A dispersion precipitation apparatus and method for a polysulfone-based resin

Abstract

The application belongs to the technical field of polysulfone resins, and particularly relates to a dispersion and precipitation device and method of a polysulfone resin. The dispersion and precipitation device provided by the application comprises a storage kettle, a spray pipe communicated with a raw material outlet of the storage kettle, a bottom surface of the spray pipe being a porous structure, a dispersion pipeline communicated with the raw material outlet of the storage kettle through the spray pipe, the dispersion pipeline comprising a screen tube and a non-porous tube nested outside the screen tube, a vibrating device 6 arranged on an outer wall of the dispersion pipeline, a spraying device 7 arranged above an inner wall of the dispersion pipeline, the dispersion pipeline comprising an inlet and an outlet, the inlet being higher than the outlet, and an inclination angle formed between the inlet and a horizontal plane being 5-10 degrees, a collection kettle communicated with the dispersion pipeline, and the collection kettle being communicated with the dispersion pipeline through a circulating pump. The product obtained by using the dispersion and precipitation device is uniform in grain drop, the dispersion and precipitation solvent can be recycled, and the solvent is saved.

Description

TECHNICAL FIELD

[0001] The application belongs to the technical field of polysulfone resins, and particularly relates to a dispersion precipitation device and method for polysulfone resins. BACKGROUND

[0002] The polysulfone resin is polymerized in a solvent system, and thus, after the polymerization is completed, the reactor is a solid-liquid mixture containing the polymer, salt, solvent and residual monomer. Therefore, the solid-liquid mixture after polymerization needs to be separated through a series of operations to obtain pure polysulfone resin. The traditional processing steps are: salt removal by filtration, dispersion precipitation, crushing, washing and drying, and finally, relatively pure polysulfone resin is obtained. The dispersion precipitation process is that the mixture after salt removal by filtration is dropped into a porous sieve under normal pressure in a free-falling form into a tank with stirring, and a large amount of dispersion precipitation solvent is added into the tank, and the mass ratio of the polysulfone resin to the dispersion precipitation solvent is generally 1:50, and even more dispersion precipitation solvent is needed, so as to solidify the polymer and prevent adhesion. However, the materials dropped into the tank are various irregular mixtures, some of which are flat, some are long strip-shaped, and some are trailing spherical, especially in the state of trailing and drawing, which can be wound together to cause the blocking of the crushing device. Moreover, after the crushing, the obtained powder has a large difference in particle size, and some become superfine powder, which loses the use value. The above-mentioned processing method has many defects, such as: 1. A large amount of dispersion precipitation agent is needed to ensure that the mixture containing the polysulfone resin is not adhered together. 2. The falling particles have different states, especially the trailing and long strip-shaped particles, which are easy to be wound together to cause the blocking of the crushing device. 3. The crushing method can bring superfine powder with low added value, and the superfine powder can be suspended in the air to harm human health, and can also produce continuous noise to harm the occupational health. SUMMARY

[0003] Therefore, the application provides a dispersion precipitation device and method for polysulfone resins. The product falling particles prepared by the dispersion precipitation device are uniform, and the dispersion precipitation solvent can be recycled to save the dispersion precipitation solvent.

[0004] In order to achieve the above-mentioned purpose, the application provides a dispersion precipitation device for polysulfone resins, which comprises a storage reactor 1, and the storage reactor 1 is provided with a raw material inlet, a nitrogen inlet and a raw material outlet.

[0005] A spray pipe 2 in communication with the raw material outlet of the storage reactor 1; the bottom surface of the spray pipe 2 is a porous structure.

[0006] A dispersion pipeline 3 is communicated with the raw material outlet of the storage tank 1 through a spray pipe 2; the dispersion pipeline 3 comprises a screen pipe and a non-porous pipe nested outside the screen pipe; the outer wall of the dispersion pipeline 3 is provided with a vibration device 6; the inner wall of the dispersion pipeline 3 is provided with a spraying device 7 above; the dispersion pipeline 3 comprises an inlet and an outlet; the position of the inlet is higher than that of the outlet, and the inclination angle formed with the horizontal plane is 5-10°.

[0007] A collection tank 4 communicated with the dispersion pipeline 3;

[0008] The collection tank 4 is communicated with the dispersion pipeline 3 through a circulating pump 5.

