CA1137076A - Fluid spray mixer - reactor system - Google Patents

Fluid spray mixer - reactor system

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Publication number
CA1137076A
CA1137076A CA000340232A CA340232A CA1137076A CA 1137076 A CA1137076 A CA 1137076A CA 000340232 A CA000340232 A CA 000340232A CA 340232 A CA340232 A CA 340232A CA 1137076 A CA1137076 A CA 1137076A
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CA
Canada
Prior art keywords
mixing chamber
spray
component
sprays
liquid
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
CA000340232A
Other languages
French (fr)
Inventor
John R. Bauer
Robin L. Grieve
Robert W. Byars
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.)
Pharmacia and Upjohn Co
Original Assignee
Upjohn Co
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 Upjohn Co filed Critical Upjohn Co
Application granted granted Critical
Publication of CA1137076A publication Critical patent/CA1137076A/en
Expired legal-status Critical Current

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Classifications

    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J14/00Chemical processes in general for reacting liquids with liquids; Apparatus specially adapted therefor
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01FMIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F25/00Flow mixers; Mixers for falling materials, e.g. solid particles
    • B01F25/20Jet mixers, i.e. mixers using high-speed fluid streams
    • B01F25/23Mixing by intersecting jets
    • B01F25/231Mixing by intersecting jets the intersecting jets having the configuration of sheets, cylinders or cones
    • 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
    • B01J19/26Nozzle-type reactors, i.e. the distribution of the initial reactants within the reactor is effected by their introduction or injection through nozzles
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29BPREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B7/00Mixing; Kneading
    • B29B7/74Mixing; Kneading using other mixers or combinations of mixers, e.g. of dissimilar mixers ; Plant
    • B29B7/76Mixers with stream-impingement mixing head
    • B29B7/7631Parts; Accessories
    • B29B7/7636Construction of the feed orifices, bores, ports
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29BPREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B7/00Mixing; Kneading
    • B29B7/74Mixing; Kneading using other mixers or combinations of mixers, e.g. of dissimilar mixers ; Plant
    • B29B7/76Mixers with stream-impingement mixing head
    • B29B7/7631Parts; Accessories
    • B29B7/7647Construction of the mixing conduit module or chamber part
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G69/00Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
    • C08G69/48Polymers modified by chemical after-treatment
    • C08G69/50Polymers modified by chemical after-treatment with aldehydes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29BPREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B7/00Mixing; Kneading
    • B29B7/74Mixing; Kneading using other mixers or combinations of mixers, e.g. of dissimilar mixers ; Plant
    • B29B7/76Mixers with stream-impingement mixing head
    • B29B7/7615Mixers with stream-impingement mixing head characterised by arrangements for controlling, measuring or regulating, e.g. for feeding or proportioning the components

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • General Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Phenolic Resins Or Amino Resins (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)

Abstract

ABSTRACT OF THE DISCLOSURE
A method and apparatus are described for intimately admixing two liquid components which react chemically with each other immediately after mixing (the mixing of phosgene and polyamines is an example). The mixing is accomplished by introducing one component in the form of a fan shaped spray into a mixing chamber, and causing this spray to intersect with twin fan-shaped sprays of the second component which latter sprays are introduced into the mixing chamber from preferably diametrically opposed locations in a direction substantially perpendicular to the direction of the first component spray.
The process and apparatus in question provide improved mixing, substantially reduce problems of solids deposition hitherto encountered in similar processes, and give products of greater uniformity and improved physical properties.

Description

~7~7~

BACKGROUND OF THE DISCLOSURE
_ 1 Field of the Invention __ _ _ This invention relates to a process for admixing liquid components and to apparatus for carrying out the admixing and is more particulaxly concerned with an improved process and app~ratus for mixing liquid components which enter into rapid chemical reaction immediataly upon admixture.
2. escri~ on of the Prior Art ,: :
lQ Certain chemical reactions which are routinely carried out on a commercial scale pos~ a very serious problem because of the speed with which the reaction takes place after the reactants are brought together.
The efficiency of mixing o such reactants is of critical importance in carrying out the desired reaction.
Thu~, if the mixture o~ reactants lS not homogeneous - when the reaction commences there will be variation, rom site to site within the reaction mixture, of the relative molar proportions of the reactants. Such variation can lead to the formation of different products at the different sites.
The reaction between phosgene and polyamines to form polyisocyanates and the reaction between aniline and formaldehyde, usually in the presence of hydrochloric acid, to form methylene-bxidged polyphenyl polyamines, are two such reactions. In both of these reactions the initiation of reaction after admixture of the reactants is almost instantaneous. Further, inefficient admixture of the reactants can g~ive xise in both cases to the formation of solid by-products which tend to separate as :~7~

