CN112691403B - 4-cyanopyridine continuous evaporation crystallization device and method - Google Patents
4-cyanopyridine continuous evaporation crystallization device and method Download PDFInfo
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- CN112691403B CN112691403B CN202011471723.1A CN202011471723A CN112691403B CN 112691403 B CN112691403 B CN 112691403B CN 202011471723 A CN202011471723 A CN 202011471723A CN 112691403 B CN112691403 B CN 112691403B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/0018—Evaporation of components of the mixture to be separated
- B01D9/0031—Evaporation of components of the mixture to be separated by heating
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D1/00—Evaporating
- B01D1/0011—Heating features
- B01D1/0017—Use of electrical or wave energy
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D1/00—Evaporating
- B01D1/30—Accessories for evaporators ; Constructional details thereof
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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
- B01J19/0053—Details of the reactor
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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
- B01J19/24—Stationary reactors without moving elements inside
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D213/00—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members
- C07D213/02—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members
- C07D213/04—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom
- C07D213/60—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D213/78—Carbon atoms having three bonds to hetero atoms, with at the most one bond to halogen, e.g. ester or nitrile radicals
- C07D213/84—Nitriles
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Abstract
The invention discloses a 4-cyanopyridine continuous evaporative crystallization device and a method, comprising a pressurizing component, a connecting pipe and an evaporative reaction kettle, wherein the device increases the air pressure in the evaporative reaction kettle by the pressurizing component, thereby reducing the crystallization temperature of 4-cyanopyridine and the boiling point temperature of other organic solvents, after the pressurizing is finished, a heating resistor heats and crystallizes a solution part to ensure that only water and other organic solvents are vaporized and 4-cyanopyridine is heated and crystallized in the evaporative crystallization process of 4-cyanopyridine, meanwhile, a condensing reflux box absorbs and re-liquefies water vapor, other organic solvents and part of 4-cyanopyridine, the water vapor drops to the right side of the evaporative reaction kettle, the heating resistor on the right side performs evaporative crystallization operation under normal pressure again, thereby separating out the 4-cyanopyridine after crystallization, and the crystal is attached to the inner wall of the right side of the evaporation reaction kettle, so that the crystallization operation steps of the 4-cyanopyridine are simplified, and the crystallization amount of the 4-cyanopyridine separated out is effectively increased.
Description
Technical Field
The invention relates to the technical field of evaporative crystallization equipment, in particular to a device and a method for continuously evaporating and crystallizing 4-cyanopyridine.
Background
4-cyanopyridine of formula C6H4N2The molecular weight is 104.11, the product is a white to light yellow needle crystal, has characteristic odor, is dissolved in ethanol, ether and benzene, is mainly used for medicine and pesticide intermediate products, is usually stored in a cool and ventilated storehouse, is far away from kindling and heat sources, and is required to be stored separately from an oxidant, so that the mixed storage is avoided. Sealed storage, adopting explosion-proof lighting and ventilation deviceMechanical equipment and tools which are easy to generate sparks are forbidden, a storage area is provided with leakage emergency treatment equipment and proper accommodating materials, when the preparation of the 4-cyanopyridine is finished, the 4-cyanopyridine is usually in a solution state, the 4-cyanopyridine is usually subjected to crystallization and recovery operation in an evaporation crystallization mode, and in the evaporation crystallization process, the evaporation temperature is difficult to control, and other substances in an organic solution are easy to simultaneously vaporize the 4-cyanopyridine, so that the problem that the content of the crystallized 4-cyanopyridine crystals is low is caused.
Disclosure of Invention
The invention aims to provide a device and a method for continuously evaporating and crystallizing 4-cyanopyridine, wherein the air pressure in an evaporation reaction kettle is increased by a pressurizing component, so that the crystallization temperature of the 4-cyanopyridine and the boiling point temperature of other organic solvents are reduced, after pressurization is finished, a heating resistor heats and crystallizes a solution part to ensure that only water, other organic solvents and a small amount of 4-cyanopyridine are vaporized and the 4-cyanopyridine is heated and crystallized in the evaporation and crystallization process of the 4-cyanopyridine, meanwhile, a condensing reflux box absorbs and re-liquefies water vapor, other organic solvents and part of the 4-cyanopyridine, the water vapor, other organic solvents and part of the 4-cyanopyridine drop to the right side of the evaporation reaction kettle, and the heating resistor on the right side performs evaporation and crystallization operation under normal pressure again, so that the 4-cyanopyridine is crystallized and separated out, and is attached to the right inner wall of the evaporation reaction vessel to solve the problems presented in the background art described above.
