Patent Application: US-201415028299-A

Abstract:
the present application relates to an improved apparatus for mixing intensification in multiphase systems , which can be operating in continuous or batch mode . the apparatus is based on oscillatory flow mixing and comprises a novel oscillatory flow reactor provided with smooth periodic constrictions . the apparatus can be fully thermostatized and it is based on a modular system , in order to achieve most of the industrial application . the new ofr is suitable for multiphase applications such as screening reactions , bioprocess , gas - liquid absorption , liquid - liquid extraction , precipitation and crystallization . regarding its size and geometry and the ability to operate at low flow rates , reagent requirements and waste are significantly reduced , as well as the operating costs , compared to the common reactor , such as continuous stirred tank reactor and the “ conventional ” ofr . the disclosed apparatus fulfil some of the gaps observed in the “ conventional ” ofr as well as in meso - ofr known . excellent heat and mass transfer is obtained . the scale - up is predictable .

Description:
the present technology will now be described with reference to the accompanying figures , which however are not to be construed as being limiting other possible embodiments falling within the scope of protection . the present application relates to an apparatus for mixing based on oscillatory flow reactors provided with smooth periodic constrictions . the present technology comprises new dimensions ranges that characterize the reactor vessel provided with smooth periodic constrictions , here defined as convergent - divergent section ( 5 ), and its arrangement in single pieces or plates , as illustrated on fig2 and 3 . the reactor vessel ( 8 ) may be made of metal , plastic , glass or any porous material . the reactor vessel ( 8 ) is characterized by a bundle of reactors ( 1 ), as illustrated on fig1 , that have alternatively straight sections ( 2 ) and convergent - divergent sections ( 5 ). each convergent - divergent section ( 5 ) consists of a convergent section ( 3 ) and a divergent section ( 4 ). the convergent section ( 3 ) gradually reduces its inner diameter , and the divergent section ( 4 ) presents a gradually increasing inner diameter . the shortest inner diameter , obtained at the junction of convergent section ( 3 ) and divergent section ( 4 ), is defined as d 0 . the inner diameter ( d ) of the straight section ( 2 ) is larger than d 0 . the convergent and divergent sections have a curved sidewall defined by the radius of curvature ( r c ) of the sidewall of the convergent section ( 3 ), the radius of curvature ( r d ) of the sidewall of the divergent section ( 4 ) and the radius of curvature ( r t ) at the convergent - divergent section ( 5 ) center . in order to obtain the best mixing condition , the reactor ( 1 ) shall fulfill the following conditions : 1 . the distance ( l ) between consecutive convergent sections ( 3 ) is 3 to 4 . 5 times the inner diameter ( d ) of the straight section ( 2 ). that is l = 3 - 4 . 5 d ; 2 . the convergent - divergent section ( 5 ) length ( l 1 ) is 1 . 4 to 2 times the inner diameter ( d ) of the straight section ( 2 ). that is l 1 = 1 . 4 - 2 d ; 3 . the shortest diameter ( d 0 ) of the convergent - divergent section ( 5 ) is 0 . 41 to 0 . 6 times the inner diameter ( d ) of the straight section ( 2 ). that is d 0 = 0 . 41 - 0 . 6 d ; 4 . the radius of curvature ( r c ) of the sidewall of the convergent section ( 3 ) is 0 . 4 to 0 . 5 times the inner diameter ( d ) of the straight section ( 2 ). that is r c = 0 . 4 - 0 . 5 d ; 5 . the radius of curvature ( r d ) of the sidewall of the divergent section ( 4 ) is 0 . 4 to 0 . 5 times the inner diameter ( d ) of the straight section ( 2 ). that is r d = 0 . 4 - 0 . 5 d ; 6 . the radius of curvature ( r t ) at the convergent - divergent section ( 5 ) center is 0 . 2 to 0 . 5 times the inner diameter ( d ) of the straight section ( 2 ). that is r t = 0 . 2 - 0 . 