CN113651713A - Synthesis method of high-purity 2-nitro-4-acetamino anisole - Google Patents
Synthesis method of high-purity 2-nitro-4-acetamino anisole Download PDFInfo
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- CN113651713A CN113651713A CN202110952926.0A CN202110952926A CN113651713A CN 113651713 A CN113651713 A CN 113651713A CN 202110952926 A CN202110952926 A CN 202110952926A CN 113651713 A CN113651713 A CN 113651713A
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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 abstract description 25
- 238000001308 synthesis method Methods 0.000 title claims description 4
- 238000006243 chemical reaction Methods 0.000 claims abstract description 177
- 238000004140 cleaning Methods 0.000 claims abstract description 120
- 238000003756 stirring Methods 0.000 claims abstract description 57
- 238000000034 method Methods 0.000 claims abstract description 54
- 239000002994 raw material Substances 0.000 claims abstract description 39
- 239000003054 catalyst Substances 0.000 claims abstract description 29
- 238000007599 discharging Methods 0.000 claims abstract description 21
- 230000002194 synthesizing effect Effects 0.000 claims abstract description 14
- 239000003444 phase transfer catalyst Substances 0.000 claims abstract description 11
- 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
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 53
- 239000007789 gas Substances 0.000 claims description 46
- 238000001125 extrusion Methods 0.000 claims description 44
- 239000011261 inert gas Substances 0.000 claims description 39
- 238000003860 storage Methods 0.000 claims description 35
- 230000033001 locomotion Effects 0.000 claims description 24
- 230000009467 reduction Effects 0.000 claims description 21
- XVAIDCNLVLTVFM-UHFFFAOYSA-N methacetin Chemical compound COC1=CC=C(NC(C)=O)C=C1 XVAIDCNLVLTVFM-UHFFFAOYSA-N 0.000 claims description 19
- 230000005540 biological transmission Effects 0.000 claims description 16
- 230000009471 action Effects 0.000 claims description 14
- 239000012295 chemical reaction liquid Substances 0.000 claims description 6
- NHGXDBSUJJNIRV-UHFFFAOYSA-M tetrabutylammonium chloride Chemical compound [Cl-].CCCC[N+](CCCC)(CCCC)CCCC NHGXDBSUJJNIRV-UHFFFAOYSA-M 0.000 claims description 6
- 239000002184 metal Substances 0.000 claims description 3
- 230000003116 impacting effect Effects 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract 1
- 239000000047 product Substances 0.000 description 17
- 238000006722 reduction reaction Methods 0.000 description 17
- 238000004128 high performance liquid chromatography Methods 0.000 description 12
- 230000008569 process Effects 0.000 description 12
- 238000006396 nitration reaction Methods 0.000 description 11
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 8
- 229910017604 nitric acid Inorganic materials 0.000 description 8
- 230000036632 reaction speed Effects 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- 238000000429 assembly Methods 0.000 description 6
- 230000000712 assembly Effects 0.000 description 6
- -1 guanidine compound Chemical class 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 238000007086 side reaction Methods 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
- 238000006555 catalytic reaction Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- CMYGXBVASMFDBY-UHFFFAOYSA-N n-(4-methoxy-2,5-dinitrophenyl)acetamide Chemical compound COC1=CC([N+]([O-])=O)=C(NC(C)=O)C=C1[N+]([O-])=O CMYGXBVASMFDBY-UHFFFAOYSA-N 0.000 description 4
- 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 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000007865 diluting Methods 0.000 description 3
- 239000012065 filter cake Substances 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 238000005984 hydrogenation reaction Methods 0.000 description 3
- 239000005457 ice water Substances 0.000 description 3
- 239000011780 sodium chloride Substances 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- CHJJGSNFBQVOTG-UHFFFAOYSA-N N-methyl-guanidine Natural products CNC(N)=N CHJJGSNFBQVOTG-UHFFFAOYSA-N 0.000 description 2
- ZRALSGWEFCBTJO-UHFFFAOYSA-N anhydrous guanidine Natural products NC(N)=N ZRALSGWEFCBTJO-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000007795 chemical reaction product Substances 0.000 description 2
- 230000006835 compression Effects 0.000 description 2
- 238000007906 compression Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- SWSQBOPZIKWTGO-UHFFFAOYSA-N dimethylaminoamidine Natural products CN(C)C(N)=N SWSQBOPZIKWTGO-UHFFFAOYSA-N 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 239000000975 dye Substances 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000012452 mother liquor Substances 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 238000004537 pulping Methods 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000013589 supplement Substances 0.000 description 2
- CZGCEKJOLUNIFY-UHFFFAOYSA-N 4-Chloronitrobenzene Chemical compound [O-][N+](=O)C1=CC=C(Cl)C=C1 CZGCEKJOLUNIFY-UHFFFAOYSA-N 0.000 description 1
- 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
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000000987 azo dye Substances 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000007810 chemical reaction solvent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000002270 dispersing agent Substances 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
- 239000010808 liquid waste 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
- 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
- 238000003825 pressing Methods 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 150000003242 quaternary ammonium salts Chemical class 0.000 description 1
- 238000011946 reduction process Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 1
- 238000010408 sweeping Methods 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
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Classifications
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- 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
Abstract
The invention discloses a method for synthesizing high-purity 2-nitro-4-acetamino anisole, which synthesizes 2-nitro-4-acetamino 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. putting the reaction raw materials 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. pushing the catalyst and the reaction raw materials which are cleaned and blown up by the cleaning device and the bottom cleaning device up and down by using the extruding device; E. extracting the product in the reaction solution by using an extraction barrel and continuously returning the extracted reaction to the reaction kettle; F. discharging the reaction completely by using a discharging device; G. and cleaning the reaction solution 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 synthesis method of high-purity 2-nitro-4-acetamino anisole.
Background
The 2-amino-4-acetamino anisole is an important intermediate for synthesizing azo dyes, is mainly used for synthesizing dispersant dark blue HGL and the like, and the currently adopted process route is that p-nitrochlorobenzene is used as a raw material and is prepared by methoxylation, hydrogenation reduction, acetylation, nitration and hydrogenation reduction, wherein the nitration process is prepared by using sulfuric acid as a solvent and nitric acid as a nitrating agent, a batching kettle is used for preparing sulfuric acid, acetyl is slowly added while cooling, the temperature is controlled, the nitric acid is slowly dropped for reaction, after the reaction is finished, the reaction liquid is dropped into cold water, products are separated out, the products are filtered, waste acid is sent to a concentration workshop for recovering the sulfuric acid, wet products are washed to be neutral by water, and after centrifugation, the wet products are added with methanol for pulping and are used for the hydrogenation reduction process;
wherein, sulfonation side reaction can occur in the pulping and dissolving process of the sulfuric acid and the p-acetamino anisole; there are documents (Liudong et al, dye and dye, 53,5, 34-47) that nitration impurities are minimum at a sulfuric acid concentration of 93%, but the amplification effect of actual industrial production is that for a nitration product workshop producing 2 million tons per year, due to the increase of the feeding amount, the time for dissolving p-acetamino anisole (50 tons) in each batch is as long as several hours, and meanwhile, the cooling process from the completion of dissolving p-acetamino anisole to the dropwise addition of nitric acid is also very 1-2 hours, at present, 93% sulfuric acid is used as a reaction solvent, and a sample is taken for analysis before the dropwise addition of nitric acid, wherein the content of a sulfonated substance is more than 5%, so that the nitration product has low purity and low yield; in the nitration process, two positions of 2 and 3 can be nitro, and 3-nitro-4-acetamino anisole and 2, 5-dinitro-4-acetamino anisole can also be generated; the by-product generated by the reaction is dissolved in dilute sulfuric acid, which brings inconvenience to the subsequent concentration of the 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 thorough degree of the reaction are influenced.
