CN116571181A - Synthesis process of trifluoroacetamide - Google Patents
Synthesis process of trifluoroacetamide Download PDFInfo
- Publication number
- CN116571181A CN116571181A CN202310550570.7A CN202310550570A CN116571181A CN 116571181 A CN116571181 A CN 116571181A CN 202310550570 A CN202310550570 A CN 202310550570A CN 116571181 A CN116571181 A CN 116571181A
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- Prior art keywords
- wall
- shell
- fixedly connected
- pipe
- reaction
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- NRKYWOKHZRQRJR-UHFFFAOYSA-N 2,2,2-trifluoroacetamide Chemical compound NC(=O)C(F)(F)F NRKYWOKHZRQRJR-UHFFFAOYSA-N 0.000 title claims abstract description 25
- 238000000034 method Methods 0.000 title claims abstract description 25
- 230000015572 biosynthetic process Effects 0.000 title claims abstract description 22
- 238000003786 synthesis reaction Methods 0.000 title claims abstract description 22
- 238000006243 chemical reaction Methods 0.000 claims abstract description 51
- 239000007788 liquid Substances 0.000 claims abstract description 42
- 239000012295 chemical reaction liquid Substances 0.000 claims abstract description 29
- 238000005485 electric heating Methods 0.000 claims abstract description 24
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 19
- 230000007797 corrosion Effects 0.000 claims abstract description 15
- 238000005260 corrosion Methods 0.000 claims abstract description 15
- 230000035484 reaction time Effects 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 40
- STSCVKRWJPWALQ-UHFFFAOYSA-N TRIFLUOROACETIC ACID ETHYL ESTER Chemical compound CCOC(=O)C(F)(F)F STSCVKRWJPWALQ-UHFFFAOYSA-N 0.000 claims description 33
- 238000010438 heat treatment Methods 0.000 claims description 14
- 230000002194 synthesizing effect Effects 0.000 claims description 10
- 238000004140 cleaning Methods 0.000 claims description 5
- 239000010865 sewage Substances 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 3
- 238000006386 neutralization reaction Methods 0.000 claims description 3
- 230000001681 protective effect Effects 0.000 claims description 3
- 238000005192 partition Methods 0.000 abstract description 5
- 229910021529 ammonia Inorganic materials 0.000 abstract description 3
- 238000010992 reflux Methods 0.000 abstract description 2
- 238000005096 rolling process Methods 0.000 description 9
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000006884 silylation reaction Methods 0.000 description 3
- XCOBLONWWXQEBS-KPKJPENVSA-N N,O-bis(trimethylsilyl)trifluoroacetamide Chemical compound C[Si](C)(C)O\C(C(F)(F)F)=N\[Si](C)(C)C XCOBLONWWXQEBS-KPKJPENVSA-N 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 230000007935 neutral effect Effects 0.000 description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- -1 amino, amino Chemical group 0.000 description 1
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 1
- 239000013064 chemical raw material Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 150000002085 enols Chemical class 0.000 description 1
- 230000010006 flight Effects 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 239000003317 industrial substance Substances 0.000 description 1
- 230000007794 irritation Effects 0.000 description 1
- 150000004812 organic fluorine compounds Chemical class 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C231/00—Preparation of carboxylic acid amides
- C07C231/02—Preparation of carboxylic acid amides from carboxylic acids or from esters, anhydrides, or halides thereof by reaction with ammonia or amines
-
- 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
- B01J19/0013—Controlling the temperature of the process
-
- 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
- B01J19/1812—Tubular reactors
- B01J19/1818—Tubular reactors in series
-
- 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
-
- 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
- B01J19/20—Stationary reactors having moving elements inside in the form of helices, e.g. screw reactors
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B9/00—Cleaning hollow articles by methods or apparatus specially adapted thereto
- B08B9/08—Cleaning containers, e.g. tanks
- B08B9/0804—Cleaning containers having tubular shape, e.g. casks, barrels, drums
- B08B9/0813—Cleaning containers having tubular shape, e.g. casks, barrels, drums by the force of jets or sprays
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a synthesis process of trifluoroacetamide, which comprises synthesis equipment, wherein the synthesis equipment comprises a case, a protection cylinder is fixedly arranged at the top of the case, a mounting hole is formed in the top of the case, a reaction tank is fixedly arranged on the inner wall of the mounting hole, an end cover is fixedly connected to the top of the reaction tank, a first shell is fixedly connected to the inside of the reaction tank, and a liquid inlet pipe is fixedly communicated with the outer wall of the first shell. According to the invention, ammonia is conveyed into the air inlet pipe through the arrangement of the second shell, the second electric heating plate, the circular ring, the connecting pipe, the air outlet hole, the arc-shaped plate, the partition plate, the one-way valve, the disc, the cavity, the rotating disc, the air inlet groove, the air inlet pipe, the air suction pump and the second motor, the second electric heating plate operates to heat reaction liquid, the corrosion-resistant pump operates to reflux the reaction liquid, the reaction liquid reenters the reaction tank, the reaction liquid is convenient to mix again, the higher conversion rate is achieved, and the reaction time is reduced.
