A falling film device for reaction solution of a dicyclopentadiene acrylate preparation system

Abstract

The application discloses a kind of dicyclopentadiene allyl ester preparation system's reaction liquid falling film device, including buffer tank, first pipe body, first water pump, second pipe body, first falling film evaporator, third pipe body, receiving tank, fourth pipe body, first deep cooler, fifth pipe body, recovery solvent tank, sixth pipe body, second water pump, seventh pipe body, second falling film evaporator, eighth pipe body, heavy component tank, ninth pipe body, second deep cooler and product tank.Through the above mode, the reaction liquid is treated by multiple falling film by multiple falling film evaporators, which can realize relatively high quality product separation and purification, so that the yield of product can be improved by 15%, and the color number and purity of the product are further improved.

Description

Technical Field

[0001] This invention relates to the field of dicyclopentadiene acrylate preparation technology, specifically to a reaction liquid falling film device for a dicyclopentadiene acrylate preparation system. Background Technology

[0002] Dicyclopentenyl acrylate (DCPA) is a colorless or pale yellow transparent liquid with the molecular formula: C 13 H 16 O2, CAS number 33791-58-1, is a monomer with excellent properties and broad application prospects. Its structure incorporates a large dicyclopentadiene group, resulting in a high glass transition temperature (Tg) for its homopolymer. It exhibits good performance in terms of hardness, water resistance, and transparency, and can be widely used in coatings, adhesives, plastic surfaces, and optical materials requiring insulation and high hardness. It is an ideal reactive diluent for photocurable materials.

[0003] Currently, the existing methods for synthesizing DCPA mainly involve slowly adding dicyclopentadiene dropwise to an acrylic acid solution containing a strong acid catalyst to undergo an electrophilic addition reaction to obtain a crude reaction solution, which is then post-treated or vacuum distilled to obtain the product dicyclopentenyl acrylate.

[0004] However, dicyclopentenyl acrylate is an ester compound containing acrylic acid double bonds. The production process is prone to polymerization, resulting in low yield, difficulty in cleaning, and even safety risks of explosive polymerization. Therefore, the reaction solution needs to be treated. In the traditional way, most conventional operation methods are to introduce high-temperature steam to inhibit polymerization by evaporation and perform flash evaporation. However, this operation results in low product distillation yield and poor purification effect. Summary of the Invention

[0005] (a) Technical problems to be solved

[0006] To address the shortcomings of existing technologies, this invention provides a reaction liquid falling film device for a dicyclopentadiene acrylate preparation system, which can solve the aforementioned technical problems.

[0007] (II) Technical Solution

[0008] To solve the above-mentioned technical problems, the present invention provides the following technical solution: a falling film device for the reaction liquid of a dicyclopentadiene acrylate preparation system, characterized in that it comprises: a buffer tank for receiving the reaction liquid for preparing dicyclopentadiene acrylate; a first tube, one end of which is connected to the output port of the buffer tank; a first water pump, the input port of which is connected to the other end of the first tube; a second tube, one end of which is connected to the output port of the first water pump; a first falling film evaporator, the top input port of which is connected to the other end of the second tube; a third tube, one end of which is connected to the bottom output port of the first falling film evaporator; a receiving tank, the input port of which is connected to the other end of the third tube; a fourth tube, one end of which is connected to the top output port of the receiving tank; a first deep cooler, the input port of which is connected to the other end of the fourth tube; and a fifth tube. One end of the tube is connected to the output port of the first cryogenic reactor; the top inlet of the solvent recovery tank is connected to the other end of the fifth tube; one end of the sixth tube is connected to the bottom output port of the receiving tank; the second water pump is connected to the other end of the sixth tube; one end of the seventh tube is connected to the output port of the second water pump; the top inlet of the second falling film evaporator is connected to the other end of the seventh tube; one end of the eighth tube is connected to the bottom output port of the second falling film evaporator; the side wall inlet of the heavy component tank is connected to the other end of the eighth tube; one end of the ninth tube is connected to the top output port of the heavy component tank; the second cryogenic reactor is connected to the other end of the ninth tube; and the top inlet of the product tank is connected to the output port of the second cryogenic reactor via the tenth tube.

