CH201516A - Process for the preparation of a solid diazonium salt. - Google Patents
Process for the preparation of a solid diazonium salt.Info
- Publication number
- CH201516A CH201516A CH201516DA CH201516A CH 201516 A CH201516 A CH 201516A CH 201516D A CH201516D A CH 201516DA CH 201516 A CH201516 A CH 201516A
- Authority
- CH
- Switzerland
- Prior art keywords
- diazonium salt
- solid
- preparation
- methylsulfuric acid
- weight
- Prior art date
Links
- 239000012954 diazonium Substances 0.000 title claims description 10
- 150000001989 diazonium salts Chemical class 0.000 title claims description 6
- 239000007787 solid Substances 0.000 title claims description 6
- 238000000034 method Methods 0.000 title claims description 5
- 238000002360 preparation method Methods 0.000 title description 2
- SXEBHIMOUHBBOS-UHFFFAOYSA-N 5-chloro-2-phenoxyaniline Chemical compound NC1=CC(Cl)=CC=C1OC1=CC=CC=C1 SXEBHIMOUHBBOS-UHFFFAOYSA-N 0.000 claims description 3
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 3
- 125000000664 diazo group Chemical group [N-]=[N+]=[*] 0.000 claims description 3
- -1 methylsulfuric acid diazonium salt Chemical class 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 2
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical class [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 claims description 2
- 238000004043 dyeing Methods 0.000 claims description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims description 2
- JZMJDSHXVKJFKW-UHFFFAOYSA-N methyl sulfate Chemical compound COS(O)(=O)=O JZMJDSHXVKJFKW-UHFFFAOYSA-N 0.000 claims description 2
- 239000011707 mineral Substances 0.000 claims description 2
- 239000000843 powder Substances 0.000 claims description 2
- 230000008021 deposition Effects 0.000 claims 1
- 125000001752 diazonium salt group Chemical group 0.000 claims 1
- 238000005185 salting out Methods 0.000 claims 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- RXQNKKRGJJRMKD-UHFFFAOYSA-N 5-bromo-2-methylaniline Chemical compound CC1=CC=C(Br)C=C1N RXQNKKRGJJRMKD-UHFFFAOYSA-N 0.000 description 1
- 238000006193 diazotization reaction Methods 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- VJWFFRAUKLEPHS-UHFFFAOYSA-N methyl hydrogen sulfate;sodium Chemical compound [Na].COS(O)(=O)=O VJWFFRAUKLEPHS-UHFFFAOYSA-N 0.000 description 1
- 239000010446 mirabilite Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 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 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Description
Verfahren zur Herstellung eines festen Diazoniumsalzes. Gegenstand des vorliegenden Zusatz patentes ist ein Verfahren zur Herstellung eines festen Diazoniumsalzes, welches da durch gekennzeichnet ist,
dass man aus einer mineralsauren Diazolösung von 1-Amino-2- phenoxy-5-chlorbenzol nach Zusatz von me- thylschwefelsaurem Natrium das methyl- schwefelsaure Diazoniumsalz in fester Form abscheidet.
<I>Beispiel:</I> 100 Gewichtsteile 1-Amino-2-phenoxy-5- chlorbenzol werden bei 25 bis 30 C portions- weise in 151,9 Gewichtsteile 40%ige Nitro- sylschwefelsäure eingetragen. Nach beende tem Eintragen wird so lange bei dieser Tem peratur gerührt, bis eine Probe in Wasser klar löslich ist. Die Diazotierung wird nun in 500 Gewichtsteile Wasser und 200 Gewichts teile Eis gegossen und die Diazolösung fil triert.
Das Filtrat wird dann mit 154,6 Ge wichtsteilen einer 41,5 gewichtsprozentigen Lösung von methylschwefelsaurem Natrium versetzt und die alsbald beginnende Abschei- dung durch Zusatz von 80 Gewichtsteilen Glaubersalz vervollständigt. Das methyl- schwefelsaure Diazoniumsalz wird bei niedri ger Temperatur getrocknet.
Das erhaltene Diazoniumsalz stellt ein gelblichweisses kristallines Pulver dar. Es besitzt eine gute Haltbarkeit und ist leicht löslich. Durch Vermischen mit den gebräuch lichen Färbereihilfsmitteln, wie wasserfreiem Natriumsulfat oder teilentwässertem Alu- miniumsulfat usw., kann es auf handels übliche Form eingestellt werden.
Process for the preparation of a solid diazonium salt. The subject of the present additional patent is a process for the production of a solid diazonium salt, which is characterized by
that one separates the methylsulfuric acid diazonium salt in solid form from a mineral acid diazo solution of 1-amino-2-phenoxy-5-chlorobenzene after addition of methylsulfuric acid.
