Reaction device for continuously preparing 3, 5-dichloro-2-pentanone

Abstract

The utility model provides a reaction device for continuously preparing 3, 5-dichloro-2-pentanone, which belongs to the technical field of chemical production and comprises a reaction kettle, a raw material ester intermediate storage tank, a raw material acid intermediate storage tank, a primary water intermediate storage tank, a catalyst intermediate storage tank, a fan, a heater, a cooler, a water segregator, a diluted hydrochloric acid receiving tank and a product receiving tank. The reaction kettle is provided with a heating part; the raw material ester intermediate storage tank, the raw material acid intermediate storage tank, the primary water intermediate storage tank and the catalyst intermediate storage tank are all connected with the reaction kettle; the fan is connected with the reaction kettle through the heater; the condenser is communicated with the reaction kettle; a feed port of the water segregator is connected with a discharge port of the condenser, and a top reflux port is connected with a reflux port at the top of the reaction kettle; the diluted hydrochloric acid receiving tank is connected with a discharge port at the bottom of the reaction kettle; and the product receiving tank is connected with a discharge port of the water segregator. According to the device, intermittent reaction is converted into continuous production, the recovery rate of a product is increased, the contact time of the product and acid is shortened, and tar is eliminated or reduced.

Description

Technical Field

[0001] The utility model belongs to the technical field of chemical production, and specifically relates to a reaction device for continuously preparing 3,5-dichloro-2-pentanone. Background Art

[0002] Prothioconazole is a pesticide fungicide, which is mainly used in the prevention and control of crop diseases and pests. In terms of hazards, prothioconazole has always been low toxic, non-teratogenic, mutagenic, and non-toxic to plants; and 3,5-dichloro-2-pentanone is an important intermediate in the production of prothioconazole. The preparation of 3,5-dichloro-2-pentanone is mainly through the reaction of α-acetyl-α-chloro-γ-butyrolactone with hydrochloric acid and distillation. However, if the product is in contact with acid for a long time, tar will be produced, which will not only reduce the product quality and yield, but also damage the production equipment in actual production.

[0003] At present, the production of 3,5-dichloro-2-pentanone in the market still adopts intermittent production, which results in large material loss, a large amount of by-product tar, and a short service life of the reactor. Utility Model Content

[0004] The embodiment of the utility model provides a reaction device for continuously preparing 3,5-dichloro-2-pentanone, aiming to solve the problems of many by-products, short equipment service life and high material loss in the current production method.

[0005] To achieve the above object, the technical solution adopted by the utility model is: to provide a reaction device for continuously preparing 3,5-dichloro-2-pentanone, comprising:

[0006] A reaction kettle provided with a heating component;

[0007] A raw material ester intermediate storage tank, which delivers the raw material α-acetyl-α-chloro-γ-butyrolactone into the reactor through a pipeline;

[0008] A raw acid intermediate storage tank, which delivers raw hydrochloric acid to the reactor through a pipeline;

[0009] A primary water intermediate storage tank, which delivers the primary water to the reactor through a pipeline;

[0010] A catalyst intermediate storage tank for delivering the catalyst into the reactor through a pipeline;

[0011] A fan, which delivers hot air into the reactor through a heater;

[0012] A condenser, the top inlet of which is connected to the top of the reactor through a pipeline;

[0013] A water separator, wherein the top feed port thereof is connected to the discharge port of the condenser, and the top reflux port thereof is connected to the reflux port at the top of the reactor;

[0014] A dilute hydrochloric acid receiving tank, whose feed port is connected to the discharge port at the bottom of the reactor; and

[0015] The product receiving tank is connected to the discharge port at the bottom of the water distributor through a pipeline.

[0016] In one achievable manner, the heating component comprises a jacket sleeved on the outside of the reactor, and the jacket is provided with a first steam inlet pipe and a first steam outlet pipe for steam to enter for heating the reactor.

[0017] In one achievable manner, a first regulating valve and a first pressure transmitter are provided on the first steam inlet pipe, and the first regulating valve is interlocked with the first pressure transmitter.

