CN110605069B - Chlorination process of 2, 4-dinitroaniline - Google Patents
Chlorination process of 2, 4-dinitroaniline Download PDFInfo
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- CN110605069B CN110605069B CN201910895639.3A CN201910895639A CN110605069B CN 110605069 B CN110605069 B CN 110605069B CN 201910895639 A CN201910895639 A CN 201910895639A CN 110605069 B CN110605069 B CN 110605069B
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- dinitroaniline
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- sodium chlorate
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J4/00—Feed or outlet devices; Feed or outlet control devices
- B01J4/001—Feed or outlet devices as such, e.g. feeding tubes
- B01J4/007—Feed or outlet devices as such, e.g. feeding tubes provided with moving parts
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J4/00—Feed or outlet devices; Feed or outlet control devices
- B01J4/02—Feed or outlet devices; Feed or outlet control devices for feeding measured, i.e. prescribed quantities of reagents
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C201/00—Preparation of esters of nitric or nitrous acid or of compounds containing nitro or nitroso groups bound to a carbon skeleton
- C07C201/06—Preparation of nitro compounds
- C07C201/12—Preparation of nitro compounds by reactions not involving the formation of nitro groups
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2204/00—Aspects relating to feed or outlet devices; Regulating devices for feed or outlet devices
- B01J2204/002—Aspects relating to feed or outlet devices; Regulating devices for feed or outlet devices the feeding side being of particular interest
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Abstract
The invention discloses a chlorination process of 2, 4-dinitroaniline, which comprises the following specific steps: adding lignosulfonate into 2, 4-dinitroaniline, and then putting the mixture into water to enable the mixture to be suspended in the water; adding hydrochloric acid into a stirring barrel, then adding the 2, 4-dinitroaniline suspension and sodium chlorate into the stirring barrel simultaneously to react to remove excessive chlorine, adding sodium bisulfate into the reactant to decompose residual chlorine, filtering, washing to be neutral, and drying to obtain the product.
Description
Technical Field
The invention belongs to the technical field of chemical material processing, and particularly relates to a chlorination process of 2, 4-dinitroaniline.
Background
The molecular formula of the 6-chloro-2, 4-dinitroaniline is C6H4BrN304, the molecular weight is 26203, and the melting point is 153-154 ℃. Is easy to sublimate. Easily dissolved in hot water and hot acetone, and dissolved in hot acetic acid. Can be used as intermediate for producing indigoid dye and some acid dye. Can make the dye itself bright and improve the colorability and fastness of the dye. The 6-chloro-2, 4-dinitroaniline is a fine chemical intermediate with development potential.
In the preparation reaction process of 6-chloro-2, 4-dinitroaniline, 2, 4-dinitroaniline and other reactants need to be added into a stirring barrel at the same time, however, the existing mixing and feeding device needs workers to manually put different raw materials into a container and stir the raw materials until the raw materials are uniformly mixed, so that the feeding amount cannot be well controlled, and the operation of the workers is troublesome.
Disclosure of Invention
The invention provides a chlorination process of 2, 4-dinitroaniline, aiming at overcoming the defects of the prior art.
In order to achieve the purpose, the invention adopts the following technical scheme: a chlorination process of 2, 4-dinitroaniline comprises the following specific steps: adding lignosulfonate into 2, 4-dinitroaniline, and then putting the mixture into water to enable the mixture to be suspended in the water; adding hydrochloric acid into a stirring barrel, then simultaneously adding 2, 4-dinitroaniline suspension and sodium chlorate into the stirring barrel to react to remove excessive chlorine, adding sodium bisulfate into reactants to decompose residual chlorine, filtering, washing to be neutral, and drying to obtain a product;
a cover plate is arranged at the top of the stirring barrel, a heating block is arranged in the stirring barrel, a plurality of storage barrels are arranged on the cover plate, stirring assemblies are arranged in the stirring barrel, a feeding hole is formed in the side wall of each storage barrel, through holes are formed in the bottoms of the storage barrels, and the storage barrels are communicated with the stirring barrel through the through holes; a push plate is arranged in the material storage barrel, a driving motor for driving the push plate to move up and down is arranged on the cover plate, and when the driving motor drives the push plate to move, the stirring assembly rotates in the stirring barrel; the 2, 4-dinitroaniline suspension and the sodium chlorate are respectively placed in different storage barrels, quantitative 2, 4-dinitroaniline suspension and sodium chlorate are respectively added into the storage barrels according to the actually required medicament amount, a driving motor drives a push plate to move downwards, the 2, 4-dinitroaniline suspension and the sodium chlorate are pushed down from a through hole, the 2, 4-dinitroaniline suspension and the sodium chlorate are simultaneously added into a stirring barrel, a stirring component rotates to stir the solution in the stirring barrel, and the 2, 4-dinitroaniline suspension and the sodium chlorate react to obtain the 6-chloro-2, 4-dinitroaniline.
