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US2445741A - Apparatus for the manufacture of explosives - Google Patents

Apparatus for the manufacture of explosives Download PDF

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Publication number
US2445741A
US2445741A US481369A US48136943A US2445741A US 2445741 A US2445741 A US 2445741A US 481369 A US481369 A US 481369A US 48136943 A US48136943 A US 48136943A US 2445741 A US2445741 A US 2445741A
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US
United States
Prior art keywords
mixture
vessel
reaction
acid
nitration
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
Application number
US481369A
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English (en)
Inventor
Arvel O Franz
Orin C Keplinger
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.)
Olin Industries Inc
Original Assignee
Olin Industries Inc
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
Priority to BE479710D priority Critical patent/BE479710A/xx
Priority to FR959787D priority patent/FR959787A/fr
Priority to NL65417D priority patent/NL65417C/xx
Application filed by Olin Industries Inc filed Critical Olin Industries Inc
Priority to US481369A priority patent/US2445741A/en
Priority to GB32441/47A priority patent/GB637561A/en
Application granted granted Critical
Publication of US2445741A publication Critical patent/US2445741A/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B17/00—Apparatus for esterification or etherification of cellulose
    • C08B17/04—Apparatus for esterification or etherification of cellulose for making cellulose nitrate
    • 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
    • C—CHEMISTRY; METALLURGY
    • C06—EXPLOSIVES; MATCHES
    • C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
    • C06B21/00—Apparatus or methods for working-up explosives, e.g. forming, cutting, drying
    • 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
    • C07C201/02—Preparation of esters of nitric acid
    • 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
    • B01J2219/00054—Controlling or regulating the heat exchange system
    • B01J2219/00056—Controlling or regulating the heat exchange system involving measured parameters
    • B01J2219/00058—Temperature measurement
    • B01J2219/00063—Temperature measurement of the reactants
    • 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
    • B01J2219/00087—Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements outside the reactor
    • B01J2219/00094—Jackets

