CN116967023B

CN116967023B - 3-Trifluoromethyl-4-nitrophenol recrystallization centrifugal device and process

Info

Publication number: CN116967023B
Application number: CN202310683348.4A
Authority: CN
Inventors: 罗汇; 孙德明; 吴刚; 姚鑫锋; 花磊
Original assignee: Jiangsu Yongchuang Pharmaceutical Technology Co ltd
Current assignee: Jiangsu Yongchuang Pharmaceutical Technology Co ltd
Priority date: 2023-06-09
Filing date: 2023-06-09
Publication date: 2024-07-05
Anticipated expiration: 2043-06-09
Also published as: CN116967023A

Abstract

The invention relates to the technical field of chemical equipment production, in particular to a 3-trifluoromethyl-4-nitrophenol recrystallization centrifugal device which comprises a base, wherein a shell is fixedly arranged on the base, a rotary strand is rotatably arranged in the shell, and an upper cover is rotatably arranged on the side wall of the shell. According to the invention, the crushing unit and the spreading unit are arranged on the upper cover, after centrifugal personnel pour materials into the centrifugal machine, the crushing unit can automatically crush the materials in the centrifugal machine uniformly, the spreading unit can automatically uniformly spread the crushed materials in the centrifugal machine, the automation and integration degree of the recrystallization centrifugal process are improved, meanwhile, the time required for crushing and debugging the centrifugal machine is reduced, and the production efficiency of the 3-trifluoromethyl-4-nitrophenol recrystallization centrifugal process is further improved. The invention also provides a 3-trifluoromethyl-4-nitrophenol recrystallization centrifugal process using the centrifugal device.

Description

3-Trifluoromethyl-4-nitrophenol recrystallization centrifugal device and process

Technical Field

The invention relates to the technical field of chemical equipment production, in particular to a 3-trifluoromethyl-4-nitrophenol recrystallization centrifugal device and a process.

Background

3-Trifluoromethyl-4-nitrophenol is a highly toxic and flammable organic substance commonly used for preparing pesticides. The existing 3-trifluoromethyl-4-nitrophenol production process comprises the following steps: respectively adding sulfuric acid, nitric acid and m-fluorobenzotrifluoride into a nitration kettle to generate nitration materials, returning the nitration materials into an enamel kettle to perform a water washing process and an alkali washing process, separating the alkali washed materials into materials, loading the materials into a plastic barrel to perform a cooling crystallization reaction, placing the cooled and crystallized materials into a filtering centrifuge to perform solid-liquid separation, then performing a water washing process on the centrifuged solid, and finally drying and storing the washed solid.

Before the existing trifluoromethyl-4-nitrophenol is subjected to a centrifugal process, the size of crystals after freezing and crystallizing the trifluoromethyl-4-nitrophenol is larger, the crystals are not suitable for being directly guided into a filter centrifuge through a conveying pipeline, a worker is required to open an upper cover of the filter centrifuge, materials in a plastic barrel are manually poured into the filter centrifuge, or the crystallized materials are firstly put into crushing equipment for crushing, then the crushed crystallized materials are transferred into the centrifuge, then the centrifugally worker manually crushes the crystals and uniformly spreads the crystals in the filter centrifuge by using a tool, so that the filter centrifuge rotates stably, if the first time is unstable, the machine is immediately stopped and spread for the second time, and the centrifugally worker needs to repeatedly debug until the filter centrifuge runs stably. However, the crystals are crushed manually, and the crushed crystals are different in size, so that the crystals are difficult to spread by workers, and therefore, the filter centrifuge is required to be debugged for many times and then rotated stably. The crystallization materials can be crushed uniformly by crushing equipment, but the time for transporting, loading and unloading the crystallization materials in the recrystallization centrifugal process is increased. The two methods waste a lot of time and affect the production efficiency of the 3-trifluoromethyl-4-nitrophenol.

Therefore, the 3-trifluoromethyl-4-nitrophenol recrystallization centrifugal device and the process are provided, a smashing unit and a spreading unit are arranged in a filtering centrifugal machine, after a worker pours materials into the filtering centrifugal machine, the smashing unit can automatically and rapidly smash crystals into fragments with approximate sizes, and the spreading unit can automatically and uniformly spread the smashed materials in the centrifugal machine, so that the time for smashing the crystallized materials by the worker and debugging the filtering centrifugal machine is reduced, and the production efficiency of the 3-trifluoromethyl-4-nitrophenol production process is improved.

Disclosure of Invention

The invention aims to provide a 3-trifluoromethyl-4-nitrophenol recrystallization centrifugal device and a process, which ensure that the crystallization materials can be uniformly spread in a rotating strand by uniformly crushing the crystallization materials, so that the centrifugal machine can stably operate, and the production efficiency of the 3-trifluoromethyl-4-nitrophenol recrystallization centrifugal process is improved; therefore, the invention improves the automation and integration degree of the 3-trifluoromethyl-4-nitrophenol recrystallization centrifugal process by installing the smashing unit on the upper cover, reduces the smashing time of the smashing step while evenly smashing the crystallized materials, and further improves the production efficiency of the 3-trifluoromethyl-4-nitrophenol recrystallization centrifugal process so as to solve the problems in the background art.

