Compressed solid composition for non-oral use

11760961 · 2023-09-19

Assignee

Inventors

Cpc classification

International classification

Abstract

A novel binder and/or disintegrant for obtaining a compressed solid composition for non-oral use, the binder and/or disintegrant being fermented molasses, a process for preparing the compressed solid composition and also a binding and/or disintegrating composition, which includes at least fermented molasses. The fermented molasses advantageously makes it possible to replace synthetic binders conventionally used in compressed solid compositions, while also being able to act as a disintegrant on contact with a liquid, especially water. Thus, a novel way is proposed for utilizing a product which was hitherto solely used in the field of agriculture and livestock farming.

Claims

1. A compressed washing and/or cleaning solid composition in the form of a single-layer or multilayer tablet for non-oral use, comprising fermented molasses as binder and/or disintegrant, a sequestrant, and optionally a surfactant in the single-layer tablet or at least one layer of the multilayer tablet, wherein the compressed washing and/or cleaning solid composition is obtained by a process comprising a compacting step carried out by the tablet comprising fermented molasses as binder and disintegrant, wherein the fermented molasses have a viscosity of 500 to 5000 mPa.Math.s and are selected from the group consisting of fermented beet molasses, fermented cane molasses, and a mixture thereof.

2. The compressed washing and/or cleaning solid composition for non-oral use according to claim 1, wherein the fermented molasses has a solids content of between 50% and 80%.

3. The compressed washing and/or cleaning solid composition for non-oral use according to claim 1, wherein the fermented molasses comprises less than 5% by weight of sugars relative to the total weight of dry extract.

4. The compressed washing and/or cleaning solid composition for non-oral use according to claim 1, wherein the fermented molasses comprises less than 1%, the percentages being expressed as dry weight relative to the total dry weight of the composition by weight of sugars relative to the total weight of dry extract.

5. The compressed washing and/or cleaning solid composition for non-oral use according to claim 1, wherein the fermented molasses have carboxymethylcellulose added thereto.

6. The compressed washing and/or cleaning solid composition for non-oral use according to claim 5, wherein the amount of carboxymethylcellulose is from 0.1% to 2%, the percentages being expressed as dry weight relative to the total dry weight of the composition.

7. The compressed washing and/or cleaning solid composition for non-oral use according to claim 5, wherein the amount of carboxymethylcellulose is from 0.1% to 1%.

8. The compressed washing and/or cleaning solid composition for non-oral use according to claim 5, wherein the amount of carboxymethylcellulose is from 0.1% to 0.5%, the percentages being expressed as dry weight relative to the total dry weight of the composition.

9. The compressed washing and/or cleaning solid composition for non-oral use according to claim 1, wherein the fermented molasses have a viscosity of 1000 to 4000 mPa.Math.s.

10. The compressed washing and/or cleaning solid composition for non-oral use according to claim 1, further comprising an active substance, a filler and optionally at least one additive chosen from effervescent agents, detergents, pelletizing additives, whitening agents, polymers, flow agents, stabilizers, anti-foaming agents, dyes, and lubricants.

11. The compressed washing and/or cleaning solid composition for non-oral use according to claim 1, wherein the compressed washing and/or cleaning solid composition for non-oral use does not contain polyethylene glycol and/or microcrystalline cellulose and/or polyvinylpyrrolidone and/or starch and/or hydroxyethyl cellulose and/or gelatin.

12. A method for washing within a dishwasher comprising washing with the compressed washing and/or cleaning solid composition for non-oral use according to claim 1 within the dishwasher.

13. A process of producing the compressed washing and/or cleaning solid composition for non-oral use according to claim 1, comprising adding a fermented molasses as binder and/or disintegrant to the sequestrant, and optionally the surfactant.

14. The process according to claim 13, wherein the fermented molasses is present in the compressed washing and/or cleaning solid composition for non-oral use at an amount by weight of 0.1% to 15% relative to the total weight of the composition.

15. A process for producing the compressed washing and/or cleaning solid composition for non-oral use according to claim 1, comprising the following steps: providing the sequestrant, and optionally: the surfactant, an active substance, a filler, and at least one additive chosen from effervescent agents, detergents, pelletizing additives, whitening agents, polymers, flow agents, stabilizers, anti-foaming agents, dyes and lubricants, and incorporating therein fermented molasses to obtain a mixture; and compacting said mixture in order to obtain said compressed washing and/or cleaning composition.