[0018] In one achievable manner, the heater is a fin-type electric heater, and a one-way check valve is provided on a pipe through which the outlet of the heater is connected to the air inlet at the upper end of the reactor.

[0019] In one achievable manner, the heater is provided with a second steam inlet pipe and a second steam outlet pipe, and the second steam inlet pipe is provided with a second regulating valve and a second pressure transmitter; the second regulating valve is interlocked with the second pressure transmitter.

[0020] In one achievable manner, a third liquid level gauge is provided on the reactor, a third regulating valve is provided on the pipeline between the discharge port of the reactor and the dilute hydrochloric acid receiving tank, and the third regulating valve is interlocked with the third liquid level gauge.

[0021] In one achievable manner, an interface meter is provided on the top of the water divider, a fourth regulating valve is provided on the pipeline between the discharge port at the bottom of the water divider and the product receiving tank, and the interface meter is interlocked with the fourth regulating valve.

[0022] In one feasible manner, a circulating water outlet pipe is provided at the upper end of the condenser, and a circulating water inlet pipe is provided at the lower end thereof, a fifth regulating valve is provided on the circulating water inlet pipe, a fifth thermometer is provided on the discharge pipe at the lower end of the condenser, and the fifth regulating valve is interlocked with the fifth thermometer.

[0023] In one achievable manner, a first feed pump, a first flow meter and a first control valve are provided on the pipeline between the raw ester intermediate storage tank and the reactor, and the first control valve is interlocked with the first flow meter.

[0024] In one feasible manner, the reactor and the dilute hydrochloric acid receiving tank are both enameled tanks; the condenser is made of a material resistant to hydrochloric acid corrosion; the water separator is made of fiberglass; the raw ester intermediate storage tank is made of stainless steel; the product receiving tank and the raw acid intermediate storage tank are both made of a material resistant to hydrochloric acid corrosion; the primary water intermediate storage tank and the catalyst intermediate storage tank are both made of stainless steel.

[0025] Compared with the prior art, the reaction device for continuously preparing 3,5-dichloro-2-pentanone provided by the utility model has the following beneficial effects: the reaction device for continuously preparing 3,5-dichloro-2-pentanone can use a blower and a heater to introduce hot air into a reactor to accelerate the extraction rate of the product in the reactor, shorten the contact time between the product and hydrochloric acid, thereby eliminating or reducing the generation of tar and improving the service life of the reactor; regarding the continuous production reaction, the raw materials are added into the reactor through a raw material ester intermediate storage tank, a raw material acid intermediate storage tank, a primary water intermediate storage tank and a catalyst intermediate storage tank for reaction; the azeotropic product steam is cooled by a condenser and condensed into liquid for receiving; the reflux port of the water separator is connected to the reflux port at the top of the reactor for reflux of acid water, thereby realizing the recycling of hydrochloric acid and reducing material loss; the discharge port of the water separator is connected to the feed port of the product receiving tank, thereby realizing the continuous reaction of 3,5-dichloro-2-pentanone.

[0026] Therefore, the reaction device for continuously preparing 3,5-dichloro-2-pentanone provided by the utility model realizes the transformation from intermittent reaction to continuous production mode, thereby improving production efficiency; speeding up the extraction rate of the product, shortening the contact time between the product and the acid, eliminating or reducing the generation of tar; improving the yield of the product, realizing the recycling and utilization of hydrochloric acid, and reducing material loss; the continuous production mode reduces the operating pressure of the workers, reduces the danger and loss caused by operating errors, and improves the level of automation. BRIEF DESCRIPTION OF THE DRAWINGS

[0027] Figure 1 A schematic diagram of the structure of a reaction device for continuously preparing 3,5-dichloro-2-pentanone provided in an embodiment of the utility model;

[0028] Description of reference numerals:

