Reaction tower for preparing acetone derivative and continuous production system
By designing the reaction tower and continuous production system, the problems of small output and poor quality in isopropyl acetone production were solved, and the large-scale continuous production of isopropyl acetone was achieved, which improved production efficiency and product quality.
Patent Information
- Application Number
- CN202422122111.1
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2024-08-30
- Publication Date
- 2025-07-22
- Estimated Expiration
- 2034-08-30
AI Technical Summary
In the prior art, the production method of isopropyl acetone is mainly two-step or one-step method. The domestic production of isopropyl acetone is small, of poor quality, and lacks a large-scale continuous production system, which hinders its large-scale application.
A reaction tower and a continuous production system are designed, including the reaction tower body, a pipe distributor, a catalyst filling area and a reaction liquid buffer zone. The catalyst is activated and regenerated by setting up a raw material inlet, a gas purging port and a regeneration liquid inlet, and the continuous production of acetone derivatives is achieved through the coordination of the raw material liquid tank, preheater, a reaction liquid buffer tank, a distillation kettle and a reaction tower.
The large-scale continuous production of isopropyl acetone has been achieved, yield and quality have been improved, and is suitable for the large-scale production of acetone derivatives.
Smart Images
Figure CN223128000U_ABST
Abstract
Description
Technical Field
[0001] The utility model relates to the technical field of preparation equipment for acetone derivatives, and particularly relates to a reaction tower and a continuous production system for preparing acetone derivatives. Background Art
[0002] Isopropylidene acetone, chemically named 4-methyl-3-penten-2-one, is an acetone derivative widely used in industry. Its most important use is to generate a commonly used solvent MIBK (methyl isobutyl ketone) through a hydrogenation reaction under appropriate conditions. It can also be used in pharmaceuticals, fine chemicals, pesticides, etc., and can also be used as a medium-boiling solvent, with a wide range of uses.
[0003] In the prior art, the related research on isopropylidene acetone mainly focuses on the production process. At present, the production methods of isopropylidene acetone are mainly divided into the "one-step method" and the "two-step method". The main production process of the "two-step method" is as follows: acetone first generates diacetone alcohol under the catalysis of a basic catalyst, and then diacetone alcohol undergoes a dehydration reaction under the catalysis of an acidic catalyst to generate isopropylidene acetone. The main production process of the "one-step method" is as follows: acetone undergoes a one-step reaction under the catalysis of a catalyst to generate isopropylidene acetone. At present, domestic isopropylidene acetone mainly comes from the by-products of the production of diacetone alcohol or isophorone. Its output is small and the quality is poor. There are few reports on the large-scale continuous production of isopropylidene acetone in China, which hinders the large-scale application of isopropylidene acetone.
[0004] Therefore, it is necessary to design a continuous production system suitable for acetone derivatives, and the prior art needs to be further improved. Summary of the Utility Model
[0005] One of the purposes of the utility model is to provide a reaction tower for preparing acetone derivatives, which can realize the activation and regeneration of the catalyst in the reaction tower.
[0006] In order to achieve the above purpose, the utility model adopts the following technical solutions:
[0007] A reaction tower for preparing acetone derivatives, which comprises a reaction tower body. Inside the reaction tower body, a tube bundle distributor, a catalyst filling area, and a reaction liquid buffer area are arranged from top to bottom. At the top of the reaction tower, a raw material inlet, a gas purge port, and a regeneration liquid inlet are respectively arranged. The raw material inlet is used to introduce the preheated raw material liquid; the preheated raw material liquid enters the tube bundle distributor through the raw material inlet, and after being distributed by the tube bundle distributor, enters the catalyst filling area; after the raw material liquid contacts the catalyst in the catalyst filling area, the reaction liquid obtained by the reaction of the raw material liquid enters the reaction liquid buffer area; at the bottom of the reaction tower body, a reaction liquid outlet is arranged, and the reaction liquid is discharged through the reaction liquid outlet.
