CN111560036B

CN111560036B - NBPT production facility

Info

Publication number: CN111560036B
Application number: CN202010405257.0A
Authority: CN
Inventors: 黄生建; 陈炯明; 李文; 梁旭华; 胡金铬; 潘海龙; 李东平
Original assignee: Zhejiang Sunfit Advanced Materials Co ltd
Current assignee: Zhejiang Sunfit Advanced Materials Co ltd
Priority date: 2020-05-14
Filing date: 2020-05-14
Publication date: 2022-11-01
Anticipated expiration: 2040-05-14
Also published as: CN111560036A

Abstract

The invention discloses NBPT production equipment, which comprises a micro heat exchanger, a micro mixer, a micro pipeline reactor, an ammoniation reactor, a water washing device, a distillation device, a crystallizing tank and a target dryer which are sequentially communicated, wherein the water washing device comprises a main washing barrel, a telescopic stirring paddle, a water washing motor, a secondary push plate and a main push plate, the secondary push plate and the main push plate can be embedded in an up-and-down sealing mode, a delayer and a water phase collector are connected onto a lower barrel, the lower end of the delayer is communicated with an organic phase outlet of the lower barrel, a connecting pipe is communicated with the water phase collector, a distillation main body of the distillation device comprises an upper cavity, an inner barrel, an outer barrel and a condenser, a stirring mechanism of the distillation device comprises a push rod, a distillation motor, a gear, a stirring rod and fan blades, and the fan blades move up and down along with the forward and backward rotation of the stirring rod in a crossed mode. The invention avoids vortex influence caused by discharging below, improves the material liquid layering effect, realizes full stirring of the material liquid to be distilled at different heights in the inner cylinder body, and enables the material liquid to be distilled to be heated uniformly.

Description

NBPT production facility

Technical Field

The invention relates to the technical field of chemical production equipment, in particular to NBPT production equipment.

Background

N-N-butyl thiophosphoric triamide (NBPT) is a high-efficiency soil urease inhibitor, has an excellent urease inhibiting effect, can obviously reduce the decomposition of urea in soil and increase the utilization rate of nitrogen by crops. The inhibition mechanism is to compete for ligand and reduce the activity of urease, nitrogen atoms in NBPT molecules and nickel atoms in urease form (N-Ni) ligand, amino compounds in the NBPT molecules and oxygen atoms in a carbamic acid bridge can also form tridentate ligand, and the tridentate ligand is firmer than monodentate ligand formed by urea and the urease, so that the contact between the urea and the urease is reduced, the hydrolysis speed of the urea is slowed down, and the utilization rate of the urea is improved. The currently adopted method for synthesizing N-N-butyl thiophosphoric triamide by continuous reaction comprises the following steps: (1) Mixing thiophosphoryl chloride and an organic solvent, precooling the mixture to a temperature of between-5 and 0 ℃ in a micro heat exchanger, then mixing the mixture with N-butylamine and an inorganic alkaline aqueous solution which are precooled to a temperature of between-5 and 0 ℃ in a micro mixer, and reacting the obtained mixture in a multi-section micro-pipeline reactor which is connected in series to obtain N-N-butyl thiophosphoryl dichloride; (2) Directly feeding N-N-butyl thiophosphoryl dichloride into an ammoniation reactor to carry out ammoniation reaction with ammonia gas, washing, layering and filtering after the ammoniation reaction is completed, decompressing and distilling filtrate to recover solvent, crystallizing and drying to obtain the N-N-butyl thiophosphoryl triamide. Because the existing equipment for producing the N-N-butyl thiophosphoric triamide still has the defects of low separation precision, unsatisfactory purity of final products, large consumption of raw materials and the like, when a traditional washing device is adopted to separate reaction by-product ammonium chloride, layered feed liquid is discharged and collected from the lower part, vortexes can appear near a liquid discharge port in the discharging process, in addition, when an organic phase is separated, a water phase layer and an organic phase layer of the feed liquid are difficult to accurately control and separate, a small part of the water phase layer can be separated out always, the separation effect of the feed liquid is influenced, and if a traditional reduced pressure distillation device is adopted to separate an organic solvent, because a stirring mechanism of the equipment rotates from one direction, stirring is not uniform enough, the organic solvent is easily heated unevenly, the reduced pressure distillation extraction rate is low, and the development and design of the equipment for producing the N-N-butyl thiophosphoric triamide with good separation effect and high reduced pressure distillation extraction rate has important industrial value.

