CN115282907A - Refining device and refining method for high-quality methyl chloroformate - Google Patents

Refining device and refining method for high-quality methyl chloroformate Download PDF

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Publication number
CN115282907A
CN115282907A CN202210826535.9A CN202210826535A CN115282907A CN 115282907 A CN115282907 A CN 115282907A CN 202210826535 A CN202210826535 A CN 202210826535A CN 115282907 A CN115282907 A CN 115282907A
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China
Prior art keywords
seat
cooling
pipe
methyl chloroformate
connecting pipe
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CN202210826535.9A
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Chinese (zh)
Inventor
马涛
王震宇
朱玉昊
胡梓杨
朱张
缪建勇
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Anhui Guangxin Agrochemcial Co Ltd
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Anhui Guangxin Agrochemcial Co Ltd
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Priority to CN202210826535.9A priority Critical patent/CN115282907A/en
Publication of CN115282907A publication Critical patent/CN115282907A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/18Stationary reactors having moving elements inside
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D3/00Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/009Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping in combination with chemical reactions
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0006Controlling or regulating processes
    • B01J19/0013Controlling the temperature of the process
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C68/00Preparation of esters of carbonic or haloformic acids
    • C07C68/08Purification; Separation; Stabilisation

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  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention discloses a refining device and a refining method for high-quality methyl chloroformate, relates to the technical field of methyl chloroformate refining device structures, and aims to solve the problem that the existing high-quality methyl chloroformate cannot well refine methyl chloroformate in a preparation process device. The heating jacket is arranged on the periphery of the outer wall of the reaction kettle, the exhaust seat is installed above the reaction kettle, the first electromagnetic valve is installed above the exhaust seat, the first connecting pipe is installed above the first electromagnetic valve, the cooling device box is installed at one end of the first connecting pipe, the spiral cooling pipe is installed inside the cooling device box, the second connecting seat is arranged on one side of the outer wall of the cooling device box, the second connecting pipe is installed on one side of the second connecting seat, the storage box is installed on one side of the second connecting pipe, the exhaust seat is arranged above the second connecting seat, the third connecting pipe is installed on one side of the exhaust seat, and the purifying device box is installed on one side of the third connecting pipe.

Description

Refining device and refining method for high-quality methyl chloroformate
Technical Field
The invention relates to the technical field of methyl chloroformate refining device structures, in particular to a refining device and a refining method for high-quality methyl chloroformate.
Background
Methyl chloroformate is an organic compound, is a colorless transparent liquid, has pungent odor, is extremely toxic, is insoluble in water, is dissolved in most organic solvents such as benzene, methanol, ether, ethanol and the like, is used as an organic synthesis intermediate, is used for preparing herbicides, bactericide carbendazim and the like in the pesticide industry, is also a raw material of pharmacy and lachrymatory toxicant, and needs to be paid attention to avoid the leakage of a refining device of the methyl chloroformate in the preparation process.
Chinese patent grant publication No. CN205815679U, grant announcement day 2016, 12 months 21 days, a methyl chloroformate low-loss reaction kettle, including cauldron body shell and the internal container of cauldron, form cavity in between cauldron body shell and the internal container of cauldron, be provided with the condensation circulating pipe that coils the internal container of cauldron in the cavity, be equipped with the feed inlet that communicates with cauldron body container on the lateral wall of cauldron body shell, cauldron body shell bottom is equipped with the discharge gate that communicates with cauldron body container, is provided with agitating unit in the internal container of cauldron, agitating unit includes first (mixing) shaft and second (mixing) shaft, and first (mixing) shaft is provided with the first stirring vane of a plurality of slopes along length direction, and the second (mixing) shaft is provided with the second stirring vane of a plurality of slopes along length direction, first (mixing) shaft and second (mixing) shaft top pass respectively cauldron body shell roof and are connected with the decelerator output that corresponds, and stirring effect is good, and the raw materials are mixed from top to bottom, and esterification reaction is abundant, and the product conversion is high, and condensation recovery effect is good.
