CN216630835U - Reaction system - Google Patents
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- CN216630835U CN216630835U CN202123332611.0U CN202123332611U CN216630835U CN 216630835 U CN216630835 U CN 216630835U CN 202123332611 U CN202123332611 U CN 202123332611U CN 216630835 U CN216630835 U CN 216630835U
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Abstract
The present invention provides a reaction system comprising: a reaction kettle; the self-suction stirrer comprises a stirring shaft and stirring blades; the guide cylinder is sleeved at one end of the stirring shaft; the flow partition plate is connected with the inner wall of the reaction kettle, and the bottom of the flow partition plate is provided with an arc-shaped curved surface; and (7) a cover plate. The utility model adopts the self-suction stirrer to match with the guide cylinder, can increase the contact area of the SBS polymer solution and the hydrogen, leads the SBS polymer solution and the hydrogen to be fully contacted, strengthens the gas-liquid mass transfer process, thereby improving the hydrogenation efficiency and simultaneously reducing the material consumption, the energy consumption and the operation cost in the hydrogenation process. Set up the apron simultaneously on stirring paddle leaf, the apron can play the effect of helping the stirring or sealed stirring paddle leaf goes up the venthole.
Description
Technical Field
The utility model relates to the technical field of chemical industry, in particular to a reaction system.
Background
Polystyrene (PS) -Polybutadiene (PB) -Polystyrene (PS) triblock copolymer (SBS) is a widely used thermoplastic elastomer, and in order to improve heat resistance, oxidation resistance and aging resistance, selective hydrogenation is usually used to saturate the double bonds of the butadiene block in the polymer, thereby preparing a hydrogenated styrene-butadiene block polymer (SEBS) with more excellent properties. In the existing SEBS preparation technology, hydrogenation reactors can be divided into three types: a kettle reactor, a tower reactor and a multi-shaft gas-liquid contact reactor.
The hydrogenation process of SEBS usually adopts a kettle type reactor, rapid stirring is carried out under certain hydrogen pressure to mix gas and liquid so as to realize hydrogenation reaction, two or more kettle type reactors are used for being connected in series, and the effluent product of a downstream reactor enters an upstream reactor for circulation after heat exchange, so that the hydrogenation degree of the product is improved.
The tower reactor is a vertically installed main body, a feed inlet is arranged near the top of the tower reactor, a material outlet is arranged at the bottom of the tower reactor, and inert materials can be filled in the tower reactor. The trickle bed is adopted for hydrogenation reaction, liquid trickles downwards into the hydrogen atmosphere, and the hydrogenation degree can reach 98% within 5 minutes. The method has high hydrogenation rate, but the temperature in the hydrogenation process is high and difficult to control stably, the dosage of the catalyst is large, the liquid holdup of the reactor is low, and the utilization rate of the unit volume of the reactor is low.
The multi-shaft gas-liquid contact reactor is internally provided with two rotary stirring devices, and polymer solution is sheared, mixed and sheared again through a plurality of fixed elements on a rotating shaft, so that a gas-liquid phase interface is continuously updated, and the hydrogenation efficiency is improved. However, the method has complex equipment structure and higher manufacturing cost.
SUMMERY OF THE UTILITY MODEL
In view of the above, the utility model provides a reaction system, and the self-priming stirrer, the guide cylinder and the flow isolating plate are arranged in the reaction kettle, so that the hydrogen can realize self-priming circulation, and meanwhile, the contact area of the hydrogen and the polymer solution is effectively increased, so that the gas-liquid contact is more sufficient, the reaction efficiency is improved, and the energy consumption and the material consumption in the production process are reduced.
In order to solve the technical problems, the utility model adopts the following technical scheme:
in a first aspect, the present invention provides a reaction system comprising:
the reaction kettle is provided with a material inlet and a material outlet;
the self-suction stirrer comprises a stirring shaft and a stirring blade, wherein one end of the stirring shaft extends into the reaction kettle, the stirring blade is arranged at one end of the stirring shaft, a first cavity extending along the length direction of the stirring shaft is arranged on the stirring shaft, and an air inlet communicated with the first cavity is arranged at one end of the stirring shaft;
the stirring paddle is provided with a second chamber, the air inlet and the stirring paddle are arranged at intervals along the length direction of the stirring shaft, the stirring paddle is positioned below the air inlet, the first chamber is communicated with the second chamber, the stirring paddle is provided with an air outlet communicated with the second chamber, and the air outlet and the stirring shaft are spaced in the radial direction of the reaction kettle;
the guide cylinder is sleeved at one end of the stirring shaft, and a guide channel penetrating along the length direction of the stirring shaft is arranged on the guide cylinder;
the flow partition plate is connected with the inner wall of the reaction kettle, and the bottom of the flow partition plate is provided with an arc-shaped curved surface;
the cover plate is arranged close to the air outlet, one end of the cover plate is movably arranged on the stirring blade, and the other end of the cover plate is stopped against the stirring blade and seals the air outlet under the condition that the cover plate is in a first state;
and under the condition that the cover plate is in the second state, the other end of the cover plate is far away from the stirring paddle and the air outlet is opened.
