System for synthesizing catalyst for silicon powder one-step method through composite route and method for preparing silicate ester from silicon powder through one-step method
The integrated catalyst synthesis system addresses inefficiencies and safety issues by using multiple storage tanks and advanced separation processes to stabilize catalysts and regulate activity, achieving high-efficiency, cost-effective, and safe production of multiple silicates.
Patent Information
- Application Number
- CN202411361184.4
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-09-27
- Publication Date
- 2024-12-27
AI Technical Summary
Existing silicon powder one-step catalyst synthesis systems are inefficient, prone to catalyst degradation during long-distance transportation, have unstable costs due to fluctuating raw material prices, and lack the ability to regulate catalyst activity and production efficiency, leading to safety risks and limited product versatility.
A composite catalyst synthesis system integrating multiple raw material storage tanks, negative pressure processes, and azeotropic solvent separation, with mass flow meters and sensors for precise control, allowing for simultaneous preparation of multiple catalysts and regulation of catalyst activity.
The system enhances production efficiency, stabilizes catalyst costs, prevents degradation, and ensures safe operation by regulating catalyst activity and solvent removal, enabling versatile production of various silicates with improved reactant utilization.
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Figure CN119186460A_ABST
Abstract
Description
Technical Field
[0001] The invention relates to the technical field of catalyst synthesis, and in particular to a system for synthesizing a catalyst for silicon powder in a one-step method through a composite route and a method for preparing silicate esters through a one-step method using silicon powder. Background Art
[0002] The one-step method of silicon powder refers to the method of using silicon powder to directly react with alkyl alcohol to produce alkyl orthosilicate. Compared with the traditional silicon tetrachloride alcoholysis process, this method is more environmentally friendly, has lower costs, and is conducive to industrial production.
[0003] In the silicon powder one-step method, it is usually necessary to add a catalyst to regulate the reaction rate, but the existing silicon powder one-step catalyst synthesis device and the methyl silicate production device are independent systems. The produced catalyst is transported in barrels and supplied to production by a diaphragm pump, which has the problem of poor efficiency and catalyst degradation during long-distance transportation. There are also many problems in the production process of the catalyst. First, due to the existence of multiple routes for catalyst synthesis, the cost of catalyst raw materials fluctuates with market conditions, which will lead to unstable catalyst costs; second, there are low-boiling point solvents in the catalyst raw materials in the finished catalyst, which will react with silicon powder and cause unnecessary dangers; third, the catalyst raw materials exist in various forms such as liquid and solid, which is inconvenient to feed; fourth, the activity of the catalyst cannot be regulated, and the reaction speed in subsequent production can only be regulated by the raw material dripping speed, and the regulation means are single; fifth, the products synthesized by the silicon powder one-step method include methyl silicate, ethyl silicate, etc., but one catalyst can only correspond to one product, and the existing catalyst production device can only prepare a catalyst suitable for the preparation of one product, and the production efficiency is low. Summary of the invention
[0004] In view of the above-mentioned deficiencies in the prior art, the object of the present invention is to provide a system for a catalyst for synthesizing silicon powder in a one-step process via a composite route, so as to solve the problems that the existing catalyst preparation system is independent of the methyl silicate production device, the catalyst is easily degraded during long-distance transportation and the production efficiency is low, and at the same time, the problem that the existing catalyst preparation system is difficult to achieve catalyst activity regulation and cannot meet different production needs is solved.
[0005] Furthermore, a method for preparing silicate from silicon powder in one step is provided.
[0006] In order to solve the above technical problems, the technical solution adopted by the present invention is as follows: A system for a catalyst for synthesizing silicon powder in one step through a composite route comprises a plurality of liquid raw material storage tanks and solid raw material storage tanks, wherein the liquid raw material storage tanks are used to store raw material liquid or azeotropic solvent, and the solid raw material storage tanks are used to store powdered solid raw materials; the bottoms of all raw material storage tanks are connected to a feed port at the top of a reactor through a discharge pipe; the bottom of the reactor is connected to a feed port of a finished product buffer tank through a pipe; the bottom of the finished product buffer tank is connected to an application end through a pipe; mass flow meters are provided on the discharge pipes of all liquid raw material storage tanks, and mass sensors are provided on all solid raw material storage tanks; and valves are provided on each pipe.
