Jet outer circulation reaction device for heterogeneous continuous synthesis
The jet-assisted external circulation reactor for heterogeneous continuous synthesis solves the problems of long reaction time and low yield in the traditional production of hydrazine hydrate, achieving rapid mixing and stable separation, and improving production efficiency and product yield.
Patent Information
- Application Number
- CN202520416398.0
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2025-03-11
- Publication Date
- 2026-03-06
- Estimated Expiration
- 2035-03-11
AI Technical Summary
In the traditional hydrogen peroxide process for the production of hydrazine hydrate, the reaction time is long, the yield of butanone is low, and oxidation side reactions are frequent, resulting in a decrease in product yield.
The heterogeneous continuous synthesis jet external circulation reactor includes a reactor, an external circulation pipe, a circulating pump, a gas phase distributor, and an oil-gas-water three-phase separator to achieve rapid material flow and stable separation of the oil and water phases. A turbine agitator promotes mixing, and the external circulation pipe and heat exchanger control the temperature.
Shorten reaction time, increase the yield of butanone azohydride, reduce oxidation side reactions, improve production efficiency and product yield, and achieve continuous synthesis.
Smart Images
Figure CN223969969U_ABST
Abstract
Description
Technical Field
[0001] This utility model relates to the field of chemical synthesis technology, specifically to a jet external circulation reaction device for heterogeneous continuous synthesis. Background Technology
[0002] Hydrazine hydrate is an important chemical raw material and a widely used chemical product. It is an important raw material for the production of foaming agents, pesticides, pharmaceuticals, dyes, developers, and reducing agents. It is also used in the manufacture of high-purity metals, synthetic fibers, rare element separation, deoxygenation of large boiler feedwater, rocket fuel, and the production of explosives. There are four main methods for the industrial production of hydrazine hydrate: the Rasching process, Bayer's ketone-hydrazine process, the urea process, and PCUK's hydrogen peroxide process.
[0003] The hydrogen peroxide process for hydrazine hydrate uses hydrogen peroxide as an oxidant, nitriles or amides as catalysts, and sodium phosphate and ammonium carboxylate as co-catalysts. Butanone and ammonia react with hydrogen peroxide to produce the intermediate butanone azide, which is then hydrolyzed to generate hydrazine hydrate. The advantages of this method are that it does not produce highly corrosive chlorides as a byproduct, has low energy consumption, and is an energy-saving and environmentally friendly green production process.
[0004] In the traditional hydrogen peroxide process for producing hydrazine hydrate, the reactor used to synthesize the intermediate methyl ethyl ketone (MEK) is a batch reactor. The operation involves adding MEK, catalyst and additives, ammonia, and hydrogen peroxide sequentially. During preparation, the generated MEK is insoluble in water and dissolves MEK to form an oil phase, which separates from the aqueous working liquid containing the catalyst. In traditional hydrogen peroxide processes, the oil and aqueous phases are separated only after the reaction is complete, and the oil phase is then purified and hydrolyzed to produce hydrazine hydrate. If the oil phase is not removed from the reaction system in a timely manner, the generated MEK is easily further oxidized and decomposed by hydrogen peroxide in the aqueous phase, thus reducing the yield of MEK. Furthermore, due to the weak reactivity of the catalyst, the concentration of hydrogen peroxide decreases after the initial consumption during the reaction, further slowing the reaction rate and prolonging the reaction time. Therefore, the batch synthesis reaction requires a longer time. The prolonged reaction time also increases the contact between the oxide and MEK, causing deep oxidation of the product and reducing the product yield.
[0005] Therefore, in response to the technical problems described above, there is an urgent need for a reaction apparatus that can shorten the reaction time and enable continuous synthesis. Summary of the Invention
[0006] The technical problem to be solved by this utility model is to provide a jet external circulation reaction device for heterogeneous continuous synthesis. This device can realize the continuous synthesis of products, shorten the synthesis reaction time, improve the yield of butanone azo, and reduce the occurrence of oxidation side reactions.
[0007] To solve the above-mentioned technical problems, the technical solution of this utility model is: a jet external circulation reaction device for heterogeneous continuous synthesis, including a reaction vessel, wherein the reaction vessel is equipped with a stirrer; an external circulation pipe is provided at the bottom of the reaction vessel, the external circulation pipe is connected to the inside of the reaction vessel, a circulation pump is provided on the external circulation pipe, and the external circulation pipe is connected to a working fluid input pipe; a gas inlet pipe is provided inside the reaction vessel, and a gas phase distributor connected to the gas inlet pipe is provided at the bottom of the reaction vessel; an overflow port is provided at the top of the reaction vessel, and the overflow port is connected to an oil-gas-water three-phase separator.
[0008] As a preferred technical solution, a heat exchanger is installed on the outer circulation pipe.
[0009] As a preferred technical solution, a static mixer is installed on the outer circulation pipe.
[0010] As a preferred technical solution, the working fluid input pipe includes a first working fluid input pipe, a second working fluid input pipe, and a third working fluid input pipe.
