CN113754557A - Method for synthesizing methoxyamine hydrochloride - Google Patents
Method for synthesizing methoxyamine hydrochloride Download PDFInfo
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- CN113754557A CN113754557A CN202111074645.6A CN202111074645A CN113754557A CN 113754557 A CN113754557 A CN 113754557A CN 202111074645 A CN202111074645 A CN 202111074645A CN 113754557 A CN113754557 A CN 113754557A
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- water
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- XNXVOSBNFZWHBV-UHFFFAOYSA-N hydron;o-methylhydroxylamine;chloride Chemical compound Cl.CON XNXVOSBNFZWHBV-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 238000000034 method Methods 0.000 title claims abstract description 23
- 230000002194 synthesizing effect Effects 0.000 title claims abstract description 22
- 238000003756 stirring Methods 0.000 claims abstract description 102
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 52
- 238000004140 cleaning Methods 0.000 claims abstract description 50
- 238000006243 chemical reaction Methods 0.000 claims abstract description 41
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims abstract description 22
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 15
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 15
- 239000007921 spray Substances 0.000 claims abstract description 15
- 239000000243 solution Substances 0.000 claims abstract description 13
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000010410 layer Substances 0.000 claims abstract description 12
- 238000002156 mixing Methods 0.000 claims abstract description 9
- WHIVNJATOVLWBW-PLNGDYQASA-N (nz)-n-butan-2-ylidenehydroxylamine Chemical compound CC\C(C)=N/O WHIVNJATOVLWBW-PLNGDYQASA-N 0.000 claims abstract description 8
- 239000011259 mixed solution Substances 0.000 claims abstract description 8
- 239000003444 phase transfer catalyst Substances 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims abstract description 5
- 239000012022 methylating agents Substances 0.000 claims abstract description 5
- 238000001704 evaporation Methods 0.000 claims abstract description 4
- 239000012044 organic layer Substances 0.000 claims abstract description 4
- 238000011010 flushing procedure Methods 0.000 claims description 26
- 230000005540 biological transmission Effects 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 6
- 238000007599 discharging Methods 0.000 claims description 5
- 239000008234 soft water Substances 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 3
- 230000008878 coupling Effects 0.000 claims description 2
- 238000010168 coupling process Methods 0.000 claims description 2
- 238000005859 coupling reaction Methods 0.000 claims description 2
- 238000010030 laminating Methods 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 14
- 150000001875 compounds Chemical class 0.000 abstract description 2
- 238000001308 synthesis method Methods 0.000 abstract description 2
- 239000012295 chemical reaction liquid Substances 0.000 description 17
- 238000005507 spraying Methods 0.000 description 10
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 9
- 238000003786 synthesis reaction Methods 0.000 description 9
- 230000015572 biosynthetic process Effects 0.000 description 7
- 239000002994 raw material Substances 0.000 description 7
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 description 6
- LPXPTNMVRIOKMN-UHFFFAOYSA-M sodium nitrite Chemical compound [Na+].[O-]N=O LPXPTNMVRIOKMN-UHFFFAOYSA-M 0.000 description 6
- 238000004891 communication Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 231100000086 high toxicity Toxicity 0.000 description 3
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 3
- 239000000376 reactant Substances 0.000 description 3
- 235000010288 sodium nitrite Nutrition 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000002912 waste gas Substances 0.000 description 3
- 230000003749 cleanliness Effects 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- VSNHCAURESNICA-NJFSPNSNSA-N 1-oxidanylurea Chemical compound N[14C](=O)NO VSNHCAURESNICA-NJFSPNSNSA-N 0.000 description 1
- 230000002337 anti-port Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- JFPVXVDWJQMJEE-IZRZKJBUSA-N cefuroxime Chemical compound N([C@@H]1C(N2C(=C(COC(N)=O)CS[C@@H]21)C(O)=O)=O)C(=O)\C(=N/OC)C1=CC=CO1 JFPVXVDWJQMJEE-IZRZKJBUSA-N 0.000 description 1
- 229960001668 cefuroxime Drugs 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- HRYZWHHZPQKTII-UHFFFAOYSA-N chloroethane Chemical compound CCCl HRYZWHHZPQKTII-UHFFFAOYSA-N 0.000 description 1
- VAYGXNSJCAHWJZ-UHFFFAOYSA-N dimethyl sulfate Chemical group COS(=O)(=O)OC VAYGXNSJCAHWJZ-UHFFFAOYSA-N 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 150000002923 oximes Chemical class 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C239/00—Compounds containing nitrogen-to-halogen bonds; Hydroxylamino compounds or ethers or esters thereof
- C07C239/08—Hydroxylamino compounds or their ethers or esters
- C07C239/20—Hydroxylamino compounds or their ethers or esters having oxygen atoms of hydroxylamino groups etherified
-
- 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
- B01J19/0006—Controlling or regulating processes
-
- 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
- B01J19/0006—Controlling or regulating processes
- B01J19/002—Avoiding undesirable reactions or side-effects, e.g. avoiding explosions, or improving the yield by suppressing side-reactions
-
- 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
- B01J19/0053—Details of the reactor
- B01J19/0066—Stirrers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The application relates to the technical field of compound synthesis methods, and discloses a method for synthesizing methoxylamine hydrochloride, which comprises the steps of firstly adding water, sodium hydroxide, butanone oxime and a phase transfer catalyst into a reaction kettle; cooling and adding a methylating agent; standing for layering to obtain an organic layer and a water layer, distilling the water layer, collecting distillate, mixing the oil layer and the distillate, and adding hydrochloric acid to obtain a mixed solution; feeding and rectifying the mixed solution from the middle of a rectifying column, recovering butanone and methanol from the top of the column, recovering methoxylamine hydrochloride solution from the bottom of the column, and evaporating and dehydrating to obtain a concentrated solution; the reaction kettle is cleaned, a stirring mechanism and a cleaning mechanism are arranged in the reaction kettle, the cleaning mechanism comprises a scraper plate, a spray pipe, a lifting assembly and a rotating assembly, and the spray pipe is connected with a water inlet pipe and a cleaning nozzle; the reaction kettle comprises a kettle body and a kettle cover, the water outlet end of the cleaning nozzle faces the side wall of the kettle body, and the scraper plate is attached to the side wall of the kettle body. This application has the effect of conveniently wasing cauldron body side wall residue.