Disclosure of Invention

The invention aims to overcome the defects of the prior art, and provides NBPT production equipment, which avoids vortex influence caused by discharging below, improves the material liquid layering effect, realizes high-purity accurate separation of ammonium chloride, realizes full stirring of material liquids to be distilled at different heights in an inner cylinder body, uniformly heats the material liquids to be distilled, and improves the final NBPT purity.

In order to achieve the purpose, the invention adopts the following technical scheme:

the NBPT production equipment comprises a micro heat exchanger, a micro mixer, a micro pipeline reactor, an ammonification reactor, a washing device, a distilling device, a crystallizing tank and a target dryer which are sequentially communicated, wherein the washing device comprises a main washing barrel, a telescopic stirring paddle arranged in the main washing barrel, a washing motor used for driving the telescopic stirring paddle to rotate, a secondary push plate and a main push plate which are arranged from top to bottom, the main washing barrel comprises a lower barrel body, the secondary push plate and the main push plate are respectively arranged in the lower barrel body in a sliding manner, a liquid inlet communicated with the ammonification reactor is arranged on the lower barrel body and positioned above the secondary push plate, air cylinders used for driving the main push plate to move are respectively arranged on two sides of the main washing barrel, the secondary push plate and the main push plate are embedded in a sealing manner from top to bottom between the secondary push plate and the main push plate under the action of the pulling force of the air cylinders and the weight of liquid injected into the space above the secondary push plate, barrel upper end one side is connected with layering ware and the aqueous phase collector all with barrel intercommunication down respectively, barrel bottom is equipped with the organic phase export down, the layering ware lower extreme passes through connecting pipe and organic phase export intercommunication, the connecting pipe passes through branch pipe and aqueous phase collector intercommunication, distillation plant includes distillation main part and rabbling mechanism, the distillation main part includes the cavity, is located cavity below and inside and outside the interior barrel and outer barrel that set up, with the condenser of interior barrel upper portion intercommunication, rabbling mechanism includes push rod, drive push rod transverse reciprocating motion's distillation motor, drives positive and negative rotation cross moving gear through the push rod, fixes terminal surface under the gear and stretches into the puddler of interior barrel and with the flabellum of puddler lower part spiro union, the flabellum is along with the positive and negative rotation cross moving and up-and-down motion of puddler.

The main section of thick bamboo of washing still includes the baffle that can dismantle the connection, the main section of thick bamboo of washing is separated into the last barrel and the lower barrel that sets up from top to bottom by the baffle, flexible stirring rake includes with the first bull stick of the pivot rigid coupling of washing motor, slide and inlay and establish in first bull stick and can follow first bull stick pivoted second bull stick, slide and inlay and establish in the second bull stick and can follow second bull stick pivoted third bull stick and the stirring leaf of rigid coupling in the third bull stick bottom, first bull stick lower extreme passes the baffle and is connected with the baffle rotation through A bearing, pass through spring coupling between the pivot of washing motor and the interior terminal surface of third bull stick lower part.

The outside level in second bull stick upper end extends and forms a pair of fixture block that the symmetry set up, the sunken a pair of draw-in groove that forms of first bull stick up end, the fixture block card is gone into in the draw-in groove and can slide from top to bottom along the draw-in groove, the outside level in third bull stick upper end extends and forms a pair of protruding blocks that the symmetry set up, the sunken a pair of recess that forms of second bull stick up end, the protruding block card is gone into in the recess and can slide from top to bottom along the recess.

The lower barrel is provided with a limiting block with uniform circumference on the inner wall of the lower portion, the secondary push plate is arranged in the lower barrel and located above the limiting block, and the main push plate is provided with a notch through which the limiting block can pass.

Inferior push pedal by interior and be equipped with a plurality of through-holes that circle outward, main push pedal includes through-hole and a plurality of circle down and be used for the shutoff to go up the boss of through-hole, every circle through-hole sets up between adjacent two circles boss down, is located through-hole lower extreme face outlying inlay in inferior push pedal and be equipped with the A sealing washer, it is sealed through the A sealing washer when through-hole in the boss embedding shutoff.

