GB834260A - Apparatus for the continuous nitration of toluene by the counter-current method - Google Patents

Apparatus for the continuous nitration of toluene by the counter-current method

Info

Publication number
GB834260A
GB834260A GB2657956A GB2657956A GB834260A GB 834260 A GB834260 A GB 834260A GB 2657956 A GB2657956 A GB 2657956A GB 2657956 A GB2657956 A GB 2657956A GB 834260 A GB834260 A GB 834260A
Authority
GB
United Kingdom
Prior art keywords
reaction
toluene
tube
acid
reaction tube
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.)
Expired
Application number
GB2657956A
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Dynamit Nobel AG
Original Assignee
Dynamit Nobel AG
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Dynamit Nobel AG filed Critical Dynamit Nobel AG
Publication of GB834260A publication Critical patent/GB834260A/en
Expired legal-status Critical Current

Links

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
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0006Controlling or regulating processes
    • B01J19/0013Controlling the temperature of the process
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/18Stationary reactors having moving elements inside
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07BGENERAL METHODS OF ORGANIC CHEMISTRY; APPARATUS THEREFOR
    • C07B43/00Formation or introduction of functional groups containing nitrogen
    • C07B43/02Formation or introduction of functional groups containing nitrogen of nitro or nitroso groups
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049Controlling or regulating processes
    • B01J2219/00051Controlling the temperature
    • B01J2219/00074Controlling the temperature by indirect heating or cooling employing heat exchange fluids
    • B01J2219/00087Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements outside the reactor
    • B01J2219/00094Jackets
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049Controlling or regulating processes
    • B01J2219/00182Controlling or regulating processes controlling the level of reactants in the reactor vessel
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/18Details relating to the spatial orientation of the reactor
    • B01J2219/185Details relating to the spatial orientation of the reactor vertical

