Reaction cooling system for preparing 2-(diphenylphosphino) methyl benzoate

Abstract

The utility model discloses a reaction cooling system for preparing 2-(diphenylphosphino) methyl benzoate, which comprises a reaction module, a condensation module and a cryogenic TCU module, a steam outlet of the reaction module is communicated with a reflux inlet through the condensation module to form circulating cooling matching, and a cooling medium of the condensation module is heat conduction oil. A heat conduction oil outlet of the condensation module is communicated with a heat conduction oil inlet through the cryogenic TCU module to form circulating secondary cooling cooperation, and the cryogenic TCU module and heat conduction oil at the heat conduction oil inlet form temperature control cooperation, so that safety accidents caused by violent reaction generated by contact between leaked cooling water in the condensation module and reactants are avoided. Meanwhile, a TCU temperature control system is introduced to provide constant-temperature cooling, blockage is prevented, and the recovery rate of the solvent is increased.

Description

Technical Field

[0001] The utility model relates to the technical field related to PP synthesis, in particular to a reaction cooling system for preparing methyl 2-(diphenylphosphino)benzoate. Background Art

[0002] In the synthesis reaction of methyl 2-(diphenylphosphino)benzoate, sodium metal and diphenylphosphine chloride can be used as raw materials, and the solvent is 1,4-dioxane for reaction. In the reaction process, the solvent and sodium metal are first added to the reactor, the temperature is raised to reflux, the sodium metal is stirred and dispersed into sodium sand, and then diphenylphosphine chloride is added dropwise under reflux to react with the sodium sand. The following problems exist in the reaction process:

[0003] 1. At present, the cooling medium of the heat exchanger is 7℃ water. If the heat exchanger leaks, water will enter the reactor through the reflux pipe, and then react violently with the sodium metal to release hydrogen and a large amount of heat, causing an explosion and a safety accident;

[0004] 2. In addition, since the melting point of the solvent 1,4-dioxane is 12°C, if the heat exchanger is kept open for a long time at 7°C, the solvent fraction will be cooled and solidified into ice, blocking the heat exchanger and causing the pressure in the kettle to increase, creating a safety risk;

[0005] 3. At this stage, a special person needs to be arranged to control the opening of the 7℃ water valve, and feel the temperature of the solvent fraction in the reflux pipe by hand. According to the temperature, it is decided whether to open the 7℃ water and how long to open it. The operation is very cumbersome. If the temperature of the reflux pipe fraction is too high, the solvent vapor will enter the exhaust pipe, causing solvent loss, and ultimately leading to a low solvent recovery rate. If the temperature of the reflux pipe fraction is too low, the solvent will still solidify and freeze, blocking the heat exchanger. Utility Model Content

[0006] The utility model provides a reaction cooling system for preparing methyl 2-(diphenylphosphino)benzoate, aiming to solve the problems of poor safety and low solvent recovery rate caused by internal leakage, ice blockage and manual operation in the reaction cooling process.

[0007] In order to solve the above technical problems, the technical solution adopted by the utility model is:

[0008] A reaction cooling system for preparing methyl 2-(diphenylphosphino)benzoate comprises a reaction module, a condensation module and a deep cooling TCU module, wherein the steam outlet of the reaction module is connected with the reflux port through the condensation module to form a circulating cooling coordination, and the cooling medium of the condensation module is heat transfer oil, the heat transfer oil outlet of the condensation module is connected with the heat transfer oil inlet through the deep cooling TCU module to form a circulating secondary cooling coordination, and the deep cooling TCU module forms a temperature control coordination with the heat transfer oil at the heat transfer oil inlet.

[0009] Preferably, the reaction module includes a reactor and a stirring paddle arranged in the reactor, and the steam outlet of the reactor is connected to the reflux port of the reactor through a condensation module to form a circulating cooling coordination.

[0010] More preferably, the condensation module includes a condensation inlet pipe, a primary heat exchanger and a condensation reflux pipe, the feed port of the primary heat exchanger is sealed connected to the steam outlet of the reactor through the condensation inlet pipe, and the discharge port of the primary heat exchanger is sealed connected to the reflux port of the reactor through the condensation reflux pipe.

