US3476669A - Apparatus for photochemical reactions - Google Patents

Apparatus for photochemical reactions Download PDF

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Publication number
US3476669A
US3476669A US540741A US3476669DA US3476669A US 3476669 A US3476669 A US 3476669A US 540741 A US540741 A US 540741A US 3476669D A US3476669D A US 3476669DA US 3476669 A US3476669 A US 3476669A
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United States
Prior art keywords
lamps
stirrer
cooling
vessel
reaction
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Expired - Lifetime
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US540741A
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English (en)
Inventor
Wilhelm Beckmann
Werner Ludwig Kengelbach
Martin Pape
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BASF SE
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BASF SE
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B28—WORKING CEMENT, CLAY, OR STONE
    • B28C—PREPARING CLAY; PRODUCING MIXTURES CONTAINING CLAY OR CEMENTITIOUS MATERIAL, e.g. PLASTER
    • B28C7/00—Controlling the operation of apparatus for producing mixtures of clay or cement with other substances; Supplying or proportioning the ingredients for mixing clay or cement with other substances; Discharging the mixture
    • B28C7/04—Supplying or proportioning the ingredients
    • B28C7/06—Supplying the solid ingredients, e.g. by means of endless conveyors or jigging conveyors
    • B28C7/08—Supplying the solid ingredients, e.g. by means of endless conveyors or jigging conveyors by means of scrapers or skips
    • B28C7/0835—Supplying the solid ingredients, e.g. by means of endless conveyors or jigging conveyors by means of scrapers or skips using skips to be hoisted along guides or to be tilted, to charge working-site concrete mixers
    • B28C7/0841—Supplying the solid ingredients, e.g. by means of endless conveyors or jigging conveyors by means of scrapers or skips using skips to be hoisted along guides or to be tilted, to charge working-site concrete mixers having mechanisms to fill the skip in its lowest position, e.g. by drag shovels, from a hopper
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
    • B01F35/90—Heating or cooling systems
    • B01F35/93—Heating or cooling systems arranged inside the receptacle
    • 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
    • B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J19/12—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electromagnetic waves
    • B01J19/122—Incoherent waves
    • B01J19/123—Ultraviolet light

