• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
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    • 专利摘要:
    The present invention relates to a procedure for an ad hoc design of triphasic aqueous-micellar systems (AM3PS). As an evolution of biphasic aqueous systems (ABS), the use of AM3PS confers undoubted economic and operational advantages over their predecessors since they allow the equivalent of two consecutive extraction processes using ABS to be carried out in a single stage. In addition, due to their similarity to ABS, these triphasic systems are applicable in various fields and industrial processes, especially in industries such as chemical, biotechnology, pharmaceutical or food. Finally, because the procedure is itself a rational construction based on experimental knowledge (own and others) of the AM3PS, the present invention allows an optimized, rational design of AM3PS directed to the desired application for later use, saving on the process time, resources and therefore money. (Machine-translation by Google Translate, not legally binding)
    公开号:ES2795551A1
    申请号:ES201900085
    申请日:2019-05-21
    公开日:2020-11-23
    发明作者:Conde Lois Morandeira；Herva Francisco Javier Deive；Braga María Angeles Sanroman；Rodriguez Ana María Rodriguez
    申请人:Universidade de Vigo；
    IPC主号:
    专利说明:

    [0002] Aqueous-micellar triphasic systems: efficient design procedure for subsequent application
    [0004] Technical sector
    [0006] The present invention relates to a procedure for an ad hoc design of aqueous micellar triphasic systems (AM3PS). AM3PS represent the evolution of traditional biphasic aqueous systems (ABS) and, therefore, the importance of this procedure lies in its applicability in the recovery and purification stages of a wide variety of industrial sectors, especially in the chemical, food , biotech and pharmaceutical. In addition, different research works highlight the potential of these aqueous systems in remediation processes and recovery of residual effluents.
    [0008] Background of the invention
    [0010] Biphasic aqueous systems (ABS) emerged in the mid-20th century as an alternative to conventional liquid-liquid extraction systems based on volatile organic solvents (Albertsson PA, 1986, Partitioning of Cell Particles and Macromolecuies, Wiley, New York, 3rd edn ,). These systems are the result of the aqueous mixture of two water-soluble compounds that are immiscible from a certain composition, generating two aqueous phases rich in each of them and with different physicochemical properties. Its mostly aqueous composition has given ABS a great competitive advantage over traditional liquid-liquid extraction systems, due to its biocompatibility when used in processes in which cells, organelles or any type of biomolecule are present (Freiré MG, Cláudio AFM, Araújo JMM, Coutinho JAP, Marrucho IM, Lopesac JNC, Rebelo LPN, 2012, biphasic Systems: a boost brought about by using ionio liquids, Chem. Soc. Rev., 41,4966-4995).
    [0012] More recently, in 2003, the ability of ionic liquids (LIs) as phase segregation agents in ABS was demonstrated (Gutowski KE, Broker GA, Wiiiauer HD, Huddleston JG, Swatloski RP, Holbrey JD, Rogers RD, 2003, Controlling the Aqueous Miscibility of Ionio Liquids: Aqueous Biphasic Systems of Water-Miscible Ionio Liquids and Water-Structuring Salts for Recycle, Metathesis, and Separations, J. AM. CHEM. S O c ., 125, 6632-663). Lys are organic salts that typically have melting temperatures below 100 ° C and whose dual molecular character gives them what is perhaps their most important characteristic, their tuneability: by combining a cation and an anion, a solvent can be designed with specific physicochemical properties (Freiré mg et al. 2012).
