Method and apparatus for refining sibs monomers

Abstract

The present disclosure relates to a SIBS monomer refining method and device, and provides a SIBS monomer refining method, which comprises the following steps: (A) monomer refining based on a micro-channel separator and a shape coalescer; (B) auxiliary agent configuration; (C) micro-channel reactor polymerization; (D) cyclone dynamic mixing blending; (E) cyclone classification separation; (F) solution refining; and (G) non-phase change cyclone drying treatment. The method simplifies the SIBS preparation process, reduces the device cost, reduces the floor area, realizes the continuous production process, reduces the operation cost, effectively improves the raw material refining purity, thereby improves the product quality and increases the yield.

Description

TECHNICAL FIELD

[0001] The present disclosure belongs to the technical field of high polymer materials, and relates to a monomer efficient refining method and device for SIBS micro-channel separator and shape coalescer, in particular to a method and device for refining raw material monomers in the preparation process of SIBS. BACKGROUND

[0002] The novel thermoplastic elastomer SIBS (i.e. integrated elastomer) is composed of styrene, isoprene and butadiene tetra-block copolymer, the middle block is polyisoprene, and it has a methyl side chain in structure, so it has good cohesion, excellent adhesion and good compatibility. Such microstructure determines that it has outstanding advantages when applied to adhesives, and is widely used in hot melt pressure sensitive adhesive, coating, plastic modification and other fields. In recent years, China has provided strong support for the high polymer material or emerging adhesive industry, and the sales volume of hot melt adhesive in China has broken through year after year, with a staggering number. In 2021, the sales volume of the hot melt adhesive industry in China can 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. However, the traditional SIBS preparation process pays less attention to the raw material refining unit, and the raw materials such as styrene and isoprene are generally purchased as crude products in the preparation process. The traditional refining method cannot maximize the purity of the monomer, and the refining process is incomplete and insufficient, thereby reducing the quality of SIBS products and increasing energy consumption. Therefore, in order to ensure the efficiency and quality of monomer refining, a new method is needed to improve the monomer refining process.

[0003] Chinese patent CN 211561936 U discloses a dehydration device and refining system for organic solvents, which achieves dehydration and refining of organic solvents through a series of condenser devices and a circulating dehydration process. However, this method has a complex process flow, cannot realize the classification of particles, and cannot separate ionic impurities in the monomer.

[0004] Chinese patent application CN 1119851255 A discloses an organic solvent refining system and method, which achieves the purpose of refining by distilling the organic solvent recovered from the vacuum evaporation tank through a pervaporation device and a vacuum evaporation tank, and then through a distillation device. However, this system has a complex process, high cost and high operating cost, and cannot easily integrate into the current SIBS preparation system.

[0005] Therefore, in view of the defects in the prior art, there is an urgent need in the art for an efficient and comprehensive SIBS monomer refining technology to achieve sufficient solid-liquid separation and oil-water separation of organic monomers and improve the refining purity. SUMMARY

[0006] The present disclosure provides a novel SIBS monomer refining method and device, thereby solving the problem of complicated production steps and discontinuous production in the existing SIBS preparation process.

[0007] In one aspect, the present disclosure provides a SIBS monomer refining method, which comprises the following steps:

[0008] (A) Monomer refining based on micro-channel 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 micro-channel separator and a shape coalescer to remove impurities therein, to obtain refined raw materials;

[0009] (B) Additive configuration;

[0010] (C) Micro-channel reactor polymerization: the refined raw materials obtained in step (A) and the additives configured in step (B) are added to a micro-channel reactor, and after the reaction is completed, the produced gum solution is added to a gum solution buffer tank, and then extracted through a micro-liquid droplet extraction tank containing an antioxidant;

[0011] (D) Cyclone dynamic mixing blending: the extracted gum solution obtained in step (C) is added to a dynamic blending tank, and stirred and blended uniformly;

[0012] (E) Cyclone classification separation: the uniformly blended gum solution obtained in step (D) is added to a cyclone classification separator, and cyclone separation is performed for gum solution coagulation;

[0013] (F) Solution refining: the solvent used in the cyclone classification separator in step (E) is subjected to reflux refining; and

[0014] (G) Non-phase change cyclone drying treatment: the coagulated gum particles obtained in step (E) are added to a non-phase change drying system, and after the gum particles are dried, they are fed to the final packaging to obtain SIBS elastomers.

