CN108424378A - 一种依卡倍特钠生产工艺 - Google Patents

一种依卡倍特钠生产工艺 Download PDF

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CN108424378A
CN108424378A CN201710076398.0A CN201710076398A CN108424378A CN 108424378 A CN108424378 A CN 108424378A CN 201710076398 A CN201710076398 A CN 201710076398A CN 108424378 A CN108424378 A CN 108424378A
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stirring
centrifugation
ecabet
reaction
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胡江海
张晓磊
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Center For Intellectual Property Investment Co Ltd
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Center For Intellectual Property Investment Co Ltd
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Priority to CN201710076398.0A priority Critical patent/CN108424378A/zh
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C303/00Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides
    • C07C303/02Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof
    • C07C303/04Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof by substitution of hydrogen atoms by sulfo or halosulfonyl groups
    • C07C303/06Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof by substitution of hydrogen atoms by sulfo or halosulfonyl groups by reaction with sulfuric acid or sulfur trioxide
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C303/00Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides
    • C07C303/32Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of salts of sulfonic acids
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C303/00Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides
    • C07C303/42Separation; Purification; Stabilisation; Use of additives
    • C07C303/44Separation; Purification

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

依卡倍特钠主要作用于一下人群1.适用于下列症状的胃粘膜损伤(糜烂、出血、红肿、水肿),急性胃炎、慢性胃炎的急性发作期。2.胃溃疡。本发明提供一种依卡倍特钠生产工艺,包括:(1)磺化反应;(2)冰解、离心;(3)碱化;(4)脱色、压滤、析晶、离心;(5)精制。

Description

一种依卡倍特钠生产工艺
技术领域
本发明涉及医药化工生产领域,尤其是依卡倍特钠生产领域。
背景技术
依卡倍特钠主要作用于一下人群1.适用于下列症状的胃粘膜损伤(糜烂、出血、红肿、水肿),急性胃炎、慢性胃炎的急性发作期。2.胃溃疡。
发明内容
本发明提供一种依卡倍特钠生产工艺,包括:(1)磺化反应;(2)冰解、离心;(3)碱化;(4)脱色、压滤、析晶、离心;(5)精制。
生产工艺
脱氢枞酸在浓硫酸作用下磺化生成脱氢枞酸磺酸,然后在氢氧化钠作用下转化为
脱氢枞酸磺酸钠即产品。
(1)磺化反应:向反应罐中抽入浓硫酸,开启搅拌,开启冰盐水阀降温,控制料液内温,向反应罐中均匀地缓慢加入脱氢枞酸(加料时间约1~2hr),加完完毕后密闭罐口,控制温度,反应。
(2)冰解、离心:开启冰盐水阀,在开启搅拌的情况下向反应罐中加入冰水进行冰解。冰解结束后,将冰解液放入衬塑离心机中离心,滤饼以冷饮用水洗涤。离心结束后,收集滤饼;用石灰中和处理废酸滤液,得硫酸钙废渣。
(3)碱化:在20L 碱液配制罐加入水,搅拌下加入固体氢氧化钠,配制成1N 氢氧化钠溶液。向60L 脱色反应罐中加入水,开启搅拌,加入冰解滤饼,搅拌。开启碱液进料阀,滴加碱液,调节pH。
(4)脱色、压滤、析晶、离心:调碱结束后,开启蒸汽阀,升温至溶解。缓慢加入活性炭。回流脱色。将脱色液,经搪瓷压滤器,压滤至60L 结晶反应罐中。开启结晶反应罐循化水阀,降温,开启结晶反应罐冰盐水阀,降温,静置保温析晶。将料液放至离心机中,离心得粗品。
(5)精制:将粗品溶入纯化水中,加热回流溶解,加活性炭搅拌回流脱色,热滤,滤液搅拌冷却,停止搅拌,静置过夜,离心过滤,用适量水洗涤,得湿品。将湿品再次溶入纯化水中,加热溶解;搅拌冷却,保温,离心,用纯化水洗涤,甩干,得湿品。湿品双锥减压干燥,得成品。
附图说明:
图1是依卡倍特钠制备反应方程式;图2是依卡倍特钠制备反应方程式。

Claims (3)

1.本发明提供一种依卡倍特钠生产工艺,包括:(1)磺化反应;(2)冰解、离心;(3)碱化;(4)脱色、压滤、析晶、离心;(5)精制。
2.权利要求1描述的:磺化反应:向反应罐中抽入浓硫酸,开启搅拌,开启冰盐水阀降温,控制料液内温,向反应罐中均匀地缓慢加入脱氢枞酸(加料时间约1~2hr),加完完毕后密闭罐口,控制温度,反应。
3.权利要求1描述的碱化:在20L 碱液配制罐加入水,搅拌下加入固体氢氧化钠,配制成1N 氢氧化钠溶液;向60L 脱色反应罐中加入水,开启搅拌,加入冰解滤饼,搅拌;开启碱液进料阀,滴加碱液,调节pH。
CN201710076398.0A 2017-02-13 2017-02-13 一种依卡倍特钠生产工艺 Pending CN108424378A (zh)

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CN201710076398.0A CN108424378A (zh) 2017-02-13 2017-02-13 一种依卡倍特钠生产工艺

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CN201710076398.0A CN108424378A (zh) 2017-02-13 2017-02-13 一种依卡倍特钠生产工艺

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CN108424378A true CN108424378A (zh) 2018-08-21

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111377836A (zh) * 2018-12-29 2020-07-07 四川科瑞德制药股份有限公司 一种依卡倍特钠晶型及其制备方法

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111377836A (zh) * 2018-12-29 2020-07-07 四川科瑞德制药股份有限公司 一种依卡倍特钠晶型及其制备方法

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Application publication date: 20180821