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CN-116586016-B - Trimethyl aluminum purifying device and process

CN116586016BCN 116586016 BCN116586016 BCN 116586016BCN-116586016-B

Abstract

The invention is suitable for the technical field of metal source organic synthesis, and provides a trimethyl aluminum purification device and a process, wherein the trimethyl aluminum purification device comprises a reaction device, a reflux device and a decompression rectification device, the decompression rectification device is connected with a flow dividing device through a pipeline connecting piece, the flow dividing device comprises a rotary drum, a rotary component is connected to the side wall of the rotary drum, a main flow pipe is arranged in the rotary drum, one end of the main flow pipe is connected with the decompression rectification device through a steering pipe, the other end of the main flow pipe is in positioning butt joint with the flow dividing component through a positioning component, pure trimethyl aluminum can be obtained through adding high-purity triethyl aluminum into a trimethyl aluminum crude product containing dimethyl aluminum chloride after reaction, the purification of the trimethyl aluminum crude product is realized, and in the process of rectifying the trimethyl aluminum after reaction, the purity of the trimethyl aluminum can be further ensured through separating liquid obtained in the temperature rising process from liquid in a temperature stable state through the flow dividing device.

Inventors

  • JIANG YONGYAO
  • WANG WEI
  • ZHOU MINGQI
  • ZHU SHUJIAO

Assignees

  • 安徽亚格盛电子新材料有限公司
  • 全椒亚格泰电子新材料科技有限公司

Dates

Publication Date
20260508
Application Date
20230523

Claims (7)

  1. 1. The trimethyl aluminum purifying device comprises a reaction device (1), a reflux device (2) and a decompression rectifying device (3), wherein the reaction device (1) is respectively connected with the reflux device (2) and the decompression rectifying device (3) through pipeline connectors, and is characterized in that the decompression rectifying device (3) is connected with a flow dividing device (4) through the pipeline connectors, the flow dividing device (4) comprises a rotary drum (42), a rotary assembly (41) is connected to the side wall of the rotary drum (42), a main flow pipe (43) is arranged in the rotary drum (42), one end of the main flow pipe (43) is connected with the decompression rectifying device (3) through a steering pipe (10), and the other end of the main flow pipe (43) is in positioning butt joint with a flow dividing assembly (45) through a positioning assembly (46); The flow distribution assembly (45) comprises a flow distribution cylinder (451), a plurality of holes are formed in the flow distribution cylinder (451), the holes are uniformly formed on the flow distribution cylinder (451) around the axial lead of the flow distribution cylinder (451), and the rotary cylinder (42) is rotated to enable the main flow pipe (43) to be in butt joint with pipelines arranged in different holes on the flow distribution cylinder (451) through the positioning assembly (46) so as to realize flow distribution of rectified liquid; The device comprises a connecting pipe (9), a rotating cylinder (42), a positioning assembly (46) and two positioning balls (462), wherein the inlet end of the steering pipe (10) is connected with the connecting pipe (9), the connecting pipe (9) is connected with a decompression rectifying device (3), the axis of the connecting pipe (9), the axis of the inlet end of the steering pipe (10) and the axis of the rotating cylinder (42) are overlapped, the axis of the outlet end of the steering pipe (10) and the axis of the main flow pipe (43) are overlapped, the positioning ring (461) is fixedly sleeved on the side wall of the main flow pipe (43) opposite to the splitting cylinder (451), and the end face of the positioning ring (461) is rotatably provided with the two positioning balls (462).
  2. 2. The trimethylaluminum purification device as recited in claim 1, wherein the rotary assembly (41) comprises a rotary motor (411), a rotary rod (412) is connected to an output shaft end of the rotary motor (411), a driving wheel (413) is sleeved on a side wall of the rotary rod (412), and the driving wheel (413) is connected with the rotary cylinder (42) through a driven wheel (414).
  3. 3. The trimethylaluminum purification apparatus as recited in claim 1 wherein said rotary drum (42) and said split drum (451) are connected by a seal assembly (44), said seal assembly (44) comprises a fixing ring (441), said fixing ring (441) is fixedly sleeved on a side wall of said split drum (451), a connecting ring (442) is fixedly connected to an end face of said fixing ring (441), and said rotary drum (42) is inserted in said connecting ring (442); sealing cotton (443) is adhered to the inner wall of the connecting ring (442), the space between the inner wall of the connecting ring (442) and the outer wall of the rotary cylinder (42) is filled and sealed by the sealing cotton (443), and an air inlet (444) and an air outlet (445) are respectively arranged on the side wall of the connecting ring (442).
  4. 4. The trimethylaluminum purification apparatus as recited in claim 1, wherein an outer ring groove (456) and an inner ring groove (457) are respectively provided at the end face of the split-flow cylinder (451), the outer ring groove (456) and the inner ring groove (457) are respectively positioned at the outer side and the inner side of the hole, liquid leakage holes (458) are provided in the outer ring groove (456) and the inner ring groove (457), and liquid leakage pipes (459) are provided in the liquid leakage holes (458).
  5. 5. A trimethylaluminum purification apparatus as defined in claim 4 wherein two of said positioning balls (462) correspond to said outer annular groove (456) and said inner annular groove (457), respectively.
  6. 6. A trimethylaluminum purification apparatus as defined in claim 3, wherein said reaction apparatus (1), said reflux apparatus (2), said vacuum rectification apparatus (3) and said seal assembly (44) are each connected to an inert gas tank (5) and an exhaust gas recovery tank (6) via piping connection.
  7. 7. A process employing a trimethylaluminum purification apparatus as claimed in any one of claims 1 to 6, wherein the process comprises the steps of: A. Adding a crude trimethylaluminum product containing oxygen, chlorine and other impurities into a reaction device under the protection of inert gas, sampling and detecting, then opening a reflux device, and starting stirring; B. slowly dripping high-purity triethylaluminum into the reaction device, slowly heating to 90-130 ℃ after the dripping is finished, and stirring for 3-6 hours; C. after the stirring reaction is finished, the reflux device is closed, the decompression rectifying device is opened, and decompression rectifying is started; D. In the process of vacuum distillation, the liquid obtained by vacuum distillation is split by a split component to obtain a front fraction, a middle fraction and a rear fraction respectively; E. and D, sampling and detecting the middle distillate obtained in the step D.

