Kettle type and pipe type 2-alkylanthraquinone synthesis device for continuous ring-closure reaction

Abstract

The utility model discloses a kettle type and pipe type 2-alkylanthraquinone synthesis device for continuous ring-closure reaction, which is characterized in that BE acid and fuming sulfuric acid can be slowly dissolved and prepared and temporarily stored through a dissolving kettle at low temperature, so that unnecessary organic matters possibly derived in the dissolving step are reduced; steam with stable temperature circulates in an interlayer of the reaction tube, compared with containers such as tanks and cylinders, the reaction tube can quickly heat a dissolving solution in a smaller and more uniform heat exchange volume and a larger heat exchange area ratio, the dissolving solution can be quickly switched to a required reaction temperature and then is stabilized at the reaction temperature, and the product yield is increased by 10-15%; the closed-loop liquid obtained by the tubular reactor can be immediately cooled by the cooler, and the quickly cooled closed-loop liquid can be immediately collected.

Description

TECHNICAL FIELD

[0001] The utility model relates to 2 -alkyl anthraquinone synthesis with equipment, especially, a kind of 2-alkyl anthraquinone synthesis device of kettle formula plus pipe continuous closed loop reaction. BACKGROUND

[0002] In 2-alkyl anthraquinone synthesis, such as 2-ethylanthraquinone synthesis, refer to Figure 2 , see the prior art CN110790655B "closed loop reaction process for producing 2-ethylanthraquinone", the first kettle tank, dissolving external circulation pump, heating device form closed loop, the first kettle tank exports BE acid and / or oleum. In the closed loop, the mixed solution of BE acid and oleum is pumped to the heater by the external circulation pump to react under heat to obtain closed loop liquid (2-alkyl anthraquinone liquid), and the closed loop liquid returns to the first kettle tank.

[0003] In practice, the optimum temperature for the reaction of the mixed solution to 2-alkyl anthraquinone is 110-130℃, and the mixed solution starts to react to obtain organic matter at ≥80℃; in a certain volume of mixed solution, only part of the area reaches 110-130℃, and the obtained closed loop liquid contains more other organic matter.

[0004] As CN110790655B "closed loop reaction process for producing 2-ethylanthraquinone", the closed loop of the prior art only relies on the heater, and the heater is still essentially a large-volume cavity heated, which is difficult to quickly heat the large-volume dissolving liquid / mixed solution to 110-130℃, and / or difficult to evenly distribute the temperature of 110-130℃ throughout the body, the yield of 2-alkyl anthraquinone is low, the treatment of wastewater obtained by separating the closed loop liquid is difficult, the treatment time is long, and the production cost is high. UTILITY MODEL CONTENTS

[0005] The utility model aims at at least solving one of the above-mentioned technical problems, providing a kind of 2-alkyl anthraquinone synthesis device of kettle formula plus pipe continuous closed loop reaction, it is convenient to accelerate dissolving liquid heating reaction, reduce other organic matter generation rate.

[0006] In order to achieve the above-mentioned purpose, the utility model adopts the technical scheme that:

[0007] A kind of 2-alkyl anthraquinone synthesis device of kettle formula plus pipe continuous closed loop reaction, including dissolving kettle, intermediate liquid buffer tank, pipe reactor and closed loop liquid storage tank;

[0008] The dissolving kettle is suitable for BE acid and oleum mixed solution, the peripheral wall of the dissolving kettle is provided with the first interlayer suitable for covering dissolving liquid and flowing cooling medium, and the dissolving kettle is provided with a thermometer suitable for detecting dissolving liquid;

[0009] The intermediate liquid buffer tank is adapted to receive the overflowed dissolving liquid from the dissolving kettle.

[0010] The tubular reactor comprises a plurality of reaction tubes connected in series, the reaction tubes are surrounded by a first jacket, and the first jacket is adapted to circulate low-pressure steam.

[0011] The closed-loop cooler is provided with a cooling jacket adapted to circulate cooling medium, and the closed-loop cooler is adapted to receive the closed-loop liquid from the tubular reactor, and / or the tubular reactor comprises a sub-tube connected in series with the plurality of reaction tubes, and the sub-tube is provided with a second jacket adapted to circulate cooling medium.

