Post-treatment equipment for polyarylester emulsion and novel treatment process thereof

Abstract

The polyarylester emulsion post-treatment equipment comprises a reaction table, a water bath cavity is formed in the middle of the reaction table, a glass reaction kettle is fixedly installed in the middle of the water bath cavity, a tank cover assembly matched with the glass reaction kettle is arranged on the glass reaction kettle, and a main supporting column is fixedly arranged on one side of the top end of the reaction table; according to the polyarylester emulsion post-treatment equipment and the novel treatment process thereof, the process is environmentally friendly, the cost is low, operation is easy, a large amount of methanol organic solvent does not need to be poured in the treatment process for demulsification, and only direct distillation recycling treatment is conducted in an original sealed reaction kettle; according to the method, the low-boiling-point reaction solvent dichloromethane can be obtained by using the methanol demulsification process, the use of a large amount of methanol organic solvent in the methanol demulsification process and the subsequent separation of the methanol and dichloromethane mixed solvent are omitted, the methanol solvent volatilized into the environment is also greatly reduced, and the environment and experiment operators are protected.

Description

Technical Field

[0001] The invention relates to the technical field of polyarylate polymerization reaction, in particular to polyarylate emulsion post-processing equipment and a new processing process thereof. Background Art

[0002] Polyarylate is a type of amorphous high-performance polymer with benzene rings and ester bonds in the main chain. It has the advantages of high heat resistance, high optical transparency, low dielectric constant, and weather resistance. Therefore, in recent years, this material has been increasingly valued in the fields of aviation, ships, electronic communications, automobiles, high-speed rail, etc. in the form of special-shaped materials, films, fibers, etc. The mass production capacity of polyarylate materials in my country is still insufficient and heavily dependent on imports. Therefore, studying the polymerization preparation process of polyarylate materials is of great significance to the localization of polyarylate materials.

[0003] At present, the polyarylate polymerization process reported in the literature mainly adopts the interfacial polymerization process. Under the collision of the homogeneous organic phase and the aqueous phase with sufficient mechanical stirring, an efficient polymerization reaction occurs at the reaction interface to obtain an emulsion of a certain viscosity. The post-treatment of the emulsion is usually to first precipitate with a large amount of methanol, dissolve with dichloromethane, and then precipitate with methanol. After the process is cycled 1-5 times, it is rinsed and dried with deionized water several times to obtain the final high-purity polyarylate product. For example, Wei Xuping, Li Xiang and others from Donghua University directly precipitated the polymer solution obtained by interfacial polymerization with methanol, further obtained a translucent viscous gel, and repeatedly washed with ethanol and deionized water. The reaction solution was poured into deionized water to precipitate a white solid. The obtained product was crushed into powder with a pulverizer and extracted with hot deionized water and ethanol. This method uses low-boiling point methanol, which is prone to solvent recovery and environmental protection problems. Yang Jie and others from Sichuan University poured the solution obtained by interfacial polymerization directly into hot deionized water to precipitate a white solid, then crushed the white product into powder with a grinder, and extracted it with hot deionized water and ethanol to obtain the final polyarylate product (containing cyclohexane or spiral ring groups). Since the organic phase solvent used is low-boiling-point dichloromethane, the industrial operation process has difficulties in terms of recovery of the mixed solution of dichloromethane and water, environmental impact of solvent volatilization, and cost.

[0004] At present, the technical solutions for post-treatment of interfacial polymerization of polyarylates have obvious problems and shortcomings in industrial production, as follows: (1) Methanol is a low-boiling point organic solvent with a boiling point of less than 65°C. Methanol is more toxic than ethanol. The large-scale use of methanol solvent in industrial production processes will bring serious safety problems, high costs, environmental pollution, and health hazards to operators; (2) Even after methanol demulsification, a small amount of methanol will remain in the sample system even after washing with a large amount of deionized water. This will cause the volatilization of low-boiling point small molecules during processing, ultimately affecting product performance. Summary of the invention

[0005] The object of the present invention is to provide a polyarylate emulsion post-treatment device and a new treatment process thereof, so as to solve the problems of the prior art proposed in the above background technology that the post-treatment technology for preparing polyarylate emulsion by interfacial polymerization is complicated in operation (usually including methanol demulsification, multiple dissolutions of dichloromethane, ethanol distillation, etc.), solvent recovery is difficult (the waste liquid includes a mixed solution of methanol and dichloromethane, a mixed solution of water, ethanol and dichloromethane), and the environment is easily polluted (low-boiling-point dichloromethane, methanol, etc. are easily volatilized into the air or inhaled into the body by the operator).

