A reaction device for continuously synthesizing high-boiling-point carboxylic acid esters

By designing a reasonable reaction device structure, timely replacement of catalysts and effective separation of moisture are achieved, and the problems of inconvenient catalyst replacement and difficulty in repairing heating devices in existing devices are solved, and the reaction efficiency and convenience of device maintenance are improved.

CN117205843BActive Publication Date: 2025-08-29HENGYANG FENGLIAN FINE CHEM CO LTD
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Patent Information

Application Number
CN202311052308.6
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2023-08-21
Publication Date
2025-08-29
Estimated Expiration
2043-08-21

AI Technical Summary

Technical Problem

The catalyst replacement in the existing continuous dehydration and esterification reaction device is inconvenient, and the heating device is not conducive to maintenance and affects the reaction efficiency.

Method used

A reaction device including a main body shell, a connecting square tube, a catalyst mixing device, a vacuum pump and a condensation absorption device is designed. Water is extracted through a vacuum pump, moisture is absorbed by silicone particles, and the rubber tube is cleaned to clean the molecular sieve tube. The catalyst movement system realizes timely replacement and separation of catalysts.

Benefits of technology

It realizes timely replacement of catalysts and effective separation of moisture, improves reaction efficiency, and simplifies the maintenance and maintenance process of the device.

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Abstract

The present invention relates to the technical field of chemical synthesis devices, and in particular to a reaction device for continuously synthesizing high-boiling-point carboxylic acid esters. A technical problem is that existing continuous dehydration esterification reaction devices cannot replace catalysts in a timely manner and lack a heating method, which is not conducive to maintenance. The technical solution is: a reaction device for continuously synthesizing high-boiling-point carboxylic acid esters, comprising a main body shell, a connecting square tube, a silica gel treatment device, and a catalyst mixing device; the main body shell is fixedly connected to a connecting square tube; the connecting square tube is connected to the silica gel treatment device; and the main body shell is connected to the catalyst mixing device. The reaction device for continuously synthesizing high-boiling-point carboxylic acid esters of the present invention achieves the functions of timely separating unsuitable catalysts, separating water from reaction products, and heating the reaction vessel through a rationally designed structure.
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Description

Technical Field

[0001] The present invention relates to the technical field of chemical synthesis devices, in particular to a reaction device for continuously synthesizing high-boiling-point carboxylic acid esters. Background Art

[0002] The most widely used method for producing organic acid esters is the esterification reaction between alcohols and carboxylic acids. However, since the esterification reaction is a reversible and extremely slow process, the conversion rate is limited. Traditional processes promote the esterification reaction by heating and accelerating stirring, but the water generated during the reaction inhibits the reaction from proceeding in the forward direction.

[0003] Chinese patent ZL201310584448.8 discloses an esterification reaction device, which uses a tubular molecular sieve membrane as a reaction container and is provided with a heating device inside the tubular molecular sieve membrane. The tubular molecular sieve membrane is filled with a fixed bed catalyst. When the reaction raw materials flow through the tubular molecular sieve membrane, they will react with the assistance of the catalyst. During the reaction, a negative pressure state is formed outside the tubular molecular sieve membrane, and the water generated by the reaction will permeate the tubular molecular sieve membrane and be extracted.

[0004] Although the above-mentioned device solves the problem of water generated by the separation reaction inhibiting the reaction, it still has some shortcomings. First, the tubular molecular sieve membrane has a slender structure, and the catalyst inside is not convenient to replace. Second, the tubular molecular sieve membrane requires an additional heating device, which is located inside and is not easy to maintain. Summary of the Invention

[0005] In order to overcome the shortcomings of existing continuous dehydration esterification reaction devices, such as the inability to replace catalysts in a timely manner and the lack of a heating method that is not conducive to maintenance, the present invention provides a reaction device for continuously synthesizing high-boiling-point carboxylic acid esters.

