Atomizing nozzle, phosphorus pentachloride synthesis reactor, phosphorus pentachloride synthesis system and phosphorus pentachloride synthesis method

By adopting a multi-nozzle design gas-liquid mixing system in the production of phosphorus pentachloride, the problems of temperature control and low purity are solved, and efficient and stable phosphorus pentachloride production is achieved, meeting the needs of continuous large-scale production.

CN119186397AActive Publication Date: 2024-12-27FUJIAN XINAN TECH CO LTD +1
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Patent Information

Application Number
CN202411423512.9
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-10-12
Publication Date
2024-12-27
Estimated Expiration
2044-10-12

AI Technical Summary

Technical Problem

The existing phosphorus pentachloride production process has problems such as difficult to control the system temperature and low product purity, and traditional batch operation cannot meet the requirements of continuous large-scale clean production.

Method used

Using atomizing nozzle and phosphorus pentachloride synthesis reactor system, the gas-liquid mixing is strengthened through the design of multiple nozzles, the size and shape of the atomized particles are controlled, the temperature in the reactor is uniform, the high temperature zone is eliminated, and the reactor is in the reactor. Set up multiple nozzles to pass liquid chlorine and cooling air to improve heat exchange effect.

Benefits of technology

The phosphorus pentachloride particles have large diameter and high purity, high raw material conversion rate (can reach 99%), high product purity (can reach 99.9%), and the temperature in the reactor can be controlled at 40℃, which meets long-term stability and safety Operation requirements.

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Abstract

The invention discloses an atomizing nozzle, a phosphorus pentachloride synthesis reactor, a phosphorus pentachloride synthesis system and a phosphorus pentachloride synthesis method.The phosphorus pentachloride synthesis reactor comprises a nozzle body, a first inlet, a second inlet, a third inlet, a fourth inlet, a fifth inlet and an outlet, and the first inlet, the second inlet, the third inlet, the fourth inlet, the fifth inlet and the outlet are formed in the nozzle body and communicate with one another; the second inlet and the fourth inlet are both used for introducing first gas, and the fifth inlet is used for introducing second gas; according to the atomizing nozzle, gas-liquid mixing can be enhanced, the size and shape of atomized particles can be controlled, in addition, by arranging the atomizing nozzle on the reactor body, the distribution uniformity of materials in the space of the reactor body is improved, and a high-temperature area in the reactor body is reduced or eliminated.
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Description

Technical Field

[0001] The invention relates to an atomizing nozzle, a phosphorus pentachloride synthesis reactor, a synthesis system and a method. Background Art

[0002] Phosphorus pentachloride is one of the important phosphorus chlorides. As a high-efficiency chlorinating agent and catalyst, it is widely used in energy, medicine, pesticides, dyes, chemical fibers and other fields. It is the raw material for the production of lithium hexafluorophosphate, phosphazene chloride, phosphorus oxychloride, azathioprine, flucytosine and other products.

[0004] The conventional phosphorus pentachloride production process is as follows: liquid phosphorus trichloride is added into a closed reactor, and chlorine gas is introduced from the bottom of the reactor to cause a chlorination reaction in the phosphorus trichloride, and the material in the reactor is transformed from a liquid phase to a solid phase; carbon dioxide gas is introduced to purge the phosphorus trichloride remaining in the phosphorus pentachloride, so that the phosphorus trichloride is replaced by carbon dioxide, and the phosphorus pentachloride in the reactor is completely transformed into a solid phase.

[0005] Although the above method is simple, it is an intermittent operation and cannot be continuously produced. The product quality and stability are poor, the operating environment is bad, and the pollution is serious. It is difficult to meet the requirements of continuous large-scale clean production. In practice, it is urgent to develop a continuous feeding method to meet the long-term stable and efficient operation of the system.