they are formed. Such deposition can, in certain circumstances, -lead to clogging of apparatus and eventually to shutdown of the reaction process.
Much attention has been paid in the prior art to the particular problem of seeking to minimize the effects of solid deposition in carrying out the above types of reactionO Thus, the use has been reported of a rotary mixer with high shear mix zone (U.S. patent 3,781,320 issued December 25, 1973 to Irwin), of a high speed mixer (U.S. patent 3,188,337 issued June 8, 1965 to Gemassmer), and of a multi-staye rotary pump (U.S. patent ~-
3,947,4g4 issued March 30, 1976 to Mitrowsky et al). ~he latter reference gives a lengthy analysis of the various prior art methods which have been utilized for this type of reaction.
~, One of the most successful devides hitherto employed in the art for carrying out the above xeactions is that described in U.S. patent 3~507,626 issued April 21, 1970 to Van Horn, and :::.
~` the improvPment~thereof whi~h is described in British Patent 1,238,669 issued May 25, 1971. In the latter reference a device is described by means of which the two streams of reactants are caused to follow init~ially parallel annular paths one of which ultimately flares ou~wardly and is united with the other, the mixed fluids being carried rapidly downstream from the point of mixing so that backmixing and deposition of by-pxoduct solids at the site of mixing are both minimized. It has been found, however, that even the use of this device gives rise eventually to the buildup of layers of solid on the walls of the mixing device adjacent the point o admixture of the two reactant streams~ This leads to channeling of product in the - mixing device and ultimately . . ~

~:~37~6 requires that the device be taken out of service for cleaning and repairs.
We have now found that the problems hitherto encountered in the art in the efficient admixing of highly reactive components can be minimized or eliminated using the novel apparatus and process which are described hexeinafter. Further, we have found that the increased e~ficiency of mixing of the reactant~ which i5 achieved by the process and apparatus herein described~ results in production of end product of improved properties not all of which appear to be a~tributable soleIy to the more efficient mlxing of the starting reac~ants.
SUMMARY OF THE INVENTION
This invention comprises a method for intimately mixing first and second liquid components which enter into reaction one with another substantially immediately after they are broughttogether which method comprises:
.
introduoin~ said first liquid component under pressure in the form of a fan-shaped spray into a substantially cylindrically shaped mixing chamber ln a direction substantially along the longitudinal axis of said mixing chamber;
simultaneously introducing said second liquid component under pressure into the path of said first li~uid component in said mixing chamber, in a direction substantially ~erpen-dicular to the direction of the spray of said `-first component, in the orm of at least two fan-shaped sprays; and conducting the resulting mixture of said 37~7~

two liquid components from said mixing chamber to a subsequent reaction zone.
The invention also comprises apparatus adapted to carry out the above process which apparatus comprises S in combination:
a substantially cylindrically shaped mixing chamber provided with exi.t means at one end thereof and a plurality of inle-t means at the other end thereof;
a first jet inlet means disposed suhstantially symmetrically in the end of the said mixing chambex remote from said exit means and having the nozzle of said jet means directed substantially along the longitudinal axis of said mixing chamber;
at least two additional jet :inlet means disposed in the slde walls of said mixing~
chamber at the end thereof remote from said exlt means, the nozzles of said jets being 20 . directed towards the longitudinal axis of said mixing chamber and in a plane at right angles~to said axis;
means for introducing a first liquid component under pressure through said first jet inlet means;
means for introducing a second liquid component under pressure simultaneously through ;each of said additional jet inlet means; and means for conducting mixed liquid components from said exi~ port to a subsequent reaction zone~

