PL9904B1 - The method of making black dyes. - Google Patents
The method of making black dyes. Download PDFInfo
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- PL9904B1 PL9904B1 PL9904A PL990428A PL9904B1 PL 9904 B1 PL9904 B1 PL 9904B1 PL 9904 A PL9904 A PL 9904A PL 990428 A PL990428 A PL 990428A PL 9904 B1 PL9904 B1 PL 9904B1
- Authority
- PL
- Poland
- Prior art keywords
- treated
- dyes
- black dyes
- making black
- added
- Prior art date
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- 239000000975 dye Substances 0.000 title claims description 7
- 238000004519 manufacturing process Methods 0.000 title 1
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 claims description 8
- 229920001021 polysulfide Polymers 0.000 claims description 4
- 239000003513 alkali Substances 0.000 claims description 3
- 150000003863 ammonium salts Chemical class 0.000 claims description 3
- 239000000988 sulfur dye Substances 0.000 claims description 3
- 229910052979 sodium sulfide Inorganic materials 0.000 claims description 2
- 238000000034 method Methods 0.000 claims 3
- SEEZWGFVHCMHJF-UHFFFAOYSA-N 2-nitrosophenol Chemical class OC1=CC=CC=C1N=O SEEZWGFVHCMHJF-UHFFFAOYSA-N 0.000 claims 1
- 239000007864 aqueous solution Substances 0.000 claims 1
- 239000007795 chemical reaction product Substances 0.000 claims 1
- 150000001896 cresols Chemical class 0.000 claims 1
- 230000003647 oxidation Effects 0.000 claims 1
- 238000007254 oxidation reaction Methods 0.000 claims 1
- 150000002989 phenols Chemical class 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 238000009835 boiling Methods 0.000 description 3
- UFBJCMHMOXMLKC-UHFFFAOYSA-N 2,4-dinitrophenol Chemical compound OC1=CC=C([N+]([O-])=O)C=C1[N+]([O-])=O UFBJCMHMOXMLKC-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- RLSSMJSEOOYNOY-UHFFFAOYSA-N m-cresol Chemical compound CC1=CC=CC(O)=C1 RLSSMJSEOOYNOY-UHFFFAOYSA-N 0.000 description 2
- 229940100630 metacresol Drugs 0.000 description 2
- 238000010926 purge Methods 0.000 description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- OXNIZHLAWKMVMX-UHFFFAOYSA-N picric acid Chemical compound OC1=C([N+]([O-])=O)C=C([N+]([O-])=O)C=C1[N+]([O-])=O OXNIZHLAWKMVMX-UHFFFAOYSA-N 0.000 description 1
- 239000005077 polysulfide Substances 0.000 description 1
- 150000008117 polysulfides Polymers 0.000 description 1
- HYHCSLBZRBJJCH-UHFFFAOYSA-N sodium polysulfide Chemical compound [Na+].S HYHCSLBZRBJJCH-UHFFFAOYSA-N 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 230000001052 transient effect Effects 0.000 description 1
- 229950002929 trinitrophenol Drugs 0.000 description 1
Description
Dwunitro- lub trójnitrofenole oddziel¬ nie lub zmieszane, dodane do nitrozonorto- lub metakrezolu, uprzednio zredukowane¬ go w roztworze siarczku sodowego, daja przez zagotowanie z wielosiarczkami alka- licznemi barwniki czarne. Barwniki te nie stosowane w farbiarstwie, nie ustepuja pod wzgledem intensywnosci czarnym barwni¬ kom siarkowym dotychczas znanym.Stwierdzono, ze jesli sie przemieni po¬ rzadek reakcji, a mianowicie gdy spowo¬ duje sie najpierw; reakcje fenolu dwu- lub trójnitrowanego z siarczkiem sodowym i doda nastepnie pochodna nitrozowana, a zakonczy dzialaniem wielosiarczku alka¬ licznego — wówczas intensywnosc uzyska¬ nego barwnika rosnie czterokrotnie, a od¬ cien zyskuje. Wynik ten jest szczególnie widoczny, jesli sie zastapi wytracanie po¬ wietrzem i kwasem przez wytracanie po¬ wietrzem i solami amonowemi.Przyklad, Dof zbiornika zelaznego, za¬ opatrzonego w mieszadlo mechaniczne, w chlodnice odplywowa i w podwójne scia¬ ny, dozwalajace na dopuszczenia naprze- mian zimnej wody i pary, wprowadza sie siarczku sodowego krystalicznego 100 kg wody 140 L Po zmieszaniu i rozpuszczeniu dodaje sie dwunitrofenolu 1, 2, 