CN114345242A

CN114345242A - Process for preparing 2, 4-dinitro-6-chloroaniline by sulfuric acid method

Info

Publication number: CN114345242A
Application number: CN202111552298.3A
Authority: CN
Inventors: 谢文秀; 代龙龙; 王建国; 朱成林; 赵立红; 常鹏
Original assignee: Ningxia Zhongsheng New Technology Co ltd
Current assignee: Ningxia Zhongsheng New Technology Co ltd
Priority date: 2021-12-17
Filing date: 2021-12-17
Publication date: 2022-04-15

Abstract

The invention discloses a process for preparing 2, 4-dinitro-6-chloroaniline by a sulfuric acid method, which comprises the following steps: processing and reacting the reaction raw materials by using a stirring device, and discharging and filtering after the reaction is finished; the stirring step comprises: A. putting the reaction raw materials and sulfuric acid into a stirring barrel; B. starting a motor and driving a stirring rotating shaft to rotate, wherein the stirring rotating shaft drives a stirring plate to rotate so as to stir the raw materials; C. introducing chlorine into the raw materials in the stirring barrel through a ventilation structure before stirring the raw materials; D. the stirring rotating shaft drives the control structure to move, and then the control structure drives the stirring plate to change the angle through the stirring adjusting structure; E. the angle of the stirring plate is adjusted through a proper speed structure according to the rotating speed of the stirring rotating shaft; through having set up ventilation structure, assurance chlorine that can be better lets in the inside of solution to guarantee that solution can not take place the backward flow, better assurance the mixed degree of consistency of chlorine and solution.

Description

Process for preparing 2, 4-dinitro-6-chloroaniline by sulfuric acid method

Technical Field

The invention belongs to the technical field of chemical reaction preparation, and particularly relates to a process for preparing 2, 4-dinitro-6-chloroaniline by a sulfuric acid method.

Background

The existing 2, 4-dinitro-6-chloroaniline needs to be chloridized by introducing chlorine into a reactant during preparation, but chlorine cannot be introduced into a reaction solution, and only chlorine can be introduced outside the solution to chloridize the surface of the solution, so that the chlorination speed is low, the chlorination degree is uneven, the quality of a reaction product is finally influenced, and if chlorine is introduced into the reaction solution, the reflux of the solution is influenced by the influence of the stable control of the air pressure of the chlorine stopping.

Disclosure of Invention

The invention provides a process for preparing 2, 4-dinitro-6-chloroaniline by a sulfuric acid method, which aims to overcome the defects of the prior art and improve the chlorination efficiency and the product quality.

In order to achieve the purpose, the invention adopts the following technical scheme: a process for preparing 2, 4-dinitro-6-chloroaniline by a sulfuric acid method comprises the following steps: processing and reacting the reaction raw materials by using a stirring device, and discharging and filtering after the reaction is finished; the stirring device comprises a stirring barrel, a motor fixedly arranged on the stirring barrel, a first bracket fixedly arranged on the stirring barrel and used for supporting the motor, an electric plate arranged on the stirring barrel, a speed-adapting structure arranged below the motor, a control structure arranged below the speed-adapting structure, a stirring rotating shaft connected with the motor, a stirring plate fixedly connected with the motor, a ventilation structure arranged on the stirring plate and a stirring adjusting structure connected with the stirring plate; the stirring step comprises:

A. putting the reaction raw materials and sulfuric acid into a stirring barrel;

B. starting a motor and driving a stirring rotating shaft to rotate, wherein the stirring rotating shaft drives a stirring plate to rotate so as to stir the raw materials;

C. introducing chlorine into the raw materials in the stirring barrel through a ventilation structure before stirring the raw materials; the ventilation structure comprises an air pump fixedly arranged below the stirring barrel, a connecting pipe fixedly connected to the air pump, an air passage communicated with the connecting pipe, a force storage cavity communicated with the air passage, a buffer component arranged inside the force storage cavity, a through hole arranged on the stirring plate, an air pipe arranged on the through hole, a boss round seat arranged inside the air pipe in a sliding manner, a lifting pipe fixedly connected to the boss round seat, a blocking block arranged above the stirring plate in a sliding manner and used for blocking the air pipe, a first control component connected to the lifting pipe and used for opening the blocking block, and a clamping component connected to the first control component; the first control assembly comprises a avoiding cavity arranged on the inner surface of the blocking block, a triangular block arranged on the avoiding cavity in a sliding manner, a sliding hole arranged on the triangular block, a first guide rod arranged in the sliding hole in a sliding manner, a pressing plate fixedly connected to the first guide rod and positioned below the triangular block, a first avoiding groove arranged below the triangular block and matched with the pressing plate, a third spring arranged in the pressing plate and the first avoiding groove and used for resetting the pressing plate, a connecting plate fixedly arranged on the first guide rod, a clamping groove arranged on the connecting plate, a telescopic baffle fixedly arranged above the triangular block and used for sealing the avoiding cavity, and a fourth spring arranged between the triangular block and the top surface of the avoiding cavity; the clamping assembly comprises a second avoiding groove arranged on the inner wall of the avoiding cavity, a third avoiding groove arranged on the top surface, a clamping block arranged in the second avoiding groove in a sliding manner, a first telescopic rod fixedly arranged between the clamping block and the second avoiding groove, a fifth spring arranged on the clamping block and used for resetting the clamping block, a first rope connected with the fifth spring and the boss round seat, a control plate arranged in the third avoiding groove in a sliding manner, a sixth spring fixedly arranged above the control plate and used for resetting the control plate, and a second rope fixedly connected with the control plate and the clamping block; the method comprises the following steps: the air pump leads chlorine gas into the stirring rotating shaft, then the stirring rotating shaft is hollow, the chlorine gas can reach the air passage through the connecting pipe and the stirring rotating shaft and is blown into the pressure storage cavity, then the chlorine gas is buffered through the buffer component to store pressure in the pressure storage cavity, then the buffer component can move after the pressure in the pressure storage cavity is sufficiently large, then the buffer component is firstly blocked in front of the through hole, namely the chlorine gas can not pass through the through hole, then the buffer component moves and can move to the rear of the through hole, therefore, the chlorine gas can enter the through hole, namely the chlorine gas reaches the vent pipe, the buffer component can drive the lifting pipe to move upwards when moving, then the boss round seat slides in the vent pipe, the lifting pipe can firstly impact the pressing plate when moving upwards, then the pressing plate drives the first guide rod to slide upwards in the sliding hole, and then the connecting plate is driven to move, the connecting plate can move upwards and approach the inner wall of the avoiding cavity, then after the pressing plate moves into the first avoiding groove, the pressing plate can not move continuously, at the moment, the lifting pipe is in contact with the triangular block, so that the triangular block can be driven to move, the elastic force of the second spring is larger than that of the fourth spring, so that the first time movement of the triangular block is upward movement until the triangular block moves to the uppermost blocked position, and then the elastic force of the sixth spring is larger than that of the fifth spring, so that the control plate is at the lowest end at the initial position, then the clamping block is pulled by the second rope to be at the position closest to the inner wall of the avoiding cavity, then the triangular block moves upwards, the connecting plate can move upwards together, then the connecting plate can not directly contact the clamping block due to the fact that the clamping block is close to the inner wall, then the clamping block contacts with a certain area, and then the connecting plate can pass through the clamping block more easily, then the connecting plate moves to the top and contacts with the control plate to push the control plate to move upwards, then the control plate compresses the sixth spring, then the control plate loosens the clamping block through the second rope, then the clamping block can be outwards popped out under the action of the fifth spring, then the clamping block can be clamped into the clamping groove to clamp the position of the connecting plate, then the position of the first guide rod and the position of the pressing plate are clamped, the position of the triangular block is clamped by the pressing plate through the first avoiding groove, then the lifting pipe can continue to move upwards, then the triangular block can not continue to move upwards, so the triangular block can be driven to move towards the directions of two sides, then the triangular block can drive the blocking block to move towards two sides, thereby the middle position of the blocking block can be opened, the vent pipe can be leaked outside, at the moment, the chlorine begins to be blown outwards, and then the air pump needs to be closed, that is, chlorine gas does not need to be blown, at the moment, the pressure in the pressure storage cavity can be reduced, so that the buffer assembly can reset, the buffer assembly resets to drive the boss round seat and the lifting pipe to move downwards, the lifting pipe moves downwards to enable the triangular block to lose force, then the triangular block is acted by the clamping groove and the clamping block and keeps the same position as the blocking block, but the triangular block cannot be acted by the two sides, so that the blocking block resets under the action of the second spring to block the vent pipe, at the moment, the solution outside the solution can be prevented from entering the vent pipe, then the buffer assembly resets continuously to drive the lifting pipe to move continuously downwards, then the lifting pipe can pull the first rope to move, the first rope is acted by the tensile force to pull the clamping block to move towards the direction of the inner wall, then the clamping block can be separated from the clamping groove and the clamping groove, so that after the blocking block is closed, the connecting plate can be reset, so that the first control component and the clamping component can be reset integrally.