In order to achieve the above purpose, the present invention provides the following technical solutions:

A3-trifluoromethyl-4-nitrophenol recrystallization centrifugal device and a process thereof comprise:

The device comprises a base, wherein a shell is fixedly arranged on the base, a rotary strand is rotationally arranged on the shell, a plurality of fan-shaped discharging holes are uniformly formed in the bottom wall of the rotary strand in a rotary mode, discharging holes communicated with the discharging holes are formed in the bottom wall of the base, an upper cover is rotationally arranged on the side wall of the shell, a leaching spray pipe penetrates through the circle center of the upper cover, a power unit for driving the rotary strand to rotate is arranged on the base, and a scraping plate unit for scraping materials on the rotary strand during discharging is arranged on the top wall of the upper cover;

The upper cover is provided with an annular through hole, the upper cover is divided into an inner circle and an outer circle by the annular through hole, an annular protective shell with a U-shaped cross section is arranged between the inner circle and the outer circle, the annular protective shell is located right above the annular through hole, sliding grooves are formed in the side wall of the annular through hole, a first gear ring is arranged in the annular through hole in a sliding mode, sliding rails matched with the sliding grooves are arranged on two sides of the first gear ring, a motor is arranged on the top wall of the upper cover, a first gear wheel matched with the first gear ring is fixedly arranged at the output end of the motor, a crushing unit for uniformly crushing crystalline materials is arranged on the bottom wall of the first gear ring, a uniformly spreading unit for spreading the crushed crystalline materials is arranged on the bottom wall of the first gear ring, and a sealing unit for preventing the crystalline materials from falling from a discharging hole to the outside of a rotating strand when the crushing unit is arranged in the bottom wall of the rotating strand.

When the existing 3-trifluoromethyl-4-nitrophenol is subjected to a centrifugal process after crystallization, firstly, manually pouring a crystallization material into a rotating strand of a centrifugal machine through a centrifugal staff, then manually crushing the crystallization material, then using a wooden stick to rotate to flatten the crystallization material, and finally starting the centrifugal machine. If the centrifuge personnel find that the rotation of the centrifuge is unstable, the centrifuge is required to be closed, then the crystalline material is re-flattened, then the centrifuge is restarted, and the centrifuge personnel need to be repeatedly debugged until the centrifuge can rotate stably. The existing centrifuges used in the 3-trifluoromethyl-4-nitrophenol centrifugal process are generally flat plate type filter centrifuges, such as PGZ series, PS series and the like. However, since the crystals of 3-trifluoromethyl-4-nitrophenol are not suitable for transportation by solid-liquid mixing, the existing centrifugation process does not use the feed line of the centrifuge itself.

The manual crushing of the crystalline material cannot ensure that the size of the crushed crystalline material is basically consistent, and the speed is low. The crystallization materials with different sizes can cause difficulty in flattening the crystallization materials by workers, so that the filtration centrifugal machine is always required to rotate stably after multiple times of experiments, a great deal of time is wasted, and the production efficiency of the 3-trifluoromethyl-4-nitrophenol is affected. Therefore, on the basis of removing the feeding pipeline of the existing centrifugal machine, the centrifugal device is provided with the annular through hole on the upper cover, and the annular through hole is positioned between the leaching spray pipe and the scraper unit and does not interfere with the leaching spray pipe and the scraper unit. The annular protective shell is arranged above the annular through hole and is divided into two parts of an inner circle and an outer circle by the annular through hole to be connected to form a whole, so that the annular protective shell has certain strength requirements, and can be made of metal materials such as 45 and 40 Cr. And a gear ring I is arranged in the annular through hole in a sliding manner through the matching of the sliding groove and the sliding rail, and teeth of the gear ring I are positioned at the top of the gear ring I. The annular protective housing still plays the guard action to ring gear one, avoids piling up impurity dust on the ring gear one and influences the rotation. The top of the upper cover is provided with a motor, and the motor adopts a speed regulating motor, such as an electromagnetic speed regulating motor, a direct current speed regulating motor, a PWM frequency conversion speed regulating motor and the like. The motor drives the gear ring to rotate through the gear, so that the crushing unit and the spreading unit are controlled to act on the crystallized materials. After the centrifugal personnel start the motor, the motor rotates rapidly to drive the crushing unit to crush the crystalline material into uniform individuals, then the motor decelerates to a set speed, the crushing unit cannot act on the crystalline material at the moment, the spreading unit uniformly spreads the crushed material in the rotating strand, the motor is automatically closed after a period of time, and the centrifugal personnel can start the centrifugal machine to perform centrifugation.

The closed unit can seal the discharge hole under the static state of rotatory strand, prevents when smashing the unit and smashes crystalline material, and crystalline material leaves from the discharge hole because of sputtering leads to partial crystalline material to not centrifugal, influences centrifugal process's eccentricity. The centrifuge rotates at a low speed during discharge, and the closed unit opens the discharge hole under the action of centrifugal force of the rotating strands.

Preferably, the crushing unit comprises a rotating shaft rotatably mounted on a bottom wall of the gear ring, a cutter is fixedly mounted at one end, far away from the first gear ring, of the rotating shaft, a second gear is fixedly mounted at one end, close to the first gear ring, of the rotating shaft, a second gear ring matched with the second gear is fixedly mounted on the bottom wall of the upper cover, and a lifting unit is mounted in the rotating shaft.

When the motor drives the first gear to rotate rapidly, the gear ring rotates under the action of the first gear, and the rotating shaft rotatably arranged at the bottom of the first gear ring moves along with the first gear ring. When the rotating shaft moves, the second gear on the rotating shaft is continuously meshed with the second gear, so that the rotating shaft can rotate under the cooperation of the second gear and the second gear, the second gear and the second gear are required to adopt a larger transmission ratio to realize the rapid rotation of a cutter so as to form a crushing effect similar to a wall breaking machine, and the second gear are required to adopt high-strength materials and structures, can be made of materials such as 20Cr and 40Cr, and simultaneously adopt a helical tooth structure or a herringbone tooth structure. The rotation of the rotating shaft drives the cutter to rotate so as to crush the crystallized materials, and the cutter is generally made of 304 stainless steel. The cutter can use Y-shaped blades or cross-shaped blades, and the length of the blades is generally 5cm-10cm and is selected according to the size of the rotating strand of the centrifugal machine because the space in the rotating strand is large. The rotating speed of the cutter of the existing wall breaking machine can reach 16000r/min, materials can be crushed into diameters of tens of micrometers to hundreds of micrometers, and the invention does not need to crush the materials to such an extent, so that the rotating speed of the cutter of the invention is 3500r/min-4000r/min, and the crushed diameter of crystalline materials is 1mm-3mm, thereby achieving the set effect.

