Chemical synthesis comprising heat treatment by intermittent dielectric heating combined with a recycling system

Abstract

This invention relates to the design of a process by intermittent dielectric heating combined with a recycling system. This process consists in subjecting reagents to electromagnetic waves selected in the frequencies ranging between 300 GHz and 3 MHz intermittently using a recycling system. This process enables the treatment of oils that are hardly absorbent as well as great investment savings. This process enables operation on different scales, whether in laboratories, on a semi-industrial or industrial scale, without forfeiting the advantages of continuous dielectric heating.

Claims

1. A process of heat treatment in a chemical synthesis comprising: circulating one or more reagents in a recycling system; subjecting said reagent(s) to electromagnetic waves intermittently, wherein the reagent(s) is/are subjected to said electromagnetic waves in one part of the recycling system and not in another part of the recycling system; wherein said heating is intermittent dielectric heating, and wherein the frequencies are microwave frequencies (MW) from about 300 MHz to about 30 GHz; or high frequencies (HF) from about 3 MHz to about 300 MHz.

2. The process according to claim 1, wherein the reagent(s) are not continuously exposed to dielectric heating but wherein all reaction mixture molecules are intermittently subjected to dielectric heating.

3. The process according to claim 1, wherein the reagent(s) are selected from the group consisting of products that hardly absorb electromagnetic waves, products that are highly absorbent of said electromagnetic waves and a mixture of both, wherein said process is either not enhanced or enhanced with one or more hardly or highly absorbent catalysts or additives and/or process gas.

4. The process according to claim 3, wherein the reagent(s) is/are selected from the group consisting of vegetable oils, animal fats or oils, compounds of animal or vegetable oils, hydrocarbons, saturated alkanes, saturated and/or unsaturated esters, saturated and/or unsaturated acids; alcohols; epoxides; amino alcohols; and amines.

5. The process according to claim 4, wherein said vegetable oils are selected from the group consisting of rapeseed oil, sunflower oil, peanut oil, olive oil, walnut oil, corn oil, soy oil, linseed oil, safflower oil, apricot kernel oil, sweet almond oil, hemp oil, grassed oil, copra oil, palm oil, cottonseed oil, Babes oil, jujube oil, sesame oil, argon oil, milk-thistle oil, gourds oil, raspberry oil, Carnage oil, enema oil, poppies oil, Brazil nut oil, castor oil, dehydrated castor oil, hazelnut oil, wheat germ oil, borage oil, oenothera oil, Tung oil, and tall oil; said animal fats or oils are selected from the group consisting of sperm-whale oil, dolphin oil, whale oil, seal oil, sardine oil, herring oil, shark (dog-fish) oil, cod-liver oil, neatsfoot oil, as well as beef, pork, horse, and mutton tallow (marrow); said compounds of animal or vegetable oils are selected from the group consisting of squalene extracted from non-saponifiable fats of vegetable oils: olive oil, peanut oil, rapeseed oil, corn germ oil, cottonseed oil, linseed oil, wheat germ oil, rice bran oil, and squalene contained in large amounts in shark (dog-fish) oil; said hydrocarbons are unsaturated, alone or in a mixture, alkene, or a saturated or unsaturated alkane; said saturated and/or unsaturated esters are selected from the group consisting of alone or in a mixture, one or several esters obtained by esterification between a monoalcohol and/or polyol and at least one saturated and/or unsaturated fatty acid; waxes; butters, phospholipids; spingolipids; and glucolipids; said saturated and/or unsaturated acids are selected from the group consisting of alone or in a mixture, one or several saturated acids, one or several monounsaturated fatty acids; one or several polyunsaturated fatty acids, one or several acids comprising conjugated dienes or conjugated trienes, and one or several acids comprising one or several hydroxyl groups; said alcohols are selected from the group consisting of glycerol, sorbitol, sucrose, mannitol, xylitol, neopentylglycol, pentaerythritol, saccharose, galactose, glucose, maltose, maltotriose, fructose, maltitol, lactitol, lactose, ribose, mellibiose, cellobiose, gentiobiose, altrose, gulose, polyalkyleneglycols, polyglycerols, polyphenols, alkylpolyglucosides, polyglucosides, glycol, pentaerythritol, 1,2-ethanediol, 1,4-butanediol; 1,6-hexanediol, aminoalcohols, epoxyalcohols, saturated or unsaturated fatty alcohols, linear or branched alcohols, vitamins sterols, hemiacetals, aminoalcohols, epoxyalcohols, propanol, ethanol, methanol, tetradecyl alcohol and their analogs; said epoxides are selected from the group consisting of alone or in a mixture, vernolic acid, coronaric acid, 1,2-epoxy-9-decene, 3-4-epoxy-1-butene, 2-3-epoxy-1-propanol, and fatty esters obtained by esterification between 2-3-epoxy-1-propanol and a fatty acid; said amino alcohols are selected from the group consisting of alone or in a mixture, monoethanol amine (MEA), diethanol amine (DEA), triethanol amine (TEA), 3-amino-1,2-propanediol, 1-amino-2-propanol; and 2-2-aminoethoxy ethanol; and said amines are selected from the group consisting of ammonia, primary, secondary and tertiary alkyl amines, fatty amines, amino alcohols, triethanol amine (TEA), 3-amino-1,2-propanediol, 1-amino-2-propanol), and ethoxylated amines, wherein said amines can be saturated or unsaturated, linear or branched.

