IE46474B1 - Process for the separation of sulphuric acid and hydriodic acid - Google Patents
Process for the separation of sulphuric acid and hydriodic acidInfo
- Publication number
- IE46474B1 IE46474B1 IE462/78A IE46278A IE46474B1 IE 46474 B1 IE46474 B1 IE 46474B1 IE 462/78 A IE462/78 A IE 462/78A IE 46278 A IE46278 A IE 46278A IE 46474 B1 IE46474 B1 IE 46474B1
- Authority
- IE
- Ireland
- Prior art keywords
- organic solvent
- sulphur dioxide
- acid
- sulphuric acid
- water
- Prior art date
Links
- 238000000034 method Methods 0.000 title claims abstract description 21
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 title claims abstract description 13
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 title claims abstract description 9
- 238000000926 separation method Methods 0.000 title claims description 11
- 235000011149 sulphuric acid Nutrition 0.000 title claims description 11
- 239000001117 sulphuric acid Substances 0.000 title claims description 9
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000007788 liquid Substances 0.000 claims abstract description 16
- 239000003960 organic solvent Substances 0.000 claims abstract description 12
- 239000000203 mixture Substances 0.000 claims abstract description 10
- 150000005215 alkyl ethers Chemical class 0.000 claims abstract description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical group CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 24
- 229910001868 water Inorganic materials 0.000 claims description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- 238000006243 chemical reaction Methods 0.000 claims description 10
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 8
- 239000004291 sulphur dioxide Substances 0.000 claims description 8
- 235000010269 sulphur dioxide Nutrition 0.000 claims description 8
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 7
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims description 6
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 4
- 229910052739 hydrogen Inorganic materials 0.000 claims description 4
- 239000001257 hydrogen Substances 0.000 claims description 4
- 229910052760 oxygen Inorganic materials 0.000 claims description 4
- 239000001301 oxygen Substances 0.000 claims description 4
- FDPIMTJIUBPUKL-UHFFFAOYSA-N pentan-3-one Chemical compound CCC(=O)CC FDPIMTJIUBPUKL-UHFFFAOYSA-N 0.000 claims description 4
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 claims description 2
- NTIZESTWPVYFNL-UHFFFAOYSA-N Methyl isobutyl ketone Chemical compound CC(C)CC(C)=O NTIZESTWPVYFNL-UHFFFAOYSA-N 0.000 claims description 2
- UIHCLUNTQKBZGK-UHFFFAOYSA-N Methyl isobutyl ketone Natural products CCC(C)C(C)=O UIHCLUNTQKBZGK-UHFFFAOYSA-N 0.000 claims description 2
- 239000011630 iodine Substances 0.000 claims description 2
- 229910052740 iodine Inorganic materials 0.000 claims description 2
- 229960004132 diethyl ether Drugs 0.000 claims 4
- 125000005907 alkyl ester group Chemical group 0.000 claims 1
- -1 alkyl ketones Chemical class 0.000 claims 1
- YNQLUTRBYVCPMQ-UHFFFAOYSA-N alpha-methyl toluene Natural products CCC1=CC=CC=C1 YNQLUTRBYVCPMQ-UHFFFAOYSA-N 0.000 claims 1
- 238000007132 Bunsen reaction Methods 0.000 abstract description 6
- 150000002148 esters Chemical class 0.000 abstract description 2
- 150000002576 ketones Chemical class 0.000 abstract description 2
- 229940071870 hydroiodic acid Drugs 0.000 abstract 1
- 238000005406 washing Methods 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- 229940035423 ethyl ether Drugs 0.000 description 3
- 239000000376 reactant Substances 0.000 description 3
- 125000000217 alkyl group Chemical group 0.000 description 2
- 125000004432 carbon atom Chemical group C* 0.000 description 2
- 150000002894 organic compounds Chemical class 0.000 description 2
- 241001230134 Phasis Species 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 229940125904 compound 1 Drugs 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229940093499 ethyl acetate Drugs 0.000 description 1
- 235000019439 ethyl acetate Nutrition 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 1
- 238000009533 lab test Methods 0.000 description 1
- WSGCRAOTEDLMFQ-UHFFFAOYSA-N nonan-5-one Chemical compound CCCCC(=O)CCCC WSGCRAOTEDLMFQ-UHFFFAOYSA-N 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/69—Sulfur trioxide; Sulfuric acid
- C01B17/90—Separation; Purification
-
- 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
- C01B7/13—Iodine; Hydrogen iodide
- C01B7/135—Hydrogen iodide
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Detergent Compositions (AREA)
Abstract
The present invention relates to a process for separating sulfuric acid and hydroiodic acid resulting from a Bunsen reaction carried out in liquid sulfur dioxide.