The crushing unit can also directly drive the cutter to rotate through the motor, so that the method is simpler in structure, the rotating speed of the cutter is faster, but the equipment cost is higher, and meanwhile, the arrangement of the electric wires is more troublesome because the rotating shaft rotates along with the gear ring, and the electric wires can be selected according to actual conditions.

The lifting unit in the rotating shaft is used for adjusting the height of the cutter and takes the centrifugal force generated when the rotating shaft rotates as a driving force. When the motor rotates rapidly, the rotating shaft rotates rapidly, the lifting unit drives the cutter to move towards the direction close to the bottom wall of the rotating strand and stop at a position 1cm-3cm away from the bottom wall of the rotating strand, and the cutter is fully contacted with the crystallization material at the moment; when the motor rotates at a low speed, the rotating shaft rotates at a low speed, and at the moment, due to insufficient centrifugal force, the lifting unit drives the cutter to move in the direction away from the bottom wall of the rotating strand and restore to an initial state, and at the moment, the cutter is not contacted with the crystallization material. The lifting unit can prevent the cutter from interfering the spreading unit to spread the crystallization material.

Preferably, the lifting unit comprises a movable groove formed in the bottom wall of the rotating shaft, the section of the movable groove is a non-revolving body, a conical movable space is formed in one end, close to the bottom wall of the rotating shaft, of the movable groove, a movable rod is elastically installed in the movable groove through an elastic piece, a cutter is fixedly installed at one end, far away from the elastic piece, of the movable rod, a centrifugal rod is symmetrically installed at one end, close to the elastic piece, of the movable rod, and a centrifugal ball is fixedly installed at one end, far away from the movable rod, of each centrifugal rod.

The movable groove is of a non-revolving body in cross section, and the movable rod slidably installed in the movable groove is of a non-revolving body in cross section, so that the movable rod can move in the movable groove along the axis direction of the rotating shaft and cannot rotate relative to the rotating shaft. When the rotating shaft rotates rapidly, the centrifugal ball moves in a direction away from the movable rod, so that the centrifugal ball is matched with the conical movable space to drive the centrifugal rod to move in a direction approaching to the horizontal direction, and meanwhile, the centrifugal rod drives the movable rod to overcome the first elastic piece to move in a direction away from the first gear ring, and a cutter at one end of the movable rod moves synchronously with the movable rod; when the rotating shaft rotates slowly, the movable rod moves towards the direction close to the first gear ring under the action of the first elastic piece due to insufficient centrifugal force, and the cutter moves synchronously along with the movable rod. The first elastic element can be a spring, a reed, a clockwork spring, etc.

Because the volume that the toper activity space needs is bigger than the movable groove, consequently can set up the pivot to echelonment, the one end that keeps away from the ring gear one is the part that the diameter is great, and the length of the great part of diameter equals the length that the cutter can flexible removal, consequently need select according to actual conditions. And the conical movable space is also arranged with smaller cross-section diameter near one end of the gear ring I. The centrifugal ball needs to rotate to generate centrifugal force to overcome the first elastic piece, and meanwhile, the centrifugal ball needs to frequently generate relative friction with the conical movable space, so that the centrifugal ball can be made of wear-resistant metal materials, such as high manganese alloy, chromium carbide alloy and the like.

The lifting unit may also be realized by using a telescopic drive unit, such as a cylinder, an electric push rod, etc. The structure is simpler, and the production and processing precision is lower. However, the equipment cost of this method is higher, and at the same time, the arrangement of the electric wires (pipelines) is troublesome because the rotating shaft rotates along with the first gear ring, and the electric wires (pipelines) can be selected according to practical situations.

Preferably, the spreading unit comprises a sleeve vertically and fixedly arranged on a bottom wall of the gear ring, a plurality of first positioning holes are uniformly formed in the sleeve, a fixing rod is slidably arranged in the sleeve, a second positioning hole matched with the first positioning holes is uniformly formed in the fixing rod, a first pushing plate is fixedly arranged at one end, far away from the first gear ring, of the fixing rod, an extension line of the first pushing plate penetrates through a center of a rotary strand, and a second pushing plate is rotatably arranged at one end, far away from the center of the rotary strand, of the first pushing plate through a torsion spring.

Since the existing 3-trifluoromethyl-4-nitrophenol is subjected to the crystallization process according to the temperature, the crystals precipitated in each vessel are substantially quantitative (generally 90%). When the centrifugal process is carried out, the crystallized materials poured into the centrifugal machine are also quantitative each time, so before the centrifugal machine is started, the first pushing plate and the second pushing plate are required to be positioned through the matching of the first positioning hole on the sleeve and the second positioning hole on the fixed rod, the first pushing plate and the second pushing plate are adjusted to be at proper heights, when the gear ring rotates, the first pushing plate and the second pushing plate rotate around the center of a rotating strand, the first pushing plate and the second pushing plate push the crushed crystallized materials with higher accumulation to the position where the crushed crystallized materials with fewer accumulation are pushed, and therefore the first pushing plate and the second pushing plate can flatten the crushed crystallized materials. The push plate can be made of light high-strength materials such as carbon fiber and polytetrafluoroethylene.

