A method and apparatus system for coagulating a special polymer

Abstract

The application provides a method and device system for special polymer precipitation. The device system comprises a solution storage tank and a precipitation device connected in sequence; a funnel is arranged in the precipitation device; the funnel is connected with a crushing device through a bend pipe; the outlet of the crushing device is divided into two branches, one of which is connected with the precipitation device, and the other is connected with a first solid-liquid separation device; a light component conveying pipe and a heavy component conveying pipe are arranged on the side wall of the precipitation device. The special polymer powder and flat round piece obtained by using the device system have more pores on the surface than conventional special polymer, so that the residual substances remaining in the round piece are more easily washed, and the finally obtained special polymer has high cleanliness. The special polymer powder can be used for blending modification or coating; and the special polymer round piece can be used for granulation, molding or film making.

Description

TECHNICAL FIELD

[0001] The present application belongs to the field of high polymer material separation, and relates to a method and device system for sedimentation of special polymers, in particular to a method and device system for simultaneously preparing special polymer powder and round sheet. BACKGROUND

[0002] In the process of generation, processing and recycling of high polymers, special polymer solution is often produced. There are many methods for separating polymers from special polymer solution, such as the method for slowly adding water to the polysulfone solution to precipitate polysulfone disclosed in CN 102888003A; the method for crushing the polysulfone solution after cooling into a film disclosed in CN 105330840A; of course, there are also methods such as polyformaldehyde and polyolefin elastomer for removing polymer solvent to obtain polymers.

[0003] Special engineering plastics such as polysulfone, polyether sulfone, polyphenyl sulfone, polyimide, polyester imide, polyether imide, polyamide imide, polyether ether ketone and polyphenylene sulfide can only be dissolved in strong polar solvents such as DMAC and NMP. Such solvents are often difficult to remove by devolatilization, and are prone to decomposition during heating, so they can only be precipitated after mixing with inert solvents, and then crushed by wet method to obtain polymers. Since the above-mentioned special engineering plastics usually have very strong toughness, it is difficult to crush them to the predetermined particle size at one time using general crushing equipment, and usually a circulating crushing method is used. However, this crushing method is the core technology of the generating enterprise, and the technical barrier is very high, so there are few reference and practical methods in the published literature patents.

[0004] For different uses of special polymers, the required crushing particle size requirements are also different. For example, for the production of coatings and modified materials, the product powder is required to be fine and light, so as to facilitate material dissolution and mixing; and for granulation, the product particles are required to be slightly larger, and the bulk density is required to be larger, which is beneficial to the granulation of the material. The general wet crushing process usually uses a continuous feeding and circulating crushing mode, which generally makes the particle size distribution of the crushed product very wide, and the product has both several millimeter-sized sheets and several micron-sized particles. Such material will cause many problems in cooperation application, such as uneven liquid film during coating preparation, and unsmooth feeding during granulation. Therefore, regardless of the application, the powder needs to have relatively uniform particle size. SUMMARY

[0005] The present application aims to provide a method and device system for sedimentation of special polymers. The special polymer powder and flat round sheet provided by the present application have more pores on the surface than conventional special polymers, so that the residual substances remaining in the interior of the sheet are more easily washed, and the finally obtained special polymer has high cleanliness. The special polymer powder can be used in blending modification or coating; and the special polymer sheet can be used in granulation, molding or film making.

[0006] To achieve the object of the present application, the present application adopts the following technical solutions:

[0007] In a first aspect, the present application provides a device system for sedimentation of special polymers, which comprises a solution storage tank and a sedimentation device connected in sequence; a hopper is arranged in the interior of the sedimentation device;

[0008] The hopper is connected with a crushing device through an elbow; the outlet of the crushing device is divided into two branches, one of which is connected with the sedimentation device, and the other is connected with a first solid-liquid separation device;

[0009] A light component conveying pipeline and a heavy component conveying pipeline are arranged on the side wall of the sedimentation device;

[0010] The light component conveying pipeline is connected with the sedimentation device through a light component slurry circulating pump; and the heavy component conveying pipeline is connected with a heavy component slurry circulating pump;

[0011] The outlet of the heavy component slurry circulating pump is divided into two branches, one of which is connected with the sedimentation device, and the other is connected with a second solid-liquid separation device.

[0012] The device system provided by the present application realizes continuous crushing of special polymer solution through continuous feeding, and simultaneously obtains light powder and heavy flat round sheet, so as to adapt to different application fields.