[0007] Furthermore, the gas outlet at the top of the reactor is connected to the gas inlet of the condenser through a pipeline, and the gas outlet of the condenser is connected to the vacuum pump and the liquid separator through pipelines.
[0008] Furthermore, the side wall of the lower end of the liquid separation tank is connected to the feed port of the reactor through a reflux pipe; the bottom of the liquid separation tank discharges the liquid through a drainage pipe; valves are provided on the reflux pipe and the drainage pipe.
[0009] Furthermore, the side walls at the upper and lower ends of the liquid separation tank are connected to the upper and lower ends of the liquid level meter via pipelines; valves are provided on the pipelines connecting the liquid separation tank and the liquid level meter.
[0010] Furthermore, a heating jacket is provided on the outer side of the finished product cache tank to keep the finished product cache tank warm.
[0011] Furthermore, the tops of all the solid raw material storage tanks are connected to the discharge end of a feed hopper through pipelines, and valves are provided on the pipelines connecting the solid raw material storage tanks and the feed hopper.
[0012] Furthermore, an agitator is provided in the finished product buffer tank.
[0013] Furthermore, there are three liquid raw material storage tanks and one solid raw material storage tank.
[0014] A method for preparing silicate using silicon powder in one step, wherein the raw materials for preparing silicate include a catalyst, and a catalyst preparation system is directly connected to a silicate preparation raw material tank through a pipeline, so that the prepared catalyst directly participates in the preparation of silicate through the pipeline.
[0015] Furthermore, the catalyst preparation system is a system for the catalyst used in the one-step synthesis of silicon powder by the composite route mentioned above; the application end is a silicate preparation raw material tank; and the silicate preparation raw material tank corresponding to the catalyst is a catalyst feed metering tank.
[0016] Compared with the prior art, the present invention has the following beneficial effects: 1. The catalyst preparation system of the present invention integrates the preparation of the catalyst, the storage device and the methyl silicate production device into a whole, avoiding the problem that the catalyst is easily degraded and the production efficiency is low during long-distance transportation. And by setting up multiple raw material storage tanks, different catalyst synthesis routes can be met at the same time, and a set of systems can be used to achieve the preparation of multiple catalysts, which is suitable for the preparation requirements of different silicates, has a wide range of applications, low cost and high production efficiency. And the present invention monitors the addition amount of the catalyst raw material by setting a mass flow meter and a mass sensor, thereby achieving the purpose of regulating the catalyst ratio. Since the activity of the catalyst is closely related to the catalyst ratio, by controlling the catalyst ratio, the catalyst activity can be regulated, thereby meeting different production requirements.
[0017] 2. The system of the present invention also integrates the negative pressure process and the azeotropic water removal process, and can realize the preparation of catalysts by the negative pressure process and the solid-liquid azeotropic separation process. By providing negative pressure conditions to the reaction system, the removal of low-boiling point solvents can be achieved to avoid excessive residual catalyst solvents, which causes the reaction rate to rise too fast when preparing silicates, resulting in danger. The setting of the separation tank and the reflux pipeline can realize the recycling of azeotropic solvents, so that the reaction of preparing catalysts by the azeotropic separation process can continue, and the utilization rate of reactants can be improved. In addition, the present invention can achieve heat preservation of the finished catalyst by arranging a heating jacket on the outside of the finished product buffer tank, reduce viscosity and prevent low-temperature crystallization. At the same time, in order to prevent stratification of the components, the agitator in the finished product buffer tank can be opened for stirring when the catalyst is output to the application end.
