CN113651713B - Synthesis method of high-purity 2-nitro-4-acetamido anisole - Google Patents
Synthesis method of high-purity 2-nitro-4-acetamido anisole Download PDFInfo
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- CN113651713B CN113651713B CN202110952926.0A CN202110952926A CN113651713B CN 113651713 B CN113651713 B CN 113651713B CN 202110952926 A CN202110952926 A CN 202110952926A CN 113651713 B CN113651713 B CN 113651713B
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- MYIUWCZXTNZSMN-UHFFFAOYSA-N n-(4-methoxy-3-nitrophenyl)acetamide Chemical compound COC1=CC=C(NC(C)=O)C=C1[N+]([O-])=O MYIUWCZXTNZSMN-UHFFFAOYSA-N 0.000 title claims description 16
- 238000001308 synthesis method Methods 0.000 title claims description 4
- 238000006243 chemical reaction Methods 0.000 claims abstract description 178
- 238000004140 cleaning Methods 0.000 claims abstract description 110
- 238000000034 method Methods 0.000 claims abstract description 57
- 238000003756 stirring Methods 0.000 claims abstract description 54
- 239000002994 raw material Substances 0.000 claims abstract description 43
- RZVAJINKPMORJF-UHFFFAOYSA-N Acetaminophen Chemical compound CC(=O)NC1=CC=C(O)C=C1 RZVAJINKPMORJF-UHFFFAOYSA-N 0.000 claims abstract description 38
- 239000003054 catalyst Substances 0.000 claims abstract description 32
- 238000001125 extrusion Methods 0.000 claims abstract description 31
- 229960005489 paracetamol Drugs 0.000 claims abstract description 28
- 238000007599 discharging Methods 0.000 claims abstract description 17
- 230000002194 synthesizing effect Effects 0.000 claims abstract description 14
- 239000003444 phase transfer catalyst Substances 0.000 claims abstract description 10
- 239000012295 chemical reaction liquid Substances 0.000 claims abstract description 9
- 238000000605 extraction Methods 0.000 claims abstract description 8
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 4
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 4
- 239000007789 gas Substances 0.000 claims description 51
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 49
- 239000011261 inert gas Substances 0.000 claims description 41
- 238000003860 storage Methods 0.000 claims description 35
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 32
- 230000009467 reduction Effects 0.000 claims description 21
- 230000005540 biological transmission Effects 0.000 claims description 19
- 230000033001 locomotion Effects 0.000 claims description 16
- 230000009471 action Effects 0.000 claims description 13
- NHGXDBSUJJNIRV-UHFFFAOYSA-M tetrabutylammonium chloride Chemical compound [Cl-].CCCC[N+](CCCC)(CCCC)CCCC NHGXDBSUJJNIRV-UHFFFAOYSA-M 0.000 claims description 8
- 239000000376 reactant Substances 0.000 claims description 4
- 239000002184 metal Substances 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 230000000903 blocking effect Effects 0.000 claims description 2
- 230000003116 impacting effect Effects 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 238000006722 reduction reaction Methods 0.000 description 16
- 239000000047 product Substances 0.000 description 15
- 230000008569 process Effects 0.000 description 11
- 238000004128 high performance liquid chromatography Methods 0.000 description 9
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 7
- 238000006396 nitration reaction Methods 0.000 description 7
- 229910017604 nitric acid Inorganic materials 0.000 description 7
- -1 nitroxyl cations Chemical class 0.000 description 7
- 230000036632 reaction speed Effects 0.000 description 7
- 238000005070 sampling Methods 0.000 description 7
- 238000010586 diagram Methods 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 238000006555 catalytic reaction Methods 0.000 description 5
- 238000007086 side reaction Methods 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- 238000006277 sulfonation reaction Methods 0.000 description 5
- 239000002253 acid Substances 0.000 description 4
- 239000006227 byproduct Substances 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- 238000001914 filtration Methods 0.000 description 4
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 4
- 238000009827 uniform distribution Methods 0.000 description 4
- 239000002699 waste material Substances 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 238000007664 blowing Methods 0.000 description 3
- 238000007865 diluting Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000012065 filter cake Substances 0.000 description 3
- 238000005984 hydrogenation reaction Methods 0.000 description 3
- 239000005457 ice water Substances 0.000 description 3
- 239000012452 mother liquor Substances 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- CZGCEKJOLUNIFY-UHFFFAOYSA-N 4-Chloronitrobenzene Chemical compound [O-][N+](=O)C1=CC=C(Cl)C=C1 CZGCEKJOLUNIFY-UHFFFAOYSA-N 0.000 description 2
- FGOFNVXHDGQVBG-UHFFFAOYSA-N N-(2-methoxyphenyl)acetamide Chemical compound COC1=CC=CC=C1NC(C)=O FGOFNVXHDGQVBG-UHFFFAOYSA-N 0.000 description 2
- 238000000429 assembly Methods 0.000 description 2
- 230000000712 assembly Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000007795 chemical reaction product Substances 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 150000002357 guanidines Chemical class 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 238000004537 pulping Methods 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 125000000218 acetic acid group Chemical group C(C)(=O)* 0.000 description 1
- 230000021736 acetylation Effects 0.000 description 1
- 238000006640 acetylation reaction Methods 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 239000000987 azo dye Substances 0.000 description 1
- 239000012267 brine Substances 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000007810 chemical reaction solvent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- NDEMNVPZDAFUKN-UHFFFAOYSA-N guanidine;nitric acid Chemical compound NC(N)=N.O[N+]([O-])=O.O[N+]([O-])=O NDEMNVPZDAFUKN-UHFFFAOYSA-N 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000006198 methoxylation reaction Methods 0.000 description 1
- SJWQCBCAGCEWCV-UHFFFAOYSA-N n-(3-amino-4-methoxyphenyl)acetamide Chemical compound COC1=CC=C(NC(C)=O)C=C1N SJWQCBCAGCEWCV-UHFFFAOYSA-N 0.000 description 1
- QGEGALJODPBPGR-UHFFFAOYSA-N n-(4-methoxy-2-nitrophenyl)acetamide Chemical compound COC1=CC=C(NC(C)=O)C([N+]([O-])=O)=C1 QGEGALJODPBPGR-UHFFFAOYSA-N 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 230000000802 nitrating effect Effects 0.000 description 1
- 125000000449 nitro group Chemical group [O-][N+](*)=O 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 150000003242 quaternary ammonium salts Chemical class 0.000 description 1
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 125000001273 sulfonato group Chemical group [O-]S(*)(=O)=O 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C231/00—Preparation of carboxylic acid amides
- C07C231/12—Preparation of carboxylic acid amides by reactions not involving the formation of carboxamide groups
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0053—Details of the reactor
-
- 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
-
- 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
- B01J19/1868—Stationary reactors having moving elements inside resulting in a loop-type movement
- B01J19/1881—Stationary reactors having moving elements inside resulting in a loop-type movement externally, i.e. the mixture leaving the vessel and subsequently re-entering it
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a method for synthesizing high-purity 2-nitro-4 acetaminophen, which uses a production line to synthesize 2-nitro-4 acetaminophen; the assembly line comprises a reaction device, a discharging device and a cleaning device; the synthesis steps are as follows: A. the reaction raw materials are put into a reaction device for reaction; B. uniformly stirring the phase transfer catalyst and the reaction raw materials by using a bottom cleaning device; C. cleaning the bottom of the reaction kettle by using a cleaning device; D. the extrusion device is used for pushing up and down the catalyst and the reaction raw materials which are cleaned and blown up by the cleaning device and the bottom cleaning device; E. extracting a product in the reaction liquid by using an extraction barrel, and continuously returning the extracted reaction to the reaction kettle; F. the reaction is totally discharged by using a discharging device; G. and (5) cleaning the reaction liquid by using a cleaning device to obtain a finished product.
Description
Technical Field
The invention belongs to the technical field of chemical material processing, and particularly relates to a method for synthesizing high-purity 2-nitro-4-acetamido anisole.
Background
2-Amino-4-acetamido anisole is an important intermediate for synthesizing azo dyes, and is mainly used for synthesizing dispersing agent deep blue HGL and the like, the currently adopted process route is that p-nitrochlorobenzene is used as a raw material, and the p-nitrochlorobenzene is prepared through methoxylation, hydrogenation reduction, acetylation, nitration and hydrogenation reduction, wherein the nitration process is that sulfuric acid is used as a solvent, nitric acid is used as a nitrating agent for preparation, sulfuric acid is prepared in a batching kettle, acetyl is slowly added under the temperature reduction, nitric acid is slowly dripped at the controlled temperature for reaction, after the reaction is finished, the reaction liquid is dripped into cold water, a product is separated out, filtration is carried out, sulfuric acid is recovered from a waste acid concentrating workshop, wet products are washed to be neutral, and the wet products are added with methanol for pulping after centrifugation for hydrogenation reduction;
Wherein, sulfonation side reaction can occur in the pulping and dissolving process of sulfuric acid and acetamido anisole; literature (Liu Dong and the like, dyes and dyeing, 53,5, 34-47) proposes that the nitrified impurities are the least under 93% sulfuric acid concentration, but the amplification effect of actual industrial production is that for a nitrified workshop producing 2 ten thousand tons per year, the time for dissolving acetaminophen ether (50 tons) in each batch is as long as a plurality of hours due to the increase of the feeding amount, and meanwhile, the cooling process from the dissolution of the acetaminophen ether to the dropwise adding of nitric acid also needs 1-2 hours, 93% sulfuric acid is used as a reaction solvent at present, and sampling and analyzing are carried out before dropwise adding of nitric acid, wherein the content of sulphonates is above 5%, so that the nitrified product has low purity and low yield; in the nitration process, two positions of 2 and 3 can be nitro, and 3-nitro-4-acetamido anisole and 2, 5-binitro-4-acetamido anisole can be generated; the byproducts generated by the reaction are dissolved in dilute sulfuric acid, which brings inconvenience to the subsequent concentration of dilute sulfuric acid; during the reaction, the reaction raw materials cannot be uniformly distributed in the concentrated sulfuric acid, so that the reaction speed and the reaction thoroughly degree are affected.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention reduces the concentration of sulfuric acid in the dissolving process of the acetaminophen ether, 80 percent sulfuric acid is used as a solvent in the dissolving process, a phase transfer catalyst is added in the dissolving process to promote the dissolving of the acetaminophen ether, the dissolving time is reduced, the quaternary ammonium salt of the phase transfer catalyst is reduced, and the catalyst is added in the nitration process to inhibit the high-purity 2-nitro-4 acetaminophen ether of which the 3-position is nitrated by side reaction.
