CN111001364A - Online monitoring intelligent high-low temperature reaction kettle - Google Patents
Online monitoring intelligent high-low temperature reaction kettle Download PDFInfo
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- CN111001364A CN111001364A CN201911314112.3A CN201911314112A CN111001364A CN 111001364 A CN111001364 A CN 111001364A CN 201911314112 A CN201911314112 A CN 201911314112A CN 111001364 A CN111001364 A CN 111001364A
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- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
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- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0006—Controlling or regulating processes
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0006—Controlling or regulating processes
- B01J19/0013—Controlling the temperature of the process
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- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
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- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00051—Controlling the temperature
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- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00162—Controlling or regulating processes controlling the pressure
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- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
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- B01J2219/00177—Controlling or regulating processes controlling the pH
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- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
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- B01J2219/00186—Controlling or regulating processes controlling the composition of the reactive mixture
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Abstract
The invention discloses an online monitoring intelligent high-low temperature reaction kettle, which relates to the technical field of new energy chemical material production, and comprises a reaction kettle body, wherein a reaction kettle jacket is arranged on the outer side of the reaction kettle body, a condensation coil pipe in the kettle is arranged in the middle of the reaction kettle body, and a flow baffle plate is arranged on the inner wall of the reaction kettle body. The structure is more reasonable, and the design is more optimized.
Description
Technical Field
The invention relates to the technical field of new energy chemical material production, in particular to an online monitoring intelligent high-low temperature reaction kettle.
Background
The transformation and upgrade speed of traditional material enterprises is accelerated. 80-90% of the material enterprises in China are traditional metal and chemical material enterprises, and the two types of enterprises have the largest market share and are the leading strength of the material industry. The development direction of transformation and upgrading of metal material enterprises is to vigorously develop special metal materials such as high-purity metal, amorphous alloy and the like, and high-quality special steel which can be used for nuclear power, supercritical thermal power, ocean engineering, automobile engineering and rail transit; the development direction of transformation and upgrading of chemical material enterprises mainly comprises synthetic rubber, engineering plastics, organosilicon materials and fluorine materials. The development of new material industry is not free from the research and development of new materials.
At present, most of research and development of new materials come from material synthesis, so a reaction kettle is often required to process the new materials, but the existing reaction kettle is not reasonable in structure and optimized in design, and certain inconvenience is brought to people.
Therefore, the person skilled in the art provides an online monitoring intelligent high-low temperature reaction kettle to solve the problems mentioned in the background art.
Disclosure of Invention
The invention aims to provide an online monitoring intelligent high-low temperature reaction kettle, which aims to solve the problems that most of the existing research and development of new materials in the background art are from material synthesis, so that the existing reaction kettle is often required to process, but the existing reaction kettle is not reasonable in structure and optimized in design, and certain inconvenience is brought to people.
In order to achieve the purpose, the invention provides the following technical scheme:
an intelligent high-low temperature reaction kettle capable of being monitored online comprises a reaction kettle body, wherein a reaction kettle jacket is arranged on the outer side of the reaction kettle body, an in-kettle condensing coil pipe is arranged in the middle of the inner part of the reaction kettle body, a flow baffle plate is arranged on the inner wall of the reaction kettle body, an overflow port is arranged at the upper end of one side of the reaction kettle body, a strip-shaped window is arranged on the surface of the reaction kettle body, a discharge port is arranged in the middle of the lower end of the reaction kettle body, a double-layer jacket kettle cover is arranged at the upper end of the reaction kettle body, a mechanical sealing bearing is arranged in the middle of the upper end of the double-layer jacket kettle cover, a stirring motor is arranged at the upper end of the mechanical sealing bearing, a feed port is arranged on the surface of the double-layer jacket kettle cover, a visible quartz window is arranged at the upper end of, a PH meter detection port is arranged on one side of the sampling port, an air inlet is arranged on one side of the PH meter detection port, a pressure gauge is arranged on one side of the air inlet, a disc type condensation reflux device is arranged at the lower end of the surface of the double-layer jacket kettle cover, a condensation reflux device liquid inlet, a condensation reflux device air outlet and a condensation reflux device liquid outlet are respectively arranged on the surface of the disc type condensation reflux device, a pressure detection port is arranged on the other side of the visible quartz window, an air outlet is arranged on one side of the pressure detection port, a cleaning port is arranged on one side of the air outlet, a temperature detection port is arranged on one side of the cleaning port, an oxygen partial pressure detection port is arranged on one side of the temperature detection port, a stirring paddle is arranged in the middle of the condensation coil pipe in the kettle, a jacket liquid outlet is arranged at the upper end of one side of the reaction kettle, the pressure detection port is connected with a feed pump through a pipeline, the lower end of the feed pump is provided with a storage barrel, the lower end of the storage barrel is provided with a stainless steel rack, a control cabinet is arranged inside the stainless steel rack, the control cabinet is electrically connected with a control center, and the feed pump is electrically connected with an alarm.
