Distillation equipment for producing and processing hafnate
By designing distillation equipment for hafnate production, optimizing process flow and equipment configuration, the problems of low efficiency and environmental pollution in hafnate production are solved, and high yield, high purity and low energy consumption are achieved, reducing production results Raw material consumption and waste emissions.
Patent Information
- Application Number
- CN202421022853.0
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2024-05-13
- Publication Date
- 2025-01-03
- Estimated Expiration
- 2034-05-13
AI Technical Summary
In the existing hafnium acid ester production process, the reactor has poor mass and heat transfer effect and low efficiency, and it is difficult to separate the product from solvents and by-products, resulting in low yields, serious environmental pollution, and increased raw material consumption.
A distillation equipment including reaction vessel, distillation kettle, rectifier, drying box and purification box was designed. Through stirring, centrifugal filtration, distillation and distillation, the raw material ratio and process flow are optimized to achieve high-purity hafnium acid. Ester production and waste emissions are reduced through drying and purification treatment, and solvent recycling.
It improves the yield and purity of hafnate ester, reduces energy consumption, reduces raw material waste and pollution, protects the environment, and increases the added value of by-products.
Smart Images
Figure CN222286410U_ABST
Abstract
Description
Technical Field
[0001] The utility model relates to a distillation device for the production and processing of hafnium esters, belonging to the technical field of fine chemical technology. Background Art
[0002] Hafnium esters are ultra-high temperature ceramic precursors and key basic raw materials for the preparation of ultra-high temperature ceramic-based composite materials. After years of development, their preparation technology has become increasingly mature, and their comprehensive performance has shown obvious advantages. They have been used in the aerospace field. There are many types of hafnium esters, and the production processes and equipment used for various hafnium esters are also different.
[0003] The existing hafnium ester production process and equipment all adopt intermittent kettle production process technology, the mass transfer and heat transfer effect of the reactor is poor, the reaction efficiency is poor, the separation of the product from the solvent and by-products is difficult, the efficiency is low, and more three wastes are generated during the production process, which has great harm to the environment. The industrial production process of hafnium ester is mainly based on the direct esterification method of alcohol and metal hafnium salt reaction, which has a low yield. Hydrogen chloride is generated during the reaction, and hydrogen chloride reacts with alcohol to form chlorinated products, which reduces the yield of hafnium ester. In order to reduce the occurrence of side reactions, vacuuming is usually used to reduce the content of hydrogen chloride in the system, but the generated hydrogen chloride and the hydrochloric acid obtained by absorption often corrode the equipment, and the hydrogen chloride removed from the system by vacuum also carries part of the raw materials, which increases the loss of alcohol and metal hafnium salt, and greatly increases the consumption of raw materials. Utility Model Content
[0004] The utility model aims to provide a distillation device for the production and processing of hafnium esters to solve the problems raised in the above-mentioned background technology.
[0005] In order to achieve the above purpose, the utility model provides the following technical solutions:
[0006] A distillation device for producing and processing hafnium esters comprises a base frame, a first reaction vessel and a second reaction vessel, wherein the first reaction vessel is arranged at the upper left of the base frame, the lower right end of the first reaction vessel is sealedly connected to a centrifuge, the lower right end of the centrifuge is sealedly connected to a distillation kettle, the right side of the distillation kettle is arranged with a second reaction vessel, the right side of the second reaction vessel is arranged with a distillation kettle, the lower right end of the distillation kettle is sealedly connected to a finished product storage tank, the distillation kettle, the second reaction vessel and the distillation kettle are all fixedly connected to the base frame, the lower end of the centrifuge is sealedly connected to a drying box, the drying box is fixedly connected to the base frame, the lower left end of the drying box is sealedly connected to a by-product silo, and the by-product silo is fixedly connected to the base frame.
[0007] Furthermore, a stirrer is fixedly connected to the upper ends of the reaction container 1 and the reaction container 2.
