CN212610370U - Continuous synthesis device of triphenylphosphine intermediate phenyl magnesium chloride - Google Patents

Abstract

The utility model discloses a continuous synthesis device of triphenyl phosphine midbody phenyl magnesium chloride belongs to the synthetic field of medical midbody. The continuous synthesis device of the triphenylphosphine intermediate phenylmagnesium chloride comprises a dryer, a solvent mixing kettle, a mixed solvent storage tank, a magnesium scrap feeder, a condenser, a primary reaction kettle, a secondary reaction kettle, a reaction liquid cooling kettle, a phenylmagnesium chloride storage tank and a chlorobenzene adding channel; the utility model discloses it is remaining that no magnesium bits is left in the reagent reaction liquid after the one-level reation kettle reaction is accomplished, has reduced the risk that produces hydrogen on next step, and whole process shortens reaction flow, reduces the equipment investment, and the energy consumption effectively reduces, reduces the risk, improves factor of safety, forms an efficient green technology.

Description

Continuous synthesis device of triphenylphosphine intermediate phenyl magnesium chloride

Technical Field

The utility model relates to a synthetic technical field of medicine intermediate especially relates to continuous synthesis device of triphenyl phosphorus intermediate phenyl magnesium chloride.

Background

At present, phenylmagnesium chloride is a key raw material for synthesizing triphenylphosphine, and the method mainly adopts intermittent production, has low efficiency, large equipment investment, high production risk and complex process.

In the actual production, the mixed solution of half toluene and tetrahydrofuran is firstly added at low temperature, then magnesium chips are added, the temperature is controlled to be about 60 ℃, chlorobenzene is slowly dripped to initiate reaction, the risk of the stage is high, and the material is easily flushed due to improper control. After the reaction is initiated, adding the other half of the mixed solution, continuously dropwise adding chlorobenzene for reaction, finishing the addition of the chlorobenzene, slowly raising the temperature to 90 ℃, and then preserving the temperature for reaction for 2 hours until the reaction is finished.

After the reaction is finished, standing to settle magnesium chip solids, transferring the magnesium chip solids to a reaction liquid to react with phosphorus trichloride in the next step, and introducing unreacted magnesium chips in the process can easily generate hydrogen to easily cause fire, so that the disadvantages of long reaction time, low equipment utilization rate and the like can be caused by slow dropwise addition at low temperature, solvent adding in times, low-temperature reaction sections and the like.

SUMMERY OF THE UTILITY MODEL

The utility model aims at solving the problems in the prior art and providing a continuous synthesis device of triphenylphosphine intermediate phenylmagnesium chloride.

In order to achieve the above purpose, the utility model adopts the following technical scheme:

continuous synthesizer of triphenyl phosphorus midbody phenyl magnesium chloride, add the passageway including desicator, solvent mixing kettle, mixed solvent storage tank, magnesium bits charging means, condenser, one-level reation kettle, second grade reation kettle, reaction liquid cooling cauldron, phenyl magnesium chloride holding vessel and chlorobenzene, desicator, solvent mixing kettle, mixed solvent storage tank, one-level reation kettle, second grade reation kettle, reaction liquid cooling cauldron, phenyl magnesium chloride holding vessel pass through the pipeline and link to each other in proper order, magnesium bits charging means discharge gate is connected on one-level reation kettle's feed inlet, the chlorobenzene adds the passageway discharge gate and connects on one-level reation kettle's feed inlet.

Preferably, the first-stage reaction kettle, the second-stage reaction kettle and the reaction liquid cooling kettle are all connected with condensers.

Preferably, stirrers are arranged in the solvent mixing kettle, the first-stage reaction kettle, the second-stage reaction kettle and the reaction liquid cooling kettle.

Preferably, the solvent in the mixed solvent storage tank is a mixed solvent of toluene and tetrahydrofuran with the volume of 1: 1.

Preferably, the reaction temperature of the first-stage reaction kettle is 95-100 ℃.

Compared with the prior art, the utility model provides a continuous synthesis device of triphenyl phosphine midbody phenyl magnesium chloride possesses following beneficial effect:

1. the continuous synthesis device of the triphenylphosphine intermediate phenylmagnesium chloride utilizes the continuous reaction equipment and design to carry out uninterrupted feeding reaction, saves each batch of initiation section and batch feeding process, and improves the reaction temperature;

2. the utility model adds the dryer to dewater the mixed solvent, ensures the water content of the solvent to be below 0.2 percent, is simple and efficient; the dosage of the magnesium chips is reduced from 1.15 equivalent to 1.04 equivalent by 10 percent;

3. the process simplifies the reaction flow, shortens the reaction time, improves the utilization rate of equipment, and has the production capacity 3.6 times of that of batch reaction under the same condition of continuous operation; meanwhile, the process safety is improved; magnesium chips are not left in the reaction liquid after the reaction of the first-stage reaction kettle is finished, so that the risk of generating hydrogen in the next step is reduced.