[0018] 3. The present invention can realize the synthesis of catalysts through different routes through the design of multiple raw material storage tanks. When the cost of catalyst raw materials fluctuates with market conditions, users can select catalyst raw materials with higher cost performance for preparation, thereby avoiding the situation of unstable catalyst costs. BRIEF DESCRIPTION OF THE DRAWINGS
[0019] Figure 1 This is a schematic diagram of the system structure of the catalyst used in the one-step method of synthesizing silicon powder by the composite route of the present invention.
[0020] In the figure, there are liquid raw material storage tank 1, solid raw material storage tank 2, reactor 3, finished product buffer tank 4, application end 5, mass flow meter 6, quality sensor 7, support frame 8, condenser 9, vacuum pump 10, separator tank 11, liquid level meter 12, heating jacket 13, feed funnel 14, and agitator 15. DETAILED DESCRIPTION
[0021] The specific implementation of the present invention is further described in detail below in conjunction with specific embodiments and drawings. Example
[0022] like Figure 1As shown, the present invention provides a system for a catalyst for a one-step method of synthesizing silicon powder by a composite route, comprising three liquid raw material storage tanks 1 and one solid raw material storage tank 2, wherein the liquid raw material storage tank 1 is used to store raw material liquid or azeotropic solvent, and the solid raw material storage tank 2 is used to store powdered solid raw materials; the bottoms of all raw material storage tanks are connected to the feed port at the top of a reactor 3 through a discharge pipe; the bottom of the reactor 3 is connected to the feed port of a finished product buffer tank 4 through a pipe; the bottom of the finished product buffer tank 4 is connected to an application end 5 through a pipe; mass flow meters 6 are provided on the discharge pipes of all liquid raw material storage tanks 1, and mass sensors 7 are provided on the solid raw material storage tank 2; valves are provided on each pipe.
[0023] In specific implementation, two support frames 8 are symmetrically arranged on the outer side wall of the solid raw material storage tank 2, which can support the solid raw material storage tank 2 to be suspended on the floor. The floor is provided with a mounting hole larger than the diameter of the solid raw material storage tank 2, and the solid raw material storage tank 2 can pass through the mounting hole and be suspended on the floor through the support frame 8; a mass sensor 7 is arranged between the floor and the support frame 8. This design has a simple structure and is easy to implement.
[0024] During specific implementation, the air outlet at the top of the reactor 3 is connected to the air inlet of the condenser 9 through a pipeline, and the air outlet of the condenser 9 is connected to the vacuum pump 10 and the liquid separator 11 through pipelines. In this way, the reactor 3 can be evacuated by the vacuum pump 10 to provide negative pressure conditions. Providing negative pressure conditions, one is because the finished catalyst has a certain viscosity, which is not conducive to solvent distillation. If atmospheric distillation is adopted, there is more solvent residue. When the catalyst with more solvent residue is used to catalyze the reaction of preparing silicate by one-step method of silicon powder, because the solvent will react with silicon powder, too much solvent will cause the reaction rate to rise suddenly. At this time, the external intervention effect takes effect slowly, and the reactants run around to other systems, which is easy to cause damage to instruments and equipment. And the reaction byproduct of preparing silicate by one-step method of silicon powder is hydrogen. If the reaction rate exceeds the maximum value of the system gas leakage, hydrogen pressure may appear at this time, which is extremely dangerous. A large amount of hydrogen is produced at the same time, which may cause the flowmeter to exceed the range, damage the flowmeter, and fail to monitor the reaction rate, causing thermal runaway, which is very easy to cause production accidents. Second, when the catalyst is prepared by the negative pressure process, the use of negative pressure is also the reaction condition of the negative pressure process. Negative pressure is needed to promote the mutual reaction between the components, and the low-boiling point by-products are converted into gaseous state by negative pressure, and the escape rate of the by-products is accelerated, so that the reaction proceeds in the positive reaction direction, the reaction speed is accelerated, and the reaction limit is increased. After the condenser 9 condenses the steam, it is temporarily stored in the separator 11, and part of the non-condensable gas enters the tail gas system for recycling and treatment through the vacuum pump 10.