In order to prevent materials from splashing out of the rotary strand in a centrifugal manner, the edge of the opening end of the rotary strand is set to be arc-shaped, and the circle center of the arc points to the axis of the rotary strand, so that the diameter of the inside of the rotary strand is larger than that of the opening of the rotary strand, and collision interference between a push plate and the rotary strand is avoided when the upper cover is opened. According to the invention, the push plate is divided into the first push plate and the second push plate, the first push plate is connected with the fixed rod, the second push plate is connected to one end of the second push plate through the torsion spring in a rotating way, when the upper cover is opened, the second push plate can be contacted with the rotating strand, the second push plate can extrude the torsion spring to rotate so as to avoid the rotating strand, and after the upper cover is completely opened, the torsion spring can enable the second push plate to recover to an initial state, and at the moment, the first push plate and the second push plate are parallel to the bottom wall of the upper cover. The principle of closing the upper cover is the same.

Compared with the cooperation through the locating hole, sleeve and dead lever can also be through seting up the screw hole in the sleeve one end of keeping away from the ring gear one, fix a position through the scale on the friction force cooperation sleeve that the bolt applyed the dead lever. Compared with the step-by-step adjustment, the positioning mode can realize adjustment at any distance, but the fixing effect of friction force is poorer than that of a bolt, so that the positioning mode can be selectively applied according to actual conditions.

Preferably, the sleeve and the rotating shaft are symmetrically arranged around the center of the first gear ring.

In order to avoid interference between the first pushing plate and the second pushing plate and the cutter, the sleeve is arranged at the position of the first gear ring, which is symmetrical to the rotating shaft, so that the sleeve is 180 degrees away from the rotating shaft on the first gear ring, and after the motor is decelerated, the crushed crystalline material can be flattened by only rotating the first gear ring for half a circle, but for the sake of safety, the motor is generally set to drive the first gear ring to rotate for 5-10 circles in a low-speed state.

Preferably, the closed unit comprises an open slot arranged on the side wall of the fan-shaped discharging hole far away from the center of the rotary strand, a fan-shaped baffle matched with the fan-shaped discharging hole is elastically installed in the open slot through a second elastic piece, a first magnet is embedded in one end of the fan-shaped baffle far away from the second elastic piece, and a second magnet which is mutually attracted with the first magnet is embedded in the side wall of the fan-shaped discharging hole near the center of the rotary strand.

When the centrifugal machine is started, the rotary strand can rotate to drive materials in the rotary strand to carry out centrifugal filtration, and when the centrifugal machine is discharged, the rotary strand can rotate at a low speed. In both cases, the fan-shaped baffle will compress the second elastic member under the action of centrifugal force to open the discharge hole. When the rotary strand is static, the sector baffle can seal the discharge hole under the action of the elastic piece II, so that when the crushing unit crushes the crystalline material, the crystalline material leaves from the discharge hole without centrifugation due to sputtering, and the eccentricity of the centrifugal process is influenced. The second elastic element can be a spring, a reed, a clockwork spring and the like.

In order to prevent the fan-shaped baffle plate from rotating just after the rotating strand starts to open a gap with the discharge hole, the crystallization material is not thrown onto the side wall of the rotating strand under the action of centrifugal force, and the discharge hole is opened at the moment, so that part of crystallization material leaves from the discharge hole without centrifugation, and the eccentricity of the centrifugation process is affected. Therefore, the invention solves the problem by controlling the rotating speed required by the fan-shaped baffle when the discharging hole starts to be opened through the matching of the magnet I and the magnet II.

Preferably, the edge of the open groove close to the bottom wall of the inner side of the rotary strand is provided with an inclined surface.

The opening groove is positioned on the side wall of the discharging hole, so that the height difference of the steps exists between the top wall of the fan-shaped baffle plate and the bottom wall of the rotating strand, and in order to prevent part of crystal materials from accumulating at the steps and not reaching the side wall of the rotating strand when the rotating strand rotates and affecting the centrifugal effect, the step is set to be an inclined surface, the inclined angle is 30-45 degrees, and the crystal materials can conveniently slide onto the bottom wall of the rotating strand from the fan-shaped baffle plate. And meanwhile, the inclined plane can scrape off the crystallization materials attached to the top wall of the fan-shaped baffle plate when the fan-shaped baffle plate moves towards the open slot, so that the crystallization materials are prevented from affecting the movement of the fan-shaped baffle plate. When the open slot edge is vertical face, can scrape the crystallization material down equally, but the crystallization material that scrapes down drops very easily because vertical face's the jam in unloading the sky, causes partial crystallization material unable centrifugal dehydration, and the inclined plane then can not appear such problem.

Preferably, a fixed block for preventing the elastic piece II from being excessively compressed is arranged on the bottom wall of the inner side of the opening groove.

In order to prevent the second elastic element from being excessively extruded by the sector baffle plate to cause the second elastic element to fail, the invention is provided with a fixed block on the bottom wall of the inner side wall of the opening groove to limit the limit position of the movement of the sector baffle plate. The fixed block can enable the magnet on the fan-shaped baffle plate to just enter the open slot for 2mm-5mm. Because the angular acceleration of the rotating strand is very large, the moving speed of the fan-shaped baffle plate when the discharging hole is opened is very high, and therefore, damping materials such as rubber, sponge and the like can be covered on the fixed block, the impact force of the fan-shaped baffle plate when the fan-shaped baffle plate is contacted with the fixed block is reduced, and the service lives of the fixed block and the fan-shaped baffle plate are prolonged.