By adding the 2, 4-dinitroaniline suspension and the sodium chlorate into the storage barrel, the 2, 4-dinitroaniline suspension and the sodium chlorate are automatically pushed to move downwards when the driving motor drives the push plate to move downwards, so that the 2, 4-dinitroaniline suspension and the sodium chlorate are always added into the stirring barrel according to the budget proportion, the reaction operation of the 2, 4-dinitroaniline suspension and the sodium chlorate is completed, the adding amount precision of the 2, 4-dinitroaniline suspension and the sodium chlorate is ensured, manual operation is not needed, and the operation difficulty of workers is reduced; the stirring assembly is driven to rotate while the feeding operation in the stirring barrel is finished through the driving motor, so that reactants are quickly mixed after being added into the stirring barrel, the reaction rate of the reactants is increased, and the preparation efficiency of the 6-chloro-2, 4-dinitroaniline is improved; solution in can directly push the agitator under the push pedal effect in the storage vat, reduce the residue of reactant in the storage vat, make to add the big reactant volume more accurate, it is extravagant to reduce the reactant.
The hydrochloric acid concentration is 32%.
And adding the 2, 4-dinitroaniline suspension and sodium chlorate into a stirring barrel, stirring for 30min, and driving out the excess chlorine after 30 min.
The 2, 4-dinitroaniline suspension and the sodium chlorate are added and stirred while the temperature of the hydrochloric acid in the stirring barrel is 25 ℃.
The ratio of the 2, 4-dinitroaniline to the lignosulfonate to the water is 366: 1: 440.
the side wall of the material storage barrel is provided with a feeding pipe matched with the feeding port, a valve assembly is arranged in the feeding pipe, the valve assembly comprises a sealing plate which is rotatably connected to the inner wall of the feeding pipe, a sealing block which is arranged on the inner wall of the feeding pipe and a supporting block which is arranged on one side of the sealing plate, the side wall of the feeding pipe is provided with a first movable groove, a supporting spring is arranged in the first movable groove, and the supporting block is arranged at the bottom end of the supporting spring; the sealing block is arranged on the other side of the sealing plate, and a through groove is formed in the sealing block; a push rod assembly matched with the sealing plate is arranged on the feeding pipe; after the use amounts of the 2, 4-dinitroaniline suspension and the sodium chlorate are calculated, the push rod assembly is pushed to enable the push rod assembly to push the sealing plate to rotate around the connecting point, the sealing plate pushes the supporting block to move towards the first movable groove, the sealing plate is separated from the sealing block, a gap is formed between the sealing plate and the sealing block, sodium chloride solution or the 2, 4-dinitroaniline is poured into the storage tank from the feeding pipe opening, and the sodium chloride solution or the 2, 4-dinitroaniline is added into the storage tank for reaction; after liquid adding is finished, the supporting spring pushes the supporting block to extend out of the first movable groove, so that the supporting block pushes the sealing plate to rotate around the connecting point, the sealing plate is in contact with the sealing block to seal the feeding pipe, and the whole liquid adding operation is finished; the reaction liquid enters the storage vat from the liquid inlet pipe and enters the storage vat along the inner wall of the liquid inlet pipe, and the liquid inlet pipe plays a guiding role on the reaction liquid so as to complete the charging operation of the storage vat; part of reaction liquid in the liquid inlet pipe passes through the sealing block through the through groove, so that the sealing block is prevented from blocking the reaction liquid to cause the retention of the reaction liquid, and the waste of the reaction liquid is reduced; under the mutual matching of the supporting block and the sealing block, a supporting force is provided for the sealing plate, so that the sealing plate and the sealing block form good matching, an effective sealing effect is achieved on the liquid inlet pipe, and the reaction liquid in the storage barrel is prevented from overflowing from the discharge pipe; when the push pedal promoted reaction liquid down the time of moving, partial reaction liquid enters into the feed tube and extrudees the closing plate in, with the closing plate extrusion on sealed piece, promote the cooperation effect of sealed piece and closing plate, and then promote the sealed effect of closing plate to the feed liquor pipe, avoid extruding reaction liquid from the feed liquor pipe.
