Liquid polycarbosilane reducing agent solution feeding device

Abstract

The utility model discloses a liquid polycarbosilane reducing agent solution feeding device which comprises a reducing agent solution bottle, a three-way valve is arranged at one end of the reducing agent solution bottle, one port of the three-way valve is connected with an inert gas inlet, and two ports of the three-way valve are connected with a detergent liquid inlet. Three ports of the three-way valve are connected with a gas phase inlet of the reducing agent solution bottle; a four-way valve is arranged at the other end of the reducing agent solution bottle, one port of the four-way valve is connected with the detergent liquid inlet, two ports of the four-way valve are connected with the inert gas inlet, three ports of the four-way valve are connected with the feeding port of the reaction kettle, and four ports of the four-way valve are connected with the liquid phase outlet of the reducing agent solution bottle. After the technical scheme is adopted, according to the feeding device provided by the utility model, the valve and the pipeline are flushed by adopting the solvent, and then the residual solvent is blown into a reaction system by using inert gas, so that a reducing agent solution can be prevented from being exposed in external air, spontaneous combustion is avoided, and potential safety hazards are avoided.

Description

Technical Field

[0001] The utility model relates to a feeding device for a liquid polycarbosilane reducing agent solution. Background Art

[0002] Liquid polycarbosilane is an ideal precursor for the preparation of silicon carbide ceramic-based composites due to its good fluidity, self-crosslinking, high ceramic yield and near-stoichiometric ratio of pyrolysis products.

[0003] Grignard coupling is the main method for synthesizing liquid polycarbosilane. Its preparation method is to use chloromethylchlorosilane to couple with Mg / THF Grignard reagent to condense into chlorinated polycarbosilane, and then reduce the chlorinated polycarbosilane with a reducing agent, and then acidify and wash, dehydrate with magnesium sulfate, and distill to obtain liquid polycarbosilane.

[0004] The reducing agents of liquid polycarbosilane include sodium borohydride reducing agent system, sodium hydride and lithium hydride reducing agent system, calcium hydride reducing agent system and lithium aluminum hydride. These reducing agents are all in powder state, and the powder is extremely flammable in the air. The powder material faces great safety risks during the process of discharging packaging, storage, transportation, unpacking and feeding. Therefore, the entire operation process must be very careful to ensure safe feeding and production. Therefore, in the process of reducing agent preparation, it is made into a liquid reducing agent, which not only solves the safety hazards of powder reducing agent, but also simplifies the reducing agent preparation process. Using liquid reducing agent as reducing agent, the reduction reaction is completed in a homogeneous system, which has the advantages of fast reduction reaction speed, high efficiency and controllable reaction rate. Liquid reducing agent is a flammable and explosive chemical. It cannot be exposed to the air during use and must be kept in a closed state. Therefore, it is very necessary to design a feeding device to feed liquid reducing agent for protection.

[0005] However, currently, when using a reducing agent solution bottle for feeding, an inert gas is simply connected to the gas phase inlet of the reducing agent solution bottle, and the liquid phase outlet of the reducing agent solution bottle is directly connected to the reactor. After the feeding is completed, when the reducing agent solution bottle is disassembled, the reducing agent solution will remain and accumulate in the valve and the pipeline. These reducing agent solutions are exposed to the air and will immediately react with the water in the air to generate a large amount of hydrogen and release a large amount of heat, resulting in spontaneous combustion, and then causing a fire, causing a safety hazard. Utility Model Content

[0006] In view of the above problems, the utility model provides a liquid polycarbosilane reducing agent solution feeding device.

[0007] In order to solve the above technical problems, the technical solution adopted by the utility model is: a liquid polycarbosilane reducing agent solution feeding device, including a reducing agent solution bottle, characterized in that: a three-way valve is provided at one end of the reducing agent solution bottle, one port of the three-way valve is connected to the inert gas inlet, the second port of the three-way valve is connected to the detergent inlet, and the three ports of the three-way valve are connected to the gas phase inlet of the reducing agent solution bottle; a four-way valve is provided at the other end of the reducing agent solution bottle, one port of the four-way valve is connected to the detergent inlet, the second port of the four-way valve is connected to the inert gas inlet, the three ports of the four-way valve are connected to the feed port of the reactor, and the four ports of the four-way valve are connected to the liquid phase outlet of the reducing agent solution bottle.

[0008] Preferably, a first inert gas inlet valve is arranged between one port of the three-way valve and the inert gas inlet, a first detergent inlet valve is arranged between the second port of the three-way valve and the detergent inlet, and a gas phase inlet valve is arranged between the third port of the three-way valve and the gas phase inlet of the reducing agent solution bottle.

[0009] Preferably, a pressure gauge is further provided between one port of the three-way valve and the inert gas inlet, and the pressure gauge is located on a side of the first inert gas inlet valve close to the three-way valve.

