CN211445574U

CN211445574U - Continuous reaction system of high-purity m/p-phthaloyl chloride

Info

Publication number: CN211445574U
Application number: CN201922494449.9U
Authority: CN
Inventors: 张聪聪; 孙丰玮; 肖广明; 张良; 刘嵩; 刘晓玉; 肖志宇; 韩楠楠
Original assignee: Shandong Kaisheng New Materials Co Ltd
Current assignee: Shandong Kaisheng New Materials Co Ltd
Priority date: 2019-12-31
Filing date: 2019-12-31
Publication date: 2020-09-08
Anticipated expiration: 2029-12-31

Abstract

The utility model relates to the technical field of organic synthesis systems, concretely relates to continuous reaction system of high-purity meta/paraphthaloyl chloride, including granulator, compounding jar and reation kettle that concatenate in proper order, reation kettle ' S gas vent external condenser, the discharge end of condenser is linked together with the feed inlet of compounding jar, reation kettle ' S inside sets up S type passageway, runs through many blast pipes on the S type passageway, and reation kettle ' S upper portion sets up the tail gas chamber, the top of blast pipe is located the tail gas intracavity, and is linked together with the tail gas chamber, the upper portion of the blast pipe that is located S type passageway inside sets up a plurality of capillary holes; the utility model discloses a continuous reaction of acyl chloride product to equipment area is little, saves space, and is simpler than intermittent type reaction operation process, and reaction equipment does not have complicated pipeline, has reduced the complexity of technology. The problem of easy crystallization of pipelines is solved, the energy consumption required by heat tracing of process pipelines is saved, and the quality of continuous reaction products is stable.

Description

Continuous reaction system of high-purity m/p-phthaloyl chloride

Technical Field

The utility model relates to an organic synthesis system technical field, concretely relates to continuous reaction system of high-purity meta/paraphthaloyl chloride.

Background

At present, a patent with the application number of 2014105170371 and the patent name of an acyl chloride continuous synthesis device and an acyl chloride continuous synthesis method discloses an acyl chloride continuous synthesis device and an acyl chloride continuous synthesis method, wherein 4 reaction kettles are arranged to realize the continuous synthesis of acyl chloride, and the method has the problems of large occupied area of equipment, high energy consumption, complex process, easy crystallization of pipelines and the like.

In addition, other similar existing devices also generally have the problems that the reaction time is long and reaction tail gas cannot be discharged in time, so that the production rate of the reaction process is severely restricted; in addition, the reaction raw material, i.e., the m/p-phthalic acid, has large particles, which affects the reaction rate.

SUMMERY OF THE UTILITY MODEL

In order to solve the defects in the technical problem, the utility model aims to provide a: the continuous reaction system of the high-purity m/p-phthaloyl chloride is provided, the discharge of reaction tail gas is better promoted, the contact area with reactants can be greatly improved, the reaction is more sufficient, and the reaction efficiency is improved; can realize continuous production, increase the productivity and reduce the energy consumption.

The utility model discloses a solve the technical scheme that its technical problem adopted and do:

the continuous reaction system of the high-purity m/p-phthaloyl chloride comprises a granulator, a mixing tank and a reaction kettle which are sequentially connected in series, wherein an exhaust port of the reaction kettle is externally connected with a condenser, a discharge end of the condenser is communicated with a feed inlet of the mixing tank, an S-shaped channel is arranged in the reaction kettle, a plurality of exhaust pipes penetrate through the S-shaped channel, the exhaust pipes are fixedly connected with the S-shaped channel, a tail gas cavity is arranged at the upper part of the reaction kettle, the top of each exhaust pipe is positioned in the tail gas cavity and communicated with the tail gas cavity, and a plurality of capillary holes are formed in the upper part of each exhaust pipe positioned in.

Preferably, a protrusion is arranged on the side wall of the S-shaped channel.

Preferably, a first valve is arranged between the granulator and the mixing tank, a second valve is arranged between the mixing tank and the reaction kettle, and a third valve is arranged between the condenser and the mixing tank.

The reaction method of the continuous reaction system of the high-purity m/p-phthaloyl chloride comprises the following steps:

1) the granulator grinds the m/p-phthalic acid, and the grinded m/p-phthalic acid can reach 50-100 microns;

2) stirring the m/p-phthalic acid, the catalyst and the thionyl chloride in a mixing tank, uniformly mixing to form an approximately uniform suspension, and standing for a period of time;

3) the suspension enters the reaction kettle from the inlet of the reaction kettle and reacts through the S-shaped channel, the suspension can continuously collide with the protrusion and the exhaust pipe in the reaction process, the effective collision frequency is greatly increased, the generated tail gas can move upwards, enters the exhaust pipe through the exhaust hole and the capillary hole and is finally discharged into the tail gas cavity through the exhaust pipe, and the suspension can fully contact and react through the rising of the tail gas in the process;

4) condensing the tail gas in the tail gas cavity through a condenser, liquefying the evaporated thionyl chloride, putting the liquefied thionyl chloride into the mixing tank again for recycling, and performing related treatment on other gases;

5) and finally, producing a crude product from a discharge hole of the reaction kettle through continuous reaction, and obtaining a pure product through simple distillation.

