CS237748B1 - Preparation method of ammonium salt of 1-diazo-2-naphtol-6-nitro-4-sulphoacid - Google Patents
Preparation method of ammonium salt of 1-diazo-2-naphtol-6-nitro-4-sulphoacid Download PDFInfo
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- CS237748B1 CS237748B1 CS249684A CS249684A CS237748B1 CS 237748 B1 CS237748 B1 CS 237748B1 CS 249684 A CS249684 A CS 249684A CS 249684 A CS249684 A CS 249684A CS 237748 B1 CS237748 B1 CS 237748B1
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- Prior art keywords
- nitro
- diazo
- naphthol
- ammonium salt
- preparation
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- 150000003863 ammonium salts Chemical class 0.000 title claims abstract description 11
- 238000002360 preparation method Methods 0.000 title claims description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000007864 aqueous solution Substances 0.000 claims abstract description 6
- 238000000746 purification Methods 0.000 claims abstract description 6
- 238000001914 filtration Methods 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims abstract description 4
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 3
- 239000011541 reaction mixture Substances 0.000 claims abstract 2
- 239000002253 acid Substances 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 4
- 239000007858 starting material Substances 0.000 claims description 2
- 125000000020 sulfo group Chemical group O=S(=O)([*])O[H] 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract 1
- 239000012452 mother liquor Substances 0.000 abstract 1
- 238000006396 nitration reaction Methods 0.000 abstract 1
- 239000000975 dye Substances 0.000 description 4
- 239000000047 product Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 239000012736 aqueous medium Substances 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
Způsob přípravy amonné soli 1-diazo-2- ~naftol-6-nitro-4-sulfokyseliny vzorce nitrací l-diazo-2-naftol-4-sulfokyseliny tak, že se výchozí surovina převede na vodný roztok s obsahem volné 1-diazo-2- -naftol-6-nitro-4-sulfokyseliny 0,7 až 1,3 mol.dra-’', vzniklý roztok se neutralizuje plynným amoniakem, popřípadě jeho koncentrovaným vodným roztokem na hodnotu pH 2,3 až 5,7, amonná sůl 1-diazo-2- -naftol-6-nitro-4-sulfokyseliny se z reakční směsi izoluje filtrací a matečné louhy se popřípadě použijí pro dalěí purifikační cyklus.Process for preparing 1-diazo-2- ammonium salt naphthol-6-nitro-4-sulfoacids of formula nitration of 1-diazo-2-naphthol-4-sulfoacid by converting the feedstock to aqueous solution containing 1-diazo-2- naphthol-6-nitro-4-sulfoacids 0.7 to 1,3 mol.dra- ', the resulting solution is neutralized ammonia gas, or its ammonia concentrated aqueous solution to pH 2.3 to 5.7, ammonium salt 1-diazo-2- naphthol-6-nitro-4-sulfoacids are isolated from the reaction mixture by filtration and mother liquor the liquors are optionally used for further processing purification cycle.
Description
Předaětem vynálezu je způsob přípravy amonná soli 1-diazo-2-naftol-6-nitro-4-aulfokyaeliny.The present invention provides a process for the preparation of the ammonium salt of 1-diazo-2-naphthol-6-nitro-4-sulfonic acid.
Amonná sůl 1-diazo-2-aaftol-6-nitro-4-sulfokyseliny vyráběná nitracl 1 - dieto-2-naftol-4-sulfokyaeliny má použití pro přípravu mořidlových, popřípadě metalokomplemnlch barviv. Průmysloví vyráběná 1 -diazo-2-nef tol-6-nitro-4-aulfokyoelina je v «hledem k vicestupňovému způsobu výroby doprovázen· ředou nežádoucích vedlejších látek, která při dmlěím zpracování značně zhoršují kvalitu odstínu a etáloeti syntetizovaných barviv·The ammonium salt of 1-diazo-2-aaftol-6-nitro-4-sulfoacid produced by nitracyl-1-diethoxy-2-naphthol-4-sulfoacid has utility for the preparation of mordant or metalocomplete dyes. The industrially produced 1-diazo-2-nef tol-6-nitro-4-aulfokyoelina is accompanied by a series of undesirable side-products which, in the course of a longer processing time, significantly deteriorate the hue quality and the etoethane of synthesized dyes.
Z těchto důvodů bývá obyčejně při jojieh přípravě nutná masioperačni izolace, která vedle výrobcích ztrát přináěí i jiné potíže.For these reasons, a massioperative insulation is usually required during preparation, which, in addition to the loss products, also causes other problems.
Nyní bylo nelezeno, So k podstatně účinějšlmu odstranění nežádoucích balaatních látek, tedy bez nutnosti méně účinné izolace ve stadiu barvivé ae dochází v případě, kdy pro ayntezu jo k diapoalcl vysoce čistá amonná sůl 1-diazo-2-naftol-6-nitro-4-sulfokyaeliny připravená neutrellsecí surové volné kyseliny amoniakem ve vodném prostředí.It has now been found that the removal of undesirable balate substances is substantially more effective, i.e. without the need for less effective isolation at the dye stage, and occurs when a high purity ammonium salt of 1-diazo-2-naphthol-6-nitro-4 - sulfoacids prepared by neutralizing the crude free acid with ammonia in an aqueous medium.