A rotating rod is connected to a rotating shaft of the distillation motor, and the outer end of the rotating rod drives a push rod to reciprocate through a fastener.

The push rod comprises a toothed rod part engaged with the gear and a slide rod part vertically connected with the toothed rod part, the toothed rod part and the slide rod part form a T-shaped structure, a pair of fixing parts for the toothed rod part to slide through are fixedly arranged on the upper portion of the upper chamber, a waist hole is formed in the slide rod part along the length direction of the slide rod part, and the fastening parts penetrate through the waist hole and are in sliding connection with the waist hole.

The heating wire is fixedly arranged on the annular outer wall of the inner cylinder body, and a wire mesh demister is arranged in the upper space of the inner cylinder body.

One side of the bottom of the inner cylinder body is provided with a feed inlet communicated with the organic phase outlet, and the other side of the bottom of the inner cylinder body is provided with a discharge outlet communicated with the crystallizing tank.

The invention has the beneficial effects that: stirring the reaction solution by a telescopic stirring paddle to accelerate the dissolution of ammonium chloride; the secondary push plate and the main push plate are pulled by the air cylinder to move upwards, and the water phase layer and the interface layer of the standing and layered material liquid overflow upwards respectively and are discharged to the water phase collector and the delayer, so that the vortex influence caused by discharging below is avoided, the material liquid layering effect is improved, and the high-purity accurate separation of ammonium chloride is realized; the interface layer is rested and layered into a water phase layer and an organic phase layer through the delayer, so that the separation precision of ammonium chloride is further improved, and the improvement of the final purity of NBPT is facilitated; make the puddler can just reverse cross operation through the mating reaction of distillation motor, push rod, gear for the flabellum up-and-down motion and then realize treating the intensive mixing of distillation feed liquid to the internal co-altitude of inner tube, make and treat that the distillation feed liquid is heated evenly, improve the distillation pull-out rate, further promote final NBPT's purity.

Drawings

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

FIG. 2 is a schematic front view of the washing apparatus of the present invention;

FIG. 3 is an enlarged view taken at A in FIG. 2;

FIG. 4 is an enlarged view at B in FIG. 2;

FIG. 5 is an enlarged view at C of FIG. 2;

FIG. 6 is an enlarged view taken at D in FIG. 2;

FIG. 7 is a schematic side view of the washing apparatus of the present invention;

FIG. 8 is a schematic top view of a secondary push plate of the present invention;

FIG. 9 is a schematic top view of the main push plate of the present invention;

FIG. 10 is a schematic view of the structure of a distillation apparatus according to the present invention;

FIG. 11 is an enlarged view at E in FIG. 10;

FIG. 12 is an enlarged view at F of FIG. 10;

FIG. 13 is an enlarged view at G of FIG. 10;

FIG. 14 is a top schematic view of a push rod mounting arrangement embodying the principles of the present invention;

FIG. 15 is an enlarged view at H in FIG. 14;

fig. 16 is an enlarged view at I in fig. 14.

In the figure: the micro heat exchanger 1, the micro mixer 2, the micro pipeline reactor 3, the ammoniation reactor 4, the water washing device 5, the main washing cylinder 51, the upper cylinder 511, the lower cylinder 512, the liquid inlet 513, the organic phase outlet 514, the partition 515, the a bearing 516, the B bearing 517, the limit block 518, the notch 519, the telescopic stirring paddle 52, the first rotating rod 521, the second rotating rod 522, the third rotating rod 523, the stirring blade 524, the clamping groove 525, the clamping block 526, the groove 527, the bump 528, the spring 529, the water washing motor 53, the secondary pushing plate 54, the upper through hole 541, the a sealing ring 542, the B sealing ring 543, the main pushing plate 55, the boss 551, the lower through hole 552, the delayer 56, the aqueous phase 57, the air cylinder 58, the connecting rod 581, the connecting pipe 59, the branch pipe 591, the distillation device 6, the distillation body 61, the upper chamber 611, the inner cylinder 612, the outer cylinder 613, the liquid inlet 614, the discharge port 615, the end cap 616, the push rod 62, the toothed rod 621, the sliding rod 622, the tooth rod 624, the fixing member 641, the fixing member 631, the waist rod 631, the fastening member 63, the fastening member 632, the gear wheel 632, the stirring rod 66, the drying rod 66, the wire mesh tank 69, the electric heating wire drying tank 8, the electric wire dryer, the electric heating wire 8 and the electric wire.