Definitions

  • This invention relates to the manufacture of explosives and more particularly to a continuous nitration apparatus for use in the manufacture of explosives,
  • the nitration process set forth herein is described and claimed in our co-pending application, Serial No. 481,368, filed March 31, 1943, issued as U. S. Patent 2,415,423.
  • Another object of the invention is to provide an improved continuous nitration apparatus for manufacturing polynitrated explosives.
  • a further object of this invention is to provide an improved apparatus for continuous nitration in which oxidation and overnitration are prevented.
  • a still further object of the invention is to provide a continuous apparatus for effecting aneflicient nitration in the manufacture of polynitrated explosives in which the temperature is readily controlled at the desired level.
  • Figure 1 shows a plan view of a nitrating apparatus illustrating one embodiment of this invention
  • Figure 2 is a vertical section, taken at XX", of
  • Figure 4 is a sectional view taken along line 44 of Figure 2.
  • the nitration reaction In the manufacture of such polynitrated explosives as tetryl, the nitration reaction is not instantaneous but requires a period of time for completion. In the manufacture of such polynitrated explosives as nitroglycerine, no extended period of time is required for the nitration reaction, but a great quantity of heat is developed during the reaction which must be dissipated in order to prevent the mixture from overheating.
  • the apparatus of the present invention is suitable for carrying out both types of reactions.
  • the tubular vessel is in the form of an upright U-tube I.
  • the U-tube is provided with external cooling or heating jackets 2, 3, 4, 5, 6, 1, and 8 having inlets and outlets 25.
  • Charging inlets 9 and ID are provided for introducing the nitrating acid and material to be nitrated into the entrance leg ll of U-tube I.
  • An outlet 12 is provided on the exit leg 13 of U- tube for discharging the spent acid and product.
  • the inlets 9 and ID for introducing the reagents into the nitrator are preferably maintained at some distance above the surface of the reaction mixture in the nitrator.
  • a plurality of agitators for instance l4, l5, I6,
  • the agitators may be so adjusted that no appreciable head of I liquid occurs in either arm II or l3 and are so shaped and arranged th'at they form the mixture into at least two zones of opposing circulation so that practically no part of the mixture in arm I3 returns to arm H.
  • An outlet I8 is provided at the bottom'of vessel I so that the nitrator can be completely drained in case of emergency, or for cleanin purposes and the like.
  • the reagents are fed in proper proportion through inlets -9 and ill in the arm H to form an initial reaction zone with thorough mixing by the agitator I4, and during the initial reaction, the mixture is cooled to the desired temperature by heat exchange with the cooling medium circulated. through the jacket 2.
  • Thermometer wells such as are illustratedat 26 may be employed to determine the temperature of the mixture in the vessel.
  • the mixture then passes through thesucceeding zones of localized agitation, the temperaturebeing controlled by meansof jackets, for instance 3, 4, 5, 6, 1, and 8, and the product and spent acid are discharged by overflowing from theoutlet l2 at a rate corresponding to the feed. of raw materials. Vents suchas 23 and 24 may be employed toremove fumesor for instance to maintain the mixture at atmospheric pressure.
  • Propeller type, paddle type,- or any other suitable type of agitators may be employed, provided they are so adjusted thatat least some of the successive. agitatorsact differently on the fluid thereadjacent, respectively.
  • the agitator shafts l1 and i9. are rotated in a clockwise direction (as seen in Figure 1)
  • the mixture in both the charging and discharging arms I I and I3, respectively tends toswirl likewise in a clockwise direction (as viewed from above), but at the bottom of the U, where the two columns of mixture join, the-direction of circulation of the one opposes. that of the other so that zones of opposing circulation. are set up.
  • any suitable mechanism may be employed for driving the shafts l1 and I9 in the same direction as viewed from above (1. e., opposite directions if viewed along the axis-of the U-tube from one end).
  • each of shafts IT and! maybe provided with pinions 3! and 39, respectively, meshing with a single drive gear38.
  • dinitromethylaniline is dissolved in 2.43 parts by weight of sulfuric acid (66 B.).
  • the nitrating acid employed contains 68% nitric acid, 16% sulfuric acid, and 16% water.
  • the diameter of the tube forming the U-shaped vessel [employed is about 16 inches and the apparatus is about 4 /2 feet high. The mixture travels about 1 1 feet in going from the inlets 9 and I9 to the outlet l2.
  • the above described nitrating acid is run into the nitrator throughinlet Illv at the rate of 18.8 gallons per houruntil'thenitrator is about A; full.
  • the feed of the acid-is then stopped and the above described solution of dinitromethylaniline is run into the-nitrator at the rate of 50 gallons per hour for an equal length of time.
  • the nitrator is sufiiciently filled for the continuous nitration operation to be started.
  • The. dinitromethylaniline solution is then fed'in through inlet 9 at a rate of about 50 gallons per hour andthenitrating acid'is simultaneously fed in.
  • the agitator l4 provides. for immediate and uniform mixing ofthe acid. and dinitromethylaniline; Agitatorshafts l1 and [9 are rotated in a' clockwisedirection (aszseen in Figure 1), the several. agitatorblades, in the form shown, being of the'type tendingjto' force at least th suspended particles of adjacent non-homogeneous mixturein a horizontalldirection. Agitators M, I6, and have their'blades so adjusted as to direct at least the suspended particles in the mixture away from the. side walls of the container,. as illustrated bythe arrows'39, and agitators. I5, 20, ancl2l have-their*blades'adjusted' so as to direct at least the suspended particles in.
