US3034867A - Continuous trinitrotoluene manufacture - Google Patents
Continuous trinitrotoluene manufacture Download PDFInfo
- Publication number
- US3034867A US3034867A US564073A US56407356A US3034867A US 3034867 A US3034867 A US 3034867A US 564073 A US564073 A US 564073A US 56407356 A US56407356 A US 56407356A US 3034867 A US3034867 A US 3034867A
- Authority
- US
- United States
- Prior art keywords
- separator
- nitrator
- outlet
- nitrobody
- acid
- 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 - Lifetime
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Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J14/00—Chemical processes in general for reacting liquids with liquids; Apparatus specially adapted therefor
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07B—GENERAL METHODS OF ORGANIC CHEMISTRY; APPARATUS THEREFOR
- C07B43/00—Formation or introduction of functional groups containing nitrogen
- C07B43/02—Formation or introduction of functional groups containing nitrogen of nitro or nitroso groups
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C201/00—Preparation of esters of nitric or nitrous acid or of compounds containing nitro or nitroso groups bound to a carbon skeleton
- C07C201/06—Preparation of nitro compounds
- C07C201/08—Preparation of nitro compounds by substitution of hydrogen atoms by nitro groups
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00051—Controlling the temperature
- B01J2219/00074—Controlling the temperature by indirect heating or cooling employing heat exchange fluids
- B01J2219/00076—Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements inside the reactor
- B01J2219/00083—Coils
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/18—Details relating to the spatial orientation of the reactor
- B01J2219/182—Details relating to the spatial orientation of the reactor horizontal
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/18—Details relating to the spatial orientation of the reactor
- B01J2219/185—Details relating to the spatial orientation of the reactor vertical
Definitions
- CONTINUOUS TRINITROTQLUENE MANUFACTURE Filed Feb. 7, 1956 2 Sheets-She et 1 E. SAMUELSEN CONTINUOUS TRINITROTOLUENE MANUFACTURE May 15, 1962 2 Sheets-Sheet 2 Filed Feb. '7, 1956 3,934,857 Patented May 15, 1962 3,034,867 CONTINUOUS TRINITROTOLUENE MANUFACTURE Eirik Samuelsen, Gullaug, Norway, assignor to Aktiebolaget Chematur, Swiss, Sweden, a corporation of Sweden, and Norsk Spraengstoiindustri A/ S, Oslo,
- This invention relates to the nitration of toluene and nitrotoluenes, and particularly to the manufacture of trinitrotoluene by continuous operation.
- the object of the present invention is, generally stated, to provide new and improved apparatus for continuous trinitrotoluene manufacture in a series of nitrators and separators in which the hold-up times of the reaction phases may be chosen at will.
- Another object of this invention is the provision of such apparatus by which the volume of the separator can be made smaller than usual, thus reducing the quantities of explosives in operation i.e. obtaining greater safety in operation.
- a further object is the provision of an apparatus by which the feed-back is accomplished by gravity.
- partially separated emulsions are fed back from the separators to the nitrators, i.e. part of the emulsions introduced into the separators are brought back to the nitrators after that part of the disperse-phase or nitrobody has separated. It is desirable to feed back a quantity amounting at least to the half part of the total quantity of the saparated products, i.e. nitrobody and acid, which are leaving the separator. Normally the return current will be larger, say 5-15 or more times, the summary of the saparated products leaving the separator.
- the apparatus according to the invention consists of a system of nitrator-separators, equipped with mixing devices, cooling devices, inlets and outlets for acids, nitrobody etc. as in other continuous toluene nitrating systems, and with means by which partly separated emulsion can be fed back to the nitrator. It is preferable to hold the level of the nitrobody in the separator above the level in the attached nitrator, to permit the partly separated emulsion to flow to the nitrator by gravity. The transport of emulsion from the nitrator to the separator can be performed with the help of a pump or the like.
- nitrator in such a way that a pumping efiect from the mixing device is obtained.
- the suction or the pumping effect from a mixing propeller-or turbine can thus be used.
