CN120169301B - Reaction separation equipment for preparing phosphorus oxytrifluoride - Google Patents
Reaction separation equipment for preparing phosphorus oxytrifluorideInfo
- Publication number
- CN120169301B CN120169301B CN202510655339.3A CN202510655339A CN120169301B CN 120169301 B CN120169301 B CN 120169301B CN 202510655339 A CN202510655339 A CN 202510655339A CN 120169301 B CN120169301 B CN 120169301B
- Authority
- CN
- China
- Prior art keywords
- heat exchange
- reaction
- exchange medium
- pipes
- tower body
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/24—Stationary reactors without moving elements inside
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/009—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping in combination with chemical reactions
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
- B01D3/32—Other features of fractionating columns ; Constructional details of fractionating columns not provided for in groups B01D3/16 - B01D3/30
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J10/00—Chemical processes in general for reacting liquid with gaseous media other than in the presence of solid particles, or apparatus specially adapted therefor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0006—Controlling or regulating processes
- B01J19/0013—Controlling the temperature of the process
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0053—Details of the reactor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J4/00—Feed or outlet devices; Feed or outlet control devices
- B01J4/001—Feed or outlet devices as such, e.g. feeding tubes
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/10—Halides or oxyhalides of phosphorus
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00051—Controlling the temperature
- B01J2219/00074—Controlling the temperature by indirect heating or cooling employing heat exchange fluids
- B01J2219/00076—Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements inside the reactor
- B01J2219/00081—Tubes
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Devices And Processes Conducted In The Presence Of Fluids And Solid Particles (AREA)
Abstract
本发明公开了一种三氟氧磷制备用反应分离设备，包括：反应分离塔体，所述反应分离塔体的下端往上依次设置有进料区、若干个反应区、以及分离区，所述进料区和分离区内固定填充有第一填料层，所述反应区内装填有第二填料层；换热机构，包含换热介质进入容器、换热介质排出容器，所述换热介质进入容器、以及换热介质排出容器的外围分别均布设置有若干个换热导管，所述换热导管之间分别纵向连接有预埋于所述第二填料层内的换热介质流通管；若干个换热介质进入管，出料端处分别向上转动安装有相应的驱动管件；若干个换热介质排出管。本发明能够有效提升各个反应区内的反应温度均匀性、以及确保物料在缓慢流通经过反应区时具有足够的均布效果。
The present invention discloses a reaction separation device for preparing phosphorus oxytrifluoride, comprising: a reaction separation tower body, wherein a feed zone, a plurality of reaction zones, and a separation zone are sequentially arranged from the lower end of the reaction separation tower body upward, wherein the feed zone and the separation zone are fixedly filled with a first packing layer, and the reaction zone is filled with a second packing layer; a heat exchange mechanism, comprising a heat exchange medium inlet container and a heat exchange medium outlet container, wherein the heat exchange medium inlet container and the heat exchange medium outlet container are respectively uniformly provided with a plurality of heat exchange pipes on the periphery thereof, wherein the heat exchange pipes are respectively longitudinally connected with a heat exchange medium circulation pipe pre-buried in the second packing layer; a plurality of heat exchange medium inlet pipes, wherein corresponding drive pipes are respectively installed at the discharge end thereof for rotating upward; and a plurality of heat exchange medium outlet pipes. The present invention can effectively improve the uniformity of the reaction temperature in each reaction zone and ensure that the material has a sufficiently uniform distribution effect when slowly flowing through the reaction zone.
Description
Technical Field
The invention relates to the field of industrial equipment for preparing phosphorus oxytrifluoride, in particular to reaction separation equipment for preparing phosphorus oxytrifluoride.
Background
At present, phosphorus oxytrifluoride (POF 3) is colorless and has a pungent odor gas in a normal state, and is weakly fuming in the air, and the preparation of the phosphorus oxytrifluoride (POF 3) mainly adopts the reaction of CaF 2 and anhydrous sulfurous acid to firstly generate CaF (SO 3 F) and then react with H 3PO4 to generate an intermediate product POF 3, but because the CaF 2 is solid, the continuous production is difficult, the process is complex, the production cost is high, and the generated CaSO 4 can pollute the environment and needs to be treated necessarily. Therefore, the preparation method of phosphorus trifluoride with higher purity by continuous reactive distillation using industrial phosphoric acid and anhydrous hydrogen fluoride as raw materials is studied and used.