In order to achieve the above purpose, the present invention adopts the following technical scheme: the synthesis method of the high-purity 2-nitro-4 acetamido anisole comprises the steps of synthesizing the 2-nitro-4 acetamido anisole by using a production line; the assembly line comprises a reaction device, a discharging device and a cleaning device; the synthesis steps are as follows: A. the reaction raw materials are put into a reaction device for reaction; the reaction device comprises a first bracket, a reaction kettle, extraction barrels, a stirring main shaft, a bottom cleaning device, a cleaning device, an extrusion device, a driving device and an arc-shaped guide block, wherein the reaction kettle is arranged above the first bracket and used for containing raw materials; the method comprises the following specific steps: adding concentrated sulfuric acid into a reaction kettle, adding tetra-n-butyl ammonium chloride, uniformly stirring the mixture by using a stirring main shaft, and slowly adding acetaminophen ether and a phase transfer catalyst; B. uniformly stirring the phase transfer catalyst and the reaction raw materials by using a bottom cleaning device; the bottom cleaning device comprises a first gas storage tank arranged above the reaction kettle, a power assembly arranged in the first gas storage tank, a first rotating shaft which is communicated with the first gas storage tank and arranged in the reaction kettle, a driving control rod piece which is arranged in the first rotating shaft and matched with the power assembly, a telescopic assembly which is arranged in the first rotating shaft and matched with the driving control rod piece, a first rod piece which is arranged below the first rotating shaft and communicated with the first rotating shaft, and a gas control assembly which is arranged in the first rotating shaft and the first rod piece and matched with the telescopic assembly; the method comprises the following specific steps: the driving device drives the first rotating shaft to rotate, the first rotating shaft drives the power assembly to rotate, the power assembly drives the control rod piece to move, the drive control rod piece drives the telescopic assembly to move, inert gas in the first rotating shaft is compressed when the telescopic assembly moves to the gas control assembly, the gas control assembly is driven to move, the inert gas in the first rotating shaft can be blown outwards at the first rod piece through the movement of the gas control assembly, the inert gas is blown to the bottom of the reaction kettle, so that a catalyst and raw materials at the bottom of the reaction kettle are better evenly distributed, and then the inert gas in the first rotating shaft is supplemented by the first gas storage tank; C. cleaning the bottom of the reaction kettle by using a cleaning device; D. the extrusion device is used for pushing up and down the catalyst and the reaction raw materials which are cleaned and blown up by the cleaning device and the bottom cleaning device; E. extracting a product in the reaction liquid by using an extraction barrel, and continuously returning the extracted reaction to the reaction kettle; F. the reaction is totally discharged by using a discharging device; G. cleaning the reaction liquid by using a cleaning device to obtain a finished product;
The catalyst is added to increase the reaction speed, and then the extraction barrel continuously filters out the reaction product, so that the proportion of reactants in the reaction kettle can be reduced in the catalytic reaction, the equilibrium state exists in the catalytic reaction due to the equilibrium reaction, the reaction can not reach the equilibrium state by reducing the proportion of the reactants, the reaction is more thorough, the stirring main shaft can stir the inside of the reaction kettle, the reaction speed is further increased, the bottom of the reaction kettle can be cleaned by the cleaning device, the reaction raw materials and the catalyst at the bottom of the reaction kettle can be rolled up by the better stirred liquid, the uniform state of the reaction raw materials and the catalyst in the liquid can be better improved, the better uniform distribution is realized in the reaction kettle, the contact area of the reaction is increased, the reaction raw materials and the catalyst can not be gathered in a stack, the reaction speed is improved, the reaction degree is improved, the reaction is more thorough, then the cleaning device can continuously blow inert gas to the bottom of the reaction kettle, the inert gas can not react with concentrated sulfuric acid, the stability of the reaction is ensured, and then the inert gas can form bubbles to move upwards at the bottom of the reaction kettle, so that the reaction raw material and the catalyst at the bottom of the reaction kettle can be better brought to the upper part, and are better stirred by the stirring main shaft, the degree of uniform distribution in the reaction kettle is further improved, the reaction is more thorough, the uniformity of the catalyst and the reaction raw material in the reaction kettle is further increased through the extrusion device, the reaction is more thorough, thereby better improving the content of the reaction kettle-nitro-driving device-acetamidophenyl ether in the reaction.
Specifically, the bottom cleaning device further comprises a first through hole, a first connecting rod, a second gas storage tank, a connecting pipe, a gas storage cavity and a second through hole, wherein the first through hole is arranged below the first rod and is communicated with the reaction kettle; the cleaning device comprises a second connecting rod arranged below the first connecting rod, a cleaning piece connected with the second connecting rod, and a first control component arranged below the first connecting rod and used for driving the second connecting rod and the cleaning piece to move; the cleaning pieces are uniformly distributed below the first connecting rod; the first connecting rod is provided with a plurality of second through holes; are uniformly arranged between the two cleaning pieces; the first rod piece is provided with four pieces; uniformly arranged on the first rotating shaft; the two first rod pieces are connected to the first connecting rod; the method comprises the following specific steps: the first rotating shaft moves to drive the first rod piece to move, the first rotating shaft also drives the second gas storage tank and the first connecting rod to move together, the first connecting rod drives the cleaning piece to move, the cleaning piece cleans the bottom surface of the reaction kettle, then the rotation of the first connecting rod can enable the cleaning piece to clean more bottom surfaces of the reaction kettle, then the expansion component compresses inert gas in the first rotating shaft, the inert gas can be blown outwards through the control of the gas control component, the inert gas can be blown to the bottom surfaces of the reaction kettle directly in the first through holes on the two first rod pieces, then the inert gas in the other two first rod pieces can reach the connecting pipe through the first through holes and then reach the gas storage cavity, and the inert gas is blown between the two cleaning pieces through the second through holes;
Through the evenly distributed of a plurality of cleaning pieces, the range that cleaning pieces cleaned has been increased, make reaction raw materials and catalyst can be better by the roll-up, thereby better evenly distributed is in reation kettle, afterwards inert gas in the first pivot can outwards blow out in first through-hole, and outwards blow out in the second through-hole, thereby increase the power of blowing through very little giving vent to anger, afterwards first member and first connecting rod also can rotate, thereby make the scope of blowing out inert gas on the bottom surface to reation kettle that can be better, thereby further increase the degree of reaction.
Specifically, the air control assembly comprises a threaded plate, a threaded rod, a fourth spring, a transmission part and a control part, wherein the threaded plate is slidably arranged in the first rotating shaft, the threaded rod is connected with the threaded plate, the fourth spring is arranged below the threaded rod and used for supporting the threaded rod, the transmission part is arranged below the fourth spring and used for guiding the threaded rod, and the control part is connected with the transmission part and positioned in the first rod; the transmission part comprises a fourth fixed plate fixedly arranged in the first rotating shaft, a first gear fixedly arranged below the threaded rod, a second gear meshed with the first gear, a third rotating shaft fixedly connected with the second gear, and a supporting block arranged below the first gear and rotationally connected with the threaded rod and the supporting block for supporting; the thread plate is in threaded connection with the threaded rod; the method comprises the following specific steps: the telescopic component drives the threaded plate to move downwards, the threaded plate drives the threaded rod to rotate through threaded connection with the threaded rod, the threaded rod rotates to drive the first gear to rotate, then the first gear drives the second gear to rotate, the second gear rotates to drive the control component to move, the control component controls the opening and closing states of the first through hole, and when the telescopic component is reset, the threaded plate is reset through the fourth spring;
The control part moves through the movement of the transmission part, so that the opening and closing states of the first through holes and the movement of the transmission part are combined with each other, the transmission part is used for compressing inert gas, so that the first through holes are opened under the condition of compression of the inert gas, the inert gas is blown out of the first through holes better, the force of the blown inert gas is further improved, the reaction raw materials and the catalyst on the bottom surface of the reaction kettle can be better blown, the reaction raw materials and the catalyst are further distributed more uniformly, and the reaction speed and the reaction are further improved thoroughly.
Specifically, the control part comprises a seventh rod piece fixedly connected with the second gear, a ninth guide block fixedly connected with the seventh rod piece, a baffle fixedly connected with the ninth guide block and rotationally arranged in the first rod piece, and a tenth guide block fixedly connected with the tenth guide block; the ninth guide block and the transmission part are rotationally connected to the first rod piece; the baffle has only a small angle; the angle of the baffle plate blocks the first through hole; the baffle rotates to open the first through hole; the method comprises the following specific steps: the second gear rotates to drive the seventh rod piece to rotate, the seventh rod piece drives the baffle to rotate in the first rod piece through the ninth guide block and the tenth guide block, and the ninth guide block and the tenth guide block enable the rotation to be more stable; the first control component of the air control component can open the first through hole once starting to rotate, so that air in the first rod piece can be blown out more quickly, and better control is performed.
