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WO2014119978A1 - Accelerated biodiesel electropurification - Google Patents

Accelerated biodiesel electropurification Download PDF

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Publication number
WO2014119978A1
WO2014119978A1 PCT/MX2013/000012 MX2013000012W WO2014119978A1 WO 2014119978 A1 WO2014119978 A1 WO 2014119978A1 MX 2013000012 W MX2013000012 W MX 2013000012W WO 2014119978 A1 WO2014119978 A1 WO 2014119978A1
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WIPO (PCT)
Prior art keywords
biodiesel
glycerin
mixture
electrodes
decantation
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Application number
PCT/MX2013/000012
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Spanish (es)
French (fr)
Inventor
Pedro Gabriel GONZÁLEZ ESTRADA
Dino Alejandro PARDO GUZMÁN
Felipe CARO RAMOS
Guillermo Javier KITAZAWA MOLINA
José Martín VELEZ DE LA ROCHA
Hiram GUTIERREZ LIZARRAGA
Adilene Margarita LAREZ MOLINA
Cinthya Araceli RUIZ PARDO
Juan Pedro CAMOU ESTEBAN
Iván Roberto KAWAMINAMI GARCÍA
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Individual
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Individual
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Priority to PCT/MX2013/000012 priority Critical patent/WO2014119978A1/en
Publication of WO2014119978A1 publication Critical patent/WO2014119978A1/en
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D17/00Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
    • B01D17/06Separation of liquids from each other by electricity