As a preferred embodiment of the present invention: the flow baffle is fixed on the kettle wall of the reaction kettle body through welding, and the flow baffle is 2-8 pieces, the flow baffle is 0.01-0.1 times of the kettle diameter away from the inner wall of the reaction kettle body, the width of the flow baffle is 0.01-0.3 times of the kettle diameter, the height of the flow baffle is 0.2-0.9 times of the kettle height, the welding angle of the flow baffle and the reaction kettle body is 0-90 degrees, the side surface of the flow baffle is provided with an overflow port, the number of the flow baffle is 1-3 from top to bottom, and the bottom of the flow baffle is provided with a discharge port.
As a preferred embodiment of the present invention: the inner diameter of the condensation coil pipe in the kettle is 0.02-0.05 times of the diameter of the kettle, the upper and lower spacing distance between the pipe and the condensation coil pipe is 0.02-0.05 times of the height of the kettle, the number of the winding turns of the condensation coil pipe in the kettle is 10-25, the diameter of the whole coil pipe after the condensation coil pipe is coiled is 0.2-0.8 times of the diameter of the kettle, and the height of the condensation coil pipe is 0.2-0.9 times of the height of the kettle.
As a preferred embodiment of the present invention: the inner diameter of a pipe used by the coil pipe in the disc type condensation reflux device is 0.02-0.05 times of the diameter of the kettle, the vertical spacing distance between the pipe and the pipe is 0.01-0.02 times of the height of the kettle, the number of turns of the coil pipe is 5-10, the diameter of the whole coil pipe is 0.1-0.3 times of the diameter of the kettle after the coil pipe is coiled, and the height of the whole coil pipe is 0.1-0.3 times of the height of the kettle.
As a preferred embodiment of the present invention: the double-layer jacket kettle cover is internally provided with water, the temperature is-30-300 ℃, the number of feed inlets on the double-layer jacket kettle cover is 3-10, the number of temperature detection ports is 1-2, the number of pressure detection ports on the pressure detection ports is 1-2, and the number of visible quartz windows is 1-2.
As a preferred embodiment of the present invention: the stirring rake is 2 ~ 3, and is anchor formula, turbine formula and three leaf oblique oars respectively.
As a preferred embodiment of the present invention: the storage vat is 3 ~ 10, and the material is 316L stainless steel.
As a preferred embodiment of the present invention: and the bottom of the stainless steel frame is fixedly provided with a caster.
Compared with the prior art, the invention has the beneficial effects that:
1. according to the online monitoring intelligent high-low temperature reaction kettle, due to the fact that the control system is designed, the temperature, the rotating speed, the PH value, the rotating speed of a peristaltic pump, the feeding speed, the oxygen partial pressure and the pressure of various materials of the reaction kettle can be conveniently and rapidly set and controlled, the PH value in the reaction kettle can be constant through the automatic PH control system, the reaction is guaranteed to be stably and automatically carried out, manual adjustment or supervision of a person is not needed, time and labor are saved, particularly, through the automatic alarm system, when any one or more of the temperature, the PH value or the pressure value cannot meet the environmental requirements of the experimental process, an experiment is automatically suspended, and an alarm is given to remind an operator, so that the situation that the error is brought to an experimental result by an improper experimental environment, even danger is generated, and improper life and property losses are caused to enterprises;
2. according to the intelligent high-low temperature reaction kettle with the online monitoring function, the designed condensation coil and the flow baffle can enable solution in the reaction kettle to be uniformly mixed and dispersed in the whole kettle body, meanwhile, the heat preservation solution in the coil can keep an experiment temperature environment, crystal nuclei can grow uniformly, an expected ideal product can be obtained in a stable experiment environment range through the adjustment of the rotating speed, the temperature and the PH and the alarm system, the circulating heat preservation solution is introduced into all jackets through the design of the double-layer jacket kettle body and the double-layer jacket kettle cover, and the whole reaction kettle is completely covered by the circulating heat preservation solution, so that the reaction process can be completely carried out in an ideal temperature environment;
3. the invention relates to an online monitoring intelligent high-low temperature reaction kettle, which is provided with a disc type condensation reflux device, wherein reaction gas generated by gasification in the reaction process can be liquefied when meeting cold and flows back into the reaction kettle, so that the material loss is prevented, the environment is protected, harmful gas generated in the reaction is prevented from flowing outwards, an overflow port can control the liquid level height and the growth trend in the kettle, an air inlet and an air outlet and oxygen partial pressure ensure the gas composition in the kettle, the pressure design ensures certain negative pressure or positive pressure, the reaction kettle can also be used for working in a low-temperature environment, the low-temperature reaction is ensured after cooling liquid is introduced, the online monitoring intelligent high-low temperature reaction kettle is suitable for producing oxidized graphene and various substances needing to be produced in the high-low temperature environment.