[0009] Preferably, the dispersion pipeline 3 is a spiral dispersion pipeline.

[0010] Preferably, the screen aperture in the screen pipe is 2-6 mm.

[0011] Preferably, the material of the dispersion pipeline 3 is stainless steel.

[0012] Preferably, the vibration device 6 comprises an ultrasonic device and / or a mechanical vibration device.

[0013] Preferably, the collection tank 4 is further provided with a stirrer.

[0014] The application further provides a method for dispersing and precipitating polysulfone resin by using the dispersion and precipitation device, which comprises the following steps:

[0015] The dispersion and precipitation solvent is placed in the collection tank 4, and the dispersion and precipitation solvent in the collection tank 4 is sprayed out from the spraying device 7 above the dispersion pipeline 3 to the lower layer of the screen pipe by the circulating pump 5;

[0016] The crude polysulfone resin after filtering and removing salt is added into the storage tank 1, nitrogen is introduced into the storage tank 1 through a nitrogen inlet to pressurize, the crude polysulfone resin is sprayed into the screen pipe of the dispersion pipeline 3 through the porous spray pipe 2, the bottom of the crude polysulfone resin is contacted with the dispersion and precipitation solvent, solidification is carried out, and the crude polysulfone resin is vibrated by the vibration device 6, passes through the dispersion pipeline 3 and enters the collection tank 4.

[0017] Preferably, the nitrogen is pressurized to a pressure of 0.1-0.3 MPa.

[0018] Preferably, the temperature of the dispersion and precipitation solvent in the collection tank 4 is 5-10℃.

[0019] Preferably, the solid content of the crude polysulfone resin is 15-35%.

[0020] This invention provides a dispersion and precipitation device for polysulfone resins, comprising a storage vessel 1, which has a raw material inlet, a nitrogen inlet, and a raw material outlet; a spray pipe 2 connected to the raw material outlet of the storage vessel 1; the bottom surface of the spray pipe 2 has a porous structure; a dispersion pipe 3 connected to the raw material outlet of the storage vessel 1 through the spray pipe 2; the dispersion pipe 3 includes a screen pipe and a non-porous pipe nested outside the screen pipe; a vibration device 6 is provided on the outer wall of the dispersion pipe 3; a spray device 7 is provided above the inner wall of the dispersion pipe 3; the dispersion pipe 3 includes an inlet and an outlet; the inlet is positioned higher than the outlet, and the inclination angle formed with the horizontal plane is 5-10°; and a collection vessel 4 connected to the dispersion pipe 3; the collection vessel 4 is connected to the dispersion pipe 3 through a circulation pump 5. In this invention, a certain amount of dispersion precipitating solvent is added to the collection vessel, and the circulation pump is turned on to spray, ensuring that the flow rate of the sprayed dispersion precipitating solvent is just enough to submerge the screen inside the dispersion pipe. After turning on the dispersion pipe vibration device 6, all the filtered and desalted crude polysulfone resin flows into the storage vessel, and then the crude polysulfone resin enters the porous spray pipe and falls into the dispersion pipe below under pressure. Under the action of spraying, a small amount of crude polysulfone resin sprayed onto the vessel wall will automatically fall into the dispersion and precipitation solvent below the pipe. With the tilt angle and vibration, it moves forward on the screen of the dispersion pipe. At this time, the polymer is in a semi-cured state on the surface and soft inside because it has just been sprayed. Under these conditions, the vibration will cause it to deform and tend to be spherical. Moreover, the vibration will accelerate the overflow of residual solvent in the polymer, which not only accelerates the curing speed and prevents them from sticking together, but also fully washes out the residual solvent. Finally, it falls into the collection vessel. There is a pipe in the collection vessel connected to a circulation pump, and the other end is connected to the dispersion pipe. When the liquid level reaches a certain set value, the circulation pump is turned on, spraying the dispersion and precipitation solvent in the vessel into the dispersion pipe. In addition, the polymer gel in the storage vessel 1 passes through the spray pipe 2 under a certain pressure. The bottom surface of the spray pipe 2 has a porous structure. By controlling the size of the porous pores on the bottom surface, the size of the sprayed polymer particles can be controlled. When the polymer comes into contact with the dispersion medium in the dispersion pipe 3, the polymer precipitates and forms small spherical particles. Attached Figure Description

[0021] Figure 1 The dispersion and precipitation apparatus for polysulfone resin provided by the present invention comprises: 1-storage vessel, 2-spray pipe, 3-dispersion pipe, 4-collection vessel, 5-circulation pump, 6-vibration device, and 7-spraying device. Detailed Implementation

[0022] The present invention provides a dispersion and precipitation device for polysulfone resin, including a storage tank 1, wherein the storage tank 1 is provided with a raw material inlet, a nitrogen inlet and a raw material outlet;

[0023] A jet pipe 2 is connected to the raw material outlet of the storage vessel 1; the bottom surface of the jet pipe 2 has a porous structure.

