1, 1, 2-tribromo-1-chloro-2, 2-difluoroethane preparation system
A novel system for producing 1,1,2-tribromo-1-chloro-2,2-difluoroethane addresses the challenges of high-pressure and costly catalyst requirements in traditional methods by optimizing the production process with controlled temperature and pressure conditions, achieving improved yield and selectivity.
Patent Information
- Application Number
- CN202421943885.4
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2024-08-12
- Publication Date
- 2025-07-15
- Estimated Expiration
- 2034-08-12
AI Technical Summary
In the prior art, the process of preparing 1,1,2-tribromo-1-chloro-2,2-difluoroethane requires high temperature and high pressure conditions, and the use of expensive catalysts is limited in yield and selectivity, the raw material cost is too high, and production is inconvenient.
The combined process of elimination reactor, addition reactor, distillation column and bromine recovery system is adopted to achieve efficient preparation of 1,1,2-tribromo-1-chloro-2,2-difluoroethane by controlling the reaction temperature and distillation process, using inexpensive catalysts such as tetrabutylammonium bromide, and performing multiple distillations to improve purity.
It realizes the efficient preparation of high-purity 1,1,2-tribromo-1-chloro-2,2-difluoroethane at room temperature and pressure, reducing production costs, simplifying the process, and improving yield and selectivity.
Smart Images
Figure CN223096777U_ABST
Abstract
Description
Technical Field
[0001] The utility model relates to the technical field of chemical production, in particular to a preparation system for 1,1,2 - tribromo - 1 - chloro - 2,2 - difluoroethane. Background Technique
[0002] 1,1,2 - tribromo - 1 - chloro - 2,2 - difluoroethane (C2HBr3ClF2), commonly known as Halon 1211, is a halogenated hydrocarbon that was once widely used as a fire extinguishing agent. The traditional method for preparing Halon 1211 is completed through multiple - step reactions, mainly involving halogen exchange and halogenation reactions. CBr3ClF2 is an important organic intermediate and is widely used in the synthesis of pharmaceuticals, pesticides, and new materials.
[0003] In the prior art, the preparation of target compounds is usually carried out through multiple - step reactions of halogenated hydrocarbons. These processes often require high - temperature and high - pressure conditions, use expensive catalysts, and have limited yields and selectivities, with excessively high raw material costs and inconvenient production. Summary of the Utility Model
[0004] The purpose of the utility model is to provide a preparation system for 1,1,2 - tribromo - 1 - chloro - 2,2 - difluoroethane, which can avoid the problems that the preparation process of halogenated hydrocarbons often requires high - temperature and high - pressure conditions, uses expensive catalysts, has limited yields and selectivities, and has excessively high raw material costs and inconvenient production.
[0005] The utility model provides a preparation system for 1,1,2 - tribromo - 1 - chloro - 2,2 - difluoroethane, comprising:
[0006] An elimination reactor, a buffer storage tank is installed at the upper end of the elimination reactor through a pipeline. The material at the bottom of the buffer storage tank is connected to an addition reactor through a pipeline connected by a delivery pump at the lower end. One side of the addition reactor is connected to an intermediate tank through a pipeline. The discharge end of the intermediate tank is connected to a first rectification column through a pipeline. One side of the first rectification column is connected to a vacuum rectification column. The lower end of the vacuum rectification column is connected to a material collection part through a pipeline.
[0007] Preferably, the top of the vacuum rectification column is connected to a third condenser through a pipeline. The discharge end of the third condenser is connected to a second reflux tank through a pipeline. The bottom of the second reflux tank is connected to the vacuum rectification column through a delivery pump.
[0008] Preferably, a stirring device is installed in the inner cavity of the addition reactor, and the reaction temperature in the inner cavity is controlled at 20 - 25 °C.
[0009] Preferably, the top of the first rectification column is connected to a second condenser through a pipeline. The lower end of the second condenser is connected to a first reflux tank. Two pipelines are arranged at the lower end of the first reflux tank. One pipeline is connected to a buffer storage tank, and the other pipeline is connected to the first rectification column.
[0010] Preferably, the bottom of the vacuum rectification column generates side reaction heavy components, and the heavy components are transported outwards through a pump installed at the bottom.