[0029] 1. Intermediate storage tank for raw ester; 2. Intermediate storage tank for raw acid; 3. Intermediate storage tank for primary water; 4. Intermediate storage tank for catalyst; 5. Reactor; 6. Jacket; 7. Fan; 8. Heater; 9. Condenser; 10. Water distributor; 11. Dilute hydrochloric acid receiving tank; 12. Product receiving tank; 13. Second steam inlet pipe; 14. Circulating water inlet pipe; 15. Circulating water outlet pipe; 16. First steam outlet pipe; 17. First steam inlet pipe; 18. First flow meter; 19. Fifth thermometer; 20. First pressure transmitter; 21. Third liquid level gauge; 22. One-way check valve; 23. Third regulating valve; 24. Fourth regulating valve; 25. Interface meter; 26. Second regulating valve; 27. Second pressure transmitter; 28. Second steam outlet pipe; 29. ​​Fifth regulating valve. DETAILED DESCRIPTION

[0030] In order to make the technical problems, technical solutions and beneficial effects to be solved by the present invention more clearly understood, the present invention is further described in detail below in conjunction with the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are only used to explain the present invention and are not used to limit the present invention.

[0031] See also Figure 1 As shown, the reaction device for continuously preparing 3,5-dichloro-2-pentanone provided by the utility model is now described. The reaction device for continuously preparing 3,5-dichloro-2-pentanone provided by the utility model uses α-acetyl-α-chloro-γ-butyrolactone and 32% hydrochloric acid as raw materials to continuously generate 3,5-dichloro-2-pentanone, and the generated 3,5-dichloro-2-pentanone is accelerated by hot air blasting and taken out from the reactor.

[0032] The utility model provides a reaction device for continuously preparing 3,5-dichloro-2-pentanone, comprising a reaction kettle 5, a raw material ester intermediate storage tank 1, a raw material acid intermediate storage tank 2, a primary water intermediate storage tank 3, a catalyst intermediate storage tank 4, a fan 7, a heater 8, a cooler, a water separator 10, a dilute hydrochloric acid receiving tank and a product receiving tank 12.

[0033] The raw material ester intermediate storage tank 1 provides the raw material α-acetyl-α-chloro-γ-butyrolactone for the reaction; the raw material acid intermediate storage tank 2 provides the raw material 32% hydrochloric acid required for the reaction; the primary water intermediate storage tank 3 provides primary water to dilute the 32% hydrochloric acid into the 20% hydrochloric acid required for the reaction; the catalyst intermediate storage tank 4 stores PEG600, which is used as a matrix for medicine and cosmetics and as a catalyst in the reaction; the blower 7 adopts a Roots blower 7 to provide hot air for the reaction, and the cold air absorbed by the Roots blower 7 is converted into hot air through the fin-type electric heater 8 and sent to the reactor 5, thereby accelerating the extraction rate of the product in the reactor 5, shortening the contact time between the product and the hydrochloric acid, and reducing the generation of tar; the heating component is a jacket 6 arranged on the reactor 5, and steam is passed through the jacket 6 to heat the reactor 5 so that the temperature in the reactor 5 reaches the working temperature, and at the same time, there is air heated by the fin-type electric heater 8 at the upper end of the reactor 5 to accelerate the extraction of 3,5-dichloro-2-pentanone.

[0034] The feed port of the dilute hydrochloric acid receiving tank 11 is connected to the discharge port of the reactor 5, and the discharge port of the dilute hydrochloric acid receiving tank 11 is connected to a pump to transport the liquid to the dilute hydrochloric acid treatment device for the next step of treatment; the external condenser 9 cools the azeotropic product vapor through circulating water, condenses it into liquid for receiving, and the lower end of the condenser 9 is provided with a tail gas exhaust pipe, and the tail gas discharged from the condenser 9 is sent to the tail gas treatment device for the next step of treatment; the feed port of the water separator 10 is connected to the discharge port of the external condenser 9, and the reflux port of the water separator 10 is connected to the reflux port at the top of the reactor 5 for the reflux of acid water, and the discharge port of the water separator 10 is connected to the feed port of the product receiving tank 12; the product receiving tank 12 is used to receive 3,5-dichloro-2-pentanone, and the discharge port of the product receiving tank 12 is connected to a pump to transport the material for the next step of reaction.

