Preparation device and preparation method of polystyrene microspheres

Abstract

The invention relates to a preparation device and a preparation method of polystyrene microspheres. The preparation device comprises an oil drop dispersing device and a curing device, the oil drop dispersing device comprises a shell, and a perforated plate and a vibration assembly which are arranged in the shell; the shell is divided into a water phase section and an oil phase section by the porous plate; the water phase section is provided with a water phase inlet; a material outlet is formed in the upper part of the water phase section; the oil drop dispersing device is connected with the curing device through the material outlet; the oil phase section is provided with an oil phase inlet; an oil phase conveying assembly is arranged in the oil phase section; the vibration assembly is arranged at the bottom of the oil drop dispersing device; the vibration assembly is connected with the oil phase conveying assembly through a lead screw. The preparation device and method provided by the invention are simple in process and convenient for industrial large-scale production, and the prepared polymer microspheres are narrower in particle size distribution and high in product percent of pass, and can be widely applied to the field of preparation of polystyrene, acrylate, methyl methacrylate and other microspheres.

Description

Technical Field

[0001] The present invention relates to the technical fields of chemical engineering and medicine, and particularly relates to a preparation device for polystyrene microspheres and a preparation method thereof. Background Art

[0002] Polymer microspheres, such as polystyrene, acrylate, methacrylate, etc., are all prepared by suspension polymerization: the monomers are dispersed into droplets through a nozzle and then added to a stirred tank containing a dispersant, and the dispersed monomer droplets are then polymerized and solidified in the stirred tank to obtain polymer microspheres.

[0003] Although the traditional suspension polymerization technology for preparing polymer microspheres has a simple process, the particle size distribution of the prepared polymer microspheres is relatively wide. To meet the requirements of narrow particle size distribution in industry, it is necessary to screen the prepared polymer microspheres, and only 30-50% of the qualified products can be obtained, resulting in a significant increase in the production cost of polymer microspheres.

[0004] To prepare polymer microspheres with a narrow particle size distribution, relevant explorations have been carried out by those skilled in the art. For example, CN119039535A discloses a large-particle-size magnetic polystyrene microsphere and its preparation method and application. Using magnetic Fe3O4 particles as the magnetic core, a large amount of initiator and monomer are adsorbed on its surface, and under the action of mechanical stirring and a dispersant or suspending agent, they are dispersed into tiny droplets, becoming the center of initiating polymerization. The monomers polymerize with each other, and the polymer molecular chains wind around the magnetic core and are solidified later to form magnetic microspheres. The particle size of the prepared magnetic polystyrene microspheres is 30 μm to 60 μm. This preparation method is simple, time-consuming, and the prepared microspheres have good dispersibility, but due to the need to use Fe3O4 particles as the magnetic core, the production cost is relatively high.

[0005] CN115536768A discloses a preparation method for large-particle-size polystyrene microspheres. A surfactant is dissolved in deionized water to form a continuous phase; analytical pure styrene is added with an oil-soluble initiator and uniformly mixed to form a dispersed phase; the aqueous phase and the oil phase containing the initiator are introduced into a focused microfluidic chip to shear to obtain styrene microspheres; the styrene microspheres are transferred into a four-necked reactor equipped with a condenser, a stirrer, and a nitrogen conduit, and after purging oxygen with nitrogen, a polymerization reaction is carried out; after the polymerization is completed, the polystyrene microspheres with uniform size are obtained after washing and vacuum drying. The prepared micron-sized polystyrene spheres have good monodispersity and large size, and the particle size is between 20 and 500 μm. However, due to the small processing capacity of the preparation device, it is difficult to be applied to the large-scale production of polystyrene microspheres.

[0006] CN212445911U discloses a device for producing polystyrene uniform spheres, which comprises a pre-polymerization kettle, a uniform particle device, a granulation tower, a centrifuge and a curing kettle connected in sequence. In the styrene pre-polymerization kettle, a bulk self-polymerization reaction is carried out under the action of additive A to obtain a primary reaction product; the primary product enters the uniform particle device to generate polystyrene oil droplets with a specific particle size. After the oil droplets are wrapped by dispersant A and then mixed with dispersant B, they are sent into the granulation tower together to continue the self-polymerization reaction to generate polystyrene particles. The product is centrifuged to obtain polystyrene particles, and the polystyrene particles enter the curing kettle for curing reaction until the reaction ends to obtain polystyrene uniform spheres. By changing the diameter of the jet holes, this device can prepare polystyrene uniform spheres with any particle size from microns to millimeters. However, since this granulation device requires a large number of high-precision jet needles and the cost is very high, it cannot be widely promoted and applied on a large scale.