Specifically, the telescopic component comprises a fourth fixed plate fixedly connected with the first rotating shaft, a third rod piece which is arranged in the first fixed plate in a sliding manner and connected with the power component, two second fixed plates fixedly connected below the first fixed plate, a plurality of third connecting rods which are connected with the second fixed plates in a staggered manner, a first pin roll which is arranged at the hinge point of the third rod piece and one third connecting rod, a first push plate which is arranged below the third connecting rod, and a hollow rod piece which is fixedly arranged below the first push plate and matched with the threaded plate; two identical second fixing plates are arranged below the third connecting rod; the second fixing plate below is connected with the first pushing plate; the method comprises the following specific steps: the power assembly drives the third rod piece to move downwards, the third rod piece drives the first pin shaft to move downwards, the first pin shaft drives the plurality of third connecting rods which are arranged in a staggered mode to move, and therefore the third connecting rods are unfolded from a superimposed state, the first push plate is driven to move downwards, the first push plate drives the hollow rod piece to move downwards, and the hollow rod piece is impacted to the threaded plate to drive the threaded plate to move downwards; the hollow rod piece stops after impacting the threaded plate, and the hollow rod piece drives the threaded plate to move downwards for a short distance;
Therefore, the screw plate can be driven to move downwards when the first push plate moves to the lowest position, so that the inert gas in the arc-shaped guide block of the telescopic assembly is compressed by the first push plate, the pressure in the arc-shaped guide block of the telescopic assembly and the pressure in the first rod piece can be increased, the inert gas can be blown out rapidly under the action of the pressure when the first through hole is opened by the movement of the gas control assembly, the speed of blowing the inert gas on the bottom surface of the reaction kettle is further improved, and the reaction speed is improved better and the reaction is more thorough.
Specifically, the power assembly comprises a second rod piece fixedly arranged in the first gas storage tank, a first disc fixedly arranged below the second rod piece, a plurality of second guide blocks fixedly arranged on the first disc, a second disc fixedly arranged above the driving control rod piece, a third guide block fixedly arranged above the second disc and matched with the second guide block, and a third spring arranged below the second disc and used for propping against the second disc to reset the second disc; the driving control rod piece is fixedly connected with the third rod piece; the method comprises the following specific steps: the driving device drives the first rotating shaft to rotate, the first rotating shaft rotates to drive the first fixing plate to rotate, the first fixing plate drives the third rod piece to rotate, the driving control rod piece drives the second disc, the driving control rod piece can be driven to reciprocate up and down through the cooperation of the third guide block and the second guide block, and therefore the third rod piece can be driven to compress inert gas in the first rotating shaft to move to provide power.
Specifically, the first control component comprises a fourth guide block fixedly arranged below the first connecting rod, a second rotating shaft rotationally connected with the second connecting rod and fixedly connected with the cleaning piece for supporting the cleaning piece, a fourth connecting rod hinged with the second rotating shaft, a third fixing plate fixedly connected with the first connecting rod, a fourth rod fixedly connected with the third fixing plate, and a first chute arranged on the fourth connecting rod and slidably connected with the fourth rod; the second connecting rod is connected to the fourth guide block in a sliding manner; an elastic metal strip is arranged in the cleaning piece; the arc-shaped guide blocks are multiple; the arc-shaped guide blocks matched with the cleaning device are positioned at the same height as the second connecting rod, and three arc-shaped guide blocks are uniformly distributed on the inner wall of the reaction kettle; the method comprises the following specific steps: the first connecting rod drives the fourth guide block to move together, so that the second connecting rod moves together, the second connecting rod is continuously matched with the arc-shaped guide block during movement, the second connecting rod is driven to slide in the fourth guide block under the action of the arc-shaped guide block, the second connecting rod is driven to reciprocate and cannot be blocked due to the fact that the arc-shaped guide block is three, the second connecting rod slides to drive the second rotating shaft to move together, then the second rotating shaft drives the fourth connecting rod to move, the fourth connecting rod moves under the cooperation of the fourth rod and the first sliding groove, namely the hinged position of the fourth connecting rod and the second rotating shaft rotates at an angle, so that the second rotating shaft can reciprocate and simultaneously drive the second rotating shaft to reciprocate, and the second rotating shaft drives the cleaning piece to move in the same manner; the cleaning piece can reciprocate the rotation when reciprocating sliding, can be better clean reaction raw materials and catalysis on the reation kettle bottom surface, make the bottom surface that leaves reation kettle that both can be better to better evenly distributed is in reation kettle's inside, thereby promotes the going on of reaction, improves the purity of reaction product.
Specifically, the extrusion device comprises a second control assembly arranged above the first connecting rod, a plurality of extrusion plates arranged above the second control assembly, and a lifting assembly, wherein the two advanced and second control assemblies and the extrusion plates are used for driving the extrusion plates to move; the extruding plate is provided with a plurality of third through holes; the lifting assembly comprises a fifth connecting rod and a sixth connecting rod which are connected with the second control assembly in a staggered manner, a second pin shaft connected with the fifth connecting rod and the sixth connecting rod, and the fifth connecting rod and the sixth connecting rod are hinged and fixed through the second pin shaft; the second control assembly comprises a fifth guide block fixedly arranged above the first connecting rod, a sixth guide block and a seventh guide block which are arranged on the fifth guide block in a sliding manner and positioned on two sides of the fifth guide block, a fifth rod piece arranged on the sixth guide block, an eighth guide block fixedly connected to the sixth guide block, a sixth rod piece arranged above the eighth guide block and matched with the arc-shaped guide block, and a first spring arranged between the two eighth guide blocks; the fifth connecting rod and the sixth connecting rod are hinged to the eighth guide block; wherein, the number of the second control components is two, and the two second control components are distributed on the two sides of the first connecting rod; the fifth rod piece is connected to a sixth guide block in one second control assembly and is connected with a seventh guide block in the other second control assembly; the sixth guide block moves to drive the seventh guide blocks on the two second control components to move; the two arc-shaped guide blocks matched with the extrusion device are symmetrically arranged on the inner wall of the reaction kettle and are at the same height with the sixth rod piece; the method comprises the following specific steps: the first connecting rod drives the extrusion device to move together, then the sixth rod is continuously matched with the arc-shaped guide blocks when moving, so that the sixth guide blocks are driven to move towards the seventh guide blocks under the action of the arc-shaped guide blocks, the sixth guide blocks on two sides move together due to the fact that the arc-shaped guide blocks are symmetrically arranged, the sixth guide blocks drive the seventh guide blocks to move together through the fifth rod, so that two eighth guide blocks on the fifth guide blocks move oppositely at the same time, the fifth connecting rod and the sixth connecting rod are driven to move together, a plurality of fifth connecting rods and a plurality of sixth connecting rods which are prevented from being overlapped together move to be unfolded, so that the second pin shafts move upwards, the plurality of second pin shafts move upwards by the same distance between the plurality of second pin shafts, and are increased simultaneously, then the second pin shafts drive the extrusion plate fixed on the second pin shafts to move upwards, and the lifting assembly agrees that the arc-shaped guide blocks of the lifting assembly are separated from the fifth guide blocks to move together, and the extrusion plate is reset under the action of the first spring to reciprocate;
The extrusion plates move upwards to enable a plurality of gaps to exist between each extrusion plate, a plurality of reaction raw materials and catalysis are added on the extrusion plates under the stirring of the stirring main shaft, then the extrusion plates are reset, the distance between the extrusion plates is shortened, the extrusion plates can pressurize the solution to the middle, so that the reaction raw materials and the catalyst are extruded to the middle position, namely, the reaction raw materials and the catalyst move from the middle to two sides and then move from the two sides to the middle, so that the reaction raw materials and the catalyst can reach the two sides from the middle irregular distribution, the reaction raw materials and the catalyst are uniformly distributed at the upper and lower positions of the two sides, and the reaction raw materials and the catalyst can be better extruded to the middle when the third through hole is reset due to the blocking of the third through hole, so that the distribution uniformity of the reaction raw materials and the catalyst in the reaction kettle is better improved, and then the sixth guide block and the seventh guide block move simultaneously to enable the up and down movement process of the extrusion plates to be better stable; thereby realizing the uniform distribution of the reaction raw materials and the catalyst and improving the reaction degree.