Drawings
Other features, objects and advantages of the invention will become more apparent upon reading of the detailed description of non-limiting embodiments with reference to the following drawings:
FIG. 1 is a schematic structural diagram of an online monitoring intelligent high-low temperature reaction kettle;
FIG. 2 is a schematic assembly diagram of an online monitoring intelligent high-low temperature reaction kettle;
FIG. 3 is a top view of an online monitoring intelligent high-low temperature reaction kettle;
in the figure: 1-a reaction kettle body; 2-reaction kettle jacket; 3-condensing coil pipe in the kettle; 4-flow baffle; 5-an overflow port; 6-bar window; 7-a discharge opening; 8-double-layer jacket kettle cover; 9-a feed inlet; 10-an air inlet; 11-gas outlet; 12-a PH meter detection port; 13-temperature detection port; 14-a pressure detection port; 15-oxygen partial pressure detection port; 16-a sampling port; 17-a pressure relief port; 18-a cleaning port; 19-visible quartz window; 20-pressure gauge; 21-a tray condensate reflux vessel; 22-a stirring motor; 23-mechanical seal bearings; 24-a stirring paddle; 25-jacket liquid inlet; 26-jacketed liquid outlet; 27-a kettle cover sealing device; 28-a control center; 29-an alarm; 30-a storage barrel; 31-stainless steel frame; 32-a feed pump; 33-control cabinet.
Detailed Description
Referring to fig. 1 to 3, in the embodiment of the invention, an online monitoring intelligent high and low temperature reaction kettle comprises a reaction kettle body 1, a reaction kettle jacket 2 is arranged on the outer side of the reaction kettle body 1, an in-kettle condensing coil 3 is arranged in the middle of the reaction kettle body 1, a flow baffle plate 4 is arranged on the inner wall of the reaction kettle body 1, an overflow port 5 is arranged at the upper end of one side of the reaction kettle body 1, a strip-shaped window 6 is arranged on the surface of the reaction kettle body 1, a discharge port 7 is arranged in the middle of the lower end of the reaction kettle body 1, a double-layer jacket kettle cover 8 is arranged at the upper end of the reaction kettle body 1, 1 to 3 overflow ports 5 are arranged on the side surface, the double-layer kettle cover 8 is welded on a kettle jacket layer, the strip-shaped window 6 is convenient for observing the liquid level and color change of reactants in the kettle, is convenient for controlling the liquid level height and product morphology, a discharge port 7, the middle part of the upper end of a double-layer jacket kettle cover 8 is provided with a mechanical seal bearing 23, the upper end of the mechanical seal bearing 23 is provided with a stirring motor 22, the stirring motor 22 has a stirring speed of 0-1400 rpm/min, stirring is driven by the mechanical seal bearing 23, 1-3 stirring paddles 24 can be arranged and are anchor type, turbine type or propeller type impellers, the surface of the double-layer jacket kettle cover 8 is provided with a feed inlet 9, the upper end of the surface of the double-layer jacket kettle cover 8 is provided with a visible quartz window 19, the kettle cover is provided with 3-10 feed inlets 9 to meet feeding requirements of different requirements, 1 air inlet 10 realizes mixing and introducing of different gases, 1 air outlet 11 and 1 PH meter detection port 12, the measurement range of the PH meter is 0-14, 1-2 temperature detection ports 13 are convenient to determine whether the temperature distribution in the kettle is even, 1-2 pressure detection ports 14 and 1 oxygen partial pressure detection port 15, the oxygen partial pressure detection range is 0-30%, 1 sampling port 16 is directly communicated with the bottom of the reaction kettle, 1 pressure relief port 17 is used for reducing the pressure, a cleaning port 18 is convenient for cleaning the interior of the reaction kettle after the reaction is finished, 1-2 visible quartz windows 19 are convenient for observing the reaction condition of materials in the