Production equipment of hafnate
By designing a pyrite production equipment including reaction container, centrifugal equipment, and distillation equipment, the problem of low income, high side reactions, equipment corrosion and environmental pollution in existing processes, realizing high yield, high purity and high purity and high purity and purity and high purity and purity and environmental pollution. Production of low energy consumption.
Patent Information
- Application Number
- CN202420928961.8
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2024-04-30
- Publication Date
- 2025-01-28
- Estimated Expiration
- 2034-04-30
AI Technical Summary
The existing hafnium acid ester production process has low yields. Hydrogen chloride is generated during the reaction, which leads to side reactions, reducing yields, and the equipment is prone to corrosion, with large loss of raw materials, and the batch kettle production process is low efficiency, with more three wastes generated, causing environmental pollution. .
Designed a kind of sorchlate production equipment, including reaction container, centrifugal equipment, distillation equipment, finished storage tanks and ammonium salt purifying dry equipment. Reduce by -products and reduce energy consumption.
It improves the yield and purity of amphodium ester, reduces raw materials consumption and equipment corrosion, reduces the generation of three wastes, improves production efficiency and product quality stability, and protects the environment.
Smart Images
Figure CN222401419U_ABST
Abstract
Description
Technical Field
[0001] The utility model relates to the technical field of fine chemical industry, and relates to a preparation technology and equipment of hafnium ester, in particular to a production equipment of hafnium ester. Background Art
[0002] Hafnium esters are ultra-high temperature ceramic precursors and are key raw materials for the preparation of ultra-high temperature ceramic-based composite materials. After years of development, its preparation process has become increasingly mature, and its comprehensive performance has shown obvious advantages. It has been applied in the aerospace field. However, the current production of hafnium esters still has the following problems:
[0003] Question 1:
[0004] The production process of hafnium esters in industry is mainly based on the direct esterification method of alcohol and metal hafnium salt, 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 esters. 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 absorbed hydrochloric acid often corrode the equipment, and the hydrogen chloride removed from the system by vacuum also carries some raw materials, which increases the loss of alcohol and metal hafnium salt, and greatly increases the consumption of raw materials. Question 2:
[0005] There are many types of hafnium esters, and the production processes and equipment used for various hafnium esters are also different. The existing production processes and equipment for hafnium esters all adopt intermittent kettle production technology, and 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 a large amount of three wastes are generated during the production process, which has a great harm to the environment.
[0006] Based on the above description, there is an urgent need for a hafnium ester production equipment that can optimize the production of hafnium ester, thereby improving the adaptability of the equipment, reducing equipment modification costs, improving production efficiency, and ensuring stable product quality. Utility Model Content
[0007] The utility model aims to provide a hafnium ester production device to solve the problems of poor product quality and low yield of existing hafnium ester production devices, as well as the problems of three wastes generated in the production process, causing environmental pollution and high energy consumption.
[0008] The technical solution adopted by the utility model to solve its technical problems is:
[0009] A production equipment of hafnium ester comprises a reaction container 1, a centrifugal device 2, a distillation device 3, a reaction container 2, a distillation device 2, a finished product storage tank 6, a drying device 7 for purifying ammonium salt, and a by-product silo 8 for by-products; wherein: the discharge port of the reaction container 1 is connected to the centrifugal device 2, and the centrifugal device 2 performs centrifugal filtration; the discharge port of the centrifugal device 2 is connected to the drying device 7, and the drying device 7 performs ammonium salt purification; the discharge port of the drying device 7 is connected to the dry by-product silo 8, and the by-product silo 8 stores by-products; the mother liquor discharge port of the centrifugal device 2 is connected to the distillation device 3, and the distillation device 3 performs distillation and purification; the discharge port of the distillation device 3 is connected to the reaction container 2, and the reaction container 2 further reacts; the discharge port of the reaction container 24 is connected to the distillation device 25, and the distillation device 25 further purifies; the discharge port of the distillation device 25 is connected to the finished product storage tank 6, and the finished product storage tank 6 is used to store hafnium ester.
[0010] The utility model also has the following additional technical features:
[0011] As a further specific optimization of the technical solution of the utility model: the recovery outlet of the distillation device 3 is connected to the reaction container 1, and the recovered alcohol D is recovered and added into the reaction container 1.
[0012] As a further specific optimization of the technical solution of the utility model: the recovery outlet of the distillation equipment 2 5 is connected to the reaction container 1, and the recovered solvent and the recovered alcohol E are recovered and added to the reaction container 1.
[0013] As a further specific optimization of the technical solution of the utility model: the reaction container 1 is also connected to a pipeline for adding metal salt A and a pipeline for adding ammonia B.
[0014] As a further specific optimization of the technical solution of the utility model: the reaction container 2 4 is also connected to a pipeline for adding alcohol C.