[0007] Although those skilled in the art have reduced the particle size distribution of polystyrene microspheres through various means, its particle size distribution is still relatively wide. Problems such as the low qualified rate of the product after screening and the high cost of the device and equipment make the production cost of narrow particle size distribution polystyrene microspheres still remain high. Therefore, there is an urgent need for a new device and method for preparing polystyrene microspheres to reduce the preparation cost and facilitate large-scale production. Summary of the Invention

[0008] To solve the above technical problems, the present invention provides a device for preparing polystyrene microspheres and a preparation method thereof. The preparation device of the present invention can evenly disperse the oil-phase material into the water-phase material by setting a porous plate, an oil-phase conveying component and a vibration component, which is beneficial to the subsequent preparation of narrow particle size distribution polystyrene microspheres; at the same time, the preparation method is simple, convenient for large-scale industrial production, the prepared polymer microspheres have a narrower particle size distribution, higher sphericity and a high qualified rate of the product.

[0009] To achieve this purpose, the present invention adopts the following technical solutions:

[0010] In the first aspect, the present invention provides a device for preparing polystyrene microspheres, and the preparation device comprises an oil droplet dispersion device and a curing device; the oil droplet dispersion device comprises a shell, a porous plate arranged inside the shell and a vibration component;

[0011] The porous plate divides the shell into a water-phase section and an oil-phase section; the water-phase section is provided with a water-phase inlet; the upper part of the water-phase section is provided with a material outlet; the oil droplet dispersion device is connected to the curing device through the material outlet;

[0012] The oil-phase section is provided with an oil-phase inlet; an oil-phase conveying component is arranged inside the oil-phase section; the vibration component is arranged at the bottom of the oil droplet dispersion device; the vibration component is connected to the oil-phase conveying component through a lead screw.

[0013] The preparation device of the present invention can control the time for the oil-phase material to pass through the porous plate and form droplets by setting the porous plate, the oil-phase delivery component and the vibration component, thereby controlling the particle size of the polystyrene microspheres.

[0014] As a preferred technical solution of the present invention, the pore diameter of the porous plate is 0.1-10 mm, such as 0.1 mm, 0.5 mm, 1 mm, 2 mm, 4 mm, 6 mm, 8 mm, 10 mm, etc., but not limited to the listed values, and other unlisted values within the above value range are equally applicable.

[0015] The thickness of the porous plate is 0.5-20 mm, such as 0.5 mm, 1 mm, 2 mm, 4 mm, 6 mm, 8 mm, 10 mm, 15 mm, 20 mm, etc., but not limited to the listed values, and other unlisted values within the above value range are equally applicable.

[0016] In the present invention, by limiting the thickness and pore diameter of the porous plate, the particle size of the polystyrene microspheres can be regulated, so that the prepared polystyrene microspheres have good sphericity, a narrow particle size distribution, and a high product qualification rate.

[0017] Preferably, the pore channel shape of the porous plate includes one of cylindrical, frustum-shaped or rectangular.

[0018] As a preferred technical solution of the present invention, a heat preservation device is provided outside the housing.

[0019] Preferably, the vibration component is connected to a driving device.

[0020] Preferably, the porous plate is fixed inside the housing by fasteners.

[0021] Preferably, a support frame is further provided outside the oil droplet dispersion device to fix the oil droplet dispersion device.

[0022] As a preferred technical solution of the present invention, the preparation device further includes an aqueous phase mixing device, an oil phase mixing device, a filtering and washing device, and a drying device;

[0023] The aqueous phase mixing device is connected to the aqueous phase inlet through a plunger pump; the oil phase mixing device is connected to the oil phase inlet through a plunger pump;

[0024] The material outlet of the curing device is connected to the filtering and washing device; the material outlet of the filtering and washing device is connected to the drying device.

[0025] In a second aspect, the present invention provides a method for preparing polystyrene microspheres, and the preparation method is carried out by using the preparation device as described in the first aspect.

[0026] The preparation method includes: the aqueous phase material enters the aqueous phase section through the aqueous phase inlet; the oil phase material enters the oil phase section through the oil phase inlet;

[0027] The oil phase material passes through the porous plate and enters the aqueous phase section under the action of the oil phase conveying assembly and the vibration assembly for pre-curing treatment; the pre-cured oil particles enter the curing device through the material outlet for curing treatment to obtain polystyrene particles; after post-treatment of the polystyrene particles, the polystyrene microspheres are obtained.

[0028] It should be noted that in the present invention, the oil phase conveying assembly conveys the oil phase material into the porous plate by upward movement, and at the same time, through the vibration action of the vibration assembly, promotes the removal of the oil phase material from the porous plate to form uniformly dispersed oil droplets in the aqueous phase material.