In practical application, the method for preparing high-purity phosphorus oxyfluoride by continuous reactive distillation finds that the equipment for preparing phosphorus oxyfluoride is complicated due to the method of reaction before separation, and in the reactive distillation column, industrial phosphoric acid is liquid, anhydrous hydrogen fluoride is gas, and the industrial phosphoric acid and the anhydrous hydrogen fluoride are in contact with each other in the process of two phases through a column plate, so that the reaction between the industrial phosphoric acid and the anhydrous hydrogen fluoride is insufficient, and therefore, the cyclic reaction must be realized by controlling the reflux mode, thereby increasing the energy consumption of the production reaction. Therefore, in the actual production process, the inventor designs a trifluoro oxygen phosphorus reaction and separation integrated preparation tower (patent application number CN 202510154810.0) through research, which effectively solves the problem of insufficient contact in the reaction process between industrial phosphoric acid and anhydrous hydrogen fluoride, and can effectively separate out high-purity concentration trifluoro oxygen phosphorus, thereby reducing the energy consumption of trifluoro oxygen phosphorus production and reducing the production cost.
However, in the actual use process of the integrated preparation tower for the reaction and separation of the trifluoro oxygen phosphorus, as the heat exchange tubes of the shell and tube heat exchanger positioned in the reaction zone are uniformly distributed and fixed in position, the space between the heat exchange tubes is relatively large to ensure the filling convenience of the packing layer in the reaction zone, so that the temperature of the whole reaction zone can be kept only by increasing the temperature of the heat exchange medium, and the reaction temperature close to the position of the heat exchange tubes is higher, so that the uniformity of the reaction temperature of the whole reaction zone is insufficient, and adverse effects are caused to the reaction process. The cyclone distributor arranged at the lower part of each reaction zone improves the uniformly distributed effect of the reaction materials to a certain extent, but in order to ensure that the materials can reach better distribution effect when passing through the cyclone distributor, the pressure of the materials passing through the cyclone distributor is required to be higher, which is obviously unreasonable for the process of synthesizing the trifluoro-oxygen phosphorus.
Therefore, the design of the reaction separation equipment for preparing the phosphorus oxyfluoride can effectively and obviously improve the uniformity of the reaction temperature in each reaction zone, ensure that the materials can still have enough uniform distribution effect when slowly flowing through each reaction zone, and further effectively ensure the controllability of the reaction process and improve the reaction effect.
Disclosure of Invention
The invention aims at solving the technical problems in the prior art, and provides a reaction separation device for preparing phosphorus trifluoride, which can effectively solve the technical problems in the prior art.
The technical scheme of the invention is as follows:
A reaction separation apparatus for preparing phosphorus oxytrifluoride, comprising:
The reaction separation tower body, the lower end of the reaction separation tower body is provided with a feeding zone, a plurality of reaction zones and a separation zone in turn upwards, the feeding zone and the separation zone are respectively and fixedly filled with a corresponding first packing layer upwards through corresponding fixed supporting plates, and the reaction zone is respectively and upwards filled with a corresponding second packing layer through corresponding movable supporting plates;
the heat exchange mechanism comprises a heat exchange medium inlet container fixedly arranged at the center of the movable supporting plate and a heat exchange medium outlet container fixedly arranged at the upper side of the middle part of the second packing layer, wherein a plurality of corresponding heat exchange pipes are respectively and uniformly distributed outwards at equal angles on the peripheries of the heat exchange medium inlet container and the heat exchange medium outlet container, heat exchange medium runner pipes which are pre-buried in the second packing layer are respectively and longitudinally connected between the heat exchange pipes, and the heat exchange medium runner pipes which are connected to different heat exchange pipes are respectively arranged in a staggered mode;
The heat exchange medium inlet pipes penetrate through and extend to the inside of the reaction separation tower body respectively, the discharge ends of the heat exchange medium inlet pipes are respectively and upwards rotatably provided with corresponding driving pipe fittings, one ends of the driving pipe fittings, which are not connected with the heat exchange medium inlet pipes, movably penetrate through the movable supporting plates and are rotatably arranged at the centers of the corresponding heat exchange medium inlet containers, the discharge ends of the driving pipe fittings are horizontally and outwards inclined and folded and are arranged in a necking shape, and inclined teeth facing the discharge ends of the driving pipe fittings are respectively arranged on the positions, which are not connected with the heat exchange pipes, of the inner side walls of the heat exchange medium inlet containers;
The heat exchange medium discharge pipes respectively penetrate through and extend to the inside of the reaction separation tower body, and the feeding ends of the heat exchange medium discharge pipes are respectively rotatably installed at the centers of the corresponding heat exchange medium discharge containers.
The reaction separation tower body is fixedly connected with a plurality of main support convex edges which are respectively positioned at the lower side of the movable support plate, and corresponding first plane bearings are respectively assembled between the bottom of the movable support plate and the main support convex edges.
