SIBS microchannel reaction method and device

Abstract

The present disclosure relates to a SIBS microchannel reaction method and apparatus, and provides a SIBS microchannel reaction method, which includes the following steps: (A) monomer refining based on a microchannel separator and a shaped coalescer; (B) auxiliary agent configuration; (C) microchannel reactor polymerization; (D) cyclone dynamic mixing and blending; (E) cyclone fractionation and separation; (F) solution refining; and (G) non-phase change cyclone drying treatment. A SIBS microchannel reaction apparatus is also provided. The method of the present disclosure simplifies the SIBS production process, reduces floor space, and lowers apparatus cost; the apparatus of the present disclosure performs polymerization reactions efficiently, with high quality, and continuously, thereby improving SIBS product quality and increasing product output.

Description

Technical Field

[0001] The present disclosure belongs to the technical field of polymer materials, and relates to a SIBS microchannel reaction method and device, and more specifically, to a method and device for generating colloid by polymerization of reaction raw materials in the SIBS preparation process. Background Art

[0002] The new thermoplastic elastomer SIBS (i.e., integrated elastomer) is composed of a tetrablock copolymer of styrene, isoprene, butadiene, and cyclohexane, with a polyisoprene middle block. Its structure features a methyl side chain, resulting in excellent cohesion, superior adhesion, and good compatibility. This microstructure dictates its outstanding superiority in adhesive applications, and it is widely used in hot melt pressure-sensitive adhesives, coatings, and plastic modification. In recent years, my country has strongly supported the polymer materials and emerging adhesives industries, resulting in impressive year-over-year sales of hot melt adhesives in my country. In 2021, sales in my country's hot melt adhesive industry could reach 1.316 million tons. SIBS hot melt pressure-sensitive adhesive is one of the fastest-growing varieties in the current hot melt adhesive market.

[0003] Traditional SIBS production processes typically use a reactor to polymerize the raw materials to form a colloid. However, the raw materials are unevenly distributed within the reactor during polymerization, resulting in incomplete reaction results. Furthermore, the raw materials reside in the reactor for a long time, forcing intermittent operation and resulting in low polymerization efficiency. Therefore, a new raw material polymerization method is needed to improve reaction quality and efficiency.

[0004] Chinese patent CN 208320781 U discloses a reactor for preparing SBS grafted adhesive resin. A loop tube facilitates reheating of the raw materials to ensure effective fusion, and a motor-driven scraper removes residual material. This process improves the quality of raw material polymerization to some extent, but it still requires long periods of stagnation and other equipment standby time, resulting in a discontinuous reaction process with low efficiency.

[0005] Therefore, in view of the above-mentioned defects in the prior art, there is an urgent need in the art for a method that can realize the continuous preparation process of SIBS and improve the quality of the polymerization reaction in the preparation of SIBS. Summary of the Invention

[0006] The present disclosure provides a novel SIBS microchannel reaction method and device, thereby solving the problems of the existing SIBS preparation process, such as complicated production steps, discontinuous production, and uneven, incomplete, and discontinuous polymerization reaction based on traditional reactors.

[0007] In one aspect, the present disclosure provides a SIBS microchannel reaction method, the method comprising the following steps:

[0008] (A) Monomer Refining Based on a Microchannel Separator and Shape Coalescer: Crude styrene, crude isoprene, crude butadiene, and crude cyclohexane raw materials are added to 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 configuration;

[0010] (C) Microchannel reactor polymerization: the refined raw material obtained in step (A) and the auxiliary agent prepared in step (B) are added to a microchannel reactor. After the reaction is completed, the generated glue is added to a glue buffer tank, and then extracted by a micro-droplet extraction tank containing an antioxidant; wherein the microchannel reactor is a pipeline type.