[0010] Preferably, a second detergent inlet valve is arranged between one port of the four-way valve and the detergent inlet, a second inert gas inlet valve is arranged between the second port of the four-way valve and the inert gas inlet, a reactor valve is arranged between the third port of the four-way valve and the reactor, and a liquid phase outlet valve is arranged between the fourth port of the four-way valve and the liquid phase outlet of the reducing agent solution bottle.

[0011] Preferably, the reducing agent solution bottle is made of steel.

[0012] Preferably, the inert gas is nitrogen.

[0013] From the above description of the structure of the utility model, it can be seen that compared with the prior art, the utility model has the following advantages:

[0014] The utility model provides a liquid polycarbosilane reducing agent solution feeding device, which uses a solvent to flush valves and pipelines, and then uses an inert gas to blow the residual solvent into the reaction system, so that the reducing agent solution is prevented from being exposed to the outside air, spontaneous combustion will not occur, and safety hazards are eliminated; and the feeding device has a simple structural design, is easy to use, and has practical application value. BRIEF DESCRIPTION OF THE DRAWINGS

[0015] The drawings constituting a part of this application are used to provide a further understanding of the present invention. The illustrative embodiments of the present invention and their descriptions are used to explain the present invention and do not constitute an improper limitation on the present invention. In the drawings:

[0016] Figure 1 The utility model is a schematic diagram of a liquid polycarbosilane reducing agent solution feeding device. DETAILED DESCRIPTION

[0017] It should be noted that, in the absence of conflict, the embodiments of the present invention and the features in the embodiments can be combined with each other.

[0018] In the description of the present utility model, it should be understood that the terms "center", "longitudinal", "lateral", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inside", "outside" and the like indicate positions or positional relationships based on the positions or positional relationships shown in the accompanying drawings, and are only for the convenience of describing the present utility model and simplifying the description, rather than indicating or implying that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore cannot be understood as a limitation on the present utility model. In addition, the terms "first", "second", etc. are only used for descriptive purposes, and cannot be understood as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Therefore, features defined as "first", "second", etc. may explicitly or implicitly include one or more of the features. In the description of the present utility model, unless otherwise specified, "multiple" means two or more.

[0019] In the description of the present invention, it should be noted that, unless otherwise clearly specified and limited, the terms "installation", "connection" and "connection" should be understood in a broad sense, for example, it can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection; it can be a direct connection, or it can be an indirect connection through an intermediate medium, or it can be the internal communication of two components. For ordinary technicians in this field, the specific meanings of the above terms in the present invention can be understood by specific circumstances.

[0020] The present invention will be described in detail below with reference to the accompanying drawings and in combination with embodiments.

[0021] Example

[0022] refer to Figure 1A liquid polycarbosilane reducing agent solution feeding device comprises a reducing agent solution bottle 10, the reducing agent solution bottle 10 is made of steel, a three-way valve 8 is arranged at one end of the reducing agent solution bottle 10, one port of the three-way valve 8 is connected to the inert gas inlet through a pipeline, two ports of the three-way valve 8 are connected to the detergent inlet through a pipeline, and three ports of the three-way valve 8 are connected to the gas phase inlet of the reducing agent solution bottle 10 through a pipeline; a four-way valve 9 is arranged at the other end of the reducing agent solution bottle 10, one port of the four-way valve 9 is connected to the detergent inlet through a pipeline, two ports of the four-way valve 9 are connected to the inert gas inlet through a pipeline, three ports of the four-way valve 9 are connected to the feed port of the reactor through a pipeline, and four ports of the four-way valve 9 are connected to the liquid phase outlet of the reducing agent solution bottle 10. With this structure, by flushing the valve and pipeline with a solvent, and then sweeping the residual solvent into the reaction system with an inert gas, the reducing agent solution can be prevented from being exposed to the outside air, spontaneous combustion will not occur, and safety hazards can be eliminated.

[0023] A first inert gas inlet valve 1 is provided between one port of the three-way valve 8 and the inert gas inlet, a first detergent inlet valve 2 is provided between the second port of the three-way valve 8 and the detergent inlet, and a gas phase inlet valve 3 is provided between the third port of the three-way valve 8 and the gas phase inlet of the reducing agent solution bottle 10; a pressure gauge 11 is also provided between one port of the three-way valve 8 and the inert gas inlet, and the pressure gauge 11 is located on a side of the first inert gas inlet valve 1 close to the three-way valve 8, and the pressure in the reducing agent solution bottle 10 is controlled by the pressure gauge 11; wherein, the first inert gas inlet valve 1, the first detergent inlet valve 2, the gas phase inlet valve 3 and the pressure gauge 11 are installed on their respective corresponding pipelines.