Auxiliary supporting convex edges which are arranged at intervals with the main supporting convex edges are fixedly connected to the reaction separation tower body at the lower side of the main supporting convex edges respectively, corresponding supporting frames are fixedly connected upwards to the auxiliary supporting convex edges through second plane bearings respectively, the driving pipe fitting penetrates through and is fixedly connected to the middle of each supporting frame, and a plurality of supporting balls with top ends propped against the bottom side of the movable supporting plate are arranged at the upper end of each supporting frame in a rolling mode.
The heat exchange medium enters the driving pipe fitting through the heat exchange medium inlet pipe and is horizontally and outwards sprayed outwards after being pressurized at the discharge end of the driving pipe fitting to form impact force on the inclined teeth on the inner side wall of the heat exchange medium entering the container, so that the heat exchange mechanism and the second packing layer are integrally driven to rotate, and the reaction force generated in the process of pressurizing and spraying the heat exchange medium along the discharge end of the driving pipe fitting drives the driving pipe fitting to rotate in the opposite direction to the rotation direction of the heat exchange mechanism and the second packing layer, so that the materials flowing through the dispersing guide plate are actively dispersed.
The heat exchange medium inlet pipe and the driving pipe fitting, the driving pipe fitting and the heat exchange medium inlet container and the heat exchange medium outlet pipe and the heat exchange medium outlet container are respectively connected in a rotating way through corresponding waterproof sealing bearings.
The reaction separation tower body is provided with an anhydrous hydrogen fluoride feeding port positioned at the bottom side of the feeding zone, the reaction separation tower body is also provided with an industrial phosphoric acid feeding port positioned at the upper side of the reaction zone, and the top of the reaction separation tower body is provided with a product discharge port for discharging the gas of the synthesized phosphorus oxytrifluoride.
And a liquid material re-distributor for uniformly distributing the industrial phosphoric acid materials is arranged at the lower side of the discharge end of the industrial phosphoric acid feed inlet.
The number of the reaction zones is two, wherein the reaction temperature of the reaction zone at the lower part is controlled to be 80-100 ℃, and the temperature of the reaction zone at the upper part is controlled to be 100-120 ℃.
The reaction separation tower body is provided with a structural redistributor at the upper part of the separation zone, and the reaction separation tower body is provided with a silk screen foam remover at the upper part of the structural redistributor.
The heat exchange device comprises a heat exchange medium discharge container, a heat exchange pipe, a heat exchange medium inlet pipe, a heat exchange medium outlet pipe, a heat exchange pipe, a plurality of corresponding water permeable holes, a photoelectric sensor, a flow adjustable pump and a discharge pump, wherein the discharge end of the heat exchange pipe is connected to the heat exchange medium discharge container in a manner of being inclined respectively, the inclination direction of the discharge end of the heat exchange pipe is opposite to that of a driving pipe, the discharge end of the heat exchange pipe is fixedly connected with a corresponding limiting ring plate respectively, the heat exchange pipe on the inner side of the limiting ring plate is fixedly connected with a corresponding fixing flange respectively, the corresponding water permeable ring plate is movably arranged on the outer side of the fixing flange through a connecting spring, a plurality of corresponding water permeable holes are uniformly distributed on the water permeable ring plate, the corresponding spray pipes are outwards arranged at the center of the water permeable ring plate in a hopper shape respectively, and the photoelectric sensor for detecting the rotation speed of a second filler layer is arranged in the reaction separation tower, and the heat exchange medium inlet pipe is connected to an external material source through the flow adjustable pump.
The invention has the advantages that:
1) The invention firstly carries out improved design on a heat exchange mechanism, which comprises a heat exchange medium inlet container fixedly arranged at the center of a movable supporting plate and a heat exchange medium outlet container fixedly arranged at the upper side of the middle part of a second packing layer, wherein the heat exchange medium inlet container is inserted into heat exchange medium circulation pipes arranged on different heat exchange pipes in a staggered way to realize uniform distribution circulation of the heat exchange medium, a driving pipe fitting is arranged at the feeding end of the heat exchange medium inlet pipe, one end of the driving pipe fitting, which is not connected with the heat exchange medium inlet pipe, is rotatably arranged at the center of the corresponding heat exchange medium inlet container, and the most main part is that the discharging end of the driving pipe fitting is horizontally and outwards inclined and is arranged in a necking shape, and simultaneously, inclined teeth facing the discharging end of the driving pipe fitting are respectively arranged on the inner side wall of the heat exchange medium inlet container.
