A system for the preparation of dimethylcarbamoyl chloride
By optimizing the reaction process and equipment configuration of the dimethylcarbamoyl chloride preparation system, and by using equipment such as synthesis kettles, light-removing kettles, and distillation columns, the problems of harsh reaction conditions and complex operation in the existing preparation process have been solved, resulting in shorter reaction time and higher product yield.
Patent Information
- Application Number
- CN202521783074.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2025-08-21
- Publication Date
- 2026-07-24
- Estimated Expiration
- 2035-08-21
AI Technical Summary
Existing processes for preparing dimethylcarbamoyl chloride suffer from problems such as harsh reaction conditions, complex operation, and large wastewater volume.
The reaction process and equipment configuration were optimized by adopting a preparation system consisting of a synthesis kettle, a photoluminescence removal kettle, a distillation column, a distillation vacuum pump, a phosgene synthesis device, and a dimethylamine buffer tank. Hydrogen chloride gas and phosgene were removed by a separate photoluminescence removal kettle between the synthesis kettle and the distillation column, and the purification was changed to distillation, reducing the operation directly in the distillation column.
The reaction time is greatly shortened, the product yield is increased, and the product quality and purity are improved.
Smart Images
Figure CN224541743U_ABST
Abstract
Description
Technical Field
[0001] This utility model relates to the field of cement production technology, and more specifically, to a system for preparing dimethylcarbamoyl chloride. Background Technology
[0002] Dimethylcarbamoyl chloride is an important chemical raw material widely used in pharmaceuticals, pesticides, and other fields. Existing processes for preparing dimethylcarbamoyl chloride mostly involve the reaction of phosgene with dimethylamine, but these processes suffer from harsh reaction conditions and complex operations. Therefore, developing a highly efficient, environmentally friendly, and easy-to-operate system for preparing dimethylcarbamoyl chloride is of great significance. Utility Model Content
[0003] This application provides a system for the preparation of dimethylcarbamoyl chloride, which solves the problems of existing dimethylcarbamoyl chloride preparation processes that mostly use phosgene to react with dimethylamine, but have harsh reaction conditions, complex operation, and large wastewater volume.
[0004] This application provides a system for preparing dimethylcarbamoyl chloride, including a synthesis vessel, a phosgene-reducing vessel, a distillation column, a distillation vacuum pump, a phosgene synthesis device, and a dimethylamine buffer tank; The phosgene synthesis apparatus is connected to a phosgene heater, the dimethylamine buffer tank is connected to a dimethylamine heater, the phosgene heater and the dimethylamine heater are respectively connected to the synthesis reactor via pipelines, the synthesis reactor is connected to a primary synthesis condenser, the primary synthesis condenser is connected to a secondary synthesis condenser, the liquid outlets of the primary synthesis condenser and the secondary synthesis condenser are connected to the synthesis reactor, the discharge pipe of the synthesis reactor is connected to the feed inlet of the phosgene-removing reactor, the phosgene-removing reactor is connected to a phosgene-removing condenser, and the discharge outlet of the phosgene-removing reactor is connected to the distillation column; The bottom outlet of the distillation column is connected to a fraction tank, the middle outlet of the distillation column is connected to a product tank, the top outlet of the distillation column is connected to a first-stage distillation condenser, the first-stage distillation condenser is connected to a second-stage distillation condenser, the first-stage distillation condenser and the second-stage distillation condenser are connected to the product tank and the fraction tank through pipelines, the second-stage distillation condenser is connected to a distillation vacuum buffer tank, and the distillation vacuum buffer tank is connected to the distillation vacuum pump.
[0005] Preferably, the distillation vacuum pump is equipped with a vacuum pump cooler, the distillation vacuum pump is provided with a cooling water pipe, the distillation vacuum pump is connected to a water supply pipe, and the outlet of the distillation vacuum pump is connected to an acidic tail gas outlet pipe.
[0006] Preferably, the synthesis vessel, the light-removing vessel, the distillation column, and the product tank are all equipped with jackets.
[0007] Preferably, the phosgene heater, the dimethylamine heater, the phosgene-removing kettle, and the distillation column are all connected to hot oil inlet pipes and hot oil return pipes, and the synthesis kettle and the product tank are all connected to cold oil inlet pipes and cold oil return pipes.