[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 98.5% or higher, and the water content is reduced to 20 ppm or less, based on the weight of the crude styrene and crude isoprene raw materials.

[0017] In another preferred embodiment, in step (A), the micro-channel separator contains three different separation processes of molecular adsorption, ion extraction, and particle filtration and interception, to remove pollutants molecules, ions, and solid particles to different degrees.

[0018] In another preferred embodiment, in step (B), the auxiliary agent is prepared by adding the initiator, coupling agent, coupling agent, activator, and terminator.

[0019] In another preferred embodiment, in step (C), the raw materials are added in a stepwise manner, and the refined cyclohexane is first added to the microchannel reactor, followed by the addition of refined styrene, refined butadiene, and refined isoprene; the concentration of the obtained SIBS glue liquid is 15-20%.

[0020] In another preferred embodiment, in step (C), the refined styrene, refined butadiene, refined isoprene, and refined cyclohexane are added in a ratio of 1:1.5:8:25:1; the reaction pressure of the microchannel reactor is 0.05-0.5 MPa, the reaction temperature is 50-130°C, and the reaction time is 20-110 min.

[0021] In another preferred embodiment, after steps (D), (E), and (F), a glue liquid with a solid content of 30-50% is obtained.

[0022] In another preferred embodiment, in step (G), the non-phase change drying system has a sorting function, and different molecular weight glue particle materials are obtained by controlling the carrier gas temperature; the non-phase change drying system uses low-temperature drying means, and when the carrier gas temperature is 40-60°C, the moisture content of the dried glue particles is reduced from 90% to 3-10%; the operating pressure of the non-phase change drying process is 0.1-0.3 MPa; the obtained SIBS elastomer has a melt index of 0.1-30.0 and an elastomer molecular weight of 70-150 thousand.

[0023] In another aspect, the present disclosure provides a SIBS monomer refining device, which comprises:

[0024] A monomer refining unit composed of a microchannel reactor and a shape coalescer connected thereto is used to perform step (A) of monomer refining based on a microchannel separator and a shape coalescer: crude styrene, crude isoprene, crude butadiene, and crude cyclohexane raw materials are added to the monomer refining unit composed of a microchannel separator and a shape coalescer to remove impurities therein, obtaining refined raw materials;

[0025] A microchannel reactor connected to the shape coalescer, a glue liquid buffer tank connected to the microchannel reactor, and a micro-liquid droplet extraction tank connected to the glue liquid buffer tank are used to perform step (C) of microchannel reactor polymerization: the refined raw materials 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 glue liquid produced is added to the glue liquid buffer tank, and then extracted through the micro-liquid droplet extraction tank containing an antioxidant;

[0026] A dynamic mixing tank connected with the micro-droplet extraction tank, used for carrying out the step (D) dynamic mixing and mixing: the extracted glue liquid obtained in the step (C) is added into the dynamic mixing tank, and stirred and mixed uniformly;

[0027] A cyclone classifier connected with the dynamic mixing tank, used for carrying out the step (E) cyclone classification: the uniformly mixed glue liquid obtained in the step (D) is added into the cyclone classifier, and the glue liquid is coagulated by using the cyclone separation method; and

[0028] A non-phase change drying system connected with the cyclone classifier, and a packaging system connected with the non-phase change drying system, used for carrying out the step (G) non-phase change cyclone drying treatment: the coagulated glue particles obtained in the step (E) are added into the non-phase change drying system, and the glue particles are dried and then fed to the final packaging to obtain the SIBS elastomer.

[0029] Advantages:

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

[0031] (1) The method of the present disclosure can realize the continuous preparation of SIBS, simplify the process, reduce the cost of the device and reduce the floor area. The existing preparation method is mostly discontinuous, and the mixing of raw materials and additives in the reaction kettle needs to be carried out in stages. After a part of the feed is completely reacted, the next batch of feed is reacted, which leads to low efficiency of the method and uneven mixing of raw materials. The method of the present disclosure replaces the reaction kettle with a micro-channel reactor, which provides a large reaction contact area for the long-distance pipeline facilities, ensuring the sufficient mixing of raw materials and additives; at the same time, the continuous preparation process can be realized, and the preparation efficiency is improved by 2-5 times.