Further, the edge of the air outlet hole is provided with a first sealing layer, the first sealing layer extends along the circumferential direction of the air outlet hole, a second sealing layer is arranged at the position, corresponding to the air outlet hole, of the other end of the cover plate, and the second sealing layer on the other end of the cover plate abuts against the first sealing layer under the condition that the cover plate is in the first state.
Furthermore, the venthole has a plurality ofly, and is a plurality of the venthole is followed stirring paddle's length direction interval sets up, every the venthole corresponds and sets up one the apron.
Furthermore, the edge area of one side of each air outlet hole, which is far away from the stirring shaft, is provided with one cover plate respectively.
Furthermore, one side of each cover plate, which is far away from the stirring shaft, is provided with a limiting table, and the cover plate is stopped against the limiting tables under the condition that the cover plate is in the second state.
Furthermore, each limiting table and the corresponding air outlet hole are arranged at intervals, and the height of each limiting table is adjustable;
and/or the limiting table has elasticity.
Further, in a case where the cover plate is in the second state, the cover plate is perpendicular to the stirring blade.
Furthermore, the guide shell is columnar, and the axis of the guide shell is collinear with the axis of the stirring shaft.
Further, the air inlet is located above the guide shell, and the stirring blade is located in the guide shell.
Further, the flow separation plate is provided with a bending angle, and the bending angle is bent towards the direction of the guide shell.
Furthermore, the included angle between the flow partition plate and the inner wall of the reaction kettle can be adjusted; and/or
The position of the flow partition plate on the inner wall of the reaction kettle can be adjusted.
Further, the distance between the flow partition plate and the stirring shaft in the radial direction of the reaction kettle is adjustable.
Further, the flow partition plate is located above the guide shell.
Further, the reaction system further comprises:
the circulating heat exchange device comprises a heat exchange tube bundle arranged inside the reaction kettle and a pipe-accompanying type jacket arranged outside the shell of the reaction kettle; and/or
Further comprising:
and the power device is connected with the other end of the stirring shaft.
The technical scheme of the utility model has the following beneficial effects:
the present invention provides a reaction system comprising: the reaction kettle is provided with a material inlet and a material outlet; the self-suction stirrer comprises a stirring shaft and a stirring blade, wherein one end of the stirring shaft extends into the reaction kettle, the stirring blade is arranged at one end of the stirring shaft, a first cavity extending along the length direction of the stirring shaft is arranged on the stirring shaft, and an air inlet communicated with the first cavity is arranged at one end of the stirring shaft; the stirring paddle is provided with a second chamber, the air inlet and the stirring paddle are arranged at intervals along the length direction of the stirring shaft, the stirring paddle is positioned below the air inlet, the first chamber is communicated with the second chamber, the stirring paddle is provided with an air outlet communicated with the second chamber, and the air outlet and the stirring shaft are spaced in the radial direction of the reaction kettle; the guide cylinder is sleeved at one end of the stirring shaft, and a guide channel penetrating along the length direction of the stirring shaft is arranged on the guide cylinder; the flow partition plate is connected with the inner wall of the reaction kettle, and the bottom of the flow partition plate is provided with an arc-shaped curved surface; the cover plate is arranged close to the air outlet, one end of the cover plate is movably arranged on the stirring blade, and the other end of the cover plate is stopped against the stirring blade and seals the air outlet under the condition that the cover plate is in a first state; and under the condition that the cover plate is in the second state, the other end of the cover plate is far away from the stirring paddle and the air outlet is opened.
The utility model adopts the self-suction stirrer to be matched with the guide cylinder, effectively overcomes the defects of large hydrogen circulation amount, low one-way utilization rate and high energy consumption in the SEBS preparation process in the prior art, can increase the contact area of the SBS polymer solution and the hydrogen, ensures that the SBS polymer solution and the hydrogen are fully contacted, and strengthens the gas-liquid mass transfer process, thereby improving the hydrogenation efficiency and simultaneously reducing the material consumption, the energy consumption and the operation cost in the hydrogenation process. Meanwhile, the bottom of the flow partition plate is provided with an arc-shaped curved surface, and the curve of the curved surface of the bottom is consistent with the flow line of the flow field in the reaction kettle in the stirring process, so that the turbulent flow loss caused by collision of the gas-liquid mixture and the bottom of the flow partition plate is reduced, the bubble coalescence probability is reduced, and the phase interface area of the gas-liquid mixture is improved. Meanwhile, the cover plate is arranged on the stirring blade, in the running process of the stirring blade, the other end of the cover plate is far away from the stirring blade and opens the air outlet hole under the second state, and the cover plate can play a role in assisting in stirring; at stirring paddle leaf bring to rest, the apron is in under the first state, and the other end of apron ends stirring paddle leaf and seal the venthole, the apron at this moment plays the effect of closed gas pocket, can guarantee that liquid does not enter into inside the stirring paddle leaf.
