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KR950701903A - Process for the production of dinitrotoluene - Google Patents

Process for the production of dinitrotoluene

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Publication number
KR950701903A
KR950701903A KR1019940704594A KR19940704594A KR950701903A KR 950701903 A KR950701903 A KR 950701903A KR 1019940704594 A KR1019940704594 A KR 1019940704594A KR 19940704594 A KR19940704594 A KR 19940704594A KR 950701903 A KR950701903 A KR 950701903A
Authority
KR
South Korea
Prior art keywords
toluene
acid
nitric
absence
reaction
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
KR1019940704594A
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Korean (ko)
Inventor
더블유. 메이슨 로버트
Original Assignee
폴 와인슈타인
올린 코포레이션
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Publication of KR950701903A publication Critical patent/KR950701903A/en
Ceased legal-status Critical Current

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Classifications

    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C201/00Preparation of esters of nitric or nitrous acid or of compounds containing nitro or nitroso groups bound to a carbon skeleton
    • C07C201/06Preparation of nitro compounds
    • C07C201/08Preparation of nitro compounds by substitution of hydrogen atoms by nitro groups
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C205/00Compounds containing nitro groups bound to a carbon skeleton
    • C07C205/06Compounds containing nitro groups bound to a carbon skeleton having nitro groups bound to carbon atoms of six-membered aromatic rings

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

Abstract

본 발명은 15분 미만의 반응시간 동안 반음온도가 20 내지 30℃인 반응기에서, 질산과 물의 합량 대 톨루엔의 몰비를 10 : 1 내지 15 : 1로 사용하고, 황산의 부재하에서, 반응도중 및 반응으로 중지시키기 위해 쌍극성 비양자성 용매의 부재하에서 무수질산과 톨루엔을 반응시켜 니트로크레졸이 존재하지 않는 생성 혼합물 중의 디니트로 톨루엔을 제공하고, 이를 쌍극성 비양자성 용매의 부재하에 진공 증류시켜 생성혼합물로 부터 미반응 질산을 제거하여 디니트로톨루엔을 제공하는 무수 질산과 톨루엔과의 액상 니트로화 반응을 특징으로 하는 디니트로톨루엔을 제조하기 위한 톨루엔의 니트로화 방법에 관한 것이다.The present invention uses a molar ratio of nitric acid and water to toluene in a reactor with a halftone temperature of 20 to 30 ° C. for a reaction time of less than 15 minutes in a ratio of 10: 1 to 15: 1, in the absence of sulfuric acid, and during the reaction. Reacting nitric anhydride with toluene in the absence of a bipolar aprotic solvent to provide dinitrotoluene in the product mixture free of nitrocresol, which is vacuum distilled in the absence of a bipolar aprotic solvent to the product mixture. The present invention relates to a nitration method of toluene for producing dinitrotoluene characterized by a liquid nitration reaction of nitric anhydride and toluene to remove unreacted nitric acid to provide dinitrotoluene.

Description

디니트로톨루엔의 제조방법 (Process for the production of dinitrotoluene)Process for the production of dinitrotoluene

본 내용은 요부공개 건이므로 전문내용을 수록하지 않았음Since this is an open matter, no full text was included.

Claims (11)

