CN111170276A - Hydrochloric acid analysis method - Google Patents
Hydrochloric acid analysis method Download PDFInfo
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- CN111170276A CN111170276A CN202010057971.5A CN202010057971A CN111170276A CN 111170276 A CN111170276 A CN 111170276A CN 202010057971 A CN202010057971 A CN 202010057971A CN 111170276 A CN111170276 A CN 111170276A
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- hydrochloric acid
- hydrogen chloride
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- copper chloride
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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
- C01B7/03—Preparation from chlorides
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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
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- Drying Of Gases (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
The invention relates to the technical field of inorganic chemistry, in particular to a hydrochloric acid analysis method. The method for resolving the hydrochloric acid comprises the following steps: mixing hydrochloric acid with the mass fraction of 20-31% with anhydrous copper chloride for 6-60 min at normal temperature, and condensing the obtained gas at-30 to-10 ℃ to obtain hydrogen chloride gas. The hydrochloric acid analysis method provided by the invention has the advantages of simpler process, higher analysis efficiency and higher yield and purity of the obtained hydrogen chloride gas. The analytic method can also avoid the equipment from being in high-temperature dangerous liquid and corrosive liquid environments such as concentrated/dilute sulfuric acid, concentrated/dilute hydrochloric acid and the like, the whole process is completed between a solid state and a gas state, the hydrogen chloride gas adsorbed on the surface of the solid is removed in the drying and regenerating process of the mixed copper chloride solid, and then the crystal water is removed, so that the acid content in the wastewater is lower. The equipment in the invention does not need to directly contact a large amount of corrosive liquid, and is beneficial to prolonging the service life of the equipment.
Description
Technical Field
The invention relates to the technical field of inorganic chemistry, in particular to a hydrochloric acid analysis method.
Background
The conventional hydrochloric acid resolving process comprises the following steps: the principle of conventional desorption, extractive distillation and pressure swing adsorption is the reverse process of HCl absorption, the hydrogen chloride gas is desorbed from concentrated hydrochloric acid by utilizing the fact that the solubility of the hydrogen chloride in water is reduced along with the rise of temperature, and the process flow, equipment and operation are relatively complex. When the hydrogen chloride is removed, the water and the hydrogen chloride are azeotroped, and the primary yield of the obtained hydrogen chloride is low. Meanwhile, the residual dilute hydrochloric acid needs to be further absorbed by the conventional analysis for thickening, the waste hydrogen chloride may be crystallized if the azeotropic point is not well controlled by using calcium chloride, the investment of conventional process equipment is relatively high, and the concentration produces acid-containing wastewater containing less than 1 wt% of hydrogen chloride.
Disclosure of Invention
In view of this, the technical problem to be solved by the present invention is to provide a hydrochloric acid resolving method, which is simpler in process, higher in resolving efficiency, and lower in acid content of the generated wastewater.
The invention provides a hydrochloric acid analysis method, which comprises the following steps:
mixing hydrochloric acid with the mass fraction of 20-31% with anhydrous copper chloride for 6-60 min at normal temperature, and condensing the obtained gas at-30 to-10 ℃ to obtain hydrogen chloride gas.
Preferably, the mass ratio of the hydrochloric acid to the anhydrous copper chloride is 3-4: 9 to 10.
Preferably, the mixing of 20-31% by mass of hydrochloric acid and anhydrous copper chloride at room temperature for 0.1-1 h specifically comprises:
dripping 20-31 wt% hydrochloric acid into anhydrous copper chloride, and mixing at normal temperature for 0.1-1 h.
Preferably, the condensation time of the obtained gas at-30 to-10 ℃ is 0.1 to 1 hour.
Preferably, after the mixing, the method further comprises:
and drying the mixed copper chloride at 100-120 ℃ for 3-5 h, and collecting the removed hydrogen chloride and crystal water.
Preferably, after collecting the removed hydrogen chloride and the crystal water, the method further comprises:
and condensing and separating the collected hydrogen chloride and the crystal water to obtain hydrogen chloride gas.