[0013] The hopper arranged in the interior of the sedimentation device can make the solid obtained by sedimentation in the sedimentation device enter the crushing device through the hopper and the elbow; the method of feeding through the hopper mouth can avoid that the special polymer solution enters the outlet of the sedimentation device too far and cannot accurately enter the outlet and the crushing device, thereby solving the problem that the special polymer solution easily blocks the outlet of the sedimentation device due to easy sedimentation.

[0014] As a preferred technical solution of the present application, the liquid outlet of the second solid-liquid separation device is connected with the sedimentation device.

[0015] Preferably, the light component conveying pipeline is arranged above the hopper mouth of the hopper.

[0016] Preferably, the heavy component delivery pipeline is arranged below the upper edge of the hopper mouth.

[0017] The present application can make the material in the settling device not remain, can realize smooth feeding and discharging, and can quickly separate heavy flat round pieces by arranging the circulating pump above and below the upper edge of the hopper mouth.

[0018] Preferably, the crushing device comprises any one of a crushing pump, a grinder, a colloid mill or a Waring shear.

[0019] Preferably, the light component slurry circulating pump comprises any one of a crushing pump, a mud pump, a centrifugal pump, a screw pump or a rotor pump.

[0020] Preferably, the heavy component slurry circulating pump comprises any one of a crushing pump, a mud pump, a centrifugal pump, a screw pump or a rotor pump.

[0021] Preferably, the first solid-liquid separation device comprises any one of a continuous centrifuge, a continuous leaf filter or an intermittent switching type closed plate filter.

[0022] Preferably, the second solid-liquid separation device comprises any one of a continuous centrifuge, a continuous leaf filter or an intermittent switching type closed plate filter.

[0023] Preferably, the ratio of the diameter of the hopper to the diameter of the settling device is 1:(3-50), for example, can be 1:3, 1:5, 1:10, 1:15, 1:20, 1:25, 1:30, 1:40 or 1:50, but is not limited to the listed values, and other values not listed in the value range are also applicable; preferably, the ratio is 1:(5-20).

[0024] Preferably, the ratio of the height from the upper edge of the hopper mouth to the bottom of the settling device to the height from the liquid surface of the settling agent in the settling device to the bottom of the settling device is (5-9.5):10, for example, can be 5:10, 6:10, 7:10, 8:10, 9:10 or 9.5:10, but is not limited to the listed values, and other values not listed in the value range are also applicable; preferably, the ratio is (6-9):10.

[0025] Preferably, the ratio of the height from the upper edge of the hopper mouth to the bottom of the settling device to the radius of the circle where the elbow pipe is located is (1-50):1, for example, can be 1:1, 2:1, 5:1, 10:1, 20:1, 30:1, 40:1 or 50:1, but is not limited to the listed values, and other values not listed in the value range are also applicable; preferably, the ratio is (2-10):1.

[0026] Preferably, the solution storage tank is internally provided with a reaction reagent.

[0027] Preferably, the reaction reagent comprises a mixed solution of a special polymer and a polar solution.

[0028] Preferably, the special polymer solution comprises any one or a combination of at least two of a soluble imide polymer, a soluble sulfone polymer, a soluble ketone polymer, a soluble aromatic sulfide polymer, an organic acid cellulose, a polyurethane, or a soluble polyamide, typically but not limitedly a combination of the soluble imide polymer, the soluble sulfone polymer, the soluble ketone polymer, and the soluble aromatic sulfide polymer, a combination of the organic acid cellulose, the polyurethane, and the soluble polyamide, a combination of the soluble imide polymer and the soluble polyamide, or a combination of the soluble sulfone polymer, the soluble ketone polymer, and the soluble aromatic sulfide polymer.

[0029] Preferably, the concentration of the special polymer solution is 10-60 wt%, for example, can be 10 wt%, 20 wt%, 30 wt%, 40 wt%, 50 wt%, or 60 wt%, but is not limited to the listed values, and other values not listed in the value range are also applicable; preferably 20-40 wt%.

[0030] Preferably, the polar solution comprises any one or a combination of at least two of N,N-dimethylacetamide, N,N-dimethylformamide, N-methylpyrrolidone, dimethyl sulfoxide, sulfolane, or butyric acid, typically but not limitedly a combination of N,N-dimethylacetamide, N,N-dimethylformamide, and N-methylpyrrolidone, a combination of dimethyl sulfoxide and sulfolane, a combination of N,N-dimethylacetamide and dimethyl sulfoxide, or a combination of N,N-dimethylacetamide, N,N-dimethylformamide, N-methylpyrrolidone, dimethyl sulfoxide, sulfolane, and butyric acid.