Description
Technical Field
The invention relates to the technical field of trifluoroacetamide production equipment, in particular to a synthesis process of trifluoroacetamide.
Background
The trifluoroacetamide is an important organic chemical raw material, is mainly used for synthesizing partial organic fluorine compounds, can also be used for preparing pesticides, medicines, industrial chemicals and the like, and can be used for preparing N, O-bis (trimethylsilyl) trifluoroacetamide. N, O-bis (trimethylsilyl) trifluoroacetamide is an important medical intermediate, is mainly used as a neutral silylation reagent in the silylation protection of amino, amino acid, phenol, carboxylic acid and enol, and has the advantages of high reaction activity, good selectivity, high reaction yield, simple post-treatment and the like as a mild neutral silylation reagent.
In the prior art, one of them takes ethyl trifluoroacetate as raw materials, and reacts with ammonia gas to prepare trifluoroacetamide, and in the preparation process, the liquid which is not completely reacted is mixed in the neutralized liquid, so that the subsequent processing and production are easily affected, and after the production is finished, the trifluoroacetamide has corrosion and irritation, and the reaction tank needs to be cleaned regularly, so that extra flushing equipment is added to extend into the reaction tank, therefore, we propose a synthesis process of trifluoroacetamide, which is used for solving the problems.
Disclosure of Invention
The invention aims to solve the defects existing in the prior art, and provides a synthesis process of trifluoroacetamide.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
the utility model provides a synthetic process of trifluoroacetamide, includes synthetic equipment, synthetic equipment includes the quick-witted case, quick-witted case top fixed mounting has a protective tube, the mounting hole has been seted up at the top of quick-witted case, the inner wall fixed mounting of mounting hole has the retort, the top fixedly connected with end cover of retort, the inside fixedly connected with first casing of retort, the outer wall fixed intercommunication of first casing has the feed liquor pipe, the inner wall fixedly connected with montant of first casing, the outer wall fixed cover of montant is equipped with a plurality of flight, the outer wall fixed mounting of first casing has a plurality of first electrical heating plates, a plurality of drain holes have evenly been seted up to the outer wall of first casing, the inner wall fixed mounting of retort has the second casing, the outer wall cover of second casing is equipped with a plurality of second electrical heating plates, the inner wall rotation of second casing is connected with the connecting pipe, a plurality of ventholes have been seted up to the outer wall of connecting pipe, the outer wall fixed intercommunication of outer wall rotation cover be equipped with the baffle, the outer wall of baffle and the inner wall fixed connection of retort, the inside of casing is equipped with the drain pipe, the inside of changeover portion of changeover valve is equipped with the drain.
Preferably, the conversion mechanism comprises a disc, the outer wall of retort and the outer wall fixed connection of disc, the cavity has been seted up to the outer wall of disc, the runner has been seted up to the outer wall of cavity, the outer wall sliding connection of disc has the rolling disc, inlet channel and air inlet tank have been seted up to the outer wall of rolling disc, the fixed intercommunication of outer wall of rolling disc has inlet tube and intake pipe, the fixed intercommunication of one end of inlet tube has the water pump, the fixed intercommunication of one end of intake pipe has the aspiration pump, the one end and the inlet channel intercommunication of inlet tube, the one end and the inlet tank intercommunication of intake pipe are through setting up the rolling disc and are taken in air and switch over, conveniently react and wash.
Preferably, the rotating mechanism comprises a second motor, a device frame is fixedly arranged at the bottom of the reaction tank, a first motor is fixedly connected with the inner wall of the device frame, the outer wall of the second motor is fixedly connected with the inner wall of the device frame, a spur gear is fixedly connected with the top of the output shaft of the first motor, the bottom of the connecting pipe is fixedly connected with the outer wall of the disc, the outer wall of the connecting pipe is communicated with the inner wall of the cavity, the top of the second motor is fixedly connected with the outer wall of the connecting pipe, an annular rack is fixedly sleeved on the outer wall of the rotating disc, the annular rack is connected with the spur gear in a meshed mode, two arc grooves are formed in the outer wall of the device frame, and the spur gear is rotated through the arrangement of the first motor, so that the annular rack drives the rotating disc to rotate.
