Device for recovering multi-component organic solvent mother liquor through supergravity reduced pressure rectification

Abstract

The utility model discloses a device for recovering multi-component organic solvent mother liquor by supergravity reduced pressure rectification, which comprises a reaction kettle, a supergravity rotating bed and a reflux pump, a material inlet is arranged on the reaction kettle, the reaction kettle is connected with a steam heating system, a gas outlet at the top of the supergravity rotating bed is connected with a first-stage condenser, and a second-stage condenser is connected with a second-stage condenser. A liquid outlet at the bottom of the primary condenser is connected with a buffer tank, an outlet at the top of the buffer tank is connected with a secondary condenser, an outlet at the bottom of the buffer tank is connected with a reflux pump, an outlet of the reflux pump is connected with a reflux pipeline and an extraction pipeline, and the reflux pipeline is communicated with a liquid reflux inlet at the top of the supergravity rotating bed; the extraction pipeline is communicated with a finished product cooler, and the finished product cooler is connected with a finished product tank and at least one fraction tank. The device can be used for separating and purifying the mother liquor containing various organic solvent components on one piece of supergravity rectification equipment, the separation efficiency is high, the operation cost is saved, and the multi-component organic solvent mother liquor is efficiently recovered.

Description

Technical Field

[0001] The utility model relates to the technical field of organic solvent distillation, in particular to a device for recovering multi-component organic solvent mother liquor by ultra-gravity vacuum distillation. Background Art

[0002] The distillation tower is the most widely used separation equipment in the chemical, pharmaceutical, environmental protection and other industrial production processes. The equipment is large in size and generally more than ten meters high. It is also one of the main energy-consuming units. How to improve the performance of the distillation process will become the key to reducing operating costs and improving economic benefits for enterprises. In order to improve the distillation performance, coupling the ultra-gravity distillation technology with the heat pump can improve the separation efficiency, reduce the equipment size, save energy and raw materials, and create new economic value for the enterprise.

[0003] The utility model patent with application number 202222568161.3 discloses a device for separating acetone water by ultra-gravity distillation, which can effectively separate and purify organic solvents containing a single component, but cannot be applied to the separation and purification of mother liquors containing multi-component organic solvents. For example, the mother liquor of tert-amyl alcohol includes acetonitrile, pyridine, tert-amyl alcohol, water, and high boiling products. The existing ultra-gravity distillation separation device cannot achieve the purpose of multi-component separation. How to further optimize the structure and process flow of ultra-gravity distillation equipment, save operating costs, and achieve efficient recovery of mother liquors containing multi-component organic solvents is an urgent problem to be solved. Utility Model Content

[0004] The purpose of the utility model is to overcome the shortcomings and deficiencies of the prior art and to provide a device for recovering mother liquor containing multi-component organic solvents by ultra-gravity vacuum distillation.

[0005] The technical scheme adopted by the utility model is as follows: a device for recovering mother liquor containing multi-component organic solvents by supergravity vacuum distillation, comprising a reactor, a supergravity rotating bed, and a reflux pump, wherein the reactor is provided with a material inlet, the reactor is connected to a steam heating system, the gas outlet at the top of the reactor is connected to the gas inlet of the supergravity rotating bed, the liquid outlet at the bottom of the supergravity rotating bed is connected to the liquid inlet at the top of the reactor, the gas outlet at the top of the supergravity rotating bed is connected to a primary condenser, and the liquid outlet at the bottom of the primary condenser is connected to a buffer tank,

[0006] The bottom outlet of the buffer tank is connected to a reflux pump, the outlet of the reflux pump is connected to a reflux pipeline and a production pipeline, the reflux pipeline is connected to the liquid reflux port at the top of the ultra-gravity rotating bed, the production pipeline is connected to a finished product cooler, and the finished product cooler is connected to a finished product tank and at least one distillation tank.

[0007] Preferably, the top outlet of the buffer tank is connected to a secondary condenser, and the secondary condenser is connected to a vacuum system, a circulating water supply pipeline, and a circulating water return pipeline.

[0008] Preferably, the finished product cooler is connected to a circulating water supply pipe and a circulating water return pipe, and the primary condenser is connected to the circulating water supply pipe and the circulating water return pipe respectively.

