Hydrocortisone acetate crude product preparation device
By installing two layers of filters in the preparation device for crude hydrocortisone acetate and using a counter-current pulse pump and an anti-friction coating, the problems of low catalyst separation efficiency and clogging were solved, achieving a highly efficient separation effect.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-12-23
- Publication Date
- 2026-03-27
AI Technical Summary
In existing prednisolone acetate preparation processes, the catalyst CrO3 has low separation efficiency and is prone to clogging, resulting in low separation efficiency.
Two layers of filter screens are installed at the bottom of the reaction vessel, and a backflow pulse pump is used for pulse rinsing. Combined with the use of a modified ultrafine glass fiber anti-friction coating, the filtration effect is improved.
It slows down the clogging of the filtration equipment, improves separation efficiency and operating time, and ensures the stability of the separation process.
Smart Images
Figure CN121732073A_ABST
Abstract
Description
Technical Field
[0001] This application relates to an apparatus for preparing crude hydrocortisone acetate. Background Technology
[0002] The bio-fermentation route for prednisolone acetate uses cortisone acetate as a substrate, undergoing dehydrogenation at the 1,2 positions to convert it to prednisolone acetate, followed by separation and purification to obtain the final prednisolone acetate product. This process features a short reaction route, mild conditions, economical and safe raw materials, and significantly reduced wastewater, making it highly suitable for industrial production. Literature reports that this process route is mature and yields a stable product quality; the specific reaction route is as follows: During the reaction, the catalyst CrO3 needs to be separated before the next step can be carried out. The existing separation method is too inefficient and is prone to clogging during use, so it is necessary to improve it. Summary of the Invention
[0003] To address the aforementioned problems, this application proposes an apparatus for preparing crude hydrocortisone acetate, comprising a reaction vessel, a first filter screen at the bottom of the reaction vessel, a filter chamber below the first filter screen, a second filter screen in the lower middle part of the filter chamber, a reflux tank at the bottom of the filter chamber via an intermediate transition pipe, an intermediate control valve on the intermediate transition pipe, a flushing pipe on the side of the reflux tank, a backflow pulse pump on the flushing pipe, and the other side of the flushing pipe connected to the filter chamber below the second filter screen. An outlet pipe is located at the bottom of the filter chamber. This application employs two layers of filtration at the bottom of the reaction vessel—the first and second filter screens—to ensure filtration effectiveness. The backflow pulse pump then performs pulse flushing to delay clogging, increase operability, and ensure separation efficiency.
[0004] Preferably, the first filter screen is a wire mesh filter. The pore size of the first filter screen is 20 mesh.
[0005] Preferably, the second filter screen includes a support frame, a central filter membrane disposed in the middle of the support frame, and outer filter screens disposed on both sides of the central filter membrane. The second filter screen has a mesh size of 50 mesh.
[0006] Preferably, the central filter membrane is a polytetrafluoroethylene (PTFE) filter membrane, and the outer filter screen is a wire mesh filter. The second filter screen in this application uses an outer filter screen that serves both a supporting and filtering function on both sides of the central filter membrane. This can protect the outer filter membrane, but improvements to the stainless steel wire mesh filter are needed to prevent particles adhering to the surface of the outer filter from directly affecting the filtration performance of the second filter screen.
[0007] Preferably, an anti-friction layer is provided on the outside of the wire mesh filter.
[0008] Preferably, the anti-friction coating comprises the following substances in parts by weight: Acrylic emulsion: 40-50 parts; Polytetrafluoroethylene emulsion: 80-100 parts; Ultrafine glass fiber; 2-4 parts; HF solution: 10-15 parts, HF mass fraction is 20-30 wt%; Nano calcium carbonate: 0.4-0.5 parts.
[0009] Preferably, both the acrylic emulsion and the polytetrafluoroethylene emulsion are water-based emulsions.
[0010] Preferably, the ultrafine glass fiber has a diameter of 1-2 μm and a length of 1-3 mm.
