CN106748661A - 一种2,3,5-三甲基氢醌生产工艺 - Google Patents

一种2,3,5-三甲基氢醌生产工艺 Download PDF

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Publication number
CN106748661A
CN106748661A CN201510807204.0A CN201510807204A CN106748661A CN 106748661 A CN106748661 A CN 106748661A CN 201510807204 A CN201510807204 A CN 201510807204A CN 106748661 A CN106748661 A CN 106748661A
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certain amount
lauryl alcohol
reaction
reactor
recovery rate
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Inventor
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 CN201510807204.0A priority Critical patent/CN106748661A/zh
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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C37/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring
    • C07C37/06—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring by conversion of non-aromatic six-membered rings or of such rings formed in situ into aromatic six-membered rings, e.g. by dehydrogenation
    • C07C37/07—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring by conversion of non-aromatic six-membered rings or of such rings formed in situ into aromatic six-membered rings, e.g. by dehydrogenation with simultaneous reduction of C=O group in that ring
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C46/00—Preparation of quinones
    • C07C46/02—Preparation of quinones by oxidation giving rise to quinoid structures
    • C07C46/06—Preparation of quinones by oxidation giving rise to quinoid structures of at least one hydroxy group on a six-membered aromatic ring
    • C07C46/08—Preparation of quinones by oxidation giving rise to quinoid structures of at least one hydroxy group on a six-membered aromatic ring with molecular oxygen

Abstract

主要生产工艺路线：1、氧化反应收得率：99.2%。将十二醇从罐区贮罐用转料泵打入计量罐，向搪瓷釜中加入一定量的十二醇，然后向反应釜内投入一定量的二水氯化铜和2,3,6-三甲基苯酚，升温到50~80℃，用空气进行氧化反应，搅拌反应12小时。2、分层、浓缩。反应合格后，降温到50℃以下，将物料转置分层釜分层，水相为催化剂溶液，浓缩后进入氧化套用。油相为十二醇和产品，转入精馏分离。3、精馏。4、还原。还原收得率：99.6%。将一定量的三甲基苯醌、甲醇置于反应釜内，投入钯碳催化剂，上升温到70~100℃，并用氢气保持反应釜内压力为0.5Mpa，反应8小时。5、过滤、浓缩。6、过滤、干燥。

Description

一种2,3,5-三甲基氢醌生产工艺
主要生产工艺路线
1、氧化
反应收得率：99.2%。将十二醇从罐区贮罐用转料泵打入计量罐，向搪瓷釜中加入一定量的十二醇，然后向反应釜内投入一定量的二水氯化铜和2,3,6—三甲基苯酚，升温到50~80℃，用空气进行氧化反应，搅拌反应12 小时。
2、分层、浓缩
反应合格后，降温到50℃以下，将物料转置分层釜分层，水相为催化剂溶液，浓缩后进入氧化套用。油相为十二醇和产品，转入精馏分离。
3、精馏
油相在温度120℃条件下，压力-0.099MPa 条件下浓缩，得通过精馏塔纯化，得到2,3,5—三甲基苯醌和十二醇。粗产品精馏残渣按固废处理。
4、还原
还原收得率：99.6%。将一定量的三甲基苯醌、甲醇置于反应釜内，投入钯碳催化剂，上升温到70~100℃，并用氢气保持反应釜内压力为0.5Mpa，反应8 小时。
5、过滤、浓缩
反应合格后，降温到50℃以下，过滤，回收催化剂钯炭，重复循环使用。再降温到20℃，搅拌1 小时。
6、过滤、干燥
产品析出后，过滤，滤饼干燥，得到最终产品2,3,5—三甲基氢醌。5~6 步收得率：98.8%总收得率：97.6%。

Claims (2)

1.一种2,3,5-三甲基氢醌生产工艺。
2.本发明生产涉及的原材料及配比。
CN201510807204.0A 2015-11-22 2015-11-22 一种2,3,5-三甲基氢醌生产工艺 Pending CN106748661A (zh)

Priority Applications (1)

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CN201510807204.0A CN106748661A (zh) 2015-11-22 2015-11-22 一种2,3,5-三甲基氢醌生产工艺

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201510807204.0A CN106748661A (zh) 2015-11-22 2015-11-22 一种2,3,5-三甲基氢醌生产工艺

Publications (1)

Publication Number Publication Date
CN106748661A true CN106748661A (zh) 2017-05-31

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Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102219665A (zh) * 2011-04-27 2011-10-19 扬州大学 2,3,5-三甲基苯醌和2,3,5-三甲基氢醌的一种合成方法

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102219665A (zh) * 2011-04-27 2011-10-19 扬州大学 2,3,5-三甲基苯醌和2,3,5-三甲基氢醌的一种合成方法

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
李军生编著: "《维生素E的生产与应用》", 31 August 2005, 中国轻工业出版社 *

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Application publication date: 20170531