Water removal system for reaction system

Abstract

The utility model discloses a water removal system for a reaction system. The water removal system comprises a reactor, a solvent storage tank, a constant-temperature heat tracing jacket, a stirrer, an oil-water separator, a gravity sensor, a condenser and a water collection tank, the gas phase outlet is communicated with an inlet of the oil-water separator through a pipeline, a gas phase outlet in the top of the oil-water separator is communicated with a gas inlet of the condenser through a pipeline, and a liquid outlet of the condenser is communicated with the inlet of the oil-water separator through a pipeline; a liquid phase outlet in the bottom of the oil-water separator is communicated with an inlet of the water collecting tank through a pipeline; and a water distribution switch is arranged at a liquid phase outlet of the oil-water separator. The solvent which does not participate in the reaction and has a boiling point similar to that of water is added into the reactor through the solvent storage tank, and the water can be discharged out of the reactor in time in the reaction process by utilizing the principle that the solvent and the water are azeotropic, so that the hydrolysis reaction is prevented, the pressure in the reactor can be prevented from being too high, the product yield can be improved, and the production cost is reduced. The usage amount of raw materials is further reduced.

Description

Technical field:

[0001] The utility model relates to a water removal device, in particular to a water removal system for a reaction system. Background technology:

[0002] Some chemical reactions, such as condensation reactions and reactions between aldehydes, ketones and alcohols, will generate water. If the generated water is not removed in time in the system, hydrolysis or other side reactions will occur, affecting the quality and output of the product. Some reactions may also be accompanied by hydrolysis or other side reactions, which may lead to safety accidents in serious cases. Therefore, how to remove water during the production process is the key to this type of reaction.

[0003] At present, the water is usually removed by drying the material under reduced pressure after the reaction is completed. However, the water cannot be removed in time; moreover, the processing cost is high and the production cycle is long. Utility model content:

[0004] In order to solve the above problems, the utility model aims to provide a reaction system water removal system.

[0005] The utility model is implemented by the following technical solutions:

[0006] A reaction system water removal system, comprising a reactor, a solvent storage tank, a constant temperature heating jacket, an agitator, an oil-water separator, a gravity sensor, a condenser and a water collection tank;

[0007] The constant temperature heating jacket is provided on the outer wall of the reactor, a feed port and a gas phase outlet are provided on the top of the reactor, and a discharge port is provided at the bottom of the reactor; the agitator is provided in the reactor; the outlet of the solvent storage tank is connected to the feed port through a pipeline;

[0008] The gas phase outlet is connected to the inlet of the oil-water separator through a pipeline, the gas phase outlet at the top of the oil-water separator is connected to the air inlet of the condenser through a pipeline, and the liquid outlet of the condenser is connected to the inlet of the oil-water separator through a pipeline; the liquid phase outlet at the bottom of the oil-water separator is connected to the inlet of the water collecting tank through a pipeline; a water diversion switch is provided at the liquid phase outlet of the oil-water separator;

[0009] The oil-water separator is arranged on a fixed support, and the gravity sensor is arranged between the fixed support and the oil-water separator;

[0010] The signal output end of the gravity sensor is signal-connected to the signal input end of the controller, and the signal output end of the controller is signal-connected to the signal input end of the water diversion switch.

[0011] Furthermore, a heat medium inlet is provided at the bottom of the constant temperature heating jacket, and a heat medium outlet is provided at the top of the constant temperature heating jacket;

[0012] A regulating valve is provided at the heat medium inlet; a temperature sensor is provided in the reactor;

[0013] The signal output end of the temperature sensor is signal-connected to the signal input end of the controller, and the signal output end of the controller is signal-connected to the signal input end of the regulating valve.

[0014] Furthermore, it also includes a dryer, the middle part of the oil-water separator is connected to the inlet of the dryer through a pipeline, and the outlet of the dryer is divided into two paths, one of which is connected to the feed port of the reactor through a pipeline; the other is connected to the inlet of the oil-water separator through a pipeline;

[0015] A micro-water content detector is provided at the outlet of the dryer, a first reflux valve is provided on the pipeline connecting the dryer and the reactor, and a second reflux valve is provided on the pipeline connecting the dryer outlet and the oil-water separator;

[0016] The signal output end of the micro-water content detector is connected to the signal input end of the controller, and the signal output end of the controller is connected to the signal input ends of the first reflux valve and the second reflux valve respectively.

[0017] Advantages of the utility model:

[0018] The utility model adds a solvent which does not participate in the reaction and has a boiling point close to that of water into a reactor through a solvent storage tank, and utilizes the principle of azeotropy of the solvent and water to discharge water from the reactor in a timely manner during the reaction, thereby preventing the occurrence of a hydrolysis reaction and preventing the pressure in the reactor from being too high, thereby improving the product yield and further reducing the amount of raw materials used. Description of the drawings:

[0019] Figure 1 It is a structural schematic diagram of this embodiment;

[0020] Figure 2 Schematic diagram of signal connection in this embodiment.