[0011] Preferably, the bottom material of the elimination reactor is connected to a filter press through a transfer pump. The filter press is connected to the MVR evaporator control system through a pipeline, and the MVR evaporator control system is connected to the bromine recovery system through a pipeline.
[0012] Preferably, the internal reaction condition of the bromine recovery system is an acidic condition, and another pipeline is connected to the MVR evaporator control system again.
[0013] Preferably, the product pipeline of the bromine recovery system is connected to a bromine recovery tank and is connected to an addition reactor to supply materials for it.
[0014] Preferably, the gas phase at the top of the elimination reactor is transported to a first condenser through a pipeline for condensation, and the first condenser is connected to a buffer storage tank.
[0015] Preferably, reboilers are arranged at the lower ends of the first rectification column and the vacuum rectification column to provide heat and upward gas flow for the first rectification column and the vacuum rectification column.
[0016] A preparation system for 1,1,2-tribromo-1-chloro-2,2-difluoroethane provided by an embodiment of the present invention adds a catalyst, such as tetrabutylammonium bromide, etc., to an elimination reactor, then adds a 10% NaOH solution, quantitatively adds 1,2-dibromo-1-chloro-2,2-difluoroethane, controls the reaction temperature at 55 - 60 °C, and the generated 1-bromo-1-chloro-2,2-difluoroethylene enters a buffer storage tank. The material at the bottom of the buffer storage tank is transported to an addition reactor through a transfer pump. After the bromine in the addition reactor fades, the reaction solution is heated to 70 - 80 °C and transferred to an intermediate tank for storage. The crude 1,1,2-tribromo-1-chloro-2,2-difluoroethane in the intermediate tank is sent to a first rectification column for rectification. 1-bromo-1-chloro-2,2-difluoroethylene is taken out from the top of the first rectification column, and the high-purity 1,1,2-tribromo-1-chloro-2,2-difluoroethane and heavy components taken out from the bottom of the first rectification column are sent to a vacuum rectification column for secondary rectification. High-purity 1,1,2-tribromo-1-chloro-2,2-difluoroethane is distilled out from the top of the vacuum rectification column, which is convenient for preparing 1,1,2-tribromo-1-chloro-2,2-difluoroethane from 1,2-dibromo-1-chloro-2,2-difluoroethane. The process is simple and the cost is relatively low. Description of the Drawings
[0017] To more clearly illustrate the technical solutions of the embodiments of the present utility model, the accompanying drawings required for the embodiments will be briefly introduced below. It should be understood that the following accompanying drawings only show some embodiments of the present utility model, and therefore should not be regarded as a limitation of the scope. For those of ordinary skill in the art, without creative efforts, other relevant accompanying drawings can also be obtained based on these drawings.
[0018] Figure 1 It is a schematic diagram of the overall system of the embodiment of the present utility model.
[0019] Description of the drawings: 100, elimination reactor; 110, first condenser; 120, buffer storage tank; 130, filter press; 140, MVR evaporator control system; 150, bromine recovery system; 200, addition reactor; 210, intermediate tank; 300, first distillation column; 310, second condenser; 320, first reflux tank; 400, vacuum distillation column; 410, third condenser; 420, second reflux tank; 430, vacuum pumping system. Detailed embodiments
[0020] In the following text, only some exemplary embodiments are simply described. As those skilled in the art can recognize, the described embodiments can be modified in various different ways without departing from the spirit or scope of the embodiments of the present utility model. Therefore, the accompanying drawings and the description are considered to be exemplary in nature rather than restrictive.
[0021] In the description of the embodiments of the present utility model, it should be understood that the orientation or positional relationships indicated by the terms "length", "vertical", "horizontal", "top", "bottom", etc. are based on the orientation or positional relationships shown in the accompanying drawings. It is only for the convenience of describing the embodiments of the present utility model and simplifying the description, rather than indicating or implying that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore cannot be understood as a limitation of the embodiments of the present utility model.
[0022] In addition, the terms "first" and "second" are only used for descriptive purposes and cannot be understood as indicating or implying relative importance or implicitly indicating the quantity of the indicated technical features. Thus, the features defined with "first" and "second" may explicitly or implicitly include one or more of such features. In the description of the embodiments of the present utility model, the meaning of "a plurality" is two or more unless otherwise specifically defined.
