WO2007026032A1 - Chemical reactor for the supercritical alcoholysis of all types of fats and oils with different types of alcohols - Google Patents

Chemical reactor for the supercritical alcoholysis of all types of fats and oils with different types of alcohols Download PDF

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Publication number
WO2007026032A1
WO2007026032A1 PCT/ES2005/070126 ES2005070126W WO2007026032A1 WO 2007026032 A1 WO2007026032 A1 WO 2007026032A1 ES 2005070126 W ES2005070126 W ES 2005070126W WO 2007026032 A1 WO2007026032 A1 WO 2007026032A1
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WIPO (PCT)
Prior art keywords
oils
fats
types
alcohols
reactor
Prior art date
Application number
PCT/ES2005/070126
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Spanish (es)
French (fr)
Inventor
Mauro Ariel Knudsen
Original Assignee
Integral Bioenergies Systems, S.L.
Mersing Huusmann, Onildo Alfredo
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Publication date
Application filed by Integral Bioenergies Systems, S.L., Mersing Huusmann, Onildo Alfredo filed Critical Integral Bioenergies Systems, S.L.
Priority to PCT/ES2005/070126 priority Critical patent/WO2007026032A1/en
Publication of WO2007026032A1 publication Critical patent/WO2007026032A1/en

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B13/00—Recovery of fats, fatty oils or fatty acids from waste materials
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
    • B01J3/008—Processes carried out under supercritical conditions
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
    • B01J3/02—Feed or outlet devices therefor
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
    • B01J3/04—Pressure vessels, e.g. autoclaves
    • B01J3/042—Pressure vessels, e.g. autoclaves in the form of a tube
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11C—FATTY ACIDS FROM FATS, OILS OR WAXES; CANDLES; FATS, OILS OR FATTY ACIDS BY CHEMICAL MODIFICATION OF FATS, OILS, OR FATTY ACIDS OBTAINED THEREFROM
    • C11C3/00—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00051—Controlling the temperature
    • B01J2219/00074—Controlling the temperature by indirect heating or cooling employing heat exchange fluids
    • B01J2219/00087—Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements outside the reactor
    • B01J2219/00094—Jackets
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00051—Controlling the temperature
    • B01J2219/00074—Controlling the temperature by indirect heating or cooling employing heat exchange fluids
    • B01J2219/00105—Controlling the temperature by indirect heating or cooling employing heat exchange fluids part or all of the reactants being heated or cooled outside the reactor while recycling
    • B01J2219/00108—Controlling the temperature by indirect heating or cooling employing heat exchange fluids part or all of the reactants being heated or cooled outside the reactor while recycling involving reactant vapours
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00051—Controlling the temperature
    • B01J2219/00121—Controlling the temperature by direct heating or cooling
    • B01J2219/0013—Controlling the temperature by direct heating or cooling by condensation of reactants
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00051—Controlling the temperature
    • B01J2219/00132—Controlling the temperature using electric heating or cooling elements
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00051—Controlling the temperature
    • B01J2219/00132—Controlling the temperature using electric heating or cooling elements
    • B01J2219/00135—Electric resistance heaters
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00051—Controlling the temperature
    • B01J2219/00159—Controlling the temperature controlling multiple zones along the direction of flow, e.g. pre-heating and after-cooling
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00182—Controlling or regulating processes controlling the level of reactants in the reactor vessel
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00761—Details of the reactor
    • B01J2219/00763—Baffles
    • B01J2219/00765—Baffles attached to the reactor wall
    • B01J2219/00777—Baffles attached to the reactor wall horizontal
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/50—Improvements relating to the production of bulk chemicals
    • Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00—Technologies for solid waste management
    • Y02W30/50—Reuse, recycling or recovery technologies
    • Y02W30/74—Recovery of fats, fatty oils, fatty acids or other fatty substances, e.g. lanolin or waxes

Definitions

  • the present invention consists of a chemical reactor in which the alcoholysis of all types of oils and fats is produced in an efficient way, and different types of alcohols can be used for this.
  • the object of the present invention is a reactor suitable for the physical and chemical transformation of all types of oils and fats in esters, in which light alcohols are used, without requiring the presence of chemical catalysts, in which glycerins are obtained in different concentrations as a by-product of the reaction.
  • Oils and fats in general are known as triglycerides, and have a structure in which three fatty acids (esters) are linked to a glyceride (heavy alcohol).
  • the transesterification of these molecules means breaking their primary structure, separating glycerol from the three fatty acids, and these fatty acids, in turn, bind with a lighter alcohol.
