P-tert-butyltoluene alkylation reaction system and use method thereof
By using p-methylbenzenesulfonic acid as a catalyst in the tert-butyltolyl alkylation reaction and recovering concentrated sulfuric acid, the problems of short service life and low reaction efficiency of concentrated sulfuric acid are solved, and efficient reaction and resource utilization are achieved.
Patent Information
- Application Number
- CN202411037192.3
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-07-31
- Publication Date
- 2024-12-13
AI Technical Summary
The existing tert-butyl toluene alkylation reaction uses concentrated sulfuric acid catalysts with short service life, large amount, serious environmental pollution and low reaction efficiency.
P-methylbenzenesulfonic acid is used as a high-efficiency catalyst, and the use of concentrated sulfuric acid is reduced through a concentrated sulfuric acid recovery device to achieve continuous addition of raw materials and reactions in the continuous reactor.
Improve reaction efficiency, reduce side reactions, make full use of catalysts, and reduce waste through concentrated sulfuric acid recovery.
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Figure CN119113950A_ABST
Abstract
Description
Technical Field
[0001] The invention relates to the technical field of p-tert-butyltoluene synthesis, and in particular to a p-tert-butyltoluene alkylation reaction system and a use method thereof. Background Art
[0002] In recent years, the three isomers of tert-butyltoluene (TBT) in the alkylation products of aromatics have attracted attention due to their uniqueness. One of the isomers, para-tert-butyltoluene (PTBT), is a derivative of toluene. It is a colorless and transparent liquid. It is an important raw material in chemical industry and also an organic intermediate of great value.
[0003] According to the difference of raw materials, the synthesis method of tert-butyltoluene is mainly divided into three technical routes: reaction of isobutylene and toluene, reaction of tert-butyl chloride and toluene, and reaction of tert-butyl alcohol and toluene. Among them, in the alkylation reaction of isobutylene and toluene, concentrated sulfuric acid is generally required as a catalyst.
[0004] However, the use of concentrated sulfuric acid as a catalyst not only has a short service life of the concentrated sulfuric acid, but also requires a large amount of concentrated sulfuric acid, high post-processing costs, serious environmental pollution, and high requirements for equipment corrosion resistance. In addition, the reaction is usually carried out intermittently in a reactor, and the alkylation reaction needs to be carried out independently in batches and small batches, resulting in low reaction efficiency. Summary of the invention
[0005] Based on this, the purpose of the present invention is to provide a p-tert-butyltoluene alkylation reaction system and a method of use, which aims to add p-toluenesulfonic acid as a high-efficiency catalyst to the existing alkylation reaction to reduce the amount of concentrated sulfuric acid used, and continuously add raw materials to carry out continuous reaction in the reactor to improve the reaction efficiency. In addition, by recovering concentrated sulfuric acid in waste, the amount of concentrated sulfuric acid used and the amount of waste acid generated are reduced.
[0006] In the first aspect, the present invention provides a para-tert-butyltoluene alkylation reaction system, including a reactor, a feeding mechanism, an opening and closing mechanism, a premixing mechanism, a static mixer, and a concentrated sulfuric acid recovery device. Among them, the top of the reactor is provided with a first liquid flow channel and a storage chamber for storing para-toluenesulfonic acid, the bottom of the storage chamber is provided with a discharge port, and the side wall of the first liquid flow channel is provided with an avoidance port; the feeding mechanism is arranged on the reactor, and the feeding mechanism includes a first sealing plate, a rotating wheel and a driving mechanism, the first sealing plate and the driving mechanism are both fixedly arranged on the reactor, the first sealing plate slides against the lower surface of the rotating wheel, and a circle of first through holes distributed in an array is provided along the circumference of the rotating wheel, the rotating wheel partially extends into the first liquid flow channel from the avoidance port, the discharge port slides against the upper surface of the rotating wheel, and the driving mechanism drives The rotating wheel rotates at a preset step angle so that one of the first through holes is located in the first liquid flow channel. The opening and closing mechanism is used to open the first liquid flow channel when isobutylene is introduced into the first liquid flow channel, and to close the first liquid flow channel when the introduction of isobutylene into the first liquid flow channel is stopped; the premixing mechanism is arranged in the reactor and below the feeding mechanism, and is used to mix concentrated sulfuric acid, isobutylene and p-toluenesulfonic acid; the static mixer is connected to the premixing mechanism; the concentrated sulfuric acid recovery device is used to recover concentrated sulfuric acid from the mixed solution in the static mixer and re-introduce it into the premixing mechanism.
[0007] In addition, the above-mentioned p-tert-butyltoluene alkylation reaction system according to the present invention may also have the following additional technical features:
[0008] Furthermore, the reactor is provided with a sliding chamber, a step opening is provided at the bottom of the first liquid flow channel, the opening and closing mechanism includes a piston, a piston rod, a second sealing plate, a magnetoelectric component, and a first fluid transmission pump, the piston is seal-slidably arranged in the sliding chamber to form a first closed chamber in the sliding chamber, the first fluid transmission pump is connected to the first closed chamber, the second sealing plate is seal-slidably arranged in the first liquid flow channel, one end of the piston rod is connected to the piston, and the other end of the piston rod extends from the sliding chamber into the first liquid flow channel and is connected to the second sealing plate, the magnetoelectric component generates a first electrical signal under the action of the introduced isobutylene to trigger the first fluid transmission pump to charge, so that the piston drives the second sealing plate to move downward until the second sealing plate moves to the step opening, and generates a second electrical signal to trigger the first fluid transmission pump to pump pressure when there is no action of isobutylene, so that the piston drives the second sealing plate to move upward until the second sealing plate closes the first liquid flow channel again.