[0011] Furthermore, the heat transfer oil outlet of the primary heat exchanger is connected to the heat transfer oil inlet of the primary heat exchanger through the deep cooling TCU module to form a circulating secondary cooling cooperation.

[0012] Furthermore, the deep-cold TCU module includes a secondary heat exchanger and a TCU temperature control system. The feed port of the secondary heat exchanger is sealedly connected to the heat transfer oil outlet of the primary heat exchanger through an oil inlet pipe, the discharge port of the secondary heat exchanger is sealedly connected to the liquid inlet of the TCU temperature control system through a connecting pipe, the liquid outlet of the TCU temperature control system is sealedly connected to the heat transfer oil inlet of the primary heat exchanger through an oil outlet pipe, and the temperature of the heat transfer oil in the oil outlet pipe forms temperature control coordination with the TCU temperature control system.

[0013] Specifically, the temperature of the heat transfer oil in the oil outlet pipe is 15°C.

[0014] More specifically, the cooling medium of the secondary heat exchanger is water.

[0015] In detail, the hot water inlet and the hot water outlet of the secondary heat exchanger are connected through an external cooling water circulation system, and the temperature of water provided by the external cooling water circulation system is 7°C.

[0016] Beneficial effects of the utility model:

[0017] 1. The utility model uses heat transfer oil to cool the steam in the condensation module to prevent water from entering the reactor and reacting violently with metallic sodium when internal leakage occurs, thereby improving safety;

[0018] 2. The utility model provides constant temperature heat transfer oil through a deep cooling TCU module and circulates and cools the heat transfer oil. On the one hand, it ensures the cooling effect and makes the temperature of the heat transfer oil always greater than the melting point of the solvent to prevent ice blockage. On the other hand, it intelligently provides constant temperature heat transfer oil, reduces the tediousness of manual operation, improves work efficiency, reduces errors caused by manual operation, and improves yield and recovery rate. BRIEF DESCRIPTION OF THE DRAWINGS

[0019] Figure 1 This is a schematic diagram of system connection of the utility model;

[0020] In the figure: 1, reaction module; 101, reaction kettle; 102, stirring paddle;

[0021] 2. Condensation module; 201. Condensation air inlet pipe; 202. Primary heat exchanger; 203. Condensation reflux pipe;

[0022] 3. Deep cooling TCU module; 301. Oil inlet pipe; 302. Secondary heat exchanger; 303. Connecting pipe; 304. TCU temperature control system; 305. Oil outlet pipe. DETAILED DESCRIPTION

[0023] As follows, embodiments are further described with reference to the accompanying drawings.

[0024] like Figure 1 As shown, as a preferred embodiment 1, a reaction cooling system for preparing methyl 2-(diphenylphosphino)benzoate includes a reaction module 1, a condensation module 2 and a deep cooling TCU module 3, the steam outlet of the reaction module 1 is connected with the reflux port through the condensation module 2 to form a circulating cooling coordination, and the cooling medium of the condensation module 2 is heat transfer oil, the heat transfer oil outlet of the condensation module 2 is connected with the heat transfer oil inlet through the deep cooling TCU module 3 to form a circulating secondary cooling coordination, and the deep cooling TCU module 3 forms a temperature control coordination with the heat transfer oil at the heat transfer oil inlet.

[0025] Embodiment 1 provides a reaction cooling system for preparing methyl 2-(diphenylphosphino)benzoate, wherein metallic sodium and diphenylphosphine chloride are used as raw materials, 1,4-dioxane is used as solvent, and the reaction is carried out in reaction module 1. Steam is generated in the process, and the steam is cooled and circulated through condensation module 2 and then refluxed to reaction module 1. Condensation module 2 uses constant temperature heat transfer oil for cooling, and deep cooling TCU module 3 cools the heat transfer oil and provides constant temperature heat transfer oil to condensation module 2 through TCU to prevent the water in the cooler from violently reacting with metallic sodium and causing explosion when internal leakage occurs. The temperature in condensation module 2 is always higher than the temperature of the solvent through TCU to prevent the freezing of the fraction from causing the heat exchanger to be blocked, thereby increasing the pressure of the reactor and posing a safety hazard. The temperature of the heat transfer oil can be intelligently controlled to be constant through TCU, and there is no need for personnel to frequently control the opening of the control valve of the cooling medium, thereby ensuring safety and improving the solvent recovery rate.

