Device for recovering monochlorodifluoromethane from preparation system
By designing a device for the difluoro-monochloromethane preparation system, the high cost of residual liquid treatment and environmental pollution problems during the preparation process are solved by using alkali solution analysis, compression and water-alkali washing technology steps, and difluoro-monochloromethane is realized efficient recycling and high-quality product production.
Patent Information
- Application Number
- CN202323590591.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2023-12-28
- Publication Date
- 2024-12-20
- Estimated Expiration
- 2033-12-28
AI Technical Summary
In the preparation process of difluoromonomethane, the treatment methods of residual liquid and distilled residual liquid have high costs and environmental pollution problems. It is difficult for the existing technology to effectively recover difluoromonomethane, resulting in high material consumption and production costs.
A device including residual liquid storage tank, alkali separator, dilute acid storage tank, alkali solution analysis tower, recycling buffer tank, compressor, condensation collection tank, water alkali wash system and distillation tower was designed, and the alkali solution was analyzed by alkali solution. , compression, alkaline washing and distillation technical steps, and recycling difluoromonomethane in steps to avoid direct incineration.
Effective recycling and treatment of difluoromonochloromethane is achieved, production costs are reduced, utilization is improved, environmental pollution is avoided, and the product quality is achieved meets the standards.
Smart Images
Figure CN222196448U_ABST
Abstract
Description
Technical Field
[0001] The utility model relates to a device for recovering difluorochloromethane from a preparation system. Background Art
[0002] Difluoromonochloromethane is a colorless, slightly sweet odorous product with a wide range of uses and stable chemical properties. It is mainly used as a refrigerant, fire extinguishing agent, and raw material for polytetrafluoroethylene resin. Since the product difluoromonochloromethane can be dissolved in acid and alkaline solutions and distillation residue contains difluoromonochloromethane, resulting in difluoromonochloromethane production loss, in the production and preparation process of difluoromonochloromethane, the material consumption level of the difluoromonochloromethane device is basically difficult to reach the theoretical consumption level of difluoromonochloromethane products. At present, when treating F22 in acid and alkaline solutions, it can only be treated in sewage stations; the distillation residue is directly incinerated in an incineration device. The above treatment methods are extremely uneconomical, and it is easy to cause pollution and has high production costs. In view of this problem, how to recover difluoromonochloromethane in the F22 preparation system has become an important issue for the sustainable development of the industry. Utility Model Content
[0003] The utility model provides a device for recovering difluoromonochloromethane from a preparation system, which can effectively treat residual liquid generated in the preparation of difluoromonochloromethane, and the treatment method is economical and reliable, avoiding treatment by direct incineration and preventing environmental pollution.
[0004] The utility model adopts the following technical scheme: The utility model also discloses a device for recovering difluoromonochloromethane from a preparation system, which includes a residual liquid storage tank, an alkali separator, a dilute acid storage tank, an alkali solution analysis tower, a recovery buffer tank, a compressor, a condensation collection tank, a water alkali washing system, a distillation tower and a finished product storage tank. The residual liquid outlet of the difluoromonochloromethane preparation device is connected to the inlet of the residual liquid storage tank, the gas phase outlet of the residual liquid storage tank is connected to the inlet Ⅰ at the top of the recovery buffer tank, the liquid phase outlet of the residual liquid storage tank is connected to the inlet of the alkali solution analysis tower through a regulating valve, and the dilute acid outlet of the water washing tower Ⅰ of the difluoromonochloromethane preparation device is connected to the inlet of the alkali solution analysis tower through a pressure reducing valve Ⅰ The alkali outlet of the alkali separator of the difluorochloromethane preparation device is connected to the inlet of the alkali solution analysis tower through a pressure reducing valve II, the outlet of the alkali solution analysis tower is connected to the inlet II on the side of the recovery buffer tank, the difluorochloromethane outlet of the recovery buffer tank is connected to the input end of the compressor, the output end of the compressor is connected to the inlet of the condensate collection tank, the outlet of the condensate collection tank is connected to the inlet of the water alkali washing system through a recovery pump, and the outlet of the water alkali washing system is connected to the finished product storage tank through a distillation tower.
