Preparation device and preparation process of sodium O-ethyl phosphonate

Abstract

The preparation device comprises a reaction kettle, a kettle cover is arranged at the upper end of the reaction kettle, a driving part is arranged on the kettle cover, a stirring structure extending into the reaction kettle is arranged at the output end of the driving part, an injection opening I for injecting triethyl phosphate is formed in the upper end of the kettle cover, and a rotating part fixed with the driving part is arranged in the kettle cover; a plurality of exchange grooves are formed in the rotating part, interlayers slide in the exchange grooves, and the upper ends and the lower ends of the interlayers are respectively supported by triethyl phosphite and gas in the reaction kettle to keep balance. Compared with the prior art, the device has the advantages that the interlayer is driven to displace through pressure change caused by toxic gas generated in the reaction kettle, the feeding amount of triethyl phosphite is dynamically changed, and when the reaction kettle reacts violently and the gas pressure is increased, the feeding amount is automatically reduced, the hydrogen phosphide generation rate is reduced from the source, and the yield of hydrogen phosphide is increased. The gas quantity is always within the treatment capacity range of the purification system, and the leakage risk of highly toxic gas is avoided.

Description

Technical Field

[0001] The present invention relates to the technical field of preparation of sodium O-ethylphosphonate, in particular to a preparation device and a preparation process of sodium O-ethylphosphonate. Background Art

[0002] Sodium O-ethylphosphonate is essentially an organophosphorus compound, with an ethyl group attached to the phosphorus via an oxygen. The phosphorus also has three oxygen atoms, two of which carry sodium ions. Its primary use is as a powerful descaling or antiscaling agent, a core component in systems such as boiler water treatment, industrial cooling water, and reverse osmosis membranes to prevent scale formation. It also serves as a corrosion inhibitor, forming a protective film on metal surfaces to slow rust and corrosion. It also acts as a dispersant, dispersing small particles already formed in water to prevent them from agglomerating and growing and clogging pipes or equipment. It is also sometimes used in cleaning agents, cyanide-free electroplating, and as a pesticide intermediate.

[0003] Currently, the main equipment for synthesizing sodium O-ethylphosphonate is a reactor. Triethyl phosphite and the required amount of water or catalyst are precisely delivered to the reactor for hydrolysis and rearrangement to produce ethylphosphonic acid. During this process, the temperature in the reactor will rise. Triethyl phosphite is flammable and easily decomposes when exposed to water or moisture, and may produce a small amount of flammable gas, such as phosphine, which is highly toxic and flammable. Improper operation may cause combustion and poisoning risks.

[0004] Based on this, in the synthesis of sodium O-ethylphosphonate, the gas generated in the reaction needs to be treated. Therefore, the outer end of the reactor is often connected to a device for treating the gas in the reaction. However, when the speed of mixing triethyl phosphite and the required amount of water or catalyst is too fast, it is easy to cause the temperature in the reactor to rise sharply, and ethanol, unreacted phosphite, and possible by-product butene to be rapidly vaporized. The gas treatment equipment will not be able to evolve in time, which may lead to overpressure. In severe cases, there is a risk of material impact, explosion, or even leakage of toxic gases. Based on this, it is necessary to control the mixing speed so that the amount of gas generated matches the speed of mixing with triethyl phosphite to avoid the gas being generated too quickly and not being able to be purified or affecting the outside world. Summary of the Invention

[0005] The present invention is directed to the problems raised by the above background technology, and the technical problem to be solved by the present invention is to provide a preparation device and a preparation process of sodium O-ethylphosphonate.

[0006] The technical solution adopted by the present invention to solve the above technical problems is: a sodium O-ethylphosphonate preparation device includes a reactor, a reactor cover at the upper end of the reactor, a driving component on the reactor cover, an output end of the driving component having a stirring structure extending into the reactor, an injection port 1 for injecting triethyl phosphite at the upper end of the reactor cover, and a rotating component fixed to the driving component inside the reactor cover; There are multiple exchange slots on the rotating part, and partitions are sliding inside the exchange slots. The upper and lower ends of the partitions are supported by triethyl phosphite and the gas in the reactor respectively to maintain balance. When the gas pressure changes, the position of the partition changes.