Description
Technical Field
The application relates to the technical field of compound synthesis methods, in particular to a method for synthesizing methoxylamine hydrochloride.
Background
Methoxylamine hydrochloride is an important chemical product and a medical intermediate, and is widely applied to color photography and film developing, and organic synthesis industry as a reducing agent to prepare oximes and produce neonomine, propargomine, hydroxyurea, cefuroxime and the like in the aspect of medicine.
The reaction kettle is one of necessary devices in the synthesis process of the methoxylamine hydrochloride as an important device in the chemical synthesis process, and the cleanliness of the reaction kettle directly influences the quality of products. The traditional reaction kettle generally comprises a kettle body and a kettle cover, wherein a part of reactants inevitably remains on the side wall of the kettle body after the reactants are mixed and reacted in the kettle body, the residues on the side wall of the kettle body are generally removed by regular cleaning, the kettle cover needs to be detached from the kettle body during cleaning, and the operation is complex and needs to be improved.
Disclosure of Invention
In order to facilitate cleaning of residues on the side wall of the kettle body, the application provides a method for synthesizing methoxyamine hydrochloride.
The method for synthesizing the methoxylamine hydrochloride adopts the following technical scheme:
a method for synthesizing methoxylamine hydrochloride is characterized in that: comprises the following steps of (a) carrying out,
s1, adding water and sodium hydroxide into the reaction kettle, stirring and dissolving at room temperature, and adding butanone oxime and a phase transfer catalyst;
s2, cooling the reaction kettle to 0-15 ℃, and adding a methylating agent into the reaction kettle;
s3, standing and layering after reaction to obtain an organic layer and a water layer, distilling the water layer, collecting distillate, combining the oil layer and the distillate, and adding hydrochloric acid to mix uniformly to obtain a mixed solution;
s4, feeding and rectifying the mixed solution from the middle of a rectifying column, controlling the temperature of the lower half part of the rectifying column to be 80-95 ℃, recovering butanone and methanol from the top of the column until no butanone is distilled, recovering methoxylamine hydrochloride solution from the bottom of the column, and heating, evaporating and dehydrating the methoxylamine hydrochloride solution at the bottom of the column to obtain hydrochloride concentrated solution;
s5, cleaning a reaction kettle, wherein a stirring mechanism and a cleaning mechanism are arranged in the reaction kettle, the cleaning mechanism comprises a scraper plate, a spray pipe rotationally connected to the scraper plate through a connecting component, a lifting component for driving the scraper plate to longitudinally move and a rotating component for driving the spray pipe to circumferentially rotate, and the spray pipe is connected with a soft water inlet pipe and a plurality of cleaning nozzles circumferentially arranged; the reaction kettle comprises a kettle body and a kettle cover, the water outlet end of the cleaning nozzle faces the side wall of the kettle body, and the scraper plate is attached to the side wall of the kettle body.
By adopting the technical scheme, sulfur dioxide, sodium nitrite and other raw materials with high toxicity are not added in the synthesis process, the emission of nitrogen oxides and other waste gases is low, the reaction condition is mild, and the operation environment is good. During rectification, the materials are added from the middle of the rectification column, methoxylamine hydrochloride is obtained at the bottom of the rectification column, butanone and methanol are obtained at the top of the rectification column, the use of organic solvents such as toluene and hexane is reduced, butanone and methoxylamine hydrochloride obtained after rectification can be separated immediately without side reaction, and the synthesis yield is high. The recovered butanone can be used for synthesizing butanone oxime, thereby reducing the investment cost and saving resources.
