CS208507B1 - Method of preparation of stabil liquid form of the 4,4'-bis/6-aniline/-4-diethanolaminotriazin-2-ylamo/stilben-22'-ammonium disulphonate - Google Patents

Abstract

Process for preparing a stable liquid form 4,4'-bis / 6-anilino-4-diethanolaminotriazine Ammonium 2-ylamino / stbene-2,2'-disulfonate so that 4,4-bis / 6-chloro-4-sininotriazin-2-ylamino / stilbene-2,2 -disulfonan sodium prepared by MS. A0 162 582 heated in aqueous suspension with diethanolamine and sodium carbonate or acid carbonate. After the reaction was complete, the reaction solution became clear by filtration, acidified with hydrochloric acid, the precipitated product is filtered off with suction and after washing with water is stirred under addition urea.

Description

( ³⁴ ) A process for the preparation of a stable ammonium 4,4'-bis / 6-anilino-4-diethynolaminotriazin-2-ylamino / stilbene-2,2'-disulfonate liquid form.

A process for the preparation of a stable ammonium 4,4'-bis / 6-anilino-4-dietanolaminotriazin-2-ylamino / stlbene-2,2'-disulfonate liquid form by substituting 4,4-bis (6-chloro-4-snilinotriazine) Sodium-2-ylamino / stilbene-2,2-disulfonate prepared according to U.S. Pat. A0 162 582 is heated in an aqueous suspension with diethanolamine and sodium carbonate or bicarbonate. After completion of the reaction, the reaction solution is clarified by filtration, acidified with hydrochloric acid, the precipitated product is filtered off with suction and, after washing with water, stirred with the addition of urea.

208 507

208 507

The present invention relates to a process for the preparation of a liquid form of ammonium 4,4'-bis / 6-anilino-4-diethanolaminotriazin-2-yl-benzo / stilban-2,2'-dlsulfonate of formula 1

(I) a substance that is stable on storage and without turbidity is mixed in any proportion with water. The liquid forms of the compounds of the aforementioned structural formula are widely used for their easy handling and good solubility in the textile industry for the optical brightening of cellulosic materials instead of solid powders. Liquid forms are usually prepared by dissolving the sodium or alkanolamine salts of the base materials in water with the addition of various hydrotropic compounds. They are also obtained by condensing the cyanuric chloride with diaminostilbendisulfocyeeline and other suitable components in the presence of an excess of trialkanolamines such as hydrogen chloride binding and reaction. the solutions of the active compounds obtained are then concentrated by evaporation to the required concentration. A disadvantage of the processes described above for the preparation of the above-mentioned compound is that its usually isolated disodium salt does not give sufficiently stable solutions and the preparation by the second process does not provide sufficient quality products.

It has now been found that a sufficiently stable and pure liquid form of the compound of the above formula can be prepared in a simple manner using isolated 4,4'-bis (6-chloro-4-anilinotriazin-2-ylamino) atilbene-2,2'-disulfonate of sodium II

its condensation in aqueous suspension with diethanolamine, isolation of the acid form of product III

and dissolving it with the addition of urea aqueous ammonia and optionally water.

The required isolated semifinished product of formula (II) is preferably prepared according to U.S. Pat. AO 162 582 and is necessary in order to obtain a high quality of the liquid form produced. In the condensation, an equivalent or preferably up to 50% increased amount of diethanolamine and an equivalent or up to 50% increased amount of sodium carbonate or bicarbonate are used. Higher amounts of diethanolamine do not interfere, nor do I interfere with larger amounts of soda. The reaction will take place without the addition of alkaline, but the reaction is slower and may not complete completely within a reasonable time. Finally, however, the mixture must also be alkalinized to form a filterable solution. The effective condensation temperature lies at 98 ° C. At a lower temperature, the reaction time of the extension of SO8 is, the higher temperature is not detrimental. The resulting reaction solution is slightly turbid and should be clarified by addition of diatomaceous earth and hot filtration. The concentration of the active ingredient in the solution is limited so that when cleracl is hot the solution is clear and that aa does not precipitate the product from the solution during filtration. Greater dilution is not a defect, but it is not economical. The clarified reaction solution ae must be acidified at a temperature close to 98 ° C. At lower temperatures, the blank of formula III is deposited in a lubricating and difficult to filter form. It is acidified and preferably with dilute 18% hydrochloric acid, although no other concentration is detrimental. It must be able to safely reach a pH of 4.5 - 5. At a lower pH, e eliminates unwanted by-products and at a higher pH losses in the filtrates occur. The paste obtained is easily washed away with traces of unwanted by-products and electrolytes by washing with water. 20 to 60 wt. % urea by weight of the paste obtained and an equivalent or even 200% increased amount of aqueous ammonia. The desired liquid form is formed by stirring and heating the mixture to a temperature of up to 50 ° C. The concentration of the active ingredient in the solution depends on the amount of water contained in the preform III and the ammonia used and the amount of urea added.

By the process according to the invention and by low-tech processes and without using alkanolamines or glycols, they produce a stable liquid form of an important optically brightener with high quality and advantageously replacing the hitherto used powder and hardly applicable form.

The described example illustrates the method of preparation without exhausting all possible variations. The parts are by weight.

Example

A mixture of 55 parts of sodium 4,4'-bis / 6-chloro-4-aniline-triazin-2-ylamino / 8-benzene-2,2'-disulfonate in the form of 120 parts of wet paste from ee is dispersed in 500 parts of water, 20 parts are added. dletanolemin and 5 parts of soda ash and heated to 98 ° C with stirring for two hours. After addition of 1 part of diatomaceous earth and activated carbon, it is hot-cured and the filtrate is acidified to pH 4.5-5 with 35 parts of an 18% hydrochloric acid solution after heating to 98 ° C. The precipitated product is filtered off with suction while hot and washed into the colorless filtrate with water. The resulting 160 parts of the paste are stirred while heating to 45 ° with 45 parts of urea and 15 parts of 24% ammonia. It is adjusted to 250 parts by the addition of water and a stable and clear solution is obtained after cooling.

Claims (1)

SUBJECT OF THE INVENTION A process for the preparation of a stable ammonium 4,4'-ble (6-anilino-4-dletanolaminotriazin-2-ylamino) atilbene-2,2'-dieulfonate of the formula I n (ch ₂ ch ₂ oh) ₂ n (ch ₂ ch ₂₎ ch) ₂ (I) 208,507, characterized in that the isolated sodium 4,4'-bis (6-chloro-4-anilinotriazin-2-ylamine) stilbene-2,2-disulfonate is heated in an aqueous suspension with an equivalent or up to 50% increased amount of diethanolamine and equivalent to up to 50% increased carbonate or sodium bicarbonate to 90 to 100 ° C until the reaction is complete, the reaction solution is clarified by filtration with diatomaceous earth, acidified at 95 to 100 ° C by addition of hydrochloric acid to pH 4.5 - 5, the precipitated product is suctioned off hot and, after washing with water, mixed with urea in an amount of 20 to 60% by weight of the paste and an equivalent or up to 200% increase in aqueous ammonia, and the mixture is heated to dissolve.