System for producing silicon hydrogen compound based on coated metal hydride
Through the clad metal hydride system, the metal hydride is coated with soluble or fusible plastic materials, which solves the problem of safe feeding and storage of metal hydrides when preparing hydrogen silicon compounds, achieves a high safety and high efficiency feeding process, and improves product quality.
Patent Information
- Application Number
- CN202520152990.4
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2025-01-23
- Publication Date
- 2025-03-25
- Estimated Expiration
- 2035-01-23
AI Technical Summary
In the prior art, metal hydrides are flammable and explosive when preparing hydrogen silicon compounds as reducing agents, and are highly sensitive to moisture, making their safe feeding and storage a challenge in industrial production.
The metal hydride system is used to tablet the metal hydride and coat it with soluble or fusible plastic materials, and transport it to the reactor through the conveying pipe to ensure improved safety and efficiency during the feeding process.
The high safety and high reliability feeding of metal hydrides are achieved, which extends the shelf life and completely separates the clad materials after reaction to avoid the impact on product quality and improves production safety and product quality.
Smart Images
Figure CN222658685U_ABST
Abstract
Description
Technical Field
[0001] The utility model belongs to the technical field of silicon-containing compounds, and in particular relates to a system for producing silicon hydride compounds based on coated metal hydrides. Background Art
[0002] Silicon hydrides, that is, organic silicon compounds containing Si-H groups in the molecule, are an important class of functional monomers with a wide range of uses. Many carbon-functional organic silicon compounds can be synthesized by the silane addition reaction of Si-H groups with unsaturated groups such as vinyl and allyl groups; the Si-H groups in silicon hydrides have strong reducing properties and can be used as reducing agents in organic synthesis; silicon hydrides can also be used as crosslinking agents for the vulcanization of addition-type silicone rubber and the curing of silicone resins. The most common method for preparing Si-H-containing compounds is to use metal hydrides such as lithium hydride, lithium aluminum hydride, sodium hydride, sodium aluminum hydride and calcium hydride as reducing agents to reduce chlorosilanes and alkoxysilanes to prepare Si-H-containing compounds. This method can prepare a wide variety of silicon hydride compounds with high yields.
[0003] Pure metal hydrides are white crystals that react violently with water and release hydrogen. In non-aqueous solvents, metal hydrides can combine with some electron-deficient compounds to form complex hydrides; both metal hydrides and complex hydrides have strong reducing properties and can reduce metal chlorides, oxides and oxygen-containing acid salts at high temperatures. However, these metal hydrides, especially lithium aluminum hydride and sodium aluminum hydride, are highly sensitive to moisture, flammable and explosive, and their safe feeding in solid state, especially in powder state, is a major challenge for large-scale industrial production. For example, in the preparation of high-performance liquid silicon carbide polymer ceramic precursors such as perhydropolycarbosilane, vinylhydropolycarbosilane, and allylhydropolycarbosilane by the Grignard coupling-reduction method, lithium aluminum hydride or sodium aluminum hydride is a key reducing agent raw material that affects product performance and batch quality consistency, and its safe feeding is one of the key processes in industrial production. Utility Model Content
[0004] In view of the above deficiencies in the prior art, the technical problem to be solved by the utility model is: to provide a system for producing silicon hydride compounds based on coated metal hydrides, to achieve separate protection of metal hydrides, and to ensure high safety and high reliability of the metal hydride reducing agent feeding operation when preparing silicon hydride compounds.
[0005] The technical solution adopted by the utility model to solve its technical problems is:
[0006] The utility model discloses a system for producing silicon hydride based on coated metal hydride, comprising a coated metal hydride storage tank, wherein the coated metal hydride storage tank is connected to a reactor through a transmission pipeline, a pickling tank is connected to the bottom of the reactor, a product tank and a recovery tank are connected to the bottom of the pickling tank, a distillation tower is connected to the product tank, a jacket is arranged on the outside of the reactor, a stirrer 1 and a stirrer 2 are arranged inside the reactor and the pickling tank respectively, a plurality of screens are arranged inside the pickling tank, a stock solution inlet and a solvent inlet are arranged on the top of the reactor, and an acid solution inlet and a precipitant inlet are arranged on the top of the pickling tank.