6. The process according to claim 4, wherein the animal or vegetable fats and oils undergo a prior treatment intended to make them more reactive or less reactive.

7. The process according to claim 4, wherein the alcohols undergo a prior treatment to make them more reactive or less reactive.

8. The process according to claim 1, wherein said process uses a catalyst or additive selected from the group consisting of the common acid catalysts, the common basic catalysts, acid and/or basic resins, zeolithes and enzymes, carbon blacks, and activated carbon fibers.

9. The process according to claim 1, wherein the heat treatments are carried out under a normal atmosphere, an oxygen-rich atmosphere, or an inert atmosphere.

10. The process according to claim 1 wherein said chemical synthesis includes a heat treatment and the use of a single reagent, or a mixture of reagents, in variable proportions, with or without catalysts, with or without process gas.

11. The process according to claim 10, wherein said chemical synthesis is selected from the group consisting of esterification, transesterification, epoxidation, sulfation, phosphatation, hydrogenation, peroxidation, isomerization, dehydration, quaternization, amidation, polymerization, polycondensation, decolorizing, deodorizing, and systems for eliminating volatile compounds.

12. The process according to claim 1, wherein said chemical synthesis is a lipochemistry reaction.

13. The process according to claim 1, wherein said chemical synthesis is selected from the group consisting of manufacturing polymers of unsaturated fatty acids, manufacturing polymers of unsaturated fatty acid esters, manufacturing polymers of unsaturated hydrocarbons and manufacturing derivatives of these products using intermittent dielectric heating under microwaves.

14. The process according to claim 1, wherein said chemical synthesis results in the synthesis of polyglycerol, polyglycerol esters, polyglycerol-6 dioleate, and/or polyglycerol-2 tristearate.

15. The process according to claim 1, wherein said microwave frequency is a standing frequency at 915 MHz (authorized frequency with a tolerance of 1.4%) or at 2.45 GHz (authorized frequency with a tolerance of 2%).

16. The process according to claim 1, wherein said high frequency is a standing frequency at 13.56 MHz with a tolerance of 0.05% or at 27.12 MHz with a tolerance of 0.6%.

17. The process according to claim 6, wherein the prior treatment is selected from the group consisting of hydrogenation, hydroxylation, epoxidation, phosphatation, sulfonation reactions or combinations thereof.

18. The process according to claim 8, wherein said common acid catalyst is selected from the group consisting of para toluene suifonic acid, sulfuric acid, phosphoric acid, perchloric acid and combinations thereof.

