A system for the preparation of mpo

Abstract

The utility model discloses a preparation system of MPO belongs to phospholene preparation technical field, including the first reation kettle and second reation kettle of being connected, be equipped with methyl dichlorophosphine feed pipe, butadiene feed pipe normal butanol feed pipe and methyl dichlorophosphine steam pipe on the first reation kettle, be equipped with chlorobutane steam pipe on the second reation kettle. Three kinds of materials enter the first reation kettle, then flow into the second reation kettle, 3 - methyl - 1 - phosphorus heterocyclic hex - 3 - en - 1 - chloride and normal butanol are reacted and get 1 - methyl - 1 - oxo - 2, 3 - dihydro - phospholene (MPO), chlorobutane and hydrogen chloride, and chlorobutane is produced and hangs distillation and comes out chlorobutane through chlorobutane steam pipe, and 3 - methyl - 1 - phosphorus heterocyclic hex - 3 - en - 1 - chloride isomerized into 2 position MPO under high temperature.

Description

Technical Field

[0001] This invention belongs to the field of phosphorocyclopentene preparation technology, specifically relating to an MPO preparation system. Background Technology

[0002] 1-Methyl-1-oxo-2,3-dihydrophosphacyclopentene (MPO) is a highly efficient catalyst mainly used in the synthesis of carbodiimides, polycarbodiimides, and modified carbodiimide isocyanates, as well as in phosgenation synthesis. Currently, there are no domestic R&D and manufacturing companies specializing in this product, leaving the domestic market largely untapped. The goal is to produce this product domestically and establish a foothold in the market. Conventional production methods primarily yield 3-position MPO, while 2-position MPO exhibits superior performance. A preparation system with a high 2-position MPO content is currently lacking. Utility Model Content

[0003] The purpose of this invention is to solve the problems of the prior art and provide an MPO preparation system. Methylphosphine dichloride and butadiene flow into the first reaction vessel through the methylphosphine dichloride feed pipe and the butadiene feed pipe, respectively. The methylphosphine dichloride and butadiene react to obtain 3-methyl-1-phosphacyclohex-3-ene-1-chloride, resulting in a mixture of 3-methyl-1-phosphacyclohex-3-ene-1-chloride and methylphosphine dichloride. The methylphosphine dichloride is then recovered under reduced pressure through the methylphosphine dichloride distillation pipe. After phosphine chloride is discharged, n-butanol is added to the first reactor through the n-butanol feed pipe to fully dissolve the solid, and then flows into the second reactor. 3-methyl-1-phosphacyclohex-3-ene-1-chloride reacts with n-butanol to obtain 1-methyl-1-oxo-2,3-dihydrophosphacyclopentene (MPO), chlorobutane, and hydrogen chloride. Chlorobutane is distilled off through the chlorobutane distillation pipe. 3-methyl-1-phosphacyclohex-3-ene-1-chloride is isomerized to MPO at the 2-position at high temperature.

[0004] This utility model is achieved through the following technical solution: An MPO preparation system includes a first reaction vessel and a second reaction vessel connected together. The first reaction vessel is provided with a methylphosphine dichloride feed pipe, a butadiene feed pipe, a n-butanol feed pipe, and a methylphosphine dichloride evaporation pipe. The second reaction vessel is provided with a chlorobutane evaporation pipe.

[0005] Preferably, the first reactor is connected to the second reactor via a feed pipe.

[0006] Preferably, the first reactor is provided with a first temperature control unit, which includes a first temperature sensor and a first heat exchange jacket on the first reactor. The first heat exchange jacket is provided with a first heat exchange inlet pipe and a first heat exchange outlet pipe, and the first heat exchange inlet pipe is provided with a first heat exchange valve.

[0007] Preferably, the second reactor is provided with a second temperature control unit, which includes a second temperature sensor and a second heat exchange jacket. The second heat exchange jacket is provided with a second heat exchange inlet pipe and a second heat exchange outlet pipe, and the second heat exchange inlet pipe is provided with a second heat exchange valve.

[0008] Preferably, the first reactor is provided with a first stirring device, and the second reactor is provided with a second stirring device.

[0009] Preferably, the first reactor is equipped with a first pressure gauge, and the second reactor is equipped with a second pressure gauge.

[0010] Preferably, the methyl dichloride evaporation pipe is equipped with a methyl dichloride cooler, a methyl dichloride storage tank, and a first exhaust pipe.

[0011] Preferably, the chlorobutane distillation pipe is equipped with a chlorobutane cooler, a chlorobutane storage tank, and a second exhaust pipe.

