EP3717615A1

EP3717615A1 - Compressed solid composition for non-oral use

Info

Publication number: EP3717615A1
Application number: EP18808026.1A
Authority: EP
Inventors: Xavier LEBRUN
Original assignee: Lesaffre et Cie SA
Current assignee: Lesaffre et Cie SA
Priority date: 2017-12-01
Filing date: 2018-11-30
Publication date: 2020-10-07
Anticipated expiration: 2038-11-30
Also published as: RU2768832C2; PT3717615T; US11760961B2; JP2023134594A; FI3717615T3; RU2020121589A; EP3717615B1; HUE061352T2; CN110114451B; JP2021504535A; WO2019106190A1; PL3717615T3; FR3074500B1; CN110114451A; ES2941537T3; US20230374421A1; FR3074500A1; DK3717615T3; RU2020121589A3; US20210171879A1

Abstract

The present invention relates to a novel binder and/or disintegrating agent for obtaining a compressed solid composition for non-oral use, wherein said binder and/or disintegrating agent is fermented molasses, to a method for producing said compressed solid composition and also to a binding and/or disintegrating composition characterized in that it comprises at least fermented molasses. The fermented molasses according to the invention advantageously makes it possible to replace the synthetic binders conventionally used in compressed solid compositions while at the same time also making it possible to act as a disintegrating agent on contact with a liquid, in particular water. The present invention thus proposes a new route of exploitation of a product which thus far has only been used in the agricultural and livestock farming field.

Description

COMPRESSED SOLID COMPOSITION FOR NON-ORAL USE

The present invention relates to a novel binding and / or disintegrating agent for obtaining a compressed solid composition for non-oral use, as well as a process for preparing said compressed solid composition.

The compressed solid compositions may be in several forms generally conditioned by the intended use in order to obtain particular properties and to ensure optimal maintenance. For some applications, it is indeed important that a compressed solid composition has good integrity before use as well as the possibility of rapid disintegration during use, especially in contact with a liquid. These properties are generally provided by binding agents and / or disintegrants.

The use of binding agents makes it possible to increase the mechanical strength of the compressed solid compositions, also called agglomerates, to a level sufficient to avoid the problems of formation of fine particles during their handling or their implementation. The advantages of the use of a binding agent are generally noted for all known compression or agglomeration techniques, such as pressure-compaction, pelletisation, granulation, nodulisation, extrusion or the like. atomization. As for them, the disintegrating agents allow the compressed solid compositions which contain them to disintegrate in contact with a liquid, and in particular in contact with water.

Finally, some agents are termed binders and disintegrants because they make it possible to obtain in a dry medium a sufficient level of mechanical strength while also offering the possibility of disintegration during contact with a liquid.

In general, many binders are known to those skilled in the art. By way of example, mention may be made of polyvinyl alcohols and their derivatives, celluloses and their derivatives, lignosulphonates, starches and their derivatives, alkaline silicates, cement, clays and finally molasses by associating the latter with lime.

Polyvinyl alcohols and their derivatives, celluloses and their derivatives, starches and starches modified physically and / or chemically, have good binder properties and allow to obtain agglomerates which meet the requirements of agglomeration techniques but do not meet not necessarily economic requirements. In fact, the necessary use doses do not generally make it possible to obtain compressed agglomerates or solid compositions under satisfactory economic conditions.

SUBSTITUTE SHEET (RULE 26) Lignosulfonates have the disadvantage of being aggressive because of their pH and their composition vis-à-vis the means of agglomeration implemented. In addition, during the combustion or during the parboiling operations necessary during the compression processes, the lignosulfonates can cause the release of harmful vapors rich in sulfuric acid. It follows that lignosulphonates are a significant cause of air pollution and corrosion. In the context of developing greener products with reduced environmental impact, lignosulphonates should be avoided.

Clays are low-cost products with binding properties but their field of application is restricted. In addition, it is often necessary to associate them with other binders. By way of example, mention may be made of amylaceous derivatives.

As for the alkali silicates, they are of a delicate handling and their prolonged use requires frequent cleaning of the installations in which they are used.

The types of binding agents used in the compositions vary depending on the final application. For example, in the field of tablets and solid compositions for detergent use, the binders used are generally synthetic binders.

For example, the document EP 1 048 716 describes a laundry composition in the form of a tablet comprising in particular clay and a surfactant. The tablet is in the form of a compressed mass of particles held together by a binder having a dispersing effect on the clay less important than polyethylene glycol 6000 (PEG 6000). Specifically, the binder is a chemical binder selected from polyethylene glycols having a molecular weight of less than 1500, amine oxide and polyvinylpyrrolidone.

WO 2005/068603 discloses tablets with improved breaking strength and a method for making them. The method comprises a step of providing a binder having a shear modulus value G of 10 to 100 GPa, a phase angle value d of at least 7 degrees, and a boiling point of at least 45 ° C at atmospheric pressure. The method then comprises a step of heating the binder beyond its boiling point followed by a step of applying said heated binder to a powder comprising a premix of detergent compounds to form a detergent composition. The last step of the process consists in transforming the detergent composition into a tablet. The binder used is chosen from the group consisting of anionic surfactants, non-anionic surfactants, polymeric materials, polyols, saccharic acids, sugar alcohols, sugar esters, fatty acids, acid esters and the like. fatty acids, fatty acid amines and mixtures thereof.

SUBSTITUTE SHEET (RULE 26) In addition to the fact that they are of synthetic origin, another disadvantage of the available binding agents stems from their main advantage. Indeed, these agents make it possible to obtain aggregates by ensuring a cohesion such that it is generally not possible to disintegrate them by contact with a liquid such as water.

