CN116571197A - Efficient mixing equipment for hexafluoropropane preparation and preparation method - Google Patents
Efficient mixing equipment for hexafluoropropane preparation and preparation method Download PDFInfo
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- CN116571197A CN116571197A CN202310660866.4A CN202310660866A CN116571197A CN 116571197 A CN116571197 A CN 116571197A CN 202310660866 A CN202310660866 A CN 202310660866A CN 116571197 A CN116571197 A CN 116571197A
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- 238000002156 mixing Methods 0.000 title claims abstract description 78
- NSGXIBWMJZWTPY-UHFFFAOYSA-N 1,1,1,3,3,3-hexafluoropropane Chemical compound FC(F)(F)CC(F)(F)F NSGXIBWMJZWTPY-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 238000006243 chemical reaction Methods 0.000 claims description 74
- 239000007788 liquid Substances 0.000 claims description 69
- 238000003756 stirring Methods 0.000 claims description 63
- 239000002994 raw material Substances 0.000 claims description 52
- 239000013067 intermediate product Substances 0.000 claims description 33
- 238000010992 reflux Methods 0.000 claims description 30
- 238000010438 heat treatment Methods 0.000 claims description 14
- 238000001179 sorption measurement Methods 0.000 claims description 14
- 230000009467 reduction Effects 0.000 claims description 13
- VMPVEPPRYRXYNP-UHFFFAOYSA-I antimony(5+);pentachloride Chemical compound Cl[Sb](Cl)(Cl)(Cl)Cl VMPVEPPRYRXYNP-UHFFFAOYSA-I 0.000 claims description 11
- 238000007599 discharging Methods 0.000 claims description 11
- 238000004519 manufacturing process Methods 0.000 claims description 10
- 239000003054 catalyst Substances 0.000 claims description 8
- 241000446313 Lamella Species 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 4
- 239000012467 final product Substances 0.000 claims description 3
- 238000000034 method Methods 0.000 claims description 3
- 238000010517 secondary reaction Methods 0.000 claims description 3
- 238000003860 storage Methods 0.000 claims description 3
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- 239000007789 gas Substances 0.000 description 44
- 239000003795 chemical substances by application Substances 0.000 description 8
- 238000002485 combustion reaction Methods 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 229920004449 Halon® Polymers 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- PXBRQCKWGAHEHS-UHFFFAOYSA-N dichlorodifluoromethane Chemical compound FC(F)(Cl)Cl PXBRQCKWGAHEHS-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- BBEAZDGZMVABIC-UHFFFAOYSA-N 1,1,1,3,3,3-hexachloropropane Chemical compound ClC(Cl)(Cl)CC(Cl)(Cl)Cl BBEAZDGZMVABIC-UHFFFAOYSA-N 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 239000012459 cleaning agent Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000003682 fluorination reaction Methods 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 239000004088 foaming agent Substances 0.000 description 1
- -1 heat transfer media Substances 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 230000009965 odorless effect Effects 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 239000003380 propellant Substances 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 239000003507 refrigerant Substances 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 239000002341 toxic gas Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D5/00—Condensation of vapours; Recovering volatile solvents by condensation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
- B01F27/05—Stirrers
- B01F27/11—Stirrers characterised by the configuration of the stirrers
- B01F27/19—Stirrers with two or more mixing elements mounted in sequence on the same axis
- B01F27/192—Stirrers with two or more mixing elements mounted in sequence on the same axis with dissimilar elements
- B01F27/1921—Stirrers with two or more mixing elements mounted in sequence on the same axis with dissimilar elements comprising helical elements and paddles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
- B01F27/80—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis
- B01F27/90—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis with paddles or arms
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
- B01F27/80—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis
- B01F27/92—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis with helices or screws
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
- B01F35/30—Driving arrangements; Transmissions; Couplings; Brakes
- B01F35/32—Driving arrangements
- B01F35/32005—Type of drive
- B01F35/3204—Motor driven, i.e. by means of an electric or IC motor
-
- 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
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J4/00—Feed or outlet devices; Feed or outlet control devices
- B01J4/001—Feed or outlet devices as such, e.g. feeding tubes
- B01J4/002—Nozzle-type elements
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F2101/00—Mixing characterised by the nature of the mixed materials or by the application field
- B01F2101/2204—Mixing chemical components in generals in order to improve chemical treatment or reactions, independently from the specific application
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses efficient mixing equipment for preparing hexafluoropropane and a preparation method thereof, and relates to the technical field of organic synthesis.