However, the existing high-quality methyl chloroformate cannot be well purified in the preparation process, so that a high-quality methyl chloroformate purifying device and a high-quality methyl chloroformate purifying method are urgently needed in the market to solve the problems.
Disclosure of Invention
The invention aims to provide a refining device and a refining method for high-quality methyl chloroformate, which aim to solve the problem that the prior device for refining the high-quality methyl chloroformate in the preparation process cannot well refine the methyl chloroformate in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme: the utility model provides a refining plant of high-quality methyl chloroformate, includes reation kettle, sealed lid is installed to reation kettle's top, reation kettle's outer wall is provided with the heating jacket all around, reation kettle's lower extreme is provided with the flowing back seat, reation kettle's top is installed the motor, one side of motor is provided with the exhaust seat, the opposite side of motor is provided with the charging seat, reation kettle's one end is provided with the feed liquor seat, the feed liquor pipe is installed to one side of feed liquor seat, the delivery pump is installed to the one end of feed liquor pipe, the lower extreme of sealed lid is provided with the rotation mount pad, the axis of rotation is installed to the below of rotation mount pad, the stirring leaf is installed to the one end of axis of rotation, solenoid valve one is installed to the top of exhaust seat, connecting pipe one is installed to the top of solenoid valve one, the cooling device case is installed to the one end of connecting pipe one, the internally mounted of cooling device case has the spiral cooling tube, the cooling tube is installed to the top of spiral cooling tube, the lower extreme of spiral cooling device is provided with two corresponding with the connecting seat with the connecting pipe, connecting pipe is installed to one side of storage second, connecting pipe one side of connecting seat, the exhaust seat is provided with the purification device top of three connecting pipe.
Preferably, the supporting seat is installed at the lower end of the reaction kettle, the flange connecting seat is arranged at the upper end of the reaction kettle, the flange mounting seat is arranged at the lower end of the sealing cover, and the flange mounting seat is fixedly connected with the flange connecting seat through a fixing bolt.
Preferably, the heating jacket is internally provided with a heating coil, and the front end of the reaction kettle is provided with a heating device box corresponding to the heating jacket.
Preferably, one end of the cooling device box is provided with an air inlet seat corresponding to the first connecting pipe, the air inlet seat is fixedly connected with the first connecting pipe through a fixing screw, one end of the inner wall of the cooling device box is provided with a first mounting seat, the other end of the inner wall of the cooling device box is provided with a second mounting seat corresponding to the exhaust seat, one end of the spiral cooling pipe is fixedly connected with the first mounting seat through a screw, and the other end of the spiral cooling pipe is fixedly connected with the second mounting seat through a screw.
Preferably, the rotating shaft is fixedly connected with the rotating mounting seat through a hexagon screw, and the rotating shaft is fixedly connected with the stirring blade through a fastening screw.
Preferably, the one end of cooling tube is provided with connecting seat one, the back flow is installed to one side of connecting seat one, the drawing liquid pump is installed to the one end of back flow, the drawing liquid pipe is installed to one side of drawing liquid pump, the one end of drawing liquid pipe is located the inside of cooling device case, the shower nozzle is installed to the below of cooling tube, the shower nozzle is provided with a plurality of, a plurality of the shower nozzle distributes in proper order at the lower extreme of cooling tube.
Preferably, one end of the purifying device box is provided with a first fixing seat corresponding to the three phases of the connecting pipe, the other end of the purifying device box is provided with a second fixing seat, the upper end of one side of the second fixing seat is provided with a gas monitoring device, and one side of the second fixing seat is provided with a second electromagnetic valve.
Preferably, the inside of purifier case is provided with the installation room, the both ends of installation room all are provided with spacing mounting groove, installation room installation internally mounted has filter equipment, filter equipment's both ends are provided with the spacing lug corresponding with spacing mounting groove, filter equipment's front end is provided with the stiff end, through fixed screw fixed connection between stiff end and the purifier case.