[0009] Furthermore, the sixth pipe is provided with a first switching valve for controlling the opening and closing of the sixth pipe, and the sixth pipe is also provided with a first check valve for directing the solution in the receiving tank to the second water pump.

[0010] Furthermore, it also includes: a delivery pipe, one end of which is connected to the bottom outlet of the reactor, and the other end is connected to the inlet of the buffer tank via a third water pump, so as to pump the reaction liquid in the reactor to the buffer tank via the third water pump.

[0011] Furthermore, the delivery pipe is provided with a second switching valve for controlling the opening and closing of the delivery pipe, and the delivery pipe is also provided with a second one-way valve for allowing the solution in the reaction vessel to flow to the buffer tank.

[0012] Furthermore, it also includes: a circulation pipe, one end of which is connected to the output port at the bottom of the recovery solvent tank, and the other end is connected to the reaction vessel via a fourth water pump, so as to pump the solution in the recovery solvent tank back to the reaction vessel via the fourth water pump.

[0013] Furthermore, the circulation pipe is provided with a third switching valve for controlling the opening and closing of the circulation pipe, and the circulation pipe is also provided with a third one-way valve for allowing the solution in the recovery solvent tank to flow into the reaction vessel.

[0014] Furthermore, it also includes: a first steam pipe, one end of which is connected to the steam outlet of the first falling film evaporator, and the other end of which is connected to the first steam inlet on the side wall of the receiving tank; a first heat exchanger, which is planar and inclinedly disposed within the receiving tank, wherein the inlet of the first heat exchanger is connected to the first steam pipe; a first discharge pipe, one end of which is connected to the first steam outlet at the bottom of the receiving tank, wherein the outlet of the first heat exchanger is connected to one end of the first discharge pipe; a second steam pipe, one end of which is connected to the steam outlet of the second falling film evaporator, and the other end of which is connected to the second steam inlet on the side wall of the receiving tank; a second heat exchanger, which is planar and inclinedly disposed within the receiving tank, wherein the inlet of the second heat exchanger is connected to the second steam pipe; a second discharge pipe, one end of which is connected to the second steam outlet at the bottom of the receiving tank, wherein the outlet of the second heat exchanger is connected to one end of the second discharge pipe; wherein the first heat exchanger and the second heat exchanger are arranged intersectingly within the receiving tank.

[0015] Furthermore, the receiving tank is also provided with a uniformly dispersing disk that communicates with the other end of the third tube, wherein the first heat exchanger and the second heat exchanger are both located below the uniformly dispersing disk.

[0016] Furthermore, the first heat exchanger is formed by bending a first copper tube, one end of which passes through the uniformly dispersed disk and is connected to the first steam pipe, and the other end of which is connected to the first discharge pipe. The second heat exchanger is formed by bending a second copper tube, one end of which passes through the uniformly dispersed disk and is connected to the second steam pipe, and the other end of which is connected to the second discharge pipe.

[0017] (III) Beneficial Effects

[0018] Compared with existing technologies, this invention provides a falling film device for the reaction liquid in a dicyclopentadiene acrylate preparation system, which has the following beneficial effects: The falling film device for the reaction liquid in the dicyclopentadiene acrylate preparation system disclosed in this invention includes a buffer tank, a first tube, a first water pump, a second tube, a first falling film evaporator, a third tube, a receiving tank, a fourth tube, a first deep cooler, a fifth tube, a solvent recovery tank, a sixth tube, a second water pump, a seventh tube, a second falling film evaporator, an eighth tube, a heavy component tank, a ninth tube, a second deep cooler, and a product tank. Through the above method, this invention performs a first falling film treatment on the reaction liquid using multiple first falling film evaporators, and then a second falling film treatment on the reaction liquid using a second falling film evaporator, enabling higher quality product separation and purification, increasing the product yield by 15%, and further improving the product's color and purity. Attached Figure Description