Disclosure of Invention
In order to overcome the defects of the prior art, the method reduces the concentration of sulfuric acid in the dissolving process of dissolving p-acetamino anisole, uses 80% sulfuric acid as a solvent in the dissolving process, adds a phase transfer catalyst in the dissolving process to promote the dissolution of p-acetamino anisole, reduces the dissolving time, adds a catalyst in the phase transfer catalyst position quaternary ammonium salt, and inhibits the occurrence of a side reaction of 3-position nitration by adding the catalyst in the nitration process.
In order to achieve the purpose, the invention adopts the following technical scheme: a method for synthesizing high-purity 2-nitro-4-acetamino anisole, which uses a flow line to synthesize the 2-nitro-4-acetamino anisole; the assembly line comprises a reaction device, a discharging device and a cleaning device; the synthesis steps are as follows: A. putting the reaction raw materials into a reaction device for reaction; the reaction device comprises a first support, a reaction kettle arranged above the first support and used for containing raw materials, extraction barrels arranged on two sides of the reaction kettle, a stirring main shaft arranged in the reaction kettle, a bottom cleaning device connected to the stirring main shaft, a cleaning device arranged below the bottom cleaning device, an extrusion device arranged above the cleaning device, a driving device arranged above the reaction kettle and used for driving the bottom cleaning device and the stirring main shaft, and an arc-shaped guide block arranged on the inner wall of the reaction kettle and matched with the cleaning device and the extrusion device; the method comprises the following specific steps: adding concentrated sulfuric acid into a reaction kettle, adding tetra-n-butyl ammonium chloride, uniformly stirring by using a stirring main shaft, and slowly adding p-acetamino anisole 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 communicated with the first gas storage tank and arranged in the reaction kettle, a drive control rod piece arranged in the first rotating shaft and matched with the power assembly, a telescopic assembly arranged in the first rotating shaft and matched with the drive control rod piece, a first rod piece arranged below the first rotating shaft and communicated with the first rotating shaft, and a gas control assembly 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 driving control rod to move, the driving control rod drives the telescopic assembly to move, the telescopic assembly moves to compress the inert gas in the first rotating shaft, the telescopic assembly drives the gas control assembly to move when moving to the gas control assembly, the gas control assembly moves to blow the inert gas in the first rotating shaft outwards at the first rod and blow the inert gas at the bottom of the reaction kettle, so that the catalyst and raw materials at the bottom of the reaction kettle are better and uniformly distributed, and then the first gas storage tank supplements the inert gas in the first rotating shaft; C. cleaning the bottom of the reaction kettle by using a cleaning device; D. pushing the catalyst and the reaction raw materials which are cleaned and blown up by the cleaning device and the bottom cleaning device up and down by using the extruding device; E. extracting the product in the reaction solution by using an extraction barrel and continuously returning the extracted reaction to the reaction kettle; F. discharging the reaction completely by using a discharging device; G. cleaning the reaction solution by using a cleaning device to obtain a finished product;
by adding the catalyst, the reaction speed is improved, then the extraction barrel can continuously filter out the reaction product, so that the proportion of reactants in the reaction kettle can be reduced in the catalytic reaction, a balanced state can exist in the catalytic reaction, the reaction can not reach the balanced state by reducing the proportion of the reactants, the reaction is more thorough, then the stirring main shaft can stir the inside of the reaction kettle, the reaction speed is further improved, the cleaning device can clean the bottom of the reaction kettle, the reaction raw materials and the catalyst at the bottom of the reaction kettle can be better rolled up by the stirred liquid, the uniform state of the reaction raw materials and the catalyst in the liquid is better improved, the reaction raw materials and the catalyst are better and uniformly distributed in the reaction kettle, the contact area of the reaction is improved, and the reaction raw materials and the catalyst can not be gathered together, influence the problem of reaction speed, thereby the reaction speed who makes this reaction still improves the degree of reaction when improving, make the reaction more thorough, later cleaning device can be continuous blows off inert gas to reation kettle's bottom, inert gas can not react with concentrated sulfuric acid, thereby the stability of reaction has been guaranteed, later inert gas blows and can form the bubble upwards to move at reation kettle's bottom, thereby can be better take the reacting material and the catalyst of reation kettle bottom to the top, thereby better by stirring main shaft stirring, thereby further improved the degree of evenly distributed in reation kettle, thereby better speed that has improved the reaction makes the reaction more thorough, further increase the degree of homogeneity of catalyst and reacting material in reation kettle through extrusion device, thereby make the reaction more thorough, thereby can be better improvement reation kettle-nitro-drive arrangement-acetamidophenyl ether content in the reaction.
The bottom cleaning device comprises a reaction kettle, a first rod, a second air storage tank, a connecting pipe, an air storage cavity and a second through hole, wherein the reaction kettle is arranged in the reaction kettle; the cleaning device comprises a second connecting rod arranged below the first connecting rod, a cleaning piece connected to the second connecting rod, and a first control assembly 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; a plurality of second through holes are formed in the first connecting rod; are uniformly arranged between the two cleaning pieces; the number of the first rod pieces is four; are 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 can drive the first rod pieces to move when moving, the second gas storage box and the first connecting rod can be driven to move together by the first rotating shaft, the first connecting rod can drive the cleaning pieces to move, the cleaning pieces clean the bottom surface of the reaction kettle, then the cleaning pieces can clean the bottom surface of the reaction kettle more by the rotation of the first connecting rod, when the inert gas in the first rotating shaft is compressed by the telescopic assembly, the inert gas can be blown out of the first through holes outwards under the control of the gas control assembly, the inert gas can be directly blown to the bottom surface of the reaction kettle in the first through holes on the two first rod pieces, and then the inert gas in the other two first rod pieces can flow to the connecting pipe through the first through holes and then flow into the gas storage cavity and can be blown between the two cleaning pieces through the second through holes;
through the evenly distributed of a plurality of cleaning pieces, the scope that cleaning pieces cleaned has been increased, make reaction raw materials and catalyst can be better rolled up, thereby better evenly distributed is in reation kettle, then 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 giving vent to anger very little, later first member and first connecting rod also can be rotatory, thereby the scope of inert gas is blown out to the bottom surface of reation kettle to the messenger that can be better, thereby further increase the degree of reaction.
The gas control assembly comprises a threaded plate, a threaded rod, a fourth spring, a transmission component and a control component, wherein the threaded plate is arranged in the first rotating shaft in a sliding mode, the threaded rod is connected to the threaded plate, the fourth spring is arranged below the threaded rod and used for propping against the threaded rod, the transmission component is arranged below the fourth spring and used for guiding the threaded rod, and the control component is connected to the transmission component and located in the first rod piece; 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 to the second gear, and a supporting block arranged below the first gear and rotatably connected to the threaded rod and the supporting block for supporting; the threaded plate is in threaded connection with the threaded rod; the method comprises the following specific steps: the telescopic assembly 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 can drive the first gear to rotate through rotation, then the first gear drives the second gear to rotate, the second gear can drive the control part to move through rotation, the control part controls the opening and closing state of the first through hole, and when the telescopic assembly resets, the threaded plate resets through the fourth spring;
make the control unit move through drive disk assembly's motion, thereby make the open-close state of first through-hole and drive disk assembly's motion combine together each other, and drive disk assembly is used for compressing inert gas, thereby inert gas just can open at the first through-hole under the circumstances of compression, thereby better messenger's inert gas goes out outwards to blow off at first through-hole, thereby further improved the inert gas's that blows off dynamics, thereby can be better blow reaction raw materials and catalyst on the reation kettle bottom surface, further make more even that both distribute, thereby further improve the reaction rate and react more thoroughly.
Specifically, the control part comprises a seventh rod piece fixedly connected to the second gear, a ninth guide block fixedly connected to the seventh rod piece, a baffle fixedly connected to the ninth guide block and rotatably arranged in the first rod piece, and a tenth guide block fixedly connected to the tenth guide block; the ninth guide block and the transmission component are rotationally connected to the first rod piece; the baffle has only a little 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 through hole is opened by the first control assembly of the air control assembly once the first control assembly starts to rotate, so that air in the first rod piece can be blown out more quickly, and the control is better.