Description
Technical Field
The invention relates to the technical field of organic synthesis, in particular to efficient mixing equipment for preparing hexafluoropropane and a preparation method thereof.
Background
1, 3-hexafluoropropane (abbreviated as C3H2F6 fa), colorless, odorless, low-toxic gas, cas690-39-1, molecular weight 152, boiling point-1.5 ℃, saturated vapor pressure 229.6kpa (20 ℃), 1, 3-hexafluoropropane is a very useful fluorine-containing organic compound and is widely used in the fields of cleaning agents, refrigerants, foaming agents, heat transfer media, propellants and the like. Meanwhile, because the boiling point and vapor pressure of the fire extinguishing agent are similar to those of a halon fire extinguishing agent, the fire extinguishing agent has the advantages of no corrosion, no electric conduction, no residue and the like, the fire extinguishing agent is also used as an ideal substitute of halon, and the hexafluoropropane fire extinguishing agent (C3H 2F 6) can extinguish class A, class B, class C and electric disasters, is suitable for a portable fire extinguisher, and is mainly used for extinguishing fire by inhibiting the chemical reaction process of combustion, so that the fire extinguishing agent can be decomposed to generate active free radicals when the fire extinguishing agent contacts flame or high-temperature surfaces, and the active substances (chain carriers) generated in the combustion chain reaction process are extracted, thereby interrupting the combustion chain reaction to achieve the aim of extinguishing fire.
The synthesis method of hexafluoropropane fire extinguishing agent is mainly liquid phase fluorination method, sbCI5 is used as catalyst, hexachloropropane and excessive liquid HF are mixed and reacted in a reaction tank after counting, and the mixing effect of each raw material is extremely important in the reaction process, because the problem that whether different reaction raw materials can fully contact and fully react is related to, the stirring structure of stirring equipment adopted by the existing reaction tank is too simple, the mixing effect is poor, and the problems of insufficient reaction, incomplete reaction and low product yield exist.
Disclosure of Invention
The invention aims to provide efficient mixing equipment for preparing hexafluoropropane and a preparation method thereof, so as to solve the problems in the background art.
In order to achieve the above purpose, the present invention provides the following technical solutions:
the utility model provides a hexafluoropropane preparation is with high-efficient mixing arrangement, includes frame, roof and mixing reaction tank and stirring subassembly, install the intermediate lamella in the middle of the frame, install the mixing reaction tank in the middle of the intermediate lamella, install the stirring subassembly on the mixing reaction tank, the roof is installed at the top of frame, install liquid conveying component on the roof, liquid conveying component bottom is connected with mixing reaction tank top, install gas conveying component on the intermediate lamella, gas conveying component is connected with mixing reaction tank top, intermediate product reflux subassembly is installed to mixing reaction tank bottom, intermediate product reflux subassembly is connected with liquid conveying component, mixing reaction tank upper portion one side is connected with the row material pipe, the row material pipe other end is connected with the adsorption tank.
As a further scheme of the invention: the stirring assembly comprises a spiral stirring shaft, a stirring rod, a reduction gear box and a stirring motor, wherein the stirring rod is arranged on the spiral stirring shaft, the top end of the spiral stirring shaft is directly connected with an output shaft of the reduction gear box arranged on the top plate, and an input shaft of the reduction gear box is directly connected with an output shaft of the stirring motor arranged on the top plate.
As still further aspects of the invention: the liquid conveying assembly comprises a liquid raw material tank, a first electromagnetic valve and a liquid flowmeter, wherein the liquid raw material tank is connected with the mixing reaction tank through a tank bottom discharging pipe, and the liquid flowmeter and the first electromagnetic valve are sequentially arranged on the tank bottom discharging pipe of the liquid raw material tank from top to bottom.
As still further aspects of the invention: the gas conveying assembly comprises a gas raw material tank, an air pump, a gas conveying pipe, a gas flowmeter and a high-pressure nozzle, wherein the gas conveying pipe is arranged on the gas raw material tank, the air pump is arranged on the gas conveying pipe, the other end of the gas conveying pipe is connected with the high-pressure nozzle arranged on the mixing reaction tank, the gas flowmeter is arranged on the gas conveying pipe, and the high-pressure nozzle is obliquely arranged towards the tank bottom discharge hole of the liquid raw material tank.