[0009] Preferably, the primary condenser, the secondary condenser and the finished product cooler are respectively one of a spirally wound tube heat exchanger, a shell and tube heat exchanger, a plate heat exchanger and a spiral plate heat exchanger.

[0010] Preferably, the mother liquor is a tert-amyl alcohol mother liquor with an initial purity of 50%-80%, which further contains one or more of acetonitrile, pyridine and high boiling substances.

[0011] Preferably, the distillation tank comprises a front distillation tank and an intermediate distillation tank.

[0012] Preferably, the working pressure of the device is -99Kpa to normal pressure, and the working temperature is 0-150°C.

[0013] Preferably, the high gravity rotating bed consists of 1-5 layers of stators and rotors, and the rotation speed is 0-1200RPM.

[0014] Preferably, the supergravity rotating bed is a baffled rotating bed or a packed rotating bed.

[0015] The beneficial effects of the utility model are as follows: the mother liquor containing multi-component organic solvents is separated and purified by utilizing the efficient mass and heat transfer efficiency of the ultra-gravity rotating bed; the ultra-gravity distillation equipment has a small volume and high separation efficiency, and can realize the separation of multi-component organic solvents under high vacuum; the ultra-gravity rotating bed equipment is coupled with the reactor, which optimizes the process flow, saves operating costs, and realizes efficient recovery of multi-component organic solvent mother liquor. BRIEF DESCRIPTION OF THE DRAWINGS

[0016] In order to more clearly illustrate the embodiments of the utility model or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the utility model. For ordinary technicians in this field, without paying creative labor, other drawings obtained based on these drawings still belong to the scope of the utility model.

[0017] Figure 1 A block diagram of an apparatus for recovering a mother liquor containing a multi-component organic solvent by ultra-gravity vacuum distillation according to an embodiment of the present invention;

[0018] In the figure, 1. ultra-gravity rotating bed; 2. reactor; 3. primary condenser; 4. secondary condenser; 5. buffer tank; 6. reflux pump; 7. reflux pipeline; 8. production pipeline; 9. finished product cooler; 10. front distillate tank; 11. intermediate distillate tank; 12. finished product tank. DETAILED DESCRIPTION

[0019] In order to make the purpose, technical solutions and advantages of the utility model clearer, the utility model will be further described in detail below with reference to the accompanying drawings.

[0020] It should be noted that all expressions using "first" and "second" in the embodiments of the present invention are for distinguishing two non-identical entities with the same name or non-identical parameters. It can be seen that "first" and "second" are only for the convenience of expression and should not be understood as limitations on the embodiments of the present invention. The subsequent embodiments will not explain this one by one.

[0021] The directions and positions mentioned in the present invention, such as "upper", "lower", "front", "back", "left", "right", "inside", "outside", "top", "bottom", "side", etc., are only for reference to the directions or positions of the drawings. Therefore, the directions and positions used are used to explain and understand the present invention, but not to limit the scope of protection of the present invention.

[0022] like Figure 1 As shown, in an embodiment of the utility model, a device for recovering a mother liquor containing a multi-component organic solvent by supergravity vacuum distillation comprises a reactor 2, a supergravity rotating bed 1, and a reflux pump 6. The reactor 2 is provided with a material inlet, the reactor 2 is connected to a steam heating system, the gas outlet at the top of the reactor 2 is connected to the gas inlet of the supergravity rotating bed 1, the liquid outlet at the bottom of the supergravity rotating bed 1 is connected to the liquid inlet at the top of the reactor 2, the gas outlet at the top of the supergravity rotating bed 1 is connected to a primary condenser 3, and the liquid outlet at the bottom of the primary condenser 3 is connected to a buffer tank 5.

[0023] The bottom outlet of the buffer tank 5 is connected to a reflux pump 6, and the outlet of the reflux pump 6 is connected to a reflux pipeline 7 and a production pipeline 8. The reflux pipeline 7 is connected to the liquid reflux port at the top of the ultra-gravity rotating bed 1, and the production pipeline 8 is connected to a finished product cooler 9, and the finished product cooler 9 is connected to a finished product tank 12 and at least one distillation tank.

[0024] The top outlet of the buffer tank 5 is connected to a secondary condenser 4, and the secondary condenser 4 is connected to a vacuum system, a circulating water supply pipeline, and a circulating water return pipeline.

