CN113277474A - Preparation method of hydrogen chloride - Google Patents
Preparation method of hydrogen chloride Download PDFInfo
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- CN113277474A CN113277474A CN202110770205.8A CN202110770205A CN113277474A CN 113277474 A CN113277474 A CN 113277474A CN 202110770205 A CN202110770205 A CN 202110770205A CN 113277474 A CN113277474 A CN 113277474A
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- hydrogen chloride
- hydrochloric acid
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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
- C01B7/0731—Purification ; Separation of hydrogen chloride by extraction
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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
- C01B7/0712—Purification ; Separation of hydrogen chloride by distillation
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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
- C01B7/0731—Purification ; Separation of hydrogen chloride by extraction
- C01B7/0737—Purification ; Separation of hydrogen chloride by extraction hydrogen chloride being extracted
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Abstract
The invention discloses a preparation method of hydrogen chloride, and relates to the field of preparation of hydrogen chloride. Extracting the hydrochloric acid solution by using an extracting agent to obtain an oil phase containing hydrogen chloride, and then carrying out reduced pressure distillation on the oil phase containing the hydrogen chloride to obtain hydrogen chloride gas; the extractant is selected from fluorine-containing phosphate extractant. The fluorine-containing phosphate with small polarity and water solubility of a single component is used as an extracting agent, so that the loss of the extracting agent can be effectively avoided. The extractant can also solve the third phase problem in the extraction process, and the separation of hydrogen chloride can be effectively realized through the reduced pressure distillation of the organic extraction phase. The extraction production process is stable and environment-friendly, the loss of the extracting agent is low, and the phenomenon that organic substances volatilize to pollute hydrogen chloride gas in the distillation process of a multi-component organic extraction system is avoided.
Description
Technical Field
The invention relates to the field of preparation of hydrogen chloride, and particularly relates to a preparation method of hydrogen chloride.
Background
The recycling of waste hydrochloric acid is a problem of resource recycling which is urgently needed to be solved by industries such as titanium white, chlor-alkali, organic silicon and the like in the current hydrochloric acid method. The waste hydrochloric acid recycling technology comprises two aspects: firstly, the membrane filtration technology is adopted to remove impurities in the waste hydrochloric acid, and the method has the problems of high equipment cost, high operation cost, limited recovery rate of pure hydrochloric acid and the like; secondly, the waste hydrochloric acid is used as a raw material to prepare the hydrogen chloride, and the hydrogen chloride is recycled to the production process. The current technology mainly focuses on the research of hydrogen chloride preparation technology, and the hydrogen chloride preparation technology is divided into a distillation method and an extractive distillation method. Wherein, the hydrogen chloride gas can be obtained only by using hydrochloric acid with the concentration higher than 20 percent through conventional distillation; the deep desorption distillation needs to increase a boiling breaker and eliminate the azeotropic point of the hydrochloric acid and water to realize high recovery rate of the hydrogen chloride, but the deep desorption distillation has the problems of concentration of the waste breaker and operation and maintenance of process equipment.
The extractive distillation method adopts organic extractant to combine with hydrogen chloride directionally, then the organic phase rich in the organic solvent is distilled under reduced pressure to remove hydrogen chloride gas, and the organic phase is recycled. For example, Guangzhou chemical 2017.8(45) describes the extraction of hydrochloric acid with trioctylamine followed by distillation of the organic extract to extract hydrogen chloride from the hydrochloric acid. Although the separation can be achieved to a certain degree, the extractant is relatively serious in loss, too fast in loss and high in cost, and a third phase appears in the extraction process, so that the phase separation effect is influenced.
In view of this, the invention is particularly proposed.
Disclosure of Invention
The present invention aims to provide a method for preparing hydrogen chloride to solve the above technical problems.
The invention aims to provide a simple and convenient hydrogen chloride recovery method. The invention uses the fluorine-containing phosphate with small polarity and water solubility of a single component as an extracting agent, and can effectively avoid the loss of the extracting agent. The extractant can also solve the third phase problem in the extraction process, and the separation of hydrogen chloride can be effectively realized through the reduced pressure distillation of the organic extraction phase. The extraction production process is stable and environment-friendly, the loss of the extracting agent is low, and the phenomenon that organic substances volatilize to pollute hydrogen chloride gas in the distillation process of a multi-component organic extraction system is avoided.
The invention is realized by the following steps:
the invention provides a preparation method of hydrogen chloride, which comprises the following steps: extracting the hydrochloric acid solution by using an extracting agent to obtain an oil phase containing hydrogen chloride, and then carrying out reduced pressure distillation on the oil phase containing the hydrogen chloride to obtain hydrogen chloride gas; the extractant is selected from fluorine-containing phosphate extractant.