Specifically, the driving device comprises a second bracket fixedly arranged above the reaction kettle, a motor fixedly arranged above the second bracket, a first conveyer belt fixedly connected to the output end of the motor, the first conveyer belt connected to the stirring main shaft, a second conveyer belt connected to the stirring main shaft, a double-worm reduction gearbox connected to the second conveyer belt, a third conveyer belt connected to the double-worm reduction gearbox, a bottom cleaning device connected to the third conveyer belt, a braking component connected to the motor, a plurality of discharging blocks for charging arranged on the reaction kettle, and two discharging grooves for discharging arranged below the reaction kettle; the brake assembly comprises a first guide block fixedly arranged above the reaction kettle, a first guide rod slidingly arranged in the first guide block, a clamping plate fixedly arranged on the first guide rod, a second spring arranged between the clamping plate and the first guide block, an electromagnet arranged on the clamping plate and the first guide block, and a clamping toothed plate arranged at the output end of the motor and matched with the clamping plate; the third conveyer belt is connected to the first rotating shaft; the stirring main shaft is provided with a plurality of stirring blades for stirring; the method comprises the following specific steps: the motor drives the first conveyer belt to move, the rotation of first conveyer belt provides power for stirring main shaft, stirring main shaft rotation can drive the second conveyer belt, the second conveyer belt drives the input of two turbine worm reducing gears, the output of two turbine worm reducing gears drives the third conveyer belt and moves, the third conveyer belt drives first pivot rotation, the first conveyer belt, the second conveyer belt, the third conveyer belt is prior art and for the transmission of speed reduction, thereby make the speed of first pivot slow down through multistage speed reduction, improve the stability of motion, afterwards the blown down tank can be opened to the workman and change the cleaning member, need guarantee stirring main shaft and first pivot can not take place any rotation when changing, this is that the electro-magnet outage can make the screens board block the card pinion rack under the effect of second spring, thereby can not take place the rotation, thereby workman's security when improving the change.
Compared with the prior art, the invention has the following advantages:
1. reducing sulfonation side reaction: in the process of dissolving acetamido anisole by sulfuric acid, 80% sulfuric acid is used for replacing 93% sulfuric acid, so that the sulfonation capability of sulfuric acid is reduced;
2. The addition of the phase transfer catalyst promotes the dissolution rate of the acetaminophen in sulfuric acid, and reduces the time for dissolving the acetaminophen, thereby reducing the occurrence of sulfonation side reaction;
3. Improving the selectivity of target products in the nitration reaction: by adding the catalyst, the side reaction of nitration of the 3-position of the benzene ring is inhibited, and guanidine compounds, nitroxyl cations and guanidine compounds have certain acting force, so that the 2-position is preferentially attacked during nitration due to large 3-position steric hindrance.
In summary, the bottom cleaning device is arranged to blow inert gas which does not react with concentrated sulfuric acid on the bottom surface of the reaction kettle, so that reaction raw materials and catalysts on the bottom surface of the reaction kettle can be blown up better, and can not sink on the bottom surface and float, and then the inert gas and the catalyst can be uniformly distributed in the reaction kettle through the cooperation of the stirring main shaft, so that the reaction speed and the reaction degree are improved; the cleaning device is arranged to clean the bottom surface of the reaction kettle, so that the reaction raw materials and the catalyst on the bottom surface of the reaction kettle float better in a physical mode, and the uniform distribution effect is improved; the extrusion device is arranged to continuously extrude the floating reaction raw materials and the catalyst, so that the floating reaction raw materials and the catalyst are more uniformly distributed in the reaction kettle, and the reaction degree is further improved.
Drawings
FIG. 1 is a schematic cross-sectional view of the present invention;
FIG. 2 is an enlarged view of FIG. 1A in accordance with the present invention;
FIG. 3 is an enlarged view of B of FIG. 1 in accordance with the present invention;
FIG. 4 is an enlarged view of C of FIG. 1 in accordance with the present invention;
FIG. 5 is a schematic diagram of a gas control assembly according to the present invention;
FIG. 6 is a schematic view of the structure of the stirring main shaft in the invention;
FIG. 7 is an enlarged view of D of FIG. 1 in accordance with the present invention;
FIG. 8 is a schematic view of a cleaning apparatus according to the present invention;
FIG. 9 is a schematic diagram of the control unit according to the present invention;
FIG. 10 is a schematic diagram of a first control assembly according to the present invention;
FIG. 11 is a schematic view of the structure of a fourth guide block according to the present invention;
FIG. 12 is a schematic view of a second link according to the present invention;
FIG. 13 is a schematic diagram of a second control assembly according to the present invention;
FIG. 14 is an enlarged view of E of FIG. 13 in accordance with the present invention;
FIG. 15 is a schematic view of a lifting assembly according to the present invention;
FIG. 16 is a schematic view showing the structure of the squeeze plate of the present invention;
FIG. 17 is a schematic view of a third link according to the present invention;
FIG. 18 is a schematic diagram of a driving device according to the present invention;
FIG. 19 is a schematic diagram of a driving device according to a second embodiment of the present invention;
FIG. 20 is a schematic view of a brake assembly according to the present invention;
FIG. 21 is a schematic view of an arc-shaped guide block according to the present invention;
FIG. 22 is a second schematic structural view of an arc-shaped guide block according to the present invention;
FIG. 23 is a schematic view of a spout according to the present invention;
Detailed Description
In order to enable those skilled in the art to better understand the present invention, the following description will make clear and complete descriptions of the technical solutions in the embodiments of the present invention with reference to the accompanying drawings in the embodiments of the present invention.
As shown in fig. 1 to 23, the method for synthesizing the high-purity 2-nitro-4 acetamido anisole synthesizes the 2-nitro-4 acetamido anisole by using a pipeline; the assembly line comprises a reaction device, a discharging device and a cleaning device; the synthesis steps are as follows: A. the reaction raw materials are put into a reaction device for reaction; the reaction device comprises a first bracket 1, a reaction kettle 2 arranged above the first bracket 1 and used for containing raw materials, extraction barrels 3 arranged on two sides of the reaction kettle 2, a stirring main shaft 8 arranged inside the reaction kettle 2, a bottom cleaning device 5 connected with the stirring main shaft 8, a cleaning device 6 arranged below the bottom cleaning device 5, an extrusion device 7 arranged above the cleaning device 6, a driving device 4 arranged above the reaction kettle 2 and used for driving the bottom cleaning device 5 and the stirring main shaft 8, and an arc-shaped guide block 9 arranged on the inner wall of the reaction kettle 2 and matched with the cleaning device 6 and the extrusion device 7; the method comprises the following specific steps: adding concentrated sulfuric acid into a reaction kettle 2, adding tetra-n-butyl ammonium chloride, uniformly stirring the mixture by using a stirring main shaft 8, and slowly adding acetaminophen ether and a phase transfer catalyst; B. uniformly stirring the phase transfer catalyst and the reaction raw materials by using a bottom cleaning device 5; the bottom cleaning device 5 comprises a first gas storage tank 51 arranged above the reaction kettle 2, a power assembly 52 arranged in the first gas storage tank 51, a first rotating shaft 59 communicated with the first gas storage tank 51 and arranged in the reaction kettle 2, a driving control rod piece 53 arranged in the first rotating shaft 59 and matched with the power assembly 52, a telescopic component 54 arranged in the first rotating shaft 59 and matched with the driving control rod piece 53, a first rod piece 56 arranged below the first rotating shaft 59 and communicated with the first rotating shaft 59, and a gas control component 55 arranged in the first rotating shaft 59 and the first rod piece 56 and matched with the telescopic component 54; the method comprises the following specific steps: the driving device 4 drives the first rotating shaft 59 to rotate, the first rotating shaft 59 drives the power assembly 52 to rotate, the power assembly 52 drives the driving control rod piece 53 to move, the driving control rod piece 53 drives the telescopic assembly 54 to move, inert gas in the first rotating shaft 59 is compressed when the telescopic assembly 54 moves to the gas control assembly 55, the gas control assembly 55 is driven to move when the telescopic assembly 54 moves to the gas control assembly 55, the inert gas in the first rotating shaft 59 is blown out at the first rod piece 56 and is blown to the bottom of the reaction kettle 2, so that catalyst and raw materials at the bottom of the reaction kettle 2 are better evenly distributed, and then the inert gas in the first rotating shaft 59 is supplemented by the first gas storage tank 51; C. the bottom of the reaction kettle 2 is cleaned by a cleaning device 6; D. the extrusion device 7 is used for pushing up and down the catalyst and the reaction raw materials which are cleaned and blown up by the cleaning device 6 and the bottom cleaning device 5; E. the product in the reaction liquid is extracted by using an extraction barrel 3, and the extracted reaction is continuously returned to the reaction kettle 2; F. the reaction is totally discharged by using a discharging device; G. and (5) cleaning the reaction liquid by using a cleaning device to obtain a finished product.
Specifically, the bottom cleaning device 5 further includes a first through hole 561 disposed below the first rod 56 and communicated with the reaction kettle 2, a first connecting rod 58 disposed below the first rod 56 and fixedly connected to the first rotating shaft 59, a second gas storage tank 57 disposed between the first connecting rod 58 and the first rod 56, a connecting pipe 562 disposed between the second gas storage tank 57 and the first through hole 561 and used for communicating the first through hole 561 and the second gas storage tank 57, a gas storage cavity 571 disposed in the second gas storage tank 57 and communicated with the first rod 56, and a second through hole 572 disposed on the first connecting rod 58 and used for communicating the gas storage cavity 571 and the reaction kettle 2; the cleaning device 6 comprises a second connecting rod 62 arranged below the first connecting rod 58, a cleaning piece 61 connected with the second connecting rod 62, and a first control assembly 63 arranged below the first connecting rod 58 and used for driving the second connecting rod 62 and the cleaning piece 61 to move; a plurality of cleaning elements 61 are uniformly distributed below the first connecting rod 58; the first connecting rod 58 is provided with a plurality of second through holes 572; are uniformly arranged between the two cleaning pieces 61; four of the first bars 56; uniformly arranged on the first rotating shaft 59; two of the first rods 56 are connected to the first link 58; the method comprises the following specific steps: when the first rotating shaft 59 moves, the first rod 56 is driven to move, the first rotating shaft 59 also drives the second gas storage tank 57 and the first connecting rod 58 to move together, the first connecting rod 58 drives the cleaning piece 61 to move, the cleaning piece 61 cleans the bottom surface of the reaction kettle 2, then the rotation of the first connecting rod 58 can enable the cleaning piece 61 to clean more bottom surfaces of the reaction kettle 2, then when the expansion component 54 compresses inert gas in the first rotating shaft 59, the inert gas can be blown out of the first through holes 561 through the control of the gas control component 55, the inert gas can be blown to the bottom surfaces of the reaction kettle 2 in the first through holes 561 on the two first rod 56, then the inert gas in the other two first rod 56 can be blown to the connecting pipe 562 through the first through holes 561, then the inert gas can be blown to the gas storage cavity 571 572, and the inert gas can be blown between the two cleaning pieces 61 through the second through holes.