Detailed Description

The invention is further described with reference to the accompanying drawings and the detailed description below:

as shown in fig. 1 to 16, an NBPT production apparatus includes a micro heat exchanger 1, a micro mixer 2, a micro pipeline reactor 3, an ammoniation reactor 4, a water washing device 5, a distillation device 6, a crystallization tank 7 and a target dryer 8 which are sequentially communicated, wherein the micro heat exchanger 1 is used for precooling mixed thiophosphoryl chloride and organic solvent to-5 to 0 ℃, the micro mixer 2 is used for fully mixing the thiophosphoryl chloride and organic solvent precooled to-5 to 0 ℃ with N-butylamine and inorganic alkaline aqueous solution precooled to-5 to 0 ℃, the micro pipeline reactor 3 is used for reacting thiophosphoryl chloride and N-butylamine to generate N-butyl thiophosphoryl dichloride, the ammoniation reactor 4 is used for reacting N-butyl thiophosphoryl dichloride with ammonia gas to generate NBPT and byproduct ammonium chloride, the water washing device 5 is mainly used for washing, standing and layering the product generated by the reaction to separate out byproduct ammonium chloride, the distillation device 6 is used for removing the organic solvent remained in the product, the crystallization tank 7 is used for conducting reduced pressure distillation on the obtained NBPT, and the target dryer is used for drying the NBPT dried by the NBPT crystal.

The micro heat exchanger 1, the micro mixer 2, the micro pipeline reactor 3, the ammonification reactor 4, the crystallization tank 7 and the target dryer 8 are common devices in the field of chemical equipment, and are not described in detail herein.

The washing device 5 includes mainly wash a section of thick bamboo 51, locate the flexible stirring rake 52 in mainly washing a section of thick bamboo 51, be used for driving the rotatory washing motor 53 of flexible stirring rake 52, from top to bottom the inferior push pedal 54 and the main push pedal 55 that set up, mainly wash a section of thick bamboo 51 including lower barrel 512, inferior push pedal 54 and main push pedal 55 slide respectively and set up under in barrel 512, be located inferior push pedal 54 top be equipped with the inlet 513 with ammoniation reactor 4 intercommunication on the barrel 512 down, mainly wash a section of thick bamboo 51 both sides and respectively be equipped with the cylinder 58 that is used for driving main push pedal 55 to remove, inferior push pedal 54 and main push pedal 55 realize inferior push pedal 54 and main push pedal 55 between upper and lower sealed gomphosis through the effect of the pulling force of cylinder 58 and the liquid weight effect of pouring into inferior push pedal 54 top space, barrel 512 upper end one side is connected with delayer 56 and the aqueous phase collector 57 that all communicates with lower barrel 512 down respectively down, barrel 512 bottom is equipped with organic phase export 514 down, the lower extreme of delayer 56 passes through connecting pipe 59 and organic phase export intercommunication, the aqueous phase connecting pipe 591 is connected with collector 57. The liquid inlet 513 is located above the initial position of the secondary push plate 54, so that the liquid enters the sealed space after the space above the secondary push plate 54 forms the sealed space. The delayer 56 is a longitudinally arranged structure with a smaller inner diameter and is used for delaminating the interface phase layer (the interface phase layer is the interface phase layer at the junction of the aqueous phase layer and the organic phase layer), the aqueous phase collector 57 is connected to the upper part of the lower cylinder 512, the delayer 56 is connected to the upper part of the lower cylinder 512, the lower end of the delayer 56 is connected to the connecting pipe 59, the connecting pipe 59 is connected to the organic phase outlet 514, and the branch pipe 591 is connected to the connecting pipe 59 and is provided with valves for controlling liquid outflow.

The main washing cylinder 51 further comprises a partition plate 515 which is detachably connected, the upper end cover part of the main washing cylinder 51 is also detachably arranged, so that the telescopic stirring paddle 52, the connecting rod 581, the secondary push plate 54 and the main push plate 55 can be conveniently installed, the main washing cylinder 51 is divided into an upper cylinder 511 and a lower cylinder 512 which are vertically arranged by the partition plate 515, and the upper end surface of the lower cylinder 512 is further provided with an organic solvent inlet and a distilled water inlet.