    [0014] Over the last decades, the remarkable research effort in this field has led to the recent discovery of aqueous multiphase systems (MuPSs), which have been claimed as the evolutionary cusp of biocompatible liquid-liquid extraction systems. The first work, published in 2012, demonstrated the ability to generate aqueous systems with more than 2 phases (up to 6) through the exclusive use of polymers and surfactants (Mace CR, Akbuiut o., Kumar AA, Shapiro ND, Derda R., Patton MR, Whitesides GM, 2012, Aqueous Multiphase Systems of Polymers and Surfactants Provide Self-Assembling Step-Gradients in Density, J. Am. Chem. Soc., 134, 9094-9097), which later found direct application in the separation nanoparticles (Akbuiut O., Mace CM, Martínez RM, Kumar AA, Nie Z., Patton MR, Whitesides GM, 2012, Separation of Nanoparticles in Aqueous Multiphase Systems through Centrifugation, Nano Lett., 12, 4060 4064) and cells for medical purposes (Kumar AA, Lim C., Moreno Y., Mace CR, Syed A., Van Tyne D., Wirth DF, Duraisingh MP, Whitesides GM, 2015, Enrichment of reticulocytes from whole blood using aqueous multiphase systems of polymers, Am. J. Hematoi., 90, 31-36). Finally, in 2017 multiphase systems incorporated the use of salts and Lys to promote, together with a polymer, the generation of 3 phases whose applicability was demonstrated in the separation of dyes and various biomolecules (Passos H., Costa SH, Fernandes AM, Freiré MG, Rogers RR, Coutinho JAP, 2017, A Triple Salting-Out Effect is Required for the Formation of lonic-Liquid-Based Aqueous Multiphase Systems, Angew. Chem. Int. Ed., 56, 15058-15062).
    [0016] MuPSs are presented as a revolution in the field of separation processes, but in itself the “multiphase” concept is very general and refers to all types of systems with more than two phases. For the procedure that is detailed in this patent, the terminology aqueous-micellar triphasic systems (AM3PSs) will be used to indicate those systems whose number of phases present is three and the number of compounds that make up the same 1 + 3, water and water-soluble respectively .
    [0018] AM3PS are therefore a type of multiple liquid-liquid equilibrium composed of a mixture of four components with the ability to generate 3 immiscible aqueous phases with different properties. As in MuPSs, its definition does not consider the use of traditional organic solvents. The use of AM3PS represents undoubted economic and operational advantages over ABS since they allow the equivalent of two consecutive extraction processes using ABS to be carried out in a single stage. In addition, AM3PS allow to maintain compatibility with most cells and biomolecules of interest typical of the chemical, biotechnology, pharmaceutical and food industries.
    [0020] This procedure therefore finds application in stages of recovery / purification of these sectors. Proof of this are the multiple works that have already demonstrated the versatility of ABS in the extraction of compounds of high interest and diverse nature such as proteins (Deive, FJ, Rodríguez, A., Pereiro, AB, Araújo, JMM, Longo, MA, Coelho, MAZ, Canongia Lopes, JN, Esperanza, JMSS, Rebelo, LPN, Marrucho, IM (2011) Ionium liquidbased aqueous biphasic system for Upase extraction. Green Chemistry 13, 390-396); (Ventura, SPM, Barros, RLF, Barbosa, JMP, Soares, CMF, Lima, AS, Coutinho, JAP (2012) Production and purification of an extracellular lipolytic enzyme using ionium liquid-based aqueous two-phase systems. Green Chemistry 14, 734-740), alkaloids (Freire, MG, Neves, CMSS, Marrucho, IM, Canongia Lopes, JN, Rebelo, LPN, Coutinho, JAP (2010) Highperformance extraction of alkaloids using aqueous two-phase systems with ionio liquids. Green Chemistry 12, 1715-1718), antibiotics (Soto, A., Arce, A., Khoshkbarchi, MK (2005) Partitioning of antibiotics in a two-liquid phase system formed by water and a room temperature ionio liquid. Separation and Purification Technology 44 , 242-246) O antioxidants (ülloa, G., Coutens, C., Sánchez, M., Sineiro, J., Fábregas, J., Deive, FJ, Rodríguez, A., Núñez, MJ (2012a) On the double role of surfactants as mycoalgae cell lysis agents and antioxidants extractants. Green Chemistry 14, 1044-1051). Furthermore, in the short life span of MuPSs, its applicability to the separation of nanoparticles (Akbulut 2012), cells in medicine (Kumar 2015) and various biomolecules (Passos 2012) has also been shown, as mentioned above. .