[0005] Furthermore, the alkali solution analysis tower is a packed tower, the tower body diameter of the alkali solution analysis tower is DN600, DN700 or DN800; the height is 9000-12000mm, the tower kettle diameter of the alkali solution analysis tower is 1200-1600mm, and the height is 1600-2000mm.
[0006] Furthermore, the compressor is configured as a two-stage compressor, and a pressure regulating valve is installed on the pipeline between the compressor and the condensate collection tank.
[0007] Furthermore, the condensation collection tank includes a collection tank body, and a condenser is installed inside the collection tank body. When the compressed difluorochloromethane enters the collection tank body, the difluorochloromethane is condensed by the condenser.
[0008] Furthermore, the water alkali washing system includes a water washing tower and an alkali washing tower, which are connected in series, wherein the water washing tower and the alkali washing tower adopt a packed tower structure, and the packed fillers are PP ball rings, PP saddle rings or PP rosettes; the packing diameter is φ25, φ38 or φ50.
[0009] The utility model has the following beneficial effects: after adopting the above technical scheme, the utility model processes the distillation residue in the preparation of difluoromonochloromethane and the difluoromonochloromethane crude product in the dilute acid and alkali separator through an alkali solution analysis tower, and then utilizes a technology combining compression, water alkali washing and distillation to recover the difluoromonochloromethane in steps, and treats the difluoromonochloromethane to obtain difluoromonochloromethane with qualified product quality, so that the residual liquid in the preparation of difluoromonochloromethane can be effectively treated, the treatment method is economical and reliable, and the treatment by direct incineration is avoided to prevent environmental pollution, and the difluoromonochloromethane obtained after the waste liquid is treated can be reused, turning waste into treasure, thereby effectively reducing the cost of producing difluoromonochloromethane in industrial production and improving the utilization rate. BRIEF DESCRIPTION OF THE DRAWINGS
[0010] In order to more clearly illustrate the embodiments of the utility model or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the utility model. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative work.
[0011] Figure 1 It is a structural schematic diagram of the utility model. DETAILED DESCRIPTION
[0012] The preferred embodiments of the present utility model patent are described in detail below in conjunction with the accompanying drawings so that the advantages and features of the present utility model patent can be more easily understood by those skilled in the art, thereby making a clearer and more definite definition of the protection scope of the present utility model patent.
[0013] exist Figure 1 The utility model also discloses a device for recovering difluoromonochloromethane from a preparation system, which comprises a residual liquid storage tank 1, an alkali separator 16, a dilute acid storage tank 5, an alkali solution analysis tower 6, a recovery buffer tank 2, a compressor 8, a condensation collection tank 9, a water alkali washing system, a distillation tower 1 and a finished product storage tank 12. The residual liquid outlet of the difluoromonochloromethane preparation device is connected to the inlet of the residual liquid storage tank 1, the gas phase outlet of the residual liquid storage tank 1 is connected to the inlet I at the top of the recovery buffer tank 2, the liquid phase outlet of the residual liquid storage tank 1 is connected to the inlet of the alkali solution analysis tower 6 through a regulating valve 3, and the difluoromonochloromethane preparation device The dilute acid outlet of the water washing tower Ⅰ14 is connected to the inlet of the dilute acid storage tank 5 through the pressure reducing valve Ⅰ13, the material outlet of the dilute acid storage tank 5 is connected to the inlet of the alkali solution analysis tower 6, the alkali solution outlet of the alkali separator 16 of the difluoromonochloromethane preparation device is connected to the inlet of the alkali solution analysis tower 6 through the pressure reducing valve Ⅱ7, the outlet of the alkali solution analysis tower 6 is connected to the inlet Ⅱ on the side of the recovery buffer tank 2, the difluoromonochloromethane outlet of the recovery buffer tank 2 is connected to the input end of the compressor 8, the output end of the compressor 8 is connected to the inlet of the condensate collection tank 9, and the outlet of the condensate collection tank 9 is connected to the water alkali washing system through the recovery pump 4. The inlet is connected, and the outlet of the water alkali washing system is connected to the finished product storage tank 12 through the distillation tower 11. The alkali solution analysis tower 6 of this embodiment is a packed tower, and the tower body diameter of the alkali solution analysis tower 6 is DN600, DN700 or DN800; the height is 9000-12000mm, the tower kettle diameter of the alkali solution analysis tower 6 is 1200-1600mm, and the height is 1600-2000mm. The compressor 8 of this embodiment is set as a two-stage compressor, and a pressure regulating valve 10 is installed on the pipeline between the compressor 8 and the condensate collection tank 9. The condensate collection tank 9 of this embodiment includes a collection tank The main body 91 is provided with a condenser 92 inside the collecting tank main body 91. When the compressed difluorochloromethane enters the collecting tank main body 91, the difluorochloromethane is condensed by the condenser 92. The water alkali washing system of this embodiment comprises a water washing tower 18 and an alkali washing tower 17. The water washing tower 18 and the alkali washing tower 17 are connected in series, wherein the water washing tower 18 and the alkali washing tower 17 adopt a packed tower structure, and the packed fillers are PP ball rings, PP saddle rings or PP rosettes; the packing diameter is φ25, φ38 or φ50, and the packed fillers of this embodiment are PP ball rings, and the packing diameter is φ25.
