DE46724C - Process for the preparation of halogen-free nitric acid and halogen-free nitric acid salts - Google Patents
Process for the preparation of halogen-free nitric acid and halogen-free nitric acid saltsInfo
- Publication number
- DE46724C DE46724C DENDAT46724D DE46724DA DE46724C DE 46724 C DE46724 C DE 46724C DE NDAT46724 D DENDAT46724 D DE NDAT46724D DE 46724D A DE46724D A DE 46724DA DE 46724 C DE46724 C DE 46724C
- Authority
- DE
- Germany
- Prior art keywords
- nitric acid
- halogen
- free nitric
- free
- 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.)
- Expired - Lifetime
Links
- GRYLNZFGIOXLOG-UHFFFAOYSA-N nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 title claims description 17
- 229910052736 halogen Inorganic materials 0.000 claims description 7
- 150000002367 halogens Chemical class 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 4
- 150000002366 halogen compounds Chemical class 0.000 claims description 3
- 235000019441 ethanol Nutrition 0.000 claims description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 2
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 2
- IOVCWXUNBOPUCH-UHFFFAOYSA-N nitrous acid Chemical compound ON=O IOVCWXUNBOPUCH-UHFFFAOYSA-N 0.000 claims 1
- FAPWRFPIFSIZLT-UHFFFAOYSA-M sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 8
- 239000011780 sodium chloride Substances 0.000 description 5
- FGIUAXJPYTZDNR-UHFFFAOYSA-N Potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 4
- VWDWKYIASSYTQR-UHFFFAOYSA-N Sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 239000002253 acid Substances 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 229910052801 chlorine Inorganic materials 0.000 description 4
- 239000000460 chlorine Substances 0.000 description 4
- ZAMOUSCENKQFHK-UHFFFAOYSA-N chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Natural products CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 2
- 239000004568 cement Substances 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 230000005484 gravity Effects 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- GQPLMRYTRLFLPF-UHFFFAOYSA-N nitrous oxide Inorganic materials [O-][N+]#N GQPLMRYTRLFLPF-UHFFFAOYSA-N 0.000 description 2
- 235000010333 potassium nitrate Nutrition 0.000 description 2
- 239000004317 sodium nitrate Substances 0.000 description 2
- 235000010344 sodium nitrate Nutrition 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 125000000218 acetic acid group Chemical group C(C)(=O)* 0.000 description 1
- 230000002378 acidificating Effects 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000005755 formation reaction Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000004323 potassium nitrate Substances 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- -1 while the rest Chemical compound 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
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/20—Nitrogen oxides; Oxyacids of nitrogen; Salts thereof
- C01B21/38—Nitric acid
- C01B21/46—Purification; Separation ; Stabilisation
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Description
KAISERLICHESIMPERIAL
PATENTAMTPATENT OFFICE
Die Halogen haltende Flüssigkeit oder, falls ein Halogen haltender fester Körper vorliegt, seine möglichst concentrirte Lösung wird mit Salpetersäure oder einem Salpetersäure oder salpetrige Säure entwickelnden Körper erwärmt, deren Menge sich nach der Menge der Flüssigkeit und ihrem Gehalt an Halogen richtet und durch Versuch festgestellt wird. Man setzt dann organische Körper hinzu, welche unter den gegebenen Umständen leicht flüchtige Halogenverbindungen bilden, als Methyl- und Aethylalkohol oder Mischungen, welche diese Körper enthalten. Von der Gröfse des Zusatzes gilt dasselbe wie von dem der Salpetersäure. Die Halogene entweichen bei der eintretenden Reaction, welche sich durch Bildung von salpetrigen und aldehydartig riechenden Dämpfen anzeigt. Man unterstützt die Reaction durch Erwärmen und beendet sie durch längeres Kochen. In dem Rückstand sind Essigsäure und andere homologe Säuren nicht nachzuweisen. Sämmtliche Halogenverbindungen werden auf diese Weise leicht angegriffen und vom Halogen befreit, mit Ausnahme der überchlorsauren Salze, welche indessen in der sauren Lauge derart ihre Schwerlöslichkeit verlieren, dafs sie durch Umkrystallisiren getrennt werden können.The halogen-containing liquid or, if a halogen-containing solid is present, its solution, as concentrated as possible, is made with nitric acid or a nitric acid or Nitrous acid-developing body warms up, the amount of which depends on the amount of liquid and their halogen content and is determined by experiment. One sets then organic bodies are added, which are easily volatile under the given circumstances Form halogen compounds, as methyl and ethyl alcohol or mixtures, which these Body included. The same applies to the size of the addition as to that of nitric acid. The halogens escape when the reaction occurs, which is formed by formation of nitrous and aldehyde-like smelling vapors. You support the reaction by heating and finished by boiling for a long time. There is acetic acid in the residue and other homologous acids cannot be detected. All halogen compounds are easily attacked in this way and freed from halogen, with the exception of the superchloric acid salts, which are in the acidic liquor lose their insolubility to such an extent that they are separated by recrystallization can be.