19. The process according to claim 8, wherein said common basic catalyst is selected from the group consisting of soda, potash, alcoholate of alkaline metals, alcoholate of alkaline-earth metals, sodium acetate, triethyl amines, pyridine derivatives and combinations thereof.

20. The process according to claim 9, wherein the heat treatments are carried out in an inert atmosphere.

21. The process according to claim 1, wherein the reagent (s) are exposed to electromagnetic waves generated with: one (1) 6 kW magnetron generator operating at a frequency of about 2450 MHz for laboratory treatments with a Total Vexp of 32 ml, or one (1) 60 kW magnetron generator operating at a frequency of about 915 MHz for industrial treatments with a Total Vexp of 4 L.

22. The process according to claim 5, wherein the fats, oils, or their derivatives are an isolated reagent, or a reaction mixture comprising two or more compounds; which reaction mixture can comprise equivalent proportions of each compound, or some compounds can be majority compounds.

23. A process of heat treatment in a chemical synthesis, comprising: circulating one or more reagents in a recycling system; subjecting said reagent(s) to electromagnetic waves intermittently, wherein the reagent (s) is/are subjected to said electromagnetic waves continuously in one part of the recycling system and not in another part of the recycling system; wherein said electromagnetic waves are selected in the frequencies ranging between 300 GHz and 3 MHz.

24. A process of heat treatment in a chemical synthesis comprising: circulating one or more reagents in a recycling system; and subjecting said reagents to electromagnetic waves intermittently, wherein the reagents are subjected to said electromagnetic waves in one part of the recycling system and not in another part of the recycling system; wherein said heat treatment is intermittent dielectric heating, wherein at least one of said reagents is a compound which hardly absorbs electromagnetic waves, and wherein the reagents are exposed to electromagnetic waves selected in the frequencies ranging between 300 GHz and 3 MHz.

25. The process according to claim 1, wherein said process is carried out on a production scale using a 915 MHz generator.

26. The method according to claim 5, wherein said vitamins are selected from the group consisting of tocopherol, ascorbic acid, and retinol and said sterols are phytosterols.

27. A process of heat treatment in a chemical synthesis comprising: circulating one or more reagents in a recycling system; and subjecting said reagent (s) to electromagnetic waves, wherein the reagent (s) is/are subjected to said electromagnetic waves continuously in one part of the recycling system and not in another part of the recycling system; wherein said heating is intermittent due to circulation in said recycling system.

Description

BRIEF DESCRIPTION OF THE FIGURES

(1) FIG. 1 illustrates a configuration subjecting several reactors to electromagnetic waves.

(2) FIG. 2 illustrates a configuration using several energy applicators on a single reactor.

(3) FIG. 3 illustrates a reactor of the dielectric heating system.

(4) FIG. 4 illustrates a reactor subjected to electromagnetic waves.

DESCRIPTION OF THE INVENTION

(5) The applicant has discovered a new heat treatment process that consists of submitting the reagent, either alone or in a mixture, to electromagnetic waves in an intermittent manner, with the help of a recycling system.

(6) The electromagnetic waves are selected in the frequencies ranging between 300 GHz and 3 MHz.

(7) This process retains the advantages of continuous dielectric heating while increasing production capacity.

(8) Description of the Equipment

(9) The intermittent heating process is simple and low-cost. It consists of: pumps reactors subjected to the electromagnetic field a dielectric system: chimney applicators, generator waveguides, iris, shortcircuit piston, cooling systems buffer reactors tanks a gas circuit, preferably for an inert gas such as nitrogen condensers measuring devices
The Pumps

(10) The pump(s) is (are) of the variable-flow type.

(11) It can be a feeder dosing pump and/or a recycling pump and/or a vacuum pump. The outflow of the recycling pump influences the time required for a molecule to transit under the waves.

(12) The pumps can be selected, for purposes of indication, from among vane pumps or piston pumps.

(13) Reactors Subjected to the Electromagnetic Field

(14) The reactors subjected to the electromagnetic field do not absorb the waves (pyrex, quartz, etc.).