[0019] Figure 1 This is a schematic diagram of the falling film device for the reaction liquid in the dicyclopentadiene acrylate preparation system of the present invention;

[0020] Figure 2 for Figure 1 A partial structural schematic diagram of another embodiment of the falling film device for the intermediate reaction liquid;

[0021] Figure 3 for Figure 2 A schematic diagram of the internal structure of the recycling tank. Detailed Implementation

[0022] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0023] like Figure 1 As shown, the falling film device for the reaction liquid of the dicyclopentadiene acrylate preparation system disclosed in this invention includes a buffer tank 10, a first tube 101, a first water pump 11, a second tube 102, a first falling film evaporator 12, a third tube 121, a receiving tank 13, a fourth tube 131, a first deep cooler 14, a fifth tube 141, a solvent recovery tank 15, a sixth tube 132, a second water pump 16, a seventh tube 133, a second falling film evaporator 17, an eighth tube 171, a heavy component tank 18, a ninth tube 181, a second deep cooler 19, and a product tank 20.

[0024] Buffer tank 10 is used to receive the reaction solution for preparing dicyclopentenyl acrylate.

[0025] One end of the first tube 101 is connected to the output port of the buffer tank 10.

[0026] The inlet of the first water pump 11 is connected to the other end of the first pipe 101.

[0027] One end of the second pipe 102 is connected to the output port of the first water pump 11.

[0028] The top inlet of the first falling film evaporator 12 is connected to the other end of the second tube 102 so that the reaction liquid in the buffer tank 10 can be pumped into the first falling film evaporator 12 by the first water pump 11.

[0029] One end of the third tube 121 is connected to the bottom output port of the first falling film evaporator 12.

[0030] The inlet on the side wall of the receiving tank 13 is connected to the other end of the third tube 121, so that the solution of the first falling film evaporator 12 is transported to the receiving tank 13 through the third tube 121.

[0031] One end of the fourth tube 131 is connected to the output port at the top of the receiving tank 13.

[0032] The inlet of the first deep cooler 14 is connected to the other end of the fourth tube 131. It should be understood that the solution output from the first falling film evaporator 12 is relatively hot, so a portion of the solution flowing into the receiving tank 13 (the crude product dicyclopentadiene acrylate) will remain at the bottom of the receiving tank 13, while the other portion of water vapor (containing unreacted acrylic acid and dicyclopentadiene) enters the first deep cooler 14 through the fourth tube 131 for condensation.

[0033] One end of the fifth tube 141 is connected to the output port of the first cryogenic cooler 14.

[0034] The top inlet of the solvent recovery tank 15 is connected to the other end of the fifth tube 141, so that the condensate (unreacted acrylic acid and dicyclopentadiene solution) condensed by the first cryogenic reactor 14 is transported to the solvent recovery tank 15 through the fifth tube.

[0035] Furthermore, the reaction liquid falling film device of the dicyclopentadiene acrylate preparation system also includes a circulation pipe 24, one end of which is connected to the output port at the bottom of the recovery solvent tank 15, and the other end of the circulation pipe 24 is connected to the reaction vessel 22 via a fourth water pump 25, so that the solution (unreacted acrylic acid and dicyclopentadiene solution) in the recovery solvent tank 15 can be pumped back to the reaction vessel 22 by the fourth water pump 25 for recycling, effectively saving costs.

[0036] Preferably, the circulation pipe 24 is provided with a third switching valve 241 for controlling the opening and closing of the circulation pipe 24, and the circulation pipe 241 is also provided with a third one-way valve 242 for directing the solution from the recovery solvent tank 15 to the reaction vessel 22.

[0037] One end of the sixth tube 132 is connected to the output port at the bottom of the receiving tank 13.