[0009] Furthermore, the magnetoelectric component includes a power-generating impeller and a voltage conversion circuit module. The power-generating impeller is electrically connected to the input port of the voltage conversion circuit module. The charging control circuit of the first fluid transmission pump is provided with a first relay in a normally open state, and the extraction control circuit of the first fluid transmission pump is provided with a second relay in a normally closed state. The input ports of the voltage conversion circuit module are both electrically connected to the first relay and the second relay. The charging control circuit and the extraction control circuit of the first fluid transmission pump are both provided with a first power-off device to de-energize the first relay and energize the second relay when the first closed chamber reaches a preset pressure.
[0010] Furthermore, the feeding mechanism also includes a sealing sleeve and a second fluid transmission pump. The sealing sleeve is inserted into the first through hole, and the middle part of the sealing sleeve is penetrated. A second closed chamber is arranged in the sealing sleeve. The side wall of the second closed chamber close to the upper surface of the rotor is a corrugated skin that can expand and contract. The charging control circuit of the second fluid transmission pump is provided with a third relay in a normally open state. After the driving mechanism drives the rotor to rotate a step angle, the third relay is triggered to be energized so that the corrugated skin expands and seals the avoidance port. The extraction control circuit of the second fluid transmission pump is provided with a fourth relay in a normally closed state. The input port of the voltage conversion circuit module is electrically connected to the fourth relay. The charging control circuit and the extraction control circuit of the second fluid transmission pump are both provided with a second power-off device to de-energize the third relay and energize the fourth relay when the second closed chamber reaches a preset pressure.
[0011] Furthermore, the reactor is provided with a second liquid flow channel, and the second liquid flow channel is used to connect the concentrated sulfuric acid delivery device and the concentrated sulfuric acid recovery device. The premixing mechanism includes a plurality of stacked laminar plates, and each layer of laminar plates is provided with a plurality of third liquid flow channels and reflux areas arranged in parallel. One end of the third liquid flow channel is connected with the second liquid flow channel, and one end of the reflux area is connected with the first liquid flow channel. The third liquid flow channel and the reflux area are connected with each other through a second through hole. The static mixer is connected with the third liquid flow channel through the second through hole, and the reflux area is connected with the first liquid flow channel to introduce a mixed solution of isobutylene and p-toluenesulfonic acid from a first direction. The first liquid flow channel is used to introduce concentrated sulfuric acid from a second direction, wherein the first direction is different from the second direction.
[0012] Furthermore, the second through holes on the side walls of adjacent third liquid flow channels are arranged in a staggered manner and distributed toward the side where concentrated sulfuric acid is input.
[0013] Furthermore, the laminar flow plate is arranged obliquely in the reactor.
[0014] Furthermore, the alkylation reaction system of tert-butyltoluene also includes a reduction mixer, which includes a shell, a first type of baffle, and a second type of baffle. The outlet of the static mixer is connected to one end of the shell, and the concentrated sulfuric acid recovery device is connected to the other end of the shell. The first type of baffle and the second type of baffle are arranged in a direction perpendicular to the axial direction of the shell and are arranged in an alternating manner. At least one first through opening is provided in the middle of the first type of baffle, and at least one second through opening is provided on the circumferential edge of the second type of baffle, and the first through opening does not overlap with the second through opening.
[0015] Furthermore, the first closed cavity is arranged adjacent to the first liquid flow channel, a limit groove is provided on the side wall of the first liquid flow channel, the limit groove is located below the rotating wheel, the first closed cavity is located above the rotating wheel, and the piston rod is movable and limited in the limit groove.
[0016] In a second aspect, the present invention further provides a method for using a p-tert-butyltoluene alkylation reaction system, which is applied to the aforementioned p-tert-butyltoluene alkylation reaction system, and the method comprises the following steps:
[0017] Step 1, adding p-toluenesulfonic acid into the storage chamber;
[0018] Step 2, start the feeding mechanism: the driving mechanism drives the rotating wheel to rotate according to a preset step angle so that one of the first through holes corresponds to the position of the first liquid flow channel;
[0019] Step 3, introducing isobutylene into the first liquid flow channel, and the opening and closing mechanism is opened under the action of isobutylene, so that the mixed solution of isobutylene and p-toluenesulfonic acid enters the premixing mechanism, and concentrated sulfuric acid is introduced into the premixing mechanism at the same time, and finally the mixed solution flows into the static mixer for reaction to obtain p-tert-butyltoluene;
[0020] Step 4: using a concentrated sulfuric acid recovery device to recover concentrated sulfuric acid from the mixed solution in the static mixer;
[0021] Step 5: repeat step 2. When the mixed solution of isobutylene and p-toluenesulfonic acid enters the premixing mechanism, the concentrated sulfuric acid recovered by the concentrated sulfuric acid recovery device and the new concentrated sulfuric acid are introduced into the premixing mechanism together.