[0008] Furthermore, the left upper end of the reaction container 1 is sealed with a proportioning feeding box, the upper end of the proportioning feeding box is sealed with a feed pipe, the upper end of the feed pipe is sealed with a raw material box, and the upper end of the raw material box is sealed with an addition pipe.
[0009] Furthermore, the proportioning feeding box is rotatably connected to a material guide paddle inside, the left end of the proportioning feeding box is fixedly connected to a fixed box, the upper front end of the fixed box is fixedly connected to a motor, the rear end of the output shaft of the motor is fixedly connected to a worm, the lower end of the worm is meshingly connected to a worm wheel, the worm wheel is fixedly connected to the material guide paddle, and the outer side of the material guide paddle is fixedly connected to a proportioning partition.
[0010] Furthermore, the distillation kettle and the upper right side of the reaction vessel 2 are both sealedly connected with a liquid pump, the right end discharge pipe of the liquid pump is sealedly connected to the reaction vessel 2 and the distillation kettle respectively, and the upper left side of the reaction vessel 2 is sealedly connected with an alcohol supplement tank.
[0011] Furthermore, a distillation recovery pipe is sealedly connected at the middle position of the upper end of the distillation kettle, the distillation recovery pipe is sealedly connected to reaction vessel one, the upper right end of the distillation recovery pipe is sealedly connected to a rectification recovery pipe, the rectification recovery pipe is sealedly connected to the distillation kettle, and a check valve is sealedly connected between the distillation recovery pipe and the rectification recovery pipe.
[0012] Furthermore, a solid waste discharge pipe is sealedly connected to the left side of the lower end of the centrifuge, a solenoid valve is sealedly connected to the upper end of the solid waste discharge pipe, the solid waste discharge pipe is sealedly connected to the drying box, a transmission shaft is fixedly connected to the lower end of the internal shaft of the centrifuge, the transmission shaft is rotatably connected to the drying box, a flap blade is fixedly connected to the lower end of the transmission shaft, and an electrically controlled switch door is fixedly connected to the lower left end of the drying box.
[0013] Furthermore, a purification box is sealedly connected to the right side of the upper end of the drying box, and an exhaust pipe is sealedly connected to the upper end of the purification box.
[0014] The beneficial effects of the utility model are:
[0015] The utility model firstly adds alcohol and solvent as raw materials into a reaction container one, continuously stirs, drips metal salt into the reaction container one according to the molar ratio of hafnium in the metal salt to alcohol, and introduces an acid-binding agent, after the reaction in the reaction container one is completed, centrifugal filtration is performed in a centrifuge, and then distilled in a distillation kettle, the obtained product can be used as an intermediate of a crude product, the intermediate continues to enter the reaction container two to participate in subsequent reactions, and then secondary distillation is performed in a rectification kettle, so as to obtain hafnium ester with higher purity, and the low-boiling point substances in the finished product are purified more perfectly, and the worm can drive the worm wheel and the guide blade to rotate under the rotation of the motor, so that the alcohol, the solvent, the metal salt and the acid-binding agent can be automatically proportioned and loaded under the rotation of the guide blade and the proportioning partition, the raw material proportioning formula is optimized, the conversion rate of the finished product is improved, and the process flow is simplified, thereby improving the stability of product quality. At the same time, compared with the traditional production process technology, the production process flow has high yield and high purity. The utility model has low energy consumption. The solid can be centrifugally filtered in the centrifuge through the centrifuge, and the filtered solid can be discharged into the drying box through the solid waste discharge pipe through the control of the electromagnetic valve. The rotation of the centrifuge can drive the transmission shaft to rotate, so that the flip blade can rotate, and the solid waste can be dried and purified. The by-product with a mellow body is sent into the by-product silo through the electric control switch door, and the harmful gas generated in the drying box can be filtered and purified through the purification box and the exhaust pipe. In this way, an ammonium salt drying treatment device is added. After the ammonium salt generated in the production process is purified and dried, the solvent recovered by the distillation recovery pipe and the rectification recovery pipe is further recycled, which reduces the cost. At the same time, the quality of the by-product meets the market demand and improves the added value of the by-product. The solvent and unreacted alcohol generated in the process can be recycled and used for reaction, which avoids the waste of raw materials and saves production costs, reduces the discharge of waste products, reduces pollution, and protects the environment. BRIEF DESCRIPTION OF THE DRAWINGS
[0016] The accompanying drawings are used to provide a further understanding of the present invention and constitute a part of the specification. They are used to explain the present invention together with the specific embodiments of the present invention and do not constitute a limitation to the present invention.