Specifically, the air control assembly 55 includes a threaded plate 551 slidably disposed in the first rotating shaft 59, a threaded rod 552 connected to the threaded plate 551, a fourth spring 553 disposed below the threaded rod 552 and used for supporting the threaded rod 552, a transmission component 554 disposed below the fourth spring 553 and used for guiding the threaded rod 552, and a control component 555 connected to the transmission component 554 and located inside the first rod 56; the transmission member 554 includes a fourth fixing plate 5541 fixedly disposed inside the first rotating shaft 59, a first gear 5542 fixedly disposed below the threaded rod 552, a second gear 5543 engaged with the first gear 5542, a third rotating shaft 5544 fixedly coupled to the second gear 5543, and a supporting block 5545 disposed below the first gear 5542 and rotatably coupled to the threaded rod 552 and the supporting block 5545 for supporting; the thread plate 551 is in threaded connection with the threaded rod 552; the method comprises the following specific steps: the telescopic component 54 drives the threaded plate 551 to move downwards, the threaded plate 551 drives the threaded rod 552 to rotate through being connected with the threaded rod 552 in a threaded mode, the threaded rod 552 rotates to drive the first gear 5542 to rotate, then the first gear 5542 drives the second gear 5543 to rotate, the second gear 5543 rotates to drive the control component 555 to move, the control component 555 controls the opening and closing states of the first through hole 561, and when the telescopic component 54 is reset, the threaded plate 551 resets through the fourth spring 553.
Specifically, the control part 555 includes a seventh rod 5551 fixedly connected to the second gear 5543, a ninth guide block 5552 fixedly connected to the seventh rod 5551, a baffle 5553 fixedly connected to the ninth guide block 5552 and rotatably disposed inside the first rod 56, and a tenth guide block 5554 fixedly connected to the tenth guide block 5554; the ninth guide block 5552 and the transmission member 554 are rotatably connected to the first lever 56; the baffle 5553 has only a slight angle; the angle of the shutter 5553 blocks the first through hole 561; the shutter 5553 rotates to open the first through hole 561; the method comprises the following specific steps: the rotation of the second gear 5543 drives the seventh rod 5551 to rotate, the seventh rod 5551 drives the baffle 5553 to rotate in the first rod 56 through the ninth guide block 5552 and the tenth guide block 5554, and the ninth guide block 5552 and the tenth guide block 5554 make the rotation more stable; the first control component 63 of the air control component 55 can open the first through hole 561 once starting to rotate, so that the air in the first rod piece 56 can be blown out more quickly, and better control is achieved.
Specifically, the telescopic assembly 54 includes a fourth fixing plate 5541 fixedly connected to the first rotating shaft 59, a third rod 542 slidably disposed in the first fixing plate 541 and connected to the power assembly 52, two second fixing plates 544 fixedly connected to the lower portion of the first fixing plate 541, a plurality of third connecting rods 545 fixedly connected to the second fixing plates 544 in a staggered manner, a first pin roll 543 at a hinge point of the third rod 542 and one third connecting rod 545, a first push plate 546 disposed below the third connecting rod 545, and a hollow rod 547 fixedly disposed below the first push plate 546 and engaged with the threaded plate 551; two identical second fixing plates 544 are arranged below the third connecting rod 545; the lower second fixing plate 544 is connected to the first push plate 546; the method comprises the following specific steps: the power assembly 52 drives the third rod 542 to move downwards, the third rod 542 drives the first pin shaft 543 to move downwards, the first pin shaft 543 drives the plurality of third connecting rods 545 which are arranged in a staggered manner to move, so that the third connecting rods 545 are unfolded from a stacked state, the first push plate 546 is driven to move downwards, the first push plate 546 drives the hollow rod 547 to move downwards, and the hollow rod 547 impacts the threaded plate 551 to drive the threaded plate 551 to move downwards; the hollow rod 547 stops after striking the screw plate 551, and the hollow rod 547 drives the screw plate 551 downward a short distance.
Specifically, the power assembly 52 includes a second rod 521 fixedly disposed inside the first air tank 51, a first disc 522 fixedly disposed below the second rod 521, a plurality of second guide blocks 523 fixedly disposed on the first disc 522, a second disc 525 fixedly disposed above the driving control rod 53, a third guide block 524 fixedly disposed above the second disc 525 and engaged with the second guide block 523, and a third spring 526 disposed below the second disc 525 and for abutting against the second disc 525 to reset the same; the driving control rod 53 is fixedly connected to the third rod 542; the method comprises the following specific steps: the driving device 4 drives the first rotating shaft 59 to rotate, the first rotating shaft 59 rotates to drive the first fixing plate 541 to rotate, the first fixing plate 541 drives the third rod 542 to rotate, so that the driving control rod 53 rotates, the driving control rod 53 drives the second disc 525, and the driving control rod 53 is driven to reciprocate up and down through the cooperation of the third guide block 524 and the second guide block 523, so that the movement of the third rod 542 drives the first push plate 546 to compress the inert gas in the first rotating shaft 59 is provided with power.
Specifically, the first control assembly 63 includes a fourth guide block 636 fixedly disposed below the first connecting rod 58, a second rotating shaft 631 rotatably connected to the second connecting rod 62 and fixedly connected to the cleaning member 61 for supporting the cleaning member 61, a fourth connecting rod 632 hinged to the second rotating shaft 631, a third fixing plate 635 fixedly connected to the first connecting rod 58, a fourth rod 634 fixedly connected to the third fixing plate 635, and a first chute 633 disposed on the fourth connecting rod 632 and slidably connected to the fourth rod 634; the second link 62 is slidably coupled to the fourth guide block 636; an elastic metal strip is arranged inside the cleaning piece 61; the number of the arc-shaped guide blocks 9 is multiple; the arc-shaped guide blocks 9 matched with the cleaning device 6 are positioned at the same height as the second connecting rod 62, and three arc-shaped guide blocks are uniformly distributed on the inner wall of the reaction kettle 2; the method comprises the following specific steps: the first connecting rod 58 drives the fourth guide block 636 to move together, so that the second connecting rod 62 moves together, the second connecting rod 62 is continuously matched with the arc-shaped guide block 9 during movement, so that the second connecting rod 62 is driven to slide in the fourth guide block 636 under the action of the arc-shaped guide block 9, the second connecting rod 62 is driven to reciprocate and not to be blocked because of three arc-shaped guide blocks 9, the second connecting rod 62 slides to drive the second rotating shaft 631 to move together, the second rotating shaft 631 then drives the fourth connecting rod 632 to move, the fourth connecting rod 632 moves under the cooperation of the fourth rod 634 and the first sliding groove 633, namely, the hinged position of the fourth connecting rod 632 and the second rotating shaft 631 rotates at an angle, so that the second rotating shaft 631 reciprocates and simultaneously drives the second rotating shaft 631 to reciprocate, and the second rotating shaft 631 drives the cleaning piece 61 to perform the same movement; the cleaning member 61 can be rotated reciprocally while sliding reciprocally, so that the reaction raw material and the catalyst on the bottom surface of the reaction vessel 2 can be cleaned better.
Specifically, the extruding device 7 includes a second control assembly 71 disposed above the first connecting rod 58, a plurality of extruding plates 73 disposed above the second control assembly 71, and a lifting assembly 72 for driving the extruding plates 73 to move by two steps and the second control assembly 71 and the extruding plates 73; the extrusion plate 73 is provided with a plurality of third through holes 731; the lifting assembly 72 comprises a fifth link 721 and a sixth link 722 which are connected to the second control assembly 71 in a staggered manner, a second pin 723 connected to the fifth link 721 and the sixth link 722, and the fifth link 721 and the sixth link 722 are hinged and fixed through the second pin 723; the second control assembly 71 includes a fifth guide block 711 fixedly disposed above the first connecting rod 58, a sixth guide block 712 and a seventh guide block 714 slidably disposed on the fifth guide block 711 and disposed on two sides of the fifth guide block 711, a fifth rod 713 disposed on the sixth guide block 712, an eighth guide block 715 fixedly coupled to the sixth guide block 712, a sixth rod 716 disposed above the eighth guide block 715 and engaged with the arc-shaped guide block 9, and a first spring 717 disposed between the two eighth guide blocks 715; the fifth link 721 and the sixth link 722 are hinged to the eighth guide block 715; wherein, two second control components 71 are distributed on two sides of the first connecting rod 58; the fifth rod 713 is connected to the sixth guide block 712 of the second control assembly 71 and is connected to the seventh guide block 714 of the second control assembly 71; the sixth guide block 712 moves to drive the seventh guide blocks 714 on the two second control assemblies 71; the two arc-shaped guide blocks 9 matched with the extrusion device 7 are symmetrically arranged on the inner wall of the reaction kettle 2 and are at the same height with the sixth rod 716; the method comprises the following specific steps: the first link 58 drives the pressing device 7 to move together, then the sixth rod 716 is continuously matched with the arc-shaped guide block 9 when moving, so that the sixth guide block 712 is driven to move towards the seventh guide block 714 under the action of the arc-shaped guide block 9, the arc-shaped guide block 9 is symmetrically arranged, the sixth guide blocks 712 on two sides move together, the sixth guide block 712 drives the seventh guide block 714 to move together through the fifth rod 713, so that the two eighth guide blocks 715 on the fifth guide block 711 move simultaneously in opposite directions, so that the fifth link 721 and the sixth link 722 are driven to move together, a plurality of fifth links 721 and a plurality of sixth links 722 which are overlapped together are unfolded, so that the second pin 723 moves upwards, the plurality of second pins 723 move upwards in the same distance as the plurality of second pins, and simultaneously increase, then the second pin 723 drives the pressing plate 73 fixed on the second pin 723 to move upwards, and the lifting assembly 723 moves upwards in a reciprocating manner, so that the lifting assembly 73 moves upwards, and the reciprocating assembly 73 is separated from the arc-shaped guide plate 73, and the reciprocating assembly 73 moves downwards, so that the reciprocating assembly 73 moves upwards, and the reciprocating assembly 73 is separated from the reciprocating assembly is moved downwards, thereby the reciprocating assembly is moved under the action of the reciprocating assembly 73.