  • esters These fatty acids bound with light alcohols are called esters and have a wide range of uses. STATE OF THE ART
  • Reactors for acid esterification using acid catalysts Reactors for biological transesterification using biological agents such as enzymes applied together with different solvents.
  • Acid-base processes which consists of a partial acid esterification of the free fatty acids existing in the raw material and a subsequent basic transesterification that acts on the remaining triglycerides;
  • - Processes under the aqueous method which uses a saturated solution of water-basic catalyst to increase the speed of obtaining methoxides to subsequently transesterify in alkaline form.
  • Good conversion rates can be achieved with basic catalysis production chemical reactors when virgin oils or fats are available, achieving conversion rates of up to 98%.
  • Oil or fat preparation can be by means of acid esterification or by saponification of free fatty acids and their subsequent separation; - Transesterification by any of the aforementioned methods;
  • esters and glycerins There are two major technical problems to be solved in the production of esters and glycerins, which are: - Simplification of the processing of oils with a high amount of free fatty acids (acidity) in the different oils, which destroy the alkaline catalyst and require a greater quantity. of processes and supplies; such as acid esterification and biological transesterification. This translates into plants with a greater number of processes and facilities, and consequently higher production costs.
  • a subject of the present invention is a chemical reactor that carries out a process by which the use of catalysts is unnecessary by means of supercritical alcoholysis, which produces a large change in the physicochemical variables of the alcohol used in the reaction.
  • the chemical reactor proposed for supercritical alcoholysis subjects the two main components of the chemical reaction, fatty acids (oils and fats of any type) and alcohol, to extreme pressure and temperature conditions, or supercritical conditions for alcohol used. Therefore, the two problems mentioned above are solved thereby:
  • the reactor has the following advantages: High speed, since the reaction time in the process carried out in this reactor is about 20 minutes, compared to the 90 minutes required in the aforementioned conventional processes, Greater simplicity of operation, since only two inputs are involved liquids,
  • a chemical reactor for supercritical alcoholysis of all types of fats and oils with various types of alcohols comprising: at least one oil supply tank 1 to be treated; at least one tank 7 for supplying a light alcohol; supply lines for oil or fat to be treated 5 and light alcohol 8; at least one oil or grease feed pump 6; - at least one light alcohol feed pump 9; at least one tubular reaction vessel 11; at least one tank or lung for depressurizing the effluents 14; heat exchangers 2 and 4 of effluents and tributaries; a heating medium for tributaries 10 and 12; - flow regulating valves 13;
  • the injection pumps are located in the initial part of the reactor in the direction of the tributaries.
  • the oil injector pump (6) receives the raw material from the heat exchangers (2 and 4) in countercurrent, which heats the oil and cools the reaction products.
  • Both fats or oils and alcohols are injected directly into the reactor at the same time; by means of the heating means (10) the tributaries are heated and by means of the pumping means the pressure is raised to a supercritical point.
  • an oil tank (1) is observed in the figure, said oil being the main tributary and product that we must process.
  • the oil through supply lines (3 and 5) to an oil supply pump (6).
  • a tank (7) of a light alcohol methyl, ethyl, propyl, butyric alcohol (7), said alcohol being the one that has to react with each of the esters or fatty acids that make up the oils , to form light chains.
  • the alcohol is led through the corresponding supply line 8 to the alcohol supply pump 9.
  • the reaction occurs within the tubes of the reactor 11.
  • the temperature is maintained by heating means 12 distributed along the tubes of the reactor.
  • heat exchangers 2 and 4 are placed, preferably in countercurrent, so that the oil, and possibly also the alcohol, take part of the heat that the effluents have.
  • the disintegration reaction of the triglycerides and the combination of the resulting esters with the supplied light alcohol takes place in a chemical reactor, where conditions of pressure and temperature high enough to make the reaction under these conditions occur spontaneously, varying the pressure and temperature values respectively depending on the composition of the oils used and the type of alcohol used.
  • the products are then passed through exchanger 2 to finish cooling the mixture and then the esters and glycerin can be separated by decantation in a separate container and evacuated by means of an outlet line 15.
