Device for purifying hydrogen sulfide gas

Abstract

The utility model relates to a device for purifying hydrogen sulfide gas. The device comprises a first adsorption tower, a second adsorption tower and a low-temperature storage tank which are sequentially communicated, a first adsorption tower feed port is formed in the bottom of the first adsorption tower, and a first adsorption tower discharge port is formed in the top of the first adsorption tower; a second adsorption tower feed port is formed in the bottom of the second adsorption tower, and a second adsorption tower discharge port is formed in the top of the second adsorption tower; a low-temperature storage tank feed port and a low-temperature storage tank discharge port are formed in the top of the low-temperature storage tank; a feed port of the first adsorption tower is communicated with a crude hydrogen sulfide gas source through a pipeline, a discharge port of the first adsorption tower is communicated with a feed port of the second adsorption tower through a pipeline, a discharge port of the second adsorption tower is communicated with a feed port of the low-temperature storage tank through a pipeline, and a discharge port of the low-temperature storage tank is communicated with the product collection bottle. Through the first adsorption tower and the second adsorption tower which are arranged in sequence, the modified 5A molecular sieve is used for sequentially performing normal-temperature adsorption and cryogenic adsorption on hydrogen sulfide, and then the low-temperature storage tank is vacuumized, so that impurities can be effectively removed, and the product purity is improved.

Description

TECHNICAL FIELD

[0001] The utility model relates to the field of gas purification, especially relates to a device for purifying hydrogen sulfide gas. BACKGROUND

[0002] High-purity hydrogen sulfide is an important electronic gas, which is applied in CVD, doping and other processes to prepare optical and electronic devices. In addition to semiconductors, hydrogen sulfide gas plays an important role in national defense chemical industry, electric light, photoconductor and photovoltaics.

[0003] Patent CN108392948A discloses a kind of hydrogen sulfide purification process and device, methanol wash acid gas is absorbed by multistage pressure swing adsorption, and different molecular sieve such as alumina, silica gel, zeolite, activated carbon is used to obtain hydrogen sulfide product with purity greater than 92% by adsorbing gas phase impurities.The method is complex, and the product purity is low.

[0004] Patent CN112408336A provides a kind of liquid absorption and rectification combined process method, part of impurity solvent of hydrogen sulfide crude product is adsorbed and liquefied after obtaining first hydrogen sulfide crude product;First hydrogen sulfide crude product is fractionated to obtain second hydrogen sulfide crude product and light waste gas;Second hydrogen sulfide crude product is fractionated to obtain hydrogen sulfide gas and heavy impurity product, and hydrogen sulfide product with content 99.99% is obtained.The method is complex, and energy consumption is high.

[0005] The problem that is difficult to solve in the process of purifying hydrogen sulfide gas is how to remove water, carbon dioxide, hydrogen and other impurities, so there is an urgent need for a hydrogen sulfide gas purification device that can simply, economically and efficiently remove impurities. UTILITY MODEL CONTENT

[0006] In order to overcome the above-mentioned problems existing in the prior art, the purpose of the utility model is to provide a device for purifying hydrogen sulfide gas, which can simply, economically and efficiently remove impurities.

[0007] In order to achieve the purpose of the utility model, the specific technical solutions provided by the utility model are as follows:

[0008] A device for purifying hydrogen sulfide gas, comprising a first adsorption tower, a second adsorption tower and a low-temperature storage tank connected in sequence;

[0009] The first adsorption tower is provided with a first adsorption tower feed port at the bottom and a first adsorption tower discharge port at the top.

[0010] The second adsorption tower is provided with a second adsorption tower feed port at the bottom and a second adsorption tower discharge port at the top.

[0011] The top of the low-temperature storage tank is provided with a low-temperature storage tank feed port and a low-temperature storage tank discharge port.

[0012] The first adsorption tower feed port is communicated with a crude hydrogen sulfide gas source through a pipeline, the first adsorption tower discharge port is communicated with the second adsorption tower feed port through a pipeline, the second adsorption tower discharge port is communicated with the low-temperature storage tank feed port through a pipeline, and the low-temperature storage tank discharge port is communicated with the product collection bottle.

