High-viscosity polymerization reaction device

Abstract

The high-viscosity polymerization reaction device comprises a high-viscosity reaction kettle, a discharging machine, a circulating pump, a feeding machine and a feeding pump, a discharging opening in the bottom of the high-viscosity reaction kettle is connected with a feeding opening of the discharging machine, a screw of the discharging machine extends into the high-viscosity reaction kettle, a first discharging opening of the discharging machine is connected with a feeding opening of the circulating pump, and a second discharging opening of the discharging machine is connected with a feeding opening of the feeding pump. A feeding port, close to the upper end, of the side portion of the high-viscosity reaction kettle is connected with a discharging port of the feeding machine, a circulating pipeline used for achieving whole material external circulation is arranged between a discharging port of the circulating pump and a feeding port in the bottom end of the feeding machine, a feeding screw rod is arranged in the circulating pipeline, external reinforced circulating stirring is formed, and the feeding screw rod is connected with the high-viscosity reaction kettle. The high-viscosity polymerization reaction device disclosed by the utility model can effectively solve the problem of non-uniform mass transfer and heat transfer of the high-viscosity polymerization reaction, and can effectively control the reaction operation conditions, accurately monitor the viscosity change of the polymerization reaction, improve the quality of the polymerization reaction, reduce the production cost and improve the production efficiency. Therefore, the product quality is ensured.

Description

Technical Field

[0001] The utility model belongs to the technical field of high-viscosity polymerization reaction, and in particular relates to a high-viscosity polymerization reaction device. Background Art

[0002] High viscosity polymerization reactions are common in the field of polymer materials. As the polymerization reaction proceeds, the molecular weight gradually increases, and the viscosity can even reach tens of millions of centipoise in the later stage. At this time, the uniformity of polymerization stirring directly affects the mass transfer and heat transfer of the reaction, and ultimately determines the uniformity of the product molecular weight, affecting the product quality. At the same time, high viscosity materials are accompanied by serious wall sticking during stirring and discharging.

[0003] At present, for high-viscosity polymerization reaction systems, most of the research focuses on the optimization of the agitator itself. The Chinese utility model patent with the announcement number CN218689481U discloses a final polycondensation reactor, and the scraper is set for stirring to solve the wall sticking phenomenon. The Chinese invention patent with the publication number CN115888467A discloses a double-helix stirring reactor for high-viscosity silicone oil production, and the stirring effect is enhanced by designing a special stirring form. The Chinese utility model patent with the announcement number CN218077503U discloses an agitator for a high-viscosity polymerization reactor, which enhances the stirring and mixing effect by setting a special spiral belt stirring. The above patents only consider the stirring mass transfer and wall sticking problems, and ignore the problems of enhanced heat transfer and discharge residue. Therefore, it is necessary to provide a better and more efficient high-viscosity polymerization reaction device. Utility Model Content

[0004] In view of the problems existing in the prior art, the purpose of the utility model is to provide a high viscosity polymerization reaction device, which can achieve efficient mass transfer and heat transfer in high viscosity polymerization reactions and can effectively control product quality by controlling key operating parameters such as viscosity and temperature.

[0005] The technical solution of the utility model is as follows:

[0006] A high-viscosity polymerization reaction device comprises a high-viscosity reactor, a discharging machine, a circulating pump, a feeding machine and a feeding pump, wherein the bottom discharging port of the high-viscosity reactor is connected to the feeding port of the discharging machine, wherein the screw of the discharging machine extends into the high-viscosity reactor to realize the discharging of high-viscosity materials and reduce residues, the first discharging port of the discharging machine is connected to the feeding port of the circulating pump, the feeding port near the upper end of the side of the high-viscosity reactor is connected to the discharging port of the feeding machine, a circulating pipeline for realizing the overall external circulation of materials is provided between the discharging port of the circulating pump and the feeding port at the bottom of the feeding machine, a feeding screw is provided inside the circulating pipeline to form an external enhanced circulating stirring to realize the enhanced mass transfer and heat transfer during the reaction process, the second discharging port of the discharging machine is connected to the feeding port of the feeding pump, and the discharging port of the feeding pump is provided with a discharging pipeline.