[0031] Preferably, the mass ratio of the special polymer and the polar solution is 1:(1.5-4), for example, can be 1:1.5, 1:2, 1:3, or 1:4, but is not limited to the listed values, and other values not listed in the value range are also applicable.

[0032] Preferably, the coagulation device is provided with a coagulation agent.

[0033] Preferably, the coagulation agent comprises a mixed solution of an inert solvent and a pore-forming agent.

[0034] Preferably, the inert solvent comprises any one or a combination of at least two of water, toluene, xylene, methanol, ethanol, or isopropanol, typically but not limitedly a combination of water, toluene, and xylene, a combination of methanol, ethanol, and isopropanol, a combination of toluene, xylene, methanol, ethanol, and isopropanol, or a combination of water, toluene, xylene, methanol, ethanol, and isopropanol.

[0035] Preferably, the pore-forming agent comprises any one or a combination of at least two of glycerol, sorbitol, glucose, fructose, erythritol or sorbitan, typically but not limited to a combination of glycerol, sorbitol and sorbitan, a combination of glucose, fructose and erythritol, or a combination of glycerol, sorbitol, glucose, fructose, erythritol and sorbitan.

[0036] Preferably, the pore-forming agent is present in an amount of 1 ‰ to 8 ‰ by mass of the inert solvent, for example, it can be 1 ‰, 2 ‰, 3 ‰, 4 ‰, 5 ‰, 6 ‰, 7 ‰ or 8 ‰, but is not limited to the listed values, and other values not listed within the range are also applicable.

[0037] The pore-forming agent described in the present application plays a role in storing pores during the precipitation process, so that the surface and interior of the special polymer solid after precipitation have more pores, which is conducive to the subsequent purification process to more easily wash out the solvent and other impurities remaining inside, and thus a high-purity polymer can be obtained.

[0038] In a second aspect, the present application provides a method for simultaneously preparing special polymer powder and round sheets, which uses the device system provided in the first aspect.

[0039] Preferably, the method comprises the following steps:

[0040] (1) Start the crushing device, the light component slurry circulating pump and the heavy component slurry circulating pump;

[0041] (2) Deliver the reaction reagent in the solution storage tank to the precipitation device, mix with the precipitation agent, and precipitate to obtain a special polymer solid;

[0042] (3) Continuously crush the special polymer solid obtained in step (2) using the crushing device until the particles after crushing meet the expected standard; and then separate to obtain special polymer powder and special polymer particles.

[0043] Preferably, during the precipitation process of step (2), the liquid surface height in the precipitation device is kept higher than the upper edge of the funnel mouth of the funnel;

[0044] Preferably, during the continuous crushing process of step (3), the liquid surface height in the precipitation device is kept higher than the upper edge of the funnel mouth of the funnel;

[0045] Preferably, during the precipitation process of step (2) and the continuous crushing process of step (3), the light component slurry in the precipitation device is circulated by the light component slurry circulating pump;

[0046] Preferably, during the precipitation process in step (2) and the continuous crushing process in step (3), the reconstituted slurry in the precipitation equipment is recycled by the reconstituted slurry circulation pump.

[0047] Preferably, the special polymer powder in step (3) is obtained through a first solid-liquid separation device;

[0048] Preferably, the special polymer particles in step (3) are obtained by a second solid-liquid separation device.

[0049] Preferably, the D95 particle size of the pulverized particles in step (3) is ≤3mm, for example, it can be 3mm, 2.8mm, 2.5mm, 2mm, 1mm, 0.5mm or 0.2mm, but is not limited to the listed values. Other unlisted values ​​within the range are also applicable.

[0050] Preferably, the average particle size of the special polymer powder in step (3) is 0.5 to 1 mm, for example, it can be 0.5 mm, 0.6 mm, 0.7 mm, 0.8 mm, 0.9 mm or 1 mm, but is not limited to the listed values. Other unlisted values ​​within the range are also applicable.

[0051] Preferably, the average particle size of the special polymer particles in step (3) is 2 to 3 mm, for example, it can be 2 mm, 2.2 mm, 2.4 mm, 2.6 mm, 2.8 mm or 3 mm, but is not limited to the listed values. Other unlisted values ​​within the range are also applicable.

[0052] Preferably, the special polymer particles in step (3) are in the shape of flat, round flakes.