[0011] (D) Cyclone dynamic mixing and blending: adding the extracted rubber solution obtained in step (C) into a dynamic blending tank, stirring and blending uniformly;

[0012] (E) Cyclone fractionation: adding the uniformly mixed glue obtained in step (D) into a cyclone fractionation separator, and using cyclone separation to agglomerate the glue;

[0013] (F) solution purification: refluxing and refining the solvent used in the cyclone fractionator in step (E); and

[0014] (G) Non-phase-change cyclone drying treatment: The coagulated particles obtained in step (E) are added to a non-phase-change drying system. After drying, the particles are fed to the final packaging to obtain the 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; 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.

[0016] In another preferred embodiment, in step (B), an auxiliary agent selected from the following group is prepared for use: an initiator, a coupling agent, a coupling agent, an activator, and a terminator.

[0017] In another preferred embodiment, in step (C), the raw materials are added in steps. After being preheated, the refined cyclohexane is first added to the microchannel reactor, and then the refined styrene, refined butadiene and refined isoprene are added in sequence.

[0018] In another preferred embodiment, in step (C), the weight ratio of refined styrene, refined butadiene, refined isoprene, refined cyclohexane and auxiliary agent is 1:1.5:8:25:1; the reaction pressure of the polymerization reaction is 0.03-0.5 MPa, and the reaction temperature is 50-130°C.

[0019] In another preferred embodiment, in step (C), a plurality of microchannel separators are arranged in series; and the production time of each batch of a single microchannel reactor is 0.8 to 2 hours.

[0020] 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 glue is 15-20%.

[0021] In another preferred embodiment, after steps (D), (E) and (F), a glue 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 0.1MPa-0.3MPa; the obtained SIBS elastomer has a melt index of 0.1~30.0 and a molecular weight of the elastomer is 70,000~150,000.

[0022] In another aspect, the present disclosure provides a SIBS microchannel reaction device, comprising:

[0023] A monomer refining unit consisting of a microchannel reactor and a shape coalescer connected thereto is used to carry out the monomer refining based on the microchannel separator and the shape coalescer in step (A): crude styrene, crude isoprene, crude butadiene and crude cyclohexane raw materials are added to the monomer refining unit consisting of the microchannel separator and the shape coalescer to remove impurities therein to obtain refined raw materials;

[0024] A microchannel reactor connected to the shape coalescer, a glue buffer tank connected to the microchannel reactor, and a micro-droplet extraction tank connected to the glue buffer tank are used to carry out microchannel reactor polymerization in step (C): the refined raw material obtained in step (A) and the auxiliary agent prepared in step (B) are added to the microchannel reactor, and after the reaction is completed, the generated glue is added to the glue buffer tank, and then extracted through a micro-droplet extraction tank containing an antioxidant; wherein the microchannel reactor is laid in a pipeline type;

[0025] The dynamic blending tank connected to the micro-droplet extraction tank is used to perform the cyclone dynamic mixing and blending in step (D): the extracted rubber solution obtained in step (C) is added to the dynamic blending tank and stirred and blended uniformly;

[0026] The cyclone classification separator connected to the dynamic blending tank is used to perform cyclone classification separation in step (E): adding the uniformly blended glue obtained in step (D) to the cyclone classification separator, and adopting cyclone separation method to perform glue coagulation; and

[0027] The non-phase-change drying system connected to the cyclone classifier and the packaging system connected to the non-phase-change drying system are used to perform the non-phase-change cyclone drying treatment in step (G): the condensed colloid particles obtained in step (E) are added to the non-phase-change drying system, and the colloid particles are dried and fed to the final packaging to obtain the SIBS elastomer.

[0028] Beneficial effects:

[0029] The main advantages of the method and apparatus disclosed herein are:

[0030] (1) The microchannel reactor disclosed in the present invention changes the traditional discontinuous SIBS preparation process into a continuous preparation process, thereby improving preparation efficiency and reducing operating costs. Existing preparation methods are mostly discontinuous, where raw materials and additives are mixed evenly in a reactor and the reaction is carried out in stages. The next batch of feed is reacted only after a portion of the feed is completely reacted, resulting in low efficiency. The method disclosed in the present invention achieves a continuous preparation process by replacing the reactor with a microchannel reactor, with continuous feeding, reaction, and discharge, and continuous equipment operation, thereby improving preparation efficiency by 2-5 times.