    [0022] The use of ABS has also been proposed as a technique for the remediation of effluents through the separation and recovery of metals (Muruchi, L., Schaeffer, N., Passos, H., Mendonga, CMN, Coutinho, JAP, Jiménez, YP , 2019, Sustainable Extraction and Separation of Rhenium and Molybdenum from Model Copper Mining Effluents Using a Polymeric Aqueous Two-Phase System, ACS Sustainable Chem. Eng., 7, 1778-1785; Gras, M., Papaiconomou, N., Schaeffer, N., Chainet, E., Tedjar, F., Coutinho, JAP, Billard, I., 2018, lonic-Liquid-Based Acidic Aqueous Biphasic Systems for Simultaneous Leaching and Extraction of Metallic lons, Chem. Int. Ed., 57,1563- 1566) residual pharmaceutical and personal hygiene products (Morandeira, L., Álvarez, MS, Deive, FJ, Sanromán, MA, Rodríguez, A., 2017, Contriving to selectively sepárate drugs with a hydrophilic ionic liquid, Separation and Purification Technology, 174, 29-38; Álvarez, MS, Esperanza, JMSS, Deive, FJ, Sanromán, MA, Rodríguez, A., 2015, A biocompatible stepping stone for the removal of emerging contaminants, Sep. Purif. Technol. 153,91-98), O industrial dyes (Álvarez, MS, Moscoso, F., Rodríguez, A., Sanromán, MA, Deive FJ, 2013, Novel physico-biological treatment for the remediation of textile dyes-containing industrial effluents, Bioresour. Technol; Passos 2017).
    [0024] Explanation of the invention
    [0026] Due to the novelty of the MuPSs and, in particular of the AM3PS, substantial shortcomings are detected regarding methods, guides and even tools that allow the design and optimization of a specific system for its implementation as an industrial process. In this sense, the present invention tries to cover this need and proposes a Procedure for an ad hoc design of AM3PSs. The proposed method allows an efficient selection of the system components based on the desired end application and, based on the experimental knowledge gathered on these systems, the optimization of design and execution times.
    [0027] For the execution of the procedure that is proposed here, the aforementioned experimental knowledge (own and others) compiled on the general operation of the AM3PSs is required and, in addition, the use of two tools that will be explained below.
    [0029] Tools:
    [0031] 1. Pyramidal representation:
    [0032] The classic way to represent an ABS is by means of a regular triangle in which each vertex is a pure compound. This allows the percentage composition of any point drawn inside to be completely defined by the distance from that point to each vertex. As an evolution of ABS (tricomponent), the natural representation of AM3PS (tetracomponent) is a regular tetrahedron, in which the three faces adjacent to the vertex of the water correspond to the ABS of the four components of AM3PS. Any 3D design software can be used for this (Figure 1). Furthermore, the models used for the 2D adjustment of ABS, such as straight lines, Merchuck (Merchuk, JC, Andrews, BA, Asenjo, JA, Aqueous two-phase systems for protein separation Studies on phase inversion, Journal of Chromatography B, 1998, 711, 285-293) O Deive (Deive, FJ, Rivas, MA, Rodríguez, A., Sodium carbonate as phase promoter in aqueous Solutions of imidazolium and pyridinium ionic liquids, J. Chem. Thermodynamics, 2011, 43 , 1153 1158), can be used for 3D modeling and the generation of the characteristic surfaces that delimit each region.
    [0033] 2. Effective-Standardized Methodology:
    [0034] This methodology is a sub-procedure that allows the identification of the "limiting ABS" of the triphasic zone, from between the lateral ones. Furthermore, it can be used to estimate the triphasic volume. To do this, the following must be done:
    [0035] i) Represent the three lateral ABSs in the same triangular diagram.