[0006] To achieve the above-mentioned purpose, the present invention provides the following technical scheme: a polyarylate emulsion post-processing device, comprising a reaction table, a water bath chamber is opened in the middle of the reaction table, a glass reactor is fixedly installed in the middle of the water bath chamber, a tank cover assembly matching the glass reactor is provided on the glass reactor, a main support is fixedly installed on one side of the top of the reaction table, a control mechanism for controlling the polymerization reaction process is fixedly installed on the top of the main support, a motor support is installed in the middle of the main support, a mixing motor is fixedly installed on the motor support, a shaft sleeve is fixedly installed on the output end of the mixing motor, an assembly pin is threadedly connected to one side of the shaft sleeve, a secondary support is fixedly installed on the other side of the top of the reaction table, two support arms are installed in the middle of the secondary support, a condensation recovery mechanism for recovering reaction products is fixedly installed on one of the support arms, and a constant pressure dripping mechanism is fixedly installed on the other support arm.

[0007] Preferably, the control mechanism includes a control box, in which a variable frequency speed regulator, a single-chip microcomputer controller and a micro air pump are fixedly installed, an air outlet of the micro air pump is fixedly connected to a constant pressure duct, a box door is hinged on the front of the control box, a control panel is fixedly installed on the outside of the box door, a touch display and a power switch are fixedly installed on the surface of the control panel, the micro air pump, variable frequency speed regulator and touch display are all electrically connected to the single-chip microcomputer controller, and the hybrid motor is electrically connected to the variable frequency speed regulator.

[0008] Preferably, the tank cover assembly comprises a glass kettle cover, an axial connector is fixedly installed in the middle of the top of the glass kettle cover, a driving shaft is rotatably connected to the axial connector, a mixing shaft is fixedly provided at the bottom end of the driving shaft, a paddle is fixedly installed at the bottom end of the mixing shaft, a distillation nozzle, a feeding port, a test port and a dripping nozzle are fixedly provided on the periphery of the top of the glass kettle cover, a sealing plug is hinged on the feeding port, a glass rod with a handle is snap-connected to the middle of the test port, an upper sealing disk is fixedly provided at the bottom of the glass kettle cover, a lower sealing disk is fixedly provided at the top of the glass reactor, and a glass cover disk is fixedly provided on the outer side of the lower sealing disk.

[0009] Preferably, the condensation recovery mechanism includes a glass condenser, the bottom end of the glass condenser is fixedly connected to a solvent recovery bottle, a spiral heat exchange tube is fixedly arranged inside the glass condenser, one end of the spiral heat exchange tube is fixedly connected to a cooling water outlet, and the other end of the spiral heat exchange tube is fixedly connected to a cooling water inlet, one side of the solvent recovery bottle is fixedly connected to a steam conduit, a valve 2 is fixedly installed in the middle of the steam conduit, the bottom end of the solvent recovery bottle is fixedly connected to a four-way glass tube, a valve 1 is fixedly installed at the connection between the solvent recovery bottle and the four-way glass tube, and the steam conduit is sleeved on the distillation pipe mouth.

[0010] Preferably, the constant-pressure dripping mechanism comprises a glass liquid storage tube, the top of which is fixedly provided with a threaded pipe mouth, a sealing pipe cap is threadedly connected to the threaded pipe mouth, the bottom end of the glass liquid storage tube is fixedly connected to a dripping hose, the top of the dripping hose is fixedly installed with a valve three, the bottom end of the dripping hose is sleeved on the dripping pipe mouth, the top of one side of the glass liquid storage tube is fixedly connected to a pressurized air pipe, an electromagnetic balancing air valve is fixedly installed on the pressurized air pipe, the constant pressure conduit is sleeved on the pressurized air pipe, and the electromagnetic balancing air valve is electrically connected to the single-chip microcomputer controller.