The refining method of the refining device of the high-quality methyl chloroformate comprises the following steps:
step 1: adding water into the reaction kettle by turning on a delivery pump, then adding the prepared methyl chloroformate solution into the reaction kettle from a feeding seat, and then heating the reaction kettle by controlling a heating coil through a heating device box to heat the mixed solution to 75 degrees;
step 2: the motor is started, the rotating shaft drives the stirring blades to rotate, the mixed solution can be stirred through the rotation of the stirring blades, so that the mixed solution can be uniformly heated, the prepared methyl chloroformate solution is heated to 75 ℃ and reaches a boiling point, and the methyl chloroformate solution is gasified;
and step 3: then, the gasified methyl chloroformate steam is discharged through an exhaust seat by opening a first electromagnetic valve, then enters a cooling pipe arranged in a cooling device box through a first connecting pipe, then the liquid pump is opened to draw the cooling liquid in the cooling device box by the liquid pump, so that the cooling liquid enters the cooling pipe through a return pipe and is sprayed out through a spray head, and therefore the spiral cooling pipe can be effectively cooled, the methyl chloroformate steam is cooled, and the sprayed cooling water is stored in the cooling device box, and the cooling water can be recycled;
and 4, step 4: the cooled methyl chloroformate is liquefied into a methyl chloroformate solution, the methyl chloroformate solution flows in the spiral cooling pipe and then enters the storage box through the connecting pipe II through the material conveying pipe to be stored, and the refined methyl chloroformate solution can be conveniently taken and used through the arranged discharging seat;
and 5: the gas that does not liquefy continues to enter into purifier incasement portion through connecting pipe three, and two filter equipment through the installation can be fine carry out filtration purification to gas, when gas monitoring device detected to reach emission standard, open through control solenoid valve two to discharge gas.
Compared with the prior art, the invention has the beneficial effects that:
1. this kind of refining plant of high-quality methyl chloroformate, add reation kettle's inside through opening the delivery pump with water, then add reation kettle's inside from reinforced seat with the methyl chloroformate solution of preparation, then heat reation kettle through heating device case control heating coil, make mixed liquid heat to 75, through opening the motor, make the axis of rotation drive stirring leaf rotate, it can stir mixed liquid to rotate through the stirring leaf, can make like this that mixed liquid can be even heat, the methyl chloroformate solution of preparation heats 75 and reaches the boiling point, gasification appears in methyl chloroformate solution this moment, then through opening the methyl chloroformate steam that the solenoid valve one made gasification, discharge through the exhaust seat, set up the methyl chloroformate that can be convenient through this kind and refine.
2. This kind of refining plant of high-quality methyl chloroformate, make gasified methyl chloroformate steam through opening solenoid valve one, discharge through the exhaust seat, then enter into the cooling tube that the cooling device incasement portion set up through connecting pipe one, then through opening the drawing liquid pump, make the drawing liquid pump draw the coolant liquid of cooling device incasement portion, make the coolant liquid enter into the inside of cooling tube through the back flow, then spray out through the shower nozzle, can effectually cool down spiral cooling tube like this, make methyl chloroformate steam cool off, the cooling water that sprays accumulates in the cooling device incasement portion, make the cooling water can circulate and use like this, methyl chloroformate liquefaction becomes methyl chloroformate solution after the cooling, methyl chloroformate solution flows in spiral cooling tube inside, then enter into the storage incasement portion through connecting pipe two and store.
3. This kind of refining plant of high-quality methyl chloroformate, the gas that does not liquefy continues to enter into purifier incasement portion through connecting pipe three, two filter equipment through the installation can be fine carry out filtration purification to gas, when gas monitoring devices detected to reach emission standard, open through control solenoid valve two, thereby discharge gas, avoid remaining gaseous direct discharge to cause the pollution to the air, and residual gas has certain toxicity, may cause bigger danger.
Drawings
FIG. 1 is an overall front view of the present invention;
FIG. 2 is an overall cross-sectional view of the present invention;
FIG. 3 is an enlarged view of a portion of the area A of FIG. 2 according to the present invention;
FIG. 4 is an enlarged view of a portion of the area B of FIG. 2 according to the present invention;
fig. 5 is a partial enlarged view of the region C of fig. 2 according to the present invention.