[0012] The closed-loop liquid storage tank and the intermediate liquid buffer tank are connected to the closed-loop cooler or the sub-tube through respective on-off valves.

[0013] Compared with the prior art, the beneficial effects of the present application include: BE acid and oleum can be slowly dissolved and temporarily stored in the dissolving kettle under low temperature control, reducing unnecessary organic matter that may be derived from the dissolving step; the reaction tube circulates stable temperature, and compared with containers such as tanks and cylinders, it has a smaller and more uniform heat exchange volume, a larger heat exchange area ratio, and can quickly heat the dissolving liquid, so that the dissolving liquid can be quickly switched to the required reaction temperature, improving the control of reaction conditions, and increasing the product yield by 10-15%; the closed-loop liquid obtained from the tubular reactor can be immediately cooled and collected.

[0014] As an improvement of the above technical solution, a metering tank is provided, which is adapted to meter the oleum to be added and direct the oleum to the dissolving kettle.

[0015] As an improvement of the above technical solution, a throttle valve is connected in series between the intermediate liquid buffer tank and the tubular reactor.

[0016] As an improvement of the above technical solution, the intermediate liquid buffer tank is connected to the tubular reactor through a preheater.

[0017] As an improvement of the above technical solution, a fifth on-off valve is provided between the preheater and the intermediate liquid buffer tank, a gas feeding inlet is provided between the fifth on-off valve and the preheater, the gas feeding inlet is adapted to be connected to nitrogen, and the tailings of the preheater and the tubular reactor are pressurized and fed into the intermediate liquid buffer tank.

[0018] As an improvement of the above technical solution, a purge outlet is provided between the preheater and the intermediate liquid buffer tank, and a purge inlet is connected to the outlet end of the closed-loop cooler, the purge inlet is adapted to be connected to steam or nitrogen to sequentially purge the closed-loop cooler, the tubular reactor and the preheater.

[0019] As the improvement of the above technical scheme, the first pressure gauge and the second pressure gauge are arranged at two ends of the tubular reactor respectively, and the first pressure gauge and the second pressure gauge are suitable for showing the pressure difference at two ends of the tubular reactor, and indicating the plugging degree of the tubular reactor.

[0020] As the improvement of the above technical scheme, the second sight glass pipe is connected in series between the purge outlet and the preheater, and the second sight glass pipe is suitable for observing the purging effect of the closed loop cooler, the tubular reactor and the preheater.

[0021] As the improvement of the above technical scheme, the bottom of the dissolving kettle is communicated with the external circulation cooler through the dissolving pump, and the external circulation cooler is suitable for cooling the dissolving solution discharged from the dissolving kettle and then returning the dissolving solution to the dissolving kettle.

[0022] As the improvement of the above technical scheme, the first sampling interface is arranged between the external circulation cooler and the dissolving pump. BRIEF DESCRIPTION OF DRAWINGS

[0023] The specific embodiment of the utility model is further described in detail below in combination with the drawings, in which:

[0024] Figure 1 The structure schematic view of the 2-alkylanthraquinone synthesis device of the kettle type plus tubular continuous closed loop reaction for the embodiment of the utility model;

[0025] Figure 2 The structure schematic view of the closed loop reaction 2-alkylanthraquinone synthesis device of the prior art.

[0026] The drawings are only one specific embodiment of the utility model, and the form and structure of the specific embodiment should not limit the widening of other embodiments.

[0027] Dissolving kettle R1, first interlayer R11, closed loop kettle R2;

[0028] Closed loop liquid storage tank V1, intermediate liquid buffer tank V2;

[0029] External circulation cooler E1, preheater E2, closed loop cooler E3, cooling interlayer E31;

[0030] Tubular reactor X1, reaction tube X11, first jacket X111;

[0031] Fourth on-off valve B4, fifth on-off valve B5, seventh on-off valve B7, eighth on-off valve B8;

[0032] Dissolving pump P1, closed loop pump P2;

[0033] Second sight glass pipe S2. DETAILED DESCRIPTION

[0034] The technical solutions in the embodiments of the utility model will be apparently and completely described in connection with the drawings in the embodiments of the utility model. Obviously, the described embodiments are only part of the embodiments of the utility model, rather than all the embodiments. Based on the embodiments in the utility model, all other embodiments obtained by those skilled in the art without creative labor fall within the scope of protection of the utility model.