[0023] In the embodiments of the present utility model, unless otherwise clearly specified and defined, terms such as "installation", "connection", "linkage", "fixation", etc. shall be understood in a broad sense. For example, it may be a fixed connection, a detachable connection, or integrated; it may be a mechanical connection, an electrical connection, or a communication connection; it may be directly connected, or indirectly connected through an intermediate medium, and may be the communication inside two components or the interaction relationship between two components. For those of ordinary skill in the art, the specific meanings of the above terms in the embodiments of the present utility model can be understood according to specific circumstances.
[0024] The following disclosure provides many different embodiments or examples for implementing different structures of the embodiments of the present utility model. To simplify the disclosure of the embodiments of the present utility model, the components and settings of specific examples are described below. Of course, they are only examples and are not intended to limit the embodiments of the present utility model. In addition, the embodiments of the present utility model may repeat reference numerals and / or reference letters in different examples. This repetition is for the purpose of simplification and clarity, and does not itself indicate the relationship between the various embodiments and / or settings discussed.
[0025] To better understand the purpose, structure and function of the present utility model, the following further describes in detail a preparation system for 1,1,2-tribromo-1-chloro-2,2-difluoroethane of the present utility model with reference to the accompanying drawings.
[0026] As Figure 1 shown, the embodiments of the present utility model provide a preparation system for 1,1,2-tribromo-1-chloro-2,2-difluoroethane, including an elimination reactor 100. A buffer storage tank 120 for temporarily storing the generated 1-bromo-1-chloro-2,2-difluoroethylene is installed at the upper end of the elimination reactor 100 through a pipeline. The material at the bottom of the buffer storage tank 120 is connected to an addition reactor 200 through a delivery pump and a pipeline connected to the lower end. One side of the addition reactor 200 is connected to an intermediate tank 210 for storing intermediate materials through a pipeline. The discharge end of the intermediate tank 210 is connected to a first rectification column 300 through a pipeline. One side of the first rectification column 300 is connected to a vacuum rectification column 400. The lower end of the vacuum rectification column 400 is connected to a material collection part through a pipeline.
[0027] A catalyst is added into the elimination reactor 100, and then a 10% NaOH solution is added. 1,2-Dibromo-1-chloro-2,2-difluoroethane is added quantitatively. The reaction temperature is controlled at 55 - 60 °C. The generated 1-bromo-1-chloro-2,2-difluoroethylene enters the buffer storage tank 120. The substances at the bottom of the buffer storage tank 120 are transported to the addition reactor 200 through a transfer pump. After the bromine element fades in the addition reactor 200, the reaction solution is heated to 70 - 80 °C and transferred to the intermediate tank 210 for storage. The crude 1,1,2-tribromo-1-chloro-2,2-difluoroethane in the intermediate tank 210 is sent to the first distillation column 300 for distillation. 1-bromo-1-chloro-2,2-difluoroethylene is taken out from the top of the first distillation column 300, and the high-purity 1,1,2-tribromo-1-chloro-2,2-difluoroethane and the heavy components taken out from the bottom of the first distillation column 300 are sent to the vacuum distillation column 400 for secondary distillation. High-purity 1,1,2-tribromo-1-chloro-2,2-difluoroethane is distilled out from the top of the vacuum distillation column 400, and the heavy components are taken out from the bottom. This method is convenient for preparing 1,1,2-tribromo-1-chloro-2,2-difluoroethane from 1,2-dibromo-1-chloro-2,2-difluoroethane, with a simple process and low cost.
[0028] The top of the vacuum distillation column 400 is connected to a third condenser 410 through a pipeline. The discharge end of the third condenser 410 is connected to a second reflux tank 420 through a pipeline. The bottom of the second reflux tank 420 is connected to the vacuum distillation column 400 through a transfer pump, and another pipeline connects the internal material collection part. The third condenser 410 is connected to a vacuum pumping system 430 through a pipeline. High-purity 1,1,2-tribromo-1-chloro-2,2-difluoroethane distilled out from the top of the vacuum distillation column 400 is sent to the third condenser 410 for condensation. The third condenser 410 is connected to the second reflux tank 420 at the lower end. The second reflux tank 420 transports the finished product 1,1,2-tribromo-1-chloro-2,2-difluoroethane, and a part of the 1,1,2-tribromo-1-chloro-2,2-difluoroethane is sent back to the vacuum distillation column 400 for circulation. The third condenser 410 is connected to the vacuum pumping system 430.
