Purification device for ethyl benzoylacetate

Abstract

The ethyl benzoylacetate purifying device comprises a raw material tank, a buffer, a first rectifying tower, a second rectifying tower and a product tank, the outlet end of the raw material tank is connected with the inlet end of the buffer, the buffer is located at the bottom of the first rectifying tower, and the outlet end of the buffer is connected with the inlet end of the bottom of the first rectifying tower; a top outlet end of the first rectifying tower is connected with a middle inlet end of the second rectifying tower; a bottom outlet end of the second rectifying tower is connected with an inlet end of the product tank; the buffer is a pipeline with the diameter larger than that of the first rectifying tower; the first rectifying tower is used for removing impurities with the boiling point higher than that of the product, the second rectifying tower is used for removing impurities with the boiling point lower than that of the product, and the buffer is matched to collect high-boiling-point viscous liquid impurities, so that the purity is remarkably improved; different from the traditional purification process, the device disclosed by the utility model can be used for obtaining high-purity ethyl benzoylacetate, the purity can reach 99.5%, the product loss rate is extremely low, and the time required by rectification can be shortened by about 30%.

Description

Technical Field

[0001] The utility model relates to the technical field of purification devices, in particular to a purification device for ethyl benzoylacetate. Background Art

[0002] Ethyl benzoyl acetate has a high melting point, high solubility, and antioxidant properties. It inhibits oxidases, helping to prevent fatty acid oxidation and extend the shelf life of food. Therefore, it is a commonly used food additive to prevent food spoilage. It is also used in solvents, lubricants, silicone rubber, vulcanized rubber, antioxidants, plastic additives, dye intermediates, and matting agents. Ethyl benzoyl acetate is an important organic compound and an important organic chemical substance with multiple applications. Application 1: It is used as an intermediate for flavonoid drugs and in the synthesis of color photographic couplers. Application 2: It is a food flavoring, primarily used in the preparation of flavors for fruit wines such as brandy. Application 3: It is used in organic synthesis. Currently, there are over 40 synthetic routes for ethyl benzoyl acetate, depending on the starting material.

[0003] Currently, patent CN201711022757.0 discloses a method for preparing ethyl benzoylacetate. This is only a laboratory preparation method, with no disclosed post-processing method, and the final product is not of high purity. After synthesizing crude ethyl benzoylacetate using benzoyl chloride and ethyl acetoacetate as the main raw materials, the system is relatively complex, and the crude product needs to be purified to obtain high-purity ethyl benzoylacetate. In particular, for large-scale production, it is necessary to propose a set of mature purification processes and purification equipment. Ethyl benzoylacetate is a liquid at normal pressure, so it is difficult to purify it using conventional purification processes such as filtration or crystallization. Distillation is used to separate multiple liquids, but previous studies have found that if direct distillation is performed, on the one hand, the impurity removal effect is poor due to the close boiling point of multiple impurities and the product. On the other hand, due to the increased viscosity of the liquid during cooling, it is easy to block the tower plate or the condenser, interfering with the impurity removal process and posing a safety hazard.

[0004] Therefore, there is an urgent need to develop a new purification device for the purification process of ethyl benzoylacetate, which can be used to stably distill the crude ethyl benzoylacetate, avoid the interference of increased liquid viscosity on the process, flexibly adjust the impact of temperature changes on the process, shorten the purification time, and improve product purity. Utility Model Content

[0005] In order to solve the above problems, the utility model provides a purification device for ethyl benzoylacetate. By setting a first distillation tower and a second distillation tower, various impurities with a boiling point close to that of the product are removed as much as possible. A buffer is set below the first distillation tower to avoid liquid flooding while collecting viscous liquid, thereby improving the separation degree. The upper and lower parts of the second distillation tower are both connected to a vacuum pump. While ensuring the vacuum degree, the distillation process can be changed by coordinated adjustment of the valve and the reboiler, thereby reducing the impact of increased liquid viscosity on the distillation.