[0024] A dispersion pipe 3 is connected to the raw material outlet of the storage vessel 1 via a spray pipe 2; the dispersion pipe 3 includes a screen pipe and a non-porous pipe nested outside the screen pipe; a vibration device 6 is provided on the outer wall of the dispersion pipe 3; a spray device 7 is provided above the inner wall of the dispersion pipe 3; the dispersion pipe 3 includes an inlet and an outlet; the inlet is located higher than the outlet, and the inclination angle formed with the horizontal plane is 5 to 10°.

[0025] A collection vessel 4 connected to the dispersion pipe 3;

[0026] The collection vessel 4 is connected to the dispersion pipeline 3 via the circulation pump 5.

[0027] Unless otherwise specified, all raw materials used in this invention are preferably commercially available products.

[0028] like Figure 1 As shown, the present invention provides a dispersion and precipitation apparatus for polysulfone resins, the apparatus comprising a storage vessel 1. In this invention, the storage vessel 1 is provided with a raw material inlet, a nitrogen inlet, and a raw material outlet. Preferably, the storage vessel is also provided with a temperature control device.

[0029] In this invention, the dispersion and sedimentation device includes a dispersion pipe 3 connected to the raw material outlet via a jet pipe 2. In this invention, the bottom surface of the jet pipe 2 has a porous structure.

[0030] In the present application, the dispersion pipeline 3 is preferably a spiral dispersion pipeline; the dispersion pipeline 3 comprises a screen tube and a non-porous tube nested outside the screen tube; the screen tube has a screen aperture of 2-6 mm, more preferably 3-4 mm. In the present application, the inner diameter of the screen tube is preferably 10-50 cm, more preferably 23-24 cm; the outer diameter is preferably 10.5-50.5 cm, more preferably 23.6-24.2 cm. In the present application, the inner diameter of the non-porous tube is preferably 20-70 cm, more preferably 40-60 cm; the outer diameter is preferably 20.5-70.5 cm, more preferably 40.5-60.5 cm. In the present application, the length of the dispersion pipeline is preferably 1-5 m, more preferably 2-3 m. In the present application, the material of the dispersion pipeline 3 is preferably stainless steel. In the present application, the inner wall of the dispersion pipeline 3 is provided with a spraying device 7 above. In the present application, the dispersion pipeline 3 comprises an inlet and an outlet; the position of the inlet is higher than that of the outlet, and the inclination angle with the ground level is preferably 5-10°. In the present application, the outer wall of the dispersion pipeline 3 is provided with a vibration device 6. In the present application, the vibration device 6 preferably comprises an ultrasonic device and / or a mechanical vibration device 6. In the present application, the dispersion pipeline 3 is preferably further provided with a temperature control device.

[0031] In the present application, the dispersion precipitation device comprises a collection kettle 4 in communication with the dispersion pipeline 3. In the present application, the collection kettle 4 is preferably further provided with a stirrer. In the present application, the collection kettle 4 is preferably further provided with a temperature control device. In the present application, the collection kettle 4 is in communication with the dispersion pipeline 3 through a circulating pump 5.

[0032] The present application also provides a method for dispersing and precipitating polysulfone-based resin using the dispersion precipitation device, comprising the following steps:

[0033] The dispersion precipitation solvent is placed in the collection kettle 4, and the dispersion precipitation solvent in the collection kettle 4 is sprayed out from the spraying device 7 above the dispersion pipeline 3 to the lower layer of the screen tube to submerge the screen tube;

[0034] The crude polysulfone-based resin after filtration and salt removal is added to the storage kettle 1, nitrogen gas is introduced into the storage kettle 1 through the nitrogen gas inlet to pressurize, and the crude polysulfone-based resin is sprayed into the screen tube of the dispersion pipeline 3 through the porous spray pipeline 2, the bottom of the crude polysulfone-based resin is in contact with the dispersion precipitation solvent, solidification is carried out, and the crude polysulfone-based resin passes through the dispersion pipeline 3 under the vibration of the vibration device 6 and enters the collection kettle 4.

