Rapid preparation and production device for phosphorus oxychloride reaction

Abstract

The invention discloses a rapid preparation production device for phosphorus oxychloride reaction, belongs to the technical field of phosphorus oxychloride reaction preparation, and aims to solve the problems that a large amount of hydrogen chloride is generated in the existing phosphorus oxychloride preparation process, the interior of a reaction kettle is corroded, and a large amount of gas is possibly generated in the heating process to cause explosion. Through separated arrangement of the heating mechanism and the reaction mechanism, heated phosphorus trichloride can react with oxygen to generate phosphorus oxychloride, the interior of the ceramic liner reactor is made of a ceramic material, corrosion of hydrogen chloride in side reaction to the reaction mechanism is prevented, and the phosphorus trichloride can be in full contact with the oxygen through blowing, so that the phosphorus oxychloride can be fully reacted with the oxygen; the cooling mechanism and the recycling mechanism are arranged in a matched mode, heating and reaction of the heating mechanism and the reaction mechanism are carried out separately, the pressure in the heating mechanism is prevented from rising, a collecting box at the lower end of the reaction mechanism receives reactants, and the cooling mechanism is used for cooling waste gas and converting the gas state into the liquid state to collect waste materials; and explosion is prevented.

Description

Technical Field

[0001] The invention relates to the technical field of phosphorus oxychloride reaction preparation, in particular to a rapid preparation production device for phosphorus oxychloride reaction. Background Art

[0002] Phosphorus oxychloride is an inorganic compound with the chemical formula POC l 3. In organic synthesis, phosphorus oxychloride is often used as a chlorinating agent, a phosphorylating agent, a dehydrating agent for amides, and a halogenating agent for alcohols, phenols, and heterocycles.

[0003] A reactor for preparing phosphorus oxychloride with the authorization announcement number CN220969130U comprises a reactor body, an oxygen supply pipe is installed on the upper side wall plate of the reactor body, one end of the oxygen supply pipe is placed on the upper end of the reactor body, the other end of the oxygen supply pipe is placed in the reactor body, one end of the oxygen supply pipe placed in the reactor body is fixedly connected to an oxygen distributor body, a homogenizing chamber is arranged in the oxygen distributor body, a flow-equalizing shell is fixedly connected to the inner side of the upper side wall plate of the oxygen distributor body, an air inlet is opened on the upper side wall plate of the oxygen distributor body, and oxygen is distributed in the oxygen distributor body by setting the oxygen distributor. After the uniform flow in the reactor, it is sprayed out through a nozzle, so that the oxygen is evenly distributed in the reactor, and the distributor is arranged at the lower part of the reactor, which increases the contact time between oxygen and liquid phosphorus trichloride, so that oxygen and phosphorus trichloride are in full contact, shortening the preparation time of phosphorus oxychloride, thereby improving the preparation efficiency. However, this phosphorus oxychloride preparation directly heats phosphorus trichloride and oxygen at high temperature to generate phosphorus oxychloride. Although the operation is simple, it has high requirements on equipment and may generate a large amount of hydrogen chloride, which may corrode the inside of the reactor. In addition, a large amount of gas may be generated during the heating process, resulting in increased pressure, which may cause accidents such as explosions.

[0004] To solve the above problems, a rapid preparation and production device for phosphorus oxychloride reaction is proposed. Summary of the invention

[0005] The purpose of the present invention is to provide a rapid preparation and production device for phosphorus oxychloride reaction, which solves the problem that the existing phosphorus oxychloride preparation in the background technology directly heats phosphorus trichloride and oxygen at high temperature to generate phosphorus oxychloride. Although the operation is simple, it has high requirements on equipment, may generate a large amount of hydrogen chloride, which may corrode the inside of the reactor, and may generate a large amount of gas during the heating process, resulting in increased pressure, which may cause accidents such as explosions.

[0006] To achieve the above-mentioned purpose, the present invention provides the following technical solutions: a rapid preparation and production device for phosphorus oxychloride reaction, comprising a heating mechanism for heating, one side of the heating mechanism is connected to a reaction mechanism for reaction, one side of the reaction mechanism is connected to a cooling mechanism for cooling, the output end of the cooling mechanism is connected to a recovery mechanism for recovering raw materials, the heating mechanism comprises an insulating outer frame, a heating component arranged at the bottom and inside of the insulating outer frame, the reaction mechanism comprises a ceramic liner reactor connected to the output end of the insulating outer frame, a driving motor rotatably arranged inside the ceramic liner reactor, the lower end of the reaction mechanism is connected to a collecting box, the cooling mechanism comprises a cooling component arranged at the output end of the ceramic liner reactor, and the recovery mechanism is arranged at the output end of the cooling component.