[0007] A further preferred solution of the present invention is: a kettle groove for installing a rotating part is opened at the upper end of the kettle cover, the upper end of the kettle groove is closed with a cover layer, an injection port is opened on the cover layer, and a connecting hole corresponding to the exchange groove is passed downward inside the kettle groove, and the connecting hole can correspond to multiple rotating exchange grooves respectively.

[0008] A further preferred solution of the present invention is that the rotating component includes a turntable, and a plurality of exchange slots are circumferentially arranged on the turntable and penetrate the turntable.

[0009] A further preferred solution of the present invention is that: an exchange port 1 is opened on the lower end surface of the turntable, and the exchange port 1 moves along the radial direction of the turntable and extends from the outside to the inside of the exchange tank; The inner wall of the kettle tank is provided with a through-hole transversely, and the outlet hole can correspond to the rotating exchange port one, and the position of the outlet hole is located on the side away from the connecting hole one; The upper end of the cover layer is also integrated with an injection port 2, and the injection port 2 is connected to an air pipe. The air pipe can cooperate with the rotating exchange tank, and when the air pipe cooperates with the corresponding exchange tank, the air outlet corresponds to the exchange port 1 of the corresponding exchange tank. The outer side of the air pipe is used to connect to the air pump to push the interlayer downward to discharge the gas.

[0010] A further preferred solution of the present invention is that: the upper end of the turntable is further penetrated by a second exchange hole corresponding in number to the exchange slots, the second exchange hole is located on the inward side of the exchange slots, and the second exchange hole penetrates the turntable downward; The upper end surface of the turntable is provided with an exchange port 2 for connecting the exchange slot and the exchange hole 2; The inner wall of the lower end of the kettle tank is also provided with a second connecting hole and a first exchange hole extending into the reactor. The second exchange hole can correspond to the first exchange hole during rotation, and when the second exchange hole corresponds to the first exchange hole, the second connecting hole corresponds to the exchange tank. A magnetic attraction structure is also provided at the upper end of the cover layer. The magnetic attraction structure is located at a position corresponding to the second upper end of the connecting hole and is used to generate a magnetic attraction effect on the corresponding partition upwards.

[0011] A further preferred solution of the present invention is that both upper and lower end surfaces of the exchange tank have a circle of separation layers, the separation layers are integrally formed with the turntable, and the separation layers on the upper and lower sides are flush with the upper and lower end surfaces of the turntable respectively.

[0012] A further preferred solution of the present invention is that the upper and lower end surfaces of the partition layer are integrally provided with an outer protruding layer, and the outer protruding layer can be embedded in the partition layer and fit tightly with the partition layer.

[0013] A further preferred solution of the present invention is that the interior of the partition is made of metal with magnetic attraction, and the exterior is covered with a protective layer.

[0014] A further preferred solution of the present invention is that a one-way valve is connected to the air pipe.

[0015] The preparation process of sodium O-ethylphosphonate comprises the following steps: Step 1: Prepare the raw materials including triethyl phosphite, pure water or dilute acid; Step 2: Hydrolysis and rearrangement reaction, the reaction is controlled by the reactor and cooling system, pure water or dilute acid is added to the reactor, and stirring and pre-cooling are performed; Step 3: Triethyl phosphite is added to the reactor by inert gas pressure, and the temperature is automatically feedback controlled; Step 4: The gas generated in the reactor is purified by passing through a dilute nitric acid spray tower, a catalytic combustion tower, and an alkaline washing tower in sequence; Step 5: Slowly add sodium hydroxide solution to ethylphosphonic acid to convert it into sodium salt, and then separate the wet crystal powder and the remaining liquid; Step 6: Place the wet powder into a drying oven and use hot air to dry out the moisture to obtain dry sodium O-ethylphosphonate powder.

[0016] Compared with the prior art, the advantages of the present invention are: 1. The pressure change caused by the generation of toxic gas in the reactor drives the displacement of the interlayer and dynamically changes the amount of triethyl phosphite fed. When the reactor reacts violently and the gas pressure rises, the feed amount is automatically reduced to reduce the rate of phosphine generation from the source, ensuring that the gas volume is always within the processing capacity of the purification system and avoiding the risk of leakage of highly toxic gas.