:~ _5_ ~3~7~

BRIEF DESCRIPTION OE THE DRAWINGS ~ ~:
.
FIGURE 1 : is a pictorial representation, partly in cross-section, of a side elevation of one embodiment of an apparatus for inter-mingling highly reactive components in accordance with the invention.
FIGURE 2 : is a ~ross-sectional view taken along the line A-A o~ the apparatus shown in FIGURE 1.
FIGU~E 3 : is a perspecti~e vlew of a jet nozzle : .
employed in the embodiment of an .:~:
apparatus according to the invention. ~:
FI&URE 3A : is a plan view~o the top of the jet ,.
: - .
nozzle shown in FIGURE 3.
FIGURE 3B :: is a~plan view of an alternative embodi~
ment of ~a~top of a~jet nozzle for use~in : the apparatus and~:method o:~ the lnvention. ~;
~ :FIGURE 4 : is a~pictorial~ representation of one ~ `
: : embodiment:~of the manner in which sprays ~ ;
: . :
.' 20 : o~ liquid components are brought together in accordance:with the invention.
~ FIGUR~ 5 : is a~:pictorial represen~a~ion of another `. : embodim~n~ o the manner in which sprays of~liquld components are brought together . - in accordance with the in~ention.
DETAILED ~ CRIPTION OF T~E INVENTION
. Re~erenoe is made: to FIGURE: l wherein there is shown .. a side eIevation, partly in:cross-section, of one -- embodiment of an apparatus in accordance with the invention and to FIGURE 2 wherein there is shown a partial cross-sectional . -6-37~6 view taken along line A~A of FIGU~E 1. The embodiment shown in FIGS. 1 and 2 is composed basically of a hollow T-shap~d housing (2) having a hollow spool (4) disposed in the crossbar section o the housing (2).
The spool (4) is provided with an annular passage (6) ; and with cylindrical channels (8), (10) and (12) each of which communicateswith a mixing chamber (14) formed by the inner walls o~ the spool (4). The mixing chamber (14) has a bell shaped opening which leads to an exit pipe ~20~ via lined pasaageway (18), said lining being of material such as tungsten carbide which will : withstand abrasion, corrosion and like forces to which : it might be subjected by the particular reaction mixture caused to pass therethrough.
Each of the cha~nels (8), (10) and (12) is adapted to receive a fan jet~spray nozzle shown respectively as ~223, (24) and (26), the nozzle tips of which project :
into the mixing chamber:(14). The precise extent to which ::, said nozzle tips project into the mixing chamber (14) is limited by the provision of flanges (28), (30~ and (32) on the outer ends o the baxrels of nozzles (22), (24) and (26~ respectively, which flanges engage with corres-ponding grooves provided in the outer ends of the respect.lve channels (8), (10) and (12). The fan jet :: 25 spray nozzle (22) and the channel (8) within which it :
is locate~ are aligned with their longi~udinal axes disposed co-axialIy with the longitudinal axis of the spool (4). The longitudinal axes of the fan jet spray nozzles (24) and (26), and the respective channels (10) and (12) in which they are housed, are aligned along a `` ~137~7~i CQmmon axis which is substantially perpendicular to the longitudinal axis of the spool (4).
Each o~ said spray jet nozzles (22~, (24) and (26) is in sliding engagement with its respective housing channels ~8), (10) and (12). The no~zles ~24) and (26) axe held in place by contact between their outer ends and the inner wall of the housing (2)o The nozzle (22) :: .
is held in place by a flange tip (34) having cylindrical .~
passageway ~35) which, in turn, is held in place in sealing engagement with the end of the crossbar section o housing (2) by means of set screws (36) and (38) . and O-ring (40)O The spool (4) is also thereby secured :~
in place in fluid tight engage~entwith the interior of housing (2) by means of O-rings (51) and (51a), and by the contact of flange (53~ with the corresponding flange : on the interior of housing (2). Additiona~l means for locking the nozzles~(22), (24) and (26) in place can ~:
be provided in the form of locking clips (not shown) and the like, if desired.
The interior of feed pipe (42) communicates with passageway (35) in spool (34) and permits one of the two fluid components which are to be mixed to be fed to fan jet spray nozzle (22). The second of the two liquid components is fed`'through inlet port (52~ via a feed ~pipe (not shown) which can be attached in sealing engage-ment at said inlet port using flange (54) and gasket surface (56). Fluid fed through inIet port (52) passes to i annular passage (6) and thence to fan je~ spray nozzles (24) and (26).
FIGURE 3 is a perspec~ive drawing illustrating the 7~6 configur~tion of a typical fan jet spray nozzlewhich can be employed in the embodiments shown in FIGURES 1 and 2. The nozzle mouth (58) shown in the jet nozzle in FIGURE 3 is elliptical in cxoss-section as can be seen more readily in FIGURE 3A which is a plan view of the top of the jet nozæle shown in FIGURE 3. While this is the preferred configuration for use in the process and apparatus of the invention, it is also possible to use other configurations. Illustratively, the nozzle mouth of the je~ noz~le~can be circular in cross-section and frusto-conical in overall - configuration with the base of the frustum uppermost as illustrated in the plan view of the top of the jet nozzle shown in FIGURE 3B.
The~ three fan~et spray nozzles (22), (24) and (26) can be identical in all respects or, in a pre~erred embodiment discussed further below, the fan iet spray nozzle~(22) is one whioh produces a smaller spray pattern arc than the other two nozzles which latter are preferably identical, i.e~ pro~uce identical spray patterns.~
In carrying out the admixing of two highly reactive fluid components using the illustrative apparatus described~above with reference to FIGURES
l, 2 and 3, a first liquid component is fed under pressure via feed pipe (42) and channel (35) to the fan jet spray nozzle ~22). Advantageously, the ; pressure used lS of the order of 150 psi to 7Q0 psi , 30 although the exact pressure employed in any given _g _ ~37~7~;