[0007] Furthermore, the heating mechanism also includes a side cover rotatably arranged on one side of the heat-insulating outer frame, a sealing member connected to the upper end of the heat-insulating outer frame, a rotating rod rotatably arranged on one end of the sealing member, and a sealing cover is fixed to the lower end of the rotating rod.

[0008] Furthermore, an inner frame is arranged inside the heat-insulating outer frame, and an external transport pipe is fixed to one side of the inner frame.

[0009] Furthermore, a phosphorus oxychloride input pipe connected to an external transmission pipe is provided on one side of the ceramic liner reactor.

[0010] Furthermore, the heating assembly includes an electromagnetic heating element fixed to the lower end of the heat-insulating outer frame, a heating base plate is provided at the upper end of the electromagnetic heating element, and a heating wire is connected to one side of the electromagnetic heating element through an electric wire.

[0011] Furthermore, the reaction mechanism also includes a three-way pipe fixed at the lower end of the ceramic liner reactor, and a bottom column arranged at the lower end of the collecting box, and a sleeve ring is surrounded between the three-way pipe and the collecting box.

[0012] Furthermore, an oxygen input pipe is provided on one side of the ceramic liner reactor, a rotating fan is connected to the output end of the driving motor, and a first sleeve nut is rotatably connected to one end of the sleeve ring.

[0013] Furthermore, the cooling mechanism also includes an exhaust gas output pipe arranged on one side of the three-way pipe, one side of the exhaust gas output pipe is connected to three groups of connecting pipes that are perpendicular to each other, a rotary switch is fixedly provided at the center of the connecting pipe, a bent pipe is connected between two groups of parallel connecting pipes, and the cooling assembly is surrounded on the outside of the bent pipe.

[0014] Furthermore, the cooling assembly includes two groups of side plates, a plurality of groups of heat sinks are arranged side by side between the two groups of side plates, and the second sleeve nuts are arranged on both sides of the side plates for fixing the heat sinks.

[0015] Furthermore, the recovery mechanism comprises a recovery box connected to the output ends of the two groups of connecting pipes, and an opening and closing pipe is provided on one side of the recovery box.

[0016] Compared with the prior art, the present invention has the following beneficial effects:

[0017] 1. The invention provides a rapid preparation and production device for phosphorus oxychloride reaction. The heating mechanism and the reaction mechanism are separately arranged. The heating component heats the phosphorus trichloride inside the heat-insulating outer frame. The smoke generated by the phosphorus trichloride is discharged into the interior of the ceramic inner liner reactor. Oxygen is input at one end of the ceramic inner liner reactor. At this time, the phosphorus trichloride heated in the ceramic inner liner reactor reacts with oxygen to generate phosphorus oxychloride. The interior of the ceramic inner liner reactor is made of ceramic material to prevent hydrogen chloride in the side reaction from corroding the reaction mechanism. The driving motor blows air upward so that the phosphorus trichloride can be fully in contact with oxygen, and the generation of side reactions can also be reduced. The existing phosphorus oxychloride preparation is solved by directly heating phosphorus trichloride and oxygen at high temperature to generate phosphorus oxychloride. Although the operation is simple, the equipment requirements are high and a large amount of hydrogen chloride may be generated, which may corrode the inside of the reactor.

[0018] 2. The present invention provides a rapid preparation and production device for phosphorus oxychloride reaction. Through the combination of a cooling mechanism and a recovery mechanism, a collection box at the lower end of the reaction mechanism receives the reactants, and the cooling mechanism is used to cool the exhaust gas and convert the gaseous state into a liquid state for waste collection to prevent explosions. This solves the problem that a large amount of gas may be generated during the heating process of the existing phosphorus oxychloride preparation, resulting in increased pressure and possible accidents such as explosions. BRIEF DESCRIPTION OF THE DRAWINGS

[0019] Figure 1 The overall structure of the present invention is shown in FIG. Figure 1 ;

[0020] Figure 2 The overall structure of the present invention is shown in FIG. Figure 2 ;

[0021] Figure 3 It is a structural schematic diagram of the heating mechanism of the present invention;

[0022] Figure 4 It is a schematic diagram of the split structure of the heating mechanism of the present invention;

[0023] Figure 5 It is a schematic diagram of the structure of the reaction mechanism, cooling mechanism and recovery mechanism of the present invention;

[0024] Figure 6 It is a schematic diagram of the split structure of the cooling mechanism of the present invention;

[0025] Figure 7 It is a structural schematic diagram of the recovery mechanism of the present invention.