16. The process according to claim 15, wherein the step of incorporation is carried out by spraying.

17. The process according to claim 15, wherein the step of compacting is carried out on a rotary press.

Description

DETAILED DESCRIPTION

(1) For the purposes of the present invention, compressed solid composition is intended to mean any composition that may be obtained by the processes of compression known to those skilled in the art, such as, for example, pressure compaction, pelletization, granulation, nodulizing, extrusion or else spray-drying. The compressed solid composition according to the invention may therefore also be considered to be an agglomerate.

(2) The compressed solid composition according to the invention may be in a multitude of compressed forms, said forms conventionally being adapted by those skilled in the art depending on the desired application. Thus, the compressed solid composition may be in the form of a single-layer or multi-layer tablet, a cake, a compressed tablet, granules, a pellet or else a lozenge. Preferably, the compressed solid composition is in the form of a single-layer or multi-layer tablet.

(3) For the purposes of the present invention, non-oral use is intended to mean that the compressed solid composition is not intended to be ingested by an animal or human and therefore especially cannot provide food for animals or humans.

(4) For the purposes of clarification, the terms “compressed” “compacted” or else “agglomerated” are indeed considered to be synonyms for the purposes of the present invention and may be used without distinction.

(5) Fermented molasses are a co-product of molasses obtained after fermentation thereof by bacteria, yeasts, or fungi, said fermentation making it possible to obtain products referred to as “valuable” such as baker's yeast, ethyl alcohol or else citric and glutamic acid. Preferably, fermented molasses is obtained by fermentation of molasses by yeasts.

(6) According to the invention, the fermented molasses may equally be obtained from beet molasses, cane molasses, or a mixture of beet molasses and cane molasses. For example, the mixture may contain up to 60% of fermented beet molasses, up to 70% of fermented beet molasses, up to 80% of fermented beet molasses, up to 90% of fermented beet molasses, or even up to 95% of fermented beet molasses. Advantageously, when the fermented molasses are a mixture of fermented beet and cane molasses, said mixture contains 90% of fermented beet molasses.

(7) Initially, the fermented molasses contain more than 90% of water, but this is advantageously concentrated in order to reduce the amount of water and to obtain higher solids contents.

(8) Thus, the solids content of the fermented molasses or of the mixture of beet molasses and cane molasses according to the invention may be from 50% to 80%. Preferably, the solids content of the fermented molasses is from 55% to 75%, and most particularly from 55% to 65%, such as, for example, approximately 60%.

(9) Conventionally, since they are intended, or were used, as fertilizer or in animal feed, fermented molasses are also defined by the distribution of nitrogen-based materials therein, and by the aminogram thereof. The fermented molasses according to the invention may therefore have a distribution of nitrogen-based materials as below: nitrogen from total amino acids: 25% to 50% of the total nitrogen nitrogen from betaine: 0% to 40% of the total nitrogen ammoniacal nitrogen: 2% to 3% of the total nitrogen.
Regarding the aminogram of the proteins of the fermented molasses according to the invention, the mean contents of amino acids may be those presented below, the ranges of values being given in g/kg of solids: Aspartic acid: 6-8 Threonine: 0.5-3 Serine and glutamic acid: 115-130 Proline: 3-4 Glycine: 4-5 Alanine: 2.5-3.5 Valine: 2.5-3.5 Methionine and cysteine: 0.5-3 Isoleucine: 1.5-2.5 Tyrosine: 2-3.5 Leucine: 3-4.5 Phenylalanine: 1-2 Lysine: 0.5-2.5 Histidine: 0.5-2 Arginine: 0.2-1

(10) As co-product resulting from fermentation, fermented molasses have a low sugar content. “Low sugar content” is intended to mean fermented molasses comprising less than 5%, less than 4%, less than 3%, less than 2%, and most particularly less than 1% by weight of sugars relative to the total weight of dry extract. Preferentially, the fermented molasses according to the invention do not contain sugars.

(11) The fermented molasses according to the invention, also termed crude fermented molasses, may undergo one or more chemical or physico-chemical treatments. For example, the fermented molasses may undergo potash removal or demineralization. Such treatments may modify the composition in terms of nitrogen-based materials of the fermented molasses. A potash removal treatment consists, for example, of acidification of the crude fermented molasses by a solution of H.sub.2SO.sub.4, followed by neutralization with aqueous ammonia.

(12) The treatments which may be applied to the fermented molasses qualitatively and quantitatively vary the mineral content. Thus, crude fermented molasses may have a crude ash content of 14% to 22% by weight relative to the crude product and a potassium content of 5% to 18% by weight relative to the crude product. On the other hand, in the case of the fermented molasses which have had the potash removed or which have been demineralized, the crude ash content ranges from 5% to 14% by weight relative to the crude product and the potassium content is generally less than 4% by weight relative to the crude product.