[0007] Furthermore, the circulation pipeline is a jacketed pipe, and a refrigerant or a heat medium is introduced into the jacketed pipe of the circulation pipeline according to the heat conditions of the reaction; the discharge pipeline is a jacketed pipe, and a heat medium is introduced into the jacket of the discharge pipeline; a jacket is provided on the inlet pipe of the discharge machine, and a refrigerant or a heat medium is introduced into the pipe for heat transfer or heat supply.

[0008] Furthermore, the high viscosity reactor is provided with a jacket or a companion pipe outside, and a heat medium or a cold medium is arranged inside the jacket or the companion pipe of the high viscosity reactor.

[0009] Furthermore, an online thermometer 1 is provided at the lower part of the high-viscosity reactor; an online thermometer 2 is provided on the circulation pipeline; and an online thermometer 3 is provided on the discharge pipeline.

[0010] Furthermore, the circulation pipeline is provided with an online viscometer for real-time monitoring of the viscosity of the polymer material.

[0011] Furthermore, an online pressure gauge and an online liquid level gauge are provided on the upper part of the high viscosity reactor.

[0012] Furthermore, the discharging machine, circulating pump, feeding machine and feeding screw are all frequency conversion devices.

[0013] Furthermore, a stirring paddle is provided inside the high-viscosity reactor, wherein the stirring paddle is a frequency conversion device.

[0014] Furthermore, a nitrogen supply pipeline and a tail gas venting pipeline are provided at the bottom of the high viscosity reactor, wherein the nitrogen supply pipeline is provided with a second regulating valve, and the tail gas venting pipeline is provided with a first regulating valve.

[0015] Compared with the prior art, the beneficial effects of the utility model are as follows:

[0016] 1) By adopting the technical solution of the utility model, the polymerization reaction device compensates for the uneven mass and heat transfer caused by the stirring dead zone through a high-flux external circulation, and sets a jacket on the external circulation pipeline to further increase the heat exchange area, improve the heat exchange coefficient, and improve the shortcomings of insufficient heat exchange area and low heat exchange coefficient of the outer jacket of the simple reactor;

[0017] 2) The discharge port at the bottom of the high-viscosity reactor is connected to the feed port of the discharge machine, wherein the screw of the discharge machine extends into the interior of the high-viscosity reactor to discharge high-viscosity materials and reduce residues;

[0018] 3) A thermometer is arranged at the bottom of the high viscosity reactor of the utility model to monitor the reaction temperature in real time, and the reaction temperature is controlled by the flow rate of the refrigerant or heat medium passing into the jacket or accompanying pipe of the reactor;

[0019] 4) The outer circulation pipeline of the feeding screw of the utility model is a jacketed pipe, and a thermometer is provided to monitor the reaction temperature in real time, and the reaction temperature is controlled by the flow of the refrigerant or heat medium passing into the jacket;

[0020] 5) A viscometer is arranged on the upper part of the outer circulation pipeline of the feeding screw of the utility model to monitor the viscosity of the reaction system in real time and indirectly regulate the degree of polymerization through the viscosity at a constant temperature;

[0021] 6) The high-viscosity polymerization reaction device of the utility model can effectively improve the problems of uneven mass transfer and heat transfer in high-viscosity polymerization reactions, and can effectively control the reaction operating conditions and accurately monitor the viscosity changes of the polymerization reactions, thereby ensuring product quality; BRIEF DESCRIPTION OF THE DRAWINGS

[0022] Figure 1 It is a schematic diagram of the overall structure of the utility model device.

