CN111137862A - Hydrogen chloride raw material gas moisture removal device and moisture removal method - Google Patents
Hydrogen chloride raw material gas moisture removal device and moisture removal method Download PDFInfo
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- CN111137862A CN111137862A CN201911354383.1A CN201911354383A CN111137862A CN 111137862 A CN111137862 A CN 111137862A CN 201911354383 A CN201911354383 A CN 201911354383A CN 111137862 A CN111137862 A CN 111137862A
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- hydrogen chloride
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- raw material
- material gas
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B7/00—Halogens; Halogen acids
- C01B7/01—Chlorine; Hydrogen chloride
- C01B7/07—Purification ; Separation
- C01B7/0706—Purification ; Separation of hydrogen chloride
- C01B7/0718—Purification ; Separation of hydrogen chloride by adsorption
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/26—Drying gases or vapours
- B01D53/261—Drying gases or vapours by adsorption
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B7/00—Halogens; Halogen acids
- C01B7/01—Chlorine; Hydrogen chloride
- C01B7/07—Purification ; Separation
- C01B7/0706—Purification ; Separation of hydrogen chloride
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The invention discloses a device and a method for removing moisture from a hydrogen chloride raw material gas, and belongs to the field of fine chemical engineering and gas treatment. The device comprises: dehydration tower, filter equipment and drying device. The method comprises the following steps: step 1, preparing slurry, and step 2, feeding the slurry into a dehydration tower through a slurry inlet, and simultaneously adding a hydrogen chloride raw material gas into the dehydration tower through a hydrogen chloride raw material gas inlet; step 3, adsorbing moisture in the hydrogen chloride feed gas by using an adsorbent in the slurry; step 4, extracting the dehydrated hydrogen chloride gas from a hydrogen chloride outlet; and 5, extracting the slurry after water absorption from the bottom of the tower kettle of the dehydration tower through a pipeline. The device and the method can realize continuous operation, form a closed dehydration system, do not generate three wastes in the dehydration process, are safe and environment-friendly, have high dehydration efficiency, simple and convenient operation, low requirements on operation temperature, pressure and the like and low process cost.
Description
Technical Field
The invention belongs to the field of fine chemical engineering and gas treatment, and particularly relates to a device and a method for removing moisture in a hydrogen chloride raw material gas.
Background
The high-purity hydrogen chloride gas plays an important role in the manufacture of semiconductor equipment, has extremely high requirements on the dryness of the hydrogen chloride in epitaxial cleaning of silicon crystals and silicon wafer etching, has strong corrosivity on the hydrous hydrogen chloride, and needs frequent maintenance and replacement of a conveying pipeline, so that the moisture in the hydrogen chloride gas is required to be removed as little as possible.
Currently, there are three main ways of drying gas: chemical dehumidification, freezing dehumidification and adsorption. The chemical dehumidification method adopts liquid such as sulfuric acid, lithium chloride, lithium bromide and glycerol to absorb moisture in gas, or adopts active solid such as sodium hydroxide, potassium hydroxide, calcium sulfate or anhydrous calcium chloride to remove water, the freezing dehumidification method adopts refrigerant such as Freon and liquid nitrogen to freeze and dry gas, and a cold accumulator and a reversible heat exchanger are utilized to freeze and remove trace water; the adsorption method is to treat a gas mixture with a porous solid adsorbent such as activated alumina, silica gel, molecular sieves, etc. to adsorb moisture in the gas onto the surface of the solid, thereby drying the gas. Although the chemical dehumidification method is simple in operation, the reaction between the gas and the desiccant is considered in use, and the freeze dehumidification method has disadvantages that the consumption of the desiccant (refrigerant) is fast and uneconomical, and the moisture is easily frozen to block the pipeline. Compared with other two methods, the adsorption method has the advantages of simple and convenient process operation, high automation degree, regeneration and use of the adsorbent and long service life. Many domestic and foreign documents report that water in hydrogen chloride is removed by adopting an adsorption method to obtain high-purity hydrogen chloride gas, but at present, no complete hydrogen chloride raw material gas moisture removal device and corresponding process method exist.
Disclosure of Invention
The invention aims to provide a device and a method for removing moisture from a hydrogen chloride raw material gas, which can realize continuous operation to form a closed dehydration system, do not generate three wastes in the dehydration process, are safe and environment-friendly, have high dehydration efficiency, simple and convenient operation, low requirements on operation temperature, pressure and the like, and have low process cost.