Definitions

  • the separation of two liquids of different density can be done by equipment designed for this purpose, called decanters. Normally, the liquid present in greater proportion forms the external phase. The liquid that is present in a smaller proportion, either in suspension or in emulsion, forming drops that, for design purposes, can be considered discrete particles.
  • Decantation or sedimentation of the suspended particles occurs because, due to their higher density, they form a phase that accumulates at the bottom of the container containing the liquid mixture.
  • the suspended drops are deposited at the bottom at a rate that is proportional to the square of the particle diameter, is also proportional to the difference between the relative densities of the two liquids, and is inversely proportional to the viscosity of the liquid that forms the phase external When heat is applied to the mixture, and therefore the viscosity decreases, the temperature is directly proportional to the rate of decantation.
  • the equation that summarizes all of the above is known as Stokes's Law.
  • Various methods are used to increase the decantation rate. Joining suspended particles or droplets is one of the procedures that greatly increases the efficiency of decanters and settlers. When the particles are solid, this process is known as flocculation; When they are liquid it is called coalescence. When the particles or drops are grouped, they form particles of greater weight and size, thereby increasing the decantation rate.
  • the presence of water in the ternary system promotes a reduction in viscosity and an increase in the polarity of the glycerin fraction, which are very advantageous in their decantation under conditions of rest or centrifugation.
  • intermediate compounds of the trans-esterification reaction such as mono- and diglycerides, or saponified compounds, derived from secondary reactions between the catalyst and triglycerides, leads to the stabilization of a persistent emulsified system.
  • the stable emulsion contains hydrated glycerin as a dispersed phase; mono- and diglyceride esters and intermediates as a dispersing phase, and saponified compounds as emulsifying agents.
  • the alcohol component remaining in the process is subdivided in proportion between the two phases.
  • a theoretical alternative in order to overcome the problem of glycerin separation would be to reduce the alcohol content by distillation and subsequent catalyst neutralization, with the addition of a mineral acid.
  • These measures may give rise to other problems for the purification process, such as the partial inversion of the reaction - with the formation of the intermediate compounds (mono and di-glycerides) and the precipitation of fatty acids, due to the neutralization of saponified compounds.
  • the point of balance between these two steps is difficult to establish and highly dependent on the characteristics of the reaction load.
  • Methanol more reactive than ethanol, is used more frequently in industrial processes. However, due to its toxicity, it is being replaced by ethanol, which in addition to being less toxic can be obtained from a renewable source.
  • the type of catalyst used, the reaction conditions, the type and concentration of impurities in the reaction medium determine the course of the yield and the by-products obtained in the trans-esterification of triglycerides.
  • One of these reaction byproducts is the formation of soaps, which leads to stable emulsions.
  • glycerin is dispersed in the biodiesel in the form of droplets; With its surfactant action, the deposit of soap molecules on the surface of the drops that give rise to the emulsion. For this reason, the step in which glycerin is separated from biodiesel constitutes a critical step in the industrial process.
  • Patent document EP2332903 refers to a process for the purification of biodiesel obtained from castor seed oil, for the purpose of promoting the efficiency of the separation of the glycerin fraction formed during the trans-esterification reaction of a mixture of petroleum-derived long chain triglycerides in the presence of ethanol and an alkaline catalyst. More specifically, the present invention relates to the application of a method for electrostatic separation of the glycerin fraction to conventional processes for the industrial production of biodiesel. The invention now proposed is intended to solve this problem by drastically reducing the time for phase separation.
  • Patent application EP2349521 describes a vertical electrostatic coalescer comprising a first and second electrode surface, and a horizontally arranged foraminous surface.
  • the first electrode surface and horizontally arranged foraminous surface are at ground potential.
  • the surfaces of the first and second electrodes share the same flat orientation with respect to the central longitudinal axis of the vessel.
  • the unique arrangement of the vessel and opposite pairs of surfaces of the first and second electrodes provide for a substantially uniform voltage field around a perimeter of the vessel and an effective voltage field for coalescence within a center of a vessel.
  • a circular distribution tube or in the form of a distribution housing, serves to absorb the impulse of the incoming emulsion current and distribute the current inside an vessel.
  • Figure 1 is a conventional perspective view of the decanter device of a mixture of biodiesel and glycerin, of the present invention.
  • Figure 2 is a side longitudinal section of the decanter device of a mixture of biodiesel and glycerin, in question.
  • Figure 3 is an upper longitudinal section of said decanter device of a mixture of biodiesel and glycerin.
  • Figure 4 is a side view of the decanter device of the present invention.
  • Figure 5 is a longitudinal section of the decanter device, in comment.
  • Figure 6 is a conventional perspective view of the internal components of the decanter device of this invention.
  • Figure 7 is a longitudinal section of Figure 6, where side perforations are seen.
  • Figure 8 is a schematic diagram of the integral system for the decantation of a mixture of biodiesel and glycerin, of the present invention.
  • Example 1 Preferred mode for the realization of the device and a system, for decanting a mixture of biodiesel with glycerin, of the present invention.
  • the present example describes one of the preferred embodiments for the realization of the decanter device for a mixture of biodiesel and glycerin, of the present invention, which comprises a horizontally arranged bottom trapezoidal tank (1) in channel "V", which is divided into two sections (I and II); where the first section is crossed longitudinally by a straight tube (2), where the mixture of biodiesel and glycerin is introduced. Side holes (3) are provided along the tube, to minimize the area of turbulence.
  • an inclined plate (4) is installed, to favor the separation of the particles by density difference, forcing the flow of mixture that leaves those holes ( 3) to ascend and descend following the path that determines the angle of inclination of such plates (4).
  • At least one first pair of electrodes (5) is inserted, which will be fed with a certain voltage, so that they form an electric field that will accelerate the decantation of the glycerin.
  • a first glycerin sensor (S1) is also included.
  • a zigzag channel is provided, which is formed by a set of vertical plates (6), to orient the flow of mixture in the horizontal path and alternate direction, and thus increase the residence time of the flow mix.
  • a second pair of electrodes (7) connected to a voltage source is placed in the final part of said zigzag channel. This also integrates a second glycerin sensor (S2).
  • an outlet control valve for glycine (A4) is provided, which deposits the glycerol in its respective container (G) and a control valve for the output of pure biodiesel (A3), the which will deposit it in its container of pure biodiesel (B2).
  • the electrical current consumption of this second pair of electrodes (7) will be indicative that the glycerin separation has been completed.
  • the amperage level of the last pair of electrodes will be used to control the feed flow received by the decanter.
  • the electrodes have their respective insulated terminals (13) so that multiple high voltage electric power supply variables (8 and 9) are connected to their respective sources.
  • the glycerin sensors (S1 and S2) are connected to a processing unit (11), to monitor and control the degree of decantation or recovery of glycerol; said processing unit (11) contains: at least one electrical conductivity sensor, at least one electrical current sensor installed in each high voltage electrode module, a conductivity indicator, with reading associated with the degree of glycerol decantation.
  • the processing unit (11) is an electronic device that receives and processes signals from the sensors, particularly the glycerin sensor (10), to make decisions about the flow of water to be injected into the decanter device and the electric field to be applied. .
  • the processing unit (11) has a multivariable modeling algorithm that minimizes in real time the glycerin impurities present in the biodiesel flow through the glycerin valve (A4), depending on the DC and AC characteristics of the voltage applied by the sources of power and luxury of water injected into the decanter.
  • the decanter device has a source of impure biodiesel (B1) and a source of water (12), which are connected, by means of pipes, to the supply tube (2) of said device; and it is provided with a control valve for the amount of impure biodiesel (A1) and a control valve for the amount of water (A2).
  • the present invention also provides a system for the decantation of a mixture of biodiesel and glycerin, where the decanter device described above intervenes. Therefore, said system comprises the decanter apparatus already referenced and all external components, to carry out a process of decanting a mixture of biodiesel and glycerin.
  • the action of the electric field is due to the polar character of the glycerol molecule. These molecules form dipoles that are electrically oriented in the same direction, in the presence of a continuous electric field, attracting each other; also the drops lose their sphericity when deformed by the action of the electric field, reduce their surface tension and favor the contact between them and therefore their coalescence.
  • coalescence is favored because the suspended drops are agitated by the variation of the electric field, favoring the contact between them, resulting in a greater coalescence, resulting in a higher decantation rate.
  • Example 2 Operation and procedure, for the decantation of a mixture of biodiesel and glycerin.
  • the flow containing the mixture of glycerol and fatty acid methyl esters enters the decanter described in example 1, through the feed tube (2) that distributes this flow through multiple perforations (3) along the feed tube (2) .
  • the inclined plates (4) orient the flow in vertical path, facilitating the decantation due to the difference in densities of the fluids that make up the mixture.
  • the first pair of electrodes (5) generates an electric field in the first section of the decanter. This electric field accelerates the decantation, as it stimulates the coalescence of the glycerin particles suspended in the biodiesel.
  • Glycerol flows through the bottom of the decanter, whose bottom has a slope.
  • the fluids pass to the second section of the decanter consisting of a series of vertical plates (6) that orient the flow in alternate directions, in order to allow a longer residence time with which a complete separation of the fluids is achieved.
  • the electric field is caused by the second pair of electrodes (7).
  • the current consumption in each section of the apparatus, by the electrodes is monitored by the processing unit (11), and is used as a reference for the degree of fluid separation.
  • the mixing feed valves, the glycerol and biodiesel outlet valves located respectively in the lower and upper part of the second section of the decanter, are controlled by said unit (11).

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  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)

Abstract

The present invention describes a novel apparatus for accelerating the biodiesel purification process by separating out glycerine by assisted settling, by means of a set of elements that includes the presence of a series of pairs of plates subjected to an alternating electrical potential difference, inducing electric fields of lesser intensity at the flow inlet for the biodiesel and glycerine to the apparatus and of greater intensity at the outlet for purified biodiesel. The apparatus induces a laminar flow of the incoming mixture of biodiesel and glycerine by means of narrow channels subjected to the presence of a high-frequency electric field to facilitate the known process of coalescence and settling of the glycerine molecule. The result is a system capable of reducing the settling rapidity to less than 10% as compared with the traditional settling system whereby the mixtures are left to stand.