In the figure: 1. a reaction kettle; 101. a flange connecting seat; 102. a liquid inlet seat; 103. a liquid discharge seat; 2. a sealing cover; 201. a flange mounting seat; 202. a feeding seat; 203. an exhaust seat; 3. fixing the bolt; 4. a heating jacket; 5. a heating coil; 6. a supporting base; 7. a heating device case; 8. a motor; 9. a first electromagnetic valve; 10. a first connecting pipe; 1001. a set screw; 11. a cooling device case; 1101. an air inlet seat; 1102. a first mounting seat; 1103. a second mounting base; 1104. a first connecting seat; 1105. a second connecting seat; 1106. an exhaust seat; 12. a liquid inlet pipe; 13. a delivery pump; 14. rotating the mounting seat; 15. a rotating shaft; 16. a hex screw; 17. stirring blades; 18. fastening screws; 19. a spiral cooling tube; 20. a delivery pipe; 21. a cooling tube; 22. a spray head; 23. a return pipe; 24. a liquid pump; 25. a liquid pumping pipe; 26. a second connecting pipe; 27. a material storage box; 28. a discharging seat; 29. a third connecting pipe; 30. a purification device case; 3001. a first fixed seat; 3002. a second fixed seat; 3003. an installation chamber; 3004. a limiting mounting groove; 31. a gas monitoring device; 32. a second electromagnetic valve; 33. a filtration device; 3301. a limiting bump; 34. a fixed end; 35. and (7) fixing the screw.
Detailed Description
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, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments.
Referring to fig. 1-5, an embodiment of the present invention is shown: the utility model provides a refining plant of high-quality methyl chloroformate, including reation kettle 1, sealed lid 2 is installed to reation kettle 1's top, reation kettle 1's outer wall is provided with heating jacket 4 all around, reation kettle 1's lower extreme is provided with flowing back seat 103, reation kettle 1's top is installed motor 8, one side of motor 8 is provided with exhaust seat 203, the opposite side of motor 8 is provided with feeding seat 202, reation kettle 1's one end is provided with feed liquor seat 102, feed liquor pipe 12 is installed to one side of feed liquor seat 102, the one end of feed liquor pipe 12 is installed delivery pump 13, the lower extreme of sealed lid 2 is provided with rotation mount 14, the axis of rotation 15 is installed to the below of rotation mount 14, stirring vane 17 is installed to the one end of axis of rotation 15, solenoid valve one 9 is installed to the top of exhaust seat 203, connecting pipe one 10 is installed to the top of solenoid valve one 9, cooling device case 11 is installed to one end of connecting pipe one 10, the internally mounted has spiral cooling device 19, cooling device case 19 is installed to the top, cooling device 19 is installed to the lower extreme, one side of connecting seat is provided with two 1105 corresponding to connecting seat 1105, connecting seat 29 one side of connecting seat 1106 is provided with the storage material of connecting pipe 20, the connecting seat 27 of connecting seat is installed to one side of connecting pipe, the purifying device of connecting seat 29, the discharging seat 26 of connecting pipe is provided with the three connecting pipe 27, discharge of discharging of connecting pipe 27, discharge seat 27.
Referring to fig. 1, a support seat 6 is installed at the lower end of a reaction kettle 1, a flange connection seat 101 is installed at the upper end of the reaction kettle 1, a flange installation seat 201 is installed at the lower end of a sealing cover 2, the flange installation seat 201 and the flange connection seat 101 are fixedly connected through a fixing bolt 3, and the reaction kettle 1 and the sealing cover 2 can be conveniently installed and fixed through the arrangement.
Referring to fig. 2, a heating coil 5 is installed inside the heating jacket 4, and a heating device box 7 corresponding to the heating jacket 4 is installed at the front end of the reaction vessel 1, so that the reaction vessel 1 can be conveniently heated.