[0029] As a preferred technical solution of the present invention, the aqueous phase material includes a dispersant; the dispersant includes any one or at least two combinations of gelatin, polyvinyl alcohol, hydroxyethyl cellulose, calcium phosphate or magnesium carbonate; typical but non-limiting examples of the combination are: the combination of gelatin and polyvinyl alcohol, the combination of polyvinyl alcohol and hydroxyethyl cellulose, the combination of hydroxyethyl cellulose and calcium phosphate, the combination of calcium phosphate and magnesium carbonate, etc.

[0030] Preferably, the oil phase material includes styrene monomer and an initiator; the initiator includes any one or at least two combinations of lauroyl peroxide, benzoyl peroxide, diisopropyl peroxydicarbonate, azobisisobutyronitrile, potassium persulfate or ammonium persulfate; typical but non-limiting examples of the combination are: the combination of lauroyl peroxide and benzoyl peroxide, the combination of benzoyl peroxide and diisopropyl peroxydicarbonate, the combination of diisopropyl peroxydicarbonate and azobisisobutyronitrile, the combination of azobisisobutyronitrile and potassium persulfate, the combination of potassium persulfate and ammonium persulfate, etc.

[0031] As a preferred technical solution of the present invention, the temperature of the aqueous phase material is 40-100°C, such as 40°C, 50°C, 60°C, 70°C, 80°C, 90°C, 100°C, etc., but is not limited to the listed values, and other unlisted values within the above numerical range are equally applicable.

[0032] The temperature of the oil phase material is 10-60°C, such as 10°C, 20°C, 30°C, 40°C, 50°C, 60°C, etc., but is not limited to the listed values, and other unlisted values within the above numerical range are equally applicable.

[0033] Preferably, the flow rate of the oil-phase material through the porous plate is 5 - 60 mL / s, such as 5 mL / s, 10 mL / s, 20 mL / s, 30 mL / s, 40 mL / s, 50 mL / s, 60 mL / s, etc., but not limited to the listed values, and other unlisted values within the above numerical range are equally applicable.

[0034] Preferably, the vibration frequency of the vibration assembly is 10 - 600 Hz, such as 10 Hz, 50 Hz, 100 Hz, 200 Hz, 300 Hz, 400 Hz, 500 Hz, 600 Hz, etc., but not limited to the listed values, and other unlisted values within the above numerical range are equally applicable.

[0035] In the present invention, by limiting the flow rate of the oil-phase material through the porous plate and the vibration frequency of the vibration assembly, polystyrene microspheres with a narrow particle size distribution can be prepared, and the product qualification rate is high.

[0036] As a preferred technical solution of the present invention, the curing treatment specifically includes: the pre-cured oil particles enter the curing device through the material outlet and continue to carry out a polymerization reaction under the action of stirring to form polystyrene particles.

[0037] Preferably, the rotation speed of the stirring is 20 - 400 rpm, such as 20 rpm, 50 rpm, 100 rpm, 200 rpm, 300 rpm, 400 rpm, etc., but not limited to the listed values, and other unlisted values within the above numerical range are equally applicable.

[0038] The temperature of the polymerization reaction is 50 - 100 °C, such as 50 °C, 60 °C, 70 °C, 80 °C, 90 °C, 100 °C, etc., but not limited to the listed values, and other unlisted values within the above numerical range are equally applicable.

[0039] As a preferred technical solution of the present invention, the post-treatment process includes: the polystyrene particles enter the filtration and washing device for filtration and washing treatment; then enter the drying device, and after drying treatment, the polystyrene microspheres are obtained.

[0040] Compared with the prior art, the present invention has at least the following beneficial effects:

[0041] The preparation device of the present invention can effectively control the particle size of polystyrene microspheres by regulating the pore size and thickness of the porous plate, the flow rate of the oil-phase material, and the frequency of the vibration assembly, thereby preparing polymer microspheres with a narrow particle size distribution, good sphericity, and high product qualification rate; the preparation method of the present invention has a simple process, low cost, and high product qualification rate, and can be widely used in the preparation fields of microspheres such as polystyrene, acrylate, and methyl methacrylate. Description of the Drawings

[0042] Figure 1 It is a schematic diagram of a device for preparing polystyrene microspheres provided by the present invention.

[0043] Figure 2 It is a front view of an oil droplet dispersion device provided by the present invention.

[0044] Figure 3 It is a sectional view of an oil droplet dispersion device provided by the present invention.

[0045] Figure 4 It is a top view of a porous plate provided by the present invention.