Description

ELECTROPURIFICACIÓN ACELERADA DE BIODIESEL  ACCELERATED BIODIESEL ELECTROPURIFICATION

CAMPO TÉCNICO DE LA INVENCIÓN TECHNICAL FIELD OF THE INVENTION

El ámbito o campo tecnológico en donde se aplica la presente invención para su utilización práctica es el de la industria del biodiesel y otros sectores industriales que requieren implementar métodos y tecnologías para la rápida separación de fluidos por decantación. The scope or technological field where the present invention is applied for practical use is that of the biodiesel industry and other industrial sectors that require implementing methods and technologies for rapid separation of fluids by settling.

ANTECEDENTES DE LA INVENCIÓN BACKGROUND OF THE INVENTION

La separación de dos líquidos de distinta densidad puede realizarse mediante equipos diseñados para tal efecto, llamados decantadores. Normalmente, el líquido presente en mayor proporción forma la fase externa. El líquido que está presente en menor proporción, ya sea en suspensión o en emulsión, formando gotas que, para efectos de diseño, pueden considerarse partículas discretas. The separation of two liquids of different density can be done by equipment designed for this purpose, called decanters. Normally, the liquid present in greater proportion forms the external phase. The liquid that is present in a smaller proportion, either in suspension or in emulsion, forming drops that, for design purposes, can be considered discrete particles.

Esto quiere decir que para los decantadores se utilizan las técnicas aplicadas al diseño de los sedimentadores. Estos últimos se utilizan para separar partículas sólidas suspendidas en un líquido. This means that for the decanters the techniques applied to the design of the settlers are used. The latter are used to separate solid particles suspended in a liquid.

La decantación o sedimentación de las partículas suspendidas sucede en virtud de que, por su mayor densidad, forman una fase que se acumula en el fondo del recipiente que contiene la mezcla de líquidos. Las gotas suspendidas se depositan en el fondo a una velocidad que es proporcional al cuadrado del diámetro de la partícula, es proporcional también a la diferencia entre las densidades relativas de los dos líquidos, y es inversamente proporcional a la viscosidad del líquido que forma la fase externa. Cuando se aplica calor a la mezcla, y disminuye por tanto la viscosidad, la temperatura resulta directamente proporcional a la velocidad de decantación. La ecuación que resume todo lo anterior es conocida como Ley de Stokes. Diversos métodos son utilizados para incrementar la velocidad de decantación. Unir partículas o gotas suspendidas es uno de los procedimientos que incrementan considerablemente la eficiencia de los decantadores y sedimentadores. Cuando las partículas son sólidas a este proceso se le conoce como floculación; cuando son líquidas se llama coalescencia. Cuando las partículas o gotas se agrupan forman partículas de mayor peso y tamaño, incrementando con ello la velocidad de decantación. Decantation or sedimentation of the suspended particles occurs because, due to their higher density, they form a phase that accumulates at the bottom of the container containing the liquid mixture. The suspended drops are deposited at the bottom at a rate that is proportional to the square of the particle diameter, is also proportional to the difference between the relative densities of the two liquids, and is inversely proportional to the viscosity of the liquid that forms the phase external When heat is applied to the mixture, and therefore the viscosity decreases, the temperature is directly proportional to the rate of decantation. The equation that summarizes all of the above is known as Stokes's Law. Various methods are used to increase the decantation rate. Joining suspended particles or droplets is one of the procedures that greatly increases the efficiency of decanters and settlers. When the particles are solid, this process is known as flocculation; When they are liquid it is called coalescence. When the particles or drops are grouped, they form particles of greater weight and size, thereby increasing the decantation rate.

Diversos estudios han demostrado que, para el caso de la mezcla de glicerol con ésteres metílicos de ácidos grasos (biodiesel), la coalescencia de las gotas de glicerol puede ser inducida mediante la acción de un campo eléctrico de alto voltaje. Otros investigadores han demostrado que las emulsiones agua-petróleo pueden separarse también en presencia de un campo eléctrico. La etapa de separación de la fracción de glicerina en el proceso industrial para la producción de biodiesel que convencionalmente se maneja como una operación separada de la de tipo decantación gravitatoria o centrífuga, casi siempre precedido por la adición de un porcentaje de agua en un intervalo de 5 a 20 %. La presencia de agua en el sistema ternario (ésteres/alcohol/glicerina) promueve una reducción en la viscosidad y un aumento de la polaridad de la fracción de glicerina, que son muy ventajosas en su decantación en condiciones de reposo o centrifugación. Sin embargo, la presencia de compuestos intermedios de la reacción de trans-esterificación, tales como mono-y diglicéridos, o compuestos saponificados, procedentes de reacciones secundarias entre el catalizador y los triglicéridos, conduce a la estabilización de un sistema emulsionado persistente. La emulsión estable contiene la glicerina hidratada como una fase dispersa; los ésteres de mono-y diglicéridos y compuestos intermedios como una fase dispersante, y los compuestos saponificados como agentes emulsionantes. El componente de alcohol restante en el proceso se subdivide en proporción entre las dos fases. Several studies have shown that, in the case of the mixture of glycerol with fatty acid methyl esters (biodiesel), the coalescence of the glycerol drops can be induced by the action of a high-voltage electric field. Other researchers have shown that water-oil emulsions can also be separated in the presence of an electric field. The stage of separation of the glycerin fraction in the industrial process for the production of biodiesel that is conventionally handled as a separate operation from the gravitational or centrifugal decantation type, almost always preceded by the addition of a percentage of water in a range of 5 to 20%. The presence of water in the ternary system (esters / alcohol / glycerin) promotes a reduction in viscosity and an increase in the polarity of the glycerin fraction, which are very advantageous in their decantation under conditions of rest or centrifugation. However, the presence of intermediate compounds of the trans-esterification reaction, such as mono- and diglycerides, or saponified compounds, derived from secondary reactions between the catalyst and triglycerides, leads to the stabilization of a persistent emulsified system. The stable emulsion contains hydrated glycerin as a dispersed phase; mono- and diglyceride esters and intermediates as a dispersing phase, and saponified compounds as emulsifying agents. The alcohol component remaining in the process is subdivided in proportion between the two phases.

Una alternativa teórica con el fin de superar el problema de separación de glicerina sería reducir el contenido de alcohol por destilación y posterior neutralización del catalizador, con la adición de un ácido mineral. Esas medidas, sin embargo, pueden dar lugar a otros problemas para el proceso de purificación, tales como la inversión parcial de la reacción - con la formación de nuevo de los compuestos intermedios (mono y di-glicéridos) y la precipitación de ácidos grasos, debido a la neutralización de los compuestos saponificados. El punto de equilibrio entre estos dos pasos es difícil de establecer y altamente dependiente de las características de la carga de reacción. A theoretical alternative in order to overcome the problem of glycerin separation would be to reduce the alcohol content by distillation and subsequent catalyst neutralization, with the addition of a mineral acid. These measures, however, may give rise to other problems for the purification process, such as the partial inversion of the reaction - with the formation of the intermediate compounds (mono and di-glycerides) and the precipitation of fatty acids, due to the neutralization of saponified compounds. The point of balance between these two steps is difficult to establish and highly dependent on the characteristics of the reaction load.

El metanol, más reactivo que el etanol, se utiliza con más frecuencia en los procesos industriales. Sin embargo, debido a su toxicidad, está siendo reemplazado por el etanol, que además de ser menos tóxico puede obtenerse de una fuente renovable. Por otro lado, el tipo de catalizador utilizado, las condiciones de reacción, el tipo y concentración de impurezas en el medio de reacción, determinar el curso del rendimiento y de los subproductos obtenidos en la trans-esterificación de los triglicéridos. Uno de estos subproductos de la reacción es la formación de jabones, que conduce a emulsiones estables. Bajo agitación, se dispersa la glicerina en el biodiesel en la forma de gotitas; con su acción tensioactivo, el depósito de jabón moléculas en la superficie de las gotas que dan lugar a la emulsión. Por esta razón, el paso en el que se separa la glicerina del biodiesel constituye un paso crítico en el proceso industrial. Methanol, more reactive than ethanol, is used more frequently in industrial processes. However, due to its toxicity, it is being replaced by ethanol, which in addition to being less toxic can be obtained from a renewable source. On the other hand, the type of catalyst used, the reaction conditions, the type and concentration of impurities in the reaction medium, determine the course of the yield and the by-products obtained in the trans-esterification of triglycerides. One of these reaction byproducts is the formation of soaps, which leads to stable emulsions. Under stirring, glycerin is dispersed in the biodiesel in the form of droplets; With its surfactant action, the deposit of soap molecules on the surface of the drops that give rise to the emulsion. For this reason, the step in which glycerin is separated from biodiesel constitutes a critical step in the industrial process.

El documento de patente EP2332903 se refiere a un procedimiento para la purificación de biodiesel obtenido a partir de aceite de semilla de ricino, para el propósito de promover la eficiencia de la separación de la fracción de glicerina formada durante la reacción de trans-esterificación de una mezcla de triglicéridos de cadena larga derivados del petróleo en presencia de etanol y de un catalizador alcalino. Más específicamente, la presente invención se refiere a la aplicación de un método para la separación electrostática de la fracción de glicerina a los procesos convencionales para la producción industrial de biodiesel. La invención que ahora se propone, pretende resolver este problema reduciendo drásticamente el tiempo para separación de las fases. La solicitud de patente EP2349521 describe un coalescedor electrostático vertical que comprende una superficie de electrodo primera y segunda, y una superficie foraminosa dispuesta horizontalmente. La superficie de los electrodos primero y superficie foraminosa dispuesta horizontalmente, están al potencial de tierra. Las superficies de los electrodos primero y segundo comparten la misma orientación plana con respecto al eje central longitudinal de la embarcación. La disposición única de la embarcación y pares opuestos de superficies de los electrodos primero y segundo, proporcionan para un campo de tensión sustancialmente uniforme alrededor de un perímetro de la embarcación y un campo de tensión efectiva para la coalescencia dentro de un centro de una vasija. Un tubo distribuidor circular o en forma de una carcasa de distribución, sirve para absorber el impulso de la corriente de emulsión entrante y distribuir la corriente en un interior de la vasija. DESCRIPCION DETALLADA DE LA INVENCIÓN Patent document EP2332903 refers to a process for the purification of biodiesel obtained from castor seed oil, for the purpose of promoting the efficiency of the separation of the glycerin fraction formed during the trans-esterification reaction of a mixture of petroleum-derived long chain triglycerides in the presence of ethanol and an alkaline catalyst. More specifically, the present invention relates to the application of a method for electrostatic separation of the glycerin fraction to conventional processes for the industrial production of biodiesel. The invention now proposed is intended to solve this problem by drastically reducing the time for phase separation. Patent application EP2349521 describes a vertical electrostatic coalescer comprising a first and second electrode surface, and a horizontally arranged foraminous surface. The first electrode surface and horizontally arranged foraminous surface are at ground potential. The surfaces of the first and second electrodes share the same flat orientation with respect to the central longitudinal axis of the vessel. The unique arrangement of the vessel and opposite pairs of surfaces of the first and second electrodes provide for a substantially uniform voltage field around a perimeter of the vessel and an effective voltage field for coalescence within a center of a vessel. A circular distribution tube or in the form of a distribution housing, serves to absorb the impulse of the incoming emulsion current and distribute the current inside an vessel. DETAILED DESCRIPTION OF THE INVENTION

Los detalles característicos de la presente invención se muestran claramente en la siguiente descripción, figuras y ejemplos, que se acompañan, los cuales se incluyen a manera de un ejemplo ilustrativo, por lo que, no deben ser considerados como limitativos, para la presente invención. The characteristic details of the present invention are clearly shown in the following description, accompanying figures and examples, which are included by way of an illustrative example, and therefore should not be considered as limiting, for the present invention.