Referring to fig. 2 and 3, an air inlet seat 1101 corresponding to the first connecting pipe 10 is disposed at one end of the cooling device box 11, the air inlet seat 1101 is fixedly connected with the first connecting pipe 10 through a fixing screw 1001, a first mounting seat 1102 is disposed at one end of the inner wall of the cooling device box 11, a second mounting seat 1103 corresponding to the exhaust seat 1106 is disposed at the other end of the inner wall of the cooling device box 11, one end of the spiral cooling pipe 19 is fixedly connected with the first mounting seat 1102 through a screw, the other end of the spiral cooling pipe 19 is fixedly connected with the second mounting seat 1103 through a screw, methyl chloroformate steam can be rapidly cooled through the cooling device box 11, and the cooling effect of the methyl chloroformate steam can be better through the spiral cooling pipe 19.
Referring to fig. 2, the rotating shaft 15 is fixedly connected with the rotating mounting seat 14 through a hexagon screw 16, and the rotating shaft 15 is fixedly connected with the stirring blade 17 through a fastening screw 18, so that the rotating shaft 15 and the rotating mounting seat 14 can be conveniently mounted and fixed, and the rotating shaft 15 and the stirring blade 17 can be conveniently mounted and fixed.
Referring to fig. 2, one end of the cooling pipe 21 is provided with a first connecting seat 1104, a return pipe 23 is installed on one side of the first connecting seat 1104, an extraction pump 24 is installed on one end of the return pipe 23, an extraction pipe 25 is installed on one side of the extraction pump 24, one end of the extraction pipe 25 is located inside the cooling device box 11, a plurality of spray heads 22 are installed below the cooling pipe 21, the plurality of spray heads 22 are sequentially distributed at the lower end of the cooling pipe 21, and through the arrangement, the cooling liquid can be uniformly sprayed, so that methyl chloroformate gas inside the spiral cooling pipe 19 is cooled.
Referring to fig. 2, 4 and 5, one end of the purifying device box 30 is provided with a first fixing seat 3001 corresponding to the third connecting pipe 29, the other end of the purifying device box 30 is provided with a second fixing seat 3002, the upper end of one side of the second fixing seat 3002 is provided with a gas monitoring device 31, one side of the second fixing seat 3002 is provided with a second electromagnetic valve 32, the gas can be filtered and purified well by installing the gas monitoring device 31, and when the gas monitoring device 31 detects that the gas reaches the emission standard, the second electromagnetic valve 32 is controlled to be opened, so that the gas is emitted.
Referring to fig. 2 and 5, an installation chamber 3003 is disposed inside the purification device box 30, two ends of the installation chamber 3003 are both provided with a limit installation slot 3004, a filter device 33 is installed inside the installation chamber 3003, two ends of the filter device 33 are provided with limit bumps 3301 corresponding to the limit installation slot 3004, a fixed end 34 is disposed at the front end of the filter device 33, the fixed end 34 is fixedly connected with the purification device box 30 through a fixing screw 35, and the filter device 33 is installed to filter and purify residual gas, so as to prevent the residual gas from being directly discharged to pollute air, and the residual gas has certain toxicity and may cause greater danger.
The refining method of the refining device of the high-quality methyl chloroformate comprises the following steps:
step 1: adding water into the reaction kettle 1 by turning on the delivery pump 13, then adding the prepared methyl chloroformate solution into the reaction kettle 1 from the feeding seat 202, and then heating the reaction kettle 1 by controlling the heating coil 5 through the heating device box 7 to heat the mixed solution to 75 degrees;
step 2: the motor 8 is turned on, the rotating shaft 15 drives the stirring blade 17 to rotate, the mixed solution can be stirred through the rotation of the stirring blade 17, so that the mixed solution can be uniformly heated, the prepared methyl chloroformate solution is heated to 75 ℃ and reaches the boiling point, and the methyl chloroformate solution is gasified;
and 3, step 3: then, the gasified methyl chloroformate steam is discharged through the exhaust seat 203 by opening the electromagnetic valve I9, then enters the cooling pipe 21 arranged in the cooling device box 11 through the connecting pipe I10, then the liquid-extracting pump 24 is opened to extract the cooling liquid in the cooling device box 11 by the liquid-extracting pump 24, so that the cooling liquid enters the cooling pipe 21 through the return pipe 23, and then is sprayed out through the spray head 22, so that the spiral cooling pipe 19 can be effectively cooled, the methyl chloroformate steam is cooled, and the sprayed cooling water is accumulated in the cooling device box 11, so that the cooling water can be recycled;
and 4, step 4: the cooled methyl chloroformate is liquefied into a methyl chloroformate solution, the methyl chloroformate solution flows in the spiral cooling pipe 19 and then enters the storage box 27 through the material conveying pipe 20 through the second connecting pipe 26 for storage, and the refined methyl chloroformate solution can be conveniently taken and used through the arranged discharging seat 28;
and 5: the unliquefied gas continues to enter the purifying device box 30 through the third connecting pipe 29, the gas can be well filtered and purified through the two installed filtering devices 33, and when the gas monitoring device 31 detects that the gas reaches the emission standard, the second electromagnetic valve 32 is controlled to be opened, so that the gas is discharged.