Specifically, the telescopic assembly comprises a fourth fixed plate fixedly connected to the first rotating shaft, a third rod piece slidably arranged in the first fixed plate and connected to the power assembly, two second fixed plates fixedly connected to the lower portion of the first fixed plate, a plurality of third connecting rods connected to the second fixed plates in a staggered manner, a first pin shaft serving as a hinge point of the third rod piece and one of the third connecting rods, a first push plate arranged below the third connecting rod, and a hollow rod piece 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 lower second fixing plate is connected with the first push 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 can drive a plurality of third connecting rods which are arranged in a staggered mode to move, and therefore the third connecting rods are unfolded from a stacked state, the first push plate can be driven to move downwards, the first push plate drives the hollow rod piece to move downwards, and the hollow rod piece impacts the threaded plate to drive the threaded plate to move downwards; the hollow rod stops after impacting the threaded plate, and the hollow rod drives the threaded plate to move downwards for a short distance;
thereby just can drive the threading board downstream when moving the below through first push pedal, thereby realized that first push pedal now compresses the inert gas in the subassembly arc guide block that stretches out and draws back, thereby can make the pressure increase in subassembly arc guide block and the first member of stretching out and drawing back, later accuse gas subassembly moves and can make inert gas outwards blow out under the effect of pressure rapidly when making first through-hole open, thereby further improved inert gas and blown the speed on the reation kettle bottom surface, thereby better improvement reaction speed and make more thorough of reaction.
The power assembly comprises a second rod piece fixedly arranged in the first air storage box, 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 drive 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 abutting against the second disc to reset the third spring; the driving control rod piece is fixedly connected to the third rod piece; the method comprises the following specific steps: the first pivot of drive arrangement drive is rotatory, it is rotatory that first pivot rotation can drive first fixed plate, first fixed plate drives the third member and rotates, thereby can make the drive control member rotate, the drive control member drives the second disc, the cooperation through third guide block and second guide block can drive the motion of reciprocating from top to bottom of drive control member, thereby can drive the inert gas's in the first pivot of first push pedal compression motion to the third member motion and provide power.
Specifically, the first control assembly comprises a fourth guide block fixedly arranged below the first connecting rod, a second rotating shaft rotatably connected to the second connecting rod and fixedly connected to the cleaning piece for supporting the cleaning piece, a fourth connecting rod hinged to the second rotating shaft, a third fixing plate fixedly connected to the first connecting rod, a fourth rod fixedly connected to the third fixing plate, and a first sliding 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 mode; an elastic metal strip is arranged inside the cleaning piece; the number of the arc-shaped guide blocks is 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 can move together, the second connecting rod can be continuously matched with the arc-shaped guide block during movement, thereby driving the second connecting rod to slide in the fourth guide block under the action of the arc-shaped guide blocks, and as the number of the arc-shaped guide blocks is three, so the second connecting rod can be driven to do reciprocating motion and can not be blocked, the second connecting rod can drive the second rotating shaft to do motion together when sliding, then the second rotating shaft drives the fourth connecting rod to do motion, the fourth connecting rod can do motion under the matching of the fourth rod piece and the first chute, namely the position where the fourth connecting rod is hinged with the second rotating shaft can rotate by an angle, so that the second rotating shaft can be driven to rotate in a reciprocating manner while reciprocating, and the second rotating shaft drives the cleaning piece to do the same motion; cleaning member can carry out reciprocating rotation in reciprocating sliding, reaction raw material and catalysis on the reation kettle bottom that can be better add and clean, 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 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 which is used for driving the extrusion plates to move along with the two steps, the second control assembly and the extrusion plates; a plurality of third through holes are formed in the extrusion plate; the lifting assembly comprises a fifth connecting rod and a sixth connecting rod which are connected to the second control assembly in a staggered mode, a second pin shaft connected to 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 at 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; the two second control assemblies are distributed on two sides of the first connecting rod; the fifth rod piece is connected to the sixth guide block in one second control assembly and is connected with the 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 assemblies 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 piece continuously cooperates with the arc-shaped guide blocks when moving, so that the sixth guide blocks are driven to move towards the seventh guide block under the action of the arc-shaped guide blocks, the arc-shaped guide blocks are symmetrically arranged, the sixth guide blocks on two sides move together, the sixth guide blocks drive the seventh guide blocks to move together through the fifth rod piece, so that two eighth guide blocks on the fifth guide blocks move oppositely at the same time, so that 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 overlapped together for prevention move so as to be unfolded, so that the second pin shafts move upwards, and the plurality of second pin shafts move upwards together, wherein the distances among the plurality of second pin shafts are the same, meanwhile, the second pin shaft drives the extrusion plate fixed on the second pin shaft to move upwards, and the lifting assembly cleaning device agrees that the arc-shaped guide block is disengaged and can reset under the action of the first spring, so that the extrusion plate can move up and down in a reciprocating manner;
the upward movement of the extrusion plates can lead to a plurality of gaps 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 can reset, the distance between the extrusion plates can be shortened, the extrusion plates can pressurize the solution to the middle, thereby, that is, the reaction raw material and the catalyst are pressed to the central position, thereby, that is, the reaction raw material and the catalyst are moved from the middle to both sides and then from both sides to the middle, so that the two are irregularly distributed from the middle to the two sides and are uniformly distributed at the upper and lower positions of the two sides, and the third through holes can block the two, therefore, the detention can be better carried out towards the middle when the third through hole is reset, so that the distribution uniformity of the third through hole and the detention through the third through hole in the reaction kettle is better improved, and the vertical movement process of the extrusion plate can be better and stable through the simultaneous movement of the sixth guide block and the seventh guide block; thereby achieving even distribution of the reaction raw material and the catalyst and improving the degree of reaction.
Specifically, the driving device comprises a second support fixedly arranged above the reaction kettle, a motor fixedly arranged above the second support, a first conveying belt fixedly connected to the output end of the motor, a first conveying belt connected to the stirring main shaft, a second conveying belt connected to the stirring main shaft, a double-turbine worm reduction gearbox connected to the second conveying belt, a third conveying belt connected to the double-turbine worm reduction gearbox, a third conveying belt connected to the bottom cleaning device, a brake assembly connected to the motor, a plurality of discharging blocks arranged on the reaction kettle and used for feeding materials, and two discharging grooves arranged below the reaction kettle and used for discharging materials; the brake assembly comprises a first guide block fixedly arranged above the reaction kettle, a first guide rod slidably 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 conveying belt is connected to the first rotating shaft; a plurality of stirring blades for stirring are arranged on the stirring main shaft; the method comprises the following specific steps: the motor drives the first conveyer belt to move, the first conveyer belt provides power for the rotation of the stirring main shaft, the rotation of the stirring main shaft drives the second conveyer belt, the second conveyer belt drives the input end of the double-turbine worm reduction gearbox, the output end of the double-turbine worm reduction gearbox drives the third conveyer belt to move, the third conveyer belt drives the first rotating shaft to rotate, the first conveyer belt, the second conveyer belt and the third conveyer belt are the prior art and are in speed reduction transmission, thereby slowing down the speed of the first rotating shaft through multi-stage speed reduction, improving the stability of movement, then workers can open the discharge chute to replace the cleaning piece, guarantee when changing that stirring main shaft and first pivot can not take place any rotation, this is that the electro-magnet outage can make the screens board block the card pinion rack under the effect of second spring to can not take place rotatoryly, thereby workman's security when improving the change.