[0006] The technical solution is: a reaction device for continuously synthesizing high-boiling-point carboxylic acid esters, comprising a main shell, a connecting square tube, a silica gel treatment device, a catalyst mixing device, a catalyst treatment device, a vacuum pump and a condensation absorption device; a connecting square tube is fixedly connected to the lower side of the main shell; the connecting square tube is connected to the silica gel treatment device; the lower side of the main shell is connected to the catalyst mixing device; a catalyst treatment device is installed on the upper surface of the catalyst mixing device; a vacuum pump is installed on the upper surface of the catalyst treatment device; the vacuum pump is connected to the condensation absorption device; a through hole is opened on the upper side of the main shell; it also includes a hollow cylindrical member, a molecular sieve tube and a silica gel delivery pipe; a hollow cylindrical member is fixedly connected to the upper and lower sides of the main shell respectively, and the hollow cylindrical member is provided with an inspection door; the two hollow cylindrical members are commonly connected to the molecular sieve tube, and a plurality of protrusions are provided on the inner wall of the molecular sieve tube; the upper hollow cylindrical member is connected to the silica gel delivery pipe, and the other end of the silica gel delivery pipe is connected to the silica gel treatment device.

[0007] Furthermore, it also includes a hollow rotating part, an air supply short tube, an air supply moving ring, a push rod, an air pump and a clean rubber tube; the two hollow cylindrical parts are slidingly connected to the hollow rotating parts on the opposite sides of each other, and are connected to a hollow rotating part directly above and directly below the same molecular sieve tube; each hollow rotating part is connected to an air supply short tube on the side away from the main shell; all the air supply short tubes on the upper side are commonly provided with an air supply moving ring, and all the air supply short tubes on the lower side are commonly connected to another air supply moving ring, and the interiors of the two air supply moving rings are hollow, and each air supply short tube is connected to the corresponding air supply moving ring; two circumferentially distributed push rods are installed on the side of each hollow cylindrical part away from the main shell, and the telescopic parts of the two push rods are commonly fixedly connected to the air supply moving ring; each air supply moving ring is connected to an air pump; the hollow rotating part directly above and the hollow rotating part directly below the same molecular sieve tube are commonly connected to two clean rubber tubes.

[0008] Furthermore, it also includes a mask; the hollow rotating part has an inclined jet hole, which is used to guide the jet to drive the hollow rotating part to rotate; each hollow rotating part is slidably connected to a mask, all the masks located above are fixedly connected to the silicone delivery pipe; all the masks located below are fixedly connected to the hollow cylindrical part.

[0009] Furthermore, it also includes a plate agglomeration filter screen; the plate agglomeration filter screen is fixedly connected to the inner wall of the hollow cylindrical member below.

[0010] Furthermore, a cleaning brush portion is provided on the outer wall of the cleaning rubber tube, and the cleaning brush portion is located on the side of the outer wall of the cleaning rubber tube close to the molecular sieve tube.

[0011] Furthermore, it also includes a support steel bar; the inner wall of the cleaning rubber tube is fixedly connected to a position near the molecular sieve tube with a support steel bar, and the support steel bar is used to prevent excessive deformation of the cleaning rubber tube when it rotates.

[0012] Furthermore, it also includes an electromagnet; the inner wall of the cleaning rubber tube is connected with the electromagnet.

[0013] Furthermore, it also includes a catalyst movement system; the catalyst movement system includes a separation cover, a separation screen and a spiral guide net; the separation cover is fixedly connected to the upper end of the main shell; the separation screen is fixedly connected to the lower side of the inner wall of the separation cover, and the separation screen is higher on the left and lower on the right; the spiral guide net is fixedly connected to the inner wall of the main shell.

[0014] Furthermore, the catalyst moving system also includes an arc plate and a separation net; each molecular sieve tube is connected to two arc plates; a separation net is connected between the arc plates connecting the opposite surfaces of each two adjacent molecular sieve tubes, and all the separation nets form a cylindrical shape.

[0015] Furthermore, the spiral guide mesh is made of a metal material with good thermal conductivity.

[0016] The beneficial effects are as follows: the reaction device for continuously synthesizing high-boiling-point carboxylic acid esters of the present invention realizes the functions of timely separation of unsuitable catalysts, separation of water in reaction products and heating of the reaction container through a rationally designed structure.

[0017] Start the vacuum pump to extract the gas inside the molecular sieve tube. Under the action of the pressure difference, water passes through the molecular sieve tube and is extracted in the form of gas. This part of the gaseous water encounters silica gel particles in the molecular sieve tube and is partially absorbed. It then rises to the inside of the hollow cylindrical part above and then enters the condensation absorption device to condense and absorb the remaining water. The dry air enters the vacuum pump.

