CN111892480B - Preparation method of 1-chloro-3, 3, 3-trifluoropropene - Google Patents
Preparation method of 1-chloro-3, 3, 3-trifluoropropene Download PDFInfo
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- CN111892480B CN111892480B CN202010786909.XA CN202010786909A CN111892480B CN 111892480 B CN111892480 B CN 111892480B CN 202010786909 A CN202010786909 A CN 202010786909A CN 111892480 B CN111892480 B CN 111892480B
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/38—Separation; Purification; Stabilisation; Use of additives
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/093—Preparation of halogenated hydrocarbons by replacement by halogens
- C07C17/20—Preparation of halogenated hydrocarbons by replacement by halogens of halogen atoms by other halogen atoms
- C07C17/202—Preparation of halogenated hydrocarbons by replacement by halogens of halogen atoms by other halogen atoms two or more compounds being involved in the reaction
- C07C17/206—Preparation of halogenated hydrocarbons by replacement by halogens of halogen atoms by other halogen atoms two or more compounds being involved in the reaction the other compound being HX
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/25—Preparation of halogenated hydrocarbons by splitting-off hydrogen halides from halogenated hydrocarbons
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- C—CHEMISTRY; METALLURGY
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- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/38—Separation; Purification; Stabilisation; Use of additives
- C07C17/383—Separation; Purification; Stabilisation; Use of additives by distillation
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- C07—ORGANIC CHEMISTRY
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- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/38—Separation; Purification; Stabilisation; Use of additives
- C07C17/389—Separation; Purification; Stabilisation; Use of additives by adsorption on solids
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Abstract
The invention discloses a preparation method of 1-chloro-3, 3, 3-trifluoropropene, which comprises the following steps: a. pretreatment of 1,1,1,3, 3-pentachloropropane raw material: 1) washing with water, 2) standing for precipitation, 3) adsorption treatment, and 4) distillation treatment; b. carrying out fluorination reaction; c. and (5) purification treatment. The invention adopts a pretreatment device to carry out impurity removal and purification treatment on the 1,1,1,3, 3-pentachloropropane which is the raw material required by the preparation of the 1-chloro-3, 3, 3-trifluoropropene, and effectively ensures the purity of the 1,1,1,3, 3-pentachloropropane through four steps of water washing, standing precipitation, adsorption and distillation, so that the subsequent fluorination reaction is more complete, the influence of impurity components in the raw material on the service life of the catalyst in the fluorination reaction in the reaction process is reduced, the service life of the catalyst is effectively prolonged, and the problems of scaling, corrosion and the like in the device in the preparation of the 1-chloro-3, 3, 3-trifluoropropene can be effectively prevented.
Description
Technical Field
The invention belongs to the technical field of preparation of 1-chloro-3, 3, 3-trifluoropropene, and particularly relates to a preparation method of 1-chloro-3, 3, 3-trifluoropropene.
Background
1-chloro-3, 3, 3-trifluoropropene (hereinafter, sometimes referred to as 1233) is a compound having a double bond in its structure, having a very short life in the atmosphere, and promising as an environmentally friendly alternative to freon without fear of ozone layer destruction and global warming. The 1-chloro-3, 3, 3-trifluoropropene may be synthesized by a liquid phase fluorination reaction using 1,1,1,3, 3-pentachloropropane as a raw material. In the preparation process of the 1,1,1,3, 3-pentachloropropane raw material, impurities such as catalyst components and the like exist in the final product 1,1,1,3, 3-pentachloropropane, and impurities such as catalyst components and the like existing in the product of the 1,1,1,3, 3-pentachloropropane raw material influence the service life of the catalyst in the fluorination reaction in which 1-chloro-3, 3, 3-trifluoropropene is prepared from 1-chloro-3, 3, 3-trifluoropropene, so that the service life of the catalyst is shortened, the fluorination reaction is inhibited, and serious blockage, corrosion and the like are caused to equipment in the preparation of the 1-chloro-3, 3, 3-trifluoropropene.
Disclosure of Invention
The invention aims to provide a technical scheme of a preparation method of 1-chloro-3, 3, 3-trifluoropropene aiming at the defects in the prior art, a pretreatment device is adopted to carry out impurity removal and purification treatment on 1,1,1,3, 3-pentachloropropane which is a raw material required by the preparation of the 1-chloro-3, 3, 3-trifluoropropene, and the four-step treatment of washing, standing, precipitating, adsorbing and distilling is adopted to effectively ensure the purity of the 1,1,1,3, 3-pentachloropropane, so that the subsequent fluorination reaction is more complete, reduce the influence of impurity components in the raw material on the service life of a catalyst in the fluorination reaction in the reaction process, effectively prolong the service life of the catalyst, and effectively prevent scaling from occurring inside the device in the preparation of the 1-chloro-3, 3, 3-trifluoropropene, Corrosion and the like.
