CN109749099B - Solid powder precipitation system and continuous precipitation method for polymer solution - Google Patents
Solid powder precipitation system and continuous precipitation method for polymer solution Download PDFInfo
- Publication number
- CN109749099B CN109749099B CN201910145891.2A CN201910145891A CN109749099B CN 109749099 B CN109749099 B CN 109749099B CN 201910145891 A CN201910145891 A CN 201910145891A CN 109749099 B CN109749099 B CN 109749099B
- Authority
- CN
- China
- Prior art keywords
- polymer solution
- fluid
- polymer
- pipe
- feeding pipe
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Landscapes
- Processes Of Treating Macromolecular Substances (AREA)
Abstract
The invention discloses a polymer solution solid powder precipitation system and a continuous precipitation method, wherein the system comprises a dispersion mixer, the dispersion mixer comprises a fluid feeding pipe, a fluid discharging pipe and a polymer solution feeding pipe, the fluid feeding pipe and the fluid discharging pipe are connected together through a connecting part, a feeding hole of the polymer solution feeding pipe is arranged on the fluid feeding pipe, and a discharging hole of the polymer solution feeding pipe is arranged in the connecting part; the fluid discharging pipe is connected with a liquid inlet of the solid-liquid separator, a liquid outlet of the solid-liquid separator is connected with the liquid storage tank, and the liquid storage tank is connected with the fluid feeding pipe through a fluid conveying pipeline. The system of the invention is adopted to separate out the polymer, and polymer solid particles with narrow distribution range and different particle size ranges can be obtained in a short time by setting the flow rates of the polymer solution and the poor solvent, thereby solving the problems of slurry coating, uneven particles, segment shape and even formation of 'coil' in the traditional method and being beneficial to industrial production.
Description
Technical Field
The invention relates to a solid powder precipitation system and a precipitation method for a polymer solution, in particular to a system and a method capable of sufficiently and continuously precipitating a polymer in a solid powder form with uniform size.
Background
The preparation of the polymeric material is usually carried out in a solvent from which the polymeric product is isolated prior to use and generally requires that the polymer be precipitated with a suitable particle size to ensure ease of subsequent isolation, washing, drying and use.
The preparation method of the polymer microparticles mainly comprises the following steps: (1) emulsion-solvent evaporation method: dispersing the polymer solution into a dispersion medium containing a surfactant by using methods such as ultrasound, strong stirring and the like to form emulsion droplets, wherein the particle size distribution of the formed polymer particles is wide, and the surfactant is difficult to remove; (2) salting out method: the polymer in the polymer solution is precipitated as solid particles by the action of the electrolyte, but it is inefficient and unsuitable for industrial applications (bindachaledler c., et al, us Patent 4,968,350 (1990)); (3) and a dialysis method: respectively adding the polymer solution and the poor solvent of the polymer to two sides of the permeable membrane, and continuously diffusing the good solvent in the polymer solution into the poor solvent to form polymer particles, wherein the method is long in time consumption and not beneficial to industrial production; (4) spray drying method: the polymer solution is sprayed into a hot gas stream to rapidly volatilize the solvent and obtain polymer particles. However, for a high boiling point solvent system, the energy consumption is high, even if the height of the drying tower is increased to ensure that the solvent is removed as much as possible, the residual solvent amount in the product still can not meet the requirement, and secondary drying (such as a fluidized bed) has to be carried out; (5) dissolution and precipitation method: the polymer solution is slowly added into a large amount of poor solvent under the stirring condition to obtain polymer precipitated particles, but because the polymer has large molecular weight and high cohesive energy, only products with large particles and wide particle size distribution can be obtained even through forced dispersion and shearing. For polymers with higher molecular weights, a coil-type product is often obtained. Meanwhile, the surface of the polymer solution droplet is firstly contacted with the poor solvent and the polymer is separated out to form a hard shell, so that the permeation of the poor solvent to the interior of the droplet is prevented or slowed down, and a wrapping structure is formed, so that the separation efficiency of the polymer is reduced, the removal rate of impurities is influenced, even a large amount of good solvent is carried in the precipitate, the risk of polymer agglomeration and pipeline blockage exists in the filtering and drying processes, and meanwhile, the later-stage use of polymer particles is greatly influenced. Therefore, it is very important to develop a simple, fast, efficient and continuous method for separating out solid polymer particles with uniform particle size.
Disclosure of Invention
The invention aims to provide a polymer solution solid powdering and precipitating system which can continuously treat a polymer solution to realize continuous precipitation of polymer solids, and the obtained polymer particles are uniform in size distribution.