[0011] Preferably, an electric heating tube and a temperature sensor are fixedly installed on the inner wall of the water bath chamber, and an addition hopper communicating with the water bath chamber is fixedly provided on one side of the reaction table.

[0012] Preferably, universal wheels are fixedly installed at the four corners of the bottom end of the reaction table, a drain pipe is fixedly connected to the bottom of the front of the reaction table, a drain valve is fixedly installed on the drain pipe, a liquid level observation window is fixedly provided in the middle of the front of the reaction table, and the capacity of the glass reactor is 20L.

[0013] A polyarylate emulsion post-treatment process comprises the following steps: S1: Prepare the aqueous reaction system: add bisphenol A, sodium hydroxide, benzyltriethylammonium chloride and deionized water into the glass reactor in sequence, start the mixing motor, and mechanically stir the added aqueous reaction system for 15 minutes until it is completely dissolved; S2: Prepare an organic reaction system: Add terephthaloyl chloride, isophthaloyl chloride and dichloromethane in a 20L beaker in sequence, and stir thoroughly using a scattering device until they are completely dissolved.

[0014] S3: Constant-pressure dropwise addition of the organic reaction system to the aqueous reaction system: Add the prepared organic reaction system to the constant-pressure dropwise addition mechanism, and add the homogeneous organic reaction system dropwise to the aqueous system under the condition of an ice-water bath at 5-15°C; S4: Prepare the end-capping reagent system. Stir and dissolve phenol, NaOH and deionized water in a 2L beaker, then pour them into the 20L reactor after the third step and stir them for 1 hour. During this time, use a glass rod to dip the reaction system into a pH test paper to adjust the pH value and observe whether the solution is neutral. If not, add a little formic acid until the solution is neutral and then terminate the reaction to obtain a special PC emulsion system. S5: Condensation recovery: first set the water bath temperature to 50-100°C, stir while heating, and observe the volatilization and collection of dichloromethane solvent in the emulsion system and the condensation recovery mechanism; S6. The precipitated product in the glass reactor is taken out and crushed first, then cleaned and filtered with high-temperature steam, and finally taken out and dried in a 100-150°C forced air oven to constant weight.

[0015] Preferably, in the step S3, the dripping time is controlled to be 3 hours. During the dripping process, the mixing motor is controlled to stir at a high speed of 300-400 r / min. After the dripping is completed, the reaction is fully stirred for 2 hours.

[0016] Compared with the prior art, the present invention has the following beneficial effects: The process is environmentally friendly, low-cost and easy to operate. In the post-treatment process of the polyarylate emulsion, there is no need to pour a large amount of methanol organic solvent into the emulsion for demulsification. The low-boiling-point reaction solvent dichloromethane can be obtained by direct distillation and recovery in the original sealed reactor, thereby eliminating the use of a large amount of methanol organic solvent in the methanol demulsification process and the subsequent separation of methanol and dichloromethane mixed solvents. At the same time, the methanol solvent volatilized into the environment is also greatly reduced, protecting the environment and experimental operators. High-purity and high-quality polyarylate material products can be manufactured. This technology uses boiling or high-temperature hot steam to clean the crushed polyarylate powder, which can effectively remove residual dichloromethane, chloride ions and other impurities coated in the material, thereby preparing high-purity polyarylate raw materials and high-quality modified polyarylate products. BRIEF DESCRIPTION OF THE DRAWINGS

[0017] Figure 1 It is a structural schematic diagram of the polyarylate emulsion post-processing equipment of the present invention; Figure 2It is a structural schematic diagram of the glass reactor of the present invention; Figure 3 It is a structural schematic diagram of the condensation recovery mechanism of the present invention; Figure 4 It is a structural schematic diagram of the constant pressure dripping mechanism of the present invention; Figure 5 It is a schematic cross-sectional structural diagram of the reaction platform of the present invention; Figure 6 It is a structural schematic diagram of the control box of the present invention; Figure 7 This is a flow chart of the post-treatment process of the polyarylate emulsion of the present invention; Figure 8 It is a schematic diagram of the post-treatment of the polyarylate emulsion of the present invention.