(13) Due to a high ash content, the crude fermented molasses have a density which may range from 1.10 to 1.50. Preferably, the density of the fermented molasses is 1.20 to 1.40, and most particularly 1.25 to 1.35.

(14) The fermented molasses according to the invention have a viscosity of 500 mPa.Math.s to 5000 mPa.Math.s, preferably of 1000 mPa.Math.s to 4000 mPa.Math.s, and a slightly acidic pH of 5 to 6.

(15) The compressed solid composition in accordance with the invention thus comprises crude or demineralized fermented molasses as binder and/or disintegrant.

(16) Said fermented molasses are present within the compressed solid composition in effective proportions. Effective proportions are intended to mean those sufficient to obtain the desired effect, namely obtaining a compressed solid composition which may especially be transported, handled and/or stored without substantial damage and which may disintegrate on contact with a liquid such as water.

(17) Advantageously, the amounts of crude or demineralized fermented molasses used within the compressed solid composition according to the invention may be from 0.1% to 15% by weight, preferentially from 0.5% to 5% by weight, and even more preferentially from 0.5% to 1.5% by weight relative to the total weight of the compressed solid composition.

(18) The binding properties thus brought to light of the fermented molasses make it possible to obtain a compressed solid composition having sufficient mechanical strength to avoid the problems of formation of fine particles during handling thereof. Advantageously, the fermented molasses also act as disintegrant, enabling the compressed solid composition to disintegrate on contact with a liquid, and especially on contact with water.

(19) By means of the compressed solid compositions according to the invention, the inventors have thus identified a novel pathway for utilizing fermented molasses but also an alternative to using synthetic binders or binders that are not conventionally used to obtain solid compositions. By way of example, mention will especially be made of polyethylene glycol, polyvinylpyrrolidone, ethoxylated fatty alcohols, starch, hydroxyethyl cellulose, gelatin or else microcrystalline cellulose.

(20) Thus, the compressed solid composition comprising fermented molasses according to the invention may not contain polyethylene glycol and/or polyvinylpyrrolidone and/or ethoxylated fatty alcohols and/or starch and/or hydroxyethyl cellulose and/or gelatin and/or microcrystalline cellulose.

(21) According to a particular embodiment, the fermented molasses may have substances added thereto, in order especially to exhibit particular physical properties. Thus, the molasses may have a compound added thereto, chosen from the group comprising cellulose-based derivatives such as carboxymethylcellulose, hemicelluloses, lignins, ethyl cellulose, methyl cellulose, hydroxypropyl cellulose, hydroxypropyl methyl cellulose, derivatives from starch production such as wheat, corn, cassava, tapioca, potato, or rice starch, dextrins and other modified starches, dextrans, sugar derivatives such as glucose, fructose, lactose, sucrose, sorbitol, glycerol, natural gums of diutan, gelan, xanthan, carrageenan type, pectins, alginates, chitosan, gum arabic, gum tragacanth, carob gum, acacia gum, agar agar, guar gum, production derivatives such as beet pulps, chicory pulps, dried or non-dried apple pomace, sugar cane bagasse, citrus pulps, fruit juice waste, waste from gum production, waste from starch production, mineral derivatives, smectites, bentonites and other silica-derived clays, lime, magnesium, and others from the same family and also mixtures of several of these compounds. Preferably, the fermented molasses have carboxymethylcellulose added thereto. The amounts of compounds to be added to the fermented molasses may be between 0.1% to 2%, preferentially from 0.1% to 1%, more preferably still from 0.1% to 0.5%, the percentages being expressed as dry weight relative to the total dry weight of the fermented molasses with substances added thereto.

(22) The compressed solid composition may also comprise one or more additives. The additives may be chosen from additives known to those skilled in the art, such as, for example, effervescent agents, detergents, sequestrants, pelletizing additives, whitening agents, polymers, surfactants, flow agents, stabilizers, anti-foaming agents, dyes, or else lubricants.

(23) As examples of stabilizers, mention may be made of esters of para-hydroxybenzoic acid, such as methylparaben and propylparaben, alcohols such as chlorobutanol, benzyl alcohol and phenylethyl alcohol, phenols such as phenol and cresol, sulfite salts such as sodium bisulfite and sodium sulfite, edetic acid salts, such as sodium edetate and tetrasodium edetate, and hydrogenated oils, sesame oil, sodium chondroitin sulfate, dibutylhydroxytoluene, adipic acid, ascorbic acid, esters of stearyl-L-ascorbate, sodium L-ascorbate, L-aspartic acid, sodium L-aspartate, sodium acetyl tryptophan, acetanilide, a solution of aprotinin, aminoethylsulfonic acid, aminoacetic acid, DL-alanine, L-alanine, benzalkonium chloride, sorbic acid.