[0014] The use method of the utility model is as follows: the utility model first collects the distillation residual liquid in the preparation of difluoromonochloromethane from the residual liquid storage tank 1, vaporizes the residual liquid in the residual liquid storage tank 1 by heating, the heat medium of the residual liquid storage tank 1 is hot water heated by steam, the light component difluoromonochloromethane is transported to the recovery buffer tank 2 for storage, the liquid phase is sent to the alkali solution analysis tower 6 through the regulating valve 3, the difluoromonochloromethane in the liquid phase is analyzed and also sent to the recovery buffer tank 2 for storage; then the dilute acid in the preparation of difluoromonochloromethane is stored in the dilute acid storage tank 5, the gas phase part of the dilute acid is sent to the alkali solution analysis tower 6 to analyze the difluoromonochloromethane and then sent to the recovery buffer tank 2 for storage, and then the difluoromonochloromethane crude product in the alkali separator 16 for the preparation of difluoromonochloromethane is sent to the alkali solution analysis tower 6 to analyze the difluoromonochloromethane The alkali solution is sent to the recovery buffer tank 2 for storage and is also used as the alkali solution of the alkali solution analysis tower 6. The alkali solution contains difluoromonochloromethane. The dilute acid comes from the water washing tower Ⅰ14 in the difluoromonochloromethane preparation equipment. The water washing tower Ⅰ13 controls the pressure at 1.25-1.35MPa. The dilute acid is sent to the dilute acid storage tank 5 through the pressure reducing valve Ⅰ13. The pressure is at normal pressure. The difluoromonochloromethane and hydrochloric acid dissolved in the dilute acid are resolved and enter the alkali solution analysis tower 6 to remove the acidic substances and recover difluoromonochloromethane. The alkali solution comes from the alkali separator 16. The pressure of the alkali separator 16 is controlled at 1.4-1.55MPa. The alkali solution is sent to the alkali solution analysis tower 6 through the pressure reducing valve Ⅱ16 to resolve the gaseous difluoromonochloromethane. The pressure of the alkali solution analysis tower 6 is controlled at 1-5kpa and the temperature is normal temperature. The difluorochloromethane stored in the recovery buffer tank 2 in step 1, the difluorochloromethane stored in the recovery buffer tank 2 in step 2, and the difluorochloromethane stored in the recovery buffer tank 2 in step 3 are compressed by a compressor 8 and transported to a condensate collection tank 9 for collection. The difluorochloromethane in the condensate collection tank 9 is transported to a water alkali washing system by a recovery pump 4 to remove acidic substances. Finally, the deacidified difluorochloromethane is put into a distillation tower 11 for refining to obtain a difluorochloromethane finished product which is stored in a finished product storage tank 12. The compressor 8 is a two-stage compressor. A pressure regulating valve 10 is arranged on the pipeline between the compressor 8 and the condensate collection tank 9. The cooling water used in the two-stage compressor is circulating water, 0°C cold water, -15°C brine or -35°C brine. The condensate collecting tank 9 is a type that combines a condenser 91 with a storage tank 92. The refrigerant of the condenser 91 is -15°C brine or -35°C brine. The water washing tower 11 and the alkali washing tower 12 of the water alkali washing system absorb and remove HCL and HF gases in the crude difluoromonochloromethane respectively. The pressure of the water washing tower 11 and the alkali washing tower 12 is controlled at 1.5-1.7MPa, the pressure of the distillation tower 11 is controlled at 0.8-1.3MPa, the tower top temperature is controlled at -10-10°C, and the tower bottom temperature is controlled at 30-60°C; the purity reaches 99.9%, the purity of the difluoromonochloromethane product reaches 99.9%, the evaporation residue is less than or equal to 0.02%, the moisture is less than or equal to 10ppm, and the acidity is less than or equal to 0.1ppm.