[0017] 2. As the gas pressure increases, the amount of triethyl phosphite added decreases, the reaction rate decreases, and the temperature rise in the kettle is suppressed, preventing safety accidents such as overheating and temperature runaway caused by excessive heat release in the reaction, without relying on external temperature sensors and controllers.

[0018] 3. Through the rotating structure of the turntable, the toxic gas is compressed by the interlayer and temporarily stored at the bottom of the exchange tank. The turntable rotates to align the exchange port with the air outlet. The inert gas in the air pipe pushes the interlayer to discharge a certain amount of gas, limiting the single emission volume and matching the treatment efficiency of the purification system.

[0019] 4. The displacement of the interlayer depends only on the air pressure difference, without motor or hydraulic pressure, and without wearing parts such as precision metering pumps, which makes the maintenance cost low and the safety high. BRIEF DESCRIPTION OF THE DRAWINGS

[0020] The present invention will be described in further detail below in conjunction with the accompanying drawings and preferred embodiments. However, those skilled in the art will appreciate that these drawings are only drawn for the purpose of explaining the preferred embodiments and therefore should not be regarded as limiting the scope of the present invention. Furthermore, unless otherwise specified, the drawings only conceptually represent the composition or structure of the described objects and may contain exaggerated displays, and the drawings are not necessarily drawn to scale.

[0021] Figure 1 It is a schematic diagram of the overall structure of the present invention; Figure 2 This is a schematic structural diagram of the kettle cover of the present invention; Figure 3 This is a schematic diagram of the separation structure of the kettle cover and the internal turntable of the present invention; Figure 4 This is a schematic diagram of a partial cross-sectional structure of a turntable according to the present invention; Figure 5 This is a partially enlarged structural diagram of the turntable and partition of the present invention; Figure 6 This is a schematic diagram of the kettle structure of the present invention; Figure 7 This is a schematic diagram of the main half-section structure of the kettle cover of the present invention; Figure 8 This is a schematic diagram of the partial cross-sectional structure of the kettle cover of the present invention; Figure 9 For the present invention Figure 8 Schematic diagram of the locally enlarged structure of A in the middle.

[0022] In the figure: 1. Reactor; 2. Reactor cover; 21. Reactor tank; 22. Connection hole 1; 23. Air outlet; 24. Connection hole 2; 25. Exchange hole 1; 3. Driving component; 4. Cover layer; 5. Injection port 1; 6. Injection port 2; 7. Air pipe; 71. One-way valve; 8. Magnetic structure; 9. Turntable; 91. Exchange tank; 911. Partition layer; 912. Exchange port 1; 913. Exchange port 2; 914. Exchange hole 2; 92. Partition layer; 921. Outer protrusion layer. DETAILED DESCRIPTION

[0023] Preferred embodiments of the present invention will be described in detail below with reference to the accompanying drawings. Those skilled in the art will appreciate that these descriptions are only illustrative and exemplary and should not be construed as limiting the scope of protection of the present invention.

[0024] It should be noted that like reference numerals denote like items in the following drawings, and thus, once an item is defined in one drawing, it may not be further defined or explained in subsequent drawings.

[0025] This embodiment mainly describes a device for preparing sodium O-ethylphosphonate, specifically as follows: In the process of preparing sodium O-ethylphosphonate, triethyl phosphite needs to react with water or dilute acid, wherein the reaction process produces highly toxic and flammable gases such as phosphine. Based on this, it is necessary to treat the generated gas during the reaction process. In order to completely treat the gas, the gas needs to be fully purified. Therefore, it is necessary to control the reaction speed to avoid excessive reaction resulting in excessive gas generation and difficulty in complete purification. In addition, excessive reaction will also cause the temperature in the reactor 1 to rise too quickly, which is likely to lead to safety problems. Based on this, a device for preparing sodium O-ethylphosphonate is proposed, such as Figure 1-Figure 3 As shown, the reactor 1 comprises a reactor cover 2 at the upper end thereof, a driving component 3 on the reactor cover 2, an output end of the driving component 3 having a stirring structure extending into the reactor 1, an injection port 5 for injecting triethyl phosphite at the upper end of the reactor cover 2, and a rotating component fixed to the driving component 3 inside the reactor cover 2; A plurality of exchange slots 91 are provided on the rotating component, and a partition 92 slides inside the exchange slot 91. The upper and lower ends of the partition 92 are supported by triethyl phosphite and the gas in the reactor 1 respectively to maintain balance. When the gas pressure changes, the position of the partition 92 changes.