As still further aspects of the invention: the intermediate product reflux assembly comprises an intermediate product discharge pipe, a second electromagnetic valve, a dephlegmator, a reflux pipe and a reflux pump, wherein the intermediate product discharge pipe is arranged at the bottom outlet connection of the mixing reaction tank, the second electromagnetic valve is arranged on the intermediate product discharge pipe, the other end of the intermediate product discharge pipe is connected with the dephlegmator, the other end of the dephlegmator is connected with the reflux pipe, the reflux pump is arranged on the reflux pipe, and the other end of the reflux pipe is connected with a gas raw material tank.
As still further aspects of the invention: the external part of the mixing reaction tank is provided with a steam heating cavity, and the upper part and the lower part of the steam heating cavity are respectively provided with a steam inlet and a liquid outlet.
As still further aspects of the invention: the mixing reaction tank is provided with a temperature transmitter, the gas flowmeter and the liquid flowmeter are all electrically connected with a controller which is arranged on the frame, and the controller is electrically connected with the stirring motor, the reflux pump, the air pump, the first electromagnetic valve and the second electromagnetic valve respectively.
A mixing preparation method of high-efficiency mixing equipment for preparing hexafluoropropane comprises the following steps,
s1, respectively injecting C into a gas raw material tank and a liquid raw material tank 3 H 2 Cl 6 Mixed gas with SbCl5 and liquid HF;
s2, simultaneously opening a first electromagnetic valve and an air pump through a controller, enabling liquid HF gas to enter a mixing reaction tank from a liquid raw material tank, pumping mixed gas of CHCl and SbCl5 from the air pump, and injecting the mixed gas and the liquid HF gas into the mixing reaction tank through a gas conveying pipe and a high-pressure nozzle for premixing;
s3, starting a stirring motor, driving a spiral stirring shaft and a stirring rod to rotate through a reduction gearbox by the stirring motor to rapidly stir the mixed raw materials in the reaction, introducing steam into a steam heating cavity to control the heating temperature to be 70-110 ℃, taking SbCl5 as a catalyst to participate in the reaction of CHCl and excessive liquid HF, and generating C3H2F6 and HCl under the condition of fully stirring and mixing by mixing equipment;
s4, after the reaction is finished, a second electromagnetic valve is opened, so that excessive HF, partial intermediate products and a catalyst SbCl5 are discharged into a dephlegmator from an intermediate product discharge pipe to be condensed, and then are conveyed to a liquid raw material tank again through a reflux pump for secondary reaction;
s5, discharging a large amount of HCl and C3H2F6 generated by the reaction into the adsorption tank through a discharge pipe, absorbing the HCl by liquid water in the adsorption tank, and discharging the residual final product C3H2F6 into a designated storage container from the adsorption tank.
Compared with the prior art, the invention has the beneficial effects that:
1. according to the invention, by arranging the high-pressure nozzle, the gaseous raw material discharged by the high-pressure nozzle and the liquid raw material discharged by the liquid raw material tank can be mixed in the initial stage of entering the mixing reaction tank, so that the raw material premixing is realized, the mixing speed is higher, the mixing is more uniform, and the reaction is more thorough.
2. According to the invention, the stirring assembly is arranged, the spiral stirring shaft in the stirring assembly can convey the reaction raw materials in the middle area in the mixing reaction tank upwards in a spiral manner, so that the raw materials roll up and down, and the stirring assembly is matched with the stirring rod to stir horizontally, so that the liquid raw materials are fully contacted with the gaseous raw materials, and the reaction is more thorough.
3. According to the invention, the intermediate product reflux assembly is arranged, so that the intermediate product after reaction can be condensed and then conveyed into the raw material tank for re-reaction, and the purpose of saving raw materials can be achieved.
Drawings
Fig. 1 is an overall external view of a high-efficiency mixing apparatus for hexafluoropropane production.
Fig. 2 is a schematic diagram of the overall structure of a high-efficiency mixing device for hexafluoropropane production.
Fig. 3 is an enlarged view of the structure at a in fig. 2 of a high-efficiency mixing apparatus for hexafluoropropane production.