[0046] Among them: 1 - aqueous phase mixing device (pure water and dispersant); 2 - oil phase mixing device (monomer and initiator); 3 - oil droplet dispersion device; 4 - curing device; 5 - filtration and washing device; 6 - drying device; 7 - aqueous phase section; 8 - porous plate; 9 - oil phase conveying component; 10 - heat preservation device; 11 - oil phase section; 12 - vibration component; 13 - support frame; 14 - driving device; 15 - fastener; 16 - lead screw. Specific embodiments

[0047] The technical solution of the present invention will be further described below in conjunction with the drawings and specific embodiments. However, the following examples are only simple examples of the present invention and do not represent or limit the scope of the claimed rights of the present invention. The scope of protection of the present invention shall be subject to the claims.

[0048] In the following application examples, the particle size of the prepared polystyrene microspheres was analyzed by a Malvern particle size analyzer Mastersizer 3000.

[0049] Example 1

[0050] This example provides a device for preparing polystyrene microspheres. The schematic diagram of the device is as Figure 1 shown. The preparation device includes an oil droplet dispersion device 3 and a curing device 4; the oil droplet dispersion device 3 includes a housing, a porous plate 8 arranged inside the housing, and a vibration component 12; the front view and sectional view of the oil droplet dispersion device are as Figure 2 and Figure 3 shown.

[0051] The porous plate 8 divides the housing into an aqueous phase section 7 and an oil phase section 11; Figure 4 is the top view of the porous plate; the aqueous phase section 7 is provided with an aqueous phase inlet; a material outlet is arranged above the aqueous phase inlet; the oil droplet dispersion device 3 is connected to the curing device 4 through the material outlet; the oil phase section 11 is provided with an oil phase inlet; an oil phase conveying component 9 is arranged inside the oil phase section 11; the vibration component 12 is arranged at the bottom of the oil droplet dispersion device 3;

[0052] The pore diameter of the porous plate is 0.3 mm; the thickness of the porous plate is 8 mm; a heat preservation device 10 is arranged outside the shell; the vibration assembly 12 is connected to the driving device 14; the vibration assembly 12 is connected to the oil phase delivery assembly 9 through a lead screw 16;

[0053] The preparation device further includes an aqueous phase mixing device 1, an oil phase mixing device 2, a filtering and washing device 5, and a drying device 6; the aqueous phase mixing device 1 is connected to the aqueous phase inlet through a plunger pump; the oil phase mixing device 2 is connected to the oil phase inlet through a plunger pump; the material outlet of the curing device 4 is connected to the filtering and washing device 5; the material outlet of the filtering and washing device 5 is connected to the drying device 6.

[0054] Example 2

[0055] This example provides a preparation device for polystyrene microspheres. The difference from Example 1 is that the thickness of the porous plate is 6 mm, and the rest are the same as those in Example 1.

[0056] Example 3

[0057] This example provides a preparation device for polystyrene microspheres. The difference from Example 1 is that the pore diameter of the porous plate is 0.4 mm, and the rest are the same as those in Example 1.

[0058] Example 4

[0059] This example provides a preparation device for polystyrene microspheres. The difference from Example 2 is that the pore diameter of the porous plate is 1 mm, and the rest are the same as those in Example 1.

[0060] Example 5

[0061] This example provides a preparation device for polystyrene microspheres. The difference from Example 1 is that the pore diameter of the porous plate is 2 mm, and the rest are the same as those in Example 1.

[0062] Example 6

[0063] This example provides a preparation device for polystyrene microspheres. The difference from Example 1 is that the pore diameter of the porous plate is 10 mm, and the rest are the same as those in Example 1.

[0064] Example 7

[0065] This example provides a preparation device for polystyrene microspheres. The difference from Example 1 is that the thickness of the porous plate is 1 mm, and the rest are the same as those in Example 1.

[0066] Example 8

[0067] This embodiment provides a preparation device for polystyrene microspheres. The difference from Embodiment 1 is that the thickness of the porous plate is 20 mm, and the rest is the same as that of Embodiment 1.

[0068] Comparative Example 1

[0069] This comparative example provides a preparation device for polystyrene microspheres. The difference from Embodiment 1 is that the vibration assembly is omitted, and the oil-phase material is only transported by the oil-phase transportation assembly, and the rest is the same as that of Embodiment 1.

[0070] Comparative Example 2

[0071] This comparative example provides a preparation device for polystyrene microspheres, which adopts the traditional stirring suspension polymerization technology. The reactor of the preparation device is a glass reaction kettle with a paddle stirrer, and a water bath temperature control system is set.

[0072] Application Example 1

[0073] This application example provides a preparation method for polystyrene microspheres, and the preparation method is carried out by using the preparation device described in Embodiment 1.

