SIBS Swirling Flow Dynamic Blending Method and Device

By using multiple small cyclone dynamic blending tanks in the SIBS preparation process, the problems of high cost and low blending efficiency of traditional blending and mixing tank devices are solved, and high-quality and efficient glue blending is achieved.

CN116003714BActive Publication Date: 2025-06-13HENGHE MATERIALS & SCI TECH CO LTD +1
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Patent Information

Application Number
CN202211722893.1
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2022-12-30
Publication Date
2025-06-13
Estimated Expiration
2042-12-30

AI Technical Summary

Technical Problem

In the traditional SIBS preparation process, the blending and stirring tank device is costly and covers a large area, and the stirring process does not have obvious effect on the vertical surface blending, resulting in low blending efficiency.

Method used

Multiple small cyclone dynamic blending tanks are used instead of large stirring tanks, and the spiral motion blending of the glue liquid is achieved through the cyclone field force, which improves the vertical surface force and improves the blending quality and efficiency.

Benefits of technology

The blending quality and efficiency are improved, the device cost and floor area are reduced, and more efficient glue blending is achieved.

✦ Generated by Eureka AI based on patent content.

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Abstract

The present disclosure relates to a method and apparatus for SIBS swirl dynamic blending, and provides a method for SIBS swirl dynamic blending. The method includes the following steps: (A) monomer refining based on a microchannel separator and a shape coalescer; (B) additive preparation; (C) polymerization in a microchannel reactor; (D) swirl dynamic mixing and blending; (E) swirl classification and separation; (F) solution refining; and (G) non-phase change swirl drying treatment. A SIBS swirl dynamic blending apparatus is also provided. The method of the present disclosure simplifies the SIBS preparation process, reduces the equipment cost, decreases the floor area, enables continuous production, and reduces the operation cost. At the same time, based on the novel swirl dynamic blending tank apparatus, the blending intensity of the glue solution can be guaranteed to the maximum extent, the blending rate of the glue solution can be increased, and the blending capacity can be improved and the blending efficiency can be increased by connecting the dynamic blending tanks in series, and the concentration of the glue solution after blending can be increased.
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Description

Technical Field

[0001] The present disclosure belongs to the technical field of polymer materials, and relates to a SIBS swirling dynamic blending method and device. Specifically, it relates to a method and device for blending the colloidal product after the polymerization reaction in the preparation process of SIBS. Background Art

[0002] The novel thermoplastic elastomer SIBS (i.e., integrated elastomer) is composed of a styrene, isoprene, butadiene, and cyclohexane tetra-block copolymer. The middle block is polyisoprene, which has a methyl side chain in its structure, so it has good cohesion, excellent adhesion performance, and good compatibility. Such a microstructure determines its outstanding superiority when applied to adhesives and is widely used in fields such as hot melt pressure-sensitive adhesives, coatings, and plastic modification. In recent years, China has provided strong support for the polymer materials or emerging adhesives industry. The sales volume of hot melt adhesives in China has broken through year after year, with astonishing quantities. In 2021, the sales volume of the hot melt adhesive industry in China reached 1.316 million tons. SIBS hot melt pressure-sensitive adhesive is one of the varieties with the fastest development in the current hot melt adhesive market.

[0003] In the traditional SIBS preparation process, a stirring tank is generally used to blend the glue liquid generated by the polymerization reaction. The traditional blending stirring tank device has high costs and large floor areas. At the same time, although the stirring process has an effect on the cross-sectional blending, the blending effect on the vertical surface of the product is not obvious, resulting in disadvantages such as low blending efficiency and incomplete blending.

[0004] Chinese Patent CN 213824379 U discloses an SBS modified asphalt stirring tank with a heating function. By providing a transmission chamber and a multi-rotating shaft transmission mechanism ring pipe, the shear stress on the horizontal and vertical planes during the stirring process is effectively increased, and the attached heating device is beneficial to improving the stirring quality. However, this device has a large floor area and high device costs, and has a low cost performance in the industrial production process. At the same time, the enhancement of the vertical plane force during the stirring process is still not intuitive enough and needs to be further enhanced.

[0005] Therefore, aiming at the defects in the above-mentioned existing technologies, there is an urgent need in the art for a glue liquid blending method that can achieve high-quality and high-efficiency SIBS preparation process. Summary of the Invention

[0006] The present disclosure provides a novel SIBS swirling dynamic blending method and device, thus solving the problems existing in the prior art.