Breve descripción de las figuras: Brief description of the figures:

La figura 1 es una vista en perspectiva convencional del dispositivo decantador de una mezcla de biodiesel y glicerina, de la presente invención.Figure 1 is a conventional perspective view of the decanter device of a mixture of biodiesel and glycerin, of the present invention.

La figura 2 es un corte longitudinal lateral del dispositivo decantador de una mezcla de biodiesel y glicerina, en cuestión. Figure 2 is a side longitudinal section of the decanter device of a mixture of biodiesel and glycerin, in question.

La figura 3 es un corte longitudinal superior de dicho dispositivo decantador de una mezcla de biodiesel y glicerina. Figure 3 is an upper longitudinal section of said decanter device of a mixture of biodiesel and glycerin.

La figura 4 es una vista lateral del dispositivo decantador, de la presente invención. Figure 4 is a side view of the decanter device of the present invention.

La figura 5 es un corte longitudinal del dispositivo decantador, en comento. La figura 6 es una vista en perspectiva convencional de los componentes internos del dispositivo decantador de esta invención. Figure 5 is a longitudinal section of the decanter device, in comment. Figure 6 is a conventional perspective view of the internal components of the decanter device of this invention.

La figura 7 es un corte longitudinal de la figura 6, donde se aprecian unas perforaciones laterales.  Figure 7 is a longitudinal section of Figure 6, where side perforations are seen.

La figura 8 es diagrama esquemático del sistema integral para la decantación de una mezcla de biodiesel y glicerina, de la presente invención.Figure 8 is a schematic diagram of the integral system for the decantation of a mixture of biodiesel and glycerin, of the present invention.

Ejemplos Examples

Ejemplo 1. Modo preferente para la realización del dispositivo y un sistema, para decantar una mezcla de biodiesel con glicerina, de la presente invención. Example 1. Preferred mode for the realization of the device and a system, for decanting a mixture of biodiesel with glycerin, of the present invention.

En relación a las figuras antes mencionadas, el presente ejemplo describe una de las modalidades preferentes para la realización del dispositivo decantador para una mezcla de biodiesel y glicerina, de la presente invención, el cual comprende un tanque trapezoidal (1) dispuesto horizontalmente, con fondo en canal "V", el cual es dividido en dos secciones (I y II); donde la primera sección es atravesada longitudinalmente por un tubo recto (2), por donde se introduce la mezcla de biodiesel y glicerina. A lo largo del tubo se proveen orificios laterales (3), para minimizar el área de turbulencia. In relation to the aforementioned figures, the present example describes one of the preferred embodiments for the realization of the decanter device for a mixture of biodiesel and glycerin, of the present invention, which comprises a horizontally arranged bottom trapezoidal tank (1) in channel "V", which is divided into two sections (I and II); where the first section is crossed longitudinally by a straight tube (2), where the mixture of biodiesel and glycerin is introduced. Side holes (3) are provided along the tube, to minimize the area of turbulence.

En cada uno de los orificios laterales (3), del tubo de alimentación (2) se instala una placa inclinada (4), para favorecer la separación de las partículas por diferencia de densidad, obligando al flujo de mezcla que sale de esos orificios (3) a ascender y descender siguiendo la trayectoria que determina el ángulo de inclinación de tales placas (4). In each of the lateral holes (3), of the feeding tube (2) an inclined plate (4) is installed, to favor the separation of the particles by density difference, forcing the flow of mixture that leaves those holes ( 3) to ascend and descend following the path that determines the angle of inclination of such plates (4).

A lo largo del dispositivo decantador, se inserta al menos, un primer par de electrodos (5), a los que se les alimentará con un determinado voltaje, para que formen un campo eléctrico que acelerará la decantación de la glicerina. También se incluye un primer sensor de glicerina (S1). En esta primera sección del dispositivo decantador lograremos una separación del 90 % de la glicerina, con un tiempo de residencia de aproximadamente 1 minuto. En una segunda sección del aparato decantador, se provee un canal zigzagueante, el cual se conforma de un conjunto de placas verticales (6), para orientar el flujo de mezcla en trayectoria horizontal y dirección alternada, y así incrementar el tiempo de residencia del flujo de la mezcla. En la parte final de dicho canal zigzagueante, se coloca un segundo par de electrodos (7) conectados a una fuente de voltaje. Así también se integra un segundo sensor de glicerina (S2). Along the decanter device, at least one first pair of electrodes (5) is inserted, which will be fed with a certain voltage, so that they form an electric field that will accelerate the decantation of the glycerin. A first glycerin sensor (S1) is also included. In this first section of the decanter device we will achieve a 90% separation of the glycerin, with a residence time of approximately 1 minute. In a second section of the decanter apparatus, a zigzag channel is provided, which is formed by a set of vertical plates (6), to orient the flow of mixture in the horizontal path and alternate direction, and thus increase the residence time of the flow mix. In the final part of said zigzag channel, a second pair of electrodes (7) connected to a voltage source is placed. This also integrates a second glycerin sensor (S2).

En el extremo final, externamente, se proveen una válvula de control de salida para la glicina (A4), la cual deposita al glicerol en su respectivo contenedor (G) y una válvula de control para la salida del biodiesel puro (A3), la cual lo depositará en su contenedor de biodiesel puro (B2). At the end end, externally, an outlet control valve for glycine (A4) is provided, which deposits the glycerol in its respective container (G) and a control valve for the output of pure biodiesel (A3), the which will deposit it in its container of pure biodiesel (B2).