instance i5 not critical. The second fluid component necessary for the xeaction is fed under pressure, advantageously substantially equal to the pressure employed for the first component, via feed inlet (52) and annular passageway (6) to each of an jet ~pray :
nozzles (24) and (26).
The two s-~reams of said second component issuing from said nozzles (24) and (26) into mixing chamber (14) are preferably identical in shape and symmetrically disposed one towards the othe.r so that the two streams intersect in a plane coinciaent with the Longitudinal axis of the mixing chamber (14). The stream of said first fluid component issuing from fan jet spray nozzle (22) into mixing chamber (14) intersects with the two opposing streams of the second fluid component thereby effecting highly efficient mixing of the two components : under conditions of high turbulence~
The precisP position of th~ individual fan jet spray nozzles and the design of the jets therein, the size and.configur tion of the mixing chamber (14) and tha spray patterns produced by the various nozzles, are all actors which influence the efficiency of the mixing of the two fluid c:mponents. The exact combination of these factors which will give the most favorable results for the mixing of a given pair of fluid components is something which can be determined by a process of trial and error~
In general r however, it is found preferable to employ fan jet spray nozzles which produce a so called "flat"
spray, i.e. a spray which is elliptical in cross-section, .

~37~6 such as illustrated in FIGURES 3 and 3A, and mo~t prefer- .
ably one in which the elliptical cross-section has a longitudinal axis which is at least 1.5 times the shortest axis. Further, it is found highly advantageous to select fan jet spray no.zles with the appxopria~e jets to produce flat sprays and to orient them in such a manner as to produce an intersecting spray pa~ern such as that shown, in highly idealized fashion, in the perspective drawing shown in FIGURE 4. In this embodiment the ~lat spray patterns issuing from fan jet spray nozzles (24) and (26) are symmetrically disposed and have an elliptical cross-section whose longitudinal axis, represented by the common axis X-X at the plane of in~ersection o~ the two streams, is perpendicular to the direction in which the spray of the other component is issuing from the fan jet spray nozzle (22). Further, the latter is a flat spray pattern having an elliptical cross-section whose longitudinal axis, represented by Y-Y at the point at which this spray pattern intersects with the sprays from nozzles (24) and (26), is perpendicular to the direction of the latter two sprays. Finally, the confiyuration and location of fan jet spray nozzle (22), relative to the configuration and location o~ the other two nozzles, is so chosen that the width of the spray-pattern of the spray issuing from :: 25 nozzle (22) is significantly less than ~he width of the spray pattern from the o~her two nozzles at the point : at which the two patterns intersect.
FIGURE 5 illustrates another type of spray pattern : which can be employed in which the flat~ spray pattern issuiny from fan je~ spray noææle (22) has been rotated 37~7~