Preferably, a 3-trifluoromethyl-4-nitrophenol recrystallization centrifugation process comprises:

S1: after the recrystallization personnel receives the water-washed material, adding a certain amount of methanol into each barrel of water-washed material immediately, stirring for 5 minutes by using a wooden stick, then placing the mixture into a brine tank for cooling and crystallizing, stirring once every one hour, and carrying out a centrifugal process when more than 90% of the material is separated out or the temperature reaches about 0 to-2 ℃;

S2: the centrifugal staff opens the upper cover of the centrifugal machine, puts the filter cloth on the centrifugal machine and rotates slowly to enable the filter cloth to be clung to the rotating strand, then pouring quantitative crystalline materials into the rotating strand of the centrifugal machine, closing the fan-shaped discharging hole by the closing unit, discharging primary mother liquor from the drain pipe of the base through the filter cloth and the rotating strand, closing the upper cover by the centrifugal staff, then starting the motor, driving the gear ring through the first gear for a set time of rapid rotation, uniformly crushing the crystalline materials by the crushing unit in the process, driving the gear ring through the gear by the motor for a set time of slow rotation, and uniformly spreading the crushed crystalline materials in the rotating strand by the spreading unit in the process;

S3: after the motor runs for a set time, the motor is automatically closed, a centrifugal person starts a power unit, the power unit drives a rotating strand to rotate, materials in the rotating strand are piled up and attached on the side wall of the rotating strand under the action of centrifugal force, primary mother liquor and crystallized materials are separated under the action of the centrifugal force, and a closed unit opens a fan-shaped discharging hole under the action of the centrifugal force;

S4: any impurity peak when centrifuging 2-nitro-5 fluorine is less than 0.2%, a small amount of methanol is used for leaching when the standard is not met through inspection, until the standard is met, mother liquor separated during leaching is leaching mother liquor, after any impurity peak when centrifuging 2-nitro-5 fluorine, a centrifugal worker starts a scraper blade unit, at the moment, a rotating strand rotates at a low speed, a scraper blade scrapes off centrifugal materials from the side wall of the rotating strand, and the centrifugal materials enter a discharge opening of a base from a fan-shaped discharge hole;

S5: after the crystallization materials are completely centrifuged, a centrifugal worker closes the power unit, and then the primary mother liquor, the leaching mother liquor and the centrifugal materials are respectively packaged by containers.

Compared with the prior art, the invention has the beneficial effects that:

1. When the 3-trifluoromethyl-4-nitrophenol is centrifuged, the crystalline material is required to be crushed uniformly, and then the crushed material is uniformly spread in a rotating strand, so that the centrifuge can rotate stably. Therefore, the crushing unit is arranged on the upper cover, and after the centrifugal personnel pour the crystalline material into the centrifugal machine, the crushing unit can automatically crush the crystalline material, so that the automation and integration degree of the 3-trifluoromethyl-4-nitrophenol recrystallization centrifugal process are improved, the time required for crushing steps and debugging the centrifugal machine is reduced, the difficulty of manually spreading the crystalline material is reduced, and the production efficiency of the 3-trifluoromethyl-4-nitrophenol recrystallization centrifugal process is improved.

2. The spreading unit can uniformly spread the crystallized materials crushed by the crushing unit in the rotating strand when the gear ring rotates at a low speed on the premise that the phenomenon that the crystallized materials are not collided and interfered with the rotating strand when the upper cover is opened and closed is met. Compared with the prior art that the crystallization material is spread by manually rotating the wooden stick, the spreading unit can rapidly spread the crushed crystallization material uniformly, so that the centrifugal machine can stably rotate, the time of material spreading step is shortened, and the production efficiency of the 3-trifluoromethyl-4-nitrophenol recrystallization centrifugal process is further improved.

3. Through installing the sealed unit in the discharge opening department, the sealed unit can be closed the discharge opening under rotatory stationary state of thigh, can open the discharge opening according to the rotational speed size of rotatory thigh voluntarily when rotatory thigh to this prevents when smashing the unit and smashes crystalline material, and crystalline material just leaves from the discharge opening because of the sputtering leads to partial crystalline material to not centrifugal, influences centrifugal process's eccentricity and centrifugal effect, but can not influence the centrifuge simultaneously and unload.

Drawings

FIG. 1 is a schematic diagram of the overall structure of the present invention;

FIG. 2 is an enlarged view of a portion of FIG. 1 at A;

FIG. 3 is a cross-sectional view B-B of FIG. 1;

FIG. 4 is a schematic view of portion I of FIG. 3;

FIG. 5 is a schematic view of section II of FIG. 3

FIG. 6 is an enlarged view of a portion of FIG. 3 at F;

FIG. 7 is an enlarged view of a portion of FIG. 4 at E;

FIG. 8 is a cross-sectional view of C-C of FIG. 3;

FIG. 9 is an enlarged view of a portion of the portion G of FIG. 8;

FIG. 10 is an enlarged view of a portion of the portion H of FIG. 8;

FIG. 11 is a sectional view of D-D of FIG. 3;

FIG. 12 is an enlarged view of a portion of the portion J of FIG. 11;

FIG. 13 is a cross-sectional view of an open slot of the present invention;

fig. 14 is a schematic view showing the overall structure of the upper cover of the present invention.

In the figure: 1. a base; 2. a housing; 3. rotating the strand; 4. a discharge hole; 5. a discharge port; 6. an upper cover; 601. an annular through hole; 7. eluting the spray pipe; 8. a squeegee unit; 9. an annular protective shell; 10. a chute; 11. a slide rail; 1201. a first gear ring; 1202. a second gear ring; 1301. a first gear; 1302. a second gear; 14. a motor; 15. a rotating shaft; 16. a cutter; 17. a movable groove; 18. a conical movable space; 19. a movable rod; 20. a centrifugal rod; 21. a centrifugal ball; 22. a sleeve; 2301. positioning holes I; 2302. positioning holes II; 2401. an elastic piece I; 2402. an elastic piece II; 25. a fixed rod; 2601. a pushing plate I; 2602. a pushing plate II; 27. an open slot; 28. a fan-shaped baffle; 2901. a first magnet; 2902. a second magnet; 30. and a fixed block.

Detailed Description

The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to fig. 1 to 14 of the drawings, and it is apparent that the embodiments of the present invention include, but are not limited to, the embodiments described below. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.