The stirring mechanism can stir the reaction liquid in the reaction kettle, and the mixing uniformity of each material component in the reaction liquid is improved. The wiper mechanism sets up in reation kettle, and after the reaction, usable wiper mechanism carries out self-cleaning to the cauldron body side wall, and the mode that compares in opening the kettle cover and wash cauldron body side wall is easy and simple to handle again, cleaning efficiency and methoxyamine hydrochloride's synthetic efficiency height. When the kettle body is cleaned, water is injected into the spraying pipe through the water inlet pipe, and water is sprayed onto the side wall of the kettle body through the cleaning nozzle, so that residues on the side wall of the kettle body are washed off. The lifting assembly is used for driving the scraper to move longitudinally, so that the spraying pipe is driven to move longitudinally, and the action range of water sprayed out of the cleaning nozzle in the vertical direction is expanded. In addition, because the scraper blade is connected with the side wall of the kettle body in an abutting mode, the scraper blade can scrape the residues on the lower side of the scraper blade when moving, so that the residues on the side wall of the kettle body which are not washed away are removed, and the cleaning effect is good. The rotating assembly is used for driving the spraying pipe to rotate in the circumferential direction, the action range of water in the horizontal direction is expanded, and the cleaning effect of the cleaning mechanism is further improved.
Preferably, the lifting assembly comprises a servo motor installed on the kettle cover, a lifting screw rod connected with the kettle body in a rotating mode and a guide rod fixedly connected with the kettle body, an output shaft of the servo motor is fixedly connected with the lifting screw rod, the lifting screw rod is in threaded connection with the scraper, and the guide rod is arranged on the scraper in a penetrating mode.
Through adopting above-mentioned technical scheme, the scraper blade receives the restriction of guide bar can not rotate, and when servo motor drive lift lead screw rotated, the scraper blade can be followed lift lead screw longitudinal movement to drive shower and washing nozzle longitudinal movement, degree of automation is high, convenient operation.
Preferably, coupling assembling is including fixing the sheath in the shower outside and rotating the many connecting rods of connection on the sheath, the connecting rod is including fixing at the connecting portion of scraper blade downside and fixing the rotation portion at the connecting portion downside, be equipped with annular rotation groove on the circumference lateral wall of sheath, the last lateral wall that rotates the groove is equipped with two rather than the concentricity and be curved connecting hole, connecting portion rotate connect in the connecting hole, rotation portion rotate connect in rotating the groove, and rotate the portion and rotate the last lateral wall butt in groove.
By adopting the technical scheme, the protective sleeve not only plays a role in protecting the spray pipe, but also reduces the contact area between the side wall of the spray pipe and the reaction liquid, so that the spray pipe is not easy to corrode; and offer connecting hole and rotation groove on the sheath surface, the mode of holing and groove on the shower is compared and is more convenient for process, can not influence the integrality and the structural strength of shower. The connecting rod is used for connecting scraper blade and sheath, and the last lateral wall in rotation groove can block the rotation portion and break away from the sheath, has improved the stability when shower rotates.
Preferably, the rotating assembly comprises a rotating motor installed on the scraper, a rotating gear fixedly connected with an output shaft of the rotating motor, and transmission teeth continuously distributed on the circumferential side wall of the sheath, and the transmission teeth are meshed with the rotating gear.
Through adopting above-mentioned technical scheme, it can drive the running gear rotation to rotate the motor, and then makes driving tooth drive sheath and shower circumferential direction, and degree of automation is high, and the scope of action of blowout moisture is big in the shower, the cleaning performance is good. The driving mode utilizes the meshing of the transmission gear and the rotating gear, so that the spraying pipe has good stability and stable water flow output when rotating.
Preferably, the diapire of the cauldron body is concave arc form and the bottom is connected with the discharging pipe, the internal washing unit that still is provided with of cauldron, washing unit includes a plurality of flushing pipes that set up along circumference, connects the high pressure nozzle at flushing pipe end portion and sets up the communicating pipe between two adjacent flushing pipes, high pressure nozzle's play water direction is towards the diapire of the cauldron body, is connected with the raceway on one of them communicating pipe.
By adopting the technical scheme, the water sprayed out by the cleaning nozzle flows downwards along the side wall of the kettle body, and the bottom wall of the kettle body is in a concave arc shape, so that the water is converged to the discharge pipe to be discharged. The water delivery pipe can be used for injecting water into the communicating pipe connected with the water delivery pipe, and water is guided to the flushing pipe through the communicating pipe and then is sprayed to the bottom wall of the kettle body through the high-pressure nozzle, so that the bottom wall of the kettle body is flushed, the cleanliness of the kettle body is further improved, and the matching precision and the finished product quality of reactants are improved.
Preferably, the bottom wall of the kettle body is provided with fixing grooves with the number equal to that of the flushing pipes, a communicating groove communicated with the fixing grooves is arranged between every two adjacent fixing grooves, and the communicating pipes are positioned in the communicating grooves; the flushing pipe comprises a moving pipe hinged to the top wall of the fixed groove and a water-through hose connected to the moving pipe, and the water-through hose is communicated with the communicating pipe and can guide water into the moving pipe; the fixed groove is far away from and is installed the removal cylinder on its open-ended lateral wall, the piston rod of removal cylinder is articulated with the one end that removes the pipe and is close to high pressure nozzle.
