046] In this embodiment, a catalyst kettle cover 11 is provided on the top of the catalyst batching kettle 1, and a batching kettle cover 31 is provided on the top of the raw material batching kettle 3. The same rectangular connecting box 22 is installed on the top of the catalyst kettle cover 11 and the batching kettle cover 31, and the two agitators 18 are rotatably connected to the catalyst kettle cover 11 and the batching kettle cover 31 through bearings.

[0047] In this embodiment, the two agitators 18 include two stirring rods 181, and the two stirring rods 181 are rotatably connected to the catalyst kettle cover 11 and the ingredient kettle cover 31. Stirring blades 182 are installed on the outer sides of the two stirring rods 181, and scraper plates 183 are installed on the bottom ends of the two stirring rods 181. The two scraper plates 183 are in contact with the inner walls of the catalyst ingredient kettle 1 and the raw material ingredient kettle 3.

[0048] Specifically, the two stirring rods 181 drive the multiple stirring blades 182 to rotate, and mix and stir with the raw materials and the catalyst respectively. The two stirring rods 181 drive the two scraper plates 183 to make circular motion. The two scraper plates 183 clean the inner walls of the catalyst batching kettle 1 and the raw material batching kettle 3 respectively to prevent materials from adhering to the inner walls of the catalyst batching kettle 1 and the raw material batching kettle 3.

[0049] In this embodiment, a servo motor 27 is installed at the bottom of the rectangular connecting box 22, and a rotating rod 24 is rotatably installed in the rectangular connecting box 22 through a bearing 23. First bevel gears 25 are fixedly installed at both ends of the rotating rod 24, and second bevel gears 26 are fixedly installed at the tops of the two stirring rods 181. The two first bevel gears 25 are meshed with the two second bevel gears 26. A worm 28 is installed on the output shaft of the servo motor 27, and a worm wheel 29 is sleeved on the outer side of the rotating rod 24, and the worm 28 is meshed with the worm wheel 29.

[0050] Specifically, the servo motor 27 drives the worm 28 to rotate, the worm 28 drives the rotating rod 24 to rotate through the worm gear 29 , and the rotating rod 24 drives the two stirring rods 181 to rotate through the two first bevel gears 25 and the two second bevel gears 26 .

[0051] In this embodiment, linear motors 21 are installed on the outer sides of the catalyst batching kettle 1 and the raw material batching kettle 3 , and the output shafts of the two linear motors 21 are fixedly installed on the bottom of the rectangular connection box 22 .

[0052] Specifically, the two linear motors 21 drive the catalyst kettle cover 11 and the batching kettle cover 31 to move upward by pushing the rectangular connecting box 22 upward, so that the agitator 18 moves upward for easy cleaning.

[0053] In this embodiment, the top of the catalyst batching kettle 1 and the raw material batching kettle 3 are both provided with sealing rings 32, and the bottom of the catalyst kettle cover 11 and the batching kettle cover 31 are both provided with sealing grooves 33, and the sealing rings 32 cooperate with the corresponding sealing grooves 33; they are used to seal the catalyst batching kettle 1 and the raw material batching kettle 3.

[0054] Working principle, connect the power supply and controller;

[0055] First, 2-6-dimethylphenol and toluene are added to the raw material batching kettle 3, and different types of catalysts are added to the inside of the catalyst batching kettle 1, and the servo motor 27 is started to drive the worm 28 to rotate, and the worm 28 drives the rotating rod 24 to rotate through the worm gear 29, and the rotating rod 24 drives the two stirring rods 181 to rotate through the two first bevel gears 25 and the two second bevel gears 26, and the two stirring rods 181 drive multiple stirring blades 182 to rotate, respectively mixing and stirring with the raw materials and the catalyst, and the two stirring rods 181 drive two scraping plates 183 to make circular motions, and the two scraping plates 183 clean the inner walls of the catalyst batching kettle 1 and the raw material batching kettle 3 respectively to prevent the inner walls of the catalyst batching kettle 1 and the raw material batching kettle 3 from being attached to the materials; the two linear motors 21 are set to drive the catalyst kettle cover 11 and the batching kettle cover 31 to move upward by pushing the rectangular connecting box 22 to move upward, so that the agitator 18 moves upward, which is convenient for cleaning;

[0056] Secondly, after the mixing is completed, the mixed raw materials are delivered to the bottom of the outer ring pipe 19 of the polymerization sleeve reactor 5 by the raw material delivery pump 4, and enter the outer ring pipe 19 in the direction of the circulation, and the prepared catalyst is injected into the mixed raw materials by the catalyst metering pump 2, and oxygen is injected into the rising section of the outer ring pipe 19. The medium in the outer ring pipe 19 forms a fluid under the pressure of the injected medium and returns to the polymerization sleeve reactor 5.

[0057] Oxidation, coupling and polymerization reactions are carried out in the outer loop tube 19 and the reactor. The reaction products enter the polymerization sleeve reactor 5 from the outer loop tube in a tangential direction. After rotational separation, the reaction products with high density are deposited at the bottom of the reactor, and the materials with low density re-enter the reactor outer loop tube in the middle of the reactor to form a circulating flow. In order to improve the reaction conversion rate, another inner loop tube 20 is provided in the lower part of the polymerization sleeve reactor 5. The catalyst and oxygen are respectively introduced into the bottom of the inner loop tube 20, and the circulating flow formed in the inner loop tube 20 also returns to the polymerization sleeve reactor 5 in a tangential direction.

[0058] Since the oxidative coupling reaction is an exothermic reaction, cooling jackets are provided on the outside of the outer ring tube 19 and the inner ring tube 20, and a coolant is connected to the cooling jacket to maintain the reaction temperature at about 25°C and inhibit the occurrence of side reactions. A tail gas cooler 6 is provided on the top of the polymerization tube reactor 5, and the uncooled tail gas is sent to the inside of the tail gas recovery device 14.