During the reaction, the heat exchange medium enters the driving pipe fitting through the heat exchange medium inlet pipe, and is horizontally and outwards sprayed obliquely after being pressurized at the discharge end of the driving pipe fitting, so that impact force is formed on the inclined teeth on the inner side wall of the heat exchange medium entering container, and the heat exchange mechanism and the second packing layer are driven to rotate integrally, and the rotation is low-speed rotation. Therefore, a circulating heat source can be effectively circulated through the whole reaction zone, so that the uniformity of the reaction temperature in the reaction zone is greatly improved, and the controllability of the reaction process and the reaction effect are effectively improved. And the low-speed rotation can not only lead to excessive wall hanging phenomenon of the material, but also obviously increase the uniformly distributed effect of the material in the second filler layer so as to assist in improving the reaction effect of the material.
2) The invention further provides a reaction separation tower body with auxiliary support flanges fixedly connected with the lower side of the main support flanges respectively, the auxiliary support flanges are fixedly connected with corresponding support frames upwards through second planar bearings respectively, and a plurality of support balls with the top ends propped against the bottom side of the movable support plate are arranged at the upper ends of the support frames in a rolling way. Along with the rotation of the movable bearing plate, the support frame forms a track-fixed support on the bottom of the movable bearing plate, so that the support stability of the movable bearing plate is effectively maintained, and the practical effect of the invention is ensured.
3) The driving pipe fitting of the invention penetrates through and is fixedly connected to the middle part of the supporting frame, and a plurality of corresponding dispersion guide plates are respectively and fixedly connected to the supporting frame in an inclined way. During the reaction, the heat exchange medium drives the driving pipe fitting to form the rotation opposite to the rotation of the heat exchange mechanism and the second packing layer along the reaction force generated in the pressurizing and spraying process of the discharging end of the driving pipe fitting, so that the materials flowing through the dispersing guide plate are actively dispersed, the materials are ensured to still have enough uniform distribution effect in the slow circulation process of each reaction area, and the controllability of the reaction process is effectively further ensured and the reaction effect is improved.
4) The rotation driving of the heat exchange mechanism and the second packing layer and the reverse rotation driving of the supporting frame provided with the dispersion guide plates adopt the liquid thrust generated by the circulation of the heat exchange medium, and other power mechanisms are not required to be additionally arranged, so that the manufacturing cost and the operation and maintenance cost of the equipment can be effectively reduced.
5) The discharge ends of the heat exchange pipes connected to the heat exchange medium discharge container are respectively arranged in an inclined mode, the inclined direction of the discharge ends is opposite to that of the driving pipe fittings, the discharge ends of the heat exchange pipes are respectively fixedly connected with corresponding limiting ring plates, the heat exchange pipes on the inner sides of the limiting ring plates are respectively fixedly connected with corresponding fixing convex edges, the outer sides of the fixing convex edges are movably provided with corresponding permeable ring plates through connecting springs, a plurality of corresponding permeable holes are uniformly distributed on the permeable ring plates, and the centers of the permeable ring plates are respectively provided with corresponding jet pipes in a bucket shape outwards. Under the conventional condition, the heat exchange medium is output through the water permeable holes of the water permeable annular plate and the spray holes of the spray pipes, and when the photoelectric sensor detects that the rotating speed of the second packing layer in the reaction separation tower body is lower than a set value, the power of the flow-adjustable material pumping pump is increased to promote the flow quantity of the heat exchange medium, so that the circulation speed and the pressure of the heat exchange medium are promoted, the water permeable annular plate and the spray pipes are driven to push outwards and abut against the limiting annular plate, the water permeable holes on the water permeable annular plate are sealed, and jet flow is formed through the spray pipes, so that the rotating speed of the second packing layer in the reaction separation tower body is assisted to be promoted, and the practical effect of the invention is effectively promoted.
Drawings
Fig. 1 is a schematic structural view of the present invention.
Fig. 2 is a schematic structural view of a heat exchange mechanism.
FIG. 3 is a schematic view of the structure of the movable supporting plate mounted on the upper side of the main supporting flange.
Fig. 4 is a partial enlarged view of a portion a in fig. 3.
Fig. 5 is a schematic view showing a structure in which a heat exchange medium discharge pipe in the second embodiment is attached to a heat exchange medium discharge container.
Fig. 6 is a schematic structural diagram of a discharge end of a heat exchange conduit in the second embodiment.
In the drawing, a reaction separation tower body 1, a feeding area 101, a reaction area 102, a separation area 103, a fixed bearing plate 2, a first packing layer 3, a movable bearing plate 4, a second packing layer 5, a heat exchange mechanism 6, a heat exchange medium inlet container 601, a heat exchange medium outlet container 602, a heat exchange conduit 603, a heat exchange medium runner pipe 604, a heat exchange medium inlet pipe 7, a driving pipe fitting 8, helical teeth 9, a heat exchange medium outlet pipe 10, a main supporting flange 11, a first plane bearing 12, an auxiliary supporting flange 13, a second plane bearing 14, a supporting frame 15, supporting balls 16, a dispersing guide plate 17, a waterproof sealing bearing 18, an anhydrous hydrogen fluoride feed inlet 19, an industrial phosphoric acid feed inlet 20, a product outlet 21, a liquid material re-distributor 22, a structural re-distributor 23, a silk-screen foam remover 24, a waste outlet 25, a limiting ring plate 26, a fixed flange 27, a connecting spring 28, a water permeable ring plate 29 and a jet pipe 30 are shown.
