Water removal equipment for Grignard reaction solvent

Abstract

The utility model provides water removal equipment for a Grignard reaction solvent, and relates to the technical field of chemical raw material production, the water removal equipment comprises a placing assembly and a dewatering and drying assembly, a calcium oxide material is placed in a grid net piece, a to-be-recycled solvent enters a reaction tank through a solvent inlet pipeline, and the to-be-recycled solvent enters the reaction tank through continuous input; the solvent slowly rises from bottom to top to cover the calcium oxide material, the calcium oxide reacts with water to generate calcium hydroxide, the calcium hydroxide is strong alkali, peroxides in THF are destroyed and cannot be enriched, the addition of an antioxidant is omitted, the cost is reduced, impurities in the product are reduced, and the product quality is improved. Finally, the dry solvent subjected to the chemical reaction flows into the condenser for cooling through the solvent outlet pipeline and then is input into the collecting tank, the to-be-recycled solvent is fully dried and dewatered by fully contacting the to-be-recycled solvent with the calcium oxide material, and then the dry solvent subjected to the chemical reaction is cooled through the condenser, so that the to-be-recycled solvent is recycled. Therefore, the dehydrated solvent can be conveniently collected.

Description

Technical Field

[0001] The present application relates to the technical field of chemical raw material production, and in particular to a device for removing water from a Grignard reaction solvent. Background Art

[0002] After the Grignard reaction is quenched, the solvent contains water. Since the quenching water is 1% hydrochloric acid, there is a small amount of acidity remaining. If you want to continue to use the solvent, you need to dry it.

[0003] In the prior art, molecular sieves or calcium carbonate are generally used in the reaction tank for water absorption and drying, and then antioxidants are added to control the safe use of peroxides in THF. Due to the difference in boiling points, the antioxidants remain in the material during desolvation. Therefore, each batch needs to be supplemented during the chemical reaction. The chemical reaction is slow, the production efficiency is low, and the production cost is increased, resulting in complex production steps, diverse chemical reactions and increased impurity content in the product. Therefore, there are deficiencies. Utility Model Content

[0004] In order to make up for the above shortcomings, the utility model provides a solvent dewatering device for Grignard reaction, which uses calcium oxide for water absorption and drying, does not require the addition of antioxidants during the production process, has a simple chemical reaction, reduces production costs, simplifies the production steps, reduces the impurity content of the product, and improves product quality.

[0005] This application is implemented as follows:

[0006] A placement component, wherein the placement component includes a reaction cell;

[0007] A dehydration and drying component, comprising a solvent inlet pipe, a grid fence, a solvent outlet pipe and a condenser, wherein the solvent inlet pipe is fixedly connected to the bottom end of the reaction tank, the grid fence is fixedly connected to the reaction tank, the solvent outlet pipe is fixedly connected to the upper end of the reaction tank, and the condenser is fixedly connected to the solvent outlet pipe.

[0008] In one embodiment of the present application, a sewage cleaning port is provided on one side of the reaction tank, and the sewage cleaning port is connected to the grid fence.

[0009] In one embodiment of the present application, the grid fence mesh comprises a grid fence and a bottom mesh plate, the bottom mesh plate is fixedly connected to the reaction tank, and the grid fence is fixedly connected to the four sides of the bottom mesh plate.

[0010] In one embodiment of the present application, solenoid valves are provided on both the solvent inlet pipe and the solvent outlet pipe.

[0011] In one embodiment of the present application, the condenser is a floating head heat exchanger.

[0012] In one embodiment of the present application, the bottom of the reaction tank is an inverted square cone.

[0013] In one embodiment of the present application, a mounting bracket is fixedly connected to the periphery of the reaction pool.

[0014] The beneficial effects of the present application are as follows: calcium oxide material is placed in a grid mesh, and the solvent to be recovered enters the reaction tank through a solvent inlet pipe. By continuously inputting, the solvent slowly rises from bottom to top to cover the calcium oxide material. Calcium oxide reacts with water to produce calcium hydroxide. Calcium hydroxide is a strong base, which destroys the peroxide in THF, thereby preventing it from being enriched, eliminating the need for the addition of antioxidants, reducing costs, and reducing the introduction of impurities into the product. Finally, the dry solvent after the chemical reaction flows through a solvent outlet pipe into a condenser for cooling, and is then input into a collection tank. The device allows the solvent to be recovered to flow from bottom to top, so that its flow rate is high. The reaction temperature of the solvent to be recovered is slowed down, so that the solvent to be recovered is fully in contact with the calcium oxide material, and the solvent to be recovered is fully dried and dehydrated. The dried solvent that has undergone the chemical reaction is then cooled by a condenser, so that the dehydrated solvent can be easily collected. During the entire drying and dehydration process, the material is fully in contact with the solvent, the chemical reaction time is sufficient, the drying and dehydration effect is good, and the water absorption is fast. There is no need to continuously add an antioxidant, thus reducing production costs and production steps. The problem of slow chemical reaction in the prior art, resulting in low dehydration efficiency, the need to continuously add an antioxidant, resulting in increased production costs, complicated production steps, diverse chemical reactions, and increased impurity content in the product is solved. BRIEF DESCRIPTION OF THE DRAWINGS

