Method for reducing energy consumption and safety risk during regeneration of artemisinin separated silica gel

Abstract

The invention relates to a method for reducing energy consumption and safety risk during regeneration of artemisinin separated silica gel, belongs to the technical field of artemisinin extraction, and discloses a mixing step: mixing a solvent with waste silica gel; a separation step: carrying out air filter pressing on the material to separate mother liquor adsorbed in the silica gel from the silica gel, and recovering the mother liquor; a cleaning step: cleaning the silica gel, and recovering the solvent; a drying step: performing vacuum drying on the silica gel to obtain dried silica gel; the four steps are integrally completed in a three-in-one silica gel regeneration tank; the silica gel regeneration device has the beneficial effects that silica gel regeneration can be completed by only one main tank body, multiple times of high-temperature heating can be avoided, and the energy consumption is greatly reduced; silica gel and a solvent are transferred in closed equipment, safety risks and solvent consumption are reduced, a safety valve is arranged on the main tank body, potential safety hazards are greatly reduced, repeated carrying can be avoided, manpower is reduced, and economic benefits are greatly increased.

Description

Technical Field

[0001] The invention relates to the technical field of silica gel regeneration, and in particular to a method for reducing energy consumption and safety risks during the regeneration of artemisinin separation silica gel. Background Art

[0002] A large amount of silica gel is needed in the process of separating and extracting artemisinin. Silica gel is a highly active adsorption material, a granular porous silicon dioxide hydrate, mainly used as a desiccant and adsorbent in column chromatography and thin layer chromatography. Its chemical properties are stable and it does not burn. Silica gel as an adsorbent becomes waste silica gel after adsorption saturation. If it is discarded, it will not only waste materials but also pollute the environment. Therefore, the waste silica gel is generally treated in a rotary kiln and reused to achieve the regeneration of silica gel.

[0003] However, the existing cost of silica gel regeneration is very high. This is mainly because the original silica gel is activated in a lump coal kiln. Lump coal is added to the kiln to heat the activation cylinder, which then transfers heat to the material, causing the silica gel to heat up, water to evaporate, and organic matter to burn to achieve the purpose of activation. This method has many disadvantages, mainly small production capacity, high energy consumption, large silica gel loss, environmental pollution, and a high proportion of labor. In particular, the temperature control of silica gel activation and regeneration is difficult to control, especially the choice of fuel and the heating method are difficult to control. Excessive temperature can easily lead to deformation of the silica gel crystals and loss of decolorization function.

[0004] The inventor has previously developed and disclosed an energy-saving silica gel regeneration and activation production system with patent number 2022114413998, which includes a feeding device, a drying device, a regeneration device, a cooling device and a screening device connected in sequence; the drying device includes a drying roller furnace, a drying furnace chamber and a burner, and the regeneration device includes a regeneration roller furnace, a regeneration furnace chamber and a burner. The drying furnace chamber and the regeneration furnace chamber are merged into the same heat-gathering furnace chamber, and the burner is merged into the same combustion heater; the chamber top of the heat-gathering furnace chamber is a curved dome-shaped chamber top, and the inner wall is affixed with a high-temperature resistant heat reflective film; a heat pipe is connected between the chamber top and the transfer bin; the beneficial effect is that the heat-gathering furnace chamber aggregates the drying device and the regeneration device together, combined with the curved dome top design, especially using a heat pipe to introduce heat into the receiving bin to the drying roller furnace and the regeneration roller furnace, and adopts a combination of indirect heating in the furnace chamber and direct heating in the roller furnace, which greatly reduces the required temperature and greatly improves the effective utilization rate of energy.

[0005] After nearly two years of further research and development, the research and development team developed methods that can further reduce energy consumption and reduce safety risks. Summary of the invention

[0006] The technical problem to be solved by the present invention is to provide a three-in-one regeneration method for separating, drying and recycling waste silica gel in order to further reduce energy consumption and safety risks.

[0007] In order to solve the above technical problems, the technical solution adopted by the present invention is a method for reducing energy consumption and safety risks during the regeneration of artemisinin separation silica gel, comprising: ① mixing step: mixing the solvent with the waste silica gel; ② separation step: performing air pressure filtration on the material to separate the mother liquor adsorbed in the silica gel from the silica gel, and recovering the mother liquor; ③ cleaning step: cleaning the silica gel and recovering the solvent; ④ drying step: vacuum drying the silica gel to obtain dry silica gel; the four steps are completed in a three-in-one silica gel regeneration tank; the prior art is to separate separation and drying in different workshops, which consumes energy and labor respectively and faces their own safety risks, while after adopting the three-in-one silica gel regeneration tank, cleaning, separation, recovery and drying can be completed in the same equipment, which greatly reduces energy consumption and safety risks.

