Acylation device for producing selegiline hydrochloride

Abstract

The utility model discloses an acylation device for producing selegiline hydrochloride, and relates to the technical field of selegiline hydrochloride production, a gas phase outlet of an acylation kettle is communicated with a cooler, and an inlet of the cooler is provided with a solvent tank; an annular liquid distributor is arranged at the upper part of the cooler, the upper part of the liquid distributor is communicated to an outlet of the solvent tank, and a plurality of liquid outlets are formed in the lower part of the liquid distributor. And sublimated aluminum trichloride is crystallized on the inner wall of the cooler in the reaction process, is washed by the solvent, is dissolved in the solvent and then enters the acylation kettle again for reaction, so that the possibility of blockage of a tail gas pipeline is avoided, the waste of the aluminum trichloride is also avoided, and raw materials are saved. Meanwhile, after aluminum trichloride is dissolved in the solvent, the catalytic effect is better, and the catalytic efficiency is improved.

Description

TECHNICAL FIELD

[0001] The utility model relates to hydrochloric selegiline production technical field, concretely relates to a kind of acylation device for hydrochloric selegiline production. BACKGROUND

[0002] Hydrochloric selegiline is a kind of selective monoamine oxidase-B inhibitor, inhibits the reuptake of dopamine and synaptic receptor.It is white crystalline powder, easily soluble in chloroform, dissolved in ethanol, slightly soluble in acetone, hardly soluble in water.

[0003] Hydrochloric selegiline production process uses hydrochloric dextromethorphan as starting material, carries out Friedel-Crafts reaction with acetic anhydride under the catalysis of anhydrous aluminum chloride, to obtain selegiline acylate.Chinese patent document CN102974280B discloses a method for improving Friedel-Crafts acyl chloride reaction yield, and the reaction device includes material acylation agent dropping device, acylation reaction kettle, water cooling device and tail gas absorption device.Although the reaction yield is improved, because of the sublimation characteristics of aluminum chloride itself, the tail gas pipeline of the reaction kettle is often blocked by aluminum chloride during the reaction, causing the pressure in the reaction kettle to be too high, which has great safety risk, and also causes waste of raw materials. SUMMARY

[0004] The technical problem to be solved by the utility model is that, in view of the deficiencies in the prior art, an acylation device for hydrochloric selegiline production is provided, which has high safety factor and saves raw materials.

[0005] To solve the above technical problems, the technical scheme of the utility model is as follows:

[0006] An acylation device for hydrochloric selegiline production, comprising an acylation kettle, a cooler connected to the gas phase outlet of the acylation kettle through a pipeline, and a solvent tank connected to the inlet of the cooler through a feed pump.

[0007] The upper part of the cooler is provided with an annular liquid distributor, the upper part of the liquid distributor is connected to the outlet of the solvent tank through a pipeline, and the lower part of the liquid distributor is provided with a plurality of liquid outlets, and the liquid outlets are arranged towards the inner wall of the cooler.

[0008] As an improved technical scheme, the outlet of the solvent tank is connected to a catalyst tank through the feed pump, and the outlet of the catalyst tank is connected to the liquid distributor through a pipeline.

[0009] As an improved technical scheme, the cooler is provided with a first stirring shaft, a plurality of connecting rods are arranged around the first stirring shaft, and a plurality of scraper plates corresponding to the connecting rods are arranged on the inner side of the cooler.

[0010] As the improved technical scheme, the bottom of the acylation kettle is provided with an annular gas distribution disc, the gas distribution disc is communicated with a nitrogen gas inlet pipeline, and the upper portion of the gas distribution disc is provided with a plurality of gas outlets.

[0011] As the improved technical scheme, the acylation kettle is provided with a second stirring shaft, the circumferential direction of the second stirring shaft is provided with a plurality of stirring rods, and the plurality of stirring rods comprise a connecting portion and a N-shaped stirring head.

[0012] As the improved technical scheme, the bottom outlet of the acylation kettle is communicated with a circulating pump through a pipeline, and the outlet of the circulating pump is communicated with the inlet of the acylation kettle through a pipeline.

[0013] As the preferred technical scheme, the bottom outlet of the acylation kettle is communicated with a circulating pump through a pipeline, and the outlet of the circulating pump is communicated with the inlet of the catalyst tank through a pipeline.

[0014] Due to the adoption of the above technical scheme, the beneficial effects of the present application are as follows:

[0015] The utility model discloses a kind of acylation devices for hydrochloric acid selegiline production, including acylation kettle, the gas phase outlet of the acylation kettle is communicated with cooler by pipeline, and the inlet of the cooler is communicated with solvent tank by feed pump;The upper portion of the cooler is equipped with annular liquid distributor, and the upper portion of the liquid distributor is communicated to the outlet of the solvent tank by pipeline, and the lower portion of the liquid distributor is equipped with a plurality of liquid outlets, and a plurality of the liquid outlet is towards the inner wall of the cooler Setting. Hydrochloric acid dextroamphetamine and acetic anhydride are added to acylation kettle to carry out fukui reaction under the catalysis of aluminium trichloride in negative pressure, and sublimed aluminium trichloride is crystallized in the inner wall of cooler during reaction process, then is washed by solvent, is dissolved in solvent again, and then is reacted in acylation kettle, avoid the possibility of tail gas pipeline blockage, also avoid the waste of aluminium trichloride, save raw materials. While aluminium trichloride is dissolved in solvent, catalytic effect is better, and catalytic efficiency is improved.