The working principle is as follows: when in use, water is added into a reaction kettle 1 by opening a delivery pump 13, then the prepared methyl chloroformate solution is added into the reaction kettle 1 from a feeding seat 202, then the reaction kettle 1 is heated by controlling a heating coil 5 through a heating device box 7, the mixed solution is heated to 75 degrees, a motor 8 is turned on, a rotating shaft 15 drives a stirring blade 17 to rotate, the mixed solution can be stirred by rotating the stirring blade 17, the mixed solution can be uniformly heated, the prepared methyl chloroformate solution is heated to 75 degrees and reaches a boiling point, the methyl chloroformate solution is gasified, then gasified by opening a solenoid valve I9, gasified methyl chloroformate vapor is discharged through an exhaust seat 203, then the mixed solution enters a cooling pipe 21 arranged in a cooling device box 11 through a first connecting pipe 10, then the prepared methyl chloroformate solution is heated to 75 degrees and reaches the boiling point, a liquid pump 24 is started to pump the cooling liquid in the cooling device box 11, the cooling liquid enters a cooling pipe 21 through a first connecting pipe 23, then is sprayed out through a spray nozzle 22, the spiral cooling device 19 can effectively cool the methyl chloroformate vapor, the cooling liquid in the cooling device box 11, the cooling device can be purified by filtering the liquefied gas, the liquefied methyl chloroformate, the liquefied gas in the cooling device 20, the cooling device can be filtered, the liquefied gas, the cooling device 20, the liquefied gas storage device can be purified by using a spiral connecting pipe 19, the spiral filtering device, the spiral methyl chloroformate storage device, the spiral cooling device 20, when the gas monitoring device 31 detects that the emission standard is met, the second electromagnetic valve 32 is controlled to be opened, so that the gas is emitted.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.

Claims (9)

1. A refining plant of high-quality methyl chloroformate, including reation kettle (1), characterized by: sealed lid (2) is installed to the top of reation kettle (1), the outer wall of reation kettle (1) is provided with heating jacket (4) all around, the lower extreme of reation kettle (1) is provided with flowing back seat (103), motor (8) are installed to the top of reation kettle (1), one side of motor (8) is provided with exhaust seat (203), the opposite side of motor (8) is provided with feeding seat (202), the one end of reation kettle (1) is provided with feed liquor seat (102), feed liquor pipe (12) is installed to one side of feed liquor seat (102), delivery pump (13) are installed to the one end of feed liquor pipe (12), the lower extreme of sealed lid (2) is provided with rotation mount pad (14), rotation axis (15) is installed to the below of rotation mount pad (14), stirring leaf (17) is installed to the one end of rotation axis (15), solenoid valve (9) is installed to the top of exhaust seat (203), connecting pipe (10) is installed to the top of solenoid valve (9), cooling device case (11) is installed to the one end of connecting pipe (10), the internally mounted of cooling device case (11) has spiral cooling tube (19), cooling tube (19) is installed the cooling tube (19), cooling tube (21) is provided with lower extreme (20), one side of cooling device case (11) outer wall is provided with two (1105) of connecting seat corresponding with conveying pipeline (20), connecting pipe two (26) are installed to one side of connecting seat two (1105), storage case (27) are installed to one side of connecting pipe two (26), the lower extreme of storage case (27) one side is provided with unloading seat (28), the top of connecting seat two (1105) is provided with exhaust seat (1106), connecting pipe three (29) are installed to one side of exhaust seat (1106), purifier case (30) are installed to one side of connecting pipe three (29).
