Efficient DMF (Dimethyl Formamide) recovery device in production process of triformyl rifamycin SV
By employing vacuum distillation and fractional distillation techniques, along with pH adjustment, the problem of inefficient DMF recovery has been solved, enabling resource recycling and purity improvement, while reducing production costs and environmental pollution.
Patent Information
- Application Number
- CN202520198565.9
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2025-02-08
- Publication Date
- 2026-02-13
- Estimated Expiration
- 2035-02-08
AI Technical Summary
In the production process of trimethylrifamycin SV, DMF, as a solvent, cannot be efficiently recovered, leading to resource waste, high production costs, and environmental pollution. Furthermore, the purity of DMF has a direct impact on product quality.
By employing reduced pressure distillation and fractional distillation techniques, combined with pH adjustment methods, and using a combination of distillation tanks and distillation columns, DMF can be efficiently recovered.
This enables the recycling of DMF resources, reduces raw material costs and the discharge of harmful substances in wastewater, improves the purity of DMF, and enhances production efficiency.
Smart Images
Figure CN223901241U_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The utility model relates to a chemical equipment technical field, concretely is a kind of high-efficiency recovery device of DMF in rifamycin SV production process. BACKGROUND
[0002] In the process of producing rifampicin intermediate rifamycin SV, dimethylformamide (DMF) as an important solvent in production cannot be efficiently recovered, and a large amount of DMF is discharged with oxazine mother liquor, facing key problems such as resource waste, high production cost and environmental pollution, which not only greatly increases the production cost of enterprises, but also leads to serious resource waste. In addition, the purity of DMF has a direct impact on the quality of the final product, and the unrecoverable DMF further limits the production efficiency of the enterprise. SUMMARY
[0003] The technical problem to be solved by the utility model is to overcome the above technical defects, and to provide a high-efficiency recovery device of DMF in rifamycin SV production process.
[0004] In order to solve the above problems, the technical scheme of the utility model is as follows: a high-efficiency recovery device of DMF in rifamycin SV production process, comprising a distillation tank and a rectifying tower;
[0005] The top of the distillation tank is provided with a gas outlet pipe, the upper part of the side is provided with an input pipe, the lower part of the side is provided with an output pipe, the bottom is penetrated and rotatably installed with a stirring shaft, a plurality of stirring blades are installed on the stirring shaft, a heating pipe is arranged at the bottom of the distillation tank, and a motor for driving the stirring shaft to rotate is installed at the bottom of the distillation tank, and the gas outlet pipe is connected with a condenser and a vacuum pump in sequence through a conduit;
[0006] The upper part of the side of the rectifying tower is provided with a liquid inlet pipe, the lower part of the side is provided with an air inlet pipe and a liquid outlet pipe, the top is provided with an air outlet pipe, one end of the liquid inlet pipe is connected with a spray tray inside the rectifying tower, a plurality of distributors are arranged inside the rectifying tower, and a PH detection probe and a dosing pipe are respectively penetrated and installed on the upper part of the two sides of the distributor on the side wall of the rectifying tower, and a peristaltic pump is connected between the liquid inlet pipe and the output pipe.
[0007] Further, a pressure gauge is further installed at the top of the distillation tank, a fixed ring is fixedly connected at the edge of the bottom of the distillation tank, and a heat insulation plate is arranged on the inner side of the fixed ring above the motor.
[0008] Further, a safety bottle is further arranged between the condenser and the vacuum pump.
[0009] Further, a packing layer is arranged on the upper and lower sides of the distributor inside the rectifying tower.
[0010] Further, a grid plate is arranged below the packing layer in the lower part of the rectifying tower.
[0011] Further, the distillation tank, the rectification tower and the distributor are provided with temperature sensors.
[0012] Further, the input pipe, the output pipe, the liquid discharge pipe and the dosing pipe are provided with electromagnetic valves.
[0013] Compared with the prior art, the utility model has the advantages that: the utility model combines the pressure reduction distillation and the rectification segmented operation technology with the pH value adjusting means, so that the DMF is recovered and the purity of the DMF reaches the production requirement, the resource recycling is realized, the raw material cost is reduced, the consumption of the DMF is reduced, the emission of the harmful substances in the wastewater is greatly reduced, and the environmental protection treatment pressure of the enterprise is reduced. BRIEF DESCRIPTION OF DRAWINGS
[0014] Figure 1 is the three-dimensional view of the utility model Figure 1 .
[0015] Figure 2 is the three-dimensional view of the utility model Figure 2 .
[0016] Figure 3 is the sectional view of the distillation tank of the utility model.
[0017] Figure 4 is the sectional view of the rectification tower of the utility model.
[0018] As shown in the drawings: 1, distillation tank; 2, rectification tower; 3, gas outlet pipe; 4, input pipe; 5, output pipe; 6, stirring shaft; 7, stirring blade; 8, heating pipe; 9, motor; 10, condenser; 11, vacuum pump; 12, pressure gauge; 13, heat insulation plate; 14, safety bottle; 15, liquid inlet pipe; 16, gas inlet pipe; 17, liquid discharge pipe; 18, exhaust pipe; 19, spraying disc; 20, distributor; 21, pH detection probe; 22, dosing pipe; 23, peristaltic pump; 24, filler layer; 25, grid plate. DETAILED DESCRIPTION
[0019] The technical solutions in the embodiments of the utility model will be clearly and completely described in combination with the drawings in the embodiments of the utility model, and obviously, the described embodiments are only part of the embodiments of the utility model, rather than all the embodiments; based on the embodiments in the utility model, all other embodiments obtained by the person skilled in the art without creative labor fall within the protection scope of the utility model.
[0020] As Figure 1 , Figure 2 and Figure 3As shown, a high-efficiency DMF recovery device in the production process of triformylrifamycin SV includes a distillation tank 1. The distillation tank 1 has an outlet pipe 3 at the top, an input pipe 4 on the upper side, an output pipe 5 on the lower side, and a stirring shaft 6 that is rotatably mounted through the bottom. Multiple stirring blades 7 are mounted on the stirring shaft 6. The bottom of the distillation tank 1 has a heating pipe 8, and a motor 9 for driving the stirring shaft 6 to rotate is installed at the bottom of the distillation tank 1. A pressure gauge 12 is also installed at the top of the distillation tank 1. A fixing ring is fixed to the bottom edge of the distillation tank 1. A heat insulation plate 13 is provided on the inner side of the fixing ring above the motor 9. The outlet pipe 3 is connected to a condenser 10 and a vacuum pump 11 in sequence through a conduit. A safety bottle 14 is also provided between the condenser 10 and the vacuum pump 11.
[0021] The distillation vessel 1 is equipped with a temperature sensor for real-time temperature monitoring, and a pressure gauge 12 monitors the pressure inside the distillation vessel 1. Oxazine mother liquor is added to the distillation vessel 1 through the input pipe 4, and the vacuum pump 11 is activated to extract air from the distillation vessel 1, thus reducing the internal pressure and decreasing the amount of moisture and other low-boiling-point components. This allows volatile impurities to evaporate at a lower temperature, preventing DMF decomposition at high temperatures. The evaporated impurities are then condensed and recovered by the condenser 10.
[0022] like Figure 1 , Figure 2 and Figure 4 As shown, the high-efficiency DMF recovery device in the production process of triformylrifamycin SV also includes a distillation column 2. The upper side of the distillation column 2 is provided with an inlet pipe 15, the lower side is provided with an air inlet pipe 16 and an outlet pipe 17, and the top is provided with an exhaust pipe 18. One end of the inlet pipe 15 is connected to a spray plate 19 inside the distillation column 2. The distillation column 2 is provided with multiple distributors 20, and the side walls of the distillation column 2 are respectively installed with pH detection probes 21 and dosing pipes 22 through the upper sides of the distributors 20. The distillation column 2 is provided with packing layers 24 on both the upper and lower sides of the distributors 20. The lower part of the distillation column 2 is provided with a grid plate 25 below the packing layers 24. The distillation column 2 is provided with temperature sensors above the distributors 20. A peristaltic pump 23 is connected between the inlet pipe 15 and the outlet pipe 5.
[0023] The peristaltic pump 23 will enter the distillation tank 1 inside the DMF mixture after the rough distillation into the rectifying column 2 for secondary separation, and the rectifying column 2 has a high-efficiency corrugated packing layer 24 to increase the contact area of the liquid and improve the separation efficiency; the pH value of the oxazine mother liquor is adjusted at different distillation stages, so that the DMF is protected from decomposition at high temperature, the acidity and alkalinity of the liquid are detected, and appropriate acid or alkali solution is added through the dosing pipe 22 according to the stability of the DMF under different pH conditions, so that the DMF is maintained in a suitable chemical environment, and the decomposition of the DMF can be significantly reduced through the adjustment of the acidity and alkalinity at different stages, and the recovery quality is improved.
[0024] In specific use, the vacuum pump 11 extracts the air inside the distillation tank 1, so that the pressure inside the distillation tank 1 is reduced, the moisture and other low-boiling-point components are reduced, and then the volatile impurities can be evaporated at a lower temperature, avoiding decomposition of the DMF under high temperature conditions; the peristaltic pump 23 will enter the distillation tank 1 inside the DMF mixture after the rough distillation into the rectifying column 2 for secondary separation, the acidity and alkalinity of the liquid are detected at different distillation stages, and appropriate acid or alkali solution is added through the dosing pipe 22 according to the stability of the DMF under different pH conditions, so that the DMF is maintained in a suitable chemical environment, and the decomposition of the DMF can be significantly reduced through the adjustment of the acidity and alkalinity at different stages, and the recovery quality is improved.
[0025] The utility model discloses a distillation and rectification segmented operation technology, combined with the acidity and alkalinity adjusting means, achieves the effect of recycling DMF and making its purity reach the production requirement, not only can realize the cyclic utilization of resources, reduce raw material cost, reduce the consumption of DMF, but also can greatly reduce the emission of harmful substances in wastewater, reduce the environmental protection treatment pressure of enterprise.
[0026] The undisclosed part in the utility model is prior art, and the specific structure and working principle will not be repeated.
[0027] It should be noted that, in this paper, relationship terms such as first and second are only used to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply any such actual relationship or order between the entities or operations. Moreover, the term "includes", "contains" or any other variant thereof is intended to cover non-exclusive inclusion, so that the process, method, article or equipment including a series of elements not only includes those elements, but also includes other elements not explicitly listed or inherent to such process, method, article or equipment.
[0028] Although the embodiments of the present application have been shown and described, it is to be understood that various changes, modifications, substitutions and variations can be made to these embodiments without departing from the principles and spirit of the present application, and the scope of the present application is defined by the appended claims and their equivalents.
[0029] The above describes the present application and its embodiments, which are not restrictive, and the embodiments shown in the drawings are only one of the embodiments of the present application, and the actual structure is not limited thereto. In summary, if a person skilled in the art is inspired, without departing from the creative purpose of the present application, without creative design, similar structure and embodiments to the technical solution, which should belong to the protection scope of the present application.
Claims
1. A device for efficiently recovering DMF in the production process of trimetacyl rifamycin SV, comprising a distillation tank (1) and a rectifying tower (2), characterized in that: the top of the distillation tank (1) is provided with a gas outlet pipe (3), the upper side is provided with an input pipe (4), the lower side is provided with an output pipe (5), the bottom is provided with a stirring shaft (6) penetrating and rotatingly installed, a plurality of stirring blades (7) are installed on the stirring shaft (6), the bottom of the distillation tank (1) is provided with a heating pipe (8), and the bottom of the distillation tank (1) is provided with a motor (9) for driving the stirring shaft (6) to rotate, and the gas outlet pipe (3) is connected with a condenser (10) and a vacuum pump (11) through a pipeline in sequence; the upper side of the rectifying tower (2) is provided with a liquid inlet pipe (15), the lower side is provided with a gas inlet pipe (16) and a liquid outlet pipe (17), and the top is provided with a gas outlet pipe (18), one end of the liquid inlet pipe (15) is connected with a spray tray (19) inside the rectifying tower (2), a plurality of distributors (20) are arranged inside the rectifying tower (2), and the side wall of the rectifying tower (2) is provided with a PH detection probe (21) and a dosing pipe (22) penetratingly installed on the upper side of both sides of the distributor (20), and the liquid inlet pipe (15) and the output pipe (5) are connected with a peristaltic pump (23). The top of the distillation tank (1) is also provided with a pressure gauge (12), the bottom edge of the distillation tank (1) is fixedly connected with a fixed ring, and the inner side of the fixed ring is provided with a heat insulation plate (13) above the motor (9).
2. The apparatus for efficient recovery of DMF in the production of triformylrifamycin SV according to claim 1, characterized in that: A safety bottle (14) is arranged between the condenser (10) and the vacuum pump (11).
3. The apparatus for efficient recovery of DMF in the production of triformylrifamycin SV according to claim 1, characterized in that: The upper and lower sides of the distributor (20) inside the rectifying tower (2) are both provided with a packing layer (24).
4. The apparatus for efficient recovery of DMF in the production of triformylrifamycin SV according to claim 1, characterized in that: The lower part of the rectifying tower (2) is provided with a grid plate (25) below the packing layer (24).
5. The apparatus for efficient recovery of DMF in the production of triformylrifamycin SV according to claim 4, characterized in that: Temperature sensors are arranged above the distributors (20) in the interior of the distillation tank (1) and the rectifying tower (2).
6. The apparatus for efficient recovery of DMF in the production of triformylrifamycin SV according to claim 1, characterized in that: