Adsorption and purification device for tetramethylsilane mixture
By using a multi-stage adsorption tower system with different adsorbents to remove impurities from a tetramethylsilane mixture, the problem of difficult purification by conventional distillation is solved, and high-purity and low-cost tetramethylsilane preparation is achieved, which has both environmental and economic benefits.
Patent Information
- Application Number
- CN202422974451.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2024-12-02
- Publication Date
- 2025-11-04
- Estimated Expiration
- 2034-12-02
AI Technical Summary
Existing technologies struggle to efficiently remove multiple impurities with similar boiling points from tetramethylsilane mixtures, making conventional distillation purification difficult and affecting the purity and cost of electronic-grade tetramethylsilane.
A multi-stage adsorption tower system was adopted, using adsorbents such as activated carbon, 13X molecular sieve, calcium oxide, calcium hydroxide, anhydrous calcium chloride and ZSM-5 molecular sieve to remove impurities through a specific sequential adsorption process, thereby obtaining ultrapure tetramethylsilane.
The preparation of high-purity (99.99%) tetramethylsilane has been achieved, reducing raw material costs and energy consumption, minimizing resource waste, and conforming to the principles of green chemistry and economy.
Smart Images
Figure CN223504857U_ABST
Abstract
Description
Technical Field
[0001] This invention belongs to the field of tetramethylsilane purification technology, specifically relating to an adsorption purification device for a tetramethylsilane mixture. Background Technology
[0002] Electronic-grade ultrapure silicon-based precursor materials are key raw materials in the manufacturing process of next-generation semiconductors, and their quality and technological content directly affect the performance and quality of the final semiconductor products. Tetramethylsilane is a very important type of silicon-based precursor, obtained as a byproduct of organosilicon material production in the chemical industry. This industrial waste, in addition to tetramethylsilane, contains many impurities with boiling points very close to tetramethylsilane, such as isopentane, 2-chloropropane, 2-methylbutane, and 1-pentene. The boiling points of these substances differ by only a few degrees, making it extremely difficult to obtain high-purity products through conventional distillation purification.
[0003] The information disclosed in this background section is intended only to enhance the understanding of the overall background of this utility model and should not be construed as an admission or in any way implying that the information constitutes prior art known to those skilled in the art. Utility Model Content
[0004] The purpose of this invention is to provide an adsorption purification device for a mixture of tetramethylsilanes, which can continuously adsorb raw materials, remove impurities contained in the raw materials, and obtain electronic-grade tetramethylsilanes.
[0005] To achieve the above objectives, the technical solution provided by a specific embodiment of this utility model is as follows:
[0006] An adsorption purification apparatus for a tetramethylsilane mixture includes a vaporizer and further includes:
[0007] The first-stage adsorption tower, connected to the vaporizer, is used to remove chlorinated alkane impurities; the first-stage adsorption tower is an adsorption tower equipped with activated carbon and / or 13X molecular sieves.
[0008] The second-stage adsorption tower is connected to the first-stage adsorption tower and is used to remove hydrochloric acid and low-carbon alkanes.
[0009] The third-stage adsorption tower, connected to the second-stage adsorption tower, is used to remove isopentane.
[0010] In one or more embodiments of this utility model, the bulk density of the 13X molecular sieve in the first-stage adsorption tower is 0.6 to 0.7 kg / L.
[0011] In one or more embodiments of this utility model, the bulk density of the activated carbon in the first-stage adsorption tower is 0.45 to 0.65 kg / L.
[0012] In one or more embodiments of this utility model, the second-stage adsorption tower is provided with an adsorbent, the bulk density of which is 0.45 to 0.55 kg / L.
[0013] In one or more embodiments of this invention, the adsorbent is calcium oxide and / or calcium hydroxide.
[0014] In one or more embodiments of this invention, the adsorbent further includes anhydrous calcium chloride.
[0015] In one or more embodiments of this utility model, the particle size of the adsorbent is 2-5 mm.
[0016] In one or more embodiments of this utility model, the third-stage adsorption tower is an adsorption tower equipped with ZSM-5 molecular sieve and / or HZSM-5 molecular sieve.
[0017] In one or more embodiments of this utility model, the bulk density of the molecular sieve in the third-stage adsorption tower is 0.6 to 0.7 kg / L.
[0018] In one or more embodiments of this utility model, the particle size of the molecular sieve in the third adsorption tower is 2-5 mm.
[0019] Compared with existing technologies, this invention, by arranging adsorption towers filled with different adsorbents or molecular sieves in a specific sequence, continuously adsorbs and removes various impurities from the raw materials, yielding electronic-grade quaternary silane with a purity of 99.99%. This silane can serve as an organosilicon source to meet the needs of the semiconductor industry for chemical vapor deposition and atomic layer deposition. Furthermore, the tail gas generated during the industrial synthesis of methylchlorosilane can be used as a starting material. After a single-stage distillation, it can be directly adsorbed and purified using the adsorption purification device of this invention. This not only significantly reduces raw material costs and energy consumption during distillation but also embodies the principles of green chemistry and economy, significantly reducing resource waste and being extremely environmentally friendly, thus possessing both economic benefits and environmental significance. Attached Figure Description
[0020] To more clearly illustrate the technical solutions in the embodiments of this utility model or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments recorded in this utility model. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.