FIG. 4 is a block diagram showing the connection of a high-efficiency mixing apparatus for hexafluoropropane production
1. A frame; 2. a top plate; 3. an intermediate plate; 4. a mixing reaction tank; 5. a steam heating chamber; 6. a stirring assembly; 601. a spiral stirring shaft; 602. a stirring rod; 603. a reduction gear box; 604. a stirring motor; 7. a gas delivery assembly; 701. a gas feed tank; 702. an air pump; 703. a gas delivery tube; 704. a gas flow meter; 705. a high pressure nozzle; 8. a liquid delivery assembly; 801. a liquid raw material tank; 802. a first electromagnetic valve; 803. a liquid flow meter; 9. an intermediate reflux assembly; 901. an intermediate product discharge pipe; 902. a second electromagnetic valve; 903. a dephlegmator; 904. a return pipe; 905. a reflux pump; 10. an adsorption tank; 11. a controller; 12. a temperature transmitter; 13. and a discharge pipe.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Referring to fig. 1-2, in the embodiment of the invention, a high-efficiency mixing device for preparing hexafluoropropane comprises a frame 1, a top plate 2, a mixing reaction tank 4 and a stirring assembly 6, wherein a middle plate 3 is installed in the middle of the frame 1, the mixing reaction tank 4 is installed in the middle of the middle plate 3, the stirring assembly 6 is installed on the mixing reaction tank 4, the stirring assembly 6 comprises a spiral stirring shaft 601, a stirring rod 602, a reduction gearbox 603 and a stirring motor 604, the stirring rod 602 is installed on the spiral stirring shaft 601, the top end of the spiral stirring shaft 601 is directly connected with an output shaft of the reduction gearbox 603 installed on the top plate 2, an input shaft of the reduction gearbox 603 is directly connected with an output shaft of the stirring motor 604 installed on the top plate 2, the spiral stirring shaft 601 in the stirring assembly 6 can upwards convey reaction raw materials in a middle area in the mixing reaction tank 4 in a spiral manner, the raw materials can roll up and down, the stirring assembly is matched with the stirring rod 602 horizontally, so that the liquid raw materials are fully contacted with gaseous raw materials, and the reaction is more thoroughly reacted.
Referring to fig. 1-3, a top plate 2 is installed at the top of a rack 1, a liquid conveying component 8 is installed on the top plate 2, the liquid conveying component 8 comprises a liquid raw material tank 801, a first electromagnetic valve 802 and a liquid flowmeter 803, the liquid raw material tank 801 is connected with a mixing reaction tank 4 through a tank bottom discharging pipe, the liquid flowmeter 803 and the first electromagnetic valve 802 are sequentially installed on the tank bottom discharging pipe of the liquid raw material tank 801 from top to bottom, the bottom end of the liquid conveying component 8 is connected with the top of the mixing reaction tank 4, a gas conveying component 7 is installed on a middle plate 3, the gas conveying component 7 comprises a gas raw material tank 701, a gas pump 702, a gas conveying pipe 703, a gas flowmeter 704 and a high-pressure nozzle 705, a gas conveying pipe 703 is installed on the gas conveying pipe 703, the other end of the gas conveying pipe 703 is connected with the high-pressure nozzle 705 installed on the mixing reaction tank 4, and the high-pressure nozzle 705 is obliquely arranged towards the tank bottom discharging hole of the liquid raw material tank 801.
Referring to fig. 1-2, a gas delivery assembly 7 is connected to the top of a mixing reaction tank 4, an intermediate product reflux assembly 9 is installed at the bottom of the mixing reaction tank 4, the intermediate product reflux assembly 9 includes an intermediate product discharge pipe 901, a second electromagnetic valve 902, a dephlegmator 903, a reflux pipe 904 and a reflux pump 905, the intermediate product discharge pipe 901 is installed at the bottom outlet of the mixing reaction tank 4, the second electromagnetic valve 902 is installed on the intermediate product discharge pipe 901, the other end of the intermediate product discharge pipe 901 is connected with the dephlegmator 903, the other end of the dephlegmator 903 is connected with the reflux pipe 904, the reflux pump 905 is installed on the reflux pipe 904, the other end of the reflux pipe 904 is connected with a gas raw material tank 701, and the intermediate product reflux assembly 9 can convey the reacted intermediate product (excessive HF, partial intermediate product and catalyst SbCl 5) into the raw material tank again after condensation for re-reaction.
Referring to fig. 1-2, an intermediate product reflux assembly 9 is connected with a liquid delivery assembly 8, one side of the upper portion of the mixing reaction tank 4 is connected with a discharge pipe 13, the other end of the discharge pipe 13 is connected with an adsorption tank 10, and liquid water (HCl is easily dissolved in water, and C3H2F6 is not easily dissolved in water) in the adsorption tank 10 is removed from HCl in the mixed product.