[0074] The preparation method includes: the aqueous-phase material enters the aqueous-phase section through the aqueous-phase inlet; the oil-phase material enters the oil-phase section through the oil-phase inlet; the oil-phase material passes through the porous plate under the action of the oil-phase transportation assembly and the vibration assembly and enters the aqueous-phase section for pre-curing treatment; the pre-cured oil particles enter the curing device through the material outlet, and after stirring, a polymerization reaction is carried out to form polystyrene particles; the rotation speed of the stirring is 200 rpm; the temperature of the polymerization reaction is 90 °C;

[0075] The polystyrene particles enter the filtration and washing device for filtration and washing treatment; then enter the drying device, and after drying treatment, the polystyrene microspheres are obtained;

[0076] The aqueous-phase material is deionized water and hydroxyethyl cellulose (concentration: 0.01 g / mL); the temperature of the aqueous-phase material is 70 °C; the oil-phase material is styrene and lauroyl peroxide (concentration: 0.06 g / mL); the temperature of the oil-phase material is 60 °C; the flow rate of the oil-phase material passing through the porous plate is 20 mL / s; the vibration frequency of the vibration assembly is 100 Hz.

[0077] The results show that the particle size of the polystyrene microspheres is mainly distributed between 0.7 and 1.1 mm, and the qualified microsphere products with a particle size of 0.8 - 0.85 mm can reach 95.1%.

[0078] Application Example 2

[0079] This application example provides a method for preparing polystyrene microspheres. The preparation method is carried out using the preparation device described in Example 1. The difference from Application Example 1 is only that the flow rate of the oil-phase material passing through the porous plate is adjusted to 30 mL / s, and the other conditions are the same as those in Application Example 1.

[0080] The results show that the particle size of the polystyrene microspheres is mainly distributed between 0.65 and 0.9 mm, and the qualified microsphere products with a particle size of 0.8 - 0.85 mm can reach 96.7%.

[0081] Application Example 3

[0082] This application example provides a method for preparing polystyrene microspheres. The preparation method is carried out using the preparation device described in Example 1. The difference from Application Example 1 is only that the flow rate of the oil-phase material passing through the porous plate is adjusted to 40 mL / s, and the other conditions are the same as those in Application Example 1.

[0083] The results show that the particle size of the polystyrene microspheres is mainly distributed between 0.6 and 0.9 mm, and the qualified microsphere products with a particle size of 0.8 - 0.85 mm can reach 97.1%.

[0084] Application Example 4

[0085] This application example provides a method for preparing polystyrene microspheres. The preparation method is carried out using the preparation device described in Example 2, and the other conditions are the same as those in Application Example 1.

[0086] The results show that the particle size of the polystyrene microspheres is mainly distributed between 0.45 and 0.9 mm, and the qualified microsphere products with a particle size of 0.8 - 0.85 mm can reach 98.2%.

[0087] Application Example 5

[0088] This application example provides a method for preparing polystyrene microspheres. The preparation method is carried out using the preparation device described in Example 3. The difference from Application Example 1 is that the flow rate of the oil-phase material passing through the porous plate is adjusted to 50 mL / s, and the other conditions are the same as those in Application Example 1.

[0089] The results show that the particle size of the polystyrene microspheres is mainly distributed between 0.65 and 0.95 mm, and the qualified microsphere products with a particle size of 0.8 - 0.85 mm can reach 98.5%.

[0090] Application Example 6

[0091] This application example provides a method for preparing polystyrene microspheres. The preparation method is carried out using the preparation device described in Example 4, and the other conditions are the same as those in Application Example 1.

[0092] The results show that the particle size of the polystyrene microspheres is mainly distributed between 2.2 and 2.8 mm, and 95.7% of the qualified microsphere products have a particle size between 2.45 and 2.55 mm.

[0093] Application Example 7

[0094] This application example provides a method for preparing polystyrene microspheres. The preparation method is carried out using the preparation device described in Example 5, and the remaining conditions are the same as those in Application Example 1.

[0095] The results show that the particle size of the polystyrene microspheres is mainly distributed between 2.7 and 3.3 mm, and 97.5% of the qualified microsphere products have a particle size between 3.0 and 3.1 mm.

[0096] Application Example 8

[0097] This application example provides a method for preparing polystyrene microspheres. The preparation method is carried out using the preparation device described in Example 6, and the remaining conditions are the same as those in Application Example 1.

[0098] The results show that the particle size of the polystyrene microspheres is mainly distributed between 11.9 and 13.6 mm, and 95.3% of the qualified microsphere products have a particle size between 12.5 and 13.0 mm.