[0032] (2) By using a micro-channel separator to replace the original rectifying column, the precision of the raw materials is improved, and the service life of the device is prolonged, and the consumption of the filler layer is reduced. The micro-channel separator contains three different mechanisms of separation process, namely molecular adsorption, ion extraction and particle filtration and interception. The three mechanisms have different degrees of removal effect on pollutant molecules, ions and solid particles, so that the separation precision of fine particles can be pushed to 100 nm, and the volume precision is improved by two orders of magnitude, and the removal rate of 100 nm pollutants is > 90%. Compared with the adsorption filler of the existing device, the micro-channel separator has a backwashing function, which can wash the filler and continue to use, prolong the service life of the device and reduce the consumption of the filler layer.

[0033] (3) The use of shape coalescer can effectively reduce energy consumption, and the use of material adsorption can reduce operation cost. The traditional raw material refining method mainly uses the difference in boiling point of raw material and water to evaporate and remove water to refine the raw material, but this method consumes a lot of energy. By using shape coalescer, the combined water is adsorbed by the coalescing material, and then a small amount of hot air is used for drying, and the energy consumption is reduced by 1 / 5-1 / 10; after the coalescing material is saturated, the coalescing material is regenerated to be continuously used, which reduces the operation cost and energy consumption. BRIEF DESCRIPTION OF DRAWINGS

[0034] The accompanying drawings are included to provide a further understanding of the present disclosure and are incorporated in and constitute a part of this specification, illustrate embodiments of the present disclosure and together with the description serve to explain the principles of the present disclosure.

[0035] Figure 1 It is a SIBS monomer refining method overall process flow diagram according to one preferred embodiment of the present disclosure.

[0036] Figure 2 It is a structure schematic diagram of a micro-channel separator according to one preferred embodiment of the present disclosure.

[0037] Figure 3 It is a structure schematic diagram of a shape coalescer according to one preferred embodiment of the present disclosure.

[0038] Reference signs:

[0039] 1: micro-channel separator

[0040] 2: shape coalescer

[0041] 3: micro-channel reactor (3-1, 3-2, 3-3, 3-4)

[0042] 4: glue liquid buffer tank

[0043] 5: micro-droplet extraction tank

[0044] 6: dynamic blending tank

[0045] 7: cyclone classifier

[0046] 8: non-phase change drying system

[0047] 9: packaging system

[0048] 10: refining tower (10-1, 10-2)

[0049] 11: condenser

[0050] 12: intermediate tank

[0051] 13: reflux tank

[0052] 14: Recycle storage tank

[0053] 15: Butadiene product tank

[0054] 16: Deheavy column

[0055] 17: Isoprene product tank

[0056] 18: Refined solvent tank

[0057] 19: Split tank

[0058] 20: Off gas condenser

[0059] 21: Stripper unit mixer

[0060] 22: Dehydrating extruder

[0061] 23: Hot water tank

[0062] 24: Dehydrating screen

[0063] 101: Gas phase outlet

[0064] 102: Mixed inlet

[0065] 103: Internal cyclone

[0066] 104: Check cone

[0067] 105: Liquid phase outlet

[0068] 106: Pressure control port

[0069] 107: Support leg

[0070] 108: Gas phase inlet

[0071] 109: Liquid phase inlet

[0072] 202: Water outlet

[0073] 203: First screen

[0074] 204: Second screen

[0075] 205: Third screen

[0076] 206: Gas phase inlet

[0077] 207: Pipe

[0078] 208: Water inlet

[0079] 209: Filter cartridge DETAILED DESCRIPTION

[0080] The endpoints of the ranges and any values disclosed herein are not limited to the precise values recited as the exact dimensions are not critical to the invention. Any numeric range recited is intended to include all values from the lower value to the upper value, inclusive of both values, and to sub-ranges falling within the specified range. In this context, individual points within a range should not be dismissed from the range merely because these points were not recited.

[0081] The applicant of the present application found through extensive and in-depth research that, in view of the defects of incompleteness and insufficiency of the existing monomer refining method, the present disclosure provides a SIBS micro-channel separator and a shape coalescer monomer efficient refining method to efficiently and high-quality improve the purity of raw materials, thereby improving the quality of SIBS products and increasing the yield of products. Based on the above findings, the present application is completed.