Preferably, the outer wall of the reaction tank contacts with the inner wall of the protection cylinder, a round hole is formed in the outer wall of the reaction tank, the inner wall of the round hole is slidably connected with the outer wall of the liquid inlet pipe, and the reaction tank is supported through the protection cylinder.
Preferably, the outer wall fixedly connected with ring of second casing, the outer wall of ring and the inner wall fixed connection of retort support the second casing through setting up the ring.
Preferably, the outer wall of the arc-shaped piece is contacted with the inner wall of the second shell, the outer wall of the connecting pipe is fixedly provided with a one-way valve, and liquid is prevented from flowing back through the stone one-way valve.
Preferably, the outer wall of the disc is provided with an annular groove, the inner wall of the annular groove is rotationally connected with an annular block, and the outer wall of the annular block is fixedly connected with the outer wall of the rotating disc.
Preferably, through holes are formed in the outer walls of the reaction tank and the second shell, and the inner walls of the through holes are rotationally connected with the outer wall of the connecting pipe.
Preferably, the sliding hole is formed in the outer wall of the rotating disc, the bearing is fixedly connected to the inner wall of the sliding hole, the inner ring of the bearing is fixedly connected with the outer wall of the output shaft of the second motor, and the connecting pipe and the arc-shaped piece are rotated through the second motor, so that liquid is stirred.
Preferably, the outer walls of the reaction tank and the machine case are provided with two assembly holes, the inner walls of the assembly holes are fixedly connected with the outer walls of the liquid outlet pipe and the drain pipe respectively, the outer walls of the liquid outlet pipe, the liquid inlet pipe and the drain pipe are fixedly provided with first valves, the outer walls of the liquid outlet pipe and the liquid inlet pipe are fixedly provided with return pipes, the outer walls of the return pipes are fixedly provided with second valves, the interior of the machine case is fixedly provided with a corrosion-resistant pump, and the input end and the output end of the corrosion-resistant pump are fixedly communicated with the outer walls of the two return pipes respectively;
the synthesis process of the trifluoroacetamide comprises the following specific method steps:
s1, conveying ethyl trifluoroacetate to a first shell through a pump, preheating the ethyl trifluoroacetate in the first shell by a first electric heating sheet at a heating temperature of 30-35 ℃ so as to facilitate subsequent reaction, and increasing the travel of the ethyl trifluoroacetate by a spiral blade to uniformly heat the ethyl trifluoroacetate.
S2, ethyl trifluoroacetate enters the second shell, the second motor is operated to enable the connecting pipe and the arc-shaped piece to rotate, the arc-shaped piece rotates to stir the ethyl trifluoroacetate, the air pump is operated to enable ammonia gas to enter the cavity and the connecting pipe through the flow channel, the ammonia gas and the ethyl trifluoroacetate are subjected to neutralization reaction, and the second electric heating piece is operated to heat reaction liquid, wherein the heating temperature is 50-170 DEG CC.
S3, after the reaction is carried out for 3 to 4 hours, the corrosion resistant pump is operated to convey the reaction liquid in the second shell into the first shell, the first valve is closed, the second valve is opened, the reaction liquid enters from the return pipe on the liquid outlet pipe, the reaction liquid is caused to return, and after the reaction liquid is returned for 3 to 5 times, the subsequent reaction time is required to reach 7 to 8 hours.
S4, the first valve and the second valve are closed, the first motor is operated to enable the water inlet groove and the flow channel to be communicated, and the water inlet groove and the cavity are staggered to perform switching operation.
S5, the water pump is operated to convey water into the cavity, the water enters the connecting pipe through the cavity, the first shell and the second shell are cleaned, the second motor is operated to enable the water to flow, a first valve on the sewage draining pipe is opened to discharge the water after the cleaning is finished, and the first electric heating sheet and the second electric heating sheet are operated to carry out drying treatment.