Specifically, the driving device 4 includes a second bracket 42 fixedly disposed above the reaction kettle 2, a motor 41 fixedly disposed above the second bracket 42, a first conveyor belt 44 fixedly connected to an output end of the motor 41, the first conveyor belt 44 connected to the stirring main shaft 8, a second conveyor belt 45 connected to the stirring main shaft 8, a double-worm reduction gearbox 46 connected to the second conveyor belt 45, a third conveyor belt 47 connected to the double-worm reduction gearbox 46, the third conveyor belt 47 connected to the bottom cleaning device 5, a brake assembly 43 connected to the motor 41, a plurality of discharging blocks 48 for charging disposed on the reaction kettle 2, and two discharging grooves 21 for discharging disposed below the reaction kettle 2; the brake assembly 43 comprises a first guide block 433 fixedly arranged above the reaction kettle 2, a first guide bar 434 slidably arranged in the first guide block 433, a clamping plate 432 fixedly arranged on the first guide bar 434, a second spring 435 arranged between the clamping plate 432 and the first guide block 433, an electromagnet 436 arranged on the clamping plate 432 and the first guide block 433, and a clamping tooth plate 431 arranged at the output end of the motor 41 and matched with the clamping plate 432; the third conveyor belt 47 is connected to the first rotation shaft 59; a plurality of stirring blades 81 for stirring are arranged on the stirring main shaft 8; the method comprises the following specific steps: the motor 41 drives the first conveyer belt 44 to move, the first conveyer belt 44 provides power for the rotation of the stirring main shaft 8, the stirring main shaft 8 rotates to drive the second conveyer belt 45, the second conveyer belt 45 drives the input end of the double-worm gear reduction box 46, the output end of the double-worm gear reduction box 46 drives the third conveyer belt 47 to move, the third conveyer belt 47 drives the first rotating shaft 59 to rotate, the first conveyer belt 44, the second conveyer belt 45 and the third conveyer belt 47 are in the prior art and are in the speed-reducing transmission, so that the speed of the first rotating shaft 59 is slowed down through multistage speed reduction, the stability of the movement is improved, a worker can open the discharge chute 21 to replace the cleaning piece 61, no rotation of the stirring main shaft 8 and the first rotating shaft 59 is ensured during the replacement, the electromagnet 436 is powered off to enable the clamping plate 432 to clamp the clamping plate 431 under the action of the second spring 435, and therefore the safety of the worker during the replacement is improved.
Example two
Adding 5kg of 93% sulfuric acid into a reaction device of a 10L reaction kettle, slowly adding 2kg of acetaminophen at 10-15 ℃ under the control of temperature of frozen brine, and keeping the temperature for 2 hours after adding for 2 hours to completely dissolve the acetaminophen; then cooling to 5 ℃ within 0.5 hours, sampling and analyzing by HPLC, wherein the content of the sulfonate is 5.2 percent, then dropwise adding nitric acid at the temperature of 0-5 ℃ for 5 hours, continuing to keep the temperature for 1 hour after the dropwise adding, and sampling and analyzing by HPLC, wherein the content of the sulfonated byproducts is 5.5 percent, 92 percent of 2-nitro-4-acetaminophen, 1.5 percent of 3-nitro-4-acetaminophen and 1 percent of 2, 5-dinitro-4-acetaminophen. Slowly dripping the reaction solution into ice water, diluting the sulfuric acid concentration to 35%, eluting yellow solid, filtering to obtain 2-nitro-4-acetamidophenyl ether wet product, wherein the COD of mother liquor waste acid is 31000mg/L, adding water into the filter cake to wash to obtain the finished product, and carrying out HPLC analysis on the content of the 2-nitro-4-acetamidophenyl ether to be 97.8%.
Example III
Adding 5kg of 80% sulfuric acid into a reaction device of a 10L reaction kettle, adding 25g of tetra-n-butyl ammonium chloride, stirring until the tetra-n-butyl ammonium chloride is completely dissolved, slowly adding 2kg of acetaminophen at 10-15 ℃ under the control of temperature of frozen salt water, keeping the temperature for 1 hour after adding for 2 hours, and completely dissolving the acetaminophen; then cooling to 5 ℃ within 0.5 hours, sampling and analyzing by HPLC, wherein the content of the sulfonate is 0.3 percent, then dropwise adding nitric acid at the temperature of 0-5 ℃ under control, continuously preserving heat for 1 hour after 5 hours, and analyzing by sampling and analyzing by HPLC, wherein the content of the sulfonate by-product is 0.6 percent, the content of the 2-nitro-4-acetaminophen ether is 97.6 percent, the content of the 3-nitro-4-acetaminophen ether is 1.2 percent, and the content of the 2, 5-dinitro-4-acetaminophen ether is 0.6 percent. Slowly dripping the reaction solution into ice water, diluting the sulfuric acid concentration to 35%, eluting yellow solid, filtering to obtain a wet product of 2-nitro-4-acetamidophenyl ether, wherein the COD of mother liquor waste acid is 15000mg/L, adding water into a filter cake, and washing to obtain a finished product, wherein the content of the 2-nitro-4-acetamidophenyl ether is 98.2% by HPLC analysis.
Example IV
Adding 5kg of 80% sulfuric acid into a reaction device of a 10L reaction kettle, adding 25g of tetra-n-butyl ammonium chloride, stirring until the tetra-n-butyl ammonium chloride is completely dissolved, slowly adding 2kg of acetaminophen at 10-15 ℃ under the control of temperature of frozen salt water, keeping the temperature for 1 hour after adding for 2 hours, and completely dissolving the acetaminophen; then cooling to 5 ℃ within 0.5 hour, and sampling and analyzing by HPLC, wherein the content of the sulfonate is 0.3%; 10g guanidine nitrate is added, stirring is continued for 0.5 hours, then nitric acid is added dropwise at the temperature of 0-5 ℃ for 5 hours, after that, the temperature is kept for 1 hour, sampling HPLC analysis is continued, wherein sulfonation byproducts are 0.4%, 2-nitro-4-acetaminophen ether is 99.2%, 3-nitro-4-acetaminophen ether is 0.3%, and 2, 5-dinitro-4-acetaminophen ether is 0.1%. Slowly dripping the reaction solution into ice water, diluting the sulfuric acid concentration to 35%, eluting yellow solid, filtering to obtain a wet product of 2-nitro-4-acetamidophenyl ether, wherein the COD of mother liquor waste acid is 5000mg/L, adding water into a filter cake, and washing to obtain a finished product, wherein the content of 2-nitro-4-acetamidophenyl ether is 99.5% by HPLC analysis.