[0082] The technical concept of the present application is as follows:

[0083] The micro-channel separator is based on the micro-channel pulsation oscillation separation technology to improve the separation precision; the shape coalescer replaces the heating separation mode by adsorption of coalescence materials, greatly reducing the energy consumption; at the same time, based on the monomer efficient refining method, the purity of the raw material refining is effectively improved, thereby improving the product quality and increasing the yield.

[0084] In a first aspect of the present disclosure, a SIBS monomer refining method is provided, which comprises the following steps:

[0085] (A) Monomer refining based on micro-channel 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 micro-channel separator and a shape coalescer to remove impurities therein, to obtain refined raw materials;

[0086] (B) Additive configuration;

[0087] (C) Micro-channel reactor polymerization: the refined raw materials obtained in step (A) and the additives configured in step (B) are added to a micro-channel reactor, and after the reaction is completed, the produced glue liquid is added to a glue liquid buffer tank, and then extracted through a micro-liquid drop extraction tank containing an antioxidant;

[0088] (D) Swirl dynamic mixing blending: the extracted glue liquid obtained in step (C) is added to a dynamic blending tank, and stirred and blended uniformly;

[0089] (E) Swirl fractional separation: the uniformly blended glue liquid obtained in step (D) is added to a swirl fractional separator, and glue liquid coagulation is carried out by adopting a swirl separation method;

[0090] (F) Solution refining: the solvent used in the swirl fractional separator in step (E) is subjected to reflux refining; and

[0091] (G) Non-phase change cyclone drying process: the condensed micelles obtained in step (E) are added to a non-phase change drying system, and the micelles are dried and then fed to final packaging to obtain SIBS elastomers.

[0092] In the present disclosure, in step (A), the weight ratio of the crude styrene, crude isoprene, crude butadiene and crude cyclohexane is 1:1-10:1.5-20:25-30, preferably 1:8:1.5:25.

[0093] 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.

[0094] In the present disclosure, in step (A), after refining, the purity of the crude styrene and crude isoprene is increased to 98.5% or more, and the water content is reduced to 20 ppm or less, based on the weight of the crude styrene and crude isoprene raw material.

[0095] In the present disclosure, in step (A), the microchannel separator contains three different mechanisms of separation process, namely molecular adsorption, ion extraction and particle filtration and interception, and the three mechanisms have different degrees of removal effect on pollutant molecules, ions and solid particles, so as to achieve the purpose of sufficient removal.

[0096] In the present disclosure, in step (A), the main method for refining the raw material in the traditional method is to use the difference in boiling point between the raw material and moisture to evaporate and remove the moisture to refine the raw material, but this method consumes a lot of energy. By using the shape coalescer instead, the coalescing material is used to adsorb the combined water, and only the coalescing material needs to be regenerated after saturation, greatly reducing the energy consumption.

[0097] In the present disclosure, in step (B), an auxiliary agent selected from the group consisting of initiators, coupling agents, coupling agents, activators, and terminating agents is configured.

[0098] In the present disclosure, the initiator includes, but is not limited to, butyllithium, Grignard reagent, n-BuLi.

[0099] In the present disclosure, the coupling agent includes, but is not limited to, tetrachlorosilane, DVB (divinylbenzene), and tin tetrachloride.

[0100] In the present disclosure, the coupling agent includes, but is not limited to, dichlorodimethylsilane.

[0101] In the present disclosure, the activator includes, but is not limited to, tetrahydrofuran (THF).

[0102] In the present disclosure, the terminating agent includes, but is not limited to, methanol, ethanol.

[0103] In the present disclosure, in step (B), the auxiliary agents are formulated into a cyclohexane solution and added into the polymerization system.

[0104] In the present disclosure, in step (C), the raw materials are added into the microchannel reactor in a stepwise manner after the refined cyclohexane is preheated, and then the refined styrene, refined butadiene and refined isoprene are added in sequence.

[0105] In the present disclosure, in step (C), the concentration of the obtained SIBS glue solution is 15-20%, for example, 15%, 16%, 17%, 18%, 19% or 20%.