El consumo de corriente eléctrica de este segundo par de electrodos (7) será indicativo de que la separación de la glicerina se ha completado. El nivel de amperaje del último par de electrodos será utilizado para controlar el flujo de alimentación recibido por el decantador. The electrical current consumption of this second pair of electrodes (7) will be indicative that the glycerin separation has been completed. The amperage level of the last pair of electrodes will be used to control the feed flow received by the decanter.

Los electrodos tienen sus respectivas terminales aisladas (13) para que se conecten con sus respectivas fuentes múltiples variables de alimentación de corriente eléctrica de alto voltaje (8 y 9). The electrodes have their respective insulated terminals (13) so that multiple high voltage electric power supply variables (8 and 9) are connected to their respective sources.

Los sensores de glicerina (S1 y S2) se conectan a una unidad de procesamiento (11), para monitorear y controlar el grado de decantación o recuperación de glicerol; dicha unida de procesamiento (11) contiene: al menos un sensor de conductividad eléctrica, al menos un sensor de corriente eléctrica instalado en cada módulo de electrodos de alto voltaje, un indicador de conductividad, con lectura asociada al grado de decantación de glicerol. La unidad de procesamiento (11) es un dispositivo electrónico que recibe y procesa señales de los sensores, particularmente del sensor de glicerina (10), para tomar decisiones sobre el flujo de agua que debe inyectar al dispositivo decantador y el campo eléctrico que debe aplicar. La unidad de procesamiento (11) cuenta con un algoritmo de modelación multivariable que minimiza en tiempo real las impurezas de glicerina presentes en el flujo de biodiesel atravesando la válvula de glicerina (A4), en función de las características DC y AC del voltaje aplicado por las fuentes de poder y e lujo de agua inyectado al decantador. The glycerin sensors (S1 and S2) are connected to a processing unit (11), to monitor and control the degree of decantation or recovery of glycerol; said processing unit (11) contains: at least one electrical conductivity sensor, at least one electrical current sensor installed in each high voltage electrode module, a conductivity indicator, with reading associated with the degree of glycerol decantation. The processing unit (11) is an electronic device that receives and processes signals from the sensors, particularly the glycerin sensor (10), to make decisions about the flow of water to be injected into the decanter device and the electric field to be applied. . The processing unit (11) has a multivariable modeling algorithm that minimizes in real time the glycerin impurities present in the biodiesel flow through the glycerin valve (A4), depending on the DC and AC characteristics of the voltage applied by the sources of power and luxury of water injected into the decanter.

El dispositivo decantador tiene una fuente de biodiesel impuro (B1) y una fuente de agua (12), las cuales se conectan, por medio de tuberías, con el tubo de alimentación (2) de dicho dispositivo; y se provee de una válvula de control de la cantidad de biodiesel impuro (A1) y una válvula de control de la cantidad de agua (A2). The decanter device has a source of impure biodiesel (B1) and a source of water (12), which are connected, by means of pipes, to the supply tube (2) of said device; and it is provided with a control valve for the amount of impure biodiesel (A1) and a control valve for the amount of water (A2).

Por lo tanto, la presente invención, también provee un sistema para la decantación de una mezcla de biodiesel y glicerina, donde interviene el dispositivo decantador antes descrito. Por lo que dicho sistema se comprende el aparato decantador ya referenciado y todos los componentes externos, para llevar a cabo un proceso de decantación de una mezcla de biodiesel y glicerina. Therefore, the present invention also provides a system for the decantation of a mixture of biodiesel and glycerin, where the decanter device described above intervenes. Therefore, said system comprises the decanter apparatus already referenced and all external components, to carry out a process of decanting a mixture of biodiesel and glycerin.

En el caso de la mezcla glicerina-biodiesel la acción del campo eléctrico se debe al carácter polar de la molécula del glicerol. Estas moléculas forman dipolos que se orientan eléctricamente en la misma dirección, en presencia de un campo eléctrico continuo, atrayéndose entre sí; también las gotas pierden su esfericidad al deformarse por la acción del campo eléctrico, reducen su tensión superficial y se favorece el contacto entre ellas y por lo tanto su coalescencia. In the case of the glycerin-biodiesel mixture, the action of the electric field is due to the polar character of the glycerol molecule. These molecules form dipoles that are electrically oriented in the same direction, in the presence of a continuous electric field, attracting each other; also the drops lose their sphericity when deformed by the action of the electric field, reduce their surface tension and favor the contact between them and therefore their coalescence.

Cuando el campo eléctrico es producido por un voltaje alterno, la coalescencia se favorece porque las gotas suspendidas son agitadas por la variación del campo eléctrico, favoreciéndose el contacto entre ellas, resultando en una mayor coalescencia, resultando una mayor velocidad de decantación. When the electric field is produced by an alternating voltage, coalescence is favored because the suspended drops are agitated by the variation of the electric field, favoring the contact between them, resulting in a greater coalescence, resulting in a higher decantation rate.

Se ha demostrado experimentalmente que, bajo ciertas condiciones de voltaje, separación yometría de electrodos, la velocidad de decantación se incrementa drásticamente. It has been experimentally demonstrated that, under certain conditions of voltage, separation and electrode geometry, the decantation rate is dramatically increased.

Ejemplo 2. Funcionamiento y procedimiento, para la decantación de una mezcla de biodiesel y glicerina. Example 2. Operation and procedure, for the decantation of a mixture of biodiesel and glycerin.

El flujo que contiene la mezcla de glicerol y metilésteres de ácidos grasos ingresa al decantador descrito en el ejemplo 1 , por el tubo de alimentación (2) que distribuye este flujo mediante perforaciones múltiples (3) a lo largo del tubo de alimentación (2). The flow containing the mixture of glycerol and fatty acid methyl esters enters the decanter described in example 1, through the feed tube (2) that distributes this flow through multiple perforations (3) along the feed tube (2) .