[0099] Application Example 9

[0100] This application example provides a method for preparing polystyrene microspheres. The preparation method is carried out using the preparation device described in Example 7, and the remaining conditions are the same as those in Application Example 1.

[0101] The results show that the particle size of the polystyrene microspheres is mainly distributed between 0.1 and 2.1 mm, and 94.5% of the qualified microsphere products have a particle size between 0.8 and 0.85 mm.

[0102] Application Example 10

[0103] This application example provides a method for preparing polystyrene microspheres. The preparation method is carried out using the preparation device described in Example 8, and the remaining conditions are the same as those in Application Example 1.

[0104] The results show that the particle size of the polystyrene microspheres is mainly distributed between 0.12 and 2 mm, and 96.7% of the qualified microsphere products have a particle size between 0.8 and 0.85 mm.

[0105] Application Example 11

[0106] This application example provides a method for preparing polystyrene microspheres. The preparation method is carried out using the preparation device described in Example 1. The difference from Application Example 1 is that the flow rate of the oil-phase material passing through the porous plate is adjusted to 4 mL / s, and the remaining conditions are the same as those in Application Example 1.

[0107] The results show that the particle size of the polystyrene microspheres is mainly distributed between 0.1 and 2.2 mm, and 92.8% of the qualified microsphere products have a particle size between 0.8 and 0.85 mm.

[0108] Application Example 12

[0109] This application example provides a method for preparing polystyrene microspheres. The preparation method is carried out using the preparation device described in Example 1. The difference from Application Example 1 is that the flow rate of the oil-phase material passing through the porous plate is adjusted to 65 mL / s, and the other conditions are the same as those in Application Example 1.

[0110] The results show that the particle size of the polystyrene microspheres is mainly distributed between 0.18 and 2 mm, and 96.5% of the qualified microsphere products have a particle size between 0.8 and 0.85 mm.

[0111] Application Example 13

[0112] This application example provides a method for preparing polystyrene microspheres. The preparation method is carried out using the preparation device described in Example 1. The difference from Application Example 1 is that the vibration frequency of the vibration component is 5 Hz, and the other conditions are the same as those in Application Example 1.

[0113] The results show that the particle size of the polystyrene microspheres is mainly distributed between 0.11 and 2.2 mm, and 93.8% of the qualified microsphere products have a particle size between 0.8 and 0.85 mm.

[0114] Application Example 14

[0115] This application example provides a method for preparing polystyrene microspheres. The preparation method is carried out using the preparation device described in Example 1. The difference from Application Example 1 is that the vibration frequency of the vibration component is 600 Hz, and the other conditions are the same as those in Application Example 1.

[0116] The results show that the particle size of the polystyrene microspheres is mainly distributed between 0.18 and 1.5 mm, and 97.9% of the qualified microsphere products have a particle size between 0.8 and 0.85 mm.

[0117] Comparative Application Example 1

[0118] This comparative application example provides a method for preparing polystyrene microspheres. The preparation method is carried out using the preparation device described in Comparative Example 1, and the other conditions are the same as those in Application Example 1.

[0119] The results show that the particle size of the polystyrene microspheres is mainly distributed between 0.1 and 2 mm, and 78.4% of the qualified microsphere products have a particle size between 0.8 and 0.85 mm.

[0120] Comparative Application Example 2

[0121] This comparative application example provides a method for preparing polystyrene microspheres. The preparation method is carried out using the preparation device described in Comparative Example 2. An aqueous phase material is added to the reactor, and stirring is started. Subsequently, an oil phase material is added, and stirring is continued until a uniform suspension of droplets is formed; the temperature is raised to carry out a polymerization reaction. The stirring speed of the polymerization reaction is 300 rpm, and the other conditions are the same as those in Application Example 1.

[0122] The results show that the particle size of the polystyrene microspheres is mainly distributed between 0.1 and 2 mm, and among them, the qualified microsphere products with a particle size of 0.8 - 0.85 mm are 16.6%.

[0123] Comparative Application Example 3

[0124] This comparative application example provides a method for preparing polystyrene microspheres. The preparation method is carried out using the preparation device described in Comparative Example 2. The stirring speed of the polymerization reaction is adjusted to 400 rpm, and the other conditions are the same as those in Application Example 1.

[0125] The results show that the particle size of the polystyrene microspheres is mainly distributed between 0.1 and 2 mm, and among them, the qualified microsphere products with a particle size of 0.8 - 0.85 mm are 30.2%.

[0126] Summary of Performance Tests

[0127] The particle size distributions of the polystyrene microspheres prepared in Test Application Examples 1 - 14 and Comparative Application Examples 1 - 3 were tested. Among them, the proportion of qualified microspheres is shown in Table 1.