The invention also aims to provide a continuous precipitation method of solid powder in polymer solution, which adopts the system to process the polymer solution, can conveniently, efficiently and continuously obtain polymer particles, and avoids the defects of polymer wrapping, caking, wide particle size distribution, solvent residue, high energy consumption and the like.
In order to achieve the purpose, the invention adopts the following technical scheme:
a polymer solution solid powdering and separating system comprises a dispersive mixer, wherein the dispersive mixer comprises a fluid feeding pipe, a fluid discharging pipe and a polymer solution feeding pipe, the fluid feeding pipe and the fluid discharging pipe are connected together through a connecting part, a feeding port of the polymer solution feeding pipe is arranged on the fluid feeding pipe, and a discharging port of the polymer solution feeding pipe is arranged in the connecting part; the fluid discharging pipe is connected with a liquid inlet of the solid-liquid separator, a liquid outlet of the solid-liquid separator is connected with the liquid storage tank, and the liquid storage tank is connected with the fluid feeding pipe through a fluid conveying pipeline.
Further, the invention realizes the precipitation of the polymer by adding the poor solvent of the polymer into the polymer solution (the mixture consisting of the polymer and the good solvent of the polymer), in the solid powdering precipitation system, the dispersing mixer is the key for realizing the precipitation of the polymer, the poor solvent of the polymer enters the dispersing mixer from the fluid feeding pipe, the polymer solution enters the dispersing mixer from the polymer solution feeding pipe, in the dispersing mixing, the poor solvent and the polymer solution are fully contacted and mixed, the powdering precipitation of the polymer is realized, and finally, the materials in the dispersing mixer are discharged to the solid-liquid separator together from the fluid discharging port for separation.
Further, the diameter of the fluid feed pipe is larger than that of the fluid discharge pipe, and the fluid feed pipe and the fluid discharge pipe are connected by a connecting part, wherein one end of the connecting part connected with the fluid feed pipe is thicker than one end connected with the fluid discharge pipe. Preferably, the connecting member is shaped like a horn. The connecting part is provided with a through hole which enables the fluid feeding pipe to be communicated with the fluid discharging pipe.
Further, the diameter of the polymer solution feed pipe is smaller than the diameter of the fluid discharge pipe.
Furthermore, two wings are provided in the connecting part, said wings being fixed in the connecting part, preferably at the outlet of the polymer solution feed pipe. Preferably, the two wings are arranged perpendicular to each other. When the system starts, under the action of the two wing plates, the poor solvent entering through the fluid feeding pipe and the polymer solution entering through the polymer solution conveying pipe form turbulence, so that the contact and collision of the poor solvent and the polymer solution are strengthened, the uniform precipitation of the polymer is facilitated, and the wrapping of the poor solvent on the polymer is prevented.
Furthermore, a bulge is arranged on the inner wall of the fluid discharge pipe. Preferably, the protrusions on the inner wall of the fluid discharge pipe are symmetrically distributed, and the protrusions are used for dispersing and crushing the precipitated polymer solids again, preventing the polymer solids from caking and agglomerating, and keeping the particle size of the polymer solids uniform. The distribution density of the bulges, the shape of the bulges and the height of the bulges can be adjusted according to the needs. Preferably, the bulge is mushroom-shaped, and the height of the whole bulge is 1/5-2/5 of the inner diameter of the fluid discharge pipe.
In order to efficiently and rapidly precipitate the polymer, the length ratio of the fluid feeding pipe to the fluid discharging pipe is preferably 1-3:1, the diameter ratio of the fluid feeding pipe to the fluid discharging pipe is preferably 1-4:1, and the diameter ratio of the fluid discharging pipe to the polymer solution feeding pipe is preferably 1-4: 1.
Furthermore, the polymer solution solid powdering and separating system also comprises a circulating pump for conveying the liquid in the liquid storage tank into the fluid conveying pipeline. The circulation pump can pump the fluid in the liquid storage tank into the dispersion mixer through the fluid conveying pipeline. The materials in the dispersing mixer are forcibly mixed and dispersed and then discharged from the fluid discharge pipe to enter the solid-liquid separator, the solid separated by the solid-liquid separator is polymer powder, the separated liquid is a mixture of poor solvent and good solvent and enters the liquid storage tank for recycling, no waste liquid is generated in the operation process of the whole system, the using amount of the poor solvent is reduced, and circulating and continuous treatment is realized.
Further, the polymer solution solid powdering and precipitation system further comprises a flow regulating valve and a flow meter for controlling the flow rate of the fluid, wherein the flow regulating valve and the flow meter are arranged on the fluid conveying pipeline.