[0023] In the figure: 1. high viscosity reactor; 2. stirring paddle; 3. discharge machine; 4. circulation pump; 5. feeder; 6. feeding screw; 7. feeding pump; 8. circulation pipeline; 9. discharge pipeline; t1. online thermometer 1; t2. online thermometer 2; t3. online thermometer 3; l1. online liquid level gauge; p1. online pressure gauge; a1. online viscometer; c1. regulating valve 1; c2. regulating valve 2. DETAILED DESCRIPTION

[0024] The present invention will be further described below in conjunction with the accompanying drawings and embodiments, but the scope of protection of the present invention is not limited to the described scope.

[0025] like Figure 1 As shown, a high viscosity polymerization reaction device includes a high viscosity reactor 1, a discharge machine 3, a circulation pump 4, a feeder 5 and a feeder pump 7. The discharge port at the bottom of the high viscosity reactor 1 is connected to the feed port of the discharge machine 3, wherein the screw of the discharge machine 3 extends into the high viscosity reactor 1 to realize the discharge of high viscosity materials and reduce residues. The discharge port 1 of the discharge machine 3 is connected to the feed port of the circulation pump 4, and the feed port on the side of the high viscosity reactor 1 near the upper end is connected to the discharge port of the feeder 5.

[0026] A stirring paddle 2 is provided inside the high viscosity reactor 1, wherein the stirring paddle 2 is a frequency conversion device, and the mixing degree of the materials in the high viscosity reactor 1 can be regulated by setting the frequency.

[0027] In this embodiment, the stirring paddle 2 can be in various forms such as frame stirring, ribbon stirring, ribbon screw stirring, etc. The stirring paddle 2 can be selected as non-variable frequency stirring according to the viscosity characteristics. The stirring paddle motor transmits various signals of power, current, and torque to the outside.

[0028] In order to realize the overall external circulation of materials, a circulation pipeline 8 is provided between the discharge port of the circulation pump 4 and the feed port at the bottom of the feeder 5, and a feeding screw 6 is provided inside the circulation pipeline 8 to form an external enhanced circulation stirring to realize enhanced mass transfer and heat transfer during the reaction. The circulation pipeline 8 is a jacketed pipe. According to the heat condition of the reaction, a refrigerant or a heat medium is introduced into the jacketed pipe of the circulation pipeline 8 to realize heat transfer from the system or heat supply to the system to control the reaction temperature.

[0029] An online thermometer t2 is provided on the circulation pipeline 8. At the same time, an online viscometer a1 is provided on the circulation pipeline 8 to monitor the viscosity of the polymer material in real time.

[0030] The discharge port 2 of the discharge machine 3 is connected to the feed port of the feed pump 7. The inlet pipe of the discharge machine 3 is provided with a jacket, and a refrigerant or a heat medium is introduced for heat transfer or heat supply. The discharge port of the feed pump 7 is provided with a discharge pipeline 9. The discharge pipeline 9 is a jacketed pipe, and a heat medium is passed through the jacket of the discharge pipeline 9. An online thermometer 3 t3 is provided on the discharge pipeline 9. For example, by regulating the flow rate of the heat medium, the discharge temperature of the discharge pipeline 9 is controlled within an appropriate range to prevent the viscosity of the polymer material from increasing during the discharge process due to the temperature drop, and the discharge cannot be performed.

[0031] In this embodiment, a jacket is provided outside the high viscosity reactor 1, and a heat medium or a coolant passes through the jacket of the high viscosity reactor 1.

[0032] An online level gauge l1 is provided on the top of the high viscosity reactor 1 to monitor the material level in the stirring reactor in real time. For example, when the liquid level in the high viscosity reactor 1 is suitable, the stirring paddle 2 is started, and then the discharging machine 3, the circulating pump 4, the feeding machine 5 and the feeding screw 6 are started. An online thermometer t1 is provided on the bottom of the high viscosity reactor 1 to monitor the online thermometer t1 and the online thermometer t2 in real time. By adjusting the flow of the refrigerant or heat medium to the high viscosity reactor 1 and the flow of the refrigerant or heat medium to the jacket of the external circulation pipeline, the temperature of the online thermometer t1 and the online thermometer t2 is controlled to be at a suitable temperature; during the reaction process, the online viscometer a1 and the motor current and torque of the stirring paddle 2 are monitored in real time to judge the viscosity change of the polymer material, and finally judge whether the quality of the polymer product is qualified and whether the reaction is terminated.