[0053] As a preferred embodiment of the present invention, the method for simultaneously preparing special polymer powder and wafers according to the second aspect of the present invention includes:

[0054] (1) Start the crushing equipment, the light component slurry circulation pump and the heavy component slurry circulation pump;

[0055] (2) The reaction reagent in the solution storage tank is transported to the precipitation equipment, mixed with the precipitation agent, and precipitated in the funnel to obtain a special polymer solid; the special polymer solid is transported to the pulverizing equipment through a bent pipe;

[0056] (3) The special polymer solid obtained in step (2) is continuously crushed using a crushing device until the crushed particles meet the expected standards; then the special polymer powder and special polymer particles are separated.

[0057] The method for determining the particle size after crushing is as follows: Take out the crushed particles from the bypass of the crushing equipment, observe and measure their particle size. If they meet the standard, open the first solid-liquid separation equipment and the second solid-liquid separation equipment; if they do not meet the standard, continue the cyclic crushing process.

[0058] During the sedimentation and pulverization process, the light component slurry circulation pump, the heavy component slurry circulation pump, and the pulverization equipment are kept running to ensure that there is no material residue in any part of the sedimentation equipment, so that the feeding and discharging can be carried out smoothly.

[0059] During the precipitation and pulverization process, it is necessary to ensure that the liquid level of the precipitating agent in the precipitation equipment is higher than the upper edge of the funnel opening.

[0060] The numerical range described in this invention includes not only the point values ​​listed above, but also any point values ​​within the numerical ranges not listed above. Due to space limitations and for the sake of brevity, this invention will not exhaustively list all the specific point values ​​included in the range.

[0061] Compared with the prior art, the present invention has the following beneficial effects:

[0062] (1) The device system provided by the present invention enables the special polymer solution to be continuously pulverized through continuous feeding, and can simultaneously obtain two kinds of solids, light powder and heavy flat discs, to adapt to different application fields;

[0063] (2) The special polymer obtained by using the device system provided by the present invention has more pores on its surface and inside, which makes it easier for the polymer to wash out the residual solvent and other impurities in the subsequent purification process, thus obtaining a clean polymer.

[0064] (3) The device system provided by the present invention uses a funnel-shaped feeding port, which avoids the liquid outlet of the precipitation equipment being too far from the liquid surface, thus preventing the solution from accurately entering the liquid outlet and the continuous crushing pump, and solves the problem of polymer solution clogging the discharge port of the precipitation equipment due to easy precipitation.

[0065] (4) In the device system provided by the present invention, the bottom of the funnel enters the continuous crushing equipment in a smooth arc manner, which avoids material blockage caused by using a right-angle elbow connection method;

[0066] (5) The device system provided by the present invention can achieve the purpose of rapid separation of heavy flat round pieces by the circulation action of two circulating pumps at the upper and lower edges of the funnel. Attached Figure Description

[0067] Figure 1 This is a diagram of the precipitation special polymer apparatus system provided in Embodiment 1 of the present invention;

[0068] Figure 2 Electron micrograph of the surface of a special polymer provided in Application Example 1 of the present invention;

[0069] Figure 3 Electron micrograph of the surface of a special polymer provided for application example 6 of the present invention.

[0070] Among them, 1 is a solution storage tank, 2 is a precipitation device, 3 is a funnel, 4 is a bend, 5 is a crushing device, 6 is the first solid-liquid separation device, 7 is a light component slurry circulation pump, 8 is a heavy component slurry circulation pump, and 9 is the second solid-liquid separation device. Detailed Implementation

[0071] The technical solution of the present invention will be further described below with reference to the accompanying drawings and specific embodiments. Those skilled in the art should understand that the embodiments described are merely illustrative of the present invention and should not be considered as specific limitations thereof.

[0072] Example 1

[0073] This embodiment provides a method such as Figure 1 The apparatus system shown includes a solution storage tank 1 and a precipitation device 2 connected in sequence; the precipitation device is equipped with a funnel 3 inside.

[0074] The funnel 3 is connected to the pulverizing device 5 via a bent pipe 4; the outlet of the pulverizing device 5 is divided into two branches, one of which is connected to the precipitation device 2, and the other is connected to the first solid-liquid separation device 6.

[0075] The side wall of the precipitation device 2 is provided with light component conveying pipes and heavy component conveying pipes;

[0076] The light component conveying pipeline is connected to the precipitation equipment 2 via the light component slurry circulation pump 7; the heavy component conveying pipeline is connected to the heavy component slurry circulation pump 8;

[0077] The outlet of the recombinant slurry circulation pump 8 is divided into two branches, one of which is connected to the sedimentation device 2, and the other is connected to the second solid-liquid separation device 9.

[0078] The light component conveying pipe is located above the upper edge of the funnel opening of the funnel 3; the heavy component conveying pipe is located below the upper edge of the funnel opening of the funnel 3.