[0013] Preferably, the second adsorption tower is externally wound with a silica gel coil pipe, the silica gel coil pipe is communicated with a low-temperature constant-temperature reaction bath, and the silica gel coil pipe is filled with 60% concentration ethylene glycol aqueous solution circulated by the low-temperature constant-temperature reaction bath.

[0014] Preferably, the diameter of the silica gel coil pipe is 12 mm, and the ratio of the diameter of the silica gel coil pipe to the diameter of the second adsorption tower is 0.26:1.

[0015] Preferably, the top of the low-temperature storage tank is further provided with a low-temperature storage tank exhaust port, and the low-temperature storage tank exhaust port is communicated with a vacuum pump through a pipeline.

[0016] Preferably, the low-temperature storage tank is externally provided with a jacket, and the jacket is provided with a liquid nitrogen inlet and a cold nitrogen outlet, and the liquid nitrogen inlet of the jacket is communicated with a liquid nitrogen tank.

[0017] Preferably, the bottom of the liquid nitrogen tank is provided with a liquid nitrogen tank discharge port, and the liquid nitrogen tank discharge port is communicated with the liquid nitrogen inlet of the jacket of the low-temperature storage tank through a pipeline.

[0018] Preferably, the ratio of the diameter to the height of the first adsorption tower and the second adsorption tower is 45:1000, and the first adsorption tower and the second adsorption tower are both internally filled with modified 5A molecular sieve.

[0019] The device for purifying hydrogen sulfide gas has the following advantages:

[0020] 1. The first adsorption tower and the second adsorption tower are sequentially arranged, the modified 5A molecular sieve is used to effectively remove impurities in the hydrogen sulfide gas, improve the purity of the hydrogen sulfide gas, and sequentially perform normal temperature adsorption and deep cold adsorption on the hydrogen sulfide by using the modified 5A molecular sieve, thereby reducing the adsorption amount of the conventional 5A molecular sieve on the hydrogen sulfide and enhancing the adsorption effect on carbon dioxide and water.

[0021] 2. The low-temperature storage tank is arranged to further ensure the purity of the hydrogen sulfide gas, so that the quality of the final product is higher, and the adsorbed gas is treated by using the method of refrigeration and negative extraction, so that low-boiling-point impurities such as hydrogen and nitrogen that are difficult to remove by adsorption can be effectively removed, and the product purity is improved.

[0022] 3. The device of the utility model has a simple structure and is easy to operate. It does not require complicated equipment and processes, which reduces production costs. In addition, through reasonable pipeline design and the size ratio of the adsorption tower, the entire purification process is more efficient and the waste of energy and resources is reduced. BRIEF DESCRIPTION OF THE DRAWINGS

[0023] Figure 1 This is a schematic diagram of a device for purifying hydrogen sulfide gas according to the present invention;

[0024] Explanation of the markings in the figure: 1. Crude hydrogen sulfide gas source; 2. First adsorption tower; 3. Second adsorption tower; 4. Silica gel coil; 5. Low-temperature constant-temperature reaction bath; 6. Low-temperature storage tank; 7. Vacuum pump; 8. Product collection bottle; 9. Liquid nitrogen tank. DETAILED DESCRIPTION

[0025] In order to further illustrate the technical means and effects adopted by the present invention to achieve the predetermined purpose, the specific implementation method, structure, characteristics and effects of the present invention are described in detail below in combination with the preferred embodiments.

[0026] Device Example 1

[0027] like Figure 1 FIG. 1 is a schematic diagram of a device for purifying hydrogen sulfide gas according to the present invention;

[0028] A device for purifying hydrogen sulfide gas comprises a crude hydrogen sulfide gas source 1, a first adsorption tower 2, a second adsorption tower 3, a cryogenic storage tank 6 and a product collecting bottle 8 connected in sequence;

[0029] The first adsorption tower 2 is provided with a first adsorption tower feed port at the bottom and a first adsorption tower discharge port at the top;

[0030] The second adsorption tower 3 is provided with a second adsorption tower feed port at the bottom and a second adsorption tower discharge port at the top;

[0031] The top of the cryogenic storage tank 6 is provided with a cryogenic storage tank feed port, a cryogenic storage tank discharge port and a cryogenic storage tank exhaust port.

