Tetramethylsilane filling system

Abstract

The utility model discloses a tetramethylsilane filling system which comprises a product storage tank provided with a liquid outlet pipe and a liquid inlet pipe; the circulating device comprises a circulating inlet pipe connected with the liquid outlet pipe, a filter connected with the circulating inlet pipe and a circulating outlet pipe connected with the filter, and the circulating outlet pipe is connected with the liquid inlet pipe; the filling tank is connected with the circulating outlet pipe; the control device is used for controlling the filling tank to be communicated with the circulating outlet pipe and closing the communication between the circulating outlet pipe and the liquid inlet pipe; or the circulation outlet pipe is controlled to be communicated with the liquid inlet pipe, and meanwhile communication between the filling tank and the circulation outlet pipe is closed. According to the tetramethylsilane filling system, low-carbon hydrocarbons and particulate matters in the product storage tank can be effectively removed, pollution to products is avoided, the operation mode and the structural unit are simple, and the tetramethylsilane filling system can be used in the subsequent filling tank treatment process only by switching the valve under the condition that new equipment is not additionally built.

Description

Technical Field

[0001] The utility model belongs to the technical field of chemical reaction equipment, in particular to a tetramethylsilane filling system. Background Art

[0002] Tetramethylsilane (4MS) is a colorless, transparent liquid that is insoluble in water but soluble in most organic solvents. It is used as a reference substance in nuclear magnetic resonance spectroscopy (NMR) spectra and is often used as aviation fuel due to its physical and chemical properties. With the recent development of the semiconductor industry, demand for high-purity tetramethylsilane (4MS > 99.99 wt%) has continued to increase. It is commonly used in the manufacture of silicon materials, low-k dielectric materials, vapor phase chemical deposition materials, plasma polymerization organic silicon films, and other applications. Silicon carbide, the mainstream material, is widely used in the photovoltaic, semiconductor, and nuclear industries.

[0003] Currently, the sources of 4MS are relatively abundant, such as directly synthesizing it from methylmagnesium chloride and trimethylchlorosilane, or purifying it from the by-products of the production of other silicon-based materials. However, the production of high-purity 4MS is quite difficult. Even after multiple distillations, it is still difficult to reach the 99.99wt% requirement. Therefore, it is necessary to add a separation step, such as using molecular sieves to adsorb impurities on the distilled product to obtain a high-purity 4MS product. However, there will be the problem of interference from particulate matter. In addition, experiments have shown that the impurities in the 4MS material will undergo a certain catalytic reaction on the adsorbent to generate low-carbon hydrocarbons. These hydrocarbons will dissolve in the 4MS product, directly affecting the product quality.

[0004] In the existing high-purity 4MS production process, the raw materials used contain only about 50wt% 4MS. After purification operations such as distillation and adsorption, a 99.99wt% product can be obtained. However, a small amount of low-carbon hydrocarbons often dissolve in the adsorbed product, which directly affects the quality of the product before filling and cannot meet the requirement of 4MS>99.99wt%.

[0005] Therefore, in view of the above technical problems, it is necessary to provide a filling system suitable for high-purity tetramethylsilane.

[0006] The information disclosed in this background technology section is only intended to increase the understanding of the overall background of the present invention, and should not be regarded as an admission or any form of suggestion that the information constitutes the prior art already known to those skilled in the art. Utility Model Content

[0007] The purpose of the utility model is to provide a tetramethylsilane filling system, which can effectively remove low-carbon hydrocarbons and particulate matter in product storage tanks to avoid contamination of the product.