Through adopting above-mentioned technical scheme, the fixed slot is used for holding the flushing pipe, the intercommunication groove is used for holding communicating pipe, has reduced the occupation space of flushing pipe and communicating pipe at cauldron body inner chamber. When the piston rod of the movable cylinder stretches, the flushing pipe can rotate around the hinged end of the flushing pipe as the circle center, so that the spraying direction of the high-pressure nozzle is changed, the action range of the high-pressure nozzle is large, and the cleaning effect of the bottom wall of the kettle body is good.
Preferably, the stirring mechanism comprises a first stirring assembly and a second stirring assembly, wherein the first stirring assembly is arranged in the middle of the kettle body, and the second stirring assembly is arranged on the side wall of the kettle body.
Through adopting above-mentioned technical scheme, first stirring subassembly and the reaction liquid contact that is located cauldron body middle part, second stirring subassembly and the reaction liquid contact that is located cauldron body side, the area of contact of rabbling mechanism and reaction liquid is big, stirring effect is good. The rotation direction of the first stirring assembly and the second stirring assembly can be controlled during stirring, so that vortexes with two opposite directions are formed in the middle and the side of the reaction liquid, and the stirring effect and the reaction uniformity of each material component in the reaction liquid are improved.
Preferably, first stirring subassembly is including installing first agitator motor on the kettle cover, with first agitator motor's output shaft fixed connection's (mixing) shaft and the stirring rake of connection at the (mixing) shaft lateral wall, (mixing) shaft and stirring rake all are located the middle part of the cauldron body, just the stirring rake is the slope setting.
Through adopting above-mentioned technical scheme, (mixing) shaft and stirring rake can be ordered about to first agitator motor and rotate for the stirring rake stirring reaction liquid. The stirring rake is the slope setting, has increased its area of contact with the reaction liquid in vertical direction, and stirring effect is good.
Preferably, the second stirring subassembly includes second agitator motor, with second agitator motor's output shaft fixed connection's driving gear, with driving gear intermeshing's driven gear and along a plurality of stirring pieces that set up at the driven gear inboard along circumference, the circumference inner wall middle part of the cauldron body is equipped with annular mounting groove, be equipped with the holding chamber on the inner wall that cauldron body axis was kept away from to the mounting groove, second agitator motor and driving gear are located the holding intracavity, driven gear rotates and connects in the mounting groove.
Through adopting above-mentioned technical scheme, when second agitator motor drive driving gear rotated, driven gear can counter drive gear antiport, and then the stirring of drive stirring piece and the reaction liquid that cauldron body lateral wall is close, degree of automation is high, and the material reaction is even.
Preferably, the bottom of driven gear is connected with the universal wheel, be equipped with annular guide rail on the diapire of mounting groove, the bottom of universal wheel is arranged in the guide rail.
Through adopting above-mentioned technical scheme, the universal wheel can follow the guide rail and remove when driven gear rotates, frictional resistance when having reduced driven gear and having rotated, and the second stirring subassembly operation is smooth and easy.
In summary, the present application includes at least one of the following beneficial technical effects:
sulfur dioxide, sodium nitrite and other substances with high toxicity are not added in the raw materials, the reaction condition is mild, the discharge amount of nitrogen oxide and other waste gases during synthesis is small, and the operation environment is good; the recovered butanone can be used for synthesizing butanone oxime, thereby reducing the investment cost and saving resources; the cleaning mechanism is used for cleaning the side wall of the kettle body, the flushing assembly is used for cleaning the bottom wall of the kettle body, the kettle body and the kettle cover do not need to be disassembled during cleaning, the operation is simple and convenient, and the synthesis efficiency is high;
when the servo motor drives the lifting screw rod to rotate, the scraper can drive the spray pipe to move longitudinally, the action range of the cleaning nozzle in the vertical direction is expanded, and residues on the side wall of the kettle body can be scraped off by the scraper; when the rotating motor drives the rotating gear to rotate, the transmission gear drives the sheath to drive the spraying pipe to rotate circumferentially, so that the action range of the cleaning nozzle in the horizontal direction is expanded, and the cleaning effect is good;
first agitator motor can order about the stirring rake stirring and be located the reaction liquid at cauldron body middle part, and the driving gear rotation can be ordered about to the second agitator motor, and then makes driven gear drive stirring piece stirring and the reaction liquid that cauldron body lateral wall is close, sets for the rotation opposite direction of stirring rake and stirring piece, and the stirring effect that the reaction liquid received is good, the reaction is even.
Drawings
FIG. 1 is a schematic structural view of a reaction vessel in the example of the present application;
FIG. 2 is a schematic sectional view of a reaction vessel in the example of the present application;
FIG. 3 is an enlarged schematic view at A in FIG. 2;
fig. 4 is a schematic partial cross-sectional view highlighting the communication pipe in the embodiment of the present application.