Drawings
FIG. 1 is a schematic diagram of the structure of a reaction system;
FIG. 2 is a schematic structural view of the stirring blade when the cover plate is in a second state;
fig. 3 is a schematic three-dimensional space diagram of the cutoff plate.
Reference numerals:
1. a reaction kettle; 2. a material inlet; 3. a material outlet; 4. a stirring shaft; 5. a stirring paddle; 6. an air inlet; 7. an air outlet; 8. a draft tube; 9. a flow isolating plate; 10. a heat exchange tube bundle; 11. a pipe-accompanied jacket; 12. a power plant; 13. a cover plate; 14. a limiting table;
H. the height of the reaction kettle 1 is equal to the height of the kettle body; l, height of the guide shell 8; c1, the distance from the bottom of the guide shell 8 to the bottom of the reaction kettle 1; c2, the distance from the bottom of the flow partition plate 9 to the top of the guide shell 8.
Detailed Description
For a further understanding of the utility model, reference will now be made to the preferred embodiments of the utility model in conjunction with the following examples, but it will be understood that the description is intended to illustrate the features and advantages of the utility model further, and not to limit the utility model.
In a first aspect, the present invention provides a reaction system, which is described below with reference to fig. 1 to 3.
The reaction system of the present invention comprises: the device comprises a reaction kettle 1, wherein a material inlet 2 and a material outlet 3 are arranged on the reaction kettle 1; the self-suction stirrer comprises a stirring shaft 4 and stirring blades 5, wherein one end of the stirring shaft 4 extends into the reaction kettle 1, the stirring blades 5 are arranged at one end of the stirring shaft 4, a first cavity extending along the length direction of the stirring shaft 4 is arranged on the stirring shaft 4, and an air inlet 6 communicated with the first cavity is arranged at one end of the stirring shaft 4; a second cavity is arranged on the stirring paddle blade 5, the air inlet 6 and the stirring paddle blade 5 are arranged at intervals along the length direction of the stirring shaft 4, the stirring paddle blade 5 is positioned below the air inlet 6, the first cavity is communicated with the second cavity, an air outlet 7 communicated with the second cavity is arranged on the stirring paddle blade 5, and the air outlet 7 and the stirring shaft 4 are spaced in the radial direction of the reaction kettle 1; the guide cylinder 8 is sleeved at one end of the stirring shaft 4, and a guide channel penetrating along the length direction of the stirring shaft 4 is arranged on the guide cylinder 8; the flow partition plate 9 is connected with the inner wall of the reaction kettle 1, and the bottom of the flow partition plate 9 is provided with an arc-shaped curved surface; the cover plate 13 is arranged close to the air outlet, one end of the cover plate 13 is movably arranged on the stirring blade, and the other end of the cover plate 13 is stopped against the stirring blade and seals the air outlet under the condition that the cover plate 13 is in the first state; in the case where the cover plate 13 is in the second state, the other end of the cover plate 13 is away from the stirring blade and opens the air outlet.
In particular, the reaction system of the present invention can be understood as: inserted a self-priming agitator in reation kettle 1, self-priming agitator includes a (mixing) shaft 4, (mixing) shaft 4 is hollow (mixing) shaft (being first cavity) to be equipped with inlet port 6 on (mixing) shaft 4, the quantity of air inlet can be injectd according to actual conditions, for example sets up inlet port quantity and be 6. Simultaneously self-priming agitator is still including setting up stirring paddle 5 at the lower extreme of (mixing) shaft 4, stirring paddle 5 is hollow structure (being the second cavity) equally, just stirring paddle 5 is last be equipped with the venthole 7 of second cavity intercommunication, venthole 7 with (mixing) shaft 4 is in spaced apart in reation kettle 1's the radial direction. The stirring shaft 4 is communicated with the stirring blade 5 (i.e. the first chamber is communicated with the second chamber), and the air inlet hole 6 on the stirring shaft 4, the first chamber of the stirring shaft 4, the air outlet hole 7 on the stirring blade 5 and the second chamber of the stirring blade 5 are communicated with each other. The guide shell 8 is sleeved at one end of the stirring shaft 4, and a guide channel penetrating along the length direction of the stirring shaft 4 is arranged on the guide shell 8.
Meanwhile, the bottom of the flow baffle 9 is provided with an arc-shaped curved surface, and the curve of the curved surface of the bottom is consistent with the streamline of the flow field in the reaction kettle 1 in the stirring process, so that the turbulent flow loss caused by collision of the gas-liquid mixture and the bottom of the flow baffle is reduced, the bubble coalescence probability is reduced, and the phase interface area of the gas-liquid mixture is increased.
