A tetramethylsilane production device

Abstract

The utility model discloses a tetramethylsilane production device, including dechlorination reation kettle, purification column, cooler and receiving tank, the dechlorination reation kettle top is equipped with the entrance and the export, and the export is connected purification column, and the purification column top export is connected cooler, and the cooler export is connected respectively purification column top entrance and receiving tank entrance, and receiving tank obtains the tetramethylsilane product after purification, the dechlorination reation kettle outer wall is equipped with the outer coil of jacket, and the outer coil can pass into cooling medium and realize the cooling of dechlorination reation kettle, and the jacket can pass into heating and carry out the temperature rise heat preservation to dechlorination reation kettle. The reation kettle can realize two kinds of functions of dechlorination reaction and distillation purification simultaneously, greatly simplifies equipment floor space and cost, improves the utilization of device, and obtains electronic grade high purity tetramethylsilane.

Description

Technical Field

[0001] This utility model relates to the field of tetramethylsilane production technology, and specifically to a tetramethylsilane production apparatus. Background Technology

[0002] Tetramethylsilane, a widely used organosilicon compound, possesses excellent surface activity and can form a dense silicon-based compound coating on the surface of various materials, thereby improving the material's adhesion, anti-aging properties, and chemical resistance. In particular, ultra-high purity (mass fraction greater than 99.99%) tetramethylsilane also shows great promise for applications in the semiconductor field.

[0003] CN119113552A discloses a purification apparatus and method for tetramethylsilane. The purification apparatus includes a feed tank for containing tetramethylsilane. A light-boiling point removal distillation column is connected to the feed tank and is used to receive the tetramethylsilane and remove low-boiling point impurities. A first heavy-boiling point removal distillation column is connected to the light-boiling point removal distillation column and is used to remove high-boiling point impurities from the tetramethylsilane. A first vaporizer is connected to the first heavy-boiling point removal distillation column and is used to vaporize the tetramethylsilane. A first adsorption unit is connected to the first vaporizer and is used to adsorb impurities with boiling points close to those of tetramethylsilane. A second heavy-boiling point removal distillation column is connected to the first adsorption unit and is used to receive the tetramethylsilane adsorbed by the first adsorption unit and remove high-boiling point impurities. A second vaporizer is connected to the second heavy-boiling point removal distillation column and is used to vaporize the tetramethylsilane. A second adsorption unit is connected to the second vaporizer and is used to adsorb impurities with boiling points close to those of tetramethylsilane. This purification apparatus and method offer good purification efficiency and low purification cost.

[0004] CN220801979U discloses a continuous production apparatus for high-purity tetramethylsilane, comprising: a raw material storage tank with an inlet and an outlet; a heavy-duty distillation column with its inlet connected to the outlet of the raw material storage tank; a light-duty distillation column with its inlet connected to the outlet of the heavy-duty distillation column via a top condenser; an adsorption system filled with a metal-organic framework material (ZIF78) and zeolite molecular sieve (13X) as adsorbents, the outlet of the light-duty distillation column being connected to a vaporizer, the material being vaporized by the vaporizer and entering the adsorption unit to adsorb and remove residual impurities after distillation and purification; and a condenser with its inlet connected to the outlet of the adsorption system and its outlet connected to the finished product storage tank. This apparatus offers advantages such as low production cost, continuous operation, and high purification efficiency.

[0005] Tetramethylsilane obtained by using chloromethane and silicon powder in a fluidized bed reactor contains a large number of impurities and byproducts. The purification equipment for tetramethylsilane also needs to improve its utilization rate, reduce costs, and obtain a high-purity product. Utility Model Content

[0006] This invention addresses the issue of incomplete removal of chlorine impurities from tetramethylsilane by providing a high-purity tetramethylsilane production apparatus. The reactor can simultaneously perform both dechlorination and distillation purification functions, greatly simplifying the equipment footprint and reducing costs, improving equipment utilization, and yielding electronic-grade high-purity tetramethylsilane.