[0018] In the figure: 1. reaction table; 2. glass reactor; 3. condensation recovery mechanism; 301. glass condenser tube; 302. spiral heat exchange tube; 303. cooling water outlet; 304. cooling water inlet; 305. solvent recovery bottle; 306. four-way glass tube; 307. valve one; 308. steam conduit; 309. valve two; 4. main support; 5. auxiliary support; 6. constant pressure dripping mechanism; 61. glass liquid storage tube; 62. pressurized air pipe; 63. electromagnetic balance air valve; 64. threaded pipe mouth; 65. sealing pipe cap; 66. dripping hose; 67. valve three; 7. support arm; 8. constant pressure conduit; 9. mixing motor; 10. shaft sleeve; 11. Driving shaft; 12. Shaft connector; 13. Glass kettle cover; 14. Motor bracket; 15. Control box; 16. Operation panel; 17. Adding bucket; 18. Liquid level observation window; 19. Drain pipe; 20. Universal wheel; 21. Micro air pump; 22. Mixing shaft; 23. Paddle; 24. Lower sealing plate; 25. Upper sealing plate; 26. Feeding port; 27. Sealing plug; 28. Test port; 29. ​​Glass rod with handle; 30. Distillation tube mouth; 31. Dropping tube mouth; 32. Assembly pin; 33. Water bath chamber; 34. Electric heating tube; 35. Temperature sensor; 36. Box door; 37. Frequency converter; 38. Single chip microcomputer controller; 39. Glass cover plate. DETAILED DESCRIPTION

[0019] The technical solutions in the embodiments of the present invention will be described clearly and completely below in conjunction with the accompanying drawings in the embodiments of the present invention.

[0020] See also Figure 1-8The present invention provides a polyarylate emulsion post-processing device, comprising a reaction table 1, a water bath chamber 33 is provided in the middle of the reaction table 1, a glass reaction kettle 2 is fixedly installed in the middle of the water bath chamber 33, a tank cover assembly matching the glass reaction kettle 2 is provided on the glass reaction kettle 2, a main support 4 is fixedly installed on one side of the top of the reaction table 1, a control mechanism for controlling a polymerization reaction process is fixedly installed on the top of the main support 4, a motor bracket 14 is installed in the middle of the main support 4, a mixing motor 9 is fixedly installed on the motor bracket 14, a shaft sleeve 10 is fixedly installed on the output end of the mixing motor 9, an assembly pin 32 is threadedly connected to one side of the shaft sleeve 10, and a sub-branch is fixedly installed on the other side of the top of the reaction table 1. Column 5, two support arms 7 are installed in the middle of the auxiliary support 5, one of the support arms 7 is fixedly installed with a condensation recovery mechanism 3 for recovering the reaction product, the other support arm 7 is fixedly installed with a constant pressure dripping mechanism 6, the inner wall of the water bath chamber 33 is fixedly installed with an electric heating tube 34 and a temperature sensor 35, one side of the reaction table 1 is fixedly provided with an adding bucket 17 connected to the water bath chamber 33, the four corners at the bottom end of the reaction table 1 are fixedly installed with universal wheels 20, the bottom of the front of the reaction table 1 is fixedly connected with a drain pipe 19, the drain pipe 19 is fixedly installed with a drain valve, the middle of the front of the reaction table 1 is fixedly provided with a liquid level observation window 18, and the capacity of the glass reactor 2 is 20L.

[0021] The control mechanism includes a control box 15, inside which a variable frequency speed regulator 37, a single-chip controller 38 and a micro air pump 21 are fixedly installed, and the air outlet of the micro air pump 21 is fixedly connected to a constant pressure conduit 8. A box door 36 is hinged on the front of the control box 15, and a control panel 16 is fixedly installed on the outside of the box door 36. A touch display and a power switch are fixedly installed on the surface of the control panel 16. The micro air pump 21, the variable frequency speed regulator 37 and the touch display are all electrically connected to the single-chip controller 38, and the hybrid motor 9 is electrically connected to the variable frequency speed regulator 37.