In addition, referring to fig. 2, in the present invention, a cover plate 13 is disposed on the stirring blade, and in the operation process of the stirring blade, the cover plate 13 is in the second state, and the other end of the cover plate 13 is far away from the stirring blade and opens the air outlet, and the cover plate 13 can play a role in assisting stirring; at stirring paddle leaf bring to rest, apron 13 is in under the first state, and the other end of apron 13 ends stirring paddle leaf and seal the venthole, apron 13 at this moment play the effect of closed gas pocket, can guarantee that liquid does not enter into inside the stirring paddle leaf.
According to some embodiments of the present invention, the edge of the air outlet hole 7 is provided with a first sealing layer, the first sealing layer extends along the circumferential direction of the air outlet hole, the other end of the cover plate 13 is provided with a second sealing layer at a position corresponding to the air outlet hole 7, and the second sealing layer on the other end of the cover plate 13 is stopped against the first sealing layer when the cover plate 13 is in the first state. Specifically, the first sealing layer and the second sealing layer may be rubber sealing rings, the rubber sealing rings are disposed along the edge of the air outlet 7, and rubber sealing rings are also disposed at corresponding positions on the cover plate 13, so that when the cover plate 13 is in the first state, the rubber sealing rings on the cover plate 13 are in contact with and seal the rubber sealing rings at the edge of the air outlet 7, thereby sealing the air outlet 7.
According to some embodiments of the present invention, the air outlet 7 has a plurality of air outlets 7, the plurality of air outlets 7 are arranged at intervals along the length direction of the stirring blade 5, and each air outlet 7 is provided with one cover plate 13.
According to some embodiments of the present invention, a side edge region of each of the air outlet holes 7 away from the stirring shaft 4 is provided with one of the cover plates 13.
According to some embodiments of the present invention, a side of each cover plate 13 away from the stirring shaft 4 is provided with a limit stop 14, and when the cover plate 13 is in the second state, the cover plate 13 abuts against the limit stop 14.
According to some embodiments of the utility model, each limiting table 14 is arranged at a distance from the corresponding air outlet 7, and the height of each limiting table 14 is adjustable; and/or the limit stop 14 is resilient.
According to some embodiments of the present invention, with the cover plate 13 in the second state, the cover plate 13 is perpendicular to the stirring blade 5.
In the utility model, the cover plate 13 is arranged on the stirring blade 5, in the running process of the stirring blade 5, the cover plate 13 is in the second state, the other end of the cover plate 13 is far away from the stirring blade 5 and opens the air outlet 7, and the cover plate 13 can play a role in assisting stirring. Preferably, in the present invention, a limit table 14 is respectively disposed on one side of each cover plate 13 away from the stirring shaft 4, the height of the limit table 14 is adjustable, the limit table 14 has elasticity, and the degree of opening of the cover plate 13 can be controlled by disposing the limit table 14.
According to some embodiments of the present invention, the guide shell 8 is cylindrical, and the axis of the guide shell 8 is collinear with the axis of the stirring shaft 4.
According to some embodiments of the present invention, the gas inlet 6 is located above the guide shell 8, so that gas can enter the first chamber through the gas inlet 6, and the stirring blade 5 is located in the guide shell 8, so as to enhance the flow of the solution, enhance the gas-liquid mass transfer process, and improve the hydrogenation efficiency.
According to some embodiments of the utility model, the reaction system further comprises: and the power device 12 is connected with the other end of the stirring shaft 4, and further drives the stirring shaft 4 to rotate.
According to some embodiments of the present invention, the power device 12 includes an electric motor, a speed reducer and a mechanical sealing device, the speed reducer directly drives the self-priming agitator to rotate, and the speed reducer is fixedly connected with the top end of the self-priming agitator; the motor is connected with the speed reducer.
The operation and working principle of the reaction system in the utility model are as follows: firstly, a reaction kettle 1 is in a sealed state in the reaction process, liquid materials and gas to be reacted are added from a material inlet 2 arranged on the reaction kettle 1, when the liquid materials are put into the reaction kettle 1, an air inlet 6 of a stirring shaft 4 is required to be ensured to be above the liquid level, and a stirring paddle 5 of a self-suction stirrer is arranged below the liquid level. After materials are added, the materials enter a cavity of the stirring shaft 4 from the air outlet 7 of the stirring blade 5, after the power device 12 is started, the stirring shaft 4 and the stirring blade 5 rotate at a high speed, so that the materials in the cavities of the stirring shaft 4 and the stirring blade 5 are thrown out from the air outlet 7 of the stirring blade 5 under the action of centrifugal force, negative pressure is generated in the cavity of the stirring shaft 4, gas above the liquid level is sucked into the cavity of the stirring shaft 4 through the air inlet 6 on the stirring shaft 4, and finally the gas is discharged into the materials from the air outlet 7 of the stirring blade 5 to form bubbles; in the process of high-speed rotation of the stirring paddle 5, bubbles with larger volume are dispersed into small bubbles by shearing the bubbles, so that the gas-liquid contact area is increased, and the gas is fully contacted with the material.