Description of reference numerals: 1. a reaction kettle; 11. a kettle body; 111. a discharge pipe; 112. mounting grooves; 113. an accommodating cavity; 114. a guide rail; 115. fixing grooves; 116. a communicating groove; 12. a kettle cover; 121. a feed pipe; 2. a stirring mechanism; 21. a first stirring assembly; 211. a first stirring motor; 212. a stirring shaft; 213. a stirring paddle; 22. a second stirring assembly; 221. a second stirring motor; 222. a driving gear; 223. a driven gear; 224. a stirring sheet; 225. a universal wheel; 3. a cleaning mechanism; 31. a squeegee; 32. a shower pipe; 321. a water inlet pipe; 322. cleaning the nozzle; 33. a lifting assembly; 331. a servo motor; 332. a lifting screw rod; 333. a guide bar; 34. a rotating assembly; 341. rotating the motor; 342. a rotating gear; 343. a transmission gear; 4. a flushing assembly; 41. a flush tube; 411. moving the tube; 412. a water hose; 42. a high pressure nozzle; 43. a communicating pipe; 44. a water delivery pipe; 45. a moving cylinder; 5. a connecting assembly; 51. a sheath; 511. a rotating groove; 512. connecting holes; 52. a connecting rod; 521. a connecting portion; 522. a rotating part.
Detailed Description
The present application is described in further detail below with reference to figures 1-4.
The embodiment of the application discloses a method for synthesizing methoxylamine hydrochloride. Referring to fig. 1 and 2, the method for synthesizing methoxyamine hydrochloride comprises the following steps:
s1, adding water and sodium hydroxide into the reaction kettle 1, stirring and dissolving at room temperature, and then adding butanone oxime and a phase transfer catalyst, wherein the phase transfer catalyst is PEG 500;
s2, cooling the interior of the reaction kettle 1 to 0-15 ℃, specifically to 5 ℃, and adding a methylating agent into the reaction kettle 1, wherein the methylating agent is dimethyl sulfate;
s3, reacting at 10 ℃ for 4 hours after the addition is completed, cooling to below 5 ℃, standing for layering to obtain an organic layer and a water layer, distilling the water layer, collecting distillate, combining the oil layer and the distillate, and adding hydrochloric acid to mix uniformly to obtain a mixed solution;
s4, transferring the mixed solution to a glass rectification column filled with spring glass filler, slowly adding butanone oxime ether hydrochloric acid solution from the middle of the rectification column for rectification, controlling the temperature of the lower half part of the rectification column to be 80-95 ℃, and specifically setting the temperature to be 86 ℃; recovering butanone and methanol from the top of the column until no butanone is distilled out, recovering methoxylamine hydrochloride solution from the bottom of the column, and heating, evaporating and dehydrating the methoxylamine hydrochloride solution at the bottom of the column to obtain hydrochloride concentrated solution;
s5, cleaning the reaction kettle 1.
Referring to fig. 1 and 2, the reaction kettle 1 includes a kettle body 11 and a kettle cover 12, wherein the kettle body 11 is located at the lower side of the kettle cover 12 and is connected with the kettle cover 12 through a plurality of bolts. The kettle cover 12 is connected with a feeding pipe 121 communicated with the interior of the kettle body 11, the bottom wall of the kettle body 11 is in a concave arc shape and is fixedly connected with a discharging pipe 111, and the discharging pipe 111 can be connected with a switch valve to control the opening or closing of the switch valve. When the methoxyamine hydrochloride is synthesized, raw materials such as water, sodium hydroxide, butanone oxime and a phase transfer catalyst can be added into the kettle body 11 from the feeding pipe 121, and the raw materials are discharged from the discharging pipe 111 after the reaction is finished.
Referring to fig. 2 and 3, a stirring mechanism 2, a cleaning mechanism 3 and a washing component 4 are arranged in the reaction kettle 1, the stirring mechanism 2 comprises a first stirring component 21 and a second stirring component 22, the first stirring component 21 is arranged in the middle of the kettle body 11, the second stirring component 22 is arranged on the side wall of the kettle body 11, and the stirring effect of the stirring mechanism 2 on the reaction liquid and the uniform reaction of the raw materials are improved under the combined action of the first stirring component 21 and the second stirring component 22.
Referring to fig. 2 and 3, the first stirring assembly 21 includes a first stirring motor 211, a stirring shaft 212 fixedly connected to an output shaft of the first stirring motor 211, and a plurality of stirring paddles 213 fixed to the stirring shaft 212, the first stirring motor 211 is installed outside the kettle cover 12, the stirring shaft 212 and the stirring paddles 213 are both located in the middle of the kettle body 11, and the stirring paddles 213 are disposed in an inclined manner and are located at a lower end of one end of the stirring shaft 212. The first stirring motor 211 may drive the stirring shaft 212 to rotate, thereby causing the stirring paddle 213 to stir the reaction liquid located in the middle of the tank 11.
Referring to fig. 2 and 3, the second stirring assembly 22 includes a second stirring motor 221, a driving gear 222 fixedly connected to an output shaft of the second stirring motor 221, a driven gear 223 engaged with the driving gear 222, and a plurality of stirring blades 224 fixed to an inner wall of the driven gear 223, wherein the plurality of stirring blades 224 are circumferentially disposed along a central axis of the driven gear 223. The inner wall of the circumference of the kettle body 11 is provided with an annular mounting groove 112, the inner wall of the mounting groove 112 away from the central axis of the kettle body 11 is provided with an accommodating cavity 113, the second stirring motor 221 and the driving gear 222 are located in the accommodating cavity 113, and the second stirring motor 221 is mounted on the upper side wall of the accommodating cavity 113. The driven gear 223 is rotatably connected in the mounting groove 112, and an end surface of the driven gear 223 far from the driving gear 222 is coplanar with an inner wall of the kettle body 11.