Compared with the prior art, the invention has the following advantages:
1. and (3) the sulfonation side reaction is reduced: in the process of dissolving p-acetamino anisole by sulfuric acid, the sulfuric acid with the concentration of 80 percent replaces 93 percent of sulfuric acid, thereby reducing the sulfonation capability of the sulfuric acid;
2. the addition of the phase transfer catalyst promotes the dissolution speed of p-acetamino anisole in sulfuric acid, and reduces the time for dissolving p-acetamino anisole, thereby reducing the occurrence of sulfonation side reaction;
3. the selectivity of the target product in the nitration reaction is improved: the catalyst is added to inhibit the side reaction of the 3-position nitration of the benzene ring, the guanidine compound is added, the nitroxyl cation and the guanidine compound have certain acting force, and the 3-position steric hindrance is large, so that the 2-position is attacked preferentially during nitration.
In summary, the bottom cleaning device is arranged, so that the inert gas which does not react with the concentrated sulfuric acid is blown onto the bottom surface of the reaction kettle, the reaction raw material and the catalyst on the bottom surface of the reaction kettle can be blown up better, the reaction raw material and the catalyst can not sink on the bottom surface and can float, and then the reaction raw material and the catalyst can be uniformly distributed in the reaction kettle through the matching with the stirring main shaft, so that the reaction speed and the reaction degree are improved; the bottom surface of the reaction kettle is cleaned by the cleaning device, so that reaction raw materials and a catalyst on the bottom surface of the reaction kettle can better float up in a physical mode, and the effect of uniform distribution is improved; the extrusion device is arranged, and the floated reaction raw materials and the catalyst are extruded continuously, so that the 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 A of FIG. 1 according to 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 view of the gas control assembly of the present invention;
FIG. 6 is a schematic structural view of a stirring spindle according to the present invention;
FIG. 7 is an enlarged view of D of FIG. 1 according to the present invention;
FIG. 8 is a schematic view of the cleaning apparatus according to the present invention;
FIG. 9 is a schematic structural view of a control unit according to the present invention;
FIG. 10 is a schematic structural diagram of a first control assembly according to the present invention;
FIG. 11 is a schematic structural view of a fourth guide block according to the present invention;
FIG. 12 is a schematic structural view of a second link according to the present invention;
FIG. 13 is a schematic structural 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 invention;
FIG. 15 is a schematic view of the lifting assembly of the present invention;
FIG. 16 is a schematic view of the structure of the pressing plate according to the present invention;
FIG. 17 is a schematic structural view of a third link according to the present invention;
FIG. 18 is a first schematic structural diagram of a driving device according to the present invention;
FIG. 19 is a second schematic structural view of a driving device according to the present invention;
FIG. 20 is a schematic view of the brake assembly of the present invention;
FIG. 21 is a first schematic structural view of an arc-shaped guide block according to the present invention;
FIG. 22 is a second schematic structural view of the arc guide block of the present invention;
FIG. 23 is a schematic view of the discharge chute of the present invention;
Detailed Description
In order to make the technical solutions of the present invention better understood, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention.
As shown in FIGS. 1 to 23, a method for synthesizing high-purity 2-nitro-4-acetamino anisole, in which 2-nitro-4-acetamino anisole is synthesized using a flow line; the assembly line comprises a reaction device, a discharging device and a cleaning device; the synthesis steps are as follows: A. putting the reaction raw materials into a reaction device for reaction; the reaction device comprises a first support 1, a reaction kettle 2 arranged above the first support 1 and used for containing raw materials, extraction barrels 3 arranged at two sides of the reaction kettle 2, a stirring main shaft 8 arranged inside the reaction kettle 2, a bottom cleaning device 5 connected to 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 by using a stirring main shaft 8, and slowly adding p-acetamino anisole 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 53 arranged in the first rotating shaft 59 and matched with the power assembly 52, a telescopic assembly 54 arranged in the first rotating shaft 59 and matched with the driving control rod 53, a first rod 56 arranged below the first rotating shaft 59 and communicated with the first rotating shaft 59, and a gas control assembly 55 arranged in the first rotating shaft 59 and the first rod 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 assembly 52 to rotate, the power assembly 52 drives the driving control rod member 53 to move, the driving control rod member 53 drives the telescopic assembly 54 to move, the telescopic assembly 54 moves to compress the inert gas in the first rotating shaft 59, the telescopic assembly 54 drives the gas control assembly 55 to move when moving to the gas control assembly 55, the movement of the gas control assembly 55 can cause the inert gas in the first rotating shaft 59 to be blown out at the first rod member 56 and blown to the bottom of the reaction kettle 2, so that the catalyst and the raw materials at the bottom of the reaction kettle 2 are better and uniformly distributed, and then the first gas storage tank 51 supplements the inert gas in the first rotating shaft 59; C. cleaning the bottom of the reaction kettle 2 by using a cleaning device 6; D. the extrusion device 7 is used for pushing the catalyst and the reaction raw materials which are cleaned and blown up by the cleaning device 6 and the bottom cleaning device 5 up and down; E. using an extraction barrel 3 to extract products in the reaction liquid and continuously returning the extracted reaction to the reaction kettle 2; F. discharging the reaction completely by using a discharging device; G. and cleaning the reaction solution by using a cleaning device to obtain a finished product.
Specifically, the bottom cleaning device 5 further comprises a first through hole 561 arranged below the first rod 56 and communicated with the reaction kettle 2, a first connecting rod 58 arranged below the first rod 56 and fixedly connected to the first rotating shaft 59, a second gas storage tank 57 arranged between the first connecting rod 58 and the first rod 56, a connecting pipe 562 arranged between the second gas storage tank 57 and the first through hole 561 and used for communicating the first through hole 561 with the second gas storage tank 57, a gas storage cavity 571 arranged in the second gas storage tank 57 and communicated with the first rod 56, and a second through hole 572 arranged on the first connecting rod 58 and used for communicating the gas storage cavity 571 with 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 distributed below the first connecting rod 58 uniformly; 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 of the first pins 56; are uniformly arranged on the first rotating shaft 59; the two first rods 56 are connected to the first connecting rods 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 moves, the second gas storage tank 57 and the first connecting rod 58 are driven 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 the bottom surface of the reaction kettle 2 more, and then when the telescopic assembly 54 compresses the inert gas in the first rotating shaft 59, the inert gas is blown out of the first through holes 561 by the control of the gas control assembly 55, and the inert gas is directly blown to the bottom surface of the reaction vessel 2 in the first through holes 561 of the two first rods 56, and then the inert gas in the other two first rods 56 passes through the first through holes 561 to the connecting pipes 562, then to the gas storage chamber 571, and is blown between the two cleaning members 61 through the second through holes 572.
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 pushing against the threaded rod 552, a transmission member 554 disposed below the fourth spring 553 and used for guiding the threaded rod 552, and a control member 555 connected to the transmission member 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 connected to the second gear 5543, and a supporting block 5545 disposed below the first gear 5542 and rotatably connected to the threaded rod 552 and the supporting block 5545 for supporting; the threaded plate 551 is threadedly connected with the threaded rod 552; the method comprises the following specific steps: the telescopic assembly 54 drives the threaded plate 551 to move downwards, 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 control part 555 to move, the control part 555 controls the opening and closing state of the first through hole 561, when the telescopic assembly 54 resets, the threaded plate 551 resets through the fourth spring 553.
Specifically, the control unit 555 includes a seventh rod 5551 fixed to the second gear 5543, a ninth guide block 5552 fixed to the seventh rod 5551, a baffle 5553 fixed to the ninth guide block 5552 and rotatably disposed inside the first rod 56, and a tenth guide block 5554 fixed to the tenth guide block 5554; the ninth guide block 5552 and the transmission member 554 are rotatably connected to the first rod 56; the baffle 5553 has only a slight angle; the angle of the baffle 5553 blocks 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 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 the rotation to be more stable; the first control member 63 of the air control member 55 will open the first through hole 561 once it starts rotating, so as to blow the air in the first rod 56 out more quickly, and thus better control can be achieved.