4. The utility model discloses shortened reaction flow, reduced the equipment investment, the energy consumption also effectively reduces, has improved factor of safety, is an efficient green technology.

Drawings

FIG. 1 is a schematic view of a part of a system of a continuous synthesis device for triphenylphosphine intermediate phenylmagnesium chloride;

FIG. 2 is a schematic view of a part of the system of the continuous synthesis device of triphenylphosphine intermediate phenylmagnesium chloride.

1. A dryer; 2. a solvent mixing kettle; 3. a mixed solvent storage tank; 4. a magnesium scrap feeder; 5. a condenser; 6. a first-stage reaction kettle; 7. a second-stage reaction kettle; 8. cooling the reaction solution in a kettle; 9. a phenylmagnesium chloride storage tank; 10. chlorobenzene addition channel.

Detailed Description

The technical solutions in the embodiments of the present invention will be described clearly and completely with reference to the accompanying drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only some embodiments of the present invention, not all embodiments.

In the description of the present invention, it is to be understood that the terms "upper", "lower", "front", "rear", "left", "right", "top", "bottom", "inner", "outer", and the like indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, and are only for convenience of description and simplicity of description, and do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and therefore, should not be construed as limiting the present invention.

Referring to fig. 1-2, a continuous synthesis device of triphenylphosphine intermediate phenylmagnesium chloride comprises a dryer 1, a solvent mixing kettle 2, a mixed solvent storage tank 3, a magnesium scrap feeder 4, a condenser 5, a primary reaction kettle 6, a secondary reaction kettle 7, a reaction liquid cooling kettle 8, a phenylmagnesium chloride storage tank 9 and a chlorobenzene adding channel 10, wherein the dryer 1, the solvent mixing kettle 2, the mixed solvent storage tank 3, the primary reaction kettle 6, the secondary reaction kettle 7, the reaction liquid cooling kettle 8 and the phenylmagnesium chloride storage tank 9 are sequentially connected through a pipeline, a discharge hole of the magnesium scrap feeder 4 is connected to a feed inlet of the primary reaction kettle 6, and a discharge hole of the chlorobenzene adding channel 10 is connected to a feed inlet of the primary reaction kettle 6;

by utilizing the continuous reaction equipment and design, the utility model can carry out uninterrupted feeding reaction, save initiation working sections and batch feeding processes of each batch, and improve the reaction temperature; meanwhile, the dryer 1 is added for dehydrating the mixed solvent, so that the moisture of the solvent is ensured to be below 0.2 percent, and the method is simple and efficient; the consumption of the magnesium chips is reduced from the original 1.15 equivalent to 1.04 equivalent by 10 percent; the process simplifies the reaction flow, shortens the reaction time, improves the utilization rate of equipment, and has the continuous production capacity 3.6 times of the production capacity of the batch reaction under the same condition; meanwhile, the process safety is improved; magnesium chips in a reagent reaction solution after the reaction of the first-stage reaction kettle 6 is completed are basically not contained, the risk of hydrogen generation in the next step is reduced, the whole process is shortened, the equipment investment is reduced, the energy consumption is effectively reduced, the risk is reduced, the safety coefficient is improved, and an efficient green process is formed.

The first-stage reaction kettle 6, the second-stage reaction kettle 7 and the reaction liquid cooling kettle 8 are all connected with a condenser 5 for controlling the temperature.

The solvent mixing kettle 2, the first-stage reaction kettle 6, the second-stage reaction kettle 7 and the reaction liquid cooling kettle 8 are all provided with stirrers, so that the uniform mixing and stirring reaction is ensured.

The solvent in the mixed solvent storage tank 3 is a mixed solvent of toluene and tetrahydrofuran with the volume of 1: 1; the reaction temperature of the first-stage reaction kettle 6 is 95-100 ℃.

Comparative example 1:

putting 2600L of toluene and tetrahydrofuran mixed solvent (the volume ratio is 1:1, the water content is lower than 0.2%) into a 10000L reaction kettle, then putting 360 kg of magnesium chips, heating to 60 ℃, slowly dropwise adding (according to chlorobenzene 250L/h) for initiating reaction, dropwise adding 1 h for initiating normally, then putting the rest 2600L of toluene and tetrahydrofuran mixed solvent into the reaction kettle, dropwise adding chlorobenzene (according to 300L/h) into the reaction kettle, completely adding 1300L of chlorobenzene for 4-5 h, simultaneously controlling the temperature to slowly rise to 90-93 ℃, keeping the temperature for 2 h, sampling and analyzing that the chlorobenzene content is lower than 1%, finishing the reaction, cooling to 30 ℃, stopping stirring, standing and settling magnesium chips, and transferring from the upper part to the next step; the whole batch takes 12 hours from the feeding to the end of the transferring.