(24) As examples of lubricants, mention may be made of stearic acids such as stearic acid, calcium stearate and magnesium stearate, waxes such as white beeswax and carnauba wax, sulfates such as sodium sulfate, silicic acid compounds such as magnesium silicate and light silicic anhydride, lauryl sulfates such as sodium lauryl sulfate, cocoa butter, carmellose calcium, carmellose sodium, callopeptide, hydrated silicon dioxide, hydrated amorphous silicon oxide, dry aluminium hydroxide gel, glycerol, light liquid paraffin, hydrogenated oil, synthetic aluminium silicate, sesame oil, wheat starch, talcum, macrogols, phosphoric acid.

(25) As examples of detergents, mention may be made of polyacrylates, acrylic/maleic copolymers, monomeric polycarbonates such as citrates, gluconates, oxydisuccinates, glyceryl mono-, di- and trisuccinates, carboxymethyl oxysuccinates, carboxymethyl oxymalonates, dipicolinates and hydroxyethyliminodiacetates.

(26) According to a particular embodiment, the compressed solid composition may also comprise at least one active substance, at least one filler and optionally at least one additive, which may be chosen from effervescent agents, detergents, sequestrants, pelletizing additives, whitening agents, polymers, surfactants, flow agents, stabilizers, anti-foaming agents, dyes or else lubricants. According to this particular embodiment, the compressed solid composition may be in tablet form and has an application in the field of household, agricultural and industrial washing and/or cleaning. By way of example of household washing and/or cleaning, mention may be made of machine washing, such as, especially, washing within a dishwasher.

(27) According to a particular embodiment, the compressed solid composition for non-oral use according to the invention has a friability of between 5% and 15%, preferably of between 5% and 11%, and most particularly of between 6% and 8%.

(28) According to a particular embodiment, the compressed solid composition for non-oral use according to the invention has a hardness of between 50 N and 90 N, preferably of between 60 N and 80 N, and most particularly of between 70 N and 75 N.

(29) According to a particular embodiment, the compressed solid composition for non-oral use according to the invention has a dust content (dust area) of less than 3, preferably less than 2.5, and most particularly less than 2.

(30) According to another particular embodiment, the compressed solid composition for non-oral use in accordance with the invention may be packaged in bags in order to protect it from moisture and to provide additional protection for handling and/or transport and/or storage. Advantageously, the bag is a biodegradable and/or water-soluble bag.

(31) According to another particular embodiment, the compressed solid composition comprising fermented molasses as binder and/or disintegrant is in the form of an effervescent cleaning cake for toilets, of dishwasher tablets, of calcium hypochlorite tablets for swimming pools, or of granulated fertilizer.

(32) By way of examples of compressed solid composition that may be in the form of a multi-layer tablet, and especially a multi-layer dishwasher tablet, mention will be made of the composition summarized in the table below:

(33) TABLE-US-00001 Components % Layer 1 Sequestrant  20-60 Fermented molasses 0.5-5 (with or without substances added thereto) Alkaline agent  30-50 Filler   0-30 Surfactant   0-10 Polymer   0-10 Dye   0-1 Pelletizing additive   0-5 100.00 Intermediate layer 2 Sequestrant  30-60 Whitening agent  25-50 Surfactant   0-10 Polymer   0-10 Pelletizing additive   0-5 100.00 Layer 3 Sequestrant  20-60 Fermented molasses 0.5-5 (with or without substances added thereto) Alkaline agent  30-50 Filler   0-30 Polymer   0-10 Surfactant   0-10 Activator   0-5 Enzyme   0-30 Dye   0-1 Pelletizing additive   0-5 100.00

(34) Another subject of the invention relates to the use of fermented molasses as binder and/or disintegrant for the production of a compressed solid composition for non-oral use.

(35) The fermented molasses are as defined above. The use of the fermented molasses as binder and/or disintegrant within a compressed solid composition is doubly advantageous. Firstly, the use according to the invention makes it possible to propose a novel way of utilizing molasses, which were hitherto solely intended for spreading or animal feed. Secondly, the use according to the invention enables the substitution of the conventionally used synthetic binders and thereby makes it possible to obtain compressed solid compositions which are more environmentally friendly.

(36) The amounts of fermented molasses used within the compressed solid composition may be from 0.1% to 15% by weight, preferentially from 0.5% to 5% by weight, and even more preferentially from 0.5% to 1.5% by weight relative to the total weight of the compressed solid composition.

(37) The compressed solid composition may be as defined above and may be in the form of a single-layer or multi-layer tablet, a cake, a compressed tablet, granules, a pellet or else a lozenge. Preferably, the compressed solid composition is in the form of a single-layer or multi-layer tablet.