[0031] (2) The microchannel separator disclosed in the present invention increases the reaction contact area, prolongs the reaction time, and improves product quality. The microchannel reactor is laid out in a pipeline-type manner, which increases the reaction contact area by 5-30 times under the same floor space, effectively increasing the residence time of raw materials and additives in the microchannel reactor, extending the polymerization reaction time, ensuring sufficient reaction of raw materials, and improving product quality.

[0032] (3) The method disclosed herein further increases the reaction contact area and improves the processing capacity by using microchannel reactors in series. BRIEF DESCRIPTION OF THE DRAWINGS

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

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

[0035] Figure 2 It is a schematic structural diagram of a microchannel separator 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 mixing tank

[0043] 7: Cyclone Classification 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: Tundish

[0049] 13: Reflux tank

[0050] 14: Heavy component storage tank

[0051] 15: Butadiene product tank

[0052] 16: Deweighting Tower

[0053] 17: Isoprene product tank

[0054] 18: Refined solvent tank

[0055] 19: Separation tank

[0056] 20: Exhaust gas condenser

[0057] 21: Stripping unit mixer

[0058] 22: Dehydration extruder

[0059] 23: Hot water tank

[0060] 24: Dewatering screen

[0061] 101: Coolant outlet

[0062] 102: Separation chamber

[0063] 103: Liquid outlet

[0064] 104: Blocking plate

[0065] 105: Flame barrier insert

[0066] 106: Separation table

[0067] 107: Coolant outlet

[0068] 108: Coolant base

[0069] 109: Reaction Pathway

[0070] 110: Coolant passage

[0071] 111: Gas passage

[0072] 112: Access Pipeline

[0073] 113: Coolant feed

[0074] 114: Coolant feed

[0075] 115: Flame barrier insert

[0076] 116: Gas feed

[0077] 117: Liquid feed

[0078] 118: Liquid feed DETAILED DESCRIPTION

[0079] The endpoints of the ranges and any values disclosed herein are not limited to the precise ranges or values, and these ranges or values should be understood to include values close to these ranges or values. For numerical ranges, the endpoints of each range, the endpoints of each range and individual point values, and the individual point values can be combined with each other to obtain one or more new numerical ranges, which should be considered to be specifically disclosed herein.

[0080] After extensive and in-depth research, the applicant of the present invention discovered that the existing SIBS preparation process has complicated production steps, the production process is intermittent, and based on the defects of the traditional reactor polymerization reaction, it is uneven, incomplete, and intermittent. The present disclosure provides a SIBS microchannel reaction method and device. By using a pipeline-type laid microchannel reactor, SIBS can be continuously produced, while simplifying the SIBS production process, reducing the floor space, and reducing the cost of the device. At the same time, the polymerization reaction can be carried out efficiently, with high quality, and continuously, thereby improving the quality of SIBS products and increasing product output. Based on the above findings, the present invention has been completed.

[0081] In a first aspect of the present disclosure, a SIBS microchannel reaction method is provided, the method comprising the following steps:

[0082] (A) Monomer Refining Based on a Microchannel Separator and Shape Coalescer: Crude styrene, crude isoprene, crude butadiene, and crude cyclohexane raw materials are added to a monomer refining unit composed of a microchannel separator and a shape coalescer to remove impurities therein and obtain refined raw materials;

[0083] (B) auxiliary agent configuration;

[0084] (C) Microchannel reactor polymerization: The refined raw material obtained in step (A) and the auxiliary agent prepared in step (B) are added to a microchannel reactor. After the reaction is completed, the generated glue is added to a glue buffer tank and then extracted by a micro-droplet extraction tank containing an antioxidant;

