Industrial acetylene impurity removal device and impurity removal method thereof

Abstract

The invention relates to an industrial acetylene impurity removal device and an impurity removal method thereof.The device is composed of an acetone adsorber, a dehydration dryer and an impurity removal adsorber, the front of the acetone adsorber is connected with a gas inlet pipe, the rear of the acetone adsorber is sequentially connected with the dehydration dryer and the impurity removal adsorber, and the rear of the impurity removal adsorber is connected with a product buffer tank through a precision filter; products are stored in the buffer tank, and a pressure regulator is further installed on the air inlet pipe and used for regulating air inlet pressure. Acetone, water, sulfur, phosphorus, arsenic and other impurities in industrial acetylene in a gas cylinder are removed through the device designed by the invention, acetone can be recycled in a centralized manner, and the impurity removal adsorption column, the acetone adsorption column and the dehydration dryer can be regenerated through nitrogen, so that continuous production and operation of the system are guaranteed.

Description

An industrial acetylene impurity removal device and method thereof Technical Field

[0001] This invention belongs to the field of acetylene production and processing technology, and relates to an industrial acetylene impurity removal device and its impurity removal method. Background Technology

[0002] High-purity acetylene gas is a very important specialty electronic gas. Due to its unique chemical properties (triple bond structure, high reactivity), it has irreplaceable applications in many high-end industrial fields. It is the "blood" and "food" of strategic emerging industries such as semiconductors, new energy, and high-end manufacturing. Its purity directly determines the performance, yield, and reliability of the final product. With the rapid development of these industries, the demand for and quality requirements of high-purity acetylene will become increasingly stringent. High-purity acetylene gas is widely used in the semiconductor, carburizing, and silicon-carbon anode industries. However, high-purity acetylene contains impurities such as sulfur and phosphorus, which can form deep-level traps in semiconductor applications, poisoning catalysts, reducing carrier lifetime, increasing leakage current, reducing device efficiency, disrupting the catalytic process, leading to uncontrollable doping, altering resistivity and doping distribution, causing device parameter drift, and affecting PN junction characteristics. In the carburizing process, it causes surface poisoning of carburized parts, grain boundary embrittlement, insufficient carburizing layer, slow carburizing rate, red network defects, and brittle scrapping of parts. In the application of carbon coating in silicon-carbon anodes, it damages the carbon layer, causing electrochemical hazards, high internal resistance, poor rate performance, rapid capacity decay, short cycle life, gas production, and safety risks.

[0003] Existing patent CN202410769462 discloses an industrial acetylene purification method, which mainly includes: a pressure reducing valve, an acetone removal adsorption tower, a sulfur and phosphorus removal catalytic adsorption tower, a water removal drying adsorption tower, a primary filter, a secondary filter, and a buffer tank. Although this method can purify process acetylene to above 3N5, as the purification device operates, the adsorbent in each adsorption tower gradually becomes saturated, and the quality of the purified acetylene product will gradually decline. Furthermore, the adsorbent needs to be replaced regularly, affecting normal use.

[0004] Therefore, an industrial acetylene impurity removal device and method are designed to overcome the above problems. Summary of the Invention

[0005] The purpose of this invention is to overcome the shortcomings of the existing technology and provide an industrial acetylene impurity removal device and method. The industrial acetylene in the gas cylinder is removed by the device designed by this invention to remove impurities such as acetone, water, sulfur, phosphorus, and arsenic from the gas. The acetone can be centrally recycled. The impurity removal adsorption column, the acetone adsorption column, and the dehydration dryer can be regenerated by nitrogen to ensure the continuous production operation of the system.

[0006] The present invention is achieved through the following technical solution: an industrial acetylene impurity removal device, which consists of an acetone adsorber, a dehydration dryer, and an impurity removal adsorber. The acetone adsorber is connected to an air inlet pipe in front and to the dehydration dryer and the impurity removal adsorber in sequence behind it. The impurity removal adsorber is connected to a product buffer tank through a precision filter to store the product in the buffer tank. A pressure regulator is also installed on the air inlet pipe for adjusting the air inlet pressure.

