DEP0022844DA - Process for the production of sulfamide and sulfamic acid - Google Patents

Description

Professor Dr., Otto Bayer and Dr. Ernst duration (both la ieverkuaen)

Kn / Seh Leverkusens, November 15, 1948

Process for the preparation of sulfamic and amidosulfonic acid

Ji β is known that SuIfamid warden shown in discontinuous and continuous process from sulfuryl chloride and ammonia kanne B © i dieaen method the whole ^ is the reaction of sulfuryl chloride besisißiiut® a certain ratio with a solvent -verdünnt and then with ammonia under intensive DurohmiBohung to the reaction brought _β Dur oh the great® VerdUjoaungaverbJiUtnle, daa wttnldi wlrd _s better® yields of sulfamic! been to eraIeIen _f mausen Grossa amounts Verdünnungamlttel continuously mitverarbeitat "Veratontet you here to a dilution, the sulfuryl the yield of sulf" amide &ehi> drops sharply "

Kb vrard © mm found that you can turn off the laughing part, great Meiigfeju Veraiirmungftinittol _? that the volume of the solvent does not change significantly during the reaction, since only sulfurylochloride cannot be mixed with ammonia, aura ammonia is added as a "special solution, and sulfuryl chloride is gradually allowed to flow into this solution medium." diluted check in accordance with dam solvent and is brought in this T@rdita.nung at the GreMschicht by weak mixing of örenzfläoheri with the liquid ammonia sur Heaktion ο Dl © © sweekmäßlgerwels mixing is achieved bq ₉ that used nian a Hührvorriohtung that the solution of Sulfuryl chloride into which ammonia looks "Since the solvent is immiscible with ammonia, it returns _? Free of sulfu" = rylchlorld, back into its layer and is used again

des SulfurylohloridB ₀ This is achieved that the diluted sulfurylohlorid used and on the other hand this Sulfupylohlorid in a diluted state with liquid immoxxiak on the örenasohloht solvent -. Ammonia ia H @ ak

tion can occur «
Ie A 48

In this Heratellungsweise needs ie in tegansati to the known! _Learn? where the reaction mixture must be set in strong turbulence , only weakly stirred? namely in the interface, line strong turbulence would the task here * which the solvent has to carry out _? destroy

The new process can also be carried out continuously with very good success The addition of sulfuryl chloride consumes ammonia continuously and the product eliminated is essentially eliminated Immoniuinchlorid and SuIfamid are consistently removed

Generally occur in the implementation τοη sulfuryl chloride with ammonia addition sulfamide still SulfamidkondeneatiQnsprodukte to that of Imidodisulfamid, Biimidotrisulfamid etc "beatehan" It is known that by several days of standing teaktionsproduktt aqueous acidic solution in hydrolyze the Kondensationsprodukta to suif = ®mid and Midosulfoneäur® " .

The processing of the reaction products can be, but significantly, simplified. The hydrolysis of the sulfamide condensation product is actually carried out at the moment * if one _p how was found? dia wäßrig® Suspension.der reaction products _f to Congo red gestallt j, this erhitstj for short © 2eit to boiling to daa already -vorhandene sulfamide trots its temperature τοη 93 ° C nieht.

Example Is

In © ineai Eeaktionsturm be 51o g flüsaigaff ammonia ©, ingefällte- The ammonia is übersehiehtet with 1.5 liters of a lentan-H © xaagemiseh®e "Di © cooling takes place by means .K & lteeol · $ DI® wirdg pumped through a built in Kühlsohlangensystem = 4o ^e g ₀ While in the upper zone of the Iiösungsmitt @ lschi © ht 4 © 5 g ■ neat sulfuryl chloride are gradually supplied dia boundary layer of ammonia-solvent aohwaeh quilted "is essentially Immoniumchlorid and sulfamide part as H®- Promotional products from ₀ This are sucked out of the reaction vessel and after the excess ammonia has evaporated, the reaction product is suspended in water. The suspension is made acidic to the Congo and heated to the boil for about 5 minutes, followed by cooling and filtering off the residual ammonium

Claims (3)

ehlorld s ordered, will the filtrate, which is mainly sulfamide _? next to it amidosulfonic acid "contains little dissolved ammonium chloride" - "evaporated with reduced brittle o The evaporation residue is extracted with methyl acetate or other specific solvents, rare isolation of the sulfamide <. The extraction residue becomes di @ amide sulfonic acid either by fractional crystallization or by reaction with concentrated acids9 whereby the amidosulfonic acid, in contrast to ammonia, goes into solution * SuIfamid and about 14 % amidosulfonic acid In a R®aktIonsturm ₉ u _e a ο © in © discharge device for the © Ä @ action product® and supply for ammonia contains »liquid ammonia is filled at a height of 15 em and the ammonia with a Htxan-Pentangemiseh at 25 em Layer overlaid to Dureh Kältesol © _? which is pumped through a built-in KUhlsohlangensyetem _s the cooling is kept at ~ 4'0 to "2o ° 0 o A stirrer _? the ammonia in the G-penzschient =» stands ensures throughout the imple ^ img for eiae the Gr © ngfläeh® * in a molar Terhlltnis 1 ι 8 l ₀ s IH) was © »unyardünntes Sulfurylohlorid in the top of the solution Mitt # lsehieht and condensed ammonia, the lower zone of the Ammoniaksehieht supplied ο Ba @ ausseheidönd © reaction product is continuously withdrawn and here, after evaporation of the excess ammonia, the sulfamide and the amidieulfone acids processed as in Example 1, Bie Auebeut © of sol amide amounts to about 80 _% of amidosulfonic acid about 2 © ^ ₉ dead »so on used sulfuryl chloride, 1} ¥ experience in the production of sulfamide and amido »ßulfoneMure _w through direct conversion of Sulfurylohlorld with llliBBlgem Jynmcmiak, ämü-axen k © niiB © ietoi © -t , & aB you © in eie'h not significantly change the volume during the heating Solvents that only look with sulfury chloride , but with ammonia misbehave to ammonia as a special sehloht and in the t @ r visually diminution of the surface and the duraates 3ul · = ft »ylohlorid in the solvent does not flow. 2) Proceed as follows. Claim. I ₉ dadureh “that the process is carried out continuously with the simultaneous addition of sulfuryl chloride and ammonia and removal of the reaction products 3) proceed according to claims 1 and 2, characterized in that the resulting mixture of seaction products is heated to boiling for a short time in an aqueous-Congo-acid medium