[0018] Start the push rod, move the upper air supply moving ring and the lower air supply moving ring downward, start the upper air pump and the lower air pump, inject air into the air supply moving ring, and the air in the air supply moving ring enters the hollow rotating part through the air supply short tube, and then enters the two clean rubber tubes connected to it. If the molecular sieve tube where the two clean rubber tubes are located is blocked, the silica gel particles below the blockage point will flow away to free up some space, and the two clean rubber tubes will expand to occupy the space, while the space above the blockage point will be filled with immovable silica gel particles. These particles will limit the expansion of the clean rubber tubes, start the push rod, move the air supply moving ring upward, and the air supply moving ring drives The hollow rotating part and the air supply short tube move upward, eventually driving the clean rubber tube to move upward. The expanded part of the clean rubber tube pushes the agglomerated silica gel particles at the blockage point upward, causing the agglomerated silica gel particles to move upward, so that the agglomerated silica gel particles no longer stick to the inner wall of the molecular sieve tube. Then the agglomerated silica gel particles move upward and encounter the protrusion, are squeezed and redispersed into small particles, and then the gas inside the clean rubber tube is released through the air pump, and the clean rubber tube returns to its original shape. The above-mentioned broken silica gel particles will begin to fall because their diameter is smaller than the inner diameter of the molecular sieve tube, and the silica gel particles that were originally blocked will continue to fall, and the interior of the above-mentioned molecular sieve tube will be unblocked again.

[0019] Start the push rod and lower the air supply moving ring to the lowest point. At this time, the mask no longer blocks the inclined air jet hole. Start the air pump to send air into the hollow rotating part. Part of the air is ejected from the inclined air jet hole, pushing the hollow rotating part to rotate. The rotating hollow rotating part drives the cleaning rubber tube to rotate. The cleaning brush on the cleaning rubber tube rubs the inner wall of the molecular sieve tube to scrape off possible stains.

[0020] In order to avoid excessive deformation of the cleaning rubber tube when the cleaning rubber tube rotates, a supporting steel bar is provided to resist the force perpendicular to the cleaning rubber tube.

[0021] Since the molecular sieve tube passes through the spiral guide net, the catalyst may be blocked by the molecular sieve tube and stop when rotating, causing blockage near the molecular sieve tube. Therefore, an arc plate and a separator net are designed. The separator net guides the catalyst to move in a circle. When the catalyst approaches the molecular sieve tube, it is guided by the arc plate to slide away from the outer surface of the molecular sieve tube, avoiding the accumulation of the catalyst. BRIEF DESCRIPTION OF THE DRAWINGS

[0022] Figure 1 This is a schematic structural diagram of a reaction device for continuously synthesizing high-boiling-point carboxylic acid esters disclosed in the present invention;

[0023] Figure 2 A cross-sectional view of a reaction apparatus for continuously synthesizing high-boiling-point carboxylic acid esters according to the present invention;

[0024] Figure 3 A partial cross-sectional view of a first embodiment of the reaction apparatus for continuously synthesizing high-boiling-point carboxylic acid esters disclosed in the present invention;

[0025] Figure 4 An exploded view of a reaction apparatus for continuously synthesizing high-boiling-point carboxylic acid esters disclosed herein;

[0026] Figure 5 A second partial cross-sectional view of the reaction apparatus for continuously synthesizing high-boiling-point carboxylic acid esters disclosed in the present invention;

[0027] Figure 6 This is a schematic structural diagram of the molecular sieve tube, hollow rotating member and clean rubber tube disclosed in the reaction device for continuous synthesis of high-boiling-point carboxylic acid esters of the present invention;

[0028] Figure 7 This is a schematic structural diagram of a cleaning rubber tube, a supporting steel bar, and an electromagnet disclosed in the reaction device for continuously synthesizing high-boiling-point carboxylic acid esters of the present invention;

[0029] Figure 8 This is a schematic structural diagram of the molecular sieve tube, curved plate, and separator net disclosed in the reaction device for continuous synthesis of high-boiling-point carboxylic acid esters of the present invention;

[0030] Figure 9 A diagram showing the state of catalyst particles moving along a spiral guide net as disclosed in the reaction device for continuously synthesizing high-boiling-point carboxylic acid esters of the present invention;

[0031] Figure 10 The present invention is a partial structural schematic diagram of a main body shell and a separation cover shell disclosed in a reaction device for continuously synthesizing high-boiling-point carboxylic acid esters.

