申请人:——
公开号:US20040019235A1
公开(公告)日:2004-01-29
Higher (meth)acrylates are prepared by reacting (meth)acrylic acid and the alcohol in the presence of at least one acidic catalyst and at least one polymerization inhibitor and in the presence of a solvent which forms an azeotropic mixture with water and distilling off and condensing the azeotropic mixture, the condensate separating into an aqueous phase and an organic phase, by a process in which
a) the esterification is carried out in a reactor having a circulation evaporator and
b) in the presence of at least 10% by weight, based on the reaction mixture, of solvent, and either
c1) at least a part of the solvent, if required a part of the catalyst (mixture) and, if required, at least a part of the polymerization inhibitor (mixture) are initially taken in the esterification reactor and heated to the boiling point of the component having the lowest boiling point in the system and, as soon as the circulation is in operation, (meth)acrylic acid and alcohol and, if required, residual catalyst, polymerization inhibitor and solvent are metered in together or separately, or
c2) at least a part of the solvent, if required a part of the catalyst (mixture), if required at least a part of the polymerization inhibitor (mixture) and at least a part of the alcohol are initially taken in the esterification reactor and heated to the boiling point of the component having the lowest boiling point in the system and, as soon as the circulation is in operation, (meth)acrylic acid and, if required, the remaining alcohol and, if required, residual catalyst, polymerization inhibitor and solvent are metered in together or separately, or
c3) at least a part of the solvent, at least a part of the catalyst (mixture), at least a part of the polymerization inhibitor (mixture) and at least a part of the (meth)acrylic acid are initially taken in the esterification reactor and heated to the boiling point of the component having the lowest boiling point in the system and, as soon as the circulation is in operation, the alcohol and, if required, the remaining (meth)acrylic acid and, if required, residual catalyst, polymerization inhibitor and solvent are metered in together or separately, or
c4) at least a part of the solvent, at least a part of the catalyst (mixture), at least a part of the polymerization inhibitor (mixture), at least a part of the alcohol and a part of the (meth)acrylic acid are initially taken in the esterification reactor and heated to the boiling point of the component having the lowest boiling point in the system and, as soon as the circulation is in operation, if required the remaining alcohol and the remaining (meth)acrylic acid and, if required, residual catalyst, polymerization inhibitor and solvent are metered in together or separately.
通过在至少一个酸性催化剂和至少一个聚合抑制剂的存在下,以及在与水形成共沸混合物的溶剂的存在下,通过反应(甲基)丙烯酸和醇制备较高的(甲基)丙烯酸酯,并蒸馏和冷凝共沸混合物,冷凝物分离成水相和有机相的过程,其中a)在具有循环蒸发器的反应器中进行酯化反应,并且b)在至少10%的溶剂存在下,基于反应混合物的重量,取所需的溶剂的一部分,如有必要,取所需的催化剂(混合物)的一部分,如有必要,取所需的聚合抑制剂(混合物)的一部分最初放入酯化反应器中并加热至系统中沸点最低的组分的沸点,一旦循环运行,(甲基)丙烯酸和醇以及如有必要的残余催化剂、聚合抑制剂和溶剂一起或分别计量,或c2)至少取所需的溶剂的一部分,如有必要取所需的催化剂(混合物),如有必要取所需的聚合抑制剂(混合物)和至少取所需的醇的一部分最初放入酯化反应器中并加热至系统中沸点最低的组分的沸点,一旦循环运行,(甲基)丙烯酸和如有必要的剩余醇以及如有必要的残余催化剂、聚合抑制剂和溶剂一起或分别计量,或c3)至少取所需的溶剂的一部分,至少取所需的催化剂(混合物)的一部分,至少取所需的聚合抑制剂(混合物)的一部分和至少取(甲基)丙烯酸的一部分最初放入酯化反应器中并加热至系统中沸点最低的组分的沸点,一旦循环运行,醇和如有必要的剩余(甲基)丙烯酸以及如有必要的残余催化剂、聚合抑制剂和溶剂一起或分别计量,或c4)至少取所需的溶剂的一部分,至少取所需的催化剂(混合物)的一部分,至少取所需的聚合抑制剂(混合物)的一部分,至少取所需的醇的一部分和(甲基)丙烯酸的一部分最初放入酯化反应器中并加热至系统中沸点最低的组分的沸点,一旦循环运行,如有必要,剩余的醇和剩余的(甲基)丙烯酸以及如有必要的残余催化剂、聚合抑制剂和溶剂一起或分别计量。