[0006] In recent years, some continuous phosphorus pentachloride production processes have been developed, such as patent document CN116920764A, which is characterized in that phosphorus trichloride is atomized into droplets and then reacts chemically with gaseous chlorine to generate phosphorus pentachloride particles. In order to control the reaction temperature, a large amount of CO2 or N2 is required as a diluent and circulating gas for cooling, resulting in a large reactor volume and difficult system temperature control. Summary of the invention

[0007] The technical problem to be solved by the present invention is to overcome the problems of difficult system temperature control and low product purity in the existing phosphorus pentachloride production, and to provide a nozzle and a phosphorus pentachloride synthesis reactor, a synthesis system and a method. The present invention can strengthen gas-liquid mixing, control the size and shape of atomized particles, so that the temperature of the liquid in the reactor is evenly controlled, eliminate the high temperature zone in the reactor, and obtain phosphorus pentachloride particles with large diameter and high purity.

[0008] The present invention solves the above technical problems through the following technical solutions:

[0009] The present invention first provides an atomizing nozzle, which comprises a nozzle body and a first inlet, a second inlet, a third inlet, a fourth inlet, a fifth inlet and an outlet which are arranged on the nozzle body and are interconnected, wherein the first inlet and the third inlet are both used for introducing liquid, the second inlet and the fourth inlet are both used for introducing a first gas, and the fifth inlet is used for introducing a second gas;

[0010] The first inlet is coaxially arranged at the top end of the nozzle body, the outlet is coaxially arranged at the bottom end of the nozzle body, the second inlet, the third inlet, the fourth inlet and the fifth inlet are all arranged on the side of the nozzle body, the second inlet is close to the first inlet, and the liquid passed into the first inlet is preliminarily atomized by the first gas passed into the second inlet, the third inlet is arranged on a branch of the fourth inlet, and the liquid passed into the third inlet is preliminarily atomized by the first gas passed into the fourth inlet; the fifth inlet is close to the outlet, and the preliminarily atomized liquid is secondarily atomized by the second gas passed into the fifth inlet.

[0011] In the present invention, the outlet is preferably an inwardly contracted structure, and the contraction angle is preferably 15 to 75°, more preferably 60°, where the contraction angle refers to the angle between the side surface of the outlet and the cross section of the outlet.

[0012] In the present invention, preferably, the second inlet, the fourth inlet, and the fifth inlet are distributed in sequence along the direction from the first inlet to the outlet;

[0013] In the present invention, preferably, the axis of the second inlet is perpendicular to the axis of the first inlet.

[0014] In the present invention, preferably, the axis of the third inlet is perpendicular to the axis of the fourth inlet.

[0015] In the present invention, preferably, the axis of the third inlet is parallel to the central axis of the nozzle body.

[0016] In the present invention, preferably, the axis of the fifth inlet is perpendicular to the central axis of the nozzle body.

[0017] In the present invention, preferably, the cross-sectional area of ​​the first inlet is smaller than the cross-sectional area of ​​the third inlet, and the cross-sectional area refers to the surface perpendicular to the liquid inlet direction. The first inlet and the second inlet are used as the start-up channel ports. At the initial stage of the reaction, a small amount of raw materials are first introduced for reaction, and the third inlet, the fourth inlet and the fifth inlet are started after the reaction is stable.

[0018] In the present invention, the cross-sectional area of ​​the fifth inlet is determined according to the amount of the second gas introduced. Preferably, the cross-sectional area of ​​the fifth inlet is greater than the cross-sectional area of ​​the third inlet.

[0019] The present invention also provides a phosphorus pentachloride synthesis reactor, which comprises a reactor body and a nozzle arranged on the reactor body;

[0020] The nozzle includes a first nozzle, which is the aforementioned atomizing nozzle, and is arranged at the top of the reactor body. The number of the first nozzle is at least one, and the first inlet and the third inlet are both used for introducing phosphorus trichloride, the second inlet and the fourth inlet are both used for introducing carbon dioxide, and the fifth inlet is used for introducing a mixed gas.

[0021] In the present invention, the first nozzles are preferably symmetrically arranged with the center of the top of the reactor body as the axis. For example, when the first nozzles are an odd number, one of the first nozzles is arranged at the center of the top of the reactor body, and the other first nozzles are symmetrically arranged with the center of the top of the reactor body as the axis; when the first nozzles are an even number, the first nozzles are symmetrically arranged with the center of the top of the reactor body as the axis.

[0022] In the present invention, the number of the first nozzles can be adjusted according to the load, for example, three.

[0023] In the present invention, preferably, the angle between the axis of the outlet of the first nozzle and the inner wall surface of the reactor body is 90°.