(15) They are typically cylindrical in shape.

(16) They are positioned inside applicators.

(17) Dielectric System: Chimney Applicators, Generator Waveguides, Iris, Shortcircuit Piston, Cooling Systems

(18) The applicators are formed by singlemode cavities that resonate at the transmission frequency according to a radiation in the direction of the waveguide.

(19) The chimneys prevent wave leakage to the outside of the waveguide. They are preferably of a conical cylindrical shape, as indicated in Application FR No 0108906 filed by this Applicant for limiting the presence of electric arcs.

(20) The waveguide(s) carries/carry the electromagnetic waves. Each waveguide can be subdivided into twoand only twowaveguides.

(21) The generators used are microwave or high-frequency generators.

(22) The microwave (MW) frequencies range from about 300 MHz to about 30 GHz, preferably standing at 915 MHz (authorized frequency with a tolerance of 1.4%) or at 2.45 GHz (authorized frequency with a tolerance of 2%).

(23) The high frequencies (HF) range from about 3 MHz to about 300 MHz, preferably standing at 13.56 MHz (authorized frequency with a tolerance of 0.05%) or at 27.12 MHz (authorized frequency with a tolerance of 0.6%).

(24) The generators are outfitted with a safety feature that allows the incident waves to pass through and that diverts the reflected waves to a water load in which the waves are absorbed.

(25) These generators also require the use of iris, of a shortcircuit piston in order to decrease the reflected power and to promote absorption of the generator-transmitted power by the reaction mixture.

(26) The system is outfitted with cooling systems in order to avoid any overheating.

(27) The Buffer Reactors

(28) The buffer reactors permit treating a larger amount of reaction mixture.

(29) The Tanks

(30) The system is outfitted with one or several feeder tank(s), receiver tank(s), filtration tank(s).

(31) The Gas Circuits

(32) The heat treatments are carried out under a normal atmosphere, or an oxygen-rich atmosphere or, preferably, an inert atmosphere.

(33) The Measuring Devices

(34) The system is outfitted with measuring devices such as manometers, thermocouples, flowmeters.

(35) This process can be used in dynamics or in continuum.

(36) Principle of Intermittent Heating

(37) The entire reaction volume is not continuously exposed to the waves; however, all molecules of the reaction mixture are intermittently subjected to the field.

(38) Various configurations may be considered for carrying out an intermittent dielectric heating.

(39) The first configuration consists in subjecting several reactors to the electromagnetic waves. See FIG. 1.

(40) The second configuration consists in using several energy applicators on a single reactor. See FIG. 2.

(41) The number of applicators depends on the desired working temperature, on the amount of product to be treated, on the reaction temperature rise time, on the dielectric constants of the reagents.

(42) Any person skilled in the art will understand that other configurations are possible besides these two and that the invention relates to all other intermediate positions.

(43) Furthermore, the applicant has discovered an original system consisting in circulating the reaction mixture in a loop, thus reducing investment costs for an equivalent production capacity. Without this recycling system, it would indeed be necessary to use a large-size reactor and a multitude of applicators in order to succeed in heating the same amount of products and to achieve the desired result, which would entail enormous costs.

(44) See FIG. 3.

(45) The intermittent dielectric heating combined with a recycling system makes it possible to increase the production capacities, which are limited under the continuous dielectric heating system, represented in FIG. 4 or FIG. 3 if the applicators cover the entire volume to be treated.

(46) This process can be used in dynamics or in continuum.

(47) According to this configuration, the entire reaction volume is not continuously exposed to the waves; however, all molecules of the reaction mixture are intermittently subjected to the field.

(48) It should be noted that, according to this principle, the invention logically should not have functioned, that is to say, it should logically not have yielded any good results. As a matter of fact, a molecule will only be subjected to the electromagnetic waves for a fraction of its circulation time, for example, 1 sec every 10 sec. Any person skilled in the art understands that this should have produced either very poor results (inefficient process) or zero results. Yet, surprisingly we obtain on the contrary very good results (see hereinbelow) accompanied by the major advantages also mentioned herein.

