Synthesis system of pentamethylindane

Abstract

The system comprises a reaction kettle and a tubular heat exchanger, a stirring mechanism is arranged in the reaction kettle, the top end of the reaction kettle is provided with a raw material dropping port and a circulating liquid inlet, and the bottom end of the reaction kettle is provided with a discharge port and a circulating liquid outlet. The circulating liquid outlet is communicated with a shell pass inlet of the shell-and-tube heat exchanger through a first guide pipe, a material pump is arranged on the first guide pipe, a shell pass outlet of the shell-and-tube heat exchanger is communicated with the circulating liquid inlet of the reaction kettle through a second guide pipe, the stirring mechanism comprises a stirring shaft, and stirring blades are distributed on the stirring shaft at equal intervals. The stirring shaft is driven by a rotating motor mounted at the top end of the reaction kettle to rotate. The tubular heat exchanger is additionally arranged to circularly cool the reaction liquid, so that the heat released by the reaction can be quickly absorbed, the reaction temperature can be effectively controlled, the reaction yield can be improved, the dripping speed can be accelerated, the reaction time can be shortened, the productivity can be improved, the energy consumption can be reduced, and the economic benefit can be improved.

Description

Technical Field

[0001] The invention relates to the technical field of pentamethylindane synthesis, in particular to a pentamethylindane synthesis system. Background Art

[0002] Galaxolide is the first synthetic musk developed by International Flavors & Fragrances (IFF) in the 1960s. It has a molecular weight of 258.4, a boiling point of 129°C (107 Pa), and a chemical name of 1,3,4,6,7,8-hexahydro-4,6,6,7,8,8-hexamethylcyclopenta-γ-2-benzopyran. It has a strong and lasting musk aroma, accompanied by a woody aroma, and is widely used in cosmetics, soap flavors and other industries.

[0003] At present, the main industrial route is to react α-methylstyrene and isopentene with phosphoric acid as a catalyst to generate pentamethylindane, and then the pentamethylindane and propylene oxide are subjected to Friedel-Crafts alkylation to obtain hexamethylindanol, and the hexamethylindanol is reacted with methylal to obtain the product galaxol. The reaction mechanism is as follows:

[0004]

[0005] In the actual industrial production of galaxolide, the reaction temperature has a significant effect on the reaction yield. However, the heat released in the middle and late stages of the reaction is large, and it is difficult for existing equipment to effectively control the reaction temperature. The temperature can often only be controlled by reducing the drop rate, resulting in prolonged reaction time, limited output, and increased energy consumption. Therefore, developing a method that can quickly absorb the heat released by the reaction is of great significance for improving the efficiency of pentamethylindane reactions and reducing energy consumption. Summary of the invention

[0006] In order to solve the problems mentioned in the above background technology, the present invention provides a synthesis system of pentamethylindane.

[0007] In order to achieve the above object, the present invention adopts the following technical solutions:

[0008] A pentamethylindane synthesis system comprises a reactor and a tube-and-tube heat exchanger, wherein a stirring mechanism is arranged in the reactor, a raw material drop-inlet and a circulating liquid inlet are arranged at the top of the reactor, a discharge port and a circulating liquid outlet are arranged at the bottom of the reactor, the circulating liquid outlet is connected to a shell-side inlet of the tube-and-tube heat exchanger through a first conduit, a material pump is arranged on the first conduit, and the shell-side outlet of the tube-and-tube heat exchanger is connected to the circulating liquid inlet of the reactor through a second conduit.

[0009] Preferably, the stirring mechanism comprises a stirring shaft, stirring blades are evenly distributed on the stirring shaft, and the stirring shaft is driven to rotate by a rotary motor installed on the top of the reaction kettle.

[0010] Preferably, the bottom end of the circulating liquid inlet extends to the interior of the reactor and is connected to a plurality of liquid separation vertical pipes.

[0011] Preferably, the plurality of liquid separation vertical tubes are distributed in a ring array, and a liquid separation horizontal tube is fixed on the liquid separation vertical tube, and a plurality of liquid outlet holes are opened on the liquid separation horizontal tube.