The preparation method of the 1-chloro-3, 3, 3-trifluoropropene is characterized by comprising the following steps:
a. pretreatment of 1,1,1,3, 3-pentachloropropane raw material:
1) and (3) water washing treatment:
(1) firstly, opening a flow dividing device close to the inlet of the top of the washing tower, rotating a rotating motor, driving a supporting screw rod to rotate by the rotating motor through a motor shaft, and moving a sleeve on the supporting screw rod along the supporting screw rod;
(2) the sleeve drives the adjusting rod group connected with the sleeve to move when moving, one end of the adjusting rod group is movably connected with the sleeve, the other end of the adjusting rod group is movably connected with one end of the shunting baffle, and the other end of the shunting baffle is rotatably connected with the bracket, so that the sleeve is ensured to drive the shunting baffle to rotate through the adjusting rod group, the shunting holes are opened, and the opening angles of the shunting holes are adjusted according to the treatment capacity and the treatment requirement of raw materials; the liquid raw material is sprayed to the water washing area in a plurality of angle directions through the shunting treatment of the shunting device, so that the raw material is fully mixed and contacted with water sprayed in the water washing area, the water washing speed is improved, the actual opening angle of the shunting hole can be controlled by controlling the rotating angle of the rotating motor, the opening size of the shunting hole can be adjusted according to the actual water washing requirement, and the water washing speed of the raw material is controlled;
(3) liquid raw materials are introduced into a washing tower, the raw materials enter from an inlet at the top of the washing tower, flow to a washing area from a flow distribution hole through the flow distribution of a flow distribution device, water is conveyed into two groups of spraying discs by a water pump and then is sprayed out from nozzles on the spraying discs, the water is sprayed upwards, the raw materials flow downwards, the water and the raw materials are mixed in a counter-flushing manner, and the raw materials entering the washing area are washed; the inlet of the water washing tower is positioned at the top, so that raw materials entering the water washing tower flow to the water washing area under the action of self gravity, meanwhile, the spraying discs spray water upwards through the spray heads, the water and the raw materials flow oppositely and are oppositely flushed and mixed, the water is fully contacted with the raw materials, the water washing quality and the water washing speed are effectively improved, impurities in the raw materials are more fully removed, and the working quality of the water washing tower is effectively improved through sequential water washing of the two groups of spraying discs;
(4) meanwhile, the circulating pump is started, the circulating pump conveys the washed raw materials into the circulating pipe from a circulating port, the raw materials are conveyed to the top of the washing tower through the circulating pipe and then enter the washing tower to be washed again, the circulating water is washed for 3-5 times, the circulating pump is closed, the suction pump is started, and meanwhile, the flow distribution device close to the bottom outlet of the washing tower is opened; the design is ingenious and reasonable, the circulating washing operation can be realized through the ingenious design of the circulating pump, and the water washing can be more sufficient through repeated circulating washing for many times, so that impurities in the raw materials can be effectively removed;
2) standing and precipitating: the raw material treated by the water washing tower flows downwards through the diversion holes, enters the conveying pipe from the outlet at the bottom of the water washing tower, is conveyed into the settling tower through the suction pump for standing and settling treatment, after standing and settling for 2-10 hours, the water layer on the upper layer is pumped away, the conveying pump is opened, and the raw material solution on the lower layer enters the conveying pipe through the outlet at the bottom of the settling tower and is conveyed into the adsorption tower through the conveying pump; conveying the mixed solution of the raw material mixed water after washing to a precipitation tower, realizing layering through standing treatment in the precipitation tower, wherein the upper layer is a water layer for dissolving impurities, the lower layer is a raw material layer with high density, the water layer on the upper layer is matched with a pump to pump, discharge and concentrate the water layer, the raw material layer on the lower layer is discharged from an outlet at the bottom of the precipitation tower for adsorption treatment, the whole design is reasonable, and a large amount of water layer is removed through standing precipitation firstly, so that subsequent adsorption treatment is facilitated, the subsequent impurity removal workload is reduced, and the service life of the adsorption layer is prolonged;
3) adsorption treatment: raw materials enter an adsorption zone through an inlet at the top of an adsorption tower, an adsorption layer is arranged in the adsorption tower, the adsorption layer comprises an activated carbon adsorption layer and a molecular sieve adsorption layer which are distributed at intervals, and the raw materials are discharged from an outlet at the bottom of the adsorption tower after adsorption treatment of the activated carbon adsorption layer and the molecular sieve adsorption layer; through multiple adsorption treatment of the plurality of activated carbon adsorption layers and the molecular sieve adsorption layers, residual moisture in the liquid raw material can be adsorbed, and residual impurities in the raw material can be further adsorbed and removed;
4) and (3) distillation treatment: conveying the raw materials subjected to adsorption treatment by the adsorption tower into a distillation kettle for further distillation treatment; the device has the advantages that the design is reasonable, most impurities are removed through washing and adsorption, the distillation treatment is carried out at last, residual impurities in the raw materials can be further removed through the distillation treatment, so that the purity of the raw materials is better, the distillation is positioned at the last step, residual moisture in the raw materials, adsorbent carried in the adsorption process and the like can be further removed through the distillation, the purity of the finally obtained raw materials is effectively improved, the influence of the impurities in the raw materials on a catalyst in the subsequent fluorination reaction is reduced, and the subsequent fluorination reaction is more complete;
b. fluorination reaction:
1) introducing the liquid 1,1,1,3, 3-pentachloropropane raw material subjected to distillation treatment into a fluorination reaction kettle, and adding a catalyst into the fluorination reaction kettle at the same time;
2) heating the fluorination reaction kettle, introducing anhydrous hydrogen fluoride into the fluorination reaction kettle after the temperature reaches 120-450 ℃, controlling the reaction pressure of the fluorination reaction kettle to be 0.08-5.5MPa, keeping for 2-5 hours, and finishing the reaction;
c. and (3) purification treatment: introducing the reacted product into a rectifying tower for rectification treatment, and then carrying out condensation reflux after rectification treatment, thereby obtaining a final finished product; the product is purified by rectification and condensation reflux, and the quality of the final product is improved.
Further, in step 3) of step a, set up the spoiler in the adsorption tower, spoiler and adsorption layer interval distribution hinder the upset through the spoiler to the raw materials for the raw materials reposition of redundant personnel, cross-mixing, fast diffusion in the adsorption zone, increase the area of contact of raw materials and adsorbed layer, thereby make raw materials and adsorbed layer fully contact mix, improve adsorption efficiency.
Further, in the step c, in the rectification treatment process, the tail gas generated by rectification is subjected to centralized recovery treatment through a tail gas collection tower, the tail gas is discharged after the recovery treatment is qualified, and the tail gas in the rectification treatment is subjected to recovery treatment, so that the air pollution caused by substances in the tail gas is avoided.
