CN112717455A - Rectification separation device and method for 2-cyanopyridine bottom material - Google Patents
Rectification separation device and method for 2-cyanopyridine bottom material Download PDFInfo
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- CN112717455A CN112717455A CN202011474198.9A CN202011474198A CN112717455A CN 112717455 A CN112717455 A CN 112717455A CN 202011474198 A CN202011474198 A CN 202011474198A CN 112717455 A CN112717455 A CN 112717455A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D19/00—Degasification of liquids
- B01D19/0042—Degasification of liquids modifying the liquid flow
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
- B01D3/32—Other features of fractionating columns ; Constructional details of fractionating columns not provided for in groups B01D3/16 - B01D3/30
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/14—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by absorption
- B01D53/1406—Multiple stage absorption
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/14—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by absorption
- B01D53/1493—Selection of liquid materials for use as absorbents
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- 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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- 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
- B01J19/18—Stationary reactors having moving elements inside
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Abstract
The invention discloses a rectification separation device and a method of 2-cyanopyridine bed charge, the device pours the prepared bed charge into a heating stirring kettle, a stirring shaft and a stirring blade are driven by a stirring motor in the heating stirring kettle to stir, and the heating is matched with a heating resistor to heat, so that ammonia water in the bed charge is accelerated to decompose into ammonia gas, the ammonia gas mixed with other gases is led into a rectification separation tower through a heat-insulating connecting pipe, firstly, the sulfuric acid solution at the bottom of a rectification shell is bubbled through an air outlet pipe, so that the sulfuric acid solution absorbs a large amount of ammonia gas, meanwhile, a small part of ammonia gas and other gases are upwards absorbed through a filter screen plate, a coarse filter filler and a fine filter filler, finally, the ammonia gas is conveyed to a liquefaction assembly through the heat-insulating connecting pipe, after the residual gas is liquefied by the liquefaction assembly, the conveying pipe is led into the heating stirring kettle again, the heating stirring kettle is continuously, the method effectively separates the ammonia water in the prepared bottom material, and avoids the ammonia gas from decomposing into ammonia gas to pollute the environment.
Description
Technical Field
The invention relates to the technical field of rectification separation, in particular to a device and a method for rectifying and separating a 2-cyanopyridine bed charge.
Background
The molecular formula of the 2-cyanopyridine is C6H4N2The molecular weight is 104.11, the crystal is white to light yellow at low temperature, is insoluble in water, is mainly used as an intermediate of pharmacy and dye, is usually stored in a cool and ventilated storehouse, is far away from a fire and a heat source, is required to be stored separately from an oxidant, is forbidden to be stored in a mixed way, needs to be stored in a sealed way, is usually stored in a dark place, is provided with an explosion-proof lighting and ventilating facility in a storage place to avoid explosion, wherein, in the synthesis process of the 2-cyanopyridine, ammonia water is generally required to be added so as to synthesize the cyano, after the 2-cyanopyridine is prepared, unreacted ammonia water still exists, and the ammonia water is easily decomposed into ammonia gas and is emitted into air, thereby causing environmental pollution, but in the prior art, no primer for preparing 2-cyanopyridine, effectively separate ammonia water or ammonia gas to lead to its preparation bed charge difficult to handle's problem.
Disclosure of Invention
The invention aims to provide a rectification separation device and a rectification separation method of a 2-cyanopyridine bed charge, wherein the preparation bed charge is poured into a heating stirring kettle, a stirring shaft and a stirring blade are driven by a stirring motor in the heating stirring kettle to stir, heating is carried out by matching with a heating resistor, ammonia water in the bed charge is accelerated to decompose into ammonia gas, ammonia gas mixed with other gases is introduced into a rectification separation tower through a heat-insulating connecting pipe, firstly, the sulfuric acid solution at the bottom of a rectification shell is bubbled through an air outlet pipe, so that the sulfuric acid solution absorbs a large amount of ammonia gas, meanwhile, a small part of ammonia gas and other gases upwards pass through a filter screen plate, a coarse filter filler and a fine filter filler to absorb, finally, the ammonia gas is conveyed to a liquefaction assembly through the heat-insulating connecting pipe, the residual gas is liquefied by the liquefaction assembly, then, the residual gas is reintroduced into the heating stirring kettle through a conveying pipe, the heating, to solve the problems set forth in the background art described above.
In order to achieve the purpose, the invention provides the following technical scheme:
the utility model provides a 2-cyanopyridine bed charge rectification separator, includes rectification knockout tower, heat preservation connecting pipe, delivery pump, heating stirred tank, liquefaction subassembly and conveyer pipe, the heat preservation connecting pipe is installed respectively to both sides about the left end of rectification knockout tower, downside install the delivery pump on the heat preservation connecting pipe, downside the terminal installation heating stirred tank of heat preservation connecting pipe, upside the liquefaction subassembly is installed to the end of heat preservation connecting pipe, through duct connections between liquefaction subassembly and the heating stirred tank.
Preferably, the rectification separation tower comprises a rectification shell, an air inlet, an air outlet guide pipe, a clamping groove, a filter screen plate, an isolation groove, a coarse filter filler, a fine filter filler, a pressure relief component, an air outlet, a liquid outlet, a sealing cover and a sealing ring, the lower end of the right side of the rectification shell is provided with an air inlet, the inner side of the air inlet is provided with an air outlet guide pipe, a clamping groove is arranged on the inner wall of the lower side of the rectification shell, a filter screen plate is arranged in the clamping groove, an isolation groove is arranged on the inner wall of the middle section of the rectification shell, coarse filter filler is arranged in the isolation groove at the lower side, fine filter filler is arranged in the isolation groove at the upper side, the top of the rectification shell is provided with a pressure relief assembly, the right upper side of the rectification shell is provided with an exhaust port, the bottom of rectification shell is equipped with the leakage fluid dram, the sealed lid of outside installation of leakage fluid dram, be equipped with the sealing washer between leakage fluid dram and the sealed lid.
Preferably, the pressure release subassembly includes sealed backing plate, pressure release pipe, limiting plate, spring base, reset spring and operating handle, the inboard installation pressure release pipe of sealed backing plate, the bottom of pressure release pipe is equipped with the limiting plate, the top of pressure release pipe is equipped with spring base, reset spring is installed in the pressure release pipe outside of spring base downside, spring base's upside is equipped with operating handle.
Preferably, the heating stirred tank includes cauldron shell, agitator motor, circulation interface, extraction opening, (mixing) shaft, stirring vane, end intermediate layer, power supply joint, heating resistor and feed inlet, cauldron shell's top installation agitator motor, cauldron shell's upside right-hand member is equipped with the circulation interface, cauldron shell's upside left end is equipped with the extraction opening, agitator motor's downside installation (mixing) shaft, the outside of (mixing) shaft is equipped with stirring vane, cauldron shell's inboard bottom is equipped with end intermediate layer, end intermediate layer's bottom is equipped with the power supply and connects, the upside installation heating resistor that the power supply connects, cauldron shell's downside right-hand member is equipped with the feed inlet.
Preferably, the liquefaction subassembly includes liquefaction shell, heat preservation intermediate layer, insulation resistance, spiral condenser pipe, comdenstion water entry and comdenstion water export, the inboard both ends of liquefaction shell are equipped with the heat preservation intermediate layer respectively, be equipped with insulation resistance in the heat preservation intermediate layer, install spiral condenser pipe between the heat preservation intermediate layer, the right downside of liquefaction shell is equipped with the comdenstion water entry, the upper left side of liquefaction shell is equipped with the comdenstion water export.
Preferably, a thread sealing cover is arranged at the tail end of the feed inlet.
The invention provides another technical scheme: a use method of a 2-cyanopyridine bottom material rectification separation device comprises the following steps:
the method comprises the following steps: pouring the prepared bed charge of the 2-cyanopyridine into a kettle shell through a feeding hole, connecting a power supply connector, heating the bed charge by a heating resistor, and driving a stirring shaft and stirring blades to fully stir by a stirring motor;
step two: gas generated by heating and stirring the bed charge is pumped out from the air extraction port through a delivery pump and is delivered to the bottom of the rectification shell, sulfuric acid solution is poured into the bottom of the rectification shell in advance, and the gas bubbles in the sulfuric acid solution through an air outlet guide pipe to eliminate most of ammonia gas;
step three: the rest small part of ammonia gas is upwards filtered and absorbed by the filter screen plate, the coarse filter filler and the fine filter filler in sequence along with other gases, continuously upwards discharged from the exhaust port and conveyed into the liquefaction assembly by the heat-insulation connecting pipe;
step four: external water pipes are connected to a condensate water inlet and a condensate water outlet, so that condensate water is filled in the liquefaction shell, and gas is conveyed to the heating stirring kettle again through the conveying pipe for cyclic rectification and separation after being condensed and liquefied through the spiral condensing pipe.
Compared with the prior art, the invention has the beneficial effects that:
the invention provides a rectification separation device and a method of 2-cyanopyridine bed charge, the device pours the prepared bed charge into a heating stirring kettle, a stirring shaft and a stirring blade are driven by a stirring motor in the heating stirring kettle to stir, and the heating is matched with a heating resistor to heat, so that ammonia water in the bed charge is decomposed into ammonia gas at an accelerated speed, ammonia gas mixed with other gases is led into a rectification separation tower through a heat-insulating connecting pipe, firstly, the sulfuric acid solution at the bottom of a rectification shell is bubbled through an air outlet pipe, so that the sulfuric acid solution absorbs a large amount of ammonia gas, meanwhile, a small part of ammonia gas and other gases are upwards absorbed through a filter screen plate, a coarse filter filler and a fine filter filler, finally, the ammonia gas is conveyed to a liquefaction assembly through the heat-insulating connecting pipe, after the residual gas is liquefied by the liquefaction assembly, the residual gas is led into the heating stirring kettle again through a conveying pipe, the, the ammonia water separator has a complete and reasonable structure, effectively separates ammonia water in the prepared bottom material, and avoids the ammonia water from decomposing into ammonia gas to pollute the environment.
Drawings
FIG. 1 is a schematic structural view of the present invention;
FIG. 2 is a schematic sectional view of a rectifying-separating column of the present invention;
FIG. 3 is an enlarged schematic view of a rectifying-separating column A of the present invention;
FIG. 4 is an enlarged schematic view of a pressure relief assembly according to the present invention;
FIG. 5 is a schematic cross-sectional view of a heated stirred tank of the present invention;
fig. 6 is a schematic sectional structure view of the liquefaction assembly of the present invention.
In the figure: 1. a rectification separation column; 101. a rectification housing; 102. an air inlet; 103. an air outlet duct; 104. a clamping groove; 105. a filter screen plate; 106. an isolation trench; 107. coarse filtration of the filler; 108. fine filtering the filler; 109. a pressure relief assembly; 1091. sealing the base plate; 1092. a pressure relief pipe; 1093. a limiting plate; 1094. a spring mount; 1095. a return spring; 1096. an operating handle; 1010. an exhaust port; 1011. a liquid discharge port; 1012. a sealing cover; 1013. a seal ring; 2. a heat-insulating connecting pipe; 3. a delivery pump; 4. heating the stirred tank; 41. a kettle shell; 42. a stirring motor; 43. a circulation interface; 44. an air extraction opening; 45. a stirring shaft; 46. a stirring blade; 47. a bottom interlayer; 48. a power supply connector; 49. a heating resistor; 410. a feed inlet; 5. a liquefaction assembly; 51. a liquefaction shell; 52. a heat-insulating interlayer; 53. a heat preservation resistor; 54. a spiral condenser tube; 55. a condensed water inlet; 56. a condensed water outlet; 6. a delivery pipe.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1, a rectification separation device for 2-cyanopyridine bed charge comprises a rectification separation tower 1, a heat-preservation connecting pipe 2, a delivery pump 3, a heating stirring kettle 4, a liquefaction component 5 and a delivery pipe 6, wherein the heat-preservation connecting pipe 2 is respectively arranged on the upper side and the lower side of the left end of the rectification separation tower 1, the delivery pump 3 is arranged on the lower side heat-preservation connecting pipe 2, the heating stirring kettle 4 is arranged at the tail end of the lower side heat-preservation connecting pipe 2, the liquefaction component 5 is arranged at the tail end of the upper side heat-preservation connecting pipe 2, and the liquefaction component 5 is connected with the heating stirring kettle 4 through.
Referring to fig. 2-3, a rectification separation tower 1 includes a rectification housing 101, an air inlet 102, an air outlet conduit 103, a clamping groove 104, a filter screen 105, an isolation groove 106, coarse filter fillers 107, fine filter fillers 108, a pressure relief assembly 109, an air outlet 1010, a liquid outlet 1011, a sealing cover 1012 and a sealing ring 1013, the air inlet 102 is disposed at the lower end of the right side of the rectification housing 101, the air outlet conduit 103 is mounted at the inner side of the air inlet 102, the clamping groove 104 is disposed on the inner wall of the lower side of the rectification housing 101, the filter screen 105 is mounted in the clamping groove 104, the isolation groove 106 is disposed on the inner wall of the middle section of the rectification housing 101, the coarse filter fillers 107 are mounted in the lower isolation groove 106, the fine filter fillers 108 are mounted in the upper isolation groove 106, the pressure relief assembly 109 is disposed at the top of the rectification housing 101, the air outlet 1010 is disposed at the upper right side of the rectification housing 101, the, a seal ring 1013 is provided between the liquid discharge port 1011 and the seal cover 1012.
Referring to fig. 4, the pressure relief assembly 109 includes a sealing pad 1091, a pressure relief pipe 1092, a limiting plate 1093, a spring base 1094, a return spring 1095 and an operating handle 1096, the pressure relief pipe 1092 is mounted on the inner side of the sealing pad 1091, the limiting plate 1093 is disposed at the bottom of the pressure relief pipe 1092, the spring base 1094 is disposed at the top of the pressure relief pipe 1092, the return spring 1095 is mounted on the outer side of the pressure relief pipe 1092 on the lower side of the spring base 1094, and the operating handle 1096 is disposed on the upper side of the spring base 1094.
Referring to fig. 5, the heating and stirring tank 4 includes a tank shell 41, a stirring motor 42, a circulation interface 43, an air extraction opening 44, a stirring shaft 45, a stirring blade 46, a bottom interlayer 47, a power supply connector 48, a heating resistor 49 and a feed inlet 410, the stirring motor 42 is installed on the top of the tank shell 41, the circulation interface 43 is installed on the right end of the upper side of the tank shell 41, the air extraction opening 44 is installed on the left end of the upper side of the tank shell 41, the stirring shaft 45 is installed on the lower side of the stirring motor 42, the stirring blade 46 is installed on the outer side of the stirring shaft 45, the bottom interlayer 47 is installed on the bottom of the inner side of the tank shell 41, the power supply connector 48 is installed on the bottom of the bottom interlayer 47, the heating resistor 49 is installed on the upper side of the.
Referring to fig. 6, the liquefaction assembly 5 includes a liquefaction shell 51, a heat-preservation interlayer 52, a heat-preservation resistor 53, a spiral condenser pipe 54, a condensed water inlet 55 and a condensed water outlet 56, the heat-preservation interlayer 52 is respectively disposed at two ends of the inner side of the liquefaction shell 51, the heat-preservation resistor 53 is disposed in the heat-preservation interlayer 52, the spiral condenser pipe 54 is installed between the heat-preservation interlayers 52, the condensed water inlet 55 is disposed at the lower right side of the liquefaction shell 51, and the condensed water outlet 56 is disposed at the upper left side of the liquefaction shell 51.
In order to better show the use flow of the rectification and separation device for the 2-cyanopyridine bottom material, the embodiment now proposes a use method of the rectification and separation device for the 2-cyanopyridine bottom material, which comprises the following steps:
the method comprises the following steps: pouring the prepared bed charge of the 2-cyanopyridine into the kettle shell 41 through the feeding hole 410, connecting the power supply connector 48, heating the bed charge by the heating resistor 49, and driving the stirring shaft 45 and the stirring blade 46 by the stirring motor 42 to fully stir;
step two: gas generated by heating and stirring the bed charge is pumped out from the pumping hole 44 through the delivery pump 3 and is delivered to the bottom of the rectification shell 101, sulfuric acid solution is poured into the bottom of the rectification shell 101 in advance, and the gas bubbles in the sulfuric acid solution through the gas outlet guide pipe 103, so that most of ammonia gas is eliminated;
step three: the remaining small part of ammonia gas goes upwards along with other gases, is sequentially filtered and absorbed by the filter screen plate 105, the coarse filter filler 107 and the fine filter filler 108, continues upwards, is discharged from the exhaust port 1010, and is conveyed into the liquefaction assembly 5 by the heat-insulation connecting pipe 2;
step four: external water pipes are connected to the condensed water inlet 55 and the condensed water outlet 56, so that the liquefaction shell 51 is filled with condensed water, and after the gas is condensed and liquefied through the spiral condensing pipe 54, the gas is conveyed into the heating stirring kettle 4 again through the conveying pipe 6 for cyclic rectification and separation.
The working principle of the invention is as follows: the invention relates to a rectification separation device and a method for 2-cyanopyridine bed charge, the device pours the prepared bed charge into a heating stirring kettle 4, a stirring shaft 45 and a stirring blade 46 are driven by a stirring motor 42 in the heating stirring kettle 4 to be stirred, and the heating resistance 49 is matched for heating, so that ammonia water in the bed charge is accelerated to be decomposed into ammonia gas, the ammonia gas mixed with other gases is led into a rectification separation tower 1 through a heat-insulating connecting pipe 2, firstly, the sulfuric acid solution at the bottom of a rectification shell 101 is bubbled through an air outlet pipe 103, so that the sulfuric acid solution absorbs a large amount of ammonia gas, meanwhile, a small part of ammonia gas and other gases are upwards absorbed through a filter screen plate 105, a rough filter filler 107 and a fine filter filler 108, finally, the ammonia gas and other gases are conveyed to a liquefaction assembly 5 through the heat-insulating connecting pipe 2, the residual gases are liquefied by the liquefaction assembly 5 and, the heating and stirring kettle 4 continues to heat and stir for the next rectification separation cycle, the device is used for rectifying and separating ammonia in bottom materials, gas is introduced into acidic washing liquid and filler on the upper side to absorb ammonia, the washing liquid is discharged to extract ammonia by a chemical method, the ammonia absorbed in the filler is washed by the washing liquid and extracted by the chemical method, the cycle aims at enabling the ammonia in the gas to be incompletely separated after the decomposed gas passes through the rectification separation tower 1 once, multiple cycles are needed to improve the absorption quality of the washing liquid and the filler on the ammonia, the washing liquid which finishes absorption after absorption is discharged through a liquid discharge port 1011, the bottom materials in the heating and stirring kettle 4 are pumped out from a feed port 410, the washing liquid is selected from acidic solutions, and hydrochloric acid or sulfuric acid solutions are generally used.
In summary, the following steps: the invention relates to a rectification separation device and a method for 2-cyanopyridine bed charge, the device pours the prepared bed charge into a heating stirring kettle 4, a stirring shaft 45 and a stirring blade 46 are driven by a stirring motor 42 in the heating stirring kettle 4 to be stirred, and the heating resistance 49 is matched for heating, so that ammonia water in the bed charge is accelerated to be decomposed into ammonia gas, the ammonia gas mixed with other gases is led into a rectification separation tower 1 through a heat-insulating connecting pipe 2, firstly, the sulfuric acid solution at the bottom of a rectification shell 101 is bubbled through an air outlet pipe 103, so that the sulfuric acid solution absorbs a large amount of ammonia gas, meanwhile, a small part of ammonia gas and other gases are upwards absorbed through a filter screen plate 105, a rough filter filler 107 and a fine filter filler 108, finally, the ammonia gas and other gases are conveyed to a liquefaction assembly 5 through the heat-insulating connecting pipe 2, the residual gases are liquefied by the liquefaction assembly 5 and, the heating and stirring kettle 4 is used for continuously heating and stirring to carry out the next rectification separation cycle, the structure of the invention is complete and reasonable, the ammonia water in the prepared bottom material is effectively separated, and the ammonia water is prevented from decomposing into ammonia gas to pollute the environment.
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 able to cover the technical solutions and the inventive concepts of the present invention within the technical scope of the present invention.
Claims (7)
1. The utility model provides a 2-cyanopyridine bed charge rectification and separation device, includes rectifying and separating tower (1), heat preservation connecting pipe (2), delivery pump (3), heating stirred tank (4), liquefaction subassembly (5) and conveyer pipe (6), its characterized in that: heat preservation connecting pipe (2), downside are installed respectively to both sides about the left end of rectification knockout tower (1) installation delivery pump (3), downside on heat preservation connecting pipe (2) the terminal installation heating stirred tank (4) of heat preservation connecting pipe (2), upside liquefaction subassembly (5) are installed to the end of heat preservation connecting pipe (2), be connected through conveyer pipe (6) between liquefaction subassembly (5) and the heating stirred tank (4).
2. The rectification separation device of 2-cyanopyridine bed charge as claimed in claim 1, characterized in that: rectifying and separating column (1) is including rectification shell (101), air inlet (102), the pipe (103) of giving vent to anger, inlay card groove (104), filter screen board (105), isolation tank (106), coarse filtration filler (107), fine filtration filler (108), pressure release subassembly (109), gas vent (1010), leakage fluid dram (1011), sealed lid (1012) and sealing washer (1013), the right side lower extreme of rectification shell (101) is equipped with air inlet (102), pipe (103) is given vent to anger in the inboard installation of air inlet (102), be equipped with inlay card groove (104) on the downside inner wall of rectification shell (101), install filter screen board (105) in inlay card groove (104), be equipped with isolation tank (106) on the middle section inner wall of rectification shell (101), downside install coarse filtration filler (107) in isolation tank (106), upside install fine filtration filler (108) in isolation tank (106), the top of rectification shell (101) is equipped with pressure release subassembly (109), the upper right side of rectification shell (101) is equipped with gas vent (1010), the bottom of rectification shell (101) is equipped with leakage fluid dram (1011), sealed lid (1012) of outside installation of leakage fluid dram (1011), be equipped with between leakage fluid dram (1011) and the sealed lid (1012) sealing washer (1013).
3. The rectification separation device of 2-cyanopyridine bed charge as claimed in claim 2, characterized in that: pressure release subassembly (109) are including sealed backing plate (1091), pressure release pipe (1092), limiting plate (1093), spring base (1094), reset spring (1095) and operating handle (1096), the inboard installation pressure release pipe (1092) of sealed backing plate (1091), the bottom of pressure release pipe (1092) is equipped with limiting plate (1093), the top of pressure release pipe (1092) is equipped with spring base (1094), reset spring (1095) are installed in pressure release pipe (1092) outside of spring base (1094) downside, the upside of spring base (1094) is equipped with operating handle (1096).
4. The rectification separation device of 2-cyanopyridine bed charge as claimed in claim 1, characterized in that: the heating stirring kettle (4) comprises a kettle shell (41), a stirring motor (42), a circulation interface (43), an air pumping hole (44), a stirring shaft (45), a stirring blade (46), a bottom interlayer (47), a power supply connector (48), a heating resistor (49) and a feed inlet (410), wherein the stirring motor (42) is installed at the top of the kettle shell (41), the circulation interface (43) is arranged at the right end of the upper side of the kettle shell (41), the air pumping hole (44) is arranged at the left end of the upper side of the kettle shell (41), the stirring shaft (45) is installed at the lower side of the stirring motor (42), the stirring blade (46) is arranged at the outer side of the stirring shaft (45), the bottom interlayer (47) is arranged at the bottom of the inner side of the kettle shell (41), the power supply connector (48) is arranged at the bottom of the bottom interlayer (47), and the heating resistor (49, the right end of the lower side of the kettle shell (41) is provided with a feeding hole (410).
5. The rectification separation device of 2-cyanopyridine bed charge as claimed in claim 1, characterized in that: liquefaction subassembly (5) are including liquefaction shell (51), heat preservation intermediate layer (52), insulation resistance (53), spiral condenser pipe (54), comdenstion water entry (55) and comdenstion water export (56), the inboard both ends of liquefaction shell (51) are equipped with insulation intermediate layer (52) respectively, be equipped with insulation resistance (53) in insulation intermediate layer (52), install spiral condenser pipe (54) between insulation intermediate layer (52), the right downside of liquefaction shell (51) is equipped with comdenstion water entry (55), the upper left side of liquefaction shell (51) is equipped with comdenstion water export (56).
6. The rectification separation device of 2-cyanopyridine bed charge as claimed in claim 4, characterized in that: and a thread sealing cover is arranged at the tail end of the feed port (410).
7. A method for using the rectification separation device of 2-cyanopyridine bed material as described in any one of claims 1 to 6, comprising the steps of:
s1: pouring the prepared bed charge of the 2-cyanopyridine into a kettle shell (41) through a feeding hole (410), connecting a power supply connector (48), heating the bed charge by a heating resistor (49), and driving a stirring shaft (45) and a stirring blade (46) by a stirring motor (42) to fully stir;
s2: gas generated by heating and stirring the bed charge is pumped out from the pumping hole (44) through the delivery pump (3) and is delivered to the bottom of the rectification shell (101), sulfuric acid solution is poured into the bottom of the rectification shell (101) in advance, and the gas bubbles in the sulfuric acid solution through the gas outlet guide pipe (103) to eliminate most of ammonia gas;
s3: the remaining small part of ammonia gas is upwards filtered and absorbed by a filter screen plate (105), a coarse filter filler (107) and a fine filter filler (108) in sequence along with other gases, continuously upwards discharged from an exhaust port (1010), and conveyed into a liquefaction assembly (5) by a heat-insulating connecting pipe (2);
s4: external water pipes are connected to a condensed water inlet (55) and a condensed water outlet (56) to ensure that condensed water is filled in the liquefaction shell (51), and gas is condensed and liquefied through the spiral condensing pipe (54) and then is conveyed to the heating stirring kettle (4) again through the conveying pipe (6) for internal circulation rectification and separation.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011474198.9A CN112717455A (en) | 2020-12-14 | 2020-12-14 | Rectification separation device and method for 2-cyanopyridine bottom material |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011474198.9A CN112717455A (en) | 2020-12-14 | 2020-12-14 | Rectification separation device and method for 2-cyanopyridine bottom material |
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| Publication Number | Publication Date |
|---|---|
| CN112717455A true CN112717455A (en) | 2021-04-30 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011474198.9A Pending CN112717455A (en) | 2020-12-14 | 2020-12-14 | Rectification separation device and method for 2-cyanopyridine bottom material |
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| CN114950055A (en) * | 2022-06-17 | 2022-08-30 | 安徽顺达环保科技股份有限公司 | Dry desulfurization and denitrification device for cement kiln flue gas and implementation method thereof |
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| CN114950055A (en) * | 2022-06-17 | 2022-08-30 | 安徽顺达环保科技股份有限公司 | Dry desulfurization and denitrification device for cement kiln flue gas and implementation method thereof |
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