D. The stirring rotating shaft drives the control structure to move, and then the control structure drives the stirring plate to change the angle through the stirring adjusting structure;

E. the angle of the stirring plate is adjusted through a proper speed structure according to the rotating speed of the stirring rotating shaft;

the invention mainly arranges a plurality of through holes on the stirring plate, thereby chlorine can be introduced into the reaction solution, then the stirring plate is arranged in a plurality of positions and can rotate along with the stirring rotating shaft, thereby chlorine can be introduced into a plurality of positions in the solution more uniformly, the time for mixing chlorine and solution can be accelerated, thereby the chlorination speed and the chlorination uniformity are greatly improved, the quality of the chlorinated solution is better, then the stirring plate can rotate along with the stirring rotating shaft during chlorination, thereby the stirring can be carried out during chlorination, the flowing speed of the solution is accelerated, and chlorine can be introduced into a plurality of positions and simultaneously can be contacted with solutions with different unit volumes under the rapid flowing of the solution, therefore, chlorine can be quickly contacted with more liquid, namely, chlorine in unit volume can be contacted with solution which is integral multiple of the volume of chlorine, so that the chlorination speed of chlorine in the solution can be better increased, then, the chlorine can be blown out under high pressure because the chlorine is introduced into the solution, the solution can flow back due to insufficient pressure after the pressure of the chlorine is reduced, namely, the chlorine can flow into a breather pipe, so that sulfuric acid is in the inside, the chlorine is easy to corrode for a long time, other reactions can occur, the service life is shortened, the subsequent chlorine is reacted before entering the solution, the whole chlorination reaction effect is influenced, and then, the triangular block is moved upwards firstly when the chlorine is pressurized, the blocking block is moved towards two sides through the triangular block, so that when the pressure on the buffer assembly is enough to blow out chlorine, the blocking block is not directly opened, the triangular block is pushed to move upwards, then the blocking block is opened through the triangular block, so that the pressure in the pressure storage cavity is larger than the pressure required by blowing out chlorine, then the air pump is used for ventilating the air and the vent pipe to have the same volume, namely the pressure in the pressure storage cavity is ensured, then when the blocking block is opened, the force for blowing out chlorine is very large, so that the solution outside the blocking block cannot flow in, then the problem of inaccurate control of the chlorine pressure and the air outlet time is avoided, the phenomenon that the solution flows back into the vent pipe is avoided, then when the air pump needs to be closed, namely chlorination is finished, the air pump stops feeding chlorine, then the pressure in the power storage cavity is reduced, so that the buffer assembly is reset, then the buffer assembly resets and drives the first control assembly and the clamping assembly to move through the lifting pipe, then the reset movement is opposite to the movement process, the blocking block is closed firstly, then the triangular block moves downwards, so that once the pressure in the power storage cavity is reduced a little, the blocking block resets, the blocking block blocks the vent pipe more quickly, the solution on the outer side is prevented from flowing back, then the blocking block is opened originally under the condition that the pressure in the power storage cavity is enough to blow out chlorine gas outwards, the time spent by the upward movement of the triangular block is added to ensure that the pressure accumulated in the power storage cavity is added with the blocking force exerted on the triangular block by a fourth spring which needs to be overcome by the upward movement of the triangular block, and the sum of the blocking force and the resultant pressure of the second spring need to be overcome by the upward movement of the blocking block to the two sides, however, the blocking block is closed under the condition that the pressure in the pressure storage cavity is smaller than the resultant pressure, so that when the blocking block is closed, the pressure in the pressure storage cavity is larger than the pressure for blowing out chlorine and smaller than the resultant pressure, and therefore backflow of the solution can be better prevented.

Furthermore, the buffering assembly comprises a first supporting plate fixedly arranged below the through hole, an eighth spring arranged between the first supporting plate and the boss round seat and used for enabling the boss round seat to reset downwards, a thrust plate arranged in the force storage cavity in a sliding mode, a plurality of pull rods fixedly arranged on the thrust plate, a seventh spring fixedly arranged on the thrust plate, and a third rope fixedly connected to the second telescopic rod of the ventilation structure and the boss round seat; a sealing plate is arranged on the thrust plate; the sealing plate is positioned below the through hole and used for sealing the through hole; the method comprises the following specific steps: chlorine gas enters the power storage cavity and then is blown onto the thrust plate, the thrust plate is pressurized, the pull rod is compressed, the thrust plate is driven to move, the through hole is originally blocked by the thrust plate and the sealing plate, the through hole is not blocked any more after the thrust plate moves, the chlorine gas can pass through the through hole, the pull rod is driven to move by the movement of the thrust plate, and the lifting pipe is pulled by the pull rod to move upwards through the third rope; the thrust plate slides and establishes in holding the power chamber, it also can't make the thrust plate take place inclination, thereby also can make a plurality of through-holes open simultaneously, time synchronization that a plurality of stop blocks opened and closed has also been realized, better control it, make chlorine can synchronous letting in and synchronous stopping, the precision of letting in chlorine has been improved, later the closing plate can be when the thrust plate resets, there is chlorine in the breather pipe can appear, later the cavity contact behind breather pipe and the thrust plate, also can arrive in the light body at seventh spring place, thereby setting through the closing plate, make chlorine can not reach in the seventh spring, thereby better utilize chlorine.

Furthermore, the speed-adapting structure comprises a rotating ring fixedly connected to the stirring rotating shaft, a latch fixedly arranged on the rotating ring, a first partition plate fixedly arranged in the stirring barrel and used for separating the speed-adapting structure from the control structure, a third support plate fixedly arranged on the first partition plate, a ninth spring fixedly connected to the third support plate, a second support plate fixedly connected to the ninth spring, a tooth socket arranged on the second support plate and used for being matched with the latch, a second telescopic rod arranged between the third support plate and the second support plate, and a first guide frame fixedly connected to the second support plate and the control structure; the method comprises the following specific steps: the stirring rotating shaft can drive the rotating ring to rotate, then the rotating ring drives the second supporting plate to move through the clamping teeth and the tooth grooves, so that the second supporting plate can be driven to move towards the direction far away from the third supporting plate, then the second telescopic rod can be stretched, then the clamping teeth on the rotating ring are few, so that the clamping teeth can be quickly disengaged from the tooth grooves, then the second supporting plate can be reset under the action of the second telescopic rod, and then the clamping teeth can be matched with the tooth grooves when the second telescopic rod does not drive the second supporting plate to be reset, so that the second supporting plate is driven to move, and therefore the second supporting plate can be driven to reciprocate under the guide of the ninth spring;

the restoring speed of the second support plate is increased along with the change of the degree of compression of the second telescopic rod, so that the rotating speed of the stirring rotating shaft is faster, the second support plate can be matched with the tooth socket and the latch after restoring is finished, the latch is matched with the tooth socket and the second telescopic rod drives the second support plate to restore to a certain stable position, namely the rotating speeds of the stirring rotating shaft are different, the second support plate can be positioned at different positions, and then the rotating speed of the stirring rotating shaft is faster, the second support plate is closer to the third support plate, otherwise, the reverse is true, and then the process of disengaging the latch from the tooth socket can be generated no matter how fast the rotating speed of the stirring rotating shaft is, so that the second support plate can reciprocate at a certain position along with the different rotating speeds of the stirring rotating shaft, so that the stirring plate can be stirred inside at a certain angle along with the different rotating speeds of the stirring rotating shaft, then, because the angle of the stirring plate is related to the stirring effect, the stirring plate is in different angles along with the change of the rotating speed of the stirring rotating shaft, namely the angle of the stirring plate is larger when the rotating speed of the stirring rotating shaft is higher, otherwise, the angle of the stirring plate is smaller, namely the angle of the stirring plate is changed along with the change of the rotating speed of the stirring rotating shaft, and then the angle of the chlorine gas blown outwards can be changed, so that the chlorine gas can be blown outwards from different angles along with the rotating speed of the stirring rotating shaft, the chlorine gas can be better uniformly distributed in the stirring barrel, the mixing speed of the chlorine gas and the solution in the stirring barrel is further improved, the chlorination speed and effect are further improved, and meanwhile, the stirring rotating shaft can drive the stirring plate to be in different stirring speeds and stirring efficiencies through different rotating speeds, that is to say the velocity of motion that can make near solution of chlorine also can change along with the angle that chlorine blew off, thereby can further make chlorine can be better and solution take place chloridizing, thereby better improvement the efficiency of chlorination, when adding the raw materials and stirring behind, also can make the stirring board carry out different stirring effect to the raw materials through the rotational speed that changes the stirring pivot, also after the angle of stirring board changes, can make the inside principle axial direction's of agitator stirring speed change, thereby can make the better stirring of raw materials, can make more relative motion produce between the raw materials through the speed that changes the stirring, thereby the speed that the stirring was mixed has been improved.