[0008] The three-in-one silica gel regeneration tank comprises a column body, a cone body, a dome shell and a driving part; the column body is provided with a column upper flange, a column lower flange, a lifting bracket, an ear plate, a cylinder heat medium ring cavity, and the cylinder heat medium ring cavity is provided with a cylinder heat medium inlet and a cylinder heat medium outlet; the cone body is provided with a cone upper flange, a cone lower flange, a first temperature sensor port, a mother liquid outlet, a solvent outlet, a cone heat medium ring cavity and a chassis, the cone heat medium ring cavity is provided with a cone heat medium inlet and a cone heat medium outlet, and the chassis is provided with a sampling valve port, a heating inlet and an outlet, a small filter liquid port, and a regenerated silica gel outlet; the dome shell is provided with a manhole, a feed port, a rack installation port, a pressure gauge port, a safety valve port, a washing Liquid inlet, cleaning port, observation mirror; the driving part includes a frame, a motor, a transmission, a rotating shaft, and a stirring blade; the upper flange of the column tube is tightly connected to the dome shell by bolts, the lower flange of the column tube is tightly connected to the upper flange of the cone tube by bolts, and the lower flange of the cone tube is tightly connected to the chassis by bolts, and the column tube body, the cone tube body and the dome shell constitute an integral regeneration tank shell; the frame is installed at the frame installation port on the dome shell, the transmission is installed on the frame, the motor is connected to the transmission, the rotating shaft is connected to the transmission and passes through the dome shell into the regeneration tank shell, and the stirring blade is installed on the rotating shaft through a connecting rod, that is, a three-in-one silica gel regeneration tank is constituted.

[0009] The dome shell is also provided with a filter port, and the filter port is provided with a filter.

[0010] The dome shell is also provided with a second washing liquid inlet, a second cleaning port, and a second temperature sensor port.

[0011] The manhole is provided with a second observation mirror and an illuminating lamp.

[0012] The stirring blade is a spiral stirring blade.

[0013] The frame is also provided with a steam interface which passes through the dome shell and is connected to the regeneration tank shell.

[0014] Compared with the prior art, the present invention has the following beneficial effects:

[0015] (1) The existing silica gel regeneration technology is combined from multiple processes that require multiple workshops to a single tank body to complete silica gel regeneration, which can avoid multiple high-temperature heating and greatly reduce energy consumption; when the dried silica gel is regenerated in the activation furnace, the consumption of natural gas is greatly reduced because the silica gel does not contain moisture, which greatly reduces energy consumption;

[0016] (2) The existing silica gel regeneration technology has safety risks in every process. Now it is combined into one tank operation. Both silica gel and solvent are transported in a closed device, reducing safety risks and solvent consumption. A safety valve is installed on the tank, which greatly reduces safety hazards.

[0017] (3) The existing silica gel regeneration technology is combined from multiple processes that require multiple workshops to one total tank to complete the silica gel regeneration, which can avoid multiple handling, reduce labor, and greatly increase economic benefits. BRIEF DESCRIPTION OF THE DRAWINGS

[0018] Figure 1 It is a schematic diagram of the overall side perspective structure of the three-in-one silica gel regeneration tank used in the present invention.

[0019] Figure 2 It is a schematic diagram of the top view of the dome shell in the three-in-one silica gel regeneration tank of the present invention.

[0020] In the figure: 1. Column body, 2. Cone body, 3. Dome shell, 4. Driving member, 101. Lifting bracket, 102. Ear plate, 103. Cylinder heat medium ring cavity, 104. Cylinder heat medium inlet, 105. Cylinder heat medium outlet, 201. Sampling valve port, 202. Heating inlet and outlet, 203. Small filter liquid port, 204. First temperature sensor port, 205. Regenerated silica gel outlet, 206. Mother liquid outlet, 207. Solvent outlet, 208. Cone heat medium ring cavity, 209. Cone heat medium inlet, 210. Conical heat medium outlet, 301. Manhole, 302. Feed port, 303. Rack installation port, 304. Pressure gauge port, 305. Safety valve port, 306. Washing liquid inlet, 307. Cleaning port, 308. Observation mirror, 309. Filter port, 310. Second washing liquid inlet, 311. Second cleaning port, 312. Second temperature sensor port, 313. Filter, 41. Rack, 42. Motor, 43. Transmission, 44. Rotating shaft, 45. Stirring blade, 46. Steam interface. DETAILED DESCRIPTION

[0021] The present invention will be further described below in conjunction with examples. The following examples are intended to illustrate the present invention rather than to further limit the present invention, and should not be used to limit the scope of protection of the present invention.