A movable cavity is arranged on the cover plate, a second movable groove is formed in the bottom of the movable cavity, a transmission ring is arranged in the second movable groove, an output shaft of the driving motor penetrates through the movable cavity, a first transmission wheel matched with the transmission ring is arranged on the output shaft of the driving motor, a second transmission wheel matched with the transmission ring is arranged in the movable cavity, a third transmission wheel matched with the second transmission wheel is further arranged in the movable cavity, and a fourth transmission wheel matched with the third transmission wheel is arranged on one side of the third transmission wheel; a screw rod is arranged in the storage barrel, the push plate is sleeved on the screw rod, the screw rod penetrates through the movable cavity, and a fifth driving wheel matched with the fourth driving wheel is arranged at the bottom of the screw rod; after the 2, 4-dinitroaniline suspension and the sodium chlorate are filled into the storage barrel, a driving motor works to drive a first driving wheel to rotate, a driving ring rotates to drive a stirring assembly to rotate, the driving ring drives all driving wheels to rotate simultaneously, a screw rod rotates relative to a push plate, the push plate moves downwards along the screw rod to push the solution in the storage barrel downwards, and the 2, 4-dinitroaniline suspension and the sodium chlorate are added into the stirring barrel to react to prepare 6-chloro-2, 4-dinitroaniline; the power of the driving motor is stably transmitted to the lead screw under the coordination of the driving wheel, so that the lead screw drives the push plate to move in the storage barrel, and the reaction liquid in the storage barrel is pushed down under the action of the push plate, thereby completing the automatic feeding operation of the reaction liquid; under the mutual cooperation of the screw rod and the push plate, the descending distance of the push plate is controlled, so that the push plate slowly descends under the action of the driving motor, and the reaction liquid is slowly and quantitatively added into the stirring barrel, so that the sodium chloride solution or the 2, 4-dinitroaniline can fully react, and the reaction effect of reactants is improved.
The invention has the following advantages: when the driving motor drives the push plate to move downwards, the 2, 4-dinitroaniline suspension and the sodium chlorate are automatically pushed to move downwards, so that the 2, 4-dinitroaniline suspension and the sodium chlorate are added into the stirring barrel according to a preset proportion all the time, the reaction operation of the 2, 4-dinitroaniline suspension and the sodium chlorate is completed, the adding amount precision of the 2, 4-dinitroaniline suspension and the sodium chlorate is ensured, manual operation is not needed, and the operation difficulty of workers is reduced.
Drawings
FIG. 1 is a schematic view of the structure of the mixing tank of the present invention.
Fig. 2 is a first schematic cross-sectional view of the mixing tank of the present invention.
Fig. 3 is an enlarged view of a portion a in fig. 2.
Fig. 4 is an enlarged view of fig. 2 at B.
Fig. 5 is an enlarged view of fig. 2 at C.
Fig. 6 is an enlarged view of fig. 2 at D.
Fig. 7 is an enlarged view of fig. 2 at E.
Fig. 8 is an enlarged view of fig. 2 at F.
FIG. 9 is a second schematic cross-sectional view of the mixing tank of the present invention.
Fig. 10 is an enlarged view at G in fig. 9.
Fig. 11 is a third schematic sectional view of the mixing tank of the present invention.
Fig. 12 is an enlarged view of fig. 11 at H.