In order to enhance the uniformity of the distribution of the reaction gas in the material, a guide cylinder 8 is further arranged in the reaction kettle 1, the upper end of the guide cylinder 8 is arranged below the liquid level of the material during the reaction, the lower end of the guide cylinder 8 is arranged below the stirring paddle 5, when the self-suction stirrer rotates at a high speed, the gas-liquid mixture is pushed to the inner wall surface of the guide cylinder 8, is hindered by the inner wall of the guide cylinder 8 and then flows downwards from the lower end of the guide cylinder 8, when the gas-liquid mixture flows through the upper end of the guide cylinder 8, the gas-liquid mixture is sucked into the guide cylinder 8, and the gas-liquid mixture circulates inside and outside the guide cylinder 8, so that the distribution of the gas in the reaction kettle 8 is more uniform.
According to some embodiments of the present invention, the stirring paddle 5 includes a plurality of stirring paddles 5, and the plurality of stirring paddles 5 are arranged at intervals along the circumferential direction of the stirring shaft 4, so as to promote the stirring effect and promote the gas-liquid contact.
According to further embodiments of the present invention, the reaction system further comprises: the flow partition plate 9, the flow partition plate 9 with the inner wall of the reaction kettle 1 is connected, the flow partition plate 9 is provided with a bend angle, and the bend angle is towards the flow guide cylinder 8.
According to other embodiments of the present invention, the flow partitioner 9 is located above the guide shell 8.
The present invention is provided with the flow separation plate 9 which can increase the residence time of the reaction gas in the reaction kettle 1 and improve the one-way conversion rate of the reaction gas, the reaction kettle is also provided with the flow separation plate 9 (as shown in figure 3), the flow separation plate 9 is connected with the inner wall of the reaction kettle 1, and the flow separation plate 9 is provided with a bend angle which is bent towards the upper end of the guide flow cylinder 8. During the stirring process, when the gas-liquid mixture flows through the lower end of the flow partition plate 9, on one hand, the reaction gas is blocked by the flow partition plate 9 and cannot directly enter the upper part of the reaction kettle 1 through the flow partition plate 9; on the other hand, the gas-liquid mixture is blocked by the flow partition plate 9 to change the flow direction, and flows along the lower end of the flow partition plate 9 to the upper end of the guide cylinder 8, so that the gas-liquid mixture enters the interior of the guide cylinder 8 to participate in the circulation process. The gas-liquid mixture at the upper end of the guide cylinder 8 is intensively flowed towards the inner part of the guide cylinder 8 by guiding the gas-liquid mixture through the flow separation plate 9, so that the circulation times of the gas in the reaction kettle 1 are improved, the gas retention time is increased, and the one-way conversion rate of the reaction gas is greatly increased.
According to other embodiments of the present invention, the included angle between the flow partitioning plate 9 and the inner wall of the reaction kettle 1 is adjustable; and/or the position of the flow partitioner 9 on the inner wall of the reaction vessel 1 is adjustable.
According to other embodiments of the present invention, the distance between the flow divider 9 and the stirring shaft 4 in the radial direction of the reaction kettle 1 is adjustable, the relative relationship between the flow divider 9 and the guide cylinder 8 can be adjusted, and the specific distance can be adjusted as required, so that the flow divider 9 and the guide cylinder 8 are reasonably matched, and at different rotation speeds, when a gas-liquid mixture flows through the lower end of the flow divider 9, the flow direction of the gas-liquid mixture can be changed by the obstruction of the flow divider 9, and the gas-liquid mixture flows along the lower end of the flow divider 9 to the upper end of the guide cylinder 8, and then enters the interior of the guide cylinder 8 to participate in the circulation process. The included angle and the position of the flow isolating plate 9 are adjustable, so that the curve of the bottom curved surface of the flow isolating plate 9 is consistent with the flow line of the flow field in the reaction kettle 1 in the stirring process; on the other hand, in the stirring process, under different material amounts and different rotating speeds, the gas-liquid mixture can change the flow direction under the obstruction of the flow partition plate 9 when flowing through the lower end of the flow partition plate 9, and flows to the upper end of the guide cylinder 8 along the lower end of the flow partition plate 9, so as to enter the inner part of the guide cylinder 8 to participate in the circulation process.