Detailed Description
For the convenience of understanding by those skilled in the art, the structure of the present invention will now be described in further detail with reference to the accompanying drawings:
embodiment one:
referring to fig. 1 to 4, a reaction separation apparatus for preparing phosphorus oxytrifluoride comprises:
the reaction separation tower body 1, wherein a feeding area 101, a plurality of reaction areas 102 and a separation area 103 are sequentially arranged at the lower end of the reaction separation tower body 1 upwards, the feeding area 101 and the separation area 103 are respectively and fixedly filled with a corresponding first packing layer 3 upwards through a corresponding fixed supporting plate 2, and the reaction areas 102 are respectively and upwards filled with a corresponding second packing layer 5 through a corresponding movable supporting plate 4;
the heat exchange mechanism 6 comprises a heat exchange medium inlet container 601 fixedly arranged at the center of the movable supporting plate 4 and a heat exchange medium outlet container 602 fixedly arranged at the upper side of the middle part of the second packing layer 5, wherein a plurality of corresponding heat exchange pipes 603 are respectively and uniformly distributed outwards at equal angles on the peripheries of the heat exchange medium inlet container 601 and the heat exchange medium outlet container 602, heat exchange medium circulation pipes 604 pre-buried in the second packing layer 5 are respectively and longitudinally connected between the heat exchange pipes 603, and the heat exchange medium circulation pipes 604 connected to different heat exchange pipes 603 are respectively arranged in a staggered manner;
The heat exchange medium inlet pipes 7 respectively penetrate through and extend to the inside of the reaction separation tower body 1, the discharge ends of the heat exchange medium inlet pipes 7 are respectively and upwards rotatably provided with corresponding driving pipe fittings 8, one ends of the driving pipe fittings 8 which are not connected with the heat exchange medium inlet pipes 7 movably penetrate through the movable supporting plates 4 and are rotatably arranged at the centers of the corresponding heat exchange medium inlet containers 601, the discharge ends of the driving pipe fittings 7 are horizontally and outwards inclined and folded and are arranged in a necking shape, and inclined teeth 9 facing the discharge ends of the driving pipe fittings 8 are respectively arranged at positions of the inner side walls of the heat exchange medium inlet containers 601 which are not connected with the heat exchange pipes 603;
The heat exchange medium discharge pipes 10 respectively penetrate and extend into the reaction separation tower body 1, and the feeding ends of the heat exchange medium discharge pipes 10 are respectively rotatably installed at the centers of the corresponding heat exchange medium discharge containers 602.
The invention firstly carries out improved design on a heat exchange mechanism 6, which comprises a heat exchange medium inlet container 601 fixedly arranged at the center of a movable supporting plate 4 and a heat exchange medium outlet container 602 fixedly arranged at the upper side of the middle part of a second packing layer 5, wherein the heat exchange medium inlet container is uniformly distributed and circulated through a heat exchange conduit 603 and a heat exchange medium circulation pipe 604 arranged on different heat exchange conduits 603 in a staggered way, a driving pipe fitting 8 is arranged at the feeding end of the heat exchange medium inlet pipe 7, one end of the driving pipe fitting 8 which is not connected with the heat exchange medium inlet pipe 7 is rotatably arranged at the center of the corresponding heat exchange medium inlet container 601, and the most importantly, the discharging end of the driving pipe fitting 8 is horizontally and outwards folded and is arranged in a necking shape, and simultaneously, the inner side wall of the heat exchange medium inlet container 601 is respectively provided with a bevel gear 9 facing the discharging end of the driving pipe fitting. During reaction, the heat exchange medium enters the driving pipe fitting 8 through the heat exchange medium inlet pipe 7, and is horizontally and outwards sprayed obliquely after being pressurized at the discharge end of the driving pipe fitting 8, so that impact force is formed on the inclined teeth 9 on the inner side wall of the heat exchange medium entering container 601, and the heat exchange mechanism 6 and the second packing layer 5 are driven to rotate integrally, and the rotation is low-speed rotation. Therefore, the circulating heat source can be effectively circulated through the whole reaction zone 102, so that the uniformity of the reaction temperature in the reaction zone 102 is greatly improved, and the controllability of the reaction process and the reaction effect are effectively improved. And this low-speed rotation not only can not lead to the material to form excessive wall built-up phenomenon, but also can obviously increase the equipartition effect of material in second packing layer 5 to the reaction effect of supplementary promotion material.