[0016] The outlet of the solvent tank is communicated with catalyst tank by the feed pump, and the outlet of the catalyst tank is communicated with the liquid distributor by pipeline. Aluminium trichloride is dissolved in organic solvent in advance, then is constantly added from catalyst tank, and reaction catalytic efficiency is improved, and the catalyst that is constantly added during reaction process is washed to the inner wall of cooler uniformly from the liquid outlet of liquid distributor, so that aluminium trichloride crystallized in the inner wall of cooler is constantly dissolved and separates from kettle wall, is re-injected into production, and catalytic effect is greatly improved, and raw material waste is avoided.

[0017] The cooler is provided with a first stirring shaft, a plurality of connecting rods are arranged in the circumference of the first stirring shaft, and the inner side of the cooler is provided with a plurality of scraping plates matched with the connecting rods.

[0018] The bottom of the acylation kettle is provided with an annular gas distribution disc, the gas distribution disc is communicated with a nitrogen gas inlet pipeline, and the upper portion of the gas distribution disc is provided with a plurality of gas outlet holes.

[0019] The acylation kettle is provided with a second stirring shaft, a plurality of stirring rods are arranged in the circumference of the second stirring shaft, and the plurality of stirring rods comprise connecting portions and N-shaped stirring heads.

[0020] The bottom outlet of the acylation kettle is communicated with a circulating pump through a pipeline, and the outlet of the circulating pump is communicated with the inlet of the acylation kettle through a pipeline.

[0021] The bottom outlet of the acylation kettle is communicated with a circulating pump through a pipeline, and the outlet of the circulating pump is communicated with the inlet of the catalyst tank through a pipeline. BRIEF DESCRIPTION OF DRAWINGS

[0022] The utility model will be further explained in connection with the drawings and examples.

[0023] Figure 1 It is the structure schematic diagram of the utility model embodiment;

[0024] Figure 2 It is the sectional view of the utility model embodiment;

[0025] Figure 3 It is Figure 2 The enlarged view of A in the figure;

[0026] Figure 4 It is Figure 2 The enlarged view of B in the figure;

[0027] Wherein: 1, acylation kettle; 2, cooler; 3, feed pump; 4, solvent tank; 5, liquid distributor; 6, liquid outlet; 7, catalyst tank; 8, first stirring shaft; 9, connecting rod; 10, scraper; 11, gas distribution disc; 12, nitrogen inlet pipeline; 13, gas outlet; 14, second stirring shaft; 15, stirring rod; 16, stirring head; 17, circulating pump. DETAILED DESCRIPTION

[0028] The utility model is further explained below in combination with the drawings and examples.

[0029] As Figures 1-4 The utility model relates to a kind of acylation devices for selegiline hydrochloride production, including acylation kettle 1, the gas phase outlet of the acylation kettle 1 is connected with cooler 2 by pipeline, the inlet of the cooler 2 is connected with solvent tank 4 by feed pump 3;The upper portion of the cooler 2 is equipped with annular liquid distributor 5, the upper portion of the liquid distributor 5 is connected to the outlet of the solvent tank 4 by pipeline, and the lower portion of the liquid distributor 5 is equipped with a plurality of liquid outlets 6, and a plurality of the liquid outlets 6 are arranged towards the inner wall of the cooler 2.Salicylic acid dextromethylamphetamine and acetic anhydride are added to acylation kettle 1 to carry out Friedel-Crafts reaction under the catalysis of negative pressure and aluminium trichloride, and sublimated aluminium trichloride is crystallized on the inner wall of cooler 2 during the reaction, then is washed by solvent, is dissolved in solvent again and then is reacted in acylation kettle 1, to avoid the possibility of tail gas pipeline blockage, while also avoiding the waste of aluminium trichloride, and saving raw materials.Aluminium trichloride is dissolved in solvent, and the catalytic effect is better, so as to improve catalytic efficiency.

[0030] The outlet of solvent tank 4 is connected with catalyst tank 7 by the feed pump 3, and the outlet of the catalyst tank 7 is connected to the liquid distributor 5 by pipeline.Aluminium trichloride is dissolved in organic solvent in advance, then is continuously added from catalyst tank 7, to improve the catalytic efficiency of reaction, and the continuously added catalyst during the reaction is washed uniformly to the inner wall of cooler 2 from the liquid outlet 6 of liquid distributor 5, so that aluminium trichloride crystallized on the inner wall of cooler 2 is continuously dissolved and separated from the kettle wall, and is put into production again, to greatly improve catalytic effect and avoid waste of raw materials.