[0021] In the figure: reactor 1, constant temperature heating jacket 2, solvent storage tank 3, agitator 4, oil-water separator 5, gravity sensor 6, condenser 7, water collecting tank 8, water distribution switch 9, fixed support 10, controller 11, regulating valve 12, temperature sensor 13, heat medium inlet 14, heat medium outlet 15, dryer 16, trace water content detector 17, first reflux valve 18, second reflux valve 19. Specific implementation method:

[0022] like Figure 1-2 A reaction system dewatering system shown includes a reactor 1, a solvent storage tank 3, a constant temperature heating jacket 2, an agitator 4, an oil-water separator 5, a gravity sensor 6, a condenser 7 and a water collection tank 8;

[0023] A constant temperature heating jacket 2 is provided on the outer wall of the reactor 1, a feed port and a gas phase outlet are provided on the top of the reactor 1, and a discharge port is provided at the bottom of the reactor 1; an agitator 4 is provided in the reactor 1; the outlet of the solvent storage tank 3 is connected to the feed port through a pipeline;

[0024] The gas phase outlet is connected to the inlet of the oil-water separator 5 through a pipeline, the gas phase outlet at the top of the oil-water separator 5 is connected to the air inlet of the condenser 7 through a pipeline, and the liquid outlet of the condenser 7 is connected to the inlet of the oil-water separator 5 through a pipeline; the liquid phase outlet at the bottom of the oil-water separator 5 is connected to the inlet of the water collecting tank 8 through a pipeline; a water diversion switch 9 is provided at the liquid phase outlet of the oil-water separator 5;

[0025] The oil-water separator 5 is arranged on a fixed support 10, and a gravity sensor 6 is arranged between the fixed support 10 and the oil-water separator 5;

[0026] The signal output end of the gravity sensor 6 is signal-connected to the signal input end of the controller 11 , and the signal output end of the controller 11 is signal-connected to the signal input end of the water diversion switch 9 .

[0027] A heat medium inlet 14 is provided at the bottom of the constant temperature heating jacket 2, and a heat medium outlet 15 is provided at the top of the constant temperature heating jacket 2;

[0028] A regulating valve 12 is provided at the heat medium inlet 14; a temperature sensor 13 is provided in the reactor 1;

[0029] The signal output end of the temperature sensor 13 is signal-connected to the signal input end of the controller 11 , and the signal output end of the controller 11 is signal-connected to the signal input end of the regulating valve 12 .

[0030] This embodiment also includes a dryer 16. The middle part of the oil-water separator 5 is connected to the inlet of the dryer 16 through a pipeline. The outlet of the dryer 16 is divided into two paths, one of which is connected to the feed port of the reactor 1 through a pipeline; and the other is connected to the inlet of the oil-water separator 5 through a pipeline.

[0031] A micro-water content detector 17 is provided at the outlet of the dryer 16, a first reflux valve 18 is provided on the pipeline connecting the dryer 16 and the reactor 1, and a second reflux valve 19 is provided on the pipeline connecting the outlet of the dryer 16 and the oil-water separator 5;

[0032] The signal output end of the trace water content detector 17 is signal-connected to the signal input end of the controller 11 , and the signal output end of the controller 11 is signal-connected to the signal input ends of the first reflux valve 18 and the second reflux valve 19 , respectively.

[0033] Job Description:

[0034] When isopropyl ester is prepared by using this embodiment, high-temperature steam is introduced into the constant temperature heating jacket 2 to provide the reactor 1 with the temperature required for the reaction, and the flow rate of the heat medium entering the constant temperature heating jacket 2 is adjusted by adjusting the opening size of the regulating valve 12, so that a constant temperature state can be maintained in the reactor 1 to ensure efficient reaction.

[0035] The reaction raw material isopropanolamine and a phase transfer catalyst are added into the reactor 1 through the feed port, sulfuric acid is then added dropwise into the reactor, and an appropriate amount of a solvent immiscible with water (the target product is insoluble in the solvent) is added into the reactor 1, the boiling point of the solvent is close to that of water, and the density is smaller than that of water. In this embodiment, toluene is used as the solvent.

[0036] Under the action of the agitator 4, the reactants are fully contacted to accelerate the reaction. During the reaction, when the internal temperature of the reaction system exceeds 102°C, the solvent and the water produced in the reaction form an azeotropic mixture, which enters the oil-water separator 5 through the gas phase outlet of the reactor 1. The gas phase in the oil-water separator 5 enters the condenser 7 and condenses into a liquid state and then returns to the oil-water separator 5. According to the different properties of water and solvent density, that is, the principle of different solvent masses under the same volume, the gravity sensor 6 is interlocked with the water diversion switch 9. Before using this embodiment, the trigger parameters of the gravity sensor 6 are preset in the controller 11 in advance. When the mixed liquid of water and toluene in the oil-water separator 5 reaches the preset upper weight limit, the water diversion switch 9 automatically opens the valve to discharge the water in the lower layer into the water collection tank 8, so that the solvent remains in the oil-water separator 5. When the gravity sensor 6 detects that the weight of the liquid in the oil-water separator 5 drops to the preset lower weight limit, the water diversion switch 9 automatically closes the valve to stop discharging liquid to the water collection tank 8.