[0007] To achieve the above objectives, the technical solution adopted by this utility model is as follows: A tetramethylsilane production apparatus includes a dechlorination reactor, a purification column, a cooler, and a receiving tank; The dechlorination reactor is equipped with an inlet and an outlet at the top. The outlet is connected to a purification column. The outlet at the top of the purification column is connected to a cooler. The outlet of the cooler is connected to the inlet at the top of the purification column and the inlet of the receiving tank, respectively. The receiving tank receives the purified tetramethylsilane product. The outer wall of the dechlorination reactor is equipped with a jacketed outer coil. The outer coil can be circulated with a cooling medium to cool down the dechlorination reactor; the jacket can be circulated with a heating medium to heat up and maintain the temperature of the dechlorination reactor.

[0008] This invention employs a dechlorination reactor with an outer coil containing a jacket. In the initial stage of production, tetramethylsilane and water enter the reactor. On the one hand, the reaction of chlorine-containing byproducts and impurities with water is an exothermic reaction. Introducing a cooling medium into the outer coil to lower the temperature is more conducive to the dechlorination reaction. On the other hand, it also prevents some impurities from overflowing directly from the top of the reactor, thereby improving the completion and effectiveness of the dechlorination reaction.

[0009] After the dechlorination reaction is complete, the reactor is heated by a jacket to evaporate the product. The product is then purified by a purification column and enters a receiving tank to obtain the purified tetramethylsilane product. A cooler is also connected to the top of the purification column to cool and reflux the distillate, improving the purification effect.

[0010] The dechlorination reactor of this invention can be used for both the dechlorination reaction stage and the product evaporation stage, making it a dual-purpose reactor that effectively improves equipment utilization and reduces production costs and floor space.

[0011] Preferably, the dechlorination reactor is equipped with a thermometer, a stirrer, a level gauge, and an inlet pipe, a nitrogen pipe, and a vent pipe.

[0012] The receiving tank is a conical tank. It can effectively achieve oil-water separation. Conventional flat-bottomed tanks or headed-bottomed tanks have a large bottom space, and the oil phase tetramethylsilane will be discharged along with it when draining. After setting it into a conical tank, the bottom space gets smaller as you go down, and the water settles at the bottom. Only the water phase is discharged and the oil phase is not discharged, so there is no loss of the oil phase.

[0013] The receiving tank is equipped with stainless steel packing material, which can further separate the product oil and water, reduce the water content and other impurities in tetramethylsilane, and improve the purity of the product.

[0014] Preferably, the purification column is packed with stainless steel Sierra ring packing.

[0015] The receiving tank is equipped with a water removal device, preferably composed of CY700 stainless steel wire mesh packing and supporting components. The oil phase received into the cooler will contain trace amounts of water. The oil phase enters from the bottom side of the receiving tank. When it passes through the water removal device, some of the water phase in the oil phase is physically broken down, causing the two phases to separate. The water phase is at the bottom, and the oil phase leaves from the upper side of the receiving tank, achieving the effect of oil-water separation.

[0016] The cooling medium includes water or an aqueous solution of ethylene glycol.

[0017] The heating medium includes saturated steam or heat transfer oil.

[0018] Compared with the prior art, the present invention has the following beneficial effects: This invention employs a reaction vessel with a jacketed external coil to achieve dual-purpose operation, effectively improving equipment utilization, reducing production costs and floor space, and controlling the tetramethylsilicic acid value to below 1 ppm, resulting in high efficiency and low cost. Attached Figure Description

[0019] Figure 1 This is a schematic diagram of the tetramethylsilane production apparatus of this utility model.

[0020] Figure 2 This is a schematic diagram of the receiving tank in this utility model. Detailed Implementation

[0021] To make the objectives, technical solutions, and advantages of this utility model clearer, the following detailed description is provided in conjunction with embodiments. It should be understood that the specific embodiments described herein are merely illustrative and not intended to limit the scope of this utility model. Modifications or equivalent substitutions made by those skilled in the art based on their understanding of the technical solutions of this utility model, without departing from the spirit and scope of the technical solutions of this utility model, should all be covered within the protection scope of this utility model.