Further, the invention also provides a continuous precipitation method of solid powder in polymer solution, which comprises the following steps:
(1) adding a poor solvent of the polymer into the liquid storage tank, and controlling the poor solvent to enter a fluid feeding pipe of the dispersion mixer through a fluid conveying pipeline according to the flow speed of 0.5-5 m/s;
(2) controlling the polymer solution to enter a dispersion mixer from a polymer solution feeding pipe according to 0.2-2% of the flow rate of the poor solvent;
(3) the polymer solution and the poor polymer solvent form turbulent flow in a connecting part of the dispersing mixer, the polymer is separated out in the contact process of the polymer solution and the poor polymer solvent, and then the mixed material continuously flows out of the fluid discharge pipe and enters a solid-liquid separator;
(4) the polymer is collected after being separated by a solid-liquid separator, and the separated liquid (polymer separated mother liquor) enters a liquid storage tank.
The method of the present invention can precipitate the polymer in the good solvent in the system of the poor solvent in the form of solid powder in a short time, and polymer particles in different particle size ranges can be prepared by adjusting the flow rates of the poor solvent and the polymer solution, which can be realized by the fluid delivery pressure. And the poor solvent can be recycled to a certain extent, so that the cost is greatly reduced.
Further, the polymer is at least one of polyimide, polyamide, polybenzoxazole, polyaniline, polycarbonate, polyacrylonitrile and epoxy resin.
Further, the polymer is a mixture of a polymer and a good solvent thereof, and the good solvent is at least one of N-methylpyrrolidone (NMP), N-Dimethylacetamide (DMAC), Tetrahydrofuran (THF), and Dimethylsulfoxide (DMSO).
Further, the poor solvent is a solvent having a solubility in the polymer of less than 2wt% at room temperature and normal pressure, and more preferably a solvent having a solubility in the polymer of less than 0.5 wt%; preferably, the poor solvent is at least one of water, methanol, ethanol, acetone, ethyl acetate and toluene.
Further, the concentration of the polymer solution is 5-50 wt%.
The polymer solution solid powder precipitation system comprises a fluid conveying pipeline, a liquid storage tank, a dispersing mixer, a solid-liquid separator and the like, wherein the dispersing mixer is special in structure, and can enable fluid to form turbulence and increase the contact area and contact uniformity of materials. The polymer solution and the poor solvent respectively enter the dispersing mixer through the polymer solution feeding pipe and the fluid feeding pipe, and realize forced mixing and precipitation at the connecting part of the dispersing mixer, and realize the homogenization of the polymer particle size when flowing through the fluid discharging pipe. The system of the invention is adopted to separate out the polymer, and the polymer solid particles with narrow distribution range and different particle size ranges can be obtained in a short time by setting the flow rates of the polymer solution and the poor solvent, thereby solving the problems of slurry coating, uneven particle, segment shape and even formation of 'coil' in the traditional method, and the mother liquor after the polymer is separated out can be recycled to extract the polymer again, thereby improving the yield. The method is convenient, efficient, rapid and controllable, and is beneficial to industrial production.
Drawings
FIG. 1 is a schematic view showing the structure of a solid-powdering precipitation system for a polymer solution according to the present invention.
FIG. 2 is a schematic view of the structure of the disperser.
FIG. 3 is a cross-sectional view of the disperser.
Fig. 4 is a schematic structural view of a wing plate.
FIG. 5 is a schematic cross-sectional view of a dispersion mixer fluid discharge pipe.
FIG. 6 is a schematic cross-sectional view of a static mixer used in comparative example 3.
In the figure, 1: a dispersion mixer; 2: a circulation pump; 3: a flow regulating valve; 4: a flow meter; 5: a fluid delivery conduit; 6: a solid-liquid separator; 7: a liquid storage tank; 8: a fluid feed conduit; 9: a fluid outlet pipe; 10: a polymer solution feed pipe; 11: a connecting member; 12: a wing plate; 13: a protrusion; 14: and a through hole.
Detailed Description
The invention will be further described with reference to the following drawings and specific examples, which are given by way of illustration only and are not intended to be limiting.
Example 1
Fig. 1 is a schematic diagram of a polymer solution solid powdering and separating system according to the present invention, which includes a dispersing mixer 1, a solid-liquid separator 6 connected to the dispersing mixer, a liquid storage tank 7 connected to the solid-liquid separator, a fluid transfer pipe 5 connected to the liquid storage tank, and a circulation pump 2 for pumping a liquid in the liquid storage tank into the fluid transfer pipe, and further includes a flow control valve 3 and a flow meter 4 disposed on the fluid transfer pipe for controlling a flow rate of the fluid. Wherein the other end of the fluid delivery conduit is connected to the disperser.