The rotating shaft of the water washing motor 53 penetrates through the upper end part of the upper cylinder 511 and is rotationally connected with the upper end part of the upper cylinder 511 through a B bearing 517, the telescopic stirring paddle 52 comprises a first rotating rod 521 fixedly connected with the rotating shaft of the water washing motor 53, a second rotating rod 522 slidably embedded in the first rotating rod 521 and capable of rotating with the first rotating rod 521, a third rotating rod 523 slidably embedded in the second rotating rod 522 and capable of rotating with the second rotating rod 522, and a stirring blade 524 fixedly connected to the bottom end of the third rotating rod 523, the lower end of the first rotating rod 521 penetrates through the partition plate 515 and is rotationally connected with the partition plate 515 through an A bearing 516, the rotating shaft of the water washing motor 53 is connected with the inner end surface of the lower part of the third rotating rod 523 through a spring 529, and the spring 529 plays a role in further stably connecting the first rotating rod 521, the second rotating rod 522 and the third rotating rod 523, and enables the telescopic stirring paddle 52 to automatically recover to an extended state after being compressed.

The specific connection structure among the first rotating rod 521, the second rotating rod 522 and the third rotating rod 523 is as follows: the upper end of the second rotating rod 522 extends outwards horizontally to form a pair of symmetrically-arranged clamping blocks 526, the upper end surface of the first rotating rod 521 is recessed to form a pair of clamping grooves 525, the clamping grooves 525 do not penetrate through the first rotating rod 521, the clamping blocks 526 are clamped in the clamping grooves 525 and can slide up and down along the clamping grooves 525, the upper end of the third rotating rod 523 extends outwards horizontally to form a pair of symmetrically-arranged lugs 528, the upper end surface of the second rotating rod 522 is recessed to form a pair of grooves 527, the grooves 527 do not penetrate through the second rotating rod 522, and the lugs 528 are clamped in the grooves 527 and can slide up and down along the grooves 527; the lower opening of the first rotating rod 521 is sealed with the annular outer wall of the second rotating rod 522 through a sealing ring embedded in the annular inner wall of the lower opening of the first rotating rod 521, the lower opening of the second rotating rod 522 is sealed with the annular outer wall of the third rotating rod 523 through a sealing ring embedded in the annular inner wall of the lower opening of the second rotating rod 522, the influence of feed liquid entering the telescopic stirring paddle 52 on the stirring and dissolving of ammonium chloride is avoided, and the loss of products is reduced.

The air cylinder 58 is fixedly connected with the main push plate 55 through a right-angle connecting rod 581, the connecting rod 581 penetrates through the partition plate 515 and the secondary push plate 54, the connecting rod 581 and the partition plate 515 are sealed through a sealing ring embedded on the partition plate 515, the connecting rod 581, the partition plate 515 and the secondary push plate 54 are sealed through a sealing ring embedded in the secondary push plate 54, and therefore a closed space can be formed between the partition plate 515 and the secondary push plate 54.

The inner wall of the lower part of the lower cylinder 512 is provided with limit blocks 518 which are uniformly distributed on the circumference, the secondary push plate 54 is arranged in the lower cylinder 512 and is positioned above the limit blocks 518, the main push plate 55 is provided with a notch 519 which can enable the limit blocks 518 to pass through, the initial position of the secondary push plate 54 is limited by the arrangement of the limit blocks 518, the downward movement of the secondary push plate 54 is prevented, and the main push plate 55 can be separated from the secondary push plate 54 so that the organic phase can flow downwards to the organic phase outlet 514 and be discharged.

The secondary push plate 54 is provided with a plurality of upper through holes 541 from inside to outside, the main push plate 55 comprises a plurality of circles of lower through holes 552 and a plurality of circles of bosses 551 for plugging the upper through holes 541, each circle of the lower through holes 552 is arranged between two adjacent circles of the bosses 551, the secondary push plate 54 positioned on the periphery of the lower end surface of the upper through holes 541 is embedded with an A sealing ring 542, and the bosses 551 are sealed by the A sealing rings 542 when being embedded into the upper through holes 541 for plugging. The upper through hole 541 is a tapered hole with a small upper part and a large lower part, the boss 551 is a tapered circular truncated cone structure with a small upper part and a large lower part, and the space between the annular outer wall of the secondary push plate 54 and the annular inner wall of the lower barrel 512 is sealed by a B sealing ring 543 embedded on the secondary push plate 54. Through the structural design, a closed space can be formed between the partition plate 515 and the secondary push plate 54, and the purpose of upwards extruding and discharging the liquid of the aqueous phase layer and the interface layer is further realized.