The terms "first" and "second" in the present application are used for the purpose of describing the order of objects only, and are not intended to represent relative importance or to describe the number of technical features indicated. Thus, a feature defining "a first" or "a second" may explicitly or implicitly include at least one such feature. The term "plurality" as used in the present application means at least two.

Referring to fig. 1 to 14, the present invention provides a 3-trifluoromethyl-4-nitrophenol recrystallization and centrifugation process, which comprises the following steps:

S1: after receiving the water washing material, the recrystallization personnel immediately adds 3kg of methanol into each barrel (30 kg of a 50L plastic barrel) of water washing material, stirs for 5 minutes by using a wooden stick, then puts the mixture into a brine tank for cooling crystallization, stirs the mixture once every one hour, and can carry out a centrifugation process when the material is separated out by more than 90% or the temperature reaches about 0 to-2 ℃;

S2: the centrifugal staff opens the upper cover 6 of the PGZ-1250 centrifuge, puts the filter cloth on the PGZ-1250 centrifuge to rotate slowly so that the filter cloth is tightly attached to the rotating strand 3, then pours 90kg of crystal materials into the rotating strand 3 of the centrifuge, the closing unit closes the sector discharge hole 4 at the moment, primary mother liquor can pass through the filter cloth and the rotating strand 3 to be discharged from the drain pipe of the base 1, the centrifugal staff closes the upper cover 6, then starts the 180WD-M16030-72V motor 14, the 180WD-M16030-72V motor 14 can drive the gear ring one 1201 to run for 0.5min at the speed of 60r/min through the gear one 1301, the crushing unit can uniformly crush the crystal materials in the process, the 180WD-M16030-72V motor 14 can drive the gear ring one 1201 to rotate slowly for a set time through the gear one 1301, and the spreading unit can uniformly spread the crushed crystal materials in the rotating strand 3 in the process;

s3: after the 180WD-M16030-72V motor 14 runs for a set time, the power unit is started by a centrifugal operator, the power unit drives the rotary strand 3 to rotate, materials in the rotary strand 3 are piled up and attached on the side wall of the rotary strand 3 under the action of centrifugal force, primary mother liquor and crystallized materials are separated under the action of the centrifugal force, and the fan-shaped discharging hole 4 is opened by the closed unit under the action of the centrifugal force;

S4: any impurity peak when centrifuging 2-nitro-5 fluorine is less than 0.2%, a small amount of methanol is used for leaching when the standard is not met through inspection, until the standard is met, mother liquor separated during leaching is leaching mother liquor, after any impurity peak when centrifuging 2-nitro-5 fluorine, a centrifuge starts a scraper unit 8, at the moment, a rotary strand 3 rotates at a low speed, a scraper scrapes off centrifugal materials from the side wall of the rotary strand 3, and the centrifugal materials enter a discharge opening 5 of a base 1 from a fan-shaped discharge hole 4;

S5: after the crystallization materials are completely centrifuged, a centrifugal worker closes the power unit, and then the primary mother liquor, the leaching mother liquor and the centrifugal materials are respectively filled into a 50L barrel, a 200L barrel and a 2000L enamel kettle.

In the first embodiment, referring to fig. 1 to 14, when the cutter 16 is driven by the cooperation of the gear and the ring gear.

After the centrifugal personnel completely pour the crystallization material into the rotating strand 3, the fixing rod 25 is adjusted to a proper position through the locating pin, then the upper cover 6 is closed, the upper cover 6 is fastened, in the closing process of the upper cover 6, the second push plate 2602 rotates to avoid after contacting the edge of the opening of the rotating strand 3, until the second push plate 2602 completely enters the rotating strand 3, and the second push plate 2602 is restored to the same horizontal plane with the first push plate 2601 under the action of the torsion spring. After the upper cover 6 is locked, the push plate and the push plate are 20cm away from the bottom wall of the inner side of the rotary strand 3, a centrifugal person starts the 180WD-M16030-72V motor 14 and the 180WD-M16030-72V motor 14 to regulate the speed of the motor 14 to 1800r/min, the 180WD-M16030-72V motor 14 can run for 0.5min at 1800r/min in the embodiment, and the transmission ratio of the gear one 1301 to the gear one 1201 is 1:30, so that the speed of the gear one 1201 is 60r/min. In the process of rotating the first gear ring 1201, the sleeve 22 and the rotating shaft 15 mounted at the bottom of the first gear ring 1201 synchronously rotate along with the first gear ring 1201, and the rotating shaft 15 also rotates due to the cooperation of the second gear 1302 and the second gear ring 1202, and the rotating speed of the rotating shaft 15 is 3600r/min because the transmission ratio of the second gear 1302 and the second gear ring 1202 is 1:60.

When the rotating shaft 15 rotates, the cross sections of the movable rod 19 and the movable groove 17 are non-revolution bodies, so that the movable rod 19 synchronously rotates along with the rotating shaft 15, and the centrifugal ball 21 on the rotating shaft 15 synchronously rotates along with the movable rod 19. Centrifugal force is generated when the centrifugal ball 21 rotates, the centrifugal ball 21 moves in a direction away from the movable rod 19, so that the centrifugal ball 21 cooperates with the conical movable space 18 to drive the centrifugal rod 20 to move in a direction approaching to the horizontal direction, meanwhile, the centrifugal rod 20 drives the movable rod 19 to overcome the spring I and move in a direction away from the gear ring I1201, the cutter 16 at one end of the movable rod 19 moves synchronously with the movable rod 19, and when the centrifugal ball 21 moves to a limiting position, the cutter 16 is 2cm away from the bottom wall of the rotary strand 3 at the moment. The cutter 16 rotates along with the rotation shaft 15 and rotates around the center of the first gear ring 1201, so that the crystallized material in the rotating strand 3 can be crushed uniformly into particles with a diameter of 1mm-3 mm. When the cutter 16 pulverizes the crystallized material, the first 2601 and the second 2602 are flattened to maintain a relative height as much as possible by stirring the crystallized material with uneven heights.