[0015] The utility model optimizes the process ratio, improves the product conversion rate, and reduces the cost. Specifically, the technical solution provided by the utility model brings the following beneficial effects:
[0016] Beneficial effects 1. The hafnium ester production equipment of the utility model is a flexible equipment. After the reaction in the reaction container 1 is completed, it is centrifugally filtered through a centrifugal device and then distilled through a distillation device. The obtained product can be used as an intermediate of a crude product. The intermediate continues to enter the reaction container 2 to participate in the subsequent reaction, and then a two-step distillation is performed to obtain a hafnium ester with higher purity, and the low-boiling point substances in the finished product are purified more perfectly.
[0017] Beneficial effect 2. Compared with traditional hafnium ester production process equipment, the hafnium ester production process method of the utility model optimizes the raw material ratio formula, improves the conversion rate of the finished product, and simplifies the process flow, thereby improving the stability of product quality. At the same time, compared with traditional production process technology, the production process flow has high yield, high purity and low energy consumption.
[0018] Beneficial effect 3. The hafnium ester production process equipment of the utility model adds an ammonium salt drying treatment device. The ammonium salt produced in the production process is purified and dried, and the recovered solvent is further recycled, which reduces the cost; at the same time, the quality of the by-products meets the market demand and increases the added value of the by-products; the solvent and unreacted alcohol produced in the process can be recycled and used in the reaction, which not only avoids the waste of raw materials and saves production costs, but also reduces the discharge of waste products, reduces pollution and protects the environment. BRIEF DESCRIPTION OF THE DRAWINGS
[0019] Figure 1 This is a schematic diagram of the structure of the hafnium ester production process equipment of the utility model;
[0020] Figure 2 The utility model is a schematic diagram of the production process flow of hafnium ester.
[0021] Explanation of the accompanying drawings: 1. Reaction vessel one; 2. Centrifugal equipment; 3. Distillation equipment; 4. Reaction vessel two; 5. Distillation equipment two; 6. Finished product storage tank; 7. Drying equipment; 8. By-product silo; A. Metal salt; B. Ammonia; C. Alcohol; D. Recovered alcohol; E. Recovered solvent and recovered alcohol. DETAILED DESCRIPTION
[0022] Exemplary embodiments of the present invention will be described in more detail below with reference to the accompanying drawings.
[0023] Example 1
[0024] A production equipment for hafnium ester includes a reaction container 1, a centrifugal device 2, a distillation device 3, a reaction container 4, a distillation device 5, a finished product storage tank 6, a drying device for ammonium salt purification 7, and a by-product silo 8.
[0025] The discharge port of the reaction vessel 1 is connected to the centrifugal device 2, which performs centrifugal filtration; the discharge port of the centrifugal device 2 is connected to the drying device 7, which performs ammonium salt purification; the discharge port of the drying device 7 is connected to the dry by-product silo 8, which performs by-product storage.
[0026] The mother liquor discharge port of the centrifugal device 2 is connected to the distillation device 3, and the distillation device 3 performs distillation and purification; the discharge port of the distillation device 3 is connected to the reaction container 2 4, and the reaction container 2 4 further reacts; the discharge port of the reaction container 2 4 is connected to the distillation device 2 5, and the distillation device 2 5 further purifies; the discharge port of the distillation device 2 5 is connected to the finished product storage tank 6, and the finished product storage tank 6 is used to store hafnium ester.
[0027] The recovery outlet of the distillation device 3 is connected to the reaction container 1, and the recovered alcohol D is recovered and added into the reaction container 1.
[0028] The recovery outlet of the distillation device 2 5 is connected to the reaction container 1 , and the recovered solvent and the recovered alcohol E are recovered and added into the reaction container 1 .
[0029] The reaction vessel 1 is also connected with a pipeline for adding metal salt A and a pipeline for adding ammonia B. Ammonia is a raw material in the production process, and its function is to neutralize the hydrogen chloride produced by the esterification reaction of hafnium chloride and alcohol, so as to push the reaction equilibrium to move toward the product direction.
[0030] The reaction vessel 2 4 is also connected to a pipeline for adding alcohol C.
[0031] In response to question 1, the utility model is a significant improvement on the direct esterification method. By adding an acid binding agent during the esterification process, the generated hydrogen chloride is neutralized, the reaction activity is increased, the reaction process is promoted, and the reaction time is shortened.
[0032] In response to question 2, the utility model is a production method that uses a solvent as a reaction environment, and then synthesizes hafnium ester by reacting alcohol with metal hafnium salt, and completes esterification and distillation purification through experiments. The production method adopted should have a fast rate and high yield, and have certain practical value.