[0007] On the one hand, the present disclosure provides a SIBS swirling dynamic blending method, which includes the following steps:

[0008] (A) Monomer Refining Based on Microchannel Separator and Shape Coalescer: Add raw materials of crude styrene, crude isoprene, crude butadiene, and crude cyclohexane into a monomer refining unit composed of a microchannel separator and a shape coalescer to remove impurities therein and obtain refined raw materials;

[0009] (B) Auxiliary Agent Preparation;

[0010] (C) Polymerization in Microchannel Reactor: Add the refined raw materials obtained in step (A) and the auxiliary agents prepared in step (B) into a microchannel reactor. After the reaction is completed, add the produced rubber solution into a rubber solution buffer tank, and then perform extraction through a micro-droplet extraction tank containing antioxidant;

[0011] (D) Swirling Flow Dynamic Mixing and Blending: Add the rubber solution obtained after extraction treatment in step (C) into a dynamic blending tank group composed of multiple small swirling flow dynamic blending tanks connected in series, and stir and blend evenly;

[0012] (E) Swirling Flow Classification and Separation: Add the evenly blended rubber solution obtained in step (D) into a swirling flow classification separator, and adopt the swirling flow separation method for rubber solution coagulation;

[0013] (F) Solution Refining: Reflux and refine the solvent used in the swirling flow classification separator in step (E); and

[0014] (G) Non-Phase-Change Swirling Flow Drying Treatment: Add the coagulated rubber particles obtained in step (E) into a non-phase-change drying system. After the rubber particles are dried, feed them to final packaging to obtain SIBS elastomer.

[0015] In a preferred embodiment, in step (A), the weight ratio of the crude styrene, crude isoprene, crude butadiene, and crude cyclohexane is: 1:1 - 10:1 - 10:20 - 30.

[0016] In another preferred embodiment, in step (A), after refining, the purity of the crude styrene and crude isoprene is increased to more than 98.5%, and the water content is reduced to less than 20 ppm, based on the weight of the crude styrene and crude isoprene raw materials.

[0017] In another preferred embodiment, in step (B), prepare auxiliary agents selected from the following group for standby: initiator, coupling agent, coupling agent, activator, terminator.

[0018] In another preferred embodiment, the initiator includes butyl lithium, Grignard reagent, n-BuLi, the coupling agent includes tetrachlorosilane, divinylbenzene, tin tetrachloride, the coupling agent includes dichlorodimethylsilane, the activator includes tetrahydrofuran, and the terminator includes methanol, ethanol.

[0019] In another preferred embodiment, in step (C), the weight ratio of refined styrene, refined butadiene, refined isoprene, refined cyclohexane to the auxiliary agent is 1:1.5:8:25:1.

[0020] In another preferred embodiment, in step (C), the reaction pressure of the polymerization reaction is 0.03 - 0.5 MPa, the reaction temperature is 50 - 130 °C, and the reaction time is 20 - 110 min.

[0021] In another preferred embodiment, in step (C), the conversion rate of crude styrene reaches 99.1%, the conversion rate of crude isoprene reaches 99.75%, and the concentration of the obtained SIBS rubber solution is 15 - 20%.

[0022] In another preferred embodiment, after steps (D), (E) and (F), a rubber solution with a solid content of 30 - 50% is obtained; in step (G), the non-phase change drying system is a mechanical + cyclone non-phase change drying system, and the operating pressure is 0.1 MPa - 0.3 MPa; the melt index of the obtained SIBS elastomer is 0.1 - 30.0, and the molecular weight of the elastomer is 70,000 - 150,000.

[0023] On the other hand, the present disclosure provides a SIBS microchannel reaction device, which includes:

[0024] A monomer refining unit composed of a microchannel reactor and a coalescer connected thereto, for performing step (A) monomer refining based on a microchannel separator and a coalescer: adding raw materials of crude styrene, crude isoprene, crude butadiene and crude cyclohexane to the monomer refining unit composed of a microchannel separator and a coalescer to remove impurities therein and obtain refined raw materials;

[0025] A microchannel reactor connected to the coalescer, a rubber solution buffer tank connected to the microchannel reactor, and a microdroplet extraction tank connected to the rubber solution buffer tank, for performing step (C) microchannel reactor polymerization: adding the refined raw materials obtained in step (A) and the auxiliary agent prepared in step (B) to the microchannel reactor, and adding the generated rubber solution to the rubber solution buffer tank after the reaction is completed, and then performing extraction through a microdroplet extraction tank containing an antioxidant;