[0031] The cooler 2 is equipped with first stirring shaft 8, and the circumferential direction of the first stirring shaft 8 is equipped with a plurality of connecting rods 9, and the inner side of the cooler 2 is equipped with a plurality of scrapers 10 adapted to the connecting rods 9.Through the washing of liquid distributor 5 and the double cooperation of scraper 10, aluminium trichloride crystallized on the inner wall of cooler 2 can be better stripped, and the removal effect is good.

[0032] The bottom of the acylation kettle 1 is provided with an annular gas distribution disc 11, the gas distribution disc 11 is communicated with a nitrogen gas inlet pipeline 12, and the upper portion of the gas distribution disc 11 is provided with a plurality of gas outlet holes 13. By continuously introducing nitrogen gas from the bottom of the acylation kettle 1, on the one hand, the water-free environment can be ensured, and on the other hand, the mixing between the raw materials is accelerated through bubbling, the reaction speed is improved, the reaction period is shortened, and the conversion rate is improved.

[0033] The acylation kettle 1 is provided with a second stirring shaft 14, the circumferential direction of the second stirring shaft 14 is provided with a plurality of stirring rods 15, and the plurality of stirring rods 15 include a connecting portion and a N-shaped stirring head 16. The N-shaped stirring head 16 plays a role of flow disturbance during stirring, accelerates the mixing between the raw materials, and the reaction is more thorough.

[0034] The bottom outlet of the acylation kettle 1 is communicated with a circulating pump 17 through a pipeline, the outlet of the circulating pump 17 is communicated to the inlet of the acylation kettle 1 through a pipeline. The material at the bottom is re-pumped into the top of the acylation kettle 1 by the circulating pump 17, the mixing of the material in the kettle is accelerated, and the reaction effect is good.

[0035] The bottom outlet of the acylation kettle 1 is communicated with a circulating pump 17 through a pipeline, the outlet of the circulating pump 17 is communicated to the inlet of the acylation kettle 1 through a pipeline. The material at the bottom is re-pumped into the top of the acylation kettle 1 by the circulating pump 17, the mixing of the material in the kettle is accelerated, and the reaction effect is good.

[0036] It should be understood that these embodiments are only used to illustrate the present application and not to limit the scope of the present application. In addition, it should be understood that after reading the content taught by the present application, those skilled in the art can make various changes or modifications to the present application, and these equivalent forms also fall within the scope defined by the appended claims of the present application.

Claims

1. A selegiline hydrochloride production acylation apparatus comprising an acylation tank, characterized by: The gas phase outlet of the acylation kettle is communicated with a cooler through a pipeline, an inlet of the cooler is communicated with a solvent tank through a feed pump; An upper portion of the cooler is provided with an annular liquid distributor, an upper portion of the liquid distributor is communicated with an outlet of the solvent tank through a pipeline, and a lower portion of the liquid distributor is provided with a plurality of liquid outlets, and the liquid outlets are arranged towards the inner wall of the cooler.

2. A selegiline hydrochloride production acylation apparatus according to claim 1, characterized in that: An outlet of the solvent tank is communicated with a catalyst tank through the feed pump, and an outlet of the catalyst tank is communicated with the liquid distributor through a pipeline.

3. A selegiline hydrochloride production acylation apparatus according to claim 1, characterized in that: The cooler is provided with a first stirring shaft, a periphery of the first stirring shaft is provided with a plurality of connecting rods, and an inner side of the cooler is provided with a plurality of scraper plates matched with the connecting rods.

4. The selegiline hydrochloride production acylation apparatus as claimed in claim 1, wherein: A bottom portion of the acylation kettle is provided with an annular gas distribution disc, the gas distribution disc is communicated with a nitrogen gas inlet pipeline, and an upper portion of the gas distribution disc is provided with a plurality of gas outlets.

5. The selegiline hydrochloride production acylation apparatus as claimed in claim 1, wherein: the acylation apparatus is a batch type apparatus. The acylation kettle is provided with a second stirring shaft, a periphery of the second stirring shaft is provided with a plurality of stirring rods, and the stirring rods include connecting portions and U-shaped stirring heads.

6. The selegiline hydrochloride production acylation apparatus as claimed in claim 1, wherein: A bottom outlet of the acylation kettle is communicated with a circulating pump through a pipeline, and an outlet of the circulating pump is communicated with an inlet of the acylation kettle through a pipeline.

7. A selegiline hydrochloride production acylation apparatus according to claim 2, characterized in that: A bottom outlet of the acylation kettle is communicated with a circulating pump through a pipeline, and an outlet of the circulating pump is communicated with an inlet of the catalyst tank through a pipeline.

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