[0035] The reaction device for continuously preparing 3,5-dichloro-2-pentanone provided by the utility model realizes the transformation from intermittent reaction to continuous production mode through the connection of various parts, thereby improving production efficiency; hot air is blown into the reaction kettle 5 by the fan 7, thereby accelerating the product extraction rate, shortening the contact time between the product and the acid, and eliminating or reducing the generation of tar; the yield of the product is improved by the heating component and the blown hot air; the recycling and utilization of hydrochloric acid is realized by the reflux of hydrochloric acid into the reaction kettle 5, thereby reducing material loss; the continuous production mode reduces the operating pressure of workers, reduces the danger and loss caused by operating errors, and improves the automation level.

[0036] Specifically, the reactor 5 is a vertical reactor 5 with upper and lower heads, four feed ports, one air inlet, one steam inlet and one reflux port are respectively arranged at the top of the reactor 5, and the discharge port is arranged at the bottom of the reactor 5. Among them, the raw material ester intermediate storage tank 1, the raw material acid intermediate storage tank 2, the primary water intermediate storage tank 3, and the catalyst intermediate storage tank 4 are respectively connected to a feed port, the heater 8 is connected to the air inlet, the steam required to be introduced into the heating component is connected to the steam inlet, the reflux port is connected to the reflux port of the water separator 10; the discharge port is connected to the dilute hydrochloric acid receiving tank 11.

[0037] It should be noted that since there are a large number of valves used in the figure, and a large number of thermometers and liquid level gauges are used, in order to facilitate description and distinguish the names of components in different parts, the article adopts the first, second, third, etc. series naming, but it does not limit the number of series components.

[0038] Combination Figure 1 As shown, in some embodiments, the heating component includes a jacket 6 mounted on the outside of the reactor 5, and the jacket 6 is provided with a first steam inlet pipe 17 and a first steam outlet pipe 16 for steam to heat the reactor 5. During operation, steam or heat transfer oil is introduced to heat the reactor 5 to maintain the required temperature for the reaction.

[0039] Combination Figure 1 As shown, in some embodiments, a first regulating valve and a first pressure transmitter 20 are provided on the first steam inlet pipe 17, and the first regulating valve is interlocked with the first pressure transmitter 20. The first pressure transmitter 20 controls the opening of the regulating valve by measuring the pressure in the jacket 6, controls the amount of steam entering the jacket 6, and thereby controls the temperature in the jacket 6. Through the interlocking of the first pressure transmitter 20 and the first regulating valve, the opening of the valve can be adjusted in real time according to the pressure value to ensure the stability of the inlet temperature of the jacket 6.

[0040] In some embodiments, see Figure 1 As shown, the heater 8 is a fin-type electric heater, and a one-way check valve 22 is provided on the pipe whose outlet is connected to the air inlet at the upper end of the reactor 5 to ensure one-way delivery of hot air and prevent the hydrochloric acid gas in the reactor 5 from entering the fin-type electric heater and causing corrosion damage to the equipment.

[0041] In some embodiments, see Figure 1 As shown, the heater 8 is provided with a second steam inlet pipe 13 and a second steam outlet pipe 28, and the second steam inlet pipe 13 is provided with a second regulating valve 26 and a second pressure transmitter 27; the second regulating valve 26 is interlocked with the second pressure transmitter 27. The steam pressure is adjusted by controlling the opening of the second regulating valve 26, and the finned electric heater is connected to the outlet of the Roots blower, so that the air is heated by the steam, providing heat for the reaction and accelerating the product extraction.

[0042] See also Figure 1 As shown, in some embodiments, the reactor 5 is provided with a third liquid level gauge 21, and a third regulating valve 23 is provided on the pipeline between the discharge port of the reactor 5 and the dilute hydrochloric acid receiving tank 11, and the third regulating valve 23 is interlocked with the third liquid level gauge 21. Through the interlocking of the liquid level gauge and the regulating valve, the opening of the regulating valve can be adjusted in real time according to the value of the liquid level gauge, thereby ensuring the volume of the liquid in the reactor 5.