After 0.5min, the 180WD-M16030-72V motor 14 is automatically decelerated to 900r/min and operated at that speed for 10s. At this time, the rotation speed of the rotating shaft 15 is 1800r/min, and the centrifugal force generated by the centrifugal ball 21 at this rotation speed is smaller than the deformation tension of the first spring, so that the first spring pulls the movable rod 19 to move toward the direction close to the first gear ring 1201, and when the centrifugal force plus the gravity of the part is balanced with the tension of the first spring, the cutter 16 is completely located above the crystallization material. At this time, the knife 16 does not agitate the crystallized material, and thus does not interfere with the flattening of the crushed crystallized material by the first 2601 and second 2602 pusher plates. After 10s, the 180WD-M16030-72V motor 14 is automatically turned off, and in the time period again, the first gear ring 1201 rotates for 5 circles, and in the process, the first push plate 2601 and the second push plate 2602 push the crushed crystalline materials with higher accumulation to the position with less accumulation to form complementation, so that the first push plate 2601 and the second push plate 2602 can uniformly flatten the crushed crystalline materials in the rotating strand 3.

After the 180WD-M16030-72V motor 14 is closed, a centrifugal force can start a power unit of the PGZ-1250 centrifugal machine, the rotating strand 3 rotates in an accelerating way, and finally rotates at a constant speed of 1000r/min, at the moment, the crystallization material can be uniformly attached to the inner side wall of the rotating strand 3 under the action of centrifugal force, and primary mother liquor can pass through the rotating strand 3 and filter cloth to be discharged from the drain hole. In the process of accelerating the rotating strand 3, when the rotating speed reaches 300r/min, the centrifugal force borne by the fan-shaped baffle 28 is greater than the attractive force between the magnet I2901 and the magnet II 2902, so that the magnet I2901 is not attached to the magnet II in the prior art, the fan-shaped baffle 28 starts to extrude the spring II to move towards the direction close to the fixed block 30, the discharging hole 4 starts to open, and the inclined surface at the edge of the open slot 27 can scrape off the crystal material attached to the top wall of the fan-shaped baffle 28 in the process, so that the crystal material is prevented from affecting the movement of the fan-shaped baffle 28. As the speed of the rotating strand 3 increases, the sector plate 28 gradually moves in a direction approaching the fixed block 30. When the rotating speed of the rotating strand 3 is 450r/min, the fan-shaped baffle 28 is in contact with the fixed block 30, and the first magnet 2901 on the fan-shaped baffle 28 just enters the open groove 27 for 2mm.

When any impurity peak is detected to be less than 0.2% during centrifuging 2-nitro-5 fluorine, a centrifugal worker starts the scraper unit 8, at the moment, the rotary strand 3 rotates at a speed of 500r/min, the discharging hole 4 is still in an open state, the scraper unit 8 drives the scraper blade to be attached to the inner side wall of the rotary strand 3 and drives the scraper to move from top to bottom, and through the cooperation of the scraper and the rotary strand 3, crystalline materials on the inner side wall of the rotary strand 3 are separated or fall off and are discharged from the discharging hole 4.

Through experiments for 2 months, the invention can improve the production efficiency of the 3-trifluoromethyl-4-nitrophenol recrystallization and centrifugation process by 10-17%.

In the second embodiment, when the cutter 16 is driven by the motor 14.

The second gear 1302, the second gear ring 1202 and the rotating shaft 15 are replaced by a motor 14, and the cutter 16 is directly driven to rotate through the output end of the motor 14. Compared with the first embodiment, the second embodiment has simpler structure and more convenient installation, and the cutter 16 can obtain a higher rotating speed, so that the crushing effect on the crystalline material is better, and the crystalline material cannot be easily disturbed when the crystalline material is matched with a gear to operate. However, the cost of the motor 14 is higher than that of the first embodiment, and the arrangement of the electric wires of the motor 14 is troublesome because the cutter 16 needs to rotate along with the ring gear 1201, which is optional for the user.

Although a number of embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made in the state and details of these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims

1. A 3-trifluoromethyl-4-nitrophenol recrystallization centrifuge apparatus, comprising: the novel automatic scraping device comprises a base (1), wherein a shell (2) is fixedly installed on the base (1), a rotary strand (3) is rotationally installed on the shell (2), a plurality of fan-shaped discharging holes (4) are uniformly formed in the bottom wall of the rotary strand (3) in a rotating mode, a discharging opening (5) communicated with the discharging holes (4) is formed in the bottom wall of the base (1), an upper cover (6) is rotationally installed on the side wall of the shell (2), a leaching spray pipe (7) is installed at the center of the upper cover (6) in a penetrating mode, a power unit for driving the rotary strand (3) to rotate is installed on the base (1), and a scraping plate unit (8) for scraping materials on the rotary strand (3) during discharging is installed on the top wall of the upper cover (6). The method is characterized in that: annular through-hole (601) has been seted up on upper cover (6), and annular through-hole (601) divide into interior circle and excircle two parts with upper cover (6), install annular protective housing (9) that the cross section is the U type between interior circle and the excircle, annular protective housing (9) are located directly over annular through-hole (601), spout (10) have all been seted up on the lateral wall of annular through-hole (601), annular through-hole (601) internally mounted have ring gear one (1201), the ring gear both sides are equipped with slide rail (11) with spout (10) complex, install motor (14) on upper cover (6) roof, motor (14) output fixed have with ring gear one (1301) complex, install on the diapire of ring gear one (1201) be used for evenly smashing the crystalline material and put even stand unit, install in rotatory strand (3) diapire and be used for preventing that the crystalline material from being smashed from dropping from the rotatory unit (3) outside of the hole when smashing.