reaction kettle from different positions, one side of each visible quartz window 19 is provided with the pressure relief port 17, one side of each pressure relief port 17 is provided with the sampling port 16, one side of each sampling port 16 is provided with a PH meter detection port 12, one side of each PH meter detection port 12 is provided with an air inlet 10, one side of each air inlet 10 is provided with a pressure gauge 20 and 1 kettle internal pressure indicator 20 for checking the pressure detectors, the detected kettle internal pressure is a considerable actual value, the inner diameter of a pipe used by the coil pipe is 0.02-0.05 times of the diameter of the kettle, and the vertical spacing distance between the pipe and the kettle is 0.01-0.02 times of the height, the number of turns of coiled pipe is 5-10, the diameter of the whole coiled pipe is 0.1-0.3 times of the diameter of the kettle after the coiled pipe is coiled, the lower end of the surface of a double-layer jacket kettle cover 8 is provided with a disc type condensation reflux device 21, the surface of the disc type condensation reflux device 21 is respectively provided with a condensation reflux device liquid inlet, a condensation reflux device gas outlet and a condensation reflux device liquid outlet, the height of the disc type condensation reflux device 21 is 0.1-0.3 times of the height of the kettle, various gases generated in the reaction process can be effectively condensed and refluxed into the reaction kettle, so that the materials can be saved, harmful gases can be prevented from entering air to pollute the atmosphere, the health is influenced, the other side of a visible quartz window 19 is provided with a pressure detection port 14, one side of the pressure detection port 14 is provided with a gas outlet 11, one side of the gas outlet 11 is provided with a cleaning port 18, one side of the cleaning port 18 is provided, a jacket liquid outlet 26 is arranged at the upper end of one side of the reaction kettle body 1, a jacket liquid inlet 25 is arranged at the lower end of one side of the reaction kettle body 1, a kettle cover sealing device 27 is arranged between the reaction kettle body 1 and the double-layer jacket kettle cover 8, the pressure detection port 14 is connected with a feed pump 32 through a pipeline, reaction materials can be pumped into the reaction kettle for reaction at a set speed of 0-4L/min through the feed pump 32, a material storage barrel 30 and 3-10 material storage barrels 30 are arranged at the lower end of the feed pump 32 and used for storing different materials needing to participate in the reaction and are placed on a stainless steel frame 31 according to feeding requirements, a stainless steel frame 31 is arranged at the lower end of the material storage barrel 30, a control cabinet 33 and a control cabinet 33 are arranged in the stainless steel frame 31, the waterproof control cabinet is adopted, all components needed by a control center 28 are integrated, the waterproof control cabinet, the control cabinet 33 is electrically connected with the control center 28, and automatically controls the PH system: the amount of acid or alkali is fixed, and the other one is adjusted to promote the display and control and automatic alarm system of constant PH, temperature, rotating speed, feeding speed, oxygen partial pressure, kettle cover lifting and the like: the alarm temperature, the PH value and the pressure value are set randomly, when the detected temperature data, the detected PH data or the detected pressure data exceed the set values, the system sends out a buzzing alarm sound to flash red light, meanwhile, feeding is stopped automatically, the system is in a pause state, and the system cannot continue to operate until the alarm is relieved or closed, the two systems are integrated in the control center 28, the feeding pump 32 is electrically connected with the alarm 29, and the alarm 29 provides visual and audible alarms.