[0022] The beneficial effects of the present invention include at least: a precise amount of p-toluenesulfonic acid can be safely added periodically through the feeding mechanism, and the raw materials are fully mixed through the premixing mechanism and the static mixer, so that the time of the alkylation reaction is shortened, thereby reducing side reactions and improving the efficiency of the alkylation reaction, and the p-toluenesulfonic acid can be fully utilized; in addition, due to the participation of p-toluenesulfonic acid as a catalyst, the amount of concentrated sulfuric acid used can be reduced accordingly, and finally, the concentrated sulfuric acid in the product after the reaction can be recovered and reused through the concentrated sulfuric acid recovery device, thereby reducing the waste of concentrated sulfuric acid. BRIEF DESCRIPTION OF THE DRAWINGS
[0023] Figure 1 It is a schematic diagram of the structure of the reactor in the embodiment of the present invention;
[0024] Figure 2 It is a schematic structural diagram of a first through hole when it is closed according to an embodiment of the present invention;
[0025] Figure 3 It is a schematic structural diagram of the first through hole of the embodiment of the present invention when it is opened;
[0026] Figure 4 is an electrical control diagram of a first fluid transmission pump in an embodiment of the present invention;
[0027] Figure 5 Schematic diagram of the structure of the sealing sleeve in an embodiment of the present invention;
[0028] Figure 6 is a schematic diagram of the structure of the pleated skin in an embodiment of the present invention;
[0029] Figure 7 is an electrical control diagram of a second fluid transmission pump in an embodiment of the present invention;
[0030] Figure 8 Schematic diagram of the structure of the premixing mechanism in an embodiment of the present invention;
[0031] Fig. 9 is an exploded view of a speed reduction mixer in an embodiment of the present invention;
[0032] Description of main component symbols:
[0033] Reactor 100, first liquid flow channel 110, avoidance port 111, step port 112, limit slot 113, material storage chamber 120, material outlet 121, sliding chamber 130, first sealed chamber 131, second liquid flow channel 140, second through hole 150;
[0034] A feeding mechanism 200, a first sealing plate 210, a rotating wheel 220, a first through hole 221, a driving mechanism 230, a sealing sleeve 240, a second closed cavity 241, a pleated skin 2411, a second fluid transmission pump 250, and a second power-off device 251;
[0035] A piston 310, a piston rod 320, a second sealing plate 330, a magnetoelectric component 340, a power generation impeller 341, a voltage conversion circuit module 342, a first fluid transmission pump 350, and a first power-off device 351;
[0036] Premixing mechanism 400, laminar flow plate 410, third liquid flow channel 411, reflux area 412;
[0037] Static mixer 500;
[0038] The speed reduction mixer 600, the housing 610, the first type of baffle 620, the first through-hole 621, the second type of baffle 630, the second through-hole 631;
[0039] The following specific implementation manner will further illustrate the present invention in conjunction with the above-mentioned drawings. DETAILED DESCRIPTION
[0040] In order to facilitate the understanding of the present invention, the present invention will be described more fully below with reference to the relevant drawings. Several embodiments of the present invention are given in the drawings. However, the present invention can be implemented in many different forms and is not limited to the embodiments described herein. On the contrary, the purpose of providing these embodiments is to make the disclosure of the present invention more thorough and comprehensive.
[0041] It should be noted that when an element is referred to as being "fixed to" another element, it may be directly on the other element or there may be a central element. When an element is considered to be "connected to" another element, it may be directly connected to the other element or there may be a central element at the same time. The terms "vertical", "horizontal", "left", "right" and similar expressions used herein are for illustrative purposes only.
[0042] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as those commonly understood by those skilled in the art of the present invention. The terms used herein in the specification of the present invention are only for the purpose of describing specific embodiments and are not intended to limit the present invention. The term "and / or" used herein includes any and all combinations of one or more related listed items.
[0043] Please refer to Figures 1 to 9 , a para-tert-butyltoluene alkylation reaction system provided by the present invention, comprising a reactor 100, a feeding mechanism 200, an opening and closing mechanism, a premixing mechanism 400, a static mixer 500, and a concentrated sulfuric acid recovery device (not shown in the drawings), wherein the interior of the reactor 100 is hollow to place the premixing mechanism 400 and the static mixer 500. In order to make the alkylation reaction have a suitable temperature, a temperature control device can be provided on the reactor 100, for example, a jacketed reactor 100 is used and a temperature control device is provided in the jacket.
[0044] The top of the reactor 100 is provided with a first liquid flow channel 110 and a storage chamber 120 for storing p-toluenesulfonic acid, and the bottom of the storage chamber 120 is provided with a discharge port 121 to discharge the toluenesulfonic acid in the storage chamber 120. In addition, a sidewall of the first liquid flow channel 110 is provided with an escape port 111. It should be noted that toluenesulfonic acid, also known as p-toluenesulfonic acid, is a non-oxidizing organic strong acid, usually appears in the form of white needles or powder crystals, is easily deliquescent, and can be dissolved in water, alcohol and other polar solvents.
[0045] The feeding mechanism 200 is arranged on the reactor 100, and is used to add methylbenzenesulfonic acid to the first liquid flow channel 110. Specifically, the feeding mechanism 200 includes a first sealing plate 210, a rotating wheel 220 and a driving mechanism 230. The first sealing plate 210 and the driving mechanism 230 are both fixedly arranged on the reactor 100. A portion of the rotating wheel 220 extends into the avoidance port 111 and extends into the first liquid flow channel 110. The driving mechanism 230 is connected to the rotating wheel 220 in a transmission manner, and drives the rotating wheel 220 to rotate at a preset step angle. The upper surface of the first sealing plate 210 slides against the lower surface of the rotating wheel 220. A circle of first through holes 221 distributed in an array is provided along the circumference of the rotating wheel 220. The discharge port 121 slides against the upper surface of the rotating wheel 220 to add methylbenzenesulfonic acid into the first through holes 221 not located in the first liquid flow channel 110. At the same time, due to the sliding contact, when the runner 220 rotates and p-toluenesulfonic acid is added, the toluenesulfonic acid can be prevented from leaking from the gap between the runner 220 and the storage chamber 120. When the p-toluenesulfonic acid in the discharge port 121 enters the first through hole 221, the p-toluenesulfonic acid in the first through hole 221 is temporarily stored due to the blocking effect of the first sealing plate 210. When it is necessary to add toluenesulfonic acid to the first liquid flow channel 110, the driving mechanism 230 drives the runner 220 to rotate at a preset step angle, so that one of the first through holes 221 extends from the avoidance port 111 into the first liquid flow channel 110, and when the runner 220 stops rotating, the first through hole 221 corresponds to the position of the first liquid flow channel 110.
