CN106608821A - 一种3-羟基-2-萘甲酸甲酯生产工艺 - Google Patents

一种3-羟基-2-萘甲酸甲酯生产工艺 Download PDF

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Publication number
CN106608821A
CN106608821A CN201510807201.7A CN201510807201A CN106608821A CN 106608821 A CN106608821 A CN 106608821A CN 201510807201 A CN201510807201 A CN 201510807201A CN 106608821 A CN106608821 A CN 106608821A
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hydroxy
etherification
reaction
value
methanol
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胡江海
张晓磊
于飞
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Ningxia Jihua Environmental Safety Technology Co Ltd
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Ningxia Jihua Environmental Safety Technology Co Ltd
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Priority to CN201510807201.7A priority Critical patent/CN106608821A/zh
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C67/00Preparation of carboxylic acid esters
    • C07C67/08Preparation of carboxylic acid esters by reacting carboxylic acids or symmetrical anhydrides with the hydroxy or O-metal group of organic compounds
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C67/00Preparation of carboxylic acid esters
    • C07C67/48Separation; Purification; Stabilisation; Use of additives
    • C07C67/60Separation; Purification; Stabilisation; Use of additives by treatment giving rise to chemical modification

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

Abstract

3-羟基-2-萘甲酸甲酯是化工中的重要原材料。3-羟基-2-萘甲酸甲酯生产工艺流程为:工艺说明①醚化反应将甲醇利用气动泵打入醚化反应釜,将98%硫酸经计量桶缓慢流入反应釜,温度控制于45℃以下(视情况开夹套进行冷却),随后将3-甲氧基-2-萘甲酸入料,入料时间控制于0.5~1小时,升温至76~83℃进行反应,温度达76℃时开始反应6小时。以3-甲氧基-2-萘甲酸计,反应转化率为94.5%,甲醇过量,剩余甲醇不进行不反应。稀释中和醚化反应结束后,降温至45~50℃时,以32%的NaOH溶液进行中和,中和温度控制于45~50℃,PH=8.8~9.5之间,中和完毕后继续搅拌30分钟后再次确认PH值,PH值确认后补充纯水,继续搅拌60分钟再次确认PH值。③脱水。

Description

一种3-羟基-2-萘甲酸甲酯生产工艺
生产 3-羟基-2-萘甲酸与甲醇、 硫酸发生醚化反应后, 经稀释中和、 脱水、 洗涤等工序 后, 得到 3-羟基-2-萘甲酸甲酯( Bon-M) 产品。
工艺说明 ①醚化反应 将甲醇利用气动泵打入醚化反应釜, 将 98%硫酸经计量桶缓慢流入反应釜, 温度 控制于 45℃ 以下( 视情况开夹套进行冷却), 随后将 3-甲氧基-2-萘甲酸入料, 入料 时间控制于 0.5~1 小时, 升温至 76~83℃ 进行反应, 温度达 76℃ 时开始反应 6 小时。以 3-甲氧基-2-萘甲酸计, 反应转化率为 94.5%, 甲醇过量, 剩余甲醇不进行不反 应
②稀释中和 醚化反应结束后, 降温至 45~50℃ 时, 以 32%的 NaOH 溶液进行中和, 中和温度 控制于 45~50℃ , PH=8.8~9.5 之间, 中和完毕后继续搅拌 30 分钟后再次确认 PH 值, PH 值确认后补充纯水, 继续搅拌 60 分钟再次确认 PH 值。
③脱水、 洗净 PH 确认无误后, 利用气动泵将反应液转至中继槽中进行脱水, 脱水温度控制于 40~50℃ , 脱水后用清水进行洗涤。 3-羟基-2-萘甲酸甲酯产品转化率以 3-甲氧基-2-萘甲酸计, 转化率为 94.5%, 甲醇 过量, 剩余不反应。

Claims (2)

1.一种3-羟基-2-萘甲酸甲酯生产工艺。
2.本发明生产涉及的原材料及配比
CN201510807201.7A 2015-11-22 2015-11-22 一种3-羟基-2-萘甲酸甲酯生产工艺 Pending CN106608821A (zh)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111686798A (zh) * 2020-03-10 2020-09-22 秦婷 一种用于制备螺四氢噻吩的binol轴手性硫脲有机催化剂

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2010029541A1 (en) * 2008-09-09 2010-03-18 Salio Nanotechnologies Ltd. MOLECULARLY IMPRINTED SMART POLYMERS (MISPs)
WO2010048302A1 (en) * 2008-10-21 2010-04-29 Oregon Health & Science University Naphthamides as anticancer agents
CN103980139A (zh) * 2014-05-27 2014-08-13 天津市斯芬克司药物研发有限公司 一种萘酸类化合物及其制备方法

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2010029541A1 (en) * 2008-09-09 2010-03-18 Salio Nanotechnologies Ltd. MOLECULARLY IMPRINTED SMART POLYMERS (MISPs)
WO2010048302A1 (en) * 2008-10-21 2010-04-29 Oregon Health & Science University Naphthamides as anticancer agents
CN103980139A (zh) * 2014-05-27 2014-08-13 天津市斯芬克司药物研发有限公司 一种萘酸类化合物及其制备方法

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111686798A (zh) * 2020-03-10 2020-09-22 秦婷 一种用于制备螺四氢噻吩的binol轴手性硫脲有机催化剂

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