A plurality of main support convex edges 11 which are respectively positioned at the lower side of the movable support plate 4 are fixedly connected on the reaction separation tower body 1, and corresponding first plane bearings 12 are respectively assembled between the bottom of the movable support plate 4 and the main support convex edges 11.
Auxiliary supporting convex edges 13 which are arranged at intervals with the main supporting convex edges 11 are fixedly connected to the reaction separation tower body 1 at the lower side of the main supporting convex edges 11 respectively, the auxiliary supporting convex edges 13 are fixedly connected with corresponding supporting frames 15 upwards through second plane bearings 14 respectively, the driving pipe fitting 8 penetrates through and is fixedly connected to the middle part of each supporting frame 15, and a plurality of supporting balls 16 with top ends abutting against the bottom side of the movable supporting plate 4 are arranged at the upper end part of each supporting frame 15 in a rolling mode.
The invention is characterized in that a main supporting convex edge 11 arranged on a reaction separation tower body 1 is matched with a first plane bearing 12 to form rotary installation on a movable supporting plate 4, so as to solve the problem of insufficient supporting stability caused by rotary installation of the movable supporting plate 4, auxiliary supporting convex edges 13 are fixedly connected to the reaction separation tower body 1 at the lower side of the main supporting convex edge 11 respectively, the auxiliary supporting convex edges 13 are fixedly connected with corresponding supporting frames 15 respectively and upwards through second plane bearings 14, and a plurality of supporting balls 16 with top ends propped against the bottom side of the movable supporting plate 4 are arranged at the upper end parts of the supporting frames 15 in a rolling way. Along with the rotation of the movable supporting plate 4, the supporting frame 15 forms a track-fixed support on the bottom of the movable supporting plate 4, so that the supporting stability of the movable supporting plate 4 is effectively maintained, and the practical effect of the invention is ensured.
The supporting frame 15 is respectively and fixedly connected with a plurality of corresponding dispersing guide plates 17 in an inclined way, during reaction, a heat exchange medium enters the driving pipe fitting 8 through the heat exchange medium inlet pipe 7 and is horizontally and outwards inclined and sprayed out after being pressurized at the discharge end of the driving pipe fitting 8, so that impact force is formed on the inclined teeth 9 on the inner side wall of the heat exchange medium inlet container 601, the heat exchange mechanism 6 and the second packing layer 5 are driven to integrally rotate, and the reaction force generated in the process of pressurizing and spraying the heat exchange medium along the discharge end of the driving pipe fitting 8 drives the driving pipe fitting 8 to rotate in the opposite direction to the rotation direction of the heat exchange mechanism 6 and the second packing layer 5, so that the materials flowing through the dispersing guide plates 17 are actively dispersed.
The driving pipe fitting 8 of the invention penetrates through and is fixedly connected to the middle part of the supporting frame 15, and a plurality of corresponding dispersion guide plates 17 are respectively and obliquely fixedly connected to the supporting frame 15. During reaction, the heat exchange medium drives the driving pipe fitting 8 to rotate in opposite directions with the heat exchange mechanism 6 and the second packing layer 5 along the reaction force generated in the pressurizing and spraying process of the discharging end of the driving pipe fitting 8, so that the materials flowing through the dispersing guide plate 17 are actively dispersed, the materials can still have enough uniform distribution effect when slowly flowing through each reaction area 102, and the controllability of the reaction process is effectively further ensured, and the reaction effect is improved.
The heat exchange medium inlet pipe 7 and the driving pipe fitting 8, the driving pipe fitting 8 and the heat exchange medium inlet container 601, and the heat exchange medium outlet pipe 10 and the heat exchange medium outlet container 602 are respectively connected in a rotating way through corresponding waterproof sealing bearings 18.
The rotation driving of the heat exchange mechanism 6 and the second packing layer 5 and the reverse rotation driving of the supporting frame 15 provided with the dispersion guide plates 17 adopt liquid thrust generated by heat exchange medium circulation, and other power mechanisms are not required to be additionally added, so that the manufacturing cost and the operation and maintenance cost of the equipment can be effectively reduced.
The reaction separation tower body 1 is provided with an anhydrous hydrogen fluoride feeding port 19 positioned at the bottom side of the feeding zone 101, the reaction separation tower body 1 is also provided with an industrial phosphoric acid feeding port 20 positioned at the upper side of the reaction zone 102, and the top of the reaction separation tower body 1 is provided with a product discharge port 21 for discharging the synthesized phosphorus oxyfluoride gas. The lower side of the discharge end of the industrial phosphoric acid feed inlet 20 is provided with a liquid material re-distributor 22 for uniformly distributing the industrial phosphoric acid materials. The number of the reaction zones 102 is two, wherein the reaction temperature of the reaction zone 102 at the lower part is controlled to be 80-100 ℃, and the temperature of the reaction zone 102 at the upper part is controlled to be 100-120 ℃.