[0106] In the present disclosure, in step (C), the weight ratio of the refined styrene, refined butadiene, refined isoprene, refined cyclohexane and auxiliary agent is 1:1.5:8:25:1; the reaction pressure of the microchannel reactor is 0.05-0.5 MPa, the reaction temperature is 50-130℃, and the reaction time is 20-110 min.

[0107] In the present disclosure, after steps (D), (E) and (F), a glue solution with a solid content of 30-50% is obtained.

[0108] In the present disclosure, in step (G), the non-phase-change drying system has a sorting function, and different molecular weight of glue particle materials are obtained by controlling the temperature of the carrier gas; the non-phase-change drying system utilizes the rapid oscillation generated by the pulsating rotation of the sludge in the cyclone to change the properties of the sludge surface and the water phase contact interface, and to strengthen the dehydration process; the non-phase-change drying system uses low-temperature drying means, and when the temperature of the carrier gas is 40-60℃, the water content of the dried glue particles is reduced from 90% to 3-10%; the operating pressure of the non-phase-change drying process is 0.1-0.3 MPa.

[0109] In the present disclosure, in step (G), the energy consumption of the non-phase-change drying system is about 1 / 5-1 / 15 of that of the heating phase-change evaporation.

[0110] In the present disclosure, the obtained SIBS elastomer has a melt index of 0.1-30.0 and an elastomer molecular weight of 70-150 thousand.

[0111] Unlike the traditional intermittent SIBS production method, the production process of the present disclosure is continuous from the raw materials to the SIBS product.

[0112] In the second aspect of the present disclosure, a monomer refining device is provided, which comprises:

[0113] The monomer refining unit composed of a micro-channel reactor and a shape coalescer connected thereto is used for carrying out the step (A) monomer refining based on a micro-channel separator and a shape coalescer: the crude styrene, crude isoprene, crude butadiene and crude cyclohexane raw materials are added into the monomer refining unit composed of a micro-channel separator and a shape coalescer to remove impurities therein to obtain refined raw materials;

[0114] The micro-channel reactor connected with the shape coalescer, the latex buffer tank connected with the micro-channel reactor and the micro-droplet extraction tank connected with the latex buffer tank are used for carrying out the step (C) micro-channel reactor polymerization: the refined raw materials obtained in the step (A) and the auxiliary agent configured in the step (B) are added into the micro-channel reactor, the produced latex is added into the latex buffer tank after the reaction is completed, and the extraction is carried out through the micro-droplet extraction tank containing the antioxidant;

[0115] The dynamic blending tank connected with the micro-droplet extraction tank is used for carrying out the step (D) dynamic mixing and blending of cyclone: the extracted latex obtained in the step (C) is added into the dynamic blending tank, and the stirring and blending are uniform;

[0116] The cyclone classifier connected with the dynamic blending tank is used for carrying out the step (E) cyclone classification: the uniformly blended latex obtained in the step (D) is added into the cyclone classifier, and the latex coagulation is carried out by the cyclone separation method; and

[0117] The non-phase change drying system connected with the cyclone classifier and the packaging system connected with the non-phase change drying system are used for carrying out the step (G) non-phase change cyclone drying treatment: the coagulated latex particles obtained in the step (E) are added into the non-phase change drying system, and the latex particles are fed to the final packaging after being dried to obtain the SIBS elastomer.

[0118] In the present disclosure, the monomer refining unit comprises: a styrene refining unit, a butadiene refining unit, an isoprene refining unit and a cyclohexane refining unit.

[0119] In the present disclosure, in the styrene refining unit, the crude styrene is subjected to solid-liquid separation through a micro-channel separator, and the separated styrene is subjected to oil-water separation through a shape coalescer and then enters a micro-channel reactor.

[0120] In the present disclosure, the device further comprises: a refining column connected with the butadiene refining unit, a condensation reflux system (composed of a condenser, an intermediate tank and a reflux tank) and a heavy component storage tank connected with the refining column, and a butadiene product tank connected with the condensation reflux system;

[0121] A heavy component removal column connected with the isoprene refining unit, a condensation reflux system (composed of a condenser and a reflux tank) connected with the heavy component removal column, and a product tank connected with the condensation reflux system; and

[0122] Two condensing reflux systems connected in sequence with the cyclohexane refining unit, and a refining agent tank connected with the condensing reflux system.

