DE48269C - Process for the preparation of alkali sulphates and calcium sulphite from manufacturing liquors containing alkali sulphite by means of calcium sulphate - Google Patents
Process for the preparation of alkali sulphates and calcium sulphite from manufacturing liquors containing alkali sulphite by means of calcium sulphateInfo
- Publication number
- DE48269C DE48269C DENDAT48269D DE48269DA DE48269C DE 48269 C DE48269 C DE 48269C DE NDAT48269 D DENDAT48269 D DE NDAT48269D DE 48269D A DE48269D A DE 48269DA DE 48269 C DE48269 C DE 48269C
- Authority
- DE
- Germany
- Prior art keywords
- sulphite
- calcium
- alkali
- sulphate
- preparation
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L Calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 title claims description 12
- LSNNMFCWUKXFEE-UHFFFAOYSA-L Sulphite Chemical compound [O-]S([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-L 0.000 title claims description 7
- 235000011132 calcium sulphate Nutrition 0.000 title claims description 6
- 239000003513 alkali Substances 0.000 title claims description 5
- 239000001175 calcium sulphate Substances 0.000 title claims description 4
- 238000000034 method Methods 0.000 title claims description 4
- 238000004519 manufacturing process Methods 0.000 title claims description 3
- 238000002360 preparation method Methods 0.000 title claims description 3
- GBAOBIBJACZTNA-UHFFFAOYSA-L Calcium sulfite Chemical compound [Ca+2].[O-]S([O-])=O GBAOBIBJACZTNA-UHFFFAOYSA-L 0.000 title claims 2
- 235000010261 calcium sulphite Nutrition 0.000 title claims 2
- 239000004295 calcium sulphite Substances 0.000 title claims 2
- 150000003467 sulfuric acid derivatives Chemical class 0.000 title claims 2
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 11
- 235000015450 Tilia cordata Nutrition 0.000 description 11
- 235000011941 Tilia x europaea Nutrition 0.000 description 11
- 239000004571 lime Substances 0.000 description 11
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 8
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Natural products OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 7
- GEHJYWRUCIMESM-UHFFFAOYSA-L Sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 description 7
- QAOWNCQODCNURD-UHFFFAOYSA-L sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 230000001264 neutralization Effects 0.000 description 4
- 150000002989 phenols Chemical class 0.000 description 4
- 239000011780 sodium chloride Substances 0.000 description 4
- 235000002639 sodium chloride Nutrition 0.000 description 4
- 239000000706 filtrate Substances 0.000 description 3
- 239000002244 precipitate Substances 0.000 description 3
- FAPWRFPIFSIZLT-UHFFFAOYSA-M sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 3
- 235000010265 sodium sulphite Nutrition 0.000 description 3
- LSNNMFCWUKXFEE-UHFFFAOYSA-N sulfonic acid Chemical compound OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 description 3
- 150000003460 sulfonic acids Chemical class 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N HCl Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- LSNNMFCWUKXFEE-UHFFFAOYSA-M bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- UXVMQQNJUSDDNG-UHFFFAOYSA-L cacl2 Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 2
- 239000001110 calcium chloride Substances 0.000 description 2
- 229910001628 calcium chloride Inorganic materials 0.000 description 2
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium monoxide Chemical compound [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 2
- 230000005591 charge neutralization Effects 0.000 description 2
- 230000000875 corresponding Effects 0.000 description 2
- 239000010446 mirabilite Substances 0.000 description 2
- PMZURENOXWZQFD-UHFFFAOYSA-L na2so4 Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 2
- UFWIBTONFRDIAS-UHFFFAOYSA-N naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 description 2
- 238000006386 neutralization reaction Methods 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 235000011121 sodium hydroxide Nutrition 0.000 description 2
- RSIJVJUOQBWMIM-UHFFFAOYSA-L sodium sulfate decahydrate Chemical compound O.O.O.O.O.O.O.O.O.O.[Na+].[Na+].[O-]S([O-])(=O)=O RSIJVJUOQBWMIM-UHFFFAOYSA-L 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- KJCVRFUGPWSIIH-UHFFFAOYSA-N 1-Naphthol Chemical compound C1=CC=C2C(O)=CC=CC2=C1 KJCVRFUGPWSIIH-UHFFFAOYSA-N 0.000 description 1
- JWAZRIHNYRIHIV-UHFFFAOYSA-N 2-Naphthol Chemical compound C1=CC=CC2=CC(O)=CC=C21 JWAZRIHNYRIHIV-UHFFFAOYSA-N 0.000 description 1
- AXCZMVOFGPJBDE-UHFFFAOYSA-L Calcium hydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-N Carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 1
- OTYBMLCTZGSZBG-UHFFFAOYSA-L Potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 150000001674 calcium compounds Chemical class 0.000 description 1
- 239000000920 calcium hydroxide Substances 0.000 description 1
- 235000011116 calcium hydroxide Nutrition 0.000 description 1
- 239000000292 calcium oxide Substances 0.000 description 1
- 235000012255 calcium oxide Nutrition 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000010908 decantation Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000010440 gypsum Substances 0.000 description 1
- 229910052602 gypsum Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- PSZYNBSKGUBXEH-UHFFFAOYSA-N naphthalene-1-sulfonic acid Chemical class C1=CC=C2C(S(=O)(=O)O)=CC=CC2=C1 PSZYNBSKGUBXEH-UHFFFAOYSA-N 0.000 description 1
- -1 phenol sulfonic acids Chemical class 0.000 description 1
- 229910052939 potassium sulfate Inorganic materials 0.000 description 1
- 239000001120 potassium sulphate Substances 0.000 description 1
- 235000011151 potassium sulphates Nutrition 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D5/00—Sulfates or sulfites of sodium, potassium or alkali metals in general
- C01D5/04—Preparation of sulfates with the aid of sulfurous acid or sulfites, e.g. Hargreaves process
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/48—Sulfites
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Paper (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Description
KAISERLICHESIMPERIAL
PATENTAMT.PATENT OFFICE.