  • the new catalyst-free alcoholysis technology has fewer processing stages, does not require the provision of steam and boilers, processing times are much shorter; and thanks to these advantages, it is possible that plants are very compact (they can fit whole in a 20 'or 40' container) and with a capacity many times less, they are also economically viable, just like an industrial plant. In this way, small plants can be installed for individual producers, thus avoiding all the logistics of collecting and transporting oils to an industrial plant. The same happens with production, which if it is small can be consumed in its entirety in one place, avoiding all the logistics of fuel distribution. We believe that this is an important factor since additional costs in the raw material and fuel are avoided, as well as additional consumption of fuels and energy.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • General Chemical & Material Sciences (AREA)
  • Liquid Carbonaceous Fuels (AREA)
  • Fats And Perfumes (AREA)

Abstract

The invention relates to a chemical reactor for the supercritical alcoholysis of all types of fats and oils with different types of alcohols. The inventive reactor comprises: a container (1) for storing the oil to be treated, a container (7) for supplying a light alcohol, lines (5, 8) for supplying influents, supply pumps (6, 9), a depressurisation container (14), heat exchangers (2, 4) for optimal use of the energy, means (10, 12) for heating the influents, a tubular reaction container (11) and flow-control valves (13).

Description

REACTOR QUÍMICO PARA LA ALCOHOLISIS SUPERCRITICA DE TODO TIPO DE GRASAS Y ACEITES CON DISTINTOS TIPOS DE ALCOHOLES.CHEMICAL REACTOR FOR SUPERCRITICAL ALCOHOLISIS OF ALL KINDS OF FATS AND OILS WITH DIFFERENT TYPES OF ALCOHOLS.
Consiste la presente invención en un reactor químico en el que se produce de un modo eficaz la alcoholisis de todo tipo de aceites y grasas, pudiendo emplear para ello distintos tipos de alcoholes.The present invention consists of a chemical reactor in which the alcoholysis of all types of oils and fats is produced in an efficient way, and different types of alcohols can be used for this.
SECTOR TÉCNICO La presente invención tiene por objeto un reactor apto para la transformación física y química de todo tipo de aceites y grasas en esteres, en el que se utilizan alcoholes ligeros, sin requerir la presencia de catalizadores químicos, en el que se obtienen glicerinas en distintas concentraciones como subproducto de la reacción.TECHNICAL SECTOR The object of the present invention is a reactor suitable for the physical and chemical transformation of all types of oils and fats in esters, in which light alcohols are used, without requiring the presence of chemical catalysts, in which glycerins are obtained in different concentrations as a by-product of the reaction.
ANTECEDENTESBACKGROUND
Los aceites y grasas en general son conocidos como triglicéridos, y poseen una estructura en la que se enlazan tres ácidos grasos (esteres) a un glicérido (alcohol pesado). La transesterificación de éstas moléculas significa romper su estructura primaria, separando el glicerol de los tres ácidos grasos, y a su vez, estos ácidos grasos se enlacen con un alcohol más ligero.Oils and fats in general are known as triglycerides, and have a structure in which three fatty acids (esters) are linked to a glyceride (heavy alcohol). The transesterification of these molecules means breaking their primary structure, separating glycerol from the three fatty acids, and these fatty acids, in turn, bind with a lighter alcohol.
Éstos ácidos grasos enlazados con alcoholes ligeros se denominan esteres y poseen una amplia gama de utilidades. ESTADO DE LA TÉCNICAThese fatty acids bound with light alcohols are called esters and have a wide range of uses. STATE OF THE ART
Actualmente los reactores químicos existentes son capaces de llevar a cabo el proceso de forma continua o discontinua, mediante tres técnicas conocidas para lograr esta transformación:Currently the existing chemical reactors are capable of carrying out the process continuously or discontinuously, using three known techniques to achieve this transformation:
Reactores para transesterificación básica que utilizan catalizadores alcalinosReactors for basic transesterification using alkaline catalysts
Reactores para esterificación acida que utilizan catalizadores ácidos, Reactores para transesterificación biológica que utilizan agentes biológicos como por ejemplo enzimas aplicadas conjuntamente con distintos solventes.Reactors for acid esterification using acid catalysts, Reactors for biological transesterification using biological agents such as enzymes applied together with different solvents.