[0008] One of the above reaction towers for preparing acetone derivatives, the above tube bundle distributor includes a raw material liquid delivery pipe, a tube bundle connection port, tube bundles, and distribution holes. The above raw material liquid delivery pipe is connected with a number of regularly arranged tube bundles through the tube bundle connection port, and the above distribution holes are arranged on the surface of each tube bundle.
[0009] One of the above reaction towers for preparing acetone derivatives, the above tube bundle connection port is arranged at the bottom of the raw material liquid delivery pipe. The above tube bundles are arranged in two upper and lower layers. The upper layer of tube bundles and the lower layer of tube bundles are cylindrical. Distribution holes are evenly arranged along the tube walls of the upper layer of tube bundles and the lower layer of tube bundles. The above distribution holes are circular.
[0010] Another object of the present utility model is to provide a continuous production system for preparing acetone derivatives, which includes a raw material liquid tank, a preheater, a reaction liquid buffer tank, a distillation kettle, and a reaction tower. The outlet of the above raw material liquid tank is connected to the above reaction tower through the preheater, and the preheated raw material liquid enters the interior of the reaction tower from the top of the above reaction tower; the bottom of the above reaction tower is connected to the reaction liquid buffer tank, and the reaction liquid obtained in the reaction tower enters the above reaction liquid buffer tank; the outlet of the above reaction liquid buffer tank is connected to the inlet of the above distillation kettle, and the outlet of the above distillation kettle is connected to the inlet of the above raw material liquid tank.
[0011] One of the above continuous production systems for preparing acetone derivatives, a distillation condenser is arranged between the above raw material liquid tank and the above distillation kettle, and a metering pump is arranged between the above raw material liquid tank and the preheater; a reaction liquid cooler is arranged between the above reaction tower and the reaction liquid buffer tank, and a transfer pump is arranged between the above reaction liquid buffer tank and the above distillation kettle.
[0012] One of the above continuous production systems for preparing acetone derivatives, the reaction temperature in the above catalyst filling area is controlled by a jacket arranged on the periphery of the catalyst filling area. Sieve holes are arranged at the bottom of the above catalyst filling area, and the reaction liquid obtained in the reaction passes through the above sieve holes and enters the reaction liquid buffer area.
[0013] One of the above continuous production systems for preparing acetone derivatives, the above reaction liquid cooler and the reaction liquid buffer tank are connected through a U-shaped elbow.
[0014] Compared with the prior art, the present utility model brings the following beneficial technical effects:
[0015] The present utility model provides a reaction tower for preparing acetone derivatives. By improving the reaction tower, for example, a raw material feed port, a gas purge port and a regeneration liquid inlet are respectively arranged at the top of the reaction tower. When the catalyst is deactivated, the feeding is stopped. At this time, nitrogen is introduced into the reaction tower through the gas purge port, and the reaction liquid in the reaction liquid buffer zone and the catalyst filling zone is purged through the reaction liquid outlet, the reaction liquid cooler and the U-shaped bend into the reaction liquid buffer tank, and then the nitrogen introduction is stopped. After the reaction liquid in the reaction tower is purged, the regeneration liquid is introduced into the reaction tower through the regeneration liquid inlet to activate and regenerate the catalyst in the catalyst filling zone of the reaction tower. After the activation and regeneration are completed, the introduction of the regeneration liquid is stopped. After the regeneration liquid in the reaction tower is cleaned up, acetone is normally introduced through the raw material feed port, and production can be resumed. Such a design method facilitates the continuous production of acetone derivatives.