[0007] in:
[0008] The top of the agitator 1 passes through the reaction kettle and is connected to a motor, and the top of the agitator 2 passes through the pickling tank and is connected to a motor.
[0009] Conveying rollers are arranged at intervals in the conveying pipe, and the conveying rollers are connected by conveying belts. Buffer platforms are arranged on the inner walls of the conveying pipe near both ends of the conveying belts.
[0010] The lower part of the jacket is provided with a circulating water inlet, and the upper part of the jacket is provided with a circulating water outlet.
[0011] The screen is fixed on the inner wall of the pickling tank by bolts, and a through hole is arranged at the center of the screen to cooperate with the second stirrer.
[0012] The bottom of the reactor is provided with a mixed liquid outlet, the top of the pickling tank is provided with a mixed liquid inlet, and the mixed liquid outlet and the mixed liquid inlet are connected through a pipeline.
[0013] A discharge port is arranged at the bottom of the pickling tank, and the discharge port is respectively connected to a product inlet on the product tank and a recovery liquid inlet on the recovery tank through pipelines.
[0014] The bottom of the product tank is provided with a product outlet, and the product outlet is connected to the middle part of the distillation tower.
[0015] A distillation outlet is arranged at the bottom of the distillation tower.
[0016] The bottom of the recovery tank is provided with a coating material outlet.
[0017] The utility model greatly improves the feeding safety and efficiency by pressing the metal hydride into tablets and adding a layer of soluble or fusible plastic inner packaging bag to the metal hydride reducing agent, removing the conventional airtight and water-blocking plastic packaging before feeding, and then feeding the reducing agent with the inner packaging as a whole bag.
[0018] The coated metal hydride refers to a metal hydride that uses a coating material that does not affect the subsequent reduction reaction and separation post-processing as the inner packaging, and its outer layer also has one or two layers of currently conventional airtight water-blocking plastic packaging. The coated metal hydride can ensure its long-term storage and safe transportation. Taking the production of liquid polycarbosilane as an example, the reaction system uses tetrahydrofuran as a solvent, the reduction reaction temperature is 50~65℃, and the post-processing separation process uses dilute hydrochloric acid and hexane or dilute hydrochloric acid and petroleum ether for acidification, extraction and washing. Therefore, the coating material uses a coating material that is soluble in tetrahydrofuran, or a plastic coating material that melts at a reaction temperature of 50~65℃ and is insoluble in hexane or petroleum ether, so that the coating material can be removed by filtration or extraction washing during the separation process, which will not affect the efficiency of the post-processing process and will not leave any residue in the liquid polycarbosilane product. The coating material includes but is not limited to ethylene-vinyl acetate copolymer EVA with a melting point of 50~85℃, thermoplastic polyurethane elastic material TPU and some polyester materials. If it is other metal hydride reaction solvent system, such as butyl ether, the melting point of the EVA material can be increased accordingly.
[0019] The beneficial effects of the utility model are:
[0020] The system for producing silicon hydride compounds from coated metal hydrides proposed in the utility model can further improve the safety and efficiency of overall feeding, thoroughly solve the problem of safe, efficient and reliable feeding of flammable and explosive solid metal hydride reducing agents, and improve the degree of automation.
[0021] The utility model can improve the storage period and transportation safety of the metal hydride by coating the metal hydride, and ensure the stability of the metal hydride during the feeding process. After the coated metal hydride enters the reaction system, the coating material on the outer layer of the metal hydride releases the metal hydride, and the metal hydride can react quickly with the reactant to ensure the stability of the added amount of the metal hydride. After the reaction is completed, the coating material can be completely separated to avoid the influence of the residual coating material on the product quality. In addition, the coating material has stable properties and will not be denatured during the reaction. After the reaction is completed, the coating material can be separated and post-processed to achieve reuse, thereby improving the production safety and product quality, and has good application prospects. BRIEF DESCRIPTION OF THE DRAWINGS
[0022] Figure 1 It is a schematic diagram of the structure of the utility model;
[0023] Figure 2 It is a schematic diagram of the screen of the utility model;
[0024] Figure 3 The utility model is a schematic diagram of the structure of a conveying roller, a conveying belt and a buffer table.