[0011] Preferably, the ultrafine glass fiber is placed in an HF solution, stirred evenly, and then reacted at 40-50°C for 30-40 minutes. Then, nano-calcium carbonate is introduced, and the mixture is stirred thoroughly for 45-60 minutes. After cooling to room temperature, a preliminary mixture is obtained. The initial mixture is then thoroughly mixed with polypropylene emulsion and polytetrafluoroethylene emulsion to obtain the spray coating. In this application, ultrafine glass fiber is modified and added to the acrylic emulsion and polytetrafluoroethylene emulsion, enabling the anti-friction coating to avoid catalyst adhesion. After filtration, it can be promptly backwashed away, making it suitable for the application environment of this application.
[0012] Preferably, the filter screen is horizontally placed on the support frame, and then a high-pressure airless sprayer is used to spray the front and back sides of the filter screen with spray liquid as the raw material. Each side is sprayed no less than 3 times, and then left to cure at room temperature for 24-36 hours to obtain an anti-friction coating.
[0013] This application can bring the following beneficial effects: 1. This application sets two layers of filtration at the bottom of the reaction vessel, namely a first filter screen and a second filter screen, to ensure filtration effect. Then, a backflow pulse pump is used to flush the vessel in a pulse manner to delay clogging, increase the working time, and ensure separation efficiency.
[0014] 2. The second filter screen of this application adopts an outer filter screen with both supporting and filtering functions on both sides of the middle filter membrane. It can protect the outer filter membrane. However, the stainless steel wire mesh filter also needs to be improved to avoid the particles adhering to the surface of the outer filter directly affecting the filtering performance of the second filter screen.
[0015] 3. This application uses ultrafine glass fiber modified and added to acrylic emulsion and polytetrafluoroethylene emulsion, which enables the anti-friction coating to have the effect of not sticking to the catalyst. After filtration, it can be backwashed out in time, which is suitable for the application environment of this application. Attached Figure Description
[0016] The accompanying drawings, which are included to provide a further understanding of this application and form part of this application, illustrate exemplary embodiments and are used to explain this application, but do not constitute an undue limitation of this application. In the drawings: Figure 1 This is a schematic diagram of the structure of this application.
[0017] Figure 2 This is a schematic diagram of the second filter screen. Detailed Implementation
[0018] To clearly illustrate the technical features of this solution, the following detailed description, in conjunction with the accompanying drawings, will be provided.
[0019] An apparatus for preparing crude hydrocortisone acetate, such as Figure 1-2 As shown, the system includes a reaction vessel 1, a first filter screen 2 at the bottom of the reaction vessel 1, a filter chamber 3 below the first filter screen 2, a second filter screen 4 in the lower middle part of the filter chamber 3, a reflux tank 6 connected to the bottom of the filter chamber 3 via an intermediate transition pipe 5, an intermediate control valve 7 on the intermediate transition pipe 5, a flushing pipe 8 on the side of the reflux tank 6, a backflow pulse pump 9 on the flushing pipe 8, the other side of the flushing pipe 8 connected to the filter chamber 3 below the second filter screen 4, and an outlet pipe 10 at the bottom of the filter chamber 3.
[0020] The first filter screen 2 is a wire mesh filter.
[0021] The second filter 2 includes a support frame 13, a central filter membrane 11 disposed in the middle of the support frame 13, and outer filter screens 12 disposed on both sides of the central filter membrane 11. The central filter membrane is a polytetrafluoroethylene (PTFE) filter membrane, and the outer filter screens are wire mesh filters. An anti-friction layer is disposed on the outer side of the wire mesh filter.
[0022] The anti-friction coating comprises the following substances in parts by weight: Acrylic emulsion: 40-50 parts; Polytetrafluoroethylene emulsion: 80-100 parts; Ultrafine glass fiber; 2-4 parts; HF solution: 10-15 parts, HF mass fraction is 20-30 wt%; Nano calcium carbonate: 0.4-0.5 parts.
[0023] Both the acrylic emulsion and the polytetrafluoroethylene emulsion are water-based emulsions.
[0024] The ultrafine glass fibers have a diameter of 1-2 μm and a length of 1-3 mm.
[0025] The ultrafine glass fiber was placed in an HF solution, stirred evenly, and then reacted at 40-50℃ for 30-40 minutes. Then, nano-calcium carbonate is introduced, and the mixture is stirred thoroughly for 45-60 minutes. After cooling to room temperature, a preliminary mixture is obtained. Then, the preliminary mixture is thoroughly mixed with the polypropylene emulsion and polytetrafluoroethylene emulsion to obtain the spraying liquid.