[0007] Preferably, two acetone adsorbers are installed side by side, each with a pipe at the top connecting to a dehydration dryer at the rear. A regeneration pipe is also installed above each adsorber, connecting to a regeneration gas equipment. A condenser is installed below each adsorber, connecting to an acetone buffer tank. The acetone buffer tank has two pipes: one is a main exhaust pipe, which allows excess gas to flow out, and the other is a storage pipe, which can recover excess acetone gas and sell it after accumulating a certain amount.

[0008] Preferably, two dehydration dryers are also provided, arranged side by side, and connected to the impurity removal adsorber at the rear. An online phosphorus pentoxide moisture meter is installed at the inlet and outlet of the two dehydration dryers. Regeneration pipes and exhaust gas pipes are also installed above and below the dehydration dryers. The regeneration pipes are connected to the regenerators, and the exhaust gas pipes are connected to the exhaust gas main pipe to discharge the exhaust gas.

[0009] Preferably, three impurity removal adsorbers are provided in parallel. The rear of the impurity removal adsorber is connected to a precision filter, and a regeneration pipe and an exhaust gas pipe are provided above and below. The regeneration pipe is connected to the regenerator, and there are two exhaust gas pipes. One is directly connected to the exhaust gas main pipe, and the other is connected to the exhaust gas main pipe through a vacuum pump.

[0010] Preferably, the regenerator is a nitrogen backflushing system, which consists of a nitrogen electric heater and a flow controller. The nitrogen electric heater backflushes the impurity remover, the dehydration dryer, and the acetone adsorber for backflushing regeneration.

[0011] Preferably, the precision filter is connected to the product buffer tank via a pipeline, and a gas chromatograph is installed on the pipeline.

[0012] A method for removing impurities from an industrial acetylene removal device, comprising the following steps: 1) Acetylene is introduced into an acetone adsorber through an inlet pipe. The acetone adsorber contains an acetone adsorption column filled with macroporous resin. Acetone is adsorbed from the acetylene gas by the macroporous resin. One acetone adsorber is used in operation, and one is on standby. The standby acetone adsorber is regenerated by backflushing the adsorption column with hot nitrogen. The acetone generated during backflushing can be condensed in a condenser and recovered into an acetone buffer tank. After accumulating to a certain amount, it is sold externally; 2) After acetone removal, the acetylene gas enters a dehydration dryer. The dryer uses a 3A or 4A molecular sieve. The dehydrated acetylene gas enters the impurity removal adsorption column. One dehydration dryer is used in operation, and one is on standby. The standby dryer is regenerated with high-temperature nitrogen. Phosphorus pentoxide is installed at the inlet and outlet of the dehydration dryer. 3) The dehydrated and dried gas enters the impurity removal adsorber, which is equipped with 3 units: one for adsorption, one for cooling, and one for high-temperature regeneration. The adsorption-regeneration-cooling cycle takes 8 hours each, and a cycle is completed in 24 hours. 4) The acetylene gas after impurity removal adsorption may contain carbon powder from the impurity removal adsorption column. Therefore, 1µm and 0.1µm precision filters are installed in series at the outlet to remove fine solid impurities in the gas. 5) A gas chromatograph is installed at the filter outlet for online detection of impurities in the acetylene gas. If the gas fails the test, the regeneration time of the impurity removal adsorption column is increased. If the gas passes the test, it enters the product buffer tank. The pressure of the product buffer tank is 0.3-0.4Mpa (0.1-0.15Mpa) to stabilize the output of acetylene gas.

[0013] Preferably, the acetone adsorber, dehydrator, and impurity removal adsorber used for standby regeneration in steps 1) to 3) are all connected to the nitrogen backflushing system, using a nitrogen electric heater, and a temperature and flow controller is installed at the outlet. Regeneration is achieved by controlling the temperature and flow through these settings.