    [0036] ii) Subtract the surface of solids from the systems (its estimation is explained in the precepts). For this, the values of the cut-off points of the projection of the solid surface with each edge that join said compounds with water are represented at the vertices of the non-aqueous compounds.
    [0037] iii) The system obtained with the smallest size is considered as limiting ABS. This allows different combinations of ABS to be superimposed and, with this, to estimate which one will generate a larger triphasic region before carrying out the experimental definition. Due to the above, the choice of ABS can easily be optimized to obtain the highest purity of phases and difference in properties between them. In addition, by using the tetrahedral representation, the final triphasic volume itself can be estimated (as discussed in the precepts).
    [0039] Precepts:
    [0041] The precepts presented here have been derived from the compilation of the information published in the pioneering research works in MuPSs and AM3PSs, as well as the experimental work carried out by the authors of this document.
    [0043] 1. For the formulation of an AM3PS a triple salting-out effect is required (Mace 2012; Passos 2017). This translates into the need for the three combinations resulting from mixing the three selected compounds with the water to generate windows of immiscibility.
    [0044] 2. When inorganic salts (or other solid compounds) are used to formulate the system, the surface of solids can approximate the interpolation of the lines of solids present in ABS from the faces of the regular tetrahedron.
    [0045] 3. The triphasic region is the result of the intersection of the 3 ternary immiscibilities represented in the 3 lateral ABSs. In the case where there is a large difference in the amplitude of these ABSs, it is evident that their intersection will be predominantly defined by the smaller biphasic region or “limiting ABS.” With this information, the triphasic volume can be estimated by performing a deepening of the lateral ABS in the tetrahedron, following the trend of the solid surface and until each one converges with its opposite aqueous edge: the triphasic volume will be, as an approximation, the one in which the 3 deepening intersects.
    [0046] 4. The triphasic region is on the surface of solids (Passos 2017), provided that precepts 1 and 2 are met and, due to precept 3, that the projection of the solid surface on the face that does not contain solid salt cuts within its region of immiscibility.
    [0047] 5. In the partition surfaces (SR), which represent the equilibrium established between the 3 phases generated, it can be concluded that: when the phases obtained are of high purity, the relative hydration between the phase rich in component A and that rich in B is very similar to that which occurs in the liquid-liquid equilibrium of lateral ABS {H2O AB}, defined by its distribution lines (RR). In this way, the slopes of the projection of the SRs on the side ABSs are practically the same as those of their RRs at these points. Obtaining pure phases is subject, through Precept 3, to the binodal curves of the faces of the pyramid reaching the binary edges.
    [0048] 6. The biphasic region surrounds the triphasic volume, being internally limited by the solid surface and, furthermore, its upper border is a surface that directly connects the 3 lateral ABSs. The shape of this surface is mainly influenced by the larger ABS and more weakly by the others in its vicinity.
    [0049] 7. The temperature influences the regions of the AM3PS with the same trend as that observed by the ABS (s) responsible for the immiscibility present in said region (limiting ABS / s). In this sense, if there is no clear limiting ABS or a phase has compounds that have opposite effects of temperature in the segregation of phases with the opposite, this precept should not be applied.
    [0050] Optimized strategy for the application of an AM3PS:
    [0051] Through the use of all the information collected in the Precepts presented in this document, the following sequence has been planted, which is the main object of this patent:
    [0052] 1. Formulation of AM3PS by choosing water-soluble compounds that generate 3 salting-out effects :
    [0053] The three binary combinations of selected water-soluble compounds (AB, AC, BC) with water must give rise to three regions of immiscibility and their aqueous mixtures must be compatible with the application requirements: For example, in an extraction of a biomolecule of interest : pH of the solution, the solubility and stability of the compound, etc.