[0022] See also Figure 1 and Figure 2 The tank cover assembly includes a glass kettle cover 13, a shaft connector 12 is fixedly installed in the middle of the top of the glass kettle cover 13, a driving shaft 11 is rotatably connected to the shaft connector 12, a mixing shaft 22 is fixedly installed at the bottom end of the driving shaft 11, a paddle 23 is fixedly installed at the bottom end of the mixing shaft 22, a distillation nozzle 30, a feeding port 26, a test port 28 and a dripping nozzle 31 are fixedly installed on the periphery of the top of the glass kettle cover 13, a sealing plug 27 is hinged on the feeding port 26, a glass rod 29 with a handle is snap-connected in the middle of the test port 28, an upper sealing disk 25 is fixedly installed at the bottom of the glass kettle cover 13, a lower sealing disk 24 is fixedly installed at the top of the glass reactor 2, and a glass cover disk 39 is fixedly installed on the outer side of the lower sealing disk 24; When in use, the sealing plug 27 is opened, and bisphenol A, sodium hydroxide, benzyltriethylammonium chloride and deionized water are added into the glass reactor 2 in sequence through the feeding port 26, and the mixing motor 9 is started. The mixing motor 9 drives the driving shaft 11 to rotate through the shaft sleeve 10, and then drives the mixing paddle 22 to rotate, and then stirs the added water phase system until the added materials are completely dissolved.

[0023] See also Figure 1 and Figure 3 The condensation recovery mechanism 3 includes a glass condenser tube 301, the bottom end of the glass condenser tube 301 is fixedly connected to a solvent recovery bottle 305, a spiral heat exchange tube 302 is fixedly arranged inside the glass condenser tube 301, one end of the spiral heat exchange tube 302 is fixedly connected to a cooling water outlet 303, and the other end of the spiral heat exchange tube 302 is fixedly connected to a cooling water inlet 304, one side of the solvent recovery bottle 305 is fixedly connected to a steam conduit 308, a valve 2 309 is fixedly installed in the middle of the steam conduit 308, the bottom end of the solvent recovery bottle 305 is fixedly connected to a four-way glass tube 306, a valve 1 307 is fixedly installed at the connection between the solvent recovery bottle 305 and the four-way glass tube 306, and the steam conduit 308 is sleeved on the distillation pipe mouth 30; When in use, after the polymerization reaction is completed, the tap water pipe of the laboratory is connected to the cooling water inlet 304 through the pipeline, and the cooling water outlet 303 is connected to the waste water pipe. After the polymerization reaction in the glass reactor 2 is completed, the valve two 309 is opened. Under the condition of water bath heating, the generated dichloromethane solvent will evaporate, enter the solvent recovery bottle 305 along the steam conduit 308, and finally rise into the glass condenser 301. During this period, tap water flows in through the cooling water inlet 304, flows in the spiral heat exchange tube 302, and flows out from the cooling water outlet 303. The steam will condense when it is cooled, and the condensed dichloromethane solvent will fall back into the solvent recovery bottle 305 under the action of gravity for temporary storage. It is only necessary to open the valve one 307 to release the dichloromethane solvent after complete recovery.

[0024] See also Figure 1 and Figure 4 The constant pressure dripping mechanism 6 includes a glass liquid storage tube 61, a threaded pipe mouth 64 is fixedly provided at the top of the glass liquid storage tube 61, a sealing pipe cap 65 is threadedly connected to the threaded pipe mouth 64, a dripping hose 66 is fixedly connected to the bottom end of the glass liquid storage tube 61, a valve 3 67 is fixedly installed on the top of the dripping hose 66, the bottom end of the dripping hose 66 is sleeved on the dripping pipe mouth 31, a pressurized air pipe 62 is fixedly connected to the top of one side of the glass liquid storage tube 61, an electromagnetic balancing air valve 63 is fixedly installed on the pressurized air pipe 62, a constant pressure conduit 8 is sleeved on the pressurized air pipe 62, and the electromagnetic balancing air valve 63 is electrically connected to the single-chip controller 38; When in use, unscrew and remove the sealing tube cap 65, add the configured organic reaction system into the glass liquid storage tube 61, re-tighten the sealing tube cap 65, and set the working pressure of the micro air pump 21. At this time, the micro air pump 21 will increase the air pressure into the glass liquid storage tube 61 through the constant pressure conduit 8 and the pressurized air pipe 62. The electromagnetic balance air valve 63 controls the constant air pressure in the glass liquid storage tube 61. Open valve three 67. Under constant air pressure conditions, the organic reaction system in the glass liquid storage tube 61 will be dripped into the glass reactor 2 through the drip hose 66 in a dripping manner, mixed with the aqueous phase reaction system in the glass reactor 2, and finally complete the polymerization reaction.

