CN114917859A - HF (Hydrogen fluoride) removing equipment for preparing vinylidene fluoride from trifluoroethane and preparation method of vinylidene fluoride - Google Patents

HF (Hydrogen fluoride) removing equipment for preparing vinylidene fluoride from trifluoroethane and preparation method of vinylidene fluoride Download PDF

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Publication number
CN114917859A
CN114917859A CN202210350886.7A CN202210350886A CN114917859A CN 114917859 A CN114917859 A CN 114917859A CN 202210350886 A CN202210350886 A CN 202210350886A CN 114917859 A CN114917859 A CN 114917859A
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frame
discharging
material taking
plate
side plate
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CN114917859B (en
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王晓东
李飞
林凯
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Zhejiang Sanmei Chemical Industry Co ltd
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Zhejiang Sanmei Chemical Industry Co ltd
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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
    • B01J19/24Stationary reactors without moving elements inside
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C17/00Preparation of halogenated hydrocarbons
    • C07C17/25Preparation of halogenated hydrocarbons by splitting-off hydrogen halides from halogenated hydrocarbons

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  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention discloses HF removing equipment for preparing vinylidene fluoride from trifluoroethane and a preparation method of the vinylidene fluoride, wherein the HF removing equipment comprises a treatment box and a replacement box, a reaction box is arranged in the treatment box, a material rack is arranged in the reaction box, and a material taking assembly and a material placing assembly are arranged in the replacement box; the preparation method comprises the following steps: 1) thermal cracking; 2) removing HF; 3) and (5) purifying. The method has simple and easily-operated process steps, obtains vinylidene fluoride by performing thermal cracking HF removal treatment on trifluoroethane, further processes the finally prepared product, effectively improves the actual product quality, adopts special HF removal equipment for treatment in the HF removal treatment, effectively ensures the actual treatment effect, adsorbs HF through sodium fluoride, regularly changes sodium fluoride particles, ensures the actual adsorption effect, adopts automatic change treatment in the sodium fluoride change process, does not need manual change, ensures more high efficiency and safety of the change operation, and reduces the potential safety hazard.

Description

HF (Hydrogen fluoride) removing equipment for preparing vinylidene fluoride from trifluoroethane and preparation method of vinylidene fluoride
Technical Field
The invention belongs to the technical field of vinylidene fluoride, and particularly relates to HF removing equipment for preparing vinylidene fluoride from trifluoroethane and a preparation method of the vinylidene fluoride.
Background
1, 1-difluoroethylene (also known as vinylidene fluoride or VDF) is one of the important varieties of fluoroolefins, and is mainly used for producing polyvinylidene fluoride resins, fluororubbers, and fluorine-containing copolymers such as vinylidene fluoride-hexafluoropropylene, vinylidene fluoride-vinylidene fluoride, vinylidene fluoride-tetrafluoroethylene-hexafluoropropylene, and the like. In addition, fluororubber obtained by copolymerizing vinylidene fluoride, hexafluoropropylene and tetrafluoroethylene becomes one of indispensable and alternative basic materials in modern industries, particularly in high-tech fields, due to excellent high temperature resistance, oil resistance, solvent resistance and physical and mechanical properties. In conclusion, the 1, 1-difluoroethylene has wide market application prospect, and great significance in the vigorous development of the 1, 1-difluoroethylene production technology.
Disclosure of Invention
The invention aims to provide HF removing equipment for preparing vinylidene fluoride from trifluoroethane and a technical scheme of a preparation method of the vinylidene fluoride, aiming at the defects in the prior art, the design is reasonable, the process steps are simple and easy to operate, the trifluoroethane is subjected to thermal cracking HF removing treatment to obtain the vinylidene fluoride, the finally prepared product is further treated, the actual product quality is effectively improved, the HF removing treatment is carried out by adopting special HF removing equipment, the actual treatment effect is effectively ensured, HF is adsorbed by sodium fluoride, and sodium fluoride particles are periodically replaced to ensure the actual adsorption effect, and automatic replacement treatment is adopted in the replacement process of the sodium fluoride without manual replacement, so that the replacement operation is more efficient and safer, and the potential safety hazard is reduced.
The raw material source is extensive, low in production cost, and is harmless, can effectively get rid of inorganic and organic impurity in the lithium hexafluorophosphate, make the lithium hexafluorophosphate product quality who obtains high, have good social value and economic value, easily promote and use, adopt the filter vat to filter treatment to the mixed liquid after the lithium hexafluorophosphate crude dissolves in the organic solvent, filtration efficiency is good, through the dual filtration of filter screen and ring filter, get rid of insoluble impurity, effectively ensure the filtrate quality after filtering, thereby improve ultimate product quality.
In order to solve the technical problems, the invention adopts the following technical scheme:
an HF removing device for preparing vinylidene fluoride from trifluoroethane is characterized in that: comprises a processing box and a replacing box, wherein a reaction box is arranged in the processing box, a material frame is arranged in the reaction box, the material frame comprises a fixed end plate and a material frame, the material frame is uniformly distributed on the fixed end plate, sodium fluoride particles are placed in the material frame, a material top cover is arranged on the top surface of the material frame, one side of the processing box is embedded in the replacing box, an opening is arranged on the side surface of the processing box embedded in the replacing box, a movable side plate is sealed and sheltered at the opening, the movable side plate is sealed and sheltered at the opening in the normal working process of the reaction box, so that the interval between the processing box and the replacing box is realized, the processing process of the processing box is not influenced, the movable side plate is fixedly connected with the fixed end plate, the movable side plate is connected with a pushing component, the movable side plate is driven to horizontally move in the replacing box by the pushing component, the movable side plate drives the material frame fixed with the movable side plate to move, thereby realizing the moving or pushing of the material frame in the reaction box, the material frame is convenient to replace, the material taking assembly and the material placing assembly are arranged in the replacing box and are connected on the mounting top plate, the mounting top plate is connected with the lifting cylinder, the lifting cylinder is fixed at the top of the replacing box, the mounting top plate is arranged in the replacing box in a crossing manner, and the two ends of the mounting top plate are just in butt fit with the side wall of the replacing box, so that the side wall of the mounting top plate attached to the replacing box moves up and down under the stretching of the lifting cylinder, thereby realizing the integral upward movement or descending of the material taking component and the material placing component, facilitating the material taking-out of the material frame by the material taking component or the material loading operation of the new material frame by the material placing component, having reasonable design, and effectively ensure the stationarity and the reliability of removal adjustment in-process, the change case is just all being provided with logical notch to the both sides face of getting material subassembly and blowing subassembly, and this logical notch department installs sealing door, the taking of the material frame of being convenient for.
The material taking assembly comprises a material taking cylinder and a material taking frame, the material taking cylinder is connected with the material taking frame, the material taking frame comprises a material taking side plate, a material taking support plate and a material taking end frame, the material taking side plate is connected with a piston rod of the material taking cylinder, the material taking side plate is slidably connected in a material taking chute for mounting the top plate, the material taking support plate is positioned on the material taking side plate, the material taking support plate and the material frame are in one-to-one correspondence, one end of the material taking support plate is fixedly connected with the material taking side plate, a material taking convex baffle plate is arranged at the other end of the material taking support plate, the material taking end frame comprises a material taking end plate and a material taking support rod, the material taking support rod is fixedly arranged on the material taking end plate, a material taking folding rod is arranged at one end of the material taking support rod, and the material taking folding rod is fixedly connected with the material taking side plate; the material taking cylinder can push the material taking frame to move so as to realize the supporting and lifting of the material taking frame by the material taking frame, thereby realizing the discharging and taking out of the material frame by matching the material taking frame with the material taking cylinder, thereby replacing sodium fluoride particles, ensuring the actual HF removing effect, supporting the material taking support plate at the bottom of the material frame, the material taking side plate is matched with the material taking baffle convex plate to ensure that the material frame is just limited and clamped between the material taking side plate and the material taking baffle convex plate, so that the stability and the reliability of the material taking and blanking process are ensured, the height of the material taking baffle convex plate is designed to be smaller than the nearest distance between two material frames which are adjacent up and down, the material taking support plate and the corresponding material taking baffle convex plate can integrally descend and move to the bottom of the corresponding material frame in actual operation, and then the material taking support plate and the corresponding material taking baffle convex plate can integrally ascend after being horizontally pushed and moved in place, so that the material frame can be accurately clamped and positioned on the material taking frame, and the safety in the actual material taking operation process is improved.