[0026] A dynamic blending tank connected to the microdroplet extraction tank, for performing step (D) swirling dynamic mixing and blending: adding the rubber solution obtained after extraction treatment in step (C) to a dynamic blending tank group composed of a plurality of small swirling dynamic blending tanks connected in series, and stirring and blending evenly;

[0027] A cyclone classifier connected to a dynamic blending tank for performing step (E) cyclone classification separation: adding the uniformly blended rubber solution obtained in step (D) into the cyclone classifier, and adopting the cyclone separation method to perform rubber solution coagulation; and

[0028] A non-phase change drying system connected to the cyclone classifier, and a packaging system connected to the non-phase change drying system for performing step (G) non-phase change cyclone drying treatment: adding the coagulated rubber particles obtained in step (E) into the non-phase change drying system, and feeding the dried rubber particles to final packaging after drying to obtain SIBS elastomer.

[0029] Beneficial effects:

[0030] The main advantages of the method and device of the present disclosure are as follows:

[0031] (1) The novel swirling dynamic blending tank of the present disclosure improves the stirring efficiency, enhances the stirring effect in the vertical plane, and thus improves the blending quality. It overcomes the disadvantages of the traditional blending and stirring tank device, such as high cost, large floor area, and obvious effect on cross-section blending during the stirring process but not obvious effect on the blending of the product in the vertical plane, resulting in low blending efficiency and incomplete blending.

[0032] (2) The method of the present disclosure uses a swirling dynamic mixing tank to replace the original large stirring tank with several swirling dynamic mixing tanks, which can realize the blending process in multiple batches and improve the blending efficiency; the novel swirling dynamic blending tank replaces the traditional stirring force with the acting force of the swirling flow field, making the colloid perform blending in a spiral motion instead of a simple cross-sectional motion, enhancing the acting force in the vertical plane, and thus improving the blending effect. Description of the Drawings

[0033] The drawings are used to provide a further understanding of the present disclosure. They only form a part of this specification to further explain the present disclosure and do not constitute a limitation to the present disclosure.

[0034] Figure 1 It is a schematic diagram of the overall process flow of the SIBS swirling dynamic blending method according to a preferred embodiment of the present disclosure.

[0035] Figure 2 It is a schematic structural diagram of the dynamic blending tank according to a preferred embodiment of the present disclosure.

[0036] Reference numerals:

[0037] 1: Microchannel separator

[0038] 2: Shape coalescer

[0039] 3: Microchannel reactor (3-1, 3-2, 3-3, 3-4)

[0040] 4: Glue Buffer Tank

[0041] 5: Micro-droplet Extraction Tank

[0042] 6: Dynamic Blending Tank

[0043] 7: Cyclone Classifying Separator

[0044] 8: Non-phase-change Drying System

[0045] 9: Packaging System

[0046] 10: Refining Tower (10-1, 10-2)

[0047] 11: Condenser

[0048] 12: Intermediate Tank

[0049] 13: Reflux Tank

[0050] 14: Heavy-component Storage Tank

[0051] 15: Butadiene Product Tank

[0052] 16: Heavy-component Removal Tower

[0053] 17: Isoprene Product Tank

[0054] 18: Fine Solvent Tank

[0055] 19: Separation Tank

[0056] 20: Tail Gas Condenser

[0057] 21: Stripping Unit Mixer

[0058] 22: Dewatering Extruder

[0059] 23: Hot Water Tank

[0060] 24: Dewatering Screen

[0061] 101: Fixed Plate

[0062] 102: Connection Port

[0063] 103: Overflow Connection Pipe

[0064] 104: Flange

[0065] 105: Annular Gap Overflow Port

[0066] 106: Flange

[0067] 107: Annular Gap

[0068] 108: Overflow Port

[0069] 109: Flange

[0070] 110: Conical section

[0071] 111: Flange

[0072] 112: Underflow port Detailed implementation mode

[0073] The endpoints and any values within the ranges disclosed herein are not limited to the exact ranges or values. These ranges or values should be understood to include values close to these ranges or values. For numerical ranges, the values between the endpoint values of each range, between the endpoint values of each range and individual point values, and between individual point values can be combined with each other to obtain one or more new numerical ranges, and these numerical ranges should be regarded as specifically disclosed herein.