[0123] In the present disclosure, in the butadiene refining unit, the crude butadiene is subjected to solid-liquid separation by a micro-channel separator, and then subjected to oil-water separation by a shape coalescer. The obtained product is sequentially introduced into a refining column connected with the butadiene refining unit, a condensing reflux system connected with the refining column and a heavy component storage tank, and a butadiene product tank connected with the condensing reflux system, and then introduced into a micro-channel reactor connected with the butadiene product tank.

[0124] In the present disclosure, in the isoprene refining unit, the crude isoprene is subjected to solid-liquid separation by a micro-channel separator, and then subjected to oil-water separation by a shape coalescer. The obtained product is sequentially introduced into a heavy component removal column connected with the isoprene refining unit, a condensing reflux system connected with the heavy component removal column, and a product tank connected with the condensing reflux system, and then introduced into a micro-channel reactor connected with the product tank.

[0125] In the present disclosure, in the cyclohexane refining unit, the crude cyclohexane is subjected to solid-liquid separation by a micro-channel separator, and then subjected to oil-water separation by a shape coalescer. The obtained product is sequentially introduced into two condensing reflux systems connected in sequence with the cyclohexane refining unit, and a refined solvent tank connected with the condensing reflux system, and then introduced into a micro-channel reactor connected with the refined solvent tank.

[0126] In the present disclosure, the auxiliary agent is added into the micro-channel reactor.

[0127] In the present disclosure, the refining raw material and the auxiliary agent are subjected to a polymerization reaction in the micro-channel reactor to obtain a SIBS product.

[0128] In the present disclosure, the obtained SIBS product is subjected to further concentration by glue solution blending, coagulation and solution refining.

[0129] In the present disclosure, the SIBS product after refining is subjected to post-treatment by a non-phase change drying system, and then sent to a final packaging system.

[0130] Reference is made to the accompanying drawings.

[0131] Figure 1 is a schematic diagram of the overall process flow of a SIBS monomer refining method according to one preferred embodiment of the present disclosure. As shown in Figure 1As shown, the crude styrene, crude butadiene, crude isoprene, crude cyclohexane raw materials are respectively added into the styrene refining unit, butadiene refining unit, isoprene refining unit, cyclohexane refining unit composed of micro-channel separator 1 and shape coalescer 2 connected therewith; wherein the styrene produced by the styrene refining unit is directly pumped from its shape coalescer 2 to the micro-channel reactor 3; the butadiene produced by the butadiene refining unit is pumped from its shape coalescer 2 to the refining column 10, the light components refined are discharged from the top of the refining column 10 and sent to the condenser 11 for condensation and then sent to the intermediate tank 12, the heavy components refined are discharged from the bottom of the refining column 10 and sent to the heavy component storage tank 14, the butadiene refined is sent to the reflux tank 13, the reflux is refluxed to the refining column 10, the butadiene is sent to the butadiene product tank 15 and then pumped to the micro-channel reactor 3; the isoprene produced by the isoprene refining unit is pumped from its shape coalescer 2 to the heavy component removal column 16, the light components are discharged from the top of the heavy component removal column 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 heavy component removal column 16, the isoprene is sent to the isoprene product tank 17 and then pumped to the micro-channel reactor 3; the cyclohexane produced by the cyclohexane refining unit is sent to the refining column 10-1 from its shape coalescer 2, the light components refined are discharged from the top of the refining column 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 refluxed to the refining column 10-1, the cyclohexane is sent to the refining column 10-2, the heavy components at the bottom are removed, the light components are discharged from the top of the refining column 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 column 10-2, the cyclohexane is sent to the refined solvent tank 18 and then pumped to the micro-channel reactor 3; at the same time, the auxiliary agent is added into the micro-channel reactor 3;