Further, the discharging component comprises a discharging cylinder and a discharging frame, the discharging cylinder is connected with the discharging frame, the discharging frame comprises a discharging side plate, a discharging support plate and a discharging end frame, the discharging side plate is connected with a piston rod of the discharging cylinder, the discharging side plate is connected in a discharging chute of the mounting top plate in a sliding manner, the discharging support plate is positioned on the discharging side plate, the discharging support plate and the material frame correspond one to one, one end of the discharging support plate is fixedly connected with the discharging side plate, the other end of the discharging support plate is provided with a discharging baffle convex plate, the discharging end frame comprises a discharging end plate and a discharging support rod, the discharging support rod is fixedly arranged on the discharging end plate, one end of the discharging support rod is provided with a discharging folding rod, the discharging folding rod is fixedly connected with the discharging side plate, the discharging cylinder can push the discharging frame to move, the discharging frame is used for placing a material frame with new sodium fluoride particles, and the feeding operation on the new material frame is realized through the cooperation of the discharging cylinder, realize the change of sodium fluoride granule, the blowing extension board supports in material frame bottom, and the material frame just in time joint is between blowing curb plate and blowing fender flange simultaneously, ensures the fail safe nature of material loading operation process, and the blowing keeps off the highly design of flange and is less than the nearest interval between two adjacent material frames from top to bottom for blowing extension board and the blowing fender flange that corresponds can wholly descend and move to the bottom that corresponds the material frame during actual operation, realize the material loading operation.
Furthermore, be provided with the clamping groove that inlays on the bottom surface of material frame, get material branch and blowing branch and all with the clamping groove phase-match that inlays, get material branch or blowing branch joint support in corresponding clamping groove that inlays, the design of clamping groove is more ingenious, and it is spacing to the material frame accurate joint of getting on material subassembly, the blowing subassembly to coordinate to get material branch and blowing branch realization, guarantees to get the stationarity and the security of material or the material frame movement accommodation process of material in-process.
Furthermore, the bottom of the reaction box is provided with a buffer cavity, the buffer cavity is internally divided into at least two partition cavities, the outer side of each partition cavity is communicated with a shunt conduit, the shunt conduit is provided with a flow control valve, the end part of the shunt conduit extends out of the processing box to be connected with the cache box, the cache box is provided with an air inlet pipe, the top end of the reaction box is provided with an air outlet pipe, the end part of the air outlet pipe extends out of the processing box to divide the buffer cavity into a plurality of partition cavities to realize the shunt of air, the impact force of the air on the material rack in the reaction box is reduced, the stability of the material rack is improved, meanwhile, the air enters the reaction box from the plurality of partition cavities, the air is diffused from multiple directions to enter the reaction box, the air is fully contacted with sodium fluoride in the material frame, the actual HF removing effect is effectively improved, and the noise of the whole equipment during working can be effectively reduced through the shunt, the design of the flow control valve can control and adjust the gas delivery flow on each flow dividing conduit, and the removal effect of the hydrogen fluoride is ensured.
Further, the promotion subassembly includes push motor, the promotion screw rod, direction sill bar and direction ejector pin, push motor is connected with the promotion screw rod, the bottom of removing the curb plate is provided with end extension board, end extension board cover is established on promotion screw rod and direction sill bar, the top of removing the curb plate is provided with top extension board, end extension board cover is established on the direction ejector pin, can drive through the promotion subassembly and remove curb plate horizontal migration, it drives fixed end plate of fixed connection with it and removes to remove the curb plate, thereby take the removal of animal material frame, realize taking out of material frame and change the operation, push motor drives the promotion screw rod and rotates, make the removal curb plate that is located on the promotion screw rod remove, it is spacing to remove the curb plate and receive the supplementary direction of direction sill bar and direction ejector pin simultaneously, make whole horizontal migration more steady reliable, improve actual operation stability and security.
Furthermore, through sockets are arranged on the side face of the reaction box opposite to the outlet, the through sockets are matched with the material frames in a one-to-one correspondence manner, the material frames are moved out or pushed into the reaction box through the through sockets, auxiliary frames are arranged in the reaction box, a group of auxiliary frames are correspondingly arranged at each through socket and comprise an upper pressure frame and a lower support frame, the bottom of the material frames in the reaction box is supported and lifted through the lower support frame, the material top cover on the top surface of the material frames is abutted and limited through the upper pressure frame, each material frame corresponds to one through socket, the material frames are moved out or pushed into the reaction box, meanwhile, each material frame inserted into the reaction box corresponds to one group of auxiliary frames, and the material frames inserted into the reaction box are supported in an auxiliary manner through the auxiliary frames, so that the structure of the whole material frame is more stable and reliable, the structural safety is improved, the upper pressure frames are limited and abutted against the top of the material top cover, the material top cover is prevented from being ejected out by gas impact, and the lower bracket is supported and lifted at the bottom of the material frame, so that the material frame is more stably placed.
Further, be provided with the bracket on the fixed end plate, bracket and material frame one-to-one, be provided with the slot on the bracket, be provided with the grafting section on the material frame, the grafting section matches and pegs graft in the slot, be provided with the extending groove on the fixed end plate, extending groove and slot one-to-one intercommunication, the tip of grafting section passes the slot and extends to peg graft in corresponding extending groove, the bracket realizes the grafting installation of material frame on the fixed end plate, realize accurate grafting between material frame and the bracket through grafting section cooperation slot, simultaneously through the design of the extending groove on the fixed end plate, every extending groove corresponds a slot, it is more firm reliable to make the grafting installation of material frame through the auxiliary design of extending groove, structural stability and security improve.
The preparation method of the vinylidene fluoride of the HF removing equipment for preparing the vinylidene fluoride based on trifluoroethane comprises the following steps:
(1) thermal cracking: introducing trifluoroethane gas into a platinized iron-nickel alloy tube, heating to 1100-1500 ℃, reacting for 0.01s at normal pressure and airspeed of 9700h -1
(2) Removing HF:
a. directly introducing the product obtained by the reaction in the step (1) into HF removing equipment, introducing gas into a cache box from a gas inlet pipe, then introducing the gas into a corresponding partition cavity through a shunt pipe, and then introducing the gas into the reaction box from the partition cavity; through the buffer treatment of the buffer cavity at the bottom of the reaction box, the gas entering the reaction box is divided by the plurality of partition cavities and enters the reaction box, so that the impact of the gas on a material frame is reduced, the gas enters the reaction box in a dispersed manner from the plurality of partition cavities, the full contact of the gas and sodium fluoride particles is ensured, the actual treatment effect is improved, and the actual treatment noise is reduced;
b. after gas enters the reaction box, the gas enters the material frame from the through hole at the bottom surface of the bottommost material frame in the reaction box, contacts with sodium fluoride particles placed in the material frame, flows out from the through hole on the material top cover at the top surface of the material frame, continues to flow upwards, sequentially contacts with sodium fluoride particles in other material frames until the gas flows out from the through hole on the material top cover at the top material frame, and is discharged from the gas outlet pipe, wherein the sodium fluoride particles placed in the material frame are 2-10nm, the reaction temperature in the reaction box is 20-80 ℃, and the reaction pressure is 0.12-0.18 MPa; the method has the advantages that the actual quality of the sodium fluoride particles is improved by controlling the particle size of the sodium fluoride particles, so that the adsorption effect of the sodium fluoride on HF is better, the actual treatment quality is improved, the adsorption effect of the sodium fluoride is further improved by controlling the reaction temperature and pressure, the HF removal effect is better, and the gas is subjected to multi-layer adsorption treatment by the design of a plurality of material frames, so that the actual treatment quality is effectively improved, and the quality of the finally obtained product is improved;
c. positioning and replacing sodium fluoride particles in the material frame; the sodium fluoride in the material frame is replaced regularly, so that the adsorption effect of the sodium fluoride is ensured, HF is removed more thoroughly and efficiently, and the quality of a final product is improved effectively;
(3) collecting the product obtained after the HF removal treatment in the step (2) into a liquid nitrogen tank, separating vinylidene fluoride in the product through low-temperature evaporation, and filtering, washing and drying to obtain a final product; the quality of the final product is effectively ensured through the treatments of low-temperature evaporation, filtration, washing and drying.