In order to achieve the purpose, the invention provides the following technical scheme:
the utility model provides a 4-cyanopyridine evaporates crystallization device in succession, includes pressurization subassembly, connecting pipe, airtight pump and evaporation reaction cauldron, the front end installation connecting pipe of pressurization subassembly, install airtight pump on the connecting pipe, the terminal installation evaporation reaction cauldron of connecting pipe.
The pressurizing assembly comprises a pressurizing shell, a movable groove, a hydraulic oil cylinder, a hydraulic motor, a limiting pressing plate, a connecting shaft, a pressurizing plate, an airtight plate sleeve, a pressure relief assembly and a supporting leg, wherein the movable groove is formed in the left side of the pressurizing shell, the hydraulic oil cylinder is installed on the left side of the movable groove, the hydraulic motor is installed on the inner side of the hydraulic oil cylinder, the limiting pressing plate is installed in the movable groove, the connecting shaft is installed at the center of the bottom of the limiting pressing plate, the pressurizing plate is installed at the tail end of the connecting shaft, the airtight plate sleeve is installed between the outer side of the pressurizing plate and the pressurizing shell in a clamping and embedding mode, the pressure relief assembly is installed on the upper side of the pressurizing shell, and the supporting leg is installed on the outer side of the bottom of the pressurizing shell.
The pressure release subassembly is including sealed cardboard, movable rod, outer spacing seat, operating handle, reset spring, seal ring, bottom limiting plate and sealed snap ring, the internally mounted movable rod of sealed cardboard, the top of movable rod is equipped with outer spacing seat, the movable rod outside between outer spacing seat and the sealed cardboard is equipped with reset spring, the upside of outer spacing seat is equipped with operating handle, the seal ring is installed in the second half section outside of movable rod, the bottom of movable rod is equipped with the bottom limiting plate, the nested sealed snap ring in the outside of bottom limiting plate.
The evaporation reaction kettle comprises a reaction kettle shell, a central isolation plate, a liquefaction assembly, a heating resistor, an external electrode, a liquid inlet, an external sealing cover and an auxiliary material adding port, wherein the central isolation plate is arranged at the inner center of the reaction kettle shell, a sealing door plate is arranged on the outer side of the front end of the reaction kettle shell, the liquefaction assembly is installed on the upper half section of the central isolation plate, the heating resistor is installed on the inner side of the bottom of the reaction kettle shell, the external electrode is connected to the center of the bottom of the heating resistor, the liquid inlet is respectively arranged at the two ends of the outer side of the reaction kettle shell, the external sealing cover is respectively installed on the two sides of the top end of the reaction kettle shell, and the auxiliary material adding port is arranged at the center of the upper end of the external sealing cover.
The liquefaction subassembly is including inlay card shell, inlay card groove, reflux condenser case, aspiration pump, auger delivery pipe and air inlet, inlay card shell's outside center department is equipped with inlay card groove, the opening part inlay card of center division board is installed in inlay card groove, inlay card shell's upper left end is equipped with the air inlet, auger delivery pipe is connected to the inboard of air inlet, auger delivery pipe's end installation aspiration pump, reflux condenser case is installed on the right side of aspiration pump.
The condensation backflow box comprises a condensation shell, a liquid dropping port, an outer clamping ring, an outer pipe connector and a condensation plate, wherein the liquid dropping port is arranged at the bottom of the condensation shell, the outer clamping ring is arranged on the outer side of the lower section of the condensation shell, the outer pipe connector is arranged on the left side of the condensation shell on the upper side of the outer clamping ring, and the condensation plate is arranged on the inner wall of the upper section of the condensation shell.