[0032] Names and serial numbers of parts in the figure: 1-main body shell, 2-connecting square tube, 3-silica gel processing device, 4-catalyst mixing device, 5-catalyst processing device, 6-vacuum pump, 7-condensation absorption device, 101-hollow cylindrical part, 102-molecular sieve tube, 103-silica gel delivery pipe, 111-hollow rotating part, 112-air supply short pipe, 113-air supply moving ring, 114-push rod, 115-air pump, 116-mask, 117-plate agglomeration filter, 121-cleaning rubber tube, 122-support steel bar, 123-electromagnet, 201-separation cover, 202-separation screen, 203-arc plate, 204-separation net, 205-spiral guide net, 1a-through hole, 102a-protrusion, 111a-inclined air jet hole, 121a-cleaning brush part, 500-catalyst particles. DETAILED DESCRIPTION

[0033] The technical solution of the present invention will be further described below with reference to the accompanying drawings.

[0034] Example 1

[0035] A reaction device for continuously synthesizing high-boiling-point carboxylic acid esters, such as Figure 1-10 As shown, it includes a main body shell 1, a connecting square tube 2, a silica gel treatment device 3, a catalyst mixing device 4, a catalyst treatment device 5, a vacuum pump 6 and a condensation absorption device 7; a connecting square tube 2 is welded to the lower side of the main body shell 1; the connecting square tube 2 is connected to the silica gel treatment device 3, the silica gel treatment device 3 is equipped with a pump for lifting the particles flowing into it from the connecting square tube 2, and the silica gel treatment device 3 is equipped with an electric heating wire for heating the above particles; the lower side of the main body shell 1 is connected to the catalyst mixing device 4; the catalyst treatment device 5 is installed on the upper surface of the catalyst mixing device 4; the vacuum pump 6 is installed on the upper surface of the catalyst treatment device 5; the vacuum pump 6 is connected to the condensation absorption device 7; the upper side of the main body shell 1 is opened with a through hole 1a, as shown Figure 10 As shown;

[0036] It also includes a hollow cylindrical member 101, a molecular sieve tube 102 and a silica gel delivery tube 103; a hollow cylindrical member 101 is welded to the upper and lower sides of the main shell 1 respectively, and the hollow cylindrical member 101 is provided with an inspection door; the two hollow cylindrical members 101 are connected to 8 molecular sieve tubes 102, and the inner wall of the molecular sieve tube 102 is provided with a plurality of protrusions 102a; the upper hollow cylindrical member 101 is connected to the silica gel delivery tube 103, and the other end of the silica gel delivery tube 103 is connected to the silica gel processing device 3.

[0037] It also includes a hollow rotating part 111, an air supply short tube 112, an air supply moving ring 113, a push rod 114, an air pump 115 and a cleaning rubber tube 121; the two hollow cylindrical parts 101 are slidably connected to 8 hollow rotating parts 111 on the opposite sides, and the same molecular sieve tube 102 is connected to a hollow rotating part 111 directly above and directly below; each hollow rotating part 111 is connected to an air supply short tube 112 on the side away from the main body shell 1; all the air supply short tubes 112 on the upper side are commonly provided with an air supply moving ring 113, and all the air supply short tubes 112 on the lower side are commonly connected to the air supply moving ring 113. Another air supply moving ring 113 is provided, and the interiors of the two air supply moving rings 113 are hollow, and each air supply short tube 112 is connected to the corresponding air supply moving ring 113; two circumferentially distributed push rods 114 are installed on the side of each hollow cylindrical member 101 facing away from the main shell 1, and the telescopic parts of the two push rods 114 are bolted together with the air supply moving ring 113; each air supply moving ring 113 is connected to an air pump 115; the hollow rotating member 111 directly above and the hollow rotating member 111 directly below the same molecular sieve tube 102 are connected together with two clean rubber tubes 121.

[0038] Before the present invention is put into operation, a valve that can be opened and closed is installed on the through hole 1a on the upper side of the main shell 1 and kept closed in advance. First, check whether all parts are intact to ensure that the device can be started normally.