[0012] Preferably, the heights of the liquid separation transverse tubes on the plurality of liquid separation vertical tubes are staggered with each other, and the positions of the liquid separation transverse tubes and the stirring blades of the stirring mechanism are staggered.

[0013] Preferably, an annular communicating vessel is fixed to the bottom end of the circulating liquid inlet, the top end of the liquid separation vertical pipe is in sliding contact with the bottom end of the annular communicating vessel through an annular baffle, an opening is provided on the annular baffle at a position corresponding to the liquid separation vertical pipe, and the liquid separation vertical pipe is connected to the stirring shaft through a transmission assembly.

[0014] Preferably, an annular guide rail is provided on the inner wall of the reactor, a moving ring is rotatably mounted on the annular guide rail, and the moving ring is fixed to the liquid separation vertical pipe.

[0015] Preferably, the transmission assembly is connected to a planetary reducer, the planetary reducer is fixed to the shell and tube heat exchanger, the planetary reducer is sleeved and installed on the outside of the stirring shaft, and the stirring shaft is fixed to the sun gear of the planetary reducer, and the planetary frame of the planetary reducer is fixed to the liquid separation vertical pipe.

[0016] Preferably, a liquid outlet is provided at the bottom end of the annular communicating vessel, the liquid outlet is an arc-shaped structure, and the position of the liquid outlet corresponds to the liquid separation vertical pipe.

[0017] Preferably, the curvature of the liquid separation vertical tube is smaller than the angle formed between adjacent liquid separation vertical tubes.

[0018] Compared with the prior art, the present invention has the following beneficial effects:

[0019] 1. The circulating liquid inlet is connected to a plurality of liquid separation vertical pipes arranged in a circular array, and the heights of the liquid separation horizontal pipes are staggered with each other and the positions of the stirring blades to avoid interference while entering the reactor from different heights, thereby improving the mixing effect and the cooling effect, and thus improving the reaction efficiency.

[0020] 2. The stirring mechanism installed in the reactor includes a stirring shaft and stirring blades distributed at equal distances, which are driven by a rotary motor to ensure that the materials are fully mixed and stirred evenly, which is beneficial to the reaction and improves the reaction efficiency.

[0021] 3. The equidistant distribution of the stirring blades further ensures the uniformity of stirring, making the reaction more complete and stable, which helps to improve product quality. Multiple liquid separation vertical pipes spray liquid alternately, increasing the liquid spraying pressure, improving the mixing effect and heat transfer effect, making the reaction more uniform and stable, thereby improving product quality.

[0022] 4. The rotational power of the stirring shaft is transmitted to the liquid separation vertical pipe through the planetary reducer, which not only simplifies the transmission structure, but also makes the rotation of the liquid separation vertical pipe synchronized with the rotation of the stirring shaft, further improving the overall efficiency of the system.

[0023] 5. By adding a shell-and-tube heat exchanger to circulate and cool the reaction liquid, the heat released by the reaction can be quickly absorbed, the reaction temperature can be effectively controlled, the reaction yield can be improved, the dropwise addition speed can be accelerated, the reaction time can be reduced, the production capacity can be increased, the energy consumption can be reduced, and the economic benefits can be improved. BRIEF DESCRIPTION OF THE DRAWINGS

[0024] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative work.

[0025] Figure 1 It is an overall schematic diagram of the present invention;

[0026] Figure 2 It is an enlarged detail view of the reaction kettle of the present invention;

[0027] Figure 3 It is a cross-sectional view of a reaction kettle of the present invention;

[0028] Figure 4 This is a front view of the internal structure of the reactor of the present invention;

[0029] Figure 5 This is a first-view stereoscopic diagram of the internal structure of the reactor of the present invention;

[0030] Figure 6 A second perspective stereoscopic view of the internal structure of the reactor of the present invention;

[0031] Figure 7 It is a third perspective stereogram of the internal structure of the reactor of the present invention;

[0032] Figure 8 This is a fourth perspective stereogram of the internal structure of the reactor of the present invention;