As shown in fig. 2, the disperser comprises a fluid feed pipe 8, a fluid discharge pipe 9 and a polymer solution feed pipe 10, wherein the fluid feed pipe and the fluid discharge pipe are connected, have no angle therebetween, and are in the same straight line. As shown in fig. 3, the fluid feeding pipe and the fluid discharging pipe are connected together by a connecting part 11, wherein the fluid feeding pipe and the fluid discharging pipe are both tubular, and wherein the fluid feeding pipe has a larger pipe diameter than the fluid discharging pipe. One end of the connecting part is connected with the fluid feeding pipe, the other end of the connecting part is connected with the fluid discharging pipe, and one end connected with the fluid feeding pipe is thicker than one end connected with the fluid discharging pipe. The connecting part is shaped like a horn, but other possible shapes can be provided. The connecting member is provided with a through hole 14 so that the fluid feed pipe and the fluid discharge pipe communicate with each other.
Further, as shown in fig. 3, mushroom-shaped protrusions 13 are uniformly distributed on the inner wall of the fluid discharge pipe, and as shown in fig. 5, the mushroom-shaped protrusions are symmetrically distributed on the inner wall of the fluid discharge pipe, so that the separated polymer can be dispersed and crushed, and can be prevented from being agglomerated and agglomerated. The polymer solution feed pipe 10 is also tubular and has a smaller diameter than the fluid discharge pipe, wherein the inlet of the polymer solution feed pipe is disposed on the fluid feed pipe and protrudes from the fluid feed pipe to facilitate the entry of the polymer solution, and the outlet of the polymer solution feed pipe is located in the connecting part from which the polymer solution flows out and is mixed with the poor solvent flowing into the fluid feed pipe in the connecting part. The connecting part is also internally provided with two wing plates which are arranged vertically and fixed in the connecting part, the mounting position of the wing plates is preferably the discharge port of a polymer solution feeding pipe, when the polymer solution and the poor solvent are mixed and contacted, because the wing plates can form turbulent flow, the polymer solution and the poor solvent can be fully contacted and dispersed under the action of the turbulent flow, the polymer can be fully separated out and dispersed, and the purposes of preventing agglomeration and agglomeration are achieved.
Preferably, the length ratio of the fluid feed pipe to the fluid discharge pipe is 1-3:1, the diameter ratio of the fluid feed pipe to the fluid discharge pipe is 1-4:1, and the diameter ratio of the fluid discharge pipe to the polymer solution feed pipe is 1-4: 1.
Preferably, the height of the integral bulge is 1/5-2/5 of the inner diameter of the fluid discharge pipe.
Except for the above-described structures, the circulating pump, the solid-liquid separator and the liquid storage tank used in the invention are all devices with conventional structures in the field, and are not described in detail herein. The person skilled in the art can select suitable devices in the prior art depending on their effect. The dispersion mixer of the present invention having the above-mentioned structure can be prepared by itself, and the apparatus disclosed in patent 200580050210.0 can be used as the dispersion mixer of the present invention.
When the polymer solution solid powder precipitation system is used, a poor solvent of a polymer is injected into a liquid storage tank, a circulating pump switch is turned on, the flow rate of the poor solvent is controlled by a flow regulating valve, the poor solvent enters a dispersing mixer at a certain speed, meanwhile, a polymer solution with a certain concentration is injected into the dispersing mixer through a polymer solution feeding pipe at a certain flow rate, the poor solvent and the polymer solution are fully mixed at a connecting part, the polymer is continuously precipitated in the process, materials entering the dispersing mixer continuously flow out of a fluid discharging pipe of the dispersing mixer at a certain speed, and the precipitated polymer is further crushed and dispersed by protrusions on the inner wall of the fluid discharging pipe in the process that the materials pass through the fluid discharging pipe, so that the precipitated polymer is prevented from caking, agglomeration and agglomeration, And the coating ensures that the polymer particles are uniform and have narrow particle size distribution. And the material flows out of the dispersing mixer and then enters a solid-liquid separator, the separation of polymer solid and liquid is realized in the solid-liquid separator, the polymer solid is collected and further operated to obtain a required product, and the liquid after the polymer is separated enters a liquid storage tank for recycling. The recycling of the polymer mother liquor can improve the yield of the polymer, and when the polymer precipitation is obviously reduced after the system is recycled for a certain time, the poor solvent is replaced by new poor solvent.