(49) Volume Exposed to the Electromagnetic Field

(50) The volume exposed to the electromagnetic field is calculated according to the formula below:
V(exposed to the field)=*R.sup.2*H
wherein: R=radius of reactor exposed to the field H=height of reactor exposed to the field
Parameter H:

(51) The height of the reactor exposed to the field typically corresponds to that of the waveguide in order to permit treating the maximum amount of material all at once.

(52) Let's take the case of heat treatments under singlemode microwave, at 2450 MHz. The height of the waveguide in Mode TE 0.1 (Transverse Electric) is equal to 45 mm. The fundamental mode of excitation TE 0.1 makes it possible for the wave to propagate as a single arch, contrary to Mode TE 0.2 which presents two field maxima, yielding a less homogenous heating.

(53) Let's take the case of heat treatments under singlemode microwave, at 915 Hz. In that case, the height of the waveguide is equal to 124 mm.

(54) Parameter R

(55) Typically, the reactor is cylindrical in shape. Its diameter may not exceed the width of the waveguide.

(56) In the case of singlemode microwave applicators, under 2450 MHz, the recommended waveguide width in order to remain in Mode TE 0.1 (Transverse Electric) ranges from about 70 to 100 mm, standing more specifically at 90 mm.

(57) In the case of the singlemode microwave applicators, under 915 MHz, the recommended waveguide width in order to remain in Mode TE 0.1 (Transverse Electric) stands at about 250 mm.

(58) Advantages of the Intermittent Dielectric Heating

(59) Contrary to the common dielectric systems this invention surprisingly permits heating volumes of materials on an industrial scale while keeping the process low-cost. Therefore, the Applicant has devised a process involving intermittent dielectric heating combined with a recycling system.

(60) The Applicant demonstrates by this invention that the reagents benefit from the advantages inherent to the electromagnetic wave technology without being continuously exposed to the field. Indeed, the benefits of the dielectric heating are preserved: 1. the reaction time is significantly reduced; 2. the reaction is carried out in a single step 3. non-use of solvent 4. energy savings (because the times are significantly shorter) 5. absence of burn-up and side reactions.
Reagents:

(61) For this invention, the reagent(s) can be selected from among the products that are hardly absorbent of electromagnetic waves or the products that are highly absorbent of said electromagnetic waves, or a mixture of both, which may or may not be enhanced by one or several hardly or highly absorbent catalysts or additives and/or process gases.

(62) Vegetable Oils

(63) As vegetable oils, we may mention, among others, rapeseed oil, sunflower oil, peanut oil, olive oil, walnut oil, corn oil, soy oil, linseed oil, safflower oil, apricot kernel oil, sweet almond oil, hemp oil, grapeseed oil, copra oil, palm oil, cottonseed oil, Babassu oil, jojoba oil, sesame oil, argan oil, milk-thistle oil, gourdseed oil, raspberry oil, Karanja oil, neem oil, poppyseed oil, Brazil nut oil, castor oil, dehydrated castor oil, hazelnut oil, wheat germ oil, borage oil, oenothera oil, Tung oil, or tall oil.

(64) Animal Fats or Oils

(65) As animal oils or fats, we can cite, among others, sperm-whale oil, dolphin oil, whale oil, seal oil, sardine oil, herring oil, shark (dog-fish) oil, cod liver oil, neatsfoot oil, as well as beef, pork, horse, mutton tallow (marrow).

(66) Animal or Vegetable Oil Compounds

(67) We can also use compounds of animal or vegetable oils such as squalene extracted from non-saponifiable fats of vegetable oils (olive oil, peanut oil, rapeseed oil, corn germ oil, cottonseed oil, linseed oil, wheat germ oil, rice bran oil) or squalene contained in massive amounts in shark (dog-fish) oil.