    [0054] 2. Complete definition of the lateral ABS obtained with the selected compounds: The biphasic regions, solids and RRs of the three ABS generated with the compounds of Step 1. The area of immiscibility of these systems must also be large enough to approach the binary axes in such a way as to increase the chances of obtaining high purity phases in the final quaternary system. The "Normalized Cash" strategy can be used to identify limiting ABS. This sub-procedure allows optimizing the result of the AM3PS prior to its execution by changing a compound in Step 1 that allows obtaining a larger limiting ABS, without significantly affecting the immiscibility windows in the other two. In addition, it can also be used to estimate the triphasic region and its SRs according to the provisions detailed above.
    [0055] 3. Screenina initial application of the AM3PS:
    [0056] By applying the precepts to the data obtained from Step 2, a fairly reliable estimate of the AM3PS can be made. To corroborate the accuracy of this estimate, it is recommended to perform a confirmation section in the pyramid. Said section is a plane that must divide the limiting ABS {H2O A B} by the fold point of its binodal and which must pass through the opposite binary edge {H2O C}. Thanks to the aforementioned, an estimate of the region in which the 3 phases are in equilibrium is obtained and, with this knowledge, an SR is proposed in which the suitability of the AM3PS for the objective application is tested. If you get good results you can move on to the next and last step.
    [0057] 4. Optimization of the application and complete definition of AM3PS:
    [0058] Once the feasibility of using AM3PS for the desired application has been demonstrated, the complete definition of the system (boundaries between regions and their SRs) and the optimization processes of said application can be addressed (mainly through the use of different SRs and proportions in them). .
    [0059] Depending on the requirements demanded of the AM3PS and the desired application, the execution of the Procedure may differ in each case. In Figure 2 an example is proposed for the execution of the sequence object of this patent by means of a decision-making algorithm, assuming an application of the system for extraction of compounds by solubility in the equilibrium phases obtained.
    [0060] Brief description of the drawings
    [0061] Figure 1 Tetrahedral representation for an AM3PS system ( software used: Autocad).
    [0062] Figure 2 Decision-making algorithm proposed for the execution of the Procedure object of this patent assuming an application of the same for the extraction of compounds by means of their solubility in the equilibrium phases.
    [0064] Figure 3 LL equilibrium for ternary systems: A - ■ {KbPO4 Triton-X102 H 2 O}, B - ▼ {ChGly Triton-X102 H 2 O} and C - ♦ {K 3 PO 4 + ChGly H 2 O}. x represents both the initial immiscible mixture and the equilibrium phases obtained in the realization of the RRs.
    [0066] Figure 4 Representation of the "Normalized Cash" methodology: A presents the original ternary systems (■ {K 3 PO 4 + Triton-X102 H 2 O}, ▼ {ChGly Triton-X102 H 2 O} and ♦ {K 3 PO 4 + ChGly H 2 O}) as well as the calculated projection of the solid line (- • -) for the system {ChGly Triton-X102 H 2 O}; B shows the result of applying the normalization (deduction of the solid line ) and therefore allows direct comparison of ABS.
    [0067] Figure 5 Execution of the "Confirmation Section" of "Step 3" of the procedure, represented in the tetrahedral diagram. The green surface shows the estimated solid surface, while the gray surface shows the cut plane on which it was worked (according to what was explained in Step 3 of the procedure). The colored dots represent: • {K 3 PO 4 + T riton-X102 H 20 }, • {ChGly Triton-X102 H 20 }, • {K 3 PO 4 + ChGly H 20 }), • limit of the
    [0068] {K 3 PO 4 + ChGly TX102 H 2 O} triphasic region and • upper limit of {K 3 PO 4 + ChGly TX102 H 2 O} biphasic region ( software used: Autocad).