Referring to fig. 4, a steam heating chamber 5 is installed outside the mixing reaction tank 4, steam inlets and liquid outlets are respectively formed in the upper portion and the lower portion of the steam heating chamber 5, the steam heating chamber 5 is connected with an external steam generator, the steam generator is electrically connected with a controller 11, a temperature transmitter 12 is installed on the mixing reaction tank 4, the temperature transmitter 12, a gas flowmeter 704 and a liquid flowmeter 803 are electrically connected with the controller 11 installed on the frame 1, the controller 11 is electrically connected with a stirring motor 604, a reflux pump 905, an air pump 702, a first electromagnetic valve 802 and a second electromagnetic valve 902 respectively, the electronic equipment is an existing mature product, various corresponding types are available on the market, a control circuit of the controller 11 can be realized through simple programming by a person skilled in the art, the invention is well known in the art, and the invention is mainly used for protecting mechanical devices, and the control mode and circuit connection are not explained in detail.
The method for preparing hexafluoropropane by mixing with high-efficiency mixing equipment comprises injecting C into gas raw material tank 701 and liquid raw material tank 801 respectively 3 H 2 Cl 6 Mixed gas with SbCl5 and liquid HF; simultaneously opening a first electromagnetic valve 802 and an air pump 702 through a controller 11, and introducing liquid HF gas into the mixing reaction tank 4 from a liquid raw material tank 801, C 3 H 2 Cl 6 The mixed gas of SbCl5 and the mixed gas is pumped by an air pump 702 and is sprayed out by a gas conveying pipe 703 and a high-pressure nozzle 705 to be premixed with liquid HF gas in a mixing reaction tank 4; then, starting a stirring motor 604, driving a spiral stirring shaft 601 and a stirring rod 602 to rotate by the stirring motor 604 through a reduction gear box 603 to rapidly stir the mixed raw materials in the reaction, introducing steam into a steam heating cavity 5 to control the heating temperature to be 70-110 ℃, taking SbCl5 as a catalyst to participate in the reaction of CHCl and excessive liquid HF, and generating C3H2F6 and HCl under the condition of fully stirring and mixing by mixing equipment; after the reaction is finished, a second electromagnetic valve 902 is opened, so that excessive HF, partial intermediate products and a catalyst SbCl5 are discharged into a dephlegmator 903 from an intermediate product discharge pipe 901 to be condensed, and then are conveyed to a liquid raw material tank 801 again through a reflux pump 905 for secondary reaction; a large amount of HCl generated by the reaction,The C3H2F6 is discharged into the adsorption tank 10 through the discharge pipe 13, HCl is absorbed by the liquid water in the adsorption tank 10, and the remaining final product C3H2F6 is discharged into a designated storage container from the adsorption tank 10.
Although the present invention has been described with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications may be made to the embodiments described, or equivalents may be substituted for elements thereof, and any modifications, equivalents, improvements and changes may be made without departing from the spirit and principles of the present invention.
Claims (8)
1. The utility model provides a hexafluoropropane preparation is with high-efficient mixing arrangement, includes frame (1), roof (2) and hybrid reaction jar (4) and stirring subassembly (6), its characterized in that: install intermediate lamella (3) in the middle of frame (1), install mixing reaction tank (4) in the middle of intermediate lamella (3), install stirring subassembly (6) on mixing reaction tank (4), roof (2) are installed at the top of frame (1), install liquid delivery module (8) on roof (2), liquid delivery module (8) bottom is connected with mixing reaction tank (4) top, install gas delivery module (7) on intermediate lamella (3), gas delivery module (7) are connected with mixing reaction tank (4) top, intermediate product backward flow subassembly (9) are installed to mixing reaction tank (4) bottom, intermediate product backward flow subassembly (9) are connected with liquid delivery module (8), mixing reaction tank (4) upper portion one side is connected with row material pipe (13), row material pipe (13) other end is connected with adsorption tank (10).
2. A high efficiency mixing apparatus for hexafluoropropane production as set forth in claim 1, wherein: stirring subassembly (6) are including spiral (601) stirring rod (602), reduction gear box (603) and agitator motor (604), install stirring rod (602) on spiral (601) stirring rod, spiral (601) top and the output shaft of installing reduction gear box (603) on roof (2) directly link, the input shaft of reduction gear box (603) and agitator motor (604) output shaft of installing on roof (2) directly link.
3. A high efficiency mixing apparatus for hexafluoropropane production as set forth in claim 1, wherein: the liquid conveying assembly (8) comprises a liquid raw material tank (801), a first electromagnetic valve (802) and a liquid flowmeter (803), wherein the liquid raw material tank (801) is connected with the mixing reaction tank (4) through a tank bottom discharging pipe, and the liquid flowmeter (803) and the first electromagnetic valve (802) are sequentially installed on the tank bottom discharging pipe of the liquid raw material tank (801) from top to bottom.
