1, 2-dibromo-2-chloro-1, 1-difluoroethane preparation system
By designing the 1,2-dibromo-2-chloro-1,1-difluoroethane preparation system and controlling the reaction conditions with catalysts and condensers, the problems of expensive catalysts and many by-products in traditional methods are solved, and an efficient and low-cost preparation process is achieved.
Patent Information
- Application Number
- CN202422545446.4
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2024-10-22
- Publication Date
- 2025-08-26
- Estimated Expiration
- 2034-10-22
AI Technical Summary
In the prior art, the conversion process of 1,1-difluoro-1,2-dichloroethane to 1,2-dibromonabolism-2-chloro-1,1-difluoroethane requires expensive catalysts and a large amount of energy, and is accompanied by the generation of a variety of intermediates and by-products, resulting in a complex separation and purification process and high energy consumption.
A 1,2-dibromo-2-chloro-1,1-difluoroethane preparation system is adopted, including reactors, scrubber, distillation tower and other equipment. By adding catalysts such as tetrabutyl ammonium bromide and NaOH solution, the reaction temperature and condenser cooling are controlled, the reaction process is simplified, and the generation of intermediate products is reduced.
The efficient preparation of 1,2-dibromon-2-chloro-1,1-difluoroethane is achieved, which simplifies the production process, reduces the generation of intermediate products, and reduces energy consumption and production costs.
Smart Images
Figure CN223263826U_ABST
Abstract
Description
Technical Field
[0001] The utility model relates to the technical field of chemical production, in particular to a 1,2-dibromo-2-chloro-1,1-difluoroethane preparation system. Background Art
[0002] In recent years, with the increasingly stringent environmental regulations and the continuous growth of industrial demand, the demand for chemical products with low environmental impact and their preparation processes has become more urgent. Especially in the production of halogenated hydrocarbon compounds, how to synthesize the target product efficiently and environmentally friendly while reducing the generation of by-products and waste has become a research hotspot in the industry. Halogenated hydrocarbon compounds such as 1,1-difluoro-1,2-dichloroethane are widely used in many industries as refrigerants, foaming agents and solvents. By converting them into other halogenated hydrocarbons such as 1,2-dibromo-2-chloro-1,1-difluoroethane through specific chemical transformations, their application range can be further expanded and economic benefits can be improved. However, traditional methods for preparing 1,2-dibromo-2-chloro-1,1-difluoroethane often have problems such as harsh reaction conditions, low selectivity, and many by-products, which not only increase production costs but also may bring environmental pollution risks.
[0003] In the prior art, the conversion of 1,1-difluoro-1,2-dichloroethane to 1,2-dibromo-2-chloro-1,1-difluoroethane usually involves a complex multi-step reaction process, including halogen replacement, dehydrogenation, addition, and other steps. These processes often require the use of expensive catalysts and a large amount of energy, and are accompanied by the generation of various intermediates and by-products, resulting in a complex separation and purification process with high energy consumption, and the treatment of the generated by-products is relatively inconvenient. Utility Model Content
[0004] The purpose of the utility model is to provide a 1,2-dibromo-2-chloro-1,1-difluoroethane preparation system, which can avoid the problems of expensive catalysts and large amounts of energy required in the process of converting 1,1-difluoro-1,2-dichloroethane to 1,2-dibromo-2-chloro-1,1-difluoroethane, and the generation of multiple intermediates and by-products.
[0005] The utility model provides a 1,2-dibromo-2-chloro-1,1-difluoroethane preparation system, comprising:
[0006] The reactor is connected to a washing tower on one side through a pipeline, the lower end of the washing tower is connected to an intermediate tank through a pipeline, the lower end of the intermediate tank is connected to a distillation tower installed at one end through a pipeline, and the lower end of the distillation tower is provided with a fifth condenser.
[0007] Preferably, the upper end of the reactor is connected to the first condenser through a pipeline, the lower end of the first condenser is connected to the gas-liquid separation tank, and the gas-liquid separation tank and the reactor are connected through a delivery pump and a pipeline.
[0008] Preferably, the reaction temperature of the reactor is controlled at 40-50°C, and the cooling temperature of the first condenser is 10-30°C.
[0009] Preferably, the top of the washing tower is connected to the third condenser through a pipeline, and the lower end of the third condenser is connected to the first reflux tank through a pipeline.
[0010] Preferably, the bottom of the washing tower is connected to a second condenser for re-cooling the bottom material through a pipeline, and the second condenser is connected to the first section of the washing tower through a pipeline.
[0011] Preferably, the temperature inside the washing tower is an exothermic reaction, and the temperature is controlled at 30-40° C. by the cooling capacity of the second condenser and the third condenser.