The pretreatment device for the raw material for the preparation method of 1-chloro-3, 3, 3-trifluoropropene is characterized in that: the pretreatment device comprises a washing tower, a precipitation tower and an adsorption tower which are sequentially arranged from left to right, the washing tower, the precipitation tower and the adsorption tower are connected through a conveying pipe, a suction pump is arranged on the conveying pipe between the washing tower and the precipitation tower, a conveying pump is arranged on the conveying pipe between the precipitation tower and the adsorption tower, a circulating port is arranged at the bottom of the washing tower and is communicated with the top of the washing tower through a circulating pipe, a circulating pump is arranged on the circulating pipe, a main support rod is arranged in the washing tower and is fixedly connected with the inner wall of the washing tower, two ends of the main support rod are respectively provided with a flow dividing device, the flow dividing devices are connected with a rotating motor, the rotating motor is fixedly connected with the end part of the main support rod through an auxiliary plate, a sealing protective cover is also covered on the rotating motor, the rotating motor is shielded and protected through the sealing protective cover, so that the service life of the rotating motor is prolonged, be provided with on the main tributary vaulting pole and spray the dish, evenly be provided with the shower nozzle on spraying the top surface of dish, be provided with interval distribution's spoiler and adsorbed layer in the adsorption tower, the adsorbed layer includes interval distribution's active carbon adsorption layer and molecular sieve adsorbed layer.
Further, the flow dividing device comprises a support and a flow dividing baffle plate, a support screw is arranged at the center of the support, one end of the support screw is connected with the support through a shaft sleeve, the other end of the support screw is connected with a motor shaft of the rotating motor, a sleeve is sleeved on the support screw in a threaded manner, a flow dividing hole is formed in the support, the flow dividing baffle plate is matched with the flow dividing hole, the flow dividing hole is shielded and sealed by the flow dividing baffle plate, the outer side end of the flow dividing baffle plate is rotatably connected with the support, the inner side end of the flow dividing baffle plate is connected with the sleeve through an adjusting rod group, one end of the adjusting rod group is movably connected with the flow dividing baffle plate, the other end of the adjusting rod group is movably connected with the sleeve, the whole structure is reasonable in design, the rotating motor rotates, the support screw is driven to rotate through the motor shaft, so that the sleeve on the support screw moves along the support screw, the sleeve moves to drive the adjusting rod group connected with the sleeve to rotate downwards, and the other end of regulating lever group is connected with reposition of redundant personnel baffle again, and the outside end of reposition of redundant personnel baffle is connected with the support rotation again to regulating lever group can stimulate reposition of redundant personnel baffle and down rotate in step, thereby open the diffluence orifice, and rotation angle and the number of turns through control rotating electrical machines, can control the opening angle of diffluence orifice, thereby the entering of strict control raw materials and get rid of the speed.
Further, the regulating rod group includes locating lever and movable rod, locating lever and movable rod adjustable connection, be provided with the link on the reposition of redundant personnel baffle, the locating lever rotates with the link to be connected, telescopic outer wall is provided with the card frame, the one end and the card frame of movable rod rotate to be connected, overall structure design benefit is reasonable, locating lever and movable rod combination form the regulating rod group, and locating lever and movable rod adjustable connection, can ensure that the regulating rod group can be according to the adaptability adjustment of opening the angle of reposition of redundant personnel baffle and doing length, and through the link, the regulating rod group and reposition of redundant personnel baffle can be convenient for in the design of card frame, installation between the sleeve, the dismouting of being convenient for.
Further, be provided with one end open-ended adjustment tank on the locating lever, the movable rod activity joint is in the adjustment tank, the both sides of adjustment tank all are provided with the spacing groove, be provided with the stopper on the movable rod, stopper and spacing groove phase-match, the spacing joint of stopper is at the spacing inslot, and the cooperation adjustment tank realizes the activity grafting between movable rod and the locating lever, thereby can change the whole length of regulating lever group, make regulating lever group can be according to the turned angle of reposition of redundant personnel baffle, the length adjustment of adaptability is to telescopic shift position, thereby guarantee the normal rotation of reposition of redundant personnel baffle and adjust, and ingenious cooperation through spacing groove and stopper, can play further spacing guide effect, make relative movement more steady between movable rod and the locating lever, ensure the overall structure firm reliability of regulating lever group.
Furthermore, the spraying discs are provided with two groups, one side of each group of spraying discs, which is provided with the spray heads, is provided with a baffle component, each baffle component comprises two arc-shaped baffle plates and an installation sleeve which are symmetrical in the left and right directions, the arc-shaped baffle plates are connected with the installation sleeves, the installation sleeves are fixed on the main support rods, the design is reasonable, one group of baffle components is arranged above each group of spraying discs, the baffle components play a role in buffering, the impact force of the raw materials on the spraying discs is reduced, meanwhile, the flow paths of the raw materials can be changed through the two arc-shaped baffle plates which are symmetrical in the left and right directions, the liquid raw materials can flow downwards in multiple angles, the spray heads spray water upwards, the liquid raw materials and the raw materials flowing downwards are mixed in a counter-flushing manner, and the raw materials are diffused in multiple angles due to the influence of the raw materials by the arc-shaped baffle plates, so that the raw materials are fully mixed and contacted with the water, and the washing speed and the washing quality are effectively improved, make the impurity clearance in the raw materials higher, baffling subassembly, spray and coil all to set up on the main tributary vaulting pole moreover, support fixedly through the main tributary vaulting pole, the main tributary vaulting pole again with wash the tower between inside the installation fixed to effectively guarantee baffling subassembly, spray the installation fastness of dish.