[0021] Figure 1 This is an adsorption flow chart of an adsorption purification device for a tetramethylsilane mixture in one embodiment of the present invention. Detailed Implementation
[0022] To enable those skilled in the art to better understand the technical solutions of this utility model, the technical solutions of the embodiments of this utility model will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of this utility model, and not all embodiments. Based on the embodiments of this utility model, all other embodiments obtained by those skilled in the art without creative effort should fall within the protection scope of this utility model.
[0023] like Figure 1 As shown in the figure, a specific embodiment of this utility model provides an adsorption purification device for a tetramethylsilane mixture, which includes a vaporizer, a first-stage adsorption tower, a second-stage adsorption tower, a third-stage adsorption tower, and a filter connected in sequence. The raw material, after being distilled in a rectification stage, enters the vaporizer for vaporization. The gas generated by vaporization enters the first-stage adsorption tower to remove chlorinated alkane impurities, then enters the second-stage adsorption tower to remove hydrochloric acid and low-carbon alkanes, then enters the third-stage adsorption tower to remove isopentane, and finally passes through the filter to remove remaining impurities, thereby obtaining ultrapure tetramethylsilane. The raw material is the enriched product of the tail gas generated during the industrial synthesis of methylsilane. The first-stage, second-stage, and third-stage adsorption towers are all 2400 mm high and have a diameter of DN400.
[0024] Furthermore, the first-stage adsorption tower is an adsorption tower equipped with activated carbon and / or 13X molecular sieve, the particle size of both activated carbon and 13X molecular sieve is 1-3 mm; the bulk density of 13X molecular sieve in the first-stage adsorption tower is 0.6-0.7 kg / L, and the bulk density of activated carbon in the first-stage adsorption tower is 0.45-0.65 kg / L.
[0025] Furthermore, the second-stage adsorption tower contains an adsorbent, specifically calcium oxide and / or calcium hydroxide, with a particle size of 2–5 mm and a bulk density of 0.45–0.55 kg / L. Since the second-stage adsorption tower primarily removes small amounts of hydrochloric acid and low-carbon alkane byproducts generated during the adsorption catalysis process, anhydrous calcium chloride is also included as an adsorbent to prevent the formation of water from the neutralization of hydrochloric acid and calcium oxide / hydroxide during adsorption, which could lead to excessive water content in the product.
[0026] Furthermore, the third-stage adsorption tower is an adsorption tower equipped with ZSM-5 molecular sieves and / or HZSM-5 molecular sieves. The bulk density of the molecular sieves in the third-stage adsorption tower is 0.6–0.7 kg / L, and the particle size is 2–5 mm.
[0027] Example 1
[0028] The adsorption purification device for a tetramethylsilane mixture includes a vaporizer, a first-stage adsorption tower, a second-stage adsorption tower, a third-stage adsorption tower, and a filter connected in sequence. The first-stage adsorption tower is filled with activated carbon with a bulk density of 0.45 kg / L, the second-stage adsorption tower is filled with calcium oxide with a bulk density of 0.5 kg / L, and the third-stage adsorption tower is filled with ZSM-5 molecular sieve with a bulk density of 0.65 kg / L.
[0029] Example 2
[0030] The adsorption purification device for a tetramethylsilane mixture includes a vaporizer, a first-stage adsorption tower, a second-stage adsorption tower, a third-stage adsorption tower, and a filter connected in sequence. The first-stage adsorption tower is filled with 13X molecular sieve with a bulk density of 0.65 kg / L, the second-stage adsorption tower is filled with calcium hydroxide with a bulk density of 0.5 kg / L, and the third-stage adsorption tower is filled with HZSM-5 molecular sieve with a bulk density of 0.7 kg / L.
[0031] Example 3
[0032] The adsorption purification device for a tetramethylsilane mixture includes a vaporizer, a first-stage adsorption tower, a second-stage adsorption tower, a third-stage adsorption tower, and a filter connected in sequence. The first-stage adsorption tower is filled with 13X molecular sieve with a bulk density of 0.65 kg / L, the second-stage adsorption tower is filled with a mixture of calcium hydroxide and anhydrous calcium chloride with a bulk density of 0.5 kg / L, and the third-stage adsorption tower is filled with ZSM-5 molecular sieve with a bulk density of 0.6 kg / L.