2. The apparatus according to claim 1, wherein said apparatus further comprises: supporting seat (6) is installed to the lower extreme of reation kettle (1), the upper end of reation kettle (1) is provided with flange joint seat (101), the lower extreme of sealed lid (2) is provided with flange mounting seat (201), pass through fixing bolt (3) fixed connection between flange mounting seat (201) and flange joint seat (101).
3. The apparatus according to claim 1, wherein said apparatus further comprises: the heating device is characterized in that a heating coil (5) is arranged inside the heating jacket (4), and a heating device box (7) corresponding to the heating jacket (4) is arranged at the front end of the reaction kettle (1).
4. The apparatus according to claim 1, wherein said apparatus further comprises: one end of the cooling device box (11) is provided with an air inlet seat (1101) corresponding to the first connecting pipe (10), the air inlet seat (1101) is fixedly connected with the first connecting pipe (10) through a fixing screw (1001), one end of the inner wall of the cooling device box (11) is provided with a first mounting seat (1102), the other end of the inner wall of the cooling device box (11) is provided with a second mounting seat (1103) corresponding to the exhaust seat (1106), one end of the spiral cooling pipe (19) is fixedly connected with the first mounting seat (1102) through a screw, and the other end of the spiral cooling pipe (19) is fixedly connected with the second mounting seat (1103) through a screw.
5. The apparatus according to claim 1, wherein said apparatus further comprises: the rotating shaft (15) is fixedly connected with the rotating mounting seat (14) through a hexagon screw (16), and the rotating shaft (15) is fixedly connected with the stirring blade (17) through a fastening screw (18).
6. The apparatus according to claim 1, wherein said apparatus further comprises: the one end of cooling tube (21) is provided with connecting seat (1104), back flow (23) are installed to one side of connecting seat (1104), drawing liquid pump (24) are installed to the one end of back flow (23), drawing liquid pipe (25) are installed to one side of drawing liquid pump (24), the one end of drawing liquid pipe (25) is located the inside of cooling device case (11), shower nozzle (22) are installed to the below of cooling tube (21), shower nozzle (22) are provided with a plurality of, a plurality of shower nozzle (22) distribute in proper order at the lower extreme of cooling tube (21).
7. The apparatus according to claim 1, wherein said apparatus further comprises: one end of the purification device box (30) is provided with a first fixing seat (3001) corresponding to the third connecting pipe (29), the other end of the purification device box (30) is provided with a second fixing seat (3002), the upper end of one side of the second fixing seat (3002) is provided with a gas monitoring device (31), and the second electromagnetic valve (32) is installed on one side of the second fixing seat (3002).
8. The apparatus according to claim 1, wherein said apparatus further comprises: the inside of purifier case (30) is provided with installation room (3003), the both ends of installation room (3003) all are provided with spacing mounting groove (3004), installation room (3003) installation internally mounted has filter equipment (33), the both ends of filter equipment (33) are provided with spacing lug (3301) corresponding with spacing mounting groove (3004), the front end of filter equipment (33) is provided with stiff end (34), through fixed screw (35) fixed connection between stiff end (34) and purifier case (30).