The specific working flow of the invention is as follows: adding concentrated sulfuric acid into the reaction kettle 2, adding tetra-n-butyl ammonium chloride, driving the first conveying belt 44 to move by the motor 41, enabling the first conveying belt 44 to provide power for the rotation of the stirring main shaft 8, namely using the stirring blades 81 on the stirring main shaft 8 to stir uniformly, slowly adding acetaminophen ether, transferring a catalyst, driving the second conveying belt 45 by rotation, enabling the second conveying belt 45 to drive the input end of the double-turbine worm reduction box 46, enabling the output end of the double-turbine worm reduction box 46 to drive the third conveying belt 47 to move, enabling the third conveying belt 47 to drive the first rotating shaft 59 to rotate, enabling the speed of the first rotating shaft 59 to be reduced by multistage speed reduction, improving the stability of movement, enabling the first rotating shaft 59 to rotate, enabling the first fixed plate 541 to drive the third rod 542 to rotate, enabling the driving control rod 53 to rotate, enabling the second disc to be driven by the driving control rod 53, enabling the third rod 542 to be driven by the cooperation of the third guide block 524 and the second guide block 523 to drive the driving rod 546 to move up and down, enabling the third rod 542 to move down and the first push plate 551 to move down, enabling the first rod 542 to move down to the hollow push plate 551 to move down, and enabling the hollow push plate 551 to move down to be in a staggered mode, and enabling the hollow rod 551 to move down to the first rod push plate to move down to the hollow plug to be reversely, and the hollow rod 551 to move down; the hollow rod 547 stops after striking the threaded plate 551, the hollow rod 547 drives the threaded plate 551 to move downwards for a short distance, the threaded plate 551 drives the threaded rod 552 to rotate through threaded connection with the threaded rod 552, the threaded rod 552 rotates to drive the first gear 5542 to rotate, then the first gear 5542 drives the second gear 5543 to rotate, the second gear 5543 rotates to drive the seventh rod 5551 to rotate, the seventh rod 5551 drives the baffle 5553 to rotate in the first rod 56 through the ninth guide block 5552 and the tenth guide block 5554, and the ninth guide block 5552 and the tenth guide block 5554 enable rotation to be more stable; the first control component 63 of the air control component 55 can open the first through holes 561 once starting to rotate, so that the air in the first rod pieces 56 can be blown outwards faster, inert air can be blown to the bottom surface of the reaction kettle 2 directly in the first through holes 561 on the two first rod pieces 56, then inert air in the other two first rod pieces 56 can be blown to the connecting pipe 562 through the first through holes 561 and then to the air storage cavity 571, and blown between the two cleaning pieces 61 through the second through holes 572, thereby better controlling, when the telescopic component 54 is reset, the screw plate 551 is reset through the fourth spring 553, the first rotating shaft 59 can drive the first connecting rod 58 to rotate, the first connecting rod 58 drives the fourth guide block 636 to move together, thereby enabling the second connecting rod 62 to move together, the second connecting rod 62 is continuously matched with the arc-shaped guide block 9 during movement, so that the second connecting rod 62 is driven to slide in the fourth guide block 636 under the action of the arc-shaped guide block 9, the second connecting rod 62 is driven to reciprocate and not to be blocked due to the fact that three arc-shaped guide blocks 9 exist, the second rotating shaft 631 is driven to move together by sliding of the second connecting rod 62, the fourth connecting rod 632 is driven to move by the second rotating shaft 631, the fourth connecting rod 632 moves under the matching of the fourth rod 634 and the first sliding groove 633, namely, the hinged position of the fourth connecting rod 632 and the second rotating shaft 631 rotates at an angle, so that the second rotating shaft 631 reciprocates and simultaneously drives the second rotating shaft 631 to reciprocate, and the second rotating shaft 631 drives the cleaning element 61 to perform the same movement; the cleaning member 61 can slide back and forth and simultaneously rotate back and forth, so that the reaction raw materials and catalysis on the bottom surface of the reaction kettle 2 can be better cleaned;
The first link 58 drives the extrusion device 7 to move together, then the sixth rod 716 is continuously matched with the arc-shaped guide block 9 to move the sixth guide block 712 towards the seventh guide block 714 under the action of the arc-shaped guide block 9, the sixth guide blocks 712 on two sides move together due to the symmetrical arrangement of the arc-shaped guide block 9, the sixth guide block 712 drives the seventh guide block 714 to move together through the fifth rod 713, so that the two eighth guide blocks 715 on the fifth guide block 711 move oppositely at the same time, the fifth link 721 and the sixth link 722 are driven to move together, the plurality of fifth links 721 and the plurality of sixth links 722 which are prevented from being overlapped together are unfolded to enable the second pin 723 to move upwards, the plurality of second pins 723 move upwards to be the same as the distance between the plurality of second pins, and increase simultaneously, and then the second pin 723 drives the lifting pin 723 fixed on the second extrusion plate 723 to move upwards to separate from the extrusion plate 73, and the lifting assembly 723 moves upwards to be matched with the arc-shaped guide plate 73 to move downwards, so that the lifting assembly 723 is reset under the action of the arc-shaped guide plate 73;
After that, the worker can open the discharge chute 21 to replace the cleaning member 61, and the stirring main shaft 8 and the first rotating shaft 59 are ensured not to rotate at all during the replacement, which is because the electromagnet 436 is powered off to enable the clamping plate 432 to clamp the clamping plate 431 under the action of the second spring 435, so that the rotation is not generated, and the safety of the worker during the replacement is improved.
It will be apparent that the described embodiments are only some, but not all, embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the present invention without making any inventive effort, shall fall within the scope of the present invention.
Claims (8)
1. The synthesis method of the high-purity 2-nitro-4-acetamido anisole is characterized by comprising the following steps: synthesizing 2-nitro-4-acetamido anisole by using a pipeline; the assembly line comprises a reaction device, a discharging device and a cleaning device; the synthesis steps are as follows: A. the reaction raw materials are put into a reaction device for reaction; the reaction device comprises a first bracket (1), a reaction kettle (2) arranged above the first bracket (1) and used for containing raw materials, extraction barrels (3) arranged on two sides of the reaction kettle (2), a stirring main shaft (8) arranged inside the reaction kettle (2), a bottom cleaning device (5) connected with the stirring main shaft (8), a cleaning device (6) arranged below the bottom cleaning device (5), an extrusion device (7) arranged above the cleaning device (6), a driving device (4) arranged above the reaction kettle (2) and used for driving the bottom cleaning device (5) and the stirring main shaft (8), and an arc-shaped guide block (9) arranged on the inner wall of the reaction kettle (2) and matched with the cleaning device (6) and the extrusion device (7); the method comprises the following specific steps: adding concentrated sulfuric acid into a reaction kettle (2), adding tetra-n-butyl ammonium chloride, uniformly stirring the mixture by using a stirring main shaft (8), and slowly adding acetaminophen ether and a phase transfer catalyst; B. uniformly stirring the phase transfer catalyst and the reaction raw materials by using a bottom cleaning device (5); the bottom cleaning device (5) comprises a first gas storage tank (51) arranged above the reaction kettle (2), a power assembly (52) arranged inside the first gas storage tank (51), a first rotating shaft (59) communicated with the first gas storage tank (51) and arranged inside the reaction kettle (2), a driving control rod piece (53) arranged inside the first rotating shaft (59) and matched with the power assembly (52), a telescopic assembly (54) arranged inside the first rotating shaft (59) and matched with the driving control rod piece (53), a first rod piece (56) arranged below the first rotating shaft (59) and communicated with the first rotating shaft (59), and a gas control assembly (55) arranged inside the first rotating shaft (59) and the first rod piece (56) and matched with the telescopic assembly (54); the method comprises the following specific steps: the driving device (4) drives the first rotating shaft (59) to rotate, the first rotating shaft (59) drives the power component (52) to rotate, the power component (52) drives the control rod piece (53) to move, the control rod piece (53) drives the telescopic component (54) to move, inert gas in the first rotating shaft (59) is compressed when the telescopic component (54) moves to the gas control component (55), the gas control component (55) is driven to move when the telescopic component (54) moves to the gas control component (55), the inert gas in the first rotating shaft (59) can be blown outwards at the first rod piece (56) and blown to the bottom of the reaction kettle (2), so that catalyst and raw materials at the bottom of the reaction kettle (2) are better evenly distributed, and then the inert gas in the first rotating shaft (59) is supplemented by the first gas storage tank (51); C. cleaning the bottom of the reaction kettle (2) by using a cleaning device (6); D. the extrusion device (7) is used for pushing up and down the catalyst and the reaction raw materials which are cleaned and blown up by the cleaning device (6) and the bottom cleaning device (5); E. extracting a product in the reaction liquid by using an extraction barrel (3) and continuously returning the extracted reactant to the reaction kettle (2); F. discharging all reactants by using a discharging device; G. and (5) cleaning the reaction liquid by using a cleaning device to obtain a finished product.
2. The method for synthesizing high-purity 2-nitro-4-acetamidoanisole according to claim 1, wherein the method comprises the steps of: the bottom cleaning device (5) further comprises a first through hole (561) which is arranged below the first rod piece (56) and is mutually communicated with the reaction kettle (2), a first connecting rod (58) which is arranged below the first rod piece (56) and fixedly connected with the first rotating shaft (59), a second gas storage box (57) which is arranged between the first connecting rod (58) and the first rod piece (56), a connecting pipe (562) which is arranged between the second gas storage box (57) and the first through hole (561) and is used for communicating the first through hole (561) and the second gas storage box (57), a gas storage cavity (571) which is arranged in the second gas storage box (57) and is mutually communicated with the first rod piece (56), and a second through hole (572) which is arranged on the first connecting rod (58) and is used for mutually communicating the gas storage cavity (571) and the reaction kettle (2); the cleaning device (6) comprises a second connecting rod (62) arranged below the first connecting rod (58), a cleaning piece (61) connected to the second connecting rod (62), and a first control assembly (63) arranged below the first connecting rod (58) and used for driving the second connecting rod (62) and the cleaning piece (61) to move; the cleaning pieces (61) are uniformly distributed below the first connecting rods (58); a plurality of second through holes (572) are formed in the first connecting rod (58); are uniformly arranged between the two cleaning pieces (61); four first bars (56); uniformly arranged on the first rotating shaft (59); wherein two first bars (56) are connected to the first bars (58); the method comprises the following specific steps: the first rotating shaft (59) can drive the first rod piece (56) to move when moving, the first rotating shaft (59) can also drive the second gas storage box (57) to move together with the first connecting rod (58), the first connecting rod (58) can drive the cleaning piece (61) to move, the cleaning piece (61) cleans the bottom surface of the reaction kettle (2), then the rotation of the first connecting rod (58) can enable the cleaning piece (61) to clean the bottom surface of the reaction kettle (2) more, then the expansion assembly (54) can enable inert gas to be blown out of the first through hole (561) through the control of the gas control assembly (55) when compressing the inert gas in the first rotating shaft (59), the inert gas can be blown out of the first through hole (561) on the two first rod pieces (56) and directly blown onto the bottom surface of the reaction kettle (2), and then the inert gas in the other two first rod pieces (56) can be blown into the connecting pipe (562) through the first through hole (561) and then into the gas storage cavity (571) through the second through hole (61).