Preferably, the condensation temperature is-30 to-10 ℃, and the condensation time is 3 to 5 hours.
The invention provides a hydrochloric acid analysis method, which comprises the following steps: mixing hydrochloric acid with the mass fraction of 20-31% with anhydrous copper chloride for 6-60 min at normal temperature, and condensing the obtained gas at-30 to-10 ℃ to obtain hydrogen chloride gas. The hydrochloric acid analysis method provided by the invention has the advantages of simpler process, higher analysis efficiency and higher yield and purity of the obtained hydrogen chloride gas. The analytic method provided by the invention can also avoid the equipment from being in high-temperature dangerous liquid and corrosive liquid environments such as concentrated/dilute sulfuric acid, concentrated/dilute hydrochloric acid and the like, the whole process is completed between a solid state and a gas state, the mixed copper chloride solid is heated, dehydrated and regenerated and then reused, and the drying and regeneration process also comprises the steps of firstly removing hydrogen chloride gas adsorbed on the surface of the solid and then removing crystal water, so that the acid content in the wastewater is lower. The equipment in the invention does not need to directly contact a large amount of corrosive liquid, and is beneficial to prolonging the service life of the equipment.
Experimental results show that the hydrochloric acid analysis method provided by the invention is simpler in process and higher in analysis efficiency, the primary yield of the obtained hydrogen chloride is not lower than 86%, the comprehensive yield is not lower than 97.7%, the purity is not lower than 99%, and both the primary yield and the purity are higher.
Compared with the conventional analytic method, the analytic method process of the hydrochloric acid provided by the invention has a better separation effect, the waste water generated by concentration by the conventional method contains less than 1 wt% of hydrogen chloride, and the waste water removed by the method contains less than 0.5 wt% of hydrogen chloride.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a hydrochloric acid analysis method, which comprises the following steps:
mixing hydrochloric acid with the mass fraction of 20-31% with anhydrous copper chloride for 6-60 min at normal temperature, and condensing the obtained gas at-30 to-10 ℃ to obtain hydrogen chloride gas.
The mass fraction of the hydrochloric acid adopted by the invention is 20-31%. In certain embodiments of the invention, the hydrochloric acid is present in an amount of 30% by weight.
In some embodiments of the invention, the mass ratio of the hydrochloric acid to the anhydrous copper chloride is 3-4: 9 to 10. In certain embodiments, the mass ratio of hydrochloric acid to anhydrous copper chloride is 4: 10. 3: 10 or 3: 9.
in some embodiments of the invention, mixing hydrochloric acid with a mass fraction of 20% -31% and anhydrous copper chloride for 0.1-1 h at normal temperature specifically comprises:
dripping 20-31 wt% hydrochloric acid into anhydrous copper chloride, and mixing at normal temperature for 10-60 min.
In some embodiments of the invention, the dropping time is 6-60 min. In certain embodiments, the time of the dropwise addition is 20min or 15 min. During the dropping process, a large amount of gas including hydrogen chloride gas and a small amount of water vapor is generated.
In the invention, hydrochloric acid with the mass fraction of 20-31% and anhydrous copper chloride are mixed at normal temperature. In certain embodiments of the invention, the time of mixing is 20min or 10 min. After the mixing is complete, substantially no gas is produced.
In certain embodiments of the invention, the dropping and mixing are both performed in an absorption dryer.
In the invention, the gas obtained after mixing is condensed at-30 to-10 ℃, and the obtained non-condensable gas is hydrogen chloride gas. The yield of the hydrogen chloride gas obtained by the method is the primary yield, and the hydrogen chloride gas obtained by the technical scheme provided by the invention has the advantages of higher primary yield and higher purity. The primary yield of the hydrogen chloride is not less than 86 percent, and the purity is not less than 99 percent.