[0008] Preferably, both the synthesis reactor and the light-removing reactor are connected to an emergency tank via pipelines.
[0009] Preferably, the outlet of the light-dissipating condenser is connected to the light-dissipating tower via a pipeline.
[0010] Preferably, the distillation column is equipped with a stirring structure.
[0011] Preferably, the synthesis secondary condenser is connected to a primary falling film absorber via a pipeline.
[0012] Preferably, the distillation secondary condenser is connected to a phosgene synthesis emergency primary destruction tower via a pipeline.
[0013] Preferably, the cooling water pipe is connected to a circulating water inlet pipe and a circulating water return pipe.
[0014] As can be seen from the above technical solution, this application provides a system for preparing dimethylcarbamoyl chloride. In use, phosgene in the phosgene synthesis device is heated and enters from the top pipe of the synthesis reactor. Dimethylamine gas in the dimethylamine buffer tank is heated and enters from the side pipe of the synthesis reactor. The gaseous substances reacted in the synthesis reactor enter the primary synthesis condenser through a pipe. The uncondensed gas in the primary synthesis condenser enters the secondary synthesis condenser for further condensation. The liquid substances condensed in the primary and secondary synthesis condensers flow back to the synthesis reactor through a pipe. The synthesis liquid in the synthesis reactor enters the photoluminescence removal vessel through the discharge pipe. The gas produced after reacting with nitrogen in the photoluminescence removal vessel enters the photoluminescence removal vessel. The liquid condensed in the condenser flows back to the condenser through a pipe. After the synthesis liquid reacts in the condenser, it enters the distillation column for purification. The purified substances in the distillation column are divided into three parts according to their boiling points: upper, middle, and lower. The substances at the bottom of the distillation column enter the fractionation tank through a pipe. The products in the middle of the distillation column go directly into the product tank. The gaseous substances at the top of the distillation column enter the first-stage condenser through a pipe for condensation. The substances that are not completely condensed then enter the second-stage condenser for further condensation. The condensed products enter the product tank through a pipe. Other substances enter the fractionation tank through a pipe for drum packaging. The distillation vacuum pump evacuates the distillation column, providing a negative pressure environment.
[0015] Compared with the prior art, the beneficial effects of this utility model are: 1. This utility model significantly shortens the reaction time and increases the product yield by optimizing the reaction process and equipment configuration.
[0016] 2. This utility model sets up a separate photoluminescence removal vessel between the synthesis vessel and the distillation column to remove hydrogen chloride gas and phosgene from the synthesized dimethylcarbamoyl chloride, changing the original photoluminescence removal and distillation operations that were directly carried out in the distillation column, which affected the purity of the product.
[0017] 3. The quality of this product is improved by changing the original distillation purification to rectification purification, thus ensuring higher product purity.
[0018] In summary, a system for the preparation of dimethylcarbamoyl chloride has significantly shortened the reaction time and increased the product yield by optimizing the reaction process and equipment configuration. Attached Figure Description
[0019] To more clearly illustrate the technical solution of this utility model, the drawings used in the embodiments will be briefly introduced below. Obviously, for those skilled in the art, other drawings can be obtained based on these drawings without any creative effort.
[0020] Figure 1 This is a schematic diagram of the synthesis section in a dimethylcarbamoyl chloride preparation system provided by this utility model; Figure 2 This is a schematic diagram of a light-removing part in a dimethylcarbamoyl chloride preparation system provided by this utility model; Figure 3 This is a schematic diagram of the distillation section in a dimethylcarbamoyl chloride preparation system provided by this utility model; Figure 4 This is a schematic diagram of the vacuum section in a dimethylcarbamoyl chloride preparation system provided by this utility model.
[0021] The reference numerals in the detailed embodiments are as follows: 1. Synthesis vessel; 2. Phosgene-removing vessel; 3. Distillation column; 4. Distillation vacuum pump; 5. Phosgene synthesis unit; 6. Phosgene heater; 7. Dimethylamine buffer tank; 8. Dimethylamine heater; 9. First-stage synthesis condenser; 10. Second-stage synthesis condenser; 11. Hot oil inlet pipe; 12. Hot oil return pipe; 13. Phosgene-removing condenser; 14. Phosgene-removing column; 15. First-stage distillation condenser; 16. Second-stage distillation condenser; 17. 18. Product tank; 19. Distillation tank; 20. Distillation vacuum buffer tank; 21. Vacuum pump cooler; 22. Stirring structure; 23. Emergency tank; 24. Jacket; 25. Cold oil inlet pipe; 26. Cold oil return pipe; 27. First-stage falling film absorber; 28. Phosgene synthesis emergency first-stage destruction tower; 29. Cooling water pipe; 30. Circulating water inlet pipe; 31. Circulating water return pipe; 32. Make-up water pipe; 33. Acidic tail gas outlet pipe. Detailed Implementation
[0022] To enable those skilled in the art to better understand the technical solutions of this utility model, the technical solutions in the embodiments of this utility model will be clearly and completely described below with reference to the accompanying drawings.