[0079] The pulverizing device 5 is a pulverizing pump, the light component slurry circulation pump 7 is a cam rotor pump, and the heavy component slurry circulation pump 8 is a cam rotor pump; the first solid-liquid separation device 6 is a continuous centrifuge; and the second solid-liquid separation device 9 is a continuous centrifuge.

[0080] The ratio of the diameter of the funnel 3 to the diameter of the precipitation device 2 is 1:10; the ratio of the height from the upper edge of the funnel opening of the funnel 3 to the bottom of the precipitation device 2 to the height from the liquid surface of the precipitating agent in the precipitation device 2 to the bottom of the precipitation device 2 is 8:10; the ratio of the height from the upper edge of the funnel opening of the funnel 3 to the bottom of the precipitation device 2 to the radius of the circle containing the bend 4 is 2:1.

[0081] The solution storage tank 1 contains 30 kg of a 35 wt% polysulfone DMAC solution; the precipitation device 2, with a volume of 200 L, contains 120 kg of water, with 0.12 kg of glycerol added to the water.

[0082] Example 2

[0083] This embodiment provides a device system for precipitating special polymers, which differs from Embodiment 1 only in that:

[0084] In this embodiment, the reaction reagent inside the solution storage tank 1 is changed to 30 kg of 20% NMP solution of polyetherimide; and the precipitant inside the precipitation device 2 is changed to 90 kg of water and 0.18 kg of glucose.

[0085] In this embodiment, the ratio of the height from the upper edge of the funnel opening of the funnel 3 to the bottom of the precipitation device 2 to the height from the liquid surface of the precipitating agent in the precipitation device 2 to the bottom of the precipitation device 2 is changed to 6:10.

[0086] The ratio of the height of the upper edge of the funnel opening of the funnel 3 to the bottom of the sedimentation device 2 to the radius of the circle containing the bend 4 is changed to 10:1;

[0087] The light component slurry circulation pump 7 and the heavy component slurry circulation pump 8 are configured as mud pumps.

[0088] Example 3

[0089] This embodiment provides a device system for precipitating special polymers, which differs from Embodiment 1 only in that:

[0090] In this embodiment, the reaction reagent inside the solution storage tank 1 is changed to 30 kg of 40% polyphenylene sulfide sulfolane solution; and the precipitant inside the precipitation device 2 is changed to 60 kg of methanol and 0.18 kg of sorbitol.

[0091] In this embodiment, the ratio of the height from the upper edge of the funnel opening of the funnel 3 to the bottom of the precipitation device 2 to the height from the liquid surface of the precipitating agent in the precipitation device 2 to the bottom of the precipitation device 2 is changed to 5:10.

[0092] The ratio of the height of the upper edge of the funnel 3 to the bottom of the sedimentation device 2 to the radius of the circle containing the bend 4 is changed to 5:1.

[0093] The crushing device 5 was replaced with a Wehrlin shear, and the light component slurry circulation pump 7 and the heavy component slurry circulation pump 8 were set as mud pumps.

[0094] Example 4

[0095] This embodiment provides a device system for precipitating special polymers, which differs from Embodiment 1 only in that:

[0096] In this embodiment, the reaction reagent inside the solution storage tank 1 is changed to 30 kg of 10% polyphenylsulfone sulfolane solution; and the precipitant inside the 500 L precipitation device 2 is changed to 300 kg of ethanol and 1.5 kg of fructose.

[0097] In this embodiment, the ratio of the height from the upper edge of the funnel opening of the funnel 3 to the bottom of the precipitation device 2 to the height from the liquid surface of the precipitating agent in the precipitation device 2 to the bottom of the precipitation device 2 is changed to 9.5:10.

[0098] Change the ratio of the height from the upper edge of the funnel opening of the funnel 3 to the bottom of the sedimentation device 2 to the radius of the circle containing the bend 4 to 1:1;

[0099] The crushing device 5 was replaced with a grinder.

[0100] Example 5

[0101] This embodiment provides a device system for precipitating special polymers, which differs from Embodiment 1 only in that:

[0102] In this embodiment, the reaction reagent inside the solution storage tank 1 is changed to 30 kg of butyric acid solution of 60% cellulose acetate butyrate; and the precipitant inside the precipitation device 2 with a volume of 1000 L is changed to 600 kg of water and 4.8 kg of dehydrated sorbitol.

[0103] In this embodiment, the ratio of the height from the upper edge of the funnel opening of the funnel 3 to the bottom of the precipitation device 2 to the height from the liquid surface of the precipitating agent in the precipitation device 2 to the bottom of the precipitation device 2 is changed to 9:10.