[0017] Figure 1 This is a front view of a distillation device for producing and processing hafnium esters according to the utility model;
[0018] Figure 2 The utility model is a distillation equipment for the production and processing of hafnium esters. Figure 1 The enlarged view of point A in the middle;
[0019] Figure 3 The utility model is a distillation equipment for the production and processing of hafnium esters. Figure 1 The enlarged view of point B in the middle;
[0020] Figure 4 This is a cross-sectional view of the installation structure of a proportioning feed box and a fixing box of a distillation device for the production and processing of hafnium esters of the utility model;
[0021] Figure 5 This is a cross-sectional view of the installation structure of a drying box of a distillation device for the production and processing of hafnium esters of the utility model;
[0022] Numbers in the figure: 1. Base frame; 2. Reaction vessel 1; 3. Centrifuge; 4. Distillation kettle; 5. Reaction vessel 2; 6. Distillation kettle; 7. Finished product storage tank; 8. Drying box; 9. By-product silo; 10. Agitator; 11. Proportioning feeding box; 12. Feed pipe; 13. Raw material box; 14. Adding pipe; 15. Guide vane; 16. Fixed box; 17. Motor; 18. Worm; 19. Worm wheel; 20. Proportioning partition; 21. Liquid pump; 22. Alcohol supplement box; 23. Distillation recovery pipe; 24. Distillation recovery pipe; 25. Check valve; 26. Solid waste discharge pipe; 27. Solenoid valve; 28. Drive shaft; 29. Flip vane; 30. Electric control switch door; 31. Purification box; 32. Exhaust pipe. DETAILED DESCRIPTION
[0023] The following will be combined with the drawings in the embodiments of the utility model to clearly and completely describe the technical solutions in the embodiments of the utility model. Obviously, the described embodiments are only part of the embodiments of the utility model, not all of the embodiments. Based on the embodiments in the utility model, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the utility model.
[0024] Example 1 Please refer to Figure 1-Figure 5 , the utility model provides a technical solution:
[0025] A distillation device for hafnium ester production and processing, comprising a base frame 1, a reaction container 1 2 and a reaction container 2 5, wherein a reaction container 1 2 is arranged on the upper left of the base frame 1, a centrifuge 3 is sealed at the lower right end of the reaction container 1 2, a distillation kettle 4 is sealed at the lower right end of the centrifuge 3, a reaction container 2 5 is arranged on the right side of the distillation kettle 4, a rectification kettle 6 is arranged on the right side of the reaction container 2 5, a finished product storage tank 7 is sealed at the lower right end of the rectification kettle 6, the distillation kettle 4, the reaction container 2 5 and the rectification kettle 6 are all fixedly connected to the base frame 1, a stirrer 10 is fixedly connected to the inner upper ends of the reaction container 1 2 and the reaction container 2 5, a liquid pump 21 is sealed at the upper right sides of the distillation kettle 4 and the reaction container 2 5, and a liquid discharge pipe at the right end of the liquid discharge pump 21 is connected to the reaction container 2 5 and the reaction container 2 5, respectively. The distillation kettles 6 are sealed and connected, and the upper left side of the reaction vessel 2 5 is sealed and connected with an alcohol supplement tank 22. First, alcohol and solvent are added as raw materials to the reaction vessel 2, and stirring is continued. Metal salt is added dropwise to the reaction vessel 2 according to the molar ratio of hafnium in the metal salt to alcohol, and an acid binding agent is introduced. After the reaction in the reaction vessel 2 is completed, centrifugal filtration is performed through a centrifuge 3, and then distilled through a distillation kettle 4. The obtained product can be used as an intermediate of the crude product. The intermediate continues to enter the reaction vessel 2 5 to participate in the subsequent reaction, and then secondary distillation is performed through the distillation kettle 6 to obtain hafnium ester with higher purity, and the low-boiling point substances in the finished product are purified more perfectly. At the same time, compared with traditional production process technology, the production process has high yield, high purity and low energy consumption.