The scheme of the invention is realized by the following technical scheme:
a device for removing moisture from a hydrogen chloride raw material gas comprises: a dehydration tower, a filtering device and a drying device; the side of the upper part of the dehydration tower is provided with a slurry inlet, the side of the lower part of the dehydration tower is provided with a hydrogen chloride feed gas inlet, the top end of the dehydration tower is provided with a dehydrated hydrogen chloride outlet, the bottom end of the dehydration tower is sequentially connected with a filtering device and a drying device through pipelines, and the filtering device and the drying device are further connected with a slurry inlet pipeline.
A method for removing moisture from a hydrogen chloride feed gas comprises the following steps:
step 4, extracting the dehydrated hydrogen chloride gas from a hydrogen chloride outlet;
and 5, extracting the slurry after water absorption from the bottom of the tower kettle of the dehydration tower through a pipeline.
Preferably, the adsorbent in step 1 is a molecular sieve and/or a zeolite.
Further, the molecular sieve is at least one of a 3A molecular sieve, a 4A molecular sieve, a 5A molecular sieve and a 13X molecular sieve, and more preferably at least one of a 5A molecular sieve and a 13X molecular sieve.
Preferably, the particle size of the adsorbent in the step 1 is 100-300 meshes.
Preferably, the solvent in step 1 is an organic solvent insoluble in water.
Further, the organic solvent is at least one of dioctyl phthalate (DOP), benzene, dichloromethane, carbon tetrachloride and anhydrous hydrogen chloride.
Preferably, the mass of the adsorbent in the step 1 accounts for 1-10% of the mass of the solvent.
Preferably, the water content of the hydrogen chloride raw material gas in the step 2 is 100ppm to 1000 ppm.
Preferably, the method further comprises a step 6 of sending the slurry obtained in the step 5 after water absorption into a filtering device to filter out the solvent, then sending the filtered slurry into a drying device to dry the adsorbent contained in the slurry, mixing the dried adsorbent with the filtered solvent to form new slurry, and then returning the new slurry into the dehydration tower through a slurry inlet.
The invention has the beneficial effects that:
the device and the method can realize continuous operation, form a closed dehydration system, do not generate three wastes in the dehydration process, are safe and environment-friendly, have high dehydration efficiency, simple and convenient operation, low requirements on operation temperature, pressure and the like and low process cost.
Drawings
Fig. 1 is a schematic structural diagram of a hydrogen chloride raw material gas moisture removal device according to the present invention.
Wherein, the device comprises a 1-dehydration tower, a 2-slurry inlet, a 3-hydrogen chloride raw material gas inlet, a 4-hydrogen chloride outlet, a 5-filtering device and a 6-drying device
Detailed Description
The invention is described in detail below by way of example with reference to the accompanying drawings.
The experimental methods described in the following examples are all conventional methods unless otherwise specified; the reagents, materials and equipment are commercially available, unless otherwise specified.
A moisture removal device for a hydrogen chloride raw material gas, as shown in figure 1, comprising: a dehydration tower 1, a filtering device 5 and a drying device 6; the side of dehydration tower upper portion sets up thick liquids entry 12, and the side of dehydration tower lower part sets up hydrogen chloride feed gas entry 3, and the dehydration tower top sets up dehydration hydrogen chloride export 4, and the dehydration tower bottom connects gradually filter equipment 5 and drying device 6 through the pipeline, and filter equipment 5 and drying device 6 still with thick liquids entry 12 pipe connection.
The main parameters in the adsorption tower of the hydrogen chloride feed gas moisture removal device comprise that the height of an adsorption layer is 3m, the inner diameter of the adsorption layer is 0.5m, the porosity of internal particles is 0.4 cubic meter/cubic meter, the porosity of external particles is 0.1 cubic meter/cubic meter, the solid density of an adsorbent is 713 kg/cubic meter, the shape factor of the adsorbent is 1, the constant mass transfer coefficient of water is 110l/s, the isothermal line parameter is 0.0082, and the constant mass transfer coefficient of hydrogen chloride is 10-10l/s, the isotherm parameter is 0.
In the case of the example 1, the following examples are given,
the method comprises the following steps:
(1) preparing slurry, wherein the slurry is formed by mixing a 13X molecular sieve with the particle size of 100 meshes and an organic solvent DOP, and the mass of the adsorbent accounts for 1% of that of the solvent;
(2) feeding the slurry into a dehydrating tower 1 through a slurry inlet 2, and simultaneously feeding the hydrogen chloride raw material gas into the dehydrating tower 1 through a hydrogen chloride raw material gas inlet 3;
(3) the slurry is in countercurrent contact with a hydrogen chloride raw material gas with the flow rate of 2L/min and the water content of 20L/min and the water content of 1000ppm, and an adsorbent in the slurry adsorbs the water in the hydrogen chloride raw material gas;
(4) the dehydrated hydrogen chloride is extracted from a dehydrated hydrogen chloride outlet 4;
(5) the slurry after water absorption is extracted from the bottom of the tower kettle of the dehydration tower 1 through a pipeline.