[0039] Silica gel particles are fed into the silica gel processing device 3, which heats and lifts the silica gel particles. The silica gel particles are sent out from the silica gel delivery tube 103 and enter the interior of the hollow cylindrical member 101 above, and then fall into the molecular sieve tube 102 connected to the above-mentioned hollow cylindrical member 101. The hot silica gel particles fall inside the molecular sieve tube 102 and heat the molecular sieve tube 102 at the same time. Thereafter, the silica gel particles fall into the interior of the hollow cylindrical member 101 below and flow back to the silica gel processing device 3 from the connecting square tube 2. The silica gel particles are heated by the silica gel processing device 3, and the moisture in the silica gel particles is also evaporated. The silica gel particles circulate in this way, continuously heating the molecular sieve tube 102.

[0040] When the temperature inside the main shell 1 is close to the temperature for the reaction, the catalyst is fed into the catalyst processing device 5, and the raw materials waiting for reaction are injected into the catalyst mixing device 4. The catalyst processing device 5 simultaneously feeds the catalyst into the catalyst mixing device 4 to mix with the raw materials. Then the raw materials mixed with the catalyst are fed into the lower side of the main shell 1. The raw materials and catalyst react inside the main shell 1. The raw materials and catalysts that enter later continuously push the raw materials and catalysts that enter earlier upward, and the raw materials that enter earlier are also continuously reacted into products. The above substances continue to move upward until they approach the top surface inside the main shell 1.

[0041] The valve installed in the through hole 1a on the upper side of the main shell 1 is opened, and the reaction product and catalyst finally flow out to the outside from the through hole 1a of the main shell 1. Thereafter, the reaction product and the catalyst are manually separated, and the reaction product and the catalyst flow out together, so that the operator can replace the catalyst at any time according to the condition of the catalyst.

[0042] During this process, water is continuously generated. The vacuum pump 6 is started to extract the gas inside the molecular sieve tube 102. Under the action of the pressure difference, the water passes through the molecular sieve tube 102 and is extracted in the form of gas. This part of the gaseous water encounters silica gel particles in the molecular sieve tube 102 and is partially absorbed. It then rises to the inside of the hollow cylindrical member 101 above and then enters the condensation absorption device 7 to condense and absorb the remaining water. The dry air enters the vacuum pump 6.

[0043] After long-term use, the silica gel particles may clump together, so there is a risk of accumulation and clogging in the molecular sieve tube 102. Therefore, it is necessary to regularly clear the molecular sieve tube 102, start the push rod 114, move the upper air supply moving ring 113 and the lower air supply moving ring 113 downward, start the upper air pump 115 and the lower air pump 115, and inject air into the air supply moving ring 113. The air in the air supply moving ring 113 enters the hollow rotating part 111 through the air supply short tube 112, and then enters the two clean rubber tubes 121 connected thereto. If the molecular sieve tube 102 where the two clean rubber tubes 121 are located is blocked, the silica gel particles below the blockage point will flow away to free up some space, and the two clean rubber tubes 121 will expand to occupy this space, while the space above the blockage point will be filled with immovable silica gel particles. These particles will restrict the clean rubber tubes 121. The tube 121 expands, starts the push rod 114, and moves the air supply moving ring 113 upward. The air supply moving ring 113 drives the hollow rotating part 111 and the air supply short tube 112 to move upward, and finally drives the clean rubber tube 121 to move upward. The expanded part of the clean rubber tube 121 pushes the agglomerated silica gel particles at the blockage point upward, so that the agglomerated silica gel particles move upward, and the agglomerated silica gel particles no longer stick to the inner wall of the molecular sieve tube 102. Then the agglomerated silica gel particles move upward and encounter the protrusion 102a, and are squeezed and dispersed into small particles. After that, the gas inside the clean rubber tube 121 is released through the air pump 115, and the clean rubber tube 121 returns to its original state. The above-mentioned crushed silica gel particles will begin to fall because their diameter is smaller than the inner diameter of the molecular sieve tube 102. The silica gel particles that were originally blocked also continue to fall, and the interior of the above-mentioned molecular sieve tube 102 is unblocked again.

[0044] Example 2

[0045] As a further improvement of Example 1, Figure 2-7As shown, a mask 116 is also included; the hollow rotating member 111 is provided with an inclined jet hole 111a, which is used to guide the jet to push the hollow rotating member 111 to rotate; each hollow rotating member 111 is slidably connected to a mask 116, and all the masks 116 located above are fixedly connected to the silicone delivery tube 103; all the masks 116 located below are fixedly connected to the hollow cylindrical member 101.