Definitions

  • FIG.3 APPARATUS FOR PHOTOCHEMICAL REACTIONS Filed April 6, 1966 FIG.3
  • this may be achieved by cleaning the light transmitting surface continuously or intermittently with a film of liquid which will dissolve the obscuring layer and will not mix with the recation liquid,
  • Another known method is to produce on the light transmitting surface a regeneratable, indifferent and light-permeable crystal layer. It is also known that the deposit may be removed mechanically by means of brushes moved manually or automatically.
  • the light transmitting surface may be kept free from deposits for long periods by using an apparatus having a vessel filled with the reaction liquid and lamps, wherein stirring means is provided in the vessel and the lamps are arranged around the stirring means so that the clearance between the lamps is 0.3 times to twice the outer diameter of the lamps and the clearance between a lamp and the inner wall of the vessel is at least 0.5 times the diameter of the lamp and the clearance between the outer edge of the stirrer and a lamp is from 0.05 times to 0.5 times the diameter of the lamp.
  • the lamp is regarded as the immersed unit consisting of the light surce proper, the cooling jacket and any outer protective tube which may be used.
  • the mid points of the lamps are arranged in a circle.
  • the lamps and stirring means are arranged vertically.
  • Some of the lamps may be replaced by cooling means having the same dimensions.
  • cooling means having the same dimensions.
  • Cooling tubes may however be provided vertically or horizontally between the lamps and the Wall of the vessel.
  • a number of units each consisting of a stirrer and lamps located around the same, are arranged in series in a vessel and the vessel is subdivided by means of partitions provided with openings and located between the units to prevent backmixing.
  • a number of vessels may be arranged in series with cooling means between the vessels.
  • the apparatus in accordance with this invention may be used for example for preparing oximes from cycloalkanes; a solvent may be used if desired and stirring is effected at 40 to 200 r.p.m.
  • the apparatus according to this invention ensures that adequate turbulence is produced in the liquid over the entire exterior surface of the lamps, so that reaction liquid is uninterruptedly directed from the interior of the vessel to the light transmitting surfaces from the interior of the vessel to the light transmitting surfaces and away again, so that the formation of deposits is impossible. It is necessary that the clearances between the lamps should not be above or below certain limits. If the clearance is too small, it has been found by experiment that a zone with too little motion forms between the two lamps. If the clearance is too great, however, a flow shadow forms on the opposite side to the flow.
  • the distance from the outer wall should also be large enough to ensure complete absorption of the chemically active light in the gap between the lamp and the wall of the vessel and to ensure adequate movement of the liquid.
  • the stirring means should be sufliciently large in diameter to ensure that the turbulence is effective throughout the reactor.
  • an adequate clearance between the edge of the stirrer and the lamps must be provided so that the lamps are not broken as a resu t of virbrations caused by too strong a load on the glass wall.
  • FIGURES 1 and 2 show diagrammatically in side elevation and transverse section an apparatus having a disc impeller mixer
  • FIGURE 3 is a side elevation of an appartus having an anchor stirrer
  • FIGURE 4 is a crosssection of an apparatus having cooling means
  • FIGURE 5 is a plan view of an arrangement of several apparatus in a vessel having partitions
  • FIGURE 6 shows diagrammatically a layout of vessels and coolers.
  • the apparatus according to the invention is installed in a reactor 1 filled with reaction liqiud.
  • Lamps 2 having an external diameter D dip into the reactor 1.
  • the lamp may emit the chemically active light in all directions into the reaction liquid.
  • a stirrer for example a blade stirrer 3, is provided in the middle of the reactor 1.
  • the lamps are located around the stirrer at regular intervals so that the clearance l between any two neighboring lamps is not less than 0.3D and not more than 2.0D Similarly, the clearance m between the lamps and the reactor wall should not be less than 0.5D.
  • the dimensions of the stirrer are chosen so that the clearance it between the outer edge of the stirrer and a lamp is from 005D to 0.5D.
  • the speed of rotation of the stirrer should be high enough to ensure turbulent flow throughout the reactor.
  • the stirrer should have a height at least equal to the light-emitting length of the lamp.
  • the stirrer may also take the form of an anchor stirrer (FIGURE 3) between the reactor wall and the lamps, the above clearances between the edge of the stirrer and the lamps being maintained.
  • the direction in which the stirrer is rotated may be reversed at definite intervals determined by the liquid and the reactor. In this way the whole of the outer surface of the lamps is directly swept by the liquid at regular intervals.
  • the same effect may also be achieved by making the lamps rotatable about their axes and carrying out a rotation of up to 180 after predetermined periods.
  • the lamps and stirrer are arranged vertically, In the case of apparatus which is not operated under pressure, the use of stufiing boxes may thus be avoided or they may be protected from direct contact with the reaction liquid which is often very corrosive.
  • Photochemical reactions may be exothermic.
  • the reaction liquid may then become hot.
  • reaction may be impaired or even completely inhibited.
  • cooling means 8 FIG. 4
  • These cooling means may replace some of the lamps and have the same geometrical dimensions as the lamps.
  • the wall of the reactor 1 may however be designed as a cooling jacket 9, or horizontal or vertical cooling coils or cooling tubes 10 may be installed. In all cases excellent heat transfer is achieved because of the turbulent flow produced by the stirrer.
  • reaction vessels may be connected in series as shown in FIGURE by arranging them in a vessel 11 which may advantageously have an elongated rectangular shape,
  • the individual reactors, each provided with stirring means 12, may be separated by partitions 14 provided with openings 13. Backmixing of the reaction liquid is thus avoided and a steady increase in the amount of reaction product is achieved in the direction of flow.
  • the series connection of individual reactors to a reaction system as shown in FIGURE 5 cannot be extended indefinitely, especially when installation of cooling units instead of individual lamps or the installation of cooling coils is to be dispensed with so as to make full use of the reaction chamber for the photosynthesis. In such cases an intermediate cooling may be provided if the rise in temperature of the reaction liquid exceeds the permissible limit.
  • the arrangement may then be as shown in FIGURE 6 where the reaction liquid, after it has flowed through the first reaction system 15, is passed through a coolingunit 16, and then through a second reaction system 17 and cooling unit 18, and if desired through further reaction systems 19, 21, 23 and 25 between which are interposed cooling units 20, 22 and 24; final cooling is effected by cooling unit 26.
  • This arrangement also has the advantage of a continuous build-up of the desired reaction product without troublesome backmixing.
  • Apparatus for carrying out photochemical reactions comprising a vessel adapted to hold a reaction liquid, stirring means having rotating stirring members for agitating the reaction liquid in said vessel, and a plurality of lamps located in said vessel at positions relative to the stirring members so that the clearance between contiguous lamps is from 0.3 times to twice the diameter of a lamp, the clearance between respective lamps and the Wall of the reactor is at least 0.5 times the lamp diameter and the clearance between the edge of the stirring members and respective lamps is from 0.05 to 0.5 times the diameter of the respective lamp.
  • cooling tubes are arranged vertically between the lamps and the wall of the reactor.
  • Apparatus for carrying out photochemical reactions as claimed in claim 1 wherein a plurality of units each comprising a stirring means and a number of lamps arranged around the same are arranged in a vessel and partitions having openings therein are provided between the units to prevent backmixing.
  • Apparatus as claimed in claim 1 comprising a plurality of said vessels containing said stirring means and said lamps, means for passing reaction liquid sequentially through said vessels, and cooling means for cooling reaction liquid as it passes between each pair of vessels.
  • said lamps are tubular lamps with respective vertical longitudinal axes and said stirring means comprises a vertical rotatably driven shaft with a plurality of vertically disposed stirring members connected to and rotatably driven by said shaft.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physics & Mathematics (AREA)
  • Electromagnetism (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Toxicology (AREA)
  • Organic Chemistry (AREA)
  • Dispersion Chemistry (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
US540741A 1965-04-09 1966-04-06 Apparatus for photochemical reactions Expired - Lifetime US3476669A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DEB0081367 1965-04-09