(38) Another subject of the invention relates to a binding and/or disintegrating composition comprising at least fermented molasses as binder.

(39) The fermented molasses in accordance with the invention may also be used as is within a binding and/or disintegrating composition containing one or more other constituents of all types, including those with a binding character, or those able, for example, to increase the mechanical strength of the final product, especially an agglomerate, or to minimize the phenomena of crumbling to which said agglomerate may be subject during the handling or storage thereof. The fermented molasses are as defined above.

(40) According to a particular embodiment, the binding composition according to the invention may also comprise a hardening agent, that is to say which is able to further improve the binding power.

(41) According to a particular embodiment, the fermented molasses may have substances added thereto, in order especially to exhibit particular physical properties. Thus, the molasses may have a compound added thereto, chosen from the group comprising cellulose-based derivatives such as carboxymethylcellulose, lignins, hemicelluloses, ethyl cellulose, methyl cellulose, hydroxypropyl cellulose, hydroxypropyl methyl cellulose, derivatives from starch production such as wheat, corn, cassava, tapioca, potato, or rice starch, dextrins and other modified starches, dextrans, sugar derivatives such as glucose, fructose, lactose, sucrose, sorbitol, glycerol, natural gums of diutan, gelan, xanthan, carrageenan type, pectins, alginates, chitosan, gum arabic, gum tragacanth, carob gum, acacia gum, agar agar, guar gum, production derivatives such as beet pulps, chicory pulps, dried or non-dried apple pomace, sugar cane bagasse, citrus pulps, fruit juice waste, waste from gum production, waste from starch production, mineral derivatives, smectites, bentonites and other silica-derived clays, lime, magnesium, and others from the same family and also mixtures of several of these compounds.

(42) Another subject of the invention relates to a process for producing a compressed solid composition for non-oral use, comprising the following steps: 1) providing an active substance, a filler and optionally at least one additive chosen from effervescent agents, detergents, sequestrants, pelletizing additives, whitening agents, polymers, surfactants, flow agents, stabilizers, anti-foaming agents, dyes or else lubricants, 2) incorporating fermented molasses to the compounds provided in the preceding step, in order to obtain a mixture, 3) compacting said mixture in order to obtain said compressed solid composition.

(43) The first step of the process therefore consists in providing an active substance, a filler and optionally at least one additive chosen from effervescent agents, detergents, sequestrants, pelletizing additives, whitening agents, polymers, surfactants, flow agents, stabilizers, anti-foaming agents, dyes or else lubricants. The active substance and the filler are chosen by those skilled in the art depending on the desired application for the compressed solid composition.

(44) The fermented molasses are then incorporated, according to a second step, into the compounds provided according to the first step of the process, so as to obtain a mixture. The fermented molasses are as defined above, namely especially the co-product obtained by fermentation of the molasses. The amounts of molasses to be incorporated according to this step may be from 0.1% to 15% by weight, preferentially from 0.5% to 5% by weight, and even more preferentially from 0.5% to 1.5% by weight relative to the total weight of the mixture.

(45) The step of incorporation may be performed via techniques that are known to those skilled in the art and which lead to obtaining a mixture. Thus, the step of incorporation may for example be obtained by spraying.

(46) Finally, the third step of the process according to the invention consists of a step of compacting, which may be carried out according to techniques known to those skilled in the art and which lead to the compression or agglomeration of the mixture prepared in the previous step. Thus, the step of compacting may for example be carried out by pressure compaction on a rotary press, by pelletization, by granulation, by nodulizing, by extrusion or else by spray-drying. By way of example, the step of compacting by pressure compaction may be carried out via a rotary press. The step of compacting thus makes it possible to obtain a compressed solid composition which may be in several forms, such as, for example, a single-layer or multi-layer tablet, a cake, a compressed tablet, granules, a pellet or else a lozenge.

(47) The process according to the invention may also comprise a step of drying after the step of incorporation and/or of compacting.

(48) The invention will be better understood using the following examples which are purely illustrative and in no way limit the scope of protection.

EXAMPLES

(49) In the following examples, the mechanical properties were measured with the following methods:

(50) Friability test: This test consists in measuring the loss of mass of the compressed solid composition after rotation in a drum at 25 revolutions/min for 2 minutes. This test is carried out using the FT2 machine supplied by SOTAX. The friability is determined according to the formula below:
F(%)=[(m1−m2)/(m1)]×100

(51) in which m1 corresponds to the mass of the composition before the rotation, and m2 to the mass of the composition after rotation.