Preferably, the poor solvent is fed into the dispersing mixer at a flow rate of 0.5m/s to 5m/s, and the flow rate of the polymer solution fed into the dispersing mixer is 0.2 to 2% of the flow rate of the poor solvent.
Preferably, the concentration of the polymer solution is 5 to 50 wt.%.
Preferably, the polymer is at least one of polyimide, polyamide, polybenzoxazole, polyaniline, polycarbonate, polyacrylonitrile and epoxy resin.
Preferably, the good solvent is at least one of N-methylpyrrolidone (NMP), N-Dimethylacetamide (DMAC), Tetrahydrofuran (THF), and Dimethylsulfoxide (DMSO).
Preferably, the poor solvent is a solvent having a solubility in the polymer of less than 2wt% at room temperature and normal pressure, more preferably a solvent having a solubility in the polymer of less than 0.5wt%, such as water, methanol, ethanol, acetone, ethyl acetate, toluene, and the like.
In the following, 1/5 disperser having a length ratio of the fluid feed pipe to the fluid discharge pipe of 2:1, a diameter ratio of the fluid discharge pipe to the polymer solution feed pipe of 3:1, and a height of the protrusions as an inner diameter of the fluid discharge pipe is exemplified as a few examples of continuous precipitation of solid powder from a polymer solution using a polymer solution solid powder precipitation system.
Example 2
The polymer solution solid powder continuous precipitation is carried out by using the polymer solution solid powder precipitation system with the structure of the embodiment, and the steps are as follows:
injecting a certain amount of deionized water into the liquid storage tank, starting a circulating pump, regulating the flow rate of the water to 1.5m/s, after the flow rate is stable, enabling a polyimide N-methyl pyrrolidone (NMP) solution with the concentration of 25wt% to enter a dispersion mixer through a polymer feed inlet, enabling the flow rate to be 2% of the flow rate of the water, separating materials flowing out of the dispersion mixer through a solid-liquid separator, and enabling the separated mixed liquid of the water and the N-methyl pyrrolidone to enter the liquid storage tank for recycling. And finally, washing and vacuum drying the polyimide particles obtained by separation to obtain the polyimide particles which are uniform, do not agglomerate and do not cake.
Example 3
The procedure of using the polymer solution solid powder precipitation system having the structure described in example to continuously precipitate the solid powder from the polymer solution was the same as in example 2, except that: the concentration of the polyimide N-methylpyrrolidone (NMP) solution was 50 wt%. The obtained polymer particles have uniform particle size, and are not agglomerated or agglomerated.
Example 4
The procedure of using the polymer solution solid powder precipitation system having the structure described in example to continuously precipitate the solid powder from the polymer solution was the same as in example 2, except that: the concentration of the polyimide N-methylpyrrolidone (NMP) solution was 10 wt%. The obtained polymer particles have uniform particle size, and are not agglomerated or agglomerated.
Example 5
The procedure of using the polymer solution solid powder precipitation system having the structure described in example to continuously precipitate the solid powder from the polymer solution was the same as in example 2, except that: the flow rate of water was 3 m/s. The obtained polymer particles have uniform particle size, and are not agglomerated or agglomerated.
Example 6
The procedure of using the polymer solution solid powder precipitation system having the structure described in example to continuously precipitate the solid powder from the polymer solution was the same as in example 2, except that: the flow rate of water was 0.75 m/s. The obtained polymer particles have uniform particle size, and are not agglomerated or agglomerated.
Example 7
The procedure of using the polymer solution solid powder precipitation system having the structure described in example to continuously precipitate the solid powder from the polymer solution was the same as in example 2, except that: the flow rate of water was 4.5 m/s. The obtained polymer particles have uniform particle size, and are not agglomerated or agglomerated.
Example 8
The procedure of using the polymer solution solid powder precipitation system having the structure described in example to continuously precipitate the solid powder from the polymer solution was the same as in example 2, except that: the polymer solution was a 25wt% polyimide N, N-Dimethylacetamide (DMAC) solution. The obtained polymer particles have uniform particle size, and are not agglomerated or agglomerated.
Example 9
The procedure of using the polymer solution solid powder precipitation system having the structure described in example to continuously precipitate the solid powder from the polymer solution was the same as in example 2, except that: the polymer solution was a 25wt% polybenzoxazole N-methylpyrrolidone (NMP) solution. The obtained polymer particles have uniform particle size, and are not agglomerated or agglomerated.
Example 10
The procedure of using the polymer solution solid powder precipitation system having the structure described in example to continuously precipitate the solid powder from the polymer solution was the same as in example 2, except that: the water was replaced with ethanol. The obtained polymer particles have uniform particle size, and are not agglomerated or agglomerated.