[0026] As a preferred embodiment 2, the reaction module 1 includes a reactor 101 and a stirring paddle 102 arranged in the reactor 101, and the steam outlet of the reactor 101 is connected to the reflux port of the reactor 101 through the condensation module 2 to form a circulating cooling coordination.

[0027] Example 2 provides a specific structure of the reaction module 1. Because the metallic sodium needs to be stirred and dispersed, and then diphenylphosphine chloride is added dropwise under the condition of solvent reflux, the basic structure includes a reaction kettle 101 and a corresponding stirring paddle 102.

[0028] As a preferred embodiment 3, the condensation module 2 includes a condensation inlet pipe 201, a primary heat exchanger 202 and a condensation reflux pipe 203, the feed port of the primary heat exchanger 202 is sealed connected to the steam outlet of the reactor 101 through the condensation inlet pipe 201, and the discharge port of the primary heat exchanger 202 is sealed connected to the reflux port of the reactor 101 through the condensation reflux pipe 203.

[0029] Example 3 provides a specific structure of the condensation module 2, which forms a steam circulation cooling loop through the condensation inlet pipe 201, the primary heat exchanger 202 and the condensation reflux pipe 203 connected in sequence, and the primary heat exchanger 202 cools the steam through heat transfer oil.

[0030] As a preferred embodiment 4, the heat transfer oil outlet of the primary heat exchanger 202 is connected to the heat transfer oil inlet of the primary heat exchanger 202 through the cryogenic TCU module 3 to form a circulating secondary cooling cooperation. The cryogenic TCU module 3 cools the heat transfer oil and provides the heat transfer oil at a constant temperature after cooling for steam cooling.

[0031] As a preferred embodiment 5, the deep-cold TCU module 3 includes a secondary heat exchanger 302 and a TCU temperature control system 304. The feed port of the secondary heat exchanger 302 is sealedly connected to the heat transfer oil outlet of the primary heat exchanger 202 through an oil inlet pipe 301, the discharge port of the secondary heat exchanger 302 is sealedly connected to the liquid inlet of the TCU temperature control system 304 through a connecting pipe 303, the liquid outlet of the TCU temperature control system 304 is sealedly connected to the heat transfer oil inlet of the primary heat exchanger 202 through an oil outlet pipe 305, and the temperature of the heat transfer oil in the oil outlet pipe 305 forms a temperature control coordination with the TCU temperature control system 304.

[0032] Example 5 provides a specific structure of a deep-cooling TCU module 3, performs primary cooling of the heat transfer oil through a secondary heat exchanger 302, performs secondary cooling through a TCU temperature control system 304 and controls the temperature of the output heat transfer oil after cooling, provides constant temperature heat transfer oil to the primary heat exchanger 202, and ensures stable operation of steam cooling.

[0033] As a preferred embodiment 6, the temperature of the heat transfer oil in the oil outlet pipe 305 is 15° C. This ensures that the temperature of the heat transfer oil provided to the primary heat exchanger 202 is always greater than the melting point of the solvent, thereby preventing the steam from freezing during the cooling process and blocking the primary heat exchanger 202, thereby posing a potential safety hazard.

[0034] As a preferred embodiment 7, the cooling medium of the secondary heat exchanger 302 is water. The secondary heat exchanger 302 uses water cooling to preliminarily cool the heat transfer oil and reduce the heat exchange energy consumption of the TCU temperature control system 304.

[0035] As a preferred embodiment 8, as a preferred embodiment 8, the hot water inlet and the hot water outlet of the secondary heat exchanger 302 are connected through an external cooling water circulation system, and the temperature of water provided by the external cooling water circulation system is 7° C. to ensure cooling efficiency.