[0024] In the present invention, when the number of the first nozzles is greater than or equal to two, preferably, the distance D between adjacent first nozzles along the radial direction of the reactor body is not less than 20 to 50 times the diameter of the outlet of the first nozzle. If the distance between adjacent first nozzles is too small, the distribution of phosphorus trichloride liquid particles will be affected, affecting the temperature control effect. If the distance is too large, the volume of the reactor will increase.

[0025] In the present invention, the phosphorus pentachloride synthesis reactor preferably further comprises a second nozzle, which is arranged on the side of the reactor body and is used to introduce a chlorine source. The chlorine source is preferably liquid chlorine, which absorbs heat and evaporates to produce chlorine gas after entering the reactor body, and can also play a role in cooling the reactor while providing chlorine gas.

[0026] Preferably, there are at least two second nozzles, and the plurality of second nozzles are symmetrically arranged along the circumference of the reactor body with the axis of the reactor body as the center, so as to increase the distribution uniformity of the chlorine source inside the reactor body.

[0027] Wherein, the second nozzle is a conventional pressure nozzle in the art.

[0028] Preferably, the outlet of the second nozzle is inclined downward, and more preferably, the angle between the axis of the outlet of the second nozzle and the inner wall surface of the reactor body is 45-90°, for example, 60°.

[0029] The second nozzle is preferably located in a region close to the top of the reactor body so that the chlorine source can participate in the reaction earlier.

[0030] In the present invention, the phosphorus pentachloride synthesis reactor preferably further comprises a third nozzle, which is arranged on the side of the reactor body and is used to introduce quenching gas to cool the interior of the reactor body. The quenching gas is preferably a mixture of carbon dioxide and chlorine.

[0031] Preferably, there are at least two third nozzles, and the plurality of third nozzles are symmetrically arranged along the circumference of the reactor body with the axis of the reactor body as the center, so as to improve the distribution uniformity of the quenching gas inside the reactor body.

[0032] Wherein, the third nozzle is a conventional pressure nozzle or air flow nozzle in the art.

[0033] Preferably, the outlet of the third nozzle is inclined downward, and more preferably, the angle between the axis of the outlet of the third nozzle and the inner wall surface of the reactor body is 45-90°, for example, 60°.

[0034] Wherein, when the aforementioned second nozzle is provided, the third nozzle may be located below the second nozzle.

[0035] In a preferred embodiment of the present invention, the nozzle includes a first nozzle, a second nozzle and a third nozzle, there are three first nozzles, one of which is arranged at the center of the top of the reactor body, and the other first nozzles are symmetrically arranged with the center of the top of the reactor body as the axis; the second nozzle and the third nozzle are both arranged on the side of the reactor body, and the third nozzle is located below the second nozzle; there are two second nozzles, and the two second nozzles are symmetrically arranged along the circumference of the reactor body with the axis of the reactor body as the center; there are two third nozzles, and the two third nozzles are symmetrically arranged along the circumference of the reactor body with the axis of the reactor body as the center.

[0036] The present invention also provides a phosphorus pentachloride continuous synthesis system, which comprises the phosphorus pentachloride synthesis reactor and a circulating fan, wherein the reactor body of the phosphorus pentachloride synthesis reactor is provided with a chlorine source inlet, a circulating gas outlet, a circulating gas inlet and a discharge port;

[0037] The circulation fan is connected between the circulation gas outlet and the circulation gas inlet, and the fifth inlet of the first nozzle is connected to the circulation fan.

[0038] In the present invention, when the second nozzle is provided, the second nozzle is provided on the chlorine source inlet.

[0039] In the present invention, when the third nozzle is provided, the third nozzle is provided on the circulating gas inlet, and the circulating gas outlet is connected to the third nozzle.

[0040] In the present invention, the circulating gas outlet is preferably arranged at the lower side of the reactor body.

[0041] In the present invention, the discharge port is preferably arranged at the bottom of the reactor body.

[0042] In the present invention, the phosphorus pentachloride continuous synthesis system may further include a cooling device, which is connected between the circulating fan and the circulating gas inlet, and is used to cool the circulating gas.

[0043] Wherein, the cooling device can be a conventional heat exchanger in the art.