(68) These animal or vegetable fats and oils, as well as their derivatives, can undergo a prior treatment intended to make them on the one hand more reactive or on the other hand less reactive. The invention relates to both an isolated reagent and a reaction mixture comprising two or more components. These reaction mixtures can include equivalent proportions of each compound; or, certain compounds can be the primary compounds.

(69) Hydrocarbons

(70) As unsaturated hydrocarbons, we can cite, alone or in a mixture, and as non-limitative examples, an alcene, for example one or several terpenic hydrocarbons, that is to say, one or several polymers of isoprene, or one or several polymers of isobutene, of styrene, of ethylene, of butadiene, of isoprene, of propene, or one or several copolymers of these alcenes.

(71) As saturated hydrocarbons, we can cite, among others, the alcanes, for example ethane, propane.

(72) Saturated and/or Unsaturated Esters

(73) As for esters of saturated and/or unsaturated fatty acids, we can use such acids either alone or as a mixture, and by way of non-limitative examples, one or several esters obtained by esterification between a monoalcohol and/or polyol and at least one saturated and/or unsaturated fatty acid; waxes; butters, phospholipids; spingolipids; glucolipids.

(74) Saturated and/or Unsaturated Acids

(75) As unsaturated fatty acids, we can use, either alone or in a mixture, and as non-limitative examples, one or several saturated acids such as caprylic acid, lauric acid, myristic acid, palmitic acid, stearic acid, arachidic acid, behenic acid, lignoceric acid, cerotic acid, one or several monounsaturated fatty acids such as oleic acid, palmitoleic acid, myristic acid, petroselenic acid, erucic acid; one or several polyunsaturated fatty acids such as for example linoleic acid, alpha and gamma linolenic acids, arachidonic acid; 5c,8c,11c,14c-eicosapentaenoic acid (EPA), 4c,7c,10c,13c,16c,19c-docosahexaenoic acid (DHA), one or several acids comprising conjugated dienes or conjugated trienes such as licanic acid, isomers of linoleic and linolenic acids; one or several acids comprising one or several hydroxyl groups such as ricinoleic acid.

(76) Alcohols

(77) As alcohols, we can mention, among others, glycerol, sorbitol, sucrose, mannitol, xylitol, neopentylglycol, pentaerythritol, saccharose, galactose, glucose, maltose, maltotriose, fructose, maltitol, lactitol, lactose, ribose, mellibiose, cellobiose, gentiobiose, altrose, gulose, polyalkyleneglycols, polyglycerols, polyphenols, alkylpolyglucosides, polyglucosides, glycol, pentaerythritol, 1,2-ethanediol, 1,4-butanediol; 1,6-hexanediol, aminoalcohols (for example, diethanol amine (DEA), triethanol amine (TEA), 3-amino-1,2-propanediol), epoxyalcohols, saturated or unsaturated fatty alcohols (for example, myristyl alcohol, oleyl alcohol, lauryl alcohol), linear or branched alcohols, vitamins (for example, tocopherol, ascorbic acid, retinol), sterols (including phytosterols), hemiacetals (for example, 1-ethoxy-1-ethanol), aminoalcohols (for example, 2-2-aminoethoxy ethanol), epoxyalcohols (for example, 2-3-epoxy-1-propanol), propanol, ethanol, methanol, tetradecyl alcohol and their analogs.

(78) The alcohols as well as their derivatives can undergo a prior treatment intended to make them more reactive or, on the contrary, less reactive, such as for example: hydrogenation, hydroxylation, epoxydation, phosphitation, sulfonation.

(79) Epoxides

(80) As epoxydes, we can use, alone or in a mixture, and as non-limitative examples, vernolic acid, coronaric acid; 1,2-epoxy-9-decene, 3-4-epoxy-1-butene, 2-3-epoxy-1-propanol, fatty esters obtained by esterification between 2-3-epoxy-1-propanol and a fatty acid (for example, Cardura E10).