[0026] In the figure: 1. heating mechanism; 11. heat-insulating outer frame; 111. inner frame; 112. external transmission pipe; 12. side cover; 13. sealing member; 131. rotating rod; 132. sealing cover; 14. heating assembly; 141. electromagnetic heating member; 142. heating bottom plate; 143. heating wire; 2. reaction mechanism; 21. ceramic liner reactor; 211. phosphorus oxychloride input pipe; 212. oxygen input pipe; 22. driving motor; 221. rotating fan; 23. three-way pipe; 24. collecting box; 25. bottom column; 26. sleeve ring; 261. first sleeve nut; 3. cooling mechanism; 31. exhaust gas output pipe; 32. connecting pipe; 33. rotating switch; 34. cooling assembly; 341. side plate; 342. second sleeve nut; 343. heat sink; 35. elbow; 4. recovery mechanism; 41. recovery box; 42. opening and closing pipe. DETAILED DESCRIPTION

[0027] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0028] In order to solve existing technical problems, such as Figure 1 As shown, the following preferred technical solutions are provided:

[0029] A rapid preparation and production device for phosphorus oxychloride reaction, comprising a heating mechanism 1 for heating, a reaction mechanism 2 for reaction connected to one side of the heating mechanism 1, a cooling mechanism 3 for cooling connected to one side of the reaction mechanism 2, a recovery mechanism 4 for recovering raw materials connected to the output end of the cooling mechanism 3, the heating mechanism 1 comprising a heat-insulating outer frame 11, a heating component 14 arranged at the bottom and inside of the heat-insulating outer frame 11, the reaction mechanism 2 comprising a ceramic liner reactor 21 connected to the output end of the heat-insulating outer frame 11, a driving motor 22 rotatably arranged inside the ceramic liner reactor 21, a collecting box 24 connected to the lower end of the reaction mechanism 2, the cooling mechanism 3 comprising a cooling component 34 arranged in communication with the output end of the ceramic liner reactor 21, and the recovery mechanism 4 arranged at the output end of the cooling component 34. The outer shell of the heat-insulating outer frame 11 is used for heat insulation. The heating component 14 heats the phosphorus trichloride inside the heat-insulating outer frame 11. The boiling point of phosphorus trichloride is 76.1°C. When the heating component 14 is heated to above 76.1°C, the smoke generated by the phosphorus trichloride will be discharged into the ceramic inner liner reactor 21. Oxygen is input at one end of the ceramic inner liner reactor 21. At this time, the heated phosphorus trichloride in the ceramic inner liner reactor 21 will react with oxygen to generate phosphorus oxychloride. The interior of the ceramic inner liner reactor 21 is made of ceramic material to prevent the hydrogen chloride in the side reaction from corroding the reaction mechanism 2. The driving motor 22 blows air upward so that the phosphorus trichloride can fully contact with oxygen and also reduce the occurrence of side reactions. The heating mechanism 1 and the reaction mechanism 2 are heated and reacted separately, which can prevent the pressure in the heating mechanism 1 from increasing. The collecting box 24 at the lower end of the reaction mechanism 2 receives the reactants. The cooling mechanism 3 is used to cool the exhaust gas, convert the gaseous state into a liquid state for waste collection, and prevent explosions.

[0030] Embodiment 1:

[0031] Combination Figure 2-Figure 6 The heating mechanism 1 also includes a side cover 12 rotatably arranged on one side of the heat-insulating outer frame 11, a sealing member 13 connected to the upper end of the heat-insulating outer frame 11, a rotating rod 131 is rotatably arranged at one end of the sealing member 13, a sealing cover 132 is fixed at the lower end of the rotating rod 131, the side cover 12 is used for observing and processing the heating component 14, the sealing cover 132 is used for closing the box body to prevent phosphorus trichloride from overflowing, and the setting of the rotating rod 131 allows the sealing cover 132 to be rotatably opened.

