阅读说明：本技术 一种d-泛酸钙制备新工艺 (Novel process for preparing D-calcium pantothenate ) 是由 吴江 于 2020-05-14 设计创作，主要内容包括：一种D-泛酸钙制备新工艺本发明涉及一种D-泛酸钙制备新工艺。本发明基本方案是：将DL-泛解酸内酯配成含量为16-26%的水溶液,加入此水溶液质量的5-15%生物酶,搅拌均匀后,在23-30℃缓慢滴加此水溶液所含D-泛解酸内酯0.49-0.51倍摩尔量的β-氨基丙酸钙含量为20%-30%的水溶液。一直反应至D-泛解酸内酯水解完全过滤出清液,滤饼生物酶循环使用。滴加过程中保持反应体系PH值为6.0-7.3之间。反应完成后清液在真空高于-0.085MPa浓缩至115-120℃,降温到65℃以下加入重量0.5-0.8倍D-泛解酸β-氨基丙酸钙的甲醇,搅拌降温到20-40℃,过滤,滤饼用甲醇洗涤、打浆、再洗涤实现纯化,几次滤液汇集起来,回收甲醇后消旋成DL-泛解酸内酯再次使用。滤饼通过105-125℃和150-160℃两级温区干燥后,降温出料即得D-泛酸钙。本发明在拆分反应的同时,一步生成D-泛酸钙的前体物质D-泛解酸β-氨基丙酸钙。避开了萃取分离D-泛解酸内酯的过程。(The invention relates to a novel process for preparing D-calcium pantothenate. The basic scheme of the invention is as follows: preparing the DL-pantoic acid lactone into an aqueous solution with the content of 16-26 percent, adding 5-15 percent of biological enzyme by mass of the aqueous solution, stirring uniformly, and slowly dropwise adding an aqueous solution with the content of 20-30 percent of beta-calcium aminopropionate with the molar weight of 0.49-0.51 time that of the D-pantoic acid lactone in the aqueous solution at 23-30 ℃. Reacting until D-pantoic acid lactone is hydrolyzed completely, filtering to obtain clear liquid, and recycling the biological enzyme in filter cakes. The PH value of the reaction system is kept between 6.0 and 7.3 in the dropping process. After the reaction is finished, concentrating the clear liquid to 115-120 ℃ under the vacuum pressure higher than-0.085 MPa, cooling to below 65 ℃, adding methanol with the weight 0.5-0.8 time that of D-pantoic acid beta-amino calcium propionate, stirring, cooling to 20-40 ℃, filtering, washing a filter cake with methanol, pulping, washing again to realize purification, collecting the filtrates for several times, and racemizing the filtrate into DL-pantoic acid lactone for reuse after recovering the methanol. Drying the filter cake in two temperature regions of 105-125 ℃ and 150-160 ℃, cooling and discharging to obtain the D-calcium pantothenate. The method can generate a precursor substance of D-calcium pantothenate, namely D-calcium pantoate beta-aminopropionate in one step during the resolution reaction. Avoids the process of extracting and separating D-pantoic acid lactone.)

一种D-泛酸钙制备新工艺

技术领域

本发明涉及一种D-泛酸钙制备新工艺。

背景技术

D-泛酸钙是维生素B5，化学名称为（R）-（+）-N-(2,4-二羟基-3，3-二甲基-1-氧代丁基)-β-丙氨酸钙盐，英文名：D-（+）-Pantothenic acid calcium salt，作为重要的营养成分，广泛用于饲料添加剂、食品添加剂、医药等领域；

D-泛酸钙合成路线，目前行业内使用的都是β-氨基丙酸与氧化钙在甲醇中反应合成β-氨基丙酸钙，过滤后再加入D-泛解酸内酯合成D-泛酸钙，通过低温结晶析出D-泛酸钙，其母液再回收甲醇、钙、D-泛解酸内酯、β-氨基丙酸等原料返回套用；回收不了或变质的物料做为废液交由环保系统处理，回收过程中利用到硫酸和大量的有机溶剂，增加了损耗而且作业环境差，这种工艺主原料综合利用率在工业生产中只能达到80-85%，并且D-泛解酸内酯还需要利用生物酶等拆分试剂从DL-泛解酸内酯中拆分再经过复杂的提取流程而得到。