[0046] It also includes a plate agglomeration filter screen 117; the plate agglomeration filter screen 117 is welded to the inner wall of the hollow cylindrical member 101 below.

[0047] A cleaning brush portion 121 a is provided on the outer wall of the cleaning rubber tube 121 , and the cleaning brush portion 121 a is located on the outer wall of the cleaning rubber tube 121 close to the molecular sieve tube 102 .

[0048] It also includes a support steel bar 122; the inner wall of the cleaning rubber tube 121 is fixedly connected to the support steel bar 122 near the molecular sieve tube 102, and the support steel bar 122 is used to prevent excessive deformation of the cleaning rubber tube 121 when it rotates.

[0049] The cleaning rubber tube 121 further includes an electromagnet 123 ; the inner wall of the cleaning rubber tube 121 is connected to the electromagnet 123 .

[0050] Since the silica gel particles need to circulate continuously, they inevitably bring in some stains. These stains will stick to the inner wall of the molecular sieve tube 102 and affect the delivery of water. Therefore, the inner wall of the molecular sieve tube 102 needs to be cleaned regularly.

[0051] Start the push rod 114 and lower the air supply moving ring 113 to the lowest point. At this time, the mask 116 no longer blocks the inclined air jet hole 111a. Start the air pump 115 to send air into the hollow rotating part 111. Part of the air is ejected from the inclined air jet hole 111a, pushing the hollow rotating part 111 to rotate. The rotating hollow rotating part 111 drives the cleaning rubber tube 121 to rotate. The cleaning brush part 121a on the cleaning rubber tube 121 rubs the inner wall of the molecular sieve tube 102 to scrape off possible stains.

[0052] In order to prevent the cleaning rubber tube 121 from being excessively deformed when the cleaning rubber tube 121 rotates, a supporting steel bar 122 is provided to resist a force perpendicular to the cleaning rubber tube 121 .

[0053] When dealing with blockage, the expanded part of the cleaning rubber tube 121 provides an upward force to the clogged compacted silicone particles. If the compacted silicone particles are clogged tightly, when the cleaning rubber tube 121 is lifted upward, due to the obstruction of the compacted silicone particles, the cleaning rubber tube 121 may bypass the compacted silicone particles and slide upward, resulting in the inability to move the compacted silicone particles. Therefore, an electromagnet 123 is added, and the electromagnet 123 is started when the two cleaning rubber tubes 121 expand. After the expanded parts of the cleaning rubber tubes 121 come into contact with each other, the electromagnet 123 presses the expanded parts of the two cleaning rubber tubes 121 together. When the cleaning rubber tube 121 is moved upward in this way, since the electromagnet 123 presses the expanded parts of the two cleaning rubber tubes 121, the cleaning rubber tube 121 will be blocked by the two electromagnets 123 when it slides, resulting in the inability to slide. It can only work together to move the compacted silicone particles at the blockage upward.

[0054] After the compacted silica gel particles are broken, smaller silica gel agglomerates are formed. Although they can fall smoothly, there is still a risk of blockage if these small particle agglomerates continue to circulate. Therefore, agglomerate filter 117 is set. After these agglomerates fall and leave the lower end of the molecular sieve tube 102, they are intercepted by the agglomerate filter 117 to avoid further circulation of these agglomerates. The intercepted agglomerates can be taken out from the inspection door of the hollow cylindrical part 101 during maintenance.

[0055] Example 3

[0056] As a further improvement of Example 2, Figure 2-4 、 Figure 8-9 As shown, it also includes a catalyst movement system; the catalyst movement system includes a separation cover 201, a separation screen 202 and a spiral guide net 205; the separation cover 201 is welded to the upper end of the main shell 1; the separation screen 202 is welded to the lower side of the inner wall of the separation cover 201, and the separation screen 202 is higher on the left and lower on the right; the spiral guide net 205 is welded to the inner wall of the main shell 1.

[0057] The catalyst moving system also includes an arc plate 203 and a separator 204; each molecular sieve tube 102 is connected to two arc plates 203; a separator 204 is connected between the arc plates 203 connecting the opposite surfaces of each two adjacent molecular sieve tubes 102, and all the separators 204 form a cylindrical shape.