[0014] As a preferred method, the three impurity removal adsorbers in step 3) are used as follows: one adsorbs, one cools, and one regenerates at high temperature. Adsorption-regeneration-cooling takes 8 hours each, completing one cycle in 24 hours. After one adsorption cycle ends, the pressure of the impurity adsorption column is reduced to the same level as the pressure in the exhaust gas pipeline. Then, room temperature nitrogen is used to pressurize and depressurize the adsorption column from the top more than 6 times, until the pressure reaches 0.2 MPa (0.1 MPa). After that, the vacuum pump is turned on, and the pressurization and depressurization are continued for 4-5 times. After multiple nitrogen pressurization and depressurization cycles, the adsorption column begins high-temperature nitrogen regeneration. During regeneration, the temperature of the impurity removal adsorption column is controlled at 100-120℃. After regeneration, the adsorption column is cooled by passing cold nitrogen from the top until it reaches below 30℃, after which it is ready for normal standby.

[0015] The beneficial effects of this invention are as follows: 1) This invention, through a three-stage series treatment of an acetone adsorber, a dehydration dryer, and a purification adsorber, can systematically remove acetone, moisture, carbon powder, and trace impurities from acetylene, significantly improving product purity. The combination of a precision filter and an online gas chromatograph ensures that the acetylene impurity content at the outlet is below the detection limit, meeting the requirements of high-purity industrial applications.

[0016] 2) This invention can condense the regenerated backflushing acetone into a buffer tank, realizing the resource recovery of acetone, reducing raw material waste and environmental pollution; the exhaust gas main pipe collects and treats the regenerated exhaust gas in a unified manner, and uses a vacuum pump for negative pressure suction to avoid the emission of harmful gases, which meets the requirements of green production.

[0017] 3) This invention uses a nitrogen electric heater and flow controller to implement precise temperature-flow control regeneration of the acetone adsorber, dehydration dryer, and impurity removal adsorber. Through the dynamic circulation of the three impurity removal adsorbers, the service life of the adsorbent is extended and the stability of continuous equipment operation is improved.

[0018] 4) The inlet pipe pressure regulator enables precise control of the inlet pressure, which, together with the product buffer tank pressure stabilization system, ensures a constant acetylene output pressure; the phosphorus pentoxide online moisture analyzer monitors the moisture content at the inlet and outlet of the dehydrator in real time and dynamically adjusts the regeneration strategy; the gas chromatograph automatically extends the regeneration time when the online detection fails, forming a closed-loop quality control system that significantly improves operational safety and product consistency.

[0019] In summary, the device of the present invention, through integrated design of structural innovation, regeneration optimization, online monitoring and resource recovery, achieves multi-dimensional improvements in acetylene purification efficiency, resource utilization, operational stability and environmental performance, and has significant technical and economic advantages and promotion and application value. Attached Figure Description

[0020] Figure 1 is a schematic diagram of the overall structure of the present invention. Detailed Implementation

[0021] To enable those skilled in the art to more clearly understand the purpose, technical solution, and advantages of the present invention, the present invention will be further described below in conjunction with the accompanying drawings and embodiments.

[0022] In the description of this invention, it should be understood that the orientation or positional relationship indicated by terms such as "upper", "lower", "left", "right", "inner", "outer", "lateral", and "vertical" is based on the orientation or positional relationship shown in the accompanying drawings and is only for the convenience of describing this invention, and is not intended to indicate or imply that the device or component referred to must have a specific orientation, and therefore should not be construed as a limitation of this invention.

[0023] The invention will now be described in detail with reference to the accompanying drawings: As shown in Figure 1, an industrial acetylene impurity removal device is provided. The device consists of an acetone adsorber 1, a dehydration dryer 2, and an impurity removal adsorber 3. The acetone adsorber 1 is connected to an air inlet pipe 4 at the front and to the dehydration dryer 2 and the impurity removal adsorber 3 at the rear in sequence. The impurity removal adsorber 3 is connected to a product buffer tank 6 via a precision filter 5 to store the product in the buffer tank. A pressure regulator 7 is also installed on the air inlet pipe 4 for adjusting the air inlet pressure.