[0032] The feed port of the first adsorption tower is connected to the crude hydrogen sulfide gas source 1 through a pipeline; the discharge port of the first adsorption tower is connected to the feed port of the second adsorption tower through a pipeline; a silicone coil 4 is wrapped around the outside of the second adsorption tower 3, and the silicone coil 4 is connected to a low-temperature constant-temperature reaction bath 5. The silicone coil 4 contains a 60% concentration ethylene glycol aqueous solution that circulates through the low-temperature constant-temperature reaction bath 5; the diameter of the silicone coil 4 is 12 mm, and the ratio of the diameter of the silicone coil 4 to the diameter of the second adsorption tower 3 is 0.26:1; the diameter and height ratio of the first adsorption tower 2 is 45:1000, and the diameter and height ratio of the second adsorption tower 3 is 45:1000.

[0033] Through reasonable pipeline design and size ratio of the adsorption tower, the whole purification process is more efficient, and the waste of energy and resources is reduced.

[0034] The first adsorption tower 2 and the second adsorption tower 3 are both filled with modified 5A molecular sieve;

[0035] Through the first adsorption tower 2 and the second adsorption tower 3 arranged in sequence, the impurities in the hydrogen sulfide gas can be effectively removed by using the adsorption performance of the modified 5A molecular sieve, thereby improving the purity of the hydrogen sulfide gas. The modified 5A molecular sieve is used to sequentially perform normal temperature adsorption and deep cold adsorption on the hydrogen sulfide, thereby reducing the adsorption amount of the conventional 5A molecular sieve on the hydrogen sulfide, and simultaneously enhancing the adsorption effect on carbon dioxide and water.

[0036] The second adsorption tower outlet is communicated with the low-temperature storage tank inlet through a pipeline, the low-temperature storage tank exhaust port is communicated with the vacuum pump 7 through a pipeline, and the low-temperature storage tank outlet is communicated with the product collection bottle 8; the low-temperature storage tank 6 is externally provided with a jacket, the jacket is provided with a liquid nitrogen inlet and a cold nitrogen outlet, the liquid nitrogen inlet of the jacket is communicated with a liquid nitrogen tank 9, and the bottom of the liquid nitrogen tank 9 is provided with a liquid nitrogen tank outlet, and specifically, the liquid nitrogen tank outlet is communicated with the liquid nitrogen inlet of the jacket through a pipeline.

[0037] The setting of the low-temperature storage tank 6 further ensures the purity of the hydrogen sulfide gas, so that the quality of the final product is higher, and the adsorbed gas is treated by the method of refrigeration and negative extraction, so that the low-boiling-point impurities such as hydrogen and nitrogen that are difficult to remove by adsorption can be effectively removed, which is beneficial to improve the product purity.

[0038] Valves are arranged on the communication pipelines between the crude hydrogen sulfide gas source 1, the first adsorption tower 2, the second adsorption tower 3, the low-temperature storage tank 6 and the product collection bottle 8.

[0039] The device for purifying hydrogen sulfide gas is simple in structure and easy to operate, and does not need complex equipment and process, thereby reducing the production cost.

[0040] A method for purifying hydrogen sulfide gas is implemented by using the device of the device embodiment 1, and includes the following steps:

[0041] S1, crude hydrogen sulfide gas with a purity of 99.5% is introduced into the first adsorption tower 2 filled with modified 5A molecular sieve at a flow rate of 5L / min, the temperature of the first adsorption tower 2 is controlled to be 20℃, and the pressure is controlled to be 0.6MPa-1MPa;

[0042] S2, the hydrogen sulfide gas after being adsorbed by the first adsorption tower 2 is introduced into the second adsorption tower 3 filled with modified 5A molecular sieve, the temperature is controlled to be-50℃, and the pressure is controlled to be 0.5MPa-0.8MPa;

[0043] S3, hydrogen sulfide gas after adsorbing the second adsorption tower 3 is passed into low temperature storage tank 6, hydrogen sulfide gas is condensed into solid in low temperature storage tank 6, and the refrigerant of low temperature storage tank 6 is liquid nitrogen, and the temperature of storage tank is controlled to be -90 DEG C;

[0044] S4, low temperature storage tank 6 is vacuumed to negative pressure, after 10 min, stop vacuumizing, then close the liquid nitrogen inlet of jacket, the temperature of low temperature storage tank 6 is slowly increased, hydrogen sulfide in low temperature storage tank 6 is gasified and filled into product collection bottle 8, and the purity of hydrogen sulfide product is 99.992%.