[0036] The working principle of this utility model:

[0037] The utility model provides a reaction cooling system for preparing methyl 2-(diphenylphosphino)benzoate. The reaction adopts metallic sodium and diphenylphosphine chloride as raw materials, 1,4-dioxane as solvent, the reaction is carried out in a reaction module 1, steam is generated in the process, the steam is cooled and circulated through a condensation module 2 and then flows back to the reaction module 1, the condensation module 2 adopts constant temperature heat transfer oil for cooling, and a deep cooling TCU module 3 cools the heat transfer oil and provides constant temperature heat transfer oil to the condensation module 2 through the TCU, so as to prevent the water in the cooler from violently reacting with metallic sodium and causing explosion when the water leaks inside, and the temperature in the condensation module 2 is always higher than the temperature of the solvent through the TCU, so as to prevent the freezing of the fraction from causing the blockage of the heat exchanger and thus increasing the pressure of the reactor, which poses a safety hazard, and the temperature of the heat transfer oil can be intelligently controlled to be constant through the TCU, without the need for personnel to frequently control the opening of a control valve of the cooling medium, thereby ensuring safety and improving the solvent recovery rate.

Claims

1. A reaction cooling system for the preparation of methyl 2-(diphenylphosphino)benzoate, characterized in that: The invention comprises a reaction module (1), a condensation module (2) and a cryogenic TCU module (3); the steam outlet of the reaction module (1) is connected to a reflux port via the condensation module (2) to form a circulating cooling combination; the cooling medium of the condensation module (2) is heat transfer oil; the heat transfer oil outlet of the condensation module (2) is connected to a heat transfer oil inlet via the cryogenic TCU module (3) to form a circulating secondary cooling combination; the cryogenic TCU module (3) forms a temperature control combination with the heat transfer oil at the heat transfer oil inlet.

2. The reaction cooling system for preparing methyl 2-(diphenylphosphino)benzoate according to claim 1, characterized in that: The reaction module (1) comprises a reaction kettle (101) and a stirring paddle (102) arranged in the reaction kettle (101); the steam outlet of the reaction kettle (101) is connected to the reflux port of the reaction kettle (101) through the condensation module (2) to form a circulating cooling system.

3. The reaction cooling system for preparing methyl 2-(diphenylphosphino)benzoate according to claim 2, characterized in that: The condensation module (2) comprises a condensation air inlet pipe (201), a primary heat exchanger (202) and a condensation reflux pipe (203); the feed port of the primary heat exchanger (202) is sealedly connected to the steam outlet of the reactor (101) via the condensation air inlet pipe (201); and the discharge port of the primary heat exchanger (202) is sealedly connected to the reflux port of the reactor (101) via the condensation reflux pipe (203).

4. The reaction cooling system for preparing methyl 2-(diphenylphosphino)benzoate according to claim 3, characterized in that: The heat transfer oil outlet of the primary heat exchanger (202) is connected to the heat transfer oil inlet of the primary heat exchanger (202) via the deep cooling TCU module (3) to form a circulating secondary cooling system.

5. The reaction cooling system for preparing methyl 2-(diphenylphosphino)benzoate according to claim 4, characterized in that: The cryogenic TCU module (3) comprises a secondary heat exchanger (302) and a TCU temperature control system (304); the feed port of the secondary heat exchanger (302) is sealedly connected to the heat transfer oil outlet of the primary heat exchanger (202) via an oil inlet pipe (301); the discharge port of the secondary heat exchanger (302) is sealedly connected to the liquid inlet of the TCU temperature control system (304) via a connecting pipe (303); the liquid outlet of the TCU temperature control system (304) is sealedly connected to the heat transfer oil inlet of the primary heat exchanger (202) via an oil outlet pipe (305); and the temperature of the heat transfer oil in the oil outlet pipe (305) forms a temperature control match with that of the TCU temperature control system (304).

6. The reaction cooling system for preparing methyl 2-(diphenylphosphino)benzoate according to claim 5, characterized in that: The temperature of the heat transfer oil in the oil outlet pipe (305) is 15°C.

7. The reaction cooling system for preparing methyl 2-(diphenylphosphino)benzoate according to claim 6, characterized in that: The cooling medium of the secondary heat exchanger (302) is water.

8. The reaction cooling system for preparing methyl 2-(diphenylphosphino)benzoate according to claim 7, characterized in that: The hot water inlet and the hot water outlet of the secondary heat exchanger (302) are connected via an external cooling water circulation system, and the temperature of water provided by the external cooling water circulation system is 7°C.

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