[0016] The present utility model provides a continuous production system for preparing acetone derivatives. Through the mutual cooperation of a raw material liquid tank, a preheater, a reaction liquid buffer tank, a distillation kettle and a reaction tower, large-scale production of acetone derivatives can be achieved. Most importantly, continuous production of acetone derivatives can be realized. BRIEF DESCRIPTION OF THE DRAWINGS
[0017] The present utility model will be further described below with reference to the accompanying drawings:
[0018] Figure 1 is a schematic structural diagram of a continuous production system for preparing acetone derivatives according to the present utility model;
[0019] Figure 2 is a schematic structural diagram of the reaction tower of the present utility model;
[0020] Figure 3 is a schematic structural diagram of a tube bundle distributor in the reaction tower of the present utility model;
[0021] In the figure:
[0022] 1, raw material liquid tank; 2, metering pump; 3, preheater; 4, reaction tower; 5, reaction liquid cooler; 6, reaction liquid buffer tank; 7, delivery pump; 8, U-shaped bend; 9, distillation kettle; 10, distillation condenser; 11, distillation kettle bottom valve; 101, raw material feed port; 102, gas purge port; 103, regeneration liquid inlet; 104, tube bundle distributor; 105, catalyst filling zone; 106, jacket; 107, reaction liquid outlet; 108, reaction liquid buffer zone; 109, reaction tower body; 110, sieve plate; 111, raw material liquid delivery pipe; 112, pipe connection port; 113, pipe; 114, distribution hole. DETAILED DESCRIPTION OF THE EMBODIMENTS
[0023] The present utility model provides a reaction tower and a continuous production system for preparing acetone derivatives. In order to make the advantages and technical solutions of the present utility model clearer and more definite, the following further illustrates the present utility model with specific embodiments.
[0024] The acetone derivatives mentioned in the present utility model are such as mesityl oxide.
[0025] As Figure 2 As shown, the present utility model first improves the reaction tower. By improving the structure of the reaction tower, it is made more suitable for the continuous production of acetone derivatives. The reaction tower 4 includes a reaction tower body 109. Inside the reaction tower body, a tube bundle distributor 104, a catalyst filling area 105, and a reaction liquid buffer area 108 are arranged from top to bottom. The function of the tube bundle distributor is to evenly distribute the materials. At the top of the reaction tower, a raw material inlet 101, a gas purge port 102, and a regenerated liquid inlet 103 are respectively arranged. The raw material inlet is used to introduce the preheated raw material liquid. The preheated raw material liquid enters the tube bundle distributor through the raw material inlet, and after being distributed by the tube bundle distributor, it enters the catalyst filling area. An outer jacket 106 is arranged on the outer wall of the reaction tower body in the outer space of the catalyst filling area and the reaction liquid buffer area to provide a suitable temperature for the reaction liquid through the outer jacket 106. The reaction liquid obtained by the reaction of the raw material liquid and the catalyst in the catalyst filling area enters the reaction liquid buffer area. A reaction liquid outlet 107 is arranged at the bottom of the reaction tower body, and the reaction liquid is discharged through the reaction liquid outlet 107.
[0026] As Figure 3 As shown, the above-mentioned tube bundle distributor includes a raw material liquid delivery pipe 111, a tube connection port 112, tube bundles 113, and distribution holes 114. The above-mentioned raw material liquid delivery pipe is connected with a number of regularly arranged tube bundles through the tube connection port. Distribution holes are arranged on the surface of each tube bundle, and the distribution holes are evenly arranged on the surface of each tube bundle. The tube bundle distributor evenly flows the raw material liquid into the catalyst filling area in the reaction tower after redistribution.
[0027] For the above-mentioned reaction tower for preparing acetone derivatives, the above-mentioned tube connection port is arranged at the bottom of the raw material liquid delivery pipe. The above-mentioned tube bundles are provided with two layers, the upper-layer tube bundle and the lower-layer tube bundle are cylindrical, and distribution holes are evenly arranged along the tube wall on the upper-layer tube bundle and the lower-layer tube bundle. The distribution holes are circular.
[0028] Specifically, the raw material inlet 101 is connected to the tube-sheet distributor. The gas purge port and the regenerant inlet are distributed on both sides of the raw material inlet. The jacket only cools down or heats up the materials in the catalyst filling area and the reaction liquid buffer area through cold and heat media. The catalyst filling area is used to fill solid catalysts. A sieve plate 110 is provided at the bottom of the catalyst filling area. Sieve holes are evenly arranged on the sieve plate 110. The sieve holes are preferably circular hole structures, which are used to support the solid catalysts and ensure that the liquid in the catalyst filling area can freely flow into the reaction liquid buffer area.