In certain embodiments of the invention, the temperature at which the mixed gases condense is-20 ℃ or-30 ℃. In some embodiments of the present invention, the condensing time is 0.1 to 1 hour. In certain embodiments, the time of condensation is 40min or 30 min.
In certain embodiments of the invention, the mixing is carried out at-30 to-10 ℃ with the resulting gas being condensed in a condenser. In certain embodiments of the invention, the condenser is a glass coil heat exchanger.
In some embodiments of the present invention, after the mixing, further comprising:
and drying the mixed copper chloride at 100-120 ℃ for 3-5 h, and collecting the removed hydrogen chloride and crystal water.
In certain embodiments of the invention, the mixed copper chloride is dried at a temperature of 120 ℃ or 110 ℃ for 4 hours or 5 hours.
In certain embodiments of the present invention, the drying is performed in an absorption dryer. The dried anhydrous copper chloride is regenerated and can be recycled.
In some embodiments of the present invention, after collecting hydrogen chloride and crystal water adsorbed by the copper chloride removal, the method further comprises:
and condensing the collected hydrogen chloride and the crystal water to obtain hydrogen chloride gas.
In some embodiments of the invention, the collected hydrogen chloride and the crystal water are condensed at-30 to-10 ℃ for 3 to 5 hours. In certain embodiments, the temperature of the condensation is-20 ℃, -10 ℃, or-30 ℃, and the time of the condensation is 4 hours or 5 hours.
In certain embodiments of the invention, the condensing of the collected hydrogen chloride and water of crystallization is carried out in a condenser. In certain embodiments of the present invention, the condenser is a glass coil condenser.
In the invention, the detection of the waste water after twice condensation shows that the content of the hydrogen chloride in the waste water is less than 0.5 wt%. The waste water generated by the concentration by the conventional method contains less than 1 wt% of hydrogen chloride, and compared with the conventional analytic method, the method has better separation effect.
The source of the above-mentioned raw materials is not particularly limited in the present invention, and may be generally commercially available.
The invention provides a hydrochloric acid analysis method, which comprises the following steps: mixing hydrochloric acid with the mass fraction of 20-31% with anhydrous copper chloride for 6-60 min at normal temperature, and condensing the obtained gas at-30 to-10 ℃ to obtain hydrogen chloride gas. The hydrochloric acid analysis method provided by the invention has the advantages of simpler process, higher analysis efficiency and higher yield and purity of the obtained hydrogen chloride gas. The analytic method provided by the invention can also avoid the equipment from being in high-temperature dangerous liquid and corrosive liquid environments such as concentrated/dilute sulfuric acid, concentrated/dilute hydrochloric acid and the like, the whole process is completed between a solid state and a gas state, the mixed copper chloride solid is heated, dehydrated and regenerated and then reused, and the drying and regeneration process also comprises the steps of firstly removing hydrogen chloride gas adsorbed on the surface of the solid and then removing crystal water, so that the acid content in the wastewater is lower. The equipment in the invention does not need to directly contact a large amount of corrosive liquid, and is beneficial to prolonging the service life of the equipment.
Experimental results show that the hydrochloric acid analysis method provided by the invention is simpler in process and higher in analysis efficiency, the primary yield of the obtained hydrogen chloride is not lower than 86%, the comprehensive yield is not lower than 97.7%, the purity is not lower than 99%, and both the primary yield and the purity are higher.
Compared with the conventional analytic method, the analytic method process of the hydrochloric acid provided by the invention has a better separation effect, the waste water generated by concentration by the conventional method contains less than 1 wt% of hydrogen chloride, and the waste water removed by the method contains less than 0.5 wt% of hydrogen chloride.
In order to further illustrate the present invention, the following examples are provided to describe the method for resolving hydrochloric acid of the present invention in detail, but they should not be construed as limiting the scope of the present invention.
The starting materials used in the following examples are all generally commercially available.