through an angle of substantially 90 from that shown in the embodiment of ~IGURE 4 so that the longitudinal axis Y-Y o~ the elliptical cross~section of said spray pattern at the point of intersection with the other two sprays is aligned in the same direction as the latter sprays. In both of ~he embodiments shown in FIGURES 4 and 5 the spray patterns illustrated serve to ensure that the fluid reactant component issuing as the spray ~rom nozæle (22) is completely surrounded and enveloped by the second fluid reactant issuing from spray nozzles ~24~ and (26). :
As will be obvious to one skilled in the art, the particular combination of spray patterns shown in FIGURES
4 and 5 can be achieved in a number of ways. Illustratively~
one can use identical nozzles, all designed to give the :' ;~ same elliptical spray pattern, in each of the three positions but locating the nozzle (22) in a position such that the distance through which~the spray from said nozzle has to travel before it intersects with the spray from the other two nozzles (24) and (26) is less than half the distance between the latter two no2zles. Alternatively, the three nozzles can be located substantially symmetrically in the mixing chamber (14) so that the distance which the spray from each nozzle has to travel before reaching the 25 point of intersection is substantially the same in all cases. However, in order to achieve the desired result in these circumstances, the fan jet spray nozzle (22) is so chosen that the maximum angl~ described by the fan spray pattern issulng therefrom is significantly less than that described by ~he fan spray patterns issuing from 3~71~76 nozzles (24) and (26). Illustratively, in such an embodiment the fan jet spray nozzle (22~ is so chosen ~' that it produces a fan spray pattern which describes an angle of about 45 while the fan spray pattern issuing from nozzles (24) and (26) describes a maximum angle of about 90.
While the above discussion and the various embodiments illustrated in FIGURES 1, 2, 4 and 5 have been limited to the use of only two fan jet spray nozzles (24) and (26) to introduce the second liquid component, it will be obvious that three or more such nozzles could also be used, the only requirement being that each such nozzle is disposed so that the :
spray therefrom is projected in a direction towards the central axis of the mixing chamber (14) and at right angles to the direction of spray from the~nozzle (22).
The~bringing toqether of the two fluid components, ;~ using any of the various embodiments described above, results in highly efficient mixing with very turbulent conditions in the mixing chamber (14). In the particular embodiments shawn in FIGURES 1 and 2 above the closed end of the mixing chamber (14), i.e. the end which ~:
houses the three nozzles (22), (24~ and (26), is shown as being hemispherical in configuration. This is a very convenient configuration insofar as it ensures that there are no "dead" spots in this location which might lead to build up of deposited solids, etc. However, this particular configur~tion is not critical to success `
and other configurations of this area of the mixing chamber can be employed without de~racting from the overall ~L~ 3~

excellent mixing achieved by the process of the invention.
The overall length of the mixing chamber (14) and diameter thereof are not critlcal to success of the method of the invention and the most appropriate dimensions to be employed or achievins optimum mixing of any particular combination of reactan~s can readily be determined by a process of trial and error.
The fluid mixture resulting from the bringing together of the two liquid components in the above manner passes in a continuous manner under pressure from the mixing chamber ~14) via the exlt pipe ~0~
to a further reaction zone (not shown) wherein the mixture is subjected to further treatment in accordance wlth procedures conventional in the art for whatever particulax reaction is being carried out. The exit~(16) from th mixing chamber (14) is shown, in the particular embodiments illustrated in ~IGU~ES 1 and 2, as having a flared bell-Like configuration. This is not a critical feature of the mixing process and apparatus of the invention but is merely a convenient manner of accomplishing a smooth~passage of miYed reactants from the mixing chamber (14) to the ~xit~pipe (20) which, in the particular embodLment shown, has a greater internal diameter than the mixing chamber itself. The particular configuration shown for exit section (16) ensures that there are no restrictions~pockets and the like which can lead to - buildup of deposits or create "dead" spots, i.e.
accumulations of mixed reactants which are bypassed by ; 30 the main stre~m of mixed reactants.
. .