[0074] After extensive and in-depth research, the applicant of the present invention found that in the existing SIBS preparation process, a stirring tank is generally used to blend the glue solution generated by the polymerization reaction. However, the traditional blending stirring tank device has high costs and large floor areas. At the same time, although the stirring process has an effect on the cross-sectional blending, the blending effect on the vertical surface of the product is not obvious, resulting in low blending efficiency and incomplete blending. The present disclosure provides a SIBS swirling dynamic blending method and device. By using multiple small swirling dynamic blending tanks instead of large stirring tanks, the blending intensity of the glue solution can be guaranteed to the maximum extent, while the blending rate of the glue solution is increased. And through the series connection of the dynamic blending tanks, the blending capacity can be increased, the blending efficiency can be improved, and the concentration of the blended glue solution can be increased. Based on the above findings, the present invention has been completed.

[0075] In the first aspect of the present disclosure, a SIBS swirling dynamic blending method is provided. The method includes the following steps:

[0076] (A) Monomer refining based on a microchannel separator and a shape coalescer: adding raw materials of crude styrene, crude isoprene, crude butadiene, and crude cyclohexane to a monomer refining unit composed of a microchannel separator and a shape coalescer to remove impurities therein and obtain refined raw materials;

[0077] (B) Auxiliary agent configuration;

[0078] (C) Polymerization in a microchannel reactor: adding the refined raw materials obtained in step (A) and the auxiliary agents configured in step (B) to a microchannel reactor. After the reaction is completed, the generated glue solution is added to a glue solution buffer tank, and then extracted through a micro-droplet extraction tank containing an antioxidant;

[0079] (D) Swirling dynamic mixing and blending: adding the glue solution obtained in step (C) after extraction treatment to a dynamic blending tank and stirring and blending it evenly;

[0080] (E) Cyclone classification separation: Add the uniformly blended rubber solution obtained in step (D) into a cyclone classifier, and use the cyclone separation method to agglomerate the rubber solution;

[0081] (F) Solution refining: Reflux and refine the solvent used in the cyclone classifier in step (E); and

[0082] (G) Non-phase change cyclone drying treatment: Add the agglomerated rubber particles obtained in step (E) into a non-phase change drying system. After the rubber particles are dried, feed them to final packaging to obtain SIBS elastomer.

[0083] In the present disclosure, in step (A), the weight ratio of the crude styrene, crude isoprene, crude butadiene, and crude cyclohexane is: 1:1 - 10:1 - 10:20 - 30, preferably 1:8:1.5:25.

[0084] In the present disclosure, in step (A), the raw material is a crudely purchased raw material, and the main impurities are irregular fine particles and moisture.

[0085] In the present disclosure, in step (A), after refining, the purity of the crude styrene and crude isoprene is increased to more than 98.5%, and the water content is reduced to less than 20 ppm, based on the weight of the crude styrene and crude isoprene raw materials.

[0086] In the present disclosure, in step (B), prepare the auxiliary agents selected from the following group for standby: initiator, coupling agent, coupling agent, activator, terminator.

[0087] In the present disclosure, the initiator includes, but is not limited to: butyl lithium, Grignard reagent, n-BuLi.

[0088] In the present disclosure, the coupling agent includes, but is not limited to: tetrachlorosilane, DVB (divinylbenzene), tin tetrachloride.

[0089] In the present disclosure, the coupling agent includes, but is not limited to: dichlorodimethylsilane.

[0090] In the present disclosure, the activator includes, but is not limited to: tetrahydrofuran (THF).

[0091] In the present disclosure, the terminator includes, but is not limited to: methanol, ethanol. In the present disclosure, in step (B), except for the activator, the auxiliary agents need to be added to the polymerization system in the form of a cyclohexane solution.

[0092] In the present disclosure, in step (C), by replacing the reaction kettle with a microchannel reactor, the SIBS preparation process is changed from a discontinuous process to a continuous process, and the feeding, reaction, and discharging are carried out continuously, increasing the preparation efficiency by 2 - 10 times.

[0093] In the present disclosure, in step (C), the raw materials are added in a stepwise manner. After preheating, the refined cyclohexane is first added to the microchannel reactor, and then the refined styrene, refined butadiene, and refined isoprene are added successively.

[0094] In the present disclosure, in step (C), the concentration of the obtained SIBS rubber solution is 15-20%, such as 15%, 16%, 17%, 18%, 19%, 20%.

[0095] In the present disclosure, in step (C), the weight ratio of refined styrene, refined butadiene, refined isoprene, refined cyclohexane to the auxiliary agent is 1:1.5:8:25:1.