Furthermore, the control structure comprises a second connecting rod hinged to the first guide frame, a limiting assembly connected to the first guide frame, a second lifting ring arranged on the stirring rotating shaft in a sliding mode and connected to the stirring adjusting structure, a control structure discharging barrel fixedly connected to the second lifting ring and matched with the limiting assembly, a control block connected to the limiting assembly, second guide rods fixedly arranged on two sides of the control block, a third telescopic rod fixedly connected to the inner walls of the control block and the stirring barrel, a tenth spring arranged between the control block and the inner wall of the stirring barrel and used for enabling the control block to reset, a resetting assembly connected to the second guide rods, and a second control assembly connected to the second guide rods; the limiting assembly comprises a fourth supporting plate hinged to the second connecting rod, a third connecting rod hinged to the fourth supporting plate, a fifth supporting plate hinged to the third connecting rod, a limiting plate fixedly connected to the fifth supporting plate and not in contact with the stirring rotating shaft, a second partition plate fixedly arranged on the inner wall of the stirring barrel and used for separating the control structure from the stirred solution, a guide post fixedly arranged on the second partition plate and used for guiding the limiting plate, and an anti-falling plate fixedly arranged above the guide post and used for limiting the limiting plate; the stirring adjusting structure comprises a pressure rod fixedly arranged below the second lifting ring, a rotating block fixedly connected to the stirring rotating shaft and rotatably arranged in the second partition plate, a first lifting ring fixedly connected to the pressure rod, a fixed rod fixedly connected to the first lifting ring, a first hinge block fixedly connected to the fixed rod, a first connecting rod hinged to the first hinge block, a second hinge block hinged to the first connecting rod, an adjusting rotating shaft rotatably connected to the stirring rotating shaft and fixedly connected to the second hinge block and the stirring plate, and a first spring arranged between the rotating block and the control structure; the pressure lever is connected to the rotating block in a sliding manner; the method comprises the following specific steps: tooth socket movement can drive the control structure ventilation structure to move, then the control structure ventilation structure can drive two fourth supporting plates to approach each other through a second connecting rod, then the fourth supporting plates can drive a control block to move in opposite directions, then the control block movement can press the control structure discharging barrel to move downwards, then a second lifting ring can move downwards, then the second lifting ring can drive a stirring plate to adjust the angle through a stirring adjusting structure, then the fourth supporting plates can move in opposite directions and can also drive a fifth supporting plate to move downwards through a third connecting rod, then the fifth supporting plate can drive a limiting plate to move downwards, then the limiting plate and the guide post are in interference fit, so that the limiting plate cannot reset automatically after moving downwards, the limiting plate can block the movement of the second lifting ring, and the maximum distance of the upward movement of the second lifting ring is limited, the second lifting ring reciprocates up and down to drive the pressure rod to reciprocate up and down, then the rotating block is used for guiding the pressure rod, then the pressure rod drives the first lifting ring to move downwards, then the first lifting ring drives the first hinging block to move downwards through the fixing rod, then the first hinging block drives the first connecting rod to move, the first connecting rod drives the second hinging block to move, then the second hinging block rotates around the adjusting rotating shaft, namely the angle of the stirring plate changes, and therefore the angle of the stirring plate changes when the second lifting ring moves downwards;

the speed-adapting structure can enable the limiting plate to be in a certain position through the limiting component and then not to change, namely, the up-and-down reciprocating motion of the second lifting ring is limited, then the swinging angle of the stirring plate is limited, namely, the control block can be driven to press the control structure charging bucket after the rotating speed of the stirring rotating shaft is changed, the second lifting ring moves downwards, and when the stirring rotating shaft drives the second supporting plate to move through the clamping teeth, the second supporting plate is not in a certain fixed position but swings in a certain fixed range in a reciprocating manner, so that the second lifting ring can be driven to move, then, the limiting component enables the limiting plate to move downwards to limit the upward resetting height of the second lifting ring, namely, the second lifting ring can not reset upwards to an initial position, thereby realizing that the control block can drive the second lifting ring to swing in an up-and-down reciprocating manner, and make the better a certain position that is in of second lifting ring through the limiting plate, later better messenger's stirring board carries out the swing of small angle, thereby the stirring board can not only carry out angle regulation in inside, can also carry out the reciprocal swing of small angle, also can make chlorine better outwards blow off from the angle of difference, better messenger's solution chloridizes, and can also be better messenger's stirring board through the reciprocal swing of stirring board stirs the raw materials, the effect of stirring has been increased, thereby can be better prepare the product, the degree of consistency of mixing in the preparation process has been increased, the quality of product is improved.

Furthermore, the resetting assembly comprises a matching rod piece fixedly connected to the second guide rod, a second guide frame fixedly connected to the matching rod piece, a fourth guide rod fixedly connected to the second guide frame, a third guide frame fixedly connected to the fourth guide rod, a fifth guide rod fixedly connected to the third guide frame, an inflator connected to the fifth guide rod, an expansion belt fixedly arranged on the second partition plate and connected to the inflator, and a resetting pipe fixedly connected to the expansion belt and the limiting plate; the control structure also comprises a clamping assembly for clamping the reset tube; the method comprises the following specific steps: the control block moves and can drive the second guide bar to move, the second guide bar drives the cooperation member bar to move, later the cooperation member bar drives the second leading truck to move, later the second leading truck drives the fourth guide bar to move, the fourth guide bar drives the third leading truck to move, the third leading truck drives the fifth guide bar to move, later the fifth guide bar can be pressed, just can make the inflater inflate to inflation in-band portion, later the inflation area can expand, later clamping component has cliied the reset tube so gas in the inflation area can not outwards blow off in reset tube department, later the control block can carry out reciprocating motion, just also can make fifth guide bar reciprocating motion, inflate to inflation in-band portion through the inflator is reciprocal, thereby realize the energy storage in inflation area.

Furthermore, the clamping assembly comprises an inclined block connected to the second control assembly, a tenth guide rod fixedly arranged on the second partition plate, two clamping plates slidably arranged on the tenth guide rod, fourth connecting rods hinged to the two clamping plates, matching plates hinged to the two fourth connecting rods, a twelfth spring fixedly arranged between the two fourth connecting rods, a ninth guide rod fixedly arranged above the matching plates, and a lifting block fixedly arranged above the ninth guide rod and matched with the inclined block; the method comprises the following specific steps: the twelfth spring normally pushes the two clamping plates to move towards the two sides, so that the two clamping plates have a movement tendency of moving towards the two sides, then the lifting block has a movement tendency of moving downwards, then the control block is not in contact with the second guide rod when the stirring rotating shaft is static, then the control block is at an initial position, at this time, the control block does not drive the oblique block to move through the second control component, then the control block can drive the second control component to move once the control block starts to move, then the oblique block can be driven to move, then the oblique block can drive the lifting block to move upwards, then the ninth guide rod can be driven to move upwards, then the two clamping plates are clamped together through the matching plate and the fourth connecting rod, the reset pipe is clamped, and the clamping plates can move towards the two sides after the control block is reset to the initial position, so that the reset tube is not blocked any more;

the second control component can move after the control block moves, the reset tube is clamped, namely, the expansion band is enabled to store energy, then, the time for stirring at each time is long, and the reciprocating distance of the control block is short, so that the stirring can be carried out for a long time without causing too much energy storage of the expansion band to be damaged, and then, after the control block is reset, namely, the stirring is finished, at the moment, the control block is reset, the second guide rod and the second control component are matched, the clamp plate is enabled not to clamp the reset tube, the expansion band can blow outwards from the reset tube, the reset tube can stretch out and draw back, and then, the reset tube can push the second lifting ring to reset, so that the whole movement reset process is realized, and the stability of the movement is better guaranteed.

Furthermore, the second control assembly comprises a sixth supporting plate fixedly arranged on the second partition plate, an eleventh spring slidably connected to the sixth supporting plate, a reset plate fixedly connected to the eleventh spring and matched with the second guide rod, an eleventh spring arranged between the reset plate and the sixth supporting plate, a fourth guide frame fixedly connected to the sixth guide rod, a seventh guide rod fixedly arranged on the second partition plate, an eighth guide rod slidably connected to the seventh guide rod and fixedly connected to the fourth guide frame, and a fifth guide frame fixedly arranged on the second partition plate and used for guiding the eighth guide rod; the eighth guide rod is fixedly connected to the inclined block; the elastic force of the sixth guide rod is greater than that of the twelfth spring; the elastic force of the tenth spring is greater than that of the sixth guide rod; the method comprises the following specific steps that a second guide rod returns to the original position, the second guide rod can be abutted to a reset plate, the reset plate is stressed, a sixth guide rod can be driven to move, the sixth guide rod drives a fourth guide frame to move, the sixth guide rod slides on a sixth supporting plate, the fourth guide frame drives an eighth guide rod to move, a seventh guide rod guides the eighth guide rod, the eighth guide rod can drive an inclined block stirring rotating shaft to move, a control block moves, the second guide rod can move, the second guide rod can not be abutted to the reset plate, the reset plate can reset under the action of an eleventh spring, the reset plate can drive the sixth guide rod to move, the eighth guide rod can be driven to move through the fourth guide frame, the inclined block can be inserted into a lifting block, and the reset tube is controlled.

Furthermore, the stirring adjusting structure also comprises guide rings which are fixedly arranged on the pressure rod and positioned at the upper end and the lower end of the first lifting ring; the upper end and the lower end of the uppermost first lifting ring and the lowermost first lifting ring are not provided with guide rings; the uppermost and lowermost first lifting rings are fixedly connected to the pressure rod, and the first lifting ring at the middle position is slidably connected to the pressure rod; a gap is reserved between the guide ring and the first lifting ring; the gaps between the two middle guide rings and the first lifting ring are different; through depression bar up-and-down motion drive first lifting ring up-and-down motion, just also can make the stirring board rotate, later two guide rings in the middle of when driving first lifting ring up-and-down motion, can be because gapped and the variation in size in clearance between guide ring and the first lifting ring, so can make first lifting ring up-and-down motion's distance different, thereby can make the rotatory angle of stirring board different, also two differences in the middle of four rotatory angles of stirring board, two upper and lower are the same, thereby can make the stirring board be in different angles and stir it, thereby better stir the solution of agitator inside and can also better make chlorine gas spout different positions simultaneously, further increase the effect of chlorination, thereby also increase the degree of consistency that the raw materials mixes, thereby the quality of product has been improved.

The raw material in the stirring barrel 1 is sulfuric acid as a solvent; the concentration of the sulfuric acid is 10-90%.