[0046] When isobutylene is introduced into the first liquid flow channel 110, the opening and closing mechanism can open the first liquid flow channel 110, so that the isobutylene and the toluenesulfonic acid in the corresponding first through hole 221 are mixed and flow into the premixing mechanism 400 through the first liquid flow channel 110. When the introduction of isobutylene into the first liquid flow channel 110 is stopped, the opening and closing mechanism can close the first liquid flow channel 110, so that the alkylation reaction area is isolated from the first liquid flow channel 110, so as to avoid the reaction from affecting the operation of adding toluenesulfonic acid and isobutylene.
[0047] The premixing mechanism 400 is arranged in the reactor 100 and below the feeding mechanism 200, and is used to mix concentrated sulfuric acid, isobutylene and p-toluenesulfonic acid so that the three are fully mixed together. The static mixer 500 is connected to the premixing mechanism 400, and the static mixer 500 changes the flow state of the fluid in the tube through the mixing unit body fixed in the tube, so as to achieve the purpose of good dispersion and full mixing between different fluids, to achieve the purpose of accelerating the alkylation reaction, reduce side reactions, and improve product quality. The concentrated sulfuric acid recovery device is used to recover concentrated sulfuric acid from the mixed solution in the static mixer 500, and re-introduce it into the premixing mechanism 400, so as to realize the recycling of concentrated sulfuric acid and reduce the waste of concentrated sulfuric acid.
[0048] In the present embodiment, p-toluenesulfonic acid is periodically added, and the time of the alkylation reaction is shortened by the premixing mechanism 400 and the static mixer 500, side reactions are reduced, the alkylation reaction efficiency is improved, and p-toluenesulfonic acid is fully utilized. At the same time, due to the participation of p-toluenesulfonic acid as a catalyst, the usage amount of the concentrated sulfuric acid can be reduced accordingly. Finally, the concentrated sulfuric acid recovery device can be used to recycle the concentrated sulfuric acid in the reaction product, thereby reducing the waste of the concentrated sulfuric acid. In addition, it should be noted that the concentrated sulfuric acid recovery device in the present application can be used by pyrolysis spent acid technology, and since this technology is prior art, it will not be repeated here.
[0049] In some optional embodiments, such as Figure 2 , Figure 3 As shown, the reaction kettle 100 is provided with a sliding chamber 130, the bottom of the first liquid flow channel 110 is provided with a stepped opening 112, the opening and closing mechanism includes a piston 310, a piston rod 320, a second sealing plate 330, a magnetoelectric component 340, and a first fluid transmission pump 350. The piston 310 is sealed and slidably arranged in the sliding chamber 130 to form a first closed chamber 131 in the sliding chamber 130. The first fluid transmission pump 350 is connected with the first closed chamber 131. The first fluid transmission pump 350 can be used to fill the first closed chamber 131 with fluid material to increase the chamber pressure of the first closed chamber 131, and can also be used to pump out the fluid in the first closed chamber 131 to reduce the chamber pressure of the first closed chamber 131. Optionally, the first fluid transmission pump 350 can be a hydraulic pump or an air pump.
[0050] In order to prevent the p-toluenesulfonic acid in the first through hole 221 from falling into the premixing mechanism 400 when the positions of the first through hole 221 and the first liquid flow channel 110 correspond, a second sealing plate 330 is provided in the first liquid flow channel 110, and the periphery of the second sealing plate 330 has good sealing performance with the inner wall of the first liquid flow channel 110. One end of the piston rod 320 is connected to the piston 310, and the other end of the piston rod 320 extends from the sliding cavity 130 into the first liquid flow channel 110 and is connected to the second sealing plate 330, so that when the piston 310 moves up and down in the sliding cavity 130, the second sealing plate 330 also moves up and down synchronously in the first liquid flow channel 110.
[0051] The magnetoelectric component 340 is used to control the first fluid transmission pump 350 to perform corresponding actions. Figure 4 As shown, when isobutylene is introduced into the first liquid flow channel 110, the impact of the isobutylene solution causes the magnetoelectric component 340 to generate a first electrical signal that triggers the first fluid transmission pump 350 to charge. As the chamber pressure of the first closed chamber 131 gradually increases, the piston 310 moves downward, and then drives the second sealing plate 330 to move downward through the piston rod 320. When the second sealing plate 330 moves to the step opening 112, the second sealing plate 330 cannot seal the first liquid flow channel 110, so that the mixed solution of isobutylene and p-toluenesulfonic acid flows into the pre-mixing mechanism 400. On the contrary, when the introduction of isobutylene into the first liquid flow channel 110 is stopped, the magnetoelectric component 340 generates a second electrical signal to trigger the first fluid transmission pump 350 to pump pressure. As the chamber pressure of the first closed chamber 131 gradually decreases, the piston 310 moves upward, and then drives the second sealing plate 330 to move upward through the piston rod 320 until the second sealing plate 330 moves to a position flush with the first sealing plate 210, which position will not hinder the rotation of the wheel 220. At this time, the second sealing plate 330 recloses the first liquid flow channel 110.
[0052] In some optional embodiments, such as Figure 2 , Figure 3 As shown, the first closed chamber 131 is arranged adjacent to the first liquid flow channel 110, and a limiting groove 113 is provided on the side wall of the first liquid flow channel 110. The limiting groove 113 is located below the rotating wheel 220, and the first closed chamber 131 is located above the rotating wheel 220. One end of the piston rod 320 passes through the limiting groove 113 and is connected to the second sealing plate 330. When the piston 310 slides up and down in the sliding chamber 130, the rod body of the piston rod 320 also slides up and down and is limited in the limiting groove 113 to prevent the piston rod 320 from moving horizontally and improve stability.