Hydrogen chloride is transferred from the hydrochloric acid solution system to an oil phase through a fluorine-containing phosphate extractant system, and the hydrogen chloride gas and an organic phase can be obtained by carrying out reduced pressure distillation on the oil phase containing the hydrogen chloride.
In one embodiment, the organic phase can be directly returned to the extractor for recycling.
In a preferred embodiment of the present invention, the hydrochloric acid solution is a waste hydrochloric acid solution, and the mass fraction of the waste hydrochloric acid solution is 5-30%.
In a preferred embodiment of the present invention, the mass fraction of the waste hydrochloric acid solution is 10-20%.
In a preferred embodiment of the present invention, the waste hydrochloric acid solution further contains impurity ions, and the impurity ions are at least one of titanium, manganese, vanadium, chromium, nickel, calcium, iron, or magnesium ions.
In a preferred embodiment of the present invention, the above-mentioned fluorinated phosphate extractant is selected from fluorinated phosphates represented by formula (I):
In a preferred embodiment of the present invention, the above-mentioned fluorinated phosphate extractant is selected from fluorinated phosphates represented by formula (I):
In a preferred embodiment of the present invention, the fluorine-containing phosphate ester-based extractant is selected from tris- (2.2.2-trifluoroethyl) phosphate and tris- (hexafluoroisopropyl) phosphate.
In a preferred embodiment of the present invention, the temperature of the reduced pressure distillation is 120-170 ℃.
In a preferred embodiment of the present invention, the temperature of the reduced pressure distillation is 120-140 ℃.
In a preferred embodiment of the present invention, the pressure of the reduced pressure distillation is-1 MPa to 0.01 MPa.
The invention has the following beneficial effects:
the invention provides a simple and convenient hydrogen chloride recovery method. Hydrogen chloride is transferred from the hydrochloric acid solution system to an oil phase through a fluorine-containing phosphate extractant system, and the hydrogen chloride gas can be obtained by carrying out reduced pressure distillation on the oil phase containing the hydrogen chloride. The inventor finds that the fluorine-containing phosphate with small polarity and water solubility of a single component is used as the extracting agent, so that the loss of the extracting agent can be effectively avoided. The extractant can also solve the third phase problem in the extraction process, and the separation of hydrogen chloride can be effectively realized through the reduced pressure distillation of the organic extraction phase. The extraction production process is stable and environment-friendly, the loss of the extracting agent is low, and the phenomenon that organic substances volatilize to pollute hydrogen chloride gas in the distillation process of a multi-component organic extraction system is avoided.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
FIG. 1 is a diagram showing the results of an extraction phase separation test.
Detailed Description
Reference will now be made in detail to embodiments of the invention, one or more examples of which are described below. Each example is provided by way of explanation, not limitation, of the invention. In fact, it will be apparent to those skilled in the art that various modifications and variations can be made in the present invention without departing from the scope or spirit of the invention. For instance, features illustrated or described as part of one embodiment, can be used on another embodiment to yield a still further embodiment.
The invention provides a preparation method of hydrogen chloride, which comprises the following steps: extracting the hydrochloric acid solution by using an extracting agent to obtain an oil phase containing hydrogen chloride, and then carrying out reduced pressure distillation on the oil phase containing the hydrogen chloride to obtain hydrogen chloride gas; the extractant is selected from fluorine-containing phosphate extractant.
Hydrogen chloride is transferred from the hydrochloric acid solution system to an oil phase through a fluorine-containing phosphate extractant system, and the hydrogen chloride gas and an organic phase can be obtained by carrying out reduced pressure distillation on the oil phase containing the hydrogen chloride.
In one embodiment, the organic phase can be directly returned to the extractor for recycling.
In a preferred embodiment of the present invention, the hydrochloric acid solution is a waste hydrochloric acid solution, and the mass fraction of the waste hydrochloric acid solution is 5-30%.
The inventors have found that when the mass fraction of the solute in the hydrochloric acid solution is in the above range, separation of hydrogen chloride can be easily achieved, and the extraction effect is good.
Optionally, the hydrochloric acid solution is 5%, 6%, 7%, 8%, 10%, 12%, 15%, 16%, 18%, 19%, 20%, 22%, 24%, 25%, 28%, or 30% by mass.
In a preferred embodiment of the present invention, the mass fraction of the waste hydrochloric acid solution is 10-20%. For example 12.5%, 13%, 13.5%, 15%, 16.5% or 20% by mass.
In a preferred embodiment of the present invention, the waste hydrochloric acid solution further contains impurity ions, and the impurity ions are at least one of titanium, manganese, vanadium, chromium, nickel, calcium, iron, or magnesium ions.
It should be noted that the content of a single impurity ion is less than 1 wt.%.
In a preferred embodiment of the present invention, the above-mentioned fluorinated phosphate extractant is selected from fluorinated phosphates represented by formula (I):
In a preferred embodiment of the present invention, the above-mentioned fluorinated phosphate extractant is selected from fluorinated phosphates represented by formula (I):
In a preferred embodiment of the present invention, the fluorine-containing phosphate ester-based extractant is selected from tris- (2.2.2-trifluoroethyl) phosphate and tris- (hexafluoroisopropyl) phosphate.
In a preferred embodiment of the present invention, the temperature of the reduced pressure distillation is 120-170 ℃.
In one embodiment, the reduced pressure distillation is performed at 120 ℃, 122 ℃, 125 ℃, 130 ℃, 135 ℃, 140 ℃, 145 ℃, 150 ℃, 155 ℃, 160 ℃, 165 ℃ or 170 ℃.
In a preferred embodiment of the present invention, the temperature of the reduced pressure distillation is 120-140 ℃.
In a preferred embodiment of the present invention, the pressure of the reduced pressure distillation is-1 MPa to 0.01 MPa. In one embodiment, the pressure of the reduced pressure distillation is-0.5 MPa to 0.01MPa, and in one embodiment, the pressure of the reduced pressure distillation is-0.1 MPa to 0.01 MPa.
It should be noted that in the extraction technology disclosed at present, the emulsification phenomenon is easy to occur when the organic phase ratio is too high, which results in incomplete layering, slow layering speed and even no layering; if the organic phase ratio is too low, the number of extraction stages is increased to improve the extraction efficiency of the objective substance. The oil-water ratio of the extraction process and the back extraction process provided by the invention is simple and easy to control, the back extraction ratio can be adjusted at will according to the extraction effect, the back extraction process is not limited by the ratio, and the extraction process is not influenced by the change of the ratio.
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The features and properties of the present invention are described in further detail below with reference to examples.
Example 1
This example provides a process for the preparation of hydrogen chloride. Specifically, a hydrochloric acid solution with a volume of 1000ml and a mass fraction of 5% is added into an extractor, the hydrochloric acid solution contains 0.01 wt.% of iron ions, tris- (2.2.2-trifluoroethyl) phosphate is used as an extracting agent at 30 ℃, an oil-water phase ratio O/a is set to 1:1 in the example, and an oil-rich phase is obtained through 3-stage extraction. Then, the mixture is subjected to reduced pressure distillation in a distillation kettle at the temperature of 120 ℃ and the pressure of-0.1 MPa to obtain hydrogen chloride gas, and the organic phase returns to the extractor.
Example 2
This example provides a process for the preparation of hydrogen chloride. Specifically, a hydrochloric acid solution with a volume of 1000ml and a mass fraction of 20% is added into an extractor, the hydrochloric acid solution contains 0.01 wt% of iron ions and 0.01 wt% of calcium ions, tris- (2.2.2-trifluoroethyl) phosphate is used as an extracting agent at 30 ℃, an oil phase and water phase ratio O/A is set to be 1:1 in the embodiment, an oil-rich phase is obtained through 3-stage extraction, then reduced pressure distillation is carried out in a distillation kettle at 140 ℃ and under-0.1 MPa to obtain hydrogen chloride gas, and an organic phase returns to the extractor.
Example 3
The only difference compared to example 1 is that the extractant in this example is tris- (hexafluoroisopropyl) phosphate.
Example 4
Adding 1000ml of 30% hydrochloric acid solution with a mass fraction of 0.01 wt.% of iron ions and 0.005 wt.% of calcium ions in the hydrochloric acid solution into an extractor, setting the ratio of oil phase to water phase to O/A to 1:1 in the example by using tris- (2.2.2-trifluoroethyl) phosphate as an extracting agent at 30 ℃, and performing 3-stage extraction to obtain an oil-rich phase. Then, the mixture is subjected to reduced pressure distillation in a distillation kettle at the temperature of 120 ℃ and the pressure of-0.1 MPa to obtain hydrogen chloride gas, and the organic phase returns to the extractor.
Example 5
Adding 1000ml of 30% hydrochloric acid solution with a mass fraction of 0.01 wt.% of iron ions and 0.005 wt.% of calcium ions in the hydrochloric acid solution into an extractor, setting the ratio of oil phase to water phase to O/A to 3:1 in the example by using tris- (2.2.2-trifluoroethyl) phosphate as an extracting agent at 30 ℃, and performing 3-stage extraction to obtain an oil-rich phase. Then, carrying out reduced pressure distillation in a distillation kettle at the temperature of 160 ℃ and the pressure of-1 MPa to obtain hydrogen chloride gas, and returning an organic phase to an extractor.
Example 6
Adding 1000ml of 30% hydrochloric acid solution with a mass fraction of 0.01 wt.% of iron ions and 0.005 wt.% of calcium ions in the hydrochloric acid solution into an extractor, setting the ratio of oil phase to water phase to O/A to 3:1 in the example by using tris- (2.2.2-trifluoroethyl) phosphate as an extracting agent at 30 ℃, and performing 4-stage extraction to obtain an oil-rich phase. Then, the mixture is subjected to reduced pressure distillation in a distillation kettle at the temperature of 170 ℃ and under the pressure of 0.01MPa to obtain hydrogen chloride gas, and the organic phase returns to the extractor.
Comparative example 1
Adding 1000ml of hydrochloric acid solution with the mass fraction of 2% into an extractor, wherein the hydrochloric acid solution contains 0.01 wt% of iron ions and 0.005 wt% of calcium ions, and at 30 ℃, taking tris- (2.2.2-trifluoroethyl) phosphate as an extracting agent, setting the oil-water phase ratio O/A to be 1:1 in the embodiment, and performing 1-stage extraction to obtain an oil-rich phase. Then, the mixture is subjected to reduced pressure distillation in a distillation kettle at the temperature of 120 ℃ and the pressure of-0.1 MPa to obtain hydrogen chloride gas, and the organic phase returns to the extractor.
The method has low extraction efficiency and low recovery significance.
Comparative example 2
The difference compared to example 1 is only the choice of extractant, the other conditions being the same.
The extractant in this example is trioctylamine.
Experimental example 1
This example performed a shake flask extraction test on the funnel contents after grade 3 extraction in example 1 and comparative example 2. Mix in a separatory funnel for the same amount of time and then stand until the two phases separate. It can be seen from the phase separation condition and the phase separation time that the embodiment has better phase separation speed and clear phase separation interface without the third phase (refer to the figure 1), while the method of the comparative example 2 has unclear phase separation interface. For the fluorine-containing phosphate, the polarity of the phosphate is very small due to the introduction of fluorine, and after the phosphate is mixed with acid, the phosphate and the acid can be quickly separated, and the phase separation time is not greatly different. The embodiments are shown by way of example.
Experimental example 2
In order to detect the loss of the extractant in the extraction system, the hydrogen chloride gas obtained in examples 1 and 2 was neutralized with 30% sodium hydroxide solution until neutral, and the resulting solution was taken out for the COD tester test (COD data is shown in table 1). The test data indicated that COD data was not detected.
TABLE 1COD data
| Serial number | TOC(mg/L) | COD(mg/L) |
| Example 1 | 2 | 10 |
| Example 2 | 1 | 8 |
| Comparative example 2 | 500 | 2100 |
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. 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 method for producing hydrogen chloride, comprising: extracting the hydrochloric acid solution by using an extracting agent to obtain an oil phase containing hydrogen chloride, and then carrying out reduced pressure distillation on the oil phase containing the hydrogen chloride to obtain hydrogen chloride gas; the extractant is selected from fluorine-containing phosphate ester extractants.
2. The method according to claim 1, wherein the hydrochloric acid solution is a waste hydrochloric acid solution, and the mass fraction of the waste hydrochloric acid solution is 5 to 30%.
3. The method according to claim 2, wherein the mass fraction of the waste hydrochloric acid solution is 10 to 20%.
4. The method according to claim 2, wherein the waste hydrochloric acid solution further contains impurity ions.
5. The method of claim 1, wherein the fluorine-containing phosphate extractant is selected from fluorine-containing phosphates represented by formula (I):
6. The method according to claim 5, wherein the fluorine-containing phosphate ester extractant is selected from fluorine-containing phosphate esters represented by formula (I):
7. The method according to claim 5 or 6, wherein the fluorine-containing phosphate ester-based extractant is selected from tris- (2.2.2-trifluoroethyl) phosphate and tris- (hexafluoroisopropyl) phosphate.
8. The method as claimed in claim 1, wherein the temperature of the reduced pressure distillation is 120-170 ℃.
9. The method as claimed in claim 8, wherein the temperature of the reduced pressure distillation is 120-140 ℃.
10. The method for producing hydrogen chloride according to claim 8, wherein the pressure of the reduced pressure distillation is from-1 MPa to 0.01 MPa.
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2021
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