[0026] Specifically, the interior of the reactor lid 2 includes a rotating component that rotates synchronously with the drive component 3. The rotating component has multiple exchange slots 91, and a partition 92 slides within the exchange slots 91. The upper end of the partition 92 is connected to the triethyl phosphite tank, and the lower end is connected to the interior of the reactor 1. When the pressure inside the reactor 1 changes, the partition 92, sandwiched between the triethyl phosphite tank and the reactor 1, can move up and down, changing the space above and below. It should be noted that the amount of gas generated by the reactor 1 is too large, which can easily affect the gas purification efficiency. Therefore, it is necessary to reduce the gas production in the reactor 1 and reduce the amount of triethyl phosphite added to achieve control. The rotating component automatically reduces the amount of triethyl phosphite added when the gas volume in the reactor 1 causes the pressure to increase, achieving a balancing effect. It should also be noted that the gas production in the reactor 1 can control the amount of triethyl phosphite added, further automatically limiting the problem of excessive temperature increases in the reactor 1. The relatively simple structure of the rotating component ensures stability even in harsh working environments.

[0027] like Figure 3 As shown, the upper end of the kettle cover 2 is provided with a kettle groove 21 for installing the rotating parts, the upper end of the kettle groove 21 is closed with a cover layer 4, an injection port 5 is provided on the cover layer 4, and a connecting hole 22 corresponding to the exchange groove 91 is passed downward inside the kettle groove 21, and the connecting hole 22 can correspond to multiple exchange grooves 91 in rotation respectively.

[0028] Specifically, the upper end of the kettle cover 2 has a kettle tank 21, and the turntable 9 is mounted within the kettle tank 21. The injection port 5 and the connecting hole 22 are located on the upper and lower sides of the kettle tank 21, respectively. The injection port 5 and the connecting hole 22 are located in the rotation path of the exchange tank 91, so that the injection port 5 and the connecting hole 22 can cooperate with the exchange tank 91. It should be noted that a triethyl phosphite storage tank is fixed to the outer end of the injection port 5. The outer end of the triethyl phosphite storage tank is connected to a pipeline for injecting inert gas. This maintains a certain pressure inside the triethyl phosphite storage tank, pushes the triethyl phosphite downward, and injects the triethyl phosphite from the storage tank into the exchange tank 91. It should be noted that maintaining a balanced pressure inside the triethyl phosphite storage tank is a conventional technique. Injecting inert gas into the triethyl phosphite storage tank via a metering pump or having a one-way valve 71 on the outside of the triethyl phosphite storage tank to only allow the inert gas to be introduced, allowing the triethyl phosphite to move into the exchange tank 91 under the action of gravity, can also be achieved.

[0029] like Figure 3 As shown, the rotating component includes a turntable 9 , and a plurality of exchange slots 91 are circumferentially arranged on the turntable 9 and pass through the turntable 9 .

[0030] Specifically, the turntable 9 rotates, and the multiple exchange slots 91 respectively cooperate with the injection port 5 and the connection hole 22 to keep the reaction kettle 1 in a continuous state. The reaction is controlled by the driving component 3, and the rotation of the driving component 3 causes the reaction inside the reactor 1 to proceed.