Specifically, the telescopic assembly 54 includes a fourth fixing plate 5541 fixed on 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 fixed below the first fixing plate 541, a plurality of third connecting rods 545 alternately connected to the second fixing plates 544, a hinge point between the third rod 542 and one of the third connecting rods 545 being a first pin 543, 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 543 to move downwards, the first pin 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, and therefore 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 hitting the threaded plate 551, and the hollow rod 547 drives the threaded plate 551 downward for 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 drive 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 used for abutting against the second disc 525 to reset the second disc 525; 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 member 542 to rotate, so that the driving control rod member 53 rotates, the driving control rod member 53 drives the second disc 525, the driving control rod member 53 is driven to reciprocate up and down through the matching of the third guide block 524 and the second guide block 523, and the third rod member 542 is driven to move to drive the first push plate 546 to compress the inert gas in the first rotating shaft 59 to provide power.
Specifically, the first control assembly 63 includes a fourth guide block 636 fixedly disposed below the first link 58, a second rotating shaft 631 rotatably connected to the second link 62 and fixedly connected to the cleaning element 61 for supporting the cleaning element 61, a fourth link 632 hinged to the second rotating shaft 631, a third fixing plate 635 fixedly connected to the first link 58, a fourth rod 634 fixedly connected to the third fixing plate 635, and a first sliding chute 633 disposed on the fourth link 632 and slidably connected to the fourth rod 634; the second connecting rod 62 is slidably connected 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 continuously cooperates 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 is not jammed due to three arc-shaped guide blocks 9, 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 chute 633, that is, the hinged position of the fourth connecting rod 632 and the second rotating shaft 631 generates angular rotation, so that the second rotating shaft 631 is driven to reciprocate while the second rotating shaft 631 rotates reciprocally, so that the second rotating shaft 631 drives the cleaning element 61 to do the same movement; the cleaning member 61 is reciprocated and rotated while reciprocating, and can clean the reaction raw material and the catalyst on the bottom surface of the reaction vessel 2 more effectively.
Specifically, the extrusion device 7 comprises a second control assembly 71 arranged above the first connecting rod 58, a plurality of extrusion plates 73 arranged above the second control assembly 71, and a lifting assembly 72 which is arranged in two steps, the second control assembly 71 and the extrusion plates 73 and is used for driving the extrusion plates 73 to move; a plurality of third through holes 731 are arranged on the extrusion plate 73; the lifting assembly 72 comprises a fifth connecting rod 721 and a sixth connecting rod 722 which are connected with the second control assembly 71 in a staggered manner, a second pin 723 connected with the fifth connecting rod 721 and the sixth connecting rod 722, and the fifth connecting rod 721 and the sixth connecting rod 722 are hinged and fixed through the second pin 723; the second control assembly 71 comprises a fifth guide block 711 fixedly arranged above the first connecting rod 58, a sixth guide block 712 and a seventh guide block 714 which are arranged on the fifth guide block 711 in a sliding manner and positioned at two sides of the fifth guide block 711, a fifth rod 713 arranged on the sixth guide block 712, an eighth guide block 715 fixedly connected to the sixth guide block 712, a sixth rod 716 arranged above the eighth guide block 715 and matched with the arc-shaped guide block 9, and a first spring 717 arranged between the two eighth guide blocks 715; the fifth link 721 and the sixth link 722 are hinged to the eighth guide block 715; two of the second control assemblies 71 are distributed on two sides of the first connecting rod 58; the fifth bar 713 is connected to the sixth guide block 712 of one of the second control assemblies 71 and is connected to the seventh guide block 714 of the other of the second control assemblies 71; the movement of the sixth guide blocks 712 drives the seventh guide blocks 714 on the two second control assemblies 71 to move; 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 squeezing device 7 to move together, and then the sixth rod 716 continuously cooperates 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, because the arc-shaped guide blocks 9 are symmetrically arranged, the sixth guide blocks 712 on both 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 and oppositely, so as to drive the fifth link 721 and the sixth link 722 to move together, so that the plurality of fifth links 721 and the plurality of sixth links 722 which are prevented from being overlapped together move to unfold, so that the second pin 723 moves, and the second pin 723 moves upwards, the plurality of second pin shafts 723 move upwards together, that is, the distances between the plurality of second pin shafts 723 are the same and are increased simultaneously, then the second pin shafts 723 drive the extrusion plates 73 fixed on the second pin shafts 723 to move upwards, the lifting assembly 72 cleaning device 6 agrees that the arc-shaped guide blocks 9 are disengaged, and the lifting assembly 72 is reset under the action of the first springs 717, so that the extrusion plates 73 move up and down in a reciprocating manner.
Specifically, the driving device 4 comprises a second support 42 fixedly arranged above the reaction kettle 2, a motor 41 fixedly arranged above the second support 42, a first conveyer belt 44 fixedly connected to an output end of the motor 41, the first conveyer belt 44 connected to the stirring main shaft 8, a second conveyer belt 45 connected to the stirring main shaft 8, a double-turbine worm reduction gearbox 46 connected to the second conveyer belt 45, a third conveyer belt 47 connected to the double-turbine worm reduction gearbox 46, the third conveyer belt 47 connected to the bottom cleaning device 5, a brake assembly 43 connected to the motor 41, a plurality of discharging blocks 48 arranged on the reaction kettle 2 for charging, and two discharging grooves 21 arranged below the reaction kettle 2 for discharging; 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 latch 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 rotating 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 drives 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, the first conveyer belt 44, the second conveyer belt 45 and the third conveyer belt 47 are the prior art and are in speed reduction transmission, so that the speed of the first rotating shaft 59 is slowed down through multi-stage speed reduction, the stability of the movement is improved, then a worker can open the discharge chute 21 to replace the cleaning piece 61, the stirring main shaft 8 and the first rotating shaft 59 are ensured not to rotate at all during replacement, the power failure of the electromagnet 436 can enable the clamping plate 432 to clamp the toothed plate 431 under the action of the second spring 435, so that rotation does not occur, thereby improving the safety of workers at the time of replacement.
Example two
5kg of 93 percent sulfuric acid is added into a reaction device of a 10L reaction kettle, the temperature of frozen saline is controlled, 2kg of p-acetamino anisole is slowly added at 10-15 ℃, the temperature is continuously kept for 2 hours after the addition of the p-acetamino anisole is finished, and the p-acetamino anisole is completely dissolved; then the temperature is reduced to 5 ℃ within 0.5 hour, the sample is taken for HPLC analysis, wherein the content of the sulfonated substance is 5.2 percent, then nitric acid is dripped at the temperature of 0-5 ℃, the temperature is kept for 1 hour after 5 hours of dripping, and the sample is taken for HPLC analysis, wherein the sulfonated by-product is 5.5 percent, 2-nitro-4-acetamino anisole 92 percent, 3-nitro-4-acetamino anisole 1.5 percent, and 2, 5-dinitro-4-acetamino anisole 1 percent. Slowly dripping the reaction liquid into ice water, diluting the sulfuric acid concentration to 35%, washing out yellow solid, filtering to obtain a wet 2-nitro-4-acetamino anisole product, wherein the COD of the mother liquid waste acid is 31000mg/L, adding water into a filter cake to wash to obtain a finished product, and analyzing by HPLC (high performance liquid chromatography) that the content of the 2-nitro-4-acetamino phenyl ether is 97.8%.