[0132] The glue solution produced by the micro-channel reactor groups 3-1, 3-2, 3-3, 3-4 is sent into the glue solution buffer tank 4, and then is extracted by the micro-liquid drop extraction tank 5 containing an antioxidant. The gas phase is discharged from the top of the glue solution buffer tank 4 and is sent into the separation tank 19. The gas phase separated from the separation tank 19 is sent into the tail gas condenser 20. The liquid phase condensed by the tail gas condenser 20 is sent into the shape coalescer 2, refined, and then sent into the cyclone classifier 7. The product is sent into the reflux tank 13, and then is screened by the dehydration screen 24, extruded by the dehydration extruder 22, and then is sent into the non-phase change drying system 8 to remove the water on the surface and in the pores of the glue particles. The residual water is sent to the RTO for treatment. The granules in the product packaging bin are sent into the packaging system 9 for metering, bagging, sealing, gold detection, re-detection, stacking, and storage. The final SIBS product is obtained. The residue liquid discharged from the separation tank 19 is sent into the shape coalescer 2. The glue solution extracted by the micro-liquid drop extraction tank 5 is sent into the dynamic mixing tank 6. After being stirred and mixed uniformly, the gas phase is discharged from the top of the dynamic mixing tank 6 and is sent into the tail gas condenser 20. The liquid phase is mixed by the stripping unit mixer 29 and is sent into the cyclone classifier 7 for cyclone separation of the glue particles. The water removed by the dehydration screen 24 and the dehydration extruder 22 is sent into the hot water tank 23 and then is sent into the shape coalescer 2. The hot water in the hot water tank 23 is returned to the stripping unit mixer 29 after adding a dispersing agent.

[0133] Figure 2 is a structural schematic diagram of a micro-channel separator according to one preferred embodiment of the present disclosure. As shown in Figure 2 , the micro-channel separator includes a gas phase outlet 101, a mixing inlet 102, an internal cyclone 103, a reverse cone 104, a liquid phase outlet 105, a pressure control port 106, a support foot 107, a gas phase inlet 108, and a liquid phase inlet 109.

[0134] Figure 3 is a structural schematic diagram of a shape coalescer according to one preferred embodiment of the present disclosure. As shown in Figure 3 , the shape coalescer 2 includes a water outlet 202, a first filter screen 203, a second filter screen 204, a third filter screen 205, a gas phase inlet 206, a pipeline 207, a water inlet 208, and a filter core 209.

[0135] Example

[0136] The present application is further described in conjunction with the specific examples. However, it should be understood that these examples are only used to illustrate the present application and do not constitute a limitation on the scope of the present application. In the following examples, the test methods not specified with specific conditions are generally performed according to the conventional conditions or the conditions suggested by the manufacturers. Unless otherwise specified, all percentages and parts are by weight.

[0137] Example 1

[0138] I. Device name 40kg / h elastomer pilot production device II. Process flow as shown in Figure 1

[0139] The material addition control ratio is shown in Table 1 below.

[0140] Table 1: Material addition control ratio

[0141]

[0142] III. Implementation effect

[0143] The process analysis data is shown in Table 2 below.

[0144] Table 2: Process analysis data

[0145]

[0146]

[0147] From the above analysis data, it can be seen that by using the method of the present application, each process index reaches the control requirement, and the produced finished product rubber also reaches the required physical and chemical indexes in the market. The yield of the finished product rubber reaches more than 99%, the isoprene conversion rate reaches 99.5%, the styrene conversion rate reaches 99.5%, and the butadiene conversion rate reaches 99.3%.

[0148] The above listed examples are merely the preferred embodiments of the present disclosure, and are not intended to limit the scope of the present disclosure. That is, equivalent changes and modifications made according to the content of the present application should all be within the technical scope of the present disclosure.

[0149] All the documents mentioned in the present disclosure are cited as references in the present application, as if each document is cited as a reference individually. In addition, it should be understood that those skilled in the art can make various changes or modifications to the present disclosure after reading the above teachings of the present disclosure, and these equivalent forms also fall within the scope defined by the claims of the present application.​