[0128] Table 1

[0129] Proportion of qualified microspheres Application Example 1 The proportion of qualified microspheres with a particle size distribution of 0.8 - 0.85 mm is 95.1% Application Example 2 The proportion of qualified microspheres with a particle size distribution of 0.8 - 0.85 mm is 96.7% Application Example 3 The proportion of qualified microspheres with a particle size distribution of 0.8 - 0.85 mm is 97.1% Application Example 4 The proportion of qualified microspheres with a particle size distribution of 0.8 - 0.85 mm is 98.2% Application Example 5 The proportion of qualified microspheres with a particle size distribution of 0.8 - 0.85 mm is 98.5% Application Example 6 The proportion of qualified microspheres with a particle size distribution of 2.45 - 2.55 mm is 95.7% Application Example 7 The proportion of qualified microspheres with a particle size distribution of 3.0 - 3.1 mm is 97.5% Application Example 8 The proportion of qualified microspheres with a particle size distribution of 12.5 - 13.0 mm is 95.3% Application Example 9 The proportion of qualified microspheres with a particle size distribution of 0.8 - 0.85 mm is 94.5% Application Example 10 The proportion of qualified microspheres with a particle size distribution of 0.8 - 0.85 mm is 96.7% Application Example 11 The proportion of qualified microspheres with a particle size distribution of 0.8 - 0.85 mm is 92.8% Application Example 12 The proportion of qualified microspheres with a particle size distribution of 0.8 - 0.85 mm is 96.5% Application Example 13 The proportion of qualified microspheres with a particle size distribution of 0.8 - 0.85 mm is 93.8% Application Example 14 The proportion of qualified microspheres with a particle size distribution of 0.8 - 0.85 mm is 97.9% Comparative Application Example 1 The proportion of qualified microspheres with a particle size distribution of 0.8 - 0.85 mm is 78.4% Comparative Application Example 2 The proportion of qualified microspheres with a particle size distribution of 0.8 - 0.85 mm is 16.6% Comparative Application Example 3 The proportion of qualified microspheres with a particle size distribution of 0.8 - 0.85 mm is 30.2%

[0130] It can be seen from the test results that:

[0131] (1) It can be seen from Application Examples 1 - 5 that the preparation device and preparation method of the present invention can prepare polystyrene microspheres with a narrow particle size distribution of 0.8 - 0.85 mm, and the qualified rate of the products can reach more than 95%.

[0132] (2) By comparing Application Example 1 with Application Examples 6 - 8, it can be seen that the preparation device of the present invention can prepare polystyrene microspheres with different particle sizes and a qualified rate exceeding 95% by limiting the pore diameter of the porous plate.

[0133] (3) By comparing Application Example 1 with Application Examples 9 - 10, it can be seen that the preparation device of the present invention can control the residence time of the oil phase material on the porous plate by limiting the thickness of the porous plate, and thus control the particle size of the polystyrene microspheres, and improve the proportion of qualified microspheres with a particle size of 0.8 - 0.85 mm.

[0134] (4) It can be seen from the comparison between Application Example 1 and Application Examples 11-12 that by limiting the flow rate of the oil-phase material passing through the porous plate in the preparation method of the present invention, the particle size of the polystyrene microspheres can be regulated, and the proportion of qualified microspheres with a particle size distribution of 0.8-0.85 mm is increased.

[0135] (5) It can be seen from the comparison between Application Example 1 and Application Examples 13-14 that by limiting the vibration frequency of the vibration component in the preparation method of the present invention, the residence time of the oil-phase material on the porous plate is regulated, and further the particle size of the polystyrene microspheres is regulated, and the proportion of qualified microspheres with a particle size distribution of 0.8-0.85 mm is increased.

[0136] (6) It can be seen from the comparison between Application Example 1 and Comparative Application Example 1 that in Comparative Application Example 1, the vibration component is omitted, and the oil-phase material is only transported by the oil-phase transport component, which prolongs the residence time of the oil-phase material on the porous plate, makes the particle size of the polystyrene microspheres larger, and thus causes the proportion of qualified microspheres with a particle size distribution of 0.8-0.85 mm to decrease.

[0137] (7) It can be seen from the comparison between Application Example 1 and Comparative Application Examples 2-3 that in Comparative Application Examples 2-3, the traditional stirring suspension polymerization technology is adopted, the oil-phase material is added to the water-phase material at a certain flow rate, and the oil droplets are evenly dispersed by stirring, and the particle size distribution of the prepared microspheres is larger, and the proportion of qualified microspheres with a particle size distribution of 0.8-0.85 mm is reduced.