[0015] Product process control and finished product testing are obtained by gas chromatography analysis. The analysis results of finished product R22 are shown in the table below:
[0016] Table - Product quality analysis results:
[0017] Without limitation to this, any changes or substitutions that are not conceived through creative work should be included in the protection scope of this utility model patent. Therefore, the protection scope of this utility model patent should be based on the protection scope defined in the claims.
Claims
1. A device for recovering difluorochloromethane from a preparation system, Its characteristics are It comprises a residual liquid storage tank (1), an alkali separator (16), a dilute acid storage tank (5), an alkali solution analysis tower (6), a recovery buffer tank (2), a compressor (8), a condensate collection tank (9), a water alkali washing system, a distillation tower (11) and a finished product storage tank (12). The residual liquid outlet of the difluorochloromethane preparation device is connected to the inlet of the residual liquid storage tank (1), the gas phase outlet of the residual liquid storage tank (1) is connected to the inlet I at the top of the recovery buffer tank (2), the liquid phase outlet of the residual liquid storage tank (1) is connected to the inlet of the alkali solution analysis tower (6) through a regulating valve (3), and the dilute acid outlet of the water washing tower I (14) of the difluorochloromethane preparation device is connected to the inlet of the dilute acid storage tank (5) through a pressure reducing valve I (13). The material outlet of the dilute acid storage tank (5) is connected to the inlet of the alkali solution analysis tower (6); the alkali solution outlet of the alkali separator (16) of the difluorochloromethane preparation device is connected to the inlet of the alkali solution analysis tower (6) through a pressure reducing valve II (7); the outlet of the alkali solution analysis tower (6) is connected to the inlet II on the side of the recovery buffer tank (2); the difluorochloromethane outlet of the recovery buffer tank (2) is connected to the input end of the compressor (8); the output end of the compressor (8) is connected to the inlet of the condensate collection tank (9); the outlet of the condensate collection tank (9) is connected to the inlet of the water alkali washing system through the recovery pump (4); and the outlet of the water alkali washing system is connected to the finished product storage tank (12) through the distillation tower (11).
2. The device for recovering difluorochloromethane from a preparation system according to claim 1, Its characteristics are The alkali solution analysis tower (6) is a packed tower. The tower body diameter of the alkali solution analysis tower (6) is DN600, DN700 or DN800 and the height is 9000-12000 mm. The tower bottom diameter of the alkali solution analysis tower (6) is 1200-1600 mm and the height is 1600-2000 mm.
3. The device for recovering chlorodifluoromethane from a preparation system according to claim 1, Its characteristics are The compressor (8) is configured as a two-stage compressor, and a pressure regulating valve (10) is installed on the pipeline between the compressor (8) and the condensate collecting tank (9).
4. The device for recovering difluorochloromethane from a preparation system according to claim 1, Its characteristics are The condensation collection tank (9) comprises a collection tank body (91), and a condenser (92) is installed inside the collection tank body (91). When the compressed difluorochloromethane enters the collection tank body (91), the difluorochloromethane is condensed by the condenser (92).
5. The device for recovering difluorochloromethane from a preparation system according to claim 1, Its characteristics are The water-alkali washing system comprises a water washing tower (18) and an alkali washing tower (17), wherein the water washing tower (18) and the alkali washing tower (17) are connected in series, wherein the water washing tower (18) and the alkali washing tower (17) adopt a packed tower structure, and the packed fillers are PP ball rings, PP saddle rings or PP rosettes; and the packing diameter is φ25, φ38 or φ50.