Compared with the prior art, the invention has the advantages that:
according to the scheme, the first shell, the vertical rods, the spiral sheets, the first electric heating sheets and the liquid outlet holes are arranged, so that the stroke of ethyl trifluoroacetate is increased, and preheating is performed; ammonia is conveyed into the air inlet pipe through the second shell, the second electric heating plate, the circular ring, the connecting pipe, the air outlet hole, the arc-shaped plate, the partition plate, the one-way valve, the disc, the cavity, the rotating disc, the air inlet groove, the air inlet pipe, the air suction pump and the second motor, the second electric heating plate is operated to heat reaction liquid, the corrosion-resistant pump is operated to reflux the reaction liquid, the reaction liquid is reentered into the reaction tank, the reaction liquid is convenient to remix, the higher conversion rate is achieved, and the reaction time is reduced; through setting up first motor, straight-tooth gear, annular rack, intake groove, intake return pipe, second valve, water pump and first valve, switch over the operation, conveniently wash the inside of first casing and second casing.
Drawings
FIG. 1 is a schematic perspective view of a synthesizing apparatus according to the present invention;
FIG. 2 is a schematic cross-sectional view of a synthesizing apparatus according to the present invention;
FIG. 3 is an enlarged schematic view of the portion A in FIG. 2 of the synthesizing apparatus according to the present invention;
FIG. 4 is an enlarged schematic view of the portion B in FIG. 2 of the synthesizing apparatus according to the present invention;
fig. 5 is a schematic view of a partial perspective structure of a synthesizing apparatus according to the present invention.
In the figure: 1. a chassis; 2. a protective cylinder; 3. a reaction tank; 4. an end cap; 5. a liquid inlet pipe; 6. a first housing; 7. a vertical rod; 8. a spiral sheet; 9. a first electric heating plate; 10. a liquid outlet hole; 11. a second housing; 12. a second electric heating plate; 13. a circular ring; 14. a connecting pipe; 15. an air outlet hole; 16. an arc-shaped sheet; 17. a partition plate; 18. a one-way valve; 19. a disc; 20. a cavity; 21. a rotating disc; 22. a water inlet tank; 23. a water inlet pipe; 24. an air inlet groove; 25. an air inlet pipe; 26. a first motor; 27. spur gears; 28. an annular rack; 29. a second motor; 30. an equipment frame; 31. a liquid outlet pipe; 32. a first valve; 33. a return pipe; 34. a second valve; 35. corrosion resistant pump.
Detailed Description
1-5, a trifluoroacetamide synthesis process comprises synthesis equipment, wherein the synthesis equipment comprises a machine case 1, a protection cylinder 2 is fixedly installed at the top of the machine case 1, a mounting hole is formed in the top of the machine case 1, a reaction tank 3 is fixedly installed on the inner wall of the mounting hole, the outer wall of the reaction tank 3 is in contact with the inner wall of the protection cylinder 2, and an end cover 4 is fixedly connected to the top of the reaction tank 3.
The inside fixedly connected with first casing 6 of retort 3, discharge valve is installed to the outer wall of first casing 6, and the fixed intercommunication of outer wall of first casing 6 has feed liquor pipe 5, and the round hole has been seted up to the outer wall of retort 3, the inner wall of round hole and the outer wall sliding connection of feed liquor pipe 5, the inner wall fixedly connected with montant 7 of first casing 6, the fixed cover of the outer wall of montant 7 is equipped with a plurality of flights 8, and helical blade 8 has increased the trifluoroacetic acid ethyl ester stroke.
The outer wall fixed mounting of first casing 6 has a plurality of first electrical heating plates 9, and first electrical heating plate 9 carries out preheating treatment to the ethyl trifluoroacetate in the first casing 6, and a plurality of play liquid holes 10 have evenly been seted up to the outer wall of first casing 6, and the ethyl trifluoroacetate passes through play liquid hole 10 and gets into in the second casing 11.
The inner wall fixed mounting of retort 3 has second casing 11, the outer wall cover of second casing 11 is equipped with a plurality of second electrical heating plates 12, second electrical heating plate 12 operation is continuously heated the reaction liquid, the outer wall fixedly connected with ring 13 of second casing 11, the outer wall of ring 13 and the inner wall fixed connection of retort 3, the inner wall rotation of second casing 11 is connected with connecting pipe 14, the through-hole has all been seted up to the outer wall of retort 3 and second casing 11, the inner wall of through-hole is connected with the outer wall rotation of connecting pipe 14.
The outer wall of connecting pipe 14 has seted up a plurality of ventholes 15, and the outer wall fixedly connected with of connecting pipe 14 a plurality of arc piece 16, and second motor 29 operation makes connecting pipe 14 and arc piece 16 rotate, makes the liquid flow, and the outer wall of arc piece 16 contacts with the inner wall of second casing 11, and the outer wall fixed mounting of connecting pipe 14 has check valve 18, and check valve 18 prevents the liquid backward flow.