(81) Amino Alcohols

(82) As amino alcohols, we can use, alone or in a mixture, and as non-limitative examples, monoethanol amine (MEA), diethanol amine (DEA), triethanol amine (TEA), 3-amino-1,2-propanediol, 1-amino-2-propanol; 2-2-aminoethoxy ethanol.

(83) Amines

(84) As amines, we can mention, among others, ammonia, primary, secondary and tertiary alkyl amines (for example, methyl amine, dimethyl amine, trimethyl amine, diethyl amine), fatty amines (for example, oleic amines, coconut alkyl amines), amino alcohols (for example, monoethanol amine (MEA), diethanol amine (DEA), triethanol amine (TEA), 3-amino-1,2-propanediol, 1-amino-2-propanol), ethoxylated amines (2-2-aminoethoxy ethanol, amino-1-methoxy-3-propane).

(85) All these amines can be saturated or nonsaturated, linear or branched.

(86) Catalysts

(87) Among the catalysts or additives, there shall be, as non-limitative examples, the common acid catalysts (para toluene sulfonic acid, sulfuric acid, phosphoric acid, perchloric acid, etc.), the common basic catalysts (soda, potash, alcoholate of alkaline metals and of alkaline-earth metals, sodium acetate, triethyl amines, pyridine derivatives, etc.), acid and/or basic resins of the Amberlite, Amberlyst, Purolite, Dowex, Lewatit types, zeolithes and enzymes, carbon blacks, and activated carbon fibers.

(88) The invention will be better understood upon reading the following description and the non-limitative examples given below.

EXAMPLES

(89) The examples given below highlight the value of the invention and will allow any person skilled in the art to easily extrapolate to other dimensions and/or geometries without departing from the true scope and spirits of the invention in its broader aspects.

(90) Additionally, the following examples, which are given solely for purposes of description and in no way of limitation, illustrate the value of the invention. These examples aim to demonstrate that the intermittent dielectric heating process is low-in-cost and permits heating reaction volumes on an industrial scale while still benefiting from the advantages of this technology.

(91) I. Volumes Exposed to Electromagnetic Waves

(92) The tests were conducted on the laboratory and on industrial scale using two (2) generators: one (1) 6 kW magnetron generator operating at the 2450 MHz frequency for the laboratory treatments one (1) 60 kW magnetron generator operating at the 915 MHz frequency for the industrial treatments

(93) TABLE-US-00001 Number of D (mm) H (mm) Unit Vexp reactors Total Vexp Pilot 30 45 32 mL 1 32 mL Industrial 100 124 1 L 4 4 L
wherein: D=diameter of cylindrical reactors=2R H=height of waveguide Unit Vexp=volume exposed continually basis to waves for one reactor Total Vexp=volume exposed continually to waves for both reactors V (exposed to the field)=*R.sup.2*H
II. Comparison between Conventional Heating and Intermittent Dielectric Heating
a. Poll/Glycerol Synthesis

(94) The tests are conducted at 260 C., in the presence of 2% sodium acetate in order to obtain a polyglycerol with a viscosity at 50 C. equal to 3600 cP.

(95) They make reference to Patent Application FR No 0108906.

(96) TABLE-US-00002 Total V of glycerol V ratio Reaction Time Intermittent Pilot 2000 mL 1/62 3 h dielectric industrial 200 L 1/50 6 h 30 min heating Conventional Schou >72 h heating
wherein: Total V of glycerol=total volume of glycerol treated V ratio=ratio between the volume exposed to waves and the total volume treated
b. Synthesis of Polyglycerol Esters
Synthesis of Polyglycerol-6 Dioleate

(97) The tests are carried out in the presence of 0.25% sodium acetate at 230 C.

(98) They make reference to Patent Application FR No 0108906.

(99) TABLE-US-00003 Total V of Reaction mixture V ratio time Intermittent 2000 mL 1/62 2 h 10 min dielectric heating Conventional 4 h 30 min heating
wherein: Total V of mixture=total volume treated V ratio=ratio between the volume exposed to waves and the total volume treated
Synthesis of Polyglycerol-2 Tristearate

(100) The tests are carried out in the presence of 0.25% sodium acetate at 260 C.