[0035] With reference to Figure 1 The utility model provides a kind of 2-alkylanthraquinone synthesis device of kettle formula plus tubular continuous closed loop reaction, including dissolving kettle R1, intermediate liquid buffer tank V2, tubular reactor X1 and closed loop liquid storage tank V1;

[0036] Dissolving kettle R1 is suitable for BE acid and mixed solution of sulfuric acid, the peripheral wall of dissolving kettle R1 is provided with the first interlayer R11 suitable for covering dissolving solution and flowing cooling medium, dissolving kettle R1 is provided with temperature gauge suitable for detecting dissolving solution, such as pointer thermometer, digital thermometer, the first interlayer R11 is suitable for making the dissolving solution in dissolving kettle R1 ≤80 ℃, preferably, the dissolving solution in dissolving kettle R1 ≤65 ℃, BE acid and sulfuric acid are stably dissolved, and dissolving solution is in stable mixed and unreacted state;

[0037] Intermediate liquid buffer tank V2 is suitable for receiving the dissolving solution overflowed from dissolving kettle R1;

[0038] Tubular reactor X1 includes multiple sections of reaction tube X11 connected in series, the peripheral wall of reaction tube X11 is surrounded by first jacket X111, and the reaction tube X11 at the head of tubular reactor X1 is suitable for receiving the dissolving solution exported from intermediate liquid buffer tank V2, the first jacket X111 is suitable for flowing low-pressure steam, and the steam temperature is 110-160 ℃ under 0.05-0.5 Mpa, when the first jacket X111 flows low-pressure steam, the first jacket X111 has stable 110-160 ℃ temperature, and the reaction tube X11 is not a cystic container, the reaction tube X11 has small and uniform heat exchange volume and large heat exchange area ratio, so that the dissolving solution can be quickly heated;

[0039] Wherein, it also includes closed loop cooler E3, the closed loop cooler E3 is provided with cooling interlayer E31 suitable for flowing cooling medium, the closed loop cooler E3 is suitable for receiving the closed loop liquid of tubular reactor X1, and / or tubular reactor X1 includes sub-pipe connected in series with the multiple sections of reaction tube X11, and the sub-pipe is provided with second jacket suitable for flowing cooling medium;

[0040] The closed loop liquid storage tank V1 and the intermediate liquid buffer tank V2 are connected with the closed loop cooler E3 or the sub-pipe through respective on-off valves, such as ball valve, gate valve, butterfly valve and the like.

[0041] It can be understood that at least one of the closed loop cooler E3 and the sub-pipe is provided. Figure 1 In an operation process as described below, the sub-pipe is not provided, and the multi-section reaction tube X11 is flowed with steam of corresponding flow, flow rate, and / or pressure, so that the multi-section reaction tube X11 discharges liquid of corresponding temperature at the outlet end, and the plurality of temperatures decreases according to a certain gradient. In some embodiments, the sub-pipe is provided, and the closed loop liquid is rapidly cooled through the sub-pipe.

[0042] Referring to Figure 1 In a specific embodiment of the utility model, the closed loop cooler E3 is provided, the intermediate liquid buffer tank V2 is communicated with the closed loop cooler E3 through the eighth on-off valve B8, and the closed loop liquid storage tank V1 is communicated with the closed loop cooler E3 through the seventh on-off valve B7.

[0043] The heat exchange equipment such as the cooler and the reaction tube X11 is provided with a main channel (capsule cavity) and a sandwich layer. It can be understood that one of the main channel and the sandwich layer is used for flowing the main material, and the other is used for flowing the heat exchange medium. The two modes are only the position exchange of the materials, and belong to the equivalent replacement.