[0035] In the present application, the solid content of the crude polysulfone-based resin is preferably 15-35%, more preferably 20-30%. In the present application, the addition amount of the dispersion precipitation solvent is preferably 2 / 3 of the volume of the collection kettle 4.

[0036] In the present application, the temperature of the dispersion precipitating solvent in the collecting kettle 4 is preferably 5-10°C, more preferably 7-8°C. In the present application, the nitrogen pressure is preferably 0.1-0.3 MPa, more preferably 0.2 MPa.

[0037] The technical solutions provided by the present application are described in detail below in conjunction with examples, but they should not be understood as limiting the scope of protection of the present application.

[0038] Example 1

[0039] Pure water is added to the collecting kettle, about 2 / 3 of the kettle capacity, the stirrer is turned on, and the cooling function of the temperature control device is started to keep the water temperature at 5°C.

[0040] The circulating pump is turned on to make the dispersion precipitating solvent in the collecting kettle sprayed from the spray nozzle above the dispersion pipeline, the flow rate is ensured to be able to submerge the screen, and the inner wall of the dispersion pipeline is kept wet.

[0041] After the PPSU crude product with a solid content of 25% after filtration and desalination is added to the storage kettle 1, the raw material inlet is closed, the raw material outlet is opened, and nitrogen is introduced into the storage kettle 1 through the nitrogen inlet to pressurize to 0.2 MPa, the pressure is kept, the crude polysulfone resin is sprayed into the dispersion pipeline through the porous spray pipeline, at this time, the bottom of the crude polysulfone resin is in contact with the dispersion precipitating solvent for solidification, at the same time, under the vibration of the vibration device 6, the crude polysulfone resin is continuously vibrated in the screen pipeline and slowly moves forward with the help of the inclination, and finally enters the collecting kettle.

[0042] Example 2

[0043] Pure water is added to the collecting kettle, about 2 / 3 of the kettle capacity, the stirrer is turned on, and the cooling function of the temperature control device is started to keep the water temperature at 5°C.

[0044] The circulating pump is turned on to make the dispersion precipitating solvent in the collecting kettle sprayed from the spray nozzle above the dispersion pipeline, the flow rate is ensured to be able to submerge the screen, and the inner wall of the dispersion pipeline is kept wet.

[0045] After the PPSU crude product with a solid content of 25% after filtration and desalination is added to the storage kettle 1, the raw material inlet is closed, the raw material outlet is opened, and nitrogen is introduced into the storage kettle 1 through the nitrogen inlet to pressurize to 0.2 MPa, the pressure is kept, the crude polysulfone resin is sprayed into the dispersion pipeline through the porous spray pipeline, at this time, the bottom of the crude polysulfone resin is in contact with the dispersion precipitating solvent for solidification, at the same time, under the vibration of the vibration device 6, the crude polysulfone resin is continuously vibrated in the screen pipeline and slowly moves forward with the help of the inclination, and finally enters the collecting kettle.

[0046] Example 3

[0047] Add pure water into the collecting kettle, about 2 / 3 of the kettle capacity, open the stirrer, start the cooling function of the temperature control device, and keep the water temperature at 5℃.

[0048] Open the circulating pump to make the dispersion precipitated solvent in the collecting kettle sprayed from the spray nozzle above the dispersion pipeline, and the flow rate is ensured to be submerged in the screen, while keeping the inner wall of the dispersion pipeline wet.

[0049] After adding the PPSU crude product with a solid content of 25% after filtering and removing salt into the storage kettle 1, close the raw material inlet, open the raw material outlet, and introduce nitrogen into the storage kettle 1 through the nitrogen inlet to pressurize to 0.1 MPa, keep the pressure, and make the polysulfone resin crude product sprayed into the dispersion pipeline through the porous spray pipeline, at this time, the bottom of the polysulfone resin crude product is in contact with the dispersion precipitated solvent for solidification, and under the vibration of the vibration device 6, the polysulfone resin crude product is continuously vibrated in the screen pipeline and slowly moves forward by means of inclination, and finally enters the collecting kettle.