[0033] An online pressure gauge p1 is provided on the top of the high viscosity reactor 1, and a nitrogen supply pipeline is provided on the top of the high viscosity reactor 1 for purging or pressure replenishment. A venting tail gas pipeline is also provided on the top of the high viscosity reactor 1 for exhaust. The nitrogen supply pipeline is provided with a regulating valve c2, and the venting tail gas pipeline is provided with a regulating valve c1. The reaction pressure can be regulated appropriately by adjusting the regulating valve c2 on the nitrogen supply pipeline and the regulating valve c1 on the venting tail gas pipeline. For example, during the feeding process, the reaction pressure is controlled by adjusting the opening of the regulating valve c1 on the venting tail gas pipeline; during the polymerization reaction process, non-condensable gas is generated, and the reaction pressure is controlled by adjusting the opening of the regulating valve c1 on the venting tail gas pipeline; during the discharging process, the reaction pressure is controlled by the regulating valve c2 on the nitrogen supply pipeline; the system purging before the reaction starts can be achieved by opening the regulating valve c2 on the nitrogen supply pipeline and the regulating valve c1 on the venting tail gas pipeline.

[0034] The discharge machine 3, circulation pump 4, feeder 5 and feed screw 6 are all frequency conversion devices with forward and reverse functions. The frequency of the equipment can be adjusted according to the needs of mass transfer and heat transfer, thereby regulating the external circulation volume. Forward rotation is the circulation process, and reverse rotation is the discharge process of the external circulation pipeline. For example, after the reaction is completed, the feed pump 7 is turned on, and the circulation pump 4, feeder 5 and feed screw 6 are set to reverse, so that the material can be discharged; by monitoring the online liquid level gauge l1 on the high-viscosity reactor 1, it can be determined whether the material in the high-viscosity reactor 1 has been transported; by detecting the motor power of the circulation pump 4, feeder 5, and feed screw 6, the discharge situation of the external circulation pipeline can be determined. Example 1

[0035] Reference now Figure 1 ,use Figure 1 The high viscosity polymerization reaction device shown is applied to the polycondensation reaction of meta-aramid fiber, and the viscosity of the material at the end of the polycondensation reaction is 1 million cp.

[0036] The polycondensation reaction process is as follows:

[0037] (1) In the early stage of the reaction, the pre-polycondensation reaction materials are transported into the high-viscosity reactor 1. When the liquid level of the online liquid level gauge l1 is appropriate, the stirring paddle 2, the discharging machine 3, the circulating pump 4, the feeding machine 5 and the feeding screw 6 are turned on, and isophthaloyl chloride is added dropwise at a constant flow rate through the feed pipeline. The reaction is an exothermic reaction. When the viscosity is below 10,000, there is no need to introduce a refrigerant into the system. It is only necessary to control the feed flow rate of isophthaloyl amide to control the reaction temperature to be maintained below 50°C;

[0038] (2) In the later stage of the reaction, when the viscosity reaches 10,000 cp, a large amount of heat will be generated during the stirring and forced circulation process. It is necessary to introduce a refrigerant into the jacket of the high-viscosity reactor 1 and the jacket of the external circulation pipeline of the feeding screw 6 to control the reaction temperature at 60°C.

[0039] (3) After the reaction is completed and the viscosity reaches 1 million cp, the reaction is completed, the feeding pump 7 is turned on, and the circulation pump 4, the feeding machine 5 and the feeding screw 6 are set to reverse, and the material is started to be discharged. During the discharging process, hot water is passed through the jacket of the discharging pipe to ensure that the material temperature during the discharging process is 50~60℃.