Existen además otros procesos industriales que modifican o complementan dos o más tipos de reactores distintos para obtener mayores conversiones, menores costes o mayor flexibilidad en los procesos, como por ejemplo: - Procesos de dos etapas básicas;There are also other industrial processes that modify or complement two or more different types of reactors to obtain higher conversions, lower costs or greater flexibility in the processes, such as: - Basic two-stage processes;
Procesos ácido-base, que consiste en una esterificación acida parcial de los ácidos grasos libres existentes en la materia prima y una transesterificación básica posterior que actúa sobre los triglicéridos restantes; - Procesos bajo el método acuoso, que utiliza una solución saturada de agua-catalizador básico para aumentar la velocidad de obtención de metóxidos para posteriormente transesterificar en forma alcalina. Con los reactores químicos de producción por catálisis básica se pueden lograr buenos porcentajes de conversión cuando se cuenta con aceites o grasas vírgenes, logrando tasas de hasta el 98% de conversión. Cuando se trabaja en el reciclado de grasas o aceites usados o con alto porcentaje de acidez, las pérdidas pueden ser de hasta un 40%, dada la gran cantidad de ácidos grasos libres que destruyen el catalizador formando jabones (que es un contaminante en el producto final de la reacción), y que como resultado detienen la reacción. Para estos casos la utilización del proceso industrial ácido-base puede ser una ayuda que tienda a reducir las pérdidas. Sin embargo, ello requiere el aumento de los procesos, el valor de los equipamientos y en consecuencia de los costes de producción. Por otro lado, se debe tener en cuenta que cuanta más cantidad de catalizadores se utilicen, más contaminados resultarán los esteres y en mayor medida la glicerina, con lo que las labores de limpieza y refino de los productos obtenidos serán más complicadas y más costosas.Acid-base processes, which consists of a partial acid esterification of the free fatty acids existing in the raw material and a subsequent basic transesterification that acts on the remaining triglycerides; - Processes under the aqueous method, which uses a saturated solution of water-basic catalyst to increase the speed of obtaining methoxides to subsequently transesterify in alkaline form. Good conversion rates can be achieved with basic catalysis production chemical reactors when virgin oils or fats are available, achieving conversion rates of up to 98%. When working on the recycling of fats or oils used or with a high percentage of acidity, the losses can be up to 40%, given the large amount of free fatty acids that destroy the catalyst forming soaps (which is a contaminant in the product end of the reaction), and as a result stop the reaction. In these cases the use of the acid-base industrial process can be an aid that tends to reduce losses. However, this requires an increase in processes, the value of equipment and, consequently, production costs. On the other hand, it should be borne in mind that the more catalysts used, the more contaminated the esters will be and to a greater extent the glycerin, with which the cleaning and refining tasks of the products obtained will be more complicated and more expensive.
Por lo tanto, las plantas químicas que logran una buena calidad del producto terminan siendo muy complejas por ser necesario incluir los siguientes procesos:Therefore, chemical plants that achieve good product quality end up being very complex due to the need to include the following processes:
Preparación del aceite o grasa; ello puede ser por medio de esterificación acida o por saponificación de los ácidos grasos libres y su posterior separación; - Transesterificación por cualquiera de los métodos antes citados;Oil or fat preparation; this can be by means of acid esterification or by saponification of free fatty acids and their subsequent separation; - Transesterification by any of the aforementioned methods;
Recuperación del alcohol sobrante;Recovery of excess alcohol;
Separación de la glicerina y otras sub-etapas de concentración;Glycerin separation and other concentration sub-stages;
Destilación de la glicerina; Lavados del éster, con posible producción de efluentes; Secado del éster.Glycerin distillation; Ester washes, with possible production of effluents; Drying of the ester.
Se presentan dos grandes problemas técnicos a solucionar en la producción de esteres y glicerinas, cuales son: - Simplificación del procesamiento de los aceites con alta cantidad de ácidos grasos libres (acidez) en los diferentes aceites, que destruyen el catalizador alcalino y requieren mayor cantidad de procesos e insumos; tales como esterificación acida y la transesterificación biológica. Esto se traduce en plantas con mayor cantidad de procesos e instalaciones, y en consecuencia mayores costes de producción.There are two major technical problems to be solved in the production of esters and glycerins, which are: - Simplification of the processing of oils with a high amount of free fatty acids (acidity) in the different oils, which destroy the alkaline catalyst and require a greater quantity. of processes and supplies; such as acid esterification and biological transesterification. This translates into plants with a greater number of processes and facilities, and consequently higher production costs.
Eliminación de la utilización de todo tipo de catalizadores que aumenten drásticamente la contaminación del éster y las glicerinas, no solo por su propia existencia en la reacción sino también por los productos indeseables que se obtienen, por ejemplo jabones.Elimination of the use of all kinds of catalysts that drastically increase the contamination of the ester and glycerins, not only due to their own existence in the reaction but also due to the undesirable products that are obtained, for example soaps.
OBJETO DE LA INVENCIÓNOBJECT OF THE INVENTION
La presente invención tiene por objeto un reactor químico que lleva a cabo un proceso por el cual se hace innecesario el uso de catalizadores mediante la alcoholisis supercrítica que produce una modificación de gran magnitud en las variables físico- químicas del alcohol utilizado en la reacción.A subject of the present invention is a chemical reactor that carries out a process by which the use of catalysts is unnecessary by means of supercritical alcoholysis, which produces a large change in the physicochemical variables of the alcohol used in the reaction.