[0104] Change the ratio of the height from the upper edge of the funnel opening of the funnel 3 to the bottom of the sedimentation device 2 to the radius of the circle containing the bend 4 to 50:1;

[0105] The pulverizing device 5 was replaced with a colloid mill.

[0106] Example 6

[0107] This embodiment provides a device system for precipitating special polymers, which differs from Embodiment 1 only in that:

[0108] In this embodiment, no pore-forming agent was added to the precipitation equipment 2.

[0109] Comparative Example 1

[0110] This comparative example provides an apparatus system for precipitating special polymers, which differs from that of Example 1 only in that:

[0111] This comparative example did not include a funnel in the precipitation device 2.

[0112] Comparative Example 2

[0113] This comparative example provides an apparatus system for precipitating special polymers, which differs from that of Example 1 only in that:

[0114] This comparative example changes bend 4 to a right-angle bend.

[0115] Application Example 1

[0116] This application example provides a method for simultaneously preparing specialty polymer powder and discs, the method being carried out within the apparatus system for precipitating specialty polymers provided in Example 1.

[0117] The method for simultaneously preparing special polymer powder and wafers includes the following steps:

[0118] (1) Start the crushing equipment, the light component slurry circulation pump and the heavy component slurry circulation pump;

[0119] (2) The reaction reagents in the solution storage tank are all transferred to the precipitation equipment within 20 minutes, mixed with the precipitation agent, and precipitated in the funnel to obtain a special polymer solid; the special polymer solid is transferred to the pulverizing equipment through a bent pipe;

[0120] (3) After continuously crushing the special polymer solid obtained in step (2) for 10 minutes using a crushing equipment, check that the crushed particles meet the expected standards.

[0121] Then, the first and second solid-liquid separation devices were opened for centrifugation to obtain special polymer powder and special polymer discs; their electron micrographs are shown below. Figure 2 As shown;

[0122] Add 4.5 kg of water to the sedimentation equipment during the centrifugation process.

[0123] Application Example 2

[0124] This application example provides a method for simultaneously preparing specialty polymer powder and discs, the method being carried out within the apparatus system for precipitating specialty polymers provided in Example 2.

[0125] The method for simultaneously preparing special polymer powder and wafers differs from Example 1 only in that:

[0126] In this application example, the mixing time of the reaction reagents and precipitant is 50 minutes, and the continuous pulverization time is 10 minutes; 3 kg of water is added to the precipitation equipment during the subsequent separation process.

[0127] Application Example 3

[0128] This application example provides a method for simultaneously preparing specialty polymer powder and discs, the method being carried out within the apparatus system for precipitating specialty polymers provided in Example 3.

[0129] The method for simultaneously preparing special polymer powder and wafers differs from Example 1 only in that:

[0130] In this application example, the mixing time of the reaction reagents and precipitant was 180 min, and the continuous pulverization time was 50 min; 6 kg of methanol was added to the precipitation equipment during the subsequent separation process.

[0131] Application Example 4

[0132] This application example provides a method for simultaneously preparing specialty polymer powder and discs, the method being carried out within the apparatus system for precipitating specialty polymers provided in Example 4.

[0133] The method for simultaneously preparing special polymer powder and wafers differs from Example 1 only in that:

[0134] In this application example, the mixing time of the reaction reagents and precipitant was 300 min, and the continuous pulverization time was 20 min; 1.5 kg of ethanol was added to the precipitation equipment during the subsequent separation process.

[0135] Application Example 5

[0136] This application example provides a method for simultaneously preparing specialty polymer powder and discs, the method being carried out within the apparatus system for precipitating specialty polymers provided in Example 5.

[0137] The method for simultaneously preparing special polymer powder and wafers differs from Example 1 only in that:

[0138] In this application example, the mixing time of the reaction reagents and precipitant was 5 minutes, and the continuous pulverization time was 1 minute; 9 kg of water was added to the precipitation equipment during the subsequent separation process.

[0139] Application Example 6

[0140] This application example provides a method for simultaneously preparing specialty polymer powder and discs, the method being carried out within the apparatus system for precipitating specialty polymers provided in Example 6.

[0141] The method for simultaneously preparing special polymer powder and wafers differs from Example 1 only in that:

[0142] In this application example, the mixing time of the reaction reagents and precipitant was 20 minutes, and the continuous pulverization time was 10 minutes; 4.5 kg of water was added to the precipitation equipment during the subsequent separation process.

[0143] The surface electron micrograph of the special polymer particles obtained in this application example is shown below. Figure 3 As shown.

