CN108947872A - 一种1,4-二氨基-2-磺酸蒽醌的合成工艺 - Google Patents

一种1,4-二氨基-2-磺酸蒽醌的合成工艺 Download PDF

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Publication number
CN108947872A
CN108947872A CN201810800351.9A CN201810800351A CN108947872A CN 108947872 A CN108947872 A CN 108947872A CN 201810800351 A CN201810800351 A CN 201810800351A CN 108947872 A CN108947872 A CN 108947872A
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Prior art keywords
diamino
anthraquinone
nitrae
isosorbide
anthraquinone sulfonate
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詹国青
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JIANGSU HUAER CHEMICAL Co Ltd
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JIANGSU HUAER CHEMICAL Co Ltd
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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
    • C07C303/08Preparation 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 halogenosulfonic 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

本发明公开了一种1,4‑二氨基‑2‑磺酸蒽醌的合成工艺,属于有机合成领域,包括如下步骤:在容器中,加入1,4‑二氨基蒽醌氧化体,邻二氯苯,维持30~50℃滴加氯磺酸,滴加完毕升温到140±3℃,保温6±1小时,降温到60~80℃,转移到含有纯碱的水中,搅拌一段时间后,调整PH值为7.5±0.1,水汽蒸馏溶剂,再降温到80±5℃,用硫酸调节PH值到1±0.2,使得1,4‑二氨基‑2‑磺酸蒽醌析出,过滤得到产品1,4‑二氨基‑2‑磺酸蒽醌。本发明所述工艺中采用的氯磺酸用量为原始工艺的三分之一,副产盐酸的量为原始工艺的三分之一,不产生二氧化硫气体。

Description

一种1,4-二氨基-2-磺酸蒽醌的合成工艺
技术领域
本发明涉及一种1,4-二氨基-2-磺酸蒽醌的合成改进工艺,属于有机合成技术领域。
背景技术
1,4-二氨基-2-磺酸蒽醌是一种重要的中间体,可以用于合成染料分散蓝60,分散蓝359等,用途广泛,市场前景大,传统的合成工艺都是1,4-二氨基蒽醌隐色体在溶剂中用氯磺酸磺化得到。从反应方程式可以看出,要得到一份的1,4-二氨基-2-磺酸蒽醌需要消耗3份的氯磺酸,其中一份用于氧化1,4-二氨基蒽醌隐色体,一份用于磺化1,4-二氨基蒽醌,而磺化时会生成一份的水,这份水又会消耗一份的氯磺酸。同时还生成3份的盐酸,一份的二氧化硫。导致氯磺酸用量大,副产物多,三废处理难。
发明内容
本发明的目的是提供一种1,4-二氨基-2-磺酸蒽醌的制备工艺,减少氯磺酸的用量,减少副产物的产生量。使得氯磺酸的用量为原始工艺的三分之一。
实现本发明目的的技术解决方案是:一种1,4-二氨基-2-磺酸蒽醌的制备工艺,包括如下步骤:
在容器中,按一定摩尔份加入下列原料或溶剂:1份1,4-二氨基蒽醌氧化体,10~15份的邻二氯苯,维持30~50℃滴加1.02~1.05份的氯磺酸,滴加完毕升温到140±3℃,保温6±1小时,降温到60~80℃,转移到含有0.5份纯碱的50~60份水中,搅拌一段时间后,调整PH值为7.5左右,水汽蒸馏溶剂,再降温到80±5℃,用硫酸调节PH值到1±0.2,使得1,4-二氨基-2-磺酸蒽醌析出,过滤得到产品1,4-二氨基-2-磺酸蒽醌。
与现有技术相比,本发明的优点是是:氯磺酸用量为原始工艺的三分之一。副产盐酸的量为原始工艺的三分之一,不产生二氧化硫气体。
具体实施方式
实施例1
500毫升四口烧瓶中,加入邻二氯苯200克,搅拌下加入1,4-二氨基蒽醌氧化体11.9克,慢慢滴加6克氯磺酸,维持滴加温度30~50摄氏度,滴加完毕,2小时升温到138℃。保温6小时,降温到75℃,转移到预先装有450毫升水及2.6克纯碱的水中,搅拌0.5小时,调整PH到7.3,蒸馏掉邻二氯苯,再用硫酸回调PH到1.1,降温到82℃,过滤,尽量抽干,少量水洗,得到产品1,4-二氨基-2-磺酸滤饼。色谱含量98.5%,不用烘干直接用于下一道工序反应。
实施例2
500毫升四口烧瓶中,加入邻二氯苯220克,搅拌下加入1,4-二氨基蒽醌氧化体11.9克,慢慢滴加6.1克氯磺酸,维持滴加温度30~50摄氏度,滴加完毕,2小时升温到134℃。保温6.5小时,降温到78℃,转移到预先装有450毫升水及2.8克纯碱的水中,搅拌0.5小时,调整PH到7.5,蒸馏掉邻二氯苯,再用硫酸回调PH到0.95,降温到80℃,过滤,尽量抽干,少量水洗,得到产品1,4-二氨基-2-磺酸滤饼。色谱含量98.1%,不用烘干直接用于下一道工序反应。