[0026] The filter screen is horizontally placed on the support frame. Then, a high-pressure airless sprayer is used to spray the front and back sides of the filter screen with spray liquid as the raw material. Each side is sprayed no less than 3 times. Then, it is left to cure at room temperature for 24-36 hours to obtain the anti-friction coating.
[0027] In practical use, the following example is used to prepare a second filter screen with an anti-friction coating. The same filtration treatment and backwashing treatment are performed on the product containing chromium oxide catalyst hydrocortisone acetate crude product. After 30 minutes of filtration and discharge, the intermediate control valve is closed, and pulse impact treatment is performed using a backflow pulse pump.
[0028] Example 1: S101. Preliminary mixing Two parts of ultrafine glass fiber were placed in 10 parts of HF solution (20wt%), stirred evenly, and then reacted at 40℃ for 40 min. Then, 0.4 parts of nano-calcium carbonate were introduced, and the mixture was stirred thoroughly for 45 minutes. After cooling to room temperature, a preliminary mixture was obtained. S102. Preparation of spraying liquid Then, the initial mixture is thoroughly mixed with 40 parts of polypropylene emulsion and 80 parts of polytetrafluoroethylene emulsion to obtain the spraying liquid.
[0029] S103. Filter screen coating The filter screen is horizontally placed on the support frame, and then sprayed on both sides of the filter screen using a high-pressure airless sprayer with spray liquid as the raw material. Each side is sprayed 3 times. Then, it is placed at room temperature for 24 hours to obtain an anti-friction coating. Then, it is assembled to prepare the No. 1 outlet filter screen.
[0030] The application was placed in the device used, and the overall pressure drop across the first and second filters was monitored. The usage time when the pressure drop exceeded 1000 Pa was recorded, for a total of 257 hours.
[0031] Example 2: S201. Preliminary mixing Four parts of ultrafine glass fiber were placed in 15 parts of HF solution (mass fraction of 30 wt%), stirred evenly, and then reacted at 50℃ for 40 min. Then, 0.5 parts of nano-calcium carbonate were introduced, and the mixture was stirred thoroughly for 45 minutes. After cooling to room temperature, a preliminary mixture was obtained. S202. Preparation of spraying liquid Then, the initial mixture is thoroughly mixed with 50 parts of polypropylene emulsion and 100 parts of polytetrafluoroethylene emulsion to obtain the spraying liquid.
[0032] S203. Filter screen coating The filter screen is horizontally placed on the support frame, and then sprayed on both sides of the filter screen using a high-pressure airless sprayer with spray liquid as the raw material. Each side is sprayed 5 times. Then, it is placed at room temperature for 36 hours to obtain an anti-friction coating. Then, it is assembled to prepare the No. 2 outlet filter screen.
[0033] The application was placed in the device in which it was used, and the pressure drop of the filter was monitored. The usage time when the pressure drop exceeded 1000 Pa was recorded. A total of 306 hours were used.
[0034] To demonstrate the validity of this application, the following comparative examples are provided: Comparative Example 1: S301. Preliminary mixing Two parts of ultrafine glass fiber were placed in 10 parts of HF solution (20 wt%), stirred evenly, and then reacted at 40°C for 40 min; the mixture was then cooled to room temperature to obtain a preliminary mixture. S302. Preparation of spraying liquid Then, the initial mixture is thoroughly mixed with 40 parts of polypropylene emulsion and 80 parts of polytetrafluoroethylene emulsion to obtain the spraying liquid.
[0035] S303. Filter screen coating The filter screen is horizontally placed on the support frame, and then sprayed on both sides of the filter screen using a high-pressure airless sprayer with spray liquid as the raw material. Each side is sprayed 3 times. Then, it is placed at room temperature for 24 hours to obtain an anti-friction coating. Then, it is assembled to prepare the No. 3 outlet filter screen.
[0036] The application was placed in the device used, and the overall pressure drop on both sides of the first and second filters was monitored. The usage time when the pressure drop exceeded 1000 Pa was recorded, for a total of 182 hours.
[0037] Comparative Example 2: S401. Preliminary mixing Two parts of ultrafine glass fiber were placed in 10 parts of HF solution (20 wt%) and stirred evenly. Then, 0.4 parts of nano-calcium carbonate were introduced and stirred thoroughly to obtain a preliminary mixture. S402. Preparation of spraying liquid Then, the initial mixture is thoroughly mixed with 40 parts of polypropylene emulsion and 80 parts of polytetrafluoroethylene emulsion to obtain the spraying liquid.