Further, in step c of step (2), the operation steps of replacing the sodium fluoride particles are as follows:
a. opening a sealing door on the side face of the replacement box, which is close to the material placing assembly, placing a material frame filled with new sodium fluoride particles on the material placing frame, wherein the material frame is just clamped between a material placing side plate and a material placing baffle plate, meanwhile, a clamping groove at the bottom of the material frame just corresponds to a material placing support rod, the material placing support rod is clamped into the clamping groove, and then the sealing door is closed;
b. the pushing assembly is started, the pushing motor drives the pushing screw to rotate, so that the movable side plate moves towards the interior of the replacement box along the pushing screw, the upper side and the lower side of the movable side plate are respectively guided by the guide ejector rod and the guide bottom rod in a limiting manner, the movable side plate drives the fixed end plate fixed with the movable side plate to move when moving, the fixed end plate further drives the animal material frame to move from the reverse box towards the interior of the replacement box until the movable side plate moves in place, and the material frame is completely moved out from the corresponding penetrating socket of the reaction box;
c. the material taking assembly moves, the material taking cylinder pushes the material taking frame to move towards the direction of the material frame moved out of the reaction box until the material taking frame moves in place, the material taking support plate moves to the position below the corresponding material frame, the lifting cylinder is started to drive the material taking assembly and the material placing assembly to integrally move upwards, so that the material taking support plate is movably supported below the corresponding material frame, meanwhile, the material frame is just limited between the material taking side plate and the material taking baffle convex plate, and meanwhile, the material taking support rod is just movably clamped in the clamping groove at the bottom of the material frame;
d. the pushing motor is started to drive the pushing screw to rotate, so that the moving side plate continues to move in the direction away from the reaction box until the moving side plate moves in place, the inserting section at the end part of the material frame is completely separated from the bracket, and the material taking cylinder is restarted to drive the material taking frame to move and reset;
e. the discharging assembly is started, the discharging air cylinder pushes the material frame, on which new sodium fluoride particles are placed, on the discharging frame to move towards the moving side plate until the material frame is moved in place, and the pushing motor is started to drive the pushing screw to rotate, so that the moving side plate moves towards the direction close to the reaction box until the insertion section at the end part of the material frame on the discharging frame is completely inserted into the insertion slot of the bracket;
f. the lifting cylinder is started to drive the material taking assembly and the material placing assembly to integrally move downwards until the material placing assembly moves downwards to the proper position, so that the material placing support rod is completely separated from the clamping groove corresponding to the material frame, meanwhile, the material placing support plate and the material placing baffle convex plate also move to the position below the corresponding material frame, and the material placing cylinder is started to drive the material placing frame to move and reset;
g. the pushing motor is started to drive the pushing screw to rotate, so that the moving side plate moves towards the reaction box, the moving side plate drives the material frame in which new sodium fluoride particles are placed to synchronously move towards the reaction box until the material frame completely moves into the reaction box through the corresponding penetrating socket, meanwhile, the fixed end plate is abutted against the side face of the reaction box to shield the penetrating socket, and the moving side plate shields and seals an opening on the side face of the treatment box;
h. and opening the side surface of the replacement box close to a sealing door of the material taking assembly, removing the material frame on the material taking frame, performing concentrated regeneration treatment on the sodium fluoride in the material frame, and recycling the sodium fluoride after the regeneration treatment.
Due to the adoption of the technical scheme, the invention has the following beneficial effects:
the method has reasonable design and simple and easily-operated process steps, the trifluoroethane is subjected to thermal cracking HF removal treatment to obtain the vinylidene fluoride, the finally prepared product is further treated, the actual product quality is effectively improved, the HF removal treatment is carried out by adopting special HF removal equipment, the actual treatment effect is effectively ensured, HF is adsorbed by the sodium fluoride, the sodium fluoride particles are periodically replaced, the actual adsorption effect is ensured, automatic replacement treatment is adopted in the replacement process of the sodium fluoride, manual replacement is not needed, the replacement operation is more efficient and safer, and the potential safety hazard is reduced.
In the invention, HF removing treatment is carried out by adopting HF removing equipment, a product obtained by thermal cracking is directly introduced into a reaction box, enters a buffer cavity from an air inlet pipe at the bottom of the reaction box, enters the reaction box after being shunted, and flows upwards from bottom to top, and gradually passes through a plurality of material frames to be contacted with sodium fluoride in the material frames, HF is effectively removed by the adsorption of the sodium fluoride, and finally is discharged from an air outlet pipe above the reaction box, the design is ingenious and reasonable, and sodium fluoride particles in the material frames are replaced after the HF removing equipment is used for a period of time, so that the actual adsorption effect is ensured, the whole replacement process is operated in an inner cavity of a replacement box, the material frames in the reaction box are pulled into the replacement box by a pushing component during replacement, the material frames are taken away by a material taking component, so that the material frames are separated from a material rack, and new material frames are placed on the material rack by a material placing component, place in this new material frame be new sodium fluoride, the rethread promotes the whole propelling movement of the material frame that the subassembly will be changed to the reaction box in, whole change operation is automatic, need not artificial pull to the material frame, avoid the injury that artificial change process high temperature caused, and also avoid the injury that gas leakage caused to the human body, place new material frame at the blowing frame earlier before the change again, manage good sealing door again, change the operation after that, after the change, just can take out old material frame after the certain time again, and regenerate the sodium fluoride granule in the material frame of taking out, realize the circulation of resource and recycle, effectively practice thrift the cost.
Drawings
The invention will be further described with reference to the accompanying drawings in which:
FIG. 1 is a schematic structural diagram of a HF removing apparatus for preparing vinylidene fluoride from trifluoroethane according to the present invention;
FIG. 2 is a schematic structural view of the movable side plate of the present invention in a state of covering the opening;
FIG. 3 is a schematic view showing a positional distribution of the top mounting plate in the replacement box according to the present invention;
FIG. 4 is a schematic view of a mounting structure of a material taking cylinder and a material placing cylinder on a top plate;
FIG. 5 is a schematic view of a distribution structure of the positions of the material taking assembly and the material placing assembly on the installation top plate;
FIG. 6 is a schematic diagram of the distribution structure of the material frames in the reaction chamber according to the present invention;
FIG. 7 is a structural view showing a state where the material frame is taken out from the reaction chamber in the present invention;
FIG. 8 is a schematic structural view of the material extracting assembly of the present invention in a state of being moved to a proper position relative to the material frame;
FIG. 9 is a schematic view of the material frame and the bracket of the present invention in a separated state;
FIG. 10 is a schematic structural view of the discharging assembly of the present invention moving and loading a new material frame;
FIG. 11 is a schematic view of a take-off assembly of the present invention;
FIG. 12 is a schematic view of the installation structure between the material frame and the bracket of the present invention;
FIG. 13 is a schematic view of the structure of the material frame of the present invention;
FIG. 14 is a schematic view showing the arrangement of the extension grooves on the fixed end plate according to the present invention;
fig. 15 is a schematic view of the distribution structure of the positions between the through-holes and the openings in the present invention.