A diferencia de los reactores químicos y procesos industriales anteriormente descritos que trabajan bajo un estado subcrítico del alcohol utilizado, es decir, en condiciones de presión y temperatura en las que cada elemento mantiene sus propiedades físico- químicas similares a las que tienen a temperatura y presión ambientales (200C, 1 bar), el reactor que se propone trabaja en condiciones en las que las propiedades y reactividad son muy diferentes.Unlike the chemical reactors and industrial processes previously described that work under a subcritical state of the alcohol used, that is, in conditions of pressure and temperature in which each element maintains its physicochemical properties similar to those at ambient temperature and pressure (20 0 C, 1 bar), the proposed reactor works under conditions in which the properties and reactivity are very different.
El reactor químico que se propone para la alcoholisis supercrítica somete a los dos componentes principales de la reacción química, los ácidos grasos (aceites y grasas de cualquier tipo) y al alcohol, a condiciones extremas de presión y temperatura, o condiciones supercríticas para el alcohol utilizado. Por lo tanto, se solucionan con ello los dos problemas citados anteriormente:The chemical reactor proposed for supercritical alcoholysis subjects the two main components of the chemical reaction, fatty acids (oils and fats of any type) and alcohol, to extreme pressure and temperature conditions, or supercritical conditions for alcohol used. Therefore, the two problems mentioned above are solved thereby:
En este estado no es necesaria la aplicación de catalizadores de ningún tipo, y además ocurre una conversión espontánea y total de todos los ácidos grasos libres a esteres (que con los sistema tradicionales planteaban problemas), así como de los ácidos grasos comunes, es decir, los triglicéridos.In this state the application of catalysts of any kind is not necessary, and in addition a spontaneous and total conversion of all free fatty acids to esters (which with traditional systems posed problems), as well as common fatty acids, that is to say , triglycerides.
Al no utilizarse catalizadores, no se contaminan los productos obtenidos ni se obtienen subproductos indeseados, tales como jabones. El proceso de refino de ambos productos es mucho más simple, ya que solo requiere una separación física de los esteres de la glicerina, y por destilación se separa el alcohol excedente de la reacción de los dos primeros productos. Además, el reactor presenta las siguientes ventajas: Alta velocidad, ya que el tiempo de reacción en el proceso llevado a cabo en este reactor es de unos 20 minutos, frente a los 90 minutos que se requiere en los procesos convencionales antedichos, Mayor simplicidad de operación, ya que tan solo intervienen dos insumos líquidos,By not using catalysts, the products obtained are not contaminated nor are unwanted by-products obtained, such as soaps. The refining process of both products is much simpler, since it only requires a physical separation of the esters of the glycerin, and by distillation the excess alcohol from the reaction of the first two products is separated. Furthermore, the reactor has the following advantages: High speed, since the reaction time in the process carried out in this reactor is about 20 minutes, compared to the 90 minutes required in the aforementioned conventional processes, Greater simplicity of operation, since only two inputs are involved liquids,
Menor tamaño de los equipos; debido a que es mayor el volumen procesado por unidad de tiempo, entonces es posible procesar un volumen igual con un equipo menor, Alta calidad y concentración de los productos obtenidos, - Menores costes de proceso por la utilización de menor cantidad de insumos y procesos,Smaller team sizes; Because the volume processed per unit of time is greater, then it is possible to process an equal volume with less equipment, High quality and concentration of the products obtained, - Lower process costs due to the use of fewer inputs and processes,
Menor cantidad de procesos involucrados y menor infraestructura necesaria,Fewer processes involved and less infrastructure needed,
Puede funcionar en modo continuo o discontinuo.It can work in continuous or discontinuous mode.
BREVE DESCRIPCIÓN DE LOS DIBUJOSBRIEF DESCRIPTION OF THE DRAWINGS
Con objeto de ilustrar la explicación que va a seguir, se adjunta una hoja de dibujos, que en una única figura representa la esencia de la presente invención, y que representa el esquema de un reactor.In order to illustrate the explanation that will follow, a sheet of drawings is attached, which in a single figure represents the essence of the present invention, and which represents the scheme of a reactor.