Las placas inclinadas (4) orientan el flujo en trayectoria vertical, facilitando la decantación debida a la diferencia de densidades de los fluidos que componen la mezcla. El primer par de electrodos (5) genera un campo eléctrico en la primera sección del decantador. Este campo eléctrico acelera la decantación, pues estimula la coalescencia de las partículas de glicerina suspendidas en el biodiesel. The inclined plates (4) orient the flow in vertical path, facilitating the decantation due to the difference in densities of the fluids that make up the mixture. The first pair of electrodes (5) generates an electric field in the first section of the decanter. This electric field accelerates the decantation, as it stimulates the coalescence of the glycerin particles suspended in the biodiesel.

El glicerol fluye por la parte de abajo del decantador, cuyo fondo tiene una pendiente. Glycerol flows through the bottom of the decanter, whose bottom has a slope.

Los fluidos pasan a la segunda sección del decantador que consiste en una serie de placas verticales (6) que orientan el flujo en direcciones alternadas, con el fin de permitir un mayor tiempo de residencia con el que se logre una separación completa de los fluidos. En esta segunda sección, el campo eléctrico es provocado por el segundo par de electrodos (7). El consumo de corriente en cada sección del aparato, por parte de los electrodos, es monitoreado por la unidad de procesamiento (11), y es utilizado como referente del grado de separación de los fluidos. Así también, las válvulas de alimentación de mezcla, las de salida de glicerol y de biodiesel, situadas respectivamente en la parte inferior y superior de la segunda sección del decantador, son controladas por dicha unidad (11). The fluids pass to the second section of the decanter consisting of a series of vertical plates (6) that orient the flow in alternate directions, in order to allow a longer residence time with which a complete separation of the fluids is achieved. In this second section, the electric field is caused by the second pair of electrodes (7). The current consumption in each section of the apparatus, by the electrodes, is monitored by the processing unit (11), and is used as a reference for the degree of fluid separation. Also, the mixing feed valves, the glycerol and biodiesel outlet valves, located respectively in the lower and upper part of the second section of the decanter, are controlled by said unit (11).

No está por demás recalcar, que los ejemplos antes descritos, son una de las tantas modalidades para la realización de la presente invención, por lo tanto, todos aquellos cambios que pudieran hacérsele a la presente invención, quedan incluidos en el alcance de la misma, ya que dichos cambios, resultan obvios para una persona versada en la materia. It should not be emphasized, however, that the examples described above are one of the many modalities for the realization of the present invention, therefore, all those changes that could be made to the present invention are included in the scope thereof, since these changes are obvious to a person versed in the matter.