The concentration of sulfuric acid used in chlorination is 10-90%, and nitrosyl sulfuric acid can be directly dripped for diazotization subsequently; and (4) coupling with a coupling compound to obtain a dye filter cake. No waste acid is generated in the whole process, and zero emission is realized; the COD of the used sulfuric acid is controlled below 5000mg/L, the selectivity to the waste sulfuric acid is wider, and most industrial waste sulfuric acid can be used indiscriminately;

in conclusion, the invention can better ensure that chlorine is introduced into the solution and the solution does not flow back through the ventilation structure, thereby better ensuring the mixing uniformity of the chlorine and the solution; set up suitable fast structure and control structure, can adjust the angle of stirring board according to the difference of stirring to change the angle that chlorine lets in, further improved the even effect that leads to in the solution of chlorine, made its mix more evenly, and make the stirring effect of product better, improve product quality.

Drawings

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

FIG. 2 is a schematic view of the present invention with the agitator removed;

FIG. 3 is an enlarged view of A of FIG. 2 according to the present invention;

FIG. 4 is an enlarged view of B of FIG. 2 according to the present invention;

FIG. 5 is a schematic structural view of a dispensing bucket according to the present invention;

FIG. 6 is a schematic structural diagram of a preferred speed structure according to the present invention;

FIG. 7 is a schematic structural diagram of a control structure according to the present invention;

FIG. 8 is a schematic structural view of a reset device according to the present invention;

FIG. 9 is an enlarged view of C of FIG. 8 according to the present invention;

FIG. 10 is a schematic view of the clamp assembly of the present invention;

FIG. 11 is a schematic view of a second lift ring according to the present invention;

FIG. 12 is a schematic view of a cushion assembly according to the present invention;

FIG. 13 is a schematic view of a stop according to the present invention;

FIG. 14 is a schematic view of the N-N position structure of the present invention;

FIG. 15 is a schematic sectional plan view of the structure of N-N in the present invention;

FIG. 16 is an enlarged view of D of FIG. 15 in accordance with the invention;

FIG. 17 is an enlarged view of E of FIG. 16 in accordance with the invention;

FIG. 18 is an enlarged view of F of FIG. 17 in accordance with the invention;

FIG. 19 is an enlarged view of G of FIG. 17 in accordance with the invention;

FIG. 20 is a schematic perspective sectional view of N-N in the present invention;

FIG. 21 is an enlarged view of H in FIG. 20 according to the present invention;

FIG. 22 is an enlarged view of I of FIG. 21 in accordance with the present invention;

FIG. 23 is a table of experimental charges of the present invention;

FIG. 24 is a table of experimental structures according to the present invention;

FIG. 25 is a drawing of a chromatogram of hexachloro-benzene according to the present invention.

Detailed Description

In order to make the technical solutions of the present invention better understood, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention.

As shown in FIGS. 1 to 25, a process for preparing 2, 4-dinitro-6-chloroaniline by a sulfuric acid method comprises the following steps: processing and reacting the reaction raw materials by using a stirring device, and discharging and filtering after the reaction is finished; the stirring device comprises a stirring barrel 1, a motor 2 fixedly arranged on the stirring barrel 1, a first support 21 fixedly arranged on the stirring barrel 1 and used for supporting the motor 2, an electric plate 3 arranged on the stirring barrel 1, a speed-adapting structure 6 arranged below the motor 2, a control structure 5 arranged below the speed-adapting structure 6, a stirring rotating shaft 4 connected to the motor 2, a stirring plate 7 fixedly connected to the motor 2, a ventilation structure 8 arranged on the stirring plate 7 and a stirring adjusting structure 9 connected to the stirring plate 7; the stirring step comprises:

A. putting reaction raw materials and sulfuric acid into a stirring barrel 1;

B. starting the motor 2 and driving the stirring rotating shaft 4 to rotate, wherein the stirring rotating shaft 4 drives the stirring plate 7 to rotate so as to stir the raw materials;

C. introducing chlorine gas into the raw materials in the stirring barrel 1 through the ventilation structure 8 before stirring the raw materials; the ventilation structure 8 comprises an air pump 89 fixedly arranged below the stirring barrel 1, a connecting pipe 891 fixedly connected to the air pump 89, an air passage 82 communicated with the connecting pipe 891, a force storage cavity 71 communicated with the air passage 82, a buffer component 83 arranged in the force storage cavity 71, a through hole arranged on the stirring plate 7, an air pipe 85 arranged on the through hole, a boss round seat 861 arranged in the air pipe 85 in a sliding manner, a lifting pipe 86 fixedly connected to the boss round seat 861, a blocking block 84 arranged above the stirring plate 7 in a sliding manner and used for blocking the air pipe 85, a first control component 87 connected to the lifting pipe 86 and used for opening the blocking block 84, and a clamping component 88 connected to the first control component 87; the first control assembly 87 comprises a avoiding cavity arranged on the inner surface of the blocking block 84, a triangular block 875 arranged on the avoiding cavity in a sliding manner, a sliding hole arranged on the triangular block 875, a first guide rod 872 arranged in the sliding hole in a sliding manner, a pressing plate 871 fixedly connected to the first guide rod 872 and positioned below the triangular block 875, a first avoiding groove arranged below the triangular block 875 and matched with the pressing plate 871, a third spring 878 arranged in the pressing plate 871 and the first avoiding groove and used for resetting the pressing plate 871, a connecting plate 873 fixedly arranged on the first guide rod 872, a clamping groove 874 arranged on the connecting plate 873, a telescopic baffle 876 fixedly arranged above the triangular block 875 and used for sealing the avoiding cavity, and a fourth spring 877 arranged between the triangular block 875 and the top surface of the avoiding cavity; the clamping assembly 88 comprises a second avoiding groove arranged on the inner wall of the avoiding cavity, a third avoiding groove arranged on the top surface, a fixture block 881 arranged in the second avoiding groove in a sliding manner, a first telescopic rod 882 fixedly arranged between the fixture block 881 and the second avoiding groove, a fifth spring 883 arranged on the fixture block 881 and used for resetting the fixture block 881, a first rope 884 connected with the fifth spring 883 and the boss circular seat 861, a control board 886 arranged in the third avoiding groove in a sliding manner, a sixth spring 887 fixedly arranged above the control board 886 and used for resetting the control board 886, and a second rope 885 fixedly connected with the control board 886 and the fixture block 881; the method comprises the following steps: the air pump 89 introduces chlorine gas into the stirring rotating shaft 4, then the stirring rotating shaft 4 is hollow, the chlorine gas reaches the air channel 82 through the connecting pipe 891 and the stirring rotating shaft 4 and is blown into the power storage chamber 71, then the chlorine gas is buffered through the buffer assembly 83, so that the pressure in the power storage chamber 71 is stored, then the buffer assembly 83 moves when the pressure in the power storage chamber 71 is sufficiently high, then the buffer assembly 83 is firstly blocked in front of the through hole, namely the chlorine gas cannot pass through the through hole, then the buffer assembly 83 moves and moves behind the through hole, so that the chlorine gas enters the through hole, namely the chlorine gas reaches the air pipe 85, the buffer assembly 83 moves to drive the lifting pipe 86 to move upwards, then the boss round seat 861 slides in the air pipe 85, the lifting pipe 86 moves upwards to first impact the pressure plate 871, then the pressure plate 871 drives the first guide rod 872 to slide upwards in the sliding hole, then the connecting plate 873 is driven to move, the connecting plate 873 is driven to move upwards and approach the inner wall of the avoiding cavity, then after the pressing plate 871 moves into the first avoiding groove, the pressing plate 871 cannot move continuously, at this time, the lifting pipe 86 is in contact with the triangular block 875, so as to drive the triangular block 875 to move, then the elastic force of the second spring 81 is greater than that of the fourth spring 877, so that the first time movement of the triangular block 875 is realized by moving upwards until the triangular block 875 moves to the uppermost blocked position, then the elastic force of the sixth spring 887 is greater than that of the fifth spring 883, so that the control plate 886 is at the lowest end at the initial position, then the fixture 881 is pulled to be at the position closest to the inner wall of the avoiding cavity by the second rope 885, then the triangular block 875 moves upwards, the connecting plate 873 moves upwards together, and then the connecting plate 873 cannot directly contact with the fixture 881 in a large area because the fixture 881 is close to the inner wall, then the fixture block 881 contacts with a little area, then the connecting plate 873 can more easily pass through the fixture block 881, then the connecting plate 873 moves to the uppermost position and contacts with the control plate 886 to push the control plate 886 to move upwards, then the control plate 886 compresses the sixth spring 887, then the control plate 886 releases the fixture block 881 through the second rope 885, then the fixture block 881 is ejected outwards under the action of the fifth spring 883, then the fixture block 881 is clamped into the clamping groove 874 to clamp the position of the connecting plate 873, then the positions of the first guide rod 872 and the pressure plate 871 are clamped, the pressure plate 871 clamps the position of the triangular block 875 through the first avoiding groove, then the lifting pipe 86 continues to move upwards, then the triangular block 875 cannot continue to move upwards, so that the triangular block 875 is driven to move towards the directions of two sides, then the triangular block 84 is driven to move towards two sides, therefore, the middle position of the blocking block 84 can be opened, the vent pipe 85 can be exposed outside, at this time, chlorine gas begins to be blown out outwards, when the air pump 89 needs to be closed later, namely, chlorine gas does not need to be blown out, at this time, the pressure in the power storage cavity 71 can be reduced, so that the buffering component 83 can be reset, the buffering component 83 can drive the boss round seat 861 and the lifting pipe 86 to move downwards, the lifting pipe 86 moves downwards to enable the triangular block 875 to lose force, then the triangular block 875 is under the action of the clamping groove 874 and the clamping block 881 and keeps the same position as the blocking block 84, but the triangular block 875 cannot be subjected to acting force towards two sides, so that the blocking block 84 can be reset under the action of the second spring 81, so that the vent pipe 85 is blocked, at this time, the solution outside the vent pipe 85 can be prevented from entering, and then the buffering component 83 can be reset continuously, drive the elevator tube 86 and continue the downward motion, later the elevator tube 86 can stimulate first rope 884 and move, first rope 884 receives the pulling force and can stimulate the direction motion of fixture block 881 towards the inner wall, later can make fixture block 881 break away from the screens with draw-in groove 874 to after blockking that piece 84 closes, can make connecting plate 873 reset, thereby can make first control assembly 87 and screens subassembly 88 wholly reset.

