FAST RELEASE BENZOIC ACID IN FEED

Abstract

The present invention relates to the use of benzoic acid prills in the feed industry. Despite of having a reduced surface area/volume ratio, the benzoic acid prills as used in the context of the present invention release benzoic acid faster than benzoic acid flakes. Compositions comprising such prills are useful for balancing the microflora in an animal's gastro-intestinal system, for acidification of feed and/or urine, and/or for reducing digestive disorders of an animal.

Claims

1. Method of producing benzoic acid prills, said method comprising the steps: (i) providing particles by spray cooling molten benzoic acid; (ii) removing non-spherical particles from the particles provided in step (i).

2. Method according to claim 1, wherein step (i) is done by spraying molten benzoic acid into a gaseous cooling medium, and wherein said gaseous cooling medium is preferably air.

3. Method according to claim 1, wherein in step (ii), the difference between the sliding friction of non-spherical particles and the rolling friction of spherical particles is used for separating non-spherical particles from spherical particles.

4. Animal food comprising benzoic acid prills.

5. Animal food according to claim 4, wherein said animal food is a feed additive, a premix or feed.

6. Animal food according to claim 4, said animal food further comprising at least one essential oil, wherein said essential oil is preferably thymol and/or eugenol.

7. Process for the preparation of animal food, said process comprising the step of adding benzoic acid prills to a composition which can be fed to an animal.

8. Process according to claim 7, wherein said animal food is a feed additive, a premix or feed.

9. Use of benzoic acid prills for acidification of feed and/or urine.

10. Use according to claim 9, wherein the urine of an animal is acidified by feeding benzoic acid prills to the animal, and wherein said animal is preferably a domestic animal, and wherein said domestic animal is preferably a farm animal, and wherein said farm animal is preferably a chicken or a pig, and wherein said farm animal is most preferably a pig.

11. Animal food, process or use according to claim 4, wherein said benzoic acid prills comprise at least 95 weight-% benzoic acid, preferably at least 98 weight-% benzoic acid, more preferably at least 99 weight-% benzoic acid, even more preferably at least 99.5 weight-% benzoic acid and most preferably at least 99.9 weight-% benzoic acid, based on the total weight of the prills.

12. Animal food, process or use according to claim 11, wherein said benzoic acid prills are free of fat-soluble auxiliary compounds.

13. Animal food, process or use according to claim 11, wherein said benzoic acid prills are spherical and/or wherein said benzoic acid prills have neither edges nor spikes.

14. Animal food, process or use according to claim 11, wherein said benzoic acid prills have an average particle size D (v,0.5) from 0.5 mm to 6 mm, more preferably from 0.5 mm to 5 mm and most preferably from 0.5 mm to 2 mm.

15. Animal food, process or use according to claim 11, wherein said benzoic acid prills are obtained.

Description

FIGURES

[0072] FIG. 1 show the result of the compaction test done in example 1. FIG. 1a shows the compaction behavior of a composition which essentially consists of benzoic acid prills. FIG. 1b shows the compaction behavior of commercially available benzoic acid flakes. The comparison of FIG. 1a with FIG. 1b shows one of the benefits of using benzoic acid prills in the feed industry: discharging benzoic acid prills out of bins, silos etc. is easy because compaction during storage is reduced or even absent.

[0073] FIG. 2 show particles consisting of benzoic acid. FIG. 2a shows particles produced in a prilling tower. Some of the particles are benzoic acid prills whereas others are a non-spherical by-product. After removal the non-spherical particles, the particles shown in FIG. 2b were obtained. FIG. 2c shows, as a comparison, benzoic acid flakes as commercially available under the tradename VevoVitall®. These flakes are neither spherical nor produced by prilling.

[0074] FIG. 3 shows the result of the dissolution tests done in example 3. On the x-axis, the duration of the dissolution test is shown in minutes. On the y-axis, the amount of dissolved benzoic acid is shown in percentages. The dissolution of three kinds of particles is shown in FIG. 3: flakes, prills and non-spherical by-product. After 60 minutes, less than 90% of the benzoic acid flakes (VevoVitall®) had been dissolved. The non-spherical by-product of the prilling process showed a similar release. Surprisingly, the benzoic acid prills of the invention dissolved quicker. After 30 minutes, 66.71% of the benzoic acid prills were dissolved whereas only 57.6% of the benzoic acid flakes were dissolved after 30 minutes.