Due to the adoption of the technical scheme, the invention has the following beneficial effects:
in the invention, the raw material 1,1,1,3, 3-pentachloropropane required by the preparation of 1-chloro-3, 3, 3-trifluoropropene is purified by removing impurities, catalyst components (metal solubilizer, hydrochloride of the metal solubilizer and the like) existing in the raw material 1,1,1,3, 3-pentachloropropane can influence the service life of the catalyst in the preparation process of 1-chloro-3, 3, 3-trifluoropropene, fluorination reaction and required devices in the preparation process of 1-chloro-3, 3, 3-trifluoropropene, and the impurities of the metal solubilizer, the hydrochloride of the metal solubilizer, iron complex thereof and the like in the 1,1,1,3, 3-pentachloropropane are removed by repeated circulating water washing, the frequency of the water washing is controlled, the water washing effect and quality are ensured, and the water washing frequency can enter a precipitation tower after reaching the set requirement, through the standing precipitation of a precipitation tower, a water layer dissolving catalyst components in 1,1,1,3, 3-pentachloropropane and a 1,1,1,3, 3-pentachloropropane raw material are separated through standing, the bottom layer is a 1,1,1,3, 3-pentachloropropane raw material solution with high density, the bottom layer raw material solution of the 1,1,1,3, 3-pentachloropropane is conveyed into an adsorption tower for adsorption treatment, through the multiple adsorption treatment of an active carbon adsorption layer and a molecular sieve adsorption layer, residual moisture in the 1,1,1,3, 3-pentachloropropane raw material solution can be adsorbed, impurities in the 1,1,1,3, 3-pentachloropropane can be further removed, the content of the catalyst impurity components in the 1,1,1,3, 3-pentachloropropane is reduced, and distillation treatment is carried out after the adsorption treatment, impurities and moisture in the 1,1,1,3, 3-pentachloropropane can be further evaporated and removed through distillation treatment, and the adsorbent carried by the 1,1,1,3, 3-pentachloropropane after adsorption treatment can be removed through evaporation, so that the purity of the finally obtained 1,1,1,3, 3-pentachloropropane raw material is improved, the content of the impurities in the 1,1,1,3, 3-pentachloropropane raw material is greatly reduced and controlled, and the problems of shortening of the service life of the catalyst, inhibiting of the fluorination reaction, corrosion of the device and the like in the 1-chloro-3, 3, 3-trifluoropropene reaction are avoided.
The invention respectively arranges the shunting devices at the inlet and the outlet in the washing tower, the shunting device at the inlet can control the opening angle of the shunting hole at the inlet according to the actual processing amount and the washing processing speed of the raw material, the shunting device at the outlet can be matched with the design of a circulating pump to ensure that the shunting hole of the shunting device at the outlet can be opened after the raw material reaches multiple washing times, so that the raw material reaching the washing times is output from the washing tower, the processing amount of the raw material conveyed into the settling tower can be controlled by controlling the angle and the closing time of the shunting hole at the outlet, two groups of spraying discs are arranged in the washing tower, two washing sprays are realized by the two groups of spraying discs, the raw material flows downwards, and the water is sprayed upwards, so that the raw material is in opposite contact with the water, the raw material is fully mixed, and the washing speed is effectively improved, and every group has all set up the baffling subassembly above spraying the dish, can slow down the impact force of raw materials to spraying the dish through the baffling subassembly, the life of extension spraying the dish to because the impact of arc baffling board, make the flow path of raw materials take place the sudden change, the raw materials diffusion that splashes continues down flow from many angles and direction, effectively improves the washing quality of raw materials, and impurity content in the control raw materials makes the purity of raw materials higher.
Drawings
The invention will be further described with reference to the accompanying drawings in which:
FIG. 1 is a schematic view showing the installation structure of a water washing column, a precipitation column and an adsorption column in the present invention;
FIG. 2 is a schematic structural view of the shunt hole of the present invention when closed;
FIG. 3 is a schematic structural diagram of the state of the adjusting rod set when the shunt hole is closed according to the present invention;
FIG. 4 is a schematic view of the structure of the shunt hole of the present invention when it is opened;
FIG. 5 is a structural diagram of the adjusting rod set when the tap hole is opened according to the present invention;
FIG. 6 is a schematic view of a portion of the enlarged structure at I in FIG. 5;
fig. 7 is a schematic view of a part of the enlarged structure at II in fig. 5.
In the figure: 1-a water washing tower; 2-a flow splitting device; 3-a rotating electrical machine; 4-a support screw; 5-a sleeve; 6-adjusting the rod group; 7-a splitter baffle; 8-a scaffold; 9-a shunt hole; 10-a spray tray; 11-a spray head; 12-a circulation pump; 13-a circulation pipe; 14-a circulation port; 15-a suction pump; 16-a delivery pipe; 17-a precipitation column; 18-a delivery pump; 19-an adsorption column; 20-an activated carbon adsorption layer; 21-a molecular sieve adsorption layer; 22-a positioning rod; 23-a movable bar; 24-an adjustment groove; 25-a limit groove; 26-a limiting block; 27-a baffle assembly; 28-arc baffle plate; 29-mounting a sleeve; 30-main support bar; 31-a spoiler; 32-a connecting frame; 33-card frame.