[0024] A second detergent inlet valve 4 is provided between one port of the four-way valve 9 and the detergent inlet, a second inert gas inlet valve 5 is provided between the second port of the four-way valve 9 and the inert gas inlet, a reactor valve 6 is provided between the third port of the four-way valve 9 and the reactor, and a liquid phase outlet valve 7 is provided between the fourth port of the four-way valve 9 and the liquid phase outlet of the reducing agent solution bottle 10; wherein, the second detergent inlet valve 4, the second inert gas inlet valve 5, the reactor valve 6 and the liquid phase outlet valve 7 are installed on their respective corresponding pipelines.

[0025] When used specifically:

[0026] Open the first inert gas inlet valve 1 and the gas phase inlet valve 3, open the liquid phase outlet valve 7 and the reactor valve 6, and introduce nitrogen into the reducing agent solution bottle 10 by controlling the inert gas pressure gauge 11, control the pressure in the reducing agent solution bottle 10 to be 0.02MPa-0.1MPa, and inject the reducing agent solution in the reducing agent solution bottle 10 into the reactor for reduction reaction;

[0027] If all the reducing agent solution in the reducing agent solution bottle 10 is used up, it is necessary to switch the reducing agent solution bottle 10 or disassemble the reducing agent solution bottle 10, and the operation is as follows: close the first inert gas inlet valve 1, open the first detergent liquid inlet valve 2 and the gas phase inlet valve 3, so that a certain amount of washing solvent can be injected into the reducing agent solution bottle 10, and then close the first detergent liquid inlet valve 2, reopen the first inert gas inlet valve 1, and open the liquid phase outlet valve 7 and the reactor valve 6, and introduce nitrogen to inject the solvent in the reducing agent solution bottle 10 into the reactor until all the washing solvent is injected into the reactor, and circulate nitrogen to replace the pipeline, and finally close all valves; the gas phase inlet valve 3, the liquid phase outlet valve 7 and the reactor valve 6 can be flushed with the washing solvent; after flushing, the gas phase inlet and the liquid phase outlet of the reducing agent solution bottle 10 can be disassembled to switch or disassemble the reducing agent solution bottle 10.

[0028] If the reducing agent solution in the reducing agent solution bottle 10 has not been completely used up and the reducing agent solution bottle 10 needs to be disassembled, the operation is as follows: close the first inert gas inlet valve 1, the gas phase inlet valve 3, the liquid phase outlet valve 7 and the reactor valve 6, open the second detergent inlet valve 4, and inject a washing solvent to flush the liquid phase outlet valve 7 and the reactor valve 6 and their pipelines. After flushing, open the second inert gas inlet valve 5, and use nitrogen to inject the remaining solvent in the valve and the pipeline into the reactor, and finally close all valves; after flushing, the gas phase inlet and the liquid phase inlet of the reducing agent solution bottle 10 can be disassembled to disassemble the reducing agent solution bottle 10.

[0029] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions and improvements made within the spirit and principles of the present invention should be included in the protection scope of the present invention.

Claims

1. A liquid polycarbosilane reducing agent solution feeding device, comprising a reducing agent solution bottle, characterized in that: A three-way valve is provided at one end of the reducing agent solution bottle, one port of the three-way valve is connected to the inert gas inlet, two ports of the three-way valve are connected to the detergent inlet, and three ports of the three-way valve are connected to the gas phase inlet of the reducing agent solution bottle; a four-way valve is provided at the other end of the reducing agent solution bottle, one port of the four-way valve is connected to the detergent inlet, two ports of the four-way valve are connected to the inert gas inlet, three ports of the four-way valve are connected to the feed port of the reactor, and four ports of the four-way valve are connected to the liquid phase outlet of the reducing agent solution bottle.

2. A liquid polycarbosilane reducing agent solution feeding device according to claim 1, characterized in that: A first inert gas inlet valve is arranged between one port of the three-way valve and the inert gas inlet, a first detergent inlet valve is arranged between the second port of the three-way valve and the detergent inlet, and a gas phase inlet valve is arranged between the third port of the three-way valve and the gas phase inlet of the reducing agent solution bottle.

3. A liquid polycarbosilane reducing agent solution feeding device according to claim 2, characterized in that: A pressure gauge is also provided between one port of the three-way valve and the inert gas inlet, and the pressure gauge is located on a side of the first inert gas inlet valve (1) close to the three-way valve.

4. A liquid polycarbosilane reducing agent solution feeding device according to claim 1, characterized in that: A second detergent inlet valve is arranged between one port of the four-way valve and the detergent inlet, a second inert gas inlet valve (5) is arranged between the second port of the four-way valve and the inert gas inlet, a reactor valve is arranged between the third port of the four-way valve and the reactor, and a liquid phase outlet valve is arranged between the fourth port of the four-way valve and the liquid phase outlet of the reducing agent solution bottle.

5. The liquid polycarbosilane reducing agent solution feeding device according to claim 1, characterized in that: The reducing agent solution bottle is made of steel.

6. A liquid polycarbosilane reducing agent solution feeding device according to claim 1, characterized in that: The inert gas is nitrogen.

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