[0029] A stirring device for stirring the materials is installed in the inner cavity of the addition reactor 200, and the reaction temperature in the inner cavity is controlled at 20 - 25 °C. Stirring cannot stop during the reaction until the bromine element fades, which is convenient for the progress of the reaction.
[0030] The top of the first rectification column 300 is connected by a pipeline to a second condenser 310 for condensing the gas phase at the top of the column. The lower end of the second condenser 310 is connected to a first reflux drum 320. The lower end of the first reflux drum 320 is provided with two groups of pipelines. One group of pipelines is connected to the buffer storage tank 120, and the other group of pipelines is connected to the first rectification column 300. Part of the 1-bromo-1-chloro-2,2-difluoroethylene coming out from the top of the first rectification column 300 is used as reflux, and the other part is returned to the buffer storage tank 120 for use.
[0031] Heavy by-products are generated at the bottom of the vacuum rectification column 400, and the heavy by-products are transported out through the pump installed at the bottom for sale, recovery and incineration or entrusted to a third party for treatment.
[0032] The bottom material of the elimination reactor 100 is connected to a filter press 130 through a transfer pump. The filter press 130 is connected to the MVR evaporator control system 140 through a pipeline. The MVR evaporator control system 140 is connected to the bromine recovery system 150 through a pipeline. After the reaction in the elimination reactor 100 is completed, the gel, sodium bromide solution and excess NaOH solution inside the elimination reactor 100 are transferred to the filter press 130. The filter cake generated inside the filter press 130 is entrusted to a third party, and the filtrate of the filter press 130 enters the MVR evaporator control system 140. The high-concentration sodium bromide solution after evaporation in the MVR evaporator control system 140 enters the bromine recovery system 150, and the precipitated salt is entrusted to a third party for treatment.
[0033] The reaction conditions inside the bromine recovery system 150 are acidic conditions, and there is another pipeline connected to the MVR evaporator control system 140 again. The high-concentration sodium bromide solution inside the bromine recovery system 150 is added with the filtrate, and the excess NaOH inside the bromine recovery system 150 is neutralized. The residual liquid after bromine recovery returns to the MVR evaporator control system 140 for concentration, centrifugation, and the recovered distilled water is recycled.
[0034] The outlet pipeline of the bromine recovery system 150 is connected to a bromine recovery tank and is also connected to the addition reactor 200 to supply materials for it. The bromine generated by the bromine recovery system 150 returns to the bromine storage tank for reuse by the addition reactor 200, saving costs and recycling.
[0035] The gas phase at the top of the elimination reactor 100 is transported through a pipeline to the first condenser 110 for condensation. The first condenser 110 is connected to the buffer storage tank 120 to ensure a cooling temperature of 10 - 30 °C to enable the reaction to proceed normally.
[0036] Reboilers are arranged at the lower ends of the first rectification column 300 and the vacuum rectification column 400 to provide heat and upward gas flow for the first rectification column 300 and the vacuum rectification column 400.
[0037] Working principle of a preparation system for 1,1,2-tribromo-1-chloro-2,2-difluoroethane: Add a catalyst, such as tetrabutylammonium bromide, etc., into the elimination reactor 100, then add 10% NaOH solution, quantitatively add 1,2-dibromo-1-chloro-2,2-difluoroethane, control the reaction temperature at 55 - 60 °C. The generated 1-bromo-1-chloro-2,2-difluoroethylene enters the buffer storage tank 120. The substances at the bottom of the buffer storage tank 120 are transported to the addition reactor 200 through a delivery pump. After the bromine in the addition reactor 200 fades, the reaction solution is heated to 70 - 80 °C and transferred to the intermediate tank 210 for storage. The crude 1,1,2-tribromo-1-chloro-2,2-difluoroethane in the intermediate tank 210 is sent to the first distillation column 300 for distillation. High-purity 1,1,2-tribromo-1-chloro-2,2-difluoroethane is drawn from the bottom of the first distillation column 300. The high-purity 1,1,2-tribromo-1-chloro-2,2-difluoroethane drawn from the bottom of the first distillation column 300 is sent to the vacuum distillation column 400 for secondary distillation. High-purity 1,1,2-tribromo-1-chloro-2,2-difluoroethane is distilled out from the top of the vacuum distillation column 400, which is convenient for preparing 1,1,2-tribromo-1-chloro-2,2-difluoroethane from 1,2-dibromo-1-chloro-2,2-difluoroethane. The process is simple and the cost is relatively low.