[0012] Preferably, the lower end of the reactor is connected to a double-effect evaporator, and the lower end of the double-effect evaporator is connected to the reactor again through a pipeline to form a loop.
[0013] Preferably, the lower end of the distillation tower is connected to a reboiler, and the upper end of the reboiler is connected to the distillation tower again through a pipeline.
[0014] Preferably, a fourth condenser is installed on one side of the distillation tower, and the material inside the fourth condenser is connected to the second reflux tank at the lower end through a pipeline.
[0015] The present invention provides a system for preparing 1,2-dibromo-2-chloro-1,1-difluoroethane. A catalyst, such as tetrabutylammonium bromide, is added to a reactor. A 10% NaOH solution is then added, followed by a certain amount of 1,1-difluoro-1,2-dichloroethane. The gaseous material 1,1-difluoro-2-chloroethylene generated inside the reactor is connected to the third section of a washing tower for feeding and washing. The material at the bottom of the washing tower reacts fully, and after the internal bromine content is tested and found to be qualified, it enters an intermediate tank. The material in the intermediate tank is sent to a distillation tower. The 1,2-dibromo-2-chloro-1,1-difluoroethane generated at the bottom of the distillation tower is cooled and then temporarily stored. 1,2-dibromo-2-chloro-1,1-difluoroethane can be prepared from 1,1-difluoro-1,2-dichloroethane. The process is simple, and no large number of intermediate products are generated, which facilitates production and processing. BRIEF DESCRIPTION OF THE DRAWINGS
[0016] In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the following is a brief introduction to the drawings required for use in the embodiments. It should be understood that the following drawings only show certain embodiments of the present invention and therefore should not be regarded as limiting the scope. For ordinary technicians in this field, other relevant drawings can be obtained based on these drawings without creative work.
[0017] Figure 1 This is a schematic diagram of the overall process structure of an embodiment of the present utility model.
[0018] Description of the drawings: 100, reactor; 110, first condenser; 200, gas-liquid separation tank; 300, washing tower; 310, third condenser; 320, second condenser; 400, first reflux tank; 500, intermediate tank; 600, distillation tower; 610, fourth condenser; 620, fifth condenser; 700, second reflux tank; 800, double-effect evaporator; 900, reboiler. DETAILED DESCRIPTION
[0019] Hereinafter, only certain exemplary embodiments are briefly described. As will be appreciated by those skilled in the art, the described embodiments may be modified in various ways without departing from the spirit or scope of the embodiments of the present invention. Therefore, the drawings and description are to be regarded as illustrative in nature and not restrictive.
[0020] In the description of the embodiments of the present invention, it should be understood that the terms "length", "vertical", "horizontal", "top", "bottom", etc. indicating the orientation or position relationship are based on the orientation or position relationship shown in the accompanying drawings, and are only for the convenience of describing the embodiments of the present invention 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 on the embodiments of the present invention.
[0021] Furthermore, the terms "first" and "second" are used for descriptive purposes only and should not be understood to indicate or imply relative importance or implicitly specify the number of the technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of the features. In the description of the embodiments of the present invention, "plurality" means two or more, unless otherwise specifically defined.
[0022] In the embodiments of the present invention, unless otherwise expressly specified or limited, the terms "installed," "connected," "connected," "fixed," etc. should be understood in a broad sense. For example, they can refer to fixed connection, detachable connection, or integration; mechanical connection, electrical connection, or communication; direct connection or indirect connection through an intermediate medium; internal communication between two components or interaction between two components. Those skilled in the art will understand the specific meanings of the above terms in the embodiments of the present invention based on specific circumstances.
[0023] The disclosure below provides many different embodiments or examples for implementing different structures of the embodiments of the present invention. In order to simplify the disclosure of the embodiments of the present invention, the components and settings of specific examples are described below. Of course, these are merely examples and are not intended to limit the embodiments of the present invention. In addition, the embodiments of the present invention may repeat reference numbers and / or reference letters in different examples. Such repetition is for the purpose of simplicity and clarity and does not in itself indicate the relationship between the various embodiments and / or settings discussed.
[0024] In order to better understand the purpose, structure and function of the present invention, the following is a further detailed description of a 1,2-dibromo-2-chloro-1,1-difluoroethane preparation system of the present invention in conjunction with the accompanying drawings.
[0025] like Figure 1 As shown, an embodiment of the present invention provides a 1,2-dibromo-2-chloro-1,1-difluoroethane preparation system, including a reactor 100 for preliminary processing of raw materials, a washing tower 300 is connected to one side of the reactor 100 through a pipeline, the lower end of the washing tower 300 is connected to an intermediate tank 500 for temporarily storing the bottom material through a pipeline, the lower end of the intermediate tank 500 is connected to a distillation tower 600 installed at one end through a pipeline, and the lower end of the distillation tower 600 is provided with a fifth condenser 620 for cooling the bottom material of the distillation tower 600.