D. The stirring rotating shaft 4 drives the control structure 5 to move, and then the control structure 5 drives the stirring plate 7 to change the angle through the stirring adjusting structure 9.

E. The angle of the stirring plate 7 is adjusted through the speed adapting structure 6 according to the rotating speed of the stirring rotating shaft 4;

specifically, the buffer assembly 83 includes a first support plate 833 fixedly disposed below the through hole, an eighth spring 834 disposed between the first support plate 833 and the boss circular seat 861 for returning the boss circular seat 861 downward, a thrust plate 836 slidably disposed in the power storage chamber 71, a plurality of tie rods 835 fixedly disposed on the thrust plate 836, a seventh spring 831 fixedly disposed on the thrust plate 836, and a third rope 832 fixedly connected to the second expansion link 65 of the ventilation structure 8 and the boss circular seat 861; a sealing plate is arranged on the thrust plate 836; the sealing plate is positioned below the through hole and used for sealing the through hole; the method comprises the following specific steps: chlorine gas enters the power accumulation cavity 71 and then is blown onto the thrust plate 836, then the thrust plate 836 is pressurized to compress the pull rod 835, so that the thrust plate 836 is driven to move, then the thrust plate 836 and the sealing plate originally block the through hole, after the thrust plate 836 moves, the through hole is not blocked any more, so that the chlorine gas can pass through the through hole, then the thrust plate 836 moves to drive the pull rod 835 to move, and the pull rod 835 pulls the lifting pipe 86 to move upwards through the third rope 832; the thrust plate 836 is slidably arranged in the power storage cavity 71, that is, there is no way to make the thrust plate 836 have an inclination angle, so that a plurality of through holes can be opened simultaneously, that is, time synchronization of opening and closing of a plurality of blocking blocks 84 is realized, the control is better performed on the thrust plate 836, chlorine can be synchronously introduced and stopped synchronously, the accuracy of introducing chlorine is improved, then, when the thrust plate 836 is reset, chlorine gas exists in the vent pipe 85, then, the vent pipe 85 is in contact with a cavity behind the thrust plate 836, that is, a light body where the seventh spring 831 is located is reached, so that the chlorine gas cannot reach the seventh spring 831 through the arrangement of the sealing plate, and thus, the chlorine gas is better utilized.

Specifically, the structure 6 with suitable speed comprises a rotating ring 61 fixedly connected to the stirring rotating shaft 4, a latch 62 fixedly arranged on the rotating ring 61, a first partition fixedly arranged inside the stirring barrel 1 and used for separating the structure 6 with suitable speed from the control structure 5, a third support plate 67 fixedly arranged on the first partition, a ninth spring 66 fixedly connected to the third support plate 67, a second support plate 63 fixedly connected to the ninth spring 66, a tooth groove 64 arranged on the second support plate 63 and used for matching with the latch 62, a second telescopic rod 65 arranged between the third support plate 67 and the second support plate 63, and a first guide frame 68 fixedly connected to the second support plate 63 and the control structure 5; the method comprises the following specific steps: the stirring rotating shaft 4 can drive the rotating ring 61 to rotate, then the rotating ring 61 drives the second supporting plate 63 to move through the latch 62 and the tooth socket 64, so as to drive the second supporting plate 63 to move towards the direction away from the third supporting plate 67, then the second telescopic rod 65 can be stretched, then the latch 62 on the rotating ring 61 is few, so that the latch 62 can be quickly disengaged from the tooth socket 64, then the second supporting plate 63 can be reset under the action of the second telescopic rod 65, then the latch 62 is matched with the tooth socket 64 when the second telescopic rod 65 does not drive the second supporting plate 63 to be reset, so as to drive the second supporting plate 63 to move, and thus the second supporting plate 63 can be guided by the ninth spring 66 to reciprocate.

Specifically, the control structure 5 comprises a second connecting rod 51 hinged to the first guide frame 68, a limiting component 52 connected to the first guide frame 68, a second lifting ring 53 slidably arranged on the stirring rotating shaft 4 and connected to the stirring adjusting structure 9, a control structure 5 discharging barrel 31 fixedly connected to the second lifting ring 53 and matched with the limiting component 52, a control block 56 connected to the limiting component 52, a second guide rod 561 fixedly arranged on two sides of the control block 56, a third telescopic rod 563 fixedly connected to the control block 56 and the inner wall of the stirring barrel 1, a tenth spring 562 arranged between the control block 56 and the inner wall of the stirring barrel 1 for resetting the control block 56, a resetting component 54 connected to the second guide rod 561, and a second control component 55 connected to the second guide rod 561; the limiting assembly 52 comprises a fourth supporting plate 521 hinged to the second connecting rod 51, a third connecting rod 522 hinged to the fourth supporting plate 521, a fifth supporting plate 523 hinged to the third connecting rod 522, a limiting plate 524 fixedly connected to the fifth supporting plate 523 and not in contact with the stirring rotating shaft 4, a second partition plate fixedly arranged on the inner wall of the stirring barrel 1 and used for separating the control structure 5 from the stirred solution, a guide column 525 fixedly arranged on the second partition plate and used for guiding the limiting plate 524, and an anti-dropping plate 526 fixedly arranged above the guide column 525 and used for limiting the limiting plate 524; the stirring adjusting structure 9 comprises a pressing rod 97 fixedly arranged below the second lifting ring 53, a rotating block 98 fixedly connected to the stirring rotating shaft 4 and rotatably arranged in the second partition plate, a first lifting ring 91 fixedly connected to the pressing rod 97, a fixing rod 92 fixedly connected to the first lifting ring 91, a first hinge block 93 fixedly connected to the fixing rod 92, a first connecting rod 94 hinged to the first hinge block 93, a second hinge block 95 hinged to the first connecting rod 94, an adjusting rotating shaft 96 rotatably connected to the stirring rotating shaft 4 and fixedly connected to the second hinge block 95 and the stirring plate 7, and a first spring 971 arranged between the rotating block 98 and the control structure 5; the pressure lever 97 is slidably connected to the rotating block 98; the method comprises the following specific steps: the tooth socket 64 can drive the ventilating structure 8 of the control structure 5 to move, then the ventilating structure 8 of the control structure 5 can drive two fourth supporting plates 521 to approach each other through the second connecting rod 51, then the fourth supporting plates 521 can drive the control block 56 to move in opposite directions, then the control block 56 can press the discharging barrel 31 of the control structure 5 to move downwards, then the second lifting ring 53 can drive the stirring plate 7 to adjust the angle through the stirring adjusting structure 9, then the fourth supporting plates 521 can drive the fifth supporting plate 523 to move downwards through the third connecting rod 522 in opposite directions, then the fifth supporting plate 523 can drive the limiting plate 524 to move downwards, then the limiting plate 524 and the guide post 525 are in interference fit, so that the limiting plate 524 cannot reset by itself after moving downwards, and the limiting plate 524 can block the movement of the second lifting ring 53, the maximum distance that makes second lift ring 53 upward movement receives the restriction, second lift ring 53 up-and-down reciprocating motion can drive depression bar 97 up-and-down reciprocating motion, later rotatory piece 98 is used for leading depression bar 97, later depression bar 97 can drive first lift ring 91 downstream, later first lift ring 91 passes through dead lever 92 and drives first articulated piece 93 downstream, later first articulated piece 93 drives first connecting rod 94 motion, first connecting rod 94 drives second articulated piece 95 and moves, later second articulated piece 95 can carry out round the rotation of adjusting pivot 96, the angle that also can make stirring board 7 changes, thereby second lift ring 53 downstream just can make the angle of stirring board 7 change.

Specifically, the reset assembly 54 includes a mating rod 541 fixedly connected to the second guide rod 561, a second guide frame 542 fixedly connected to the mating rod 541, a fourth guide rod 543 fixedly connected to the second guide frame 542, a third guide frame 544 fixedly connected to the fourth guide rod 543, a fifth guide rod 545 fixedly connected to the third guide frame 544, an air pump 546 connected to the fifth guide rod 545, an expansion belt 547 fixedly arranged on the second partition and connected to the air pump 546, and a reset tube 548 fixedly connected to the expansion belt 547 and the limit plate 524; the control structure 5 further includes a clamping assembly 57 for clamping the reset tube 548; the method comprises the following specific steps: the movement of the control block 56 drives the second guide rod 561 to move, the second guide rod 561 drives the matching rod 541 to move, then the matching rod 541 drives the second guide frame 542 to move, then the second guide frame 542 drives the fourth guide rod 543 to move, the fourth guide rod 543 drives the third guide frame 544 to move, the third guide frame 544 drives the fifth guide rod 545 to move, then the fifth guide rod 545 is pressed, that is, the air pump 546 is inflated into the expansion band 547, then the expansion band 547 is expanded, then the clamp assembly 57 clamps the reset tube 548, so that the air in the expansion band 547 is not blown out at the reset tube 548, then the control block 56 reciprocates, that is, the fifth guide rod 545 reciprocates, the inflation pump 546 is used to reciprocally inflate the expansion belt 547, thereby accumulating energy in the expansion belt 547.