Example 1
50g of hydrochloric acid with the mass content of 30 percent is dripped into 125g of anhydrous copper chloride in an absorption dryer at normal temperature, the dripping time is 20min, after the dripping and mixing are completed for 20min, the generated gas is condensed for 40min at the temperature of minus 20 ℃ in a glass coil heat exchanger, and then 12.9g of dry gas is obtained, the yield of hydrogen chloride is 86 percent, and the purity is 99.1 percent. And drying the copper chloride mixed for 20min in an absorption dryer at 120 ℃ for 4h, collecting the removed hydrogen chloride and crystal water, condensing the collected hydrogen chloride and crystal water in another glass coil heat exchanger at-20 ℃ for 4h to obtain 35.3g of water and 1.75g of hydrogen chloride gas, wherein the dried anhydrous copper chloride is 125 g. Through collection and calculation, the comprehensive yield of the hydrogen chloride gas is 97.7%, and the purity is 99.1%.
The detection of the waste water after the two times of condensation shows that the content of the hydrogen chloride in the waste water is 0.47 wt%.
Example 2
30g of hydrochloric acid with the mass content of 25 percent is dripped into 100g of anhydrous copper chloride in an absorption dryer at normal temperature, the dripping time is 15min, after the dripping and mixing are completed for 10min, the generated gas is condensed for 30min at the temperature of minus 20 ℃ in a glass coil heat exchanger to obtain 6.7g of dry gas, the yield of the hydrogen chloride is 89.3 percent, and the purity is 99 percent. And drying the copper chloride mixed for 10min in an absorption dryer at 120 ℃ for 5h, collecting the removed hydrogen chloride and crystal water, condensing the collected hydrogen chloride and crystal water in another glass coil heat exchanger at-20 ℃ for 5h to obtain 22.5g of water and 0.65g of hydrogen chloride gas, wherein the dried anhydrous copper chloride is 100 g. Through collection and calculation, the comprehensive yield of the hydrogen chloride gas is 98 percent, and the purity is 99 percent.
The detection of the waste water after the two times of condensation shows that the content of the hydrogen chloride in the waste water is 0.39 wt%.
Example 3
50g of hydrochloric acid with the mass content of 20 percent is dripped into 150g of anhydrous copper chloride in an absorption dryer at normal temperature, the dripping time is 20min, after the dripping and mixing are completed for 20min, the generated gas is condensed for 40min at minus 30 ℃ in a glass coil heat exchanger to obtain 8.9g of dry gas, the yield of the hydrogen chloride is 89 percent, and the purity is 99.2 percent. And drying the copper chloride mixed for 20min in an absorption dryer at 110 ℃ for 4h, collecting the removed hydrogen chloride and crystal water, condensing the collected hydrogen chloride and crystal water in another glass coil heat exchanger at-30 ℃ for 4h to obtain 40g of water and 0.89g of hydrogen chloride gas, wherein the dried anhydrous copper chloride is 150 g. Through collection and calculation, the comprehensive yield of the hydrogen chloride gas is 97.9 percent, and the purity is 99.2 percent.
The detection of the waste water after the two times of condensation shows that the content of the hydrogen chloride in the waste water is 0.45 wt%.
Comparative example 1
In the conventional analysis method, hydrogen chloride in concentrated hydrochloric acid is analyzed by heating, but hydrogen chloride azeotropes with water, and only concentrated hydrochloric acid with hydrochloric acid concentration higher than 20% can be analyzed, so that the primary yield is low, and the primary yield is lower than 36% in the case of 31% concentrated hydrochloric acid.
And through a calcium chloride analytic method and a concentrated sulfuric acid analytic method, after primary analysis, additional equipment needs to be put into the calcium chloride solution and dilute sulfuric acid for concentration operation, equipment is in a high-temperature corrosive liquid environment for a long time in the concentration process and seriously corrodes the equipment, and meanwhile, the acid content of wastewater generated in the concentration process is higher (the hydrogen chloride content in the wastewater is 0.7-1 wt%), so that the environmental impact is larger.