Detailed Description
A chlorination process of 2, 4-dinitroaniline comprises the following specific steps: adding lignosulfonate into 2, 4-dinitroaniline, and then putting the mixture into water to enable the mixture to be suspended in the water; adding hydrochloric acid into a stirring barrel, then simultaneously adding 2, 4-dinitroaniline suspension and sodium chlorate into the stirring barrel to react to remove excessive chlorine, adding sodium bisulfate into reactants to decompose residual chlorine, filtering, washing to be neutral, and drying to obtain a product; the concentration of the hydrochloric acid is 32%; adding the 2, 4-dinitroaniline suspension and sodium chlorate into a stirring barrel, stirring for 30min, and driving out excessive chlorine after 30 min; adding the 2, 4-dinitroaniline suspension and sodium chlorate into the stirring tank, and stirring while keeping the temperature of hydrochloric acid in the stirring tank at 25 ℃; the ratio of the 2, 4-dinitroaniline to the lignosulfonate to the water is 366: 1: 440.
as shown in fig. 1-12, a cover plate 2 is arranged at the top of the stirring barrel 1, a heating block is arranged in the stirring barrel 1, a thermometer is further arranged on the side wall of the stirring barrel, and the temperature in the stirring barrel is controlled under the cooperation of the heating block and the thermometer, so that the reaction temperature is controlled in a schematic range, and the normal operation of the reaction is ensured; the cover plate 2 is provided with two storage barrels 21, the stirring component is arranged in the stirring barrel 1, the side wall of each storage barrel 21 is provided with a feeding hole, the bottom of each storage barrel 21 is provided with a through hole, and the storage barrels 21 are communicated with the stirring barrel 1 through the through holes; a push plate 240 is arranged in the storage vat 21, a driving motor 24 for driving the push plate 240 to move up and down is arranged on the cover plate 2, and when the driving motor 24 drives the push plate 240 to move, the stirring assembly rotates in the stirring vat 1; the 2, 4-dinitroaniline suspension and the sodium chlorate are respectively placed in different storage barrels 21, quantitative 2, 4-dinitroaniline suspension and sodium chlorate are respectively added into the storage barrels 21 according to the actually reflected required medicament amount, a driving motor 24 drives a push plate 240 to move downwards, the 2, 4-dinitroaniline suspension and the sodium chlorate are pushed down from the through holes, the 2, 4-dinitroaniline suspension and the sodium chlorate are simultaneously added into a stirring barrel 1, and a stirring assembly rotates to stir the solution in the stirring barrel 1, so that the 2, 4-dinitroaniline suspension and the sodium chlorate react to obtain the 6-chloro-2, 4-dinitroaniline.
By adding the 2, 4-dinitroaniline suspension and the sodium chlorate into the storage barrel, the 2, 4-dinitroaniline suspension and the sodium chlorate are automatically pushed to move downwards when the driving motor drives the push plate to move downwards, so that the 2, 4-dinitroaniline suspension and the sodium chlorate are always added into the stirring barrel according to the budget proportion, the reaction operation of the 2, 4-dinitroaniline suspension and the sodium chlorate is completed, the adding amount precision of the 2, 4-dinitroaniline suspension and the sodium chlorate is ensured, manual operation is not needed, and the operation difficulty of workers is reduced; the stirring assembly is driven to rotate while the feeding operation in the stirring barrel is finished through the driving motor, so that reactants are quickly mixed after being added into the stirring barrel, the reaction rate of the reactants is increased, and the preparation efficiency of the 6-chloro-2, 4-dinitroaniline is improved; solution in can directly push the agitator under the push pedal effect in the storage vat, reduce the residue of reactant in the storage vat, make to add the big reactant volume more accurate, it is extravagant to reduce the reactant.