The water washing device 5 is mainly used for washing and standing the product after the reaction is finished to separate the ammonium chloride by-product. The working principle of the water washing device 5 is as follows: in an initial state, the secondary push plate 54 and the main push plate 55 are in a separated state, the starting air cylinder 58 drives the main push plate 55 to move upwards to enable the boss 551 to be embedded into the upper through hole 541, the operation of the air cylinder 58 is stopped, a small part of organic solvent is injected into the lower barrel 512, at the moment, under the combined action of the gravity of the organic solvent and the pulling force of the air cylinder 58, the main push plate 55 and the secondary push plate 54 are completely embedded in a sealing manner, the injection of the organic solvent is stopped, a product obtained after the reaction of the ammoniation reactor 4 is injected, distilled water is simultaneously injected, the washing motor 53 is started to stir, so that ammonium chloride is fully dissolved in the distilled water, the stirring is stopped, standing and layering are carried out, an aqueous phase layer (ammonium chloride aqueous solution), an interface layer and an organic phase layer (NBPT and organic solvent) distributed from top to bottom are obtained, the air cylinder 58 is started, a valve at the joint of the aqueous phase collector 57 and the lower barrel 512 is opened, the main push plate 55 and the secondary push plate 54 and the aqueous phase layer is extruded and discharged to the aqueous phase collector 57, closing a valve at the joint of the water phase collector 57 and the lower cylinder 512, opening a valve at the joint of the delayer 56 and the lower cylinder 512, discharging the interface layer to the delayer 56, wherein the telescopic stirring paddle 52 is compressed under the thrust of the secondary push plate 54 in the process, the spring 529 is also gradually compressed, the interface layer is layered into a water phase layer and an organic phase layer again after the interface layer is layered by standing of the delayer 56, the obtained organic phase layer is discharged to the organic phase outlet 514, the water phase layer is discharged to the water phase collector 57, the cylinder 58 is started again to enable the main push plate 55 to move downwards, the residual organic phase layer in the lower cylinder 512 gradually falls under the self gravity, and the secondary push plate 54 also gradually falls, in the process, the secondary push plate 54 and the main push plate 55 are still in a sealed embedding state, and the secondary push plate 54 does not move downwards when the secondary push plate 54 moves downwards and abuts against the limiting block 518, the main push plate 55 moves downwards continuously to separate from the secondary push plate 54, the organic phase layer in the lower cylinder 512 flows to the organic phase outlet 514 through the upper through hole 541 and the lower through hole 552, the precise separation of the material liquid is completed, and the telescopic stirring paddle 52 is restored to the initial extension state under the action of gravity and the elastic force of the spring 529.

The distillation device 6 comprises a distillation main body 61 and a stirring mechanism, wherein the distillation main body 61 comprises an upper cavity 611, an inner cylinder 612 and an outer cylinder 613 which are arranged below and inside and outside the upper cavity 611, and a condenser 67 communicated with the upper part of the inner cylinder 612, a heating wire 68 is fixedly arranged on the annular outer wall of the inner cylinder 612 and used for heating liquid in the inner cylinder 612, and a wire mesh demister 69 is arranged in the upper space of the inner cylinder 612 and used for eliminating foam carried in evaporated gas, so that the problem that the foam enters the condenser 67 to be crystallized to cause the wall bonding of a heat exchange tube of the condenser 67 and influence the distillation effect is avoided.

The stirring mechanism comprises a push rod 62, a distillation motor 63 for driving the push rod 62 to transversely reciprocate, a gear 64 for driving the push rod 62 to rotate forward and backward in a crossed mode, a stirring rod 65 fixed on the lower end face of the gear 64 and extending into the inner cylinder 612, and fan blades 66 in threaded connection with the lower portion of the stirring rod 65, wherein the fan blades 66 move up and down along with the forward and backward rotation of the stirring rod 65 in a crossed mode. The upper chamber 611 comprises a detachably connected end cover 616, which facilitates the installation of the relevant components of the upper chamber 611, the gear 64 is fixed to the end cover 616 by a fixing rod 641, and the gear 64 and the fixing rod 641 are rotatably connected by a bearing; the stirring rod 65 is rotatably connected with the partition board which separates the upper chamber 611 and the inner cylinder 612 and the bottom of the stirring rod 65 and the bottom of the inner cylinder 612 through bearings, so that smooth rotation of the stirring rod 65 is ensured.