  • each leg of'the U-tube there are zones of locally opposing circulation wherein'at least the suspended particles travel outwardly or inwardly in relationto the central axlsof the tube depending upon the angle of the blades of each stirrer spider to the radius. Consequently at least the suspended particles follow a generally spiral course, of travel down one legof the U-tube and up the otherleg'to the discharge outlet, the spiral varying in diameter and pitch depending upon the angle at which the blades are set' on' the stirrer with-theresultthat'a crossmixing effect of components is obtained while the mixture. as:a' whole continues to swirl in one direction inone leg; of the U-tube and in.
  • the mixture is kept at. a reactiontemperature. of; about 55? C. by flowing, water. or other. coolantas-required through the temperature controlling jackets 2, 3, 4, 5, 6, I, and 8.
  • the mixture in the '5 initial reaction zone has a purplish colorwhich disappears usually before reaching the bottom of the U-shaped vessel l and changes to'a yellow color which persists up to the outlet l2.
  • Tetryl is obtained in a yield correspondingto about 95% to 99% of theoretical, having a-pale yellow color and after moderate washing, a melting point in the range of about 127 C. to 129 C. and an acidity calculated as sulfuric acid, equal to about 0.1% to 0.3%, or even less.
  • the nitration temperature is maintained from the time of mixing of the raw materials until the reaction is completed, the necessity of starting the reaction at relatively low temperatures as in customary processes and equipment is avoided and a shorter nitration cycle is thus provided,
  • the precipitation of tetryl during nitration tends to thicken the mixture and thus materially aids in the baffling effect, resulting from the zones of opposing circulation, which prevents undesirable intermixing of the various strata of the mixture in the nitrator.
  • the nitrating acid employed is composed of about 50% nitric acid and 50% sulfuric acid.
  • the nitrator has about the same dimensions as those described in the above embodiment for the nitrator used in the manufacture of tetryl.
  • the nitrator is filled with a spent acid containing about 20% nitric acid, 64% sulfuric acid, and 16% water.
  • Anhydrous glycerine is then fed in through inlet 9 at a rate of about 18.1 gallons per hour and the nitrating acid is simultaneously fed in through inlet If!
  • the mixture in the nitrator is kept at a reaction temperature of about 16 C- to 20 C. by flowing any suitable refrigerant through the jackets 2, 3, 4, 5, 6, 1, and 8. Any fumes that develop during the reaction are readily disposed of through vents 23 and 24.
  • the large amount of heat involved in such reactions is readily dissipated in accordance with this invention by means of the large cooling surface provided per unit volume of reaction mixture and the turbulence of agitation,
  • the apparatus of this invention can be used in the manufacture of other polynitrated explosive compounds presenting similar manufacturing problems, for instance trinitrotoluene, s-cyclotrimethylenetrinitramine, tetranitroaniline, picric acid, trinitroresorcinol, pentaerythiii an U
  • the solution to be 'nitrated and the nitrating acid after being thoroughly mixed in the initial reactionzone in the nitrator tend to travel toward the discharge outlet with practically no intermixing with subsequently added raw materials, or with more completely reacted materials, while at the same time a thorough localized circulation of the mixture is provided until the reaction is complete and the productis discharged from the nitrator.
  • Continuous nitrating apparatus comprising a vessel having elongated substantially vertical portions connected at the bottom, agitator shafts in each of said substantially vertical portions, agitators carried by said shafts at a plurality of elevations in each of said substantially vertical portions, said agitators at one elevation having blades slanted substantially opposite tothe blades of an agitator at a different elevation in each of said substantially vertical portions, means for controlling the temperature of the contents of said vessel, inlets for the reagents at one end of said vessel and an outlet for the reaction products at the other end of said vessel.
  • Continuous nitration apparatus comprising a vessel formed of two upwardly extending arms connected together at the bottom to form a continuous substantially unrestricted passage therethrough, agitators at a plurality of elevations in each of said arms with at least one of said agitators in at least one of said arms having its impelling surface pitched substantially opposite to the impelling surface of an agitator in said arm at a different elevation, inlets for the raw materials at one end of said vessel, and an outlet for discharging the reaction products from the other end of said vessel.
  • Continuous nitration apparatus comprising a vessel formed of two upwardly extending arms connected together at the bottom to form a continuous substantially unrestricted passage therethrough, agitating means having agitators at a plurality of elevations in each of said arms with at least one of said agitators in one arm having its impelling surface slanted to direct at least the suspended particles of mixture contained in the vessel in a direction opposite that of at least one agitator in the other arm, means for controlling the temperature of the contents of said vessel, inlets for the reagents at one end of said vessel, and an outlet for the reaction products at the other end of said vessel.
  • Continuous nitration apparatus comprising a vessel formed of two upwardly extending arms connected together at the bottom to form a continous substantiall unrestricted passage therethrough, an agitator shaft in each of said arms, agitators carried by said shafts at a plurality of elevations, means for rotating said agitator shafts 2 inaopposite ,di-rectionssarsuviewed alongythesaxisof said vessel from one end onlygmeansior.controh ling: the temperature: oiitha-contents: of; said ivessel;v inlets; for: thezreagentsat; oneeend: of said vessel, and: anx-outlet: for: the reaction" products atitherothergend'oiisaidlvessel.
  • the axis of the vessel and the column of fluid adjacent a succeeding agi-. tator. swirlsinthe-opposite direction, the first agitator shaft.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Biochemistry (AREA)
  • Materials Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Mixers Of The Rotary Stirring Type (AREA)
US481369A 1943-03-31 1943-03-31 Apparatus for the manufacture of explosives Expired - Lifetime US2445741A (en)