Landscapes

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

Abstract

<PICT:0834260/III/1> Apparatus for the continuous treatment of a liquid by another liquid by the countercurrent method with simultaneous separation of the product from the residuary material, characterized by a vertically - disposed reaction tube (1) for holding the reaction liquid, said tube being free of internal baffles, an outlet (3) at or adjacent to the upper end of the product and an outlet (2) disposed at the lower end for discharging by siphoning the residuary treatment liquid, an inlet (6) for supplying the treatment liquid at a distance from the upper end of the reaction tube determined by the desired intensity of the emulsification and by the desired rate of throughput of the treating liquid, and a further inlet tube (7) for supplying a reactant at the same distance from the lower end, the region of the reaction tube situated between said two inlets being provided with a stirring device (9) which effects only radial whirling of the reaction liquid. The reation tube may be enclosed in a tubular jacket, not illustrated, for the purpose of adjusting the reaction temperature by the admission of a cooling or heating medium. This jacket is advantageously subdivided by partitions into sections, on account of the unequal temperature conditions obtaining at different levels of the reaction tube.ALSO:<PICT:0834260/IV (b)/1> Apparatus for the continuous nitration of toluene by the countercurrent method with simultaneous separation of the nitrated toluene from the residuary acid, characterized by a vertically disposed reaction tube (1) for holding the reaction liquid, said tube being free of internal baffles, an outlet (3) at or adjacent to the upper end for the nitrated toluene and an outlet (2) disposed at the lower end for discharging by siphoning the residuary acid, an inlet 6 for supplying the nitrating acid at a distance from the upper end of the reaction tube determined by the desired intensity of the emulsification and by the desired rate of throughput of the acid, and a further inlet tube 7 for supplying toluene at the same distance from the lower end, the region of the reaction tube situated between said two inlets being provided with a stirring device 9 which effects only radial whirling of the reaction liquid. The reaction tube may be enclosed in a tubular jacket, not illustrated, for the purpose of adjusting the reaction temperature by the admission of a cooling or heating medium. This jacket is advantageously subdivided by partitions into sections, on account of the unequal temperature conditions obtaining at different levels of the reaction tube. The length of the siphon tube 2 is so selected that during nitration the upper zone of the reaction tube 1 is filled, for example, with mononitrotoluene, the lower zone with residuary acid, and the middle reaction zone with toluene and fresh nitrating acid in addition to said two liquid components. The two level tubes 5 and 8 are filled with toluene and nitrating acid to a determined level, depending on the specific gravities. This equilibrium of the system is maintained when the stirring mechanism is in rotation, since whirling in the radial direction only is effected by said stirring mechanism. The equilibrium is disturbed as soon as toluene and nitrating acid are introduced into the level tubes 8 and 5, respectively, from above. This current of liquid continues in the reaction tube; the heavier nitrating acid in the reaction zone sinks downward, while the lighter toluene rises to the top. The two nonmiscible liquids thereby react with one another and, providing suitable temperatures and times of stay are observed, a complete conversion takes place of the toluene to mononitrotoluene, or of an already nitrated toluene to a higher stage of nitration. The nitrated product is separated in the decomposition zone from the acid residues and leaves the reaction tube through the outlet 3. The nitrating acid, which travels through the reaction zone in the opposite direction, is separated in the lower decomposition zone, in the form of residuary acid, from the toluene or mononitrotoluene and passes out through the siphon 2 from the reaction tube. The reaction liquids are thus supplied and discharged automatically and continuously without requiring throttle or shut-off members. Using the apparatus of the invention and with an inlet 6 spaced from the upper end of the reaction tube 1 at a distance equal to onequarter of the length of the tube 1 and an inlet 7 spaced from the lower end of the tube by the same distance nitrating acid, containing 34.5% by weight of nitric acid and 62.8% by weight of sulphuric acid and having a specific gravity of 1.77, was used to treat 200 c.cs. of toluene and 75 c.c. of water per hour at a temperature of about 40 DEG C. at the toluene inlet and about 75 DEG C. at the acid inlet, with a reaction temperature of about 75 DEG C. and maintained by hot water.
GB2657956A 1955-09-17 1956-08-30 Apparatus for the continuous nitration of toluene by the counter-current method Expired GB834260A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DED21316A DE1062234B (en) 1955-09-17 1955-09-17 Device for the continuous nitration of toluene according to the countercurrent principle

Publications (1)

Publication Number Publication Date
GB834260A true GB834260A (en) 1960-05-04

Family

ID=7037039

Family Applications (1)

Application Number Title Priority Date Filing Date
GB2657956A Expired GB834260A (en) 1955-09-17 1956-08-30 Apparatus for the continuous nitration of toluene by the counter-current method

Country Status (2)

Country Link
DE (1) DE1062234B (en)
GB (1) GB834260A (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4022844A (en) * 1972-02-25 1977-05-10 Societe Nationale Des Poudres Et Explosifs Process for continuous production of trinitrotoluene
CN102276470A (en) * 2010-06-08 2011-12-14 中国石油化工集团公司 Method for nitrifying aromatic hydrocarbon compound by continuous countercurrent

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE655339C (en) * 1934-11-28 1938-01-13 Meissner Fa Josef Process and device for the continuous nitration of aromatic hydrocarbons which are liquid at normal temperature
US2363834A (en) * 1942-06-30 1944-11-28 Hercules Powder Co Ltd Nitration apparatus
DE858245C (en) * 1945-06-12 1952-12-04 Der Niederlaendische Staat Process for the nitration of toluene to trinitrotoluene
AT180569B (en) * 1952-03-18 1954-12-27 Prb Nv Device for continuous nitration, especially of aromatic hydrocarbons

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4022844A (en) * 1972-02-25 1977-05-10 Societe Nationale Des Poudres Et Explosifs Process for continuous production of trinitrotoluene
CN102276470A (en) * 2010-06-08 2011-12-14 中国石油化工集团公司 Method for nitrifying aromatic hydrocarbon compound by continuous countercurrent

Also Published As

Publication number Publication date
DE1062234B (en) 1959-07-30

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