The side wall of the storage vat 21 is provided with a feeding pipe 22 matched with the feeding hole, the feeding pipe 22 is internally provided with a valve assembly, the valve assembly comprises a sealing plate 221 which is rotatably connected to the inner wall of the feeding pipe 22, a sealing block 223 which is arranged on the inner wall of the feeding pipe 22 and a supporting block 222 which is arranged on one side of the sealing plate 221, the side wall of the feeding pipe 22 is provided with a first movable groove, a supporting spring is arranged in the first movable groove, and the supporting block 222 is arranged at the bottom end of the supporting spring; the sealing block 223 is arranged on the other side of the sealing plate 221, and a through groove is formed in the sealing block 223; a push rod assembly matched with the sealing plate 221 is arranged on the feeding pipe 22; after the usage amount of the 2, 4-dinitroaniline suspension and the sodium chlorate is calculated, the push rod assembly is pushed to enable the push rod assembly to push the sealing plate 221 to rotate around the connection point, the sealing plate 221 pushes the supporting block 223 to move towards the first movable groove, the sealing plate 221 is separated from the sealing block 223 in contact, a gap is formed between the sealing plate 221 and the sealing block 223, sodium chloride solution or 2, 4-dinitroaniline is poured from the inlet of the feeding pipe 22, and the sodium chloride solution or the 2, 4-dinitroaniline is added into the storage barrel 21 for reaction; after liquid adding is finished, the supporting spring pushes the supporting block 222 to extend out of the first movable groove, so that the supporting block 222 pushes the sealing plate 221 to rotate around the connecting point, the sealing plate 221 is in contact with the sealing block 223 to seal the feeding pipe 22, and the whole liquid adding operation is finished; the reaction liquid enters the storage vat from the liquid inlet pipe and enters the storage vat along the inner wall of the liquid inlet pipe, and the liquid inlet pipe plays a guiding role on the reaction liquid so as to complete the charging operation of the storage vat; part of reaction liquid in the liquid inlet pipe passes through the sealing block through the through groove, so that the sealing block is prevented from blocking the reaction liquid to cause the retention of the reaction liquid, and the waste of the reaction liquid is reduced; under the mutual matching of the supporting block and the sealing block, a supporting force is provided for the sealing plate, so that the sealing plate and the sealing block form good matching, an effective sealing effect is achieved on the liquid inlet pipe, and the reaction liquid in the storage barrel is prevented from overflowing from the discharge pipe; when the push pedal promoted reaction liquid down the time of moving, partial reaction liquid enters into the feed tube and extrudees the closing plate in, with the closing plate extrusion on sealed piece, promote the cooperation effect of sealed piece and closing plate, and then promote the sealed effect of closing plate to the feed liquor pipe, avoid extruding reaction liquid from the feed liquor pipe.
The push rod assembly comprises a lantern ring 224 sleeved on the feeding pipe, a first connecting plate 225 arranged on the lantern ring, a second connecting plate arranged on the first connecting plate and a push rod 226 arranged on the second connecting plate, and a limiting block matched with the lantern ring is arranged on the side wall of the feeding pipe to prevent the lantern ring from being separated from the feeding pipe under the action of the limiting block; when adding reaction liquid in toward the storage vat, promote the lantern ring along the inlet pipe lateral wall, the lantern ring drives the push rod and moves toward the inlet pipe, makes the push rod promote the closing plate around the tie point upset, makes closing plate and sealed piece throw off the contact, and the inlet pipe is in the open mode to in leading-in to the storage vat with reaction liquid, make the automatic filling of reaction liquid in the storage vat to the agitator.
A baffle 227 is arranged at one end of the feeding pipe, a first sliding block is arranged on the baffle, a first sliding groove matched with the first sliding block is arranged at the port of the feeding pipe, a groove matched with the push rod is formed in the baffle, the number of the baffles is two, and the two baffles are matched with each other to seal the feeding pipe; the rubber pads are arranged on the inner walls of the grooves, when the reaction liquid is filled into the storage barrel, the baffle plate is pushed along the first sliding chute to move to the two sides of the feeding pipe, and the feeding pipe is in an open state so as to be convenient for adding the reaction liquid into the storage barrel; after the reaction liquid is filled, the lantern ring is pushed upwards to enable the lantern ring to be contacted with the limiting block, the push rod is pulled out of the feeding pipe and pushes the baffle plate towards the push rod, the push rod is embedded into the groove and fixed under the action of the rubber pad, the push rod is prevented from automatically sliding into the feeding pipe, and the matching effect of the sealing plate and the sealing block is guaranteed; the feeding pipe is closed under the action of the baffle plate, so that impurities are prevented from entering the feeding pipe, the purity of the reaction liquid is guaranteed, and the reaction quality is improved.