In the reaction process, after industrial phosphoric acid is fed through the industrial phosphoric acid feed inlet 20, the industrial phosphoric acid is uniformly dispersed and fed into the reaction zone 102 positioned at the upper part under the action of the liquid material re-distributor 22, anhydrous hydrogen fluoride gas is fed through the anhydrous hydrogen fluoride feed inlet 19, and is actively dispersed and fed into the reaction zone 102 positioned at the lower part through the supporting frame 15 and the dispersing guide plate 17 which are rotatably arranged, the uniformly-arranged industrial phosphoric acid and the anhydrous hydrogen fluoride are fully contacted and reacted in the second packing layer 5 of the reaction zone 102, the generated phosphorus oxyfluoride gas after the reaction is fractionated through the first packing layer 3 on the separation zone 103 and then fed into the next procedure along the product discharge outlet 21, and redundant industrial phosphoric acid liquid and a small amount of generated side reaction liquid residues can be discharged and concentrated and collected regularly through the waste outlet 25 at the bottom of the reaction separation tower body 1.
The reaction separation tower 1 is provided with a structural redistributor 23 at the upper part of the separation area 103, and the reaction separation tower 1 is provided with a wire mesh foam remover 24 at the upper part of the structural redistributor 23.
The resistance and the path of the lifting gas of the trifluoro oxygen phosphorus are increased through the first packing layer 3 of the upper separation zone 103, so that the mist of the industrial phosphoric acid carried in the lifting gas of the trifluoro oxygen phosphorus is accumulated and absorbed through the contact of the surface of the first packing layer 3 and flows back into the reaction zone 102 after sedimentation, therefore, the mist separation of the trifluoro oxygen phosphorus and the carried industrial phosphoric acid can be well realized through the separation zone 103, the purity of the trifluoro oxygen phosphorus product is improved, the structural redistributor 23 and the wire mesh foam remover 24 are arranged at the upper part of the reaction separation tower body 1, the industrial phosphoric acid carried in the trifluoro oxygen phosphorus can be further removed through the wire mesh foam remover, and the captured mist and the generated liquid enter the separation zone 103 through the structural redistributor 22 to realize the gas-liquid separation.
Embodiment two:
Referring to fig. 5-6, the difference between this embodiment and the first embodiment is that the discharge ends of the heat exchange tubes 603 connected to the heat exchange medium discharge container 602 are respectively disposed in an inclined manner, the inclination direction of the discharge ends of the heat exchange tubes 603 is opposite to that of the driving tube 8, the discharge ends of the heat exchange tubes 603 are respectively and fixedly connected with corresponding stop collar plates 26, the heat exchange tubes 603 inside the stop collar plates 26 are respectively and fixedly connected with corresponding fixing flanges 27, the corresponding water permeable collar plates 29 are movably mounted on the outer sides of the fixing flanges 27 through connecting springs 28, a plurality of corresponding water permeable holes are uniformly distributed on the water permeable collar plates 29, corresponding jet pipes 30 are respectively disposed in the center of the water permeable collar plates 29 in a bucket shape outwards, photoelectric sensors (not identified) for detecting the rotation speed of the second filler layers 5 are disposed in the reaction separation tower body 1, and the heat exchange medium inlet pipes 7 are connected to an external material source through flow adjustable material pumps (not identified).
Conventionally, the heat exchange medium is output through the water permeable holes of the water permeable ring plate 29 and the spray holes of the spray pipes 30, and when the photoelectric sensor detects that the rotation speed of the second packing layer 5 in the reaction separation tower body 1 is lower than a set value, the power of the flow-adjustable pumping pump is increased to increase the flow rate of the heat exchange medium, so as to increase the circulation speed and pressure of the heat exchange medium, drive the water permeable ring plate 29 and the spray pipes 30 to push out outwards and abut against the limiting ring plate 26, so that the water permeable holes on the water permeable ring plate 29 are closed, and jet flow is formed through the spray pipes 30, so that the rotation speed of the second packing layer 5 in the reaction separation tower body 1 is increased in an auxiliary manner, and the practical effect of the invention is effectively improved.