[0015] In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the following is a brief introduction to the drawings required for use in the embodiments. It should be understood that the following drawings only show certain embodiments of the present invention and therefore should not be regarded as limiting the scope. For ordinary technicians in this field, other relevant drawings can be obtained based on these drawings without creative work.

[0016] Figure 1 A schematic structural diagram of a Grignard reaction solvent dewatering device is provided for an embodiment of the present application;

[0017] Figure 2 A schematic structural diagram of a dehydration and drying component is provided for an embodiment of the present application;

[0018] Figure 3 A schematic structural diagram of a grid fence mesh member is provided for the embodiment of the present application;

[0019] In the figure: 100 - placement component; 110 - reaction tank; 120 - sewage outlet; 130 - mounting bracket; 200 - dehydration and drying component; 210 - solvent inlet pipe; 220 - grid fence; 221 - grid fence; 222 - bottom mesh plate; 230 - solvent outlet pipe; 240 - condenser; DETAILED DESCRIPTION

[0020] The following embodiments of the present invention are described in detail with reference to the accompanying drawings. In the absence of conflict, the following embodiments and features in the embodiments may be combined with each other.

[0021] like Figure 1-Figure 3 As shown, according to an embodiment of the present application, a device for removing water from a Grignard reaction solvent includes:

[0022] The placement component 100 includes a reaction tank 110;

[0023] The dehydration and drying component 200 includes a solvent inlet pipe 210, a grid fence 220, a solvent outlet pipe 230 and a condenser 240. The solvent inlet pipe 210 is fixedly connected to the bottom end of the reaction tank 110, the grid fence 220 is fixedly connected to the reaction tank 110, the solvent outlet pipe 230 is fixedly connected to the upper end of the reaction tank 110, and the condenser 240 is fixedly connected to the solvent outlet pipe 230. The calcium oxide material is placed in the grid mesh 220, and the solvent to be recovered enters the reaction tank 110 through the solvent inlet pipe 210. Through continuous input, the solvent slowly rises from bottom to top to cover the calcium oxide material. Calcium oxide reacts with water to produce calcium hydroxide. Calcium hydroxide is a strong base, which destroys the peroxide in THF, thereby preventing it from being enriched, eliminating the need for antioxidants, reducing costs and reducing impurities in the product. Finally, the dry solvent after the chemical reaction flows through the solvent outlet pipe 230 into the condenser 240 for cooling, and then is input into the collection tank. This device allows the solvent to be recovered to flow from bottom to top. The speed is slowed down, so that the solvent to be recovered is fully in contact with the calcium oxide material, so that the solvent to be recovered is fully dried and dehydrated, and then the dried solvent that has undergone the chemical reaction is cooled by the condenser 240, so as to facilitate the collection of the dehydrated solvent. During the entire drying and dehydration process, the material is fully in contact with the solvent, the chemical reaction time is sufficient, the drying and dehydration effect is good, and the water absorption is fast. There is no need to continuously add antioxidants, which reduces production costs and production steps, and solves the problems of slow chemical reactions in the prior art, resulting in low dehydration efficiency, and the need to continuously add antioxidants, resulting in increased production costs, complex production steps, diverse chemical reactions and increased impurity content in the product.

[0024] like Figure 2As shown, a cleaning port 120 is provided on one side of the reaction tank 110, and the cleaning port 120 is connected to the grid fence 220. The cleaning port 120 is convenient for cleaning the material residue on the grid fence 220 after chemical drying and dehydration. Solenoid valves are provided on the solvent inlet pipe 210 and the solvent outlet pipe 230. The solenoid valve is used to control the inlet and outlet of the solvent. The condenser 240 is a floating head heat exchanger. Heat is usually generated after a chemical reaction. At this time, the solvent liquid temperature is relatively high. The floating head heat exchanger can quickly cool the solvent, thereby being able to collect the solvent more quickly and improve production efficiency. A mounting bracket 130 is fixedly connected to the surrounding side of the reaction tank 110. The mounting bracket 130 is used to fix the reaction tank 110.