The outer wall of the connecting pipe 14 is rotatably sleeved with a partition plate 17, the outer wall of the partition plate 17 is fixedly connected with the inner wall of the reaction tank 3, a conversion mechanism is arranged in the machine case 1, a liquid outlet pipe 31 and a sewage drain pipe are fixedly communicated with the outer wall of the second shell 11, and a rotating mechanism is arranged in the machine case 1.
As shown in fig. 1-5, the conversion mechanism comprises a disc 19, the outer wall of the reaction tank 3 is fixedly connected with the outer wall of the disc 19, a cavity 20 is formed in the outer wall of the disc 19, a flow channel is formed in the outer wall of the cavity 20, ammonia gas enters the flow channel from the air inlet pipe 25, enters the cavity 20 through the flow channel, and the ammonia gas enters the connecting pipe 14 from the cavity 20.
The outer wall sliding connection of disc 19 has rolling disc 21, the ring channel has been seted up to the outer wall of disc 19, the inner wall rotation of ring channel is connected with the annular piece, the outer wall of annular piece and rolling disc 21's outer wall fixed connection, inlet channel 22 and inlet channel 24 have been seted up to rolling disc 21's outer wall, rolling disc 21's outer wall fixed intercommunication has inlet tube 23 and intake pipe 25, the fixed intercommunication of inlet tube 23's one end has the water pump, the fixed intercommunication of one end of intake pipe 25 has the aspiration pump, the aspiration pump operation is with ammonia transportation to in the intake pipe 25, the one end and the inlet channel 22 intercommunication of inlet tube 23, the one end and the inlet channel 24 intercommunication of intake pipe 25.
As shown in fig. 1-5, the rotating mechanism comprises a second motor 29, a sliding hole is formed in the outer wall of the rotating disc 21, a bearing is fixedly connected to the inner wall of the sliding hole, the inner ring of the bearing is fixedly connected with the outer wall of the output shaft of the second motor 29, the bearing assists the second motor 29 to rotate, the rotating disc 21 is prevented from rotating, an equipment frame 30 is fixedly installed at the bottom of the reaction tank 3, and the first motor 26 is fixedly connected to the inner wall of the equipment frame 30.
The outer wall of the second motor 29 is fixedly connected with the inner wall of the equipment frame 30, the equipment frame 30 supports the first motor 26 and the second motor 29, a spur gear 27 is fixedly connected to the top of an output shaft of the first motor 26, the spur gear 27 is operated by operation of the first motor 26, an annular rack 28 is rotated by rotation of the spur gear 27, and the rotating disc 21 is rotated by rotation of the annular rack 28, so that switching operation is performed.
The bottom of connecting pipe 14 and the outer wall fixed connection of disc 19, the outer wall of connecting pipe 14 and the inner wall intercommunication of cavity 20, the top of second motor 29 and the outer wall fixed connection of connecting pipe 14, the outer wall fixed cover of rolling disc 21 is equipped with annular rack 28, the meshing is connected between annular rack 28 and the straight gear 27, two arc grooves 36 have been seted up to the outer wall of equipment frame 30.
Two assembly holes are formed in the outer walls of the reaction tank 3 and the machine case 1, the inner walls of the assembly holes are fixedly connected with the outer walls of the liquid outlet pipe 31 and the drain pipe respectively, the outer walls of the liquid outlet pipe 31, the liquid inlet pipe 5 and the drain pipe are fixedly provided with first valves 32, and the first valves 32 on the drain pipe are opened for discharging after cleaning.
The outer walls of the liquid outlet pipe 31 and the liquid inlet pipe 5 are fixedly provided with return pipes 33, the outer wall of the return pipe 33 is fixedly provided with a second valve 34, the interior of the case 1 is fixedly provided with a corrosion resistant pump 35, the input end and the output end of the corrosion resistant pump 35 are respectively fixedly communicated with the outer walls of the two return pipes 33, and the corrosion resistant pump 35 operates to convey the reaction liquid in the second shell 11 into the first shell 6;
the synthesis process of the trifluoroacetamide comprises the following specific method steps:
s1, conveying ethyl trifluoroacetate to a first shell 6 through a pump, and preheating the ethyl trifluoroacetate in the first shell 6 by a first electric heating sheet 9 at a heating temperature of 30-35 ℃ to facilitate subsequent reaction, wherein the spiral blades 8 increase the stroke of the ethyl trifluoroacetate, so that the ethyl trifluoroacetate is uniformly heated.