Example 11
The procedure of using the polymer solution solid powder precipitation system having the structure described in example to continuously precipitate the solid powder from the polymer solution was the same as in example 2, except that: the polymer solution was a 25wt% polyaniline N-methylpyrrolidone (NMP) solution. The obtained polymer particles have uniform particle size, and are not agglomerated or agglomerated.
Example 12
The procedure of using the polymer solution solid powder precipitation system having the structure described in example to continuously precipitate the solid powder from the polymer solution was the same as in example 2, except that: the polymer solution was a 40wt% solution of polyacrylonitrile in dimethylsulfoxide. The obtained polymer particles have uniform particle size, and are not agglomerated or agglomerated.
Example 13
The procedure of using the polymer solution solid powder precipitation system having the structure described in example to continuously precipitate the solid powder from the polymer solution was the same as in example 2, except that: the polymer solution was a 5wt% polycarbonate in tetrahydrofuran. The obtained polymer particles have uniform particle size, and are not agglomerated or agglomerated.
Example 14
The procedure of using the polymer solution solid powder precipitation system having the structure described in example to continuously precipitate the solid powder from the polymer solution was the same as in example 2, except that: the polymer solution was a 30wt% solution of epoxy resin N-methylpyrrolidone (NMP). The obtained polymer particles have uniform particle size, and are not agglomerated or agglomerated.
Comparative example 1
About 3L of deionized water was poured into a 5L plastic beaker, and a shear grinding head of a high shear grinder (Nantong mixing equipment Co., Ltd., model: ME-100L) was mounted to be completely immersed in the deionized water, and set to a rotation speed of 2000 rpm. 500ml of a 25wt% polyimide N-methylpyrrolidone (NMP) solution was slowly dropped (about 30 min) into the beaker, and then, shearing pulverization was continued for 10 min. And finally, washing and vacuum drying the polyimide particles obtained by separation to obtain the polymer particles. The resulting polymer particles have a non-uniform particle size distribution.
Comparative example 2
About 3L of deionized water was poured into a 5L plastic beaker, and a conventional stirrer was mounted, the propeller being a stainless steel three-blade propeller type, and the propeller being completely immersed in the deionized water at a set rotation speed of 350 rpm. 500ml of a 25wt% polyimide N-methylpyrrolidone (NMP) solution was slowly dropped (about 30 min) into the beaker, and then, shearing pulverization was continued for 10 min. And finally, washing and vacuum drying the polyimide particles obtained by separation to obtain the polymer particles. The polymer particles obtained are in the form of coils with a diameter of about 2.0 mm and a small number of long strips with a length of 0.2-3 cm.
Comparative example 3
The polymer solution was subjected to continuous precipitation of solid powder using the system and method of example 2, except that: the dispersion mixer was replaced with a static mixer, which was manufactured by Tianjin multi-state mixing machine, Inc., and a schematic structural view thereof is shown in FIG. 6. Water and polymer solution respectively enter from a feed inlet on the left side of the static mixer and then flow out from a discharge outlet on the right side of the static mixer, and a stirring device is arranged in the static mixer.
The polymer particles obtained in the above examples and comparative examples were measured for particle size and particle size distribution using a laser particle size distribution measuring apparatus model BT-9300S from Baitt instruments Ltd, and the results are shown in Table 1.
As can be seen from the comparison between the above examples and comparative examples, the invention can realize the continuous precipitation of the polymer, and has the advantages of simple operation, strong mechanization, less time consumption, low energy consumption, uniform particle size distribution of the obtained particles, and suitability for industrial application.
Claims (12)
1. A polymer solution solid powdering and separating device is characterized in that: the dispersing mixer comprises a fluid feeding pipe, a fluid discharging pipe and a polymer solution feeding pipe, wherein the fluid feeding pipe and the fluid discharging pipe are connected together through a connecting part, no angle exists between the fluid feeding pipe and the fluid discharging pipe, the fluid feeding pipe and the fluid discharging pipe are positioned on the same straight line, a feeding port of the polymer solution feeding pipe is arranged on the fluid feeding pipe, and a discharging port of the polymer solution feeding pipe is arranged in the connecting part; the fluid discharge pipe is connected with a liquid inlet of the solid-liquid separator, a liquid outlet of the solid-liquid separator is connected with the liquid storage tank, and the liquid storage tank is connected with the fluid feed pipe through a fluid conveying pipeline;
the connecting part is provided with a through hole which enables the fluid feeding pipe to be communicated with the fluid discharging pipe;
the diameter of the fluid feeding pipe is larger than that of the fluid discharging pipe, and one end of the connecting part connected with the fluid feeding pipe is thicker than that connected with the fluid discharging pipe;
two wing plates are also arranged in the connecting part, the two wing plates are mutually perpendicular and are fixedly arranged at the discharge port of the polymer solution feed pipe;
the inner wall of the discharge pipe is provided with symmetrically distributed bulges.