[0025] In specific implementation, the side wall of the lower end of the liquid separator 11 is connected to the feed port of the reactor 3 through a reflux pipe; the bottom of the liquid separator 11 discharges the liquid through a drainage pipe; valves are provided on the reflux pipe and the drainage pipe. In this way, when the catalyst is prepared by the solid-liquid azeotropic separation process, the azeotrope condensed by the condenser 9 can be left to stand in the liquid separator 11 for stratification, and the lower layer of waste liquid can flow out through the drainage pipe for hazardous waste treatment, and the upper layer of azeotropic solvent can flow back to the reactor 3 through the reflux pipe for recycling. The byproduct water produced is continuously taken out through azeotropy, so that the reaction continues and the utilization rate of the reactants is improved.
[0026] In specific implementation, the side walls at the upper and lower ends of the liquid separation tank 11 are connected to the upper and lower ends of the liquid level gauge 12 through pipes, and valves are provided on the pipes connecting the liquid separation tank 11 and the liquid level gauge 12. In this way, it is convenient to observe the liquid separation of the condensate in the liquid separation tank 11, determine the liquid level position of the liquid separation through the liquid level gauge 12, and facilitate the reflux and discharge operations of the liquid.
[0027] In specific implementation, a heating jacket 13 is provided on the outer side of the finished product buffer tank 4 to keep the finished product buffer tank 4 warm. Since the catalyst has a certain viscosity, the heating jacket 13 is provided on the outer side of the finished product buffer tank 4 to keep the catalyst warm, reduce the viscosity and prevent low-temperature crystallization, and facilitate the transportation and use of the catalyst.
[0028] In specific implementation, the top of the solid raw material storage tank 2 is connected to the discharge end of the feed hopper 14 through a pipeline, and a valve is provided on the pipeline connecting the solid raw material storage tank 2 and the feed hopper 14. In this way, it is convenient to add the powdered solid raw material and avoid the raw material from spilling everywhere.
[0029] In specific implementation, the finished product buffer tank 4 is provided with an agitator 15. In this way, the catalyst can be prevented from being stratified, and the catalyst can be transported and used more easily.
[0030] Working principle: (1) Solid-liquid azeotropic separation process: When the catalyst is prepared by the azeotropic separation process, in the liquid raw material storage tank 1, two liquid raw material storage tanks 1 are used to store different azeotropic solvents respectively, and one liquid raw material storage tank 1 is used to store raw material liquid; the solid raw material storage tank 2 is used to store powdered solid raw material.
[0031] During operation: open the valves on all the discharge pipes, measure through the mass flowmeter 6 and the mass sensor 7, close the valves on the discharge pipes when the mass flowmeter 6 and the mass sensor 7 reach the set values, and the feeding is completed. Then, the reactor 3 starts to heat up for reaction, and the steam generated during the heating process flows out through the gas outlet of the reactor 3, flows into the liquid separator 11 for storage after being condensed by the condenser 9, and observes the liquid separation in the liquid separator 11 through the liquid level meter 12 to determine the liquid separation level position, and after the lower layer of waste liquid is discharged, the remaining azeotropic solvent can be refluxed to the reactor 3 through the pipeline connected to the liquid separator 11 and the reactor 3 for continuous reaction, thereby realizing the recycling of the solvent and the continuous removal of by-product water. After the reaction is completed, turn on the vacuum pump 10, keep the valve on the pipeline connected to the bottom of the liquid separator 11 closed, and the low-boiling point components such as the solvent are condensed by the condenser 9, part of which is retained in the liquid separator 11, and part of the non-condensable gas flows into the tail gas system through the vacuum pump 10 for recycling. After the low-boiling point components are completely or mostly removed, turn off the vacuum pump 10 and stop heating the reactor 3, open the valve on the pipeline connecting the reactor 3 and the finished product buffer tank 4, and allow the finished catalyst to flow into the finished product buffer tank 4 for temporary storage. When the application end 5 needs the catalyst to react, open the valve on the pipeline connecting the finished product buffer tank 4 and the application end 5 to transport the catalyst to the application end 5 for application. Since the catalyst has a certain viscosity, in specific implementation, a heating jacket 13 is set on the outside of the finished product buffer tank 4 to achieve thermal insulation of the catalyst, reduce viscosity and prevent low-temperature crystallization. At the same time, in order to prevent stratification of the components, the agitator 15 can be turned on for stirring when the catalyst is output to the application end 5, so as to facilitate the transportation and use of the catalyst.