(52) Disintegration: This test consists in measuring the disintegration time of the compressed solid composition in a liquid medium. The test is carried out by an apparatus that performs back-and-forth movements while fully submerged. For this purpose, the compressed solid composition is placed in a basket and undergoes 60 back-and-forth movements per minute in a vessel filled with water heated to 30° C.±1° C.

(53) The first back-and-forth movement corresponds to T.sub.0 and when there is no longer any compressed solid composition residue left in the basket, the time which has passed since T.sub.0 corresponds to the disintegration time. The disintegration time value is given in minutes and corresponds to the mean of 5 measurements.

(54) Hardness: The hardness is calculated using a Synergie 100 tensile testing machine (MTS) and the Test Works 4 software, and corresponds to the force required to break the compressed solid composition. The hardness is expressed in Newtons (N) and corresponds to the mean of 5 measurements.

(55) Dust content: The measurement is carried out using the DustMon L machine and the DustMon L software, according to the manufacturer's recommendations. The measurement consists in evaluating the concentration of dust of a mass of compressed solid composition when dropped, as it passes in front of a laser beam. The value is given in “dust area”.

(56) Solids content: Karl Fischer method.

Example 1: Preparation of a Compressed Solid Composition for Non-Oral Use, Comprising Fermented Molasses as Binder and/or Disintegrant

(57) For this example, the compressed solid composition is in the form of a multi-layer tablet composed of a first layer, an intermediate layer and a third layer.

(58) A mixture of fermented beet and cane molasses is used. The mixture contains approximately 90% of fermented beet molasses and approximately 10% of fermented cane molasses. The fermented molasses have a solids content of 60%. These fermented molasses then have carboxymethylcellulose added thereto at an amount (dry/dry) of 0.2%.

(59) The fermented molasses with carboxymethylcellulose added thereto are mixed at an amount (dry/dry) with other compounds in order to obtain the first and third layers of the tablet. The compositions of all the layers of the tablet are summarized below:

(60) TABLE-US-00002 Components % Layer 1 (6 g) Sequestrant 35 Fermented molasses with 0.5 substances added thereto Alkaline agent 40 Filler 10 Surfactant 5 Polymer 5 Dye 0.5 Pelletizing additive 4 100.00 Intermediate layer 2 (6 g) Sequestrant 50 Whitening agent 30 Surfactant 8 Polymer 9 Pelletizing additive 3 100.00 layer 3 (4 g) Sequestrant 32 Fermented molasses with 0.5 substances added thereto Alkaline agent 40 Filler 10 Polymer 5 Surfactant 5 Activator 3 Dye 0.5 Pelletizing additive 4 100.00

(61) Each composition is then compacted one to the other using a rotary press so as to obtain a compressed solid composition in the form of a multi-layer tablet.

(62) The mechanical properties of said tablet were measured according to the protocols described above and the results are presented in table 1 below:

(63) TABLE-US-00003 TABLE 1 Multi-layer tablet Friability (%) 7.1 Disintegration (min) 10 Hardness (N) 71 Dust content 1.7

(64) The compressed solid composition according to the invention has good mechanical properties and may thus be readily handled and transported without being broken or generating large amounts of fines. It also has a disintegration time which is compatible with applications in the field of cleaning, for which disintegration times of less than 12 min (based on the protocol described above) are generally desired.

Comparative Example 1: Preparation of a Compressed Solid Composition for Non-Oral Use, Comprising Polyethylene Glycol (PEG) as Binder and/or Disintegrant

(65) In order to compare the properties obtained and to demonstrate the advantage of the compressed solid compositions comprising fermented molasses as binder and/or disintegrant, a second multi-layer tablet was prepared.

(66) Polyethylene glycol is mixed at an amount (dry/dry) with other compounds in order to obtain the first and third layers of the tablet. The compositions of all the layers of the tablet are summarized below:

(67) TABLE-US-00004 Components % Layer 1 (6 g) Sequestrant 35 Polyethylene glycol 2 Alkaline agent 40 Filler 10 Surfactant 5 Polymer 3.5 Dye 0.5 Pelletizing additive 4 100.00 Intermediate layer 2 (6 g) Sequestrant 50 Whitening agent 30 Surfactant 8 Polymer 9 Pelletizing additive 3 100.00 Layer 3 (4 g) Sequestrant 32 Polyethylene glycol 2 Alkaline agent 40 Filler 10 Polymer 3.5 Surfactant 5 Activator 3 Dye 0.5 Pelletizing additive 4 100.00

(68) Each composition is then compacted according to the same protocol as example 1 using a rotary press so as to obtain a compressed solid composition in the form of a multi-layer tablet.