[0025] Through this arrangement, under the action of the vacuum system, the uncondensed steam of the primary condenser 3 will enter the secondary condenser 4 from the buffer tank 5, and will be further condensed into condensate by the secondary condenser 4 and then return to the buffer tank 5, thereby further improving the recovery rate of the solvent and improving the recovery efficiency.

[0026] The finished product cooler 9 is connected to a circulating water supply pipe and a circulating water return pipe, and the primary condenser 3 is connected to the circulating water supply pipe and the circulating water return pipe respectively.

[0027] The primary condenser 3, the secondary condenser 4 and the finished product cooler 9 are respectively one of a spirally wound tube heat exchanger, a shell and tube heat exchanger, a plate heat exchanger and a spiral plate heat exchanger.

[0028] The mother liquor is a tert-amyl alcohol mother liquor with an initial purity of 50%-80%, and further contains one or more of acetonitrile, pyridine and high boiling substances.

[0029] The distillate tank comprises a front distillate tank 10 and a middle distillate tank 11 .

[0030] The working pressure of the device is -99Kpa to normal pressure, and the working temperature is 0-150℃.

[0031] The ultra-gravity rotating bed 1 is composed of 1-5 layers of stators and rotors, and the rotation speed is 0-1200RPM.

[0032] The supergravity rotating bed 1 is a baffled rotating bed or a packed rotating bed.

[0033] Example 1

[0034] The device is used to distill and recover tert-amyl alcohol. The tert-amyl alcohol mother liquor is transported from the feed port to the reactor 2. The mother liquor is composed of 6% acetonitrile, 5% pyridine, 78% kg tert-amyl alcohol, 1% water, and 10% high boiling point. The vacuum system is evacuated to -60KPa, and then the material in the reactor 2 is heated by the steam heating system. After the material boils, the steam enters the supergravity rotating bed 1, and then enters the primary condenser 3 from the supergravity rotating bed 1 for condensation. The condensate enters the buffer tank 5. The uncondensed steam of the primary condenser 3 will enter the secondary condenser 4 through the buffer tank 5, and return to the buffer tank after being condensed into condensate by the secondary condenser 4. 5. After the buffer tank 5 has a certain liquid level, it is refluxed to the supergravity rotating bed 1 through the reflux pump 6. The speed of the supergravity rotating bed 1 is set to 400RPM. After reflux for a period of time, the reflux ratio is adjusted. The reflux and production are carried out through the reflux pump 6, the reflux pipeline 7 and the production pipeline 8. The produced material enters the finished product cooler 9 for cooling. When the top temperature of the supergravity rotating bed is stabilized between 50-60°C, it is produced into the front fraction tank 10. When the top temperature is stabilized between 60°C and 65°C, it is produced into the middle fraction tank 11. When the top temperature exceeds 65°C, the system is evacuated to -95KPa and produced into the finished product tank 12. When the top temperature exceeds 65°C, the production is stopped.

[0035] The product is condensed into a buffer tank through a primary condenser, and then refluxed into a supergravity rotating bed through the buffer tank. The front fraction acetonitrile is first distilled and taken out to the front fraction tank, and then the mixed liquid of acetonitrile, water and tert-amyl alcohol is taken out to the middle fraction tank, and finally the finished product tert-amyl alcohol is collected to the finished product tank. Finally, pyridine and high boiling products remain at the bottom of the kettle, and the purity of the recovered tert-amyl alcohol is greater than 98%.

