CH149708A - Process for the preparation of an acidic wool dye of the anthraquinone series. - Google Patents
Process for the preparation of an acidic wool dye of the anthraquinone series.Info
- Publication number
- CH149708A CH149708A CH149708DA CH149708A CH 149708 A CH149708 A CH 149708A CH 149708D A CH149708D A CH 149708DA CH 149708 A CH149708 A CH 149708A
- Authority
- CH
- Switzerland
- Prior art keywords
- gray
- blue
- preparation
- acidic
- anthraquinone series
- Prior art date
Links
- 210000002268 wool Anatomy 0.000 title claims description 7
- 230000002378 acidificating effect Effects 0.000 title claims description 5
- 238000000034 method Methods 0.000 title claims description 4
- 238000002360 preparation method Methods 0.000 title claims description 4
- PYKYMHQGRFAEBM-UHFFFAOYSA-N anthraquinone Natural products CCC(=O)c1c(O)c2C(=O)C3C(C=CC=C3O)C(=O)c2cc1CC(=O)OC PYKYMHQGRFAEBM-UHFFFAOYSA-N 0.000 title claims description 3
- 150000004056 anthraquinones Chemical class 0.000 title claims description 3
- 239000000975 dye Substances 0.000 claims description 7
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 6
- 239000004327 boric acid Substances 0.000 claims description 6
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 claims description 4
- 229910052753 mercury Inorganic materials 0.000 claims description 4
- 150000001875 compounds Chemical class 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- UQGNORZJBSUDEX-UHFFFAOYSA-N [B].OS(O)(=O)=O Chemical compound [B].OS(O)(=O)=O UQGNORZJBSUDEX-UHFFFAOYSA-N 0.000 claims description 2
- 239000000843 powder Substances 0.000 claims description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical class [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- -1 Oxides or salts Chemical class 0.000 description 2
- LSNNMFCWUKXFEE-UHFFFAOYSA-N Sulfurous acid Chemical compound OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
Landscapes
- Coloring (AREA)
Description
Verfahren zur Darstellung eines sauren Wollfarbstoffes der Antbrachinonreihe. Nach der deutschen Patentschrift 414865 erhält man Wollfarbstoffe durch Sulfieren von Amino- oder Alkylaminodianthrachino- nylaminen mittelst Oleum bei An- oder<B>Ab-</B> wesenheit von Borsäure.
Es wurde nun gefunden, dass die Sul- fierung dieser Dianthrachirionylaminderivate mit borsäurehaltigem Oleum wesentlich ra scher erfolgt und zu leichter löslichen, wahr scheinlich höher sulfierten Produkten führt, welche für Färberzwecke von besonderem Wert sind, wenn man sie bei Gegenwart von Quecksilber oder dessen Verbindungen wie Oxyde oder Salze, vorzugsweise bei Tempe raturen zwischen ungefähr 120-150<B>0</B> aus führt.
Es war nicht vorauszusehen, dass das Quecksilber oder seine Salze oder Oxyde unter diesen Bedingungen den Eintritt von Suliogruppen erleichtern würde, ohne die gleichzeitige Bildung von Oxydationsprodtik- ten züi begünstigen, wie dies bei Abwesen- heit von Borsäure der Fall ist (siehe zum Beispiel<B>D.</B> R. P.<B>472356,</B> Beispiel<B>3).</B>
Gegenstand vorliegenden Patentes ist ein Verfahren zur Darstellung eines sauren Woll farbstoffes der Anthrachinonreihe, dadurch gekennzeichnet, dass man 4..4'-Diamino-1.1'- dianthrachinonylamin mit Oleum bei Gegen wart von Borsäure und, Quecksilber oder dessen Verbindungen, wie Salze oder Oxyde, auf Temperaturen zwischen 120 und<B>150 0<I>C</I></B> erhitzt.
<I>Beispiel:</I> <B>10</B> Gewiebtsteile 4.4'-Diai,.üino-1.1'-diaii- thrachinonylamin werden unter Rühren in 1510 Gewichtsteilen Oleum von<B>27</B> "/o SU3, in dem zuvor 4 Teile Borsäure aufgelöst und 0,2 Teile HgO suspendiert waren, gelöst und dann auf 135-140<B>0</B> zirka<B>3</B> Stunden erhitzt. Die Schmelze wird nach dem Abkühlen in <B>800</B> Teile Wasser eingerührt, das mit #venig schwefliger Säure versetzt war, sodann mit <B>600</B> Teilen gesättigter Kochsalzlösung auf- gekocht.
Der abgeschiedene Farbstoff wird abfiltriert und mit verdünnter Kochsalzlösung neutral gewaschen.
Das Produkt ist ein blaugratie#3 Pulver, das sich in Wasser grünstichig blaugrau, in konzentrierter Schwefelsäure blaugrau, in Bor- Schwefelsäure schmutzig-grün löst. Es färbt ungebeizte Wolle aus saurem Bade in kräf tigen blaugrauen Tönen von hervorragenden Echtheitseigenschaften.
Process for the preparation of an acidic wool dye of the antbrachinone series. According to German patent specification 414865, wool dyes are obtained by sulphonating amino or alkylaminodianthraquinonylamines by means of oleum in the presence or absence of boric acid.
It has now been found that the sulphation of these dianthrachirionylamine derivatives with boric acid-containing oleum takes place much more rapidly and leads to more soluble, probably more sulphonated products which are of particular value for dyeing purposes if they are used in the presence of mercury or its compounds such as Oxides or salts, preferably at temperatures between about 120-150 <B> 0 </B> from.
It could not be foreseen that mercury or its salts or oxides would facilitate the entry of sulio groups under these conditions without promoting the simultaneous formation of oxidation products, as is the case in the absence of boric acid (see for example < B> D. </B> RP <B> 472356, </B> Example <B> 3). </B>
The present patent is a process for the preparation of an acidic wool dye of the anthraquinone series, characterized in that 4..4'-diamino-1.1'-dianthraquinonylamine with oleum in the presence of boric acid and mercury or its compounds, such as salts or oxides , heated to temperatures between 120 and <B> 150 0 <I> C </I> </B>.
<I> Example: </I> <B> 10 </B> parts by weight of 4.4'-diai, .üino-1.1'-diaiithrachinonylamine are mixed with stirring in 1510 parts by weight of oleum of <B> 27 </B> "/ o SU3, in which 4 parts of boric acid were previously dissolved and 0.2 parts of HgO were suspended, dissolved and then heated to 135-140 <B> 0 </B> hours for about <B> 3 </B> hours After cooling, it was stirred into 800 parts of water to which slightly sulphurous acid had been added, then boiled up with 600 parts of saturated sodium chloride solution.
The deposited dye is filtered off and washed neutral with dilute sodium chloride solution.
The product is a blue-gray # 3 powder that dissolves in water with a greenish blue-gray, in concentrated sulfuric acid blue-gray, in boron-sulfuric acid a dirty green. It dyes unstained wool from acid baths in strong blue-gray tones with excellent fastness properties.
Claims (1)
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE149708X | 1929-06-07 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CH149708A true CH149708A (en) | 1931-09-30 |
Family
ID=5673492
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CH149708D CH149708A (en) | 1929-06-07 | 1930-06-05 | Process for the preparation of an acidic wool dye of the anthraquinone series. |
Country Status (1)
| Country | Link |
|---|---|
| CH (1) | CH149708A (en) |
-
1930
- 1930-06-05 CH CH149708D patent/CH149708A/en unknown
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