[0024] Two acetone adsorbers 1 are arranged side by side. Each adsorber has a pipe at the top that connects to the dehydration dryer 2 at the rear. A regeneration pipe 8 is also provided above each adsorber, which is connected to the regeneration gas equipment 9. A condenser 10 is provided below each adsorber, which is connected to the acetone buffer tank 11. The acetone buffer tank 11 has two pipes: one is a main exhaust pipe 12, which can discharge excess gas, and the other is a storage pipe 13, which can recover excess acetone gas and sell it after accumulating a certain amount.

[0025] Two dehydration dryers 2 are also provided, arranged side by side, and connected to the impurity removal adsorber 3 at the rear. The inlet and outlet of the two dehydration dryers 2 are equipped with online phosphorus pentoxide moisture meters 15. Regeneration pipes 8 and exhaust gas pipes 16 are also installed above and below the dehydration dryers 2. The regeneration pipes 8 are connected to the regenerator 9, and the exhaust gas pipes 16 are connected to the exhaust gas main pipe 12 to discharge the exhaust gas.

[0026] Three impurity removal adsorbers 3 are arranged in parallel. The rear of each impurity removal adsorber 3 is connected to the precision filter 5. Above and below, there are regeneration pipes 8 and exhaust gas pipes 14. The regeneration pipes 8 are connected to the regenerator 9. There are two exhaust gas pipes 14. One is directly connected to the exhaust gas main pipe 12, and the other is connected to the exhaust gas main pipe 12 through the vacuum pump 17.

[0027] The regenerator 9 is a nitrogen backflushing system, which consists of a nitrogen electric heater 18 and a flow controller 19. The nitrogen electric heater 18 backflushes to the impurity removal adsorber 3, the dehydration dryer 2, and the acetone adsorber 1 for backflushing regeneration.

[0028] The precision filter 5 is connected to the product buffer tank 6 via a pipe, and a gas chromatograph 20 is installed on the pipe.

[0029] A method for removing impurities from an industrial acetylene removal device, comprising the following steps: 1) Acetylene is introduced into an acetone adsorber 1 through an inlet pipe 4. The acetone adsorber 1 contains an acetone adsorption column 21 filled with macroporous resin. Acetone is adsorbed from the acetylene gas by the macroporous resin. One acetone adsorber 1 is used in operation, and the backup acetone adsorber 1 is regenerated by backflushing the adsorption column 21 with hot nitrogen. The regenerated backflushed acetone can be condensed by a condenser 10 and recovered into an acetone buffer tank 1, where it is accumulated to a certain amount before being sold. 2) After acetone removal, the acetylene gas enters a dehydration dryer 2, which uses a 3A or 4A molecular sieve. The dehydrated acetylene gas enters a removal adsorption column 22. The dehydration dryer 2 is used in operation, and the backup dryer is regenerated with high-temperature nitrogen. Pentoxide is installed at the inlet and outlet of the dehydration dryer 2. 15) The dehydrated and dried gas enters the impurity removal adsorber 3. There are 3 adsorbers 3, one for adsorption, one for cooling, and one for high-temperature regeneration. The adsorption-regeneration-cooling cycle takes 8 hours each, and a cycle is completed in 24 hours. 2) The acetylene gas after impurity removal adsorption may contain carbon powder from the impurity removal adsorption column 22. Therefore, a 1μm and 0.1μm precision filter 5 is installed in series at the outlet to remove fine solid impurities in the gas. 3) A gas chromatograph 20 is installed at the filter outlet for online detection to detect impurities in the acetylene gas. If the gas fails the test, the regeneration time of the impurity removal adsorption column 22 is increased. If the gas passes the test, it enters the product buffer tank 6. The pressure of the product buffer tank 6 is 0.3-0.4Mpa (0.1-0.15Mpa) to stabilize the output of acetylene gas.