[0026] Specifically, Figure 1 , Figure 2 and Figure 4 As shown, the left side of the upper end of the reaction container 2 is sealedly connected to a proportioning feeding box 11, the upper end of the proportioning feeding box 11 is sealedly connected to a feeding pipe 12, the upper end of the feeding pipe 12 is sealedly connected to a raw material box 13, the upper end of the raw material box 13 is sealedly connected to an adding pipe 14, the interior of the proportioning feeding box 11 is rotatably connected to a material guide vane 15, the left end of the proportioning feeding box 11 is fixedly connected to a fixed box 16, the upper front end of the fixed box 16 is fixedly connected to a motor 17, the rear end of the output shaft of the motor 17 is fixedly connected to a worm 18, and the lower end of the worm 18 is fixedly connected to the lower end of the worm 18. The end of the worm gear 19 is meshedly connected, the worm gear 19 is fixedly connected to the guide vane 15, and the outer side of the guide vane 15 is fixedly connected to a proportioning partition 20. Under the rotation of the motor 17, the worm 18 can drive the worm gear 19 and the guide vane 15 to rotate, so that the rotation of the guide vane 15 and the proportioning partition 20 can automatically proportion and feed the alcohol, solvent, metal salt and acid binding agent, optimize the raw material proportioning formula, improve the conversion rate of the finished product, simplify the process flow, and thus improve the stability of product quality.
[0027] Example 2 Please refer to Figure 2 and Figure 5The difference between this embodiment and embodiment 1 is that: the lower end of the centrifuge 3 is sealed with a drying box 8, the drying box 8 is fixedly connected to the bottom frame 1, the lower left end of the drying box 8 is sealed with a by-product silo 9, the by-product silo 9 is fixedly connected to the bottom frame 1, the middle position of the upper end of the distillation kettle 4 is sealed with a distillation recovery pipe 23, the distillation recovery pipe 23 is sealed with the reaction vessel 2, the upper right end of the distillation recovery pipe 23 is sealed with a rectification recovery pipe 24, the rectification recovery pipe 24 is sealed with the rectification kettle 6, the distillation recovery pipe 23 is sealed with the rectification recovery pipe 24, and the rectification recovery pipe 24 is sealed with the rectification kettle 6. A check valve 25 is sealed between the distillation recovery pipe 24, a solid waste discharge pipe 26 is sealed to the left side of the lower end of the centrifuge 3, a solenoid valve 27 is sealed to the upper end of the solid waste discharge pipe 26, the solid waste discharge pipe 26 is sealed to the drying box 8, a transmission shaft 28 is fixedly connected to the lower end of the internal shaft of the centrifuge 3, the transmission shaft 28 is rotatably connected to the drying box 8, a flip blade 29 is fixedly connected to the lower end of the transmission shaft 28, an electric control switch door 30 is fixedly connected to the lower left end of the drying box 8, and a purification box is sealed to the right side of the upper end of the drying box 8. 31, the upper end of the purification box 31 is sealed and connected with an exhaust pipe 32, the solid can be centrifugally filtered in the centrifuge 3 by the centrifuge 3, and the filtered solid can be discharged into the drying box 8 through the solid waste discharge pipe 26 by the control of the electromagnetic valve 27, and the transmission shaft 28 can be driven to rotate under the rotation of the centrifuge 3, so that the flip blade 29 can rotate, so that the solid waste can be dried and purified, and the mellow by-product is sent into the by-product silo 9 through the electric control switch door 30, and the harmful gas generated in the drying box 8 can be filtered and purified by the purification box 31 and the exhaust pipe 32. In this way, an ammonium salt drying treatment device is added, and the ammonium salt generated in the production process is purified and dried, and the solvent recovered by the distillation recovery pipe 23 and the rectification recovery pipe 24 is further recycled, which reduces the cost. At the same time, the quality of the by-product meets the market demand and improves the added value of the by-product. The solvent and unreacted alcohol generated in the process can be recycled and used for reaction, which not only avoids the waste of raw materials, saves production costs, but also reduces the discharge of waste products, reduces pollution, and protects the environment.