[0045] The utility model discloses a first adsorption tower 2 and second adsorption tower 3 set gradually, utilize the adsorption of modified 5A molecular sieve, can effectively remove the impurity in hydrogen sulfide gas, improve the purity of hydrogen sulfide gas, use modified 5A molecular sieve to hydrogen sulfide is sequentially carried out normal temperature adsorption and cryogenic adsorption, has reduced the adsorption amount of conventional 5A molecular sieve to hydrogen sulfide, has strengthened the adsorption effect of carbon dioxide and water to 5A molecular sieve simultaneously. The setting of low temperature storage tank 6 further ensures the purity of hydrogen sulfide gas, so that the quality of the product obtained finally is higher, and the method of freezing and extracting negative pressure is used to treat the gas after adsorption, can effectively remove hydrogen, nitrogen and other low-boiling-point impurities that are difficult to remove by adsorption, and is favorable to improving product purity.

[0046] The above-mentioned is only the preferred embodiment of the utility model, and does not limit the utility model in any form, although the utility model has disclosed above with the preferred embodiment, however, is not used to limit the utility model, any person skilled in the art, within the scope of the utility model technical scheme, can make a little more change or modification as equivalent embodiment of equivalent change with the disclosed technical content, but as long as not departing from the utility model technical scheme content, according to the technical essence of the utility model, any simplification modification, equivalent change and modification of the above embodiment, still belongs to the scope of the utility model technical scheme.

Claims

1. An apparatus for purifying hydrogen sulfide gas, characterized by, The first adsorption tower, the second adsorption tower and the low-temperature storage tank are sequentially communicated. The first adsorption tower is provided with a first adsorption tower feed inlet at the bottom and a first adsorption tower discharge outlet at the top. The second adsorption tower is provided with a second adsorption tower feed inlet at the bottom and a second adsorption tower discharge outlet at the top. The low-temperature storage tank is provided with a low-temperature storage tank feed inlet and a low-temperature storage tank discharge outlet at the top. The first adsorption tower feed inlet is communicated with a crude hydrogen sulfide gas source through a pipeline, the first adsorption tower discharge outlet is communicated with the second adsorption tower feed inlet through a pipeline, the second adsorption tower discharge outlet is communicated with the low-temperature storage tank feed inlet through a pipeline, and the low-temperature storage tank discharge outlet is communicated with a product collection bottle.

2. The apparatus for purifying hydrogen sulfide gas according to claim 1, wherein The second adsorption tower is externally wound with a silica gel coil pipe, which is communicated with a low-temperature constant temperature reaction bath, and the silica gel coil pipe is filled with 60% volume concentration of ethylene glycol aqueous solution circulated by the low-temperature constant temperature reaction bath.

3. The apparatus for purifying hydrogen sulfide gas according to claim 2, wherein The diameter of the silica gel coil pipe is 12 mm, and the ratio of the diameter of the silica gel coil pipe to the diameter of the second adsorption tower is 0.26:

1.

4. The apparatus for purifying hydrogen sulfide gas according to claim 1, wherein The low-temperature storage tank is further provided with a low-temperature storage tank exhaust port at the top, which is communicated with a vacuum pump through a pipeline.

5. The apparatus for purifying hydrogen sulfide gas according to claim 1, wherein The low-temperature storage tank is externally provided with a jacket, which is provided with a liquid nitrogen inlet and a cold nitrogen outlet, and the liquid nitrogen inlet of the jacket is communicated with a liquid nitrogen tank.

6. The apparatus for purifying hydrogen sulfide gas according to claim 5, wherein The liquid nitrogen tank is provided with a liquid nitrogen tank discharge outlet at the bottom, which is communicated with the liquid nitrogen inlet of the low-temperature storage tank jacket through a pipeline.

7. The apparatus for purifying hydrogen sulfide gas according to claim 1, wherein The ratio of the diameter to the height of the first adsorption tower and the second adsorption tower is 45:1000, and the first adsorption tower and the second adsorption tower are both internally filled with modified 5A molecular sieve.

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