Referring to fig. 2 and 3, when the driving gear 222 is driven to rotate by the second stirring motor 221, the driven gear 223 is driven to rotate by the driving gear 222, so that the stirring blade 224 stirs the reaction solution near the sidewall of the tank 11. When the first stirring assembly 21 and the second stirring assembly 22 work simultaneously, the rotation directions of the output shafts of the first stirring motor 211 and the second stirring motor 221 are set to be the same direction, and then the stirring blades 224 and the stirring paddles 213 rotate in opposite directions, so that the reaction liquid forms two different eddy currents in two directions, and the raw materials react uniformly.
Referring to fig. 2 and 3, a plurality of universal wheels 225 are connected to the bottom of the driven gear 223, an annular guide rail 114 is disposed on the inner wall of the lower side of the mounting groove 112, and the bottom of each universal wheel 225 is located in the guide rail 114. When the driven gear 223 rotates, the universal wheel 225 moves along the guide rail 114, and the frictional resistance received by the driven gear 223 is reduced, so that the driven gear 223 moves smoothly.
Referring to fig. 2 and 3, the cleaning mechanism 3 includes a scraper 31, a spray pipe 32, a lifting assembly 33 and a rotating assembly 34, the spray pipe 32 is rotatably connected with the scraper 31 through a connecting assembly 5, the scraper 31 is attached to the side wall of the kettle body 11, and a through hole for the stirring sheet 224 to pass through is formed in the edge of the scraper 31. The spraying pipe 32 is connected with a soft water inlet pipe 321 and a plurality of cleaning nozzles 322, the plurality of cleaning nozzles 322 are circumferentially arranged on the spraying pipe 32, and the water outlet ends of the cleaning nozzles 322 face the side wall of the kettle body 11. The water injected from the water inlet pipe 321 to the shower pipe 32 can be sprayed onto the sidewall of the kettle 11 through the cleaning nozzle 322, so as to wash away the residue on the sidewall of the kettle 11.
Referring to fig. 2 and 3, the connecting assembly 5 includes a sheath 51 and a plurality of connecting rods 52 rotatably connected to the sheath 51, the sheath 51 is fixed on the outer side of the shower pipe 32, the bottom end of the shower pipe 32 extends beyond the sheath 51, and the plurality of connecting rods 52 are circumferentially distributed along the central axis of the sheath 51. The link 52 includes a connecting portion 521 and a rotating portion 522 fixed on the lower side of the connecting portion 521, the upper end of the connecting portion 521 is fixedly connected with the lower end surface of the scraper 31, an annular rotating groove 511 is provided on the circumferential outer wall of the sheath 51, two arc-shaped connecting holes 512 are provided on the upper side wall of the rotating groove 511, and the connecting holes 512 and the rotating groove 511 are concentrically arranged. The connecting portion 521 is positioned in the connecting hole 512 and is rotatable with respect to the connecting hole 512, the rotating portion 522 is positioned in the rotating groove 511 and is rotatable with respect to the rotating groove 511, and the rotating portion 522 abuts against an upper side wall of the rotating groove 511. The link 52 not only serves to connect the sheath 51 and the squeegee 31, but also does not interfere with the relative rotation of the sheath 51 and the squeegee 31.
Referring to fig. 2 and 3, the rotating assembly 34 includes a rotating motor 341 mounted on the upper side of the scraper 31, a rotating gear 342 fixedly connected to an output shaft of the rotating motor 341, and a plurality of driving teeth 343 fixed to the sheath 51, wherein the driving teeth 343 are continuously distributed along the circumferential inner wall of the sheath 51, and the driving teeth 343 are engaged with the rotating gear 342. The rotating motor 341 is a motor capable of rotating in forward and reverse directions, and when the rotating gear 342 is driven to rotate, the transmission gear 343 drives the sheath 51 to drive the shower pipe 32 to rotate, so as to expand the action range of the cleaning nozzle 322 in the horizontal direction.
Referring to fig. 2 and 3, the lifting assembly 33 includes a servo motor 331 installed outside the kettle cover 12, a lifting screw 332 rotatably connected to the kettle 11, and a guide rod 333 fixedly connected to the kettle 11, wherein an output shaft of the servo motor 331 faces downward and is fixedly connected to the lifting screw 332, the lifting screw 332 is in threaded connection with the scraper 31, and the guide rod 333 is inserted into the scraper 31. The servo motor 331 can drive the lifting screw rod 332 to rotate, so that the scraper 31 drives the spray pipe 32 to move longitudinally, the action range of the cleaning nozzle 322 in the vertical direction is expanded, and the cleaning effect is good.