[0059] The reaction product flows from the bottom of the polymerization sleeve reactor 5 to the gas-liquid separation tank 7, stands in the gas-liquid separation tank 7, and after the dissolved oxygen is separated, the reaction product is sent to the upper part of the rotary disc extraction tower 9 through the extraction tower feed pump 8. Before entering the rotary disc extraction tower 9, the inhibitor solution is injected through the auxiliary solution replenisher 15, and the extractant is injected into the lower part of the rotary disc extraction tower 9. The extractant dissolved with toluene is discharged from the top of the rotary disc extraction tower 9, and the final product PPE is discharged from the bottom of the rotary disc extraction tower 9.

[0060] Embodiment 2

[0061] The rest of the embodiment 2 is the same as the embodiment 1, except that a stirrer is also provided inside the rotary disc extraction tower 9, and the stirrer is used to stir during the extraction operation to improve the extraction effect.

[0062] The above description is only a preferred specific implementation manner of this embodiment, but the protection scope of this embodiment is not limited thereto. Any technician familiar with the technical field can make equivalent replacements or changes according to the technical scheme and inventive concept of this embodiment within the technical scope disclosed in this embodiment, and they should be covered by the protection scope of this embodiment.

Claims

1. A polyphenylene ether polymerization reaction device, characterized in that: include: A catalyst batching kettle (1) is used to mix and batch the catalyst; A raw material batching kettle (3) is used to mix the raw materials. A stirrer (18) is provided in both the catalyst batching kettle (1) and the raw material batching kettle (3); A polymerization sleeve reactor (5) is used to mix raw materials and catalysts for reaction. A catalyst metering pump (2) is connected between the catalyst batching kettle (1) and the polymerization sleeve reactor (5), and a raw material delivery pump (4) is connected between the raw material batching kettle (3) and the polymerization sleeve reactor (5); A tail gas cooler (6) is connected to the polymerization tube reactor (5) and is used to cool the tail gas; A gas-liquid separation tank (7), which is connected to the bottom of the polymerization tube reactor (5) and is used to separate gas and liquid; The rotary disc extraction tower (9) is used to extract the reaction materials and is connected to the gas-liquid separation tank (7) via an extraction tower feed pump (8).

2. A polyphenylene ether polymerization reaction device according to claim 1, characterized in that: The exhaust gas cooler (6) is connected to a weapon processor (14).

3. A polyphenylene ether polymerization reaction device according to claim 1, characterized in that: The top of the rotary disc extraction tower (9) is connected to an auxiliary solution replenisher (15), and the auxiliary solution is replenished by the auxiliary solution replenisher (15) before the reaction material enters the rotary disc extraction tower (9).

4. A polyphenylene ether polymerization reaction device according to claim 1, characterized in that: The outer side of the polymerization tube reactor (5) is connected to an outer ring pipe (19) and an inner ring pipe (20), wherein the outer ring pipe (19) is connected to a raw material delivery pump (4), and the inner ring pipe (20) is connected to a catalyst metering pump (2).

5. A polyphenylene ether polymerization reaction device according to claim 4, characterized in that: The outer ring tube (19) and the inner ring tube (20) are both connected to an oxygen port (12), and cooling jackets are provided on the outer sides of the outer ring tube (19) and the inner ring tube (20), and a coolant is connected to the cooling jackets.

6. A polyphenylene ether polymerization reaction device according to claim 1, characterized in that: The catalyst batching kettle (1) is provided with a catalyst kettle cover (11) on the top, and the raw material batching kettle (3) is provided with a batching kettle cover (31) on the top. The catalyst kettle cover (11) and the batching kettle cover (31) are provided with a same rectangular connection box (22) on the top. The two agitators (18) are rotatably connected to the catalyst kettle cover (11) and the batching kettle cover (31) via bearings.

7. A polyphenylene ether polymerization reaction device according to claim 6, characterized in that: The two stirrers (18) include two stirring rods (181), the two stirring rods (181) are rotatably connected to the catalyst kettle cover (11) and the batching kettle cover (31), the outer sides of the two stirring rods (181) are both equipped with stirring blades (182), the bottom ends of the two stirring rods (181) are both equipped with scraping plates (183), and the two scraping plates (183) are in contact with the inner walls of the catalyst batching kettle (1) and the raw material batching kettle (3).

8. A polyphenylene ether polymerization reaction device according to claim 6, characterized in that: A servo motor (27) is installed at the bottom of the rectangular connection box (22), a rotating rod (24) is rotatably installed in the rectangular connection box (22) through a bearing (23), first bevel gears (25) are fixedly installed at both ends of the rotating rod (24), second bevel gears (26) are fixedly installed at the top ends of the two stirring rods (181), the two first bevel gears (25) are meshed with the two second bevel gears (26), a worm (28) is installed on the output shaft of the servo motor (27), a worm wheel (29) is sleeved on the outer side of the rotating rod (24), and the worm (28) is meshed with the worm wheel (29).

9. A polyphenylene ether polymerization reaction device according to claim 6, characterized in that: Linear motors (21) are installed on the outside of the catalyst batching kettle (1) and the raw material batching kettle (3), and the output shafts of the two linear motors (21) are fixedly installed on the bottom of the rectangular connection box (22).

10. A polyphenylene ether polymerization reaction device according to claim 1, characterized in that: The tops of the catalyst batching kettle (1) and the raw material batching kettle (3) are both provided with sealing rings (32), the bottoms of the catalyst kettle cover (11) and the batching kettle cover (31) are both provided with sealing grooves (33), and the sealing rings (32) are matched with the corresponding sealing grooves (33).

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