In the figure: 1-a treatment box; 2, replacing the box; 3-a reaction box; 4-material shelf; 5-fixing the end plate; 6-material frame; 7-material top cover; 8-opening; 9-moving the side plate; 10-a pushing assembly; 11-a take-off assembly; 12-a discharge assembly; 13-installing a top plate; 14-a lifting cylinder; 15-material taking cylinder; 16-a material taking frame; 17-material taking side plate; 18-taking a material supporting plate; 19-a material taking end frame; 20-material taking baffle convex plate; 21-material taking end plate; 22-a take out support bar; 23-material taking folding rod; 24-a discharging cylinder; 25-a discharging frame; 26-discharging side plates; 27-a discharging support plate; 28-discharge end frame; 29-a discharge chute; 30-a material taking chute; 31-a discharging convex baffle; 32-discharge end plate; 33-a discharging support rod; 34-discharging folding rod; 35-clamping groove; 36-a partition cavity; 37-a shunt conduit; 38-cache box; 39-air inlet pipe; 40-an air outlet pipe; 41-a flow control valve; 42-a pushing motor; 43-pushing the screw; 44-a guide bottom bar; 45-guiding ejector rods; 46-a bottom extension plate; 47-a top extension panel; 49-through socket; 50-pressing the frame; 51-a push-down frame; 52-a carrier; 53-slot; 54-a plug section; 55-an extension slot; 56-mounting notch.
Detailed Description
As shown in figures 1 to 15, for the HF removing equipment for preparing the vinylidene fluoride from the trifluoroethane, the HF removing equipment comprises a treatment box 1 and a replacement box 2, a reaction box 3 is arranged in the treatment box 1, a material frame 4 is arranged in the reaction box 3, the material frame 4 comprises a fixed end plate 5 and a material frame 6, the material frame 6 is uniformly distributed on the fixed end plate 5, sodium fluoride particles are placed in the material frame 6, a material top cover 7 is arranged on the top surface of the material frame 6, one side of the treatment box 1 is embedded in the replacement box 2, an opening 8 is arranged on the side surface of the treatment box 1 embedded in the replacement box 2, a movable side plate 9 is sealed and shielded at the opening 8, the movable side plate 9 is sealed and shielded at the position of the opening 8 in the normal working process of the reaction box 3, so that the interval between the treatment box 1 and the replacement box 2 can not influence the treatment process of the treatment box 1, and the movable side plate 9 is fixedly connected with the fixed end plate 5, the movable side plate 9 is connected with the pushing assembly 10, the movable side plate 9 is driven by the pushing assembly 10 to horizontally move in the replacing box 2, the movable side plate 9 drives the material frame 4 fixed with the movable side plate to move, so that the material frame 6 is moved out or pushed into the reaction box 3, the material frame 6 is convenient to replace, a material taking assembly 11 and a material discharging assembly 12 are arranged in the replacing box 2, the material taking assembly 11 and the material discharging assembly 12 are connected onto a mounting top plate 13, the mounting top plate 13 is connected with a lifting cylinder 14, the lifting cylinder 14 is fixed at the top of the replacing box 2, the mounting top plate 13 is arranged in the replacing box 2 in a crossing mode, two ends of the mounting top plate 13 are just in abutting fit with the side wall of the replacing box 2, the side wall of the mounting top plate 13 attached to the replacing box 2 moves up and down under the stretching of the lifting cylinder 14, and the whole material taking assembly 11 and the material discharging assembly 12 moves up or down, the material taking component 11 is convenient to take out the material frame 6 or the material feeding component 12 is convenient to feed the new material frame 6, the design is reasonable, and the stability and the reliability in the moving and adjusting process are effectively ensured.
The material taking assembly 11 comprises a material taking cylinder 15 and a material taking frame 16, the material taking cylinder 15 is connected with the material taking frame 16, the material taking frame 16 comprises a material taking side plate 17, the material taking support plate 18 and the material taking end frame 19 are arranged, the material taking side plate 17 is connected with a piston rod of the material taking cylinder 15, the material taking side plate 17 is connected in a material taking chute 30 of the mounting top plate 13 in a sliding mode, the material taking chute 30 is designed to enable the movement adjustment of the material taking frame 16 to be more stable and reliable, the material taking support plate 18 is located on the material taking side plate 17, the material taking support plate 18 corresponds to the material frames 6 one by one, one end of the material taking support plate 18 is fixedly connected with the material taking side plate 17, the other end of the material taking support plate 18 is provided with a material taking convex plate 20, the material taking end frame 19 comprises a material taking end plate 21 and a material taking support rod 22, the material taking support rod 22 is fixedly arranged on the material taking end plate 21, one end of the material taking support rod 22 is provided with a material taking folding rod 23, and the material taking folding rod 23 is fixedly connected with the material taking side plate 17; the material taking cylinder 15 can push the material taking frame 16 to move, so that the material taking frame 16 can support and lift the material frame 6, the material taking frame 16 is matched with the material taking cylinder 15 to realize the material taking of the material frame 6, sodium fluoride particles are replaced, the actual HF removing effect is ensured, the material taking support plate 18 is supported at the bottom of the material frame 6, the material taking side plate 17 is matched with the material taking convex baffle plate 20 to ensure that the material frame 6 is just limited and clamped between the material taking side plate and the material taking convex baffle plate, the stable reliability of the material taking and material discharging process is ensured, the height of the material taking convex baffle plate 20 is designed to be smaller than the nearest distance between two adjacent material frames 6, the material taking support plate 18 and the corresponding material taking convex baffle plate 20 can integrally descend to move to the bottom of the corresponding material frame 6 during the actual operation, and the material taking frame 6 can be accurately clamped and positioned on the material taking frame 16 through the integral ascending after the material taking frame is pushed and moved to the right position by water level, the safety in the actual material taking operation process is improved.
The discharging component 12 comprises a discharging cylinder 24 and a discharging frame 25, the discharging cylinder 24 is connected with the discharging frame 25, the discharging frame 25 comprises a discharging side plate 26, a discharging support plate 27 and a discharging end frame 28, the discharging side plate 26 is connected with a piston rod of the discharging cylinder 24, the discharging side plate 26 is connected in a discharging chute 29 of the mounting top plate 13 in a sliding manner, the discharging chute 29 is designed to enable the discharging frame 25 to move and adjust more stably and reliably, the stability of the whole structure is improved, the discharging support plate 27 is positioned on the discharging side plate 17, the discharging support plate 27 corresponds to the material frame 6 one by one, one end of the discharging support plate 27 is fixedly connected with the discharging side plate 17, the other end of the discharging support plate 27 is provided with a discharging convex baffle plate 31, the discharging end frame 28 comprises a discharging end plate 32 and a discharging support rod 33, the discharging support rod 33 is fixedly arranged on the discharging end plate 32, one end of the discharging support rod 33 is provided with a discharging folding rod 34, and the discharging folding rod 34 is fixedly connected with the discharging side plate 26, blowing cylinder 24 can promote the removal of blowing frame 25, be used for placing the material frame 6 of putting new sodium fluoride granule on the blowing frame 25, realize the material loading operation to new material frame 6 through blowing cylinder 24 cooperation blowing frame 25, realize the change of sodium fluoride granule, blowing extension board 27 supports in the material frame 6 bottom, material frame 6 just in time joint is between blowing curb plate 26 and blowing fender flange 31, ensure the fail safe nature of material loading operation process, and blowing fender flange 31 highly designs to be less than the nearest interval between two adjacent material frames 6 from top to bottom, make blowing extension board 27 and the blowing fender flange 31 that corresponds can wholly descend and move to the bottom that corresponds material frame 6 during actual operation, realize the material loading operation.