A movable cavity is arranged on the cover plate 2, a second movable groove is arranged at the bottom of the movable cavity, a transmission ring 25 is arranged in the second movable groove, an output shaft of the driving motor 24 penetrates through the movable cavity, a first transmission wheel 241 matched with the transmission ring 25 is arranged on the output shaft of the driving motor 24, a second transmission wheel 26 matched with the transmission ring 25 is arranged in the movable cavity, a third transmission wheel 27 matched with the second transmission wheel 26 is further arranged in the movable cavity, and a fourth transmission wheel 281 matched with the third transmission wheel 27 is arranged on one side of the third transmission wheel 27; a screw rod 2301 is arranged in the storage vat 21, the push plate 240 is sleeved on the screw rod 2301, the screw rod 2301 is arranged in the movable cavity in a penetrating manner, and a fifth driving wheel 230 matched with the fourth driving wheel 281 is arranged at the bottom of the screw rod 2301; the inner wall of the storage barrel is provided with a second chute, the side wall of the push plate is provided with a second slide block, and the second slide block and the second chute are matched with each other to limit the push plate, so that the push plate can move up and down along the side wall of the lead screw when the lead screw rotates; after the 2, 4-dinitroaniline suspension and sodium chlorate are filled into the storage barrel 21, a driving motor 24 works to drive a first driving wheel 241 to rotate, a driving ring 25 rotates to drive a stirring component to rotate, meanwhile, the driving ring 25 drives all driving wheels to rotate, so that a screw rod 2301 rotates relative to a push plate 240, the push plate 240 moves downwards along the screw rod 2301 to push the solution in the storage barrel 21 downwards, and the 2, 4-dinitroaniline suspension and the sodium chlorate are added into the stirring barrel 1 to react to prepare 6-chloro-2, 4-dinitroaniline; the power of the driving motor is stably transmitted to the lead screw under the coordination of the driving wheel, so that the lead screw drives the push plate to move in the storage barrel, and the reaction liquid in the storage barrel is pushed down under the action of the push plate, thereby completing the automatic feeding operation of the reaction liquid; under the mutual cooperation of the screw rod and the push plate, the descending distance of the push plate is controlled, so that the push plate slowly descends under the action of the driving motor, and the reaction liquid is slowly and quantitatively added into the stirring barrel, so that the sodium chloride solution or the 2, 4-dinitroaniline can fully react, and the reaction effect of reactants is improved.
A connecting shaft 28 is arranged in the movable cavity, a fourth driving wheel is sleeved on the connecting shaft, a supporting ring 29 is arranged below the fourth driving wheel, an electromagnet is arranged above the fourth driving wheel, and the fourth driving wheel is made of magnetic materials; the connecting shaft has a fixing function on the fourth driving wheel, and the contact area between the fourth driving wheel and the inner wall of the movable cavity is reduced under the action of the support ring, so that the friction force applied to the fourth driving wheel during rotation is reduced, and the power is stably transmitted; when only need drive stirring subassembly during operation, the electro-magnet circular telegram produces magnetic force, makes the up motion of fourth drive wheel under magnetic force, and fourth drive wheel and third drive wheel dislocation make on the power of third drive wheel no longer transmit to the fifth drive wheel, and the storage vat is no longer reinforced in to the agitator tank, and the stirring subassembly is at the agitator internal rotation by oneself.
The stirring assembly comprises a first connecting ring 11 arranged in the stirring barrel and a plurality of stirring rods 111 arranged on the inner wall of the first connecting ring, and taking two stirring rods as an example, a first push block 112 is arranged at the top of the first connecting ring, a second movable groove is communicated with the outer side of the movable cavity, and a second push block 251 matched with the first push block is arranged at the bottom of the transmission ring; after the cover plate covers the stirring barrel, the first push block and the second push block are positioned in the same circumference, when the driving motor drives the driving ring to rotate, the driving ring drives the second push block to rotate, the second push block rotates for a certain distance and then is contacted with the first push block, the second push block is pushed to move under the action of the first push block, so that the second push block drives the first connecting ring to rotate, the stirring rod rotates in the stirring barrel to stir solution, the reaction liquid is fully contacted and then reacts, and the reaction speed of the reaction liquid is improved; under the mutual cooperation of the first pushing block and the second pushing block, the cover plate can be easily covered on the stirring barrel, and the first pushing block and the second pushing block are directly contacted after the transmission ring rotates, so that the power on the transmission ring is transmitted to the first connecting ring, and reliable power is provided for the rotation of the stirring rod; after the reaction is accomplished, open the apron, can directly take out first connecting ring from the agitator to do the clearance to first connecting ring and agitator, reduce the clearance degree of difficulty of agitator.