[0085] (D) Cyclone dynamic mixing and blending: adding the extracted rubber solution obtained in step (C) into a dynamic blending tank, stirring and blending uniformly;

[0086] (E) Cyclone fractionation: adding the uniformly mixed glue obtained in step (D) into a cyclone fractionation separator, and using cyclone separation to agglomerate the glue;

[0087] (F) solution purification: refluxing and refining the solvent used in the cyclone fractionator in step (E); and

[0088] (G) Non-phase-change cyclone drying treatment: The coagulated particles obtained in step (E) are added to a non-phase-change drying system. After drying, the particles are fed to the final packaging to obtain the SIBS elastomer.

[0089] 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.

[0090] In the present disclosure, in step (A), the raw material is a crude purchased raw material, and the main impurities are irregular fine particles and moisture.

[0091] In the present disclosure, in step (A), after purification, the purity of 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.

[0092] In the present disclosure, in step (B), an auxiliary agent selected from the following group is prepared for use: an initiator, a coupling agent, a coupling agent, an activator, and a terminator.

[0093] In the present disclosure, the initiator includes, but is not limited to, butyllithium, Grignard reagent, and n-BuLi.

[0094] In the present disclosure, the coupling agent includes, but is not limited to: tetrachlorosilane, DVB (divinylbenzene), and tin tetrachloride.

[0095] In the present disclosure, the coupling agent includes, but is not limited to: dichlorodimethylsilane.

[0096] In the present disclosure, the activating agent includes, but is not limited to, tetrahydrofuran (THF).

[0097] In the present disclosure, the terminator includes, but is not limited to: methanol and ethanol.

[0098] In the present disclosure, in step (B), except for the activator, the auxiliary agents must be prepared into a cyclohexane solution and added to the polymerization system.

[0099] In the present disclosure, in step (C), the microchannel reactor is laid out in a pipeline type, which increases the reaction contact area by 5-30 times under the same floor space, effectively increasing the residence time of raw materials and additives in the microchannel reactor and prolonging the polymerization reaction time.

[0100] In the present disclosure, in step (C), by replacing the reactor with a microchannel reactor, the SIBS preparation process is changed from an intermittent process to a continuous process, and the feeding, reaction, and discharge are carried out continuously, thereby increasing the preparation efficiency by 2-10 times.

[0101] In the present disclosure, in step (C), the raw materials are added in steps. After being preheated, the refined cyclohexane is first added to the microchannel reactor, and then the refined styrene, refined butadiene and refined isoprene are added in sequence.

[0102] In the present disclosure, in step (C), the concentration of the obtained SIBS glue is 15-20%, for example, 15%, 16%, 17%, 18%, 19%, or 20%.

[0103] In the present disclosure, in step (C), the weight ratio of refined styrene, refined butadiene, refined isoprene, refined cyclohexane and the auxiliary agent is 1:1.5:8:25:1.

[0104] In the present disclosure, in step (C), the polymerization reaction process pressure is controlled at 0.03-0.19 MPa, for example, 0.03 MPa, 0.05 MPa, 0.07 MPa, 0.09 MPa, 0.11 MPa, 0.13 MPa, 0.15 MPa, 0.17 MPa, 0.19 MPa, preferably 0.05-0.15 MPa.

[0105] In the present disclosure, in step (C), the polymerization reaction process temperature is controlled at 50-130°C, for example, 50°C, 60°C, 70°C, 80°C, 90°C, 100°C, 110°C, 120°C, 130°C, preferably 50°C to 110°C.

[0106] In the present disclosure, in step (C), the polymerization reaction process is an intermittent operation unit, and the production time of each batch of a single microchannel reactor is about 0.8 to 2 hours, for example, 0.8 hours, 1.0 hours, 1.2 hours, 1.4 hours, 1.6 hours, 1.8 hours, 2.0 hours, preferably 1.6 hours.