[0029] As Figure 1 shown, when the above reaction tower is applied to a continuous production system for preparing acetone derivatives, it further includes: a raw material liquid tank 1, a metering pump 2, a preheater 3, a reaction liquid cooler 5, a reaction liquid buffer tank 6, a transfer pump 7, a distillation kettle 9 and a distillation condenser 10. Among them, the raw material liquid tank 1 is connected to the distillation kettle 9 through the distillation condenser 10. At the same time, the raw material liquid tank 1 is respectively connected to the top of the reaction tower through the metering pump 2 and the preheater 3.
[0030] The bottom of the reaction tower is connected to the top of the reaction liquid buffer tank through the reaction liquid cooler 5 and a U-shaped bend 8. The bottom of the reaction liquid buffer tank is connected to the distillation kettle through a transfer pump. A distillation kettle bottom valve 11 is provided at the bottom of the distillation kettle.
[0031] The usage method of the continuous production system of the present utility model is as follows:
[0032] Turn on the metering pump, pump acetone in the raw material liquid tank to the preheater for preheating and temperature raising. The preheated acetone enters the reaction tower from the top of the reaction tower, contacts the catalyst in the catalyst filling area in the reaction tower and undergoes a condensation-dehydration reaction. Then the reaction liquid flows through the reaction liquid cooler to cool down, and then flows into the reaction liquid buffer tank through the U-shaped bend. Then turn on the transfer pump, and transfer the reaction liquid in the reaction liquid buffer tank to the distillation kettle for distillation by the transfer pump. The unreacted acetone vaporizes and enters the raw material liquid tank after being condensed by the distillation condenser. The distillation residue is crude isopropylidene acetone, which goes to the next process through the distillation kettle bottom valve, and so on in a cycle.
[0033] When the catalyst is deactivated, stop feeding and producing. Then, nitrogen is introduced into the reaction tower through the gas purge port, and the reaction liquid in the reaction liquid buffer area and the catalyst filling area is purged to the reaction liquid buffer tank through the reaction liquid outlet, the reaction liquid cooler and the U-shaped bend, and then stop introducing nitrogen. After the reaction liquid in the reaction tower is purged, regenerant is introduced into the reaction tower through the regenerant inlet to activate and regenerate the catalyst in the catalyst filling area of the reaction tower. After the activation and regeneration are completed, stop introducing the regenerant. After the regenerant in the reaction tower is cleaned up, acetone is normally introduced through the raw material inlet to resume production.
[0034] The following further describes the present utility model with specific embodiments.
[0035] Example 1:
[0036] Taking the preparation of mesityl oxide as an example.
[0037] Using the above continuous production system for preparing acetone derivatives, the specific operation steps are as follows:
[0038] Start the metering pump, pump the raw material acetone in the raw material liquid tank (filled with acetone) to the preheater through the metering pump for preheating. The preheated acetone enters the tube bundle distributor 104 through the raw material inlet 101. After being distributed by the tube bundle distributor 104, the raw material liquid flows out through the distribution holes 114 on the tube 113 and enters the catalyst filling area 105, where it contacts the resin catalyst and undergoes a chemical reaction. The reaction temperature is controlled by the jacket 106. The reaction liquid enters the reaction liquid buffer zone 108 through the sieve holes 110 at the bottom of the catalyst filling area 105, and then enters the reaction liquid cooler 5 through the reaction liquid outlet 107. The cooled reaction liquid enters the reaction liquid buffer tank 6 through the U-shaped bend pipe 8. The reaction liquid in the reaction liquid buffer tank 6 is transported to the distillation kettle 9 through the transfer pump 7. The distillation kettle 9 is heated for distillation. The unreacted raw material acetone is vaporized by distillation, condensed in the distillation condenser, and then enters the raw material liquid tank, realizing the continuous reuse of acetone. The residue in the distillation kettle 9 is the crude mesityl oxide. By opening the bottom valve 11 of the distillation kettle, it can be transferred to the purification process for purification.