[0028] Working principle of the utility model: when the device is used, alcohol and solvent are first added as raw materials into the reaction container 2, and stirred continuously. Metal salt is added dropwise into the reaction container 2 according to the molar ratio of hafnium in the metal salt to alcohol, and an acid binding agent is introduced. After the reaction in the reaction container 2 is completed, centrifugal filtration is performed in the centrifuge 3, and then distillation is performed in the distillation kettle 4. The obtained product can be used as an intermediate of the crude product. The intermediate continues to enter the reaction container 5 to participate in the subsequent reaction, and then secondary distillation is performed in the rectification kettle 6, so as to obtain a product with higher purity. The high hafnium ester can purify the low-boiling point substances in the finished product more perfectly, and the worm 18 can drive the worm wheel 19 and the guide vane 15 to rotate under the rotation of the motor 17, so that the alcohol, solvent, metal salt and acid binding agent can be automatically proportioned and loaded under the rotation of the guide vane 15 and the proportioning partition 20, the raw material proportioning formula is optimized, the conversion rate of the finished product is improved, and the process flow is simplified, thereby improving the stability of product quality. At the same time, compared with the traditional production process technology, the production process has a higher yield. The invention discloses a method for preparing the present invention, wherein the present invention has the advantages of high purity, high purity, low energy consumption, and can centrifuge and filter the solid in the centrifuge 3 through the centrifuge 3, and can discharge the filtered solid into the drying box 8 through the solid waste discharge pipe 26 through the control of the electromagnetic valve 27, and can drive the transmission shaft 28 to rotate under the rotation of the centrifuge 3, so that the flip blade 29 can rotate, so that the solid waste can be dried and purified, and the by-product with a mellow body can be sent into the by-product silo 9 through the electric control switch door 30, and the harmful gas generated in the drying box 8 can be filtered and purified through the purification box 31 and the exhaust pipe 32. In this way, an ammonium salt drying treatment device is added, and the ammonium salt generated in the production process is purified and dried, and the solvent recovered by the distillation recovery pipe 23 and the rectification recovery pipe 24 is further recycled, which reduces the cost. At the same time, the quality of the by-product meets the market demand and improves the added value of the by-product. The solvent and unreacted alcohol generated in the process can be recycled and used for reaction, which not only avoids the waste of raw materials, saves production costs, but also reduces the discharge of waste products, reduces pollution, and protects the environment.
[0029] Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and variations may be made to the embodiments without departing from the principles and spirit of the present invention, and that the scope of the present invention is defined by the appended claims and their equivalents.