[0044] In the present invention, the phosphorus pentachloride continuous synthesis system may further include a gas purification and separation device, which is arranged between the circulating gas outlet and the circulating fan and is used to purify the circulating gas.

[0045] Wherein, the gas purification and separation device can be a bag filter.

[0046] In the present invention, the phosphorus pentachloride continuous synthesis system may further include a product tank, and the product tank is connected to the discharge port.

[0047] In the present invention, the phosphorus pentachloride continuous synthesis system may further include a phosphorus trichloride storage tank, a first chlorine storage tank and a carbon dioxide storage tank, wherein the phosphorus trichloride storage tank is connected to the first inlet and the third inlet of the first nozzle, the carbon dioxide storage tank is connected to the second inlet and the fourth inlet of the first nozzle, and the first chlorine storage tank is connected to the chlorine source inlet.

[0048] In the present invention, the circulating fan may also be connected to a second chlorine storage tank for replenishing chlorine to the circulating gas.

[0049] The present invention also provides a method for continuously synthesizing phosphorus pentachloride, which adopts the phosphorus pentachloride continuous synthesis system described above for synthesis, and comprises the following steps: passing phosphorus trichloride liquid into the reactor body through the first nozzle, passing a chlorine source into the reactor body through the chlorine source inlet, and reacting.

[0050] In the present invention, the circulating gas includes chlorine and carbon dioxide, and the volume concentration of the chlorine is preferably 5-85%, for example 35%.

[0051] In the present invention, the velocity of the gas at the outlet of the first nozzle is preferably 0.1-300 m / s, such as 20 m / s. The velocity of the liquid at the outlet of the first nozzle is preferably 0.01-100 m / s, such as 1 m / s.

[0052] In the present invention, when the aforementioned second nozzle is provided, the pressure drop of the second nozzle is preferably 0.03-0.1 MPa, for example 0.05 MPa.

[0053] In the present invention, when the third nozzle is provided, the velocity of the outlet of the third nozzle is preferably 5 to 50 m / s, for example, 10 m / s.

[0054] The positive and progressive effects of the present invention are:

[0055] (1) The atomizing nozzle of the present invention can enhance gas-liquid mixing and control the size and shape of atomized particles.

[0056] (2) By arranging the atomizing nozzle of the present invention on the reactor body, the uniformity of the distribution of the material in the space of the reactor body is improved, and the high temperature area in the reactor body is reduced or eliminated. In some embodiments of the present invention, the temperature in the reactor can be controlled at 40° C.;

[0057] The present invention further improves the heat exchange effect between the material and the heat exchange medium (such as the cooled circulating gas) by arranging a plurality of nozzles in layers on the side of the reactor body for introducing liquid chlorine and quenching gas.

[0058] (3) The raw material conversion rate of the present invention is high (can reach 99%) and the product purity is high (can reach 99.9%). BRIEF DESCRIPTION OF THE DRAWINGS

[0059] Figure 1 Schematic diagram of the nozzle structure.

[0060] Figure 2 This is a schematic diagram of the structure of the phosphorus pentachloride synthesis reactor.

[0061] Figure 3 This is a schematic diagram of the structure of the continuous synthesis system of phosphorus pentachloride.

[0062] Description of Reference Numerals

[0063] First nozzle 1

[0064] Nozzle body 101

[0065] First entrance 102

[0066] Second entrance 103

[0067] The third entrance 104

[0068] Fourth Entrance 105

[0069] Fifth Entrance 106

[0070] Exit 107

[0071] Second nozzle 2

[0072] The third nozzle 3

[0073] Reactor body 4

[0074] Chlorine source entrance 401

[0075] Recycle gas outlet 402

[0076] Circulating gas inlet 403

[0077] Discharge port 404

[0078] Circulation fan 5

[0079] Cooling device 6

[0080] Gas purification and separation device 7

[0081] Phosphorus trichloride storage tank 8

[0082] Carbon dioxide storage tank 9

[0083] First chlorine storage tank 10

[0084] Second chlorine storage tank 11

[0085] Product tank 12 DETAILED DESCRIPTION

[0086] The present invention is further described below by way of examples, but the present invention is not limited to the scope of the examples.