[0031] like Figure 3-Figure 6 The lower end surface of the turntable 9 is provided with an exchange port 912, which moves radially along the turntable 9 and extends from the outside to the exchange slot 91; The inner wall of the kettle tank 21 is provided with a through-hole 23, which can correspond to the rotating exchange port 1 912 and is located on the side away from the connecting hole 1 22. The upper end of the cover layer 4 is also integrated with an injection port 2 6, and the injection port 2 6 is connected to the outside of the air pipe 7. The air pipe 7 can cooperate with the rotating exchange tank 91, and when the air pipe 7 cooperates with the corresponding exchange tank 91, the air outlet 23 corresponds to the exchange port 1 912 of the corresponding exchange tank 91. The outer side of the air pipe 7 is used to connect to the air pump to push the partition 92 downward to discharge the gas.

[0032] Specifically, the upper and lower end surfaces of the turntable 9 respectively have an exchange port 2 913 and an exchange port 1 912, wherein the exchange port 2 913 and the exchange port 1 912 extend laterally along the upper and lower end surfaces of the turntable 9, respectively. The exchange port 1 912 extends from the outside of the turntable 9 into the exchange tank 91. The inner wall of the side of the kettle tank 21 has an air outlet 23. The rotating turntable 9 will align the exchange port 1 912 with the air outlet 23, and then when the partition 92 moves downward, the gas can be discharged along the exchange port 1 912 and the air outlet 23. It should be noted that when the exchange port 1 912 is located in the kettle tank 21 and rotates, it is blocked by the inner wall of the kettle tank 21 and is therefore in a closed state. The gas can be discharged outward only when the exchange port 1 912 and the air outlet 23 overlap or partially overlap.

[0033] like Figure 5 and Figure 6 As shown, the upper end of the turntable 9 is further penetrated by a number of second exchange holes 914 corresponding to the number of exchange slots 91. The second exchange holes 914 are located on the inward side of the exchange slots 91, and the second exchange holes 914 penetrate the turntable 9 downward. The upper end surface of the turntable 9 is provided with a second exchange port 913 for connecting the exchange slot 91 and the second exchange hole 914; The inner wall of the lower end of the kettle tank 21 is further provided with a second connecting hole 24 and an exchange hole 1 25 extending into the reactor 1. The second exchange hole 914 can correspond to the exchange hole 1 25 during rotation. When the exchange hole 914 corresponds to the exchange hole 1 25, the second connecting hole 24 corresponds to the exchange tank 91. The upper end of the cover layer 4 is further provided with a magnetic attraction structure 8 , which is located at a position corresponding to the upper end of the second connecting hole 24 and is used to generate a magnetic attraction effect on the corresponding partition layer 92 upwards.

[0034] Specifically, the exchange port 2 913 is a connecting channel for discharging triethyl phosphite. The upper end of the turntable 9 is penetrated by exchange holes 2 914 of a corresponding number to the exchange tank 91. The exchange hole 1 25 on the inner wall of the lower end of the kettle tank 21 is located on the path of the exchange hole 2 914 when it rotates. When the turntable 9 rotates, the exchange hole 1 25 is controlled to cooperate with the exchange hole 2 914, and the upper end of the partition 92 is adsorbed by the magnetic structure 8, so that the partition 92 pushes the triethyl phosphite upward, and moves from the exchange hole 1 25 and the exchange hole 2 914 to enter the reactor 1.

[0035] It should be noted that the magnetic attraction structure 8 is a detachable magnet.

[0036] like Figure 5 As shown, the upper and lower end surfaces of the exchange tank 91 each have a circle of separation layer 911, the separation layer 911 and the turntable 9 are integrally formed, and the separation layers 911 on the upper and lower sides are flush with the upper and lower end surfaces of the turntable 9 respectively.

[0037] like Figure 5As shown, the upper and lower end surfaces of the partition layer 92 are integrally provided with an outer protruding layer 921 . The outer protruding layer 921 can be embedded in the partition layer 911 and fits tightly with the partition layer 911 .

[0038] Specifically, such as Figure 5 As shown, the thickness of the partition layer 911 is the same as that of the exchange port 1 912 and the exchange port 2 913, and is also the same as that of the outer protruding layer 921, so that the exchange port 1 912 and the exchange port 2 913 are always separated by the partition layer 92. It should also be noted that the partition layer 92 and the exchange slot 91 are in a sealed state to avoid leakage between the upper and lower surfaces of the partition layer 92. It should also be noted that the upper and lower end surfaces of the partition layer 92 are integrally provided with the outer protruding layer 921 and can cooperate with the partition layer 91. When cooperated, the contact area can be increased, further improving the sealing effect.