[0096] In the present disclosure, in step (C), the reaction pressure of the polymerization reaction is 0.03 - 0.5 MPa, the reaction temperature is 50 - 130 °C, and the reaction time is 20 - 110 min.

[0097] In the present disclosure, in step (C), the conversion rate of crude styrene can reach 99.1%, and the conversion rate of crude isoprene can reach 99.75%.

[0098] In the present disclosure, in step (C), the concentration of the obtained SIBS rubber solution is 15-20%, such as 15%, 16%, 17%, 18%, 19%, 20%.

[0099] In the present disclosure, in step (D), the swirling dynamic blending tank is a dynamic blending tank group composed of multiple small swirling dynamic blending tanks connected in series.

[0100] In the present disclosure, after steps (D), (E), and (F), a rubber solution with a solid content of 30-50% is obtained.

[0101] In the present disclosure, in step (G), the operating pressure of the non-phase change drying process is 0.1 MPa - 0.3 MPa.

[0102] In the present disclosure, in step (G), the energy consumption of the non-phase change drying system is approximately 1 / 5 - 1 / 15 of that of heating phase change evaporation.

[0103] In the present disclosure, the obtained SIBS elastomer has a melt index of 0.1 - 30.0, and the molecular weight of the elastomer is 70,000 - 150,000.

[0104] In the second aspect of the present disclosure, a SIBS microchannel reaction device is provided, and the device includes:

[0105] A monomer purification unit composed of a microchannel reactor and a shape coalescer connected thereto, for performing step (A) monomer purification based on a microchannel separator and a shape coalescer: adding raw materials of crude styrene, crude isoprene, crude butadiene, and crude cyclohexane to the monomer purification unit composed of a microchannel separator and a shape coalescer to remove impurities therein, thereby obtaining purified raw materials;

[0106] A microchannel reactor connected to the shape coalescer, a glue solution buffer tank connected to the microchannel reactor, and a micro-droplet extraction tank connected to the glue solution buffer tank, for performing step (C) microchannel reactor polymerization: adding the purified raw materials obtained in step (A) and the additives prepared in step (B) to the microchannel reactor, and after the reaction is completed, adding the produced glue solution to the glue solution buffer tank, and then performing extraction through the micro-droplet extraction tank containing an antioxidant;

[0107] A dynamic blending tank connected to the micro-droplet extraction tank, for performing step (D) swirling dynamic mixing and blending: adding the glue solution obtained after extraction treatment in step (C) to the dynamic blending tank and stirring and blending it evenly;

[0108] A cyclone classifier separator connected to the dynamic blending tank, for performing step (E) cyclone classification separation: adding the evenly blended glue solution obtained in step (D) to the cyclone classifier separator and performing glue solution coagulation by means of cyclone separation; and

[0109] A non-phase change drying system connected to the cyclone classifier separator, and a packaging system connected to the non-phase change drying system, for performing step (G) non-phase change swirling drying treatment: adding the coagulated rubber particles obtained in step (E) to the non-phase change drying system, and after the rubber particles are dried, feeding them to final packaging to obtain SIBS elastomer.

[0110] In the present disclosure, the monomer purification unit includes: a styrene purification unit, a butadiene purification unit, an isoprene purification unit, and a cyclohexane purification unit.

[0111] In the present disclosure, in the styrene purification unit, crude styrene undergoes solid-liquid separation through a microchannel separator, and the separated styrene then undergoes oil-water separation through a shape coalescer and enters the microchannel reactor.

[0112] In the present disclosure, the device further includes: a refining tower connected to the butadiene purification unit, a condensation reflux system (composed of a condenser, an intermediate tank, and a reflux tank) and a heavy component storage tank connected to the refining tower, and a butadiene product tank connected to the condensation reflux system;

[0113] A deweighting tower connected to the isoprene purification unit, a condensation reflux system (composed of a condenser and a reflux tank) connected to the deweighting tower, and a product tank connected to the condensation reflux system; and

[0114] Two condensation reflux systems connected successively to the cyclohexane refining unit, and a refining agent tank connected to the condensation reflux system.

[0115] In the present disclosure, the swirling dynamic blending tank blends the rubber solution through a swirling flow field, effectively improving the stirring effect of the mixed rubber solution in the vertical plane.