[0044] It can be understood that in order to ensure that the liquid can overcome the drop between the dissolution kettle R1, the intermediate liquid buffer tank V2, the tubular reactor X1 and the closed loop liquid storage tank V1 and the like, and ensure the flow, the pump is arranged in some links. Referring to Figure 1 The closed loop pump P2 is suitable for pumping the dissolution liquid of the intermediate liquid buffer tank V2 to the tubular reactor X1, and the closed loop pump P2 is communicated with the lower end of the intermediate liquid buffer tank V2 and is used for fully pumping the dissolution liquid of the intermediate liquid buffer tank V2.

[0045] Referring to Figure 1 The operation process of the utility model includes the BE acid dissolution step, the dissolution liquid buffering step, and the closed loop reaction step.

[0046] The BE acid dissolution step can be that the dissolution kettle R1 contains oleum, a first sandwich layer R11 of the dissolution kettle R1 flows a cooling medium such as cooling water (tap water, ice water and the like), when the dissolution kettle R1 is ≤35℃, the BE acid is slowly added to the dissolution kettle R1, for example, 0.3±0.1 m 3 / h, if the thermometer shows >60℃, the addition of the BE acid is paused, and the temperature of the dissolution liquid is reduced to ≤35℃.

[0047] The preferred embodiment further includes a metering tank, the metering tank is suitable for metering the oleum to be added and guiding the oleum to the dissolution kettle R1. The utility model can add 3000-3400 kg of oleum to the dissolution kettle R1 through the metering tank, slowly add the BE acid to the dissolution kettle R1 for 2-3 h, and stir the dissolution kettle R1 for 0.5 h after the addition is completed.

[0048] The dissolved solution is stored in the intermediate liquid storage tank V2.

[0049] The closed loop reaction step can be: opening the "intermediate liquid storage tank V2, closed loop pump P2, tubular reactor X1, closed loop cooler E3, intermediate liquid storage tank V2" on the closed loop line, i.e. opening the on-off valve on the line;

[0050] The closed loop pump P2 is started, the tubular reactor X1 is opened, and the dissolved solution starts to flow along the closed loop line;

[0051] A thermometer is arranged at the output end of each reaction tube X11, and steam with corresponding pressure, flow rate and / or flow volume is introduced into each reaction tube X11, so that the temperature at the output end of each reaction tube X11 is sequentially scaled to 125-130℃, 120-130℃, 115-130℃, and 110-120℃ in the direction of the flow of the dissolved solution, and the closed loop cooler E3 is suitable for cooling the material to ≤70℃;

[0052] When the temperature at the output end of each reaction tube X11 reaches the required value, the output end of the closed loop cooler E3 is switched to communicate with the closed loop liquid storage tank V1, i.e. the on-off valve corresponding to the closed loop liquid storage tank V1 is opened and the on-off valve corresponding to the intermediate liquid storage tank V2 is closed, and the dissolved solution is reacted at a primary temperature of 125-130℃ to a large proportion, and the subsequent reaction tubes gradually consume the dissolved solution, so that a large proportion of the dissolved solution evolves into closed loop liquid, which is suitable for being introduced into the closed loop liquid storage tank V1.

[0053] When the closed loop line needs to be stopped for a short period of time, the steam supply to the first jacket X111 of the reaction tube X11 is stopped, and the output end of the closed loop cooler E3 is switched to communicate with the intermediate liquid storage tank V2.

[0054] Referring to Figure 1 The tubular reactor X1 is provided with four reaction tubes X11, and no auxiliary pipe is arranged, each reaction tube X11 is in the shape of U, and steam with corresponding pressure, flow rate and / or flow volume is introduced into each reaction tube X11 to obtain a corresponding temperature.

[0055] Compared with the prior art, the application has the following beneficial effects: the BE acid and oleum can be controlled at low temperature by the dissolving kettle R1, the dissolved solution can be slowly dissolved and temporarily stored, and unnecessary organic matter possibly derived from the dissolving step can be reduced; the reaction tube X11 has a stable temperature, and compared with a tank, a cylinder and other containers, it has a small and uniform heat exchange volume and a large heat exchange area ratio, so that the dissolved solution can be quickly heated to the required reaction temperature, the control of the reaction condition is improved, and the product yield is increased by 10-15%; and the closed loop liquid obtained by the tubular reactor can be immediately cooled and collected.