[0087] Example 1

[0088] This embodiment discloses an atomizing nozzle, such as Figure 1As shown, it comprises: it comprises a nozzle body 101 and a first inlet 102, a second inlet 103, a third inlet 104, a fourth inlet 105, a fifth inlet 106 and an outlet 107 which are arranged on the nozzle body 101 and are connected to each other, the first inlet 102 and the third inlet 104 are both used for introducing liquid, the second inlet 103 and the fourth inlet 105 are both used for introducing the first gas, and the fifth inlet 106 is used for introducing the second gas;

[0089] The first inlet 102 is coaxially disposed at the top end of the nozzle body 101 , and the outlet 107 is coaxially disposed at the bottom end of the nozzle body 101 ;

[0090] The second inlet 103, the fourth inlet 105 and the fifth inlet 106 are all located at the side of the nozzle body 101. The second inlet 103, the fourth inlet 105 and the fifth inlet 106 are sequentially distributed along the direction from the first inlet 102 to the outlet 107. The axis of the second inlet 103 is perpendicular to the axis of the first inlet 102, the axis of the third inlet 104 is parallel to the central axis of the nozzle body 101, and the axis of the fourth inlet 105 is perpendicular to the axis of the third inlet 104. The second inlet 103 is close to the first inlet 102, and the first gas introduced into the second inlet 103 is used to preliminarily atomize the liquid introduced into the first inlet 102. The third inlet 104 is provided on the branch of the fourth inlet 105, and the first gas introduced into the fourth inlet 105 is used to preliminarily atomize the liquid introduced into the third inlet 104. The fifth inlet 106 is close to the outlet 107, and the axis of the fifth inlet 106 is perpendicular to the central axis of the nozzle body 101. The outlet 107 is an inwardly contracted structure with a contraction angle of 60°.

[0091] The first inlet 102 and the second inlet 103 are used as the start-up channel ports. In the initial stage of the reaction, a small amount of raw materials are introduced for reaction. After the reaction is stable, the third inlet 104, the fourth inlet 105 and the fifth inlet 106 are started. The cross-sectional area of ​​the first inlet 102 is smaller than the cross-sectional area of ​​the third inlet 104, and the cross-sectional area of ​​the fifth inlet 106 is larger than the cross-sectional area of ​​the third inlet 104.

[0092] Example 2

[0093] This embodiment discloses a phosphorus pentachloride synthesis reactor, such as Figure 2 As shown, it comprises: a reactor body 4 and nozzles arranged on the reactor body 4 . The reactor body 4 is a cylindrical structure. The nozzles comprise a first nozzle 1 , a second nozzle 2 and a third nozzle 3 .

[0094] The first nozzle is the atomizing nozzle described in Example 1. There are three first nozzles 1, one of which is arranged at the center of the top of the reactor body 4, and the other two first nozzles 1 are arranged symmetrically with the center of the top of the reactor body 4 as the axis. The axis of the outlet of the first nozzle 1 is at an angle of 90° to the inner wall of the reactor body 4. The first inlet 102 and the third inlet 104 are both used to introduce phosphorus trichloride, the second inlet 103 and the fourth inlet 105 are both used to introduce carbon dioxide, and the fifth inlet 106 is used to introduce a mixed gas, which is a mixture of carbon dioxide and chlorine. The spacing D between adjacent first nozzles 1 is 20 times the diameter d of the outlet of the first nozzle 1.

[0095] The second nozzle 2 and the third nozzle 3 are both arranged on the side of the reactor body 4, and the third nozzle 3 is located below the second nozzle 2. The second nozzle 2 is used to introduce a chlorine source. There are two second nozzles 2, which are symmetrically arranged along the circumference of the reactor body 4 with the axis of the reactor body 4 as the center. The outlet of the second nozzle 2 is inclined downward, and the angle between the outlet axis of the second nozzle 2 and the inner wall surface of the reactor body 4 is 60°; the second nozzle 2 is a pressure nozzle, and the pressure nozzle structure is the nozzle structure described in Example 1 in CN1164442A.