Storage vat top is equipped with top cap 23, the storage vat top is equipped with the second go-between, the top cap bottom be equipped with second go-between matched with third go-between, the second go-between passes through the screw with the third go-between and links to each other, after the agitator finishes using, rotate the top cap, turn the top cap from the storage vat top, driving motor drive lead screw rotates, make the push pedal up move, make the push pedal deviate from the lead screw, so that take out the push pedal from the storage vat, thereby can be convenient do the clearance to storage vat inner wall and push pedal, avoid remaining chemical composition in the storage vat to cause the influence to the follow-up use of agitator.
A connecting pipe 210 penetrates through the through hole, a sealing film 2101 is arranged at the top of the connecting pipe, the sealing film is a plastic film, a supporting plate is arranged at the bottom of the sealing film, and the supporting plate is made of a metal sheet and provides supporting force for the sealing film so that the sealing film is in a horizontal state; four sealing films are arranged in one connecting pipe, each sealing film is in a quarter-circle shape, and the four sealing films are matched with each other to seal the connecting pipe, so that reaction liquid in the storage barrel is prevented from leaking out of the through hole; when the push pedal moves down and extrudes the reaction liquid in the storage vat, the reaction liquid pushes the sealing membrane to overturn in the connecting pipe, so that the connecting pipe is in an open state, and the reaction liquid in the storage vat falls down from the connecting pipe, so that the reaction liquid is added into the stirring vat to react.
The screw threads in the two storage tanks can be adjusted according to actual conditions, so that the push plates can be lowered by different heights when the screw rods on the left side and the right side rotate for the same number of turns; the diameters of the fifth driving wheels at the bottoms of the screw rods in the two storage barrels can be adjusted, so that the push plates in different storage barrels can be lowered by different distances within the same time, and the adding requirements of different medicaments with different components can be met.
Claims (1)
1. A chlorination process of 2, 4-dinitroaniline is characterized by comprising the following steps: the method comprises the following specific steps: adding lignosulfonate into 2, 4-dinitroaniline, and then putting the mixture into water to enable the mixture to be suspended in the water; adding hydrochloric acid into a stirring barrel, then simultaneously adding 2, 4-dinitroaniline suspension and sodium chlorate into the stirring barrel to react to remove excessive chlorine, adding sodium bisulfate into reactants to decompose residual chlorine, filtering, washing to be neutral, and drying to obtain a product; a cover plate (2) is arranged at the top of the stirring barrel (1), a heating block is arranged in the stirring barrel (1), a plurality of storage barrels (21) are arranged on the cover plate (2), a stirring assembly is arranged in the stirring barrel (1), a feeding hole is formed in the side wall of each storage barrel (21), a through hole is formed in the bottom of each storage barrel (21), and each storage barrel (21) is communicated with the stirring barrel (1) through the through hole; a push plate (240) is arranged in the storage barrel (21), a driving motor (24) for driving the push plate (240) to move up and down is arranged on the cover plate (2), and when the driving motor (24) drives the push plate (240) to move, the stirring assembly rotates in the stirring barrel (1); the 2, 4-dinitroaniline suspension and the sodium chlorate are respectively placed in different storage barrels (21), quantitative 2, 4-dinitroaniline suspension and sodium chlorate are respectively added into the storage barrels (21) according to the actually reflected required medicament amount, a driving motor (24) drives a push plate (240) to move downwards, the 2, 4-dinitroaniline suspension and the sodium chlorate are pushed downwards from a through hole, the 2, 4-dinitroaniline suspension and the sodium chlorate are simultaneously added into a stirring barrel (1), a stirring assembly rotates to stir the solution in the stirring barrel (1), and the 2, 4-dinitroaniline suspension and the sodium chlorate react to obtain 6-chloro-2, 4-dinitroaniline; a movable cavity is arranged on the cover plate (2), a second movable groove is formed in the bottom of the movable cavity, a transmission ring (25) is arranged in the second movable groove, an output shaft of the driving motor (24) penetrates through the movable cavity, a first transmission wheel (241) matched with the transmission ring (25) is arranged on the output shaft of the driving motor (24), a second