[0026] A catalyst, such as tetrabutylammonium bromide, is added to the reactor 100, followed by a 10% NaOH solution and a certain amount of 1,1-difluoro-1,2-dichloroethane. The gaseous material 1,1-difluoro-2-chloroethylene generated in the reactor 100 is connected to the third section of the washing tower 300 for feeding and washing. The material at the bottom of the washing tower 300 reacts fully and enters the intermediate tank 500 after the internal bromine content is tested to be qualified. The material in the intermediate tank 500 is sent to the distillation tower 600. The 1,2-dibromo-2-chloro-1,1-difluoroethane generated at the bottom of the distillation tower 600 is cooled and temporarily stored. 1,2-dibromo-2-chloro-1,1-difluoroethane can be prepared from 1,1-difluoro-1,2-dichloroethane. The process is simple, and no large number of intermediate products are generated, which facilitates production and processing.
[0027] Furthermore, the upper end of the reactor 100 is connected to the first condenser 110 through a pipeline for condensing the gas phase inside the reactor 100. The lower end of the first condenser 110 is connected to the gas-liquid separation tank 200. The gas-liquid separation tank 200 is connected to the reactor 100 through a delivery pump and a pipeline. The reactor 100 cools the generated material through the first condenser 110, while the 1,1-difluoro-2-chloroethylene in the material will not be condensed. The evaporated 1,1-difluoro-1,2-dichloroethane will be condensed and enter the gas-liquid separation tank 200. The liquid phase 1,1-difluoro-1,2-dichloroethane inside the gas-liquid separation tank 200 is returned to the reactor 100 for reaction, so that the 1,1-difluoro-1,2-dichloroethane product can be recycled and reused, saving costs and facilitating product generation.
[0028] Furthermore, the reaction temperature of the reactor 100 is controlled at 40-50°C, and the cooling temperature of the first condenser 110 is controlled at 10-30°C.
[0029] Furthermore, the top of the washing tower 300 is connected to the third condenser 310 through a pipeline, and the lower end of the third condenser 310 is connected to the first reflux tank 400 through a pipeline. A pipeline for adding a quantitative amount of bromine is also provided on one side of the first reflux tank 400, and is connected to the bromine supply pipeline. The gas phase at the top of the washing tower 300 enters the first reflux tank 400 after condensation through the third condenser 310, and a quantitative amount of bromine is added to the first reflux tank 400. The gas phase enters the second stage of the washing tower 300 through the reflux pump to participate in the reaction, so as to facilitate the recycling of the material inside the gas phase and avoid the generation of other excess products.
[0030] Furthermore, the bottom of the washing tower 300 is connected to a second condenser 320 for re-cooling the bottom material through a pipeline. The second condenser 320 is connected to a section of the washing tower 300 through a pipeline, and the bottom material of the washing tower 300 is re-condensed and then put into the washing tower 300 for re-washing.
[0031] Furthermore, the temperature inside the washing tower 300 is an exothermic reaction, and the temperature is controlled at 30-40° C. by the cooling capacity of the second condenser 320 and the third condenser 310 .
[0032] Furthermore, the lower end of the reactor 100 is connected to a double-effect evaporator 800, and the upper end of the double-effect evaporator 800 is installed with a pipeline for adding hydrochloric acid solution, and is connected to the liquid supply part. The lower end of the double-effect evaporator 800 is connected to the reactor 100 through a pipeline. After the reaction in the reactor 100 is complete, the excess alkali liquid at the bottom of the reactor 100 enters the double-effect evaporator 800 for concentration and recovery, and part of the concentrated liquid is added with hydrochloric acid solution for neutralization. Double-effect evaporation is carried out, water is recovered, and sodium chloride salt can be sold and entrusted to a third party for processing to increase profits.
[0033] Furthermore, a reboiler 900 is connected to the lower end of the distillation tower 600 to provide the necessary heat for the distillation tower 600, so that the liquid at the bottom of the tower is partially vaporized, and it helps to achieve the separation of light and heavy components. The heavy components remain more in the liquid and eventually accumulate at the bottom of the tower. At the same time, the steam generated provides the required upward air flow in the tower. The upper end of the reboiler 900 is connected to the distillation tower 600 again through a pipeline to transport the steam.