Detailed Description
As shown in FIGS. 1 and 5, the process for preparing 1-chloro-3, 3, 3-trifluoropropene according to the present invention comprises the steps of:
a. pretreatment of 1,1,1,3, 3-pentachloropropane raw material:
1) and (3) water washing treatment:
(1) firstly, opening a flow dividing device 2 close to an inlet at the top of a washing tower 1, rotating a rotating motor 3, driving a supporting screw rod 4 to rotate by the rotating motor 3 through a motor shaft, connecting the top end of the supporting screw rod 4 with a bracket 8 through a shaft sleeve, and moving a sleeve 5 on the supporting screw rod 4 along the supporting screw rod 4;
(2) the sleeve 5 drives the adjusting rod group 6 connected with the sleeve to move when moving, one end of the adjusting rod group 6 is movably connected with the sleeve 5, the other end of the adjusting rod group 6 is movably connected with one end of the shunting baffle 7, and the other end of the shunting baffle 7 is rotatably connected with the bracket 8, so that the sleeve 5 is ensured to drive the shunting baffle 7 to rotate through the adjusting rod group 6, the shunting hole 9 is opened, and the opening angle of the shunting hole 9 is adjusted according to the processing amount and the processing requirement of raw materials; the liquid raw material is sprayed to the washing area in a plurality of angular directions to flow through the shunting treatment of the shunting device 2, so that the raw material is fully mixed and contacted with the water sprayed in the washing area, the washing speed is improved, the actual opening angle of the shunting hole 9 can be controlled by controlling the rotation angle of the rotating motor 3, the opening size of the shunting hole 9 can be adjusted according to the actual washing requirement, and the washing speed of the raw material is controlled;
(3) liquid raw materials are introduced into a washing tower 1, the raw materials enter from an inlet at the top of the washing tower 1, flow to a washing area from a diversion hole 9 through diversion of a diversion device 2, water is conveyed into two groups of spraying discs 10 by a water pump and then is sprayed out from spray nozzles 11 on the spraying discs 10, the water is sprayed upwards, the raw materials flow downwards, the water and the raw materials are mixed in a counter-flushing manner, and the raw materials entering the washing area are washed; the inlet of the water washing tower 1 is positioned at the top, so that raw materials entering the water washing tower 1 flow to a water washing area under the action of self gravity, meanwhile, the spraying discs 10 spray water upwards through the spray nozzles 11, the water and the raw materials flow oppositely and are mixed in a counter flushing manner, the water is fully contacted with the raw materials, the water washing quality and the water washing speed are effectively improved, impurities in the raw materials are removed more fully, and the working quality of the water washing tower 1 is effectively improved through sequential water washing of the two groups of spraying discs 10;
(4) meanwhile, the circulating pump 12 is started, the circulating pump 12 conveys the washed raw materials into the circulating pipe 13 from the circulating port 14, the raw materials are conveyed to the top of the washing tower 1 through the circulating pipe 13 and then enter the washing tower 1 for washing treatment again, the circulating water is washed for 3-5 times, the circulating pump 12 is closed, the suction pump 15 is started, and the flow dividing device 2 close to the outlet at the bottom of the washing tower 1 is opened; the design is ingenious and reasonable, the circulating water washing operation can be realized through the ingenious design of the circulating pump 12, and the water washing can be more sufficient through repeated circulating water washing for many times, so that impurities in the raw materials can be effectively removed;
2) and (3) standing and precipitating: the raw material treated by the water washing tower 1 flows downwards through the diversion hole 9, enters the conveying pipe 16 from the outlet at the bottom of the water washing tower 1, is conveyed into the settling tower 17 through the suction pump 15 for standing and settling treatment, after standing and settling for 2-10 hours, the upper water layer is pumped away, the conveying pump 18 is opened, and the lower raw material solution enters the conveying pipe 16 through the outlet at the bottom of the settling tower 17 and is conveyed into the adsorption tower 19 through the conveying pump 18; the mixed solution of the washed raw material mixed water is conveyed to a precipitation tower 17, layering is realized through standing treatment in the precipitation tower 17, the upper layer is a water layer for dissolving impurities, the lower layer is a raw material layer with high density, the water layer on the upper layer is matched with a pump to pump, discharge and concentrate the water layer, the raw material layer on the lower layer is discharged from an outlet at the bottom of the precipitation tower 17 for adsorption treatment, the whole design is reasonable, a large amount of water layer is removed through standing precipitation firstly, so that the subsequent adsorption treatment is facilitated, the subsequent impurity removal workload is reduced, and the service life of the adsorption layer is prolonged;
3) and (3) adsorption treatment: raw materials enter an adsorption zone through an inlet at the top of an adsorption tower 19, an adsorption layer is arranged in the adsorption tower 19 and comprises activated carbon adsorption layers 20 and molecular sieve adsorption layers 21 which are distributed at intervals, and the raw materials are discharged from an outlet at the bottom of the adsorption tower 19 after adsorption treatment of the activated carbon adsorption layers 20 and the molecular sieve adsorption layers 21; through multiple adsorption treatment of the plurality of activated carbon adsorption layers 20 and the molecular sieve adsorption layers 21, residual moisture in the liquid raw material can be adsorbed, and residual impurities in the raw material can be further adsorbed and removed; the flow blocking plate 31 is arranged in the adsorption tower 19, the flow blocking plate 31 and the adsorption layer are distributed at intervals, and the flow blocking plate 31 is used for blocking and disturbing raw materials, so that the raw materials are divided, mixed in a cross mode and quickly diffused in the adsorption area, the contact area between the raw materials and the adsorption layer is increased, the raw materials and the adsorption layer are fully contacted and mixed, and the adsorption efficiency is improved;
4) and (3) distillation treatment: conveying the raw materials adsorbed by the adsorption tower 19 into a distillation still for further distillation treatment; the device has the advantages that the design is reasonable, most impurities are removed through washing and adsorption, the distillation treatment is carried out at last, residual impurities in the raw materials can be further removed through the distillation treatment, so that the purity of the raw materials is better, the distillation is positioned at the last step, residual moisture in the raw materials, adsorbent carried in the adsorption process and the like can be further removed through the distillation, the purity of the finally obtained raw materials is effectively improved, the influence of the impurities in the raw materials on a catalyst in the subsequent fluorination reaction is reduced, and the subsequent fluorination reaction is more complete;
b. fluorination reaction:
1) introducing the liquid 1,1,1,3, 3-pentachloropropane raw material subjected to distillation treatment into a fluorination reaction kettle, and simultaneously adding a catalyst into the fluorination reaction kettle;
2) heating the fluorination reaction kettle, introducing anhydrous hydrogen fluoride into the fluorination reaction kettle after the temperature reaches 120-450 ℃, controlling the reaction pressure of the fluorination reaction kettle to be 0.08-5.5MPa, keeping for 2-5 hours, and finishing the reaction;
c. and (3) purification treatment: introducing the reacted product into a rectifying tower for rectification treatment, and then carrying out condensation reflux after rectification treatment, thereby obtaining a final finished product; the product is purified through rectification and condensation reflux, so that the quality of the final product is improved; in the rectification treatment process, tail gas generated by rectification is subjected to concentrated recovery treatment through a tail gas collection tower, the tail gas is discharged after the recovery treatment is qualified, and the tail gas in the rectification treatment is subjected to recovery treatment, so that the air pollution caused by substances in the tail gas is avoided.