Bei der technischen Darstellung von Phenolen durch Verschmelzen sulfosaurer Salze mit Aetznatron erhält man nach Ausfällung der betreffenden Phenole mit Salz- oder Schwefelsäure Laugen, die neben Kochsalz oder Glaubersalz bedeutende Mengen von Natriummonosulfit neben etwas Bisulfit enthalten.In the technical preparation of phenols by fusing sulfonic acid salts with caustic soda obtained after precipitation of the phenols in question with hydrochloric or sulfuric acid Alkalis, which, in addition to table salt or Glauber's salt, contain significant amounts of sodium monosulfite in addition to some bisulfite.
Zur Entfernung dieser Sulfite und Abscheidung der schwefligen Säure in nutzbarer Form kann man in bekannter Weise aus den mit Aetzkalk neutralisirten Flüssigkeiten durch Chlorcalciumlösung neutralen schwefligsauren Kalk fällen, erhält jedoch dann im Filtrat nur geringwerthiges Kochsalz.To remove these sulphites and separate the sulphurous acid in a usable form can be obtained in a known manner from liquids neutralized with quicklime by means of calcium chloride solution Precipitate neutral sulphurous lime, but then get only little value in the filtrate Table salt.
Wir haben nun gefunden, dafs an Stelle von Chlorcalcium schwefelsaurer Kalk sich in
ganz analoger Weise mit der durch Kalk alkalisch gemachten Lösung von Natriumsulfit
umsetzt. Man erhält hierbei im Filtrat statt des Kochsalzes Glaubersalz. Die Umsetzung
verläuft im Sinne folgender Gleichung:
Ca SOi + Na2 SO3 = Ca S O3 + Na2 SO4.We have now found that instead of calcium chloride, lime sulphate reacts in a completely analogous manner with the sodium sulphite solution made alkaline by lime. Instead of the common salt, Glauber's salt is obtained in the filtrate. The implementation proceeds in the sense of the following equation:
Ca SO i + Na 2 S O 3 = Ca S O 3 + Na 2 S O 4 .
Die Umwandlung tritt nicht nur bei einer bestimmten Concentration und Temperatur der Lösung ein, diese Bedingungen können vielmehr innerhalb weiter Grenzen schwanken; Concentration und Temperatur müssen nur derartig gewählt sein, dafs das entstehende Sulfat in Lösung zu bleiben vermag.The conversion does not only occur at a certain concentration and temperature of the Solution, these conditions can rather vary within wide limits; Concentration and temperature need only be chosen in such a way that the resulting Sulphate is able to stay in solution.
Als schwefelsauren Kalk kann man entweder natürlichen fein gemahlenen, gebrannten oder gefällten Gyps anwenden. Auch die Doppelsalze von schwefelsaurem Kalk mit schwefelsaurem Natron und schwefelsaurem Kali wirken ihrem Gehalt an schwefelsaurem Kalk entsprechend. Feine Vertheilung des Calciumsulfate, gutes Durchrühren desselben mit der Sulfitlösung und erhöhte Temperatur beschleunigen die Umsetzung.As sulphate of lime you can either use natural finely ground, burnt or Apply felled gypsum. Also the double salts of sulphate of lime with sulphate of lime Soda and potassium sulphate act according to their lime sulphate content. Fine distribution of the calcium sulphate, stir it well with the Sulphite solution and increased temperature accelerate the implementation.
Ein für den Procefs sehr geeignetes Calciumsulfat erhält man meist als Nebenproduct bei der Darstellung der eingangs erwähnten sulfosäuren Salze bezw. bei der Absättigung der Rohsulfosäuren mit Kalk behufs Abscheidung der überschüssigen Schwefelsäure.Calcium sulphate, which is very suitable for the process, is usually obtained as a by-product the representation of the aforementioned sulfonic acid salts respectively. in the saturation of the Crude sulfonic acids with lime to separate excess sulfuric acid.
Anstatt die Laugen nach Abscheidung der Phenole von den Sulfiten zu befreien, -kann man auch direct die Schmelzlösung, nach Neutralisation des überschüssigen Alkalis mit Schwefelsäure, mit einer dem vorhandenen Sulfit entsprechenden Menge Calciumsulfat behandeln. Es ist hierbei nicht zu befürchten, dafs die Kalkverbindung des betreffenden Phenols in Niederschlag oder Lösung geht (s. Patent No. 48270).Instead of removing the sulphites from the alkalis after separating the phenols, -can one also directly the melt solution, after neutralization of the excess alkali with Sulfuric acid, treat with an amount of calcium sulfate corresponding to the amount of sulfite present. It is not to be feared here that the calcium compound of the concerned Phenol goes into precipitate or solution (see Patent No. 48270).
Ganz in derselben Weise kann man die Sulfite auch aus Schmelzlösungen entfernen, die keine Phenole, sondern Phenolsulfosäuren enthalten, also z. B. die beim partiellen Verschmelzen von Naphtalinpolysulfosäuren resultirenden verschiedenen Naphtolsulfosäuren.The sulphites can also be removed from molten solutions in exactly the same way, which contain no phenols but phenol sulfonic acids, e.g. B. the partial merging various naphthalene sulfonic acids resulting from naphthalene polysulfonic acids.
Auch den bei der Herstellung von Cellulose nach dem Sulfitverfahren resultirenden schwefligsauren Laugen läfst sich nach der Neutralisation mit Kalk die schweflige Säure mittelst Calciumsulfate entziehen.Also the sulphurous acid resulting from the production of cellulose by the sulphite process After neutralization with lime, the sulphurous acid can be removed by means of alkalis Withdraw calcium sulfate.
Als Beispiel diene folgender specieller Fall: Das 20 bis 30° B. zeigende Filtrat des durch Schwefelsäure aus der Lösung der Natronschmelze ausgefällten α- oder ß-Naphtols wird in einem mit Rührwerk mit Dampfzutritt versehenen Holzbottich durch Zusatz von Kalkmilch alkalisch gemacht, bis nahe zum Sieden erhitzt und dann unter stetem Rühren und Kochen eine dem vorhandenen neutralen Natriumsulfit entsprechende Menge gefällten schwefelsauren Kalks, der mit Wasser zu einem dünnen Brei angerührt ist, allmälig eingetragen. Durch Probenehmen überzeugt man sich von der Entfernung des Natriumsulfits. Man trennt schliefslich den als krystallinischen Niederschlag sich absetzenden schwefligsauren Kalk durch Decantation oder Filtration und Auswaschen von der Natriumsulfatlösung, welche entweder direct oder nach gehörigem Eindampfen zur Krystallisaüon gebracht wird.The following special case serves as an example: The filtrate of the through 20 to 30 ° B. Sulfuric acid from the solution of the sodium hydroxide precipitated α- or ß-naphthol in a wooden tub equipped with a stirrer with steam access by adding milk of lime made alkaline, heated to near boiling and then, with constant stirring and boiling, add a neutral one to the existing one Sodium sulphite corresponding amount of precipitated sulphate of lime, which with water becomes a thin pulp is mixed, gradually added. By taking samples you can convince yourself of the removal of the sodium sulfite. Finally, the crystalline precipitate is separated settling sulphurous lime by decantation or filtration and washing out of the sodium sulphate solution, which either directly or after proper evaporation to the Krystallisaüon is brought.
Claims (1)
Publications (1)
| Publication Number | Publication Date |
|---|---|
| DE48269C true DE48269C (en) |
Family
ID=323257
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| DENDAT48269D Active DE48269C (en) | Process for the preparation of alkali sulphates and calcium sulphite from manufacturing liquors containing alkali sulphite by means of calcium sulphate |
Country Status (1)
| Country | Link |
|---|---|
| DE (1) | DE48269C (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5813706A (en) * | 1997-05-21 | 1998-09-29 | Hydrant Repair Parts, Inc. | Variable radial orientation pipe connector |
-
0
- DE DENDAT48269D patent/DE48269C/en active Active
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5813706A (en) * | 1997-05-21 | 1998-09-29 | Hydrant Repair Parts, Inc. | Variable radial orientation pipe connector |
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