[0138] In summary, the present invention provides a preparation device and a preparation method for polystyrene microspheres. Through the setting of the porous plate, the oil-phase transport component and the vibration component, the particle size of the polystyrene microspheres can be effectively regulated. At the same time, by limiting the flow rate of the oil-phase material passing through the porous plate and the vibration frequency, the particle size of the polystyrene microspheres can be further controlled, so as to prepare polystyrene microspheres with a narrow particle size distribution, high sphericity and high product qualification rate. Moreover, the preparation method is simple and suitable for large-scale production.

[0139] The applicant declares that the above description is only the specific implementation manner of the present invention, but the protection scope of the present invention is not limited thereto. Those skilled in the art should understand that any changes or substitutions that can be easily thought of by any person skilled in the art within the technical scope disclosed by the present invention fall within the protection scope and the disclosure scope of the present invention.

Claims

1. A preparation device for polystyrene microspheres, characterized in that, The preparation device includes an oil droplet dispersion device and a curing device; the oil droplet dispersion device includes a housing, a porous plate disposed inside the housing, and a vibration assembly; The porous plate divides the housing into an aqueous phase section and an oil phase section; the aqueous phase section is provided with an aqueous phase inlet; the upper part of the aqueous phase section is provided with a material outlet; the oil droplet dispersion device is connected to the curing device through the material outlet; The oil phase section is provided with an oil phase inlet; an oil phase conveying assembly is disposed inside the oil phase section; the vibration assembly is disposed at the bottom of the oil droplet dispersion device; the vibration assembly is connected to the oil phase conveying assembly through a lead screw.

2. The preparation device according to claim 1, wherein The pore diameter of the porous plate is 0.1 - 10 mm; the thickness of the porous plate is 0.5 - 20 mm.

3. The preparation device according to claim 1 or 2, characterized in that, A heat preservation device is disposed outside the housing; Preferably, the vibration assembly is connected to a driving device; Preferably, the porous plate is fixed inside the housing through a fastener; Preferably, a support frame is further disposed outside the oil droplet dispersion device for fixing the oil droplet dispersion device.

4. The preparation device according to any one of claims 1-3, characterized in that, The preparation device further includes an aqueous phase mixing device, an oil phase mixing device, a filtration and washing device, and a drying device; The aqueous phase mixing device is connected to the aqueous phase inlet through a plunger pump; the oil phase mixing device is connected to the oil phase inlet through a plunger pump; The material outlet of the curing device is connected to the filtration and washing device; The material outlet of the filtration and washing device is connected to the drying device.

5. A method for preparing polystyrene microspheres, characterized in that, The preparation method is carried out using the preparation device according to any one of claims 1 - 4.

6. The preparation method according to claim 5, characterized in that, The preparation method includes: the aqueous phase material enters the aqueous phase section through the aqueous phase inlet; the oil phase material enters the oil phase section through the oil phase inlet; The oil phase material passes through the porous plate under the action of the oil phase conveying assembly and the vibration assembly and enters the aqueous phase section for pre - curing treatment; the pre - cured oil particles enter the curing device through the material outlet for curing treatment to obtain polystyrene particles; after post - treatment of the polystyrene particles, the polystyrene microspheres are obtained.

7. The preparation method according to claim 5 or 6, characterized in that The aqueous phase material includes a dispersant; the dispersant includes any one or a combination of at least two of gelatin, polyvinyl alcohol, hydroxyethyl cellulose, calcium phosphate, or magnesium carbonate; Preferably, the oil phase material includes styrene monomer and an initiator; the initiator includes any one or a combination of at least two of lauroyl peroxide, benzoyl peroxide, diisopropyl peroxydicarbonate, azobisisobutyronitrile, potassium persulfate, or ammonium persulfate.

8. The preparation method according to any one of claims 5 to 7, characterized in that, The temperature of the aqueous phase material is 40 - 100 °C; the temperature of the oil phase material is 10 - 60 °C; Preferably, the flow rate of the oil phase material passing through the porous plate is 5 - 60 mL / s; Preferably, the vibration frequency of the vibration assembly is 10 - 600 Hz.

9. The preparation method according to any one of claims 5-8, characterized in that, The curing treatment specifically includes: the pre - cured oil particles enter the curing device through the material outlet and continue to carry out a polymerization reaction under stirring to form polystyrene particles; Preferably, the rotation speed of the stirring is 20 - 400 rpm; the temperature of the polymerization reaction is 50 - 100 °C.

10. The preparation method according to any one of claims 5-9, characterized in that, The post-treatment process includes: the polystyrene particles enter the filtration and washing device for filtration and washing treatment; then enter the drying device, and after drying treatment, the polystyrene microspheres are obtained.

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