[0033] In the figure: reactor 1, raw material dropping port 101, discharge port 102, circulating liquid inlet 103, circulating liquid outlet 104, rotating motor 2, stirring shaft 201, stirring blade 202, annular communicating vessel 3, liquid outlet 301, annular baffle 4, liquid separation vertical pipe 401, annular guide rail 402, liquid separation horizontal pipe 403, liquid outlet hole 404, planetary reducer 5, shell and tube heat exchanger 6, first conduit 601, second conduit 602. DETAILED DESCRIPTION

[0034] In order to make the purpose, technical solution and advantages of the embodiments of the present invention clearer, the technical solution in the embodiments of the present invention will be clearly and completely described below in conjunction with the drawings in the embodiments of the present invention. Obviously, the described embodiments are part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0035] Example 1

[0036] Reference Figure 1-8 A pentamethylindane synthesis system comprises a reactor 1 and a tube-and-tube heat exchanger 6, wherein a stirring mechanism is provided in the reactor 1, a raw material drop-inlet 101 and a circulating liquid inlet 103 are provided at the top of the reactor 1, a discharge port 102 and a circulating liquid outlet 104 are provided at the bottom of the reactor 1, the circulating liquid outlet 104 is connected to the shell-side inlet of the tube-and-tube heat exchanger 6 through a first conduit 601, and a material pump is provided on the first conduit 601, and the shell-side outlet of the tube-and-tube heat exchanger 6 is connected to the circulating liquid inlet 103 of the reactor 1 through a second conduit 602;

[0037] Mix methyl styrene and isopentene in a mass ratio of 1.7:1, and use a drip pump to pump the mixture into a reactor 1 filled with 4000 kg of 89% phosphoric acid at a certain speed. Turn on the material pump to allow the reaction liquid to flow between the reactor 1 and the tube-in-tube heat exchanger 6 (heat exchange area of ​​40 m 2 ) circulates between the reactor and the reactor, and the methyl styrene and isopentene mixture is slowly dripped into the reactor by the drip pump, and the reaction begins under the action of the catalyst phosphoric acid. The temperature monitoring system monitors the temperature of the reaction liquid in real time (the upper limit temperature is 34°C and the lower limit temperature is 30°C). When the temperature reaches the set upper limit value, the temperature control system automatically opens the cooling water valve, so that the cooling water cools the reaction liquid through the shell and tube heat exchanger 6. As the temperature drops, the opening of the cooling water valve is gradually reduced. When the temperature is lower than the set lower limit value, the cooling water valve is closed and the cooling is stopped. During the reaction process, the dripping speed of the dripping pump is adjusted in time according to the change of temperature to control the reaction rate and ensure the smooth progress of the reaction. When the reaction reaches the expected degree (the mass of the methyl styrene and isopentene mixture is 3420kg), the material is stopped from being dripped, the circulation pump and the temperature control system are closed, and the reaction product is subjected to subsequent treatment.

[0038] Among them, the stirring mechanism includes a stirring shaft 201, on which stirring blades 202 are evenly distributed, and the stirring shaft 201 is driven to rotate by a rotating motor 2 installed on the top of the reactor 1. Through the stirring shaft 201 and the stirring blades 202 in the stirring mechanism, the system can ensure that the materials in the reactor 1 are fully mixed and evenly stirred, thereby improving the reaction efficiency and product quality. The evenly distributed stirring blades 202 further ensure the uniformity of stirring.

[0039] Among them, the bottom end of the circulating liquid inlet 103 extends to the interior of the reactor 1 and is connected to multiple liquid separation vertical pipes 401. This design allows the circulating liquid to cover the materials in the reactor 1 more widely, improves the heat exchange efficiency, and helps to control the reaction temperature.

[0040] The plurality of liquid separation vertical pipes 401 are distributed in a circular array, and a liquid separation horizontal pipe 403 is fixed on the liquid separation vertical pipe 401 , and a plurality of liquid outlet holes 404 are opened on the liquid separation horizontal pipe 403 .