(6) And (2) after the slurry after water absorption is extracted from the bottom of the tower kettle of the dehydrating tower 1 through a pipeline, filtering out the solvent through a filtering device 5, drying the adsorbent contained in the solvent through a drying device 6, mixing the dried adsorbent with the filtered solvent to form new slurry, and returning the new slurry into the adsorbing tower 1 through a slurry inlet 2.
(7) Through detection, the water content in the hydrogen chloride gas collected by the outlet 4 is 0.1ppm, and the requirements of 5N-grade and above 5N-grade hydrogen chloride on water impurities are met.
In the case of the example 2, the following examples are given,
the method comprises the following steps:
(1) preparing slurry, wherein the slurry is formed by mixing a 13X molecular sieve with the particle size of 300 meshes and an organic solvent benzene, and the mass of an adsorbent accounts for 10% of the mass of the solvent;
(2) feeding the slurry into a dehydrating tower 1 through a slurry inlet 2, and simultaneously feeding the hydrogen chloride raw material gas into the dehydrating tower 1 through a hydrogen chloride raw material gas inlet 3;
(3) the slurry is in countercurrent contact with a hydrogen chloride raw material gas with the water content of 500ppm and the flow rate of 10L/min, and an adsorbent in the slurry adsorbs water in the hydrogen chloride raw material gas;
(4) the dehydrated hydrogen chloride is extracted from a dehydrated hydrogen chloride outlet 4;
(5) the slurry after water absorption is extracted from the bottom of the tower kettle of the dehydration tower 1 through a pipeline.
(6) And (2) after the slurry after water absorption is extracted from the bottom of the tower kettle of the dehydrating tower 1 through a pipeline, filtering out the solvent through a filtering device 5, drying the adsorbent contained in the solvent through a drying device 6, mixing the dried adsorbent with the filtered solvent to form new slurry, and returning the new slurry into the adsorbing tower 1 through a slurry inlet 2.
(7) Through detection, the water content in the hydrogen chloride gas collected by the outlet 4 is 0.4ppm, and the requirements of 5N-grade and above 5N-grade hydrogen chloride on water impurities are met.
In the case of the example 3, the following examples are given,
the method comprises the following steps:
(1) preparing slurry, wherein the slurry is formed by mixing a 5A molecular sieve with the particle size of 150 meshes and an organic solvent dichloromethane, and the mass of an adsorbent accounts for 5% of that of the solvent;
(2) feeding the slurry into a dehydrating tower 1 through a slurry inlet 2, and simultaneously feeding the hydrogen chloride raw material gas into the dehydrating tower 1 through a hydrogen chloride raw material gas inlet 3;
(3) the slurry is in countercurrent contact with a hydrogen chloride raw material gas with the water content of 100ppm and the flow rate of 20L/min, and an adsorbent in the slurry absorbs the water in the hydrogen chloride raw material gas;
(4) the dehydrated hydrogen chloride is extracted from a dehydrated hydrogen chloride outlet 4;
(5) the slurry after water absorption is extracted from the bottom of the tower kettle of the dehydration tower 1 through a pipeline.
(6) And (2) after the slurry after water absorption is extracted from the bottom of the tower kettle of the dehydrating tower 1 through a pipeline, filtering out the solvent through a filtering device 5, drying the adsorbent contained in the solvent through a drying device 6, mixing the dried adsorbent with the filtered solvent to form new slurry, and returning the new slurry into the adsorbing tower 1 through a slurry inlet 2.
(7) Through detection, the water content in the hydrogen chloride gas collected by the outlet 4 is 0.2ppm, and the requirements of 5N-grade and above 5N-grade hydrogen chloride on water impurities are met.
In the case of the example 4, the following examples are given,
the method comprises the following steps:
(1) preparing slurry, wherein the slurry is formed by mixing a 5A molecular sieve with the particle size of 200 meshes and an organic solvent of carbon tetrachloride, and the mass of an adsorbent accounts for 8% of that of the solvent;
(2) feeding the slurry into a dehydrating tower 1 through a slurry inlet 2, and simultaneously feeding the hydrogen chloride raw material gas into the dehydrating tower 1 through a hydrogen chloride raw material gas inlet 3;
(3) the slurry is in countercurrent contact with a hydrogen chloride raw material gas with the water content of 5000ppm and the flow rate of 5L/min, and an adsorbent in the slurry adsorbs water in the hydrogen chloride raw material gas;
(4) the dehydrated hydrogen chloride is extracted from a dehydrated hydrogen chloride outlet 4;
(5) the slurry after water absorption is extracted from the bottom of the tower kettle of the dehydration tower 1 through a pipeline;
(6) and (2) after the slurry after water absorption is extracted from the bottom of the tower kettle of the dehydrating tower 1 through a pipeline, filtering out the solvent through a filtering device 5, drying the adsorbent contained in the solvent through a drying device 6, mixing the dried adsorbent with the filtered solvent to form new slurry, and returning the new slurry into the adsorbing tower 1 through a slurry inlet 2.