[0022] The present invention provides a method for reducing energy consumption and safety risks during the regeneration of artemisinin separation silica gel. The existing method comprises: ① mixing step: mixing the solvent with the waste silica gel; ② separation step: performing air pressure filtration on the material to separate the mother liquor adsorbed in the silica gel from the silica gel, and recovering the mother liquor; ③ cleaning step: cleaning the silica gel and recovering the solvent; ④ drying step: vacuum drying the silica gel to obtain dry silica gel; in actual production, the separation work and the drying work are separated and carried out in different workshops, which consume energy and manpower respectively, and face safety risks in each workshop respectively. In this embodiment, the four steps are completed in a three-in-one silica gel regeneration tank; in this way, after adopting the three-in-one silica gel regeneration tank, cleaning, separation, recovery and drying can be completed in the same equipment, which greatly reduces energy consumption and safety risks.

[0023] The three-in-one silica gel regeneration tank comprises a column body 1, a cone body 2, a dome shell 3 and a driving member 4; the column body 1 is provided with a column upper flange, a column lower flange, a lifting bracket 101, an ear plate 102, a cylinder heat medium ring cavity 103, and the cylinder heat medium ring cavity 103 is provided with a cylinder heat medium inlet 104 and a cylinder heat medium outlet 105; the cone body 2 is provided with a cone upper flange, a cone lower flange, a first temperature sensor port 204, a mother liquid outlet 206, a solvent outlet 207, a cone heat medium ring cavity 208 and a bottom plate, and the cone The heat medium ring cavity 208 is provided with a cone heat medium inlet 209 and a cone heat medium outlet 210. The chassis is provided with a sampling valve port 201, a heating inlet and outlet 202, a small filter liquid port 203, and a regenerated silica gel outlet 205; the dome shell 3 is provided with a manhole 301, a feed port 302, a rack installation port 303, a pressure gauge port 304, a safety valve port 305, a washing liquid inlet 306, a cleaning port 307, and an observation mirror 308; the dome shell 3 is also provided with a second washing liquid inlet 310, a second cleaning port 311, The second temperature sensor port 312 and the filter port, the filter port is provided with a filter 313; the manhole 301 is provided with a second observation mirror and a lighting lamp; the driving member 4 includes a frame 41, a motor 42, a transmission 43, a rotating shaft 44, and a stirring blade 45; the stirring blade 45 is a spiral stirring blade; the frame 41 is also provided with a steam interface 46 that passes through the dome shell 3 and connects to the regeneration tank shell; the upper flange of the column is tightly connected to the dome shell 3 by bolts, and the lower flange of the column is connected to the upper flange of the cone The cone lower flange is tightly connected with the chassis by bolts, and the column body 1, the cone body 2 and the dome shell 3 constitute an integral regeneration tank shell; the frame 41 is installed at the frame installation port 303 on the dome shell 3, the transmission 43 is installed on the frame 41, the motor 42 is connected to the transmission 43, the rotating shaft 44 is connected to the transmission 43 and passes through the dome shell 3 into the regeneration tank shell, and the stirring blade 45 is installed on the rotating shaft 44 through a connecting rod, so as to constitute a three-in-one silica gel regeneration tank.

[0024] When using, i.e. regenerating the silica gel for separating artemisinin, the following steps are followed:

[0025] ① Prepare silica gel and molten salt in proportion, and put silica gel from the feed port 302 and molten salt from the washing liquid inlet 306 into the three-in-one silica gel regeneration tank respectively, so that the silica gel and molten salt are mixed into a fluid.

[0026] ② Close all valves, start the motor 42, make the rotating shaft 44 drive the stirring blade 45 to stir the fluid evenly, and set the stirring time.

[0027] ③ After the stirring is completed, the fluid is heated and flashed in the tank; the filter port 309 is opened to allow the oil vapor generated by the flashing to be filtered through the filter 310 and then discharged, thereby obtaining liquid oil storage.