[0034] Furthermore, a fourth condenser 610 for cooling the internal material is installed on one side of the distillation tower 600. The internal material of the fourth condenser 610 is connected to the second reflux tank 700 at the lower end through a pipeline. The second reflux tank 700 returns the condensed 1,1-difluoro-1,2-dichloroethane to the reactor 100 through the pipeline for reaction, so as to facilitate the recovery and reuse of 1,1-difluoro-1,2-dichloroethane.
[0035] The working principle of a 1,2-dibromo-2-chloro-1,1-difluoroethane preparation system is as follows: a catalyst, such as tetrabutylammonium bromide, is added into a reactor 100, followed by a 10% NaOH solution and a certain amount of 1,1-difluoro-1,2-dichloroethane. The gaseous material 1,1-difluoro-2-chloroethylene generated in the reactor 100 is connected to the third section of a washing tower 300 for feeding and washing. The material at the bottom of the washing tower 300 reacts fully and enters an intermediate tank 500 after being tested for qualified bromine content. The material in the intermediate tank 500 is sent to a distillation tower 600. The 1,2-dibromo-2-chloro-1,1-difluoroethane generated at the bottom of the distillation tower 600 is cooled and temporarily stored. 1,2-dibromo-2-chloro-1,1-difluoroethane can be prepared from 1,1-difluoro-1,2-dichloroethane. The process is simple, and no large number of intermediate products are generated, making production and processing convenient.
[0036] It is understood that the present invention is described by way of certain embodiments, and those skilled in the art will appreciate that various changes or equivalent substitutions may be made to these features and embodiments without departing from the spirit and scope of the present invention. Furthermore, under the guidance of the present invention, these features and embodiments may be modified to suit specific circumstances and materials without departing from the spirit and scope of the present invention. Therefore, the present invention is not limited to the specific embodiments disclosed herein, and all embodiments falling within the scope of the claims of this application are intended to be protected by the present invention.
Claims
1. A system for preparing 1,2-dibromo-2-chloro-1,1-difluoroethane, characterized in that: include: A reactor (100) is provided, wherein one side of the reactor (100) is connected to a washing tower (300) via a pipeline, the lower end of the washing tower (300) is connected to an intermediate tank (500) via a pipeline, the lower end of the intermediate tank (500) is connected to a distillation tower (600) installed at one end via a pipeline, and a fifth condenser (620) is provided at the lower end of the distillation tower (600).
2. A 1,2-dibromo-2-chloro-1,1-difluoroethane preparation system according to claim 1, characterized in that: The upper end of the reactor (100) is connected to the first condenser (110) through a pipeline, the lower end of the first condenser (110) is connected to the gas-liquid separation tank (200), and the gas-liquid separation tank (200) and the reactor (100) are connected through a delivery pump and a pipeline.
3. A 1,2-dibromo-2-chloro-1,1-difluoroethane preparation system according to claim 2, characterized in that: The reaction temperature of the reactor (100) is controlled at 40-50°C, and the cooling temperature of the first condenser (110) is 10-30°C.
4. A 1,2-dibromo-2-chloro-1,1-difluoroethane preparation system according to claim 3, characterized in that: The top of the washing tower (300) is connected to the third condenser (310) through a pipeline, and the lower end of the third condenser (310) is connected to the first reflux tank (400) through a pipeline.
5. A 1,2-dibromo-2-chloro-1,1-difluoroethane preparation system according to claim 4, characterized in that: The bottom of the washing tower (300) is connected to a second condenser (320) for re-cooling the bottom material through a pipeline, and the second condenser (320) is connected to a first section of the washing tower (300) through a pipeline.
6. A system for preparing 1,2-dibromo-2-chloro-1,1-difluoroethane according to claim 5, characterized in that: The internal temperature of the washing tower (300) is an exothermic reaction, and the temperature is controlled at 30-40°C by the cooling capacity of the second condenser (320) and the third condenser (310).
7. A system for preparing 1,2-dibromo-2-chloro-1,1-difluoroethane according to claim 6, characterized in that: The lower end of the reactor (100) is connected to a double-effect evaporator (800), and the lower end of the double-effect evaporator (800) is connected to the reactor (100) again through a pipeline to form a loop.
8. A system for preparing 1,2-dibromo-2-chloro-1,1-difluoroethane according to claim 7, characterized in that: The lower end of the distillation tower (600) is connected to a reboiler (900), and the upper end of the reboiler (900) is connected to the distillation tower (600) again through a pipeline.
9. A system for preparing 1,2-dibromo-2-chloro-1,1-difluoroethane according to claim 8, characterized in that: A fourth condenser (610) is installed on one side of the distillation tower (600), and the material inside the fourth condenser (610) is connected to the second reflux tank (700) at the lower end through a pipeline.