[0011] As a preferred technical solution, the agitator is a turbine agitator.
[0012] As a preferred technical solution, the end of the outer circulation pipe is equipped with a working fluid injector that extends to the bottom of the reactor.
[0013] As a preferred technical solution, a baffle is provided inside the reaction vessel.
[0014] As a preferred technical solution, the gas phase distributor is annular.
[0015] Compared with the prior art, the present invention has at least the following beneficial effects:
[0016] (1) This device enables rapid flow of materials during the reaction process, promotes mass transfer between gas and liquid or liquid and liquid phases during the reaction process, and increases the reaction rate. Compared with the traditional batch production method, it can significantly improve production efficiency and shorten reaction time.
[0017] (2) The working fluid is fed continuously, which can ensure that the raw material (hydrogen peroxide) in the main reaction zone of the reactor is kept at a high concentration, which is conducive to accelerating the reaction rate and shortening the reaction time. Ammonia gas is injected into the reactor through the gas phase distributor at the bottom of the reactor to ensure the ammonia concentration of the reaction system. At the same time, it promotes the increase of the difference in the rising speed between the oil phase product (butanone azide) and the aqueous phase, which is conducive to the separation of products, reduces the contact between products and hydrogen peroxide, reduces the oxidation side reaction of products, and improves the product yield.
[0018] (3) This device utilizes the characteristic that the oil phase product is insoluble in the aqueous system to realize the continuous synthesis of the product and the stable separation of the oil phase product and the aqueous working fluid, which shortens the synthesis reaction time and improves production efficiency.
[0019] (4) The oil phase products generated during the reaction can be separated from the reaction solution in a timely manner, thereby effectively preventing the product from being oxidized, reducing oxidative byproducts, and improving the product yield.
[0020] (5) The working fluid, which flows rapidly through an external circulating pump, can dilute the heat of reaction as a raw material. The heat of reaction can then be removed through a heat exchanger, which helps to maintain the temperature stability within the reaction system.
[0021] (6) The material in the secondary reaction zone inside the reactor can be radially mixed by the turbine agitator, which is conducive to the separation of oil and water phases. Gravity and air flotation promote the separation of oil and water phases. Attached Figure Description
[0022] The following figures are intended only to illustrate and explain the present invention and do not limit the scope of the present invention. Wherein:
[0023] Figure 1 This is a schematic diagram of the structural relationship of an embodiment of the present utility model;
[0024] Figure 2 This is a schematic diagram of the working fluid injector in an embodiment of this utility model;
[0025] Figure 3 This is a schematic diagram of the gas phase distributor in an embodiment of this utility model;
[0026] Figure 4 This is a schematic diagram of the state of the liquid inside the reactor.
[0027] In the diagram: 1-Reaction vessel; 2-Outer circulation pipe; 3-Turbine stirrer; 4-Circulation pump; 5-Static mixer; 6-Working fluid injector; 7-Gas phase distributor; 8-Overflow port; 9-Oil-gas-water three-phase separator; 10-Heat exchanger; 11-Main reaction zone; 12-Secondary reaction zone; 13-Overflow zone; 14-First working fluid inlet pipe; 15-Second working fluid inlet pipe; 16-Third working fluid inlet pipe; 17-Gas inlet pipe; 18-Baffle. Detailed Implementation
[0028] The present invention will be further described below with reference to the accompanying drawings and embodiments. In the following detailed description, only certain exemplary embodiments of the present invention are described by way of illustration. Undoubtedly, those skilled in the art will recognize that various modifications can be made to the described embodiments without departing from the spirit and scope of the present invention. Therefore, the drawings and description are illustrative in nature and not intended to limit the scope of the claims.
[0029] like Figure 1 As shown, the heterogeneous continuous synthesis jet external circulation reaction device includes a reactor 1, which is equipped with a stirrer 3, preferably a turbine stirrer, to facilitate radial mixing of materials in the secondary reaction zone within the reactor and to facilitate the staggered separation of oil and water phases. An external circulation pipe 2 is located at the bottom of the reactor 1, communicating with the interior of the reactor 1. A circulation pump 4 is installed on the external circulation pipe 2, which is connected to a working fluid input pipe. The working fluid input pipe includes a first working fluid input pipe 14, a second working fluid input pipe 15, and a third working fluid input pipe 16. A gas inlet pipe 17 is installed inside the reactor 1, and a gas phase distributor 7 communicating with the gas inlet pipe 17 is located at the bottom of the reactor 1. An overflow port 8 (located at 75% of the reactor's height) is located at the top of the reactor 1, and the overflow port 8 is connected to an oil-gas-water three-phase separator 9 via a discharge pipeline.