The invention provides another technical scheme: the use method of the 4-cyanopyridine continuous evaporative crystallization device comprises the following steps:
the method comprises the following steps: pouring the 4-cyanopyridine solution into an evaporation reaction kettle, installing a pressurizing assembly at a liquid inlet on one side of the evaporation reaction kettle, closing and sealing various openings, and detecting the air tightness in the evaporation reaction kettle by using the pressurizing assembly;
step two: the forward movement of a pressurizing plate in the pressurizing assembly is utilized, and the air is conveyed to the evaporation reaction kettle by the airtight pump, so that the air pressure in the whole evaporation reaction kettle is improved;
step three: heating crystallization operation is carried out on the 4-cyanopyridine solution inside by using a heating resistor in the evaporation reaction kettle, and steam generated by heating rises to the vicinity of the liquefaction component;
step four: sucking steam from an air inlet through an air suction pump in the liquefaction assembly, conveying the steam into a condensation reflux box through a spiral conveying pipe, and dripping the steam to the right side of the evaporation reaction kettle through a liquid dripping port after liquefaction is finished by a condensation plate;
step five: and (3) heating and crystallizing the solution again by using the heating resistor on the right side, after the heating and crystallizing are finished, pumping out the liquid in the evaporation reaction kettle, and scraping the 4-cyanopyridine crystals on the inner wall of the evaporation reaction kettle.
Compared with the prior art, the invention has the beneficial effects that:
the invention provides a 4-cyanopyridine continuous evaporative crystallization device and a method, the device increases the air pressure in an evaporative reaction kettle by a pressurizing component, thereby reducing the crystallization temperature of 4-cyanopyridine and the boiling point temperature of other organic solvents, after pressurization is finished, a heating resistor heats and crystallizes a solution part to ensure that only water, other organic solvents and a small amount of 4-cyanopyridine are vaporized in the evaporative crystallization process of the 4-cyanopyridine, the 4-cyanopyridine is heated and crystallized, meanwhile, a condensing reflux box absorbs and re-liquefies water vapor, other organic solvents and part of the 4-cyanopyridine, and drops on the right side of the evaporative reaction kettle, the heating resistor on the right side carries out evaporative crystallization operation under normal pressure again, thereby the 4-cyanopyridine is crystallized, separated out and attached to the inner wall on the right side of the evaporative reaction kettle, the invention has a complete and reasonable structure, simplifies the crystallization operation steps of the 4-cyanopyridine and effectively improves the crystallization amount of the 4-cyanopyridine.
Drawings
FIG. 1 is a schematic view of the structure of the present invention;
FIG. 2 is a schematic cross-sectional view of the compression assembly of the present invention;
FIG. 3 is an enlarged schematic view of a pressure relief assembly according to the present invention;
FIG. 4 is a schematic sectional view of an evaporation reactor of the present invention;
FIG. 5 is a schematic cross-sectional structural view of a liquefaction package of the present invention;
FIG. 6 is a schematic cross-sectional view of a reflux condenser tank according to the present invention.
In the figure: 1. a pressurizing assembly; 101. a pressurized housing; 102. a movable groove; 103. a hydraulic cylinder; 104. a hydraulic motor; 105. a limiting pressure plate; 106. a connecting shaft; 107. a pressurizing plate; 108. an airtight plate sleeve; 109. a pressure relief assembly; 1091. a sealing clamping plate; 1092. a movable rod; 1093. an outer limiting seat; 1094. an operating handle; 1095. a return spring; 1096. a sealing gasket; 1097. a bottom limiting plate; 1098. sealing the snap ring; 1010. supporting legs; 2. a connecting pipe; 3. an airtight pump; 4. evaporating the reaction kettle; 41. a reaction kettle shell; 42. a central separator plate; 43. a liquefaction assembly; 431. the shell is embedded in a clamping manner; 432. a clamping groove; 433. a condensing reflux box; 4331. a condensing shell; 4332. a drip port; 4333. an outer snap ring; 4334. an outer tube interface; 4335. a condensing plate; 434. an air pump; 435. a spiral conveying pipe; 436. an air inlet; 44. a heating resistor; 45. an external electrode; 46. a liquid inlet; 47. an outer sealing cover; 48. and (5) adding auxiliary materials.
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 continuous evaporative crystallization apparatus for 4-cyanopyridine includes a pressurizing assembly 1, a connecting pipe 2, an airtight pump 3 and an evaporation reactor 4, wherein the connecting pipe 2 is installed at the front end of the pressurizing assembly 1, the airtight pump 3 is installed on the connecting pipe 2, and the evaporation reactor 4 is installed at the end of the connecting pipe 2.