[0038] The inlet of the second water pump 16 is connected to the other end of the sixth pipe 132.

[0039] Preferably, the sixth tube 132 is provided with a first switching valve 1321 for controlling the opening and closing of the sixth tube 132, and the sixth tube 132 is also provided with a first check valve 1322 for directing the solution from the receiving tank 13 to the second water pump 16.

[0040] One end of the seventh pipe 133 is connected to the output port of the second water pump 16.

[0041] The inlet at the top of the second falling film evaporator 17 is connected to the other end of the seventh tube 133.

[0042] One end of the eighth tube 171 is connected to the output port at the bottom of the second falling film evaporator 17.

[0043] The inlet on the side wall of the recombinant tank 18 is connected to the other end of the eighth tube 171.

[0044] One end of the ninth tube 181 is connected to the outlet at the top of the recombinant tank 18.

[0045] The inlet of the second cryogenic unit 19 is connected to the other end of the ninth tube 181;

[0046] The inlet at the top of the product tank 20 is connected to the outlet of the second cryogenic unit 19 via the tenth tube 191.

[0047] It should be understood that the solution output from the second falling film evaporator 17 is relatively hot. Therefore, a portion of the solution (heavy components) flowing into the heavy component tank 18 will remain in the heavy component tank 18, while the remaining water vapor (containing qualified product dicyclopentadiene acrylate) enters the second cryostat 19 through the ninth tube 181 for condensation and is ultimately contained in the product tank 20. Additionally, the heavy components remaining in the heavy component tank 18 include acrylic polymers and dicyclopentadiene polymers, which, due to their relatively high boiling points, remain in the heavy component tank 18.

[0048] Furthermore, the falling film device for the reaction liquid in the dicyclopentadiene acrylate preparation system also includes a delivery pipe 21, one end of which is connected to the bottom outlet of the reactor 22, and the other end of which is connected to the inlet of the buffer tank 10 via a third water pump 23, so that the reaction liquid in the reactor 22 can be pumped into the buffer tank 10 by the third water pump 23. It should be understood that the reactor 22 is used to input dicyclopentadiene and an acrylic acid solution containing a strong acid catalyst, in order to prepare dicyclopentadiene acrylate within the reactor 22.

[0049] Preferably, the conveying pipe 21 is provided with a second switching valve 211 for controlling the opening and closing of the conveying pipe 21, and the conveying pipe 21 is also provided with a second one-way valve 212 for causing the solution in the reaction vessel 22 to flow to the buffer tank 10.

[0050] Furthermore, such as Figure 2-3 As shown, the reaction liquid falling film device of the dicyclopentadiene acrylate preparation system also includes a first steam pipe 31, a first heat exchanger 32, a first discharge pipe 33, a second steam pipe 34, a second heat exchanger 35, and a second discharge pipe 36.

[0051] One end of the first steam pipe 31 is connected to the steam outlet of the first falling film evaporator 12, and the other end of the first steam pipe 31 is connected to the first steam inlet on the side wall of the receiving tank 13.

[0052] The first heat exchanger 32 is planar and inclinedly disposed in the receiving tank 13. The inlet of the first heat exchanger 32 is connected to the first steam pipe 31, so that the water vapor output by the first falling film evaporator 12 enters the first heat exchanger 32 through the first steam pipe 31.

[0053] It should be understood that the first falling film evaporator 12 outputs relatively high-temperature steam. In this embodiment, the water vapor output by the first falling film evaporator 12 is recycled and reused, and then fed back into the first heat exchanger 32 to exchange heat with the crude product dicyclopentadiene acrylate in the receiving tank 13. This allows the unreacted acrylic acid and dicyclopentadiene solution to evaporate more fully into the first cryogenic cooler 14, resulting in less residual unreacted acrylic acid and dicyclopentadiene solution and greater energy savings.