3. The method for synthesizing high-purity 2-nitro-4-acetamidoanisole according to claim 2, wherein the method comprises the steps of: the air control assembly (55) comprises a threaded plate (551) arranged in the first rotating shaft (59) in a sliding manner, a threaded rod (552) connected to the threaded plate (551), a fourth spring (553) arranged below the threaded rod (552) and used for supporting the threaded rod (552), a transmission part (554) arranged below the fourth spring (553) and used for guiding the threaded rod (552), and a control part (555) connected to the transmission part (554) and positioned in the first rod piece (56); the transmission part (554) comprises a fourth fixed plate (5541) fixedly arranged in the first rotating shaft (59), a first gear (5542) fixedly arranged below the threaded rod (552), a second gear (5543) meshed with the first gear (5542), a third rotating shaft (5544) fixedly connected with the second gear (5543), and a supporting block (5545) arranged below the first gear (5542) and rotationally connected with the threaded rod (552) and the supporting block (5545) for supporting; the thread plate (551) is in threaded connection with the threaded rod (552); the method comprises the following specific steps: the telescopic component (54) drives the threaded plate (551) to move downwards, the threaded plate (551) drives the threaded rod (552) to rotate through being connected with the threaded rod (552) in a threaded mode, the threaded rod (552) rotates to drive the first gear (5542) to rotate, then the first gear (5542) drives the second gear (5543) to rotate, the second gear (5543) rotates to drive the control component (555) to move, the control component (555) controls the opening and closing states of the first through hole (561), and when the telescopic component (54) resets, the threaded plate (551) resets through the fourth spring (553).
4. The method for synthesizing high-purity 2-nitro-4-acetamidoanisole according to claim 3, wherein the method comprises the steps of: the control part (555) comprises a seventh rod piece (5551) fixedly connected with the second gear (5543), a ninth guide block (5552) fixedly connected with the seventh rod piece (5551), a baffle plate (5553) fixedly connected with the ninth guide block (5552) and rotationally arranged in the first rod piece (56), and a tenth guide block (5554) fixedly connected with the tenth guide block (5554); the ninth guide block (5552) and the transmission part (554) are rotatably connected to the first rod piece (56); the angle of the baffle plate (5553) is used for blocking the first through hole (561); the baffle (5553) rotates to open the first through hole (561); the method comprises the following specific steps: the second gear (5543) rotates to drive the seventh rod piece (5551) to rotate, the seventh rod piece (5551) drives the baffle plate (5553) to rotate in the first rod piece (56) through a ninth guide block (5552) and a tenth guide block (5554), and the ninth guide block (5552) and the tenth guide block (5554) enable rotation to be stable; the first control member (63) of the air control member (55) opens the first through hole (561) upon starting rotation.
5. The method for synthesizing high-purity 2-nitro-4-acetamidoanisole according to claim 4, wherein the method comprises the steps of: the telescopic assembly (54) comprises a fourth fixed plate (5541) fixedly connected to the first rotating shaft (59), a third rod (542) which is slidably arranged in the first fixed plate (541) and connected to the power assembly (52), two second fixed plates (544) fixedly connected below the first fixed plate (541), a plurality of third connecting rods (545) which are connected with the second fixed plates (544) in a staggered manner, a first pin roll (543) at the hinge point of the third rod (542) and one third connecting rod (545), a first push plate (546) arranged below the third connecting rod (545), and a hollow rod (547) which is fixedly arranged below the first push plate (546) and matched with the threaded plate (551); two identical second fixing plates (544) are arranged below the third connecting rod (545); the lower second fixing plate (544) is connected to the first push plate (546); the method comprises the following specific steps: the power assembly (52) drives the third rod piece (542) to move downwards, the third rod piece (542) drives the first pin shaft (543) to move downwards, the first pin shaft (543) can drive the plurality of third connecting rods (545) which are arranged in a staggered mode to move, and accordingly the third connecting rods (545) are unfolded from a stacked state, the first push plate (546) is driven to move downwards, the first push plate (546) drives the hollow rod piece (547) to move downwards, and the hollow rod piece (547) is impacted to the threaded plate (551) to drive the threaded plate (551) to move downwards; the hollow rod (547) stops after impacting the threaded plate (551), and the hollow rod (547) drives the threaded plate (551) to move downwards for a short distance.
6. The method for synthesizing high-purity 2-nitro-4-acetamidoanisole according to claim 5, wherein the method comprises the steps of: the power assembly (52) comprises a second rod (521) fixedly arranged in the first gas storage tank (51), a first disc (522) fixedly arranged below the second rod (521), a plurality of second guide blocks (523) fixedly arranged on the first disc (522), a second disc (525) fixedly arranged above the driving control rod (53), a third guide block (524) fixedly arranged above the second disc (525) and matched with the second guide block (523), and a third spring (526) arranged below the second disc (525) and used for propping against the second disc (525) to reset the second disc; the driving control rod piece (53) is fixedly connected to the third rod piece (542); the method comprises the following specific steps: the driving device (4) drives the first rotating shaft (59) to rotate, the first rotating shaft (59) rotates to drive the first fixed plate (541) to rotate, the first fixed plate (541) drives the third rod piece (542) to rotate, so that the driving control rod piece (53) rotates, the driving control rod piece (53) drives the second disc (525), and the driving control rod piece (53) is driven to reciprocate up and down through the cooperation of the third guide block (524) and the second guide block (523).
7. The method for synthesizing high-purity 2-nitro-4-acetamidoanisole according to claim 2, wherein the method comprises the steps of: the first control assembly (63) comprises a fourth guide block (636) fixedly arranged below the first connecting rod (58), a second rotating shaft (631) rotatably connected with the second connecting rod (62) and fixedly connected with the cleaning piece (61) for supporting the cleaning piece (61), a fourth connecting rod (632) hinged with the second rotating shaft (631), a third fixing plate (635) fixedly connected with the first connecting rod (58), a fourth rod piece (634) fixedly connected with the third fixing plate (635), and a first chute (633) arranged on the fourth connecting rod (632) and slidably connected with the fourth rod piece (634); the second connecting rod (62) is connected to the fourth guide block (636) in a sliding manner; an elastic metal strip is arranged in the cleaning piece (61); the arc-shaped guide blocks (9) are multiple; the arc-shaped guide blocks (9) matched with the cleaning device (6) are positioned at the same height as the second connecting rod (62), and three arc-shaped guide blocks are uniformly distributed on the inner wall of the reaction kettle (2); the method comprises the following specific steps: the first connecting rod (58) drives the fourth guide block (636) to move together, so that the second connecting rod (62) moves together, the second connecting rod (62) is continuously matched with the arc-shaped guide block (9) during movement, the second connecting rod (62) is driven to slide in the fourth guide block (636) under the action of the arc-shaped guide block (9), the arc-shaped guide block (9) can drive the second connecting rod (62) to reciprocate and can not be blocked, the second connecting rod (62) slides to drive the second rotating shaft (631) to move together, then the second rotating shaft (631) drives the fourth connecting rod (632) to move, the fourth connecting rod (632) moves under the cooperation of the fourth rod (634) and the first sliding groove (633), namely, the hinged position of the fourth connecting rod (632) and the second rotating shaft (631) can rotate at an angle, the second rotating shaft (631) can reciprocate, and the second rotating shaft (631) can be driven to reciprocate, and the second rotating shaft (631) can also be driven to reciprocate, so that the second rotating shaft (631) can drive the second rotating shaft (61) to perform the same cleaning motion.
8. The method for synthesizing high-purity 2-nitro-4-acetamidoanisole according to claim 1, wherein the method comprises the steps of: the driving device (4) comprises a second bracket (42) fixedly arranged above the reaction kettle (2), a motor (41) fixedly arranged above the second bracket (42), a first conveying belt (44) fixedly connected to the output end of the motor (41), a second conveying belt (45) connected to the stirring main shaft (8), a double-turbine worm reduction gearbox (46) connected to the second conveying belt (45), a third conveying belt (47) connected to the double-turbine worm reduction gearbox (46), a brake component (43) connected to the motor (41), a plurality of discharging blocks (48) arranged on the reaction kettle (2) and used for charging, and two discharging grooves (21) arranged below the reaction kettle (2), wherein the third conveying belt (47) is connected to the bottom cleaning device (5); the brake assembly (43) comprises a first guide block (433) fixedly arranged above the reaction kettle (2), a first guide rod (434) slidably arranged in the first guide block (433), a clamping plate (432) fixedly arranged on the first guide rod (434), a second spring (435) arranged between the clamping plate (432) and the first guide block (433), an electromagnet (436) arranged on the clamping plate (432) and the first guide block (433), and a clamping toothed plate (431) arranged at the output end of the motor (41) and matched with the clamping plate (432); the third conveyor belt (47) is connected to the first shaft (59); a plurality of stirring blades (81) for stirring are arranged on the stirring main shaft (8); the method comprises the following specific steps: the motor (41) drives the first conveyer belt (44) to move, the first conveyer belt (44) provides power for the rotation of the stirring main shaft (8), the rotation of the stirring main shaft (8) can drive the second conveyer belt (45), the second conveyer belt (45) drives the input end of the double-turbine worm reduction gearbox (46), the output end of the double-turbine worm reduction gearbox (46) drives the third conveyer belt (47) to move, the third conveyer belt (47) drives the first rotating shaft (59) to rotate, and the first conveyer belt (44), the second conveyer belt (45) and the third conveyer belt (47) are in speed-reducing transmission, so that the speed of the first rotating shaft (59) is slowed down through multistage speed reduction.
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