DESCRIPCIÓN DETALLADA DE LA INVENCIÓNDETAILED DESCRIPTION OF THE INVENTION
Se propone, por tanto, un reactor químico para la alcoholisis supercrítica de todo tipo de grasas y aceites con varios tipos de alcoholes, que comprende: al menos un depósito 1 de alimentación de aceite a tratar ; al menos un depósito 7 de suministro de un alcohol ligero; líneas de alimentación del aceite o grasa a tratar 5 y del alcohol ligero 8; al menos una bomba de alimentación del aceite o grasa 6; - al menos una bomba de alimentación del alcohol ligero 9; al menos un recipiente tubular de reacción 11 ; al menos un depósito o pulmón de despresurización de los efluentes 14; intercambiadores de calor 2 y 4 de los efluentes y los afluentes; un medio calefactor de los afluentes 10 y 12; - válvulas reguladoras de caudal 13;Therefore, a chemical reactor for supercritical alcoholysis of all types of fats and oils with various types of alcohols is proposed, comprising: at least one oil supply tank 1 to be treated; at least one tank 7 for supplying a light alcohol; supply lines for oil or fat to be treated 5 and light alcohol 8; at least one oil or grease feed pump 6; - at least one light alcohol feed pump 9; at least one tubular reaction vessel 11; at least one tank or lung for depressurizing the effluents 14; heat exchangers 2 and 4 of effluents and tributaries; a heating medium for tributaries 10 and 12; - flow regulating valves 13;
En este reactor las bombas inyectoras se encuentran en la parte inicial del reactor en el sentido de los afluentes. La bomba inyectora de aceite (6) recibe la materia prima desde los intercambiadores de calor (2 y 4) en contracorriente, que calienta el aceite y enfría los productos de la reacción.In this reactor the injection pumps are located in the initial part of the reactor in the direction of the tributaries. The oil injector pump (6) receives the raw material from the heat exchangers (2 and 4) in countercurrent, which heats the oil and cools the reaction products.
Tanto las grasas o aceites como los alcoholes son inyectados al mismo tiempo directamente en el reactor; mediante los medios calefactores (10) se calientan los afluentes y mediante los medios de bombeo se eleva la presión hasta un punto supercrítico.Both fats or oils and alcohols are injected directly into the reactor at the same time; by means of the heating means (10) the tributaries are heated and by means of the pumping means the pressure is raised to a supercritical point.
Conforme a la invención, se observa en la figura un depósito de aceite (1) siendo dicho aceite el afluente principal y producto que debemos procesar. El aceite por medio de unas líneas de alimentación (3 y 5) hasta una bomba (6) de alimentación de aceite. Por otra parte, se dispone un depósito (7) de un alcohol ligero (alcohol metílico, etílico, propílico, butírico...), siendo dicho alcohol el que ha de reaccionar con cada uno de los esteres o ácidos grasos que componen los aceites, para formar cadenas ligeras. El alcohol es conducido a través de la correspondiente línea de alimentación 8 hasta la bomba de alimentación de alcohol 9.According to the invention, an oil tank (1) is observed in the figure, said oil being the main tributary and product that we must process. The oil through supply lines (3 and 5) to an oil supply pump (6). On the other hand, there is a tank (7) of a light alcohol (methyl, ethyl, propyl, butyric alcohol ...), said alcohol being the one that has to react with each of the esters or fatty acids that make up the oils , to form light chains. The alcohol is led through the corresponding supply line 8 to the alcohol supply pump 9.
Una vez que los aceites o grasas y el alcohol ligero poseen la temperatura y presión adecuada, ocurre la reacción dentro de los tubos del reactor 11. En esta etapa la se mantiene la temperatura por medios de calefacción 12 distribuidos a lo largo de los tubos del reactor. Por cuanto se deben alcanzar unas condiciones de presión y temperatura elevadas, y por cuanto los efluentes salen calientes del reactor, se colocan intercambiadores de calor 2 y 4, preferentemente en contracorriente, de modo que el aceite, y posiblemente también el alcohol, tomen parte del calor que tienen los efluentes. La reacción de disgregación de los triglicéridos y la combinación de los esteres resultantes con el alcohol ligero suministrado tiene lugar en un reactor químico, en el que se dan condiciones de presión y temperatura suficientemente elevadas para hacer que la reacción en esas condiciones sea espontánea, variando los valores de presión y de temperatura respectivamente en función de la composición de los aceites empleados y del tipo de alcohol utilizado.Once the oils or fats and light alcohol have the appropriate temperature and pressure, the reaction occurs within the tubes of the reactor 11. In this stage, the temperature is maintained by heating means 12 distributed along the tubes of the reactor. As high pressure and temperature conditions must be reached, and as the effluents leave the reactor hot, heat exchangers 2 and 4 are placed, preferably in countercurrent, so that the oil, and possibly also the alcohol, take part of the heat that the effluents have. The disintegration reaction of the triglycerides and the combination of the resulting esters with the supplied light alcohol takes place in a chemical reactor, where conditions of pressure and temperature high enough to make the reaction under these conditions occur spontaneously, varying the pressure and temperature values respectively depending on the composition of the oils used and the type of alcohol used.