Priority Applications (5)

Application Number Priority Date Filing Date Title
BE479710D BE479710A (fr) 1943-03-31
FR959787D FR959787A (fr) 1943-03-31
NL65417D NL65417C (fr) 1943-03-31
US481369A US2445741A (en) 1943-03-31 1943-03-31 Apparatus for the manufacture of explosives
GB32441/47A GB637561A (en) 1943-03-31 1947-12-09 Improvements in or relating to continuous nitration apparatus

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
US481369A US2445741A (en) 1943-03-31 1943-03-31 Apparatus for the manufacture of explosives

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US2445741A true US2445741A (en) 1948-07-20

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US481369A Expired - Lifetime US2445741A (en) 1943-03-31 1943-03-31 Apparatus for the manufacture of explosives

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US (1) US2445741A (fr)
BE (1) BE479710A (fr)
FR (1) FR959787A (fr)
GB (1) GB637561A (fr)
NL (1) NL65417C (fr)

Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2809961A (en) * 1957-10-15 L callahan
US2927845A (en) * 1956-05-15 1960-03-08 Hercules Powder Co Ltd Apparatus for manufacture of nitrocellulose
US3087971A (en) * 1953-12-07 1963-04-30 Samuelsen Eirik Method for trinitrotoluene manufacture
US3210160A (en) * 1961-10-23 1965-10-05 Little Inc A Apparatus for forming an explosive component from a melt
US3434804A (en) * 1964-08-06 1969-03-25 Ici Ltd Apparatus utilizing a webbed stirrer for continuous mixing
US4104804A (en) * 1974-04-18 1978-08-08 Sargeant Ralph G Method for drying explosive materials
US4770773A (en) * 1986-03-28 1988-09-13 The Boeing Company Mixer reactor for iron-catalyzed hydrogen peroxide oxidation process
US20030063521A1 (en) * 2001-08-31 2003-04-03 Xerox Corporation High intensity blending tool with optimized risers for increased intensity when blending toners
CN102600784A (zh) * 2012-03-26 2012-07-25 江苏沙家浜化工设备有限公司 反应釜
US20190300715A1 (en) * 2014-07-31 2019-10-03 Gregory Cole Pot hole filler composition and method of making same
CN115304433A (zh) * 2022-01-13 2022-11-08 江西宜丰国泰化工有限责任公司 一种实现高效率混合的炸药生产用动态混合器

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106824030B (zh) * 2017-02-08 2019-11-15 郑州高富肥料有限公司 一种连续化反应器

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1363368A (en) * 1920-03-04 1920-12-28 Sonsthagen Asbjorn Machine for mixing liquid, semiliquid, or viscid materials
US1961420A (en) * 1931-02-11 1934-06-05 Hildebrandt Karl Apparatus for continuous extraction of oils and fats
US2076988A (en) * 1936-03-24 1937-04-13 Wilbur M Garrett Cotton cleaner
US2103592A (en) * 1934-10-27 1937-12-28 Hercules Powder Co Ltd Method for stabilizing nitrocellulose
US2194666A (en) * 1935-10-31 1940-03-26 Meissner Josef Nitration of aromatic hydrocarbons

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1363368A (en) * 1920-03-04 1920-12-28 Sonsthagen Asbjorn Machine for mixing liquid, semiliquid, or viscid materials
US1961420A (en) * 1931-02-11 1934-06-05 Hildebrandt Karl Apparatus for continuous extraction of oils and fats
US2103592A (en) * 1934-10-27 1937-12-28 Hercules Powder Co Ltd Method for stabilizing nitrocellulose
US2194666A (en) * 1935-10-31 1940-03-26 Meissner Josef Nitration of aromatic hydrocarbons
US2076988A (en) * 1936-03-24 1937-04-13 Wilbur M Garrett Cotton cleaner

Cited By (16)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2809961A (en) * 1957-10-15 L callahan
US3087971A (en) * 1953-12-07 1963-04-30 Samuelsen Eirik Method for trinitrotoluene manufacture
US2927845A (en) * 1956-05-15 1960-03-08 Hercules Powder Co Ltd Apparatus for manufacture of nitrocellulose
US3210160A (en) * 1961-10-23 1965-10-05 Little Inc A Apparatus for forming an explosive component from a melt
US3434804A (en) * 1964-08-06 1969-03-25 Ici Ltd Apparatus utilizing a webbed stirrer for continuous mixing
US4104804A (en) * 1974-04-18 1978-08-08 Sargeant Ralph G Method for drying explosive materials
US4770773A (en) * 1986-03-28 1988-09-13 The Boeing Company Mixer reactor for iron-catalyzed hydrogen peroxide oxidation process
US20030198127A1 (en) * 2001-08-31 2003-10-23 Xerox Corporation High intensity blending tool with optimized risers for increased intensity when blending toners
US20030063521A1 (en) * 2001-08-31 2003-04-03 Xerox Corporation High intensity blending tool with optimized risers for increased intensity when blending toners
US6752561B2 (en) 2001-08-31 2004-06-22 Xerox Corporation High intensity blending tool with optimized risers for increased intensity when blending toners
US6805481B2 (en) * 2001-08-31 2004-10-19 Xerox Corporation High intensity blending tool with optimized risers for increased intensity when blending toners
CN102600784A (zh) * 2012-03-26 2012-07-25 江苏沙家浜化工设备有限公司 反应釜
US20190300715A1 (en) * 2014-07-31 2019-10-03 Gregory Cole Pot hole filler composition and method of making same
US11124651B2 (en) * 2014-07-31 2021-09-21 Gregory Cole Pot hole filler composition and method of making same
CN115304433A (zh) * 2022-01-13 2022-11-08 江西宜丰国泰化工有限责任公司 一种实现高效率混合的炸药生产用动态混合器
CN115304433B (zh) * 2022-01-13 2023-12-19 江西宜丰国泰化工有限责任公司 一种实现高效率混合的炸药生产用动态混合器

Also Published As

Publication number Publication date
GB637561A (en) 1950-05-24
FR959787A (fr) 1950-04-05
BE479710A (fr)
NL65417C (fr)

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