[0116] In the present disclosure, the large stirring tank is replaced by multiple small swirling dynamic blending tanks in the swirling dynamic blending tank. Under the same volume, the operation volume of the swirling dynamic blending tank is much larger than that of the traditional blending tank. By replacing it, the floor area of the device is greatly reduced and the device cost is reduced.

[0117] In the present disclosure, in the butadiene refining unit, crude butadiene undergoes solid-liquid separation through a microchannel separator and then oil-water separation through a shape coalescer. The obtained product sequentially enters a refining tower connected to the butadiene refining unit, a condensation reflux system and a heavy component storage tank connected to the refining tower, and a butadiene product tank connected to the condensation reflux system, and then enters a microchannel reactor connected to the butadiene product tank.

[0118] In the present disclosure, in the isoprene refining unit, crude isoprene undergoes solid-liquid separation through a microchannel separator and then oil-water separation through a shape coalescer. The obtained product sequentially enters a de-heavy tower connected to the isoprene refining unit, a condensation reflux system connected to the de-heavy tower, and a product tank connected to the condensation reflux system, and then enters a microchannel reactor connected to the product tank.

[0119] In the present disclosure, in the cyclohexane refining unit, crude cyclohexane undergoes solid-liquid separation through a microchannel separator and then oil-water separation through a shape coalescer. The obtained product sequentially enters two condensation reflux systems successively connected to the cyclohexane refining unit, a refined solvent tank connected to the condensation reflux system, and then enters a microchannel reactor connected to the refined solvent tank.

[0120] In the present disclosure, the auxiliary agent is added to the channel reactor.

[0121] In the present disclosure, the refined raw materials and the auxiliary agent undergo a polymerization reaction in the microchannel reactor to obtain SIBS products.

[0122] In the present disclosure, the obtained SIBS products are further concentrated through rubber solution blending, coagulation, and solution refining.

[0123] In the present disclosure, the refined SIBS products are sent to the final packaging system after post-treatment by the non-phase change drying system.

[0124] The following refers to the accompanying drawings.

[0125] Figure 1Schematic diagram of the overall process flow of the SIBS swirling dynamic blending method according to a preferred embodiment of the present disclosure. As Figure 1 shown, the raw materials of crude styrene, crude butadiene, crude isoprene, and crude cyclohexane are respectively added to the styrene refining unit, butadiene refining unit, isoprene refining unit, and cyclohexane refining unit composed of a microchannel separator 1 and a shape coalescer 2 connected thereto; among them, the styrene produced by the styrene refining unit is directly pumped from its shape coalescer 2 to the microchannel reactor 3; the butadiene produced by the butadiene refining unit is pumped from its shape coalescer 2 to the refining tower 10, the light components obtained by refining are discharged from the top of the refining tower 10 and sent to the condenser 11 for condensation and then sent to the intermediate tank 12, the heavy components obtained by refining are discharged from the bottom of the refining tower 10 and sent to the heavy component storage tank 14, the butadiene obtained by refining is sent to the reflux tank 13, the reflux is returned to the refining tower 10, the butadiene is sent to the butadiene product tank 15, and then pumped to the microchannel reactor 3; the isoprene produced by the isoprene refining unit is pumped from its shape coalescer 2 to the heavy component removal tower 16 to remove heavy components, the light components are discharged from the top of the heavy component removal tower 16 and sent to the condenser 11 for condensation and then sent to the reflux tank 13, part of the components are returned to the heavy component removal tower 16, the isoprene is sent to the isoprene product tank 17, and then pumped to the microchannel reactor 3; the cyclohexane produced by the cyclohexane refining unit is sent from its shape coalescer 2 to the refining tower 10-1, the light components obtained by refining are discharged from the top of the refining tower 10-1 and sent to the condenser 11 for condensation and then sent to the reflux tank 13, the light components are discharged from the top of the reflux tank 13 and sent to the condenser 11 for condensation and then sent to the refined solvent tank 18, part of the components are returned to the refining tower 10-1, the cyclohexane is sent to the refining tower 10-2 to remove the bottom heavy components, the light components are discharged from the top of the refining tower 10-2 and sent to the condenser 11 for condensation and then sent to the reflux tank 13, part of the components are returned to the refining tower 10-2, the cyclohexane is sent to the refined solvent tank 18, and then pumped to the microchannel reactor 3; at the same time, an additive is added to the microchannel reactor 3;