[0008] In order to achieve the above-mentioned purpose, the technical solution provided by a specific embodiment of the present invention is as follows:

[0009] A tetramethylsilane filling system, comprising:

[0010] Product storage tank, equipped with liquid outlet pipe and liquid inlet pipe;

[0011] A circulation device, comprising a circulation inlet pipe connected to the liquid outlet pipe, a filter connected to the circulation inlet pipe, and a circulation outlet pipe connected to the filter, wherein the circulation outlet pipe is connected to the liquid inlet pipe;

[0012] Filling tank, connected to the circulation outlet pipe;

[0013] The control device controls the filling tank to be connected to the circulation outlet pipe and closes the connection between the circulation outlet pipe and the liquid inlet pipe; or controls the circulation outlet pipe to be connected to the liquid inlet pipe and closes the connection between the filling tank and the circulation outlet pipe.

[0014] In one or more embodiments of the present invention, the filling tank is provided with a through pipe connected to the circulation outlet pipe, and the control device includes a first valve provided on the circulation outlet pipe and a second valve provided on the through pipe, and the first valve is located between the liquid inlet pipe and the through pipe.

[0015] In one or more embodiments of the present invention, there are several filling tanks, the circulation outlet pipe is connected to a branch main pipe located between the first valve and the filter, and the through pipes on the several filling tanks are all connected to the branch main pipe.

[0016] In one or more embodiments of the present invention, the circulation device further includes a circulation pump located between the liquid outlet pipe and the filter, and the circulation pump is connected to the circulation inlet pipe.

[0017] In one or more embodiments of the present invention, the filling tank is provided with a liquid return pipe, the liquid return pipe is connected to the liquid inlet pipe, and a third valve is provided on the liquid return pipe.

[0018] In one or more embodiments of the present invention, the product storage tank is provided with a nitrogen inlet pipe for filling the product storage tank with nitrogen.

[0019] In one or more embodiments of the present invention, the product storage tank is provided with an emptying port.

[0020] In one or more embodiments of the present invention, the product storage tank is provided with a condenser.

[0021] In one or more embodiments of the present invention, at least two filters are provided.

[0022] Compared with the existing technology, the utility model utilizes a circulation pump and a filter to filter the material in the product storage tank and then transports it back to the product storage tank, thereby ensuring the purity of the material in the product storage tank, and by switching different valves on the pipeline, the filling tank to be filled is processed and filled. The whole system has high safety, simple operation, low implementation cost, and can be applied to actual production. BRIEF DESCRIPTION OF THE DRAWINGS

[0023] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the following briefly introduces the drawings required for use in the embodiments or the description of the prior art. Obviously, the drawings described below are only some embodiments recorded in the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying any creative work.

[0024] Figure 1 This is a schematic structural diagram of the tetramethylsilane filling system in Example 1 of the present utility model;

[0025] Figure 2 This is a schematic structural diagram of the tetramethylsilane filling system in Example 2 of the present utility model.

[0026] Description of main reference numerals:

[0027] 1. Product storage tank; 11. Liquid outlet pipe; 12. Liquid inlet pipe; 13. Nitrogen pipe; 14. Drain port; 21. Circulation inlet pipe; 22. Circulation pump; 23. Filter; 24. Circulation outlet pipe; 25. Branch main pipe; 3. Filling tank; 31. Through pipe; 32. Liquid return pipe; 41. First valve; 42. Second valve; 43. Third valve. DETAILED DESCRIPTION

[0028] In order to enable those skilled in the art to better understand the technical solutions of the present invention, the following will be combined with the drawings of the embodiments of the present invention to clearly and completely describe the technical solutions of the embodiments of the present invention. Obviously, the embodiments described are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative efforts should fall within the scope of protection of the present invention.

[0029] Example 1

[0030] like Figure 1As shown, the tetramethylsilane filling system in one embodiment of the present invention includes a product storage tank 1, which is provided with a liquid outlet pipe 11 and a liquid inlet pipe 12. The liquid outlet pipe 11 is connected to a circulation inlet pipe 21, and the circulation inlet pipe 21 is connected to a filter 23. At the same time, the circulation inlet pipe 21 is also connected to a circulation pump 22 located between the liquid outlet pipe 11 and the filter 23. The circulation pump 22 is used to transport the 4MS product in the product storage tank 1 to the filter 23 to remove particulate matter in the product and achieve a decontamination effect. Of course, in order to further enhance the decontamination effect, multiple filters 23 can be provided. In this embodiment, two filters 23 are provided in parallel.