- the nitrator can also be made in the form of an U-vessel with propeller or turbine in one leg. The liquid in the other leg will thus give a higher level to be used for transport of emulsion to the separator.
- FIGURE 1 shows a nitrator 1 with attached separator 2.
- the nitrator 1 is equipped with mixing propeller 3, driven 'by an electrical motor 4, cooling coils 5, inlets 6 and 7 for toluene or nitrobody respectively nitrating acid.
- the outlet 8 of the nitrator is connected to the inlet 9 of the separator.
- Through inlet 10 supplementary acid can be introduced.
- a lattice, sieve or net work 11 to distribute the incoming emulsion.
- the amount of partly separated emulsion can be regulated by a valve 16.
- Separated nitrobody is continuously overflowing at the liquid level of the separator through outlet 17 and separated acid through an outlet 18 from the bottom of the separator.
- the nitrator as well as the separator can be modified in many ways. Instead of using a nitrator of ordinary shape as illustrated in FIG. 1, it can for instance be given the shape of an U-pipe as will be described in the following example.
- the separator can have a conical inlet to get a good distribution of the emulsion Without net work and the like.
- the outlet 12 for partly separated emulsion can have an adjustable prolongation for instance in the shape of a telescopic tube to make it possible to regulate the outlet in vertical as well as horizontal directions.
- the outlet can also be arranged in one or more of the sides of the separator. It is possible to give the separator vessel the form of a parallelepiped or a lying cylinder with more or less conical ends or of a standing cylinder with tangential inlet for the emulsion.
- FIGURE 2 there is shown a combination of two apparatus units, each consisting of nitrator and separator.
- a complete apparatus for the manufacture of trinitrotoluene out of toluene at least three apparatus units are needed, one unit for each step of nitration. Normally 5-8 or more units are used as the reaction than are easier to control and higher output is obtained. The principle of a complete series of units will however be easily understood already from a combination of two apparatus units.
- the nitrators 1c, 1d are in this case formed as U-tubes with propeller or turbine 30, 3d in one leg 19c, 19d communicating with the other leg 2%, 20d through bottom pipe 21c, 21d. At the upper part of the legs there is an overflow pipe 22c, 22d. With the propeller 3c, 3d in function the liquid will rise in the leg 20c, 20d thus creating sufficient liquid level in the separators 2c, 2d to transport partly separated emulsion back to the nitrators without an extra pumping device.
- Toluene or separated nitrobody from a preceding unit In the separator there is K 3 in the apparatus series is continuously introduced in the nitrator through inlet 60 and is reacted with separated acid coming from separator 2d through pipe 23d and introduced through inlet 70.
- Extra acid Extra acid
- Part of the circulating reaction mixture is removed through outlets 8c and conducted to the separator through inlet 9c.
- the reaction mixture partly separates in the separator; the separated nitrobody being led to the next nitrator 1d through overflow-outlet 17c and inlet 6d of the said apparatus.
- the separated acid is led through outlet 18c through overflow-pipe 230 to the preceding nitrator, or in the case of nitrator 1c being the first one in the unit series, to a spent acid tank or to a denitrator.
- Partly separated emulsion the quantity being regulated by valve 16c, flows back to the nitrator 1c through pipe 120 and 140 respectively, and inlet c.
- nitrator 1d and separator 2d the operation principle is the same.
- trinitrotoluene is withdrawn from the separator 2d through outlet 17d and fresh nitrating acid, or the components of nitrating acid, introduced into the nitrator through inlets 7d and 10d.
- Separated acid is removed from separator 2d through overflow-outlet 18d and conducted through pipe line 23d to the nitrator 10.
- feed-back of partly separated emulsion has special advantages over feed-back of separated components.
- the whole system will be easier to control as the change of the conditions in one unit will not influence the other units. This is easily understood from the fact that the streams of separated products overflowing from the outlets of the separator are of the same size even if the proportions of nitrobody and acid, respectively, the hold up time of the phases are changed in the nitrators.