Claims

REIVINDICACIONES Un dispositivo decantador para una mezcla de biodiesel y glicerina, que comprende: un tanque trapezoidal (1) dispuesto horizontalmente, con fondo en canal "V", el cual es dividido en dos secciones; donde la primera sección es atravesada longitudinalmente por un tubo recto (2), por donde se introduce la mezcla de biodiesel y glicerina; a lo largo del tubo se proveen orificios laterales (3), de modo que el flujo de la mezcla ingresa al recipiente rectangular dividido, para minimizar el área de turbulencia; en cada uno de los orificios laterales (3), del tubo de alimentación (2) se instala una placa inclinada (4), para favorecer la separación de las partículas por diferencia de densidad, obligando al flujo que sale de esos orificios (3) a ascender y descender siguiendo la trayectoria que determina el ángulo de inclinación de tales placas (4); a lo largo del dispositivo decantador, se inserta al menos, un primer par de electrodos (5), a los que se les alimentará con un determinado voltaje, para que formen un campo eléctrico que acelerará la decantación de la glicerina; en una segunda sección del aparato decantador, se provee un canal zigzagueante, el cual se conforma de un conjunto de placas verticales (6), para orientar el flujo en trayectoria horizontal y dirección alternada; en la parte final de dicho canal zigzagueante, se coloca un segundo par de electrodos (7) conectados a una fuente de voltaje; un sensor de glicerina (S1 y S2) se coloca en cada una de las secciones, y en extremo opuesto, al extremo de entrada, del aparato decantador, se provee una válvula de salida de la glicerina (A4) y una válvula de salida de biodiesel (A3). A decanter device for a mixture of biodiesel and glycerin, which comprises: a trapezoidal tank (1) arranged horizontally, with a "V" channel bottom, which is divided into two sections; where the first section is crossed longitudinally by a straight tube (2), through which the biodiesel and glycerin mixture is introduced; Side holes (3) are provided along the tube, so that the mixture flow enters the divided rectangular container, to minimize the turbulence area; In each of the side holes (3) of the feed tube (2), an inclined plate (4) is installed to promote the separation of the particles due to the difference in density, forcing the flow to come out of those holes (3). to ascend and descend following the trajectory determined by the angle of inclination of said plates (4); Throughout the decanting device, at least a first pair of electrodes (5) is inserted, which will be fed with a certain voltage, so that they form an electric field that will accelerate the decantation of the glycerin; In a second section of the settling device, a zigzagging channel is provided, which is made up of a set of vertical plates (6), to guide the flow in a horizontal path and alternating direction; In the final part of said zigzag channel, a second pair of electrodes (7) connected to a voltage source is placed; A glycerin sensor (S1 and S2) is placed in each of the sections, and at the opposite end, to the inlet end, of the decanter apparatus, a glycerin outlet valve (A4) and a glycerin outlet valve are provided. biodiesel (A3). El dispositivo decantador de la anterior reivindicación, donde los electrodos tienen sus respectivas terminales aisladas (13) para que se conecten con sus respectivas fuentes múltiples variables de alimentación de corriente eléctrica de alto voltaje (8 y 9). Un sistema para la decantación de una mezcla de biodiesel y glicerina, que comprende: i) un dispositivo decantador de una mezcla de biodiesel y glicerina, como el descrito en las reivindicaciones anteriores; The decanter device of the previous claim, where the electrodes have their respective insulated terminals (13) so that they are connected with their respective multiple variable sources of high voltage electric current power (8 and 9). A system for decanting a mixture of biodiesel and glycerin, comprising: i) a decanting device for a mixture of biodiesel and glycerin, as described in the preceding claims; ii) una fuente de mezcla de biodiesel impuro (B1), la cual se conecta el tubo de alimentación (2) del dispositivo decantador; ii) a source of impure biodiesel mixture (B1), which is connected to the feed tube (2) of the decanter device; iii) una fuente de agua (12), la cual se conecta con el tubo de alimentación (2) del dispositivo; iii) a water source (12), which is connected to the feeding tube (2) of the device; iv) una válvula de control de la cantidad de biodiesel impuro (A1) se coloca en la tubería que conduce al tubo alimentador (2); iv) a valve to control the amount of impure biodiesel (A1) is placed in the pipe that leads to the feeder tube (2); v) una válvula de control de la cantidad de agua (A2) se provee en la conexión que conecta al tubo de alimentación (2); v) a water quantity control valve (A2) is provided in the connection that connects to the feed tube (2); vi) una unidad de procesamiento (11), para monitorear y controlar el grado de decantación o recuperación de glicerol; dicha unida de procesamiento contiene: al menos un sensor de conductividad eléctrica, al menos un sensor de corriente eléctrica instalado en cada módulo de electrodos de alto voltaje, un indicador de conductividad, con lectura asociada al grado de decantación de glicerol; y vi) a processing unit (11), to monitor and control the degree of decantation or recovery of glycerol; said processing unit contains: at least one electrical conductivity sensor, at least one electric current sensor installed in each high voltage electrode module, a conductivity indicator, with a reading associated with the degree of glycerol decantation; and vii) fuentes múltiples variables de alimentación de corriente eléctrica de alto voltaje (8 y 9), para alimentar a los electrodos; vii) multiple variable sources of high voltage electrical current supply (8 and 9), to feed the electrodes; viii) una válvula (A3) de control de la cantidad de biodiesel puro que sale del dispositivo, se provee en su respectiva salida; viii) a valve (A3) to control the amount of pure biodiesel that comes out of the device is provided at its respective outlet; ix) una válvula (A4) de control de la cantidad de glicerina y agua que salen del dispositivo, se proveen en su respectiva salida; ix) a valve (A4) to control the amount of glycerin and water coming out of the device, provided at its respective outlet; x) un contenedor de biodiesel puro (B2) se coloca al final de la tubería de salida, después de la válvula A3; y x) a container of pure biodiesel (B2) is placed at the end of the outlet pipe, after valve A3; and xi) un contenedor de glicerina y agua se provee al final de la tubería de salida, después de la válvula A4. xi) a container of glycerin and water is provided at the end of the outlet pipe, after valve A4. Un procedimiento para la decantación de una mezcla de biodiesel y glicerina, que comprende: ingresar una mezcla de glicerol y metilésteres de ácidos grasos ingresa a un dispositivo decantador, como el descrito en las reivindicaciones 1 y 2, por medio del tubo de alimentación A procedure for the decantation of a mixture of biodiesel and glycerin, which comprises: entering a mixture of glycerol and methyl esters of fatty acids enters a decanter device, such as the one described in claims 1 and 2, through the feed tube (2) que distribuye a la mezcla mediante perforaciones múltiples (2) which distributes to the mixture through multiple perforations (3) a lo largo del tubo de alimentación (2). (3) along the feed tube (2). orientar el flujo de la mezcla en trayectoria vertical, por medio de las placas inclinadas direct the flow of the mixture in a vertical path, by means of the inclined plates (4), facilitando la decantación debida a la diferencia de densidades de los fluidos que componen la mezcla; (4), facilitating decantation due to the difference in densities of the fluids that make up the mixture; aplicar un campo eléctrico en la primera sección del dispositivo, para acelerar la decantación y estimular la coalescencia de las partículas de glicerina suspendidas en el biodiesel; apply an electric field in the first section of the device, to accelerate the decantation and stimulate the coalescence of the glycerin particles suspended in the biodiesel; pasar los fluidos a la segunda sección del dispositivo decantador, donde se orienta el flujo de mezcla en direcciones alternadas, con el fin de permitir un mayor tiempo de residencia con el que se logre una separación completa de los fluidos; passing the fluids to the second section of the decanter device, where the mixture flow is oriented in alternating directions, in order to allow a longer residence time with which a complete separation of the fluids is achieved; provocar un campo eléctrico en esta segunda sección por el segundo par de electrodos (7); y causing an electric field in this second section by the second pair of electrodes (7); and recolectar el biodiesel purificado, y la glicerina y agua en recipientes separados. Collect the purified biodiesel, and the glycerin and water in separate containers. 5. El método de conformidad con la reivindicación anterior, donde en la primera sección del dispositivo decantador, se separa el 90 % de la glicerina, con un tiempo de residencia de aproximadamente 1 minuto. 5. The method according to the previous claim, wherein in the first section of the decanter device, 90% of the glycerin is separated, with a residence time of approximately 1 minute. 6. El método según las reivindicaciones 4 y 5, donde el consumo de corriente en cada sección del aparato, por parte de los electrodos, es monitoreado por una unidad de procesamiento (1 ), y es utilizado como referente del grado de separación de los fluidos; así también, las válvulas de alimentación de mezcla y agua, las de salida de glicerol y de biodiesel, son controladas por dicha unidad (11). 6. The method according to claims 4 and 5, where the current consumption in each section of the apparatus, by the electrodes, is monitored by a processing unit (1), and is used as a reference for the degree of separation of the electrodes. fluids; Likewise, the mixture and water supply valves, the glycerol and biodiesel outlet valves, are controlled by said unit (11).
PCT/MX2013/000012 2013-01-29 2013-01-29 Accelerated biodiesel electropurification Ceased WO2014119978A1 (en)

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CN104474743A (en) * 2014-12-04 2015-04-01 中国科学院广州能源研究所 Device for continuously separating biodiesel and glycerine
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