[0107] In the present disclosure, in step (C), multiple microchannel separators may be arranged in series to further increase the reaction contact area and improve the processing capacity.

[0108] In the present disclosure, in step (C), the crude styrene conversion rate can reach 99.1%, and the crude isoprene conversion rate can reach 99.75%.

[0109] In the present disclosure, in step (C), the concentration of the obtained SIBS glue is 15-20%, for example, 15%, 16%, 17%, 18%, 19%, or 20%.

[0110] In the present disclosure, after steps (D), (E) and (F), a glue solution with a solid content of 30-50% is obtained.

[0111] In the present disclosure, in step (G), the non-phase-change drying process operates at a pressure of 0.1 MPa to 0.3 MPa.

[0112] In the present disclosure, in step (G), the energy consumption of the non-phase-change drying system is approximately 1 / 5 to 1 / 15 of that of the heating phase-change evaporation.

[0113] In the present disclosure, the melt index of the obtained SIBS elastomer is 0.1 to 30.0, and the molecular weight of the elastomer is 70,000 to 150,000.

[0114] In a second aspect of the present disclosure, a SIBS microchannel reaction device is provided, comprising:

[0115] A monomer refining unit consisting of a microchannel reactor and a shape coalescer connected thereto is used to carry out the monomer refining based on the microchannel separator and the shape coalescer in step (A): crude styrene, crude isoprene, crude butadiene and crude cyclohexane raw materials are added to the monomer refining unit consisting of the microchannel separator and the shape coalescer to remove impurities therein to obtain refined raw materials;

[0116] A microchannel reactor connected to the shape coalescer, a glue buffer tank connected to the microchannel reactor, and a micro-droplet extraction tank connected to the glue buffer tank are used to perform microchannel reactor polymerization in step (C): the refined raw material obtained in step (A) and the auxiliary agent prepared in step (B) are added to the microchannel reactor, and after the reaction is completed, the generated glue is added to the glue buffer tank, and then extracted by a micro-droplet extraction tank containing an antioxidant;

[0117] The dynamic blending tank connected to the micro-droplet extraction tank is used to perform the cyclone dynamic mixing and blending in step (D): the extracted rubber solution obtained in step (C) is added to the dynamic blending tank and stirred and blended uniformly;

[0118] The cyclone classification separator connected to the dynamic blending tank is used to perform cyclone classification separation in step (E): adding the uniformly blended glue obtained in step (D) to the cyclone classification separator, and adopting cyclone separation method to perform glue coagulation; and

[0119] The non-phase-change drying system connected to the cyclone classifier and the packaging system connected to the non-phase-change drying system are used to perform the non-phase-change cyclone drying treatment in step (G): the condensed colloid particles obtained in step (E) are added to the non-phase-change drying system, and the colloid particles are dried and fed to the final packaging to obtain the SIBS elastomer.

[0120] In the present disclosure, the monomer refining unit includes: a styrene refining unit, a butadiene refining unit, an isoprene refining unit, and a cyclohexane refining unit.

[0121] In the present disclosure, in the styrene refining unit, crude styrene is separated into solid and liquid by a microchannel separator, and the separated styrene is separated into oil and water by a shape coalescer before entering a microchannel reactor.

[0122] In the present disclosure, the device further comprises: a refining tower connected to the butadiene refining unit, a condensation reflux system (consisting 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;

[0123] a deweighting column connected to the isoprene refining unit, a condensation reflux system (consisting of a condenser and a reflux tank) connected to the deweighting column, and a product tank connected to the condensation reflux system; and

[0124] Two condensation reflux systems connected to the cyclohexane refining unit in series, and a refining agent tank connected to the condensation reflux system.

[0125] In the present disclosure, in a butadiene refining unit, crude butadiene passes through a microchannel separator for solid-liquid separation, and then passes through a shape coalescer for oil-water separation. The resulting 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.