Claims (3)

1.一种1,4-二氨基-2-磺酸蒽醌的合成工艺,其特征在于,包括如下步骤:
在容器中,加入1,4-二氨基蒽醌氧化体,邻二氯苯,维持30~50℃滴加氯磺酸,滴加完毕升温到140±3℃,保温6±1小时,降温到60~80℃,转移到含有纯碱的水中,搅拌一段时间后,调整PH值为7.5±0.1,水汽蒸馏溶剂,再降温到80±5℃,用硫酸调节PH值到1±0.2,使得1,4-二氨基-2-磺酸蒽醌析出,过滤得到产品1,4-二氨基-2-磺酸蒽醌。
2.如权利要求1所述的工艺,其特征在于,1,4-二氨基蒽醌氧化体与氯磺酸的摩尔比为1:1.02~1.05。
3.如权利要求1所述的工艺,其特征在于,1,4-二氨基蒽醌氧化体与邻二氯苯的摩尔比为1:10~15。
CN201810800351.9A 2018-07-20 2018-07-20 一种1,4-二氨基-2-磺酸蒽醌的合成工艺 Pending CN108947872A (zh)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114163359A (zh) * 2021-12-14 2022-03-11 江苏亚邦染料股份有限公司 一种超重力反应器制备1,4-二氨基蒽醌-2-磺酸的方法

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5754162A (ja) * 1980-09-18 1982-03-31 Sumitomo Chem Co Ltd Antorakinonkeichukanbutsunoseizohoho
JPS5762250A (en) * 1980-10-02 1982-04-15 Sumitomo Chem Co Ltd Preparation of anthraquinone intermediate
US4699735A (en) * 1985-01-24 1987-10-13 Ciba-Geigy Corporation Process for the preparation of 1,4-diaminoanthraquinone-2-sulfonic acid
CN104529837A (zh) * 2014-12-22 2015-04-22 浙江闰土研究院有限公司 一种1,4-二氨基蒽醌-2-磺酸的清洁生产工艺

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5754162A (ja) * 1980-09-18 1982-03-31 Sumitomo Chem Co Ltd Antorakinonkeichukanbutsunoseizohoho
JPS5762250A (en) * 1980-10-02 1982-04-15 Sumitomo Chem Co Ltd Preparation of anthraquinone intermediate
US4699735A (en) * 1985-01-24 1987-10-13 Ciba-Geigy Corporation Process for the preparation of 1,4-diaminoanthraquinone-2-sulfonic acid
CN104529837A (zh) * 2014-12-22 2015-04-22 浙江闰土研究院有限公司 一种1,4-二氨基蒽醌-2-磺酸的清洁生产工艺

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114163359A (zh) * 2021-12-14 2022-03-11 江苏亚邦染料股份有限公司 一种超重力反应器制备1,4-二氨基蒽醌-2-磺酸的方法
CN114163359B (zh) * 2021-12-14 2023-08-08 江苏亚邦染料股份有限公司 一种超重力反应器制备1,4-二氨基蒽醌-2-磺酸的方法

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