The pretreatment device of the raw materials for the preparation method of the 1-chloro-3, 3, 3-trifluoropropene comprises a water washing tower 1, a precipitation tower 17 and an adsorption tower 19 which are sequentially arranged from left to right, the water washing tower 1, the precipitation tower 17 and the adsorption tower 19 are connected through a conveying pipe 16, the conveying pipe 16 between the water washing tower 1 and the precipitation tower 17 is provided with a suction pump 15, the conveying pipe 16 between the precipitation tower 17 and the adsorption tower 19 is provided with a conveying pump 18, the bottom of the water washing tower 1 is provided with a circulation port 14, the circulation port 14 is communicated with the top of the water washing tower 1 through a circulation pipe 13, the circulation pipe 13 is provided with a circulation pump 12, the water washing tower 1 is internally provided with a main support rod 30, the main support rod 30 is fixedly connected with the inner wall of the water washing tower 1, the main support rod 30 plays a main support role and can be convenient for supporting and installing each component in the water washing tower, two ends of the main support rod 30 are respectively provided with a flow dividing device 2, flow divider 2 is connected with rotating electrical machines 3, rotating electrical machines 3 passes through the accessory plate and main tributary vaulting pole 30's tip fixed connection, still covered sealed safety cover on rotating electrical machines 3, shelter from the protection through sealed safety cover to rotating electrical machines 3, the life of extension rotating electrical machines 3, be provided with on the main tributary vaulting pole 30 and spray dish 10, evenly be provided with shower nozzle 11 on the top surface of spray dish 10, it communicates the washing tower 1 outside to establish through a conduction pipe to spray dish 10, the water pump is carried the water source in the conduction pipe, enter into spray dish 10 from the conduction pipe again, finally spout from shower nozzle 11, be provided with interval distribution's spoiler 31 and adsorbed layer in the adsorption tower 19, the adsorbed layer includes interval distribution's active carbon adsorption layer 20 and molecular sieve adsorbed layer 21.
The flow dividing device 2 comprises a support 8 and a flow dividing baffle 7, a support screw 4 is arranged at the center of the support 8, one end of the support screw 4 is connected with the support 8 through a shaft sleeve, the other end of the support screw 4 is connected with a motor shaft of the rotating motor 3, a sleeve 5 is sleeved on the support screw 4 in a threaded manner, a flow dividing hole 9 is formed in the support 8, the flow dividing baffle 7 is matched with the flow dividing hole 9, the flow dividing hole 9 is shielded and sealed by the flow dividing baffle 7, the outer side end of the flow dividing baffle 7 is rotatably connected with the support 8, the inner side end of the flow dividing baffle 7 is connected with the sleeve 5 through an adjusting rod group 6, one end of the adjusting rod group 6 is movably connected with the flow dividing baffle 7, the other end of the adjusting rod group 6 is movably connected with the sleeve 5, the whole structure is reasonably designed, the rotating motor 3 rotates, the support screw 4 is driven to rotate through the motor shaft, so that the sleeve 5 on the support screw 4 moves along the support screw 4, the sleeve 5 moves to drive the adjusting rod group 6 connected with the sleeve to rotate downwards, the other end of the adjusting rod group 6 is connected with the shunt baffle 7, the outer side end of the shunt baffle 7 is connected with the support 8 in a rotating mode, the adjusting rod group 6 can pull the shunt baffle 7 to rotate downwards synchronously, the shunt hole 9 is opened, the rotating angle and the rotating number of turns of the rotating motor 3 are controlled, the opening angle of the shunt hole 9 can be controlled, and the entering and removing speed of raw materials is strictly controlled.
Regulating stem group 6 includes locating lever 22 and movable rod 23, locating lever 22 and the adjustable connection of movable rod 23, be provided with the link 32 on the reposition of redundant personnel baffle 7, locating lever 22 rotates with link 32 to be connected, the outer wall of sleeve 5 is provided with card frame 33, the one end and the card frame 33 of movable rod 23 rotate to be connected, overall structure design benefit is reasonable, locating lever 22 and the combination of movable rod 23 form regulating stem group 6, and locating lever 22 and the adjustable connection of movable rod 23, can ensure that regulating stem group 6 can be according to the opening angle of reposition of redundant personnel baffle 7 and do the adaptability adjustment of length, and through link 32, regulating stem group 6 and reposition of redundant personnel baffle 7 can be convenient for in the design of card frame 33, installation between the sleeve 5, the dismouting of being convenient for.
An adjusting groove 24 with an opening at one end is arranged on the positioning rod 22, the movable rod 23 is movably clamped in the adjusting groove 24, both sides of the adjusting groove 24 are provided with a limiting groove 25, the movable rod 23 is provided with a limiting block 26, the limiting block 26 is matched with the limiting groove 25, the limiting block 26 is clamped in the limiting groove 25 in a limiting way, and the movable rod 23 is movably inserted and connected with the positioning rod 22 by matching with the adjusting groove 24, thereby changing the whole length of the adjusting rod group 6, leading the adjusting rod group 6 to be capable of carrying out adaptive length adjustment according to the rotation angle of the flow dividing baffle 7 and the moving position of the sleeve 5, thereby ensuring the normal rotation adjustment of the shunt baffle 7, and through the smart matching of the limiting groove 25 and the limiting block 26, can play further spacing guide effect for relative movement is more steady between movable rod 23 and the locating lever 22, ensures the overall structure of regulating lever group 6 reliable and firm performance.
The spraying discs 10 are provided with two groups, one side of each group of spraying discs 10, which is provided with the spray heads 11, is provided with a baffle component 27, each baffle component 27 comprises two arc-shaped baffle plates 28 and a mounting sleeve 29 which are symmetrical in the left and right, the arc-shaped baffle plates 28 are connected with the mounting sleeves 29, the mounting sleeves 29 are fixed on a main support rod 30, the design is reasonable, one group of baffle components 27 is arranged above each group of spraying discs 10, the baffle components 27 play a role of buffering, the impact force of raw materials on the spraying discs 10 is reduced, meanwhile, the flow paths of the raw materials can be changed through the two arc-shaped baffle plates 28 which are symmetrical in the left and right, so that the liquid raw materials flow downwards at multiple angles, meanwhile, the spray heads 11 spray water upwards and are mixed with the raw materials flowing downwards in a counter-flushing manner, and the raw materials are diffused at multiple angles due to the influence of the arc-shaped baffle plates 28, so that the raw materials are fully mixed and contacted with the water, effectively improve washing speed and washing quality for impurity clearance in the raw materials is higher, and baffling subassembly 27, spray tray 10 all set up on main tributary vaulting pole 30 moreover, support fixedly through main tributary vaulting pole 30, main tributary vaulting pole 30 again with wash tower 1 inside between the installation fixed, thereby effectively guarantee baffling subassembly 27, spray tray 10's installation fastness.