S2, ethyl trifluoroacetate enters the second shell 11, the second motor 29 is operated to enable the connecting pipe 14 and the arc-shaped piece 16 to rotate, the arc-shaped piece 16 rotates to stir the ethyl trifluoroacetate, the air pump is operated to enable ammonia gas to enter the cavity 20 and the connecting pipe 14 through the flow channel, the ammonia gas and the ethyl trifluoroacetate are subjected to neutralization reaction, and the second electric heating piece 12 is operated to heat reaction liquid, wherein the heating temperature is 50-170 ℃.
S3, after 3-4 hours of reaction, the corrosion-resistant pump 35 is operated to convey the reaction liquid in the second shell 11 into the first shell 6, the first valve 32 is closed, the second valve 34 is opened, the reaction liquid enters from the return pipe 33 on the liquid outlet pipe 31, the reaction liquid is caused to return, after 3-5 times of return, the subsequent reaction time is required to reach 7-8 hours.
S4, the first valve 32 and the second valve 34 are closed, the first motor 26 is operated to enable the water inlet groove 22 to communicate with the flow passage, and the air inlet groove 24 and the cavity 20 are staggered to perform switching operation.
S5, the water pump is operated to convey water into the cavity 20, the water enters the connecting pipe 14 through the cavity 20, the first shell 6 and the second shell 11 are cleaned, the second motor 29 is operated to enable the water to flow, the first valve 32 on the sewage draining pipe is opened to be discharged after the cleaning is finished, and the first electric heating sheet 9 and the second electric heating sheet 12 are operated to carry out drying treatment.
Working principle: when the device is used, ethyl trifluoroacetate is conveyed into the liquid inlet pipe 5 through the pump, enters the first shell 6 through the liquid inlet pipe 5, flows into the liquid outlet hole 10 through the spiral blade 8, at the moment, the first electric heating sheet 9 carries out preheating treatment on the ethyl trifluoroacetate in the first shell 6, the heating temperature is 30-35 ℃, the subsequent reaction is facilitated, the travel of the ethyl trifluoroacetate is increased through the spiral blade 8, the ethyl trifluoroacetate is uniformly heated, the ethyl trifluoroacetate enters the second shell 11, in the continuous adding process, the second motor 29 is operated to rotate the connecting pipe 14, the connecting pipe 14 is rotated to rotate the arc-shaped sheet 16, the arc-shaped sheet 16 is rotated to stir the ethyl trifluoroacetate, the sucking pump is operated to convey ammonia gas into the air inlet pipe 25, the ammonia gas enters the flow passage from the air inlet pipe 25, enters the cavity 20 through the flow passage, the ammonia gas enters the connecting pipe 14 from the cavity 20, the air outlet hole 15 enters the second shell 11, the ammonia gas and the ethyl trifluoroacetate are neutralized and react, and the second electric heating sheet 12 is operated to heat the reaction liquid, and the heating temperature is 50-170 ℃; after 3 to 4 hours of reaction, the corrosion resistant pump 35 is operated to convey the reaction liquid in the second shell 11 into the first shell 6, the first valve 32 is closed, wherein the first valve 32 on the drain pipe is always in a closed state, the second valve 34 is opened to enable the reaction liquid to enter from the return pipe 33 on the liquid outlet pipe 31, the reaction liquid is enabled to flow back and enter the reaction tank 3 again, the reaction liquid is convenient to be remixed, a higher conversion rate is achieved, the reaction time is reduced, after 3 to 5 times of backflow, the reaction time of the reaction liquid in the second shell 11 is required to reach 7 to 8 hours, the second valve 34 is closed to enable the first valve 32 on the liquid outlet pipe 31 to be opened, the liquid in the second shell 11 is discharged, and when the interiors of the first shell 6 and the second shell 11 are cleaned, the first valve 32 and the second valve 34 are closed, the first motor 26 is operated to operate the spur gear 27, the spur gear 27 is rotated to rotate the annular rack 28, the annular rack 28 is rotated to rotate the rotating disc 21, the rotating disc 21 is rotated to enable the water inlet groove 22 to communicate with the flow passage, the air inlet groove 24 is staggered with the cavity 20, the switching operation is carried out, the water pump is operated to convey water into the water inlet pipe 23, the water enters the cavity 20 through the water inlet pipe 23 and enters the connecting pipe 14 through the cavity 20, the inside of the first shell 6 and the inside of the second shell 11 are cleaned, the second motor 29 is operated to enable the connecting pipe 14 and the arc-shaped piece 16 to rotate, water flows, the first valve 32 on the drain pipe is opened to be discharged after the cleaning is finished, and the first electric heating piece 9 and the second electric heating piece 12 are operated to dry the inside of the first shell 6 and the second shell 11.