[0012] Preferably, the first exhaust pipe and the second exhaust pipe are connected to the exhaust manifold, and a vacuum pump is installed on the exhaust manifold.

[0013] Preferably, the feed pipe, the methyl dichloride feed pipe, the butadiene feed pipe, the n-butanol feed pipe, the methyl dichloride distillation pipe, the chlorobutane distillation pipe, the first exhaust pipe, and the second exhaust pipe are all equipped with switch valves, and the methyl dichloride feed pipe, the butadiene feed pipe, and the n-butanol feed pipe are all equipped with flow meters.

[0014] Compared with the prior art, this utility model has the following advantages and beneficial effects: I. This utility model provides an MPO preparation system in which methylphosphine dichloride and butadiene flow into a first reaction vessel through methylphosphine dichloride feed pipe and butadiene feed pipe, respectively. The methylphosphine dichloride and butadiene react to obtain 3-methyl-1-phosphacyclohexane-3-ene-1-chloride, resulting in a mixture of 3-methyl-1-phosphacyclohexane-3-ene-1-chloride and methylphosphine dichloride. After methylphosphine dichloride is recovered under reduced pressure through a methylphosphine dichloride distillation pipe, the mixture is then... Butanol is added to the first reactor through the n-butanol feed pipe to fully dissolve the solid, and then flows into the second reactor. 3-methyl-1-phosphacyclohex-3-ene-1-chloride reacts with n-butanol to give 1-methyl-1-oxo-2,3-dihydrophosphacyclopentene (MPO), chlorobutane, and hydrogen chloride. Chlorobutane is distilled off through the chlorobutane distillation pipe. 3-methyl-1-phosphacyclohex-3-ene-1-chloride is isomerized to MPO at the 2-position at high temperature.

[0015] II. The MPO preparation system provided by this utility model has a first temperature control unit that facilitates the adjustment of the temperature inside the first reaction vessel, so that the reaction between methylphosphine dichloride and butadiene to obtain 3-methyl-1-phosphacyclohex-3-ene-1-chloride is more complete. III. The MPO preparation system provided by this utility model has a second temperature control unit that facilitates the adjustment of the temperature inside the second reaction vessel, resulting in a more thorough reaction of 3-methyl-1-phosphacyclohex-3-ene-1-chloride with n-butanol to obtain 1-methyl-1-oxo-2,3-dihydro-phosphacyclopentene (MPO), chlorobutane, and hydrogen chloride; more thorough recovery of methylphosphine dichloride; more thorough distillation of chlorobutane; and better high-temperature isomerization of 1-methyl-1-oxo-2,3-dihydro-phosphacyclopentene.

[0016] IV. The MPO preparation system provided by this utility model, with the configuration of a methylphosphine dichloride cooler, a methylphosphine dichloride storage tank, a chlorobutane cooler, and a chlorobutane storage tank, makes the recovery of methylphosphine dichloride more thorough and the distillation of chlorobutane more thorough.

[0017] V. The MPO preparation system provided by this utility model, with its switch valve and flow meter settings, enables more precise feeding of methylphosphine dichloride, butadiene, and n-butanol, and more thorough distillation of methylphosphine dichloride and chlorobutane. Attached Figure Description

[0018] Figure 1 This is a schematic diagram of the structure of this utility model; Figure 2 This is a schematic diagram of the structure of Embodiment 2 of this utility model.

[0019] The components are: 1. First reactor; 2. Second reactor; 3. Methylphosphine dichloride feed pipe; 4. Butadiene feed pipe; 5. n-Butanol feed pipe; 6. Methylphosphine dichloride distillation pipe; 7. Chlorobutane distillation pipe; 8. Feed pipe; 9. First temperature sensor; 10. First heat exchange jacket; 11. First heat exchange inlet pipe; 12. First heat exchange outlet pipe; 13. First heat exchange valve; 14. Second temperature sensor; 15. Second heat exchange jacket; 16. Second heat exchange valve. 17. Inlet pipe; 18. Second heat exchange outlet pipe; 19. Second heat exchange valve; 20. First stirring device; 21. Second stirring device; 22. First pressure gauge; 23. Methylphosphine dichloride cooler; 24. Methylphosphine dichloride storage tank; 25. First exhaust pipe; 26. Chlorobutane cooler; 27. Chlorobutane storage tank; 28. Second exhaust pipe; 29. ​​Main exhaust pipe; 30. Vacuum pump; 31. Switch valve; 32. Flow meter. Detailed Implementation

[0020] The present invention will be further described in detail below with reference to the embodiments, but the implementation of the present invention is not limited thereto.