[0053] In some optional embodiments, such as Figures 2 to 4As shown, the magnetoelectric component 340 includes a power generation impeller 341 and a voltage conversion circuit module 342. The power generation impeller 341 is electrically connected to the input port of the voltage conversion circuit module 342. Under the impact of the added isobutylene solution, the power generation impeller 341 rotates to generate electricity, which is then transmitted to the voltage conversion circuit module 342, thereby outputting a stable voltage. The charging control circuit of the first fluid transmission pump 350 is provided with a first relay KM1 in a normally open state. When the voltage output by the voltage conversion circuit module 342 acts on the first relay KM1, the coil of the first relay KM1 is energized, and its normally open electric contact switch KM1-1 is closed. At this time, the charging control circuit of the first fluid transmission pump 350 is energized, and then the first fluid transmission pump 350 is controlled to pressurize the first closed chamber 131. For example, when the first fluid transmission pump 350 uses an air pump, the air pump fills gas into the first closed chamber 131 to increase the pressure, and the increased pressure of the gas pushes the piston 310 downward. In addition, the pumping control circuit of the first fluid transmission pump 350 is provided with a second relay KM2 in a normally closed state. When the voltage output by the voltage conversion circuit module 342 acts on the second relay KM2, the coil of the second relay KM2 is energized, and its normally closed electric switch KM2-1 is opened. At this time, the pumping control circuit of the first fluid transmission pump 350 is not energized. When the voltage conversion circuit module 342 does not output voltage, the coil of the second relay KM2 is not energized, and its normally closed electric switch KM2-1 is closed. At this time, the pumping control circuit of the first fluid transmission pump 350 is energized, and then the first fluid transmission pump 350 is controlled to pump pressure on the first closed chamber 131. For example, when the first fluid transmission pump 350 uses an air pump, the air pump extracts the gas in the first closed chamber 131 and reduces the pressure, and the reduced pressure of the gas pushes the piston 310 upward.
[0054] In addition, the first power-off device 351 is provided on both the charging control circuit and the extraction control circuit of the first fluid transmission pump 350. When the pressure is increased so that the second sealing plate 330 moves to the corresponding position of the step opening 112, the first power-off device 351 triggers the coil of the first relay KM1 to lose power, so that the first fluid transmission pump 350 stops the charging operation on the first closed chamber 131. Similarly, when the pressure is reduced so that the second sealing plate 330 moves to a position flush with the first sealing plate 210, the first power-off device 351 triggers the coil of the second relay KM2 to be energized, so that the first fluid transmission pump 350 stops the extraction operation on the first closed chamber 131. The first power-off device 351 can adopt a combined functional module of a single-chip microcomputer and a pressure sensor. The single-chip microcomputer detects the chamber pressure in the first closed chamber 131 through the pressure sensor, and then controls the first relay KM1 or the second relay KM2 according to the pressure value.
[0055] In some optional embodiments, such as Figure 5 , Figure 6As shown, the feeding mechanism 200 further includes a sealing sleeve 240 and a second fluid transmission pump 250. The sealing sleeve 240 is inserted into the first through hole 221, and the middle of the sealing sleeve 240 is penetrated so that when the second sealing plate 330 moves to the step opening 112, isobutylene and p-toluenesulfonic acid can fall from the middle hollow of the sealing sleeve 240 into the premixing mechanism 400. In order to prevent the isobutylene solution from entering other first through holes 221 and the discharge port 121 from the avoidance port 111 when isobutylene is introduced into the first liquid flow channel 110, a second closed chamber 241 is provided in the sealing sleeve 240, and the side wall of the second closed chamber 241 close to the upper surface of the runner 220 is a pleated skin 2411 that can expand and contract. When fluid material is filled into the second closed chamber 241, the chamber pressure of the second closed chamber 241 increases, causing the pleated skin 2411 to expand, thereby blocking the gap between the avoidance port 111 and the wheel 220. Conversely, when fluid material is extracted from the second closed chamber 241, the chamber pressure of the second closed chamber 241 decreases, causing the pleated skin 2411 to contract, thereby not affecting the rotation of the wheel 220 at the avoidance port 111.
[0056] In order to realize the automatic control of pressure increase and pressure reduction, Figure 7As shown, the charging control circuit of the second fluid transmission pump 250 is provided with a third relay KM3 in a normally open state. After the driving mechanism 230 drives the runner 220 to rotate a step angle, the driving mechanism 230 triggers the third relay KM3 to be energized, and its normally open electric contact switch KM3-1 is closed. At this time, the charging control circuit of the second fluid transmission pump 250 is energized, thereby controlling the second fluid transmission pump 250 to pressurize the second closed chamber 241. In order to maintain the triggering effect, a self-locking circuit can be added to the third relay KM3, so that after the trigger signal is cancelled, the third relay KM3 remains in an energized state. Exemplarily, when the second closed chamber 241 uses an air pump, the air pump fills the second closed chamber 241 with gas to increase the pressure, and the gas pressure pushes the pleated skin 2411 to expand upward, thereby blocking the gap between the avoidance port 111 and the runner 220. In addition, the pumping and pressure control circuit of the second fluid transmission pump 250 is provided with a fourth relay KM4 in a normally closed state, and the input port of the voltage conversion circuit module 342 is electrically connected to the fourth relay KM4. When the runner 220 needs to be rotated, since isobutylene is not introduced into the first liquid flow channel 110 at this time, the voltage conversion circuit module 342 does not output voltage, the coil of the fourth relay KM4 loses power, and its normally closed electric switch KM4-1 is closed. At this time, the pumping and pressure control circuit of the second fluid transmission pump 250 is powered, and then the second fluid transmission pump 250 pumps and presses the second closed chamber 241. For example, when the second fluid transmission pump 250 uses an air pump, the air pump extracts the gas in the second closed chamber 241 and reduces the pressure. The pressure reduction of the gas pushes the pleated skin 2411 to shrink downward, and then does not block the gap between the avoidance port 111 and the runner 220. At this time, the avoidance port 111 produces a small resistance force or no resistance force on the rotation of the runner 220. Similarly, when there is no need to rotate the wheel 220, since isobutylene needs to be introduced into the first liquid flow channel 110, the voltage conversion circuit module 342 outputs a voltage, the coil of the fourth relay KM4 is energized, and its normally closed electric switch KM4-1 is opened. At this time, the pressure extraction control circuit of the second fluid transmission pump 250 is not energized, and the second fluid transmission pump 250 does not perform a pressure extraction operation.