EXAMPLE III
Adding 5kg of 80% sulfuric acid into a reaction device of a 10L reaction kettle, adding 25g of tetra-n-butylammonium chloride, stirring until the sulfuric acid is completely dissolved, controlling the temperature by using frozen saline water, slowly adding 2kg of p-acetamino anisole at the temperature of 10-15 ℃, keeping the temperature for 1 hour after the addition is finished, and completely dissolving the p-acetamino anisole; then the temperature is reduced to 5 ℃ within 0.5 hour, the sample is taken for HPLC analysis, wherein the content of the sulfonated substance is 0.3 percent, then nitric acid is dripped at the temperature of 0-5 ℃, the temperature is kept for 1 hour after 5 hours of dripping, and the sample is taken for HPLC analysis, wherein the sulfonated by-product is 0.6 percent, 2-nitro-4-acetamino anisole is 97.6 percent, 3-nitro-4-acetamino anisole is 1.2 percent, and 2, 5-dinitro-4-acetamino anisole is 0.6 percent. Slowly dripping the reaction liquid into ice water, diluting the sulfuric acid concentration to 35%, washing out yellow solid, filtering to obtain a wet 2-nitro-4-acetamino anisole product, wherein the COD (chemical oxygen demand) of mother liquor waste acid is 15000mg/L, adding water into a filter cake to wash to obtain a finished product, and analyzing by HPLC (high performance liquid chromatography) that the content of the 2-nitro-4-acetamino phenyl ether is 98.2%.
Example four
Adding 5kg of 80% sulfuric acid into a reaction device of a 10L reaction kettle, adding 25g of tetra-n-butylammonium chloride, stirring until the sulfuric acid is completely dissolved, controlling the temperature by using frozen saline water, slowly adding 2kg of p-acetamino anisole at the temperature of 10-15 ℃, keeping the temperature for 1 hour after the addition is finished, and completely dissolving the p-acetamino anisole; then the temperature is reduced to 5 ℃ within 0.5 hour, and a sample is taken for HPLC analysis, wherein the content of the sulfonate is 0.3%; adding 10g of guanidine nitrate, continuously stirring for 0.5 hour, then controlling the temperature to be 0-5 ℃, dropwise adding nitric acid, continuously keeping the temperature for 1 hour after 5 hours of dropwise adding nitric acid, and sampling and analyzing by HPLC, wherein the sulfonation by-product is 0.4 percent, the 2-nitro-4-acetamino anisole is 99.2 percent, the 3-nitro-4-acetamino anisole is 0.3 percent, and the 2, 5-dinitro-4-acetamino anisole is 0.1 percent. Slowly dripping the reaction liquid into ice water, diluting the sulfuric acid concentration to 35%, washing out yellow solid, filtering to obtain a wet 2-nitro-4-acetamino anisole product, wherein the COD (chemical oxygen demand) of mother liquor waste acid is 5000mg/L, adding water into a filter cake to wash to obtain a finished product, and analyzing by HPLC (high performance liquid chromatography) that the content of the 2-nitro-4-acetamino phenyl ether is 99.5%.
The specific working process of the invention is as follows: concentrated sulfuric acid is added into a reaction kettle 2, then tetra-n-butylammonium chloride is added, a motor 41 drives a first conveyer belt 44 to move, the first conveyer belt 44 provides power for rotation of a stirring main shaft 8, namely, the stirring main shaft 8 is uniformly stirred by using a stirring blade 81, then p-acetamido anisole and a phase transfer catalyst are slowly added, then rotation drives a second conveyer belt 45, the second conveyer belt 45 drives an input end of a double-turbine worm reduction gearbox 46, an output end of the double-turbine worm reduction gearbox 46 drives a third conveyer belt 47 to move, the third conveyer belt 47 drives a first rotating shaft 59 to rotate, so that the speed of the first rotating shaft 59 is slowed down through multi-stage speed reduction, the stability of the movement is improved, the first rotating shaft 59 rotates to drive a first fixing plate 541 to rotate, the first fixing plate 541 drives a third rod member 542 to rotate, the driving control rod 53 can rotate, the driving control rod 53 drives the second disc 525, the driving control rod 53 can drive the driving control rod 53 to reciprocate up and down through the matching of the third guide block 524 and the second guide block 523, the third rod 542 can be driven to move downwards, the third rod 542 can drive the first pin 543 to move downwards, the first pin 543 can drive a plurality of third connecting rods 545 which are arranged in a staggered mode to move, the third connecting rods 545 can be unfolded from a superposed state, the first push plate 546 can be driven to move downwards, the first push plate 546 can drive 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 hitting the threaded plate 551, the hollow rod 547 drives the threaded plate 551 to move downward for a short distance, the threaded plate 551 drives the threaded rod 552 to rotate through being in 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 make the rotation more stable; the first control assembly 63 of the gas control assembly 55 once starts to rotate can open the first through hole 561, so that the gas in the first rod 56 can be blown out more quickly, and the inert gas can be blown directly to the bottom surface of the reaction vessel 2 in the first through holes 561 on the two first rods 56, and then the inert gas in the other two first rods 56 can pass through the first through holes 561 to the connecting pipes 562, and then to the gas storage chamber 571, and can be blown between the two sweeping members 61 through the second through hole 572, so as to better control, when the telescopic assembly 54 is reset, the threaded 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 can drive the fourth guide block 636 to move together, so that the second connecting rod 62 can move together, and the second connecting rod 62 can constantly cooperate with the arc-shaped guide block 9 when moving, so as to drive the second connecting rod 62 to slide in the fourth guide block 636 under the action of the arc-shaped guide block 9, the arc-shaped guide blocks 9 are three, so that the second connecting rod 62 is driven to reciprocate and cannot be locked, 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 matching of the fourth rod 634 and the first sliding groove 633, that is, the position where the fourth connecting rod 632 is hinged to the second rotating shaft 631 generates angular rotation, so that the second rotating shaft 631 is driven to reciprocate while the second rotating shaft 631 reciprocates, and the second rotating shaft 631 drives the cleaning member 61 to perform the same movement; the cleaning piece 61 can perform reciprocating rotation while sliding in a reciprocating manner, so that reaction raw materials and catalytic additive on the bottom surface of the reaction kettle 2 can be better cleaned;
the first link 58 drives the squeezing device 7 to move together, and then the sixth rod 716 continuously cooperates with the arc-shaped guide block 9 when moving, so as to drive the sixth guide block 712 to move towards the seventh guide block 714 under the action of the arc-shaped guide block 9, because the arc-shaped guide blocks 9 are symmetrically arranged, the sixth guide blocks 712 on both 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 simultaneously move towards each other, so as to drive the fifth link 721 and the sixth link 722 to move together, so as to move the plurality of fifth links 721 and the plurality of sixth links 722 which are prevented from being overlapped together and to unfold, so as to move the second pin 723, and the second pin 723 moves upwards, the plurality of second pin shafts 723 move upwards together, that is, the distances between the plurality of second pin shafts 723 are the same and are increased simultaneously, then the second pin shafts 723 drive the extrusion plates 73 fixed on the second pin shafts 723 to move upwards, the lifting assembly 72 cleaning device 6 agrees that the arc-shaped guide blocks 9 are disengaged, and the lifting assembly 72 is reset under the action of the first springs 717, so that the extrusion plates 73 move up and down in a reciprocating manner;
then, a worker can open the discharge chute 21 to replace the cleaning piece 61, and when the cleaning piece is replaced, it is ensured that the stirring main shaft 8 and the first rotating shaft 59 do not rotate, and the clamping plate 432 is clamped on the clamping plate 431 under the action of the second spring 435 when the electromagnet 436 is powered off, so that the rotation cannot occur, and the safety of the worker during replacement is improved.