[0032] (2) Negative pressure process: When the negative pressure process is used to prepare the catalyst, the three liquid raw material storage tanks 1 store three different raw material liquids respectively.
[0033] During operation: open the valve on the discharge pipe of the liquid raw material storage tank 1, and keep the valve on the discharge pipe of the solid raw material storage tank 2 closed, measure through the mass flowmeter 6, and close the valve on the discharge pipe when the mass flowmeter 6 reaches the set value, and the feeding is completed. Then, the reactor 3 starts to heat up for reaction, and the vacuum pump 10 is turned on at the same time. As the reaction proceeds, the low-boiling point components gradually evaporate from the gas outlet of the reactor 3, and are condensed by the condenser 9 and flow into the liquid separator 11 for temporary storage. The non-condensable gas produced by some reactions is recycled through the condenser 9 and the vacuum pump 10 to the tail gas treatment system. After the reaction is completed and the low-boiling point components are completely or mostly removed, turn off the vacuum pump 10 and stop heating the reactor 3, open the valve on the pipeline connecting the reactor 3 and the finished product buffer tank 4, so that the finished catalyst flows into the finished product buffer tank 4 for temporary storage, and when the application end 5 needs the catalyst to react, open the valve on the pipeline connecting the finished product buffer tank 4 and the application end 5, and transport the catalyst to the application end 5 for application. Since the catalyst has a certain viscosity, in specific implementation, a heating jacket 13 is installed on the outside of the finished product buffer tank 4 to keep the catalyst warm, reduce the viscosity and prevent low-temperature crystallization. At the same time, in order to prevent the components from stratifying, the agitator 15 can be turned on for stirring when the catalyst is output to the application end 5, so as to facilitate the transportation and use of the catalyst.
[0034] The catalyst preparation system of the present invention integrates the preparation, storage device and methyl silicate production device of the catalyst into a whole, avoiding the problem that the catalyst is easily degraded and the production efficiency is low during long-distance transportation. And by setting a plurality of raw material storage tanks, different catalyst synthesis routes can be met at the same time, and a set of systems can be used to achieve the preparation of multiple catalysts, which is suitable for the preparation requirements of different silicates, has a wide range of applications, low cost and high production efficiency. And the present invention monitors the addition amount of the catalyst raw material by setting a mass flow meter and a mass sensor, thereby achieving the purpose of regulating the catalyst ratio. Since the activity of the catalyst is closely related to the catalyst ratio, by controlling the catalyst ratio, the regulation of the catalyst activity can be achieved, thereby meeting different production requirements. In addition, the system of the present invention also integrates the negative pressure process and the azeotropic water removal process, and can realize the preparation of catalysts by two processes of negative pressure process and solid-liquid azeotropic liquid separation process, and by providing negative pressure conditions to the reaction system, the removal of low boiling point solvents can be achieved, avoiding excessive residual catalyst solvents obtained, so that when preparing silicates, the reaction rate rises too fast, resulting in danger. The arrangement of the separation tank and the reflux pipeline can realize the recycling of the azeotropic agent, so that the reaction of preparing the catalyst by the azeotropic separation process can continue, thereby improving the utilization rate of the reactants.
[0035] It should be noted that the application end described in the present invention is a silicate production device, specifically a catalyst feed metering tank in the silicate production device.