- Apparatus for nitration of toluene and nitrotoluenes in a series of units each consisting of reactor and separator, the outlet from the reactor connected with the inlet of the separator, feeding means to feed nitrobody and nitrating acid in countercurrent through the system, the separator having an outlet between the top and bottom thereof for partly separated emulsion of nitrobody and acid, and recycling means to return partly separated emulsion of nitrobody and acid from said outlet from the separator to reactor in at least one unit of the series.
- Apparatus according to claim 1 for nitration of toluene and nitrotoluenes to trinitrotoluene in a series of units each consisting of reactor and separator, in each unit the nitrator having a mixing device adapted to feed reaction mixture to the separator and partly separated emulsion from the separator to the reactor.
- Reactor-separator unit consisting of a reactor, with mixing device, the outlet from the reactor connected with the inlet of the separator, the separator having an outlet near the top, an outlet at the bottom ascending to the proximity of the top outlet level, and a third outlet bettween the top and the bottom level, this intermediate outlet connected with the reactor, feeding means to feed mixture from the reactor to the separator and mixture from the intermediate outlet of the separator to the reactor.
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US142999A US3087973A (en) | 1956-02-07 | 1961-09-14 | Continuous trinitrotoluene manufacture |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
SE350638X | 1955-03-23 |
Publications (1)
Publication Number | Publication Date |
---|---|
US3034867A true US3034867A (en) | 1962-05-15 |
Family
ID=20308627
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
US564073A Expired - Lifetime US3034867A (en) | 1955-03-23 | 1956-02-07 | Continuous trinitrotoluene manufacture |
Country Status (6)
Country | Link |
---|---|
US (1) | US3034867A (fr) |
BE (1) | BE546349A (fr) |
CH (1) | CH350638A (fr) |
DE (1) | DE1048875B (fr) |
FR (1) | FR1147136A (fr) |
NL (2) | NL95140C (fr) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3160669A (en) * | 1962-04-13 | 1964-12-08 | Sumitomo Chemical Co | Emulsion process of producing aromatic nitro compounds |
US3844723A (en) * | 1969-04-14 | 1974-10-29 | Shinetsu Chemical Co | Multi-stage counter-current liquid-liquid contact apparatus |
Families Citing this family (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE1179187B (de) * | 1960-10-05 | 1964-10-08 | Metallgesellschaft Ag | Vorrichtung und Verfahren zur Durchfuehrung von Reaktionen |
Citations (11)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US1124496A (en) * | 1913-07-21 | 1915-01-12 | Alphonse Emile Verge | Manufacture of derivatives of toluene. |
US1241017A (en) * | 1914-08-31 | 1917-09-25 | Ferdinando Quartieri | Process for the manufacture of trinitrotoluene. |
US1297170A (en) * | 1917-12-05 | 1919-03-11 | Chance And Hunt Ltd | Nitration process. |
US1638045A (en) * | 1922-11-27 | 1927-08-09 | John W Livingston | Manufacture of nitrobenzene |
US2363834A (en) * | 1942-06-30 | 1944-11-28 | Hercules Powder Co Ltd | Nitration apparatus |
US2370558A (en) * | 1945-02-27 | Nitration of aromatic compounds | ||
US2402180A (en) * | 1942-07-04 | 1946-06-18 | Trojan Powder Co | Trinitrotoluene manufacture |
US2475095A (en) * | 1945-06-12 | 1949-07-05 | Directie Staatsmijnen Nl | Toluene nitration process |
US2594675A (en) * | 1945-11-19 | 1952-04-29 | Bofors Ab | Liquid reactor |
US2729549A (en) * | 1950-09-29 | 1956-01-03 | Shell Dev | Method and apparatus for contacting and separating liquid phases by settling |