[0096] The third nozzle 3 is used to introduce quenching gas. There are two third nozzles 3. The two third nozzles 3 are symmetrically arranged along the circumference of the reactor body 4 with the axis of the reactor body 4 as the center. The outlet of the third nozzle 3 is inclined downward, and the angle between the outlet axis of the third nozzle 3 and the inner wall surface of the reactor body 4 is 60°; the third nozzle 3 is an airflow nozzle, and the airflow nozzle structure is the nozzle structure described in Example 2 in CN105057128B.

[0097] Example 3

[0098] This embodiment discloses a continuous synthesis system of phosphorus pentachloride. Figure 3 As shown, it includes: the phosphorus pentachloride synthesis reactor recorded in Example 2, a circulating fan 5, a cooling device 6, a gas purification and separation device 7, a phosphorus trichloride storage tank 8, a carbon dioxide storage tank 9, a first chlorine storage tank 10, a second chlorine storage tank 11 and a product tank 12.

[0099] The reactor body 4 is provided with a chlorine source inlet 401 , a circulating gas outlet 402 , a circulating gas inlet 403 and a discharge port 404 . The circulating gas outlet 402 is arranged at the lower side of the reactor body, and the discharge port 404 is arranged at the bottom of the reactor body 4 .

[0100] The second nozzle 2 is arranged on the chlorine source inlet 401, the third nozzle 3 is arranged on the circulating gas inlet 403, the circulating gas outlet 402 is connected to the third nozzle 3, the circulating fan 5 is connected between the circulating gas outlet 402 and the third nozzle 3, and the fifth inlet 106 of the first nozzle 1 is connected to the circulating fan 5 for receiving the circulating gas coming out of the circulating fan 5.

[0101] The gas purification and separation device 7, the circulating fan 5, and the cooling device 6 are sequentially connected between the circulating gas outlet 402 and the circulating gas inlet 403 along the circulating gas flow direction. The cooling device 6 is used to cool the circulating gas, and the cooling device 6 is a heat exchanger. The gas purification and separation device 7 is used to purify the circulating gas, and the gas purification and separation device 7 is a bag filter.

[0102] The phosphorus trichloride storage tank 8 is connected to the first inlet 102 and the third inlet 104 of the first nozzle 1, the carbon dioxide storage tank 9 is connected to the second inlet 103 and the fourth inlet 105 of the first nozzle 1, the first chlorine storage tank 10 is connected to the chlorine source inlet 401, the first chlorine storage tank 10 contains liquid chlorine, the second chlorine storage tank 11 is connected to the circulating fan 5 for replenishing chlorine to the circulating gas, the product tank 12 is connected to the discharge port 404, and the bottom discharge port of the gas purification and separation device 7 is also connected to the product tank 12.

[0103] The above continuous synthesis system is used to synthesize phosphorus pentachloride, and the synthesis method includes:

[0104] Phosphorus trichloride liquid is introduced into the reactor body 4 through the first nozzle 1, and liquid chlorine is introduced into the reactor body 4 through the chlorine source inlet 401 to carry out the reaction.

[0105] The pressure in the reactor body 4 is normal pressure, the liquid raw material is phosphorus trichloride, the phosphorus trichloride flow rate is 13.7 tons / h, the circulating gas is a mixed gas of chlorine and carbon dioxide, the chlorine volume concentration is 35%, and the circulating gas volume is 9000Nm 3 / h, the set operating temperature is 40°C, the velocity of the gas at the outlet of the first nozzle is 20m / s, the velocity of the liquid at the outlet of the first nozzle is 1m / s; the pressure drop of the second nozzle is 0.05MPa, and the velocity of the outlet of the third nozzle is 10m / s.

[0106] The reaction results are:

[0107] The conversion rate of raw materials is 99%, the purity of the product phosphorus pentachloride is 99.9%, the D32 particle size of phosphorus pentachloride is 20-30um, and the maximum temperature in the furnace is 40°C. The nozzle and reactor have been running continuously for 1 year without any failure, meeting the requirements of long-term stable and safe operation.

[0108] Comparative Example 1

[0109] This comparative example adopts the scheme described in Example 1 of patent CN116920764A for synthesis, wherein the phosphorus trichloride flow rate is 13.7 tons / h, the circulating gas volume is 14000Nm 3 / h.