Referring to fig. 2, the pressurizing assembly 1 includes a pressurizing housing 101, a movable groove 102, a hydraulic cylinder 103, a hydraulic motor 104, a limiting pressing plate 105, a connecting shaft 106, a pressurizing plate 107, an airtight plate sleeve 108, a pressure relief assembly 109 and a supporting leg 1010, the movable groove 102 is arranged on the left side of the pressurizing housing 101, the hydraulic cylinder 103 is arranged on the left side of the movable groove 102, the hydraulic motor 104 is arranged on the inner side of the hydraulic cylinder 103, the limiting pressing plate 105 is arranged in the movable groove 102, the connecting shaft 106 is arranged at the center of the bottom of the limiting pressing plate 105, the pressurizing plate 107 is arranged at the tail end of the connecting shaft 106, the airtight plate sleeve 108 is arranged between the outer side of the pressurizing plate 107 and the pressurizing housing 101 in a clamping and embedding manner, the pressure relief assembly 109 is arranged on the upper side of the pressurizing housing 101, and the supporting leg 1010 is arranged on the outer side of the bottom end of the pressurizing housing 101.
Referring to fig. 3, the pressure relief assembly 109 includes a sealing clamping plate 1091, a movable rod 1092, an outer limiting seat 1093, an operating handle 1094, a return spring 1095, a sealing washer 1096, a bottom limiting plate 1097 and a sealing ring 1098, the movable rod 1092 is installed inside the sealing clamping plate 1091, the outer limiting seat 1093 is installed at the top of the movable rod 1092, the return spring 1095 is installed outside the movable rod 1092 between the outer limiting seat 1093 and the sealing clamping plate 1091, the operating handle 1094 is installed on the upper side of the outer limiting seat 1093, the sealing washer 1096 is installed on the outer side of the lower half section of the movable rod 1092, the bottom limiting plate 1097 is installed at the bottom of the movable rod 1092, and the sealing ring 1098 is nested outside the bottom limiting plate 1097.
Referring to fig. 4, the evaporation reactor 4 includes a reactor shell 41, a central isolation plate 42, a liquefaction assembly 43, a heating resistor 44, an external electrode 45, a liquid inlet 46, an external sealing cover 47, and an auxiliary material adding port 48, the central isolation plate 42 is disposed at the center of the inside of the reactor shell 41, a sealing door plate is disposed at the outer side of the front end of the reactor shell 41, an opening of the central isolation plate 42 is embedded in an embedding groove 432, the liquefaction assembly 43 is mounted at the upper half section of the central isolation plate 42, the heating resistor 44 is mounted at the inner side of the bottom of the reactor shell 41, the bottom center of the heating resistor 44 is connected to the external electrode 45, the liquid inlet 46 is disposed at each of the two ends of the outside of the reactor shell 41, the external sealing cover 47 is mounted at each of the two sides of the top end of the reactor shell 41, and the auxiliary material adding port 48 is disposed at the center of the upper end of the external sealing cover 47.
Referring to fig. 5, the liquefaction assembly 43 includes a clamping casing 431, a clamping groove 432, a condensation return tank 433, an air suction pump 434, a spiral delivery pipe 435 and an air inlet 436, the clamping groove 432 is disposed at the center of the outer side of the clamping casing 431, the air inlet 436 is disposed at the left upper end of the clamping casing 431, the spiral delivery pipe 435 is connected to the inner side of the air inlet 436, the air suction pump 434 is installed at the end of the spiral delivery pipe 435, and the condensation return tank 433 is installed at the right side of the air suction pump 434.
Referring to fig. 6, the condensing reflux tank 433 includes a condensing shell 4331, a liquid dropping port 4332, an outer snap ring 4333, an outer tube port 4334 and a condensing plate 4335, the bottom of the condensing shell 4331 is provided with the liquid dropping port 4332, the outer snap ring 4333 is disposed on the outer side of the lower half section of the condensing shell 4331, the outer tube port 4334 is disposed on the left side of the condensing shell 4331 above the outer snap ring 4333, and the condensing plate 4335 is disposed on the inner wall of the upper half section of the condensing shell 4331.