It is to be understood that the described embodiments are merely a few embodiments of the invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Claims (9)
1. The synthesis method of the high-purity 2-nitro-4-acetamino anisole is characterized by comprising the following steps: synthesizing 2-nitro-4-acetamino anisole by using an assembly line; the assembly line comprises a reaction device, a discharging device and a cleaning device; the synthesis steps are as follows: A. putting the reaction raw materials into a reaction device for reaction; the reaction device comprises a first support (1), a reaction kettle (2) arranged above the first support (1) and used for containing raw materials, extraction barrels (3) arranged at two sides of the reaction kettle (2), a stirring main shaft (8) arranged in the reaction kettle (2), a bottom cleaning device (5) connected to 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-butylammonium chloride, uniformly stirring by using a stirring main shaft (8), and slowly adding p-acetamino anisole 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 assembly (52) to rotate, the power assembly (52) drives the driving control rod (53) to move, the driving control rod (53) drives the telescopic assembly (54) to move, the telescopic assembly (54) can compress inert gas in the first rotating shaft (59) when moving to the gas control assembly (55), the gas control assembly (55) is driven to move when moving to the gas control assembly (55), the inert gas in the first rotating shaft (59) can be blown outwards at the first rod (56) by the movement of the gas control assembly (55) and blown to the bottom of the reaction kettle (2), so that catalysts and raw materials at the bottom of the reaction kettle (2) are better and uniformly 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 the catalyst and the reaction raw materials which are cleaned and blown up by the cleaning device (6) and the bottom cleaning device (5) up and down; E. using an extraction barrel (3) to extract products in the reaction liquid and continuously returning the extracted reaction to the reaction kettle (2); F. discharging the reaction completely by using a discharging device; G. and cleaning the reaction solution by using a cleaning device to obtain a finished product.
2. The method for synthesizing high-purity 2-nitro-4-acetamino anisole according to claim 1, characterized in that: the bottom cleaning device (5) further comprises a first through hole (561) which is arranged below the first rod piece (56) and communicated with the reaction kettle (2), a first connecting rod (58) which is arranged below the first rod piece (56) and fixedly connected to the first rotating shaft (59), a second air 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 air storage box (57) and the first through hole (561) and used for communicating the first through hole (561) and the second air storage box (57), an air storage cavity (571) which is arranged in the second air storage box (57) and communicated with the first rod piece (56), and a second through hole (572) which is arranged on the first connecting rod (58) and used for communicating the air 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 rod (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 rods (56); are uniformly arranged on the first rotating shaft (59); the two first rods (56) are connected to the first connecting rod (58); the method comprises the following specific steps: the first rotating shaft (59) can drive the first rod (56) to move when moving, the first rotating shaft (59) can also drive the second gas storage tank (57) and the first connecting rod (58) to move together, 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 first connecting rod (58) rotates to enable the cleaning piece (61) to clean more of the bottom surface of the reaction kettle (2), then the telescopic assembly (54) compresses the inert gas in the first rotating shaft (59), the inert gas can be blown out from the first through holes (561) through the control of the gas control assembly (55), the inert gas can be directly blown to the bottom surface of the reaction kettle (2) in the first through holes (561) on the two first rods (56), and then the inert gas in the other two first rods (56) can pass through the first through holes (561) to the connecting pipe (562), then enters the air storage cavity (571) and is blown between the two cleaning pieces (61) through the second through hole (572).
3. The method for synthesizing high-purity 2-nitro-4-acetamino anisole according to claim 2, characterized in that: the gas control assembly (55) comprises a threaded plate (551) arranged in the first rotating shaft (59) in a sliding mode, a threaded rod (552) connected to the threaded plate (551), a fourth spring (553) arranged below the threaded rod (552) and used for pushing against 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 located inside the first rod (56); the transmission component (554) comprises a fourth fixing 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 to the second gear (5543), and a supporting block (5545) arranged below the first gear (5542) and rotatably connected to the threaded rod (552) and the supporting block (5545) for supporting; the threaded plate (551) is in threaded connection with the threaded rod (552); the method comprises the following specific steps: flexible subassembly (54) drive screw plate (551) and move down, screw plate (551) drive threaded rod (552) through with threaded rod (552) threaded connection and rotate, threaded rod (552) are rotatory can drive first gear (5542) and rotate, later first gear (5542) drive second gear (5543) and rotate, second gear (5543) are rotatory can drive control unit (555) and move, the open-close state of first through-hole (561) of control unit (555) control, when flexible subassembly (54) reset, screw plate (551) reset through fourth spring (553).
4. The method for synthesizing high-purity 2-nitro-4-acetamino anisole according to claim 3, characterized in that: the control component (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 rotatably 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 component (554) are rotatably connected to the first rod piece (56); the baffle (5553) has only a little angle; the angle of the baffle (5553) blocks the first through hole (561); the baffle (5553) rotates to open the first through hole (561); the method comprises the following specific steps: the seventh rod piece (5551) is driven to rotate by the rotation of the second gear (5543), the seventh rod piece (5551) drives the baffle (5553) to rotate in the first rod piece (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 the rotation to be more 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-acetamino anisole according to claim 4, characterized in that: the telescopic assembly (54) comprises a fourth fixing plate (5541) fixedly connected to the first rotating shaft (59), a third rod piece (542) which is slidably arranged in the first fixing plate (541) and connected to the power assembly (52), two second fixing plates (544) fixedly connected below the first fixing plate (541), a plurality of third connecting rods (545) which are connected to the second fixing plates (544) in a staggered mode, a first pin shaft (543) serving as a hinge point of the third rod piece (542) and one third connecting rod (545), a first push plate (546) arranged below the third connecting rod (545), and a hollow rod piece (547) 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 (542) to move downwards, the third rod (542) drives the first pin shaft (543) to move downwards, the first pin shaft (543) can drive the third connecting rods (545) which are arranged in a staggered mode to move, and therefore the third connecting rods (545) are unfolded from a stacked state, the first push plate (546) can be 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 member (547) stops after impacting the threaded plate (551), and the hollow rod member (547) drives the threaded plate (551) to move downwards for a short distance.
6. The method for synthesizing high-purity 2-nitro-4-acetamino anisole according to claim 2, characterized in that: the power assembly (52) comprises a second rod piece (521) fixedly arranged in the first air storage box (51), a first disc (522) fixedly arranged below the second rod piece (521), a plurality of second guide blocks (523) fixedly arranged on the first disc (522), a second disc (525) fixedly arranged above the drive control rod piece (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 abutting against the second disc (525) to reset the second disc (525); the driving control rod piece (53) is fixedly connected with 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 fixing plate (541) to rotate, the first fixing plate (541) drives the third rod piece (542) to rotate, so that the driving control rod piece (53) can rotate, the driving control rod piece (53) drives the second disc (525), and the driving control rod piece (53) can drive the driving control rod piece (53) to reciprocate up and down through the matching of the third guide block (524) and the second guide block (523).
7. The method for synthesizing high-purity 2-nitro-4-acetamino anisole according to claim 2, characterized in that: 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 to the second connecting rod (62) and fixedly connected to the cleaning piece (61) for supporting the cleaning piece (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 piece (634) fixedly connected to the third fixing plate (635), and a first sliding 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 with a fourth guide block (636) in a sliding mode; an elastic metal strip is arranged inside the cleaning piece (61); a plurality of arc-shaped guide blocks (9) are arranged; 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) can move together, the second connecting rod (62) can be continuously matched with the arc-shaped guide block (9) when moving, so that the second connecting rod (62) can be driven to slide in the fourth guide block (636) under the action of the arc-shaped guide block (9), the second connecting rod (62) can be driven to reciprocate and cannot be clamped because of three arc-shaped guide blocks (9), the second connecting rod (62) can be driven to slide to drive the second rotating shaft (631) to move together, then the second rotating shaft (632) drives the fourth connecting rod (632) to move, the fourth connecting rod (631) can move under the matching of the fourth rod (634) and the first sliding chute (633), namely, the hinged position of the fourth connecting rod (632) and the second rotating shaft (631) can rotate angularly, therefore, the second rotating shaft (631) can reciprocate and simultaneously drive the second rotating shaft (631) to rotate in a reciprocating manner, and the second rotating shaft (631) drives the cleaning piece (61) to move in the same manner.