[0058] The spiral guide net 205 is made of a metal material with good thermal conductivity.

[0059] When the raw materials react in the main shell 1, there are still some minor problems. First, the device is heat-transferred by the molecular sieve tube 102, but too much distribution of the molecular sieve tube 102 will affect the flow of the catalyst and the reactants, and too little distribution will result in uneven heating. In order to better transfer heat, the temperature of the molecular sieve tube 102 will be slightly higher than the reaction temperature, which may make the temperature of the outer surface of the molecular sieve tube 102 higher than the boiling point of the alcohol participating in the reaction, resulting in the local generation of alcohol vapor on the outer surface of the molecular sieve tube 102, and small bubbles will be coated on the outer surface of the molecular sieve tube 102, which will make the alcohol separate from the outer surface of the molecular sieve tube 102. The reaction results in insufficient reactants, affecting the reaction. On the other hand, the coated small bubbles have low thermal conductivity, affecting heat transfer. For the above two considerations, a spiral guide net 205 is designed. When the catalyst and reactants rise, the catalyst is guided by the spiral guide net 205 and rotates. The rotating catalyst drives the liquid reactants to rotate. When the catalyst rotates, it will scratch the outer surface of the molecular sieve tube 102, taking away some small bubbles. The rotating reactants allow the reactants at the same height to be evenly mixed, and at the same time, it will also take away the small bubbles and redistribute them in the reactants.

[0060] Since the molecular sieve tube 102 passes through the spiral guide net 205, the catalyst may be blocked by the molecular sieve tube 102 and stop when rotating, resulting in blockage near the molecular sieve tube 102. Therefore, the arc plate 203 and the separation net 204 are designed. The separation net 204 guides the catalyst to move in a circle. When the catalyst approaches the molecular sieve tube 102, it is guided by the arc plate 203 to slide away from the outer surface of the molecular sieve tube 102, thereby avoiding the accumulation of the catalyst.

[0061] At the same time, in order to automatically separate the catalyst and the reaction product, a separation cover 201 and a separation screen 202 are set. The reaction product and the catalyst flow into the separation cover 201 from the through hole 1a on the upper side of the main shell 1. The catalyst is screened by the separation screen 202 which is higher on the left and lower on the right, and is sent to the catalyst treatment device 5 under the action of gravity. After treatment, it is continued to be recycled. When the catalyst can no longer be used, the expired catalyst is taken out from the catalyst treatment device 5 and a new catalyst is added. The reaction product that has passed through the separation screen 202 flows out from the left side of the separation cover 201.

[0062] The technical principles of the embodiments of the present invention have been described above in conjunction with specific embodiments. These descriptions are intended solely to explain the principles of the embodiments of the present invention and should not be construed in any way as limiting the scope of protection of the embodiments of the present invention. Based on the explanations herein, those skilled in the art will be able to conceive of other specific implementations of the embodiments of the present invention without inventive effort, and such implementations will fall within the scope of protection of the embodiments of the present invention.

Claims

1. A reaction device for continuously synthesizing high-boiling-point carboxylic acid esters, comprising a main body shell (1), a connecting square tube (2), a silica gel treatment device (3), a catalyst mixing device (4), a catalyst treatment device (5), a vacuum pump (6) and a condensation absorption device (7); the connecting square tube (2) is fixedly connected to the lower side of the main body shell (1); the connecting square tube (2) is connected to the silica gel treatment device (3); the lower side of the main body shell (1) is connected to the catalyst mixing device (4); the catalyst treatment device (5) is installed on the upper surface of the catalyst mixing device (4); the vacuum pump (6) is installed on the upper surface of the catalyst treatment device (5); the vacuum pump (6) is connected to the condensation absorption device (7); a through hole (1a) is opened on the upper side of the main body shell (1); characterized in that: It also includes a hollow cylindrical member (101), a molecular sieve tube (102) and a silica gel delivery tube (103); the upper side and the lower side of the main body shell (1) are respectively fixedly connected to a hollow cylindrical member (101), and the hollow cylindrical member (101) is provided with an inspection door; the two hollow cylindrical members (101) are commonly connected to the molecular sieve tube (102), and the inner wall of the molecular sieve tube (102) is provided with a plurality of protrusions (102a); the upper hollow cylindrical member (101) is connected to the silica gel delivery tube (103), and the other end of the silica gel delivery tube (103) is connected to the silica gel processing device (3); The invention also comprises a hollow rotating member (111), an air supply short tube (112), an air supply moving ring (113), a push rod (114), an air pump (115) and a cleaning rubber tube (121); the two hollow cylindrical members (101) are slidably connected to the hollow rotating member (111) on opposite sides, and the upper and lower sides of the same molecular sieve tube (102) are respectively connected to a hollow rotating member (111); the side of each hollow rotating member (111) facing away from the main body shell (1) is connected to the air supply short tube (112); all the air supply short tubes (112) on the upper side are commonly provided with an air supply moving ring (113), and all the air supply short tubes (112) on the lower side are commonly connected to the air supply moving ring (113). Another air supply moving ring (113) is provided, and the interiors of the two air supply moving rings (113) are hollow, and each air supply short tube (112) is connected to the corresponding air supply moving ring (113); two circumferentially distributed push rods (114) are installed on the side of each hollow cylindrical member (101) facing away from the main body shell (1), and the telescopic parts of the two push rods (114) are fixedly connected to the air supply moving ring (113); each air supply moving ring (113) is connected to an air pump (115); the hollow rotating member (111) directly above and the hollow rotating member (111) directly below the same molecular sieve tube (102) are connected to two clean rubber tubes (121).