Description

Trimethyl aluminum purifying device and process Technical Field The invention belongs to the technical field of metal source organic synthesis, and particularly relates to a trimethyl aluminum purification device and process. Background MO source is high-purity metal organic compound, and is the support material for growing semiconductor microstructure material by advanced Metal Organic Chemical Vapor Deposition (MOCVD), metal Organic Molecular Beam Epitaxy (MOMBE) and other techniques. Because the MO source products are required to have extremely high purity, most of MO source compounds are extremely sensitive to oxygen and water, spontaneous combustion can occur when the MO source compounds are exposed to air, and explosion can occur when the MO source products are exposed to water, the development of the MO source is a high and new technology integrating the synthesis and preparation, ultrapure purification, ultrapure analysis and ultrapure filling under extreme conditions. High purity trimethylaluminum is one of the main MO source species and is widely used in solar energy, organic Al sources of full-color LEDs, third generation semiconductors and radio frequency integrated circuit high-K materials. The performance of the deposited layer of the semiconductor material has a great relation with the purity of trimethylaluminum, namely, the performance of the trimethylaluminum is influenced by a very small amount of impurities, the main impurities of the trimethylaluminum are organic silicon, organic oxygen and organic chlorine which are introduced in the synthesis stage, the service performance of the trimethylaluminum is seriously influenced, and the chlorine impurities are dimethyl aluminum chloride (Me 2 AlCl) and the boiling point of the trimethylaluminum are the same, so that the conventional rectification cannot remove the chlorine impurities, and the development of the process for preparing the high-purity trimethylaluminum with high efficiency and simplicity is particularly important. The invention discloses a high-purity trimethylaluminum preparation device and a use method thereof, wherein the high-purity trimethylaluminum preparation device comprises four systems, namely a sodium reduction purification system, a physical chromatography filtering device, a rectification purification system and a photocatalysis tail gas absorption tank, wherein the sodium reduction purification system comprises a purification kettle and an oil bath tank, the rectification purification system comprises a final distillation kettle and a primary distillation kettle, the physical chromatography filtering device comprises an upper layer formed by active carbon with the particle size of 1-2 mu m, a middle layer formed by austenitic stainless steel particles with the particle size of 0.5-0.8 mu m, and a three-layer chromatography device formed by alumina powder with the particle size of 0.1-0.2 mu m, and treatment liquid in the photocatalysis tail gas absorption tank is mixed with hydrogen dioxide and titanium dioxide according to the mass ratio of 200:1-2 and is turbid liquid which is uniformly stirred. The product prepared by the invention has high purity, good stability, controllable and easy process and clean and complete tail gas treatment. However, the above patent still has some disadvantages: In addition, in the process of rectifying and purifying by a rectifying and purifying system, the chromatographic purification trimethylaluminum obtained in the step S3 and ① is required to be sequentially put into a primary rectifying still and a final rectifying still under the protection of nitrogen, wherein the distillation temperature of the primary rectifying still is set to 132-137 ℃, and the distillation temperature of the final rectifying still is set to 118-123 ℃, and because of the gradual temperature rising process in the distillation process, the distilled product obtained in the temperature rising stage and the distilled product obtained in the temperature constant stage are required to be separated, otherwise, the purity of the finally obtained trimethylaluminum is reduced. Disclosure of Invention The invention provides a trimethylaluminum purification device and process, which aims to solve the defects and the defects of the prior art in the background art, and the trimethylaluminum purified by the device and the process has high purity, high yield and simple operation. The invention discloses a trimethylaluminum purification device, which comprises a reaction device, a reflux device and a reduced pressure rectification device, wherein the reaction device is respectively connected with the reflux device and the reduced pressure rectification device through pipeline connectors, the reduced pressure rectification device is connected with a flow dividing device through pipeline connectors, the flow dividing device comprises a rotary drum, the side wall of the rotary drum is connected with a rotary assembly, a ma