[0126] In the present disclosure, in the isoprene refining unit, crude isoprene passes through a microchannel separator for solid-liquid separation, and then passes through a shaped coalescer for oil-water separation. The resulting product sequentially enters a de-weighting column connected to the isoprene refining unit, a condensation reflux system connected to the de-weighting column, and a product tank connected to the condensation reflux system, and then enters a microchannel reactor connected to the product tank.

[0127] In the present disclosure, in a cyclohexane refining unit, crude cyclohexane passes through a microchannel separator for solid-liquid separation, and then passes through a shape coalescer for oil-water separation. The resulting product then enters two condensation and reflux systems connected to the cyclohexane refining unit, followed by a refined solvent tank connected to the condensation and reflux systems, and then enters a microchannel reactor connected to the refined solvent tank.

[0128] In the present disclosure, the auxiliary agent is added into the channel reactor.

[0129] In the present disclosure, the refined raw materials and additives undergo polymerization reaction in a microchannel reactor to obtain SIBS products.

[0130] In the present disclosure, the concentration of the obtained SIBS product is further increased through glue blending, coagulation, and solution refining.

[0131] In the present disclosure, the refined SIBS product is sent to the final packaging system after post-processing in a non-phase change drying system.

[0132] Please refer to the accompanying drawings below.

[0133] Figure 1 FIG. 1 is a schematic diagram of the overall process flow of the SIBS microchannel reaction method according to a preferred embodiment of the present disclosure. Figure 1As shown, crude styrene, crude butadiene, crude isoprene, and crude cyclohexane raw materials are respectively added to a styrene refining unit, a butadiene refining unit, an isoprene refining unit, and a cyclohexane refining unit consisting of a microchannel separator 1 and a shape coalescer 2 connected thereto; wherein, the styrene produced in the styrene refining unit is directly pumped from its shape coalescer 2 to the microchannel reactor 3; the butadiene produced in the butadiene refining unit is pumped from its shape coalescer 2 to the refining tower 10, the refined light component is 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 refined heavy component is discharged from the bottom of the refining tower 10 and sent to the heavy component storage tank 14, the refined butadiene is sent to the reflux tank 13, the reflux is refluxed 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 in the isoprene refining unit is pumped from its shape coalescer 2 to the deweighting tower 16 The heavy components are removed, and the light components are discharged from the top of the de-weighting tower 16 and sent to the condenser 11 for condensation and then sent to the reflux tank 13. Part of the components are refluxed to the de-weighting tower 16, and 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, and the light components obtained by the refinement 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 sent to the cyclohexane product tank 17, and then pumped to the microchannel reactor 3; the cyclohexane produced by the cyclohexane refining unit is sent from the shape coalescer 2 to the refining tower 10-1, and the light components obtained by the refinement 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 top of the reflux tank 13 is discharged and sent to the condenser 11 for condensation and then sent to the refined solvent tank 18. Part of the components are refluxed to the refining tower 10-1, and the cyclohexane is sent to the refining tower 10-2 to remove the heavy components at the bottom of the tower. 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 refluxed to the refining tower 10-2, and the cyclohexane is sent to the refined solvent tank 18, and then pumped to the microchannel reactor 3; at the same time, the additive is added to the microchannel reactor 3;