Una vez los productos obtenidos a alta presión y temperatura son enfriados mediante el intercambio de calor en los correspondientes intercambiadores de calor 4, los efluentes se conducen a un pulmón 14 de despresurización, donde se separa por destilación el alcohol excedente de la reacción (vaporización o flashing), cuyos vapor deberían condensarse y podrían ser reciclados en el depósito 7 de un alcohol ligero, no estando representado el correspondiente equipamientoOnce the products obtained at high pressure and temperature are cooled by means of heat exchange in the corresponding heat exchangers 4, the effluents are led to a depressurization chamber 14, where the excess alcohol from the reaction is distilled off (vaporization or flashing), whose steam should condense and could be recycled in tank 7 of a light alcohol, the corresponding equipment not being represented
Después pasan los productos por el intercambiador 2 para terminar de enfriar la mezcla y luego pueden separarse por decantación los esteres y la glicerina en un recipiente aparte y ser evacuados por medio de una línea de salida 15.The products are then passed through exchanger 2 to finish cooling the mixture and then the esters and glycerin can be separated by decantation in a separate container and evacuated by means of an outlet line 15.
Mediante el uso de este reactor se obtienen las siguientes ventajas: Medio Ambiente: Los procesos convencionales que utilizan catalizadores, inevitablemente generan distintos efluentes; debido a que para eliminar las trazas de catalizador residual y jabones que se forman en la reacción de transesterificación, generalmente se eliminan mediante un proceso neutralización con ácidos débiles (como ácido fosfórico al 85%) y agua que es la encargada de arrastrar los mencionados contaminantes, como así también monoglicéridos, diglicéridos y trazas de metanol residual. En el proceso libre de catalizadores propuesto, los 2 primeros contaminantes no existen ya que no se utiliza catalizador y por tanto no se forman jabones, con lo que se evita el consumo de agua y la generación de efluentes líquidos secundarios indeseados; y en el caso de que quedaran trazas de monoglicéridos, diglicéridos y metanol; estos se eliminan con un filtro de Sílica GeI que atrapa esos contaminantes del combustible obtenido, tras su separación de la glicerina y antes de ir al tanque de almacenaje. Estos filtros de Sílica GeI se pueden regenerar indefinidamente mediante la utilización de calor (2600C) por lo tanto, tampoco generan ningún tipo de efluente. Logística y transporte:By using this reactor the following advantages are obtained: Environment: Conventional processes that use catalysts inevitably generate different effluents; Because to eliminate traces of residual catalyst and soaps that form in the transesterification reaction, they are generally eliminated by means of a neutralization process with weak acids (such as 85% phosphoric acid) and water, which is responsible for entraining the aforementioned contaminants. , as well as monoglycerides, diglycerides and traces of residual methanol. In the proposed catalyst-free process, the first 2 contaminants do not exist since no catalyst is used and therefore no soaps are formed, thereby avoiding the consumption of water and the generation of unwanted secondary liquid effluents; and in the event that traces of monoglycerides, diglycerides and methanol remain; These are removed with a Silica GeI filter that traps these contaminants from the fuel obtained, after separating them from glycerin and before going to the storage tank. These Silica GeI filters can be regenerated indefinitely by using heat (260 0 C) therefore, they do not generate any type of effluent either. Logistics and Transportation:
La nueva tecnología de alcoholisis libre de catalizadores, posee menos etapas de procesamiento, no requiere de provisión de vapor y calderas, los tiempos de procesamiento son mucho menores; y gracias a estas ventajas es posible que plantas sean muy compactas (caben enteras dentro de un container de 20' o 40') y de una capacidad muchas veces menor, también sean viables económicamente, al igual que una planta industrial. De esta manera se pueden instalar plantas pequeñas para productores individuales, evitando así toda la logística de recogida y transportes de aceites hacia una planta industrial. Lo mismo ocurre con la producción, que si es pequeña puede ser consumida en su totalidad en un solo lugar, evitando toda la logística de distribución del combustible. Creemos que este es un factor importante ya que se evitan costos adicionales en la materia prima y el combustible, como así también consumos adicionales de combustibles y energía.The new catalyst-free alcoholysis technology, has fewer processing stages, does not require the provision of steam and boilers, processing times are much shorter; and thanks to these advantages, it is possible that plants are very compact (they can fit whole in a 20 'or 40' container) and with a capacity many times less, they are also economically viable, just like an industrial plant. In this way, small plants can be installed for individual producers, thus avoiding all the logistics of collecting and transporting oils to an industrial plant. The same happens with production, which if it is small can be consumed in its entirety in one place, avoiding all the logistics of fuel distribution. We believe that this is an important factor since additional costs in the raw material and fuel are avoided, as well as additional consumption of fuels and energy.