According to further embodiments of the present invention, the reaction system further comprises: the circulating heat exchange device comprises a heat exchange tube bundle 10 arranged inside the reaction kettle 1 and a pipe accompanying type jacket 11 arranged outside the shell of the reaction kettle 1. The circulating heat exchange device is mainly used for regulating and controlling the reaction temperature in the reaction kettle.
According to other embodiments of the present invention, the upper end of the reaction kettle 1 is provided with the material inlet 2, and the lower end of the reaction kettle 1 is provided with the material outlet 3; the material inlet includes a gas inlet, a first inlet, and a second inlet.
The utility model is further illustrated by the following specific examples.
Example 1
Reaction system: as shown in fig. 1.
The parameters of each device are as follows: reaction kettle 1: the height H is 900mm, and the diameter is 500 mm; a stirring shaft 4: the diameter of the opening is 6mm, and the number of the openings is 6; and (3) a guide shell 8: height L is 400mm, diameter is 240mm, C1 is 0.25L; stirring blade 5: the diameter is 158mm, the number of the blades is 6, each blade is provided with two air outlet holes 7, and two cover plates 13 are correspondingly arranged on each air outlet hole; the flow isolating plate 9: the width is 56mm, bending angle is 45 degrees, the bottom of flow partition plate 9 has the arc bending surface, and the characteristic line of curved surface is the elliptical arc, and the major axis of elliptical arc is adjustable with the minor axis than, and is preferred here to be 2: 1, C2 ═ 0.1L; the effective volume in the kettle is 150L.
Hydrogenation catalyst: the catalyst is prepared by mixing nickel naphthenate and triisobutyl aluminum according to the molar ratio of aluminum to nickel of 5:1, and aging at 60 ℃ for 30 minutes, wherein the dosage of the catalyst is 0.06g of Ni/100g of SBS polymer glue solution.
The operation method comprises the following steps: hydrogen is respectively introduced into the reaction kettle 1 from 3 material inlets 2 at the top of the reaction kettle 1, 10 wt.% SBS polymer glue solution, inert solvent alkane and the hydrogenation catalyst are added, and the gauge pressure of the hydrogen is kept at 2.0 MPa. Starting a power device, setting the rotating speed of a self-suction stirrer to be 600RPM, starting a jacket heat exchange device, and maintaining the temperature in the reaction kettle to be 65 ℃.
And (3) testing: the liquid level difference method is used for testing the hydrogen gas content in the reactor in the reaction process, the high-speed camera shooting method is used for measuring the bubble volume and the gas average residence time, the sampling is carried out from a material outlet 3 at the bottom of the reaction kettle 1 after 120min of reaction, and the iodine method is adopted for measuring the hydrogenation degree of a polybutadiene block (PB segment) in a product, and the specific mode is as follows: weighing 40mg of product dry glue, placing the product dry glue into a 250ml iodine measuring bottle, adding 20ml of chloroform solvent, accurately transferring 1.0ml of bromine-iodine solution into the bottle after the dry glue is completely dissolved, adding 10ml of 10% (w.t.) KI solution and 20ml of deionized water after a period of light-resistant reaction, and adding Na2S2O3Titrating standard solution by using 0.5% (w.t.) starch solution as an indicator until the end point (colorless), and recording Na consumed in the experiment2S2O3Volume V of standard solution, Na consumed in blank experiment2S2O3Volume V of standard solution0Na consumption of SBS measured by the same method2S2O3Volume V of standard solution1Degree of hydrogenation ═ V (V-V)1)/(V0-V1) X 100%, and measuring the hydrogenation degree of a polystyrene block (PS section) in the product by adopting an ultraviolet spectrophotometry, wherein the specific mode is as follows: 0.5g of the product dry glue is weighed and dissolved by 50mL of chloroform, the absorbance of the product is measured, and the hydrogenation degree of the polystyrene block is determined by a polystyrene concentration-absorbance standard curve. The reaction product is SEBS, and the hydrogenation quality of the SEBS is shown in Table 1.
Example 2
Reaction system: as shown in fig. 1.
The parameters of each device are as follows: reaction kettle 1: height H is 3000mm, diameter 800 mm; a stirring shaft 4: the diameter of the opening is 6mm, and the number of the openings is 6; and (3) a guide shell 8: the height L is 900mm, the diameter is 380mm, and C1 is 0.25L; stirring blade 5: the diameter is 270mm, the number of the blades is 6, each blade is provided with two air outlet holes 7, and two cover plates 13 are correspondingly arranged on each air outlet hole; the flow isolating plate 9: the width is 100mm, bending angle 45, and the bottom of flow partition board 9 has the arc bending surface, and the characteristic line of curved surface is the elliptical arc, and the major axis of elliptical arc is adjustable with the minor axis than, and is preferred here to be 2: 1, C2 ═ 0.1L; the effective volume in the kettle is 1500L.