    [0070] Figure 6 Evaluation of the application collected in "Step 3" of the procedure, represented in the tetrahedral diagram. The red surface shows the SR obtained while the gray surface shows the cutting plane on which the work was done (as explained in Step 3). The colored dots represent: ^ {^ PO 4 + Triton-X102 H 2 O}, • {ChGly Triton-X102 H 20 }, • {K 3 PO 4 + ChGly H 2 O}), • limit of the triphasic region of {K 3 PO 4 + ChGly TX102 H 20 }, • upper limit of the biphasic region of {K 3 PO 4 + ChGly TX102 H 2 O} and / or initial immiscible mixture of TS and equilibrium points obtained from { K 3 P 04 + ChGly TX102 H 2 O} ( software used: Autocad).
    [0072] Figure 7 Complete definition of the system and optimization of the application, as shown in Step 4, represented in the tetrahedral diagram. The red surface shows the SRs obtained. The colored dots represent: • {K 3 PO 4 + Triton-X102 H 20 }, • {ChGly Triton-X102 H 20 }, • {K 3 PO 4 + ChGly H 20 }), • limit of the triphasic region of {K 3 PO 4 + ChGly TX102 H 20 }, • upper limit of the biphasic region of {K 3 PO 4 + ChGly TX102 H 20 } and / or initial immiscible mixture of SRs and equilibrium points obtained from {K 3 PO 4 + ChGly TX102 H 20 } ( software used: Autocad).
    [0074] Table 1 Composition and density of the immiscible mixtures prepared and the 3 equilibrium phases obtained for each one, which make up the SRs made (Figures 7 D, E and F).
    [0076] Preferred embodiment of the invention
    [0078] This section illustrates how the procedure described in this document should be carried out. As the applications can be very varied, it will only be explained how to apply this sequence with special emphasis on the design and definition of the system.
    [0079] Design of a three-phase aqueous-micellar system for its subsequent application:
    [0081] 1. Formulation of AM3PS by choosing water-soluble compounds that generate 3 salting-out effects:
    [0083] According to Precept 1, the selected non-aqueous compounds must be capable of generating three salting-out effects in their ternary combinations with water. In this sense, K 3 PO 4 , Choline Glycine (ChGly) and Triton-X102, all of them of marked biocompatible character, have shown to satisfy this criterion by being able to generate 3 ABS: {K 3 PO 4 + Triton-X102 H 20 } (Álvarez MS, Moscoso F., Rodríguez A., Sanromán MA, Deive FJ, 2012, Tritón X surfactants to form aqueous biphasic Systems: Experiment and correlation, J. Chem. Thermodynamics, 54, 385-392), {ChGly Triton -X102 H 20 } (previously carried out by the authors) and {K 3 PO 4 + ChGly H 20 } (Passos 2017). In the case presented here, it is not particularized for a specific application, which avoids posing special requirements and makes the choice of water-soluble compounds made not requiring further testing (stability of molecules or biostructures in solutions of said compounds).
    [0084] Therefore, the tetracomponent system {K 3 PO 4 + ChGly Triton-X102 H 20 } is selected as a candidate for the AM3PS formulation. An operating temperature of 30 ° C is also established, since it is in the usual optimal range for most biomolecules.
    [0086] 2. Complete definition of the lateral ABS obtained with the selected compounds:
    [0087] However, in the previous research works, which concluded the triple salting-out effect between the selected compounds, solid lines were not defined and / or operating temperatures other than those proposed for this example were used. Therefore, it is necessary to obtain the complete data experimentally. To do this, mixtures of the water-soluble compounds were prepared to which water was added gradually and while stirring, interspersing centrifugation processes that allowed evaluating the existence of solids. For the determination of the binodal curve, the turbidimetric method was used (Albertsson, pa, John Wiley and Sons, New York, 1986). The results are presented in Figure 3.
    [0089] According to precept 5, the RRs provide information on the hydration that occurs between the phases of the SRs of the generated AM3PS. Because the phases obtained in the RRs are of high purity, the relative hydrations between phases will be similar to those observed in these ternary systems. Therefore, according to these data, it is deduced that the phases rich in K 3 PO 4 and in ChGly will have similar hydrations, while the surfactant phase will be much less hydrated than the previous two.