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art will be able to apply equally to the technical solution of the present invention and the inventive concept thereof, within the scope of the present invention.
Claims (10)
1. The synthesis process of trifluoroacetamide is characterized by comprising synthesis equipment, wherein the synthesis equipment comprises a machine case (1), a protection barrel (2) is fixedly installed at the top of the machine case (1), a mounting hole is formed in the top of the machine case (1), a reaction tank (3) is fixedly installed on the inner wall of the mounting hole, an end cover (4) is fixedly connected to the top of the reaction tank (3), a first shell (6) is fixedly connected to the inside of the reaction tank (3), a liquid inlet pipe (5) is fixedly communicated with the outer wall of the first shell (6), a vertical rod (7) is fixedly connected to the inner wall of the first shell (6), a plurality of spiral pieces (8) are fixedly sleeved on the outer wall of the vertical rod (7), a plurality of first electric heating pieces (9) are fixedly installed on the outer wall of the first shell (6), a plurality of liquid outlet holes (10) are uniformly formed in the outer wall of the first shell (6), a second shell (11) is fixedly installed on the inner wall of the reaction tank (3), a plurality of second shells (12) are fixedly connected to the outer wall of the second shell (11), a plurality of arc-shaped connecting pipes (14) are fixedly connected with the outer wall of the second shell (6), a plurality of arc-shaped connecting pipes (14) are fixedly connected with one another, the outer wall of connecting pipe (14) rotates the cover and is equipped with baffle (17), the outer wall of baffle (17) and the inner wall fixed connection of retort (3), the inside of machine case (1) is equipped with conversion mechanism, the fixed intercommunication of outer wall of second casing (11) has drain pipe (31) and blow off pipe, the inside of machine case (1) is equipped with rotary mechanism.
2. The process for synthesizing the trifluoroacetamide as claimed in claim 1, wherein the conversion mechanism comprises a disc (19), the outer wall of the reaction tank (3) is fixedly connected with the outer wall of the disc (19), a cavity (20) is formed in the outer wall of the disc (19), a runner is formed in the outer wall of the cavity (20), a rotating disc (21) is slidably connected with the outer wall of the disc (19), a water inlet groove (22) and a water inlet groove (24) are formed in the outer wall of the rotating disc (21), a water inlet pipe (23) and a water inlet pipe (25) are fixedly communicated with each other on the outer wall of the rotating disc (21), a water pump is fixedly communicated with one end of the water inlet pipe (23), a suction pump is fixedly communicated with one end of the water inlet pipe (23) and one end of the water inlet groove (22), and one end of the water inlet pipe (25) is communicated with the water inlet groove (24).
3. The process for synthesizing the trifluoroacetamide as recited in claim 2, wherein the rotating mechanism comprises a second motor (29), an equipment frame (30) is fixedly installed at the bottom of the reaction tank (3), a first motor (26) is fixedly connected to the inner wall of the equipment frame (30), a spur gear (27) is fixedly connected to the top of an output shaft of the first motor (26), the bottom of the connecting pipe (14) is fixedly connected with the outer wall of the disc (19), the outer wall of the connecting pipe (14) is communicated with the inner wall of the cavity (20), an annular rack (28) is fixedly sleeved on the outer wall of the rotating disc (21), the annular rack (28) is in meshed connection with the spur gear (27), and two arc-shaped grooves (36) are formed in the outer wall of the equipment frame (30).
4. The synthesis process of trifluoroacetamide as claimed in claim 1, wherein the outer wall of the reaction tank (3) is in contact with the inner wall of the protective cylinder (2), the outer wall of the reaction tank (3) is provided with a round hole, and the inner wall of the round hole is in sliding connection with the outer wall of the liquid inlet pipe (5).
5. The synthesis process of trifluoroacetamide as claimed in claim 1, wherein the outer wall of the second housing (11) is fixedly connected with a ring (13), and the outer wall of the ring (13) is fixedly connected with the inner wall of the reaction tank (3).
6. The process for synthesizing trifluoroacetamide as claimed in claim 1, wherein the outer wall of the arcuate piece (16) is in contact with the inner wall of the second housing (11), and the outer wall of the connecting tube (14) is fixedly provided with a one-way valve (18).