[0033] Example 4
[0034] The adsorption purification device for a tetramethylsilane mixture includes a vaporizer, a first-stage adsorption tower, a second-stage adsorption tower, a third-stage adsorption tower, and a filter connected in sequence. The first-stage adsorption tower is filled with activated carbon with a bulk density of 0.45 kg / L, the second-stage adsorption tower is filled with a mixture of calcium oxide and anhydrous calcium chloride with a bulk density of 0.5 kg / L, and the third-stage adsorption tower is filled with ZSM-5 molecular sieve with a bulk density of 0.65 kg / L.
[0035] Example 5
[0036] The adsorption purification device for a tetramethylsilane mixture includes a vaporizer, a first-stage adsorption tower, a second-stage adsorption tower, a third-stage adsorption tower, and a filter connected in sequence. The first-stage adsorption tower is filled with a mixture of activated carbon and 13X molecular sieve with a bulk density of 0.65 kg / L. The second-stage adsorption tower is filled with a mixture of calcium oxide and anhydrous calcium chloride with a bulk density of 0.5 kg / L. The third-stage adsorption tower is filled with HZSM-5 molecular sieve with a bulk density of 0.65 kg / L.
[0037] Example 6
[0038] The adsorption purification device for a tetramethylsilane mixture includes a vaporizer, a first-stage adsorption tower, a second-stage adsorption tower, a third-stage adsorption tower, and a filter connected in sequence. The first-stage adsorption tower is filled with activated carbon with a bulk density of 0.45 kg / L, the second-stage adsorption tower is filled with a mixture of calcium oxide and anhydrous calcium chloride with a bulk density of 0.5 kg / L, and the third-stage adsorption tower is filled with HZSM-5 molecular sieve with a bulk density of 0.65 kg / L.
[0039] The products obtained after adsorption using the adsorption purification device in Examples 1-6 have a tetramethylsilane content greater than 99.99% and a water content less than 5 ppm, indicating that the adsorption purification device of this invention can effectively remove various impurities from the raw materials and obtain ultrapure tetramethylsilane products.
[0040] It will be apparent to those skilled in the art that this invention is not limited to the details of the exemplary embodiments described above, and that it can be implemented in other specific forms without departing from the spirit or essential characteristics of this invention. Therefore, the embodiments should be considered illustrative and non-limiting in all respects, and the scope of this invention is defined by the appended claims rather than the foregoing description. Thus, it is intended that all variations falling within the meaning and scope of equivalents of the claims be included within this invention. No reference numerals in the claims should be construed as limiting the scope of the claims.
[0041] Furthermore, it should be understood that although this specification describes embodiments, not every embodiment contains only one independent technical solution. This narrative style is merely for clarity. Those skilled in the art should consider the specification as a whole, and the technical solutions in each embodiment can also be appropriately combined to form other embodiments that can be understood by those skilled in the art.
Claims
1. An adsorption purification apparatus for a tetramethylsilane mixture, comprising a vaporizer, characterized in that, Also includes: The first-stage adsorption tower, connected to the vaporizer, is used to remove chlorinated alkane impurities. The first-stage adsorption tower is an adsorption tower equipped with activated carbon and / or 13X molecular sieve; The second-stage adsorption tower is connected to the first-stage adsorption tower and is used to remove hydrochloric acid and low-carbon alkanes. The third-stage adsorption tower, connected to the second-stage adsorption tower, is used to remove isopentane.
2. The adsorption purification apparatus for a tetramethylsilane mixture according to claim 1, characterized in that, The bulk density of the 13X molecular sieve in the first-stage adsorption tower is 0.6–0.7 kg / L.
3. The adsorption purification apparatus for a tetramethylsilane mixture according to claim 1, characterized in that, The bulk density of the activated carbon in the first-stage adsorption tower is 0.45–0.65 kg / L.
4. The adsorption purification apparatus for a tetramethylsilane mixture according to claim 1, characterized in that, The second-stage adsorption tower contains an adsorbent with a bulk density of 0.45–0.55 kg / L.
5. The adsorption purification apparatus for a tetramethylsilane mixture according to claim 4, characterized in that, The adsorbent is calcium oxide and / or calcium hydroxide.
6. The adsorption purification apparatus for a tetramethylsilane mixture according to claim 5, characterized in that, The adsorbent also includes anhydrous calcium chloride.
7. The adsorption purification apparatus for a tetramethylsilane mixture according to claim 4, characterized in that, The particle size of the adsorbent is 2-5 mm.
8. The adsorption purification apparatus for a tetramethylsilane mixture according to claim 1, characterized in that, The third-stage adsorption tower is an adsorption tower equipped with ZSM-5 molecular sieve and / or HZSM-5 molecular sieve.
9. The adsorption purification apparatus for a tetramethylsilane mixture according to claim 8, characterized in that, The bulk density of the molecular sieve in the third-stage adsorption tower is 0.6–0.7 kg / L.
10. The adsorption purification apparatus for a tetramethylsilane mixture according to claim 8, characterized in that, The molecular sieve in the third adsorption tower has a particle size of 2-5 mm.