[0030] In steps 1) to 3), the standby acetone adsorber 1, dehydrator 2, and impurity removal adsorber 3 are all connected to the nitrogen backflushing system, using a nitrogen electric heater 18, and a temperature and flow controller 19 is set at the outlet. Regeneration is achieved by controlling the temperature and flow through these settings.

[0031] The three impurity removal adsorbers 3 in step 3) are used as follows: one adsorbs, one cools down, and one regenerates at high temperature. Adsorption-regeneration-cooling takes 8 hours each, and a cycle is completed in 24 hours. After one adsorption cycle is completed, the pressure of the impurity adsorption column is reduced to the same level as the pressure of the exhaust gas pipeline 14. Then, room temperature nitrogen is used to pressurize and depressurize the column from the top of the adsorption column more than 6 times, and the pressure is increased to 0.2 MPa (0.1 MPa). Then, the vacuum pump 17 is turned on and pressurization and depressurization are continued for 4-5 times. After the adsorption column has been pressurized and depressurized multiple times, the adsorption column begins high-temperature nitrogen regeneration. During regeneration, the temperature of the impurity removal adsorption column 22 is controlled at 100-120℃. After regeneration, the adsorption column is cooled by passing cold nitrogen from the top. After cooling down to below 30℃, it is ready for normal standby.

[0032] The device of this invention removes impurities such as acetone, water, sulfur, phosphorus, and arsenic from industrial acetylene in gas cylinders. Acetone can be centrally recycled. The impurity removal adsorption column, acetone adsorption column, and dehydration dryer can be regenerated with nitrogen, ensuring continuous production operation of the system. The acetylene produced by this invention can achieve a purity of over 3N, and the total amount of metallic impurities such as sulfur, phosphorus, and arsenic in the acetylene is reduced to below 3 ppm, with continuous operation time reaching several years.

[0033] The device of this invention achieves multi-dimensional improvements in acetylene purification efficiency, resource utilization, operational stability, and environmental performance through integrated design of structural innovation, regeneration optimization, online monitoring, and resource recovery. It has significant technical and economic advantages and application value.

[0034] The specific embodiments described herein are merely illustrative of the principles and effects of the invention and are not intended to limit the invention. Any person skilled in the art can modify or alter the above embodiments without departing from the spirit and scope of the invention. Therefore, all equivalent modifications or alterations made by those skilled in the art without departing from the spirit and technical concept disclosed in this invention should still be covered by the claims of this invention.

Claims

1. An industrial acetylene impurity removal device, comprising an acetone adsorber, a dehydration dryer, and an impurity removal adsorber, characterized in that: The acetone adsorber is connected to an air inlet pipe at the front and to a dehydrator and a purification adsorber in sequence at the rear. The purification adsorber is connected to a product buffer tank via a precision filter to store the product in the buffer tank. A pressure regulator is also installed on the air inlet pipe for adjusting the air inlet pressure.

2. The industrial acetylene impurity removal device according to claim 1, characterized in that: Two acetone adsorbers are installed side by side. Each adsorber has a pipe at the top that connects to the dehydration dryer at the rear. A regeneration pipe is also installed above each adsorber, which connects to the regeneration gas equipment. A condenser is installed below each adsorber, which connects to the acetone buffer tank. The acetone buffer tank has two pipes: one is a main exhaust pipe, which allows excess gas to flow out, and the other is a storage pipe, which can recover excess acetone gas and sell it after accumulating a certain amount.

3. The industrial acetylene impurity removal device according to claim 2, characterized in that: Two dehydration dryers are also provided, arranged side by side, and connected to the impurity removal adsorber at the rear. An online phosphorus pentoxide moisture meter is installed at the inlet and outlet of the two dehydration dryers. Regeneration pipes and exhaust gas pipes are also installed above and below the dehydration dryers. The regeneration pipes are connected to the regenerators, and the exhaust gas pipes are connected to the exhaust gas main pipe to discharge the exhaust gas.