According to this process, this liquid is mixed with organic solvents chosen from the group formed by the lower alkyl ethers, the ketones, the esters or mixtures thereof.
Description
This invention relates to a process for the separation of sulphuric acid and hydriodic acid.
According to the present invention there is provided a process for the separation of sulphuric acid and hydriodic acid from a mixture containing them which process comprises bringing together the said mixture, liquid sulphur dioxide and at least one organic solvent whereby two phases are formed, one of said phases comprising liquid sulphur dioxide, organic solvent and hydriodic acid and the other of said phases comprising sulphuric acid. The invention also includes within its scope a method of preparing hydrogen and/or oxygen from water when employing the above-mentioned separation process.
It is known to decompose water into hydrogen and oxygen using thermal energy only, by way of a cycle of chemical reactions.
One proposed cycle has the following steps:
1) S02 + 2H2O + I2-> 2HI + H2SO4
2) 2HI-).H2 + I2
3) H2SO4->H20 + SO2 + 1/2 02
The first reaction, known as the Bunsen reaction, runs at room temperature? the second at 400°C or above and the third at
650° C or above. The Bunsen reaction, however, cannot be completed because at a moderate sulphuric, acid concentration it reaches an equilibrium. Moreover, it is very difficult to separate HI and H2S04 from each other.
The overall reaction of the above cycle is Η,,Ο—) + 1/2 02 if all reactants are recycled into the cycle.
However,as has been said, a problem is the separation of H2SO^ and HX resulting from the Bunsen reaction.
In Patent Specification No. 44444 we propose to perform the Bunsen reaction in liquid S02 as a solvent. In liquid SO,, sulphuric acid is almost insoluble, so that during the reaction two separated layers are formed. One layer contains liquid SOj, I2, a limited amount of water and HI (the sulphurous phase).
The other layer contains at the outset only concentrated HjSO^ (the sulphuric phase). When an excess of water is added this latter phase will be diluted with water and then most of the HI present in the sulphurous phase will dissolve in the sulphuric phase.
It has been found that a better separation of H2S°4 and HI in the two layers can be effected when an organic solvent preferably selected from lower alkyl ethers, esters and ketones or mixtures thereof, is added to the sulphurous phase. By lower alkyl'1 in accordance with this specification is meant alkyl containing not more than eight carbon atoms and preferably not more than four carbon atoms. The separation of both acids can be completed by washing the sulphurous phase, after completion of the reaction, with a small amount of water, to eliminate the rest of the H2S0^ therefrom. This washing water can then be used as reactant water in the Bunsen reaction.
It is preferred to use organic solvents which are completely soluble in liquid SC>2 and only slightly soluble in water.
In laboratory experiments which are described hereafter by way of example of embodiments of the invention, liquid SC>2 (boiling point -10. 2°e) was charged to a separation funnel and the iodine and organic solvent added. To the dark brown reactant mixture water was added dropwise. The reaction was complete when the solution had become colourless. The resulting layers were separa ted and the sulphurous layer was washed with a small amount of water. It is also possible to separate the sulphuric layer from the sulphurous one during the reaction, before it is completed.
The following table shows by way of example the results of some experiments.
Run Composition of starting solution ml water added for complete reac. (ml) SO 2 g *2 g organic compound ml other organic compound 1 100 10 Ethylether 30 - - 14 2 · 11 II 40 - - 14 3 II '· II 50 - - 14 4 II II II 75 - - 14 5 li II II 100 - - 13.5 6 II II 11 150 - - 13.5 7 II il II 100 - - 13.5 8 II II II 50 - - 13.5 9 II 75 - - 14 10 II II 75 - - 14 11 II II il 75 - - 14 12 II II Methylethyl Ketone 30 — 18.7 13 II II Diethyl Ketone 50 - 18.5 14 11 II M.I.B.K. 50 - - 20 15 II ll Ethylether 30 Ethyl- acetate 70 16.5 16 II II 75 Benzene 7.5 14 17 II II II 60 Benzene 6.0 14 18 II II II 60 M.I.B.K. 8.0 14 19 II II II 30 Acetone 5.0 14 20 II Acetone 20 - - 14 21 58 It Ethylether 50 - - 14 22 45 II II 50 - - 17 23 38 II II 50 - - 20 24 100 II II 50 - - 14 25 100 15 II 50 - - 25 26 100 20 II 50 - - 37 )
4647 4
Table (Continued)
water added for wash. (ml) temperature sulphuric phase solutic J washing phasi n solution = suIphurous phase solution react. (°C) separat. (°C)H2S°4 g HI gH2S°4 g HI gH2S°4 g : hi g 2 -10 -10 3.276 0.112 0.072 0.092 0.720 9.920 2 It II 3.355 0.143 0.046 0.084 0.644 9.824 2 II II 3.630 0.070 0.173 0.100 0.215 9.980 2 It 3.469 0.031 0.259 0.064 0.313 9.850 2 II II 3.453 0.028 0.327 0.046 0.230 10.048 2 II It 3.150 0.090 0.370 0.110 0.597 9.830 - II -20 3.724 0.051 - - 0.137 10.110 - II II 3.783 0.128 - - 0.280 .9.930 4 It -5 3.531 0.043 0.237 0.128 0.100 9.677 4 II -12 3.606 0.028 0.356 0.360 0.027 9.580 4 ' -17 3.550 0.039 0.363 0.142 0.039 10.040 - It -10 3.500 0.455 - - 0.466 9.690 4 II ft 3.740 0.468 0.270 0.660 - 8.990 - II -20 3.895 1.430 - - - 2 '· -20 3.763 nihil 0.362 nihil nihil 9.88 4 II -10 3.724 0.090 0.190 0.497 0.016 8.455 4 II It 3.784 0.098 0.137 0.308 0.046 9.80 4 II 3.822 0.063 0.182 0.203 nihil 9.843 4 II ΙΓ 3.092 0.153 0.882 0.576 0.120 9.286 4 II II 3.410 0.152 0.310 0.125 0.125 9.849 4 11 II 3.471 0.033 0.516 0.149 0.073 10.00 4 II II 3.760 0.075 0.310 0.239 nihil 9.75 4 II ii 3.997 0.181 0.207 0.366 0.029 9.548 4 It II 3.606 0.028 0.356 0.360 0.027 9.580 5 II 5.798 0.366 0.247 0.734 - 13.89 5 - II tl 7.602 1.657 0.289 0.960 0:230 17.60
Explanation of the numerals appearing at the side of the table:- 1) The reaction was not yet complete. 2) In the washing process 20 ml of diethyl ether was added. 3) M.I.B.K is methyl isobutyl ketone.
- 7 butyl ketone.
From the table it can be seen that a very low temperature in the separation step has a favourable effect on the separation of H2SO4 and Hl. The solubility of the first acid in liquid S02 decreases rapidly when the temperature is lowered (runs 7, 8, 11 and 15).
Furthermore, runs 3, 4 and 5 show that the effect of the use of diethyl ether is optimal if it is used in a ratio to liquid S02 between 1:1 and 0.5:1.
Claims (10)
1. A process for the separation of sulphuric acid and hydriodic acid from a mixture containing them which process comprises bringing together the said mixture, liquid sulphur dioxide and at least one organic solvent whereby two phases are formed, one of said phases comprising liquid sulphur dioxide, organic solvent and hydriodic acid and the other of said phases comprising sulphuric acid.
2. A process as claimed in claim 1 wherein the mixture of sulphuric acid and hydriodic acid is formed by reacting together sulphur dioxide, water and iodine.
3. A process as claimed in claim 2 wherein the said reaction forms part of a cycle of chemical reactions whose overall result is to decompose water into hydrogen and oxygen.
4. A process as claimed in any one of the preceding claims wherein the organic solvent is completely soluble in liquid sulphur dioxide but only slightly soluble in water.
5. A process as claimed in claim 4 wherein the organic solvent is selected from lower alkyl ethers, lower alkyl esters and lower alkyl ketones.
6. A process as claimed in any one of claims 1 to 3 wherein the organic solvent is selected from diethylether, acetone, methylethyl ketone, diethyl ketone, methyl isobutyl ketone, ethyl acetate and benzene, and mixtures thereof.
7. A process as claimed in claim 6 wherein the organic solvent is diethyl ether and wherein the proportion of diethyl ether to liquid sulphur dioxide is from 0.5 to 1.0 ml of diethyl ether to 1 g of liquid sulphur dioxide.
8. A process as claimed in any one of the preceding claims
9. A process as claimed in claim 8 when performed at a temperature no higher than -15°C. 10. A process as claimed in claim 1 substantially as 5 hereinbefore described in any one of the specific examples. 11. Sulphuric acid and hydriodic acid whenever separated by a process as claimed in any one of the preceding claims. 12. Hydrogen whenever prepared by a process as claimed in claim 3. - 9 when performed at a temperature no higher than -12° C.
10. 13. Oxygen whenever prepared by a process as claimed in claim 3.
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| GB14941/77A GB1577630A (en) | 1977-04-07 | 1977-04-07 | Process for the separation of sulphuric acid and hydriodic acid |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| IE780462L IE780462L (en) | 1978-10-07 |
| IE46474B1 true IE46474B1 (en) | 1983-06-29 |
Family
ID=10050245
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| IE462/78A IE46474B1 (en) | 1977-04-07 | 1978-03-07 | Process for the separation of sulphuric acid and hydriodic acid |
Country Status (9)
| Country | Link |
|---|---|
| BE (1) | BE865690A (en) |
| DE (1) | DE2815593C2 (en) |
| DK (1) | DK145878A (en) |
| FR (1) | FR2386480A1 (en) |
| GB (1) | GB1577630A (en) |
| IE (1) | IE46474B1 (en) |
| IT (1) | IT1102477B (en) |
| LU (1) | LU79382A1 (en) |
| NL (1) | NL7803696A (en) |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2339330A (en) * | 1942-04-08 | 1944-01-18 | Colgate Palmolive Peet Co | Preparing anhydrous hydrogen halides |
| US3333924A (en) * | 1964-01-10 | 1967-08-01 | Hazen Research | Recovery of acids |
| JPS547515B2 (en) * | 1974-04-27 | 1979-04-07 | ||
| DE2634662A1 (en) * | 1975-08-04 | 1977-02-17 | Gen Atomic Co | PROCESS FOR THE THERMOCHEMICAL PRODUCTION OF HYDROGEN |
-
1977
- 1977-04-07 GB GB14941/77A patent/GB1577630A/en not_active Expired
-
1978
- 1978-03-07 IE IE462/78A patent/IE46474B1/en unknown
- 1978-03-31 IT IT48702/78A patent/IT1102477B/en active
- 1978-03-31 DK DK145878A patent/DK145878A/en not_active Application Discontinuation
- 1978-04-04 FR FR7809928A patent/FR2386480A1/en active Granted
- 1978-04-05 BE BE1008812A patent/BE865690A/en not_active IP Right Cessation
- 1978-04-05 LU LU79382A patent/LU79382A1/en unknown
- 1978-04-06 NL NL7803696A patent/NL7803696A/en not_active Application Discontinuation
- 1978-04-07 DE DE2815593A patent/DE2815593C2/en not_active Expired
Also Published As
| Publication number | Publication date |
|---|---|
| IT7848702A0 (en) | 1978-03-31 |
| IT1102477B (en) | 1985-10-07 |
| IE780462L (en) | 1978-10-07 |
| DE2815593C2 (en) | 1986-12-18 |
| BE865690A (en) | 1978-07-31 |
| FR2386480A1 (en) | 1978-11-03 |
| GB1577630A (en) | 1980-10-29 |
| DE2815593A1 (en) | 1978-10-19 |
| LU79382A1 (en) | 1978-07-12 |
| NL7803696A (en) | 1978-10-10 |
| FR2386480B1 (en) | 1981-07-31 |
| DK145878A (en) | 1978-10-08 |
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