[0144] Application Example 7

[0145] This application example provides a method for simultaneously preparing specialty polymer powder and discs, the method being carried out within the apparatus system for precipitating specialty polymers provided in Example 6.

[0146] The method for simultaneously preparing special polymer powder and wafers differs from Example 1 only in that:

[0147] In this application example, the continuous pulverization in step (3) is changed to a single pulverization. The special polymer solid obtained by centrifugation cannot be separated into powder and discs. Only solid particles with a particle size of 3-5 mm and a bulk density of 0.04 g / ml can be obtained, with a yield of 98.5%.

[0148] Comparative Application Example 1

[0149] This comparative application example provides a method for simultaneously preparing specialty polymer powder and discs, the method being carried out within the apparatus system for precipitating specialty polymers provided in Comparative Example 1.

[0150] The method for simultaneously preparing special polymer powder and wafers includes:

[0151] When the pulverizing equipment is turned on, the reaction reagents are continuously added to the precipitation equipment. Due to the impact of the water flow, the downstream solution cannot accurately enter the pulverizing equipment. Therefore, after 5 minutes of feeding, the precipitation equipment becomes clogged and needs to be stopped to clean the material.

[0152] Comparative Application Example 2

[0153] This comparative application example provides a method for simultaneously preparing specialty polymer powder and discs, the method being carried out within the apparatus system for precipitating specialty polymers provided in Comparative Example 1.

[0154] During the operation of the method for simultaneously preparing special polymer powder and discs, when the precipitate in the funnel passes through the right-angle bend, the precipitate becomes blocked at the right-angle bend, causing the equipment to be unable to continue operating, and thus requiring shutdown to clean the material.

[0155] The special polymer powder and special polymer discs obtained in Application Examples 1-6 were washed and dried four times in one go, and then tested. The test results are shown in Table 1.

[0156] Table 1

[0157]

[0158] In summary, the specialty polymer powder and flat discs obtained using the apparatus system provided by this invention have more pores on their surface compared to conventional specialty polymers, making it easier to clean residual substances inside the discs and resulting in a high degree of cleanliness in the final specialty polymer. The specialty polymer powder can be used for blending modification or coatings; the specialty polymer discs can be used for granulation, molding, or film formation.

[0159] The applicant declares that the detailed structural features of the present invention are illustrated through the above embodiments, but the present invention is not limited to the above detailed structural features, that is, it does not mean that the present invention must rely on the above detailed structural features to be implemented. Those skilled in the art should understand that any improvements to the present invention, equivalent substitutions for the components selected in the present invention, additions of auxiliary components, selection of specific methods, etc., all fall within the protection scope and disclosure scope of the present invention.

[0160] The applicant declares that the detailed process flow of this invention is illustrated by the above embodiments, but this invention is not limited to the above detailed process flow, that is, it does not mean that this invention must rely on the above detailed process flow to be implemented. Those skilled in the art should understand that any improvements to this invention, equivalent substitutions of raw materials for the product of this invention, addition of auxiliary components, and selection of specific methods, etc., all fall within the protection scope and disclosure scope of this invention.

Claims

1. A method for simultaneously preparing specialty polymer powder and wafers, comprising using an apparatus system for precipitating specialty polymers, characterized in that, The device system includes a solution storage tank and a precipitation device connected in sequence. The precipitation device has a funnel inside. The funnel is connected to a pulverizing device via a bend in the pipe. The outlet of the pulverizing device is divided into two branches, one connected to the precipitation device and the other connected to a first solid-liquid separation device. The precipitation device contains a precipitating agent, with the liquid level of the precipitating agent higher than the upper edge of the funnel opening. The side wall of the precipitation device has a light component conveying pipe and a heavy component conveying pipe. The light component conveying pipe is located above the upper edge of the funnel opening; the heavy component conveying pipe is located below the upper edge of the funnel opening. The light component conveying pipe is connected to the precipitation device via a light component slurry circulation pump; the heavy component conveying pipe is connected to the heavy component slurry circulation pump. The outlet of the heavy component slurry circulation pump is divided into two branches, one connected to the precipitation device and the other connected to a second solid-liquid separation device. The ratio of the diameter of the funnel to the diameter of the precipitation device is 1:(3~50); the ratio of the height from the upper edge of the funnel opening to the bottom of the precipitation device to the height from the liquid surface of the precipitating agent in the precipitation device to the bottom of the precipitation device is (5~9.5):10; the ratio of the height from the upper edge of the funnel opening to the bottom of the precipitation device to the radius of the circle containing the bend is (1~50):

