Method for preparing an aromatic composition including a compound containing two solids having organoleptic properties

Abstract

A method for preparing an aromatic pulverulent composition having a melting point Tf, comprising: i) feeding at least two pulverulent elementary solids having organoleptic properties into a mixer, whose chamber has been preheated beforehand to a temperature T lower than Tf, such solids being separately fed into the mixer; ii) mixing the pulverulent elementary solids in the mixer, in the absence of any external liquid phase, at a temperature T lower than Tf, at least one of the pulverulent elementary solids being fed into the mixer at a temperature Ti, such that the mixing occurs under isothermal conditions at a temperature set at such temperature T; and iii) recovering the aromatic pulverulent composition. This method is particularly suitable for preparing a composition essentially including a vanillin and ethylvanillin compound.

Claims

1. A process for preparing a pulverulent aromatic composition having a melting point Tf, comprising: i) introducing into a mixer, whose chamber has been heated beforehand to a temperature T lower than Tf, wherein T is of between 48 and 53 C., at least two pulverulent elementary solids with organoleptic properties, wherein one of said pulverulent elementary solids is vanillin, and the other pulverulent elementary solid is ethylvanillin, said pulverulent elementary solids being introduced separately into said mixer, ii) mixing in said mixer, in the absence of any external liquid phase, said pulverulent elementary solids at a temperature T lower than Tf, at least one of said pulverulent elementary solids being introduced into said mixer at a temperature Ti such that the mixing takes place under isothermal conditions at a temperature set at said temperature T, and iii) recovering said pulverulent aromatic composition.

2. The preparation process as claimed in claim 1, wherein said pulverulent elementary solids have a melting point greater than or equal to 40 C.

3. The preparation process as claimed in claim 1, wherein said at least two pulverulent elementary solids are introduced at said temperature Ti, said temperature Ti being chosen such that T20 C.TiT+20 C. in said step (ii).

4. The preparation process as claimed in claim 1, wherein the vanillin and the ethylvanillin are preheated to a temperature of between 50 and 65 C.

5. The preparation process as claimed in claim 1, wherein said steps i) and ii) are performed under an atmosphere of wet nitrogen or of dry nitrogen.

6. The preparation process as claimed in claim 1, further comprising at least one step selected from the group consisting of: introducing at least one excipient during the implementation of said step ii); and mixing at least one excipient with said pulverulent aromatic composition recovered after said step iii).

7. The preparation process as claimed in claim 6, wherein the total amount of said at least one excipient is introduced at room temperature into said mixer heated to said temperature T.

8. The preparation process as claimed in claim 6, wherein said at least one excipient is selected from the group consisting of fatty substances, fatty alcohols, sugars, polysaccharides, silica, vanillin, and ethylvanillin.

9. The preparation process as claimed in claim 1, wherein said pulverulent aromatic composition has a melting point Tf greater than or equal to 30 C.

10. The preparation process as claimed in claim 1, wherein the mixing of said solids in step ii) is performed under a humid atmosphere.

11. The preparation process as claimed in claim 10, wherein a gas stream sparged through liquid water is supplied to said mixer to provide said humid atmosphere.

Description

EXAMPLE 1

(1) 2100 g of vanillin (VA) powder and 900 g of ethylvanillin (EVA) powder are heated at 60 C. overnight in an oven. The VA/EVA mass ratio is 70/30. The humidity of these powders is 0.1% by weight.

(2) A ploughshare mixer equipped with a 15 liter tank heated via a jacket is preheated to 51 C. The jacket is fed with water thermostatically maintained at 52 C.

(3) A circulation of wet nitrogen is established in the mixer at a flow rate of 200 l/h. Humidification of the nitrogen stream is ensured by sparging it through water maintained at 40 C. so as to obtain 25 g of water per kg of nitrogen. The feed line between the water bath and the mixer is maintained at 45 C. so as to avoid any condensation in the pipes.