[0038] It can be understood that the present utility model is described through some embodiments. As is known to those skilled in the art, without departing from the spirit and scope of the present utility model, various changes or equivalent replacements can be made to these features and embodiments. Additionally, under the teaching of the present utility model, these features and embodiments can be modified to adapt to specific situations and materials without departing from the spirit and scope of the present utility model. Therefore, the present utility model is not limited by the specific embodiments disclosed herein, and all embodiments falling within the scope of the claims of this application belong to the scope protected by the present utility model.
Claims
1. A preparation system for 1,1,2-tribromo-1-chloro-2,2-difluoroethane, characterized in that, Including: An elimination reactor, the upper end of the elimination reactor is installed with a buffer storage tank through a pipeline, the material at the bottom of the buffer storage tank is connected with an addition reactor through a delivery pump and a pipeline connected to the lower end, one side of the addition reactor is connected with an intermediate tank through a pipeline, the discharge end of the intermediate tank is connected with a first rectification column through a pipeline, one side of the first rectification column is connected with a vacuum rectification column, and the lower end of the vacuum rectification column is connected with a material collection part through a pipeline.
2. The preparation system of 1,1,2-tribromo-1-chloro-2,2-difluoroethane according to claim 1, characterized in that, The top of the vacuum rectification column is connected with a third condenser through a pipeline, the discharge end of the third condenser is connected with a second reflux tank through a pipeline, and the bottom of the second reflux tank is connected with the vacuum rectification column through a delivery pump.
3. The preparation system of 1,1,2-tribromo-1-chloro-2,2-difluoroethane according to claim 2, characterized in that, A stirring device is installed in the inner cavity of the addition reactor, and the reaction temperature in the inner cavity is controlled at 20 - 25 °C.
4. The preparation system of 1,1,2-tribromo-1-chloro-2,2-difluoroethane according to claim 3, characterized in that, The top of the first rectification column is connected with a second condenser through a pipeline, the lower end of the second condenser is connected with a first reflux tank, and two groups of pipelines are arranged at the lower end of the first reflux tank, one group of pipelines is connected with the buffer storage tank, and the other group of pipelines is connected with the first rectification column.
5. A preparation system for 1,1,2-tribromo-1-chloro-2,2-difluoroethane according to claim 4, characterized in that, Side reaction heavy components are generated at the bottom of the vacuum rectification column, and the heavy components are transported outwards through a pump body installed at the bottom.
6. The preparation system of 1,1,2-tribromo-1-chloro-2,2-difluoroethane according to claim 5, characterized in that, The material at the bottom of the elimination reactor is connected with a filter press through a delivery pump, the filter press is connected with an MVR evaporator control system through a pipeline, and the MVR evaporator control system is connected with a bromine recovery system through a pipeline.
7. The preparation system of 1,1,2-tribromo-1-chloro-2,2-difluoroethane according to claim 6, characterized in that, The internal reaction condition of the bromine recovery system is an acidic condition, and there is another pipeline connected with the MVR evaporator control system again.
8. A preparation system for 1,1,2-tribromo-1-chloro-2,2-difluoroethane according to claim 7, characterized in that, The product pipeline of the bromine recovery system is connected with a bromine recovery tank, and is connected with the addition reactor to supply materials for it.
9. A preparation system for 1,1,2-tribromo-1-chloro-2,2-difluoroethane according to claim 8, characterized in that, The gas phase at the top of the elimination reactor is transported to a first condenser through a pipeline for condensation, and the first condenser is connected with the buffer storage tank.
10. A preparation system for 1,1,2-tribromo-1-chloro-2,2-difluoroethane according to claim 9, characterized in that, Reboilers are arranged at the lower ends of the first rectification column and the vacuum rectification column, which are used to provide heat and upward gas flow for the first rectification column and the vacuum rectification column.