Specifically, the clamping assembly 57 includes a sloping block 571 connected to the second control assembly 55, a tenth guide rod 574 fixedly disposed on the second partition plate, two clamping plates 575 slidably disposed on the tenth guide rod 574, a fourth connecting rod 576 hinged to the two clamping plates 575, a mating plate 577 hinged to the two fourth connecting rods 576, a twelfth spring 578 fixedly disposed between the two fourth connecting rods 576, a ninth guide rod 573 fixedly disposed above the mating plate 577, and a lifting block 572 fixedly disposed above the ninth guide rod 573 and mated to the sloping block 571; the method comprises the following specific steps: the twelfth spring 578 normally pushes the two clamping plates 575 to move towards two sides, so that the two clamping plates 575 move towards two sides, and then the lifting block 572 moves downwards, and then when the stirring shaft 4 is stationary, the control block 56 does not contact the second guide rod 561, and then the control block 56 is in the initial position, and then the control block 56 does not drive the inclined block 571 to move through the second control component 55, and then the control block 56 once starts moving, and then the second control component 55 moves, and then the inclined block 571 drives the lifting block 572 upwards, and then the ninth guide rod 573 moves upwards, and then the two clamping plates 575 are clamped together through the matching plate 577 and the fourth connecting rod 576, the reset tube 548 is clamped, and when the control block 56 is reset to the initial position, the clamping plates 575 move towards two sides, thereby no longer seizing the reset tube 548.

Specifically, the second control assembly 55 includes a sixth support plate 554 fixedly disposed on the second partition, an eleventh spring 553 slidably coupled to the sixth support plate 554, a reset plate 551 fixedly coupled to the eleventh spring 553 and engaged with the second guide bar 561, the eleventh spring 553 disposed between the reset plate 551 and the sixth support plate 554, a fourth guide frame 555 fixedly coupled to the sixth guide bar 552, a seventh guide bar 556 fixedly disposed on the second partition, an eighth guide bar 557 slidably coupled to the seventh guide bar 556 and fixedly coupled to the fourth guide frame 555, and a fifth guide frame 558 fixedly disposed on the second partition for guiding the eighth guide bar 557; the eighth guide rod 557 is fixedly connected to the inclined block 571; the elastic force of the sixth guide rod 552 is greater than that of the twelfth spring 578; the elastic force of the tenth spring 562 is greater than that of the sixth guide rod 552; the specific steps are that the second guide bar 561 returns to the original position and abuts against the reset plate 551, then the reset plate 551 is subjected to pressure to drive the sixth guide bar 552 to move, then the sixth guide bar 552 drives the fourth guide frame 555 to move, the sixth guide bar 552 slides on the sixth support plate 554, the fourth guide frame 555 drives the eighth guide bar 557 to move, the seventh guide bar 556 guides the eighth guide bar 557, then the eighth guide bar 557 drives the inclined block 571 stirring rotating shaft 4 to move, then the control block 56 moves to move the second guide bar 561, then the second guide bar 561 does not abut against the reset plate 551 any more, then the reset plate 551 is reset under the action of the eleventh spring 553, so that the reset plate 551 drives the sixth guide bar 552 to move, then the eighth guide bar 557 is driven to move by the fourth guide frame 555, thereby causing the ramp block 571 to be inserted into the lift block 572 to control the reset tube 548.

Specifically, the stirring adjustment structure 9 further includes a guide ring 99 fixedly disposed on the pressing rod 97 and located at the upper and lower ends of the first lifting ring 91; the upper and lower ends of the uppermost and lowermost first lifting rings 91 are not provided with guide rings 99; the uppermost and lowermost first lifting rings 91 are fixedly connected to the pressure lever 97, and the intermediate first lifting ring 91 is slidably connected to the pressure lever 97; a gap is reserved between the guide ring 99 and the first lifting ring 91; the gaps between the two middle guide rings 99 and the first lifting ring 91 are different; the first lifting ring 91 is driven to move up and down by the up-and-down reciprocating motion of the pressure lever 97, that is, the stirring plate 7 is rotated, then when the two guide rings 99 in the middle drive the first lifting ring 91 to move up and down, due to the gap between the guide ring 99 and the first elevation ring 91 and the difference in size of the gap, the first elevating ring 91 is caused to reciprocate up and down at different distances, so that the agitating plates 7 are caused to rotate at different angles, that is, two of the four agitating plates 7 are different in rotation angle, the upper and lower are the same, thereby can make stirring board 7 be in different angles and stir it to better stir 1 inside solution of agitator and can also better make chlorine gas spout different positions simultaneously, further increase the effect of chlorination, thereby also increase the degree of consistency that the raw materials mixes, thereby improved the quality of product.

Experimental conditions: introducing chlorine into 35% sulfuric acid to verify the purity and yield of hexachloro.

And (3) experimental operation: 1. 60g of 2, 4-dinitroaniline and 0.28gMF are weighed in a 500ml flask and are beaten for 30 minutes; 2. heating to 25 ℃, starting to introduce chlorine gas until the introduced chlorine gas reaches 30g, and sampling and detecting an end point (94%);

3. when the temperature reaches the end point, the temperature is increased to 63 ℃, the temperature is kept for one hour, and the temperature is reduced to 50 ℃;

4. finally discharging and filtering.

5. Experimental procedures figures 23-25.

It is to be understood that the described embodiments are merely a few embodiments of the invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

Claims

1. A technology for preparing 2, 4-dinitro-6-chloroaniline by a sulfuric acid method is characterized by comprising the following steps: the method comprises the following steps: processing and reacting the reaction raw materials by using a stirring device, and discharging and filtering after the reaction is finished; the stirring device comprises a stirring barrel (1), a motor (2) fixedly arranged on the stirring barrel (1), a first support (21) fixedly arranged on the stirring barrel (1) and used for supporting the motor (2), an electric plate (3) arranged on the stirring barrel (1), a speed-adapting structure (6) arranged below the motor (2), a control structure (5) arranged below the speed-adapting structure (6), a stirring rotating shaft (4) connected to the motor (2), a stirring plate (7) fixedly connected to the motor (2), an air-ventilating structure (8) arranged on the stirring plate (7) and a stirring adjusting structure (9) connected to the stirring plate (7);

the stirring step comprises:

A. putting reaction raw materials and sulfuric acid into a stirring barrel (1);

B. starting the motor (2) and driving the stirring rotating shaft (4) to rotate, wherein the stirring rotating shaft (4) drives the stirring plate (7) to rotate so as to stir the raw materials;