(4) After preheating the mixer to 51 C., the preheated vanillin is introduced into said mixer and the preheated ethylvanillin is then introduced therein. The mixer stirrer is switched on at a speed of 100 rpm, i.e. a speed at the end of the paddles of 1.25 m/s for 5 minutes. The stirring is then reduced to a speed of 40 rpm (i.e. a speed of 0.5 m/s at the end of the paddles) and is maintained for 1 hour. The heating of the water feeding the jacket is then stopped and, by natural cooling, the temperature of the product is brought to 35 C. The mixer stirring and the nitrogen circulation are stopped and the mixer is emptied. The product is then recovered.

(5) The product is screened through 1 mm; the undersize (particles with a size of less than 1 mm) represents 56% by weight of the total mass. The 1 mm oversize (granules with a size of greater than 1 mm) is milled using a Quadro Comill mill equipped with a 1 mm grate. The two fractions are then combined and the mixture is homogenized to give the pulverulent composition with organoleptic properties.

(6) The melting point of the composition obtained is determined by differential calorimetric analysis as described previously. The thermogram obtained has a main peak which corresponds to the vanillin/ethylvanillin compound. The melting point (Tonset), which corresponds to the maximum slope of the peak, is 59.5 C.

(7) The X-ray diffraction spectrum of the composition has characteristic lines at angles 2=20.7-25.6-27.5-28.0 as illustrated in figure 1 and which differentiate it from the spectra of vanillin and of ethylvanillin.

(8) The flowability index and the caking index, measured as described previously using an annular cell, are, respectively, 9.6 and 0.14.

EXAMPLE 2

(9) 2000 g of the composition, obtained in example 1, after the screening operation are mixed with 3000 g of Glucidex IT12 (maltodextrin) sold by Roquette. The mixing is performed at room temperature in a ploughshare mixer for a time of 5 minutes. The flowability index and the caking index, measured as described previously using an annular cell, are, respectively, 15 and 0.56. The X-ray diffraction spectrum of the composition thus obtained as a mixture with an excipient based on maltodextrin has characteristic lines at angles 2=20.7-25.6-27.5-28.0.

EXAMPLE 3

(10) 1400 g of vanillin (VA) powder and 600 g of ethylvanillin (EVA) powder are heated at 60 C. overnight in an oven. The VA/EVA mass ratio is 70/30. The humidity of these powders is 0.1% by weight.

(11) A ploughshare mixer equipped with a 15 liter tank heated via a jacket is preheated to 52 C. The jacket is fed with water thermostatically maintained at 52 C. The mixer is placed under an inert atmosphere provided by flushing with dry nitrogen (40 l/h). After preheating the mixer to 52 C., the preheated vanillin is introduced into said mixer and the preheated ethylvanillin is then introduced therein. The mixer stirrer is switched on at a speed of 100 rpm, i.e. a speed at the end of the paddles of 1.25 m/s, for 5 minutes. The stirring is then reduced to a speed of 40 rpm and is maintained for 1 hour.

(12) 3 kg of Glucidex IT12 sold by Roquette (maltodextrin) are then added, at room temperature, to the mixer containing the VA-EVA mixture in which the transformation at 52 C. takes place, to obtain the desired composition. The jacket temperature is maintained at T=52 C. and the mixture is stirred at 100 rpm for 5 minutes. Heating of the water feeding the jacket is then stopped, and the mixer stirring and the nitrogen circulation are stopped. The mixer is emptied and the product is then recovered and cooled naturally in the ambient air.

(13) The particle size of the product is checked by screening: the size of the particles (equivalent diameter) forming the product thus obtained is less than 1 mm. No milling operation is necessary. The melting point of the product obtained is determined by differential calorimetric analysis as described previously. The thermogram obtained has a main peak which corresponds to the vanillin/ethylvanillin compound. The melting point (Tonset), which corresponds to the maximum slope of the peak, is 58.5 C.

(14) The X-ray diffraction spectrum of the particles has characteristic lines at angles 2=20.7-25.6-27.5-28.0. The flowability index and the caking index, measured as described previously using an annular cell, are, respectively, 13 and 0.58.