[0021] Example 1 like Figure 1 As shown, this embodiment provides an MPO preparation system, including a first reaction vessel 1 and a second reaction vessel 2 connected together. The first reaction vessel 1 is provided with a methyl dichloride feed pipe 3, a butadiene feed pipe 4, a n-butanol feed pipe 5 and a methyl dichloride distillation pipe 6, and the second reaction vessel 2 is provided with a chlorobutane distillation pipe 7.

[0022] Example 2 like Figure 2 As shown, this embodiment provides an MPO preparation system, including a first reaction vessel 1 and a second reaction vessel 2 connected together. The first reaction vessel 1 is provided with a methyl dichloride feed pipe 3, a butadiene feed pipe 4, a n-butanol feed pipe 5 and a methyl dichloride distillation pipe 6, and the second reaction vessel 2 is provided with a chlorobutane distillation pipe 7.

[0023] The first reactor 1 is connected to the second reactor 2 via a feed pipe 8.

[0024] The first reaction vessel 1 is provided with a first temperature control unit, which includes a first temperature sensor 9 and a first heat exchange jacket 10. The first heat exchange jacket 10 is provided with a first heat exchange inlet pipe 11 and a first heat exchange outlet pipe 12. The first heat exchange inlet pipe 11 is provided with a first heat exchange valve 13.

[0025] The second reaction vessel 2 is provided with a second temperature control unit, which includes a second temperature sensor 14 and a second heat exchange jacket 15. The second heat exchange jacket 15 is provided with a second heat exchange inlet pipe 16 and a second heat exchange outlet pipe 17. The second heat exchange inlet pipe 16 is provided with a second heat exchange valve 18.

[0026] The first reaction vessel 1 is equipped with a first stirring device 19, and the second reaction vessel 2 is equipped with a second stirring device 20.

[0027] The first reactor 1 is equipped with a first pressure gauge 21, and the second reactor 2 is equipped with a second pressure gauge 22.

[0028] The methyl dichloride evaporation pipe 6 is equipped with a methyl dichloride cooler 23, a methyl dichloride storage tank 24, and a first exhaust pipe 25.

[0029] The chlorobutane distillation pipe 7 is equipped with a chlorobutane cooler 26, a chlorobutane storage tank 27, and a second exhaust pipe 28.

[0030] The first exhaust pipe 25 and the second exhaust pipe 28 are connected to the exhaust manifold 29, and a vacuum pump 30 is installed on the exhaust manifold 29.

[0031] Among them, the feed pipe 8, the methyl dichloride feed pipe 3, the butadiene feed pipe 4, the n-butanol feed pipe 5, the methyl dichloride distillation pipe 6, the chlorobutane distillation pipe 7, the first exhaust pipe 25 and the second exhaust pipe 28 are all equipped with switch valves 31, and the methyl dichloride feed pipe 3, the butadiene feed pipe 4 and the n-butanol feed pipe 5 are all equipped with flow meters 32.

[0032] Among them, the first temperature sensor 9, the first heat exchange jacket 10, the first heat exchange valve 13, the second temperature sensor 14, the second heat exchange jacket 15, the second heat exchange valve 18, the first stirring device 19, the second stirring device 20, the first pressure gauge 21, the second pressure gauge 22, the methylphosphine dichloride cooler 23, the methylphosphine dichloride storage tank 24, the chlorobutane cooler 26, the chlorobutane storage tank 27, the vacuum pump 30, the switching valve 31, and the flow meter 32 are all prior art and will not be described in detail here.

[0033] Compared with the prior art, this utility model has the following advantages and beneficial effects: I. This utility model provides an MPO preparation system in which methylphosphine dichloride and butadiene flow into a first reaction vessel 1 through methylphosphine dichloride feed pipe 3 and butadiene feed pipe 4, respectively. The methylphosphine dichloride and butadiene react to obtain 3-methyl-1-phosphacyclohexane-3-ene-1-chloride, resulting in a mixture of 3-methyl-1-phosphacyclohexane-3-ene-1-chloride and methylphosphine dichloride. After methylphosphine dichloride is recovered under reduced pressure through methylphosphine distillation pipe 6, the mixture is then... Butanol is added to the first reactor 1 through the n-butanol feed pipe 5 to fully dissolve the solid, and then flows into the second reactor 2. 3-methyl-1-phosphacyclohex-3-ene-1-chloride reacts with n-butanol to obtain 1-methyl-1-oxo-2,3-dihydrophosphacyclopentene (MPO), chlorobutane, and hydrogen chloride. Chlorobutane is distilled off through the chlorobutane distillation pipe 7. 3-methyl-1-phosphacyclohex-3-ene-1-chloride is isomerized to MPO at the 2-position at high temperature.