In the invention, the raw material 1,1,1,3, 3-pentachloropropane required by the preparation of 1-chloro-3, 3, 3-trifluoropropene is purified by removing impurities, catalyst components (metal solubilizer, hydrochloride of the metal solubilizer and the like) existing in the raw material 1,1,1,3, 3-pentachloropropane can influence the service life of the catalyst in the preparation process of 1-chloro-3, 3, 3-trifluoropropene, fluorination reaction and required devices in the preparation process of 1-chloro-3, 3, 3-trifluoropropene, but the invention removes impurities such as the metal solubilizer, the hydrochloride of the metal solubilizer and iron complex thereof in the 1,1,1,3, 3-pentachloropropane by circulating water washing for many times, controls the washing times of the water, ensures the washing effect and quality, and can enter the settling tower 17 after the washing times of the water reach the set requirements, through the standing precipitation of the precipitation tower 17, the water layer dissolving the catalyst component in the 1,1,1,3, 3-pentachloropropane and the 1,1,1,3, 3-pentachloropropane raw material are separated through standing, the bottom layer is 1,1,1,3, 3-pentachloropropane raw material solution with large density, the bottom layer 1,1,1,3, 3-pentachloropropane raw material solution is conveyed into the adsorption tower 19 for adsorption treatment, through the multiple adsorption treatment of the active carbon adsorption layer 20 and the molecular sieve adsorption layer 21, the residual moisture in the 1,1,1,3, 3-pentachloropropane raw material solution can be adsorbed, the impurities in the 1,1,1,3, 3-pentachloropropane can be further removed, the content of the catalyst impurity component in the 1,1,1,3, 3-pentachloropropane is reduced, the distillation treatment is carried out after the adsorption treatment, impurities and moisture in the 1,1,1,3, 3-pentachloropropane can be further evaporated and removed through distillation treatment, and the adsorbent carried by the 1,1,1,3, 3-pentachloropropane after adsorption treatment can be removed through evaporation, so that the purity of the finally obtained 1,1,1,3, 3-pentachloropropane raw material is improved, the content of the impurities in the 1,1,1,3, 3-pentachloropropane raw material is greatly reduced and controlled, and the problems of shortening of the service life of the catalyst, inhibiting of the fluorination reaction, corrosion of the device and the like in the 1-chloro-3, 3, 3-trifluoropropene reaction are avoided.
In the invention, the inlet and the outlet of the washing tower 1 are respectively provided with the flow dividing device 2, the opening angle of the flow dividing hole 9 at the inlet can be controlled by the flow dividing device 2 at the inlet according to the actual processing capacity and the washing processing speed of the raw materials, the flow dividing device 2 at the outlet can be matched with the design of the circulating pump 12 to ensure that the flow dividing hole 9 of the flow dividing device 2 at the outlet can be opened only after the raw materials reach a plurality of times of washing, so that the raw materials reaching the times of washing are output from the washing tower 1, the processing capacity of conveying the raw materials into the settling tower 17 can be controlled by controlling the angle and the closing time of the flow dividing hole 9 at the outlet, two groups of spraying discs 10 are arranged in the washing tower 1, the raw materials can realize twice washing spraying once through the washing tower through the two groups of spraying discs 10, and the raw materials flow downwards and the water is sprayed upwards, make raw materials and water counterpulsation contact, the intensive mixing, effectively improve washing speed, and every group sprays the top of dish 10 and has all set up baffling subassembly 27, the impact force of raw materials to spraying dish 10 can be slowed down through baffling subassembly 27, the life of dish 10 is sprayed in the extension, and because the impact of arc baffling board 28, make the flow path of raw materials take place the sudden change, the raw materials diffusion of splashing, continue down flow from many angles and direction, effectively improve the washing quality of raw materials, impurity content in the control raw materials, make the purity of raw materials higher.
