Classifications

• • C—CHEMISTRY; METALLURGY
  • C07—ORGANIC CHEMISTRY
  • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
  • C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
  • C07C51/42—Separation; Purification; Stabilisation; Use of additives

Definitions

• the present invention relates to a solid calcium lactate composition, in the form of particles of substantially spherical shape, having a particle size such that the majority of the particles have dimensions of between 280 and 550 microns; the present invention also relates to a method for obtaining this type of calcium lactate.
• Calcium lactate or calcium hydroxy-2-propanoate is the calcium salt of lactic acid, a natural acid produced by bacterial fermentation on starch or molasses. It exists in different forms: anhydrous, monohydrate, trihydrate and pentahydrate. Calcium lactate has physicochemical characteristics that are particularly well suited for the enrichment of a wide range of food products and for calcium supplementation.
• Calcium present as a mineral salt in the body, accounts for 2% of body weight. 99% of it is found in the bones and teeth to which it provides rigidity and strength. The remaining percentage (1%) circulates in the blood and contributes to the proper functioning of the nervous and cardiovascular systems. When an insufficient amount of calcium circulates in the blood, it is renewed by the calcium of the bones. The bones thus lose calcium continuously. To avoid deficiencies, sources of growth delays, bone fragility and osteoporosis, calcium must be "replenished" by food.
• Milk and dairy products are now the main source of calcium in the diet for many populations. However, many people find it difficult to meet their daily needs via this type of product. Several reasons explain this phenomenon, they are of order: - cultural
• the flow capacity and the percentage of fines of the ingredients used in tablet formulation are important parameters for the production of this dosage form. Indeed, the powders having a high degree of flow capacity offer the advantage of being able to support high production speeds. Similarly, the reduction of electrostatic and pneumatic spraying of fines helps to increase yields and keep rooms and machines clean.
• the sources of calcium are in the form of a powder having a granular distribution unevenly uniform and containing a large percentage of fine particles. These characteristics limit the ability to the flow of the powder and hence its use in the production of tablets.
• Supplementation in the form of calcium powders may also be offered to consumers. These usually contain calcium carbonate or calcium citrate, which is poorly soluble in water. The consumer will usually have to wait patiently for the dissolution of the powder before consuming the product. In the opposite case, the undissolved particles will be able to considerably reduce the organoleptic qualities of the solution as well as its absorption by the organism.
• the known compositions comprise in addition to calcium lactate, a significant amount of citrate or malate Ca, but this does not lead despite the desired properties, given their deficiency in terms of solubility in water, but also because of their impact on the taste of the product.
• most sources of calcium, including calcium lactate are in the form of clusters of particles highly sensitive to the attrition phenomenon and can therefore limit its use.
• the spherical shape has the advantage that it is much more resistant to this phenomenon, thus generating a lower percentage of fines and increasing the rate of dissolution of the ingredient.
• the ingredient obtained is composed of particles having poor handling properties (powdery fines) and flow (grains of irregular shapes in particular).
• Spray drying which consists in spraying a liquid into a mist of fine droplets and bringing these fine droplets into contact with the hot air in a drying chamber, generates, for its part, an ingredient with a rich particle size distribution. in fine powdery and difficult to dissolve.
• Another object of the invention is also a method for obtaining solid Ca lactate particles, in the form of particles of substantially spherical shape.
• the concentration of calcium lactate solution that can vary from 20 to 60% by weight is supplied by spray (atomization) in a fluidized bed where the suspension is maintained in suspension. fine particles of calcium lactate. Air flow conditions (to keep the bed in suspension at the spray nozzles), flow and concentration of the calcium lactate solution, and temperature are controlled to allow for growth in size. particles mainly by layer (onion structure) and not by agglomeration of these fine particles.
• Ca lactate concentrations of between 20% and 50% are used, an air temperature at the inlet of the atomization chamber of less than 80 ° C. to obtain particles whose dimensions increase in size but which ultimately have a particle size such that there is 50 to 80% of the particles whose dimensions are between 280 and 550 microns.
• a preferred way of using the technology is to produce the spherical calcium lactate beads in two stages.
• the first (granulation-crystallization) operated at low temperature will consist of forming the porous beads by spraying in a fluidized bed consisting of fine particles and the second to bring it to the desired hygrometry level.
• This second step may be operated in a fluidized bed or by any other technology known to those skilled in the art.
• the spray drying technologies traditionally used call for the use of high incoming air temperatures aimed at rapidly attaining a low product hygrometry.
• the finished products generally comprise a large part of fines.
• a variation of the conventional process provides agglomerated products with larger particle sizes. After partial drying by atomization at inlet air temperatures above 120 ° C., the particles are agglomerated in a porous layer on a conveyor belt dryer. A final step of crushing or crumbling is then necessary to obtain a granulated powder having the desired dimensions.
• a preferred route for directly obtaining spherical granulated particles is the use of a technology granulation in a fluidized bed.
• this process requires that the particles "floating" in the air of the fluidized bed do not tend to stick together.
• the use of high temperatures promotes the particle sticking phenomenon and leads to a large caking that can block the installation.
• the Applicant has now found that by operating at low temperature, the calcium lactate is allowed to remain in a non-sticky crystalline form and thus ensure good fluidization of the particles.
• Flow capacity can be defined as the ability of a powder to flow smoothly under the effect of gravity or any other force.