[0126] The rubber solution produced by the microchannel reactor groups 3-1, 3-2, 3-3, and 3-4 is sent into the rubber solution buffer tank 4, and then extracted through the micro-droplet extraction tank 5 containing antioxidant. The gas phase is discharged from the top of the rubber solution buffer tank 4 and sent into the separation tank 19. The separated gas phase is sent into the tail gas condenser 20. The condensed liquid phase is sent into the shape coalescer 2, refined, and then sent into the hydrocyclone classifier 7 for separation. The obtained product is sent into the reflux tank 13, then screened by the dehydration sieve 24, sent into the dehydration extruder 22 for extrusion, and then sent into the non-phase change drying system 8 to remove the moisture on the surface and in the pores of the rubber particles. The residual water is sent to the RTO for treatment. The granular materials in the product packaging silo enter the packaging system 9, and after metering, sewing, sealing, metal detection, weight inspection, palletizing, and finished product warehousing, the final SIBS product is obtained. The slag liquid discharged from the separation tank 19 is sent into the shape coalescer 2. The rubber solution treated by the micro-droplet extraction tank 5 enters the dynamic blending tank 6, is stirred and blended evenly, and the gas phase is discharged from the top and sent into the tail gas condenser 20. The liquid phase is mixed by the stripping unit mixer 29 and then enters the hydrocyclone classifier 7 for rubber particle hydrocyclone separation. The moisture removed by the dehydration sieve 24 and the dehydration extruder 22 is sent into the hot water tank 23 and then sent into the shape coalescer 2. The hot water in the hot water tank 23 is added with a dispersant and then returned to the stripping unit mixer 29 together.

[0127] Figure 2 is a schematic structural diagram of a dynamic blending tank according to a preferred embodiment of the present disclosure. As Figure 2 shown, the dynamic blending tank includes: a fixed plate 101, a connection port 102, an overflow connection pipe 103, a flange 104, an annular gap overflow port 105, a flange 106, an annular gap 107, an overflow port 108, a flange 109, a conical section 110, a flange 111, and an underflow port 112.

[0128] Example

[0129] The present invention will be further described below in conjunction with specific embodiments. However, it should be understood that these embodiments are only used to illustrate the present invention and do not constitute a limitation to the scope of the present invention. The test methods without specific conditions in the following embodiments are usually carried out under conventional conditions or according to the conditions recommended by the manufacturer. Unless otherwise specified, all percentages and parts are by weight.

[0130] Example 1:

[0131] I. Device Name

[0132] 40 kg / h elastomer pilot production device

[0133] II. Process Flow

[0134] As Figure 1 shown.

[0135] The control ratio of material addition is shown in Table 1 below.

[0136] Table 1: Material addition control ratio

[0137]

[0138] III. Implementation effects

[0139] The process analysis data are shown in Table 2 below.

[0140] Table 2: Process analysis data

[0141]

[0142]

[0143] It can be seen from the above analysis data that by using the method of the present invention, all process indexes meet the control requirements, and the finished rubber produced also meets the physical and chemical indexes required by the market. The yield of the finished rubber reaches more than 99%, the conversion rate of isoprene reaches 99.5%, the conversion rate of styrene reaches 99.5%, and the conversion rate of butadiene reaches 99.3%.

[0144] The above-listed embodiments are only preferred embodiments of the present disclosure, and are not used to limit the scope of implementation of the present disclosure. That is, equivalent changes and modifications made according to the content of the patent scope of this application should all fall within the technical scope of the present disclosure.

[0145] All documents mentioned in the present disclosure are cited as references in this application, just as if each document was cited separately as a reference. In addition, it should be understood that after reading the above teachings of the present disclosure, those skilled in the art can make various changes or modifications to the present disclosure, and these equivalent forms also fall within the scope defined by the appended claims of this application.

Claims

1. A method for SIBS swirl dynamic blending, the method comprises the following steps: (A) Monomer refining based on a microchannel separator and a shape coalescer: adding raw materials of crude styrene, crude isoprene, crude butadiene and crude cyclohexane into a monomer refining unit composed of a microchannel separator and a shape coalescer to remove impurities therein, and obtaining refined raw materials; (B) Auxiliary agent preparation; (C) Polymerization in a microchannel reactor: adding the refined raw materials obtained in step (A) and the auxiliary agents prepared in step (B) into a microchannel reactor, adding the produced rubber solution into a rubber solution buffer tank after the reaction is completed, and then performing extraction through a micro-droplet extraction tank containing an antioxidant; (D) Swirl dynamic mixing and blending: adding the rubber solution obtained in step (C) after extraction treatment into a dynamic blending tank group composed of multiple small swirl dynamic blending tanks connected in series, and stirring and blending evenly; (E) Swirl classification and separation: adding the evenly blended rubber solution obtained in step (D) into a swirl classification separator, and performing rubber solution coagulation by adopting a swirl separation method; (F) Solution refining and non-phase change swirl drying treatment: refluxing and refining the solvent used in the swirl classification separator in step (E); and adding the coagulated rubber particles obtained in step (E) into a non-phase change drying system, feeding the dried rubber particles to final packaging after drying, and obtaining SIBS elastomer.