[0110] The reaction results are:

[0111] The conversion rate of the raw material is 96%, the purity of the product phosphorus pentachloride is 99.8%, the D32 particle size of phosphorus pentachloride is 100-1000um, and the maximum temperature in the furnace is 80°C.

Claims

1. An atomizing nozzle, characterized in that: It comprises a nozzle body and a first inlet, a second inlet, a third inlet, a fourth inlet, a fifth inlet and an outlet which are arranged on the central axis of the nozzle body and are connected to each other, wherein the first inlet and the third inlet are used to introduce liquid, the second inlet and the fourth inlet are used to introduce a first gas, and the fifth inlet is used to introduce a second gas; The first inlet is coaxially arranged at the top end of the nozzle body, the outlet is coaxially arranged at the bottom end of the nozzle body, the second inlet, the third inlet, the fourth inlet and the fifth inlet are all arranged on the side of the nozzle body, the second inlet is close to the first inlet, and the liquid passed into the first inlet is preliminarily atomized by the first gas passed into the second inlet, the third inlet is arranged on a branch of the fourth inlet, and the liquid passed into the third inlet is preliminarily atomized by the first gas passed into the fourth inlet; the fifth inlet is close to the outlet, and the preliminarily atomized liquid is secondarily atomized by the second gas passed into the fifth inlet.

2. The atomizing nozzle according to claim 1, characterized in that The outlet is an inwardly contracted structure, with a contraction angle of 15 to 75°, preferably 60°, where the contraction angle refers to the angle between the side of the outlet and the cross section of the outlet; And / or, the second inlet, the fourth inlet, and the fifth inlet are distributed in sequence along the direction from the first inlet to the outlet; and / or, the axis of the second inlet is perpendicular to the axis of the first inlet; and / or, the axis of the third inlet is parallel to the central axis of the nozzle body; and / or, the axis of the fourth inlet is perpendicular to the axis of the third inlet; and / or, the axis of the fifth inlet is perpendicular to the central axis of the nozzle body; and / or, the cross-sectional area of ​​the first inlet is smaller than the cross-sectional area of ​​the third inlet, the cross-sectional area being a plane perpendicular to the liquid inlet direction; And / or, the cross-sectional area of ​​the fifth inlet is greater than the cross-sectional area of ​​the third inlet.

3. A phosphorus pentachloride synthesis reactor, characterized in that: It includes a reactor body and a nozzle arranged on the reactor body; The nozzle includes a first nozzle, which is the atomizing nozzle according to claim 1 or 2, and is arranged at the top of the reactor body. The number of the first nozzle is at least one, the first inlet and the third inlet are both used for introducing phosphorus trichloride, the second inlet and the fourth inlet are both used for introducing carbon dioxide, and the fifth inlet is used for introducing a mixed gas.

4. The phosphorus pentachloride synthesis reactor according to claim 3, characterized in that: The first nozzles are symmetrically arranged with the center of the top of the reactor body as an axis. When the first nozzles are an odd number, one of the first nozzles is arranged at the center of the top of the reactor body, and the other first nozzles are symmetrically arranged with the center of the top of the reactor body as an axis. When the first nozzles are an even number, the first nozzles are symmetrically arranged with the center of the top of the reactor body as an axis. When the number of the first nozzles is greater than or equal to two, the distance D between adjacent first nozzles along the radial direction of the reactor body is not less than 20 to 50 times the diameter of the outlet of the first nozzle; and / or, the number of the first nozzles is three; And / or, the angle between the axis of the outlet of the first nozzle and the inner wall surface of the reactor body is 90°.