~L~37~76 Similarly the use of the special liner (18), which is shown in the paxticular embodiments illustrated in FIGURES 1 and 2, is an optional feature intended to ensure longer life of the apparatus~ i.e. to protect against corrosion and abrasive forces and the like, and is not a critical eature of the method and apparatus of the invention.
The method of the in~ention can be applied to achieve mixing of any of a wide variety of reactants which are known to undergo rapid reaction lmmediately after they are;brought together and which, therefore, require highly efficient and rapid mixing in order to ensure a homogeneous reaction mixture and, hence, a ;~ homogeneous reactlon product. Illustrative of such - 15 reactions are that which involve the reaction between polyami~es and phosgene (both components being employed as solutions in an inert solvent such as chloroben~ene~

.
; to produce the corresponding isocyanates and the reaction between aniline (as an aqueous solution containing hydrochloric acid) and aqueous formaldehyde to produce a mixture o methylene~bridged polyphenyl po}yamines. `~``
Both of these reactions are wPll-recognized in the art as capable of producing unwanted by-products so~e of :
which are solid in nature. The formation o~ these solid by-products nas caused considerable problems in carrying out the reactions in question because of rapid .
buildup of deposits of the solids in the apparatus hitherto employed to bring the reactants together. In many instances the buildup of solids occurs so rapidly that it is necessary to shut down the process to effect --1 5~

3~7~ 1 cleaning of the apparatus at frequent intervals. Such ~`
requiremen~s are clearly highly undesirable particularly in pxocesses which are required to be run on a continuous basis.
The use of the method and apparatus of this invention has been found to obviate the difficulties hitherto involved in reactions of the above type and has enabled the reactions in question to be carried out continuously over prolonged periods with no significant buildup of solid deposits. Furthex, it is found that the reaction products achieved by use of the method and apparatus of the invention are characterized by a markedly improved uniformity of composition and a markedly lower proportion of undesirable by-products than products produced in accordance with prior procedures.
The process of reactlng polyamines with phosgene to produce polylsocyanates and the process of reacting :-~ aniline with formaldehyde (generally in the presence of : aqueous hydrochloric acid incorporated in the aniline :
stream~ to produce methylene bridged polyphenyl polyamines are both characterized by the fact that one reactant, ~ ;
namely phosgene in the first case and aniline in the second case, is generally present in. excess of the stoichiometric amount required for the reaction. In all such cases the reactant which is to be employed in excess is the reactant which is fed to the two nozzles (24)and ~26) in the ~ embodiments shown in FIGURE5 1 and 2 and the other reactant is the one fed to the nozzle (22).
It is to be understood that, while tha method and ~: 30 apparatus of the invention have been described above by -` ` il3 ~0~76 reference to certain particular embodiments thereof, it is to be clearly understood that these embodiments have been given for purposes of illustration only and are not intended to be limiting. The scope of the S invantion i5 bounded only by the scope o the claims which are set out hereafter.

.

.
'' ' . :' ' :. . - .

~ 17

Claims

A method for intimately mixing first and second liquid components which enter into reaction one with the other substantially immediately after they are brought together which method comprises:
introducing said first liquid component under pressure in the form of a fan-shaped spray into a substantially cylindrically shaped mixing chamber in a direction substantially along the longi-tudinal axis of said mixing chamber;
simultaneously introducing said second liquid component under pressure into the path of said first liquid component in said mixing chamber, in a direction substantially perpendicular to the spray of said first component, in the form of at least two fan shaped sprays; and conducting the resulting mixture of said two liquid components from said mixing chamber to a subsequent reaction zone.

The process of Claim 1 wherein the inlet means providing the fan shaped sprays of said second component are located in substantially diametrically opposed positions in the wall of said mixing chamber.

The process of Claim 1 wherein each of said fan shaped sprays of said first and second liquid components has a cross section in the form of an ellipse, the longitudinal axes of each of said ellipses being aligned in the same plane and in substantially the same direction at the point of intersection of said fan shaped sprays.

The process of Claim 1 wherein each of said fan shaped sprays of said first and second liquid components has a cross-section in the form of an ellipse, the longitudinal axes of each of said ellipses being aligned in the same plane at the point of intersection of said fan shaped sprays, the longitudinal axes of the elliptical cross-section of the fan shaped sprays of said second component being coincidental at the intersection of said sprays but that of the cross-section of said first spray being at an angle to the said common longitudinal axes at the intersection of the other two sprays.