Be provided with clamping groove 35 on the bottom surface of material frame 6, it all matches with clamping groove 35 to get material branch 22 and blowing branch 33, it supports in corresponding clamping groove 35 to get material branch 22 or the joint of blowing branch 33, clamping groove 35's design is more ingenious, it realizes getting material subassembly 11, accurate joint is spacing on the blowing subassembly 12 to material frame 6 to coordinate to get material branch 22 and blowing branch 33, guarantee to get the stationarity and the security of getting material or the in-process material frame 6 removal accommodation process of blowing.
The bottom of the reaction box 3 is provided with a buffer cavity, the buffer cavity is internally divided into at least two partition cavities 36, the outer side of each partition cavity 36 is communicated with a shunt guide pipe 37, the shunt guide pipe 37 is provided with a flow control valve 41, the end part of the shunt guide pipe 37 extends out of the treatment box 1 to be connected with a buffer box 38, the buffer box 38 is provided with an air inlet pipe 39, the top end of the reaction box 3 is provided with an air outlet pipe 40, the end part of the air outlet pipe 40 extends out of the treatment box 1 to divide the buffer cavity into a plurality of partition cavities 36 to realize the shunting of the gas, the impact force of the gas on a material rack 4 in the reaction box 3 is reduced, the stability of the material rack 4 is improved, meanwhile, the gas enters the reaction box 3 from the plurality of partition cavities 36, the gas diffuses into the reaction box 3 from multiple directions to ensure that the gas fully contacts with sodium fluoride in the material frame 6, the actual HF removing effect is effectively improved, and the noise of the whole equipment during operation can be effectively reduced through the shunting, and the design of the flow control valve 41 can control and adjust the gas delivery flow on each shunting conduit 37, thereby ensuring the removal effect of the hydrogen fluoride.
The pushing assembly 10 comprises a pushing motor 42, a pushing screw rod 43, a guiding bottom rod 44 and a guiding ejector rod 45, the pushing motor 42 is connected with the pushing screw rod 43, the bottom of the movable side plate 9 is provided with a bottom extension plate 46, the bottom extension plate 46 is sleeved on the pushing screw rod 43 and the guiding bottom rod 44, the top of the movable side plate 9 is provided with a top extension plate 47, the bottom extension plate 46 is sleeved on the guiding ejector rod 45, the pushing assembly 10 can drive the movable side plate 9 to move horizontally, the movable side plate 9 drives a fixed end plate 5 fixedly connected with the movable side plate 9 to move, so that the material frame 6 with animals moves, the material frame 6 is taken out and replaced, the pushing motor 42 drives the pushing screw rod 43 to rotate, the movable side plate 9 on the pushing screw rod 43 moves, meanwhile, the movable side plate 9 is limited by the guiding bottom rod 44 and the guiding ejector rod 45, so that the whole horizontal movement is more stable and reliable, improve the stability and safety of actual operation.
The side face of the reaction box 3 opposite to the outlet is provided with a through socket 49, the through sockets 49 are matched with the material frames 6 in a one-to-one correspondence manner, the material frames 6 are moved out or pushed into the reaction box 3 through the through sockets 49, an auxiliary frame is arranged in the reaction box 3, a group of auxiliary frames are correspondingly arranged at each through socket 49 and comprise an upper pressure frame 50 and a lower support frame 51, the bottom of the material frame 6 in the reaction box 3 is supported and lifted through the lower support frame 51, a material top cover 7 on the top surface of the material frame 6 is abutted and limited through the upper pressure frame 50, each material frame 6 corresponds to one through socket 49, the material frame 6 is moved out or pushed into the reaction box 3, each material frame 6 inserted into the reaction box 3 corresponds to one group of auxiliary frames, the auxiliary frames are used for supporting the material frames 6 inserted into the reaction box 3, and the structure of the whole material frame 4 is more stable and reliable, improve structural security, go up the top of pressing the frame 50 spacing conflict at material top cap 7, avoid gas impact to make material top cap 7 ejecting, and the bottom bracket supports lifts in the bottom of material frame 6 for placing of material frame 6 is more firm.
Be provided with bracket 52 on the fixed end plate 5, bracket 52 and material frame 6 one-to-one, be provided with slot 53 on the bracket 52, be provided with grafting section 54 on the material frame 4, grafting section 54 matches and pegs graft in slot 53, be provided with extending groove 55 on the fixed end plate 5, extending groove 55 and slot 53 one-to-one intercommunication, the tip of grafting section 54 passes slot 53 and extends and pegs graft in corresponding extending groove 55, bracket 52 realizes the grafting installation of material frame 6 on fixed end plate 5, cooperate the accurate grafting between material frame 6 and the bracket 52 through grafting section 54, simultaneously through the design of extending groove 55 on the fixed end plate 5, every extending groove 55 corresponds a slot 53, make the grafting installation of material frame 6 more firm reliable through the auxiliary design of extending groove 55, improve structural stability and security.