Claims
1. A distillation device for the production and processing of hafnium esters, comprising a base frame (1), a reaction vessel 1 (2) and a reaction vessel 2 (5), characterized in that: A reaction container 1 (2) is provided at the upper left of the base frame (1); a centrifuge (3) is sealed at the lower right end of the reaction container 1 (2); a distillation kettle (4) is sealed at the lower right end of the centrifuge (3); a reaction container 2 (5) is provided on the right side of the distillation kettle (4); a rectification kettle (6) is provided on the right side of the reaction container 2 (5); a finished product storage tank (7) is sealed at the lower right end of the rectification kettle (6); the distillation kettle (4), the reaction container 2 (5) and the rectification kettle (6) are all fixedly connected to the base frame (1); a drying box (8) is sealed at the lower end of the centrifuge (3); the drying box (8) is fixedly connected to the base frame (1); a by-product silo (9) is sealed at the lower left end of the drying box (8); and the by-product silo (9) is fixedly connected to the base frame (1).
2. The distillation equipment for the production and processing of hafnium ester according to claim 1, characterized in that: The upper ends of the reaction container 1 (2) and the reaction container 2 (5) are both fixedly connected with a stirrer (10).
3. The distillation equipment for the production and processing of hafnium ester according to claim 1, characterized in that: The left side of the upper end of the reaction container 1 (2) is sealedly connected to a proportioning feeding box (11), the upper end of the proportioning feeding box (11) is sealedly connected to a feeding pipe (12), the upper end of the feeding pipe (12) is sealedly connected to a raw material box (13), and the upper end of the raw material box (13) is sealedly connected to an addition pipe (14).
4. The distillation equipment for the production and processing of hafnium ester according to claim 3, characterized in that: The proportioning loading box (11) is rotatably connected to a material guide vane (15) inside, the left end of the proportioning loading box (11) is fixedly connected to a fixed box (16), the upper front end of the fixed box (16) is fixedly connected to a motor (17), the rear end of the output shaft of the motor (17) is fixedly connected to a worm (18), the lower end of the worm (18) is meshingly connected to a worm wheel (19), the worm wheel (19) is fixedly connected to the material guide vane (15), and the outer side of the material guide vane (15) is fixedly connected to a proportioning partition (20).
5. The distillation equipment for the production and processing of hafnium ester according to claim 1, characterized in that: The distillation kettle (4) and the upper right side of the reaction vessel (5) are both sealedly connected to a liquid pump (21), the right end of the liquid discharge pipe of the liquid pump (21) is sealedly connected to the reaction vessel (5) and the distillation kettle (6) respectively, and the upper left side of the reaction vessel (5) is sealedly connected to an alcohol supplement tank (22).
6. The distillation equipment for the production and processing of hafnium ester according to claim 1, characterized in that: A distillation recovery pipe (23) is sealedly connected to the middle position of the upper end of the distillation kettle (4), the distillation recovery pipe (23) is sealedly connected to the reaction vessel 1 (2), the upper right end of the distillation recovery pipe (23) is sealedly connected to a rectification recovery pipe (24), the rectification recovery pipe (24) is sealedly connected to the rectification kettle (6), and a check valve (25) is sealedly connected between the distillation recovery pipe (23) and the rectification recovery pipe (24).
7. The distillation equipment for the production and processing of hafnium ester according to claim 1, characterized in that: The left side of the lower end of the centrifuge (3) is sealedly connected to a solid waste discharge pipe (26), the upper end of the solid waste discharge pipe (26) is sealedly connected to a solenoid valve (27), the solid waste discharge pipe (26) is sealedly connected to the drying box (8), the lower end of the internal shaft of the centrifuge (3) is fixedly connected to a transmission shaft (28), the transmission shaft (28) is rotatably connected to the drying box (8), the lower end of the transmission shaft (28) is fixedly connected to a flip blade (29), and the lower left end of the drying box (8) is fixedly connected to an electric control switch door (30).
8. The distillation equipment for the production and processing of hafnium ester according to claim 1, characterized in that: The upper right side of the drying box (8) is sealedly connected to a purification box (31), and the upper end of the purification box (31) is sealedly connected to an exhaust pipe (32).