申请人:BASF SE
公开号:US20190002389A1
公开(公告)日:2019-01-03
A process for continuously preparing the tert-butyl ester of an ethylenically unsaturated carboxylic acid, by a) reacting an ethylenically unsaturated carboxylic acid with isobutene in the presence of an acidic catalyst to give an esterification mixture; b) removing the acidic catalyst; c) removing low-boiling components; and d) supplying a tert-butyl ester-comprising liquid to a distillation apparatus and subjecting it to purifying distillation in the distillation apparatus, where
d
1
) in the distillation apparatus the tert-butyl ester-comprising liquid is separated into a tert-butyl ester-comprising gaseous top product and a carboxylic acid-comprising liquid bottom product;
d
2
) the tert-butyl ester-comprising gaseous top product is at least partly condensed and the condensate is recycled partly as reflux to the distillation apparatus;
d
3
) the carboxylic acid-comprising liquid bottom product is recycled at least partly to step a);
d
4
) carboxylic acid-comprising liquid bottom product is drawn off and passed to a heater; a superheated, liquid recycle stream is taken from the heater; and the superheated recycle stream is let down into the distillatiuon apparatus; and
d
5
) at least in the top region of the distillation apparatus, the distillation apparatus walls in contact with the vapor, at least in sub-regions, are heated and/or thermally insulated. In the course of the process, the separation of the tert-butyl ester from unreacted carboxylic acid is carried on with a particularly low level of accompanying polymerization both of the tert-butyl ester and of the carboxylic acid.
一种连续制备乙烯基不饱和羧酸叔丁酯的方法,包括以下步骤:a)在酸性催化剂存在下,将乙烯基不饱和羧酸与异丁烯反应,得到酯化混合物;b)去除酸性催化剂;c)去除低沸点成分;d)将含有叔丁酯的液体供给蒸馏设备,在蒸馏设备中进行纯化蒸馏,其中d1)在蒸馏设备中,将含有叔丁酯的液体分离成含有叔丁酯的气态顶部产品和含有羧酸的液态底部产品;d2)将含有叔丁酯的气态顶部产品至少部分冷凝,所得冷凝物部分作为回流物回收至蒸馏设备;d3)将含有羧酸的液态底部产品至少部分回收至步骤a);d4)将含有羧酸的液态底部产品抽出并通过加热器,从加热器中取出过热的液态回收流,将过热的回收流放入蒸馏设备中;d5)至少在蒸馏设备的顶部区域,与蒸汽接触的蒸馏设备壁面至少在子区域中加热和/或热绝缘。在该过程中,从未反应的羧酸中分离出叔丁酯,伴随的叔丁酯和羧酸的聚合水平特别低。