2. The method according to claim 1, characterized in that, in step (A), the weight ratio of the crude styrene, crude isoprene, crude butadiene, and crude cyclohexane is 1: 1-10: 1-10: 20-30.

3. The method according to claim 1, characterized in that, in step (A), after refining, the purity of the crude styrene and crude isoprene is increased to more than 98.5%, and the water content is reduced to less than 20 ppm, based on the weight of the crude styrene and crude isoprene raw materials.

4. The method according to claim 1, characterized in that, in step (B), auxiliary agents selected from the following group are prepared for standby: initiator, coupling agent, coupling agent, activator, terminator.

5. The method according to claim 1, characterized in that, in step (C), the weight ratio of refined styrene, refined butadiene, refined isoprene, refined cyclohexane to the auxiliary agent is 1: 1.5: 8: 25:

1.

6. The method according to claim 1, characterized in that, in step (C), the reaction pressure of the polymerization reaction is 0.03-0.5 MPa, the reaction temperature is 50-130 °C, and the reaction time is 20-110 min.

7. The method according to claim 1, characterized in that, in step (C), the conversion rate of styrene reaches 99.1%, the conversion rate of isoprene reaches 99.75%, and the concentration of the obtained SIBS rubber solution is 15-20%.

8. The method according to claim 1, characterized in that, after steps (D), (E) and (F), a rubber solution with a solid content of 30-50% is obtained; in step (F), the non-phase change drying system is a mechanical + swirl non-phase change drying system, and the operating pressure is 0.1 MPa-0.3 MPa; the number average molecular weight of the elastomer is 70,000-150,000.

9. An SIBS microchannel reaction device, the device comprises: A monomer refining unit composed of a microchannel reactor (1) and a shape coalescer (2) connected thereto, for performing step (A) monomer refining based on a microchannel separator and a shape coalescer: adding raw materials of crude styrene, crude isoprene, crude butadiene and crude cyclohexane into the monomer refining unit composed of a microchannel separator and a shape coalescer to remove impurities therein, and obtaining refined raw materials; A microchannel reactor (3) connected to the shape coalescer (2), a glue solution buffer tank (4) connected to the microchannel reactor (3), and a micro-droplet extraction tank (5) connected to the glue solution buffer tank (4), for performing step (C) microchannel reactor polymerization: adding the refined raw materials obtained in step (A) and the additives prepared in step (B) into the microchannel reactor, adding the produced glue solution into the glue solution buffer tank after the reaction is completed, and then performing extraction through the micro-droplet extraction tank containing an antioxidant; wherein, the microchannel reactor (3) is laid in a pipeline type; A dynamic blending tank (6) connected to the micro-droplet extraction tank (5), for performing step (D) swirling dynamic mixing and blending: adding the glue solution obtained after extraction treatment in step (C) into a dynamic blending tank group composed of a plurality of small swirling dynamic blending tanks connected in series, and stirring and blending evenly; A cyclone classifier (7) connected to the dynamic blending tank (6), for performing step (E) cyclone classification and separation: adding the evenly blended glue solution obtained in step (D) into the cyclone classifier, and performing glue solution coagulation by adopting a cyclone separation method; and A non-phase change drying system (8) connected to the cyclone classifier (7), and a packaging system (9) connected to the non-phase change drying system (8), for performing step (F) solution refining and non-phase change swirling drying treatment: performing reflux refining on the solvent used in the cyclone classifier in step (E); and adding the coagulated rubber particles obtained in step (E) into the non-phase change drying system, feeding the dried rubber particles to final packaging, and obtaining SIBS elastomer.

Citation Information

Patent Citations

  • SBS modified asphalt stirring tank with heating function

    CN213824379U

  • Industrial production methods of trans-1,4-butadiene-isoprene copolymer rubber (TBIR), and device for implementing method

    CN107686536A

  • Hydrogenation reaction method of conjugated diene-containing polymer

    CN114539446A