In this embodiment (please refer to fig. 1 and fig. 2), the flow baffle 4 is fixed on the kettle wall of the reaction kettle body 1 by welding, and there are 2 to 8 flow baffle 4, the distance between the flow baffle 4 and the inner wall of the reaction kettle body 1 is 0.01 to 0.1 times of the kettle diameter, the width of the flow baffle 4 is 0.01 to 0.3 times of the kettle diameter, the height of the flow baffle 4 is 0.2 to 0.9 times of the kettle height, the welding angle between the flow baffle 4 and the reaction kettle body 1 is 0 to 90 degrees, and the side surface is provided with the overflow port 5, the number of the flow baffle 4 is 1 to 3 from top to bottom, and the bottom is provided with the discharge port.
The inner diameter of an inner pipe welded in the kettle is 0.02-0.05 times of the diameter of the kettle, the vertical spacing distance between the pipes is 0.02-0.05 times of the height of the kettle, the number of coiled coils is 10-25, the diameter of the whole coiled pipe is 0.2-0.8 times of the diameter of the kettle after the coiled pipe is coiled, a condensing coiled pipe 3 with the height of 0.2-0.9 times of the height of the kettle is welded on the wall of the kettle, 2-8 straight flow baffles 4 are welded on the wall of the kettle, the diameter of the kettle is 0.01-0.1 times of the diameter of the kettle, the width of the straight flow baffles is 0.01-0.3 times of the diameter of the kettle, the height of the straight flow baffles is 0.2-0.9 times of the height of the kettle, the straight flow baffles are uniformly distributed at an angle of 0-90 degrees with the welding angle of the reaction kettle, the straight flow baffles are provided with 1-3 material overflowing ports 5 from top to bottom on the side surfaces, the straight flow baffles are welded on the kettle jacket layer, a strip-shaped window 6 for observing.
In this embodiment (see fig. 1 and 2), the inner diameter of the pipe of the condensation coil 3 in the kettle is 0.02-0.05 times of the diameter of the kettle, the vertical spacing distance between the pipes is 0.02-0.05 times of the height of the kettle, the number of turns of the condensation coil 3 in the kettle is 10-25, and the diameter of the whole coil after being coiled is 0.2-0.8 times of the diameter of the kettle and the height is 0.2-0.9 times of the height of the kettle.
Wherein, the kettle is covered with 3-10 feed inlets 9 to meet the feeding requirements of different requirements, 1 air inlet 10 to realize the mixed introduction of different gases, 1 air outlet 11, 1 PH meter detection port 12, the measurement range of the PH meter is 0-14, 1-2 temperature detection ports 13 to determine whether the temperature distribution in the kettle is uniform, 1-2 pressure detection ports 14, 1 oxygen partial pressure detection port 15, the oxygen partial pressure detection range is 0-30%, 1 sampling port 16 directly passing through the bottom of the reaction kettle, 1 pressure relief port 17 for preventing the pressure in the reaction kettle from being too large, a cleaning port 18 convenient for cleaning the interior of the kettle after the reaction is finished, 1-2 visual quartz windows 19 to facilitate the observation of the reaction condition of the materials in the kettle from different positions, 1 kettle pressure indicator 20 for calibrating the pressure detector to ensure that the detected pressure in the kettle is a considerable actual value, the inner diameter of the pipe used by the coil pipe is 0.02-0.05 times of the diameter of the kettle, the vertical spacing distance between the pipes is 0.01-0.02 times of the height of the kettle, the number of coil pipe coiling turns is 5-10, and the diameter of the whole coil pipe is 0.1-0.3 times of the diameter of the kettle after the coil pipe is coiled.
In this embodiment (see fig. 1 and fig. 2), the inner diameter of the pipe used by the coil in the disc-type condensate reflux device 21 is 0.02-0.05 times of the diameter of the kettle, the vertical spacing distance between the pipes is 0.01-0.02 times of the height of the kettle, the number of coil turns is 5-10, the diameter of the whole coil after being coiled is 0.1-0.3 times of the diameter of the kettle, and the height is 0.1-0.3 times of the height of the kettle.
Wherein, highly be the disc condensation return-flow ware 21 of cauldron height 0.1 ~ 0.3 times, effectually with all kinds of gaseous condensation backward flows to reation kettle that produce among the reaction sequence in, can save the material can prevent again that harmful gas from getting into the air in the polluted atmosphere, influence healthyly.