[0025] A polyarylate emulsion post-treatment process comprises the following steps: S1: preparing a water phase reaction system: sequentially adding bisphenol A, sodium hydroxide, benzyltriethylammonium chloride and deionized water into a glass reactor 2, starting a mixing motor 9, and mechanically stirring the added water phase reaction system for 15 min until the system is completely dissolved; S2: Prepare an organic reaction system: add terephthaloyl chloride, isophthaloyl chloride and dichloromethane in a 20L beaker in sequence, and stir thoroughly using a scattering device until they are completely dissolved; S3: Add the organic reaction system to the aqueous reaction system under constant pressure: Add the configured organic reaction system to the constant pressure drop adding mechanism, and add the uniform organic reaction system to the aqueous system drop by drop in an ice water bath at 5-15°C; control the drop adding time to 3h, and during the drop adding process, control the mixing motor 9 to stir at high speed, and control the speed to 300-400r / min. After the drop adding, fully stir and react for 2h; S4: Prepare the end-capping reagent system, stir and dissolve phenol, NaOH and deionized water in a 2L beaker, then pour into the 20L reactor after the third step and stir and react for 1 hour. During this period, use a glass rod to dip the reaction system into a pH test paper to adjust the pH value and observe whether the solution is neutral. If not, add a little formic acid until the solution is neutral and then terminate the reaction to obtain a special PC emulsion system; S5: Condensation recovery: first set the water bath temperature to 50-100°C, while heating and stirring, and observe the volatilization and collection of the dichloromethane solvent in the emulsion system and the condensation recovery mechanism 3; S6. The precipitated product in the glass reactor 2 is taken out and crushed first, then cleaned and filtered with high-temperature steam, and finally taken out and dried in a 100-150° C. forced air oven to constant weight.

[0026] When the embodiment of the present application is used: open the sealing plug 27, add bisphenol A, sodium hydroxide, benzyltriethylammonium chloride and deionized water into the glass reactor 2 in sequence through the feeding port 26, close the feeding port 26, start the mixing motor 9, the mixing motor 9 drives the driving shaft 11 to rotate through the shaft sleeve 10, and then drives the mixing paddle 22 to rotate, and then stirs the added aqueous phase system, and the stirring time is controlled to be 15 minutes until the added materials are completely dissolved, then add terephthaloyl chloride, isophthaloyl chloride and dichloromethane in sequence to a 20L beaker, use a scattering device to fully stir until completely dissolved, then unscrew and remove the sealing tube cap 65, add the configured organic reaction system into the glass liquid storage tube 61, and weigh Tighten the sealing pipe cap 65 again. At this time, the micro air pump 21 will increase the air pressure in the glass liquid storage tube 61 through the constant pressure conduit 8 and the pressurized air pipe 62. The electromagnetic balance air valve 63 controls the constant air pressure in the glass liquid storage tube 61. Then, add an appropriate amount of low-temperature water to the water bath chamber 33 through the adding bucket 17. The water temperature is 5-15°C and can cover the surface of the glass reactor 2. Open the valve 3 67. Under constant air pressure conditions, the organic reaction system in the glass liquid storage tube 61 will be dripped into the glass reactor 2 through the dripping hose 66, and mixed with the water phase reaction system in the glass reactor 2. The reaction is mixed and reacted while dripping. After the dripping is completed, continue to stir and mix for 2 hours to finally complete the polymerization reaction. After the polymerization reaction is completed, the electric heating tube 34 is controlled to continuously heat the water in the water bath chamber 33. When the water temperature reaches 50°C, the valve 2 309 is opened and the water is continuously heated to 100°C. The dichloromethane solvent generated during the process will volatilize and enter the solvent recovery bottle 305 along the steam conduit 308, and finally rise into the glass condenser tube 301. The steam will condense when it is cooled. The condensed dichloromethane solvent will fall back into the solvent recovery bottle 305 for temporary storage under the action of gravity. The volatilization and collection of the dichloromethane solvent in the emulsion system and the condensation recovery mechanism 3 are continuously observed during the entire recovery process until The precipitated product in the glass reactor 2 is dried and solidified, and after being taken out, it is first broken, then cleaned and filtered with high-temperature steam, and finally taken out and dried in a 100-150°C forced air oven to constant weight. The polyarylate emulsion is directly distilled while stirring, and most of the dichloromethane solvent is evaporated and recovered. Finally, the precipitated "cake-like" polyarylate product is broken and cleaned with continuous high-temperature steam or boiling water for multiple times, thereby eliminating the use of a large amount of methanol organic solvent in the methanol demulsification process and the subsequent separation of methanol and dichloromethane mixed solvents, and the methanol solvent volatilized into the environment is also greatly reduced, thereby protecting the environment and the experimental operators.