C. introducing chlorine gas into the raw materials in the stirring barrel (1) through a ventilation structure (8) before stirring the raw materials; the ventilation structure (8) comprises an air pump (89) fixedly arranged below the stirring barrel (1), a connecting pipe (891) fixedly connected to the air pump (89), an air passage (82) communicated with the connecting pipe (891), a force storage cavity (71) communicated with the air passage (82), a buffer component (83) arranged in the force storage cavity (71), a through hole arranged on the stirring plate (7), an air pipe (85) arranged on the through hole, a boss round seat (861) arranged in the air pipe (85) in a sliding manner, a lifting pipe (86) fixedly connected to the boss round seat (861), a blocking block (84) arranged above the stirring plate (7) in a sliding manner and used for blocking the air pipe (85), a first control component (87) connected to the lifting pipe (86) and used for opening the blocking block (84), and a clamping component (88) connected to the first control component (87); the first control component (87) comprises a avoiding cavity arranged on the inner surface of the blocking block (84), a triangular block (875) arranged on the avoiding cavity in a sliding manner, a sliding hole arranged on the triangular block (875), a first guide rod (872) arranged in the sliding hole in a sliding manner, a pressing plate (871) fixedly connected to the first guide rod (872) and positioned below the triangular block (875), and a first avoiding groove arranged below the triangular block (875) and matched with the pressing plate (871), the third spring (878) is arranged in the pressing plate (871) and the first avoiding groove and used for resetting the pressing plate (871), the connecting plate (873) is fixedly arranged on the first guide rod (872), the clamping groove (874) is arranged on the connecting plate (873), the telescopic baffle (876) is fixedly arranged above the triangular block (875) and used for sealing the avoiding cavity, and the fourth spring (877) is arranged between the triangular block (875) and the top surface of the avoiding cavity; the clamping assembly (88) comprises a second avoiding groove arranged on the inner wall of the avoiding cavity, a third avoiding groove arranged on the top surface, a fixture block (881) arranged in the second avoiding groove in a sliding manner, a first telescopic rod (882) fixedly arranged between the fixture block (881) and the second avoiding groove, a fifth spring (883) arranged on the fixture block (881) and used for resetting the fixture block (881), a first rope (884) connected with the fifth spring (883) and the boss round seat (861), a control plate (886) arranged in the third avoiding groove in a sliding manner, a sixth spring (887) fixedly arranged above the control plate (886) and used for resetting the control plate (886), and a second rope (885) fixedly connected with the control plate (886) and the fixture block (881); the method comprises the following steps: the air pump (89) introduces chlorine into the stirring rotating shaft (4), then the stirring rotating shaft (4) is hollow, the chlorine can reach the air passage (82) through the connecting pipe (891) and the stirring rotating shaft (4) and is blown into the force accumulation cavity (71), then the chlorine is buffered through the buffer component (83), the pressure accumulation is carried out in the force accumulation cavity (71), then the buffer component (83) can move after the pressure in the force accumulation cavity (71) is enough, then the buffer component (83) is firstly blocked in front of the through hole, namely the chlorine can not pass through the through hole, then the buffer component (83) moves and can move to the rear of the through hole, therefore the chlorine can enter the through hole, namely the chlorine reaches the air pipe (85), the buffer component (83) can drive the lifting pipe (86) to move upwards when moving, then the boss round seat (861) slides in the air pipe (85), the lifting pipe (86) moves upwards to impact the pressing plate (871), then the pressing plate (871) drives the first guide rod (872) to slide upwards in the sliding hole, then the connecting plate (873) is driven to move, the connecting plate (873) is driven to move upwards and approach the inner wall of the avoiding cavity, then after the pressing plate (871) moves into the first avoiding groove, the pressing plate (871) cannot move continuously, at the moment, the lifting pipe (86) is in contact with the triangular block (875) to drive the triangular block (875) to move, then, the elastic force of the second spring (81) is greater than that of the fourth spring (877), so that the first-time movement of the triangular block (875) is realized by the upward movement until the triangular block (875) moves to the uppermost blocking position, then, the elastic force of the sixth spring (887) is greater than that of the fifth spring (883), and therefore, the initial position is the lowest control plate (886), then the clamping block (881) is pulled to be positioned at the position closest to the inner wall of the avoiding cavity through the second rope (885), then the triangular block (875) moves upwards, the connecting plate (873) moves upwards together, then the connecting plate (873) cannot be directly contacted with the clamping block (881) in a large area due to the fact that the clamping block (881) is close to the inner wall, then the clamping block (881) is contacted with a point area, then the connecting plate (873) can more easily pass through the clamping block (881), then the connecting plate (873) moves to the uppermost direction and can be contacted with the control plate (886), the control plate (886) is pushed to move upwards, then the control plate (886) compresses the sixth spring (887), then the control plate (886) loosens the clamping block (881) through the second rope (885), then the clamping block (881) can be outwards ejected under the action of the fifth spring (883), then the clamping block (881) can be clamped into the clamping groove (874), and the position of the connecting plate (873) can be clamped, then the positions of the first guide rod (872) and the pressure plate (871) are clamped, the position of the triangular block (875) is clamped by the pressure plate (871) through the first avoiding groove, then the lifting pipe (86) continues to move upwards, then the triangular block (875) cannot continue to move upwards, so the triangular block (875) is driven to move towards the two sides, then the triangular block (875) drives the blocking block (84) to move towards the two sides, the middle position of the blocking block (84) is opened, the vent pipe (85) is exposed outside, at the moment, chlorine gas is blown outwards, then the air pump (89) is required to be closed, namely, the chlorine gas is not required to be blown, at the moment, the pressure in the power storage cavity (71) is reduced, the buffer assembly (83) is reset, the buffer assembly (83) resets and drives the boss circular seat (861) and the lifting pipe (86) to move downwards, the lifting pipe (86) moves downwards to enable the triangular block (875) to lose force, then the triangular block (875) is under the action of the clamping groove (874) and the clamping block (881) and keeps the same position as the blocking block (84), but the triangular block (875) cannot be under the action of force towards two sides, so that the blocking block (84) can reset under the action of the second spring (81), the vent pipe (85) is blocked, the solution outside the solution can be prevented from entering the interior of the vent pipe (85), then the buffer assembly (83) continuously resets to drive the lifting pipe (86) to continuously move downwards, then the lifting pipe (86) can pull the first rope (884) to move, the first rope (884) is under the action of pulling force to pull the clamping block (881) to move towards the direction of the inner wall, then the clamping block (881) can be separated from the clamping groove (874), and then after the blocking block (84) is closed, the connecting plate (873) is reset, so that the first control assembly (87) and the blocking assembly (88) are reset integrally.

D. The stirring rotating shaft (4) drives the control structure (5) to move, and then the control structure (5) drives the stirring plate (7) to change the angle through the stirring adjusting structure (9).

E. The angle of the stirring plate (7) is adjusted through the speed adapting structure (6) according to the rotating speed of the stirring rotating shaft (4).

2. The process for preparing 2, 4-dinitro-6-chloroaniline by the sulfuric acid method according to claim 1, which is characterized in that: the buffer assembly (83) comprises a first supporting plate (833) fixedly arranged below the through hole, an eighth spring (834) arranged between the first supporting plate (833) and the boss round seat (861) and used for enabling the boss round seat (861) to reset downwards, a thrust plate (836) arranged in the force storage cavity (71) in a sliding mode, a plurality of pull rods (835) fixedly arranged on the thrust plate (836), a seventh spring (831) fixedly arranged on the thrust plate (836), and a third rope (832) fixedly connected to a second telescopic rod (65) and the boss round seat (861) of the ventilation structure (8); a sealing plate is arranged on the thrust plate (836); the sealing plate is positioned below the through hole and used for sealing the through hole; the method comprises the following specific steps: chlorine enters the power accumulating cavity (71) and then is blown on the thrust plate (836), the thrust plate (836) is pressurized to compress the pull rod (835), so that the thrust plate (836) is driven to move, the thrust plate (836) and the sealing plate block the through hole originally, the through hole is not blocked any more after the thrust plate (836) moves, so that chlorine can pass through the through hole, the pull rod (835) is driven to move by the movement of the thrust plate (836), and the pull rod (835) pulls the lifting pipe (86) to move upwards through the third rope (832); the thrust plate (836) is arranged in the power storage cavity (71) in a sliding mode, namely, the inclination angle of the thrust plate (836) cannot be made, so that a plurality of through holes can be opened simultaneously, namely, the time synchronization of opening and closing of a plurality of blocking blocks (84) is realized, the control is better performed on the thrust plate, chlorine can be synchronously introduced and stopped, the accuracy of chlorine introduction is improved, then, when the thrust plate (836) is reset, chlorine gas exists in the vent pipe (85), then, the vent pipe (85) is in contact with a cavity behind the thrust plate (836), namely, a light body where the seventh spring (831) is located is reached, and therefore, the chlorine gas cannot reach the seventh spring (831) through the arrangement of the sealing plate, and the chlorine gas is better utilized.

3. The process for preparing 2, 4-dinitro-6-chloroaniline by the sulfuric acid method according to claim 1, which is characterized in that: the speed-adapting structure (6) comprises a rotating ring (61) fixedly connected to the stirring rotating shaft (4), a latch (62) fixedly arranged on the rotating ring (61), a first partition plate fixedly arranged in the stirring barrel (1) and used for separating the speed-adapting structure (6) from the control structure (5), a third support plate (67) fixedly arranged on the first partition plate, a ninth spring (66) fixedly connected to the third support plate (67), a second support plate (63) fixedly connected to the ninth spring (66), a tooth socket (64) arranged on the second support plate (63) and used for being matched with the latch (62), a second telescopic rod (65) arranged between the third support plate (67) and the second support plate (63), and a first guide frame (68) fixedly connected to the second support plate (63) and the control structure (5); the method comprises the following specific steps: the stirring rotating shaft (4) can drive the rotating ring (61) to rotate, then the rotating ring (61) drives the second supporting plate (63) to move through the latch (62) and the tooth groove (64), thereby driving the second supporting plate (63) to move away from the third supporting plate (67), then the second telescopic rod (65) is stretched, then the latch (62) on the rotating ring (61) is less, therefore, the latch (62) can be quickly separated from the tooth socket (64), then the second supporting plate (63) can be reset under the action of the second telescopic rod (65), and the latch (62) can be matched with the tooth socket (64) when the second telescopic rod (65) does not drive the second supporting plate (63) to be reset, thereby moving the second support plate (63) and thus causing the second support plate (63) to reciprocate under the guidance of the ninth spring (66).