[0038] S403. Filter screen coating The filter screen is horizontally placed on the support frame, and then sprayed on both sides of the filter screen using a high-pressure airless sprayer with spray liquid as the raw material. Each side is sprayed 3 times. Then, it is placed at room temperature for 24 hours to obtain an anti-friction coating. Then, it is assembled to prepare the No. 4 outlet filter screen.
[0039] The application was placed in the device used, and the overall pressure drop across the first and second filters was monitored. The usage time when the pressure drop exceeded 1000 Pa was recorded, for a total of 155 hours.
[0040] The various embodiments in this specification are described in a progressive manner. Similar or identical parts between embodiments can be referred to interchangeably. Each embodiment focuses on describing the differences from other embodiments. In particular, the system embodiments are basically similar to the method embodiments, so the description is relatively simple; relevant parts can be referred to the descriptions in the method embodiments.
[0041] The above are merely embodiments of this application and are not intended to limit the scope of this application. Various modifications and variations can be made to this application by those skilled in the art. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of this application should be included within the scope of the claims of this application.
Claims
1. An apparatus for preparing crude hydrocortisone acetate, characterized in that: The device includes a reaction vessel, a first filter screen at the bottom of the reaction vessel, a filter chamber below the first filter screen, a second filter screen in the lower middle part of the filter chamber, a reflux tank at the bottom of the filter chamber via an intermediate transition pipe, an intermediate control valve on the intermediate transition pipe, a flushing pipe on the side of the reflux tank, a backflow pulse pump on the flushing pipe, the other side of the flushing pipe being connected to the filter chamber below the second filter screen, and an outlet pipe at the bottom of the filter chamber.
2. The apparatus for preparing crude hydrocortisone acetate according to claim 1, characterized in that: The first filter screen is a wire mesh filter.
3. The apparatus for preparing crude hydrocortisone acetate according to claim 1, characterized in that: The second filter screen includes a support frame, a central filter membrane is disposed in the middle of the support frame, and external filter screens are disposed on both sides of the central filter membrane.
4. The apparatus for preparing crude hydrocortisone acetate according to claim 3, characterized in that: The middle filter membrane is a polytetrafluoroethylene filter membrane, and the outer filter screen is a wire mesh filter.
5. The apparatus for preparing crude hydrocortisone acetate according to claim 4, characterized in that: An anti-friction layer is provided on the outside of the wire mesh filter.
6. The apparatus for preparing crude hydrocortisone acetate according to claim 5, characterized in that: The anti-friction coating comprises the following substances in parts by weight: Acrylic emulsion: 40-50 parts; Polytetrafluoroethylene emulsion: 80-100 parts; Ultrafine glass fiber; 2-4 parts; HF solution: 10-15 parts, HF mass fraction is 20-30 wt%; Nano calcium carbonate: 0.4-0.5 parts.
7. The apparatus for preparing crude hydrocortisone acetate according to claim 6, characterized in that: Both the acrylic emulsion and the polytetrafluoroethylene emulsion are water-based emulsions.
8. The apparatus for preparing crude hydrocortisone acetate according to claim 6, characterized in that: The ultrafine glass fibers have a diameter of 1-2 μm and a length of 1-3 mm.
9. The apparatus for preparing crude hydrocortisone acetate according to claim 8, characterized in that: The ultrafine glass fiber was placed in an HF solution, stirred evenly, and then reacted at 40-50℃ for 30-40 minutes. Then, nano-calcium carbonate is introduced, and the mixture is stirred thoroughly for 45-60 minutes. After cooling to room temperature, a preliminary mixture is obtained. Then, the preliminary mixture is thoroughly mixed with the polypropylene emulsion and polytetrafluoroethylene emulsion to obtain the spraying liquid.
10. The apparatus for preparing crude hydrocortisone acetate according to claim 9, characterized in that: The filter screen is horizontally placed on the support frame. Then, a high-pressure airless sprayer is used to spray the front and back sides of the filter screen with spray liquid as the raw material. Each side is sprayed no less than 3 times. Then, it is left to cure at room temperature for 24-36 hours to obtain the anti-friction coating.