[0023] See Figure 1-4 This application proposes a system for the preparation of dimethylcarbamoyl chloride. In order to solve the problems of existing dimethylcarbamoyl chloride preparation processes that mostly use the reaction of phosgene and dimethylamine, but have problems such as harsh reaction conditions and complex operation, this application proposes a system for the preparation of dimethylcarbamoyl chloride. By optimizing the reaction process and equipment configuration, the reaction time is greatly shortened and the product yield is improved.
[0024] Specifically, a system for preparing dimethylcarbamoyl chloride includes a synthesis reactor 1, a phosgene-reducing reactor 2, a distillation column 3, a distillation vacuum pump 4, a phosgene synthesis device 5, and a dimethylamine buffer tank 7. The phosgene synthesis device 5 is connected to a phosgene heater 6, and the dimethylamine buffer tank 7 is connected to a dimethylamine heater 8. The phosgene heater 6 and the dimethylamine heater 8 are respectively connected to the synthesis reactor 1 through pipes. The phosgene in the phosgene synthesis device 5 is heated and then enters from the top pipe of the synthesis reactor 1. The dimethylamine gas in the dimethylamine buffer tank 7 is heated and then exits from the synthesis reactor 1. The gaseous substances reacting in the synthesis reactor 1 enter through a side pipe. The synthesis reactor 1 is connected to a primary synthesis condenser 9, which in turn is connected to a secondary synthesis condenser 10. Gases that have not yet condensed in the primary synthesis condenser 9 enter the secondary synthesis condenser 10 for further condensation. The secondary synthesis condenser 10 is connected to a primary falling film absorber 26 via a pipe. Light-containing tail gas that also fails to condense in the secondary synthesis condenser 10 is then transported through a pipe to the primary falling film absorber 26 for absorption treatment. The outlets of the primary condenser 9 and the secondary condenser 10 are connected to the synthesis vessel 1. The liquid condensed in the primary condenser 9 and the secondary condenser 10 flows back to the synthesis vessel 1 through pipes. The outlet pipe of the synthesis vessel 1 is connected to the inlet of the photoluminescence removal vessel 2. The synthesis liquid in the synthesis vessel 1 enters the photoluminescence removal vessel 2 through the outlet pipe to remove hydrogen chloride gas and phosgene from the synthesized dimethylcarbamoyl chloride. The photoluminescence removal vessel 2 is connected to the photoluminescence removal condenser 13. The gas generated after nitrogen removal in the photoluminescence removal vessel 2 enters the photoluminescence removal condenser 13. The light-removing condenser 13 changes the original method of directly performing light removal and distillation in the distillation column, which affects product purity. The outlet of the light-removing condenser 13 is connected to the light-breaking tower 14 through a pipeline. The liquid condensed in the light-removing condenser 13 flows back to the light-removing kettle 2 through a pipeline. The gaseous substances that are not condensed in the light-removing condenser 13 enter the light-breaking tower 14 for processing through a pipeline. The outlet of the light-removing kettle 2 is connected to the distillation column 3. The distillation column 3 is equipped with a stirring structure 21. After the synthesis liquid is removed in the light-removing kettle 2, it enters the distillation column 3 for purification. The bottom outlet of distillation column 3 is connected to a fraction tank 18, the middle outlet of distillation column 3 is connected to a product tank 17, and the top outlet of distillation column 3 is connected to a first-stage distillation condenser 15. The first-stage distillation condenser 15 is connected to a second-stage distillation condenser 16. The first-stage and second-stage distillation condensers 15 and 16 are connected to the product tank 17 and the fraction tank 18 via pipes. The purified substance in distillation column 3 is divided into three parts (upper, middle, and lower) according to its boiling point. The substance at the bottom of distillation column 3 enters the fraction tank 18 through pipes for drum packaging. The product in the middle section of column 3 enters the product tank 17 directly. The gaseous substances at the top of column 3 enter the first-stage distillation condenser 