[0041] Among them, the heights of the liquid separation transverse tubes 403 on the multiple liquid separation vertical tubes 401 are staggered with each other, and the positions of the liquid separation transverse tubes 403 and the stirring blades 202 of the stirring mechanism are staggered. The heights of the liquid separation transverse tubes 403 are staggered with each other and with the stirring blades 202, which avoids mutual interference and ensures the stable operation of the system. The circulated liquid can enter the reaction liquid retained in the reactor 1 from different heights, further improving the mixing effect and the cooling effect.

[0042] Among them, an annular communicating vessel 3 is fixed to the bottom end of the circulating liquid inlet 103, and the top of the liquid separation vertical pipe 401 is in sliding contact with the bottom end of the annular communicating vessel 3 through an annular baffle 4. An opening is provided on the annular baffle 4 at a position corresponding to the liquid separation vertical pipe 401, and the liquid separation vertical pipe 401 is connected to the stirring shaft 201 through a transmission component.

[0043] Among them, an annular guide rail 402 is provided on the inner wall of the reactor 1, and a moving ring is rotatably installed on the annular guide rail 402. The moving ring is fixed to the liquid separation vertical pipe 401. The cooperation of the annular guide rail 402 and the moving ring provides stable support and guidance for the rotation of the liquid separation vertical pipe.

[0044] Among them, the transmission component is connected to the planetary reducer 5, the planetary reducer 5 is fixed to the shell-and-tube heat exchanger 6, the planetary reducer 5 is sleeved and installed on the outside of the stirring shaft 201, and the stirring shaft 201 is fixed to the sun gear of the planetary reducer 5, and the planetary frame of the planetary reducer 5 is fixed to the liquid separation vertical pipe 401. The rotational power of the stirring shaft 201 is transmitted to the liquid separation vertical pipe 401 through the planetary reducer 5, so that the liquid separation vertical pipe can rotate with the stirring shaft 201. This design not only simplifies the transmission structure, but also keeps the rotation of the liquid separation vertical pipe synchronized with the rotation of the stirring shaft, further improving the overall efficiency of the system.

[0045] Among them, a liquid outlet 301 is opened at the bottom end of the annular communicating vessel 3, and the liquid outlet 301 is an arc-shaped structure. The position of the liquid outlet 301 corresponds to the liquid separation vertical pipe 401. The curvature of the liquid separation vertical pipe 401 is smaller than the angle formed between adjacent liquid separation vertical pipes 401. Due to the deceleration effect of the planetary reducer 5 sets, the rotation speed of the liquid separation vertical pipe 401 is reduced. When the liquid separation vertical pipe 401 rotates to the position corresponding to the liquid outlet 301, the circulating liquid can enter the liquid separation vertical pipe 401. Since the curvature of the liquid separation vertical pipe 401 is smaller than the angle formed between adjacent liquid separation vertical pipes 401, only one liquid separation vertical pipe 401 will enter the circulating liquid at the same time. Multiple liquid separation vertical pipes 401 alternately spray liquid, which can greatly increase the liquid spraying pressure, improve the mixing effect and heat transfer effect, and can cool down and accelerate the reaction more quickly.

[0046] Example 2

[0047] 1. Preparation of the reactor: Select a pentamethylindane reactor and connect it to the temperature control system to ensure the sealing and stability of the reactor and related equipment.

[0048] 2. Material preparation: Mix methyl styrene and isopentene in a mass ratio of 1.7:1 to form 3420 kg of a mixture, and use a drip pump to pump the mixture into a reactor filled with 4000 kg of 89% phosphoric acid at a rate of 150 kg / h.

[0049] 3. Reaction start: Turn on the circulation pump to circulate the reaction solution in the reactor. Slowly drip the methylstyrene and isopentene mixture into the reactor through the drip pump, and start the reaction under the action of the catalyst phosphoric acid.