[0030] A heat exchanger 10 is installed on the outer circulation pipe 2. The working fluid, which flows rapidly through the circulating pump 4, serves as the reaction raw material and dilutes the heat of reaction. The heat exchanger 10 then removes the heat of reaction, which helps maintain a stable temperature within the reaction system. A static mixer 5 is installed on the outer circulation pipe 2 to ensure thorough mixing of the various working fluids before they enter the reactor. A working fluid injector 6, extending to the bottom of the reactor 1, is installed at the end of the outer circulation pipe 2. (Reference) Figure 2 The working fluid injector 6 can use common structures such as venturi tubes, vortex jet tubes or nozzles to achieve the injection of working fluid.
[0031] In this embodiment, a baffle 18 is provided inside the reaction vessel 1 to facilitate homogeneous mixing of the liquid and gas in the reaction vessel, making the reaction more complete and uniform.
[0032] refer to Figure 3 In this embodiment, the gas phase distributor 7 is an annular structure with several downward spray-type air distribution holes arranged along its circumference.
[0033] The continuous synthesis method using the above-mentioned apparatus specifically includes the following steps:
[0034] S1. Prepare the first working solution by mixing formamide, ammonium formate and water in a certain proportion;
[0035] S2. Dissolve disodium hydrogen phosphate and EDTA-2Na in hydrogen peroxide solution to form a second working solution;
[0036] S3. Add the first working liquid and the third working liquid (butanone) into the reactor 1 through the outer circulation pipe 2 at the bottom of the reactor 1. Turn on the turbine stirrer 3 and the circulation pump 4 to maintain the external circulation flow rate of the working liquid at 400 L / h and the stirrer speed at 700 rpm. Continuously introduce ammonia gas into the mixed working liquid in the reactor 1 at a flow rate of 2.8 M3 / h. Pump the second working liquid into the static mixer 5 at a flow rate of 30 mol / h. After the second working liquid is fully mixed with the first working liquid and the third working liquid, it is sprayed into the bottom of the reactor 1 through the working liquid injector 6 and completely back-mixed with the ammonia gas coming out through the annular gas phase distributor 7 to ensure the ammonia concentration in the reaction system.
[0037] refer to Figure 4 The bottom of reactor 1 is the main reaction zone 11, where the synthesis reaction proceeds rapidly. The methyl ethyl ketone (MEK) produced by the reaction is insoluble in water. After dissolving MEK, the MEK product floats up and separates from the aqueous phase. The product floats up in reactor 1 and enters the secondary reaction zone 12. Under the action of turbine stirrer 3, the oil and water phases mix radially. Under the action of gravity and air flotation, the oil and water phases flow upwards in a staggered manner. As the reaction proceeds, the liquid level in the reactor continues to rise, and the oil phase gradually floats up and separates from the aqueous phase, entering the overflow zone 13. The oil phase product at the top of the liquid level overflows from the overflow port 8 at the top of the reactor and enters the oil-gas-water three-phase separator 9 for separation and collection.
[0038] The above description is merely an illustrative embodiment of this utility model and is not intended to limit the scope of this utility model. For example, a baffle may be added inside the reaction vessel 1 or a spiral nozzle may be installed at the gas distribution hole. Any equivalent changes and modifications made by those skilled in the art without departing from the concept and principles of this utility model shall fall within the protection scope of this utility model.
Claims
1. A jetted outer loop reaction apparatus for heterogeneous continuous synthesis, comprising a reaction vessel, said reaction vessel provided with a stirrer; characterized in that: The bottom of the reaction kettle is provided with an outer loop pipe which is communicated with the inside of the reaction kettle, a circulating pump is arranged on the pipeline of the outer loop pipe, and a working liquid input pipe is connected to the outer loop pipe; a gas inlet pipe is arranged in the reaction kettle, and a gas phase distributor which is communicated with the gas inlet pipe is arranged at the bottom of the reaction kettle; an overflow port is arranged at the top of the reaction kettle, and the overflow port is connected to an oil-gas-water three-phase separator.
2. The jetted outer loop reaction apparatus for heterogeneous continuous synthesis of claim 1, wherein: A heat exchanger is arranged on the pipeline of the outer loop pipe.
3. The jetted outer loop reaction apparatus for heterogeneous continuous synthesis of claim 1, wherein: A static mixer is arranged on the pipeline of the outer loop pipe.
4. The jetted outer loop reaction apparatus for heterogeneous continuous synthesis of claim 1, wherein: The working liquid input pipe comprises a first working liquid input pipe, a second working liquid input pipe and a third working liquid input pipe.
5. The jetted outer loop reaction apparatus for heterogeneous continuous synthesis of claim 1, wherein: The stirrer is a turbine stirrer.
6. The jetted outer loop reaction apparatus for heterogeneous continuous synthesis of claim 1, wherein: A working liquid injector which extends into the bottom of the reaction kettle is mounted at the end of the outer loop pipe.
7. The jetted outer loop reaction apparatus for heterogeneous continuous synthesis of claim 1, wherein: A baffle is arranged in the reaction kettle.
8. The jetted outer loop reaction apparatus for heterogeneous continuous synthesis of any one of claims 1 to 7, wherein: The gas phase distributor is annular.