• Different methods of measuring the flow of powders have been documented in the literature. Comparative analysis of different analytical methods by JL Ilari (Ilari JL, Flow Properties of Industrial Milk Powders, Milk Tech 82 (2002) 383-399.) Led to the recommendation of the physical properties analyzer method. Hosokawa. This method, which is particularly well suited to analyzing the flow of dairy powders, can also be applied to calcium lactate powders.
• the Hosokawa apparatus thus makes it possible to measure on the powders seven main physical characteristics relating to their flow properties but also to landslide.
• the seven characteristics measured are described in the manual edited by Hosokawa Micron Corp. (Hosokawa Micromeritics Laboratory, Manual for the Use of Hosokawa powder tester, Hosokawa Micron Corp., Osaka, Japan, 1981. Below is a brief description of the measurements taken:
• the angle of repose is to measure the angle of a stack of particles previously dispersed by a vibrating screen and collected by a funnel and then deposited on a work plane.
• the angle of fall which consists in measuring the angle of the same pile of powder after having subjected it to an impact (vertical fall of a fixed height of an object of determined mass)
• the difference angle is deduced;
• the spatula angle the angle of a stack of powder deposited on a spatula is measured
• the uniformity the powder passes through three superposed vibrating screens and the method consists in weighing the quantity of powder retained by each sieve after a determined vibration duration.
• This parameter is a numerical value obtained by dividing the width of the pores of the sieves passing 60% of the powder by the width of the pores of the sieves passing 10% of the powder. The greater the uniformity of the powder, the more the ratio described above is close to 1.
• a watch glass is placed vertically on a trap on which the powder is deposited.
• the quantity of powder collected on the watch glass is determined after abrupt opening of the hatch. This characteristic also makes it possible to highlight the presence of fines in the powder. The greater the quantity of powder collected on the watch glass, the lower the quantity of dust and the dispersibility value.
• Each measured physical characteristic is assigned an index. The sum of these indexes makes it possible to determine the index of flow or landslide, which corresponds to a degree of flow or landslide.
• a calcium lactate having a high flow index of greater than 80, or even greater than 90 is obtained, which corresponds to a degree of flow described as "fairly good". "Or” very good ".
• the uniformity and the spatula angle of the calcium lactate described in the invention respectively have values of less than 2 and 30 °.
• a uniformity value> 2 and a spatula angle value> 30 ° decrease the flow index and thus reduce the ease of use of calcium lactate. At present it is these types of product that we meet on the market.
• the calcium lactate described in the invention has a high index of landslide greater than 60, which corresponds to a degree of landslide described as "good enough" and greater than what is currently found on the market. .
• the attrition phenomenon can be demonstrated by the following method: place 100g ⁇ 0.01 g of the test sample (whose particle size distribution obtained by sieving method is known) on a sieve whose size of the openings of mesh wire mesh is 100 microns and activate the vibrating sieve type Retsch AS200 amplitude 0,95mm / 'g.
• the sieving time is fixed at 1 hour.
• the particle size distribution of attrition-sensitive samples evolves as follows: the amount of small particles increases while that of large ones decreases.
• the dissolution rate is determined by the following method, hereinafter defined by the term "METHOD”: in a volume of demineralized water of 100 ml maintained at 25 ° C. ⁇ 10 ° C. in a 500 ml beaker equipped with a magnet bar rotating at a controlled speed of 400 rpm ⁇ 20 rpm, 5 g ⁇ 0.01 g of calcium lactate sample are introduced. A chronometer is activated at the precise moment of the addition of the product and stopped as soon as disappearance / solubilization of the last visible particle. The dissolution rate is then represented by the time required for the dissolution of the entire sample.
• the calcium lactate described in the invention has the particularity of being both robust enough to provide good resistance to attrition and porous than to allow rapid dissolution (dissolution rate of less than 3 minutes).
• a calcium lactate pentahydrate powder was prepared in two separate steps.
• a 32% calcium lactate solution was sputtered in a fluidized granulator continuously fed with fines.
• the bottom sieve of the fluidized bed has a surface of 0.45 m 2.
• the air temperature at the inlet of the atomization chamber can fluctuate but remains between 52 and 55 ° C.
• the incoming air flow is adjusted to 1700 m3 / h.
• a second step of the method the wet particles obtained in the first step are subjected to a heat treatment to bring the calcium lactate to the desired hygrometry level.
• This second step takes place in a fluidized bed for which the temperature of the incoming air is 125 ° C.
• a product is always obtained in the form of substantially spherical particles and having a moisture content of about 23%, and whose physicochemical properties are shown in Table 1 and whose particle size distribution is repeated. in Table 2.
• a calcium lactate powder was prepared according to a usual method and a powder was obtained in the physicochemical properties shown in Table 1 and whose particle size distribution is given in Table 2. .
• the calcium lactate described in the invention has a particle size such that one has 50 to 80% of the particles whose dimensions are between 280 and 550 microns.
• the calcium lactate obtained according to the state of the art has, for its part, a particle size such that one has more than 55% of particles whose dimensions are between 0 and 280 microns.
• the calcium lactate described in the invention does not generate particles smaller than 100 microns when it is subjected to an attrition phenomenon. . It has a lower susceptibility to attrition than the calcium lactate obtained according to the state of the art.

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• Chemical & Material Sciences (AREA)
• Organic Chemistry (AREA)
• Engineering & Computer Science (AREA)
• Oil, Petroleum & Natural Gas (AREA)
• Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
• Coloring Foods And Improving Nutritive Qualities (AREA)

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• 2008
  • 2008-12-24 BE BE2008/0701A patent/BE1018560A3/fr active
• 2009
  • 2009-11-18 CN CN2009801499777A patent/CN102245556A/zh active Pending
  • 2009-11-18 WO PCT/EP2009/065397 patent/WO2010072474A1/fr active Application Filing
  • 2009-11-18 EP EP09756726A patent/EP2376416A1/de not_active Withdrawn

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