CN101234958B - 一种碱竹木质素制备香兰素的方法 - Google Patents
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Abstract
本发明公开了一种碱竹木质素制备香兰素的方法，制备步骤包括：(1)干状碱竹木质素放入含有质量百分比为4％的硫磺的质量百分比浓度为25％的氢氧化钠水溶液中，在90℃下反应60min，然后在50℃、0.08MPa真空度下，将水蒸发掉，得到反应粗样；(2)将反应粗样放入热裂解炉中，冲入为氮气，然后迅速升温到380℃，在添加量为1克/公斤的铜催化剂作用下进行定向热裂解，热裂解汽冷却后，得热解产物；(3)在180℃温度、0MPa真空度下，将热解产物中低沸点物质除去，然后在220℃温度、0MPa真空度下，蒸出香兰素。该香兰素纯度达到70以上。
Description
技术领域
本发明涉及的是一种利用碱竹木质素制备香兰素的方法。
背景技术
香兰素是重要的食用香料，具有香荚兰豆香气及浓郁的奶香。广泛用于糖果、冰淇淋、饮料及烟草、酒类等行业作定香剂并起助香作用，还可作香皂、牙膏、香水等各类化妆用品中的加香调香剂和其它产品的祛臭加香剂，在医药上可生产多巴、甲基多巴、增效剂TMP等，还用作电镀光亮剂。
在全球范围，由于香兰素的供应存在缺口，因此其价格一路涨势不停。目前，全球对合成香兰素的需求量每年大约在16000吨左右，对天然香兰素的需求量只有大约40吨。而造成需求差别悬殊的原因在于：合成香兰素的价格仅为天然香兰素价格的百分之一。合成香兰素是天然香兰素的一种便宜的替代品，不仅可以替代天然香兰素，而且可以作为搀杂性香兰素提取物的补充。
在欧洲和美国这些成熟市场，香兰素的年增长率稳定在2％左右；在中国，其市场增长速度超过10％。
有业内人士分析，这次涨价也是对当前能源价格居高不下直接作出的一个反应，因为油、气的价格近年来一直持续增长，而用于生产香兰素的原材料都是耗能大户；不过，只要市场还维持着供应短缺的现状，各方都必须要承担价格高企的压力，未来要改变这种现状就要等待有朝一日冲破相关技术的瓶颈了。
发明内容
本发明所要解决的技术问题是提供一种操作工艺简单，可控性好，成本低，不需要昂贵的设备，易于产业化的碱竹木质素制备香兰素的方法。
为了解决上述技术问题，本发明提供的碱竹木质素制备香兰素的方法，制备步骤包括：
(1)、干状碱竹木质素放入含有质量百分比为4％的硫磺的质量百分比浓度为25％的氢氧化钠水溶液中，在90℃下反应60min，然后在50℃、0.08MPa真空度下，将水蒸发掉，得到反应粗样；
(2)、将反应粗样放入热裂解炉中，冲入为氮气，然后迅速升温到380℃，在添加量为1克/公斤的铜催化剂作用下进行定向热裂解， 热裂解汽冷却后，得热解产物；
(3)、在180℃温度、0MPa真空度下，将热解产物中低沸点物质除去，然后在220℃温度、0MPa真空度下，蒸出香兰素。
采用上述技术方案的碱竹木质素制备香兰素的方法，生产的香兰素纯度达到70以上。本发明提供的方法操作工艺简单，可控性好，成本低，也不需要昂贵的设备，易于产业化，而且消化了大量环境污染物碱竹木质素，具有良好环境效益、社会效益和经济效益，具有良好的工业化应用前景。
综上所述，本发明是一种操作工艺简单，可控性好，成本低，不需要昂贵的设备，易于产业化的碱竹木质素制备香兰素的方法。
具体实施方式
通过下面给出的本发明的具体实施例可以进一步清楚地理解本发明，但下述实施例并不是对本发明的限定。
实施例1：
碱竹木质素制备香兰素的方法，制备步骤包括：
(1)、干状碱竹木质素放入含有质量百分比为4％的硫磺的质量百分比浓度为25％的氢氧化钠水溶液中，在90℃下反应60min，然后在50℃、0.08MPa真空度下，将水蒸发掉，得到反应粗样；
(2)、将反应粗样放入热裂解炉中，冲入为氮气，然后迅速升温到380℃，在添加量为1克/公斤的铜催化剂作用下进行定向热裂解，热裂解汽冷却后，得热解产物；
(3)、在180℃温度、0MPa真空度下，将热解产物中低沸点物质除去，然后在220℃温度、0MPa真空度下，蒸出香兰素。
Claims (1)
1.一种碱竹木质素制备香兰素的方法，其特征是：制备步骤包括：
(1)、干状碱竹木质素放入含有质量百分比为4％的硫磺的质量百分比浓度为25％的氢氧化钠水溶液中，在90℃下反应60min，然后在50℃、0.08MPa真空度下，将水蒸发掉，得到反应粗样；
(2)、将反应粗样放入热裂解炉中，冲入为氮气，然后迅速升温到380℃，在添加量为1克/公斤的铜催化剂作用下进行定向热裂解，热裂解汽冷却后，得热解产物；
(3)、在180℃温度、0MPa真空度下，将热解产物中低沸点物质除去，然后在220℃温度、0MPa真空度下，蒸出香兰素。
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| CN108084005B (zh) | 2013-01-24 | 2023-04-18 | 罗地亚经营管理公司 | 用于纯化天然香草醛的方法 |
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