(101) They make reference to Patent Application FR No 0108906.

(102) TABLE-US-00004 Total V of Reaction mixture V ratio time Intermittent 2000 mL 1/62 1 h 40 min dielectric heating Conventional 4 to 5 h heating
wherein: Total V of mixture=total volume treated V Ratio=ratio between the volume exposed to waves and the total volume treated
c. Conclusion

(103) Even if the entire reaction volume is not exposed to electromagnetic waves, the reaction times under intermittent dielectric heating are considerably lower than those obtained with conventional heating.

(104) III. Comparison Between Intermittent Dielectric Heating and Continuous Dielectric Heating

(105) a. Efficiency of Intermittent Dielectric Heating

(106) The table below shows the efficiency of intermittent dielectric heating compared with continuous dielectric heating which is typically used.

(107) The tests are carried out under the same conditions (composition of reaction mixtures, temperatures, catalysts, etc.) at the laboratory scale (use of a Synthewave 402) which uses continuous dielectric heating at the pilot scale, using a 2450 MHz generator that uses intermittent dielectric heating and at the production scale using a 915 MHz generator that uses intermittent dielectric heating

(108) The synthesis tested consists in manufacturing unsaturated fatty acid polymers, unsaturated fatty acid esters, unsaturated hydrocarbons, unsaturated derivatives of these compounds, alone or in a mixture.

(109) TABLE-US-00005 Pilot Industrial Laboratory Extrapolated Extrapolated Mop MOi Mop MOi Mop V.sub.treated 25 2000 2000 200000 200000 (mL) V ratio 1/1 1/62 1/1 1/50 1/1 t.sub.reaction 2 h 15 min 2 h 15 min 2 h 15** 2 h 15 2 h 15** (h)
wherein: Mop=continuous microwave heating Extrapolated Mop=continuous microwave heating in the case of treatment of 200 kg of product Moi=intermittent microwave heating V.sub.treated=reaction volume treated V ratio=ratio between the volume exposed to electromagnetic waves and the total reaction volume t.sub.reaction=reaction time **: Treating a large amount of products requires a reaction time greater than or equal to that for a lower amount. The reaction time is 2 h 15 for 25 mL of product. Thus, it can be asserted that the reaction time needed to treat 200 kg of the same mixture will be greater than or equal to 2 h 15.

(110) This table shows that the reaction times are unchanged, whether one works on 25 mL, 2 kg, or 200 kg. However, in the case of pilot and industrial tests (2 kg and 200 kg), the entire volume is not subjected to dielectric heating: laboratory test (continuous dielectric heating): the entire volume is exposed to electromagnetic waves with Ratio=1/1 pilot test (intermittent dielectric heating): only 1/62 of the volume is exposed to the field industrial test (intermittent dielectric heating): only 1/50 of the volume is exposed to the field
b. Lowering of Investment Costs

(111) If we had to treat 200 liters of product using continuous dielectric heating, we would have to expose all 200 liters to the electromagnetic waves.

(112) By working at the 2450 MHz frequency, the maximum volume exposed by applicator is 32 mL. Here this configuration is not advantageous at all. In fact, we would need 6250 applicators.

(113) By working at the 915 MHz frequency, the maximum volume exposed by applicator is 1 L.

(114) We would then need 200 applicators.

(115) For this invention, intermittent dielectric heating makes it possible to use only four (4) applicators, that is to say, 50 times less (a ratio consistent with that given in the preceding table) for the same production capacity.

(116) We can compare the investment costs: X=investment cost of a system with intermittent dielectric heating, 4 channels, recycling Y=investment cost of a system with continuous dielectric heating, 200 channels, without recycling Y=10*X

(117) The investment cost would then be 10 times higher in the case of a continuous dielectric heating compared with intermittent dielectric heating. This is essentially due to the cost of applicators, which is much higher than the rest of the system (buffer reactor, recycling pump, etc.).