[0006] On the one hand, the present invention provides a purification device for ethyl benzoylacetate, comprising a raw material tank, a buffer, a first distillation tower, a second distillation tower and a product tank, wherein the outlet end of the raw material tank is connected to the inlet end of the buffer, the buffer is located at the bottom of the first distillation tower, the outlet end of the buffer is connected to the inlet end of the bottom of the first distillation tower, the top outlet end of the first distillation tower is connected to the middle inlet end of the second distillation tower, and the bottom outlet end of the second distillation tower is connected to the inlet end of the product tank; the buffer is a pipeline having a diameter larger than that of the first distillation tower.

[0007] In some embodiments, a heating jacket is further included, and the heating jacket is disposed outside the raw material tank.

[0008] In some embodiments, a reboiler is further included, wherein the inlet end of the reboiler is connected to the lower end of the second distillation tower, and the outlet end of the reboiler is connected to the middle inlet end of the second distillation tower.

[0009] In some embodiments, a vacuum pump is further included, and the vacuum pump is connected to both the top outlet end of the second distillation column and the inlet end of the product tank.

[0010] Furthermore, it also includes a first buffer tank, the top outlet end of the second distillation tower is connected to the inlet end of the first buffer tank, and the outlet end of the first buffer tank is connected to the vacuum pump.

[0011] Furthermore, the top outlet of the second distillation tower is connected to the inlet of the first buffer tank via a first pipeline, and a first control valve is provided in the first pipeline path connecting the top outlet of the second distillation tower and the inlet of the first buffer tank.

[0012] Furthermore, the outlet end of the first buffer tank is connected to the vacuum pump via a second pipeline, and a second control valve is provided in the second pipeline path connecting the outlet end of the first buffer tank and the vacuum pump.

[0013] Furthermore, it also includes a second buffer tank, the outlet end of the product tank is connected to the inlet end of the second buffer tank, and the outlet end of the second buffer tank is connected to the vacuum pump.

[0014] Furthermore, the product tank outlet and the second buffer tank inlet are connected via a third pipeline, and a third control valve is provided in the third pipeline path connecting the product tank outlet and the second buffer tank inlet.

[0015] Furthermore, the outlet end of the second buffer tank is connected to the vacuum pump via a fourth pipeline, and a fourth control valve is provided in the fourth pipeline path connecting the outlet end of the second buffer tank and the vacuum pump.

[0016] The beneficial technical effects of the utility model are:

[0017] 1. The utility model provides a novel purification device for ethyl benzoylacetate. Different from the traditional purification process, the device of the utility model can obtain high-purity ethyl benzoylacetate with a purity of up to 99.5%, an extremely low product loss rate, and can also shorten the distillation time by about 30%.

[0018] 2. The first distillation tower is set up to remove impurities with a higher boiling point than the product, and the second distillation tower is set up to remove impurities with a lower boiling point than the product. A buffer is used to collect high-boiling point viscous liquid impurities, which significantly improves the purity.

[0019] 3. The vacuum pump is connected to both ends of the second distillation tower, and a control valve is provided to adjust the pressure difference between the upper and lower ends of the second distillation tower. The reboiler re-evaporates the liquid at the bottom of the second distillation tower to the middle of the second distillation tower, and can adjust the temperature. By setting the pressure difference and temperature, it can be flexibly adjusted to reduce the viscosity of the liquid, significantly improving the production efficiency. The operation is convenient, and the central control program can be set for automatic adjustment.

[0020] 4. Set up a buffer tank to prevent liquid from being directly sucked into the pump and to avoid the occurrence of vortexes, thereby improving the stability of the production process. BRIEF DESCRIPTION OF THE DRAWINGS

[0021] Figure 1 This is an overall schematic diagram of the purification device for ethyl benzoyl acetate of the present invention;

[0022] Figure markings: 1-raw material tank, 2-heating jacket, 3-buffer, 4-first distillation tower, 5-first pipeline, 6-second distillation tower, 7-second pipeline, 8-first control valve, 9-third pipeline, 10-second control valve, 11-first buffer tank, 12-reboiler, 13-product tank, 14-fourth pipeline, 15-third control valve, 16-second buffer tank, 17-fifth pipeline, 18-fourth control valve, 19-vacuum pump. DETAILED DESCRIPTION

[0023] The present invention will be further described below in conjunction with the accompanying drawings and embodiments. Identical components are denoted by the same reference numerals. It should be noted that the terms "front," "rear," "left," "right," "upper," and "lower" used in the following description refer to directions in the accompanying drawings, and the terms "bottom," "top," "inner," and "outer" refer to directions toward or away from the geometric center of a particular component, respectively.

