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An electroslag refining apparatus includes upper and lower integral crucibles, with the lower crucible having a drain. In situ hot start is effected by depositing in the lower crucible a pre-refined starter. The starter is melted in the lower crucible to form a starter pool, and slag is deposited at

An electroslag refining apparatus includes upper and lower integral crucibles, with the lower crucible having a drain. In situ hot start is effected by depositing in the lower crucible a pre-refined starter. The starter is melted in the lower crucible to form a starter pool, and slag is deposited atop the starter pool for being melted thereby to develop a slag pool thereatop. An ingot electrode is lowered through the upper crucible to immerse a tip thereof into the slag pool. The electrode is powered to effect resistance heating of the slag pool to melt the electrode tip. The slag and starter pools are increased in volume into the upper crucible, with the drain then being opened to effect steady state operation.

대표청구항 ▼

An electroslag refining apparatus includes upper and lower integral crucibles, with the lower crucible having a drain. In situ hot start is effected by depositing in the lower crucible a pre-refined starter. The starter is melted in the lower crucible to form a starter pool, and slag is deposited at

An electroslag refining apparatus includes upper and lower integral crucibles, with the lower crucible having a drain. In situ hot start is effected by depositing in the lower crucible a pre-refined starter. The starter is melted in the lower crucible to form a starter pool, and slag is deposited atop the starter pool for being melted thereby to develop a slag pool thereatop. An ingot electrode is lowered through the upper crucible to immerse a tip thereof into the slag pool. The electrode is powered to effect resistance heating of the slag pool to melt the electrode tip. The slag and starter pools are increased in volume into the upper crucible, with the drain then being opened to effect steady state operation. m 2, wherein one reactive intermediate is Ziprasidone free base and the other reactive intermediate is aqueous HCl solution. 10. The process of claim 1, wherein said product is Ziprasidone hydrochloride monohydrate. 11. The process of claim 1, wherein said product is Voriconazole free base. 12. The process of claim 2, wherein said basic intermediate is selected from sodium acetate, potassium acetate, sodium hydroxide, potassium hydroxide, sodium carbonate, sodium bicarbonate, and said acidic intermediate is Voriconazole R-(-)-camphorsulfonic acid salt. 13. The process of claim 1, wherein each of said liquid jet streams emerges from a nozzle having an outlet hole and with each said nozzle from which each jet stream emerges directed sufficiently downward to ensure that said liquid jet streams emerging from each nozzle will not enter said outlet hole of said substantially diametrically opposite nozzle. 14. The process of claim 1, wherein said product produced upon crystallization is solvated. 15. The process of claim 2, wherein one reactive intermediate is 5,8,14-triazatetracyclo[10.3.1.02,11.04,9]-hexadeca-2(11),3,5,7,9-pentaene free base and the other reactive intermediate is a L-tartaric acid solution. 16. The process of claim 1, wherein said product is 5,8,14-triazatetracyclo[10.3.1.02,11.04,9]-hexadeca-2(11),3,5,7,9-pentaene (L)-tartrate. 17. The process of claim 1, wherein the linear velocity of the jet streams is at least 5 m/sec. 18. The process of claim 1, wherein a sonication probe is included with said impinging jet streams. 19. A process for synthesis and crystallization of a pharmaceutical compound comprising contacting one or more jet streams of a solution in a first solvent of a first reactive intermediate and one or more jet streams of a solution in a second solvent of a second reactive intermediate, said jet streams impinging to create turbulence at their point to impact under conditions of temperature and pressure which permit reaction of said first and second reactive intermediates to produce a product; and, selecting said first and second solvents so that said product is insoluble in a mixture of said first and second solvents; and said jet streams impinging to create turbulence at their point of impact and each jet stream having sufficient linear velocity to achieve micromixing of said solutions followed by reaction of first and second reactive intermediates, followed by nucleation of said product and production of a crystalline product having small crystals of controlled particle size, wherein said crystals of said product meet bioavailability requirements, wherein said first reactive intermediate is selected from Ziprasidone free base or 5,8,14-triazatetracyclo[10.3.1.02,11.04,9]-hexadeca-2(11),3,5,7,9-pentaene free base, and said second reactive intermediate is selected from HCl or L-tartaric acid. 20. The process of claim 19, wherein said first reactive intermediate is Ziprasidone free base and said second reactive intermediate is HCl. 21. The process of claim 19, wherein said crystalline product is Ziprasidone hydrochloride monohydrate. 22. The process of claim 19, wherein said first reactive intermediate is 5,8,14-triazatetracyclo[10.3.1.02,11.04,9]-hexadeca-2(11),3,5,7,9-pentaene free base and said second reactive intermediate is a L-tartaric acid. 23. The process of claim 19 wherein said crystalline product is 5,8,14-triazatetracyclo[10.3.1.02,11.04,9]-hexadeca-2(11),3,5,7,9-pentaene (L)-tartrate. 24. A process for synthesis and crystallization of a pharmaceutical compound comprising contacting one or more jet streams of a solution in a first solvent of a first reactive intermediate and one or more jet streams of a solution in a second solvent of a second reactive intermediate, said jet streams impinging to create turbulence at their point of impact under conditions of temperature and pr