Experimental results show that the hydrochloric acid analysis method provided by the invention is simpler in process, higher in analysis efficiency and environment-friendly, and the obtained hydrogen chloride is not lower than 86% in primary yield, not lower than 97.7% in comprehensive yield, not lower than 99% in purity, and higher in primary yield and purity.
Compared with the conventional analytic method, the analytic method process of the hydrochloric acid provided by the invention has a better separation effect, the waste water generated by concentration by the conventional method contains less than 1 wt% of hydrogen chloride, and the waste water removed by the method contains less than 0.5 wt% of hydrogen chloride.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (7)
1. A method for resolving hydrochloric acid comprises the following steps:
mixing hydrochloric acid with the mass fraction of 20-31% with anhydrous copper chloride for 6-60 min at normal temperature, and condensing the obtained gas at-30 to-10 ℃ to obtain hydrogen chloride gas.
2. The analytical method according to claim 1, wherein the mass ratio of the hydrochloric acid to the anhydrous copper chloride is 3 to 4: 9 to 10.
3. The analytic method according to claim 1, wherein mixing hydrochloric acid with a mass fraction of 20% to 31% with anhydrous copper chloride at room temperature for 0.1 to 1 hour is specifically:
dripping 20-31 wt% hydrochloric acid into anhydrous copper chloride, and mixing at normal temperature for 0.1-1 h.
4. The analysis method according to claim 1, wherein the obtained gas is condensed at-30 to-10 ℃ for 0.1 to 1 hour.
5. The analysis method according to claim 1, further comprising, after the mixing:
and drying the mixed copper chloride at 100-120 ℃ for 3-5 h, and collecting the removed hydrogen chloride and crystal water.
6. The desorption method according to claim 5, further comprising, after collecting the desorbed hydrogen chloride and crystal water:
and condensing and separating the collected hydrogen chloride and the crystal water to obtain hydrogen chloride gas.
7. The analysis method according to claim 6, wherein the temperature of the condensation is-30 to-10 ℃, and the time of the condensation is 3 to 5 hours.
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| CN202010057971.5A CN111170276A (en) | 2020-01-16 | 2020-01-16 | Hydrochloric acid analysis method |
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| CN202010057971.5A CN111170276A (en) | 2020-01-16 | 2020-01-16 | Hydrochloric acid analysis method |
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Citations (4)
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| US6968114B2 (en) * | 2003-04-17 | 2005-11-22 | Ut-Battelle, Llc | Cladding for high temperature optical component and method of making same |
| CN101215062A (en) * | 2007-12-26 | 2008-07-09 | 郝屿 | Method and system for reclaiming valuable resource in acidic etching waste liquid |
| CN101443115A (en) * | 2006-03-16 | 2009-05-27 | 巴斯福催化剂公司 | Exchange cation selection in ETS-4 to control adsorption strength and effective pore diameter |
| CN102516022A (en) * | 2011-12-06 | 2012-06-27 | 中南大学 | Comprehensive processing method of vinyl chloride synthetic gas |
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2020
- 2020-01-16 CN CN202010057971.5A patent/CN111170276A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6968114B2 (en) * | 2003-04-17 | 2005-11-22 | Ut-Battelle, Llc | Cladding for high temperature optical component and method of making same |
| CN101443115A (en) * | 2006-03-16 | 2009-05-27 | 巴斯福催化剂公司 | Exchange cation selection in ETS-4 to control adsorption strength and effective pore diameter |
| CN101215062A (en) * | 2007-12-26 | 2008-07-09 | 郝屿 | Method and system for reclaiming valuable resource in acidic etching waste liquid |
| CN102516022A (en) * | 2011-12-06 | 2012-06-27 | 中南大学 | Comprehensive processing method of vinyl chloride synthetic gas |
Non-Patent Citations (3)
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| 张向宇: "《实用化学手册》", 31 October 2011, 国防工业出版社 * |
| 张颖 等: "盐对盐酸-水体系气液平衡的影响", 《精细化工》 * |
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Application publication date: 20200519 |