5 d ; 7 . the open area ( α ) takes the values range between 17 % and 36 %. the reactor vessel ( 8 ) characterized by a bundle of reactors ( 1 ) may be incorporated in a single piece reactor ( 6 ) or in a plate reactor ( 16 ), as illustrated on fig2 and 3 . the single piece reactor ( 6 ) consists of two concentric tubes , where the inner tube , here defined as reactor vessel ( 8 ), presents a bundle of reactors ( 1 ), and an external tube used as jacket ( 7 ) for reactor vessel ( 8 ) thermostatization , or mass transfer , if reactor vessel ( 8 ) is made of porous material . the jacket ( 7 ) has an inlet ( 12 ) and an outlet ( 13 ). the single piece reactor ( 6 ) can be arranged in parallel , series as shown in fig2 , or both . the single piece reactors ( 6 ) are butt connected by straight tubes . alternatively , the reactor links ( 14 ) can be u tubes . the first single piece reactor ( 6 ) is connected to an oscillatory unit ( 10 ), which induces a simple harmonic motion to the fluid in the reactor vessel ( 8 ), by a mixing chamber ( 9 ) provided with several inlets ( 11 ). the plate reactor ( 16 ) comprises a continuous serpentine reactor vessel ( 8 ), characterized by a bundle of reactors ( 1 ), and an external tube used as jacket ( 7 ) for reactor vessel ( 8 ) thermostatization , or mass transfer , if reactor vessel ( 8 ) is made of porous material . the jacket ( 7 ) has an inlet ( 12 ) and an outlet ( 13 ). this reactor vessel ( 8 ) has a plurality of inlets or outlets ( 15 ), to allow the addition of reactants or other substances , or sample collection . the plate reactor ( 16 ) can be arranged in parallel by stacking up the plates . the plate reactors ( 16 ) are butt connected by u tubes . the first plate reactor ( 16 ) is connected to an oscillatory unit ( 10 ), which induces a simple harmonic motion to the fluid in the reactor vessel ( 8 ), by a mixing chamber ( 9 ) provided with several inlets ( 11 ). fig2 illustrates a plan view of the oscillatory flow reactor apparatus based on single piece reactors ( 6 ) characterized by two concentric tubes , where the inner tube , here defined as reactor vessel ( 8 ), presents a bundle of reactors ( 1 ), and the external tube is used as jacket ( 7 ) for reactor vessel ( 8 ) thermostatization , or mass transfer if reactor vessel ( 8 ) is made of porous material . fig3 shows a plan view of the oscillatory flow reactor apparatus based on plate reactor ( 16 ), constituted by an inner tube , here defined as reactor vessel ( 8 ), presenting a bundle of reactors ( 1 ), an external tube used as jacket ( 7 ) for reactor vessel ( 8 ) thermostatization , or mass transfer if reactor vessel ( 8 ) is made of porous material , and several inlets or outlets ( 15 ), to allow the addition of reactants or other substances , or sample collection . single piece reactors ( 6 ) and plate reactors ( 16 ) can be closed using a close valve at reactor exit ( 17 ). single piece reactors ( 6 ) and plate reactors ( 16 ) can be combined . the number , size and length of the single piece reactor ( 6 ), plate reactor ( 16 ) or single piece reactor ( 6 ) and plate reactor ( 16 ) combinations are designed according to the system specification . single piece reactors ( 6 ) and plate reactors ( 16 ) can be operated in batchwise or continuously . the liquid or multiphase fluids are fed to the reactor vessel ( 8 ) through the inlets ( 11 ) of the mixing chamber ( 9 ). the liquid or multiphase fluid is oscillated in the axial direction by means of oscillatory unit ( 10 ), developing an efficient mixing mechanism where fluid moves from the walls to the center of the tube with intensity controlled by the oscillation frequency ( f ) and amplitude ( x 0 ). the formation and dissipation of eddies in the reactor results into significant enhancement in processes such as heat transfer , mass transfer , particle mixing and separation , beyond others . 1 . the distance ( l ) between consecutive convergent sections ( 3 ) is 3 to 4 . 5 times the inner diameter ( d ) of the straight section ( 2 ), preferably 3 . 25 d ; 2 . the convergent - divergent section ( 5 ) length ( l 1 ) is 1 . 4 to 2 times the inner diameter ( d ) of the straight section ( 2 ), preferably 1 . 5 d ; 3 . the shortest diameter ( d 0 ) of the convergent - divergent section ( 5 ) is 0 . 41 to 0 . 6 times the inner diameter ( d ) of the straight section ( 2 ), preferably 0 . 42 d ; 4 . the radius of curvature ( r c ) of the sidewall of the convergent section ( 3 ) is 0 . 4 to 0 . 5 times the inner diameter ( d ) of the straight section ( 2 ), preferably 0 . 47 d ; 5 . the radius of curvature ( r d ) of the sidewall of the divergent section ( 4 ) is 0 . 4 to 0 . 5 times the inner diameter ( d ) of the straight section ( 2 ), preferably 0 . 47 d ; 6 . the radius of curvature ( r t ) at the convergent - divergent section ( 5 ) center is 0 . 2 to 0 . 5 times the inner diameter ( d ) of the straight section ( 2 ), preferably 0 . 