CN1304296C - 医药级牡蛎碳酸钙的生产方法 - Google Patents

医药级牡蛎碳酸钙的生产方法 Download PDF

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CN1304296C
CN1304296C CNB2004100308837A CN200410030883A CN1304296C CN 1304296 C CN1304296 C CN 1304296C CN B2004100308837 A CNB2004100308837 A CN B2004100308837A CN 200410030883 A CN200410030883 A CN 200410030883A CN 1304296 C CN1304296 C CN 1304296C
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calcium carbonate
calcium
oyster
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CN1562760A (zh
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李卫平
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All American World China Pharmaceutical Co ltd
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Abstract

本发明公开了一种原料药的生产方法，特别是一种医药级牡蛎碳酸钙的生产方法，属于医药原料药技术领域。本发明通过由活性钙直接与二氧化碳在双层密闭容器中干法反应制得。本发明的优点就在于：生产工艺简单，易于控制，制得的产品纯度高，成本较低，无污染，完全符合国家药品标准。

Description

医药级牡蛎碳酸钙的生产方法
发明领域
本发明涉及一种原料药的生产方法，特别是一种医药级牡蛎碳酸钙的生产方法，属于医药原料药技术领域。
背景技术
医药级牡蛎碳酸钙是国家药品监督管理局和国家药典委员会规定的用来取代活性钙的一种原料药，这是因为：活性钙为无污染的牡蛎壳，经高温煅烧、水解后制得的原料药，主要成分为Ca(OH)2，钙含量为46～53％，pH值大于11，属于强碱性，对肠胃有刺激性。医药级牡蛎碳酸钙的新国家药品标准WS-10001-(HD-1034)-2002规定：牡蛎碳酸钙为无污染的牡蛎壳，经高温煅烧、转化制得的碳酸钙(CaCO3)，钙含量应为39.4～40.4％。新标准开始实施以后，产品研制的焦点就集中在如何由活性钙制备医药级牡蛎碳酸钙上，更多的研究集中在如何把活性钙的钙含量和碱度(pH)降下来。本发明人发现，目前主要有以下几种情况：向活性钙中添加柠檬酸、苹果酸；将活性钙或牡蛎壳，经高温煅烧后直接用有机酸(醋酸、柠檬酸、苹果酸、葡萄糖酸等)水溶液中和；向活性钙包装内加入干冰(此法钙含量分布不均、产品潮湿)等。以上方法都不能生产出完全符合国家药品标准的医药级牡蛎碳酸钙。也有人用向活性钙水溶液中通入二氧化碳气体(CO2)的方法进行转化的，存在生产工艺较长，劳动强度大，浪费严重，成本较高等问题。更有甚者，直接向活性钙中掺入钙含量较低的有机酸钙等，不能保证产品主要成分是CaCO3。
发明内容
针对以上问题，本发明人进行了深入研究。本发明的目的就在于提供一种生产工艺简单、易于进行质量控制、完全符合国家药品标准的医药级牡蛎碳酸钙的生产方法。
其特征就在于可以由以下两种方法来实现：
(1)取1摩尔质量的符合原药品标准的活性钙，放入一带有夹层的双层密闭不锈钢容器内(可以是回转真空干燥机或混合机)，由顶部通过压力表和减压阀直接充入食品级或医药级的二氧化碳气体(CO2)，二氧化碳气体(CO2)的用量为1～1.5摩尔质量，夹层内用冷水或热水控制温度为35～90℃，让充分反应3～24小时以后即可得到符合国家药品标准的医药级牡蛎碳酸钙。其化学反应方程式为：
(2)取1摩尔质量的食品级碳酸氢铵，放入一带有夹层的双层密闭反应釜内，加2～5倍水溶解后，加入0.75～1摩尔质量的符合原药品标准的活性钙，控制温度为35～90℃，让充分反应3～24小时以后，搅拌并冷水降温至25℃，过滤沉淀，洗涤干燥即可得到符合国家药品标准的医药级牡蛎碳酸钙。其化学反应方程式为： ，氨气可以回收制作氨水。
本发明的优点就在于：生产工艺简单，易于控制，制得的产品纯度高，成本较低，无污染。
具体实施方式
例1：取74kg符合原药品标准的活性钙，放入一带有夹层的双层密闭回转真空干燥机内，由顶部通过压力表和减压阀直接充入54kg的食品级二氧化碳气体(CO2)，夹层内用冷水或热水控制温度为65℃，让充分反应10小时，得到牡蛎碳酸钙99.5kg，经检测钙含量为40.05％，其他各项指标都符合标准要求。
例2：在带有夹层的双层密闭反应釜内，加150kg水，放入79kg食品级碳酸氢铵，搅拌溶解后，加入60kg符合原药品标准的活性钙，控制温度为90℃，让充分反应5小时以后，搅拌并冷水降温至25℃，过滤沉淀，用水洗涤，干燥后得到牡蛎碳酸钙74.1kg，经检测钙含量为39.7％，其他各项指标都符合标准要求。

Claims (3)

1.一种医药级牡蛎碳酸钙的生产方法，其特征在于由以下方法来实现：
取1摩尔质量的符合原药品标准的活性钙，放入一带有夹层的双层密闭不锈钢容器内，由顶部通过压力表和减压阀直接充入食品级或医药级的二氧化碳气体，夹层内用冷水或热水控制温度为35～90℃，充分反应3～24小时以后得到符合国家药品标准WS-10001-(HD-1034)-2002的医药级牡蛎碳酸钙。
2.一种如权利要求1所述的医药级牡蛎碳酸钙的生产方法，其特征在于二氧化碳气体的用量摩尔数为活性钙摩尔数的1～1.5倍。
3.一种如权利要求1所述的医药级牡蛎碳酸钙的生产方法，其特征在于所述的不锈钢容器为回转真空干燥机或混合机。
CNB2004100308837A 2004-04-09 2004-04-09 医药级牡蛎碳酸钙的生产方法 Expired - Lifetime CN1304296C (zh)

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CN103007721B (zh) * 2012-11-26 2015-01-28 东南大学 基于氨循环的碳酸化固定燃煤烟气中co2的方法和装置
CN104255793B (zh) * 2014-10-16 2017-07-18 李卫平 绿色食品消毒剂活性牡蛎钙及其制备方法

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1150125A (zh) * 1995-11-02 1997-05-21 于惠生 一种碳酸钙的制备方法
CN1094900C (zh) * 1997-03-19 2002-11-27 Fp颜料有限公司 制备沉淀碳酸钙的设备和方法
CN1442363A (zh) * 2002-03-01 2003-09-17 新加坡纳米材料科技有限公司 一种微细晶须状碳酸钙的制备方法
WO2003106344A1 (en) * 2002-06-18 2003-12-24 Specialty Minerals (Michigan) Inc. Process for the production of precipitated calcium carbonates and product produced thereby

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1150125A (zh) * 1995-11-02 1997-05-21 于惠生 一种碳酸钙的制备方法
CN1094900C (zh) * 1997-03-19 2002-11-27 Fp颜料有限公司 制备沉淀碳酸钙的设备和方法
CN1442363A (zh) * 2002-03-01 2003-09-17 新加坡纳米材料科技有限公司 一种微细晶须状碳酸钙的制备方法
WO2003106344A1 (en) * 2002-06-18 2003-12-24 Specialty Minerals (Michigan) Inc. Process for the production of precipitated calcium carbonates and product produced thereby

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