[0039] like Figure 5 As shown, the interior of the barrier 92 is a metal with magnetic properties, and the exterior is covered with a protective layer. It should be noted that the protective layer is made of stainless steel and is non-magnetic. It should also be noted that the turntable 9 is also made of stainless steel and is also non-magnetic.

[0040] like Figure 2 As shown, a one-way valve 71 is connected to the air pipe 7. It should be noted that the one-way valve 71 is used to transmit the gas transmitted from the air pipe 7 in one direction, and during the one-way transmission process, the gas transmitted is an inert gas to avoid reaction with triethyl phosphite. It should also be noted that although the outside of the air pipe 7 is connected to the air pump, the inert gas driven by the air pump only needs to drive the air pump. Figure 7 The partition 92 shown in the figure produces a pushing movement downward to discharge the toxic gas at the lower end of the partition 92. Therefore, the compression amount of the inert gas pushed to the upper end of the partition 92 is relatively small. This is manually controlled, and also Figure 7 As shown in FIG, the toxic gas at the lower end of the partition 92 that cooperates with the connecting hole 1 22 is compressed relatively more, so even if inert gas moves into the reactor 1, the gas is generally discharged outward.

[0041] It should be noted that during the synthesis of sodium O-ethylphosphonate, the gas in the trachea 7 will move into the reactor 1. When triethyl phosphite reacts with pure water or dilute acid in the reactor 1, if an inert gas is present in the system, the water vapor partial pressure in the reactor 1 can be reduced, the rate of non-target hydrolysis can be slowed down, the interference of hydrolysis by-products on the synthesis of sodium O-ethylphosphonate can be reduced, and the purity of the product can be improved.

[0042] The preparation process of sodium O-ethylphosphonate comprises the following steps: Step 1: Prepare the raw materials including triethyl phosphite, pure water or dilute acid; Step 2: Hydrolysis and rearrangement reaction, the reaction is controlled by reactor 1 and cooling system, pure water or dilute acid is added to reactor 1, and stirring and pre-cooling are performed; Step 3: adding triethyl phosphite to the reactor 1 by inert gas pressurization, and automatically controlling the temperature by feedback; Step 4: The gas generated in the reactor 1 is purified by passing through a dilute nitric acid spray tower, a catalytic combustion tower, and an alkaline washing tower in sequence; Step 5: Slowly add sodium hydroxide solution to ethylphosphonic acid to convert it into sodium salt, and then separate the wet crystal powder and the remaining liquid; Step 6: Place the wet powder into a drying oven and use hot air to dry out the moisture to obtain dry sodium O-ethylphosphonate powder.

[0043] Working principle: The outer end of injection port 15 is connected to a storage tank of triethyl phosphite, and the triethyl phosphite storage tank is injected into the reactor 1 by means of inert gas pressurization. When the triethyl phosphite is injected into the reactor 1 and reacts with pure water or dilute acid, toxic gas is generated. The toxic gas in the closed reactor 1 will cause the air pressure to increase. When the injected triethyl phosphite continues to increase, the pressure in the reactor 1 is too high, which can easily cause danger. Although the generated toxic gas can be discharged, the purification effect of the discharge is limited. It needs to be discharged in a certain amount to avoid exceeding the purification limit. Unpurified toxic gas can also have a serious impact on the environment. Therefore, when the air pressure in the reactor 1 increases, it is necessary to replace the slow-release triethyl phosphite, or even stop the injection of triethyl phosphite. Although metering pumps can effectively control metering, their key parts have a short lifespan and are complex to maintain, making them easily damaged. Triethyl phosphite is also easily hydrolyzed and corrosive. Leaked triethyl phosphite can form an explosive mixture when exposed to air. Therefore, a structure for replacing triethyl phosphite is proposed.