[0025] In the figure: 1. Coated metal hydride storage tank; 2. Transmission pipeline; 3. Reactor; 4. Pickling tank; 5. Product tank; 6. Recovery tank; 7. Raw liquid inlet; 8. Solvent inlet; 9. Jacket; 10. Mixed liquid outlet; 11. Mixed liquid inlet; 12. Acid liquid inlet; 13. Precipitant inlet; 14. Discharge port; 15. Product inlet; 16. Product outlet; 17. Recovery liquid inlet; 18. Distillation tower; 19. Coating material outlet;
[0026] 201, conveying roller; 202, conveyor belt; 203, buffer table; 301, agitator 1; 401, screen; 402, agitator 2; 901, circulating water inlet; 902, circulating water outlet; 1801, distillation outlet. DETAILED DESCRIPTION
[0027] The embodiments of the present utility model are further described below in conjunction with the accompanying drawings.
[0028] Example 1
[0029] like Figure 1-3 As shown, the system for producing silicon hydride based on coated metal hydride described in the utility model includes a coated metal hydride storage tank 1, the coated metal hydride storage tank 1 is connected to a reactor 3 through a transmission pipeline 2, the bottom of the reactor 3 is connected to a pickling tank 4, the bottom of the pickling tank 4 is connected to a product tank 5 and a recovery tank 6, the product tank 5 is connected to a distillation tower 18, a jacket 9 is provided on the outside of the reactor 3, a stirrer 1 301 and a stirrer 2 402 are respectively provided inside the reactor 3 and the pickling tank 4, a plurality of screens 401 are provided inside the pickling tank 4, a raw liquid inlet 7 and a solvent inlet 8 are provided on the top of the reactor 3, and an acid liquid inlet 12 and a precipitant inlet 13 are provided on the top of the pickling tank 4.
[0030] A plurality of metal hydrides coated with EVA are stored in the coated metal hydride storage tank 1, which are directly transported to the reactor 3 through the transmission pipeline 2 during the reaction. After the reaction is completed, the mixed liquid is uniformly transported to the pickling tank 4 for washing. A plurality of screens 401 are arranged in the pickling tank 4 to fully mix the acid solution and the organic product, increase the contact area between the acid solution and the organic product, and improve the efficiency of pickling. The precipitant can separate the EVA from the organic product. The reprocessing of EVA can realize the recycling of EVA and reduce waste, and the purity and yield of the silicon hydride compound can be improved after the organic product is distilled.
[0031] The top of the stirrer 1 301 passes through the reaction kettle 3 and is connected to a motor, and the top of the stirrer 2 402 passes through the pickling tank 4 and is connected to a motor.
[0032] Conveyor rollers 201 are arranged at intervals in the conveyor pipe 2, and the conveyor rollers 201 are connected by a conveyor belt 202. Buffer tables 203 are arranged on the inner wall of the conveyor pipe 2 near both ends of the conveyor belt 202. The conveyor belt 202 can slowly and orderly transport the coated metal hydride to the reactor 3, and the buffer tables 203 at both ends of the conveyor belt 202 can buffer the coated metal hydride.
[0033] A circulating water inlet 901 is provided at the lower portion of the jacket 9 , and a circulating water outlet 902 is provided at the upper portion of the jacket 9 .
[0034] The screen 401 is fixed on the inner wall of the pickling tank 4 by bolts, and a through hole is provided at the center of the screen 401 to cooperate with the stirrer 2 402. When the stirrer 2 402 stirs, the mixed liquid continuously impacts the screen 401, and the screen 401 breaks the mixed liquid so that the acid can fully wash the organic product.
[0035] A mixed liquid outlet 10 is provided at the bottom of the reactor 3, and a mixed liquid inlet 11 is provided at the top of the pickling tank 4. The mixed liquid outlet 10 and the mixed liquid inlet 11 are connected through a pipeline.
[0036] A discharge port 14 is provided at the bottom of the pickling tank 4 , and the discharge port 14 is respectively connected to a product inlet 15 on the product tank 5 and a recovery liquid inlet 17 on the recovery tank 6 through pipelines.
[0037] A product outlet 16 is provided at the bottom of the product tank 5 , and the product outlet 16 is connected to the middle of the distillation tower 18 .
[0038] A distillation outlet 1801 is provided at the bottom of the distillation tower 18 .
[0039] A coating material outlet 19 is provided at the bottom of the recovery tank 6 .