[0075] FIG. 4 shows the result of the test done in example 4. The first line of pictures in FIG. 4 is the backside view of a jolting volumeter after 0 taps, after 375 taps, after 1125 taps and after 1500 taps. The second line of pictures in FIG. 4 shows the upper part of the same jolting volumeter after the same number of taps whereas the third line of pictures in FIG. 4 shows the lower part of the same jolting volumeter after the same number of taps.

[0076] FIG. 4 illustrates that the benzoic acid prills of the invention are suitable for producing animal food such as a feed additive.

EXAMPLES

Example 1

[0077] Particles consisting of benzoic acid were produced in a prilling tower by spraying liquid benzoic acid into a gaseous cooling medium (air). Physical characteristics of the obtained particles were measured and compared with the physical characteristics of commercially available benzoic acid flakes (VevoVitall®). The result of this comparison is summarized in below TABLE 1.

TABLE-US-00001 TABLE 1 Benzoic Acid particles Benzoic Acid produced in prilling Sample Flakes VevoVitall ® tower composition 100% benzoic acid 100% benzoic acid Aspect white coarse powder/ Mixture of white small broken flakes spherical particles and non-spherical crystals Smell very strong typical but less strong Flowability through Agway 6/high 5/high funnel, orifice 11.3 mm (sec/100 g) Dusting Heubach (mg/25 28/low 3/very low g)/Rating Bulk density (kg/l) 0.60 0.65 Tapped density (kg/l) 0.68 0.68 Particle size Average D (v, 0.5) 1.3 mm 1.12 mm <0.425 mm 1.7%   0% 0.425-0.600 mm 4.3%  0.2% 0.600-0.850 mm 10.9% 12.3% >0.850 mm 83.1% 87.5% Compaction 50-60% of Area left, no compaction falls apart when touched

Flowability

[0078] For examining flow properties, an Agway funnel flow test was done. In accordance with the procedure, a funnel [electropolished metal, thickness about 1.5 mm, conical configuration, one opening (orifice) having a 11.3 mm I.D. (inside diameter); 225 mm long; angle between its longitudinal axis and the wall is 10.5 degrees] was placed in a suitable ring stand with the orifice of the funnel located approximately 200 mm from a table top. 100 g of test material were weighed and poured into the above described funnel. Any loss of material from the funnel orifice was prevented by covering the orifice with a finger or plate. The material was permitted to flow from the funnel by removal of the plate and if needed slightly tapping the outside of funnel side wall with a finger or other rod like implement. The time required to empty the funnel was noted. The procedure was repeated at least three times, taking an average and recording it as the flow time. Analysis of the flow properties is based on the flow time recorded, the visual flow behavior, and the number of taps to the funnel side wall necessary to initiate or maintain flow. Flow or non-flow through the Agway funnel serves as a useful vehicle in measuring the relative flowability of a product and for predicting potential flow problems in e.g. emptying silos.

[0079] Example 1 shows that flowability of benzoic acid particles produced in prilling tower is high (even though non-spherical by-product had not yet been removed).

Dusting

[0080] For determination of dust generated by the handling of benzoic acid particles, a commercially available dustmeter from Heubach® (Langelsheim, Germany) was used.

[0081] Example 1 shows that safety at work in the feed industry is significantly improved when using benzoic acid particles which are produced in prilling tower.

Particle Size

[0082] Particle size as indicated in Table 1 was measured by Laser Diffraction; Malvern Mastersizer 2000, MIE volume distribution. The fundamental size distribution derived by this technique is volume based. This means that when the result indicates, for example, that 4% of the distribution is in the size category 0.600 mm-0.850 mm, this means that the total volume of all particles with diameters in this range represents 4% of the total volume of all particles in the distribution. D (v, 0.5), D (v, 0.1) and D (v, 0.9) are standard “percentile” readings from the analysis. D (v, 0.5) is the size in mm at which 50% of the sample is smaller and 50% is larger.

[0083] Example 1 shows that the benzoic acid particles produced in the prilling tower have a similar average particle size as commercially available benzoic acid flakes.