15 through a pipeline for condensation. The incompletely condensed substances then enter the second-stage distillation condenser 16 for further condensation. The condensed product enters the product tank 17 through a pipeline. Other substances enter the distillation tank 18 through a pipeline for drum processing. The second-stage distillation condenser 16 is connected to the phosgene synthesis emergency first-stage destruction tower 27 through a pipeline. The phosgene synthesis emergency first-stage destruction tower 27 is generally not used, but is activated for use in case of an accident with excessive negative pressure. The secondary condenser 16 of the distillation unit is connected to the distillation vacuum buffer tank 19, which is connected to the distillation vacuum pump 4. The distillation vacuum pump 4 evacuates the distillation column 3, providing a negative pressure environment. A vacuum pump cooler 20 is installed on the distillation vacuum pump 4 to cool it down. A cooling water pipe 28 is installed inside the distillation vacuum pump 4, connected to a circulating water inlet pipe 29 and a circulating water return pipe 30. The cooling water pipe 28 cools the liquid inside the distillation vacuum pump 4. A water supply pipe 31 is connected to the distillation vacuum pump 4 to supply tap water. An acidic tail gas outlet pipe 32 is connected to the outlet of the distillation vacuum pump 4. The acidic gas extracted from the distillation column 3 by the vacuum pump 4 is output from the acidic tail gas pipe 32. The synthesis vessel 1, the phosgene removal vessel 2, the distillation column 3 and the product tank 17 are all equipped with jackets 23. The phosgene heater 6, the dimethylamine heater 8, the phosgene removal vessel 2 and the distillation column 3 are all connected to hot oil supply pipes 11 and hot oil return pipes 12, which provide heat to the unit. The synthesis vessel 1 and the product tank 17 are both connected to cold oil supply pipes 24 and cold oil return pipes 25, which cool the unit. The synthesis vessel 1 and the phosgene removal vessel 2 are both connected to emergency tanks 22 through pipes. Emergency tanks 22 are not used under normal circumstances, but are activated when a system accident occurs.
[0025] As can be seen from the above technical solution, in the use of a system for preparing dimethylcarbamoyl chloride, phosgene in the phosgene synthesis device 5 is heated and enters from the top pipe of the synthesis vessel 1. Dimethylamine gas in the dimethylamine buffer tank 7 is heated and enters from the side pipe of the synthesis vessel 1. The gaseous substances after reaction in the synthesis vessel 1 enter the primary synthesis condenser 9 through the pipe. The uncondensed gas in the primary synthesis condenser 9 enters the secondary synthesis condenser 10 for further condensation. The liquid substances condensed in the primary synthesis condenser 9 and the secondary synthesis condenser 10 flow back to the synthesis vessel 1 through the pipe. The synthesis liquid in the synthesis vessel 1 enters the photoluminescence removal vessel 2 through the discharge pipe to remove hydrogen chloride gas and phosgene from the synthesized dimethylcarbamoyl chloride. The gas produced after the reaction with nitrogen in the photoluminescence removal vessel 2 is... The substance enters the photoluminescence condenser 13. The liquid condensed in the photoluminescence condenser 13 flows back to the photoluminescence reactor 2 through a pipe. After the synthesis liquid reacts in the photoluminescence reactor 2, it enters the distillation column 3 for purification. The purified substance in the distillation column 3 is divided into three parts according to the different boiling points: upper, middle and lower. The substance at the bottom of the distillation column 3 enters the fractionation tank 18 through a pipe. The product in the middle of the distillation column 3 directly enters the product tank 17. The gaseous substance at the top of the distillation column 3 enters the first-stage distillation condenser 15 through a pipe for condensation. The substance that is not completely condensed then enters the second-stage distillation condenser 16 for condensation. The condensed product enters the product tank 17 through a pipe. Other substances enter the fractionation tank 18 through a pipe for barrel processing. The distillation vacuum pump 4 evacuates the distillation column 3 to provide a negative pressure environment.