Hydrogenation catalyst: the catalyst is prepared by mixing nickel naphthenate and triisobutyl aluminum according to the molar ratio of aluminum to nickel of 5:1, and aging at 60 ℃ for 30 minutes, wherein the dosage of the catalyst is 0.06g of Ni/100g of SBS polymer glue solution.
The operation method comprises the following steps: introducing hydrogen into the reaction kettle 1 from 3 material inlets 2 at the top end of the reaction kettle 1, adding 10 wt.% SBS polymer glue solution, inert solvent alkane and the hydrogenation catalyst, and keeping the hydrogen gauge pressure at 2.0 MPa. Starting a power device, setting the rotating speed of a self-suction stirrer to be 600RPM, starting a jacket heat exchange device, and maintaining the temperature in the reaction kettle to be 65 ℃.
And (3) testing: the test items and the test methods are the same as those of example 1, the reaction product is SEBS, and the hydrogenation quality is shown in Table 1.
Example 3
Reaction system: the reaction vessel had an effective volume of 150L as in example 1.
Hydrogenation catalyst: the mixture of the biscyclopentadienyltitanium dichloride catalyst and n-butyllithium is prepared by mixing the lithium and the titanium according to the molar ratio of 5:1 and aging the mixture for 30 minutes at 60 ℃, wherein the dosage of the catalyst is 0.05mMol Ti/100g SBS polymer glue solution.
The operation method comprises the following steps: hydrogen is respectively introduced into the reaction kettle 1 from 3 material inlets 2 at the top of the reaction kettle 1, 10 wt.% SBS polymer glue solution, inert solvent alkane and the hydrogenation catalyst are added, and the gauge pressure of the hydrogen is kept at 2.0 MPa. Starting a power device, setting the rotating speed of a self-suction stirrer to be 600RPM, starting a jacket heat exchange device, and maintaining the temperature in the reaction kettle to be 65 ℃.
And (3) testing: the test items and the test methods are the same as those of example 1, the reaction product is SEBS, and the hydrogenation quality is shown in Table 1.
Example 4
Reaction system: the same procedure as in example 2 was repeated, except that the effective volume in the reaction vessel was 1500L.
Hydrogenation catalyst: the biscyclopentadienyl titanium dichloride catalyst and n-butyllithium mixture are mixed according to the lithium-titanium molar ratio of 5:1, and the mixture is aged for 30 minutes at 60 ℃ to obtain the catalyst, wherein the dosage of the catalyst is 0.05mMol Ti/100g SBS polymer glue solution.
The operation method comprises the following steps: introducing hydrogen into the reaction kettle 1 from 3 material inlets 2 at the top end of the reaction kettle 1, adding 10 wt.% SBS polymer glue solution, inert solvent alkane and the hydrogenation catalyst, and keeping the hydrogen gauge pressure at 2.0 MPa. Starting a power device, setting the rotating speed of a self-suction stirrer to be 600RPM, starting a jacket heat exchange device, and maintaining the temperature in the reaction kettle to be 65 ℃.
And (3) testing: the test items and the test methods are the same as those of example 1, the reaction product is SEBS, and the hydrogenation quality is shown in Table 1.
Comparative example 1
Reaction system: compared to example 1, the reaction system in comparative example 1 has neither flow baffle 8 nor flow divider 9, the other being the same.
Hydrogenation catalyst: same as in example 1.
The operation method comprises the following steps: same as in example 1.
And (3) testing: the test items and the test methods are the same as those of example 1, the reaction product is SEBS, and the hydrogenation quality is shown in Table 1.
Comparative example 2
Reaction system: compared to example 2, the reaction system in comparative example 2 has neither flow baffle 8 nor flow divider 9, the other being the same.
Hydrogenation catalyst: same as in example 2.
The operation method comprises the following steps: same as in example 2.
And (3) testing: the test items and the test methods are the same as those of example 1, the reaction product is SEBS, and the hydrogenation quality is shown in Table 1.
Comparative example 3
A reaction system: in comparison with example 1, the reaction system in comparative example 3 used a flow partitioning plate whose bottom was flat, and the others were the same.
Hydrogenation catalyst: same as in example 1.
The operation method comprises the following steps: same as in example 1.
And (3) testing: the test items and the test methods are the same as those of example 1, the reaction product is SEBS, and the hydrogenation quality is shown in Table 1.
Comparative example 4
A reaction system: compared with the example 1, the stirring shaft in the reaction system in the comparative example 4 is a solid stirring shaft, the stirring blade is solid, and the rest is the same.
Hydrogenation catalyst: same as in example 1.
The operation method comprises the following steps: same as in example 1.
And (3) testing: the test items and the test methods are the same as those of example 1, the reaction product is SEBS, and the hydrogenation quality is shown in Table 1.