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 (6)
- A process for producing 1-chloro-3, 3, 3-trifluoropropene, which comprises the steps of:a. pretreatment of 1,1,1,3, 3-pentachloropropane raw material:1) and (3) water washing treatment: the pretreatment device comprises a water washing tower, a settling tower and an adsorption tower which are sequentially arranged from left to right, the water washing tower, the settling tower and the adsorption tower are connected through a conveying pipe, a suction pump is arranged on the conveying pipe between the water washing tower and the settling tower, a conveying pump is arranged on the conveying pipe between the settling tower and the adsorption tower, a circulation port is arranged at the bottom of the water washing tower and is communicated with the top of the water washing tower through a circulation pipe, a circulation pump is arranged on the circulation pipe, a main support rod is arranged in the water washing tower and is fixedly connected with the inner wall of the water washing tower, flow dividing devices are arranged at two ends of the main support rod and are connected with a rotating motor, the rotating motor is fixedly connected with the end part of the main support rod through an auxiliary plate, and a spraying disc is arranged on the main support rod, the top surface of the spraying disc is uniformly provided with spray heads, the adsorption tower is internally provided with spoilers and adsorption layers which are distributed at intervals, and the adsorption layers comprise activated carbon adsorption layers and molecular sieve adsorption layers which are distributed at intervals;(1) the raw materials are pretreated through a pretreatment device, water washing treatment is firstly carried out, a flow dividing device close to the inlet of the top of a water washing tower is opened, a rotating motor rotates, the rotating motor drives a supporting screw rod to rotate through a motor shaft, and a sleeve on the supporting screw rod moves along the supporting screw rod;(2) the sleeve drives the adjusting rod group connected with the sleeve to move when moving, one end of the adjusting rod group is movably connected with the sleeve, the other end of the adjusting rod group is movably connected with one end of the shunting baffle, and the other end of the shunting baffle is rotatably connected with the bracket, so that the sleeve is ensured to drive the shunting baffle to rotate through the adjusting rod group, the shunting hole is opened, and the opening angle of the shunting hole is adjusted according to the processing amount and the processing requirement of the raw materials;(3) liquid raw materials are introduced into a washing tower, the raw materials enter from an inlet at the top of the washing tower, flow to a washing area from a flow distribution hole through the flow distribution of a flow distribution device, water is conveyed into two groups of spraying discs by a water pump and then is sprayed out from nozzles on the spraying discs, the water is sprayed upwards, the raw materials flow downwards, the water and the raw materials are mixed in a counter-flushing manner, and the raw materials entering the washing area are washed;(4) meanwhile, the circulating pump is started, the circulating pump conveys the washed raw materials into the circulating pipe from a circulating port, the raw materials are conveyed to the top of the washing tower through the circulating pipe and then enter the washing tower to be washed again, the circulating water is washed for 3-5 times, the circulating pump is closed, the suction pump is started, and meanwhile, the flow distribution device close to the bottom outlet of the washing tower is opened;2) standing and precipitating: the raw material treated by the water washing tower flows downwards through the diversion holes, enters the conveying pipe from the outlet at the bottom of the water washing tower, is conveyed into the settling tower through the suction pump for standing and settling treatment, after standing and settling for 2-10 hours, the water layer on the upper layer is pumped away, the conveying pump is opened, and the raw material solution on the lower layer enters the conveying pipe through the outlet at the bottom of the settling tower and is conveyed into the adsorption tower through the conveying pump;3) adsorption treatment: raw materials enter an adsorption zone through an inlet at the top of an adsorption tower, an adsorption layer is arranged in the adsorption tower, the adsorption layer comprises an activated carbon adsorption layer and a molecular sieve adsorption layer which are distributed at intervals, and the raw materials are discharged from an outlet at the bottom of the adsorption tower after adsorption treatment of the activated carbon adsorption layer and the molecular sieve adsorption layer; the adsorption tower is internally provided with a spoiler, the spoiler and the adsorption layer are distributed at intervals, and the spoiler is used for obstructing and disturbing raw materials, so that the raw materials are divided, mixed in a cross way and quickly diffused in an adsorption zone; 4) And (3) distillation treatment: conveying the raw materials subjected to adsorption treatment by the adsorption tower into a distillation kettle for further distillation treatment;b. fluorination reaction:1) introducing the liquid 1,1,1,3, 3-pentachloropropane raw material subjected to distillation treatment into a fluorination reaction kettle, and adding a catalyst into the fluorination reaction kettle at the same time;2) heating the fluorination reaction kettle, introducing anhydrous hydrogen fluoride into the fluorination reaction kettle after the temperature reaches 120-450 ℃, controlling the reaction pressure of the fluorination reaction kettle to be 0.08-5.5MPa, keeping for 2-5 hours, and finishing the reaction;c. and (3) purification treatment: and introducing the reacted product into a rectifying tower for rectification treatment, and then performing condensation reflux after rectification treatment to obtain a final finished product.
- 2. The process for producing 1-chloro-3, 3, 3-trifluoropropene according to claim 1, wherein: in the step c, in the rectification treatment process, the tail gas generated by rectification is subjected to centralized recovery treatment through a tail gas collection tower, and is discharged after the recovery treatment is qualified.
- 3. The process for producing 1-chloro-3, 3, 3-trifluoropropene according to claim 1, comprising: the shunting device comprises a support and a shunting baffle, a supporting screw is arranged at the center of the support, one end of the supporting screw is connected with the support through a shaft sleeve, the other end of the supporting screw is connected with a motor shaft of the rotating motor, a sleeve is sleeved on the supporting screw in a threaded manner, shunting holes are formed in the support, the shunting baffle is matched with the shunting holes, the shunting holes are shielded and sealed by the shunting baffle, the outer side end of the shunting baffle is rotatably connected with the support, the inner side end of the shunting baffle is connected with the sleeve through an adjusting rod group, one end of the adjusting rod group is movably connected with the shunting baffle, and the other end of the adjusting rod group is movably connected with the sleeve.
- 4. The process for producing 1-chloro-3, 3, 3-trifluoropropene according to claim 3, characterized by: the adjusting rod group comprises a positioning rod and a movable rod, the positioning rod is adjustably connected with the movable rod, a connecting frame is arranged on the shunting baffle, the positioning rod is rotatably connected with the connecting frame, a clamping frame is arranged on the outer wall of the sleeve, and one end of the movable rod is rotatably connected with the clamping frame.
- 5. The process for producing 1-chloro-3, 3, 3-trifluoropropene according to claim 4, wherein: the adjustable clamp is characterized in that an adjusting groove with an opening at one end is formed in the positioning rod, the movable rod is movably clamped in the adjusting groove, limiting grooves are formed in two sides of the adjusting groove, limiting blocks are arranged on the movable rod and are matched with the limiting grooves, and the limiting blocks are clamped in the limiting grooves.
- 6. The process for producing 1-chloro-3, 3, 3-trifluoropropene according to claim 1, wherein: the spraying disc is provided with two groups, one side of each spraying disc, which is provided with a spray head, is provided with a baffle assembly, the baffle assemblies comprise two arc-shaped baffle plates and an installation sleeve, the arc-shaped baffle plates are symmetrical in the left and right directions, the arc-shaped baffle plates are connected with the installation sleeve, and the installation sleeve is fixed on the main support rod.
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| US9045386B2 (en) * | 2010-02-18 | 2015-06-02 | Honeywell International Inc. | Integrated process and methods of producing (E)-1-chloro-3,3,3-trifluoropropene |
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