4. The process for preparing 2, 4-dinitro-6-chloroaniline by the sulfuric acid method according to claim 3, which is characterized in that: the control structure (5) comprises a second connecting rod (51) hinged to the first guide frame (68), a limiting component (52) connected to the first guide frame (68), a second lifting ring (53) arranged on the stirring rotating shaft (4) in a sliding manner and connected to the stirring adjusting structure (9), a control structure (5) discharging barrel (31) fixedly connected to the second lifting ring (53) and matched with the limiting component (52), and a control block (56) connected to the limiting component (52), the device comprises a second guide rod (561) fixedly arranged on two sides of a control block (56), a third telescopic rod (563) fixedly connected to the control block (56) and the inner wall of a stirring barrel (1), a tenth spring (562) arranged between the control block (56) and the inner wall of the stirring barrel (1) and used for resetting the control block (56), a resetting component (54) connected to the second guide rod (561), and a second control component (55) connected to the second guide rod (561); the limiting assembly (52) comprises a fourth supporting plate (521) hinged to the second connecting rod (51), a third connecting rod (522) hinged to the fourth supporting plate (521), a fifth supporting plate (523) hinged to the third connecting rod (522), a limiting plate (524) fixedly connected to the fifth supporting plate (523) and not in contact with the stirring rotating shaft (4), a second partition plate fixedly arranged on the inner wall of the stirring barrel (1) and used for separating the control structure (5) from the stirred solution, a guide post (525) fixedly arranged on the second partition plate and used for guiding the limiting plate (524), and an anti-falling plate (526) fixedly arranged above the guide post (525) and used for limiting the limiting plate (524); the stirring adjusting structure (9) comprises a pressing rod (97) fixedly arranged below the second lifting ring (53), a rotating block (98) fixedly connected to the stirring rotating shaft (4) and rotatably arranged in the second partition plate, a first lifting ring (91) fixedly connected to the pressing rod (97), a fixing rod (92) fixedly connected to the first lifting ring (91), a first hinging block (93) fixedly connected to the fixing rod (92), a first connecting rod (94) hinged to the first hinging block (93), a second hinging block (95) hinged to the first connecting rod (94), an adjusting rotating shaft (96) rotatably connected to the stirring rotating shaft (4) and fixedly connected to the second hinging block (95) and the stirring plate (7), and a first spring (971) arranged between the rotating block (98) and the control structure (5); the pressure lever (97) is slidably connected to the rotating block (98); the method comprises the following specific steps: the tooth socket (64) moves to drive the ventilation structure (8) of the control structure (5) to move, then the ventilation structure (8) of the control structure (5) can drive the two fourth supporting plates (521) to approach each other through the second connecting rod (51), then the fourth supporting plates (521) can drive the control block (56) to move in opposite directions, then the control block (56) moves to press the material discharge barrel (31) of the control structure (5) to move downwards, then the second lifting ring (53) can drive the stirring plate (7) to adjust the angle through the stirring adjusting structure (9), then the fourth supporting plates (521) move in opposite directions and also drive the fifth supporting plate (523) to move downwards through the third connecting rod (522), then the fifth supporting plate (522) can drive the limiting plate (524) to move downwards, and then the limiting plate (524) and the guide column (525) are in interference fit, thereby limiting plate (524) can't reset by oneself after the downstream, thereby limiting plate (524) can block the motion of second lift ring (53), make the biggest distance of second lift ring (53) upward movement receive the restriction, second lift ring (53) up-and-down reciprocating motion can drive depression bar (97) up-and-down reciprocating motion, later rotatory piece (98) are used for leading depression bar (97), later depression bar (97) can drive first lift ring (91) downstream, later first lift ring (91) drive first articulated piece (93) downstream through dead lever (92), later first articulated piece (93) drive first connecting rod (94) motion, first connecting rod (94) drive second articulated piece (95) and move, later second articulated piece (95) can carry out the rotation round regulation pivot (96), just also make the angle of stirring board (7) change, so that the downward movement of the second lifting ring (53) changes the angle of the stirring plate (7).

5. The process for preparing 2, 4-dinitro-6-chloroaniline by the sulfuric acid method according to claim 4, which is characterized in that: the resetting assembly (54) comprises a matching rod piece (541) fixedly connected to the second guide rod (561), a second guide frame (542) fixedly connected to the matching rod piece (541), a fourth guide rod (543) fixedly connected to the second guide frame (542), a third guide frame (544) fixedly connected to the fourth guide rod (543), a fifth guide rod (545) fixedly connected to the third guide frame (544), an inflator (546) connected to the fifth guide rod (545), an expansion belt (547) fixedly arranged on the second partition plate and connected to the inflator (546), and a resetting pipe (548) fixedly connected to the expansion belt (547) and the limiting plate (524); the control structure (5) further comprises a clamping assembly (57) for clamping the reset tube (548); the method comprises the following specific steps: the control block (56) moves to drive the second guide rod (561), the second guide rod (561) drives the matching rod piece (541) to move, then the matching rod piece (541) drives the second guide frame (542) to move, then the second guide frame (542) drives the fourth guide rod (543) to move, the fourth guide rod (543) drives the third guide frame (544) to move, the third guide frame (544) drives the fifth guide rod (545) to move, then the fifth guide rod (545) is pressed, namely the inflator (546) is inflated into the expansion belt (547), then the expansion belt (547) is expanded, then the clamping assembly (57) clamps the reset pipe (548) so that air in the expansion belt (547) cannot be blown out from the reset pipe (548), then the control block (56) reciprocates, namely the fifth guide rod (545) reciprocates, the inflation is performed to the inside of the expansion belt (547) by reciprocating the inflator (546).

6. The process for preparing 2, 4-dinitro-6-chloroaniline by the sulfuric acid method according to claim 5, which is characterized in that: the clamping assembly (57) comprises a sloping block (571) connected to the second control assembly (55), a tenth guide rod (574) fixedly arranged on the second partition plate, two clamping plates (575) slidably arranged on the tenth guide rod (574), fourth connecting rods (576) hinged to the two clamping plates (575), a matching plate (577) hinged to the two fourth connecting rods (576), a twelfth spring (578) fixedly arranged between the two fourth connecting rods (576), a ninth guide rod (573) fixedly arranged above the matching plate (577), and a lifting block (572) fixedly arranged above the ninth guide rod (573) and matched with the sloping block (571); the method comprises the following specific steps: the twelfth spring (578) normally pushes the two clamping plates (575) to move towards two sides, so that the two clamping plates (575) have a movement tendency towards two sides, then the lifting block (572) has a movement tendency towards a downward movement, then when the stirring rotating shaft (4) is static, the control block (56) is not in contact with the second guide rod (561), then the control block (56) is in a starting position, at the moment, the control block (56) does not drive the inclined block (571) to move through the second control component (55), then once the control block (56) starts to move, the second control component (55) is driven to move, then the inclined block (571) drives the lifting block (572) to move upwards, then the ninth guide rod (573) is driven to move upwards, and then the two clamping plates (575) are clamped together through the matching plate (577) and the fourth connecting rod (576), the reset tube (548) is clamped, and after the control block (56) is reset to the initial position, the clamping plate (575) is moved to two sides, so that the reset tube (548) is not clamped any more.

7. The process for preparing 2, 4-dinitro-6-chloroaniline by the sulfuric acid method according to claim 6, which is characterized in that: the second control assembly (55) comprises a sixth supporting plate (554) fixedly arranged on the second partition plate, an eleventh spring (553) in sliding connection with the sixth supporting plate (554), a reset plate (551) fixedly connected with the eleventh spring (553) and matched with the second guide rod (561), the eleventh spring (553) arranged between the reset plate (551) and the sixth supporting plate (554), a fourth guide frame (555) fixedly connected with the sixth guide rod (552), a seventh guide rod (556) fixedly arranged on the second partition plate, an eighth guide rod (557) in sliding connection with the seventh guide rod (556) and fixedly connected with the fourth guide frame (555), and a fifth guide frame (558) fixedly arranged on the second partition plate and used for guiding the eighth guide rod (557); the eighth guide rod (557) is fixedly connected to the inclined block (571); the elastic force of the sixth guide rod (552) is greater than the elastic force of the twelfth spring (578); an elastic force of the tenth spring (562) is greater than an elastic force of the sixth guide rod (552); the method comprises the specific steps that the second guide rod (561) returns to the original position and abuts against the reset plate (551), then the reset plate (551) is pressed to drive the sixth guide rod (552) to move, then the sixth guide rod (552) drives the fourth guide frame (555) to move, the sixth guide rod (552) slides on the sixth support plate (554), the fourth guide frame (555) drives the eighth guide rod (557) to move, the seventh guide rod (556) guides the eighth guide rod (557), then the eighth guide rod (557) drives the inclined block (571) to stir the rotating shaft (4) to move, then the control block (56) moves to enable the second guide rod (561) to move, then the second guide rod (561) does not abut against the reset plate (551), then the reset plate (551) resets under the action of the eleventh spring (553), and accordingly the reset plate (551) drives the sixth guide rod (552) to move, and then the eighth guide rod (557) is driven to move by the fourth guide frame (555), so that the inclined block (571) can be inserted into the lifting block (572) to control the reset tube (548).

8. The process for preparing 2, 4-dinitro-6-chloroaniline by the sulfuric acid method according to claim 1, which is characterized in that: the stirring adjusting structure (9) further comprises guide rings (99) which are fixedly arranged on the pressure lever (97) and are positioned at the upper end and the lower end of the first lifting ring (91); the upper end and the lower end of the first lifting ring (91) at the uppermost part and the lowermost part are not provided with a guide ring (99); the uppermost and lowermost first lifting rings (91) are fixedly connected to the pressure rod (97), and the first lifting ring (91) at the middle position is slidably connected to the pressure rod (97); a gap is reserved between the guide ring (99) and the first lifting ring (91); the gaps between the middle two guide rings (99) and the first lifting ring (91) are different; the first lifting ring (91) is driven to move up and down by the up-and-down reciprocating motion of the pressure lever (97), namely the stirring plate (7) can rotate, when the first lifting ring (91) is driven to move up and down by the two guide rings (99) in the middle, the distance between the first lifting ring (91) and the first lifting ring (91) can be different due to the gaps between the guide rings (99) and the first lifting ring (91) and the sizes of the gaps, so that the up-and-down reciprocating motion distances of the first lifting ring (91) are different, the rotating angles of the stirring plate (7) can be different, namely the two rotating angles in the middle of the four stirring plates (7) are different and the upper part and the lower part are the same, the stirring plates (7) can be stirred at different angles, the solution in the stirring barrel (1) can be stirred better, chlorine gas can be sprayed to different positions, the chlorination effect is further increased, and the uniformity of raw material mixing is increased, thereby improving the quality of the product.

9. The process for preparing 2, 4-dinitro-6-chloroaniline by the sulfuric acid method according to claim 1, which is characterized in that: the raw material in the stirring barrel 1 is sulfuric acid as a solvent; the concentration of the sulfuric acid is 10-90%.