[0056] Referring to Figure 1The closed loop kettle R2 is suitable for receiving the dissolving solution of the dissolving kettle R1, a second interlayer suitable for covering and heating the dissolving solution is arranged on the peripheral wall of the closed loop kettle R2, the closed loop kettle R2 is provided with a stirring paddle suitable for stirring the dissolving solution in the closed loop kettle R2, and the closed loop kettle R2 is suitable for overflowing the closed loop solution obtained by reaction to the closed loop solution storage tank V1.

[0057] The dissolving solution of the intermediate solution buffer tank V2 can approach room temperature 25℃ instead of 60℃. In some embodiments of the utility model, the intermediate solution buffer tank V2 guides the dissolving solution to the tubular reactor X1 through the preheater E2. After preheating, the dissolving solution can be quickly raised to the required temperature in the reaction tube X11.

[0058] Preferably, the peripheral wall of the intermediate solution buffer tank V2 is provided with a heat preservation layer, and the intermediate solution buffer tank V2 can maintain the temperature of the 35-60℃ dissolving solution of the dissolving kettle R1 for a certain period of time.

[0059] In some embodiments of the utility model, a throttling valve is connected in series between the intermediate solution buffer tank V2 and the tubular reactor X1. In some specific embodiments, the dissolving solution is guided to the tubular reactor X1 at a flow rate of 1.5±0.2 m 3 / h, which is more convenient for controlling the liquid temperature of the reaction tube X11.

[0060] In some embodiments of the utility model, a fifth on-off valve B5 is arranged between the preheater E2 and the intermediate solution buffer tank V2, a gas feeding inlet is arranged between the fifth on-off valve B5 and the preheater E2, the gas feeding inlet is communicated with a fourth on-off valve B4 to control the opening and closing of the gas feeding inlet, the gas feeding inlet is suitable for connecting nitrogen, and the tailings of the preheater E2 and the tubular reactor X1 are pressurized and fed into the intermediate solution buffer tank V2.

[0061] In some embodiments of the utility model, a purging outlet is arranged between the preheater E2 and the intermediate solution buffer tank V2, and a purging inlet is communicated with the outlet end of the closed loop cooler E3, the purging inlet is suitable for introducing steam or nitrogen to sequentially purge the closed loop cooler E3, the tubular reactor X1 and the preheater E2. That is, the closed loop cooler E3, the tubular reactor X1 and the preheater E2 are reversely purged.

[0062] Further preferably, a second sight glass tube S2 is connected in series between the purging outlet and the preheater E2, and the second sight glass tube S2 is adapted to observe the purging effect of the closed loop cooler E3, the tubular reactor X1 and the preheater E2. By using steam to heat the stubborn material in the closed loop cooler E3, the tubular reactor X1 and the preheater E2, the flow of the steam is also adapted to purge the stubborn material and the residual material, i.e. the second sight glass tube S2 observes that there is no colorless condensed water in it, and then the residual material and the water vapor are purged by using nitrogen, so that the closed loop cooler E3, the tubular reactor X1 and the preheater E2 are kept clean and dry after shutdown, i.e. the second sight glass tube S2 observes that there is no obvious water vapor in it.

[0063] Preferably, the purging outlet is connected to a collection tank, so as to avoid the material blown out of the purging outlet from splashing and injuring people; and the purging effect can be determined by the second sight glass tube S2.

[0064] In some embodiments of the present application, the bottom of the dissolving kettle R1 is connected to an external circulation cooler E1 through a dissolving pump P1, and the external circulation cooler E1 is provided with an external cooling layer, and the external circulation cooler E1 is adapted to cool the dissolving solution discharged from the dissolving kettle R1 and then return it to the dissolving kettle R1.

[0065] In some embodiments of the present application, the tubular reactor X1 is provided with a first pressure gauge and a second pressure gauge at two ends thereof, i.e. instruments for measuring fluid pressure, such as a pointer type instrument similar to a thermometer or a digital instrument, and the first pressure gauge and the second pressure gauge are adapted to display the pressure difference between the two ends of the tubular reactor X1 and indicate the sealing degree of the tubular reactor X1.