[0031] Furthermore, the filter 23 is connected to a circulation outlet pipe 24, which is connected to the liquid inlet pipe 12. After being filtered by the filter 23, the product flows into the product storage tank 1 through the circulation outlet pipe 24 and the liquid inlet pipe 12. Thus, the filter 23 is used to remove particulate matter in the product before filling, thereby ensuring the purity of the product in the product storage tank 1.

[0032] Furthermore, the product storage tank 1 is provided with a nitrogen pipe 13. After the product storage tank 1 is filled with 4MS product, nitrogen can be filled into the product storage tank 1 through the nitrogen pipe 13 to pressurize and maintain 0.4MPa to prevent the product from vaporizing after passing through the filter 23. At the same time, after the product passes through the filter 23, the low-carbon hydrocarbons dissolved in the material may be volatilized and separated. Therefore, the product storage tank 1 is also provided with an emptying port 14. The emptying port 14 is intermittently opened to discharge the low-carbon hydrocarbons and discharge the low-carbon hydrocarbons into the exhaust system. The product storage tank 1 is also provided with a sampling port, and the purity of the material in the product storage tank 1 can be analyzed through the sampling port before circulating filtration. The product storage tank 1 is also provided with a condenser, which can condense the volatilized 4MS product back into the product storage tank 1.

[0033] Furthermore, the tetramethylsilane filling system also includes a filling tank 3, which is connected to a through pipe 31, and a circulation outlet pipe 24 is connected to the through pipe 31. In order to control the product to selectively flow to the filling tank 3 or the product storage tank 1 after passing through the filter 23, a first valve 41 located between the through pipe 31 and the liquid inlet pipe 12 is provided on the circulation outlet pipe 24, and a second valve 42 is provided on the through pipe 31. When the product needs to be cleaned of impurities, the second valve 42 is closed and the first valve 41 is opened to connect the liquid inlet pipe 12 and the circulation outlet pipe 24, so that the product flows into the product storage tank 1 after passing through the filter 23, and after circulating outflow and inflow, the impurity removal purpose is achieved through the filter 23. When filling is performed, the first valve 41 is closed and the second valve 42 is opened to connect the circulation outlet pipe 24 and the through pipe 31, so that the product flows into the filling tank 3 after passing through the filter 23, thereby completing the filling.

[0034] Before filling, in order to ensure the cleanliness of the filling tank 3, it is necessary to fill the filling tank 3 with an appropriate amount of product for padding treatment, and then fill it when the cleanliness of the filling tank 3 meets the requirements. Specifically, the filling tank 3 is connected to a return liquid pipe 32, and the return liquid pipe 32 is connected to the liquid inlet pipe 12. A third valve 43 is also provided on the return liquid pipe 32. When padding treatment is required, close the first valve 41, open the second valve 42 and the third valve 43, so that the product enters the filling tank 3 and then flows back into the product storage tank 1. The product in the product storage tank 1 is then filtered through the filter 23. When the 4MS purity in the filling tank 3 is detected to be greater than 99.99wt%, it means that the cleanliness of the filling tank 3 meets the requirements and can be filled normally. The first valve 41, the second valve 42 and the third valve 43 in the present invention are all ball valves.

[0035] Before using the tetramethylsilane filling system in this embodiment, the material in the product storage tank 1 is first analyzed by gas chromatography. If the heavy component content is greater than 0.01wt%, the material in the product storage tank 1 is re-transported to the adsorption device for impurity removal. During normal use, before filling the filling tank 3, the material in the product storage tank 1 is circulated and filtered using the circulation pump 22 and the filter 23, and the material in the product storage tank 1 is analyzed by gas chromatography. If the 4MS content in the material reaches 99.99wt%, it is qualified and can be filled. During filling, close the first valve 41, open the second valve 42 and the third valve 43, first perform padding treatment on the filling tank 3, and then close the third valve 43 for filling after the cleanliness of the filling tank 3 meets the requirements.