The preparation method of the vinylidene fluoride of the HF removing equipment for preparing the vinylidene fluoride based on trifluoroethane comprises the following steps:
(1) thermal cracking: introducing trifluoroethane gas into a platinized iron-nickel alloy tube, heating to 1100-1500 ℃, reacting for 0.01s at normal pressure and airspeed of 9700h -1
(2) Removing HF:
a. directly introducing a product obtained by the reaction in the step (1) into HF removing equipment, introducing gas into a cache box 38 from a gas inlet pipe 39, then introducing the gas into a corresponding partition cavity 36 through a shunt conduit 37, and then introducing the gas into the reaction box 3 from the partition cavity 36; through the buffer treatment of the buffer cavity at the bottom of the reaction box 3, the gas entering the reaction box 3 is divided into a plurality of partition cavities 36 and enters the reaction box 3, so that the impact of the gas on the material rack 4 is reduced, and the gas is dispersed and enters from the plurality of partition cavities 36, so that the full contact between the gas and sodium fluoride particles is ensured, the actual treatment effect is improved, and the actual treatment noise is reduced;
b. after entering the reaction box 3, the gas enters the material frame 6 from the through hole at the bottom surface of the bottommost material frame 6 in the reaction box 3, contacts with sodium fluoride particles arranged in the material frame 6, flows out from the through hole on the material top cover 7 at the top surface of the material frame 6, continues to flow upwards, sequentially contacts with the sodium fluoride particles in other material frames 6 until the gas flows out from the through hole on the material top cover 7 of the topmost material frame 6, and is discharged from the gas outlet pipe 40, the sodium fluoride particles arranged in the material frame 6 are 2-10nm, the reaction temperature in the reaction box 3 is 20-80 ℃, and the reaction pressure is 0.12-0.18 MPa; the particle size of the sodium fluoride particles is controlled, the actual quality of the sodium fluoride particles is improved, the adsorption effect of the sodium fluoride on HF is better, the actual treatment quality is improved, the adsorption effect of the sodium fluoride is further improved by controlling the reaction temperature and pressure, the HF removal effect is better, and the gas is subjected to multi-layer adsorption treatment by the design of the material frames 6, so that the actual treatment quality is effectively improved, and the quality of the finally obtained product is improved;
c. positioning and replacing sodium fluoride particles in the material frame 6; the sodium fluoride in the material frame 6 is replaced regularly, so that the adsorption effect of the sodium fluoride is ensured, HF is removed more thoroughly and efficiently, and the quality of a final product is effectively improved;
the operation steps for replacing the sodium fluoride particles are as follows:
a. opening a sealing door on the side surface of the replacement box 2 close to the discharging component 12, then placing a material frame 6 filled with new sodium fluoride particles on the discharging frame 25, wherein the material frame 6 is just clamped between the discharging side plate 26 and the discharging baffle convex plate 31, meanwhile, a clamping groove 35 at the bottom of the material frame 6 just corresponds to the discharging support rod 33, the discharging support rod 33 is clamped into the clamping groove 35, and then closing the sealing door; before replacement operation, a new material frame 6 is placed on the material placing frame 25 in advance, so that subsequent operation is facilitated, the placing stability of the material frame 6 on the material placing frame 25 is effectively ensured through matched clamping of the material placing side plates 26 and the material placing baffle convex plates 31 and supporting clamping of the material placing support rods 33, the sealing door is closed after placing, potential safety hazards in the replacement process are avoided, and the operation safety performance is improved;
b. the pushing assembly 10 is started, the pushing motor 42 drives the pushing screw rod 43 to rotate, the movable side plate 9 moves towards the inside of the replacement box 2 along the pushing screw rod 43, the upper side and the lower side of the movable side plate 9 are respectively limited and guided by the guide top rod 45 and the guide bottom rod 44, the movable side plate 9 drives the fixed end plate 5 fixed with the movable side plate to move when moving, the fixed end plate 5 drives the material frame 6 to move from the reverse box to the cavity of the replacement box 2 until the movable side plate 9 moves in place, and the material frame 6 is completely moved out from the corresponding penetrating socket 49 of the reaction box 3; the material frame 6 in the reaction box 3 is integrally pulled out through the pushing assembly 10, so that the material frame 6 can be conveniently taken out by the taking assembly 11, and in the pulling-out process of the material frame 6, the whole pulling-out process is more stable and reliable through multiple guiding limit of the pushing screw 43, the guiding ejector rod 45 and the guiding bottom rod 44;
c. the material taking assembly 11 moves, the material taking cylinder 15 pushes the material taking frame 16 to move towards the material frame 6 moved out of the reaction box 3 until the material taking frame 16 moves in place, the material taking support plate 18 moves to the position below the corresponding material frame 6, the lifting cylinder 14 is started to drive the material taking assembly 11 and the material placing assembly 12 to integrally move upwards, so that the material taking support plate 18 is movably supported below the corresponding material frame 6, meanwhile, the material frame 6 is just limited between the material taking side plate 17 and the material taking baffle convex plate 20, and meanwhile, the material taking support rod 22 is just movably clamped in the embedding clamping groove 35 at the bottom of the material frame 6; after the material frame 6 is completely moved into the replacement box 2, the material taking assembly 11 is matched with the lifting cylinder 14 to move the material taking frame 16 and the material frame 4 in place, so that the clamping, supporting and lifting of the material taking frame 16 on the material frame 6 are ensured;
d. the pushing motor 42 is started to drive the pushing screw 43 to rotate, so that the moving side plate 9 continues to move in the direction away from the reaction box 3 until the moving side plate 9 moves in place, the insertion section 54 at the end part of the material frame 6 is completely separated from the bracket 52, and the material taking cylinder 15 is restarted to drive the material taking frame 16 to move and reset; the material frame 6 is completely separated from the bracket 52 through the pushing assembly 10, and the material frame 6 is removed through the material taking assembly 11;
e. when the feeding assembly 12 is started, the feeding cylinder 24 pushes the material frame 6 on the feeding frame 25, on which new sodium fluoride particles are placed, to move towards the moving side plate 9 until the material frame is moved in place, and the pushing motor 42 is started to drive the pushing screw 43 to rotate, so that the moving side plate 9 moves towards the direction close to the reaction box 3 until the insertion section 54 at the end part of the material frame 6 on the feeding frame 25 is completely inserted into the insertion slot 53 of the bracket 52; after the material taking component 11 with the animal material frame 6 is moved out, the material placing component 12 drives the material frame 6 on the material placing rack 25 to move in place, so that the material frames 6 correspond to the brackets 52 one by one, and the brackets 52 are driven by the pushing motor 42 to move in place and are inserted into the material frames 6;
f. the lifting cylinder 14 is started to drive the material taking assembly 11 and the material placing assembly 12 to integrally move downwards until the material placing assembly 12 moves downwards to the proper position, so that the material placing support rod 33 is completely separated from the clamping groove 35 corresponding to the material frame 6, meanwhile, the material placing support plate 27 and the material placing baffle plate 31 also move to the position below the corresponding material frame 6, and the material placing cylinder 24 is started to drive the material placing frame 25 to move and reset; after the bracket 52 and the material frame 6 are completely inserted, the lifting cylinder 14 and the material placing cylinder 24 drive the material placing frame 25 to move and reset, so that the material placing assembly 12 cannot influence the next pushing motor 42 to push the material frame 6 into the reaction box 3;
g. the pushing motor 42 is started to drive the pushing screw 43 to rotate, so that the moving side plate 9 moves towards the reaction box 3, the moving side plate 9 drives the material frame 6 in which new sodium fluoride particles are placed to move towards the reaction box 3 synchronously until the material frame 6 passes through the corresponding through socket 49 and moves into the reaction box 3 completely, meanwhile, the fixed end plate 5 abuts against the side surface of the reaction box 3 to shield the through socket 49, and the moving side plate 9 shields and seals the opening 8 on the side surface of the treatment box 1; the fixed end plate 5 shields the sealing penetrating socket 49, the movable side plate 9 shields the sealing opening 8, and the shielding sealing performance can be ensured by matching with the design of a sealing gasket, so that the self sealing performance of the treatment box 1 and the reaction box 3 is ensured after the material frame 6 moves in place in the reaction box 3, the gas leakage in the treatment process is effectively prevented, and meanwhile, after the material frame 6 moves in place in the reaction box 3, the auxiliary support limiting is carried out on the material frame 6 through the auxiliary frame, the structural stability and reliability of the whole material frame 4 are ensured, and the whole treatment process is smoother;
h. opening a sealing door on the side surface of the replacement box 2 close to the material taking assembly 11, removing the material frame 6 on the material taking frame 16, performing concentrated regeneration treatment on sodium fluoride in the material frame 6, and recycling the regenerated sodium fluoride; the sodium fluoride at the replacement part is regenerated and reused, so that the waste of resources is effectively reduced, and the cost is saved;
(3) collecting the product obtained after the HF removal treatment in the step (2) into a liquid nitrogen tank, separating vinylidene fluoride in the product through low-temperature evaporation, and filtering, washing and drying to obtain a final product; the quality of the final product is effectively ensured through the treatments of low-temperature evaporation, filtration, washing and drying.
The method has reasonable design and simple and easily-operated process steps, the trifluoroethane is subjected to thermal cracking HF removal treatment to obtain the vinylidene fluoride, the finally prepared product is further treated, the actual product quality is effectively improved, the HF removal treatment is carried out by adopting special HF removal equipment, the actual treatment effect is effectively ensured, HF is adsorbed by the sodium fluoride, the sodium fluoride particles are periodically replaced, the actual adsorption effect is ensured, automatic replacement treatment is adopted in the replacement process of the sodium fluoride, manual replacement is not needed, the replacement operation is more efficient and safer, and the potential safety hazard is reduced.