8. The method for synthesizing high-purity 2-nitro-4-acetamino anisole according to claim 1, characterized in that: the extrusion device (7) comprises a second control assembly (71) arranged above the first connecting rod (58), a plurality of extrusion plates (73) arranged above the second control assembly (71), two steps, the second control assembly (71) and the extrusion plates (73), and a lifting assembly (72) for driving the extrusion plates (73) to move; a plurality of third through holes (731) are formed in the extrusion plate (73); the lifting assembly (72) comprises a fifth connecting rod (721) and a sixth connecting rod (722) which are connected to the second control assembly (71) in a staggered mode, a second pin shaft (723) connected to the fifth connecting rod (721) and the sixth connecting rod (722), and the fifth connecting rod (721) and the sixth connecting rod (722) are hinged and fixed through the second pin shaft (723); the second control assembly (71) comprises a fifth guide block (711) fixedly arranged above the first connecting rod (58), a sixth guide block (712) and a seventh guide block (714) which are arranged on the fifth guide block (711) in a sliding manner and positioned at two sides of the fifth guide block (711), a fifth rod piece (713) arranged on the sixth guide block (712), an eighth guide block (715) fixedly connected to the sixth guide block (712), a sixth rod piece (716) arranged above the eighth guide block (715) and matched with the arc-shaped guide block (9), and a first spring (717) arranged between the two eighth guide blocks (715); the fifth link (721) and the sixth link (722) are hinged to the eighth guide block (715); the method comprises the following specific steps: the first connecting rod (58) drives the extrusion device (7) to move together, then the sixth rod piece (716) continuously cooperates with the arc-shaped guide block (9) when moving, so that the sixth guide block (712) is driven to move towards the direction of the seventh guide block (714) under the action of the arc-shaped guide block (9), because the arc-shaped guide blocks (9) are 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 piece (713), so that two eighth guide blocks (715) on the fifth guide block (711) simultaneously move towards each other, so that the fifth connecting rod (721) and the sixth connecting rod (722) are driven to move together, and a plurality of fifth connecting rods (721) and a plurality of sixth connecting rods (722) which are overlapped together to be prevented move so as to be unfolded, therefore, the second pin shaft (723) can move upwards, the plurality of second pin shafts (723) move upwards together, the distances between the plurality of second pin shafts (723) are the same and are increased at the same time, then the second pin shaft (723) can drive the extrusion plate (73) fixed on the second pin shaft (723) to move upwards, the lifting assembly (72) cleaning device (6) agrees that the arc-shaped guide block (9) is disengaged, and the lifting assembly can reset under the action of the first spring (717), so that the extrusion plate (73) can move up and down in a reciprocating mode.
9. The method for synthesizing high-purity 2-nitro-4-acetamino anisole according to claim 1, characterized in that: the driving device (4) comprises a second support (42) fixedly arranged above the reaction kettle (2), a motor (41) fixedly arranged above the second support (42), a first conveying belt (44) fixedly connected to the output end of the motor (41), a first conveying belt (44) connected to the stirring main shaft (8), 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 third conveying belt (47) connected to the bottom cleaning device (5), a braking assembly (43) connected to the motor (41), a plurality of discharging blocks (48) arranged on the reaction kettle (2) and used for feeding, and two discharging grooves (21) arranged below the reaction kettle (2) and used for discharging; 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 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 rotating 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: motor (41) drive first conveyer belt (44) and move, first conveyer belt (44) provide power for the rotation of stirring main shaft (8), stirring main shaft (8) are rotatory can drive second conveyer belt (45), second conveyer belt (45) drive the input of two turbine worm reducing gear boxes (46), the output of two turbine worm reducing gear boxes (46) drives third conveyer belt (47) and moves, third conveyer belt (47) drive first pivot (59) rotatory, first conveyer belt (44), second conveyer belt (45), third conveyer belt (47) are prior art and for the transmission of speed reduction, thereby make the speed of first pivot (59) slow down through multistage speed reduction, improve the stability of motion.
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|---|---|---|---|---|
| CN117654417A (en) * | 2024-01-29 | 2024-03-08 | 常州市武进虹灵化工有限公司 | High-efficient mixed dissolution reaction cauldron |
Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2011143370A (en) * | 2010-01-15 | 2011-07-28 | Takuma Co Ltd | Reactor and method for producing reaction product by using the same |
| CN103114548A (en) * | 2013-03-06 | 2013-05-22 | 张铁民 | Road combined snow clearer |
| WO2019204082A1 (en) * | 2018-04-20 | 2019-10-24 | Exxonmobil Chemical Patents Inc. | Reverse flow reactors having high purge efficiencies while containing asymmetric feeds, methods of using same, and pyrolysis products made from same |
| JP6623447B1 (en) * | 2019-06-17 | 2019-12-25 | 濱州方新電脳有限公司 | Dust control terminal of cement mixer |
| CN110642733A (en) * | 2019-09-11 | 2020-01-03 | 浙江工业大学 | Process for continuously producing aminobenzoate derivative and synthesis system thereof |
| CN210252238U (en) * | 2019-04-25 | 2020-04-07 | 湖北巴司特科技股份有限公司 | Reation kettle is used in production of waterborne cold-coating zinc resin |
| CN210752622U (en) * | 2019-04-26 | 2020-06-16 | 四川同舟化工科技有限公司 | Polycarboxylate water reducing agent production reaction material is swept dropwise jar with blowback |
| CN211800799U (en) * | 2020-01-07 | 2020-10-30 | 安徽省双科药业有限公司 | Double-layer glass reaction kettle device for producing bendazac lysine bulk drug |
| CN212017820U (en) * | 2019-12-25 | 2020-11-27 | 四川星明能源环保科技有限公司 | Reaction unit is used in production of low-cost vanadium electrolyte |
| JP2021013920A (en) * | 2019-07-15 | 2021-02-12 | 張偉萍 | Device for preparing solid-liquid mixed chemical reagent |
| CN112403402A (en) * | 2020-11-13 | 2021-02-26 | 徐州亚兴医疗科技有限公司 | Circulating reflux type catalytic reaction kettle and working method thereof |
Patent Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2011143370A (en) * | 2010-01-15 | 2011-07-28 | Takuma Co Ltd | Reactor and method for producing reaction product by using the same |
| CN103114548A (en) * | 2013-03-06 | 2013-05-22 | 张铁民 | Road combined snow clearer |
| WO2019204082A1 (en) * | 2018-04-20 | 2019-10-24 | Exxonmobil Chemical Patents Inc. | Reverse flow reactors having high purge efficiencies while containing asymmetric feeds, methods of using same, and pyrolysis products made from same |
| CN210252238U (en) * | 2019-04-25 | 2020-04-07 | 湖北巴司特科技股份有限公司 | Reation kettle is used in production of waterborne cold-coating zinc resin |
| CN210752622U (en) * | 2019-04-26 | 2020-06-16 | 四川同舟化工科技有限公司 | Polycarboxylate water reducing agent production reaction material is swept dropwise jar with blowback |
| JP6623447B1 (en) * | 2019-06-17 | 2019-12-25 | 濱州方新電脳有限公司 | Dust control terminal of cement mixer |
| JP2021013920A (en) * | 2019-07-15 | 2021-02-12 | 張偉萍 | Device for preparing solid-liquid mixed chemical reagent |
| CN110642733A (en) * | 2019-09-11 | 2020-01-03 | 浙江工业大学 | Process for continuously producing aminobenzoate derivative and synthesis system thereof |
| CN212017820U (en) * | 2019-12-25 | 2020-11-27 | 四川星明能源环保科技有限公司 | Reaction unit is used in production of low-cost vanadium electrolyte |
| CN211800799U (en) * | 2020-01-07 | 2020-10-30 | 安徽省双科药业有限公司 | Double-layer glass reaction kettle device for producing bendazac lysine bulk drug |
| CN112403402A (en) * | 2020-11-13 | 2021-02-26 | 徐州亚兴医疗科技有限公司 | Circulating reflux type catalytic reaction kettle and working method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117654417A (en) * | 2024-01-29 | 2024-03-08 | 常州市武进虹灵化工有限公司 | High-efficient mixed dissolution reaction cauldron |
| CN117654417B (en) * | 2024-01-29 | 2024-05-07 | 常州市武进虹灵化工有限公司 | High-efficient mixed dissolution reaction cauldron |
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