[0050] 4. Temperature monitoring and control: The temperature monitoring system monitors the temperature of the reaction liquid in real time. When the temperature reaches 34°C, the temperature control system automatically opens the cooling water valve to allow the cooling water to pass through the reactor jacket to cool the reaction liquid. As the temperature drops, the opening of the cooling water valve is gradually reduced. When the temperature is below 30°C, the cooling water valve is closed to stop cooling.

[0051] 5. Reaction process control: During the reaction process, the dripping speed of the dripping pump is adjusted in time according to the change of temperature to control the reaction rate and ensure the smooth progress of the reaction.

[0052] 6. End of reaction: When 3420 kg of the mixed material has been added dropwise, the addition of materials is stopped. After keeping warm for one hour, the circulation pump and the temperature control system are turned off, and the reaction product is subjected to subsequent treatment.

[0053] Example 3

[0054] 1. Preparation of the reactor: Select a pentamethylindane reactor and install a heat exchanger with a heat exchange area of ​​40m at the bottom of the reactor.2 The shell and tube heat exchanger is connected with the temperature control system. Ensure the sealing and stability of the reactor and related equipment.

[0055] 2. Material preparation: Mix methyl styrene and isopentene in a mass ratio of 1.7:1 to form 3420 kg of a mixture, and use a drip pump to pump the mixture into a reactor filled with 4000 kg of 89% phosphoric acid at a rate of 200 kg / h.

[0056] 3. Reaction start: Turn on the circulation pump to circulate the reaction liquid between the reactor and the shell-and-tube heat exchanger. Slowly drip the methylstyrene and isopentene mixture into the reactor through the drip pump, and start the reaction under the action of the catalyst phosphoric acid.

[0057] 4. Temperature monitoring and control: The temperature monitoring system monitors the temperature of the reaction liquid in real time. When the temperature reaches 34°C, the temperature control system automatically opens the cooling water valve, allowing the cooling water to cool the reaction liquid through the shell-and-tube heat exchanger. As the temperature drops, the opening of the cooling water valve is gradually reduced. When the temperature is below 30°C, the cooling water valve is closed and the cooling is stopped.

[0058] 5. Reaction process control: During the reaction process, the dripping speed of the dripping pump is adjusted in time according to the change of temperature to control the reaction rate and ensure the smooth progress of the reaction.

[0059] 6. End of reaction: When 3420 kg of the mixed material has been added dropwise, the addition of materials is stopped. After keeping warm for one hour, the circulation pump and the temperature control system are turned off, and the reaction product is subjected to subsequent treatment.

[0060] Table 1 Comparison of reaction effects of adding shell-and-tube heat exchangers

[0061] Reaction time / h Indane content / % Isomer content / % Example 1 26 59.46 6.84 Example 2 18 61.42 6.64

[0062] As shown in Table 1, adding a shell-and-tube heat exchanger and a matching temperature control system to the pentamethylindane reactor can quickly absorb the heat released by the reaction, effectively control the reaction temperature, and improve the reaction yield; it can also speed up the dropwise addition, reduce the reaction time, and increase the production capacity; it can also reduce energy consumption and improve economic benefits.

[0063] In the description of the present invention, it should be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inside", "outside", "clockwise", "counterclockwise", "axial", "radial", "circumferential" and the like indicate orientations or positional relationships based on the orientations or positional relationships shown in the accompanying drawings, and are only for the convenience of describing the present invention and simplifying the description, and do not indicate or imply that the referred device or element must have a specific orientation, be constructed and operated in a specific orientation, and therefore should not be understood as limiting the present invention.

[0064] In the present invention, unless otherwise clearly specified and limited, the terms "set", "install", "connect", "connect", "fix" and the like should be understood in a broad sense, for example, it can be a fixed connection, a detachable connection, or an integral one; it can be a mechanical connection, a direct connection, or an indirect connection through an intermediate medium, it can be the internal connection of two elements or the interaction relationship between two elements. For ordinary technicians in this field, the specific meanings of the above terms in the present invention can be understood according to specific circumstances.

[0065] The control method of the present invention is automatic control through a controller. The control circuit of the controller can be implemented by simple programming by technicians in this field. The provision of power is also common knowledge in this field. The present invention is mainly used to protect mechanical devices, so the present invention will no longer explain the control method and circuit connection in detail.