[0032] An inner frame 111 is arranged inside the heat-insulating outer frame 11 , an external transport pipe 112 is fixed to one side of the inner frame 111 , and phosphorus trichloride is built in the inner frame 111 and is transported through the external transport pipe 112 after being heated.

[0033] A phosphorus oxychloride input pipe 211 connected to an external transmission pipe 112 is provided on one side of the ceramic inner liner reactor 21 . The external transmission pipe 112 is connected to the phosphorus oxychloride input pipe 211 to realize the transportation of phosphorus trichloride into the ceramic inner liner reactor 21 .

[0034] The heating assembly 14 includes an electromagnetic heating element 141 fixed at the lower end of the insulation outer frame 11, a heating base plate 142 is arranged at the upper end of the electromagnetic heating element 141, a heating wire 143 is connected to one side of the electromagnetic heating element 141 through an electric wire, the electromagnetic heating element 141 provides heat for the heating base plate 142, the heating wire 143 is energized to generate heat, and the outer wall is heated. The synchronous heating of the lower end and the outer wall can balance the heating effect and improve the heating efficiency.

[0035] The reaction mechanism 2 also includes a three-way pipe 23 fixed at the lower end of the ceramic liner reactor 21, a bottom column 25 arranged at the lower end of the collecting box 24, a sleeve ring 26 is surrounded between the three-way pipe 23 and the collecting box 24, the three-way pipe 23 is arranged at the lower end of the ceramic liner reactor 21, and the collecting box 24 is connected to the lower end of the ceramic liner reactor 21 through the three-way pipe 23. The generated phosphorus oxychloride directly enters the collecting box 24. The bottom column 25 is used to place the collecting box 24, and the sleeve ring 26 is used to close the three-way pipe 23 and the collecting box 24.

[0036] An oxygen input pipe 212 is provided on one side of the ceramic liner reactor 21, and a rotary fan 221 is connected to the output end of the driving motor 22. One end of the sleeve ring 26 is rotatably connected to a first sleeve nut 261. The rotary fan 221 is used to blow air upward so that the phosphorus trichloride input by the phosphorus oxychloride input pipe 211 and the oxygen input by the oxygen input pipe 212 can fully react. The first sleeve nut 261 is used to fix the sleeve ring 26, lock the collection box 24 and the three-way pipe 23, so that the collection box 24 can be disassembled.

[0037] Embodiment 2:

[0038] Combination Figure 5-Figure 7 The cooling mechanism 3 also includes an exhaust gas output pipe 31 arranged on one side of the three-way pipe 23. One side of the exhaust gas output pipe 31 is connected with three groups of connecting pipes 32 which are perpendicular to each other. A rotary switch 33 is fixedly arranged at the center of the connecting pipe 32. A bend pipe 35 is connected between two groups of parallel connecting pipes 32. The cooling component 34 is surrounded on the outside of the bend pipe 35. The exhaust gas output pipe 31 is bent upward so that the exhaust gas can be discharged through the exhaust gas output pipe 31. A bend pipe 35 is connected between two groups of parallel connecting pipes 32. The cooling component 34 on the outside of the bend pipe 35 cools down the exhaust gas. The setting of the rotary switch 33 can control the output channel of the exhaust gas and determine whether to pass through the cooling component 34.

[0039] The cooling assembly 34 includes two groups of side panels 341, and multiple groups of heat sinks 343 are arranged side by side between the two groups of side panels 341. The second sleeve nuts 342 are arranged on both sides of the side panels 341 to fix the heat sinks 343. The bent pipe 35 passes through the heat sink 343. The heat sink 343 realizes heat dissipation and cooling for the bent pipe 35. The side panels 341 and the second sleeve nuts 342 are matched to lock the heat sink 343.

[0040] The recovery mechanism 4 includes a recovery box 41 connected to the output ends of the two groups of connecting pipes 32. An opening and closing pipe 42 is provided on one side of the recovery box 41. The recovery box 41 is used to collect waste gas. The opening and closing pipe 42 can be opened to clean the recovery box 41.

[0041] It should be noted that, in this article, relational terms such as first and second, etc. are only used to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Moreover, the terms "include", "comprise" or any other variants thereof are intended to cover non-exclusive inclusion, so that a process, method, article or device including a series of elements includes not only those elements, but also other elements not explicitly listed, or also includes elements inherent to such process, method, article or device.