Referring to fig. 2 and 4, the flushing assembly 4 includes a plurality of flushing pipes 41, high-pressure nozzles 42 connected to ends of the flushing pipes 41, and communicating pipes 43 respectively disposed between two adjacent flushing pipes 41, a water outlet direction of the high-pressure nozzles 42 faces a bottom wall of the kettle 11, and one of the communicating pipes 43 is connected with a soft water pipe 44. The bottom wall of the kettle body 11 is provided with fixing grooves 115 with the same number as the flushing pipes 41 along the circumferential direction, communication grooves 116 communicated with the fixing grooves 115 are arranged between every two adjacent fixing grooves 115, and each communication pipe 43 is positioned in each communication groove 116. The water pipe 44 may be used to inject water into the communicating pipe 43, so that the water flows into the flushing pipe 41 and is sprayed to the bottom wall of the kettle body 11 through the high pressure nozzle 42.
Referring to fig. 2 and 4, the flushing pipe 41 includes a moving pipe 411 and a water hose 412 fixed to a side wall of the moving pipe 411, the moving pipe 411 is hinged to an upper inner wall of the fixing groove 115, the high pressure nozzle 42 is connected to an end of the moving pipe 411 remote from a portion where it is hinged to the fixing groove 115, and an end of the water hose 412 remote from the moving pipe 411 is connected to the communicating pipe 43 adjacent thereto. The side wall of the fixed groove 115 far from the central axis of the kettle body 11 is provided with a movable cylinder 45, and a piston rod of the movable cylinder 45 is hinged with one end of the movable pipe 411 close to the high-pressure nozzle 42. When the piston rod of the moving cylinder 45 extends or retracts, the moving pipe 411 can be driven to rotate at one end close to the high-pressure nozzle 42, so that the water flow spraying direction of the high-pressure nozzle 42 is changed, and the washing effect is improved.
The implementation principle of the method for synthesizing methoxylamine hydrochloride in the embodiment of the application is as follows: the synthetic raw materials are not added with sulfur dioxide, sodium nitrite and other substances with high toxicity, the reaction condition is mild, the discharge amount of nitrogen oxide and other waste gases during synthesis is small, the operation environment is good, and the energy is saved and the environment is protected. After the reaction is finished, water is injected from the water inlet pipe 321 to the shower pipe 32, so that the water is sprayed from the cleaning nozzle 322 to the side wall of the kettle 11, thereby flushing the residue on the side wall of the kettle 11. The lifting assembly 33 can drive the scraper 31 to move longitudinally, not only expands the action range of the cleaning nozzle 322 in the vertical direction, but also can scrape the residues which are not flushed off the side wall of the kettle body 11. The rotating assembly 34 can drive the spraying pipe 32 to rotate circumferentially, so that the action range of the cleaning nozzle 322 in the horizontal direction is expanded, and the cleaning effect is good. The water pipe 44 is used for injecting water into the communicating pipe 43, so that the water is sprayed from the high-pressure nozzle 42 to the bottom wall of the kettle body 11, thereby flushing the bottom wall of the kettle body 11. The cleaning mode does not need to disassemble the kettle cover 12 and the kettle body 11, the operation is convenient, and the synthesis efficiency of the methoxylamine hydrochloride is high.
The above embodiments are preferred embodiments of the present application, and the protection scope of the present application is not limited by the above embodiments, so: all equivalent changes made according to the structure, shape and principle of the present application shall be covered by the protection scope of the present application.
Claims (10)
1. A method for synthesizing methoxylamine hydrochloride is characterized in that: comprises the following steps of (a) carrying out,
s1, adding water and sodium hydroxide into the reaction kettle (1), stirring and dissolving at room temperature, and adding butanone oxime and a phase transfer catalyst;
s2, cooling the reaction kettle (1) to 0-15 ℃, and adding a methylating agent into the reaction kettle (1);
s3, standing and layering after reaction to obtain an organic layer and a water layer, distilling the water layer, collecting distillate, combining the oil layer and the distillate, and adding hydrochloric acid to mix uniformly to obtain a mixed solution;
s4, feeding and rectifying the mixed solution from the middle of a rectifying column, controlling the temperature of the lower half part of the rectifying column to be 80-95 ℃, recovering butanone and methanol from the top of the column until no butanone is distilled, recovering methoxylamine hydrochloride solution from the bottom of the column, and heating, evaporating and dehydrating the methoxylamine hydrochloride solution at the bottom of the column to obtain hydrochloride concentrated solution;
s5, cleaning a reaction kettle (1), wherein a stirring mechanism (2) and a cleaning mechanism (3) are arranged in the reaction kettle (1), the cleaning mechanism (3) comprises a scraper (31), a spray pipe (32) rotationally connected to the scraper (31) through a connecting component (5), a lifting component (33) used for driving the scraper (31) to longitudinally move and a rotating component (34) used for driving the spray pipe (32) to circumferentially rotate, and a soft water inlet pipe (321) and a plurality of cleaning nozzles (322) circumferentially arranged are connected to the spray pipe (32); reation kettle (1) is including the cauldron body (11) and kettle cover (12), the lateral wall of the play water end orientation cauldron body (11) of washing nozzle (322), scraper blade (31) and the lateral wall laminating of the cauldron body (11).