15분 미만의 반응시간 동안 반응온도가 20 내지 30℃인 반응기에서, 질산과 물의 합량 대 톨루엔의 몰비를 10 : 1 내지 15 : 1로 사용하고, 황산의 부재하에서, 반응 도중 및 반응을 중지 시키기 위해 쌍극성 비양자성 용매의 부재하에서 무수질산과 톨루엔을 반응시켜 니트로크레졸이 존재하지 않는 생성혼합물 중의 디니트로톨루엔을 제공하고, 이를 쌍극성 비양자성 용매의 부재하에 진공 증류시켱 생성혼합물로 부터 미반응 질산을 제거하여 디니트로톨루엔을 제공하는 무수 질산과 톨루엔과의 액상 디니트로화 반응을 특징으로 하는 니트로톨루엔을 제조하기 위한 톨루엔의 니트로화 방법.In a reactor with a reaction temperature of 20 to 30 ° C. for a reaction time of less than 15 minutes, using a molar ratio of nitric acid and water to toluene in a ratio of 10: 1 to 15: 1, in the absence of sulfuric acid, stopping and during the reaction To react dinitrotoluene in the product mixture which is free of nitrocresol in the absence of a bipolar aprotic solvent, which is distilled off by vacuum distillation in the absence of a bipolar aprotic solvent. A nitration method of toluene for producing nitrotoluene characterized by a liquid dinitrolation reaction of nitric anhydride with toluene to remove reactive nitric acid to give dinitrotoluene. 제l항에 있어서, 몰비가 11 : 1 내지 12 : 1임을 특징으로 하는 방법.The method of claim 1 wherein the molar ratio is from 11: 1 to 12: 1. 제1항에 있어서, 무수 질산의 산 함량이 산과 물의 합량을 기준으로 하여 95 내지 100중량%임을 특징으로 하는 방법.The method of claim 1, wherein the acid content of nitric anhydride is 95 to 100% by weight based on the total amount of acid and water. 제1항에 있어서, 진공 증류가 약50 내지 약300mmHg의 압력에서 수행됨을 특징으로 하는 방법.The method of claim 1 wherein vacuum distillation is performed at a pressure of about 50 to about 300 mm Hg. 제1항에 있어서, 진공 증류 후에 생성흔함물로부터 디니트로톨루엔을 상분리하는 단계를 추가로 포함함을 특징으로 하는 방법.The method of claim 1, further comprising the step of phase separating dinitrotoluene from the product residue after vacuum distillation. 제5항에 있어서, 상분리가 생성물의 혼합물에 물 또는 묽은 질산의 부가에 의해 일어남을 특징으로 하는 방법.6. A process according to claim 5, wherein the phase separation occurs by addition of water or dilute nitric acid to the mixture of products. 제1항에 있어서, 니트로화 반응이 5분 미만 동안 수행됨을 특징으로 하는 방법.The method of claim 1 wherein the nitration reaction is carried out for less than 5 minutes. 제1항에 있어서, 무수 질산의 산 농도가 95 내지 100중량%임을 특징으로 하는 방법.The method of claim 1, wherein the acid concentration of nitric anhydride is 95 to 100% by weight. 제1항에 있어서, 무수 질산의 산농도가 98중랑%이상임을 특징으로 하는 방법.The method according to claim 1, wherein the acid concentration of nitric anhydride is 98 mu% or more. 반응온도가 20 내지 30℃인 반응기에서 황산의 부재하에서 반응 도중 및 반응을 중지시키기 위해 쌍극성 비양자성 용매의 부재하에서 질산과 물의 합량 대 톨루엔의 몰비를 11 : 1ㅇ 내지 12 : 1로 하고 질산과 물의 합량을 기준으로 하여 산 함량이 95 내지 100중량%인 무수 질산을 톨루엔과 약 5분미만 동안 액상 니트로화 반응시킴을 특징어로 하는, 니트로크레졸이 제거된 생성혼합물 중의 디니트로톨루엔을 제공하기 위한 톨루엔의 니트로화 방법.In a reactor having a reaction temperature of 20 to 30 ° C. in the absence of sulfuric acid and in the absence of a bipolar aprotic solvent in order to stop the reaction, the molar ratio of nitric acid to water to toluene is 11: 1 to 12: 1 and nitric acid is used. Providing dinitrotoluene in the nitrocresol-free product mixture characterized by subjecting nitric anhydride having an acid content of 95 to 100% by weight based on the total amount of water and liquid to nitrate with toluene for less than about 5 minutes. Method of nitration of toluene. 생성물에 모노니트로크레졸 및 디니트로크레졸 화합물이 존재하지 않음을 특징으로 하는 제1항의 방법에 의해 생성된 생성혼합물.A product mixture produced by the method of claim 1 wherein the product is free of mononitrocresol and dinitrocresol compounds. ※ 참고사항 : 최초출원 내용에 의하여 공개하는 것임.※ Note: The disclosure is based on the initial application.
KR1019940704594A 1992-06-17 1993-06-01 Process for the production of dinitrotoluene Ceased KR950701903A (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
US90021392A 1992-06-17 1992-06-17
US07/900,213 1992-06-17
PCT/US1993/005081 WO1993025503A1 (en) 1992-06-17 1993-06-01 Process for the production of dinitrotoluene

Publications (1)

Publication Number Publication Date
KR950701903A true KR950701903A (en) 1995-05-17

Family

ID=25412168

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Application Number Title Priority Date Filing Date
KR1019940704594A Ceased KR950701903A (en) 1992-06-17 1993-06-01 Process for the production of dinitrotoluene

Country Status (7)

Country Link
EP (1) EP0649400A1 (en)
KR (1) KR950701903A (en)
AU (1) AU665843B2 (en)
BR (1) BR9306554A (en)
CA (1) CA2138391A1 (en)
RU (1) RU2106338C1 (en)
WO (1) WO1993025503A1 (en)

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE10307140A1 (en) * 2003-02-20 2004-09-09 Bayer Ag Two-stage nitration of toluene to produce dinitrotoluene has an adiabatic and then an isothermal stage so as to give heat savings and improve safety
RU2295953C2 (en) * 2004-07-12 2007-03-27 Тиберий Георгиевич Незбайло Hydrophilic and hydrophobic compositions for treatment infectious or viral diseases and method for their using
DE102005050106B4 (en) * 2005-10-18 2008-04-30 Josef Meissner Gmbh & Co. Kg Recovery of nitrating acid mixtures from nitrite processes

Family Cites Families (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3928395A (en) * 1972-10-05 1975-12-23 Ciba Geigy Ag Process for the nitration of aromatic compounds
US4495372A (en) * 1982-11-05 1985-01-22 Uniroyal, Inc. Preparation of mono-nitro aromatic compounds
US4935557A (en) * 1984-08-07 1990-06-19 Air Products And Chemicals, Inc. Conitration of mixed aromatic hydrocarbons
US5001272A (en) * 1988-06-22 1991-03-19 Olin Corporation Process for the production of dinitrotoluene
AU3863089A (en) * 1988-06-22 1990-01-12 Olin Corporation Process for the production of dinitrotoluene or mononitrobenzene
US4918250A (en) * 1989-04-21 1990-04-17 Olin Corporation Process for the production of dinitrotoluene using an inorganic salt as a phase separation agent
US5099079A (en) * 1990-07-26 1992-03-24 Olin Corporation Process for separating acid from nitro substituted aromatics using a molten nitrate salt
US5099080A (en) * 1991-03-08 1992-03-24 Olin Corporation Process for preparing dinitrotoluene
US5245092A (en) * 1991-03-15 1993-09-14 Olin Corporation Process for preparing dinitrotoluene with low by-product content

Also Published As

Publication number Publication date
BR9306554A (en) 1998-09-15
EP0649400A4 (en) 1995-02-14
EP0649400A1 (en) 1995-04-26
AU4396393A (en) 1994-01-04
CA2138391A1 (en) 1993-12-23
WO1993025503A1 (en) 1993-12-23
RU94046238A (en) 1996-10-10
AU665843B2 (en) 1996-01-18
RU2106338C1 (en) 1998-03-10

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