[0042] The above description is only a preferred specific implementation manner of the present invention, but the protection scope of the present invention is not limited thereto. Any technician familiar with the technical field can make equivalent replacements or changes according to the technical scheme and inventive concept of the present invention within the technical scope disclosed by the present invention, which should be covered by the protection scope of the present invention.

Claims

1. A rapid production device for phosphorus oxychloride reaction, comprising a heating mechanism (1) for heating, characterized in that: One side of the heating mechanism (1) is connected to a reaction mechanism (2) for reaction, one side of the reaction mechanism (2) is connected to a cooling mechanism (3) for temperature reduction, and the output end of the cooling mechanism (3) is connected to a recovery mechanism (4) for recovering raw materials; The heating mechanism (1) comprises a heat-insulating outer frame (11), a heating component (14) arranged at the bottom and inside of the heat-insulating outer frame (11), the reaction mechanism (2) comprises a ceramic inner liner reactor (21) connected to the output end of the heat-insulating outer frame (11), and a drive motor (22) arranged inside the ceramic inner liner reactor (21) for rotation, the lower end of the reaction mechanism (2) is connected to a collecting box (24), the cooling mechanism (3) comprises a cooling component (34) arranged in communication with the output end of the ceramic inner liner reactor (21), and the recovery mechanism (4) is arranged at the output end of the cooling component (34).

2. A rapid preparation production device for phosphorus oxychloride reaction as claimed in claim 1, characterized in that: The heating mechanism (1) further comprises a side cover (12) rotatably arranged on one side of the heat-insulating outer frame (11), a sealing member (13) connected to the upper end of the heat-insulating outer frame (11), a rotating rod (131) rotatably arranged at one end of the sealing member (13), and a sealing cover (132) fixed to the lower end of the rotating rod (131).

3. A rapid preparation production device for phosphorus oxychloride reaction as claimed in claim 1, characterized in that: An inner frame (111) is arranged inside the heat-insulating outer frame (11), and an external transport pipe (112) is fixed to one side of the inner frame (111).

4. A rapid preparation production device for phosphorus oxychloride reaction as claimed in claim 2, characterized in that: A phosphorus oxychloride input pipe (211) connected to an external transmission pipe (112) is provided on one side of the ceramic liner reactor (21).

5. A rapid preparation production device for phosphorus oxychloride reaction as claimed in claim 1, characterized in that: The heating assembly (14) comprises an electromagnetic heating element (141) fixed at the lower end of the heat-insulating outer frame (11); a heating base plate (142) is provided at the upper end of the electromagnetic heating element (141); and a heating wire (143) is connected to one side of the electromagnetic heating element (141) via an electric wire.

6. A rapid preparation production device for phosphorus oxychloride reaction as claimed in claim 1, characterized in that: The reaction mechanism (2) further comprises a three-way pipe (23) fixed at the lower end of the ceramic liner reactor (21), a bottom column (25) arranged at the lower end of the collection box (24), and a sleeve ring (26) is surrounded between the three-way pipe (23) and the collection box (24).

7. A rapid preparation production device for phosphorus oxychloride reaction as claimed in claim 1, characterized in that: An oxygen input pipe (212) is provided on one side of the ceramic liner reactor (21), a rotating fan (221) is connected to the output end of the driving motor (22), and a first sleeve nut (261) is rotatably connected to one end of the sleeve ring (26).

8. A rapid preparation production device for phosphorus oxychloride reaction as claimed in claim 6, characterized in that: The cooling mechanism (3) further comprises an exhaust gas output pipe (31) arranged on one side of the three-way pipe (23); one side of the exhaust gas output pipe (31) is connected to three groups of mutually perpendicular connecting pipes (32); a rotary switch (33) is fixedly arranged at the center of the connecting pipe (32); a bent pipe (35) is connected between two groups of parallel connecting pipes (32); and the cooling assembly (34) is surrounded on the outside of the bent pipe (35).

9. A rapid preparation production device for phosphorus oxychloride reaction as claimed in claim 1, characterized in that: The cooling assembly (34) comprises two groups of side plates (341), a plurality of groups of heat sinks (343) are arranged side by side between the two groups of side plates (341), and the second sleeve nuts (342) are arranged on both sides of the side plates (341) for fixing the heat sinks (343).

10. A rapid preparation production device for phosphorus oxychloride reaction as claimed in claim 8, characterized in that: The recovery mechanism (4) comprises a recovery box (41) connected to the output ends of the two groups of connecting tubes (32), and an opening and closing tube (42) is provided on one side of the recovery box (41).

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