32 d ; 7 . the open area ( α ) takes the values range between 17 % and 36 %, preferably , 18 %; 8 . the oscillation frequency of the medium is between 1 and 6 hz ; 9 . the oscillation amplitude of the medium is between 0 and 0 . 5 times the distance ( l ) between consecutive convergent sections ( 3 ). the disclosed technology can be used in mass and heat transfer intensification . in particular , the disclosed technology can be used in mixing intensification between liquid / liquid , liquid / gas and liquid / solid phases . the disclosed technology overcome the disadvantages of the conventional ofr , based on annular baffles , especially in what concerns the dead zones decreasing and the quick cleaning process . the disclosed technology also overcome the disadvantages of the meso - ofr based on spc , especially in what concerns the decrease of the secondary nucleation , agglomeration and clogging problems . as the disclosed technology is based on a modular system , it allows a quick reactor change according to the industries needs , a distinguishing and striking characteristic of other reactors . the disclosed technology can be operated in batchwise or continuously , this characteristic being of particular relevance in chemical , bio - chemical , biological and pharmaceutical industry . the disclosed technology offers unique features in comparison with conventional chemical reactors . it is suitable for multiphase applications such as screening reactions , bioprocess , gas - liquid absorption , precipitation and crystallization operating in batch or continuous mode . as example : crystallization process — this technology offers a metastable zone increase , a better supersaturation control and a narrow crystal size distribution in crystallization of active pharmaceutical ingredients such as paracetamol and proteins such as lysozyme , beyond others ; precipitation — a mixing intensification of the solution from the first contact moments , that results in a single species precipitation without the presence of others contaminant species typical of bad mixing and always present in others reactors , was observed in the hydroxyapatite ( hap ) precipitation process ; gas - liquid systems — a significant mass transfer increase , up to ten - fold , in comparison with conventional reactors was observed ; liquid - liquid extraction — significant increase of the contact area and an uniform drops distribution inside of the reactor when compared with conventional reactors was observed . some tests were made using the technology now disclosed using different systems and ofr - spc arrangements : gas - liquid systems : the mass transfer coefficient ( kla ) values obtained with the novel ofr , as illustrated in fig2 , represented a up to ten - fold increase in comparison with a bubble column and up to eight - fold increase in comparison with the conventional ofr ; liquid - liquid extraction : a good performance in liquid - liquid mixing was observed . it is possible to control the drop size varying the oscillation frequency and amplitude . a significant increase of the contact area was observed ; liquid - solid system : particles can be well suspended in a volume concentration up to 40 %; crystallization : a continuous crystallization of hydroxyapatite ( hap ) was successfully obtained . using the apparatus , as illustrated in fig3 , it was possible to obtain hap with high chemical purity . a decrease up to 75 % of the time required to obtain the crystals , when compared with the common crystallizers , was also verified . furthermore , it has been shown that the mean particle size and the aggregation degree of the prepared hap particles can be controlled by changing the residence time of the solution in the reactor . these results show the capability of the present apparatus , operating in continuous or batch mode , for mixing intensification using multiphase systems . 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[ 35 ] r .- h . chang , continuous tubular flow reactor and corrugated reactor tube for the reactor , u . s . 2012 / 0171090 a , 2012 . the description , of course , is in no way limited to the embodiments described in this document and any person skilled in the art may envisage many possibilities of modifying it , sticking to the general idea , as defined in the claims . the preferred embodiments described above may obviously be combined together . the following claims define additionally some preferred embodiments .