2. The method for synthesizing methoxyamine hydrochloride according to claim 1, wherein: lifting unit (33) including install servo motor (331) on kettle cover (12), with the cauldron body (11) rotate lift lead screw (332) of being connected and with the guide bar (333) of the cauldron body (11) fixed connection, the output shaft and the lift lead screw (332) fixed connection of servo motor (331), lift lead screw (332) and scraper blade (31) threaded connection, guide bar (333) are worn to establish on scraper blade (31).
3. The method for synthesizing methoxyamine hydrochloride according to claim 1, wherein: coupling assembling (5) are including fixing sheath (51) in shower (32) outside and rotating many connecting rods (52) of connection on sheath (51), connecting rod (52) are including fixing connecting portion (521) of scraper blade (31) downside and fixing rotation portion (522) of connecting portion (521) downside, be equipped with annular rotation groove (511) on the circumference lateral wall of sheath (51), the last lateral wall that rotates groove (511) is equipped with two rather than the concentricity and is curved connecting hole (512), connecting portion (521) rotate to be connected in connecting hole (512), rotate portion (522) and rotate and connect in rotation groove (511), and rotate portion (522) and rotate the last lateral wall butt in groove (511).
4. The method for synthesizing methoxyamine hydrochloride according to claim 3, wherein: the rotating assembly (34) comprises a rotating motor (341) arranged on the scraper (31), a rotating gear (342) fixedly connected with an output shaft of the rotating motor (341) and transmission teeth (343) continuously distributed on the circumferential side wall of the sheath (51), and the transmission teeth (343) are meshed with the rotating gear (342).
5. The method for synthesizing methoxyamine hydrochloride according to claim 1, wherein: the diapire of the cauldron body (11) is concave arc shape and bottom is connected with discharging pipe (111), still be provided with in the cauldron body (11) and wash subassembly (4), wash subassembly (4) including a plurality of flushing pipes (41) that set up along circumference, connect high pressure nozzle (42) at flushing pipe (41) tip and set up communicating pipe (43) between two adjacent flushing pipes (41), the diapire of the play water direction of high pressure nozzle (42) towards the cauldron body (11), be connected with raceway (44) on one of them communicating pipe (43).
6. The method for synthesizing methoxyamine hydrochloride according to claim 5, wherein: fixing grooves (115) with the same number as the flushing pipes (41) are formed in the bottom wall of the kettle body (11), a communicating groove (116) communicated with the fixing grooves (115) is formed between every two adjacent fixing grooves (115), and the communicating pipe (43) is located in the communicating groove (116); the flushing pipe (41) comprises a moving pipe (411) hinged on the top wall of the fixed groove (115) and a water-through hose (412) connected to the moving pipe (411), and the water-through hose (412) is communicated with the communicating pipe (43) and can guide water into the moving pipe (411); and a movable cylinder (45) is arranged on the side wall of the fixing groove (115) far away from the opening of the fixing groove, and a piston rod of the movable cylinder (45) is hinged with one end of the movable pipe (411) close to the high-pressure nozzle (42).
7. The method for synthesizing methoxyamine hydrochloride according to claim 1, wherein: the stirring mechanism (2) comprises a first stirring assembly (21) and a second stirring assembly (22), wherein the first stirring assembly (21) is arranged in the middle of the kettle body (11), and the second stirring assembly (22) is arranged on the side wall of the kettle body (11).
8. The method for synthesizing methoxyamine hydrochloride according to claim 7, wherein: first stirring subassembly (21) including install first agitator motor (211) on kettle cover (12), with output shaft fixed connection's (mixing) shaft (212) of first agitator motor (211) and connect stirring rake (213) at (mixing) shaft (212) lateral wall, (mixing) shaft (212) and stirring rake (213) all are located the middle part of the cauldron body (11), just stirring rake (213) are the slope setting.
9. The method for synthesizing methoxyamine hydrochloride according to claim 7, wherein: second stirring subassembly (22) include second agitator motor (221), with output shaft fixed connection's of second agitator motor (221) driving gear (222), with driving gear (222) intermeshing driven gear (223) and along a plurality of stirring piece (224) of setting at driven gear (223) inboard along circumference, the circumference inner wall middle part of the cauldron body (11) is equipped with annular mounting groove (112), be equipped with on the inner wall of cauldron body (11) axis is kept away from in mounting groove (112) holding chamber (113), second agitator motor (221) and driving gear (222) are located holding chamber (113), driven gear (223) rotate to be connected in mounting groove (112).
10. The method for synthesizing methoxyamine hydrochloride according to claim 9, wherein: the bottom of driven gear (223) is connected with universal wheel (225), be equipped with annular guide rail (114) on the diapire of mounting groove (112), the bottom of universal wheel (225) is located in guide rail (114).
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| CN202111074645.6A CN113754557A (en) | 2021-09-14 | 2021-09-14 | Method for synthesizing methoxyamine hydrochloride |
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| CN116078761A (en) * | 2023-02-22 | 2023-05-09 | 四川英创力电子科技股份有限公司 | Device and method for efficiently cleaning tank wall of liquid medicine |
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