DE199618C - - Google Patents
Info
- Publication number
- DE199618C DE199618C DE1904199618D DE199618DA DE199618C DE 199618 C DE199618 C DE 199618C DE 1904199618 D DE1904199618 D DE 1904199618D DE 199618D A DE199618D A DE 199618DA DE 199618 C DE199618 C DE 199618C
- Authority
- DE
- Germany
- Prior art keywords
- zinc dust
- aldehyde
- sulphurous acid
- zinc
- hydrosulfite
- 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.)
- Expired - Lifetime
Links
- 238000000034 method Methods 0.000 claims description 8
- HCHKCACWOHOZIP-UHFFFAOYSA-N zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 7
- 125000002485 formyl group Chemical class [H]C(*)=O 0.000 claims description 4
- LSNNMFCWUKXFEE-UHFFFAOYSA-N sulfonic acid Chemical compound OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 claims description 2
- SUOFREPYJDSUTJ-UHFFFAOYSA-N [Fe].S(O)(O)=O Chemical compound [Fe].S(O)(O)=O SUOFREPYJDSUTJ-UHFFFAOYSA-N 0.000 claims 1
- 150000001875 compounds Chemical class 0.000 claims 1
- 229910052751 metal Inorganic materials 0.000 claims 1
- 239000002184 metal Substances 0.000 claims 1
- 150000002739 metals Chemical class 0.000 claims 1
- GRWZHXKQBITJKP-UHFFFAOYSA-L dithionite(2-) Chemical class [O-]S(=O)S([O-])=O GRWZHXKQBITJKP-UHFFFAOYSA-L 0.000 description 5
- -1 aldehyde bisulfite Chemical class 0.000 description 4
- WSFSSNUMVMOOMR-UHFFFAOYSA-N formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 4
- 150000003839 salts Chemical class 0.000 description 4
- 239000011780 sodium chloride Substances 0.000 description 4
- 238000005185 salting out Methods 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- JVBXVOWTABLYPX-UHFFFAOYSA-L Sodium dithionite Chemical compound [Na+].[Na+].[O-]S(=O)S([O-])=O JVBXVOWTABLYPX-UHFFFAOYSA-L 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 230000000875 corresponding Effects 0.000 description 1
- 239000008098 formaldehyde solution Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000012452 mother liquor Substances 0.000 description 1
- 235000011837 pasties Nutrition 0.000 description 1
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M sodium bisulfite Chemical compound [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 description 1
- 229940001607 sodium bisulfite Drugs 0.000 description 1
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 description 1
- 239000012258 stirred mixture Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 150000003751 zinc Chemical class 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 150000003752 zinc compounds Chemical class 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C313/00—Sulfinic acids; Sulfenic acids; Halides, esters or anhydrides thereof; Amides of sulfinic or sulfenic acids, i.e. compounds having singly-bound oxygen atoms of sulfinic or sulfenic groups replaced by nitrogen atoms, not being part of nitro or nitroso groups
- C07C313/02—Sulfinic acids; Derivatives thereof
- C07C313/04—Sulfinic acids; Esters thereof
Description
KAISERLICHESIMPERIAL
PATENTAMT.PATENT OFFICE.
Per allgemeinen Verwendung von Hydrosulfiten stand bisher deren geringe Haltbarkeit entgegen, die schon während der Darstellung die Erzielung guter Ausbeuten sehrThe general use of hydrosulfites has so far been their low durability contrary to the fact that very good yields are achieved even during the presentation
.5 erschwerte..5 difficult.
Es ist schon bekannt, Hydrosulfite durchIt is already known to make hydrosulfites
Behandlung mit Aldehyden haltbar zu machen.To make treatment with aldehydes durable.
Dieses an sich vorteilhafte Verfahren gehtThis method, which is advantageous in itself, works
aber von fertigem Hydrosulfit, und zwarbut from finished hydrosulfite, namely
ίο festem Natriumhydrosulfit, aus. Wenn auch dieses Salz durch das Aussalzverfahren zugänglich ist, so weiß doch jeder, der mit Hydrosulfiten arbeitet, daß die Darstellung von festem Natriumhydrosulfit aus Natriumbisulfit ein technisch schwieriger un.d noch keineswegs glatte Ausbeuten liefernder Prozeß ist.ίο solid sodium hydrosulphite, from. If also this salt is accessible through the salting out process, everyone knows who with Hydrosulfite works that the production of solid sodium hydrosulfite from sodium bisulfite a technically difficult and by no means smooth yields process is.