[0044] A triethyl phosphite storage tank is connected to the injection port 5, and the outer end of the triethyl phosphite storage tank is connected to an air pump through a pipeline. The air pump is used to transport inert gas to maintain a certain pressure in the triethyl phosphite storage tank. It should be noted that the air pump maintains the pressure position of the triethyl phosphite storage tank within a certain range by continuously or intermittently injecting inert gas. This is an existing technology. When the pressure of the storage tank drops to the set lower limit, the air pump starts and replenishes gas into the tank. When the pressure rises to the upper limit, the air pump stops working to avoid overpressure. Based on this, if Figure 3As shown, an exchange slot 91 of the turntable 9 corresponds to the connecting hole 1 22 , so that the lower end of the partition 92 is supported by the gas generated by the reactor 1, and the upper end is filled with triethyl phosphite. When the gas in the reactor 1 changes, a pressure difference is formed between the pressure in the reactor 1 and the pressure in the triethyl phosphite storage tank. Therefore, the partition 92 can move upward or downward, thereby changing the amount of triethyl phosphite received by the upper end of the partition 92. The amount of triethyl phosphite received by the upper end of the partition 92 is the amount injected into the reactor 1, achieving an automatic adjustment function. When the pressure in the reactor 1 is high, the amount of triethyl phosphite injected can be reduced. Conversely, when the pressure in the reactor 1 is low, the amount of triethyl phosphite injected can be increased. This automatically adjusts the reaction level in the reactor 1.

[0045] Secondly, if Figure 7 As shown, after triethyl phosphite is present at the upper end of barrier 92, turntable 9 rotates to the lower end of injection port 2 6 . Air pressure from air pipe 7 pushes barrier 92 downward, causing the toxic gas at the lower end of barrier 92 to move along exchange port 1 912 and outlet 23 , thereby discharging and purifying the gas. It should be noted that during toxic gas discharge, the maximum discharge volume is the volume stored in the space below barrier 92 when barrier 92 reaches its upper limit. This limits the discharge volume to avoid affecting purification.

[0046] Afterwards, if Figure 8 and Figure 9 As shown, the turntable 9 continues to rotate, so that the partition 92 is located at the lower end of the magnetic attraction structure 8. Under the action of the magnetic attraction, the partition 92 is lowered and adsorbed upward. At the same time, the exchange hole 2 914 is connected with the exchange hole 1 25, and the upper end of the partition 92 is connected with the exchange hole 2 914 through the exchange port 2 913. The lower end of the partition 92 is connected with the interior of the reactor 1 through the connecting hole 24. The pressure difference between the upper and lower parts of the partition 92 is the same, and the upper and lower directions of the partition 92 can be achieved. Movement, based on this, is completed to inject triethyl phosphite.

[0047] Subsequently, the turntable 9 continues to rotate, and the partition 92 corresponds to the injection port 1 5 and the connecting hole 1 22 again, completing the repetitive work.

[0048] In the description of the present invention, it should be noted that the terms "upper", "lower", "front", "back", "inside", "outside", etc. indicate orientations or positional relationships based on the orientations or positional relationships shown in the accompanying drawings, or are the orientations or positional relationships in which the inventive product is usually placed when in use. They are only for the convenience of describing the present invention and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation. Therefore, they should not be understood as limiting the present invention.

[0049] The above is a detailed introduction to the sodium O-ethylphosphonate preparation device provided by the present invention. Specific examples are used herein to illustrate the principles and implementation methods of the present invention. The description of the above embodiments is only intended to help understand the present invention and its core ideas. It should be noted that, for those skilled in the art, without departing from the principles of the present invention, several improvements and modifications may be made to the present invention, and such improvements and modifications also fall within the scope of protection of the claims of the present invention.

Claims

1. A device for preparing sodium O-ethylphosphonate, comprising a reactor, a reactor cover at the upper end of the reactor, a driving component on the reactor cover, and a stirring structure extending into the reactor at the output end of the driving component, characterized in that: The upper end of the kettle cover is provided with an injection port 1 for injecting triethyl phosphite, and the interior of the kettle cover is provided with a rotating component fixed to the driving component; There are multiple exchange slots on the rotating part, and partitions are sliding inside the exchange slots. The upper and lower ends of the partitions are supported by triethyl phosphite and the gas in the reactor respectively to maintain balance. When the gas pressure changes, the position of the partition changes.