TABLE 1 Effect of different operating conditions and hydrogenation catalyst types on the quality of SEBS
The data in the table 1 show that the self-priming stirrer is matched with the guide cylinder and the flow isolating plate, so that the defects of large hydrogen circulation amount, low one-way utilization rate and high energy consumption in the prior art are effectively overcome, the SBS polymer solution and the hydrogen are in full contact by increasing the contact area of the SBS polymer solution and the hydrogen, the gas-liquid mass transfer process is strengthened, the hydrogenation efficiency is improved, and the material consumption, the energy consumption and the operation cost in the hydrogenation process are reduced; at stirring paddle shutdown, the apron is in under the first state, and the apron at this moment plays the effect of closed gas pocket, can guarantee that liquid does not enter into inside the stirring paddle.
Unless defined otherwise, technical or scientific terms used herein shall have the ordinary meaning as understood by one of ordinary skill in the art to which this invention belongs. The use of "first," "second," and similar terms in the present application do not denote any order, quantity, or importance, but rather the terms are used to distinguish one element from another. The terms "connected" or "coupled" and the like are not restricted to physical or mechanical connections, but may include electrical connections, whether direct or indirect. "upper", "lower", "left", "right", and the like are used merely to indicate relative positional relationships, and when the absolute position of the object being described is changed, the relative positional relationships are changed accordingly.
While the foregoing is directed to the preferred embodiment of the present invention, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the utility model as defined in the appended claims.
Claims (8)
1. A reaction system, comprising:
the reaction kettle is provided with a material inlet and a material outlet;
the self-suction stirrer comprises a stirring shaft and a stirring blade, wherein one end of the stirring shaft extends into the reaction kettle, the stirring blade is arranged at one end of the stirring shaft, a first cavity extending along the length direction of the stirring shaft is arranged on the stirring shaft, and an air inlet communicated with the first cavity is arranged at one end of the stirring shaft;
the stirring paddle is provided with a second chamber, the air inlet and the stirring paddle are arranged at intervals along the length direction of the stirring shaft, the stirring paddle is positioned below the air inlet, the first chamber is communicated with the second chamber, the stirring paddle is provided with an air outlet communicated with the second chamber, and the air outlet and the stirring shaft are spaced in the radial direction of the reaction kettle;
the guide cylinder is sleeved at one end of the stirring shaft, and a guide channel penetrating along the length direction of the stirring shaft is arranged on the guide cylinder;
the flow partition plate is connected with the inner wall of the reaction kettle, and the bottom of the flow partition plate is provided with an arc-shaped curved surface;
the cover plate is arranged close to the air outlet, one end of the cover plate is movably arranged on the stirring blade, and the other end of the cover plate is stopped against the stirring blade and seals the air outlet under the condition that the cover plate is in a first state;
and under the condition that the cover plate is in the second state, the other end of the cover plate is far away from the stirring blade and opens the air outlet.
2. The reaction system according to claim 1, wherein the edge of the gas outlet hole is provided with a first sealing layer extending along the circumferential direction of the gas outlet hole, the other end of the cover plate is provided with a second sealing layer at a position corresponding to the gas outlet hole, and the second sealing layer on the other end of the cover plate abuts against the first sealing layer in the case where the cover plate is in the first state.
3. The reaction system according to claim 1, wherein the gas outlet is provided in plurality, and the plurality of gas outlets are arranged at intervals along the length direction of the stirring blade, and each gas outlet is provided with one corresponding cover plate.
4. The reaction system according to claim 3, wherein a side edge region of each of the air outlet holes away from the stirring shaft is provided with one of the cover plates.
5. The reaction system according to claim 1, wherein each of the cover plates is provided with a limit stop at a side thereof away from the stirring shaft, and the cover plate abuts against the limit stop when the cover plate is in the second state.
6. The reaction system of claim 5, wherein each of the limiting tables is spaced apart from the corresponding gas outlet, and the height of the limiting table is adjustable;
and/or the limiting table has elasticity.
7. The reaction system of claim 1, wherein the gas inlet is located above the draft tube and the stirring blade is located in the draft tube.
8. The reaction system of claim 1, further comprising:
the circulating heat exchange device comprises a heat exchange tube bundle arranged inside the reaction kettle and a pipe-accompanying type jacket arranged outside the shell of the reaction kettle; and/or
Further comprising:
and the power device is connected with the other end of the stirring shaft.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202123332611.0U CN216630835U (en) | 2021-12-28 | 2021-12-28 | Reaction system |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202123332611.0U CN216630835U (en) | 2021-12-28 | 2021-12-28 | Reaction system |
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| Publication Number | Publication Date |
|---|---|
| CN216630835U true CN216630835U (en) | 2022-05-31 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202123332611.0U Active CN216630835U (en) | 2021-12-28 | 2021-12-28 | Reaction system |
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| Country | Link |
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| CN (1) | CN216630835U (en) |
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2021
- 2021-12-28 CN CN202123332611.0U patent/CN216630835U/en active Active
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