    [0091] According to the procedure, it is also convenient to use the normalized effective methodology to find the limiting ABS and thus more accurately estimate the final behavior of the AM3PS. The results are collected in Figure 4.
    [0093] To carry out the "Normalized Cash" procedure, it is necessary to deduct the surface of solids for each system. Precept 2 establishes that this surface can approximate the interpolation of the solid lines of the lateral ABS with the salt that causes this phenomenon, so the surface passes through the lines of those ABS. However, the {ChGly Triton-X102 H 2 O} system does not contain solids, so it is necessary to apply the surface projection. Again, as the solid surface is defined by the solid lines of the other ABS, this projection can be calculated joining the point where these lines intersect the axes common to this system (line - • - in Figure 3A). Once the procedure is applied, redefining the vertices, Figure 3B is obtained. The use of this methodology allows us, according to Precept 3, to establish that the limiting ABS is clearly the {K 3 PO 4 + ChGly H 20 } system. This means that the triphasic region will be mostly defined by this lateral immiscibility and, therefore, the region in question can be approximated to a volume located on the surface of solids and of height and width very similar to that of limiting ABS.
    [0095] 3. Initial screening of the AM3PS application:
    [0097] All the knowledge acquired during Step 2, together with the application of the knowledge collected in the precepts, allows estimating the regions of the AM3PS (solid, biphasic and triphasic). However, in this step it is recommended to define a confirmation section to verify that the triphasic region actually exists and that it adjusts to the estimates made. For this, in this work, mixtures of water-soluble components ABC were prepared in the required proportions to which water was added gradually and while stirring, interspersing centrifugation processes that allowed evaluating each of the regions: the existence of solids or the number of phases. . The turbidimetric method (Albertsson, p.a. 1986) can also be used to define the biphasic zone. The information obtained through this action is shown in Figure 5.
    [0099] Figure 5 shows that there is indeed a three-phase system and that the surface of solids and the amplitude of the system agree with the estimates made in Precepts 2, 3 and 4. The information collected in this figure shows an idea of the range of mixtures that they can be used to generate three phases. An SR is then performed in the middle of said region.
    [0101] The SR performed corresponds to the quaternary mixture represented in Figure 6 (white point in the middle of the SR) and required a natural separation time (by gravity) of 48 h. This time can be reduced to less than one min by centrifugation at 2113 RCFs (Relative Centrifugal Force). The phases obtained present a high purity, since they clearly reach the edges of the pyramid in two of the cases and are very close in the third. Furthermore, the relative hydrations between phases are similar to those shown in the RRs of ternary systems (Figure 3), which is consistent with Precept 5. The properties of this SR are collected in Table 1 (SR2).
    [0103] The SR described can be used in different applications, such as the extraction of biological molecules or structures by preferential solubility in one of the phases, as well as the separation of insoluble solids by difference in densities. It is at this point, on this SR, where the initial tests to assess the suitability of the system for the desired application must be carried out. If you achieve promising results, you can then move on to the next step.
    [0105] 4. Optimization of the application and full definition of AM3PS:
    [0107] After having demonstrated the applicability of AM3PS, we proceed to its complete definition and optimization. Defining the system requires an experimental search for the limits of equilibrium and operation. For this, the previously explained procedures were used. Knowledge of the regions is essential to always keep a process that you want to implement at an industrial level under control, as well as to identify any deviation from it. On the other hand, process optimization is performed by describing several SRs, since each one has different properties, so that the three-phase balance that best meets the objectives of the desired application is chosen. The results are presented in Table 1 and in Figure 7.