(69) The mechanical properties of said tablet were measured according to the same protocols as example 1 and the results are presented in table 2 below:

(70) TABLE-US-00005 TABLE 2 Comparative multi- layer tablet Friability (%) 3 Disintegration (min) 8 Hardness (N) 75 Dust content 2

(71) The mechanical properties obtained with “conventional” PEG-based compressed solid compositions are thus comparable with the compressed solid compositions according to the invention based on fermented molasses as binder and/or disintegrant.

(72) Thus, as demonstrated by this comparison, the use of fermented molasses according to the invention as binder and/or disintegrant is also a good alternative to the conventionally used chemical binders, while enabling a novel way to utilize a product hitherto solely intended for spreading or animal feed.

Example 2: Demonstration of the Binding Effect of the Fermented Molasses According to the Invention

(73) The aim of this example is to demonstrate the good binding properties of the fermented molasses according to the invention.

(74) A—Products Used: Carbon black: ENSACO® (Imerys); particle size distribution: Dv10=3.15 μm; Dv50=11.8 μm; Dv90=33.7 μm. Binder solution 1: fermented cane molasses having a solids content of 60%. Binder solution 2: mixture containing 90% fermented beet molasses and 10% fermented cane molasses, and having a solids content of 60%. Binder solution 3 (control): Bretax C (lignosulfonate, Burgo). Bretax C is a known commercially available binder.

(75) Each of the binder solutions is used so as to be sprayed onto the carbon black and enable the granulation thereof.

(76) B—Dry Granulation

(77) The carbon black is placed in the (51) vessel of a pilot shear mixer within which the stirring member is set to rotate.

(78) For each binder solution, an amount by weight of 5% by weight relative to the weight of the carbon black is sprayed inside the vessel using a bi-fluid nozzle so as to enable the granulation of the carbon black.

(79) The parameters of the pilot mixer are as follows: Linear speed: 14.1 m/s, Spraying rate: 5 g/min, Pulsed pressure: 0.1 bar.

(80) The different tests performed are summarized in table 3 below:

(81) TABLE-US-00006 TABLE 3 Mass of Mass of carbon Binder solution solution Duration of Tests black (g) sprayed sprayed (g) mixing (s) 1 300 Binder solution 1 15.8 282 2 300 Binder solution 2 15.8 280 3 300 Binder solution 3 15.8 252

(82) C—Particle Size Analyses:

(83) For each of the tests, the granules of carbon black obtained were analysed by laser particle size analysis in order to analyse the effect of each binder solution.

(84) Apparatus used for the measurement: Mastersizer 3000 (Malvern) Aero S accessory.

(85) Operation parameters: Dry route, Pressure: 0.5 bar, Blank measurement time: 30 seconds, Measurement time: 60 seconds.

(86) D—Results of the Particle Size Analyses:

(87) TABLE-US-00007 TABLE 4 Particle size parameter Dv10 (μm) Dv50 (μm) Dv90 (μm) Crude ENSACO ® 3.15 11.8 33.7 carbon black Test 1 3.87 15.5 44.9 Test 2 4.03 16.3 71.8 Test 3 3.73 15.5 43.2

(88) In comparison with a control binder solution, the results demonstrate that the fermented molasses according to the invention makes it possible to obtain a binding effect on the carbon black which is just as effective (test 1 vs test 3) or even more effective (test 2 vs test 3).

(89) This example thus demonstrates the very good binding properties of the fermented molasses according to the invention and the fact that the latter may advantageously be used in compressed solid compositions as binder.

Example 3: Demonstration of the Binding and Disintegrating Effect of the Fermented Molasses According to the Invention

(90) The fermented molasses is used in this example to granulate a powder of fermented cane molasses. The products used are summarized below:

(91) A—Products Used: Fermented cane molasses powder having a solids content of 97%. Fermented molasses 1: fermented cane molasses having a solids content of 60%. Fermented molasses 2: mixture of fermented beet and cane molasses. The mixture contains approximately 90% of fermented beet molasses and approximately 10% of fermented cane molasses. The fermented molasses has a solids content of 60%. This fermented molasses then has carboxymethylcellulose added thereto at an amount (dry/dry) of 0.2%.

(92) The fermented molasses 1 and 2 are used as binding and/or disintegrating composition on the fermented cane molasses powder. The fermented molasses are used to granulate the powder, and to thus obtain compressed solid compositions. The granules obtained were then analysed.

(93) B—Particle Size Analysis:

(94) Apparatus used for the laser particle size measurement: Mastersizer 3000 (Malvern), as above.

(95) The fermented cane molasses powder was analysed by laser particle size analysis and has the following characteristics: Dv10=18.1 μm, Dv50=77.5 μm, Dv90=234 μm, distribution width (span)=2.788.