[0036] Example 2

[0037] The device is used to distill and recover tert-amyl alcohol. The tert-amyl alcohol mother liquor is transported to the reactor 2 from the feed port. The mother liquor consists of 3% acetonitrile, 4% pyridine, 80% kg tert-amyl alcohol, 1% water, and 12% high boiling substances. The mother liquor is evacuated to -60 KPa by a vacuum system. Then, the material in the reactor 2 is heated by a steam heating system. After the material boils, the steam passes through the reactor 2 and enters the supergravity rotating bed 1. The supergravity rotating bed 1 then enters the primary condenser 3 for condensation. The condensate enters the buffer tank 5. The uncondensed steam of the primary condenser 3 enters the secondary condenser 4 via the buffer tank 5. After being condensed into condensate by the secondary condenser 4, it returns to the buffer tank 5. When the buffer tank 5 has After a certain liquid level, the liquid is refluxed to the supergravity rotating bed 1 through the reflux pump 6 and the reflux pipeline 7. The speed of the supergravity rotating bed 1 is set to 500RPM. After a period of reflux, the reflux ratio is adjusted. The liquid is refluxed and extracted through the reflux pump 6, the reflux pipeline 7 and the extraction pipeline 8. The extracted material enters the finished product cooler 9 for cooling. The top temperature of the supergravity rotating bed is stabilized between 50-60°C and is extracted into the front fraction tank 10. The top temperature is stabilized between 60°C and 65°C and is extracted into the middle fraction tank 11. When the top temperature exceeds 65°C, the system is evacuated to -95KPa and extracted into the finished product tank 12. When the top temperature exceeds 65°C, the extraction is stopped. The purity of the recovered tertiary amyl alcohol is greater than 99%. The above disclosure is only the preferred embodiment of the utility model, and it is certainly not used to limit the scope of the rights of the utility model. Therefore, the equivalent changes made according to the claims of the utility model are still within the scope of the utility model.

Claims

1. A device for recovering a mother liquor containing a multi-component organic solvent by supergravity vacuum distillation, comprising a reactor (2), a supergravity rotating bed (1), and a reflux pump (6), wherein the reactor (2) is provided with a material inlet, the reactor (2) is connected to a steam heating system, the gas outlet at the top of the reactor (2) is connected to the gas inlet of the supergravity rotating bed (1), the liquid outlet at the bottom of the supergravity rotating bed (1) is connected to the liquid inlet at the top of the reactor (2), the gas outlet at the top of the supergravity rotating bed (1) is connected to a primary condenser (3), and the liquid outlet at the bottom of the primary condenser (3) is connected to a buffer tank (5), characterized in that: The bottom outlet of the buffer tank (5) is connected to a reflux pump (6), the outlet of the reflux pump (6) is connected to a reflux pipeline (7) and a production pipeline (8), the reflux pipeline (7) is connected to a liquid reflux port at the top of the supergravity rotating bed (1), the production pipeline (8) is connected to a finished product cooler (9), and the finished product cooler (9) is connected to a finished product tank (12) and at least one fraction tank.

2. The device for recovering a mother liquor containing a multi-component organic solvent by ultra-gravity vacuum distillation according to claim 1, characterized in that: The top outlet of the buffer tank (5) is connected to a secondary condenser (4), and the secondary condenser (4) is connected to a vacuum system, a circulating water supply pipeline, and a circulating water return pipeline.

3. The device for recovering a mother liquor containing a multi-component organic solvent by ultra-gravity vacuum distillation according to claim 1, characterized in that: The finished product cooler (9) is connected to a circulating water supply pipe and a circulating water return pipe, and the primary condenser (3) is connected to the circulating water supply pipe and the circulating water return pipe respectively.

4. The device for recovering a mother liquor containing a multi-component organic solvent by ultra-gravity vacuum distillation according to claim 2, characterized in that: The primary condenser (3), the secondary condenser (4) and the finished product cooler (9) are respectively one of a spirally wound tube heat exchanger, a shell and tube heat exchanger, a plate heat exchanger and a spiral plate heat exchanger.

5. The device for recovering a mother liquor containing a multi-component organic solvent by ultra-gravity vacuum distillation according to claim 1, characterized in that: The distillate tank comprises a front distillate tank (10) and an intermediate distillate tank (11).

6. The device for recovering a mother liquor containing a multi-component organic solvent by ultra-gravity vacuum distillation according to claim 1, characterized in that: The working pressure of the device is -99Kpa to normal pressure, and the working temperature is 0-150℃.

7. The device for recovering a mother liquor containing a multi-component organic solvent by ultra-gravity vacuum distillation according to claim 1, characterized in that: The ultra-gravity rotating bed (1) is composed of 1 to 5 layers of stators and rotors, and has a rotation speed of 0 to 1200 RPM.

8. The device for recovering a mother liquor containing a multi-component organic solvent by ultra-gravity vacuum distillation according to any one of claims 1 to 4, characterized in that: The supergravity rotating bed (1) is a baffled rotating bed or a packed rotating bed.

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