2. The reaction device for continuously synthesizing high-boiling-point carboxylic acid esters according to claim 1, characterized in that: The invention also includes a mask (116); the hollow rotating member (111) is provided with an inclined air jet hole (111a), and the inclined air jet hole (111a) is used to guide the air jet to push the hollow rotating member (111) to rotate; each hollow rotating member (111) is slidably connected to a mask (116), and all the masks (116) located above are fixedly connected to the silicone delivery tube (103); and all the masks (116) located below are fixedly connected to the hollow cylindrical member (101).

3. The reaction device for continuously synthesizing high-boiling-point carboxylic acid esters according to claim 1, characterized in that: It also includes a plate agglomeration filter screen (117); the inner wall of the lower hollow cylindrical member (101) is fixedly connected with the plate agglomeration filter screen (117).

4. The reaction device for continuously synthesizing high-boiling-point carboxylic acid esters according to claim 1, characterized in that: The outer wall of the cleaning rubber tube (121) is provided with a cleaning brush portion (121a), and the cleaning brush portion (121a) is located on the side of the outer wall of the cleaning rubber tube (121) close to the molecular sieve tube (102).

5. The reaction device for continuously synthesizing high-boiling-point carboxylic acid esters according to claim 4, characterized in that: The cleaning rubber tube (121) further comprises a supporting steel bar (122); the supporting steel bar (122) is fixedly connected to the inner wall of the cleaning rubber tube (121) near the molecular sieve tube (102); the supporting steel bar (122) is used to prevent the cleaning rubber tube (121) from excessive deformation when rotating.

6. The reaction device for continuously synthesizing high-boiling-point carboxylic acid esters according to claim 5, characterized in that: The cleaning rubber tube (121) further comprises an electromagnet (123); the inner wall of the cleaning rubber tube (121) is connected with the electromagnet (123).

7. A reaction device for continuously synthesizing high-boiling-point carboxylic acid esters according to any one of claims 1 to 6, characterized in that: The invention also includes a catalyst moving system; the catalyst moving system includes a separation cover (201), a separation screen (202) and a spiral guide net (205); the upper end of the main shell (1) is fixedly connected to the separation cover (201); the lower side of the inner wall of the separation cover (201) is fixedly connected to the separation screen (202), and the separation screen (202) is higher on the left and lower on the right; and the inner wall of the main shell (1) is fixedly connected to the spiral guide net (205).

8. The reaction device for continuously synthesizing high-boiling-point carboxylic acid esters according to claim 7, characterized in that: The catalyst moving system also includes an arc plate (203) and a separation net (204); each molecular sieve tube (102) is connected to two arc plates (203); a separation net (204) is connected between the arc plates (203) connected to the opposite surfaces of each two adjacent molecular sieve tubes (102), and all the separation nets (204) form a cylindrical shape.

9. The reaction device for continuously synthesizing high-boiling-point carboxylic acid esters according to claim 7, characterized in that: The spiral guide net (205) is made of a metal material with good thermal conductivity.

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