(96) C—Tests Performed

(97) Test 1:

(98) For this test, the granulation is carried out on a wet granulator (model VG-25, GLATT), according to the following conditions:

(99) TABLE-US-00008 TABLE 5 Compressed air pressure (bar) 1.5 Pump setting Masterflex L/S 18 tubing 4 ml/min Mixer (rpm) 500 Grinder (rpm) 1000 Jacketed cryostat ° C. 15

(100) 1501.4 g of fermented cane molasses powder is placed within the granulator. The granulation is then carried out with 10% by weight of a liquid solution of molasses 1 relative to the weight of powder. The amount of solution sprayed is 150 g and the content of liquid solution of molasses 1 sprayed/crude fermented cane molasses powder is 10%.

(101) Analysis of the Granules Obtained:

(102) The granules obtained were analysed under the same conditions as the fermented cane molasses powder and have the following characteristics: Dv10=62.4 μm, Dv50=166 μm, Dv90=629 μm, distribution width (span)=3.442.

(103) In comparison with the powder, these particle size values show that the fermented molasses has a binding effect and makes it possible to obtain compressed solid compositions in granule form.

(104) Test 2:

(105) For this test, the granulator is the same as that of test 1 and the operating conditions are the same, with the exception of the mixer setting, which is set to 600 rpm.

(106) 1500 g of fermented cane molasses powder is placed within the granulator and the granulation is carried out with 5% of a liquid solution of molasses 2. The amount of solution sprayed is 75 g and the content of solution sprayed/crude cane molasses powder is 5%.

(107) Analysis of the Granules Obtained:

(108) The granules obtained were analysed under the same conditions as the fermented cane molasses powder and has the following characteristics: Dv10=55.4 nm, Dv50=127 nm, Dv90=305 nm, distribution width (span)=1.965.

(109) In comparison with the powder, these particle size values show that the fermented molasses has a binding effect and makes it possible to obtain compressed solid compositions in granule form. The distribution width here is less than the powder, reflecting a more centred size distribution of the particles of the granules.

(110) B—Wettability Test

(111) The wettability of the granules obtained in tests 1 and 2 is compared to that of the fermented cane molasses powder according to the following protocol: Place 100 ml of distilled water at 20° C. in a 400 ml beaker, Take 10 g of the sample and place it on the surface of the water at the same time as starting the timer, Stop the timer when the sample is entirely wetted.

(112) The results are presented below in table 6:

(113) TABLE-US-00009 TABLE 6 Duration (s) Fermented cane molasses powder 115 Granules of test 1 8 Granules of test 2 5

(114) The duration here expresses the time required by the different samples to succeed in passing the air/water interface.

(115) The results show that the granules obtained have a significant reduction in wettability. The fermented molasses according to the invention makes it possible to improve this parameter and thereby demonstrate the good binding properties.

(116) C—Disintegration Test

(117) The disintegration test is carried out on the granules obtained in the preceding tests 1 and 2 in order to highlight the disintegrating effect of the fermented molasses. The test is carried out according to the following protocol: Sample 10 g of the sample to be tested and sieve is to as to recover the 180-125 μm sieved fraction, Take the sieve comprising the 180-125 μm sieved fraction and place it above a 21 beaker, Add 400 ml of distilled water at 20° C. so that the sieve dips into the surface, Stir at approximately 300 rpm.

(118) The change in the weight of the combined mixture is monitored over time from as soon as the first m1 of distilled water are added. This makes it possible to reflect the decrease in the weight of the sample as a function of time.

(119) The results are presented in table 7 below:

(120) TABLE-US-00010 TABLE 7 Fermented cane molasses Granules Granules Time (s) powder of test 1 of test 2  10  3.1  1.4  20  2.7  30 − 0.5  1.2  50  0.3  60  −5.2 −1.7 −1.2  90  −8.4 −2.2 −3.1 120  −9.2 −2.9 −5.8 150 −10.5 −4.5 −6.7 180 −10.6 −5.2 −7.4 210 End of −5.9 −8.2 270 test (0 g) −6.6 −9.2 330 −7.4 End of 390 −7.9 test (0 g) 450 −8.5 510 End of test (0 g)

(121) The positive values at the start of the test reflect the absorption of water by the granules. Over time, the results show that, under the action of water, the granules obtained from the fermented molasses according to the invention may entirely disintegrate, thereby demonstrating the disintegrating effect of said fermented molasses.

(122) In conclusion, this example thus demonstrates the binding and disintegrating properties of the fermented molasses according to the invention. Indeed, the use thereof makes it possible to obtain compressed solid compositions in granule form, said granules being able to subsequently disintegrate under the action of water.