5. The phosphorus pentachloride synthesis reactor according to claim 3 or 4, characterized in that: The phosphorus pentachloride synthesis reactor further comprises a second nozzle, which is arranged on the side of the reactor body and is used to introduce a chlorine source; Preferably, there are at least two second nozzles, and the plurality of second nozzles are symmetrically arranged along the circumference of the reactor body with the axis of the reactor body as the center; Preferably, the second nozzle is a pressure nozzle; Preferably, the outlet of the second nozzle is inclined downward, and more preferably, the angle between the axis of the outlet of the second nozzle and the inner wall surface of the reactor body is 45-90°, for example 60°; Preferably, the second nozzle is located in a region close to the top of the reactor body; And / or, the phosphorus pentachloride synthesis reactor further comprises a third nozzle, the third nozzle is arranged on the side of the reactor body, and the third nozzle is used to introduce quenching gas; Preferably, there are at least two third nozzles, and the plurality of third nozzles are symmetrically arranged along the circumference of the reactor body with the axis of the reactor body as the center; Preferably, the third nozzle is an airflow nozzle; Preferably, the outlet of the third nozzle is inclined downward, and more preferably, the angle between the axis of the outlet of the third nozzle and the inner wall surface of the reactor body is 45-90°, for example 60°; Preferably, when the phosphorus pentachloride synthesis reactor further comprises a second nozzle, the second nozzle is arranged on the side of the reactor body, the second nozzle is used for introducing a chlorine source, and the third nozzle is located below the second nozzle.

6. The phosphorus pentachloride synthesis reactor according to claim 3 or 4, characterized in that: The nozzles include a first nozzle, a second nozzle and a third nozzle. There are three first nozzles, one of which is arranged at the center of the top of the reactor body, and the other first nozzles are symmetrically arranged with the center of the top of the reactor body as the axis; the second nozzle and the third nozzle are both arranged on the side of the reactor body, and the third nozzle is located below the second nozzle; there are two second nozzles, and the two second nozzles are symmetrically arranged along the circumference of the reactor body with the axis of the reactor body as the center; there are two third nozzles, and the two third nozzles are symmetrically arranged along the circumference of the reactor body with the axis of the reactor body as the center.

7. A phosphorus pentachloride continuous synthesis system, characterized in that: It comprises the phosphorus pentachloride synthesis reactor according to any one of claims 3 to 6 and a circulating fan, wherein the reactor body of the phosphorus pentachloride synthesis reactor is provided with a chlorine source inlet, a circulating gas outlet, a circulating gas inlet and a discharge port; The circulation fan is connected between the circulation gas outlet and the circulation gas inlet, and the fifth inlet of the first nozzle is connected to the circulation fan.

8. The phosphorus pentachloride continuous synthesis system according to claim 7, characterized in that: When a second nozzle is provided, the second nozzle is provided on the chlorine source inlet; When a third nozzle is provided, the third nozzle is provided on the circulating gas inlet, and the circulating gas outlet is connected to the third nozzle; And / or, the circulating gas outlet is arranged at the lower side of the reactor body; And / or, the discharge port is arranged at the bottom of the reactor body; And / or, the phosphorus pentachloride continuous synthesis system further comprises a cooling device, wherein the cooling device is connected between the circulating fan and the circulating gas inlet; the cooling device is preferably a heat exchanger; And / or, the phosphorus pentachloride continuous synthesis system further comprises a gas purification and separation device, which is arranged between the circulating gas outlet and the circulating fan; the gas purification and separation device is preferably a bag filter; And / or, the phosphorus pentachloride continuous synthesis system further comprises a product tank, and the product tank is connected to the discharge port; And / or, the phosphorus pentachloride continuous synthesis system further comprises a phosphorus trichloride storage tank, a first chlorine storage tank and a carbon dioxide storage tank, the phosphorus trichloride storage tank is connected to the first inlet and the third inlet of the first nozzle, the carbon dioxide storage tank is connected to the second inlet and the fourth inlet of the first nozzle, and the first chlorine storage tank is connected to the chlorine source inlet; And / or, the circulating fan is also connected to a second chlorine storage tank.

9. A method for continuous synthesis of phosphorus pentachloride, characterized in that: The phosphorus pentachloride continuous synthesis system according to claim 7 or 8 is used for synthesis, and comprises the following steps: introducing phosphorus trichloride liquid into the reactor body through the first nozzle, introducing a chlorine source into the reactor body through the chlorine source inlet, and reacting.

10. The method for continuous synthesis of phosphorus pentachloride according to claim 9, characterized in that: The circulating gas includes chlorine and carbon dioxide, and the volume concentration of the chlorine is 5-85%, for example, 35%; and / or, the velocity of the gas at the outlet of the first nozzle is 0.1 to 300 m / s, for example 20 m / s; And / or, the velocity of the liquid at the outlet of the first nozzle is 0.01-100 m / s, for example, 1 m / s.

Citation Information

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