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US3476669A true US3476669A (en) 1969-11-04

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US (1) US3476669A (cs)
AT (1) AT266792B (cs)
BE (1) BE679305A (cs)
CH (1) CH441237A (cs)
DE (1) DE1249831B (cs)
GB (1) GB1136116A (cs)
NL (1) NL147043B (cs)
SE (1) SE301634B (cs)

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3628010A (en) * 1968-07-04 1971-12-14 Ciba Geigy Ag Photochemical reactor with nozzle means to spray a reaction liquid on the walls of the reactor
US3993911A (en) * 1973-02-07 1976-11-23 Alfred Graentzel Photochemical reactor
US4517063A (en) * 1984-02-13 1985-05-14 The Standard Oil Company Photochemical reactor and method for carrying out photochemical reactions therein
US4849183A (en) * 1986-08-29 1989-07-18 Sunstar Giken Kabushiki Kaisha Continuous photochemical reactor
US5137607A (en) * 1990-04-27 1992-08-11 Wisconsin Alumni Research Foundation Reactor vessel using metal oxide ceramic membranes
US5370845A (en) * 1991-08-30 1994-12-06 Alliant Techsystems Process and apparatus for photolytic degradation of explosives
US20050092932A1 (en) * 2003-10-29 2005-05-05 Keith Bircher Fluid treatment device
CN106745484A (zh) * 2017-01-16 2017-05-31 苏州湛清环保科技有限公司 一种带搅拌装置的光化学废水处理反应器
US10865369B2 (en) 2007-01-23 2020-12-15 Kilr-Chilr, Llc Fermentation methods