1. The method includes the following steps: (1) starting the pulverizing equipment, the light component slurry circulation pump and the heavy component slurry circulation pump; (2) transporting the reaction reagent in the solution storage tank to the precipitation equipment, mixing it with the precipitation agent, and precipitating to obtain a special polymer solid; (3) continuously pulverizing the special polymer solid obtained in step (2) using the pulverizing equipment until the pulverized particles meet the expected standards; then opening the first solid-liquid separation equipment and the second solid-liquid separation equipment, obtaining special polymer powder through the first solid-liquid separation equipment, and obtaining special polymer particles through the second solid-liquid separation equipment; The solution storage tank is equipped with reaction reagents; the reaction reagents include a mixture of a special polymer solution and a polar solution; the special polymer solution includes any one or a combination of at least two of the following: soluble imide polymer, soluble sulfone polymer, soluble ketone polymer, soluble aromatic sulfide polymer, organic acid cellulose, polyurethane or soluble polyamide. In the precipitation process described in step (2) and the continuous pulverization process described in step (3), the light component slurry in the precipitation equipment is circulated by a light component slurry circulation pump; in the precipitation process described in step (2) and the continuous pulverization process described in step (3), the heavy component slurry in the precipitation equipment is circulated by a heavy component slurry circulation pump. In step (2), during the precipitation process, the liquid surface level in the precipitation equipment is kept higher than the upper edge of the funnel opening; in step (3), during the continuous pulverization process, the liquid surface level in the precipitation equipment is kept higher than the upper edge of the funnel opening. The D95 particle size of the pulverized particles in step (3) is ≤3mm; the average particle size of the special polymer powder in step (3) is 0.5~1mm; the average particle size of the special polymer particles in step (3) is 2~3mm; the shape of the special polymer particles in step (3) includes flat round flakes.

2. The method according to claim 1, characterized in that, The liquid outlet of the second solid-liquid separation device is connected to the precipitation device.

3. The method according to claim 1, characterized in that, The pulverizing equipment includes any one of a pulverizing pump, a grinder, a colloid mill, or a Weilling shear.

4. The method according to claim 3, characterized in that, The pulverizing equipment includes a pulverizing pump.

5. The method according to claim 1, characterized in that, The light component slurry circulation pump includes any one of a crushing pump, a mud pump, a centrifugal pump, a screw pump, or a rotary pump.

6. The method according to claim 1, characterized in that, The recombinant slurry circulation pump includes any one of a crushing pump, a mud pump, a centrifugal pump, a screw pump, or a rotary pump.

7. The method according to claim 1, characterized in that, The first solid-liquid separation device includes any one of a continuous centrifuge, a continuous leaf filter, or an intermittent switching closed plate filter.

8. The method according to claim 1, characterized in that, The second solid-liquid separation device includes any one of a continuous centrifuge, a continuous leaf filter, or an intermittent switching closed plate filter.

9. The method according to claim 1, characterized in that, The ratio of the diameter of the funnel to the diameter of the precipitation device is 1:(5~20).

10. The method according to claim 1, characterized in that, The ratio of the height from the upper edge of the funnel opening to the bottom of the precipitation equipment to the height from the surface of the precipitating agent in the precipitation equipment to the bottom of the precipitation equipment is (6~9):

10.

11. The method according to claim 1, characterized in that, The ratio of the height from the upper edge of the funnel opening to the bottom of the sedimentation equipment to the radius of the circle containing the bend is (2~10):

1.

12. The method according to claim 1, characterized in that, The concentration of the special polymer solution is 10~60wt%.

13. The method according to claim 12, characterized in that, The concentration of the special polymer solution is 20~40wt%.

14. The method according to claim 1, characterized in that, The polar solution includes any one or a combination of at least two of N,N-dimethylacetamide, N,N-dimethylformamide, N-methylpyrrolidone, dimethyl sulfoxide, sulfolane, or butyric acid.

15. The method according to claim 1, characterized in that, The mass ratio of the special polymer to the polar solution is 1:(1.5~4).

16. The method according to claim 1, characterized in that, The precipitant comprises a mixed solution of an inert solvent and a pore-forming agent.

17. The method according to claim 16, characterized in that, The inert solvent includes any one or a combination of at least two of water, toluene, xylene, methanol, ethanol, or isopropanol.

18. The method according to claim 16, characterized in that, The pore-forming agent includes any one or a combination of at least two of glycerol, sorbitol, glucose, fructose, erythritol, or dehydrated sorbitol.

19. The method according to claim 16, characterized in that, The content of the pore-forming agent is 1‰ to 8‰ of the mass of the inert solvent.

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