[0034] II. The MPO preparation system provided by this utility model has a first temperature control unit that facilitates the adjustment of the temperature inside the first reaction vessel 1, so that the reaction of methylphosphine dichloride and butadiene to obtain 3-methyl-1-phosphacyclohex-3-ene-1-chloride is more thorough. III. The MPO preparation system provided by this utility model has a second temperature control unit that facilitates the adjustment of the temperature inside the second reaction vessel 2, resulting in a more thorough reaction of 3-methyl-1-phosphacyclohex-3-ene-1-chloride with n-butanol to obtain 1-methyl-1-oxo-2,3-dihydro-phosphacyclopentene (MPO), chlorobutane, and hydrogen chloride; more thorough recovery of methylphosphine dichloride; more thorough distillation of chlorobutane; and better high-temperature isomerization effect of 1-methyl-1-oxo-2,3-dihydro-phosphacyclopentene.

[0035] IV. The MPO preparation system provided by this utility model, with the setting of methyl dichloride cooler 23, methyl dichloride storage tank 24, chlorobutane cooler 26 and chlorobutane storage tank 27, makes the recovery of methyl dichloride more thorough and the distillation of chlorobutane more thorough.

[0036] V. The MPO preparation system provided by this utility model, with the setting of the switching valve 31 and the flow meter 32, makes the feeding of methylphosphine dichloride, butadiene and n-butanol more precise, and the distillation of methylphosphine dichloride and chlorobutane more thorough.

[0037] The above description is merely a preferred embodiment of the present utility model and is not intended to limit the present utility model in any way. Any simple modifications or equivalent changes made to the above embodiments based on the technical essence of the present utility model shall fall within the protection scope of the present utility model.

Claims

1. A system for preparing MPO, characterized in that: The reactor includes a first reactor (1) and a second reactor (2) connected to each other. The first reactor (1) is equipped with a methyl dichloride feed pipe (3), a butadiene feed pipe (4), a n-butanol feed pipe (5) and a methyl dichloride distillation pipe (6). The second reactor (2) is equipped with a chlorobutane distillation pipe (7).

2. The MPO preparation system according to claim 1, characterized in that: The first reactor (1) is connected to the second reactor (2) through the feed pipe (8).

3. The MPO preparation system according to claim 2, characterized in that: The first reaction vessel (1) is provided with a first temperature control unit. The first temperature control unit includes a first temperature sensor (9) and a first heat exchange jacket (10) on the first reaction vessel (1). The first heat exchange jacket (10) is provided with a first heat exchange inlet pipe (11) and a first heat exchange outlet pipe (12). The first heat exchange inlet pipe (11) is provided with a first heat exchange valve (13).

4. The MPO preparation system according to claim 3, characterized in that: The second reaction vessel (2) is provided with a second temperature control unit. The second temperature control unit includes a second temperature sensor (14) provided on the second reaction vessel (2) and a second heat exchange jacket (15) provided on the second reaction vessel (2). The second heat exchange jacket (15) is provided with a second heat exchange inlet pipe (16) and a second heat exchange outlet pipe (17). The second heat exchange inlet pipe (16) is provided with a second heat exchange valve (18).

5. The MPO preparation system according to claim 4, characterized in that: The first reactor is equipped with a first stirring device (19), and the second reactor is equipped with a second stirring device (20).

6. The MPO preparation system according to claim 5, characterized in that: The first reactor is equipped with a first pressure gauge (21), and the second reactor is equipped with a second pressure gauge (22).

7. The MPO preparation system according to claim 6, characterized in that: The methyl dichloride evaporation pipe (6) is equipped with a methyl dichloride cooler (23), a methyl dichloride storage tank (24), and a first exhaust pipe (25).

8. The MPO preparation system according to claim 7, characterized in that: The chlorobutane distillation pipe (7) is equipped with a chlorobutane cooler (26), a chlorobutane storage tank (27), and a second exhaust pipe (28).

9. The MPO preparation system according to claim 8, characterized in that: The first exhaust pipe (25) and the second exhaust pipe (28) are connected to the exhaust manifold (29), and a vacuum pump (30) is installed on the exhaust manifold (29).

10. The MPO preparation system according to claim 9, characterized in that: A switch valve (31) is provided on the feed pipe (8), methyl dichloride feed pipe (3), butadiene feed pipe (4), n-butanol feed pipe (5), methyl dichloride distillation pipe (6), chlorobutane distillation pipe (7), first exhaust pipe (25) and second exhaust pipe (28), and a flow meter (32) is provided on the methyl dichloride feed pipe (3), butadiene feed pipe (4) and n-butanol feed pipe (5).

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