In der britischen Patentschrift 5867/1903 ist außer diesem Verfahren noch ein zweites beschrieben: die Reduktion der Aldehyd-Bisulfit - Verbindung mit Zinkstaub und Schwefelsäure oder einer anderen, wie Säure wirkenden Substanz.In British Patent 5867/1903 In addition to this process, a second process is described: the reduction of the aldehyde bisulfite - Connection with zinc dust and sulfuric acid or another such as acid acting substance.
Man kommt auf diese Weise allerdings ebenfalls, ohne erst Hydrosulfit zu isolieren, direkt zu Aldehyd-Hydrosulfit-Verbindungen. Diese befinden sich aber in Lösung mit andern Salzen, von denen sie durch Aussalzen getrennt werden sollen. Auch wenn das Aussalzen ein vollständiges, also nicht mit Verlusten verbundenes wäre, so haftet diesem Verfahren mindestens der Fehler an, daß das ausgesalzene Präparat durch Hängenbleiben der Mutterlauge mit Nebensalzen verunreinigt ist. - 'In this way, however, one also comes without isolating hydrosulphite, directly to aldehyde hydrosulfite compounds. But these are in solution with others Salts from which they are to be separated by salting out. Even if the salting out would be complete, i.e. not associated with losses, this procedure is liable at least the error that the salted-out preparation got stuck the mother liquor is contaminated with secondary salts. - '
Bei dem nachfolgend beschriebenen Verfahren kommt man direkt zu reinen Aldehyd-Hydrosulfiten, frei von Nebensalzen und frei von Aldehyd-Bisulfit. Das Verfahren beruht darauf, daß man in ein Gemisch von 65 Teilen Zinkstaub und 80 Teilen Formaldehyd (von 40 Prozent) nur so viel schweflige Säure einleitet, daß der Zinkstaub gerade verschwindet. Man erhält, je nachdem man bei der Reaktion wenig oder viel Wasser oder eine andere indifferente Flüssigkeit zugibt, ein festes oder pasten förmiges Reaktionsprodukt, bestehend aus der gesuchten schwerlöslichen Zinkvefbindung. Statt des Formaldehyds können entsprechende Mengen anderer. Aldehyde benutzt werden.The process described below leads directly to pure aldehyde hydrosulfites, free from minor salts and free from aldehyde bisulfite. The procedure is based ensure that a mixture of 65 parts of zinc dust and 80 parts of formaldehyde (from 40 percent) only introduces so much sulphurous acid that the zinc dust just disappears. Depending on the reaction, little or a lot of water or something else is obtained indifferent liquid is added, consisting of a solid or pasty reaction product from the sparingly soluble zinc compound sought. Instead of the formaldehyde, corresponding amounts of others can be used. Aldehydes used will.
In ein gut gerührtes Gemisch von 65 kg Zinkstaubund 80 kg Formaldehydlösung von 40 Prozent wird schweflige Säure bis zum Verschwinden des Zinkstaubs geleitet. Statt des Zinks kann auch Eisen verwendet werden. Die entstandene Paste des schwer löslichen Zinksalzes ist ohne weiteres gebrauchsfertig.In a well-stirred mixture of 65 kg zinc dust and 80 kg formaldehyde solution of 40 percent of the sulphurous acid is discharged until the zinc dust disappears. Instead of of the zinc, iron can also be used. The resulting paste of the poorly soluble Zinc salt is readily ready to use.
Man kann sie auch abfiltrieren, waschen und im Vakuum trocknen.They can also be filtered off, washed and vacuum dried.
Claims (1)
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
AT37921D AT37921B (en) | 1904-09-14 | 1906-01-24 | Process for the preparation of durable double compounds of aldehydes with reduction products of sulphurous acid. |
Publications (1)
Publication Number | Publication Date |
---|---|
DE199618C true DE199618C (en) |
Family
ID=462318
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
DE1904199618D Expired - Lifetime DE199618C (en) | 1904-09-14 | 1904-09-14 |
Country Status (1)
Country | Link |
---|---|
DE (1) | DE199618C (en) |
-
1904
- 1904-09-14 DE DE1904199618D patent/DE199618C/de not_active Expired - Lifetime
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