2. The 3-trifluoromethyl-4-nitrophenol recrystallization centrifugal device according to claim 1, wherein: the crushing unit comprises a rotating shaft (15) which is rotatably arranged on the bottom wall of a first gear ring (1201), a cutter (16) is fixedly arranged at one end, far away from the first gear ring (1201), of the rotating shaft (15), a second gear (1302) is fixedly arranged at one end, close to the first gear ring (1201), of the rotating shaft (15), a second gear ring (1202) matched with the second gear (1302) is fixedly arranged on the bottom wall of the upper cover (6), and a lifting unit is arranged in the rotating shaft (15).

3. A 3-trifluoromethyl-4-nitrophenol recrystallization centrifuge apparatus according to claim 2, wherein: the lifting unit comprises a movable groove (17) formed in the bottom wall of the rotating shaft (15), the section of the movable groove (17) is a non-revolving body, a conical movable space (18) is formed in one end, close to the bottom wall of the rotating shaft (15), of the movable groove (17), a movable rod (19) is elastically mounted in the movable groove (17) through an elastic piece (2401), a cutter (16) is fixedly mounted at one end, far away from the elastic piece (2401), of the movable rod (19), a centrifugal rod (20) is symmetrically mounted at one end, close to the elastic piece (2401), of the movable rod (19), and a centrifugal ball (21) is fixedly mounted at one end, far away from the movable rod (19), of each centrifugal rod (20).

4. The 3-trifluoromethyl-4-nitrophenol recrystallization centrifugal device according to claim 1, wherein: the spreading unit comprises a sleeve (22) which is vertically and fixedly arranged on the bottom wall of a first gear ring (1201), a plurality of first positioning holes (2301) are uniformly formed in the sleeve (22), a fixing rod (25) is slidably arranged in the sleeve (22), a second positioning hole (2302) which is matched with the first positioning holes (2301) is uniformly formed in the fixing rod (25), a first push plate (2601) is fixedly arranged at one end, far away from the first gear ring (1201), of the fixing rod (25), an extension line of the first push plate (2601) penetrates through the center of a circle of a rotating strand (3), and a second push plate (2602) is rotatably arranged at one end, far away from the center of the circle of the rotating strand (3), of the push plate (2601) through a torsion spring.

5. The 3-trifluoromethyl-4-nitrophenol recrystallization centrifugal device according to claim 4, wherein: the sleeve (22) and the rotating shaft (15) are symmetrically arranged around the center of the first gear ring (1201).

6. The 3-trifluoromethyl-4-nitrophenol recrystallization centrifugal device according to claim 1, wherein: the closed unit comprises an open slot (27) formed in the side wall of the center of the circle of the fan-shaped discharging hole (4) far away from the rotary strand (3), a fan-shaped baffle (28) matched with the fan-shaped discharging hole (4) is elastically installed in the open slot (27) through a second elastic piece (2402), a first magnet (2901) is embedded in one end of the fan-shaped baffle (28) far away from the second elastic piece (2402), and a second magnet (2902) which is mutually attracted with the first magnet (2901) is embedded in the side wall of the fan-shaped discharging hole (4) near the center of the rotary strand (3).

7. The 3-trifluoromethyl-4-nitrophenol recrystallization centrifugal device according to claim 6, wherein: an inclined surface is formed at the edge of the opening groove (27) close to the bottom wall of the inner side of the rotary strand (3).

8. The 3-trifluoromethyl-4-nitrophenol recrystallization centrifugal device according to claim 6, wherein: a fixed block (30) for preventing the elastic piece II (2402) from being excessively compressed is arranged on the bottom wall of the inner side of the opening groove (27).

9. A recrystallization centrifugation process of a 3-trifluoromethyl-4-nitrophenol recrystallization centrifugation apparatus according to any one of claims 1 to 8, wherein:

S2: the centrifugal staff opens the upper cover (6) of the centrifugal machine, puts the filter cloth on the centrifugal machine and rotates slowly to enable the filter cloth to be closely attached to the rotary strand (3), then the quantitative crystalline material is poured into the rotary strand (3) of the centrifugal machine, the fan-shaped discharging hole (4) is sealed by the sealing unit, primary mother liquor can be discharged from the drain pipe of the base (1) through the filter cloth and the rotary strand (3), the centrifugal staff closes the upper cover (6), then the motor (14) is started, the motor (14) drives the gear ring I (1201) to rotate for a set time rapidly through the gear I (1301), the crushing unit can crush the crystalline material uniformly in the process, the motor (14) drives the gear ring I (1201) to rotate for a set time slowly through the gear I (1301), and the spreading unit spreads the crushed crystalline material uniformly in the rotary strand (3) in the process;

s3: after the motor (14) runs for a set time, the motor is automatically closed, a centrifugal person starts a power unit, the power unit drives the rotary strand (3) to rotate, materials in the rotary strand (3) are piled and attached on the side wall of the rotary strand (3) under the action of centrifugal force, primary mother liquor and crystallized materials are separated under the action of the centrifugal force, and the closed unit opens the fan-shaped discharging hole (4) under the action of the centrifugal force;

S4: any impurity peak when centrifuging 3-trifluoromethyl-4-nitrophenol is less than 0.2%, a small amount of methanol is used for eluting until the standard is not met through inspection, mother liquor separated during eluting is eluting mother liquor, after any impurity peak when centrifuging 3-trifluoromethyl-4-nitrophenol, a scraper unit (8) is started by a centrifuge, a scraper scrapes off centrifugal materials from the side wall of a rotating strand (3), and the centrifugal materials enter a discharge opening (5) of a base (1) from a sector discharge hole (4);