[0043] See also Figure 1 As shown, in some embodiments, an interface meter 25 is provided on the top of the water distributor 10, and a fourth regulating valve 24 is provided on the pipeline between the discharge port at the bottom of the water distributor 10 and the product receiving tank 12, and the interface meter 25 is interlocked with the fourth regulating valve 24. The interface meter 25 is interlocked with the fourth regulating valve 24 to control the valve opening, adjust the flow rate, perform water distribution and production, and maintain a relatively stable liquid level.

[0044] Combination Figure 1 As shown, in some embodiments, a circulating water outlet pipe 15 is provided at the upper end of the condenser 9, and a circulating water inlet pipe 14 is provided at the lower end thereof. A fifth regulating valve 29 is provided on the circulating water inlet pipe 14, and a fifth thermometer 19 is provided on the discharge pipe at the lower end of the condenser 9. The fifth regulating valve 29 is interlocked with the fifth thermometer 19, and the discharge temperature is controlled by adjusting the circulating water flow rate, so that when the discharge temperature increases, the circulating water flow rate increases, and when the discharge temperature decreases, the circulating water flow rate decreases.

[0045] Combination Figure 1 As shown, in some embodiments, a first feed pump, a first flow meter 18 and a first control valve are provided on the pipeline between the raw ester intermediate storage tank 1 and the reactor 5, and the first control valve is interlocked with the first flow meter 18. Similarly, a second feed pump is provided on the pipeline between the raw acid intermediate storage tank 2 and the reactor 5; a third feed pump is provided on the pipeline between the primary water intermediate storage tank 3 and the reactor 5; and a fourth feed pump is provided on the pipeline between the catalyst intermediate tank and the reactor 5. The flow rate of the added raw material is adjusted by adjusting the opening of the control valve. Through interlocking, the switch size of the valve can be adjusted in real time according to the value of the flow meter.

[0046] In some embodiments, Figure 1 As shown, the reaction kettle 5 and the dilute hydrochloric acid receiving tank 11 are both enameled tanks; the condenser 9 is made of a material resistant to hydrochloric acid corrosion, such as a graphite modified condenser, a graphite condenser, a silicon carbide condenser, etc.; the water separator 10 is made of fiberglass; the raw ester intermediate storage tank 1 is made of stainless steel, such as S31603 or S22053.

[0047] The materials of the product receiving tank 12 and the raw acid intermediate storage tank 2 are both hydrochloric acid corrosion-resistant materials, such as glass fiber reinforced plastics, steel-lined PE, steel-lined PTFE, etc.

[0048] The primary water intermediate storage tank 3 and the catalyst intermediate storage tank 4 are both made of stainless steel. The primary water and the catalyst are not highly corrosive, and using ordinary steel can reduce the manufacturing cost.

[0049] In the above embodiments, the description of each embodiment has its own emphasis. For parts that are not described or recorded in detail in a certain embodiment, reference can be made to the relevant descriptions of other embodiments.

[0050] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions and improvements made within the spirit and principles of the present invention should be included in the protection scope of the present invention.

Claims

1. A reaction device for continuously preparing 3,5-dichloro-2-pentanone, characterized in that: include: A reaction kettle (5) is provided with a heating component; The raw material ester intermediate storage tank (1) is used to deliver the raw material α-acetyl-α-chloro-γ-butyrolactone into the reaction kettle (5) through a pipeline; A raw acid intermediate storage tank (2) is used to deliver raw hydrochloric acid to the reactor (5) through a pipeline; A primary water intermediate storage tank (3) is used to deliver the primary water to the reactor (5) through a pipeline; A catalyst intermediate storage tank (4) is used to deliver the catalyst into the reactor (5) through a pipeline; A fan (7) sends hot air into the reaction kettle (5) through a heater (8); A condenser (9), the top inlet of which is connected to the top of the reaction kettle (5) through a pipeline; A water separator (10), the top feed port of which is connected to the discharge port of the condenser (9), and the top reflux port of which is connected to the reflux port at the top of the reactor (5); A dilute hydrochloric acid receiving tank (11), whose feed port is connected to the discharge port at the bottom of the reactor (5); and The product receiving tank (12) is connected to the discharge port at the bottom of the water distributor (10) through a pipeline.