[0036] Example 2

[0037] like Figure 2 As shown, the difference between this embodiment and embodiment 1 is that two filling tanks 3 are provided, the circulation outlet pipe 24 is connected to a branch main pipe 25, the branch main pipe 25 is located between the first valve 41 and the filter 23, and the through pipes 31 on the filling tanks 3 are all connected to the branch main pipe 25, so that the material flowing out of the filter 23 can flow into the two filling tanks 3 through the branch main pipe 25. Of course, in other embodiments, the number of filling tanks 3 can also be set to 3, 4, 6, etc.

[0038] It will be apparent to those skilled in the art that the present invention is not limited to the details of the exemplary embodiments described above and that the present invention can be implemented in other specific forms without departing from the spirit or essential characteristics of the present invention. Therefore, the embodiments should be considered in all respects as illustrative and non-restrictive, and the scope of the present invention is defined by the appended claims, not the foregoing description, and all variations within the meaning and range of equivalents of the claims are intended to be encompassed within the present invention. Any reference sign in a claim should not be construed as limiting the claim to which it relates.

[0039] In addition, it should be understood that although this specification is described in terms of implementation methods, not every implementation method contains only one independent technical solution. This narrative method of the specification is only for the sake of clarity. Those skilled in the art should regard the specification as a whole. The technical solutions in each embodiment can also be appropriately combined to form other implementation methods that can be understood by those skilled in the art.

Claims

1. A tetramethylsilane filling system, characterized in that: include: Product storage tank, equipped with liquid outlet and liquid inlet pipes; A circulation device, comprising a circulation inlet pipe connected to the liquid outlet pipe, a filter connected to the circulation inlet pipe, and a circulation outlet pipe connected to the filter, wherein the circulation outlet pipe is connected to the liquid inlet pipe; Filling tank, connected to the circulation outlet pipe; The control device controls the filling tank to be connected to the circulation outlet pipe and closes the connection between the circulation outlet pipe and the liquid inlet pipe; or controls the circulation outlet pipe to be connected to the liquid inlet pipe and closes the connection between the filling tank and the circulation outlet pipe.

2. The tetramethylsilane filling system according to claim 1, characterized in that: The filling tank is provided with a through pipe connected to the circulation outlet pipe, and the control device includes a first valve provided on the circulation outlet pipe and a second valve provided on the through pipe, wherein the first valve is located between the liquid inlet pipe and the through pipe.

3. The tetramethylsilane filling system according to claim 2, characterized in that: There are several filling tanks, and the circulation outlet pipe is connected to a branch main pipe located between the first valve and the filter, and the through pipes on the several filling tanks are all connected to the branch main pipe.

4. The tetramethylsilane filling system according to claim 1, characterized in that: The circulation device further comprises a circulation pump located between the liquid outlet pipe and the filter, and the circulation pump is connected to the circulation inlet pipe.

5. The tetramethylsilane filling system according to claim 1, characterized in that: The filling tank is provided with a liquid return pipe, the liquid return pipe is connected to the liquid inlet pipe, and the liquid return pipe is provided with a third valve.

6. The tetramethylsilane filling system according to claim 1, characterized in that: The product storage tank is provided with a nitrogen inlet pipe for filling the product storage tank with nitrogen.

7. The tetramethylsilane filling system according to claim 1, characterized in that: The product storage tank is provided with an emptying port.

8. The tetramethylsilane filling system according to claim 1, characterized in that: The product storage tank is provided with a condenser.

9. The tetramethylsilane filling system according to claim 1, characterized in that: At least two filters are provided.

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