[0025] like Figure 3 As shown, the grid fence mesh 220 includes a grid bar 221 and a bottom mesh plate 222. The bottom mesh plate 222 is fixedly connected to the reaction tank 110, and the grid bar 221 is fixedly connected to the periphery of the bottom mesh plate 222. The grid bar 221 and the bottom mesh plate 222 are arranged in combination to allow the calcium oxide material to be placed in the reaction tank 110, so that it can fully contact the solvent, and to prevent the waste residue of the material after the reaction from falling directly into the reaction tank 110, thereby not affecting subsequent cleaning. The bottom of the reaction tank 110 is an inverted square cone. The inverted square cone provides a certain amount of reserved space for the solvent, allowing the solvent to flow slowly in the reaction tank 110 and contact the calcium oxide material.

[0026] In summary, the working principle of a Grignard reaction solvent dewatering device according to an embodiment of the present invention is as follows: calcium oxide material is placed on the bottom mesh plate 222, and the solvent to be recovered enters the reaction tank 110 through the solvent inlet pipe 210. Through continuous input, the solvent slowly rises from bottom to top to cover the calcium oxide material. Calcium oxide reacts with water to produce calcium hydroxide. Calcium hydroxide is a strong base, which destroys the peroxide in THF, thereby preventing it from being enriched, eliminating the need for the addition of antioxidants, reducing costs, and reducing the introduction of impurities into the product. Finally, the dry solvent after the chemical reaction passes through the solvent outlet pipe 230, flows into the condenser 240 for cooling, and is then input into the collection tank. This device slows down the flow rate of the solvent to be recovered by allowing it to flow from bottom to top. When the solvent flows, it contacts the calcium oxide material and starts a dehydration reaction. When the solvent flows to the solvent outlet pipe 230, the solvent to be recovered has been fully contacted with the calcium oxide material, so that the solvent to be recovered is fully dried and dehydrated. The dried solvent that has undergone the chemical reaction is then cooled by the condenser 240, so as to facilitate the collection of the dehydrated solvent. During the entire drying and dehydration process, the material is fully in contact with the solvent, the chemical reaction time is sufficient, the drying and dehydration effect is good, and the water absorption is fast. There is no need to continuously add antioxidants, which reduces production costs and production steps, and solves the problems in the prior art of slow chemical reaction, resulting in low dehydration efficiency, and the need to continuously add antioxidants, resulting in increased production costs, complex production steps, diverse chemical reactions and increased impurity content in the product.

[0027] The above are merely examples of the present application and are not intended to limit the scope of protection of the present application. For those skilled in the art, the present application may have various changes and variations. Any modifications, equivalent replacements, improvements, etc. made within the spirit and principles of the present application should be included within the scope of protection of the present application. It should be noted that similar numbers and letters represent similar items in the following drawings, so once an item is defined in one drawing, it does not need to be further defined and explained in the subsequent drawings.

Claims

1. A solvent dewatering device for Grignard reaction, characterized in that: include: A placement assembly (100), wherein the placement assembly (100) includes a reaction pool (110); A dehydration and drying component (200) includes a solvent inlet pipe (210), a grid fence member (220), a solvent outlet pipe (230) and a condenser (240), wherein the solvent inlet pipe (210) is fixedly connected to the bottom end of the reaction tank (110), the grid fence member (220) is fixedly connected to the inside of the reaction tank (110), the solvent outlet pipe (230) is fixedly connected to the upper end of the reaction tank (110), and the condenser (240) is fixedly connected to the solvent outlet pipe (230).

2. The device for removing water from a Grignard reaction solvent according to claim 1, characterized in that: A sewage cleaning port (120) is provided on one side of the reaction tank (110), and the sewage cleaning port (120) is connected to the grid fence (220).

3. The device for removing water from a Grignard reaction solvent according to claim 1, characterized in that: The grid fence mesh (220) includes a grid fence (221) and a bottom mesh plate (222), wherein the bottom mesh plate (222) is fixedly connected to the inside of the reaction tank (110), and the grid fence (221) is fixedly connected to the four sides of the bottom mesh plate (222).

4. The device for removing water from a Grignard reaction solvent according to claim 1, characterized in that: The solvent inlet pipe (210) and the solvent outlet pipe (230) are both provided with electromagnetic valves.

5. The device for removing water from a Grignard reaction solvent according to claim 1, characterized in that: The condenser (240) is a floating head heat exchanger.

6. The device for removing water from a Grignard reaction solvent according to claim 1, characterized in that: The bottom of the reaction tank (110) is an inverted square cone.

7. The device for removing water from a Grignard reaction solvent according to claim 1, characterized in that: A mounting bracket (130) is fixedly connected to the periphery of the reaction pool (110).

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