In the invention, HF removing treatment is carried out by adopting HF removing equipment, a product obtained by thermal cracking is directly introduced into a reaction box 3, enters a buffer cavity from an air inlet pipe 39 at the bottom of the reaction box 3, enters the reaction box 3 after being shunted, airflow flows upwards from bottom to top, gradually passes through a plurality of layers of material frames 6, is contacted with sodium fluoride in the material frames 6, effectively removes HF through the adsorption of the sodium fluoride, and is finally discharged from an air outlet pipe 40 at the upper part, the design is ingenious and reasonable, sodium fluoride particles in the material frames 6 are replaced after the HF removing equipment is used for a period of time, thereby ensuring the actual adsorption effect, the whole replacement process is operated in the inner cavity of a replacement box 2, the material frames 6 in the reaction box 3 are pulled into the replacement box 2 by a pushing component 10 during replacement, the material frames 6 are taken away by a material taking component 11, so that the material frames 6 and a material rack 4 are separated, the new material frame 6 is placed on the material frame 4 through the material placing component 12, new sodium fluoride is placed in the new material frame 6, the replaced material frame 6 is integrally pushed into the reaction box 3 through the pushing component 10, the whole replacement operation is automatic, the material frame 6 does not need to be pulled and pulled manually, the damage caused by high temperature in the manual replacement process is avoided, the damage to a human body due to gas leakage is also avoided, the new material frame 6 is placed on the material placing frame 25 before replacement, a sealing door is managed, then the replacement operation is carried out, after the replacement is finished, the old material frame 6 is taken out after a certain time, sodium fluoride particles in the taken material frame 6 are regenerated, the recycling of resources is realized, and the cost is effectively saved.
The above are only specific embodiments of the present invention, but the technical features of the present invention are not limited thereto. Any simple variations, equivalent substitutions or modifications based on the present invention to achieve substantially the same technical effects are within the scope of the present invention.

Claims (10)

1. An HF removing device for preparing vinylidene fluoride from trifluoroethane is characterized in that: including handling the case and changing the case, it is provided with the reaction box to handle the incasement, be provided with the material frame in the reaction box, the material frame is including fixed end plate and material frame, material frame evenly distributed is in on the fixed end plate, the sodium fluoride granule has been placed in the material frame, be provided with the material top cap on the top surface of material frame, the embedding of one side of handling the case is in change on the case, it is in to handle the case embedding be provided with the opening on changing the side of case, the sealed removal curb plate that shelters from of opening part, remove the curb plate with fixed end plate fixed connection, it is connected with the promotion subassembly to remove the curb plate, it gets material subassembly and blowing subassembly to be provided with in the change case, get the material subassembly with the blowing subassembly is connected on the installation roof, the installation roof is connected with lift cylinder.
2. The apparatus for removing HF for preparing vinylidene fluoride from trifluoroethane according to claim 1, wherein the apparatus comprises: the material taking assembly comprises a material taking cylinder and a material taking frame, the material taking cylinder is connected with the material taking frame, the material taking frame comprises a material taking side plate, a material taking support plate and a material taking end frame, the material taking side plate is connected with a piston rod of the material taking cylinder, the material taking side plate is connected in a material taking chute of the mounting top plate in a sliding mode, the material taking support plate is located on the material taking side plate, the material taking support plate corresponds to the material frame in a one-to-one mode, one end of the material taking support plate is fixedly connected with the material taking side plate, a material taking convex plate is arranged at the other end of the material taking support plate, the material taking end frame comprises a material taking end plate and a material taking support rod, the material taking support rod is fixedly arranged on the material taking end plate, a material taking folding rod is arranged at one end of the material taking support rod, and the material taking side plate is fixedly connected with the material taking end plate.
3. The apparatus for removing HF for preparing vinylidene fluoride from trifluoroethane according to claim 2, wherein the apparatus comprises: the discharging assembly comprises a discharging cylinder and a discharging frame, the discharging cylinder is connected with the discharging frame, the discharging frame comprises a discharging side plate, a discharging support plate and a discharging end frame, the discharging side plate is connected with a piston rod of the discharging cylinder, the discharging side plate is connected in a discharging chute of the mounting top plate in a sliding mode, the discharging support plate is located on the discharging side plate, the discharging support plate corresponds to the material frame in a one-to-one mode, one end of the discharging support plate is fixedly connected with the discharging side plate, a discharging baffle plate is arranged at the other end of the discharging support plate, the discharging end frame comprises a discharging end plate and a discharging support rod, the discharging support rod is fixedly arranged on the discharging end plate, a discharging folding rod is arranged at one end of the discharging support rod, and the discharging folding rod is fixedly connected with the discharging side plate.
4. The apparatus for removing HF for preparing vinylidene fluoride from trifluoroethane according to claim 3, wherein the apparatus comprises: the bottom surface of the material frame is provided with an embedding clamping groove, the material taking support rod and the material discharging support rod are matched with the embedding clamping groove, and the material taking support rod or the material discharging support rod is clamped and supported in the corresponding embedding clamping groove.
5. The apparatus for removing HF for preparing vinylidene fluoride from trifluoroethane according to claim 1, wherein the apparatus comprises: the bottom of reaction box is provided with the cushion chamber, the cushion intracavity separates into two at least wall chambeies, every the outside in wall chamber all communicates there is the reposition of redundant personnel pipe, be provided with flow control valve on the reposition of redundant personnel pipe, the tip of reposition of redundant personnel pipe extends it is connected with the buffer memory case to handle the case, be provided with the intake pipe on the buffer memory case, the top of reaction box is provided with the outlet duct, the tip of outlet duct extends it handles the case.
6. The apparatus for removing HF for preparing vinylidene fluoride from trifluoroethane according to claim 1, wherein the apparatus comprises: the pushing assembly comprises a pushing motor, a pushing screw rod, a guiding bottom rod and a guiding ejector rod, the pushing motor is connected with the pushing screw rod, a bottom extension plate is arranged at the bottom of the moving side plate and sleeved on the pushing screw rod and the guiding bottom rod, a top extension plate is arranged at the top of the moving side plate and sleeved on the guiding ejector rod.
7. The apparatus for removing HF for preparing vinylidene fluoride from trifluoroethane according to claim 1, wherein the apparatus comprises: the reaction box is just right be provided with the socket that runs through on the side of export, run through the socket with material frame one-to-one matches, through run through the socket and realize the material frame is in shifting out or pushing of reaction box, be provided with the auxiliary frame in the reaction box, every run through the correspondence of socket department and be provided with a set of auxiliary frame, the auxiliary frame is including last pressure frame and lower support frame, through it is right to support the frame down in the reaction box the bottom of material frame supports and lifts, through it is right to go up the pressure frame the material top cap is contradicted spacingly.
8. The apparatus for removing HF for preparing vinylidene fluoride from trifluoroethane according to claim 1, wherein the apparatus comprises: the material frame is characterized in that brackets are arranged on the fixed end plate and correspond to the material frames one to one, slots are formed in the brackets, inserting sections are arranged on the material frame and are inserted into the slots in a matching mode, extending grooves are formed in the fixed end plate and communicated with the slots in a one to one correspondence mode, and the end portions of the inserting sections penetrate through the slots and extend into the corresponding extending grooves in an inserting mode.