[0054] One end of the first discharge pipe 33 is connected to the first steam outlet at the bottom of the receiving tank 13, wherein the outlet of the first heat exchanger 32 is connected to one end of the first discharge pipe 33.

[0055] One end of the second steam pipe 34 is connected to the steam outlet of the second falling film evaporator 17, and the other end of the second steam pipe 34 is connected to the second steam inlet on the side wall of the receiving tank 13.

[0056] The second heat exchanger 35 is planar and inclinedly disposed in the receiving tank 13. The inlet of the second heat exchanger 35 is connected to the second steam pipe 34, so that the water vapor output by the second falling film evaporator 17 enters the second heat exchanger 35 through the second steam pipe 34.

[0057] It should be understood that the second falling film evaporator 17 outputs relatively high-temperature steam. In this embodiment, the water vapor output by the second falling film evaporator 17 is recycled and reused, and then fed back into the second heat exchanger 35 to exchange heat with the crude product dicyclopentadiene acrylate in the receiving tank 13. This allows the unreacted acrylic acid and dicyclopentadiene solution to evaporate more fully into the first cryogenic cooler 14, resulting in less residual unreacted acrylic acid and dicyclopentadiene solution and greater energy savings.

[0058] One end of the second discharge pipe 36 is connected to the second steam outlet at the bottom of the receiving tank 13, wherein the outlet of the second heat exchanger 35 is connected to one end of the second discharge pipe 36.

[0059] In this embodiment, the first heat exchanger 32 and the second heat exchanger 35 are arranged alternately in the receiving tank 13, which makes the heat exchange effect better.

[0060] Furthermore, the receiving tank 13 is also equipped with a uniform dispersion disk 130 connected to the other end of the third tube 121, wherein the first heat exchanger 32 and the second heat exchanger 35 are both located below the uniform dispersion disk 130. It should be understood that the uniform dispersion disk 130 is provided with through holes at both the top and bottom. The solution transported by the third tube 121 will enter the uniform dispersion disk 130 and be evenly distributed. The solution is evenly scattered on the first heat exchanger 32 and the second heat exchanger 35 for heat exchange, and the steam evaporates evenly.

[0061] Preferably, the first heat exchanger 32 is formed by bending a first copper tube, one end of which passes through the uniform dispersion plate 130 and connects to the first steam pipe 31, and the other end of which connects to the first discharge pipe 33. The second heat exchanger 35 is formed by bending a second copper tube, one end of which passes through the uniform dispersion plate 130 and connects to the second steam pipe 14, and the other end of which connects to the second discharge pipe 36. It should be understood that the first heat exchanger 32, formed by bending a first copper tube to form a partially planar heat exchanger, and the second heat exchanger 35, formed by bending a second copper tube to form a partially planar heat exchanger, increase the heat exchange area and improve the heat exchange effect.

[0062] It should be noted that the terms "comprising," "including," or any other variations thereof are intended to cover non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements includes not only those elements but also other elements not expressly listed, or elements inherent to such a process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising one..." does not exclude the presence of other identical elements in the process, method, article, or apparatus that includes said element.

[0063] Although embodiments of the invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the invention, the scope of which is defined by the appended claims and their equivalents.