[0066] The above description is only a preferred specific implementation manner of the present invention, but the protection scope of the present invention is not limited thereto. Any technician familiar with the technical field can make equivalent replacements or changes according to the technical scheme and inventive concept of the present invention within the technical scope disclosed by the present invention, which should be covered by the protection scope of the present invention.

Claims

1. A system for synthesizing pentamethylindane, comprising a reaction vessel (1) and a shell-and-tube heat exchanger (6), characterized in that: The reactor (1) is provided with a stirring mechanism, the top of the reactor (1) is provided with a raw material drop-inlet (101) and a circulating liquid inlet (103), the bottom of the reactor (1) is provided with a discharge port (102) and a circulating liquid outlet (104), the circulating liquid outlet (104) is connected to the shell-side inlet of the shell-and-tube heat exchanger (6) through a first conduit (601), and a material pump is provided on the first conduit (601), and the shell-side outlet of the shell-and-tube heat exchanger (6) is connected to the circulating liquid inlet (103) of the reactor (1) through a second conduit (602).

2. A synthesis system of pentamethylindane according to claim 1, characterized in that: The stirring mechanism comprises a stirring shaft (201), stirring blades (202) are evenly distributed on the stirring shaft (201), and the stirring shaft (201) is driven to rotate by a rotating motor (2) installed at the top of the reaction kettle (1).

3. A synthesis system of pentamethylindane according to claim 2, characterized in that: The bottom end of the circulating liquid inlet (103) extends to the interior of the reaction kettle (1) and is connected to a plurality of liquid separation vertical pipes (401).

4. A synthesis system of pentamethylindane according to claim 3, characterized in that: The plurality of liquid separation vertical pipes (401) are distributed in a circular array, and a liquid separation horizontal pipe (403) is fixed on the liquid separation vertical pipe (401), and a plurality of liquid outlet holes (404) are opened on the liquid separation horizontal pipe (403).

5. A synthesis system of pentamethylindane according to claim 4, characterized in that: The liquid separation transverse tubes (403) on the plurality of liquid separation vertical tubes (401) are staggered in height, and the liquid separation transverse tubes (403) and the stirring blades (202) of the stirring mechanism are staggered in position.

6. A synthesis system of pentamethylindane according to claim 3, characterized in that: An annular communicating vessel (3) is fixed to the bottom end of the circulating liquid inlet (103); the top end of the liquid separation vertical pipe (401) is in sliding contact with the bottom end of the annular communicating vessel (3) via an annular baffle (4); an opening is provided on the annular baffle (4) at a position corresponding to the liquid separation vertical pipe (401); and the liquid separation vertical pipe (401) is connected to the stirring shaft (201) via a transmission assembly.

7. A synthesis system of pentamethylindane according to claim 6, characterized in that: An annular guide rail (402) is provided on the inner wall of the reaction kettle (1), and a moving ring is rotatably mounted on the annular guide rail (402), and the moving ring is fixed to the liquid separation vertical pipe (401).

8. A synthesis system of pentamethylindane according to claim 6, characterized in that: The transmission assembly is connected to a planetary reducer (5), the planetary reducer (5) is fixed to the shell-and-tube heat exchanger (6), the planetary reducer (5) is sleeved and installed on the outside of the stirring shaft (201), the stirring shaft (201) is fixed to the sun gear of the planetary reducer (5), and the planetary carrier of the planetary reducer (5) is fixed to the liquid separation vertical pipe (401).

9. A pentamethylindane synthesis system according to claim 6, characterized in that: A liquid outlet (301) is provided at the bottom end of the annular communicating vessel (3); the liquid outlet (301) is an arc-shaped structure, and the position of the liquid outlet (301) corresponds to the liquid separation vertical pipe (401).

10. A pentamethylindane synthesis system according to claim 6, characterized in that: The curvature of the liquid separation vertical tube (401) is smaller than the angle formed between adjacent liquid separation vertical tubes (401).

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