Es de aplicación en la fabricación de reactores para el tratamiento de aceites residuales. It is applicable in the manufacture of reactors for the treatment of residual oils.

Claims

REIVINDICACIONES
1.- Reactor químico para la alcoholisis supercrítica de todo tipo de grasas y aceites con varios tipos de alcoholes, caracterizado por comprender: - al menos un depósito de alimentación de aceite a tratar (1); al menos un depósito de suministro de un alcohol ligero (7); líneas de alimentación del aceite o grasa a tratar (5) y del alcohol ligero1.- Chemical reactor for supercritical alcoholysis of all types of fats and oils with various types of alcohols, characterized by comprising: - at least one oil supply tank to be treated (1); at least one tank for supplying a light alcohol (7); supply lines for oil or fat to be treated (5) and light alcohol
(8); al menos una bomba de alimentación del aceite o grasa (6); - al menos una bomba de alimentación del alcohol ligero (9); al menos un recipiente tubular de reacción (11); al menos un depósito o pulmón de despresurización de los efluentes (14); intercambiadores de calor de los efluentes y los afluentes (2,4); un medio calefactor de los afluentes (10,12); - válvulas reguladoras de caudal (13); siendo las bombas inyectoras la parte inicial del reactor en el sentido de los afluentes, recibiendo la bomba inyectora de aceite la materia prima desde los intercambiadores de calor (2 y 4) en contracorriente, que calienta el aceite y enfría los productos de la reacción; tanto las grasas o aceites como los alcoholes son inyectados al mismo tiempo directamente en el reactor; mediante los medios calefactores (10,12) se calientan los afluentes y mediante los medios de bombeo se eleva la presión hasta un punto supercrítico. (8); at least one oil or grease feed pump (6); - at least one light alcohol feeding pump (9); at least one tubular reaction vessel (11); at least one tank or lung for depressurizing the effluents (14); effluent and tributary heat exchangers (2,4); a tributary heating medium (10,12); - flow regulating valves (13); the injector pumps being the initial part of the reactor in the direction of the tributaries, the oil injector pump receiving the raw material from the counter-current heat exchangers (2 and 4), which heats the oil and cools the reaction products; both fats or oils and alcohols are injected directly into the reactor at the same time; By means of the heating means (10, 12) the tributaries are heated and by means of the pumping means the pressure is raised to a supercritical point.
2.- Reactor químico para la alcoholisis supercrítica de todo tipo de grasas y aceites con varios tipos de alcoholes, según la reivindicación 1, caracterizado porque el reactor (11) está conectado al intercambiador de calor (4) que enfría los esteres y glicerina obtenidos, enfriando dicho intercambiador los productos a una temperatura subcrítica del alcohol utilizado, estando el intercambiador conectado directamente a la válvula reguladora de caudal (13) que despresuriza los productos de la reacción dentro del pulmón de despresurización (14), donde los productos obtenidos, esteres y glicerina, son sometidos a una presión subcrítica, y pueden ser separados.2.- Chemical reactor for supercritical alcoholysis of all types of fats and oils with various types of alcohols, according to claim 1, characterized in that the reactor (11) is connected to the heat exchanger (4) that cools the esters and glycerin obtained , said exchanger cooling the products to a subcritical temperature of the alcohol used, the exchanger being directly connected to the flow regulating valve (13) that depressurizes the reaction products inside the depressurization lung (14), where the obtained products, esters and glycerin, are subjected to subcritical pressure, and can be separated.
3.- Reactor químico para la alcoholisis supercrítica de todo tipo de grasas y aceites con varios tipos de alcoholes, según cualquiera de las reivindicaciones 1 y 2, caracterizado por comprender además de una línea de recuperación de vapores que se obtienen al despresurizar la mezcla a una temperatura superior a la de ebullición del alcohol utilizado; que son enfriados y condensados para reciclarse en el depósito (7) del alcohol ligero; eEl calor aportado por este vapor en su condensación también puede ser aprovechado en calentamiento de los afluentes. 3.- Chemical reactor for the supercritical alcoholysis of all types of fats and oils with various types of alcohols, according to any of claims 1 and 2, characterized in that it also comprises a vapor recovery line that is obtained by depressurizing the mixture at a temperature higher than the boiling point of the alcohol used; which are cooled and condensed for recycling in the light alcohol tank (7); eThe heat contributed by this steam in its condensation can also be used in heating the tributaries.
PCT/ES2005/070126 2005-09-01 2005-09-01 Chemical reactor for the supercritical alcoholysis of all types of fats and oils with different types of alcohols WO2007026032A1 (en)

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