In this embodiment (see fig. 1 and fig. 2), water is disposed inside the double-layer jacket kettle cover 8, and the temperature is-30 ℃ to 300 ℃, the number of the feed ports 9 on the double-layer jacket kettle cover 8 is 3 to 10, the number of the temperature detection ports 13 is 1 to 2, the number of the pressure detection ports 14 on the pressure detection ports 14 is 1 to 2, and the number of the visible quartz windows 19 is 1 to 2.
Wherein, the cooling or heating mode of the water in the double-layer jacket kettle cover 8 is circulating environment-friendly temperature liquid.
In the present embodiment (see fig. 1 and fig. 2), the number of the stirring paddles 24 is 2-3, and the stirring paddles are respectively an anchor type, a turbine type, and a three-blade inclined paddle.
Wherein, the stirring speed of the stirring motor 22 is 0-1400 rpm/min, the stirring is driven by the mechanical seal bearing 23, 1-3 stirring paddles 24 can be arranged, and are anchor type, turbine type and propeller type impellers, the liquid inlet 25 of the kettle jacket is arranged, and the medium of the heating or cooling device is water, oil or liquid nitrogen.
In this embodiment (please refer to fig. 1 and fig. 2), the storage tanks 30 are 3-10 and made of 316L stainless steel.
Wherein, 3 ~ 10 storage tanks 30 are used for storing different materials that need participate in the reaction.
In this embodiment (see fig. 1 and fig. 2), casters are fixedly mounted at the bottom of the stainless steel frame 31.
Wherein, the bottom of the stainless steel frame 31 is fixedly provided with casters to move the equipment.
It is to be noted that the invention is an online monitoring intelligent high-low temperature reaction kettle, which comprises a reaction kettle body 1, a reaction kettle jacket 2, an in-kettle condensing coil 3, a flow baffle 4, an overflow port 5, a strip-shaped window 6, a discharge port 7, a double-layer jacket kettle cover 8, a feed inlet 9, an air inlet 10, an air outlet 11, a pH meter detection port 12, a temperature detection port 13, a pressure detection port 14, an oxygen partial pressure detection port 15, a sampling port 16, a pressure relief port 17, a cleaning port 18, a visible quartz window 19, a pressure gauge 20, a disc type condensing reflux device 21, a stirring motor 22, a mechanical seal bearing 23, a stirring paddle 24, a jacket liquid inlet 25, a jacket liquid outlet 26, a kettle cover sealing device 27, a control center 28, an alarm 29, a material storage bucket 30, a stainless steel frame 31, a feed pump 32 and a control cabinet 33, wherein the components are all common standard components or components known by technicians in the field, the structure and principle are known to the skilled person through technical manuals or through routine experimentation.
The working principle of the invention is as follows: when the reaction kettle works, for preparing the entecavir intermediate, a user injects (3R, 4S) -4-benzyloxy-3-methylene benzyloxy-2- (2, 2-dimethyl- [1,3] -dioxolane) -cyclopentadienyl alcohol), triphenylphosphine, anhydrous tetrahydrofuran concentrated hydrochloric acid, a tetrahydrofuran solution of diethyl azodicarboxylate (DEAD), anhydrous methanol, a sodium periodate aqueous solution, sodium borohydride, dichloromethane, 4-dimethylamino pyridine and methylsulfonyl chloride into different liquid storage barrels 30 respectively, covers the kettle body 1, heats and dissolves the mixture, connects a feed pump 32 with a feed port 9 under the protection of nitrogen gas through a gas inlet 7, adds (3R, 4S) -4-benzyloxy-3-methylene benzyloxy-2- (2, 2-dimethyl- [1,3] -dioxolane) -cyclopentadienyl alcohol), triphenylphosphine and anhydrous tetrahydrofuran concentrated hydrochloric acid are stirred for 1 hour, then tetrahydrofuran solution of diethyl azodicarboxylate (DEAD) is dripped, after the reaction is finished, a 4A molecular sieve is added through a visible quartz window 19, the temperature is raised and stirred for 12 hours, after the complete reaction, the product A is obtained through column chromatography separation, the product A and the anhydrous ethanol are added into a kettle body 1, the concentrated hydrochloric acid is dripped into the kettle body at room temperature, the reaction is stirred for 3 hours, the solvent is removed under reduced pressure at the room temperature, the residue is dissolved by adding the anhydrous methanol, the temperature is reduced to 0 ℃, the stirring is carried out, the aqueous solution of sodium iodate is slowly added, the dropwise addition is finished, the stirring is carried out for 2 hours, sodium borohydride is added, the stirring is carried out at the room temperature for 2 hours, the product B is obtained through filtering, rotary evaporation and column chromatography separation, dichloromethane is added into, introducing nitrogen into the product B and 4-dimethylaminopyridine, stirring, reducing the reaction temperature to 0 ℃, dropwise adding methylsulfonyl chloride, stirring at 0 ℃ for 1 hour, heating to room temperature, stirring for 3 hours, adding a dichloromethane dilution system, washing, separating liquid, filtering, performing rotary evaporation on the filtrate, performing column chromatography separation and the like to obtain the entecavir intermediate. After the reaction is finished, the control center 28 is closed, the air guide pipe, the PH meter, the oxygen detector and the charging pipe are removed, the kettle cover is opened, the kettle cover is lifted, and the discharge opening 7 is opened for discharging and cleaning. For preparing the nano catalyst CdS/g-C3N4 at low temperature, a user respectively stores deionized water and absolute ethyl alcohol in different storage barrels 30, connects a feed pump 32 and a feed inlet 9, firstly puts calcium chloride powder into a reaction kettle body 1 through a visible quartz window 19, then adds the deionized water and the absolute ethyl alcohol into the reaction kettle body 1 through the feed pump 32 and the feed inlet 9, stirs until the deionized water and the absolute ethyl alcohol are completely dissolved, then, carbon nitride is dispersed and arranged in the prepared cadmium chloride solution for 90 minutes by ultrasonic treatment, the temperature is set to-20 ℃, the mixture is stirred for 60 minutes, simultaneously, the sodium sulfide solution is prepared on another same device by the same steps and the same mode, finally the sodium sulfide solution is dripped into the cadmium chloride solution by setting a speed through a feeding pump 32, stirring for 90 minutes, carrying out suction filtration at low temperature, washing and drying to finally obtain the nano catalyst CdS/g-C3N 4. After the reaction is finished, the control center 28 is closed, the air guide pipe, the PH meter, the oxygen detector and the charging pipe are removed, the kettle cover is opened, the kettle cover is lifted, and the discharge opening 7 is opened for discharging and cleaning.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention are equivalent to or changed within the technical scope of the present invention.
Claims (8)
1. An online monitoring intelligent high-low temperature reaction kettle comprises a reaction kettle body (1) and is characterized in that a reaction kettle jacket (2) is arranged on the outer side of the reaction kettle body (1), a condensation coil pipe (3) in the kettle is arranged in the middle of the reaction kettle body (1), a flow baffle plate (4) is arranged on the inner wall of the reaction kettle body (1), an overflow port (5) is arranged at the upper end of one side of the reaction kettle body (1), a bar-shaped window (6) is arranged on the surface of the reaction kettle body (1), a discharge port (7) is arranged in the middle of the lower end of the reaction kettle body (1), a double-layer jacket kettle cover (8) is arranged at the upper end of the reaction kettle body (1), a mechanical sealing bearing (23) is arranged in the middle of the upper end of the double-layer jacket kettle cover (8), a stirring motor (22) is arranged at the upper end of the mechanical sealing bearing (23), a feed inlet (9) is, the surface upper end of the double-layer jacket kettle cover (8) is provided with a visible quartz window (19), one side of the visible quartz window (19) is provided with a pressure relief port (17), one side of the pressure relief port (17) is provided with a sampling port (16), one side of the sampling port (16) is provided with a PH meter detection port (12), one side of the PH meter detection port (12) is provided with an air inlet (10), one side of the air inlet (10) is provided with a pressure gauge (20), the surface lower end of the double-layer jacket kettle cover (8) is provided with a disc type condensation reflux device (21), the surface of the disc type condensation reflux device (21) is respectively provided with a condensation reflux device liquid inlet, a condensation reflux device air outlet and a condensation reflux device liquid outlet, the other side of the visible quartz window (19) is provided with a pressure detection port (14), and one side of the, a cleaning port (18) is arranged on one side of the gas outlet (11), a temperature detection port (13) is arranged on one side of the cleaning port (18), an oxygen partial pressure detection port (15) is arranged on one side of the temperature detection port (13), a stirring paddle (24) is arranged in the middle of the condensing coil pipe (3) in the kettle, a jacket liquid outlet (26) is arranged at the upper end of one side of the reaction kettle body (1), a jacket liquid inlet (25) is arranged at the lower end of one side of the reaction kettle body (1), a kettle cover sealing device (27) is arranged between the reaction kettle body (1) and the double-layer jacket kettle cover (8), the pressure detection port (14) is connected with a feed pump (32) through a pipeline, a storage barrel (30) is arranged at the lower end of the feed pump (32), a stainless steel frame (31) is arranged at the lower end of the storage barrel (30), a control cabinet (, the control cabinet (33) is electrically connected with a control center (28), and the feeding pump (32) is electrically connected with an alarm (29).