Způsob přípravy amonné soli l-diazo-2-naftol-6-nitro-4-aulfokyzeliny vzorce «A process for the preparation of the ammonium salt of 1-diazo-2-naphthol-6-nitro-4-sulfonic acid of the formula
nitřecí 1-diazo-2-naftol-4-sulfokyaeliny spočívá podle vynálezu v toa, že ae výchozí surovina převede ne vodný roztok z obsahem volné 1-diazo-2-naftol-6-nitro-4-sulfokyseliny 0,7 až 1,3 mol.dm~3, vzniklý roztok se neutralizuje plynným amoniakem, popřípadě jeho koncentrovaným vodným roztokem na hodnotu pH 2,3 až 5,7, amonná sůl 1-diazo-2-naftol-6-nitro-4-sulfokysoliay ao z reekční směsi izoluje filtrací a matečné louhy se popřípadě použijí pro dalěí purifikečni proces.According to the invention, the nitro-1-diazo-2-naphthol-4-sulfo-acid is based on the fact that the starting material converts into an aqueous solution from a content of free 1-diazo-2-naphthol-6-nitro-4-sulfoacid of 0.7 to 1; 3 mol.dm-3, the resulting solution is neutralized with ammonia gas or a concentrated aqueous solution thereof to a pH of 2.3 to 5.7, 1-diazo-2-naphthol-6-nitro-4-sulfo-acidic ammonium salt the mixture is isolated by filtration and the mother liquors are optionally used for further purification process.
Uvedeným způsobem se získá vysoce čisté surovina, vhodná pro přípravu dříve uvedených barviv, ve výtěžku 80 % až 95 %, přičemž jak bylo uvedeno, lze s výhodou matečné louhy opakované použít pro dalěí purifikečni cyklus, čímž se i avýíí výtěžnost čisticího procesu. T 'In this way, a high purity raw material suitable for preparing the aforementioned dyes is obtained in a yield of 80% to 95%, and as mentioned, the mother liquors can advantageously be re-used for the next purification cycle, thereby increasing the yield of the purification process. T '
Způsob čištění 1-diazo-2-naftol-6-nitro-4-aulfokysellny podle vynálezu je déle popeán následujícím příkladem, který však není jeho omezením.The method of purification of 1-diazo-2-naphthol-6-nitro-4-sulfonic acid according to the invention is described in more detail by the following non-limiting example.
PříkladExample
500 kg surové pasty a obsahem 65 % volné 1-diazo-2-naftol-6-nitro-4-sulfokyzeliny ze za stálého míchání rozpustí v , 200 diP vody při teplotě 16 až 23 °C a do vzniklého roztoku se uvádí koncentrovaný roztok amoniaku v takovém množství, aby bylo dosaženo výsledné hodnoty pH 3,5, kdy také začne z reakčnl aměai vypadávat avětložlutá krystalická látka, odpovídající amonné soli 1-diazo-2-naftol-6-nitro-4-sulfokyaeliny. Vzniklé suspenze se míchá až 1 hodinu a po této době se krystalický produkt oddělí filtrací.500 kg of crude paste containing 65% free 1-diazo-2-naphthol-6-nitro-4-sulfoacidine was dissolved in 200 diP of water at 16 to 23 ° C with stirring and the resulting solution was treated with concentrated ammonia solution. in such an amount as to obtain a final pH of 3.5, at which time also a pale yellow crystalline substance corresponding to the ammonium salt of 1-diazo-2-naphthol-6-nitro-4-sulfocyanel also starts to precipitate from the reaction. The resulting suspension was stirred for up to 1 hour, after which time the crystalline product was collected by filtration.
Filtrát obsahující vedle rozpuštěných balaatních příměsi i 8 % soli 1-diazo-2-nařtol-6-nitro-4-aulfokyaeliny může být použit pro rozpuštění dalěí dávky výchozí suroviny, přičemž počet cyklů je omezen výchozí a požadovanou kvalitou 1-diazo-2-naftol-6-nitro-4-aulfpkyaeliny, resp. její amonné soli.The filtrate containing 8% of 1-diazo-2-naphthol-6-nitro-4-sulfonyl acid salt in addition to the dissolved balate admixtures can be used to dissolve another batch of feedstock, the number of cycles being limited by the starting and desired quality of 1-diazo-2- naphthol-6-nitro-4-sulfonyl acids, respectively. its ammonium salts.
Claims (1)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CS249684A CS237748B1 (en) | 1984-04-02 | 1984-04-02 | Preparation method of ammonium salt of 1-diazo-2-naphtol-6-nitro-4-sulphoacid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CS249684A CS237748B1 (en) | 1984-04-02 | 1984-04-02 | Preparation method of ammonium salt of 1-diazo-2-naphtol-6-nitro-4-sulphoacid |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CS237748B1 true CS237748B1 (en) | 1985-10-16 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CS249684A CS237748B1 (en) | 1984-04-02 | 1984-04-02 | Preparation method of ammonium salt of 1-diazo-2-naphtol-6-nitro-4-sulphoacid |
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| Country | Link |
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| CS (1) | CS237748B1 (en) |
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1984
- 1984-04-02 CS CS249684A patent/CS237748B1/en unknown
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