[0027] Although the present invention has been described in detail with reference to the aforementioned embodiments, it is still possible for those skilled in the art to modify the technical solutions described in the aforementioned embodiments, or to make equivalent substitutions for some of the technical features therein. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the protection scope of the present invention.

Claims

1. A polyarylate emulsion post-processing device, comprising a reaction table (1), characterized in that: A water bath chamber (33) is provided in the middle of the reaction table (1), a glass reactor (2) is fixedly installed in the middle of the water bath chamber (33), and a tank cover assembly matching the glass reactor (2) is provided on the glass reactor (2). A main support (4) is fixedly installed on one side of the top of the reaction table (1), and a control mechanism for controlling the polymerization reaction process is fixedly installed on the top of the main support (4). A motor support (14) is installed in the middle of the main support (4), and a mixing motor (9) is fixedly installed on the motor support (14). A shaft sleeve (10) is fixedly installed at the output end of the mixing motor (9), and an assembly pin (32) is threadedly connected to one side of the shaft sleeve (10). A secondary support (5) is fixedly installed on the other side of the top of the reaction table (1), and two support arms (7) are installed in the middle of the secondary support (5), one of which is fixedly installed with a condensation recovery mechanism (3) for recovering reaction products, and the other of which is fixedly installed with a constant pressure dripping mechanism (6).

2. A polyarylate emulsion post-processing equipment according to claim 1, characterized in that: The control mechanism comprises a control box (15), wherein a variable frequency speed regulator (37), a single chip controller (38) and a micro air pump (21) are fixedly installed inside the control box (15), an air outlet of the micro air pump (21) is fixedly connected to a constant pressure conduit (8), a box door (36) is hingedly connected to the front of the control box (15), a control panel (16) is fixedly installed on the outside of the box door (36), a touch display and a power switch are fixedly installed on the surface of the control panel (16), the micro air pump (21), the variable frequency speed regulator (37) and the touch display are all electrically connected to the single chip controller (38), and the hybrid motor (9) is electrically connected to the variable frequency speed regulator (37).

3. A polyarylate emulsion post-processing equipment according to claim 2, characterized in that: The tank cover assembly comprises a glass kettle cover (13), wherein a shaft connection member (12) is fixedly mounted in the middle of the top of the glass kettle cover (13), a driving shaft (11) is rotatably connected to the shaft connection member (12), a mixing shaft (22) is fixedly mounted at the bottom end of the driving shaft (11), a paddle (23) is fixedly mounted at the bottom end of the mixing shaft (22), a distillation pipe opening (30), a material adding opening (26), a test opening (28) and a dripping pipe opening (31) are fixedly mounted on the periphery of the top of the glass kettle cover (13), a sealing plug (27) is hingedly mounted on the material adding opening (26), a glass rod (29) with a handle is snap-connected to the middle of the test opening (28), an upper sealing disk (25) is fixedly mounted on the bottom of the glass kettle cover (13), a lower sealing disk (24) is fixedly mounted on the top of the glass reactor (2), and a glass cover disk (39) is fixedly mounted on the outer side of the lower sealing disk (24).