[0036] The present invention also provides a one-step method for preparing silicate from silicon powder. The raw materials for preparing silicate include a catalyst. The catalyst preparation system is directly connected to the silicate preparation raw material tank through a pipeline, so that the prepared catalyst directly participates in the preparation of silicate through the pipeline.
[0037] The catalyst preparation system is a system for the catalyst used in the one-step synthesis of silicon powder by the composite route; the application end in the catalyst preparation system is a silicate preparation raw material tank; in specific implementation, the silicate preparation raw material tank is a catalyst feed metering tank.
[0038] Finally, it should be noted that the above embodiments are only used to illustrate the technical solution of the present invention rather than to limit the technical solution. Those skilled in the art should understand that those modifications or equivalent substitutions of the technical solution of the present invention that do not depart from the purpose and scope of the technical solution should be included in the scope of the claims of the present invention.
Claims
1. A system for a catalyst for synthesizing silicon powder in one step by a composite route, characterized in that: It comprises several liquid raw material storage tanks and solid raw material storage tanks, the liquid raw material storage tanks are used to store raw material liquid or azeotropic solvent, the solid raw material storage tanks are used to store powdered solid raw materials; the bottoms of all raw material storage tanks are connected to the feed port at the top of the reactor through discharge pipes; the bottom of the reactor is connected to the feed port of the finished product buffer tank through a pipe; the bottom of the finished product buffer tank is connected to the application end through a pipe; the discharge pipes of all liquid raw material storage tanks are provided with mass flow meters, and all solid raw material storage tanks are provided with mass sensors; and valves are provided on each pipe.
2. The system for using a catalyst for synthesizing silicon powder in one step by a composite route according to claim 1, characterized in that: The gas outlet at the top of the reactor is connected to the gas inlet of the condenser through a pipeline, and the gas outlet of the condenser is connected to the vacuum pump and the liquid separation tank through pipelines respectively.
3. The system for using a catalyst for synthesizing silicon powder in one step by a composite route according to claim 2, characterized in that: The side wall of the lower end of the liquid separation tank is connected to the feed port of the reactor through a reflux pipe; the bottom of the liquid separation tank discharges the liquid through a drainage pipe; valves are provided on the reflux pipe and the drainage pipe.
4. The system for using a catalyst for synthesizing silicon powder in one step by a composite route according to claim 3, characterized in that: The side walls at the upper and lower ends of the liquid separation tank are correspondingly connected to the upper and lower ends of the liquid level meter through pipelines; valves are arranged on the pipelines connecting the liquid separation tank and the liquid level meter.
5. The system for a catalyst for synthesizing silicon powder in one step by a composite route according to claim 1, characterized in that: The outer side of the finished product buffer tank is provided with a heating jacket to keep the finished product buffer tank warm.
6. The system for using a catalyst for synthesizing silicon powder in one step by a composite route according to claim 1, characterized in that: The tops of all solid raw material storage tanks are connected to the discharge end of a feed hopper through pipelines, and valves are arranged on the pipelines connecting the solid raw material storage tanks and the feed hopper.
7. The system for using a catalyst for synthesizing silicon powder in one step by a composite route according to claim 1, characterized in that: The finished product buffer tank is provided with an agitator.
8. The system for using a catalyst for synthesizing silicon powder in one step by a composite route according to claim 1, characterized in that: There are three liquid raw material storage tanks and one solid raw material storage tank.
9. A method for preparing silicate from silicon powder in one step, characterized in that: The raw materials for preparing silicate include catalysts. The catalyst preparation system is directly connected to the silicate preparation raw material tank through a pipeline, so that the prepared catalyst directly participates in the preparation of silicate through the pipeline.
10. The method for preparing silicate from silicon powder in one step according to claim 9, characterized in that: The catalyst preparation system is a system for a catalyst for synthesizing silicon powder in a one-step method by a composite route as described in any one of claims 1 to 8; the application end is a silicate preparation raw material tank; and the silicate preparation raw material tank corresponding to the catalyst is a catalyst feed metering tank.