Wherein the catalyst is one or more of a catalyst with a boiling point lower than that of m/p-phthaloyl chloride under high vacuum conditions such as triphenylphosphine oxide, phenanthroline or 4-dimethylamino quinoline, or a catalyst with a boiling point higher than that of m/p-phthaloyl chloride under high vacuum conditions such as DMF (dimethyl formamide), isoquinoline and the like; the reactor is heated by steam or heat conducting oil.

Compared with the prior art, the utility model discloses following beneficial effect has:

1. the utility model discloses a continuous reaction of acyl chloride product to equipment area is little, saves space, and is simpler than intermittent type reaction operation process, and reaction equipment does not have complicated pipeline, has reduced the complexity of technology. The problem of easy crystallization of pipelines is solved, the energy consumption required by heat tracing of process pipelines is saved, and the quality of continuous reaction products is stable.

2. Without agitation, collisions between molecules are achieved in three dimensions: (1) the tube is internally provided with a bulge and an exhaust pipe, so that the effective collision times are increased while the tube moves transversely; (2) tail gas generated in the reaction process moves upwards, and intermingled with meta/para acid moves upwards so as to be fully contacted with thionyl chloride; (3) the flow of the next layer at the turn of the S-shaped channel enables the S-shaped channel to be fully mixed and fully contacted.

Drawings

Fig. 1 is a schematic structural diagram of the present invention.

In the figure: 1. a granulator; 2. a first valve; 3. a mixing tank; 4. a second valve; 5. a reaction kettle; 6. an exhaust hole; 7. a protrusion; 8. a discharge port; 9. an S-shaped channel; 10. capillary pores; 11. an exhaust pipe; 12. a condenser; 13. a tail gas cavity; 14. a third valve.

Detailed Description

The embodiments of the present invention are further described below:

example 1

As shown in fig. 1, continuous reaction system of p terephthaloyl chloride between high purity, including granulator 1, compounding jar 3 and reation kettle 5 that concatenate in proper order, reation kettle 5 'S external condenser 12 of gas vent, the discharge end of condenser 12 is linked together with compounding jar 3' S feed inlet, reation kettle 5 'S inside sets up S type passageway 9, runs through many blast pipes 11 on the S type passageway 9, blast pipe 11 and S type passageway 9 are fixed to meet, and reation kettle 5' S upper portion sets up tail air cavity 13, the top of blast pipe 11 is located tail air cavity 13 to be linked together with tail air cavity 13, the upper portion that is located S type passageway 9 inside blast pipe 11 sets up a plurality of capillary holes 10.

Wherein, a bulge 7 is arranged on the side wall of the S-shaped channel 9; set up first valve 2 between granulator 1 and the compounding jar 3, set up second valve 4 between compounding jar 3 and reation kettle 5, set up third valve 14 between condenser 12 and the compounding jar 3.

1) the granulator 1 grinds the m/p-phthalic acid, and the grinded m/p-phthalic acid can reach 50-100 microns;

2) stirring the m/p-phthalic acid, the catalyst and the thionyl chloride in a mixing tank 3, uniformly mixing to form an approximately uniform suspension, and staying for a period of time;

3) the suspension enters the reaction kettle 5 from the inlet of the reaction kettle 5 and reacts through the S-shaped channel 9, the suspension can continuously collide with the protrusion 7 and the exhaust pipe 11 in the reaction process, the effective collision frequency is greatly increased, the generated tail gas can move upwards, enters the exhaust pipe 11 through the exhaust hole 6 and the capillary hole 10 and is finally exhausted into the tail gas cavity 13 through the exhaust pipe 11, and the suspension can fully contact and react due to the rising of the tail gas in the process;

4) the tail gas in the tail gas cavity 13 is condensed by the condenser 12, the evaporated thionyl chloride is liquefied and put into the mixing tank 3 again for recycling, and other gases are treated correspondingly;

5) and finally, producing a crude product from a discharge port 8 of the reaction kettle 5 through continuous reaction, and obtaining a pure product through simple distillation.

Claims

1. The utility model provides a continuous reaction system of high-purity meta/terephthaloyl chloride, includes granulator (1), compounding jar (3) and reation kettle (5) that concatenate in proper order, and the external condenser (12) of gas vent of reation kettle (5), the discharge end of condenser (12) are linked together with the feed inlet of compounding jar (3), its characterized in that, reation kettle 'S (5) inside sets up S type passageway (9), runs through many blast pipes (11) on S type passageway (9), blast pipe (11) and S type passageway (9) are fixed to be met, and reation kettle' S (5) upper portion sets up tail air cavity (13), the top of blast pipe (11) is located tail air cavity (13) to be linked together with tail air cavity (13), the upper portion of blast pipe (11) that is located S type passageway (9) inside sets up a plurality of capillary holes (10).

2. The continuous reaction system of high purity m/p-phthaloyl chloride according to claim 1, characterized in that the S-shaped channels (9) are provided on their side walls with protuberances (7).

3. The continuous reaction system of high purity m/p-phthaloyl chloride according to claim 1, characterized in that a first valve (2) is arranged between the granulator (1) and the mixing tank (3), a second valve (4) is arranged between the mixing tank (3) and the reaction vessel (5), and a third valve (14) is arranged between the condenser (12) and the mixing tank (3).