2. The apparatus for powdering and separating a polymer solution according to claim 1, wherein: the connecting part is horn-shaped.
3. The apparatus for powdering and separating a polymer solution according to claim 1, wherein: the convex shape is mushroom-shaped.
4. The apparatus for powdering and separating a polymer solution solid according to claim 1 or 3, wherein: the height of the integral bulge is 1/5-2/5 of the inner diameter of the fluid discharge pipe.
5. The apparatus for powdering and separating a polymer solution according to claim 1, wherein: the length ratio of the fluid feeding pipe to the fluid discharging pipe is 1-3:1, the diameter ratio of the fluid feeding pipe to the fluid discharging pipe is 1-4:1, and the diameter ratio of the fluid discharging pipe to the polymer solution feeding pipe is 1-4: 1.
6. The apparatus for powdering and separating a polymer solution according to claim 1, wherein: the liquid storage tank is connected with the liquid conveying pipeline through a pipeline.
7. A method for powdering and precipitating a polymer solution, comprising the step of powdering and precipitating a polymer solution in the polymer solution solid-powder precipitation apparatus according to any one of claims 1 to 6, the method comprising:
(1) adding a poor solvent of the polymer into the liquid storage tank, and controlling the poor solvent to enter a fluid feeding pipe of the dispersion mixer through a fluid conveying pipeline according to the flow speed of 0.5-5 m/s;
(2) controlling the polymer solution to enter a dispersion mixer from a polymer solution feeding pipe according to 0.2-2% of the flow rate of the poor solvent;
(3) the polymer solution and the poor polymer solvent form turbulent flow in a connecting part of the dispersing mixer, the polymer is separated out in the contact process of the polymer solution and the poor polymer solvent, and then the mixed material continuously flows out of the fluid discharge pipe and enters a solid-liquid separator;
(4) the polymer is collected after being separated by a solid-liquid separator, and the separated liquid enters a liquid storage tank.
8. The method for powdering and precipitating a solid in a polymer solution according to claim 7, wherein: the polymer solution is a mixture of a polymer and a good solvent therefor.
9. The method for powdering and precipitating a solid in a polymer solution according to claim 7, wherein: the concentration of the polymer solution is 5-50 wt%.
10. The method for powdering and precipitating a solid in a polymer solution according to claim 7, wherein: the polymer is at least one of polyimide, polyamide, polybenzoxazole, polyaniline, polycarbonate, polyacrylonitrile and epoxy resin.
11. The method for powdering and precipitating a solid in a polymer solution according to claim 7, wherein: the good solvent is at least one of N-methyl pyrrolidone, N-dimethylacetamide, tetrahydrofuran and dimethyl sulfoxide.
12. The method for powdering and precipitating a solid in a polymer solution according to claim 7, wherein: the poor solvent is at least one of water, methanol, ethanol, acetone and toluene.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910145891.2A CN109749099B (en) | 2019-02-27 | 2019-02-27 | Solid powder precipitation system and continuous precipitation method for polymer solution |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910145891.2A CN109749099B (en) | 2019-02-27 | 2019-02-27 | Solid powder precipitation system and continuous precipitation method for polymer solution |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN109749099A CN109749099A (en) | 2019-05-14 |
| CN109749099B true CN109749099B (en) | 2022-01-25 |
Family
ID=66406839
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910145891.2A Active CN109749099B (en) | 2019-02-27 | 2019-02-27 | Solid powder precipitation system and continuous precipitation method for polymer solution |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109749099B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110402664A (en) * | 2019-08-29 | 2019-11-05 | 李清川 | A kind of agricultural fertilizer, application powder blower |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004292544A (en) * | 2003-03-26 | 2004-10-21 | Sumitomo Chem Co Ltd | Method for producing polymer particle |
| CN1688632A (en) * | 2002-09-13 | 2005-10-26 | 通用电气公司 | Method and apparatus for preparing a poly(arylene ether) |
| CN101208272A (en) * | 2005-06-20 | 2008-06-25 | 株式会社Ohr实验室 | Ballast water processing device |