Families Citing this family (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE4205864C1 (cs) * 1992-02-26 1993-06-24 Rudolf 5120 Herzogenrath De Pelzer
NO945037L (no) * 1993-12-27 1995-06-28 Shinetsu Chemical Co Fremgangsmåte og apparat til fremstilling av vinylkloridpolymer
DE29608441U1 (de) * 1996-05-09 1996-08-01 Eisenwerke Fried. Wilh. Düker GmbH & Co, 97753 Karlstadt Anlage für die Entkeimung strömender Medien, wie Wasser
WO2014002134A1 (ja) * 2012-06-26 2014-01-03 東レ株式会社 シクロアルカノンオキシムの製造方法
DE102017102165B4 (de) * 2017-02-03 2024-05-08 EKATO Rühr- und Mischtechnik GmbH Rührvorrichtung und Verfahren mit einer Rührvorrichtung
DE102017110079A1 (de) * 2017-05-10 2018-11-15 EKATO Rühr- und Mischtechnik GmbH Rührorganvorrichtung

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR1384368A (fr) * 1964-02-21 1965-01-04 Procédé de fabrication de nouveaux polysaccharides
GB1017242A (en) * 1962-07-27 1966-01-19 Toyo Rayon Co Ltd Method of photonitrosation of cycloalkane

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1017242A (en) * 1962-07-27 1966-01-19 Toyo Rayon Co Ltd Method of photonitrosation of cycloalkane
FR1384368A (fr) * 1964-02-21 1965-01-04 Procédé de fabrication de nouveaux polysaccharides

Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3628010A (en) * 1968-07-04 1971-12-14 Ciba Geigy Ag Photochemical reactor with nozzle means to spray a reaction liquid on the walls of the reactor
US3993911A (en) * 1973-02-07 1976-11-23 Alfred Graentzel Photochemical reactor
US4517063A (en) * 1984-02-13 1985-05-14 The Standard Oil Company Photochemical reactor and method for carrying out photochemical reactions therein
US4849183A (en) * 1986-08-29 1989-07-18 Sunstar Giken Kabushiki Kaisha Continuous photochemical reactor
US5137607A (en) * 1990-04-27 1992-08-11 Wisconsin Alumni Research Foundation Reactor vessel using metal oxide ceramic membranes
US5308454A (en) * 1990-04-27 1994-05-03 Wisconsin Alumni Research Foundation Reactor process using metal oxide ceramic membranes
US5370845A (en) * 1991-08-30 1994-12-06 Alliant Techsystems Process and apparatus for photolytic degradation of explosives
US5516970A (en) * 1991-08-30 1996-05-14 Global Environmental Solutions, Inc. Process and apparatus for photolytic degradation of explosives
US5524545A (en) * 1991-08-30 1996-06-11 Global Environmental Solutions, Inc. Process and apparatus for photolytic degradation of explosives
US20050092932A1 (en) * 2003-10-29 2005-05-05 Keith Bircher Fluid treatment device
US7385204B2 (en) 2003-10-29 2008-06-10 Calgon Carbon Corporation Fluid treatment device
US10865369B2 (en) 2007-01-23 2020-12-15 Kilr-Chilr, Llc Fermentation methods
CN106745484A (zh) * 2017-01-16 2017-05-31 苏州湛清环保科技有限公司 一种带搅拌装置的光化学废水处理反应器

Also Published As

Publication number Publication date
DE1249831B (de) 1967-09-14
SE301634B (cs) 1968-06-17
AT266792B (de) 1968-11-25
NL147043B (nl) 1975-09-15
GB1136116A (en) 1968-12-11
NL6604549A (cs) 1966-10-10
BE679305A (cs) 1966-10-10
CH441237A (de) 1967-08-15

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