9. The purification method based on the purification apparatus for high-quality methyl chloroformate according to any one of claims 1 to 8, characterized by comprising the steps of:
step 1: adding water into the reaction kettle (1) by turning on a delivery pump (13), then adding the prepared methyl chloroformate solution into the reaction kettle (1) from a feeding seat (202), and then heating the reaction kettle (1) by controlling a heating coil (5) through a heating device box (7) to heat the mixed solution to 75 degrees;
step 2: the motor (8) is turned on to enable the rotating shaft (15) to drive the stirring blade (17) to rotate, the mixed solution can be stirred through the rotation of the stirring blade (17), so that the mixed solution can be uniformly heated, the prepared methyl chloroformate solution is heated to 75 ℃ to reach a boiling point, and the methyl chloroformate solution is gasified;
and step 3: then, the gasified methyl chloroformate steam is discharged through an exhaust seat (203) by opening a first electromagnetic valve (9), then enters a cooling pipe (21) arranged in a cooling device box (11) through a first connecting pipe (10), and then is sprayed out through a spray head (22) by opening a liquid pump (24), so that the liquid pump (24) pumps the cooling liquid in the cooling device box (11), the cooling liquid enters the cooling pipe (21) through a return pipe (23), and the cooling liquid can be effectively cooled down through a spiral cooling pipe (19), the sprayed cooling water is stored in the cooling device box (11), and the cooling water can be recycled;
and 4, step 4: the cooled methyl chloroformate is liquefied into a methyl chloroformate solution, the methyl chloroformate solution flows in the spiral cooling pipe (19), then enters the storage box (27) through the connecting pipe II (26) through the conveying pipe (20) to be stored, and the refined methyl chloroformate solution can be conveniently taken and used through the arranged discharging seat (28);
and 5: the unliquefied gas continues to enter the purifying device box (30) through the connecting pipe III (29), the gas can be well filtered and purified through the two installed filtering devices (33), and when the gas monitoring device (31) detects that the gas reaches the discharge standard, the gas is opened through the control electromagnetic valve II (32), so that the gas is discharged.
CN202210826535.9A 2022-07-13 2022-07-13 Refining device and refining method for high-quality methyl chloroformate Pending CN115282907A (en)

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Citations (9)

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CN204854401U (en) * 2015-08-17 2015-12-09 河北冠润药业有限公司 Gas -liquid cooling system for chemical production
CN206082496U (en) * 2016-05-28 2017-04-12 安徽广信农化股份有限公司 But recovery type methyl chloroformate apparatus for producing
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CN109731538A (en) * 2019-03-19 2019-05-10 绵阳市鑫瑞龙扬科技有限责任公司 A kind of online multiple fluorinated systems
CN212741286U (en) * 2020-05-27 2021-03-19 湖南维康酒业有限公司 Distilling machine for processing selenium-rich lake wine
CN213853192U (en) * 2020-11-10 2021-08-03 扬州秀新化工科技有限公司 Fine separation equipment for industrial hemp
CN113398613A (en) * 2021-06-30 2021-09-17 安徽广信农化股份有限公司 Distillation device for azoxystrobin synthesis and distillation method thereof
CN216538436U (en) * 2021-11-12 2022-05-17 佛山市盛代环保化工有限公司 Cooling device for curing agent

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN204854401U (en) * 2015-08-17 2015-12-09 河北冠润药业有限公司 Gas -liquid cooling system for chemical production
CN206082496U (en) * 2016-05-28 2017-04-12 安徽广信农化股份有限公司 But recovery type methyl chloroformate apparatus for producing
CN108043347A (en) * 2017-11-28 2018-05-18 别名洋 A kind of chemical reaction kettle and application method with emission-control equipment
CN108465339A (en) * 2018-04-29 2018-08-31 成都奕州环保科技有限公司 A kind of bitumen flue gas condensation cleaning processing unit
CN109731538A (en) * 2019-03-19 2019-05-10 绵阳市鑫瑞龙扬科技有限责任公司 A kind of online multiple fluorinated systems
CN212741286U (en) * 2020-05-27 2021-03-19 湖南维康酒业有限公司 Distilling machine for processing selenium-rich lake wine
CN213853192U (en) * 2020-11-10 2021-08-03 扬州秀新化工科技有限公司 Fine separation equipment for industrial hemp
CN113398613A (en) * 2021-06-30 2021-09-17 安徽广信农化股份有限公司 Distillation device for azoxystrobin synthesis and distillation method thereof
CN216538436U (en) * 2021-11-12 2022-05-17 佛山市盛代环保化工有限公司 Cooling device for curing agent

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