There are provided methods for producing solid anhydrous methylolhydantoins. Initially, an aqueous stirrable medium is dehydrated and heated to yield a substantially anhydrous stirrable melt. The aqueous stirrable medium includes (A) a solute selected from the group consisting of (i) a dimethyloldimethylhydantoin, (ii) a hydantoin reactant, (iii) a formaldehyde source reactant, or (iv) a combination of any of the foregoing; and (B) optionally a catalyst. A molten system is then provided by adding, to the stirrable melt, a reactant mixture which includes (A)(i) the same or a different hydantoin reactant, (ii) a substantially anhydrous formaldehyde source reactant which may be the same as or different than the formaldehyde source reactant, or (iii) a combination thereof; and (B) optionally, the same or a different catalyst; wherein the molten system includes (i) at least one hydantoin reactant and (ii) at least one dehydrated formaldehyde source reactant or substantially anhydrous formaldehyde source reactant. The at least one hydantoin reactant and the at least one dehydrated formaldehyde source reactant or substantially anhydrous formaldehyde source reactant in the molten system are reacted, while reaction water is removed, to yield anhydrous molten methylolhydantoin. Finally, the molten methylolhydantoin is solidified. Alternatively, solid anhydrous methylolhydantoin is produced by reacting, in an aqueous stirrable medium as above, a reactant mixture of (i) the same or a different hydantoin reactant, (ii) a substantially anhydrous formaldehyde source reactant which may be the same as or different than the formaldehyde source reactant, or (ii) a combination thereof and (iv) optionally, the same as or different catalyst; wherein (i) at least one hydantoin reactant and (ii) at least one formaldehyde source reactant or substantially anhydrous formaldehyde reactant is present; while heating to at least the melting temperature of the methylolhydantoin and while removing substantially all water; to yield a molten methylolhydantoin; and subsequently solidifying the molten methylolhydantoin. These methods can be practiced as batch processes or as semi-continuous processes.
本发明提供了生产固体无
水甲基海因的方法。首先,对含
水可搅拌介质进行脱
水和加热,以得到基本无
水的可搅拌熔体。
水性可搅拌介质包括:(A) 选自以下组别的溶质:(i) 二甲基二羟甲基海因,(ii) 海因反应物,(iii)
甲醛源反应物,或 (iv) 上述任一物质的组合;以及 (B) 可选催化剂。然后通过向可搅拌熔体中加入反应物混合物来提供熔融体系,该反应物混合物包括 (A)(i)相同或不同的海因反应物,(ii)与
甲醛源反应物相同或不同的基本无
水甲醛源反应物,或 (iii) 上述反应物的组合;(B) 可选地,相同或不同的催化剂;其中熔融体系包括 (i) 至少一种海因反应物和 (ii) 至少一种脱
水甲醛源反应物或基本无
水甲醛源反应物。熔融体系中的至少一种海因反应物和至少一种脱
水甲醛源反应物或基本无
水甲醛源反应物发生反应,同时除去反应
水,生成无
水熔融甲基海因。最后,将熔融的甲基海因固化。另一种方法是,在上述
水性可搅拌介质中,通过以下反应物混合物反应制得固态无
水甲基海因:(i) 相同或不同的海因反应物;(ii) 与
甲醛源反应物相同或不同的基本无
水甲醛源反应物;或 (ii) 它们的组合;(iv) 可选的相同或不同的催化剂;其中(i)至少存在一种海因反应物和(ii)至少存在一种
甲醛源反应物或基本无
水的
甲醛反应物;同时加热至至少
甲醇海因的熔化温度,并除去基本所有的
水;得到熔融的
甲醇海因;随后将熔融的
甲醇海因凝固。这些方法可以分批进行,也可以半连续进行。