[0026] Other embodiments of the present invention will readily occur to those skilled in the art upon consideration of the specification and practice of the applications disclosed herein. The present invention is intended to cover any variations, uses, or adaptations of the invention that follow the general principles of the invention and incorporate common knowledge or customary techniques in the art disclosed herein. The specification and examples are to be considered exemplary only, and the true scope of the invention is indicated by the claims.
[0027] It should be understood that this utility model is not limited to the precise structure described above and shown in the accompanying drawings, and various modifications and changes can be made without departing from its scope. The embodiments of this utility model described above do not constitute a limitation on the scope of protection of this utility model.
Claims
1. A system for preparing dimethylcarbamoyl chloride, characterized in that: It includes a synthesis reactor (1), a phosgene reactor (2), a distillation column (3), a distillation vacuum pump (4), a phosgene synthesis device (5), and a dimethylamine buffer tank (7); The phosgene synthesis apparatus (5) is connected to a phosgene heater (6), the dimethylamine buffer tank (7) is connected to a dimethylamine heater (8), the phosgene heater (6) and the dimethylamine heater (8) are respectively connected to the synthesis vessel (1) through pipes, the synthesis vessel (1) is connected to a synthesis primary condenser (9), the synthesis primary condenser (9) is connected to a synthesis secondary condenser (10), the liquid outlets of the synthesis primary condenser (9) and the synthesis secondary condenser (10) are connected to the synthesis vessel (1), the discharge pipe of the synthesis vessel (1) is connected to the feed inlet of the phosgene-removing vessel (2), the phosgene-removing vessel (2) is connected to a phosgene-removing condenser (13), and the discharge outlet of the phosgene-removing vessel (2) is connected to the distillation column (3). The bottom outlet of the distillation column (3) is connected to a fraction tank (18), the middle outlet of the distillation column (3) is connected to a product tank (17), the top outlet of the distillation column (3) is connected to a first-stage distillation condenser (15), the first-stage distillation condenser (15) is connected to a second-stage distillation condenser (16), the first-stage distillation condenser (15) and the second-stage distillation condenser (16) are connected to the product tank (17) and the fraction tank (18) through pipes, the second-stage distillation condenser (16) is connected to a distillation vacuum buffer tank (19), and the distillation vacuum buffer tank (19) is connected to the distillation vacuum pump (4).
2. The system for preparing dimethylcarbamoyl chloride according to claim 1, characterized in that: The distillation vacuum pump (4) is equipped with a vacuum pump cooler (20), the distillation vacuum pump (4) is provided with a cooling water pipe (28), the distillation vacuum pump (4) is connected with a water supply pipe (31), and the outlet of the distillation vacuum pump (4) is connected with an acidic tail gas pipe (32).
3. The system for preparing dimethylcarbamoyl chloride according to claim 1, characterized in that: The synthesis vessel (1), the light-removing vessel (2), the distillation column (3) and the product tank (17) are all equipped with jackets (23).
4. The system for preparing dimethylcarbamoyl chloride according to claim 1, characterized in that: The phosgene heater (6), the dimethylamine heater (8), the phosgene reactor (2) and the distillation column (3) are all connected to a hot oil inlet pipe (11) and a hot oil return pipe (12), and the synthesis reactor (1) and the product tank (17) are all connected to a cold oil inlet pipe (24) and a cold oil return pipe (25).
5. The system for preparing dimethylcarbamoyl chloride according to claim 1, characterized in that: Both the synthesis reactor (1) and the light-removing reactor (2) are connected to an emergency tank (22) via pipelines.
6. The system for preparing dimethylcarbamoyl chloride according to claim 1, characterized in that: The outlet of the light-reducing condenser (13) is connected to the light-reducing tower (14) via a pipe.
7. The system for preparing dimethylcarbamoyl chloride according to claim 1, characterized in that: The distillation column (3) is equipped with a stirring structure (21).
8. The system for preparing dimethylcarbamoyl chloride according to claim 1, characterized in that: The synthesis secondary condenser (10) is connected to a primary falling film absorber (26) via a pipe.
9. The system for preparing dimethylcarbamoyl chloride according to claim 1, characterized in that: The distillation secondary condenser (16) is connected to the phosgene synthesis emergency primary destruction tower (27) via a pipeline.
10. The system for preparing dimethylcarbamoyl chloride according to claim 2, characterized in that: The cooling water pipe (28) is connected to a circulating water inlet pipe (29) and a circulating water return pipe (30).