4. A high efficiency mixing apparatus for hexafluoropropane production as set forth in claim 1, wherein: the gas delivery assembly (7) comprises a gas raw material tank (701), an air pump (702), a gas delivery pipe (703), a gas flowmeter (704) and a high-pressure nozzle (705), wherein the gas delivery pipe (703) is arranged on the gas raw material tank (701), the air pump (702) is arranged on the gas delivery pipe (703), the other end of the gas delivery pipe (703) is connected with the high-pressure nozzle (705) arranged on the mixing reaction tank (4), the gas flowmeter (704) is arranged on the gas delivery pipe (703), and the high-pressure nozzle (705) is obliquely arranged towards a tank bottom discharge hole of the liquid raw material tank (801).
5. A high efficiency mixing apparatus for hexafluoropropane production as set forth in claim 1, wherein: intermediate product backward flow subassembly (9) include intermediate product discharge pipe (901), second solenoid valve (902), dephlegmator (903), back flow (904) and reflux pump (905), intermediate product discharge pipe (901) are installed in mixed retort (4) bottom exit linkage, install second solenoid valve (902) on intermediate product discharge pipe (901), intermediate product discharge pipe (901) other end is connected with dephlegmator (903), dephlegmator (903) other end is connected with back flow (904), install reflux pump (905) on back flow (904), back flow (904) other end is connected with gaseous head tank (701).
6. A high efficiency mixing apparatus for hexafluoropropane production as set forth in claim 1, wherein: the mixing reaction tank (4) is externally provided with a steam heating cavity (5), and the upper part and the lower part of the steam heating cavity (5) are respectively provided with a steam inlet and a liquid outlet.
7. A high efficiency mixing apparatus for hexafluoropropane production as set forth in claim 1, wherein: the mixing reaction tank (4) is provided with a temperature transmitter (12), the temperature transmitter (12), a gas flowmeter (704) and a liquid flowmeter (803) are electrically connected with a controller (11) arranged on the frame (1), and the controller (11) is electrically connected with a stirring motor (604), a reflux pump (905), an air pump (702), a first electromagnetic valve (802) and a second electromagnetic valve (902) respectively.
8. The mixing preparation method of the efficient mixing equipment for preparing hexafluoropropane according to any one of claims 1 to 7, characterized in that: the method comprises the steps of,
s1, C is respectively injected into a gas raw material tank (701) and a liquid raw material tank (801) 3 H 2 Cl 6 And SbCl 5 Mixed gas and liquid HF;
s2, simultaneously opening a first electromagnetic valve (802) and an air pump (702) through a controller (11), enabling liquid HF gas to enter a mixing reaction tank (4) from a liquid raw material tank (801), and C 3 H 2 Cl 6 The mixed gas of SbCl5 and the mixed gas is pumped out by an air pump (702) and is sprayed out by a gas conveying pipe (703) and a high-pressure nozzle (705) to be premixed with liquid HF gas in a mixing reaction tank (4);
s3, starting a stirring motor (604), driving a spiral stirring shaft (601) and a stirring rod (602) to rotate by the stirring motor (604) through a reduction gear box (603) to rapidly stir the mixed raw materials in the reaction, simultaneously introducing steam into a steam heating cavity (5) to control the heating temperature to be 70-110 ℃, taking SbCl5 as a catalyst to participate in the reaction of CHCl and excessive liquid HF, and generating C3H2F6 and HCl under the condition of fully stirring and mixing by mixing equipment;
s4, after the reaction is finished, a second electromagnetic valve (902) is opened, so that excessive HF, partial intermediate products and a catalyst SbCl5 are discharged into a dephlegmator (903) from an intermediate product discharge pipe (901) to be condensed, and then are conveyed to a liquid raw material tank (801) again through a reflux pump (905) for secondary reaction;
s5, discharging a large amount of HCl and C3H2F6 generated by the reaction into the adsorption tank (10) through a discharge pipe (13), absorbing the HCl by liquid water in the adsorption tank (10), and discharging the residual final product C3H2F6 into a designated storage container from the adsorption tank (10).
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| CN117844610A (en) * | 2023-12-31 | 2024-04-09 | 枣庄市杰诺生物酶有限公司 | Preparation device and method of high-purity aminobutyric acid |
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