[0057] Exemplarily, when the second fluid transmission pump 250 adopts an air pump, the air pump extracts the gas in the second closed chamber 241 to reduce the pressure. The reduced pressure of the gas pushes the pleated skin 2411 to shrink downward, thereby not blocking the gap between the avoidance port 111 and the impeller 220. At this time, the avoidance port 111 produces a small resistance force or no resistance force on the rotation of the impeller 220.
[0058] In addition, a second power-off device 251 is provided on both the charging control circuit and the extraction control circuit of the second fluid transmission pump 250. When the pressure is increased so that the pleated skin 2411 expands to a certain extent, the second power-off device 251 triggers the coil of the third relay KM3 to lose power, so that the second fluid transmission pump 250 stops the charging operation on the second closed chamber 241. Similarly, when the pressure is reduced so that the pleated skin 2411 shrinks to a certain extent, the second power-off device 251 triggers the coil of the fourth relay KM4 to be energized, so that the second fluid transmission pump 250 stops the extraction operation on the second closed chamber 241. The second power-off device 251 can adopt a combined functional module of a single-chip microcomputer and a pressure sensor. The single-chip microcomputer detects the chamber pressure in the second closed chamber 241 through the pressure sensor, and then controls the third relay KM3 or the fourth relay KM4 according to the pressure value.
[0059] In some optional embodiments, such as Figure 1 , Figure 8 As shown, the reactor 100 is provided with a second liquid flow channel 140, the second liquid flow channel 140 is connected to the premixing mechanism 400, the second liquid flow channel 140 is used to connect the concentrated sulfuric acid delivery device and the concentrated sulfuric acid recovery device, and the concentrated sulfuric acid delivery device is used to pass new concentrated sulfuric acid into the premixing mechanism 400 through the second liquid flow channel 140. The premixing mechanism 400 includes a plurality of laminar flow plates 410 stacked in layers, each of which is provided with a plurality of third liquid flow channels 411 arranged in parallel, and each of which is provided with a reflux area 412, one end of the third liquid flow channel 411 is connected to the second liquid flow channel 140, and the reflux area 412 is connected to the first liquid flow channel 110. The same layer of laminar flow plates 410 and the adjacent third liquid flow channels 411 in the upper and lower layers of laminar flow plates 410 are connected through the second through hole 150, and the third liquid flow channel 411 is connected to the reflux area 412 through the second through hole 150. The reflux area 412 is used to reflux and mix the mixed solution of isobutylene and p-toluenesulfonic acid, so that p-toluenesulfonic acid is fully dissolved in the isobutylene solution, and then mixed with the concentrated sulfuric acid in the third liquid flow channel 411 through the second through hole 150. In addition, in order to fully mix the mixed solution of concentrated sulfuric acid and isobutylene, convection needs to be generated when the two meet, so the direction of the mixed solution of isobutylene and p-toluenesulfonic acid and the direction of the concentrated sulfuric acid are set to be different.
[0060] In some optional embodiments, such as Figure 8As shown, in order to further fully mix the mixed solution of concentrated sulfuric acid and isobutylene, the second through holes 150 between adjacent third liquid flow channels 411 in the same layer of laminar flow plates 410 are staggered and distributed to the left side of the input concentrated sulfuric acid. Optionally, the second through holes 150 between adjacent third liquid flow channels 411 in the upper and lower layers of laminar flow plates 410 can be staggered or coaxially arranged. At this time, part of the concentrated sulfuric acid is blocked after flowing into the right side of the third liquid flow channel 411 and refluxes, which increases the degree of convection and makes the added materials fully mixed. Moreover, the length of the area on the right side of the third liquid flow channel 411 where the second through hole 150 is not arranged increases with the number of layers, so that the degree of convection generated by the laminar flow plate 410 of the next layer is reduced, avoiding the flow rate of the mixed solution flowing out of the last layer of laminar flow plates 410 being too large to affect the alkylation reaction.
[0061] In some optional embodiments, such as Figure 1 As shown, in order to facilitate sufficient mixing of the added materials, the laminar flow plate 410 is tiltedly arranged in the reactor 100, so that the materials can quickly pass through the second through holes 150 by gravity, reducing the residence time of the mixed solution and reducing side reactions.