[0050] Comparative Example 1

[0051] Add pure water into the dispersion kettle to 2 / 3 of the kettle capacity, open the cooling function, keep the water temperature in the kettle at 5℃, and open the stirring in the kettle;

[0052] After filtering and removing salt, the PPSU crude product with a solid content of 25% flows into the storage kettle, flows into the discharge screen body through the pipeline at normal pressure, and enters the dispersion kettle in the form of free fall; under the action of stirring, large particles of polymer slowly fall to the bottom of the dispersion kettle, while small particles of polymer are suspended in the dispersion precipitated solvent, which have different shapes and sizes, and tailing PPSU polymer appears in the later stage, which will be wound on the stirring paddle.

[0053] The PPSU small particles prepared in Examples 1-3 and Comparative Example 1 are washed for 3 times, the residues are detected, the particle size is measured, and the samples are injection molded, and the optical and mechanical properties of the samples are detected, and the detection results are shown in Tables 1-2.

[0054] Table 1 Optical property detection results of PPSU small particles prepared in Examples 1-3 and Comparative Example 1

[0055]

[0056] Table 2 Mechanical property detection results of PPSU small particles prepared in Examples 1-3 and Comparative Example 1

[0057]

[0058] It should be noted that those skilled in the art can make some improvements and refinements without departing from the principles of the present application, and these improvements and refinements should be considered as the protection scope of the present application.

Claims

1. An apparatus for dispersion precipitation of a polysulfone-based resin, characterized by comprising: It comprises a storage tank (1) provided with a raw material inlet, a nitrogen inlet and a raw material outlet; A spray pipe (2) in communication with the raw material outlet of the storage tank (1); the bottom surface of the spray pipe (2) is a porous structure; A dispersion pipeline (3) in communication with the raw material outlet of the storage tank (1) through the spray pipe (2); the dispersion pipeline (3) comprises a screen tube and a non-porous tube nested outside the screen tube; the outer wall of the dispersion pipeline (3) is provided with a vibration device (6); A spraying device (7) is arranged above the inner wall of the dispersion pipeline (3); the dispersion pipeline (3) comprises an inlet and an outlet; the position of the inlet is higher than that of the outlet, and the inclination angle formed with the horizontal plane is 5-10°; A collection tank (4) in communication with the dispersion pipeline (3); The collection tank (4) is in communication with the dispersion pipeline (3) through a circulating pump (5); The dispersion pipeline (3) is a spiral dispersion pipeline; The vibration device (6) comprises an ultrasonic device and / or a mechanical vibration device.

2. The dispersion precipitation apparatus according to claim 1, wherein The screen aperture of the screen tube is 2-6 mm.

3. The dispersion precipitation apparatus of claim 1, wherein The material of the dispersion pipeline (3) is stainless steel.

4. The dispersion precipitation apparatus of claim 1, wherein The collection tank (4) is further provided with a stirrer.

5. A method for dispersing and precipitating a polysulfone-based resin using the dispersing and precipitating apparatus according to any one of claims 1 to 4, characterized by, It comprises the following steps: The dispersion precipitation solvent is placed in the collection tank (4), and the dispersion precipitation solvent in the collection tank (4) is sprayed out from the spraying device (7) above the dispersion pipeline (3) to the lower layer of the screen tube by the circulating pump (5); The polysulfone resin crude product after filtering and desalination is added into the storage tank (1), nitrogen is introduced into the storage tank (1) through the nitrogen inlet for pressurization, the polysulfone resin crude product is sprayed into the screen tube of the dispersion pipeline (3) through the porous spray pipe (2), the bottom of the polysulfone resin crude product contacts with the dispersion precipitation solvent, solidification is carried out, and the polysulfone resin crude product passes through the dispersion pipeline (3) under the vibration of the vibration device (6) and enters the collection tank (4).

6. The method of claim 5, wherein, The nitrogen is pressurized to a pressure of 0.1-0.3 MPa.

7. The method of claim 5, wherein, The temperature of the dispersion precipitation solvent in the collection tank (4) is 5-10℃.

8. The method of claim 5, wherein, The solid content of the polysulfone resin crude product is 15-35%. The temperature of the dispersion precipitation solvent in the collection tank (4) is 5-10℃. The solid content of the polysulfone resin crude product is 15-35%.

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