7. The synthesis process of trifluoroacetamide as claimed in claim 2, wherein the outer wall of the disc (19) is provided with an annular groove, the inner wall of the annular groove is rotatably connected with an annular block, and the outer wall of the annular block is fixedly connected with the outer wall of the rotating disc (21).
8. The synthesis process of trifluoroacetamide as claimed in claim 1, wherein the outer walls of the reaction tank (3) and the second shell (11) are provided with through holes, and the inner walls of the through holes are rotatably connected with the outer wall of the connecting pipe (14).
9. A process for synthesizing trifluoroacetamide as claimed in claim 3, wherein the outer wall of the rotary disc (21) is provided with a sliding hole, the inner wall of the sliding hole is fixedly connected with a bearing, and the inner ring of the bearing is fixedly connected with the outer wall of the output shaft of the second motor (29).
10. The synthesis process of the trifluoroacetamide as claimed in claim 1, wherein two assembly holes are respectively formed in the outer walls of the reaction tank (3) and the chassis (1), the inner walls of the assembly holes are fixedly connected with the outer walls of the liquid outlet pipe (31) and the drain pipe respectively, the first valves (32) are respectively fixedly arranged on the outer walls of the liquid outlet pipe (31), the liquid inlet pipe (5) and the drain pipe, the return pipes (33) are respectively fixedly arranged on the outer walls of the liquid outlet pipe (31) and the liquid inlet pipe (5), the second valves (34) are respectively fixedly arranged on the outer walls of the return pipes (33), the corrosion resisting pump (35) is fixedly arranged in the chassis (1), and the input end and the output end of the corrosion resisting pump (35) are respectively fixedly communicated with the outer walls of the two return pipes (33);
the synthesis process of the trifluoroacetamide comprises the following specific method steps:
s1, conveying ethyl trifluoroacetate to a first shell (6) through a pump, and carrying out preheating treatment on the ethyl trifluoroacetate in the first shell (6) by a first electric heating sheet (9), wherein the heating temperature is 30-35 ℃, so that subsequent reaction is facilitated, and the stroke of the ethyl trifluoroacetate is increased by a spiral blade (8), so that the ethyl trifluoroacetate is uniformly heated;
s2, ethyl trifluoroacetate enters a second shell (11), a second motor (29) operates to enable a connecting pipe (14) and an arc-shaped piece (16) to rotate, the arc-shaped piece (16) rotates to stir the ethyl trifluoroacetate, an air pump operates to enable ammonia gas to enter a cavity (20) and the connecting pipe (14) through a flow channel to perform neutralization reaction between the ammonia gas and the ethyl trifluoroacetate, and a second electric heating piece (12) operates to heat reaction liquid, wherein the heating temperature is 50-170 ℃;
s3, after 3-4 hours of reaction, the corrosion resistant pump (35) operates to convey the reaction liquid in the second shell (11) into the first shell (6), the first valve (32) is closed, the second valve (34) is opened, the reaction liquid enters from the upper return pipe (33) of the liquid outlet pipe (31), the reaction liquid is caused to flow back, and after 3-5 times of backflow, the subsequent reaction time is required to reach 7-8 hours;
s4, closing the first valve (32) and the second valve (34), and operating the first motor (26) to enable the water inlet tank (22) to be communicated with the flow passage, wherein the water inlet tank (24) is in error with the cavity (20), so as to perform switching operation;
s5, the water pump is operated to convey water into the cavity (20), the water enters the connecting pipe (14) through the cavity (20), the first shell (6) and the second shell (11) are cleaned, the second motor (29) is operated to enable the water to flow, the first valve (32) on the sewage draining pipe is opened to be discharged after the cleaning is finished, and the first electric heating sheet (9) and the second electric heating sheet (12) are operated to perform drying treatment.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310550570.7A CN116571181A (en) | 2023-05-16 | 2023-05-16 | Synthesis process of trifluoroacetamide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310550570.7A CN116571181A (en) | 2023-05-16 | 2023-05-16 | Synthesis process of trifluoroacetamide |
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| Publication Number | Publication Date |
|---|---|
| CN116571181A true CN116571181A (en) | 2023-08-11 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310550570.7A Pending CN116571181A (en) | 2023-05-16 | 2023-05-16 | Synthesis process of trifluoroacetamide |
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| Country | Link |
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| CN (1) | CN116571181A (en) |
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2023
- 2023-05-16 CN CN202310550570.7A patent/CN116571181A/en active Pending
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