US2761768A (en) * | 1952-03-18 | 1956-09-04 | Pouderies Reunis De Belgiques | Circulation nitrating apparatus |
Family Cites Families (10)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
GB124461A (en) * | 1916-01-07 | 1919-04-03 | Chance And Hunt Ltd | An Improved Nitration Process and Apparatus therefor. |
GB126355A (en) * | 1917-01-08 | 1919-05-15 | Clayton Aniline Co Ltd | A Process of and Apparatus for the Continuous Nitration of Organic Liquids. |
US2213211A (en) * | 1938-07-28 | 1940-09-03 | Du Pont | Method of precipitation |
DE740444C (de) * | 1939-04-18 | 1943-10-21 | Emil Fischer | Verfahren zur Durchfuehrung von Faellungen aus verduennten Loesungen, insbesondere zur Aufbereitung von Wasser, in Rohrsystemen |
US2213907A (en) * | 1939-12-02 | 1940-09-03 | Du Pont | Method of precipitation |
DE740772C (de) * | 1940-05-06 | 1944-04-25 | Karl Schmid | Verfahren um zwei, getrennte Phasen bildende Fluessigkeiten von verschiedenem, spezifischem Gewicht kontinuierlich zur gegenseitigen Einwirkung zu bringen |
US2460987A (en) * | 1945-02-23 | 1949-02-08 | Universal Oil Prod Co | Mixing and separating apparatus |
DE858245C (de) * | 1945-06-12 | 1952-12-04 | Der Niederlaendische Staat | Verfahren zur Nitrierung von Toluol zu Trinitrotoluol |
GB665921A (en) * | 1949-02-03 | 1952-02-06 | Bofors Ab | Improved method of and apparatus for carrying out physical and/or chemical operations involving treatment of a liquid with another liquid immiscible therewith |
AT180569B (de) * | 1952-03-18 | 1954-12-27 | Prb Nv | Vorrichtung zur kontinuierlichen Nitrierung, insbesondere von aromatischen Kohlenwassertoffen |
-
0
- NL NL205079D patent/NL205079A/xx unknown
- NL NL95140D patent/NL95140C/xx active
- BE BE546349D patent/BE546349A/xx unknown
-
1956
- 1956-02-07 US US564073A patent/US3034867A/en not_active Expired - Lifetime
- 1956-02-27 FR FR1147136D patent/FR1147136A/fr not_active Expired
- 1956-03-06 DE DEA24434A patent/DE1048875B/de active Pending
- 1956-03-23 CH CH350638D patent/CH350638A/de unknown
Patent Citations (11)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US2370558A (en) * | 1945-02-27 | Nitration of aromatic compounds | ||
US1124496A (en) * | 1913-07-21 | 1915-01-12 | Alphonse Emile Verge | Manufacture of derivatives of toluene. |
US1241017A (en) * | 1914-08-31 | 1917-09-25 | Ferdinando Quartieri | Process for the manufacture of trinitrotoluene. |
US1297170A (en) * | 1917-12-05 | 1919-03-11 | Chance And Hunt Ltd | Nitration process. |
US1638045A (en) * | 1922-11-27 | 1927-08-09 | John W Livingston | Manufacture of nitrobenzene |
US2363834A (en) * | 1942-06-30 | 1944-11-28 | Hercules Powder Co Ltd | Nitration apparatus |
US2402180A (en) * | 1942-07-04 | 1946-06-18 | Trojan Powder Co | Trinitrotoluene manufacture |
US2475095A (en) * | 1945-06-12 | 1949-07-05 | Directie Staatsmijnen Nl | Toluene nitration process |
US2594675A (en) * | 1945-11-19 | 1952-04-29 | Bofors Ab | Liquid reactor |
US2729549A (en) * | 1950-09-29 | 1956-01-03 | Shell Dev | Method and apparatus for contacting and separating liquid phases by settling |
US2761768A (en) * | 1952-03-18 | 1956-09-04 | Pouderies Reunis De Belgiques | Circulation nitrating apparatus |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3160669A (en) * | 1962-04-13 | 1964-12-08 | Sumitomo Chemical Co | Emulsion process of producing aromatic nitro compounds |
US3844723A (en) * | 1969-04-14 | 1974-10-29 | Shinetsu Chemical Co | Multi-stage counter-current liquid-liquid contact apparatus |
Also Published As
Publication number | Publication date |
---|---|
FR1147136A (fr) | 1957-11-19 |
CH350638A (de) | 1960-12-15 |
NL95140C (fr) | |
NL205079A (fr) | |
BE546349A (fr) | |
DE1048875B (de) | 1959-01-22 |
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