    [0109] The choice of the TSs for the optimization of the application aims to map the evolution of the equilibrium established between the three phases throughout the triphasic region. In this sense, the TS carried out comprise the majority of the triphasic volume and show high purity in the phases obtained, with the exception of a notable variation in terms of the impurity of salt existing in the phase rich in Ll when the equilibrium contains more quantity of Water. Although this phenomenon is not desirable for an extraction application through the solubility of the target compounds, it does increase the ability of the system to significantly vary the densities of the middle phase (rich in Ll) and lower phase (rich in salt), as shown in the Table 1, which is interesting for separation processes through the use of this property. In addition, the data samples presented here were found to have high chemical stability over time.
    [0111] Industrial application
    [0113] As has already been stated throughout the document, the applicability of the procedure object of this patent lies in the inherent characteristics of AM3PS, since this procedure is the first of its kind that is aimed at applying and knowing these systems. In this sense, given that the three-phase equilibrium of an AM3PS is an evolution of ABS, its use implies undoubted economic and operational advantages compared to said ABS, since they allow the equivalent of two consecutive extraction processes to be carried out in a single stage by means of ABS. It can therefore be said that due to this, AM3PS are also applicable in processes that require ABS, the latter being widely used in the food, chemical and especially pharmaceutical and biotechnology industries. Moreover, in general, they can be used in any process that requires a separation stage. Finally, it should be noted that the state-of-the-art research being carried out globally indicates that ABS (and therefore AM3PS) can be used as effective remediation / recovery techniques for contaminated effluents.
    权利要求:
    Claims (5)
    [1]
    1. Procedure for an ad hoc design of triphasic aqueous-micellar systems (AM3PS) that allows:
    1. An efficient selection of system components based on the desired application.
    II. The optimization of the AM3PS through the correct choice of the ABS components that comprise it, without the need to proceed to the total definition of the final system.
    III. The proper evaluation of the target application without the need to perform the full definition of the quaternary system.
    [2]
    2. Process according to claim 1 that is made up of 4 stages.
    I. Formulation of AM3PS by choosing water-soluble compounds that generate 3 salting-out effects .
    II. Complete definition of the lateral ABS obtained with the selected compounds.
    III. Initial screening of the AM3PS application.
    IV. Optimization of the application and complete definition of the AM3PS.
    [3]
    3. Procedure according to claims 1 and 2, characterized in that Step 2 "Complete definition of the lateral ABS obtained with the selected compounds" incorporates the use of the "Normalized Effective" methodology. This sub-procedure allows the detection of the limiting ABS of the triphasic region and, thanks to it, the triphasic volume can be optimized by choosing the water-soluble compounds and the ABS they generate.
    [4]
    4. Process according to claims 1 and 2 that is applicable to AM3PS formulated with all those aqueous mixtures of the following water-soluble compounds: inorganic salts, organic salts, ionic liquids, polymers, surfactants, amino acids, proteins, organic acids and carbohydrates.
    [5]
    5. Process according to claims 1 and 2 of application for systems based on an L-L-L balance, whether or not they contain water, which adds the use of organic solvents to Claim 4.
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    ES2126867T3|1999-04-01|PARTICULATE TRAINING METHOD USING A SUPERCRITICAL FLUID, AEROGEL PARTICLES SO FORMED AND ANTI-SWEAT CONTAINING AEROGEL PARTICLES.
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    Andrews et al.1994|The effects of pH and ionic strength on the partitioning of four proteins in reverse micelle systems
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    Chang et al.1982|Proteolytic degradation of calf thymus terminal deoxynucleotidyl transferase.
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    Geiger et al.1992|Structure of stable and metastable water. Analysis of Voronoi polyhedra of molecular dynamics models
    Nakao et al.2017|A Framework for deformation estimation of elastic bodies from monocular images
    Smillie et al.1958|Properties of calf thymus histone isolated by three different methods
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    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    WO2012024688A1|2010-08-20|2012-02-23|President And Fellows Of Harvard College|Multiphase systems and uses thereof|
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