[0024] like Figure 1 As shown, the purification device of ethyl benzoyl acetate of the present invention includes a raw material tank 1, a first distillation tower 4, and a second distillation tower 6 connected in sequence, the top outlet end of the second distillation tower 6 is connected to the inlet end of the first buffer tank 11, the bottom outlet end of the second distillation tower 6 is connected to the inlet end of the product tank 13, the outlet end of the product tank 13 is connected to the inlet end of the second buffer tank 16, and the outlet end of the first buffer tank 11 and the outlet end of the second buffer tank 16 are both connected to a vacuum pump 19.

[0025] A heating jacket 2 is provided on the outside of the raw material tank 1. The top outlet end of the raw material tank 1 is connected to the buffer 3. The buffer 3 is located at the bottom of the first distillation tower 4. The buffer 3 is a section of steel pipe with a diameter larger than that of the first distillation tower 4; the top outlet end of the first distillation tower 4 is connected to the middle inlet end of the second distillation tower 6 through a first pipeline 5, and the top outlet end of the second distillation tower 6 is connected to the inlet end of the second buffer tank 16 through a second pipeline 7, and a first control valve 8 is provided on the second pipeline 7; the second distillation tower 6 is also provided with a reboiler 12; the bottom outlet end of the second distillation tower 6 is connected to the inlet end of the product tank 13, and the outlet end of the product tank 13 is connected to the inlet end of the second buffer tank 16 through a fourth pipeline 14, and a third control valve 15 is provided on the fourth pipeline 14; the outlet end of the first buffer tank 11 is connected to the vacuum pump 19 through a third pipeline 9, and a second control valve 10 is provided on the third pipeline 9. The outlet end of the second buffer tank 16 is connected to the vacuum pump 19 through a fifth pipeline 17, and a fourth control valve 18 is provided on the fifth pipeline 17.

[0026] The operating principle of the purification device of ethyl benzoyl acetate of the utility model:

[0027] First, add the crude benzoyl ethyl acetate solution to the raw material tank 1, turn on the heating jacket 2 and set it to a suitable temperature, turn on the vacuum pump 19, open the first control valve 8, the second control valve 9, the third control valve 15 and the fourth control valve 18, and perform reduced pressure distillation. The crude benzoyl ethyl acetate solution in the raw material tank 1 evaporates into organic vapor and moves upward;

[0028] The organic vapor enters the buffer 3, which has a larger diameter than the first distillation tower 4, reducing the occurrence of flooding. More importantly, the high-boiling-point portion of the organic vapor evaporated from the crude benzoylethyl ethyl solution will immediately condense into a liquid with a higher viscosity. The larger diameter ensures that most of the liquid with a higher viscosity is collected in the buffer 3, without clogging the tower plates, thereby improving the separation efficiency of the distillation.

[0029] The primary function of the first distillation tower 4 is to remove impurities with a boiling point higher than ethyl benzoylacetate. Ethyl benzoylacetate and impurities with lower boiling points flow along the first pipe 5 into the middle portion of the second distillation tower 6. The second distillation tower 6 is provided with a reboiler 12 as a heat source, and a portion of the liquid at the bottom of the second distillation tower 6 is continuously extracted and re-evaporated back into the middle portion of the second distillation tower 6. The lower boiling point impurities escape from the top outlet of the second distillation tower 6, and the ethyl benzoylacetate flows from the bottom of the second distillation tower 6 into the product tank 13.

[0030] The key point of the operation is that if it is found that the viscosity of the product liquid increases and blocks the trays of the second distillation tower 6, the first control valve 8 is immediately adjusted to reduce the flow rate. Then, inside the second distillation tower 6, the vacuum degree at the top is small and the vacuum degree at the bottom is large, forming a downward pressure difference, which drives the viscous liquid downward. At the same time, the reduction of the vacuum degree at the bottom is conducive to reducing the viscosity of the liquid. At this time, the reboiler 12 is adjusted again to increase the heating temperature according to the adjustment amount of the first control valve 8, so as to quickly evaporate the low-boiling-point impurities in the viscous liquid. The first control valve 8 and the reboiler 12 can be connected to the central control program for automatic control.

