CN102774811A - Method for preparing hydrogen chloride gas from hydrochloric acid solution - Google Patents
Method for preparing hydrogen chloride gas from hydrochloric acid solution Download PDFInfo
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- CN102774811A CN102774811A CN201210244799XA CN201210244799A CN102774811A CN 102774811 A CN102774811 A CN 102774811A CN 201210244799X A CN201210244799X A CN 201210244799XA CN 201210244799 A CN201210244799 A CN 201210244799A CN 102774811 A CN102774811 A CN 102774811A
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- hydrochloric acid
- hydrogen chloride
- chloride gas
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Abstract
The invention belongs to the technical field of preparation methods in inorganic chemical industry, and particularly relates to a method for preparing hydrogen chloride gas from hydrochloric acid solution. The basic technique is implemented in a way that: an extractant is utilized to extract hydrochloric acid solution at normal temperature, so that chlorine hydride and a small amount of water enter the extractant phase; after the extractant phase is dewatered, rectification is carried out to release the hydrogen chloride gas, wherein the extractant can be recycled; and a neutral phosphorus organic substance, which contains a phosphorus-oxygen double bond, is used as a complexing agent, and can be used for complexing extraction on the hydrochloric acid due to the strong electronegativity of the oxygen atom. The extractant has moderate acting force on the hydrochloric acid, so that the hydrochloric acid can be effectively extracted into the organic phase and easily separated from the organic phase, and chlorine hydride escapes from the organic phase in the form of gas. The method is simple and effective, and has wide application range.
Description
Technical field
The invention belongs to inorganic chemical industry preparation method technical field, particularly a kind of method of from hydrochloric acid soln, producing hydrogen chloride gas.
Background technology
Can produce a large amount of low concentration of salt acid solutions in association areas such as medicine, iron and steel and inorganic chemical industries,, directly be used for very difficulty of Industrial processes because the concentration ratio of acid is lower.For with the hydrochloric acid recycling, can adopt rectifying or method of extraction to be achieved.
Conventional distillation is difficult to obtain concentration of hydrochloric acid and is higher than the solution of 20.2 wt%, thereby proposes various improved methods in succession, like variable-pressure rectification, with salt rectifying and sulfuric acid extracting rectifying etc.HCl-H under the different pressures
2The azeotrope of O system is formed different, and the water through in the stage variable pressure rectifying separation Hydrogen chloride can obtain concentrated hydrochloric acid.The metal chloride that in dilute hydrochloric acid solution, adds high density in the rectifying is (like MgCl
2), can change azeotropic point and form, thereby obtain concentrated hydrochloric acid solution.Bibliographical information is also arranged, in dilute hydrochloric acid solution, add the vitriol oil, can improve HCl H
2The relative volatility of O obtains hydrogen chloride gas through rectifying.Aforesaid method operation inconvenience, higher to equipment requirements, and also energy consumption is big.
Hydrochloric acid is extracted, and extraction agent commonly used has primary isoamyl alcohol and tertiary amine.Primary isoamyl alcohol and hydrochloric acid reactive force are moderate, can extract a certain amount of water simultaneously, yet extraction agent pass through processes such as rectifying mutually, still can only obtain dilute hydrochloric acid solution.The ability of tertiary amine extraction hydrochloric acid is stronger, for avoiding occurring third phase, adopts polar organic matter as thinner usually.Behind the tertiary amine extraction hydrochloric acid, be difficult to reclaim hydrochloric acid through modes such as washing, rectifying.Though patent US4115530 proposes to adopt nonpolar organic matter as thinner, can obtain hydrogen chloride gas mutually through the rectifying extraction agent, consequent third phase can be unfavorable to extraction process.
Summary of the invention
Not enough to prior art, the invention provides a kind of method of from hydrochloric acid soln, producing hydrogen chloride gas.
A kind of method of from hydrochloric acid soln, producing hydrogen chloride gas is characterized in that, the concrete steps of this method are following:
(1) preparation extraction agent: adopting the neutral phosphonic type organic is complexing agent, and complexing agent and mixing diluents are stirred, and wherein the volume(tric)fraction of complexing agent is 10% ~ 100%;
(2) extraction hydrochloric acid: extraction hydrochloric acid soln under normal temperature and pressure conditions, separate obtaining the extraction agent phase, the volume ratio of extraction agent and hydrochloric acid soln is 0.02 ~ 50 in the extraction process;
(3) reclaim extraction agent: extraction phase is dewatered through the mode of warm air bubbling or rectifying, discharge hydrogen chloride gas through multistage rectification or distillation again.
Said neutral phosphonic type organic is one or more in SULPHOSUCCINIC ACID ESTER, phosphonic acid ester, phosphinate and the trialkylphosphine oxide; The structural formula of said SULPHOSUCCINIC ACID ESTER, phosphonic acid ester, phosphinate and trialkylphosphine oxide is respectively
,
,
and
, and wherein R, R' or R'' are H or C1 ~ C12 alkyl.
Said thinner is one or more in halogenated aryl hydrocarbon, C8 ~ C12 ether, C4 ~ C10 alcohol, C4 ~ C10 ester, kerosene and the gasoline of halogenated alkane, C6 ~ C12 aromatic hydrocarbons, C6 ~ C12 of C4 ~ C16 alkane, C1 ~ C16.
The massfraction of hydrochloric acid is not higher than 40% in the said hydrochloric acid soln.
The dispose procedure of said hydrogen chloride gas carries out under the condition of normal pressure, decompression or inert gas purge.
Beneficial effect of the present invention is:
Basic technology of the present invention is for adopting extraction agent normal temperature extraction hydrochloric acid soln, and hydrogenchloride and less water get into the extraction agent phase.Behind the extraction agent phase dehydration, discharge hydrogen chloride gas through rectifying, extraction agent can be recycled.The two keys of the phosphorous oxygen of neutral Phosphorus organic cpds, wherein the Sauerstoffatom electronegativity is more intense, can carry out complexometric extraction to hydrochloric acid.This kind of extractants and hydrochloric acid reactive force are moderate, and hydrochloric acid can be extracted into organic phase effectively, also separates from organic phase than being easier to, and hydrogenchloride is overflowed from organic phase with gas form.This method is simple effectively, the scope of application is extensive.
Description of drawings
Fig. 1 is a kind of process flow diagram of from hydrochloric acid soln, producing the method for hydrogen chloride gas.
Embodiment
The invention provides a kind of method of from hydrochloric acid soln, producing hydrogen chloride gas, the present invention is further specified below in conjunction with accompanying drawing and embodiment.
Embodiment 1
Using 50 mL volume(tric)fractions is that 50% trialkylphosphine oxide (TRPO)+50% N-BUTYL ACETATE mixing solutions is extraction agent, extracts 50 mL massfractions and be 11% hydrochloric acid soln, and the concentration of hydrochloric acid of the extraction agent phase that obtains is 0.72 mol/L, behind the extraction agent phase dehydration, at N
2Carry out reflux distillation 4 h under the purging condition, concentration of hydrochloric acid is lower than 0.1 mol/L in the extraction phase, and extraction agent is able to reclaim.Extract hydrochloric acid soln once more with extraction agent, its extracting power is constant basically.
Embodiment 2
Using 50 mL volume(tric)fractions is that 60% trialkylphosphine oxide (TRPO)+40% dodecyl mixing solutions is extraction agent; Extract 50 mL massfractions and be 10% hydrochloric acid soln; The concentration of hydrochloric acid of the extraction agent phase that obtains is 0.78 mol/L, after the extraction phase dehydration, distills 40 min in the condition of normal pressure refluxed; The middle mutually concentration of hydrochloric acid of extraction agent is 0.12 mol/L, and extraction agent is able to reclaim.Extract hydrochloric acid soln once more with extraction agent, its extracting power is constant basically.
Embodiment 3
Using 50 mL volume(tric)fractions is that TOPO (TOPO)+60%1-chlorodecane mixing solutions of 40% is extraction agent; Extract 50 mL massfractions and be 8% hydrochloric acid soln; The concentration of hydrochloric acid of the extraction agent phase that obtains is 0.53 mol/L, after the extraction phase dehydration, distills 30 min in the condition of normal pressure refluxed; The middle mutually concentration of hydrochloric acid of extraction agent is 0.13 mol/L, and extraction agent is able to reclaim.Extract hydrochloric acid soln once more with extraction agent, its extracting power is constant basically.
Embodiment 4
Using 50 mL volume(tric)fractions is that 50% trialkylphosphine oxide (TRPO)+50% nonane mixing solutions is extraction agent; Extract 50 mL massfractions and be 15% hydrochloric acid soln; The concentration of hydrochloric acid of the extraction agent phase that obtains is 0.67 mol/L, after the extraction phase dehydration, distills 1 h in the reduced pressure refluxed; The middle mutually concentration of hydrochloric acid of extraction agent is 0.07 mol/L, and extraction agent is able to reclaim.Extract hydrochloric acid soln once more with extraction agent, its extracting power is constant basically.
Embodiment 5
Using 50 mL volume(tric)fractions is that 45% TOPO (TOPO)+55% sulfonated kerosene mixing solutions is extraction agent; Extract 50 mL massfractions and be 12% hydrochloric acid soln; The concentration of hydrochloric acid of the extraction agent phase that obtains is 0.67 mol/L, after the extraction phase dehydration, distills 1 h in the condition of normal pressure refluxed; The middle mutually concentration of hydrochloric acid of extraction agent is 0.09 mol/L, and extraction agent is able to reclaim.Extract hydrochloric acid soln once more with extraction agent, its extracting power is constant basically.
Claims (5)
1. a method of from hydrochloric acid soln, producing hydrogen chloride gas is characterized in that, the concrete steps of this method are following:
(1) preparation extraction agent: adopting the neutral phosphonic type organic is complexing agent, and complexing agent and mixing diluents are stirred, and wherein the volume(tric)fraction of complexing agent is 10% ~ 100%;
(2) extraction hydrochloric acid: extraction aqueous hydrochloric acid under normal temperature and pressure conditions, separate obtaining the extraction agent phase, the volume ratio of extraction agent and hydrochloric acid soln is 0.02 ~ 50 in the extraction process;
(3) reclaim extraction agent: extraction phase is dewatered through warm air bubbling or rectifying mode, discharge hydrogen chloride gas through multistage rectification or distillation again.
2. a kind of method of from hydrochloric acid soln, producing hydrogen chloride gas according to claim 1; It is characterized in that: said neutral phosphonic type organic is one or more in SULPHOSUCCINIC ACID ESTER, phosphonic acid ester, phosphinate and the trialkylphosphine oxide; The structural formula of said SULPHOSUCCINIC ACID ESTER, phosphonic acid ester, phosphinate and trialkylphosphine oxide is respectively
,
,
and
, and wherein R, R' or R'' are H or C1 ~ C12 alkyl.
3. a kind of method of from hydrochloric acid soln, producing hydrogen chloride gas according to claim 1 is characterized in that: said thinner is one or more in halogenated aryl hydrocarbon, C8 ~ C12 ether, C4 ~ C10 alcohol, C4 ~ C10 ester, kerosene and the gasoline of halogenated alkane, C6 ~ C12 aromatic hydrocarbons, C6 ~ C12 of C4 ~ C16 alkane, C1 ~ C16.
4. a kind of method of from hydrochloric acid soln, producing hydrogen chloride gas according to claim 1, it is characterized in that: the massfraction of hydrochloric acid is not higher than 40% in the said hydrochloric acid soln.
5. a kind of method of from hydrochloric acid soln, producing hydrogen chloride gas according to claim 1, it is characterized in that: the dispose procedure of said hydrogen chloride gas carries out under the condition of normal pressure, decompression or inert gas purge.
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|---|---|---|---|
| CN201210244799XA CN102774811A (en) | 2012-07-13 | 2012-07-13 | Method for preparing hydrogen chloride gas from hydrochloric acid solution |
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|---|---|---|---|
| CN201210244799XA CN102774811A (en) | 2012-07-13 | 2012-07-13 | Method for preparing hydrogen chloride gas from hydrochloric acid solution |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104058369A (en) * | 2014-06-26 | 2014-09-24 | 四川宇丰化工材料有限公司 | Method for recovering and treating hydrochloric acid contained in polyvinyl butyral production wastewater |
| CN113277474A (en) * | 2021-07-07 | 2021-08-20 | 福建富仕新材料有限责任公司 | Preparation method of hydrogen chloride |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1125630A (en) * | 1995-08-28 | 1996-07-03 | 山东大学 | Purification method of by-product hydrobromic acid |
| CN102502500A (en) * | 2011-11-07 | 2012-06-20 | 韩扶军 | Device for producing hydrogen chloride by resolving hydrochloric acid |
-
2012
- 2012-07-13 CN CN201210244799XA patent/CN102774811A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1125630A (en) * | 1995-08-28 | 1996-07-03 | 山东大学 | Purification method of by-product hydrobromic acid |
| CN102502500A (en) * | 2011-11-07 | 2012-06-20 | 韩扶军 | Device for producing hydrogen chloride by resolving hydrochloric acid |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104058369A (en) * | 2014-06-26 | 2014-09-24 | 四川宇丰化工材料有限公司 | Method for recovering and treating hydrochloric acid contained in polyvinyl butyral production wastewater |
| CN104058369B (en) * | 2014-06-26 | 2016-07-06 | 四川宝利丰科技有限公司 | Polyvinyl butyral resin produces the HCl recovery processing method in waste water |
| CN113277474A (en) * | 2021-07-07 | 2021-08-20 | 福建富仕新材料有限责任公司 | Preparation method of hydrogen chloride |
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Application publication date: 20121114 |