[0022] Example 1 like Figure 1 and Figure 2 As shown, a tetramethylsilane production apparatus includes a dechlorination reactor R01, a purification column S01, a cooler E01, and a receiving tank V01. The dechlorination reactor R01 has an inlet and an outlet at the top. The outlet is connected to the purification column S01. The outlet at the top of the purification column is connected to the cooler E01. The outlet of the cooler E01 is connected to the inlet at the top of the purification column S01 and the inlet of the receiving tank V01. The receiving tank V01 receives the purified tetramethylsilane product. The outer wall of the dechlorination reactor R01 is equipped with an outer coil 1 with a jacket 2. The outer coil 1 can be circulated with a cooling medium to cool down the dechlorination reactor R01; the jacket 2 can be circulated with a heating medium to raise and maintain the temperature of the dechlorination reactor. The dechlorination reactor R01 is equipped with a thermometer 3, a stirrer 4, and a level gauge 5. At the inlet, there is a nitrogen pipe 8, a vent pipe 9, and feed pipes 6 and 7. Tetramethylsilane crude product and water are added to feed pipes 6 and 7, respectively.

[0023] The purification column is filled with 20 kg of stainless steel Sittall ring packing, with a specification of 12 mm * 12 mm. The receiving tank V01 is a conical tank and a dehydration device, which is equipped with CY700 stainless steel wire mesh packing to dehydrate the product delivered from the cooler E01, thereby reducing the water content of the tetramethylsilane product.

[0024] 250 kg of deionized water was added to the dechlorination reactor R01 in one go, along with a 45% ethylene glycol aqueous solution as the cooling medium. The temperature of the dechlorination reactor R01 was slowly reduced to 5°C. 200 kg of crude tetramethylsilane with a purity of 70%–75% was then slowly introduced into the reactor over 3–5 hours, with the internal temperature controlled at 5–20°C via an external coil. After the crude tetramethylsilane was introduced, the reactor was stirred and the dechlorination reaction was carried out for 8 hours. After the reaction, the reactor was washed with water, adding 300 kg of deionized water each time, stirring for 2 hours, letting stand for 2 hours, and then draining the water. This process was repeated until the oil phase acid value was less than 1 ppm. Steam at 0.3 MPa was introduced into the jacket to raise the reactor temperature to 28.4°C, and the tetramethylsilane was evaporated and purified. The product was purified by a purification column, cooler, and receiving tank to obtain chlorine-free tetramethylsilane with a purity of 85%–88% and an acid value less than 1 ppm.

Claims

1. A tetramethylsilane production apparatus, characterized in that, Includes a dechlorination reactor, purification column, cooler, and receiving tank; The dechlorination reactor is equipped with an inlet and an outlet at the top. The outlet is connected to a purification column. The outlet at the top of the purification column is connected to a cooler. The outlet of the cooler is connected to the inlet at the top of the purification column and the inlet of the receiving tank, respectively. The receiving tank receives the purified tetramethylsilane product. The outer wall of the dechlorination reactor is equipped with a jacketed outer coil. The outer coil can be circulated with a cooling medium to cool down the dechlorination reactor; the jacket can be circulated with a heating medium to heat up and maintain the temperature of the dechlorination reactor.

2. The tetramethylsilane production apparatus according to claim 1, characterized in that, The dechlorination reactor is equipped with a thermometer, a stirrer, and a level gauge. The inlet is equipped with a feed pipe, a nitrogen pipe, and a vent pipe.

3. The tetramethylsilane production apparatus according to claim 1, characterized in that, The receiving container is a conical container.

4. The tetramethylsilane production apparatus according to claim 1, characterized in that, The receiving tank is equipped with stainless steel packing material.

5. The tetramethylsilane production apparatus according to claim 1, characterized in that, The purification column is filled with stainless steel Sierra ring packing.

6. The tetramethylsilane production apparatus according to claim 1, characterized in that, The receiving tank is equipped with a water removal device.

7. The tetramethylsilane production apparatus according to claim 1, characterized in that, The cooling medium includes water or an aqueous solution of ethylene glycol.

8. The tetramethylsilane production apparatus according to claim 1, characterized in that, The heating medium includes saturated steam or heat transfer oil.

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