Beispiel: 1. Zu dem Gemisch von 300 kg Salpeter von 1 pCt. Chlornatrium und 330 kg Schwefelsäure von 6o° B. läfst man, sobald die Destillation beginnt, durch ein im Deckel eingekittetes schwanenhalsartiges Eisenrohr so schnell, als die hierbei eintretende Reaction es gestattet, Spiritus zulaufen, bis das Destillat sich chlorfrei erweist. Es genügen in der Regel 7 kg Spiritus von 92° Tralles. Sodann wird die Vorlage gewechselt. Man erhält in der gut zu kühlenden ersten Vorlage eine geringe Menge an Untersalpetersäure und chlorreicher Salpetersäure, während die übrige, in der zweiten Vorlage aufgefangene Salpetersäure frei von Chlor ist.Example: 1. To the mixture of 300 kg saltpeter of 1 pCt. Sodium chloride and 330 kg As soon as the distillation begins, sulfuric acid of 60 ° B. is passed through a cement cemented into the lid Gooseneck-like iron pipe as quickly as the reaction which occurs here allowed to run in spirit until the distillate proves to be chlorine-free. It suffices in the Usually 7 kg of spirit from 92 ° Tralles. Then the template is changed. You get in the first template, which is easy to cool, contains a small amount of subnitric acid and chlorine-rich Nitric acid, while the rest of the nitric acid collected in the second receiver is free of chlorine.
2. 100 kg Natriumsalpeter von 0,3 pCt. Chlornatrium in 80 kg Wasser gelöst, mit 5 kg technischer Salpetersäure vom specifischen Gewicht 1,4 gekocht und dann mit 5 kg Spiritus von 92° Tralles versetzt, längere Zeit schliefslich gekocht, erweisen sich als halogenfrei.2. 100 kg sodium nitrate of 0.3 pCt. Sodium chloride dissolved in 80 kg of water, with 5 kg of technical nitric acid of specific gravity 1.4 cooked and then mixed with 5 kg of spirit of 92 ° Tralles, for a long time finally cooked, turn out to be halogen-free.
3. Zu dem Gemisch von 300 kg Salpeter von ι pCt. Chlornatrium und 330 kg Schwefelsäure von 6o° B. läfst man, sobald die Destillation beginnt, durch ein im Deckel eingekittetes schwanenhalsartiges Eisenrohr so schnell, als die hierbei eintretende Reaction es gestattet, Methylalkohol zulaufen, bis das Destillat sich chlorfrei erweist. Es genügen in der Regel ι ο kg Holzgeist von 88° Tralles. Man erhält in der gut zu kühlenden ersten Vorlage eine geringe Menge an Untersalpetersäure und chlorreicher Salpetersäure, während die übrige, in der zweiten Vorlage aufgefangene Salpetersäure frei von Chlor ist.3. To the mixture of 300 kg saltpetre from ι pCt. Sodium chloride and 330 kg sulfuric acid from 60 ° B., as soon as the distillation begins, it is passed through a cement cemented into the lid gooseneck-like iron pipe as quickly as the resulting reaction allows, Add methyl alcohol until the distillate is chlorine-free. It suffices in the Usually ι ο kg wood spirit from 88 ° Tralles. The first template, which is easy to cool, is obtained a small amount of subnitric acid and chlorine-rich nitric acid, while the rest, nitric acid collected in the second receiver is free of chlorine.