[0028] ④ Close the filter port 309, open the cleaning port 307, and pour clean water into the cleaning port 307 to wash the silica gel and molten salt.

[0029] ⑤ Centrifugally separate the washed silica gel and molten salt; open the regenerated silica gel outlet 205, dry the separated solid silica gel to obtain dry silica gel, and transport the dried silica gel to the activation furnace for regeneration; open the solvent outlet 207, discharge the separated liquid molten salt water mixture through the solvent outlet and evaporate it to remove water, and recover the obtained molten salt.

[0030] This method has the following breakthroughs: (1) Each can of silica gel drying can recover about 1,300 L of solvent; (2) When the dried silica gel is regenerated in the activation furnace, because the silica gel does not contain water, the natural gas consumed per hour is at least 10 cubic meters less than before, which greatly reduces energy consumption; (3) After the original process silica gel is used up, water is used to replace the solvent in the silica gel. The replacement speed is slow and the time is long. After the replacement, there is always solvent residue in the silica gel, exposing the silica gel and the residual solvent to the air for transportation, increasing safety risks and solvent consumption. After the improvement, both silica gel and solvent are transported in closed equipment, reducing safety risks and solvent consumption.

Claims

1. A method for reducing energy consumption and safety risks during the regeneration of artemisinin separation silica gel, comprising: ① Mixing step: mixing the solvent with the waste silica gel; ② Separation step: perform air pressure filtration on the material to separate the mother liquor adsorbed in the silica gel from the silica gel, and recover the mother liquor; ③ Cleaning step: clean the silica gel and recover the solvent; ④ Drying step: vacuum dry the silica gel to obtain dry silica gel; the characteristic is that the four steps are completed in one three-in-one silica gel regeneration tank.

2. The method for reducing energy consumption and safety risks during regeneration of artemisinin separation silica gel according to claim 1, characterized in that The three-in-one silica gel regeneration tank comprises a column body, a cone body, a dome shell and a driving part; the column body is provided with a column upper flange, a column lower flange, a lifting bracket, an ear plate, a cylinder heat medium ring cavity, and the cylinder heat medium ring cavity is provided with a cylinder heat medium inlet and a cylinder heat medium outlet; the cone body is provided with a cone upper flange, a cone lower flange, a first temperature sensor port, a mother liquid outlet, a solvent outlet, a cone heat medium ring cavity and a chassis, the cone heat medium ring cavity is provided with a cone heat medium inlet and a cone heat medium outlet, and the chassis is provided with a sampling valve port, a heating inlet and an outlet, a small filter liquid port, and a regenerated silica gel outlet; the dome shell is provided with a manhole, a feed port, and a rack mounting port , pressure gauge port, safety valve port, washing liquid inlet, cleaning port, observation mirror; the driving part includes a frame, a motor, a transmission, a rotating shaft, and a stirring blade; the upper flange of the column cylinder is tightly connected to the dome shell by bolts, the lower flange of the column cylinder is tightly connected to the upper flange of the cone cylinder by bolts, and the lower flange of the cone cylinder is tightly connected to the chassis by bolts to form an integral regeneration tank shell; the frame is installed at the frame installation port on the dome shell, the transmission is installed on the frame, the motor is connected to the transmission, the rotating shaft is connected to the transmission and passes through the dome shell into the regeneration tank shell, and the stirring blade is installed on the rotating shaft through a connecting rod.

3. The method for reducing energy consumption and safety risks during regeneration of artemisinin separation silica gel according to claim 2, characterized in that The dome shell is also provided with a filter port, and the filter port is provided with a filter.

4. The method for reducing energy consumption and safety risks during regeneration of artemisinin separation silica gel according to claim 3, characterized in that The dome shell is also provided with a second washing liquid inlet, a second cleaning port, and a second temperature sensor port.

5. The method for reducing energy consumption and safety risks during regeneration of artemisinin separation silica gel according to claim 4, characterized in that The manhole is provided with a second observation mirror and an illuminating lamp.

6. The method for reducing energy consumption and safety risks during regeneration of artemisinin separation silica gel according to claim 5, characterized in that The stirring blade is a spiral stirring blade.

7. The method for reducing energy consumption and safety risks during regeneration of artemisinin separation silica gel according to claim 6, characterized in that The frame is also provided with a steam interface which passes through the dome shell and is connected to the regeneration tank shell.

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