Claims

1. A falling film apparatus for the reaction liquid in a dicyclopentadiene acrylate preparation system, characterized in that, include: Buffer tank, used to receive the reaction solution for the preparation of dicyclopentenyl acrylate; The first tube has one end connected to the output port of the buffer tank; The first water pump has its inlet connected to the other end of the first pipe. The second pipe has one end connected to the output port of the first water pump; The first falling film evaporator has its top inlet connected to the other end of the second tube; The third tube has one end connected to the bottom outlet of the first falling film evaporator; The receiving tank has an inlet on its side wall connected to the other end of the third tube. The fourth tube has one end connected to the output port at the top of the receiving tank; The first deep cooler has its inlet connected to the other end of the fourth tube; The fifth tube has one end connected to the output port of the first deep cooler; A solvent recovery tank, the top inlet of which is connected to the other end of the fifth tube; The sixth tube has one end connected to the output port at the bottom of the receiving tank; The second water pump has its inlet connected to the other end of the sixth pipe. The seventh pipe body has one end connected to the output port of the second water pump; The second falling film evaporator has its top inlet connected to the other end of the seventh tube. The eighth tube is connected at one end to the output port at the bottom of the second falling film evaporator; The recombinant container has an inlet on its side wall connected to the other end of the eighth tube. The ninth tube, one end of which is connected to the output port at the top of the recombinant component tank; The second cryostat has its inlet connected to the other end of the ninth tube. The product tank has its top inlet connected to the outlet of the second cryogenic unit via a tenth tube. The delivery pipe has one end connected to the bottom outlet of the reactor and the other end connected to the inlet of the buffer tank via a third water pump, so that the reaction liquid in the reactor can be pumped into the buffer tank by the third water pump. The circulation pipe has one end connected to the output port at the bottom of the solvent recovery tank, and the other end connected to the reactor via a fourth water pump, so that the solution in the solvent recovery tank can be pumped back to the reactor via the fourth water pump. The first steam pipe has one end connected to the steam outlet of the first falling film evaporator and the other end connected to the first steam inlet on the side wall of the receiving tank. The first heat exchanger is planar in shape and inclinedly disposed in the receiving tank, wherein the inlet of the first heat exchanger is connected to the first steam pipe; The first discharge pipe has one end connected to the first steam outlet at the bottom of the receiving tank, wherein the outlet of the first heat exchanger is connected to one end of the first discharge pipe. The second steam pipe has one end connected to the steam outlet of the second falling film evaporator and the other end connected to the second steam inlet on the side wall of the receiving tank. The second heat exchanger is planar in shape and inclinedly disposed in the receiving tank, wherein the inlet of the second heat exchanger is connected to the second steam pipe; The second discharge pipe has one end connected to the second steam outlet at the bottom of the receiving tank, wherein the outlet of the second heat exchanger is connected to one end of the second discharge pipe. The first heat exchanger and the second heat exchanger are arranged alternately inside the receiving tank.

2. The reaction liquid falling film device of the dicyclopentadiene acrylate preparation system according to claim 1, characterized in that, The sixth pipe is provided with a first switching valve for controlling the opening and closing of the sixth pipe, and the sixth pipe is also provided with a first check valve for directing the solution in the receiving tank to the second water pump.

3. The reaction liquid falling film device of the dicyclopentadiene acrylate preparation system according to claim 1, characterized in that, The delivery pipe is equipped with a second switching valve for controlling the opening and closing of the delivery pipe, and the delivery pipe is also equipped with a second one-way valve for directing the solution from the reactor to the buffer tank.

4. The falling film device for the reaction solution of the dicyclopentadiene acrylate preparation system according to claim 1, characterized in that, The circulation pipe is equipped with a third switching valve for controlling the opening and closing of the circulation pipe, and the circulation pipe is also equipped with a third one-way valve for allowing the solution in the recovery solvent tank to flow into the reaction vessel.

5. The reaction liquid falling film device of the dicyclopentadiene acrylate preparation system according to claim 1, characterized in that, The receiving tank is also provided with a uniformly dispersing disk that is connected to the other end of the third tube, wherein the first heat exchanger and the second heat exchanger are both located below the uniformly dispersing disk.

6. The reaction liquid falling film device for the dicyclopentadiene acrylate preparation system according to claim 5, characterized in that, The first heat exchanger is formed by bending a first copper tube. One end of the first copper tube passes through the uniformly dispersed disk and is connected to the first steam pipe. The other end of the first copper tube is connected to the first discharge pipe. The second heat exchanger is formed by bending a second copper tube. One end of the second copper tube passes through the uniformly dispersed disk and is connected to the second steam pipe. The other end of the second copper tube is connected to the second discharge pipe.

Images