4. 100 kg Natriumsalpeter von 0,3 pCt. Chlornatrium in 80 kg Wasser gelöst, mit 5 kg technischer Salpetersäure vom specifischen Gewicht 1,4 gekocht und dann mit 7 bis 8 kg Holzgeist von 88° Tralles versetzt, längere Zeit schliefslich gekocht, erweisen sich als halogenfrei. 4. 100 kg sodium nitrate of 0.3 pCt. Sodium chloride dissolved in 80 kg of water, with 5 kg of technical nitric acid of specific gravity 1.4 cooked and then mixed with 7 to 8 kg of wood spirit from 88 ° Tralles, for a long time finally cooked, turn out to be halogen-free.
Claims (2)
Publications (1)
| Publication Number | Publication Date |
|---|---|
| DE46724C true DE46724C (en) |
Family
ID=321811
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| DENDAT46724D Expired - Lifetime DE46724C (en) | Process for the preparation of halogen-free nitric acid and halogen-free nitric acid salts |
Country Status (1)
| Country | Link |
|---|---|
| DE (1) | DE46724C (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4471938A (en) * | 1982-11-01 | 1984-09-18 | United Technologies Corporation | Modulating poppet valve |
-
0
- DE DENDAT46724D patent/DE46724C/en not_active Expired - Lifetime
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4471938A (en) * | 1982-11-01 | 1984-09-18 | United Technologies Corporation | Modulating poppet valve |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| DE562820C (en) | Process for stabilizing low molecular weight chlorinated hydrocarbons | |
| DE46724C (en) | Process for the preparation of halogen-free nitric acid and halogen-free nitric acid salts | |
| DE593384C (en) | Process for stabilizing liquid chlorinated hydrocarbons | |
| DE1543020C3 (en) | ||
| DE733694C (en) | Process for the production of halogenated ketones | |
| DE142939C (en) | ||
| DE622966C (en) | Process for the conversion of isovanillin into 4-oxy-3-ethoxybenzaldehyde | |
| DE509149C (en) | Process for the preparation of nuclear methylated hydrocarbons | |
| DE1223383B (en) | Process for the preparation of pentafluorophenyl magnesium chloride | |
| DE74132C (en) | Process for the representation of lead white | |
| DE624695C (en) | Process for the production of potassium tetraoxalate | |
| DE711822C (en) | Separation procedure | |
| DE263354C (en) | ||
| DE552833C (en) | Process for the production of the anhydrides and chlorides of monovalent saturated acids of the fatty series | |
| DE580633C (en) | Obtaining technically silica-free hydrofluoric acid from hydrofluoric acid containing silica | |
| DE843695C (en) | Process for the production of unsaturated organic halides by exchanging halogen atoms | |
| DE535650C (en) | Process for the preparation of cellulose esters of saturated fatty acids which are soluble in organic agents and are highly acid-resistant | |
| DE177173C (en) | ||
| DE473976C (en) | Generation of calcium hypochlorite | |
| DE1014981B (en) | Process for the production of trichloroacetonitrile | |
| DE901775C (en) | Process for the production of hexachlorocyclohexane | |
| DE1076669B (en) | Process for the preparation of 2-chlorobutadiene-1, 3 | |
| DE78882C (en) | Process for the preparation of higher homologues of catechol | |
| DE1252682B (en) | Process for the preparation of 1,5-dihydroxyhexaorganotrisiloxanes | |
| AT230861B (en) | Process for the preparation of propargyl bromide and / or 2-chloro-3-bromo-propene-1 |