4 22 kg 500Reakcja odbywa sie z poczatku na zim¬ no, a pózniej ogrzewa sie az do redukcji.Nastepnie oziebia sie i dodaje: nitrozo-orto- lub metakrezolu 35 kg albo nitrozofenolu 31 kg.Reakcje przeprowadza sie na zimno, a nastepnie ogrzewa sie az do rozpoczecia reakcji. Wtedy wstrzymuje sie (doplyw pary i pozostawia reakcje samej sobie, Gdy reakcja uspokoila sie, dodaje sie na zimno wielosiarczku sodowego, uzyskane¬ go, mieszajac na goraco az do rozpuszcze¬ nia sie 110 kg siarczku sodowego krysta¬ licznego i 60 kg kwiatu siarkowego.Po dodaniu wielosiarczku podnosi sie temperature az do wrzenia, w której u- trzymuje sie przez 6 do 7 godzin, az do znikniecia zabarwien przejsciowych. Czyn¬ nosc te wykonywa sie, pozwalajac odpa¬ rowanej wodzie po skropleniu sie splynac do przyrzadu zpowrotem.Po ukonczeniu tej czynnosci, zwiekszy¬ la sie objetosc mieszaniny o objetosc wo¬ dy i jest utleniona przez strumien powie¬ trza. Temperature podnosi sie nastepnie az do wrzenia i straca przez dodatek soli amonowej. Wydzielony barwnik saczy sie, myje i suszy.Mozna dwunitrofenol zastapic czescio¬ wo lub w calosci przez trójnitrofenol, zwiekszajac ilosc siarczku sodu, uzytego na pierwszem miejscu.Otrzymane barwniki staja sie plynne przez bezposrednie zmieszanie z krysta¬ licznym siarczkiem sodowym, PL PLThe dinitro- or trinitrophenols, separately or mixed, added to the nitrosonortho- or metacresol, previously reduced in sodium sulphide solution, give black dyes by boiling with alkali polysulphides. These dyes, not used in dyeing, do not yield in intensity to the black sulfur dyes known hitherto. It has been found that if the order of the reaction is changed, namely when it is first caused reaction of the di- or trinitrated phenol with sodium sulphide and then the nitrosated derivative will be added, and it will end with the action of alkali polysulphide - then the intensity of the dye obtained increases fourfold and the shade becomes less. This result is particularly evident if the purging of air and acid is replaced by purging with air and ammonium salts. For example, for an iron tank equipped with a mechanical agitator, a drain cooler and a double wall permitting admission of pressure - of cold water and steam, the crystalline sodium sulphide is introduced 100 kg of water 140 L After mixing and dissolving, 1, 2, 4 22 kg of dinitrophenol are added 500 The reaction takes place initially in the cold, and then it is heated until reduction. cooled and added: nitroso-ortho- or metacresol 35 kg or nitrosophhenol 31 kg. Reactions are carried out in the cold and then heated until the reaction starts. Then the flow of steam is stopped (and the reaction is left to itself. When the reaction has calmed down, the sodium polysulfide obtained is added cold, while hot stirring, until 110 kg of crystalline sodium sulfide and 60 kg of sulfur flower are dissolved. After the polysulfide has been added, the temperature is raised to the boiling point for 6 to 7 hours, until the transient colors are gone. This is done by letting the condensed evaporated water run back to the instrument. this activity, the volume of the mixture is increased by the volume of water and is oxidized by the air stream. The temperature is then raised to boiling point and lost by adding ammonium salt. The separated dye is filtered, washed and dried. The dinitrophenol can be replaced with some - either by or entirely by trinitrophenol, increasing the amount of sodium sulphide used in the first place. The resulting dyes become fluid by mixing directly with the crystal abundant sodium sulphide, PL PL
Claims (3)
Publications (1)
| Publication Number | Publication Date |
|---|---|
| PL9904B1 true PL9904B1 (en) | 1929-02-28 |
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