[0066] In some embodiments of the present application, a first sampling interface is arranged between the external circulation cooler E1 and the dissolving pump P1, so as to determine the compatibility of B acid and oleum and determine whether to continue stirring and external circulation; and a second sampling interface is arranged between the intermediate liquid buffer tank V2 and the preheater E2.

[0067] The above embodiments are only used to illustrate the technical solutions of the present application but not to limit it, and any modification or equivalent replacement within the spirit and scope of the present application should be covered in the scope of the technical solutions of the present application.

Claims

1. A 2-alkylanthraquinone synthesis apparatus of a kettle-tube continuous closed loop reaction, characterized by, The device comprises a dissolving kettle, an intermediate liquid buffer tank, a tubular reactor and a closed loop liquid storage tank. The dissolving kettle is suitable for mixing and dissolving BE acid and oleum, and the peripheral wall of the dissolving kettle is provided with a first interlayer suitable for covering the dissolving liquid and circulating cooling medium. The intermediate liquid buffer tank is suitable for receiving the overflow of the dissolving kettle. The tubular reactor comprises a plurality of reaction tubes connected in series, and the peripheral wall of the reaction tube is surrounded by a first jacket. The closed loop cooler is provided with a cooling interlayer suitable for circulating cooling medium, and the closed loop cooler is suitable for receiving the closed loop liquid of the tubular reactor. The closed loop liquid storage tank and the intermediate liquid buffer tank are connected to the closed loop cooler or the auxiliary pipe through respective on-off valves.

2. The 2-alkylanthraquinone synthesis apparatus of tubular continuous closed loop reaction according to claim 1, characterized by, The metering tank is suitable for metering the oleum to be added and guiding the oleum to the dissolving kettle.

3. The 2-alkylanthraquinone synthesis apparatus of tubularization of a continuous closed loop reaction according to claim 1, characterized by, A throttle valve is connected in series between the intermediate liquid buffer tank and the tubular reactor.

4. The 2-alkylanthraquinone synthesis apparatus of any one of claims 1 to 3, wherein The intermediate liquid buffer tank guides the dissolving liquid to the tubular reactor through a preheater.

5. The 2-alkylanthraquinone synthesis apparatus of kettle plus tubular continuous closed loop reaction according to any one of claims 1 to 3, characterized in that, A fifth on-off valve is provided between the preheater and the intermediate liquid buffer tank, a gas inlet is provided between the fifth on-off valve and the preheater, the gas inlet is suitable for connecting nitrogen, and the preheater, the tail of the tubular reactor and the intermediate liquid buffer tank are pressurized to send nitrogen into the intermediate liquid buffer tank.

6. The 2-alkylanthraquinone synthesis apparatus of tubularization of a continuous closed loop reaction according to claim 4, characterized by, A purge outlet is provided between the preheater and the intermediate liquid buffer tank, and a purge inlet is connected to the outlet end of the closed loop cooler.

7. The 2-alkylanthraquinone synthesis apparatus of tubular-in-pot continuous closed loop reaction according to claim 6, characterized in that, A first pressure gauge and a second pressure gauge are respectively provided at the two ends of the tubular reactor, and the first pressure gauge and the second pressure gauge are suitable for displaying the pressure difference between the two ends of the tubular reactor and indicating the sealing degree of the tubular reactor.

8. The 2-alkylanthraquinone synthesis apparatus of tubularization of a continuous closed loop reaction according to claim 6, characterized by, A second sight glass pipe is connected in series between the purge outlet and the preheater, and the second sight glass pipe is suitable for observing the purging effect of the closed loop cooler, the tubular reactor and the preheater.

9. The 2-alkylanthraquinone synthesis apparatus of kettle plus tubular continuous closed loop reaction according to any one of claims 1 to 3, characterized in that, The bottom of the dissolving kettle is connected to an external circulation cooler through a dissolving pump, and the external circulation cooler is suitable for cooling the dissolving liquid discharged from the dissolving kettle and then guiding it back to the dissolving kettle.

10. The 2-alkylanthraquinone synthesis apparatus of tubular-in-pot continuous closed loop reaction according to claim 9, characterized in that, A first sampling interface is provided between the external circulation cooler and the dissolving pump.

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