It should be noted that the implementation principle and the technical effects of the present embodiment are the same as those of the first embodiment, and for brevity, reference may be made to the corresponding content of the first embodiment.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
Claims (10)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202510655339.3A CN120169301B (en) | 2025-05-21 | 2025-05-21 | Reaction separation equipment for preparing phosphorus oxytrifluoride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202510655339.3A CN120169301B (en) | 2025-05-21 | 2025-05-21 | Reaction separation equipment for preparing phosphorus oxytrifluoride |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN120169301A CN120169301A (en) | 2025-06-20 |
| CN120169301B true CN120169301B (en) | 2025-08-05 |
Family
ID=96036329
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202510655339.3A Active CN120169301B (en) | 2025-05-21 | 2025-05-21 | Reaction separation equipment for preparing phosphorus oxytrifluoride |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN120169301B (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110743470A (en) * | 2019-10-31 | 2020-02-04 | 河北美邦工程科技股份有限公司 | Gas-liquid phase chloroethylene production device and process |
| CN117654419A (en) * | 2024-02-02 | 2024-03-08 | 福建省巨颖高能新材料有限公司 | Reaction equipment for preparing nitro compound by fluorination process and synthesis method |
Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101396647B (en) * | 2007-09-29 | 2011-03-16 | 中科合成油技术有限公司 | Gas-liquid-solid three-phase suspended bed reactor for f-t synthesis and use thereof |
| CN110201624A (en) * | 2019-07-09 | 2019-09-06 | 青岛科技大学 | A kind of contiguous segmentation charging reactor for synthetic reaction |
| CN111111566A (en) * | 2019-12-27 | 2020-05-08 | 江苏奥克化学有限公司 | Packed tower reactor for producing cyclic carbonate and production method |
| CN219559622U (en) * | 2023-07-18 | 2023-08-22 | 成都新晨新材科技有限公司 | Stirred reactor for poly(p-phenylenebenzobisoxazole-polyphosphoric acid) system |
| CN119608050B (en) * | 2025-02-12 | 2025-05-23 | 福建省德旭新材料有限公司 | Trifluoro oxygen phosphorus reaction and separation integral type preparation tower |
| CN120172369B (en) * | 2025-05-21 | 2025-08-08 | 福建省德旭新材料有限公司 | A method for preparing phosphorus oxyfluoride based on reaction separation equipment |
-
2025
- 2025-05-21 CN CN202510655339.3A patent/CN120169301B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110743470A (en) * | 2019-10-31 | 2020-02-04 | 河北美邦工程科技股份有限公司 | Gas-liquid phase chloroethylene production device and process |
| CN117654419A (en) * | 2024-02-02 | 2024-03-08 | 福建省巨颖高能新材料有限公司 | Reaction equipment for preparing nitro compound by fluorination process and synthesis method |
Also Published As
| Publication number | Publication date |
|---|---|
| CN120169301A (en) | 2025-06-20 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN120172369B (en) | A method for preparing phosphorus oxyfluoride based on reaction separation equipment | |
| CN106430108A (en) | System and method for preparing hydrogen peroxide through anthraquinone method under supergravity condition | |
| CN120169301B (en) | Reaction separation equipment for preparing phosphorus oxytrifluoride | |
| CN107469376A (en) | A kind of energy-efficient chemical separating bubble column | |
| CN207493242U (en) | One kind can make the equally distributed rectifying column of liquid | |
| CN109621467A (en) | A kind of direct discharging structure of crystal salt waste evaporator plant | |
| CN219580231U (en) | Falling film absorber | |
| CN108261792A (en) | Novel air dynamic formula stirs catalytic distillation device | |
| CN105195064B (en) | Improved reaction separation synchronous reactor | |
| CN220779058U (en) | A continuous distillation tower | |
| CN115869890B (en) | Continuous production equipment and method for triethyl phosphate | |
| CN215996680U (en) | Plate-type axial reactor | |
| CN203408489U (en) | Hypergravity rotating packed bed device for rectification | |
| CN206951203U (en) | A kind of high performance water reducing agent of polyocarboxy acid reactor | |
| CN113559676A (en) | A kind of liquid inlet structure of falling film absorption tower for chemical production, absorption tower and operation method | |
| CN102240459A (en) | Solution concentrator unit | |
| CN210145535U (en) | Accurate separator of pyridine chloride | |
| CN114805086A (en) | Process and system for producing diphenylamine by adopting aniline continuous condensation method | |
| CN223555529U (en) | An enzyme distillation extraction device | |
| CN202179861U (en) | Solution concentrating unit | |
| CN201179356Y (en) | High-efficiency rotary rectification bed | |
| CN201161929Y (en) | Energy conservation humidification roller | |
| CN212916913U (en) | Condensate recovery device for packed tower | |
| CN120022689B (en) | A dust removal spray column for adjustable explosion-proof spraying system | |
| CN220460307U (en) | Acetylene gas purifying system |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |