Separation and purification device for preparing fluorine-containing intermediate
By designing a separation and purification device prepared by fluorine-containing intermediates, reacting with heating mixing chambers and cooling chambers, and processing them by filtering dry parts, the safety hazards and purification problems of fluorine-containing intermediates in the prior art are solved, and the problem of purification difficulty is realized. No wastewater discharge and efficient purification improve product quality.
Patent Information
- Application Number
- CN202421021790.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2024-05-11
- Publication Date
- 2024-12-27
- Estimated Expiration
- 2034-05-11
AI Technical Summary
The synthesis method of fluorine-containing intermediates in the prior art has problems such as safety hazards, serious equipment corrosion, many by-products, and difficulty in purification. In particular, the diazotization reaction produces a large amount of acidic wastewater with high salt content and many crude impurities. , It is difficult to purify.
A separation and purification device for preparing fluorine-containing intermediates is designed, including heating mixing chambers, cooling chambers and filtering drying parts. Calcium nitrite is used as diazotization reagent, and reacts by heating mixing chambers and cooling chambers, and filtering drying parts are used. Perform treatment to achieve wastewater discharge and efficient purification.
It has achieved wastewater discharge, reduced production costs, easy control of decomposition reaction process, fewer impurities in crude products, and improved product quality and yield.
Smart Images
Figure CN222238820U_ABST
Abstract
Description
Technical Field
[0001] The utility model relates to the technical field of purification and preparation of fluorine-containing intermediates, in particular to a separation and purification device for the preparation of fluorine-containing intermediates. Background Art
[0002] In recent years, fluorinated intermediates are gradually showing great growth potential as they are widely used in the chemical, pharmaceutical and agricultural industries. In particular, in the pharmaceutical field, fluorinated intermediates are required in the synthesis of various pharmaceutical compounds. Therefore, fluorinated intermediates are becoming more and more important, and research and development activities are becoming increasingly active.
[0003] Fluorinated intermediates are mainly used in the production of APIs in the pharmaceutical industry. Trends show that in the production of pharmaceutical compounds, the demand for aromatic fluorinated intermediates is becoming more and more common, and their proportion in drug varieties is increasing. Organic fluorinated compounds have strong stability, physiological activity, fat solubility and sulfur-water properties, and can adjust parameters such as electronics and lipophilicity. Therefore, many fluorinated drugs have relatively small dosage, low toxicity, high efficacy, and strong metabolic capacity in terms of performance, which has a significant impact on the pharmacodynamics and pharmacokinetic properties of drugs. Due to the superior performance of fluorinated drugs, the research and development of fluorinated drugs has promoted the expansion of the domestic and foreign markets for fluorinated intermediates.
[0004] As for fluorine-containing intermediates, there are almost no natural substances and they can only be synthesized by artificial chemical methods. The synthesis methods of fluorine-containing intermediates usually include: diazotization reaction to replace amino group, halogen exchange method where fluorine replaces other halogens, direct fluorination method, and fluorination method with special fluorinating agents.
[0005] Among these methods, the halogen exchange method in which fluorine replaces other halogens and the fluorination method using special fluorinating agents both need to be carried out at high temperatures, which poses a great safety hazard. The direct fluorination method has the disadvantages of high risk of raw materials, difficult process control, serious equipment corrosion, many by-products, and difficulty in purification.
[0006] The diazotization reaction in the prior art replaces the amination method. In the diazotization reaction, sodium nitrite is used as a diazotization reagent. The reaction produces a large amount of acidic wastewater with high salt content, making it difficult to treat the three wastes. In the decomposition reaction, solid dry powder is used for direct thermal decomposition, which results in a violent reaction, a difficult process to control, a large amount of impurities in the crude product, and great difficulty in purification. Summary of the invention
[0007] In view of this, the purpose of the utility model is to provide a separation and purification device for preparing fluorine-containing intermediates that can realize the decomposition and purification operation of fluorine-containing intermediates and realize the preparation and molding of fluorine-containing intermediates.
[0008] The utility model is realized by the following method: a separation and purification device for preparing fluorine-containing intermediates, comprising a heating mixing bin, wherein the right side of the heating mixing bin is connected to a cooling bin via a connecting piece, a filtering and drying element is arranged on the right side of the cooling bin, and the lower surface of the cooling bin is connected to the filtering and drying element via a feeding pipe; a first feeding pipe is connected to the left end of the upper surface of the heating mixing bin, and a second feeding pipe is connected to the upper end of the left side surface of the heating mixing bin.
[0009] Furthermore, the connecting piece includes a connecting pipe, and a water pump is connected to the lower end of the right side surface of the heating mixing bin, and the water pump is connected to the cooling bin via the connecting pipe.
[0010] Furthermore, a plurality of cooling pipes are equidistantly arranged in the left and right side walls of the cooling bin, a driving motor is embedded in the middle of the bottom surface of the cooling bin, an output end of the driving motor is connected to a rotating shaft, stirring blades are equidistantly arranged on the rotating shaft, and droppers are connected to both left and right ends of the upper surface of the cooling bin, and an electromagnetic valve is arranged on the dropper.
[0011] Furthermore, the filter drying element includes a filter box, the feed pipe is connected to the filter box, a suction pump is arranged on the feed pipe, an activated carbon filter plate is drawable at the lower end of the front side of the filter box, an annular baffle plate is arranged on the activated carbon filter plate, a drying box is arranged on the upper surface of the filter box, and a draw-out opening is opened at both the upper and lower ends of the front side of the drying box.
[0012] Furthermore, it also includes a distillation box body, wherein a feed port is opened at the left end of the upper surface of the distillation box body, a water inlet pipe is connected to the right end of the upper surface of the distillation box body, an air outlet pipe is connected to the right end of the upper surface of the distillation box body, and a plurality of heating pipes are embedded in the lower surface of the distillation box body at equal distances.
[0013] The beneficial effects of the utility model are as follows: a heating and mixing chamber, a cooling chamber and a filtering and drying component are added to the device, so that the preparation and purification of fluorine-containing intermediates can be realized; by adopting calcium nitrite as a diazotization reagent, the diazo mother liquor after the reaction can be recycled after treatment, so that no wastewater discharge can be achieved, and the discharge of three wastes is greatly reduced, thereby reducing the production cost; the decomposition reaction is carried out smoothly in the solvent n-hexane, the process is easy to control, the crude product has few impurities, and is easy to purify, thereby improving the product quality and yield. BRIEF DESCRIPTION OF THE DRAWINGS
[0014] Figure 1 It is a structural schematic diagram of the utility model.
[0015] Figure 2 It is a structural schematic diagram of the distillation box. DETAILED DESCRIPTION
[0016] The utility model is further described below in conjunction with the accompanying drawings.
[0017] See also Figure 1 and Figure 2 As shown, the utility model provides an embodiment: a separation and purification device for preparing fluorine-containing intermediates, comprising a heating and mixing bin 1, the heating and mixing bin 1, the right side of the heating and mixing bin 1 is connected to a cooling bin 3 through a connecting piece 2, the right side of the cooling bin 3 is provided with a filter drying element 4, the lower surface of the cooling bin 3 is connected to the filter drying element 4 through a feeding pipe 5; the left end of the upper surface of the heating and mixing bin 1 is connected to a first feeding pipe 11, and the upper end of the left side of the heating and mixing bin 1 is connected to a second feeding pipe 12. The hydrochloric acid solution with a mass fraction of 15-20% and the naphthylamine are transported to the heating and mixing bin 1 for mixing, heated and stirred until dissolved, and then transported to the cooling bin 3 for cooling, cooled to below 8°C, and calcium nitrite is slowly dripped to perform a diazo reaction. After the dripping is completed, stirring is continued for 0.5-1 hour to achieve the purification of the fluorine-containing intermediates.
[0018] Please continue reading Figure 1 As shown, in one embodiment of the utility model, the connecting member 2 includes a connecting pipe 21, and a water pump 22 is connected to the lower end of the right side of the heating and mixing chamber 1, and the water pump 22 is connected to the cooling chamber 3 through the connecting pipe 21. The mixed solution is transported to the cooling chamber 3 through the action of the water pump 22.
[0019] Please continue reading Figure 1 As shown, in one embodiment of the utility model, a plurality of cooling pipes 31 are arranged at equal distances in the left and right side walls of the cooling chamber 3, a driving motor 32 is embedded in the middle of the inner bottom surface of the cooling chamber 3, a rotating shaft 33 is connected to the output end of the driving motor 32, stirring blades 34 are arranged at equal distances on the rotating shaft 33, and droppers 35 are connected to both ends of the upper surface of the cooling chamber 3, and a solenoid valve 36 is arranged on the dropper 35. The driving motor 32 can drive the stirring blade 34 to rotate, and calcium nitrite and fluoroboric acid solution with a mass fraction of 40-55% are respectively dripped in through the dropper 35 for uniform stirring.
[0020] Please continue reading Figure 1As shown, in one embodiment of the utility model, the filter drying element 4 includes a filter box 41, the feed pipe 5 is connected to the filter box 41, the feed pipe 5 is provided with a pumping pump 42, the filter box 41 is provided with an activated carbon filter plate 43 at the lower end of the front side, the activated carbon filter plate 43 is provided with an annular baffle plate 44, the filter box 41 is provided with a drying box 45 on the upper surface, and the upper and lower ends of the front side of the drying box 45 are provided with a pulling opening (not shown). By passing hot air into the drying box 45, drying is achieved, and filtering can be achieved through the filter box 41. The filtrate is first decolorized with activated carbon, and then filtered by adding sulfuric acid solution and reused. The obtained filter cake is a diazonium fluoroborate double salt of naphthylamine, which is heated and dried.
[0021] Please continue reading Figure 2 As shown, in one embodiment of the utility model, a distillation box 6 is further included, wherein a feed port 61 is provided at the left end of the upper surface of the distillation box 6, a water inlet pipe 62 is connected to the right end of the upper surface of the distillation box 6, an air outlet pipe 63 is connected to the right end of the upper surface of the distillation box 6, and a plurality of heating pipes 64 are embedded at equal distances in the lower surface of the distillation box 6. The dried diazofluoroborate double salt can be subjected to thermal decomposition reaction through the heating pipes 64 to obtain a n-hexane solution of a fluorine-containing intermediate, and then the n-hexane solution of the fluorine-containing intermediate is distilled to obtain a purified fluorine-containing intermediate.
[0022] The heating tube, solenoid valve, material pump, water pump, activated carbon filter plate, cooling tube and driving motor in the utility model are all prior art, which can be clearly understood by those skilled in the art and will not be described in detail here.
[0023] The above description is only a preferred embodiment of the present invention. All equivalent changes and modifications made according to the scope of the patent application of the present invention should fall within the scope of the present invention.
Claims
1. A separation and purification device for preparing fluorine-containing intermediates, characterized in that: It includes a heating mixing bin, the right side of which is connected to a cooling bin via a connecting piece, a filtering and drying element is arranged on the right side of the cooling bin, and the lower surface of the cooling bin is connected to the filtering and drying element via a feeding pipe; the left end of the upper surface of the heating mixing bin is connected to a first feeding pipe, and the upper end of the left side surface of the heating mixing bin is connected to a second feeding pipe.
2. The separation and purification device for preparing a fluorine-containing intermediate according to claim 1, characterized in that: The connecting piece includes a connecting pipe, and a water pump is connected to the lower end of the right side surface of the heating and mixing bin. The water pump is connected to the cooling bin via the connecting pipe.
3. The separation and purification device for preparing a fluorine-containing intermediate according to claim 1, characterized in that: A plurality of cooling pipes are arranged at equal distances in the left and right side walls of the cooling bin, a driving motor is embedded in the middle of the bottom surface of the cooling bin, an output end of the driving motor is connected to a rotating shaft, stirring blades are arranged at equal distances on the rotating shaft, and droppers are connected to the left and right ends of the upper surface of the cooling bin, and an electromagnetic valve is arranged on the dropper.
4. The separation and purification device for preparing a fluorine-containing intermediate according to claim 1, characterized in that: The filter drying element includes a filter box, the feed pipe is connected to the filter box, a suction pump is arranged on the feed pipe, an activated carbon filter plate is drawn out at the lower end of the front side of the filter box, an annular baffle plate is arranged on the activated carbon filter plate, a drying box is arranged on the upper surface of the filter box, and a drawing opening is opened at both the upper and lower ends of the front side of the drying box.
5. The separation and purification device for preparing a fluorine-containing intermediate according to claim 1, characterized in that: It also includes a distillation box body, a feed inlet is opened at the left end of the upper surface of the distillation box body, a water inlet pipe is connected to the right end of the upper surface of the distillation box body, an air outlet pipe is connected to the right end of the upper surface of the distillation box body, and a plurality of heating pipes are embedded in the lower surface of the distillation box body at equal distances.