In order to better show the use flow of the continuous 4-cyanopyridine evaporative crystallization device, the embodiment now proposes a use method of the continuous 4-cyanopyridine evaporative crystallization device, which comprises the following steps:
the method comprises the following steps: pouring the 4-cyanopyridine solution into the evaporation reaction kettle 4, installing the pressurizing assembly 1 at a liquid inlet 46 at one side of the evaporation reaction kettle 4, closing and sealing various openings, and detecting the air tightness in the evaporation reaction kettle 4 by using the pressurizing assembly 1;
step two: by utilizing the forward movement of the pressurizing plate 107 in the pressurizing assembly 1 and the air-tight pump 3 for conveying air to the evaporation reaction kettle 4, the air pressure in the whole evaporation reaction kettle 4 is improved;
step three: heating crystallization operation is carried out on the 4-cyanopyridine solution in the evaporation reaction kettle 4 by using a heating resistor 44, and steam generated by heating rises to the vicinity of the liquefaction component 43;
step four: the steam is sucked from an air inlet 436 by an air suction pump 434 in the liquefaction assembly 43, is conveyed into a condensation reflux box 433 by a spiral conveying pipe 435, is liquefied by a condensation plate 4335, and then is dripped to the right side of the evaporation reaction kettle 4 through a liquid dripping port 4332;
step five: the solution is heated and crystallized again by the right heating resistor 44, after the heating and crystallization are finished, the liquid in the evaporation reaction kettle 4 is pumped out, and the 4-cyanopyridine crystals on the inner wall of the evaporation reaction kettle 4 are scraped.
The working principle of the invention is as follows: the invention relates to a 4-cyanopyridine continuous evaporative crystallization device and a method, wherein the pressure in an evaporative reaction kettle 4 is increased by a pressurizing component 1, so as to reduce the crystallization temperature of 4-cyanopyridine and the boiling point temperature of other organic solvents, after the pressurization is finished, a heating resistor 44 heats and crystallizes a solution part, so as to ensure that only water, other organic solvents and a small amount of 4-cyanopyridine are vaporized, the 4-cyanopyridine is heated and crystallized, meanwhile, water vapor, other organic solvents and part of 4-cyanopyridine are absorbed and re-liquefied by a condensation reflux box 433 and drop to the right side of the evaporative reaction kettle 4, the heating resistor 44 on the right side carries out evaporative crystallization operation under normal pressure again, so as to separate out the 4-cyanopyridine after crystallization, and the crystal is attached to the right inner wall of the evaporation reaction kettle 4, the solid crystals finally attached to the inner wall of the evaporation reaction kettle 4 are all 4-cyanopyridine, the solution part is water and other impurities, and after the evaporation crystallization is finished and the solution part is extracted, the solid impurities are washed and discharged by deionized water, and then the 4-cyanopyridine solid crystals are obtained by drying.
In summary, the following steps: the invention relates to a 4-cyanopyridine continuous evaporative crystallization device and a method, wherein the pressure in an evaporative reaction kettle 4 is increased by a pressurizing component 1, so as to reduce the crystallization temperature of 4-cyanopyridine and the boiling point temperature of other organic solvents, after the pressurization is finished, a heating resistor 44 heats and crystallizes a solution part, so as to ensure that only water, other organic solvents and a small amount of 4-cyanopyridine are vaporized, the 4-cyanopyridine is heated and crystallized, meanwhile, water vapor, other organic solvents and part of 4-cyanopyridine are absorbed and re-liquefied by a condensation reflux box 433 and drop to the right side of the evaporative reaction kettle 4, the heating resistor 44 on the right side carries out evaporative crystallization operation under normal pressure again, so as to separate out the 4-cyanopyridine after crystallization, and the crystal is attached to the inner wall of the right side of the evaporation reaction kettle 4, the structure of the invention is complete and reasonable, the crystallization operation steps of the 4-cyanopyridine are simplified, and the crystallization amount of the 4-cyanopyridine separated out is effectively improved.