[0062] In some optional embodiments, such as Fig. 9 As shown, since the flow rate of the mixed solution flowing out of the static mixer 500 is relatively high, it is not convenient to separate and extract the reaction product tert-butyltoluene, and to recover the concentrated sulfuric acid in the reaction mixture. For this reason, the tert-butyltoluene alkylation reaction system also includes a reduction mixer 600, and the reduction mixer 600 includes a shell 610, a first type of baffle 620, and a second type of baffle 630. The outlet of the static mixer 500 is connected to one end of the shell 610, and the concentrated sulfuric acid recovery device is connected to the other end of the shell 610. Specifically, in order to achieve pressure reduction, the setting direction of the first type baffle 620 and the second type baffle 630 is perpendicular to the axial direction of the shell 610, and the first type baffle 620 and the second type baffle 630 are staggered and arranged, wherein at least one first through hole 621 is provided in the middle of the first type baffle 620, and at least one second through hole 631 is provided on the circumferential edge of the second type baffle 630, and the first through hole 621 does not overlap with the second through hole 631, so that the blocking effect of the first type baffle 620 and the second type baffle 630 on the solution can be improved, so that the mixed solution can be decelerated.
[0063] In a second aspect, the present invention further provides a method for using a p-tert-butyltoluene alkylation reaction system, which is applied to the aforementioned p-tert-butyltoluene alkylation reaction system, and the method comprises the following steps:
[0064] Step 1: adding p-toluenesulfonic acid into the storage chamber 120;
[0065] Step 2, start the feeding mechanism 200: the driving mechanism 230 drives the rotating wheel 220 to rotate according to a preset step angle, so that one of the first through holes 221 corresponds to the position of the first liquid flow channel 110;
[0066] Step 3: introducing isobutylene into the first liquid flow channel 110, and the opening and closing mechanism is opened under the action of isobutylene, so that the mixed solution of isobutylene and p-toluenesulfonic acid enters the premixing mechanism 400, and at the same time, concentrated sulfuric acid is introduced into the premixing mechanism 400 to mix the concentrated sulfuric acid with the mixed solution of isobutylene and p-toluenesulfonic acid, and finally the mixed solution flows into the static mixer 500 for alkylation reaction, and finally p-tert-butyltoluene can be obtained;
[0067] Step 4: using a concentrated sulfuric acid recovery device to recover concentrated sulfuric acid from the mixed solution in the static mixer 500;
[0068] Step 5: repeat step 2. When the mixed solution of isobutylene and p-toluenesulfonic acid enters the pre-mixing mechanism 400, the concentrated sulfuric acid recovered by the concentrated sulfuric acid recovery device and the new concentrated sulfuric acid are introduced into the pre-mixing mechanism 400 together.
[0069] In the description of this specification, the description with reference to the terms "one embodiment", "some embodiments", "examples", "specific examples", or "some examples" means that the specific features, structures, materials or characteristics described in conjunction with the embodiment or example are included in at least one embodiment or example of the present invention. In this specification, the schematic representation of the above terms does not necessarily refer to the same embodiment or example. Moreover, the specific features, structures, materials or characteristics described may be combined in any one or more embodiments or examples in a suitable manner.
[0070] The above-mentioned embodiments only express several implementation methods of the present invention, and the description thereof is relatively specific and detailed, but it cannot be understood as limiting the scope of the patent of the present invention. It should be pointed out that, for ordinary technicians in this field, several variations and improvements can be made without departing from the concept of the present invention, which all belong to the protection scope of the present invention. Therefore, the protection scope of the patent of the present invention shall be subject to the attached claims.
Claims
1. A p-tert-butyltoluene alkylation reaction system, characterized in that: The p-tert-butyltoluene alkylation reaction system comprises a reaction kettle, a feeding mechanism, an opening and closing mechanism, a premixing mechanism, a static mixer, and a concentrated sulfuric acid recovery device; The top of the reactor is provided with a first liquid flow channel and a storage cavity for storing p-toluenesulfonic acid, the bottom of the storage cavity is provided with a discharge port, and the side wall of the first liquid flow channel is provided with an avoidance port; The feeding mechanism is arranged on the reaction kettle, and the feeding mechanism comprises a first sealing plate, a rotating wheel and a driving mechanism. The first sealing plate and the driving mechanism are both fixedly arranged on the reaction kettle, the first sealing plate slides against the lower surface of the rotating wheel, a circle of first through holes distributed in an array is arranged along the circumference of the rotating wheel, the rotating wheel extends into the first liquid flow channel from the avoidance portion, and the driving mechanism drives the rotating wheel to rotate at a preset step angle so that one of the first through holes is located in the first liquid flow channel, and the discharge port slides against the upper surface of the rotating wheel; The opening and closing mechanism is used to open the first liquid flow channel when isobutylene is introduced into the first liquid flow channel, and to close the first liquid flow channel when the introduction of isobutylene into the first liquid flow channel is stopped; The premixing mechanism is arranged in the reactor and below the feeding mechanism, and is used to mix concentrated sulfuric acid, isobutylene and p-toluenesulfonic acid; The static mixer is connected to the premixing mechanism; The concentrated sulfuric acid recovery device is used to recover concentrated sulfuric acid from the mixed solution in the static mixer and reintroduce it into the premixing mechanism.
2. The alkylation reaction system of p-tert-butyltoluene according to claim 1, characterized in that: The reactor is provided with a sliding cavity, and the bottom of the first liquid flow channel is provided with a stepped opening; The opening and closing mechanism includes a piston, a piston rod, a second sealing plate, a magnetoelectric component, and a first fluid transmission pump. The piston is sealably slidably disposed in the sliding cavity to form a first closed cavity in the sliding cavity. The first fluid transmission pump is connected to the first closed cavity. The second sealing plate is sealably slidably disposed in the first liquid flow channel. One end of the piston rod is connected to the piston, and the other end of the piston rod extends from the sliding cavity into the first liquid flow channel and is connected to the second sealing plate. The magnetoelectric component generates a first electrical signal under the action of the introduced isobutylene to trigger the first fluid transmission pump to charge, so that the piston drives the second sealing plate to move downward until the second sealing plate moves to the step mouth, and generates a second electrical signal to trigger the first fluid transmission pump to pump pressure when there is no isobutylene, so that the piston drives the second sealing plate to move upward until the second sealing plate recloses the first liquid flow channel.