[0134] The glue produced by the microchannel reactor groups 3-1, 3-2, 3-3, and 3-4 is sent to the glue buffer tank 4, and then extracted by the micro-droplet extraction tank 5 containing an antioxidant. The gas phase is discharged from the top of the glue buffer tank 4 and sent to the separation tank 19. The separated gas phase is sent to the tail gas condenser 20. The condensed liquid phase is sent to the shape coalescer 2 and then refined and sent to the cyclone classifier 7 for separation. The obtained product is sent to the reflux tank 13, and then screened by the dehydration screen 24 and sent to the dehydration extruder 22 for extrusion and then sent to the non-phase change drying system 8 to achieve the removal of moisture on the surface and in the pores of the glue particles, and the residual water is removed by RTO treatment. The pellets in the product packaging silo are The final SIBS product is obtained by entering the packaging system 9 for metering, sewing, sealing, metal inspection, re-inspection, palletizing, and storage of finished products; the slag liquid discharged from the separation tank 19 is sent to the shape coalescer 2; the glue liquid extracted by the micro-droplet extraction tank 5 enters the dynamic blending tank 6, and after stirring and blending, the gas phase is discharged from the top and sent to the tail gas condenser 20. The liquid phase is mixed by the stripping unit mixer 29 and then enters the cyclone classification separator 7 for cyclone separation of glue particles; the water removed by the dewatering screen 24 and the dewatering extruder 22 is sent to the hot water tank 23 and then to the shape coalescer 2; the hot water in the hot water tank 23 is added with dispersant and returned to the stripping unit mixer 29.

[0135] Figure 2 FIG is a schematic structural diagram of a microchannel separator according to a preferred embodiment of the present disclosure. Figure 2 As shown, the microchannel separator includes: a coolant outlet 101, a separation chamber 102, a liquid outlet 103, a baffle 104, a flame barrier insert 105, a separation platform 106, a coolant outlet 107, a coolant base 108, a reaction passage 109, a coolant passage 110, a gas passage 111, a passage pipe 112, a coolant feed 113, a coolant feed 114, a flame barrier insert 115, a gas feed 116, a liquid feed 117, and a liquid feed 118.

[0136] Example

[0137] The present invention will be further described below with reference to specific examples. However, it should be understood that these examples are intended to illustrate the present invention only and are not intended to limit the scope of the invention. The test methods in the following examples, where specific conditions are not specified, were generally performed under conventional conditions or as recommended by the manufacturer. Unless otherwise indicated, all percentages and parts are by weight.

[0138] Example 1:

[0139] 1. Device Name

[0140] 40kg / h elastomer pilot production unit

[0141] 2. Process

[0142] like Figure 1 shown.

[0143] The material addition control ratio is shown in Table 1 below.

[0144] Table 1: Material addition control ratio

[0145]

[0146] 3. Implementation Effect

[0147] The process analysis data are shown in Table 2 below.

[0148] Table 2: Process analysis data

[0149]

[0150]

[0151] The above analysis data shows that the method of the present invention achieves all process parameters that meet control requirements, and the finished rubber product also meets the physical and chemical indicators required by the market. The finished rubber yield reaches over 99%, the isoprene conversion rate reaches 99.5%, the styrene conversion rate reaches 99.5%, and the butadiene conversion rate reaches 99.3%.

[0152] The above-listed embodiments are merely preferred embodiments of the present disclosure and are not intended to limit the scope of implementation of the present disclosure. That is, any equivalent changes and modifications made based on the content of the patent application should fall within the technical scope of the present disclosure.

[0153] All documents mentioned in this disclosure are incorporated herein by reference, just as if each document were incorporated herein by reference individually. It should also be understood that after reading the above teachings of this disclosure, those skilled in the art may make various changes or modifications to this disclosure, and that such equivalents also fall within the scope of the claims appended hereto.

Claims

1. A SIBS microchannel reaction method, the method comprising the following steps: (A) Monomer Refining Based on a Microchannel Separator and Shape Coalescer: Crude styrene, crude isoprene, crude butadiene, and crude cyclohexane raw materials are added to a monomer refining unit composed of a microchannel separator and a shape coalescer to remove impurities therein and obtain refined raw materials; (B) auxiliary agent configuration; (C) Microchannel reactor polymerization: the refined raw material obtained in step (A) and the auxiliary agent prepared in step (B) are added to a microchannel reactor. After the reaction is completed, the generated glue is added to a glue buffer tank, and then extracted by a micro-droplet extraction tank containing an antioxidant; wherein the microchannel reactor is a pipeline type. (D) Cyclone dynamic mixing and blending: adding the extracted rubber solution obtained in step (C) into a dynamic blending tank and stirring and blending uniformly; (E) Cyclone fractionation: adding the uniformly mixed glue obtained in step (D) into a cyclone fractionation separator, and using cyclone separation to agglomerate the glue; (F) solution purification: refluxing and refining the solvent used in the cyclone fractionator in step (E); and (G) Non-phase-change cyclone drying treatment: The condensed particles obtained in step (E) are added to a non-phase-change drying system. After drying, the particles are fed to the final packaging to obtain the SIBS elastomer.