[0037] Since the volume of the oil-water separator 5 is known, when the oil-water separator 5 is filled with water, the total weight M1 of the oil-water separator 5 can be known; when the oil-water separator 5 is filled with toluene, the total weight M2 of the oil-water separator 5 can also be known; in this embodiment, in order to prevent water from entering the subsequent dryer 16, the preset upper weight limit can be set to 0.95*M1; similarly, in order to avoid discharging the solvent into the sump 8, the preset lower weight limit can be set to 1.05*M2.

[0038] The solvent in the oil-water separator 5 is further passed through the dryer 16 to further remove the water contained in the solvent. The water content in the dried solvent can be detected using the micro-water content detector 17. When the detected water content is within the process allowable content range, the first valve is opened to return the dried solvent to the reactor 1 for reuse; when the detected water content exceeds the process allowable content range, the second valve is opened to return the dried solvent to the oil-water separator 5 to participate in oil-water separation again.

[0039] Through this embodiment, a solvent with a boiling point close to that of water is used, and the principle of azeotropy between the solvent and water is utilized, so that water can be discharged from the reactor 1 in a timely manner during the reaction process to prevent the occurrence of hydrolysis reaction, and to prevent the pressure in the reactor 1 from being too high, thereby increasing the product yield and reducing the amount of raw materials used.

[0040] Since toluene does not participate in the reaction, the recovered toluene can be returned to the reactor 1 for recycling after oil-water separation and drying. The solvent recovery rate can reach 80.7%.

[0041] Even if a small amount of toluene remains in the target product in the reactor 1, the target product can be obtained by natural air drying for 24 hours or heating under reduced pressure at 60° C. for 30 minutes, due to the volatility of toluene.

[0042] After multiple experimental verifications, through this embodiment, the yield of the target product can be increased by 7.0-8.7%, the amount of raw materials used can be reduced by 6.9%-7.6%, and the preparation time for preparing the same amount of product can be reduced by 8.5-10 hours.

[0043] 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, improvements, etc. 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 system water removal system, characterized in that: It includes reactor, solvent storage tank, constant temperature heating jacket, agitator, oil-water separator, gravity sensor, condenser and water collection tank; The constant temperature heating jacket is provided on the outer wall of the reactor, a feed port and a gas phase outlet are provided on the top of the reactor, and a discharge port is provided at the bottom of the reactor; the agitator is provided in the reactor; the outlet of the solvent storage tank is connected to the feed port through a pipeline; The gas phase outlet is connected to the inlet of the oil-water separator through a pipeline, the gas phase outlet at the top of the oil-water separator is connected to the air inlet of the condenser through a pipeline, and the liquid outlet of the condenser is connected to the inlet of the oil-water separator through a pipeline; the liquid phase outlet at the bottom of the oil-water separator is connected to the inlet of the water collecting tank through a pipeline; a water diversion switch is provided at the liquid phase outlet of the oil-water separator; The oil-water separator is arranged on a fixed support, and the gravity sensor is arranged between the fixed support and the oil-water separator; The signal output end of the gravity sensor is signal-connected to the signal input end of the controller, and the signal output end of the controller is signal-connected to the signal input end of the water diversion switch.

2. A reaction system water removal system according to claim 1, characterized in that: A heat medium inlet is provided at the bottom of the constant temperature heating jacket, and a heat medium outlet is provided at the top of the constant temperature heating jacket; A regulating valve is provided at the heat medium inlet; a temperature sensor is provided in the reactor; The signal output end of the temperature sensor is signal-connected to the signal input end of the controller, and the signal output end of the controller is signal-connected to the signal input end of the regulating valve.

3. A reaction system water removal system according to claim 1, characterized in that: It also includes a dryer, the middle part of the oil-water separator is connected to the inlet of the dryer through a pipeline, and the outlet of the dryer is divided into two paths, one of which is connected to the feed port of the reactor through a pipeline; the other is connected to the inlet of the oil-water separator through a pipeline; A micro-water content detector is provided at the outlet of the dryer, a first reflux valve is provided on the pipeline connecting the dryer and the reactor, and a second reflux valve is provided on the pipeline connecting the dryer outlet and the oil-water separator; The signal output end of the micro-water content detector is connected to the signal input end of the controller, and the signal output end of the controller is connected to the signal input ends of the first reflux valve and the second reflux valve respectively.

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