4. A polyarylate emulsion post-processing equipment according to claim 3, characterized in that: The condensation recovery mechanism (3) comprises a glass condenser (301), the bottom end of the glass condenser (301) is fixedly connected to a solvent recovery bottle (305), a spiral heat exchange tube (302) is fixedly arranged inside the glass condenser (301), one end of the spiral heat exchange tube (302) is fixedly connected to a cooling water outlet (303), and the other end of the spiral heat exchange tube (302) is fixedly connected to a cooling water inlet (304), one side of the solvent recovery bottle (305) is fixedly connected to a steam conduit (308), a valve 2 (309) is fixedly installed in the middle of the steam conduit (308), the bottom end of the solvent recovery bottle (305) is fixedly connected to a four-way glass tube (306), a valve 1 (307) is fixedly installed at the connection between the solvent recovery bottle (305) and the four-way glass tube (306), and the steam conduit (308) is sleeved on the distillation pipe mouth (30).

5. A polyarylate emulsion post-processing device according to claim 3, characterized in that: The constant pressure dripping mechanism (6) comprises a glass liquid storage tube (61), the top end of the glass liquid storage tube (61) is fixedly provided with a threaded pipe mouth (64), the threaded pipe mouth (64) is threadedly connected with a sealing pipe cap (65), the bottom end of the glass liquid storage tube (61) is fixedly connected with a dripping hose (66), the top end of the dripping hose (66) is fixedly installed with a valve three (67), the bottom end of the dripping hose (66) is sleeved on the dripping pipe mouth (31), the top of one side of the glass liquid storage tube (61) is fixedly connected with a pressurized air pipe (62), the pressurized air pipe (62) is fixedly installed with an electromagnetic balancing air valve (63), the constant pressure conduit (8) is sleeved on the pressurized air pipe (62), and the electromagnetic balancing air valve (63) is electrically connected to the single chip controller (38).

6. A polyarylate emulsion post-processing device according to claim 2, characterized in that: An electric heating tube (34) and a temperature sensor (35) are fixedly mounted on the inner wall of the water bath chamber (33), and an addition hopper (17) communicating with the water bath chamber (33) is fixedly disposed on one side of the reaction table (1).

7. The polyarylate emulsion post-processing equipment according to claim 1, characterized in that: Universal wheels (20) are fixedly mounted on the four corners at the bottom of the reaction table (1); a drainage pipe (19) is fixedly connected to the bottom of the front of the reaction table (1); a drainage valve is fixedly mounted on the drainage pipe (19); a liquid level observation window (18) is fixedly arranged in the middle of the front of the reaction table (1); and the capacity of the glass reactor (2) is 20L.

8. A polyarylate emulsion post-treatment process according to any one of claims 1 to 7, characterized in that: The following steps are involved: S1: preparing a water phase reaction system: sequentially adding bisphenol A, sodium hydroxide, benzyltriethylammonium chloride and deionized water into a glass reactor (2), starting a mixing motor (9), and mechanically stirring the added water phase reaction system for 15 minutes until the solution is completely dissolved; S2: Prepare an organic reaction system: add terephthaloyl chloride, isophthaloyl chloride and dichloromethane in a 20L beaker in sequence, and stir thoroughly using a scattering device until they are completely dissolved; S3: Constant-pressure dropwise addition of the organic reaction system to the aqueous reaction system: Add the prepared organic reaction system to the constant-pressure dropwise addition mechanism, and add the homogeneous organic reaction system dropwise to the aqueous system under the condition of an ice-water bath at 5-15°C; S4: Prepare the end-capping reagent system. Stir and dissolve phenol, NaOH and deionized water in a 2L beaker. Pour them into the 20L reactor after the third step and stir them for 1 hour. During this time, use a glass rod to dip the reaction system into a pH test paper to adjust the pH value. Observe whether the solution is neutral. If not, add a little formic acid until the solution is neutral and then terminate the reaction. The special PC emulsion system can be obtained. S5: Condensation recovery: first set the water bath temperature to 50-100°C, while heating and stirring, observe the volatilization and collection of the dichloromethane solvent in the emulsion system and the condensation recovery mechanism (3); S6. The precipitated product in the glass reactor (2) is taken out and crushed, then cleaned and filtered using high-temperature steam, and finally taken out and dried in a 100-150° C. forced air oven to constant weight.

9. A polyarylate emulsion post-treatment process according to claim 8, characterized in that: In the step S3, the dripping time is controlled to be 3 hours. During the dripping process, the mixing motor (9) is controlled to stir at a high speed of 300-400 r / min. After the dripping is completed, the mixture is stirred and reacted for 2 hours.

Images