3. The alkylation reaction system of p-tert-butyltoluene according to claim 2, characterized in that: The magnetoelectric component includes a power-generating impeller and a voltage conversion circuit module. The power-generating impeller is electrically connected to the input port of the voltage conversion circuit module. The charging control circuit of the first fluid transmission pump is provided with a first relay in a normally open state, and the extraction control circuit of the first fluid transmission pump is provided with a second relay in a normally closed state. The input ports of the voltage conversion circuit module are both electrically connected to the first relay and the second relay. The charging control circuit and the extraction control circuit of the first fluid transmission pump are both provided with a first power-off device to de-energize the first relay and energize the second relay when the first closed chamber reaches a preset pressure.
4. The p-tert-butyltoluene alkylation reaction system according to claim 3, characterized in that: The feeding mechanism also includes a sealing sleeve and a second fluid transmission pump. The sealing sleeve is inserted into the first through hole and is arranged through the middle part. A second closed chamber is arranged in the sealing sleeve. The side wall of the second closed chamber close to the upper surface of the rotating wheel is a corrugated skin that can expand and contract. The charging control circuit of the second fluid transmission pump is provided with a third relay in a normally open state. After the driving mechanism drives the rotating wheel to rotate a step angle, the third relay is triggered to be energized so that the corrugated skin expands and seals the avoidance port. The extraction control circuit of the second fluid transmission pump is provided with a fourth relay in a normally closed state. The input port of the voltage conversion circuit module is electrically connected to the fourth relay. The charging control circuit and the extraction control circuit of the second fluid transmission pump are both provided with a second power-off device to de-energize the third relay and energize the fourth relay when the second closed chamber reaches a preset pressure.
5. The alkylation reaction system of tert-butyltoluene according to any one of claims 1 to 4, characterized in that the reactor is provided with a second liquid flow channel, the second liquid flow channel is used to connect the concentrated sulfuric acid delivery device and the concentrated sulfuric acid recovery device, the premixing mechanism includes a plurality of stacked laminar flow plates, each layer of the laminar flow plates is provided with a plurality of third liquid flow channels and reflux areas arranged in parallel, one end of the third liquid flow channel is connected to the second liquid flow channel, one end of the reflux area is connected to the first liquid flow channel, the third liquid flow channel and the reflux area are connected to each other through a second through hole, the static mixer is connected to the third liquid flow channel through the second through hole, the reflux area is connected to the first liquid flow channel, so as to introduce a mixed solution of isobutylene and p-toluenesulfonic acid from a first direction, the first liquid flow channel is used to introduce concentrated sulfuric acid from a second direction, wherein, The first direction is different from the second direction.
6. The p-tert-butyltoluene alkylation reaction system according to claim 5, characterized in that: The second through holes on the side walls adjacent to the third liquid flow channels are arranged in a staggered manner and distributed toward the side where concentrated sulfuric acid is input.
7. The p-tert-butyltoluene alkylation reaction system according to claim 6, characterized in that: The laminar flow plate is arranged obliquely in the reactor.
8. The p-tert-butyltoluene alkylation reaction system according to claim 7, characterized in that: The para-tert-butyltoluene alkylation reaction system also includes a reduction mixer, which includes a shell, a first type of baffle, and a second type of baffle. The outlet of the static mixer is connected to one end of the shell, and the concentrated sulfuric acid recovery device is connected to the other end of the shell. The first type of baffle and the second type of baffle are arranged in a direction perpendicular to the axial direction of the shell and are arranged in a staggered manner. At least one first through opening is provided in the middle of the first type of baffle, and at least one second through opening is provided on the circumferential edge of the second type of baffle, and the first through opening does not overlap with the second through opening.
9. The p-tert-butyltoluene alkylation reaction system according to claim 2, characterized in that: The first sealed cavity is arranged adjacent to the first liquid flow channel. A limiting groove is provided on the side wall of the first liquid flow channel. The limiting groove is located below the rotating wheel. The first sealed cavity is located above the rotating wheel. The piston rod is movably limited in the limiting groove.
10. A method for using a p-tert-butyltoluene alkylation reaction system, characterized in that: Applied to the alkylation reaction system of p-tert-butyltoluene according to any one of claims 1 to 9, the method of use comprises the following steps: Step 1, adding p-toluenesulfonic acid into the storage chamber; Step 2, starting the feeding mechanism: the driving mechanism drives the rotating wheel to rotate at a preset step angle so that one of the first through holes corresponds to the position of the first liquid flow channel; Step 3, introducing isobutylene into the first liquid flow channel, and under the action of isobutylene, the opening and closing mechanism opens, so that the mixed solution of isobutylene and p-toluenesulfonic acid enters the premixing mechanism, and at the same time, concentrated sulfuric acid is introduced into the premixing mechanism, and finally the mixed solution flows into the static mixer for reaction to obtain p-tert-butyltoluene; Step 4: using the concentrated sulfuric acid recovery device to recover concentrated sulfuric acid from the mixed solution in the static mixer; Step 5, repeating step 2, when the mixed solution of isobutylene and p-toluenesulfonic acid enters the pre-mixing mechanism, the concentrated sulfuric acid recovered by the concentrated sulfuric acid recovery device and the new concentrated sulfuric acid are introduced into the pre-mixing mechanism together.