2. The reaction device for continuously preparing 3,5-dichloro-2-pentanone according to claim 1, characterized in that: The heating component comprises a jacket (6) sleeved on the outside of the reaction kettle (5), and the jacket (6) is provided with a first steam inlet pipe (17) and a first steam outlet pipe (16) for steam to enter to heat the reaction kettle (5).

3. The reaction device for continuously preparing 3,5-dichloro-2-pentanone according to claim 2, characterized in that: The first steam inlet pipe (17) is provided with a first regulating valve and a first pressure transmitter (20), and the first regulating valve is interlocked with the first pressure transmitter (20).

4. The reaction device for continuously preparing 3,5-dichloro-2-pentanone according to claim 1, characterized in that: The heater (8) is a fin-type electric heater, and a one-way check valve (22) is provided on a pipeline whose outlet of the heater (8) is connected to the air inlet at the upper end of the reaction kettle (5).

5. The reaction device for continuously preparing 3,5-dichloro-2-pentanone according to claim 1, characterized in that: The heater (8) is provided with a second steam inlet pipe (13) and a second steam outlet pipe (28); the second steam inlet pipe (13) is provided with a second regulating valve (26) and a second pressure transmitter (27); the second regulating valve (26) is interlocked with the second pressure transmitter (27).

6. The reaction device for continuously preparing 3,5-dichloro-2-pentanone according to claim 1, characterized in that: The reactor (5) is provided with a third liquid level gauge (21), and a third regulating valve (23) is provided on the pipeline between the discharge port of the reactor (5) and the dilute hydrochloric acid receiving tank (11), and the third regulating valve (23) is interlocked with the third liquid level gauge (21).

7. The reaction device for continuously preparing 3,5-dichloro-2-pentanone according to claim 1, characterized in that: An interface meter (25) is provided at the top of the water distributor (10), and a fourth regulating valve (24) is provided on the pipeline between the discharge port at the bottom of the water distributor (10) and the product receiving tank (12), and the interface meter (25) is interlocked with the fourth regulating valve (24).

8. The reaction device for continuously preparing 3,5-dichloro-2-pentanone according to claim 1, characterized in that: A circulating water outlet pipe (15) is provided at the upper end of the condenser (9), and a circulating water inlet pipe (14) is provided at the lower end thereof; a fifth regulating valve (29) is provided on the circulating water inlet pipe (14); a fifth thermometer (19) is provided on the discharge pipe at the lower end of the condenser (9); and the fifth regulating valve (29) is interlocked with the fifth thermometer (19).

9. The reaction device for continuously preparing 3,5-dichloro-2-pentanone according to claim 1, characterized in that: A first feed pump, a first flow meter (18) and a first control valve are arranged on the pipeline between the raw ester intermediate storage tank (1) and the reactor (5), and the first control valve is interlocked with the first flow meter (18).

10. The reaction device for continuously preparing 3,5-dichloro-2-pentanone according to claim 1, characterized in that: The reaction kettle (5) and the dilute hydrochloric acid receiving tank (11) are both enameled tanks; the condenser (9) is made of a material resistant to hydrochloric acid corrosion; the water separator (10) is made of glass fiber reinforced plastics; the raw ester intermediate storage tank (1) is made of stainless steel; the product receiving tank (12) and the raw acid intermediate storage tank (2) are both made of a material resistant to hydrochloric acid corrosion; the primary water intermediate storage tank (3) and the catalyst intermediate storage tank (4) are both made of stainless steel.

Images