Example 1:

the process comprises the following steps of connecting three kettles, wherein a first-stage reaction kettle 6, a second-stage reaction kettle 7 and a reaction liquid cooling kettle 8 are continuous, the first two stages are reaction kettles, the second stage is a cooling kettle, the first-stage reaction kettle 6 and the second-stage reaction kettle 7 are subjected to batch reaction to produce two batches of qualified reaction liquid by adopting a comparison case 1, the temperature is kept at 95 ℃, and simultaneously, a mixed solvent of toluene and tetrahydrofuran (the volume ratio is 1:1, the water content is lower than 0.2%) per hour is adopted: chlorobenzene: magnesium chips 1200L: 300L: feeding 75kg of raw materials according to a proportion, controlling the reaction temperature to be 95-100 ℃, and after the continuous reaction is carried out for 24 hours, sampling chlorobenzene content GC at the outlet of a 2-level kettle: 0.62 percent.

Example 2:

the procedure of example 1 was followed, and the amounts of the feed were adjusted to simultaneously obtain a mixed solvent of toluene and tetrahydrofuran (1: 1 by volume, water content less than 0.2%) per hour: chlorobenzene: magnesium chips 2400L: 600L: 150kg, controlling the reaction temperature to be 95-100 ℃, and after continuously reacting for 24 hours, sampling the chlorobenzene content GC at the outlet of the secondary reaction kettle 7: 0.68 percent.

Example 3:

the procedure of example 1 was followed, and the amounts of the feed were adjusted to simultaneously obtain a mixed solvent of toluene and tetrahydrofuran (1: 1 by volume, water content less than 0.2%) per hour: chlorobenzene: magnesium chips 3600L: 900L: 225kg, controlling the reaction temperature to be 95-100 ℃, and after continuously reacting for 24 hours, sampling the chlorobenzene content GC at the kettle outlet of the secondary reaction kettle 7: 0.84 percent.

Example 4:

the procedure of example 1 was followed, and the amounts of the feed were adjusted to simultaneously obtain a mixed solvent of toluene and tetrahydrofuran (1: 1 by volume, water content less than 0.2%) per hour: chlorobenzene: magnesium chips 4800L: 1200L: 300kg, controlling the reaction temperature to be 95-100 ℃, and after continuously reacting for 24 hours, sampling the chlorobenzene content GC at the outlet of the secondary reaction kettle 7: 0.98 percent.

Example 5:

the procedure of example 1 was followed, and the amounts of the feed were adjusted to simultaneously obtain a mixed solvent of toluene and tetrahydrofuran (1: 1 by volume, water content less than 0.2%) per hour: chlorobenzene: magnesium chips 4800L: 1200L: 300kg, controlling the reaction temperature to be 110-: 0.8 percent, but the content of impurities is higher than 2.5 percent, and the reflux quantity is too large, so the material is easy to wash.

Example 6:

the procedure of example 1 was followed, and the amounts of the feed were adjusted to simultaneously obtain a mixed solvent of toluene and tetrahydrofuran (1: 1 by volume, water content less than 0.2%) per hour: chlorobenzene: magnesium chips 3600L: 900L: 216kg, controlling the reaction temperature to be 95-100 ℃, and after the continuous reaction is carried out for 24 hours, sampling the chlorobenzene content GC at the outlet of the secondary reaction kettle 7: 1.5 percent.

The above, only be the concrete implementation of the preferred embodiment of the present invention, but the protection scope of the present invention is not limited thereto, and any person skilled in the art is in the technical scope of the present invention, according to the technical solution of the present invention and the utility model, the concept of which is equivalent to replace or change, should be covered within the protection scope of the present invention.

Claims (4)

1. A continuous synthesis device of triphenylphosphine intermediate phenylmagnesium chloride is characterized by comprising a dryer (1), a solvent mixing kettle (2), a mixed solvent storage tank (3), a magnesium scrap feeder (4), a condenser (5), a primary reaction kettle (6), a secondary reaction kettle (7), a reaction liquid cooling kettle (8), a phenylmagnesium chloride storage tank (9) and a chlorobenzene adding channel (10), the dryer (1), the solvent mixing kettle (2), the mixed solvent storage tank (3), the primary reaction kettle (6), the secondary reaction kettle (7), the reaction liquid cooling kettle (8) and the phenyl magnesium chloride storage tank (9) are connected in sequence through pipelines, the discharge hole of the magnesium scrap feeder (4) is connected with the feed hole of the first-stage reaction kettle (6), and the discharge hole of the chlorobenzene adding channel (10) is connected to the feed inlet of the first-stage reaction kettle (6).

2. The continuous synthesis device of triphenylphosphine intermediate phenylmagnesium chloride according to claim 1, wherein the first-stage reaction vessel (6), the second-stage reaction vessel (7) and the reaction solution cooling vessel (8) are connected with a condenser (5).

3. The continuous synthesis device of triphenylphosphine intermediate phenylmagnesium chloride according to claim 1, wherein stirrers are arranged in the solvent mixing kettle (2), the first-stage reaction kettle (6), the second-stage reaction kettle (7) and the reaction solution cooling kettle (8).

4. The continuous synthesis device of triphenylphosphine intermediate phenylmagnesium chloride according to any one of claims 1-3, wherein the reaction temperature of the primary reaction kettle (6) is 95-100 ℃.

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