2. The online monitoring intelligent high-low temperature reaction kettle according to claim 1, wherein the flow baffle plate (4) is fixed on the kettle wall of the reaction kettle body (1) by welding, the number of the flow baffle plate (4) is 2-8, the distance between the flow baffle plate (4) and the inner wall of the reaction kettle body (1) is 0.01-0.1 times of the kettle diameter, the width of the flow baffle plate (4) is 0.01-0.3 times of the kettle diameter, the height of the flow baffle plate (4) is 0.2-0.9 times of the kettle height, the welding angle between the flow baffle plate (4) and the reaction kettle body (1) is 0-90 degrees, the side surface of the flow baffle plate is provided with overflow ports (5), the number of the flow baffle plate (4) is 1-3 from top to bottom, and the bottom of the flow baffle plate is provided with discharge ports.
3. The intelligent high-low temperature reaction kettle with the online monitoring function as claimed in claim 1, wherein the inner diameter of the pipe of the condensation coil pipe (3) in the kettle is 0.02-0.05 times of the diameter of the kettle, the distance between the pipe and the pipe is 0.02-0.05 times of the height of the kettle, the number of turns of the condensation coil pipe (3) in the kettle is 10-25, the diameter of the whole coil pipe after being turned up is 0.2-0.8 times of the diameter of the kettle, and the height of the whole coil pipe is 0.2-0.9 times of the height of the kettle.
4. The online monitoring intelligent high-low temperature reaction kettle according to claim 1, wherein the inner diameter of a pipe used by a coil pipe in the disc type condensation reflux device (21) is 0.02-0.05 times of the diameter of the kettle, the vertical spacing distance between the pipe and the pipe is 0.01-0.02 times of the height of the kettle, the number of coil pipe coiling turns is 5-10, the diameter of the whole coil pipe after coiling is 0.1-0.3 times of the diameter of the kettle, and the height of the whole coil pipe is 0.1-0.3 times of the height of the kettle.
5. The online monitoring intelligent high-low temperature reaction kettle according to claim 1, wherein water is arranged inside the double-layer jacket kettle cover (8), the temperature is-30 ℃ to 300 ℃, the number of the feed inlets (9) on the double-layer jacket kettle cover (8) is 3 to 10, the number of the temperature detection ports (13) is 1 to 2, the number of the pressure detection ports (14) is 1 to 2, and the number of the visible quartz windows (19) is 1 to 2.
6. The on-line monitoring intelligent high-low temperature reaction kettle according to claim 1, wherein the number of the stirring paddles (24) is 2-3, and the stirring paddles are respectively an anchor type, a turbine type and a three-blade inclined paddle.
7. The on-line monitoring intelligent high-low temperature reaction kettle as claimed in claim 1, wherein the number of the material storage barrels (30) is 3-10, and the material is 316L stainless steel.
8. The on-line monitoring intelligent high-low temperature reaction kettle according to claim 1, wherein casters are fixedly mounted at the bottom of the stainless steel frame (31).
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| Application Number | Priority Date | Filing Date | Title |
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| CN201911314112.3A CN111001364A (en) | 2019-12-19 | 2019-12-19 | Online monitoring intelligent high-low temperature reaction kettle |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201911314112.3A CN111001364A (en) | 2019-12-19 | 2019-12-19 | Online monitoring intelligent high-low temperature reaction kettle |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113477204A (en) * | 2021-07-14 | 2021-10-08 | 南京延长反应技术研究院有限公司 | Mixing device |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113477204A (en) * | 2021-07-14 | 2021-10-08 | 南京延长反应技术研究院有限公司 | Mixing device |
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