[0040] The high-viscosity polymerization reaction device is used to achieve efficient mass transfer and heat transfer in the high-viscosity aramid polymerization reaction. After completing the above process, the forced external circulation greatly improves the reaction mass transfer effect. The reaction time is reduced from 2 hours to 1 hour, the reaction discharge residue is reduced from 10% to 2%, and the reaction conversion rate is increased from 92% to 98%, greatly improving product quality.

Claims

1. A high-viscosity polymerization reaction device, comprising a high-viscosity reactor (1), a discharge machine (3), a circulation pump (4), a feeder (5) and a feeder pump (7), wherein the discharge port at the bottom of the high-viscosity reactor (1) is connected to the feed port of the discharge machine (3), wherein the screw of the discharge machine (3) extends into the interior of the high-viscosity reactor (1) to discharge the high-viscosity material and reduce the residue, the discharge port of the discharge machine (3) is connected to the feed port of the circulation pump (4), and the feed port on the side of the high-viscosity reactor (1) near the upper end is connected to the discharge port of the feeder (5), characterized in that A circulation pipeline (8) for realizing the overall external circulation of materials is provided between the discharge port of the circulation pump (4) and the feed port at the bottom end of the feeder (5). A feeding screw (6) is provided inside the circulation pipeline (8) to form an external enhanced circulation stirring to realize enhanced mass transfer and heat transfer during the reaction process. The second discharge port of the discharger (3) is connected to the feed port of the feed pump (7), and the discharge port of the feed pump (7) is provided with a discharge pipeline (9).

2. A high viscosity polymerization reaction device according to claim 1, characterized in that The circulation pipeline (8) is a jacketed pipe, and a refrigerant or a heat medium is introduced into the jacketed pipe of the circulation pipeline (8) according to the reaction heat conditions; the discharge pipeline (9) is a jacketed pipe, and a heat medium is introduced into the jacket of the discharge pipeline (9); the inlet pipe of the discharge machine (3) is provided with a jacket, and a refrigerant or a heat medium is introduced into the inlet pipe for heat transfer or heat supply.

3. A high viscosity polymerization reaction device according to claim 1, characterized in that The high viscosity reactor (1) is provided with a jacket or a companion pipe outside, and a heat medium or a cold medium is arranged inside the jacket or the companion pipe of the high viscosity reactor (1).

4. A high viscosity polymerization reaction device according to claim 1, characterized in that An online thermometer 1 (t1) is provided at the lower part of the high-viscosity reactor (1); an online thermometer 2 (t2) is provided on the circulation pipeline (8); and an online thermometer 3 (t3) is provided on the discharge pipeline (9).

5. A high viscosity polymerization reaction device according to claim 1, characterized in that The circulation pipeline (8) is provided with an online viscometer (a1) for real-time monitoring of the viscosity of the polymer material.

6. A high viscosity polymerization reaction device according to claim 5, characterized in that An online pressure gauge (p1) and an online liquid level gauge (l1) are provided on the upper part of the high viscosity reactor (1).

7. A high viscosity polymerization reaction device according to claim 1, characterized in that The discharging machine (3), the circulating pump (4), the feeding machine (5) and the feeding screw (6) are all frequency conversion devices.

8. A high viscosity polymerization reaction device according to claim 1, characterized in that The high-viscosity reactor (1) is provided with a stirring paddle (2) inside, wherein the stirring paddle (2) is a frequency conversion device.

9. A high viscosity polymerization reaction device according to claim 1, characterized in that A nitrogen supply pipeline and a tail gas discharge pipeline are provided at the bottom of the high viscosity reactor (1), wherein the nitrogen supply pipeline is provided with a second regulating valve (c2), and the tail gas discharge pipeline is provided with a first regulating valve (c1).

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