Compaction Test

[0084] The result of the compaction test is shown in FIGS. 1a and 1b. For testing compaction, a metal tube (solid ring) with 5 cm bore diameter (≈20 cm.sup.2) was filled with 15 g of test material. For simulating weight, a metal cylinder with 5 cm diameter (weight is 1.25 kg corresponding to 0.625 N/cm.sup.2=6′250 N/m.sup.2 simulating a weight of 625 kg on an area of 1 m.sup.2) was placed on the test material in the metal tube. This setting was then stored for 1 to 5 days at Room Temperature (RT≈25° C.)/ambient humidity (≈60%). The cylinder has then cautiously been removed and the product was assessed visually and with the aid of a spatula. Rating was then done with 2 scales: (1) Block size of compacted material after removal of weights expressed by percent of block circular area (surface) compared to tube diameter and (2) required force to separate the block.

[0085] Example 1 shows that the benzoic acid particles produced in the prilling tower are significantly less prone to compaction.

Visual Inspection

[0086] Microscopic inspection of the benzoic acid particles produced in the prilling tower as used in example 1 shows a mixture of spherical prills and uneven crystal-shaped particles (cf. FIG. 2a). Microscopic inspection of commercially available VevoVitall® benzoic acid flakes confirms the absence of spherical particles (cf. FIG. 2c).

Example 2

[0087] In Example 2, non-spherical particles (by-product) contained in the benzoic acid particles which had been produced in the prilling tower, were removed. The thus obtained spherical benzoic acid prills are shown in FIG. 2b.

[0088] For removal of the non-spherical by-product, the benzoic acid particles which had been produced in the prilling tower were moved over an inclined surface. Spherical prills rolled like marbles and thus arrived faster than the non-spherical by-product at the bottom of the inclined surface. After this separation process, flowability, bulk density and tapped density was measured again. The result is shown in below TABLE 2:

TABLE-US-00002 TABLE 2 Benzoic acid separated prills by-product (“spherical (“non-spherical Sample fraction”) fraction”) Flowability through Agway 5 7 funnel, orifice 11.3 mm (sec/100 g) Bulk density (kg/l) 0.72 0.64 Tapped density (kg/l) 0.75 0.69

[0089] In case of separated by-product, it took 7 seconds to empty the Agway funnel. For the benzoic acid prills, it took only 5 second to the same Agway funnel under the same conditions. Thus, example 2 confirms that flowability of benzoic acid prills as herein described is high.

Example 3

[0090] In Example 3, dissolution of various kinds of benzoic acid particles was tested. The samples whose dissolution rates were tested are further described in below TABLE 3:

TABLE-US-00003 TABLE 3 sample composition representative picture Benzoic acid prills 100% benzoic FIG. 2b (“spherical fraction”) acid separated by-product 100% benzoic cf. non-spherical particles (“non-spherical fraction”) acid in FIG. 2a benzoic acid flakes 100% benzoic FIG. 2c (VevoVitall ®) acid

[0091] Dissolution was measured in a USP-4 release tester (Sotax CE 7 smart). This device uses a flow cell. The following parameters were used in the dissolution test: [0092] Test temperature: 37.0° C. [0093] Pump delivery: 8 ml/min. [0094] Cell: 12 mm [0095] Buffer: HCl pH 2

[0096] Samples were taken inter alia after 5, 10, 15, 30 and 60 minutes and concentration of released benzoic acid was measured.

[0097] The result of the dissolution tests is shown in FIG. 3. Spherical benzoic acid prills dissolved faster than benzoic acid flakes whereas the separated, non-spherical by-product dissolved approximately as fast as the benzoic acid flakes (cf. FIG. 3). This is surprising as all samples are particles consisted of benzoic acid only.

Example 4

[0098] In example 4, a feed additive was produced by mixing benzoic acid prills with a commercially available powder. The powder comprises a mixture of encapsulated essential oil. The volume of the mixture before and after tapping was the determined using a commercially available Jolting volumeter (J. Engelsmann A G, Ludwigshafen, Germany). An empty graduated 250 ml glass cylinder (accuracy 2 ml) was used.

[0099] Before starting the test, a volume of 174 ml was tested. After 1125 taps the volume was reduced to 150 ml. The volume did not further decrease after a total of 1500 taps. FIG. 4 shows that the mixture in the glass volumeter did not show any signs of de-mixing, not even after 1500 taps.

[0100] Example 4 shows that benzoic acid prills are suitable for manufacturing feed additives, pre-mixes and feed.