The process of Claims 3 or 4 wherein the elliptical cross-sections of the two fan shaped sprays of said second component are substantially equal in size at the point at which their paths intersect and have a common longitu-dinal axis in the plane of intersection of said paths which axis is longer than that of the elliptical cross-section of the fan shaped spray of said first component at the point at which its path intersects that of the afore-said fan shaped sprays of said second component.

The process of Claim 1 wherein said first liquid component is a solution of polymethylene polyphenyl polyamines in an inert organic solvent.

The process of Claim 6 wherein said second liquid component is a solution of phosgene in an inert organic solvent.

The process of Claim 1 wherein said first liquid com-ponent is an aqueous solution of formaldehyde.

The process of Claim 8 wherein said second liquid component is an aqueous solution of a mixture of aniline and aniline hydrochloride.

The process of Claim 1 wherein the mixture of said first and second components is caused to pass through an expansion zone as it exits from said mixing chamber.

The process of Claim 1 wherein the relative molar proportions of said first and second components and the pressures at which they are introduced into said mixing chamber are maintained at a preselected level throughout said mixing process.

The process of Claim 1 wherein the said second component is introduced in an amount which is in excess of that proportion which represents the stoichiometric ratio in the reaction which ensues between said first and second components.

An apparatus adapted to achieve intimate mixing of two liquid components which enter into reaction one with the other substantially immediately after they are brought together, which apparatus comprises in combination:
a substantially cylindrically shaped mixing chamber provided with exit means at one end thereof and a plurality of inlet means at the other end thereof;
a first jet inlet means disposed substantially symmetrically in the end of the said mixing chamber remote from said exit means and having the nozzle of said jet means directed substantially along the longitudinal axis of said mixing chamber;
at least two additional jet inlet means disposed in the side walls of said mixing chamber at the end thereof remote from said exit means, the nozzles of said jets being directed towards the longitudinal axis of said mixing chamber and in a plane substantially at right angles to said axis;
means for introducing a first liquid component under pressure through said first jet inlet means;
means for introducing a second liquid component under pressure simultaneously through each of said additional jet inlet means; and means for conducting mixed liquid components from said exit port to a subsequent reaction zone; each of said first and said additional jet inlet means being provided with shaping means for forming said liquid com-ponents into flat spray patterns; said first jet inlet means and said additional jet inlet means being so arranged relative to each other that the paths of all of said flat sprays formed from said liquid components intersect at a common locus.

Apparatus according to Claim 13 wherein said exit means is frusto-conical in configuration.

Apparatus according to Claim 13 wherein said additional jet inlet means comprise two jet means disposed diametrically opposite each other in the side wall of said mixing chamber.

Apparatus according to Claim 13 wherein each of said jet inlet means has a nozzle shaped to produce a fan shaped spray from liquid passing therethrough under pressure.

Apparatus according to Claim 13 wherein each of said jet inlet means has a nozzle shaped to produce a fan shaped spray of elliptical cross-section from liquid passing therethrough under pressure.
Page Twenty-two of Twenty-two pages.
CA000340232A 1978-12-13 1979-11-20 Fluid spray mixer - reactor system Expired CA1137076A (en)

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CA (1) CA1137076A (en)
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DE (1) DE2950216A1 (en)
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GB2036586B (en) 1983-05-11
JPS612410B2 (en) 1986-01-24
MX149499A (en) 1983-11-15
HU180563B (en) 1983-03-28
DE2950216A1 (en) 1980-06-26
DE2950216C2 (en) 1989-06-29
GB2036586A (en) 1980-07-02
JPS5584527A (en) 1980-06-25
YU303879A (en) 1983-01-21
FR2443871A1 (en) 1980-07-11
PT70519A (en) 1979-12-01
IT7951058A0 (en) 1979-12-11
FR2443871B1 (en) 1988-09-02
IT1164091B (en) 1987-04-08
NL7908823A (en) 1980-06-17
DD147624A5 (en) 1981-04-15
ES486723A0 (en) 1980-12-16
BR7908013A (en) 1980-09-09
BE880606A (en) 1980-06-13
ES8103663A1 (en) 1981-03-16
ES493632A0 (en) 1981-03-16
ES8101402A1 (en) 1980-12-16

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