A rotating rod 631 is connected to the rotating shaft of the distillation motor 63, and the outer end of the rotating rod 631 drives the push rod 62 to reciprocate through a fastener 632.

The push rod 62 comprises a toothed rod portion 621 meshed with the gear 64 and a sliding rod portion 622 perpendicularly connected with the toothed rod portion 621, the toothed rod portion 621 and the sliding rod portion 622 form a T-shaped structure, a pair of fixing pieces 624 for the toothed rod portion 621 to slide through is fixedly arranged at the upper portion of the upper chamber 611, a waist hole 623 is arranged on the sliding rod portion 622 along the length direction of the sliding rod portion, and the fastening piece 632 penetrates through the waist hole 623 and is in sliding connection with the waist hole 623.

And a feed inlet 614 communicated with the organic phase outlet 514 is formed in one side of the bottom of the inner cylinder body 612, and a discharge outlet 615 communicated with the crystallizing tank 7 is formed in the other side of the bottom of the inner cylinder body 612.

The operating principle of the stirring mechanism is as follows: with reference to fig. 14 as a reference direction, the distillation motor 63 is started, the distillation motor 63 drives the rotary rod 631 to rotate circularly on a horizontal plane, the rotary rod 631 drives the fastener 632 to slide in the waist hole 623, when the fastener 632 slides clockwise by 180 degrees, the push rod 62 moves rightward to drive the gear 64 to rotate clockwise, the gear 64 drives the stirring rod 65 to rotate clockwise to further move the fan blade 66 upward, when the fastener 632 continues to slide clockwise by 180 degrees, the push rod 62 moves leftward to drive the gear 64 to rotate counterclockwise, and the gear 64 drives the stirring rod 65 to rotate counterclockwise to further move the fan blade 66 downward; the reciprocating motion realizes the up-and-down stirring of the liquid in the inner cylinder body 612, so that the stirring is more sufficient, the distilled liquid is uniformly heated, and the distillation extraction rate is improved.

The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.

Claims

1. The utility model provides a NBPT production facility, includes micro heat exchanger (1), micro mixer (2), micro pipeline reactor (3), ammoniation reactor (4), washing unit (5), distillation plant (6), crystallizer (7) and target dryer (8) that communicate in proper order, its characterized in that: the washing device (5) comprises a main washing cylinder (51), a telescopic stirring paddle (52) arranged in the main washing cylinder (51), a washing motor (53) used for driving the telescopic stirring paddle (52) to rotate, a secondary push plate (54) and a main push plate (55) which are arranged from top to bottom, wherein the main washing cylinder (51) comprises a lower cylinder body (512), the secondary push plate (54) and the main push plate (55) are respectively arranged in the lower cylinder body (512) in a sliding manner, a liquid inlet (513) communicated with the ammoniation reactor (4) is arranged on the lower cylinder body (512) above the secondary push plate (54), two sides of the main washing cylinder (51) are respectively provided with a cylinder (58) used for driving the main push plate (55) to move, the device is characterized in that the secondary push plate (54) and the main push plate (55) are in upper and lower sealing embedding between the secondary push plate (54) and the main push plate (55) under the action of the pulling force of the air cylinder (58) and the weight of liquid injected into a space above the secondary push plate (54), one side of the upper end of the lower cylinder (512) is respectively connected with a delayer (56) and a water phase collector (57) which are communicated with the lower cylinder (512), an organic phase outlet (514) is arranged at the bottom of the lower cylinder (512), the lower end of the delayer (56) is communicated with the organic phase outlet (514) through a connecting pipe (59), and the connecting pipe (59) is communicated with the water phase collector (57) through a branch pipe (591) Distillation plant (6) are including distillation main part (61) and rabbling mechanism, distillation main part (61) include cavity (611), be located cavity (611) below and inside and outside inner tube body (612) and outer barrel (613) that set up, condenser (67) with inner tube body (612) upper portion intercommunication, the rabbling mechanism includes push rod (62), drive push rod (62) horizontal reciprocating motion's distillation motor (63), drive gear (64) of positive and negative rotation cross operation through push rod (62), fix terminal surface under gear (64) and stretch into puddler (65) of inner tube body (612) and flabellum (66) with puddler (65) lower part spiro union, flabellum (66) are along with the positive and negative rotation cross operation and up-and-down motion of puddler (65).