| CN101547965A (en) * | 2006-12-05 | 2009-09-30 | Lg化学株式会社 | Apparatus and method for recovering polymer |
| JP2011038024A (en) * | 2009-08-14 | 2011-02-24 | National Institute Of Advanced Industrial Science & Technology | Method for producing polyamic acid fine particle and polyimide fine particle continuously |
| CN102391497A (en) * | 2011-09-13 | 2012-03-28 | 金发科技股份有限公司 | Quickly discharging method for preparing resin |
| CN102838760A (en) * | 2012-08-06 | 2012-12-26 | 清华大学 | Preparation method for polymer nanoparticles |
-
2019
- 2019-02-27 CN CN201910145891.2A patent/CN109749099B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1688632A (en) * | 2002-09-13 | 2005-10-26 | 通用电气公司 | Method and apparatus for preparing a poly(arylene ether) |
| JP2004292544A (en) * | 2003-03-26 | 2004-10-21 | Sumitomo Chem Co Ltd | Method for producing polymer particle |
| CN101208272A (en) * | 2005-06-20 | 2008-06-25 | 株式会社Ohr实验室 | Ballast water processing device |
| CN101547965A (en) * | 2006-12-05 | 2009-09-30 | Lg化学株式会社 | Apparatus and method for recovering polymer |
| JP2011038024A (en) * | 2009-08-14 | 2011-02-24 | National Institute Of Advanced Industrial Science & Technology | Method for producing polyamic acid fine particle and polyimide fine particle continuously |
| CN102391497A (en) * | 2011-09-13 | 2012-03-28 | 金发科技股份有限公司 | Quickly discharging method for preparing resin |
| CN102838760A (en) * | 2012-08-06 | 2012-12-26 | 清华大学 | Preparation method for polymer nanoparticles |
Also Published As
| Publication number | Publication date |
|---|---|
| CN109749099A (en) | 2019-05-14 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JP5632459B2 (en) | Non-adhesion treatment method for polymer pellets and centrifugal dehydrator used in this method | |
| JP2004535930A (en) | Method of producing nanometer-sized powder and nanometer-sized sparsely aggregated powder | |
| CN109749099B (en) | Solid powder precipitation system and continuous precipitation method for polymer solution | |
| US5368385A (en) | Continuous solution method and apparatus | |
| WO2012086328A1 (en) | Emulsification device, polymer particle production apparatus provided with emulsification device, and polymer particle production method using production apparatus | |
| CN102086240A (en) | Equipment and method for producing uniform particle ion exchange resin beads | |
| CN107720916A (en) | A kind of novel rotary waterfall formula blender | |
| CN108392961A (en) | Nano bubble organic waste gas treatment method and system | |
| CN1792421A (en) | Equipment for blending light-wt. dry powder material | |
| CN112142881B (en) | Method for agglomerating ABS grafted latex and device used by same | |
| CN202845300U (en) | Particle screening device of liquid-solid fluid containing solid particles | |
| CN106188313A (en) | The method producing the low-substituted hydroxypropyl cellulose of purification | |
| US4890929A (en) | Method and apparatus for manufacturing coagulated grains from polymer latex | |
| US3055856A (en) | Aqueous suspension of carbon black, apparatus and method for preparing same, method for mixing same with rubber, and product obtained thereby | |
| CN111941681B (en) | Device and method for producing polystyrene uniform balls | |
| KR20150143157A (en) | manufacturing method of polymer particle | |
| JP4252664B2 (en) | Method and apparatus for producing powder coating fine particles | |
| CN110407256B (en) | Production process of nanoscale iron oxide | |
| KR20150051900A (en) | Process for preparing polymer powder | |
| JP2004148174A (en) | Method and apparatus for manufacturing fine particles by using supercritical fluid | |
| JP2011194366A (en) | Method for manufacturing fine particle and apparatus for manufacturing fine particle | |
| WO2001016196A1 (en) | Process for producing polymer particles | |
| CN220328659U (en) | Washing device for polyvinyl butyral resin | |
| JP3470838B2 (en) | Dissolution method of water-soluble polymer powder | |
| CN221085549U (en) | Safe and environment-friendly discharging granulating device for oxidized polyethylene wax oxidation process |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20220718 Address after: 252300 no.369, Qinghe West Road, shizilou office, Yanggu County, Liaocheng City, Shandong Province Patentee after: BOMI TECHNOLOGY Co.,Ltd. Address before: 100083 a-711, 6th floor, building 1, 18 Zhongguancun East Road, Haidian District, Beijing Patentee before: POME SCI-TECH CO.,LTD. Patentee before: BOMI TECHNOLOGY Co.,Ltd. |
|
| TR01 | Transfer of patent right |