transmission wheel (26) matched with the transmission ring (25) is arranged in the movable cavity, a third transmission wheel (27) matched with the second transmission wheel (26) is further arranged in the movable cavity, and a fourth transmission wheel (281) matched with the third transmission wheel (27) is arranged on one side of the third transmission wheel (27); a screw rod (2301) is arranged in the storage barrel (21), the push plate (240) is sleeved on the screw rod (2301), the screw rod (2301) penetrates through the movable cavity, and a fifth driving wheel (230) matched with the fourth driving wheel (281) is arranged at the bottom of the screw rod (2301); after the 2, 4-dinitroaniline suspension and sodium chlorate are filled into the storage barrel (21), a driving motor (24) works to drive a first driving wheel (241) to rotate, a driving ring (25) rotates to drive a stirring component to rotate, meanwhile, the driving ring (25) drives all driving wheels to rotate, a screw rod (2301) rotates relative to a push plate (240), the push plate (240) moves downwards along the screw rod (2301), the solution in the storage barrel (21) is pushed downwards, and the 2, 4-dinitroaniline suspension and the sodium chlorate are added into the stirring barrel (1) to react to prepare 6-chloro-2, 4-dinitroaniline;
the concentration of the hydrochloric acid is 32%;
adding the 2, 4-dinitroaniline suspension and sodium chlorate into a stirring barrel, stirring for 30min, and driving out excessive chlorine after 30 min;
adding the 2, 4-dinitroaniline suspension and sodium chlorate into the stirring tank, and stirring while keeping the temperature of hydrochloric acid in the stirring tank at 25 ℃;
the ratio of the 2, 4-dinitroaniline to the lignosulfonate to the water is 366: 1: 440, a step of;
the side wall of the storage barrel (21) is provided with a feeding pipe (22) matched with the feeding hole, a valve assembly is arranged in the feeding pipe (22), the valve assembly comprises a sealing plate (221) rotatably connected to the inner wall of the feeding pipe (22), a sealing block (223) arranged on the inner wall of the feeding pipe (22) and a supporting block (222) arranged on one side of the sealing plate (221), the side wall of the feeding pipe (22) is provided with a first movable groove, a supporting spring is arranged in the first movable groove, and the supporting block (222) is arranged at the bottom end of the supporting spring; the sealing block (223) is arranged on the other side of the sealing plate (221), and a through groove is formed in the sealing block (223); a push rod assembly matched with the sealing plate (221) is arranged on the feeding pipe (22); after the usage amount of the 2, 4-dinitroaniline suspension and the sodium chlorate is calculated, the push rod assembly is pushed to enable the push rod assembly to push the sealing plate (221) to rotate around the connection point, the sealing plate (221) pushes the supporting block (223) to move towards the first movable groove, the sealing plate (221) is separated from the sealing block (223) in contact, a gap is formed between the sealing plate (221) and the sealing block (223), sodium chloride solution or 2, 4-dinitroaniline is poured into the storage barrel (21) from the inlet of the feeding pipe (22), and the sodium chloride solution or the 2, 4-dinitroaniline is added into the storage barrel (21) for reaction; after liquid adding is finished, the supporting spring pushes the supporting block (222) to extend out of the first movable groove, so that the supporting block (222) pushes the sealing plate (221) to rotate around the connecting point, the sealing plate (221) is in contact with the sealing block (223) to seal the feeding pipe (22), and the whole liquid adding operation is finished.
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| CN111440098B (en) * | 2020-05-14 | 2021-03-16 | 绍兴上虞联谊化工有限公司 | Preparation process of sulfonated para-ester serving as dye intermediate |
| CN111672357B (en) * | 2020-06-10 | 2021-05-04 | 浙江圆融科技有限公司 | Preparation equipment and process of efficient nano photocatalyst disinfectant |
| CN111876174A (en) * | 2020-07-31 | 2020-11-03 | 北京高冉帆畅文化有限公司 | Industrial sludge pyrolysis gasification mechanical blast furnace |
| CN112915911B (en) * | 2021-01-26 | 2022-02-22 | 浙江科宝新材料科技有限公司 | Brightener processing method |
| CN113511975A (en) * | 2021-06-25 | 2021-10-19 | 宁夏中盛新科技有限公司 | Safe and environment-friendly preparation process of 2, 4-dinitroaniline |
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Address after: 312300 No. 7 Weisan Road, Shangyu Economic and Technological Development Zone, Hangzhou Bay, Shaoxing City, Zhejiang Province Patentee after: Zhejiang Huixiang New Material Technology Co., Ltd Address before: No.7, Weisan Road, Shangyu economic and Technological Development Zone, Hangzhou Bay Patentee before: ZHEJIANG HUIXIANG CHEMICAL INDUSTRY Co.,Ltd. |