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 (2)
1. The utility model provides a 4-cyanopyridine evaporates crystallization device in succession, includes pressure components (1), connecting pipe (2), airtight pump (3) and evaporation reaction cauldron (4), its characterized in that: a connecting pipe (2) is arranged at the front end of the pressurizing assembly (1), an airtight pump (3) is arranged on the connecting pipe (2), and an evaporation reaction kettle (4) is arranged at the tail end of the connecting pipe (2);
the pressurizing assembly (1) comprises a pressurizing shell (101), a movable groove (102), a hydraulic oil cylinder (103), a hydraulic motor (104), a limiting pressure plate (105), a connecting shaft (106), a pressurizing plate (107), an airtight plate sleeve (108), a pressure relief assembly (109) and supporting legs (1010), wherein the movable groove (102) is arranged on the left side of the pressurizing shell (101), the hydraulic oil cylinder (103) is installed on the left side of the movable groove (102), the hydraulic oil motor (104) is installed on the inner side of the hydraulic oil cylinder (103), the limiting pressure plate (105) is installed in the movable groove (102), the connecting shaft (106) is installed at the center of the bottom of the limiting pressure plate (105), the pressurizing plate (107) is installed at the tail end of the connecting shaft (106), the airtight plate sleeve (108) is installed between the outer side of the pressurizing plate (107) and the pressurizing shell (101) in a clamping and embedding manner, the pressure relief assembly (109) is installed on the upper side of the pressurizing shell (101), the outer side of the bottom end of the pressurizing shell (101) is provided with a supporting leg (1010);
the pressure relief assembly (109) comprises a sealing clamp plate (1091), a movable rod (1092), an outer limiting seat (1093), an operating handle (1094), a reset spring (1095), a sealing washer (1096), a bottom limiting plate (1097) and a sealing clamp ring (1098), the movable rod (1092) is arranged inside the sealing clamp plate (1091), the outer limiting seat (1093) is arranged at the top of the movable rod (1092), the reset spring (1095) is arranged on the outer side of the movable rod (1092) between the outer limiting seat (1093) and the sealing clamp plate (1091), the operating handle (1094) is arranged on the upper side of the outer limiting seat (1093), the sealing washer (1096) is arranged on the outer side of the lower half section of the movable rod (1092), the bottom limiting plate (1097) is arranged at the bottom of the movable rod (1092), and the sealing clamp ring (1098) is nested and arranged on the outer side of the bottom limiting plate (1097);
the evaporation reaction kettle (4) comprises a reaction kettle shell (41), a central isolation plate (42), a liquefaction assembly (43), a heating resistor (44), an external electrode (45), a liquid inlet (46), an external sealing cover (47) and an auxiliary material adding port (48), a central isolation plate (42) is arranged at the center of the inner part of the reaction kettle shell (41), a sealing door plate is arranged on the outer side of the front end of the reaction kettle shell (41), a liquefaction component (43) is arranged on the upper half section of the central isolation plate (42), the inner side of the bottom of the reaction kettle shell (41) is provided with a heating resistor (44), the center of the bottom of the heating resistor (44) is connected with an external electrode (45), liquid inlets (46) are respectively arranged at the two ends of the outer side of the reaction kettle shell (41), outer sealing covers (47) are respectively arranged on two sides of the top end of the reaction kettle shell (41), an auxiliary material adding port (48) is formed in the center of the upper end of the outer sealing cover (47);
the liquefaction assembly (43) comprises a clamping and embedding shell (431), a clamping and embedding groove (432), a condensation backflow box (433), an air suction pump (434), a spiral conveying pipe (435) and an air inlet (436), wherein the clamping and embedding groove (432) is formed in the center of the outer side of the clamping and embedding shell (431), an opening of the central isolation plate (42) is clamped and embedded in the clamping and embedding groove (432), the air inlet (436) is formed in the upper left end of the clamping and embedding shell (431), the spiral conveying pipe (435) is connected to the inner side of the air inlet (436), the air suction pump (434) is installed at the tail end of the spiral conveying pipe (435), and the condensation backflow box (433) is installed on the right side of the air suction pump (434);
condensation return-flow case (433) are including condensation shell (4331), drip mouth (4332), outer snap ring (4333), outer tube interface (4334) and condensing plate (4335), the bottom of condensation shell (4331) is equipped with drip mouth (4332), the lower half section outside of condensation shell (4331) is equipped with outer snap ring (4333), condensation shell (4331) the left side of outer snap ring (4333) upside is equipped with outer tube interface (4334), be equipped with condensing plate (4335) on the first section inner wall of condensation shell (4331).
2. A method for using the continuous evaporative crystallization apparatus for 4-cyanopyridine according to claim 1, comprising the steps of:
s1: pouring the 4-cyanopyridine solution into an evaporation reaction kettle (4), installing a pressurizing assembly (1) at a liquid inlet (46) at one side of the evaporation reaction kettle (4), closing and sealing various openings, and detecting the air tightness in the evaporation reaction kettle (4) by using the pressurizing assembly (1);
s2: the forward movement of a pressurizing plate (107) in the pressurizing assembly (1) is utilized, and the gas is conveyed to the evaporation reaction kettle (4) by the airtight pump (3), so that the gas pressure in the whole evaporation reaction kettle (4) is improved;
s3: heating crystallization operation is carried out on the 4-cyanopyridine solution in the evaporation reaction kettle (4) by using a heating resistor (44), and steam generated by heating rises to the vicinity of the liquefaction component (43);
s4: the steam is sucked from an air inlet (436) through an air suction pump (434) in the liquefaction assembly (43), is conveyed into a condensation reflux box (433) through a spiral conveying pipe (435), is liquefied through a condensing plate (4335), and then is dripped to the right side of the evaporation reaction kettle (4) through a liquid dripping port (4332);
s5: heating crystallization operation is carried out on the solution again by a heating resistor (44) on the right side, after the heating crystallization is finished, liquid in the evaporation reaction kettle (4) is pumped out, and 4-cyanopyridine crystals on the inner wall of the evaporation reaction kettle (4) are scraped.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011471723.1A CN112691403B (en) | 2020-12-14 | 2020-12-14 | 4-cyanopyridine continuous evaporation crystallization device and method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011471723.1A CN112691403B (en) | 2020-12-14 | 2020-12-14 | 4-cyanopyridine continuous evaporation crystallization device and method |
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| CN110655489A (en) * | 2019-11-11 | 2020-01-07 | 安徽瑞邦生物科技有限公司 | Method for purifying 4-cyanopyridine by volatilization and recrystallization |
| CN113940356A (en) * | 2021-07-08 | 2022-01-18 | 安徽广信农化股份有限公司 | Indoxacarb microemulsion and preparation method thereof |
| CN114113398B (en) * | 2021-11-29 | 2023-07-07 | 安徽泽升科技有限公司 | Pretreatment analysis system and method for medical intermediate |
| CN115178213B (en) * | 2022-07-11 | 2023-06-27 | 西安国康瑞金制药有限公司 | Preparation system and preparation process of dexamethasone sodium phosphate |
| CN117463556B (en) * | 2023-12-27 | 2024-03-12 | 福建省德旭新材料有限公司 | Preparation facilities of solid super acidic catalyst for preparation of ethylene sulfate |
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| CN201454142U (en) * | 2009-07-27 | 2010-05-12 | 四川华通能源材料有限公司 | Novel crystallization kettle for chemical industry |
| CN203355349U (en) * | 2013-08-07 | 2013-12-25 | 湖北宜恒茶油产业科技有限责任公司 | Crystallizing tank with air compression function |
| CN105582689A (en) * | 2016-03-10 | 2016-05-18 | 黄斌 | Reaction crystallizer for crystallization |
| CN208275041U (en) * | 2017-12-22 | 2018-12-25 | 南京工业大学 | Recrystallization device for efficient purification and reuse of salt slag after pesticide wastewater treatment and separation |
| CN209519378U (en) * | 2018-12-27 | 2019-10-22 | 天津市绿禾食品添加剂有限公司 | A kind of evaporated crystallization device extracted for Iodine |
| CN209952276U (en) * | 2019-05-12 | 2020-01-17 | 江苏嘉泰蒸发设备股份有限公司 | Integrated evaporative crystallization device |
| CN211411056U (en) * | 2019-10-08 | 2020-09-04 | 常州百特环保科技有限公司 | Sewage flocculating agent production is with crystallization solidification equipment |
| CN110655489A (en) * | 2019-11-11 | 2020-01-07 | 安徽瑞邦生物科技有限公司 | Method for purifying 4-cyanopyridine by volatilization and recrystallization |
| CN211676388U (en) * | 2020-02-20 | 2020-10-16 | 江苏紫东食品有限公司 | Continuous crystallization device for potassium chloride |
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| CN212069793U (en) * | 2020-04-24 | 2020-12-04 | 江西省欧陶科技有限公司 | Blowing device for sodium metasilicate pentahydrate discharge pipe |
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