2. The NBPT production apparatus of claim 1, wherein: the main barrel (51) of washing still includes baffle (515) of dismantling the connection, main barrel (51) are separated into upper barrel (511) and lower barrel (512) that set up from top to bottom by baffle (515), flexible stirring rake (52) include with the first bull stick (521) of the pivot rigid coupling of washing motor (53), slide and inlay and establish in first bull stick (521) and can follow first bull stick (521) pivoted second bull stick (522), slide and inlay and establish in second bull stick (522) and can follow second bull stick (522) pivoted third bull stick (523) and rigid coupling stirring leaf (524) in third bull stick (523) bottom, baffle (515) are passed through to first bull stick (521) lower extreme and are connected with baffle (515) rotation through A bearing (516), the pivot of washing motor (53) is connected through spring (529) between the interior terminal surface of third bull stick (523) lower part.

3. The NBPT production apparatus of claim 2, wherein: the outside horizontal extension in second bull stick (522) upper end forms fixture block (526) that a pair of symmetry set up, the terminal surface is sunken to form a pair of draw-in groove (525) on first bull stick (521), fixture block (526) are gone into in draw-in groove (525) and can slide from top to bottom along draw-in groove (525), the outside horizontal extension in third bull stick (523) upper end forms lug (528) that a pair of symmetry set up, the terminal surface is sunken to form a pair of recess (527) on second bull stick (522), lug (528) are gone into in recess (527) and can slide from top to bottom along recess (527).

4. The NBPT production apparatus of claim 2, wherein: the lower barrel (512) is provided with limiting blocks (518) which are uniformly distributed on the circumference on the inner wall of the lower portion of the lower barrel (512), the secondary push plate (54) is arranged in the lower barrel (512) and is positioned above the limiting blocks (518), and the main push plate (55) is provided with a notch (519) through which the limiting blocks (518) can pass.

5. The NBPT production apparatus of claim 1, wherein: the secondary push plate (54) is provided with a plurality of upper through holes (541) from inside to outside, the main push plate (55) comprises a plurality of lower through holes (552) and a plurality of bosses (551) for plugging the upper through holes (541), each lower through hole (552) is arranged between two adjacent bosses (551), an A sealing ring (542) is embedded on the secondary push plate (54) which is positioned at the periphery of the lower end face of the upper through hole (541), and the bosses (551) are sealed by the A sealing ring (542) when being embedded and plugged into the upper through holes (541).

6. The NBPT production apparatus of claim 1, wherein: a rotating rod (631) is connected to a rotating shaft of the distillation motor (63), and the outer end of the rotating rod (631) drives the push rod (62) to reciprocate through a fastener (632).

7. The NBPT production apparatus of claim 6, wherein: the push rod (62) comprises a toothed rod part (621) meshed with the gear (64) and a sliding rod part (622) vertically connected with the toothed rod part (621), the toothed rod part (621) and the sliding rod part (622) form a T-shaped structure, a pair of fixing parts (624) allowing the toothed rod part (621) to pass through in a sliding mode are fixedly arranged on the upper portion of the upper cavity (611), a waist hole (623) arranged along the length direction of the sliding rod part (622) is formed in the sliding rod part, and the fastener (632) penetrates through the waist hole (623) and is in sliding connection with the waist hole (623).

8. The NBPT production apparatus of claim 1, wherein: the heating wire (68) is fixedly arranged on the annular outer wall of the inner cylinder body (612), and a wire mesh demister (69) is arranged in the upper space of the inner cylinder body (612).

9. The NBPT production apparatus of claim 1, wherein: and a feeding hole (614) communicated with the organic phase outlet (514) is formed in one side of the bottom of the inner cylinder body (612), and a discharging hole (615) communicated with the crystallizing tank (7) is formed in the other side of the bottom of the inner cylinder body (612).