[0033] Example 2
[0034] A production process of hafnium ester comprises the following steps:
[0035] Step 1, add alcohol C and solvent in a mass ratio of 1:5±3.5 as raw materials into distillation equipment 25, and continue stirring;
[0036] The added alcohol C is one or more of n-propanol, isopropanol, n-butanol, and isobutanol;
[0037] The added solvent is one or more of benzene, xylene, n-heptane and petroleum ether;
[0038] Step 2, adding metal salt A dropwise to reaction vessel 1 according to the molar ratio of hafnium in the metal salt to alcohol C being 1:3±1.5, and introducing an acid binding agent, wherein the chemical molar ratio of the acid binding agent to hafnium in the metal salt A is 3±0.5:1;
[0039] The metal salt added dropwise is one or more of hafnium tetrachloride and hafnium trichloride;
[0040] The acid binding agent introduced is one or more of pyridine, triethylamine and liquid ammonia;
[0041] Step 3, centrifuge through centrifugal device 2, then distill through distillation device 3, add the obtained liquid as intermediate raw material and alcohol C into reaction container 2 4, stir and heat;
[0042] The reaction vessel 2 4 into which the intermediate raw materials are added is a distillation kettle;
[0043] The added alcohol C is one or more of n-propanol, isopropanol, n-butanol, and isobutanol;
[0044] Step 4, after the reaction of the intermediate raw material and alcohol C in the reaction container 2 4 is completed, the final finished product hafnium ester is obtained by distillation in the distillation equipment 2 5, and the hafnium ester is temporarily stored in the finished product storage tank 6.
[0045] Step 5, the recovered solvent and recovered alcohol E obtained by distillation through the distillation device 3 in step 3 are added to the reaction container 1 of step 2; the recovered alcohol D obtained by distillation through the distillation device 5 in step 4 is added to the reaction container 1 of step 2;
[0046] Step 6, after the reaction in the reaction vessel 1 is completed, the discharge port is connected to the centrifugal device 2 for centrifugal filtration, and the solid after centrifugation enters the drying device 7, and after purification, enters the by-product silo 8;
[0047] The production process method and equipment of the utility model can realize flexible production, are suitable for the production of hafnium ester, and have high yield, high purity and low energy consumption.
[0048] Example 3
[0049] Synthesis of n-propyl hafnium ester:
[0050] Hafnium tetrachloride, n-propanol and a solvent are added into a reaction container one, wherein the molar ratio of hafnium tetrachloride to n-propanol is 1:3, petroleum ether or xylene is used as the solvent, stirring is started, and the temperature is raised to 90±5°C; ammonia is introduced into the reaction container one, and the molar ratio of ammonia to hafnium tetrachloride is 3.5:1, and the reaction is continued until it ends; after the reaction, centrifugal filtration and distillation are performed to obtain n-propyl hafnium ester, n-propanol is added into the reaction container two, and the final product is obtained by distillation, wherein the yield is above 96.0%, and the metal content Hfwt% is 32.26±0.1%.
[0051] The above detailed description of the embodiments of the present invention provided in the accompanying drawings is not intended to limit the scope of the claimed invention but merely represents selected embodiments of the present invention.
Claims
1. A production equipment for hafnium ester, characterized in that: It comprises a reaction container (1), a centrifugal device (2), a distillation device (3), a reaction container (4), a distillation device (5), a finished product storage tank (6), a drying device for ammonium salt purification (7), and a by-product silo (8); wherein: The discharge port of the reaction container 1 (1) is connected to a centrifugal device (2), and the centrifugal device (2) performs centrifugal filtration; the discharge port of the centrifugal device (2) is connected to a drying device (7), and the drying device (7) performs ammonium salt purification; the discharge port of the drying device (7) is connected to a dry by-product silo (8), and the by-product silo (8) performs by-product storage; The mother liquor discharge port of the centrifugal device (2) is connected to the distillation device (3), and the distillation device (3) performs distillation and purification; the discharge port of the distillation device (3) is connected to the reaction container (4), and the reaction container (4) further reacts; the discharge port of the reaction container (4) is connected to the distillation device (5), and the distillation device (5) further purifies; the discharge port of the distillation device (5) is connected to the finished product storage tank (6), and the finished product storage tank (6) is used to store hafnium ester.
2. The production equipment of hafnium ester according to claim 1, characterized in that: The recovery outlet of the distillation device (3) is connected to the reaction container (1), and the recovered alcohol D is recovered and added to the reaction container (1).
3. The production equipment of hafnium ester according to claim 1, characterized in that: The recovery outlet of the distillation device 2 (5) is connected to the reaction container 1 (1), and the recovery solvent and the recovery alcohol E are recovered and added into the reaction container 1 (1).
4. The production equipment of hafnium ester according to claim 1, characterized in that: The reaction container 1 (1) is also connected to a pipeline for adding metal salt A and a pipeline for adding ammonia gas B.
5. The production equipment of hafnium ester according to claim 1, characterized in that: The reaction container 2 (4) is also connected to a pipeline for adding alcohol C.