(7) Through detection, the water content in the hydrogen chloride gas collected by the outlet 4 is 0.5ppm, and the requirements of 5N-grade and above 5N-grade hydrogen chloride on water impurities are met.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A device for removing moisture in a hydrogen chloride raw material gas is characterized by comprising: a dehydration tower, a filtering device and a drying device; the side of the upper part of the dehydration tower is provided with a slurry inlet, the side of the lower part of the dehydration tower is provided with a hydrogen chloride feed gas inlet, the top end of the dehydration tower is provided with a dehydrated hydrogen chloride outlet, the bottom end of the dehydration tower is sequentially connected with a filtering device and a drying device through pipelines, and the filtering device and the drying device are further connected with a slurry inlet pipeline.
2. A method for removing moisture from a hydrogen chloride raw material gas is characterized by comprising the following steps:
step 1, preparing slurry, wherein the slurry is formed by mixing an adsorbent and a solvent;
step 2, feeding the slurry into a dehydration tower through a slurry inlet, and simultaneously adding a hydrogen chloride raw material gas into the dehydration tower through a hydrogen chloride raw material gas inlet;
step 3, the slurry is in countercurrent contact with the hydrogen chloride feed gas, and an adsorbent in the slurry adsorbs moisture in the hydrogen chloride feed gas;
step 4, extracting the dehydrated hydrogen chloride gas from a hydrogen chloride outlet;
and 5, extracting the slurry after water absorption from the bottom of the tower kettle of the dehydration tower through a pipeline.
3. The process according to claim 2, wherein the adsorbent in step 1 is molecular sieve and/or zeolite.
4. The method for removing moisture from a hydrogen chloride raw material gas as claimed in claim 3, wherein the molecular sieve is at least one of a 3A molecular sieve, a 4A molecular sieve, a 5A molecular sieve and a 13X molecular sieve.
5. The method for removing moisture from a hydrogen chloride raw material gas as claimed in claim 2, wherein the particle size of the adsorbent in step 1 is 100-300 meshes.
6. The process for removing water from a hydrogen chloride raw material gas as claimed in claim 2, wherein the solvent used in step 1 is a water-insoluble organic solvent.
7. The moisture removal method for a hydrogen chloride raw material gas as claimed in claim 6, wherein the organic solvent is at least one of dioctyl phthalate, benzene, methylene chloride, carbon tetrachloride and anhydrous hydrogen chloride.
8. The method for removing moisture from a hydrogen chloride raw material gas as claimed in claim 2, wherein the mass of the adsorbent in step 1 is 1-10% of the mass of the solvent.
9. The method for removing moisture from a hydrogen chloride raw material gas according to claim 2, wherein the water content of the hydrogen chloride raw material gas in the step 2 is 100ppm to 1000 ppm.
10. The method for removing moisture from a hydrogen chloride raw material gas as claimed in any one of claims 2 to 9, further comprising a step 6 of feeding the slurry obtained in the step 5 after water absorption into a filtering device to filter out a solvent, then feeding the filtered slurry into a drying device to dry an adsorbent contained therein, mixing the dried adsorbent with the filtered solvent to form a new slurry, and then returning the new slurry into the dehydration tower through a slurry inlet.
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| CN201911354383.1A CN111137862A (en) | 2019-12-25 | 2019-12-25 | Hydrogen chloride raw material gas moisture removal device and moisture removal method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114558430A (en) * | 2021-12-29 | 2022-05-31 | 安徽华塑股份有限公司 | Industrial dehydration process for aqueous hydrogen chloride gas |
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2019
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| CN114558430A (en) * | 2021-12-29 | 2022-05-31 | 安徽华塑股份有限公司 | Industrial dehydration process for aqueous hydrogen chloride gas |
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Address after: 057550 No. five Weir Road, chemical industry gathering area, Feixiang District, Handan, Hebei, 1 Applicant after: China shipbuilding (Handan) Perry Special Gas Co.,Ltd. Address before: No.1 Weiwu Road, chemical industry gathering area, Feixiang County, Handan City, Hebei Province Applicant before: PERIC SPECIAL GASES Co.,Ltd. |
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Application publication date: 20200512 |