2. The method according to claim 1, wherein 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; 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.

3. The method according to claim 1, wherein In step (B), auxiliary agents selected from the group consisting of an initiator, a coupling agent, a coupling agent, an activator, and a terminator are prepared for use.

4. The method according to claim 1, wherein In step (C), the raw materials are added in steps. After being preheated, the refined cyclohexane is first added to the microchannel reactor, and then the refined styrene, refined butadiene and refined isoprene are added in sequence.

5. The method according to claim 1, wherein In step (C), the weight ratio of refined styrene, refined butadiene, refined isoprene, refined cyclohexane and the auxiliary agent is 1:1.5:8:25:1; the reaction pressure is 0.03-0.5 MPa, and the reaction temperature is 50-130°C.

6. The method according to claim 1, wherein In step (C), multiple microchannel separators are arranged in series; the production time of each batch of a single microchannel reactor is 0.8 to 2 hours.

7. The method according to claim 1, wherein In step (C), the crude styrene conversion rate reaches 99.1%, the crude isoprene conversion rate reaches 99.75%, and the concentration of the obtained SIBS glue is 15-20%.

8. The method according to claim 1, wherein After steps (D), (E) and (F), a glue solution with a solid content of 30-50% is obtained; in step (G), the non-phase change drying system is a mechanical + cyclonic non-phase change drying system, and the operating pressure is 0.1MPa-0.3MPa; the obtained SIBS elastomer has a melt index of 0.1-30.0 and a molecular weight of 70,000-150,000.

9. A SIBS microchannel reaction device, comprising: A monomer refining unit consisting of a microchannel separator (1) and a shape coalescer (2) connected thereto is used to carry out step (A) of monomer refining based on the microchannel separator and the shape coalescer: crude styrene, crude isoprene, crude butadiene and crude cyclohexane raw materials are added to the monomer refining unit consisting of the microchannel separator and the shape coalescer to remove impurities therein and obtain refined raw materials; A microchannel reactor (3) connected to the shape coalescer (2), a glue buffer tank (4) connected to the microchannel reactor (3), and a micro-droplet extraction tank (5) connected to the glue buffer tank (4) are used to carry out step (C) microchannel reactor polymerization: the refined raw material obtained in step (A) and the auxiliary agent configured in step (B) are added to the microchannel reactor, and after the reaction is completed, the generated glue is added to the glue buffer tank, and then extracted through a micro-droplet extraction tank containing an antioxidant; wherein the microchannel reactor (3) is a pipeline type laying; The dynamic blending tank (6) connected to the micro-droplet extraction tank (5) is used to perform the cyclone dynamic mixing and blending in step (D): adding the extracted glue obtained in step (C) into the dynamic blending tank, stirring and blending uniformly; The cyclone classification separator (7) connected to the dynamic blending tank (6) is used to perform the cyclone classification separation in step (E): adding the uniformly blended glue obtained in step (D) into the cyclone classification separator, and adopting the cyclone separation method to perform glue coagulation; and The non-phase-change drying system (8) connected to the cyclone classifier (7) and the packaging system (9) connected to the non-phase-change drying system (8) are used to perform the non-phase-change cyclone drying treatment in step (G): the condensed colloid particles obtained in step (E) are added to the non-phase-change drying system, and the colloid particles are dried and fed to the final packaging to obtain the SIBS elastomer.

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