4. The industrial acetylene impurity removal device according to claim 3, characterized in that: Three impurity removal adsorbers are arranged in parallel. The rear of each adsorber is connected to a precision filter, and the top and bottom are provided with regeneration pipes and exhaust gas pipes. The regeneration pipes are connected to the regenerators, and there are two exhaust gas pipes. One is directly connected to the exhaust gas main pipe, and the other is connected to the exhaust gas main pipe through a vacuum pump.

5. The industrial acetylene impurity removal device according to claim 4, characterized in that: The regenerator is a nitrogen backflushing system, which consists of a nitrogen electric heater and a flow controller. The nitrogen electric heater backflushes the impurity remover, the dehydration dryer, and the acetone adsorber for backflushing regeneration.

6. The industrial acetylene impurity removal device according to claim 4, characterized in that: The precision filter is connected to the product buffer tank via a pipeline, and a gas chromatograph is installed on the pipeline.

7. The method for removing impurities from the industrial acetylene removal device according to any one of claims 1-6, characterized in that, The method includes the following steps: 1) Acetylene is introduced into the acetone adsorber through the inlet pipe. The acetone adsorber is equipped with an acetone adsorption column filled with macroporous resin. Acetone is adsorbed from the acetylene gas by the macroporous resin. One acetone adsorber is used and one is on standby. The standby acetone adsorber is regenerated by backflushing the adsorption column with hot nitrogen. The acetone generated by backflushing can be condensed by a condenser and recycled into an acetone buffer tank. After accumulating to a certain amount, it is sold externally; 2) After acetone is removed from the acetylene gas, the gas enters a dehydration dryer. The dryer uses 3A or 4A molecular sieves. The dehydrated acetylene gas enters the impurity removal adsorption column. One dehydration dryer is used and one is on standby. The standby dryer is regenerated by high-temperature nitrogen. An online phosphorus pentoxide moisture meter is installed at the inlet and outlet of the dehydration dryer; 3) Dehydration After being dried by water, the gas enters the impurity removal adsorber, which has three units: one for adsorption, one for cooling, and one for high-temperature regeneration. The adsorption-regeneration-cooling cycle takes 8 hours each, completing one cycle in 24 hours. 4) The acetylene gas after impurity removal adsorption may contain carbon powder from the adsorption column. Therefore, 1µm and 0.1µm precision filters are installed in series at the outlet to remove fine solid impurities from the gas. 5) A gas chromatograph is installed at the filter outlet for online detection of impurities in the acetylene gas. If the gas fails the test, the regeneration time of the adsorption column is increased. If the gas passes the test, it enters the product buffer tank. The pressure of the product buffer tank is 0.3-0.4 MPa (0.1-0.15 MPa) to stabilize the output of acetylene gas.

8. The method for removing impurities from the industrial acetylene removal device according to claim 7, characterized in that: In steps 1) to 3), the standby acetone adsorber, dehydrator, and impurity removal adsorber for regeneration are all connected to the nitrogen backflushing system. A nitrogen electric heater is used, and a temperature and flow controller is installed at the outlet. Regeneration is achieved by controlling the temperature and flow through the settings.

9. The method for removing impurities from the industrial acetylene removal device according to claim 7, characterized in that: The usage method of the three impurity removal adsorbers in step 3) is as follows: one adsorbs, one cools down, and one performs high-temperature regeneration. Adsorption-regeneration-cooling takes 8 hours each, and a cycle is completed in 24 hours. After one adsorption cycle is completed, the pressure of the impurity adsorption column is reduced to the same level as the pressure of the exhaust gas pipeline. Then, room temperature nitrogen is used to pressurize and depressurize the adsorption column from the top more than 6 times, and the pressure is increased to 0.2 MPa (0.1 MPa). After that, the vacuum pump is turned on, and the pressurization and depressurization are continued for 4-5 times. After the adsorption column has been pressurized and depressurized multiple times, the adsorption column begins high-temperature nitrogen regeneration. During regeneration, the temperature of the impurity removal adsorption column is controlled at 100-120℃. After the regeneration is completed, the adsorption column is cooled down by passing cold nitrogen from the top. After the temperature drops below 30℃, it is ready for normal standby.

Images