9. The preparation method of vinylidene fluoride of the HF removing equipment for preparing vinylidene fluoride based on trifluoroethane is characterized by comprising the following steps: the method comprises the following steps:
(1) thermal cracking: introducing trifluoroethane gas into a platinized iron-nickel alloy tube, heating to 1100-1500 ℃, reacting for 0.01s at normal pressure and airspeed of 9700h -1
(2) HF removal:
a. directly introducing the product obtained by the reaction in the step (1) into HF removing equipment, introducing gas into a cache box from a gas inlet pipe, then introducing the gas into a corresponding partition cavity through a shunt pipe, and then introducing the gas into the reaction box from the partition cavity;
b. after gas enters the reaction box, the gas enters the material frame from the through hole at the bottom surface of the bottommost material frame in the reaction box, contacts with sodium fluoride particles placed in the material frame, flows out from the through hole on the material top cover at the top surface of the material frame, continues to flow upwards, sequentially contacts with sodium fluoride particles in other material frames until the gas flows out from the through hole on the material top cover at the top material frame, and is discharged from the gas outlet pipe, wherein the sodium fluoride particles placed in the material frame are 2-10nm, the reaction temperature in the reaction box is 20-80 ℃, and the reaction pressure is 0.12-0.18 MPa;
c. positioning and replacing sodium fluoride particles in the material frame;
(3) and (3) collecting the product obtained after the HF removal treatment in the step (2) into a liquid nitrogen tank, separating vinylidene fluoride in the product through low-temperature evaporation, and filtering, washing and drying to obtain the final product.
10. A method for producing vinylidene fluoride according to claim 9, characterized in that: in step c of the step (2), the operation steps of replacing sodium fluoride particles are as follows:
a. opening a sealing door on the side face of the replacement box, which is close to the material placing assembly, placing a material frame filled with new sodium fluoride particles on the material placing frame, wherein the material frame is just clamped between a material placing side plate and a material placing baffle plate, meanwhile, a clamping groove at the bottom of the material frame just corresponds to a material placing support rod, the material placing support rod is clamped into the clamping groove, and then the sealing door is closed;
b. the pushing assembly is started, the pushing motor drives the pushing screw to rotate, so that the movable side plate moves towards the interior of the replacement box along the pushing screw, the upper side and the lower side of the movable side plate are respectively guided by the guide ejector rod and the guide bottom rod in a limiting manner, the movable side plate drives the fixed end plate fixed with the movable side plate to move when moving, the fixed end plate further drives the animal material frame to move from the reverse box to the exterior of the replacement box cavity until the movable side plate moves in place, and the material frame is completely moved out of the corresponding penetrating socket of the reaction box;
c. the material taking assembly moves, the material taking cylinder pushes the material taking frame to move towards the direction of the material frame moved out of the reaction box until the material taking frame moves in place, the material taking support plate moves to the position below the corresponding material frame, the lifting cylinder is started to drive the material taking assembly and the material placing assembly to integrally move upwards, so that the material taking support plate is movably supported below the corresponding material frame, meanwhile, the material frame is just limited between the material taking side plate and the material taking baffle convex plate, and meanwhile, the material taking support rod is just movably clamped in the clamping groove at the bottom of the material frame;
d. the pushing motor is started to drive the pushing screw to rotate, so that the moving side plate continues to move in the direction away from the reaction box until the moving side plate moves in place, the inserting section at the end part of the material frame is completely separated from the bracket, and the material taking cylinder is restarted to drive the material taking frame to move and reset;
e. the discharging assembly is started, the discharging air cylinder pushes the material frame, on which new sodium fluoride particles are placed, on the discharging frame to move towards the moving side plate until the material frame is moved in place, and the pushing motor is started to drive the pushing screw to rotate, so that the moving side plate moves towards the direction close to the reaction box until the insertion section at the end part of the material frame on the discharging frame is completely inserted into the insertion slot of the bracket;
f. the lifting cylinder is started to drive the material taking assembly and the material placing assembly to integrally move downwards until the material placing assembly moves downwards to the proper position, so that the material placing support rod is completely separated from the clamping groove corresponding to the material frame, meanwhile, the material placing support plate and the material placing baffle convex plate also move to the position below the corresponding material frame, and the material placing cylinder is started to drive the material placing frame to move and reset;
g. the pushing motor is started to drive the pushing screw to rotate, so that the moving side plate moves towards the reaction box, the moving side plate drives the material frame in which new sodium fluoride particles are placed to move towards the reaction box synchronously until the material frame passes through the corresponding penetrating socket and moves into the reaction box completely, meanwhile, the fixed end plate abuts against the side face of the reaction box to shield the penetrating socket, and the moving side plate shields and seals an opening on the side face of the treatment box;
h. and opening the side surface of the replacement box close to a sealing door of the material taking assembly, removing the material frame on the material taking frame, performing concentrated regeneration treatment on the sodium fluoride in the material frame, and recycling the sodium fluoride after the regeneration treatment.
CN202210350886.7A 2022-04-02 2022-04-02 HF (hydrogen fluoride) removal equipment for preparing vinylidene fluoride from trifluoroethane and preparation method of vinylidene fluoride Active CN114917859B (en)

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Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN203728144U (en) * 2014-01-16 2014-07-23 合肥凯邦电机有限公司 Material taking device for tool plate
CN106346230A (en) * 2016-11-21 2017-01-25 苏州鑫润旺精密机械有限公司 First crankshaft feeding assembly of crankshaft connecting rod assembly machine
CN108722449A (en) * 2018-05-04 2018-11-02 同济大学 A kind of hydrofluorocarbon dehydrofluorination prepares the catalyst and preparation method and applications of Fluorine containing olefine
CN208612141U (en) * 2018-06-29 2019-03-19 江西天行化工有限责任公司 A kind of hydrogen fluoride absorption and regeneration device
CN208732689U (en) * 2018-05-11 2019-04-12 浙江水利水电学院 A kind of Dynamic Membrane Water feeding treatment device of high temperature sintering material production
CN211302644U (en) * 2019-09-04 2020-08-21 江西渠成氟化学有限公司 Ammonium bifluoride tail gas absorbing device
CN111633819A (en) * 2020-04-22 2020-09-08 生态环境部华南环境科学研究所 Device for preparing regenerated mixed brick from waste cement material and preparation method thereof
CN111729469A (en) * 2020-06-12 2020-10-02 中船重工(邯郸)派瑞特种气体有限公司 Adsorption tower for removing impurity particles in gas
CN213977485U (en) * 2020-10-23 2021-08-17 常熟三爱富振氟新材料有限公司 Dry method separator in vinylidene fluoride production
CN214489510U (en) * 2021-04-14 2021-10-26 中山火炬职业技术学院 Accurate material taking and assembling device

Patent Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN203728144U (en) * 2014-01-16 2014-07-23 合肥凯邦电机有限公司 Material taking device for tool plate
CN106346230A (en) * 2016-11-21 2017-01-25 苏州鑫润旺精密机械有限公司 First crankshaft feeding assembly of crankshaft connecting rod assembly machine
CN108722449A (en) * 2018-05-04 2018-11-02 同济大学 A kind of hydrofluorocarbon dehydrofluorination prepares the catalyst and preparation method and applications of Fluorine containing olefine
CN208732689U (en) * 2018-05-11 2019-04-12 浙江水利水电学院 A kind of Dynamic Membrane Water feeding treatment device of high temperature sintering material production
CN208612141U (en) * 2018-06-29 2019-03-19 江西天行化工有限责任公司 A kind of hydrogen fluoride absorption and regeneration device
CN211302644U (en) * 2019-09-04 2020-08-21 江西渠成氟化学有限公司 Ammonium bifluoride tail gas absorbing device
CN111633819A (en) * 2020-04-22 2020-09-08 生态环境部华南环境科学研究所 Device for preparing regenerated mixed brick from waste cement material and preparation method thereof
CN111729469A (en) * 2020-06-12 2020-10-02 中船重工(邯郸)派瑞特种气体有限公司 Adsorption tower for removing impurity particles in gas
CN213977485U (en) * 2020-10-23 2021-08-17 常熟三爱富振氟新材料有限公司 Dry method separator in vinylidene fluoride production
CN214489510U (en) * 2021-04-14 2021-10-26 中山火炬职业技术学院 Accurate material taking and assembling device

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