Claims

1. A method for refining SIBS monomers, comprising the following steps: (A) monomer refining based on micro-channel separator and shape coalescer: crude styrene, crude isoprene, crude butadiene and crude cyclohexane raw materials are fed into a monomer refining unit consisting of a micro-channel separator and a shape coalescer to remove impurities therein, to obtain refined raw materials; (B) auxiliary agent preparation; (C) micro-channel reactor polymerization: the refined raw materials obtained in step (A) and the auxiliary agent prepared in step (B) are fed into a micro-channel reactor, and after the reaction is completed, the produced latex is fed into a latex buffer tank, and then extracted through a micro-droplet extraction tank containing an antioxidant; (D) cyclone dynamic mixing blending: the extracted latex obtained in step (C) is fed into a dynamic blending tank, and stirred and blended uniformly; (E) cyclone classification separation: the uniformly blended latex obtained in step (D) is fed into a cyclone classification separator, and latex coagulation is carried out by cyclone separation; (F) solution refining: the solvent used in the cyclone classification separator in step (E) is subjected to reflux refining; and (G) non-phase change cyclone drying treatment: the coagulated latex particles obtained in step (E) are fed into a non-phase change drying system, and after the latex particles are dried, they are fed into final packaging to obtain SIBS elastomers. 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. In step (A), after refining, the purity of the crude styrene and crude isoprene is increased to 98.5% or higher, and the water content is reduced to 20 ppm or less, based on the weight of the crude styrene and crude isoprene raw materials. In step (A), the micro-channel separator contains three different separation processes of molecular adsorption, ion extraction, and particle filtration and interception to remove pollutants, ions and solid particles to different degrees. In step (B), the auxiliary agent is prepared from the group consisting of initiators, coupling agents, coupling agents, activators, and terminating agents. In step (C), the raw materials are added in a stepwise manner, and the refined cyclohexane is preheated and then added into the micro-channel reactor, and then the refined styrene, refined butadiene and refined isoprene are added in sequence; the concentration of the obtained SIBS latex is 15-20%. In step (C), the weight ratio of the refined styrene, refined butadiene, refined isoprene, refined cyclohexane and auxiliary agent is 1:1.5:8:25:1; the reaction pressure of the micro-channel reactor is 0.05-0.5 MPa, the reaction temperature is 50-130°C, and the reaction time is 20-110 min. After steps (D), (E) and (F), a latex with a solid content of 30-50% is obtained.

2. The method of claim 1, wherein, ​ 3. The method of claim 1, wherein, ​ 4. The method of claim 1, wherein, ​ 5. The method of claim 1, wherein, ​ 6. The method of claim 1, wherein, ​ 7. The method of claim 6, wherein, ​ 8. The method of claim 1, wherein, ​ 9. The method of claim 1, wherein, In step (G), the non-phase change drying system has a sorting function, and different molecular weight of colloidal particles are obtained by controlling the temperature of the carrier gas; the non-phase change drying system uses low-temperature drying means, and when the temperature of the carrier gas is 40-60 ℃, the moisture content of the dried colloidal particles is reduced from 90% to 3-10%; the operating pressure of the non-phase change drying process is 0.1-0.3 MPa; the obtained SIBS elastomer has a melt index of 0.1-30.0, and the molecular weight of the elastomer is 70-150 thousand.

10. A monomer refining device, comprising: a monomer refining unit composed of a microchannel separator (1) and a shape coalescer (2) connected thereto, for performing step (A) of monomer refining based on the microchannel separator and the shape coalescer: adding crude styrene, crude isoprene, crude butadiene and crude cyclohexane raw materials into the monomer refining unit composed of the microchannel separator and the shape coalescer to remove impurities therein to obtain refined raw materials; a microchannel reactor (3) connected to the shape coalescer (2), a latex buffer tank (4) connected to the microchannel reactor (3), and a micro-droplet extraction tank (5) connected to the latex buffer tank (4), for performing step (C) of microchannel reactor polymerization: adding the refined raw materials obtained in step (A) and the adjuvants configured in step (B) into the microchannel reactor, and after the reaction is completed, the produced latex is added into the latex buffer tank, and then extracted through the micro-droplet extraction tank containing antioxidants; a dynamic blending tank (6) connected to the micro-droplet extraction tank (5), for performing step (D) of dynamic mixing and blending by cyclone: adding the extracted latex obtained in step (C) into the dynamic blending tank, and stirring and blending uniformly; a cyclone classifier (7) connected to the dynamic blending tank (6), for performing step (E) of cyclone classification: adding the uniformly blended latex obtained in step (D) into the cyclone classifier, and performing latex coagulation by cyclone separation; 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 (G) of non-phase change cyclone drying treatment: adding the coagulated colloidal particles obtained in step (E) into the non-phase change drying system, and feeding the dried colloidal particles to the final packaging to obtain SIBS elastomer.

Images