[0039] After the resin catalyst in the catalyst filling area 105 in the reaction tower 4 is deactivated, the reaction process stops. Compressed air or nitrogen is introduced through the gas purge port 102 at the top of the reaction tower 4 to blow out the residual liquid in the reaction tower 4. Then, the gas purge port 102 is closed, and the catalyst in the catalyst filling area 105 in the reaction tower 4 is activated and regenerated through the regeneration liquid inlet 103. After the catalyst regeneration is completed, by switching the process flow, the production of mesityl oxide can be resumed.
[0040] The reaction tower and the continuous production system defined by the present utility model can also be applied to fields similar to the preparation of acetone derivatives.
[0041] The parts not described in the present utility model can be realized by referring to the prior art.
[0042] It should be noted that any equivalent method or obvious variant method made by those skilled in the art under the teaching of this specification should be within the protection scope of the present utility model.
Claims
1. A reaction tower for preparing acetone derivatives, which comprises a reaction tower body, and is characterized in that: Inside the reaction tower body, a tube bundle distributor, a catalyst filling area, and a reaction liquid buffer area are arranged from top to bottom. At the top of the reaction tower, a raw material inlet, a gas purge port, and a regenerated liquid inlet are respectively arranged. The raw material inlet is used for introducing the preheated raw material liquid. The preheated raw material liquid enters the tube bundle distributor through the raw material inlet, and after being distributed by the tube bundle distributor, enters the catalyst filling area. After the raw material liquid contacts the catalyst in the catalyst filling area, the reaction liquid obtained from the reaction of the raw material liquid enters the reaction liquid buffer area. A reaction liquid outlet is arranged at the bottom of the reaction tower body, and the reaction liquid is discharged through the reaction liquid outlet.
2. The reaction tower for preparing acetone derivatives according to claim 1, characterized in that: The tube bundle distributor includes a raw material liquid delivery pipe, a tube connection port, tube bundles, and distribution holes. The raw material liquid delivery pipe is connected to a number of regularly arranged tube bundles through the tube connection port, and the distribution holes are arranged on the surface of each tube bundle.
3. The reaction tower for preparing acetone derivatives according to claim 2, characterized in that: The tube connection port is arranged at the bottom of the raw material liquid delivery pipe. The tube bundles are arranged in two layers, the upper layer of tube bundles and the lower layer of tube bundles are cylindrical, and the distribution holes are evenly arranged along the tube wall of the upper layer of tube bundles and the lower layer of tube bundles. The distribution holes are circular.
4. A continuous production system for preparing acetone derivatives, characterized in that, It includes a raw material liquid tank, a preheater, a reaction liquid buffer tank, a distillation kettle, and the reaction tower according to any one of claims 1 to 3. The outlet of the raw material liquid tank is connected to the reaction tower through the preheater, and the preheated raw material liquid enters the interior of the reaction tower from the top of the reaction tower. The bottom of the reaction tower is connected to the reaction liquid buffer tank, and the reaction liquid obtained from the reaction in the reaction tower enters the reaction liquid buffer tank. The outlet of the reaction liquid buffer tank is connected to the inlet of the distillation kettle, and the outlet of the distillation kettle is connected to the inlet of the raw material liquid tank.
5. A continuous production system for preparing acetone derivatives according to claim 4, characterized in that: A distillation condenser is arranged between the raw material liquid tank and the distillation kettle, and a metering pump is arranged between the raw material liquid tank and the preheater. A reaction liquid cooler is arranged between the reaction tower and the reaction liquid buffer tank, and a transfer pump is arranged between the reaction liquid buffer tank and the distillation kettle.
6. A continuous production system for preparing acetone derivatives according to claim 4, characterized in that: The reaction temperature in the catalyst filling area is controlled by a jacket arranged on the periphery of the catalyst filling area. A sieve hole is arranged at the bottom of the catalyst filling area, and the reaction liquid obtained from the reaction passes through the sieve hole and enters the reaction liquid buffer area.
7. A continuous production system for preparing acetone derivatives according to claim 5, characterized in that: The reaction liquid cooler and the reaction liquid buffer tank are connected through a U-shaped bend pipe.