[0031] After the distillation is stabilized for a period of time, all the ethyl benzoyl acetate in the raw material tank 1 is evaporated, leaving only impurities, and the product tank 13 is filled with ethyl benzoyl acetate product. The second control valve 10 and the fourth control valve 18 are closed, and the vacuum pump 19 is turned off. The raw material tank 1, the first buffer tank 11 and the second buffer tank 16 are opened respectively to release the impurities; and the product tank 13 is opened to release the ethyl benzoyl acetate product.

[0032] The product obtained using the device of the present invention has a purity of 99.5% and a water content of approximately 0.2% as determined by high-performance liquid chromatography. Conventional distillation, on the other hand, only yields a product with a purity of approximately 90% and a water content of approximately 5%. The device of the present invention reduces product loss and yields significantly. Calculated based on the concentration and mass before and after purification, the product loss rate is only approximately 1%. The purification time consumed by the device of the present invention is 30% shorter than that of direct distillation.

[0033] The above description is merely a preferred embodiment of the present invention. The scope of protection of the present invention is not limited to the above embodiment. All technical solutions based on the concept of the present invention are within the scope of protection of the present invention. It should be noted that for those skilled in the art, certain improvements and modifications that do not depart from the principles of the present invention should also be considered within the scope of protection of the present invention.

Claims

1. A purification device for ethyl benzoyl acetate, characterized in that: It includes a raw material tank, a buffer, a first distillation tower, a second distillation tower and a product tank. The outlet of the raw material tank is connected to the inlet of the buffer. The buffer is located at the bottom of the first distillation tower. The outlet of the buffer is connected to the inlet of the bottom of the first distillation tower. The top outlet of the first distillation tower is connected to the middle inlet of the second distillation tower. The bottom outlet of the second distillation tower is connected to the inlet of the product tank. The buffer is a pipeline with a diameter larger than that of the first distillation tower.

2. The purification device of ethyl benzoylacetate according to claim 1, wherein: The device also includes a heating jacket, which is arranged outside the raw material tank.

3. The purification device of ethyl benzoylacetate according to claim 1, wherein: It also includes a reboiler, the inlet end of the reboiler is connected to the lower end of the second distillation tower, and the outlet end of the reboiler is connected to the middle inlet end of the second distillation tower.

4. The purification device of ethyl benzoylacetate according to claim 1, wherein: The utility model also comprises a vacuum pump, which is connected to the top outlet end of the second distillation tower and the inlet end of the product tank.

5. The purification device of ethyl benzoylacetate according to claim 4, wherein: It also includes a first buffer tank, the top outlet end of the second distillation tower is connected to the inlet end of the first buffer tank, and the outlet end of the first buffer tank is connected to a vacuum pump.

6. The purification device for ethyl benzoylacetate according to claim 5, wherein: The top outlet of the second distillation tower is connected to the inlet of the first buffer tank via a first pipeline. A first control valve is provided in the first pipeline connecting the top outlet of the second distillation tower and the inlet of the first buffer tank.

7. The purification device for ethyl benzoylacetate according to claim 5, wherein: The outlet end of the first buffer tank is connected to the vacuum pump via a second pipeline, and a second control valve is provided in the second pipeline path connecting the outlet end of the first buffer tank and the vacuum pump.

8. The purification device for ethyl benzoylacetate according to claim 4, wherein: It also includes a second buffer tank, the outlet end of the product tank is connected to the inlet end of the second buffer tank, and the outlet end of the second buffer tank is connected to the vacuum pump.

9. The purification device for ethyl benzoylacetate according to claim 8, wherein: The product tank outlet and the second buffer tank inlet are connected via a third pipeline, and a third control valve is provided in the third pipeline path connecting the product tank outlet and the second buffer tank inlet.

10. The purification device for ethyl benzoylacetate according to claim 8, wherein: The outlet end of the second buffer tank is connected to the vacuum pump via a fourth pipeline, and a fourth control valve is provided in the fourth pipeline path connecting the outlet end of the second buffer tank and the vacuum pump.

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