2. The O-ethyl sodium phosphonate preparation device according to claim 1, wherein The upper end of the kettle cover is provided with a kettle groove for installing the rotating parts. The upper end of the kettle groove is closed with a cover layer. An injection port is provided on the cover layer. A connecting hole corresponding to the exchange groove is passed downwardly through the inside of the kettle groove. The connecting hole can correspond to multiple exchange grooves in rotation respectively.

3. The O-ethyl sodium phosphonate preparation device according to claim 2, wherein The rotating component comprises a rotating disk, and a plurality of exchange slots are circumferentially arranged on the rotating disk and pass through the rotating disk.

4. The O-ethyl sodium phosphonate preparation device according to claim 3, wherein The lower end surface of the turntable is provided with an exchange port 1, which moves along the radial direction of the turntable and extends from the outside to the exchange slot; The inner wall of the kettle tank is provided with a through-hole transversely, and the outlet hole can correspond to the rotating exchange port one, and the position of the outlet hole is located on the side away from the connecting hole one; The upper end of the cover layer is also integrated with an injection port 2, and the injection port 2 is connected to an air pipe. The air pipe can cooperate with the rotating exchange tank, and when the air pipe cooperates with the corresponding exchange tank, the air outlet corresponds to the exchange port 1 of the corresponding exchange tank. The outer side of the air pipe is used to connect to the air pump to push the interlayer downward to discharge the gas.

5. The O-ethyl sodium phosphonate preparation device according to claim 1, wherein The upper end of the turntable is also penetrated by a second exchange hole corresponding to the number of the exchange slots. The second exchange hole is located on the inward side of the exchange slot and passes through the turntable downward. The upper end surface of the turntable is provided with an exchange port 2 for connecting the exchange slot and the exchange hole 2; The inner wall of the lower end of the kettle tank is also provided with a second connecting hole and a first exchange hole extending into the reactor. The second exchange hole can correspond to the first exchange hole during rotation, and when the second exchange hole corresponds to the first exchange hole, the second connecting hole corresponds to the exchange tank. A magnetic attraction structure is also provided at the upper end of the cover layer. The magnetic attraction structure is located at a position corresponding to the second upper end of the connecting hole and is used to generate a magnetic attraction effect on the corresponding partition upwards.

6. The sodium O-ethylphosphonate preparation device according to claim 3, wherein The upper and lower end surfaces of the exchange tank are each provided with a circle of separation layers, the separation layers are integrally formed with the turntable, and the separation layers on the upper and lower sides are flush with the upper and lower end surfaces of the turntable respectively.

7. The sodium O-ethylphosphonate preparation device according to claim 6, wherein The upper and lower end surfaces of the partition layer are integrally provided with outer protruding layers, and the outer protruding layers can be embedded in the partition layer and fit tightly with the partition layer.

8. The sodium O-ethylphosphonate preparation device according to claim 7, wherein The inside of the partition is made of magnetic metal and the outside is covered with a protective layer.

9. The sodium O-ethylphosphonate preparation device according to claim 4, wherein A one-way valve is connected to the air pipe.

10. A process for preparing sodium O-ethylphosphonate, characterized in that: The sodium O-ethylphosphonate preparation device according to any one of claims 1 to 9 comprises the following steps: Step 1: Prepare the raw materials including triethyl phosphite, pure water or dilute acid; Step 2: Hydrolysis and rearrangement reaction, the reaction is controlled by the reactor and cooling system, pure water or dilute acid is added to the reactor, and stirring and pre-cooling are performed; Step 3: Triethyl phosphite is added to the reactor by inert gas pressure, and the temperature is automatically feedback controlled; Step 4: The gas generated in the reactor is purified by passing through a dilute nitric acid spray tower, a catalytic combustion tower, and an alkaline washing tower in sequence; Step 5: Slowly add sodium hydroxide solution to ethylphosphonic acid to convert it into sodium salt, and then separate the wet crystal powder and the remaining liquid; Step 6: Place the wet powder into a drying oven and use hot air to dry out the moisture to obtain dry sodium O-ethylphosphonate powder.

Images