<I> Example: </I> 100 parts by weight of 1-amino-2-phenoxy-5-chlorobenzene are introduced in portions at 25 to 30 ° C. into 151.9 parts by weight of 40% strength nitrosylsulfuric acid. After the end of the entry system, the mixture is stirred at this temperature until a sample is clearly soluble in water. The diazotization is then poured into 500 parts by weight of water and 200 parts by weight of ice and the diazo solution is fil trated.
154.6 parts by weight of a 41.5 percent by weight solution of sodium methylsulfuric acid are then added to the filtrate, and the separation which soon begins is completed by adding 80 parts by weight of Glauber's salt. The methyl sulfuric acid diazonium salt is dried at a lower temperature.
The diazonium salt obtained is a yellowish-white crystalline powder. It has a good shelf life and is easily soluble. By mixing it with the usual dyeing auxiliaries, such as anhydrous sodium sulphate or partially dehydrated aluminum sulphate, etc., it can be adjusted to the commercially available form.
Claims (1)
Applications Claiming Priority (4)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE201517X | 1936-03-10 | ||
| DE201516X | 1936-03-10 | ||
| DE201514X | 1936-03-10 | ||
| CH199458T | 1937-03-08 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CH201516A true CH201516A (en) | 1938-11-30 |
Family
ID=27429710
Family Applications (3)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CH201514D CH201514A (en) | 1936-03-10 | 1937-03-08 | Process for the preparation of a solid diazonium salt. |
| CH201517D CH201517A (en) | 1936-03-10 | 1937-03-08 | Process for the preparation of a solid diazonium salt. |
| CH201516D CH201516A (en) | 1936-03-10 | 1937-03-08 | Process for the preparation of a solid diazonium salt. |
Family Applications Before (2)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CH201514D CH201514A (en) | 1936-03-10 | 1937-03-08 | Process for the preparation of a solid diazonium salt. |
| CH201517D CH201517A (en) | 1936-03-10 | 1937-03-08 | Process for the preparation of a solid diazonium salt. |
Country Status (1)
| Country | Link |
|---|---|
| CH (3) | CH201514A (en) |
-
1937
- 1937-03-08 CH CH201514D patent/CH201514A/en unknown
- 1937-03-08 CH CH201517D patent/CH201517A/en unknown
- 1937-03-08 CH CH201516D patent/CH201516A/en unknown
Also Published As
| Publication number | Publication date |
|---|---|
| CH201517A (en) | 1938-11-30 |
| CH201514A (en) | 1938-11-30 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CH201516A (en) | Process for the preparation of a solid diazonium salt. | |
| DE605577C (en) | Process for the preparation of solid diazonium salts | |
| DE609476C (en) | Process for the preparation of solid diazonium salts | |
| DE606942C (en) | Process for the preparation of solid diazonium salts | |
| CH176221A (en) | Process for producing a diazo compound in solid form. | |
| CH175876A (en) | Process for the preparation of a dry diazonium salt. | |
| DE873696C (en) | Process for the production of aluminum triformate or other neutral salts of aluminum with water-soluble organic acids | |
| CH137100A (en) | Process for producing a solid diazoazo compound. | |
| CH137099A (en) | Process for producing a solid diazoazo compound. | |
| CH199458A (en) | Process for the preparation of a solid diazonium salt. | |
| DE586355C (en) | Process for the preparation of diazo compounds in solid form | |
| DE654448C (en) | Process for the preparation of solid diazonium salts | |
| DE655047C (en) | Process for the preparation of aryldiazonium salts | |
| CH201515A (en) | Process for the preparation of a solid diazonium salt. | |
| CH176218A (en) | Process for producing a diazo compound in solid form. | |
| CH137101A (en) | Process for producing a solid diazoazo compound. | |
| DE631640C (en) | Process for the preparation of 2íñ3-aminobromanthraquinonesulfonic acid | |
| CH118614A (en) | Process for making a durable diazo compound. | |
| CH169243A (en) | Process for the preparation of 5-chloro-2-benzoyl-acetylamino-1-methoxybenzene-3-sulfonic acid. | |
| CH134940A (en) | Process for producing a solid diazoazo compound. | |
| CH123637A (en) | Process for the production of a dry diazo preparation. | |
| CH147033A (en) | Process for the production of a preparation suitable for preparing a solution of a nitrosodiazo compound of the diphenylamine series. | |
| CH202158A (en) | Process for the preparation of a diphenyl series hydrazine. | |
| CH118607A (en) | Process for making a durable diazo compound. | |
| CH118618A (en) | Process for making a durable diazo compound. |