[0040] Working principle and process:
[0041] The coated metal hydride storage tank 1 stores a number of EVA coated metal hydrides. When performing a reduction reaction, the silane compound is first added into the reactor 3 through the stock solution inlet 7, and then tetrahydrofuran is added through the solvent inlet 8. Hot water above 60° C. is introduced into the jacket 9 to ensure that the reaction in the reactor 3 can be fully carried out. EVA is dissolved in the tetrahydrofuran solution, and the coated metal hydride is released and reacts with the reactant. After the reaction is completed, the mixed solution is transported to the pickling tank 4, and acid is added through the acid solution inlet 12 to wash the organic product in the mixed solution. Petroleum ether is added as a precipitant to leave the EVA coated material in the aqueous phase, thereby separating it from the organic product. Subsequently, the organic product and the aqueous phase are transported to the product tank 5 and the recovery tank 6 respectively. The organic product in the product tank 5 is rectified by the distillation tower 18 to obtain a relatively pure silicon hydride compound, and the aqueous phase in the recovery tank 6 is treated to precipitate EVA. The EVA can be used again for coating the metal hydride after cleaning and reprocessing.
Claims
1. A system for producing silicon hydride based on coated metal hydride, comprising a coated metal hydride storage tank (1), characterized in that: The coated metal hydride storage tank (1) is connected to a reactor (3) via a transmission pipeline (2); the bottom of the reactor (3) is connected to a pickling tank (4); the bottom of the pickling tank (4) is connected to a product tank (5) and a recovery tank (6); the product tank (5) is connected to a distillation tower (18); a jacket (9) is arranged outside the reactor (3); a stirrer 1 (301) and a stirrer 2 (402) are arranged inside the reactor (3) and the pickling tank (4), respectively; a plurality of screens (401) are arranged inside the pickling tank (4); a stock solution inlet (7) and a solvent inlet (8) are arranged at the top of the reactor (3); and an acid solution inlet (12) and a precipitant inlet (13) are arranged at the top of the pickling tank (4).
2. The system for producing silicon hydride based on coated metal hydride according to claim 1, characterized in that: The top of the stirrer 1 (301) passes through the reaction kettle (3) and is connected to a motor, and the top of the stirrer 2 (402) passes through the pickling tank (4) and is connected to a motor.
3. The system for producing silicon hydride based on coated metal hydride according to claim 1, characterized in that: Conveying rollers (201) are arranged at intervals in the conveying pipe (2); the conveying rollers (201) are connected by conveying belts (202); and buffer platforms (203) are arranged on the inner walls of the conveying pipe (2) near both ends of the conveying belts (202).
4. The system for producing silicon hydride based on coated metal hydride according to claim 1, characterized in that: A circulating water inlet (901) is provided at the lower part of the jacket (9), and a circulating water outlet (902) is provided at the upper part of the jacket (9).
5. The system for producing silicon hydride based on coated metal hydride according to claim 1, characterized in that: The screen (401) is fixed on the inner wall of the pickling tank (4) by means of bolts, and a through hole is provided at the center of the screen (401) in coordination with the second agitator (402).
6. The system for producing silicon hydride based on coated metal hydride according to claim 1, characterized in that: A mixed liquid outlet (10) is provided at the bottom of the reaction kettle (3), and a mixed liquid inlet (11) is provided at the top of the pickling tank (4). The mixed liquid outlet (10) and the mixed liquid inlet (11) are connected via a pipeline.
7. The system for producing silicon hydride based on coated metal hydride according to claim 1, characterized in that: A discharge port (14) is provided at the bottom of the pickling tank (4), and the discharge port (14) is respectively connected to a product inlet (15) on the product tank (5) and a recovery liquid inlet (17) on the recovery tank (6) through pipelines.
8. The system for producing silicon hydride based on coated metal hydride according to claim 1, characterized in that: A product outlet (16) is provided at the bottom of the product tank (5), and the product outlet (16) is connected to the middle of the distillation tower (18).
9. The system for producing silicon hydride based on coated metal hydride according to claim 1, characterized in that: A distillation outlet (1801) is provided at the bottom of the distillation tower (18).
10. The system for producing silicon hydride based on coated metal hydride according to claim 1, characterized in that: A coating material outlet (19) is provided at the bottom of the recovery tank (6).