Thus, there is a need for new binding agents for the manufacture of compressed solid compositions for non-oral use, said binding agents being able to replace the synthetic binding agents conventionally used and also making it possible to act as disintegrating agents in contact with a liquid, especially water.

It is therefore the merit of the Applicant to have found that this objective could be achieved surprisingly, and against all odds, by means of molasses fermented whereas the latter was until now considered as a fermentation residue. 'having as only interest to be valued in the field of agriculture and breeding as fertilizer spreading or feed.

A first object of the invention relates to a compressed solid composition for non-oral use comprising fermented molasses as a binder and / or disintegrating agent.

In general, molasses is a substance known to those skilled in the art. It is a co-product of the production of sugar from sugar beet and sugar cane, or brown sugar from refineries. The process of manufacturing sugar, whether it is made from cane or beet, ends after the crystallization stage to obtain sugar on the one hand and molasses on the other hand. In general, it is generally accepted that sugar processes generate about 35 to 40 kg of molasses per ton of beet and 30 to 35 kg of molasses per tonne of cane. At the French national level alone, annual production amounts to several tens of thousands of tons.

In terms of composition, the dry matter content of molasses varies little and is commonly between 70% and 76%. Molasses have very low or no levels of raw celluloses and fat.

As a coproduct of sugar manufacture, molasses contain significant amounts of sugar. The total sugar content is essentially the same, regardless of the origin of the molasses, generally between 58% and 70% of the dry mass (DM), but has some variations according to the industrial process applied to beet molasses.

However, depending on the origin of molasses, beet or cane, if the sugar content is similar, the composition of these total sugars is very different. Thus, in beet molasses, almost all sugars are in the form of sucrose, whereas in the

SUBSTITUTE SHEET (RULE 26) cane molasses, sucrose represents only about 2/3 of the total sugars, ie 30% to 40% of the raw product.

Molasses is a very viscous substance which represents a disadvantage for its transport and storage. On the other hand, this high viscosity is an advantage for animal feed and is generally used to feed ruminants and horses, mixed with straw or other cellulosic foods such as bran, or as a binder in rations. complete, see again to encourage the ingestion of unpalatable food. Indeed, thanks to the presence of sugars, amino acids and salts, molasses is a food whose flavor and smell stimulate the appetite and promote the digestion of animals.

As an alternative to animal feed, molasses are also used by manufacturers for the production of so-called "noble" products via fermentation processes. Indeed, through the fermentation mechanisms available to certain microorganisms, molasses makes it possible to obtain baker's yeast, ethyl alcohol, citric and glutamic acids, lysine or antibiotics, and generates also liquid fermentation residues which correspond to fermented molasses.

Until now, fermented molasses has been considered as a fermentation residue whose only interest is to be valorized in the field of agriculture and animal husbandry as fertilizer or animal feed. . Indeed, the chemical composition of fermented molasses, despite a depletion of the compounds due to fermentation, still gives them an attraction in feeding ruminants both for their energy intake and their nitrogen value.

It is therefore the merit of the Applicant, by proposing a compressed solid composition for non-oral use comprising fermented molasses as a binding agent and / or disintegrating, to have unearthed a new way of valorization of fermented molasses in thus going against what was conventionally implemented for their use.

For the purposes of the present invention, the term "compressed solid composition" is intended to mean any composition obtainable by the compression methods known to those skilled in the art, such as, for example, pressure-compaction, pelletisation, granulation, nodulisation, extrusion or atomization. The compressed solid composition according to the invention can therefore also be considered as an agglomerate.

The compressed solid composition according to the invention may be in a multitude of compressed forms, said forms being conventionally adapted by those skilled in the art depending on the desired application. Thus, the compressed solid composition can occur

SUBSTITUTE SHEET (RULE 26) in the form of a single layer or multilayer tablet, a roller, a tablet, a granule, a pellet or a pellet. Preferably, the compressed solid composition is in the form of a single-layer or multilayer tablet.

For non-oral use is meant in the sense of the present invention that the compressed solid composition is not intended to be ingested by an animal or a human and therefore can not in particular support its diet.

For the purpose of clarification, the terms "compressed", "compressed", "compacted" or "agglomerated" are well regarded as synonyms within the meaning of the present invention and may be used interchangeably.

Fermented molasses is a co-product of the molasses obtained after fermentation of the latter by bacteria, yeasts or fungi, said fermentation making it possible to obtain so-called "noble" products such as baker's yeast, ethyl alcohol or citric and glutamic acid. Preferably, the fermented molasses is obtained via the fermentation of molasses by yeasts.

According to the invention, the fermented molasses can also 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% fermented beet molasses, up to 70% fermented beet molasses, up to 80% fermented beet molasses, up to 90% fermented beet molasses. or up to 95% fermented beet molasses. Advantageously, when the fermented molasses is a mixture of fermented molasses of beet and cane, said mixture contains 90% of fermented molasses of beet.

Initially, the fermented molasses contains more than 90% water but the latter is advantageously concentrated in order to reduce the quantity of water and to obtain higher solids content.

Thus, the solids content of the fermented molasses, or the mixture of beet molasses and cane molasses according to the invention can be from 50% to 80%. Preferably, the dry matter content of the fermented molasses is 55% to 75%, and more particularly 55% to 65%, for example about 60%.

Conventionally, since it is intended or used as a fertilizer or in animal feed, fermented molasses is also defined by its distribution in nitrogenous matter and by its aminogram. The fermented molasses according to the invention can thus have a distribution of nitrogenous materials as follows:

SUBSTITUTE SHEET (RULE 26) Nitrogen of total amino acids: 25% to 50% of total nitrogen

betaine nitrogen: 0% to 40% of total nitrogen

Ammonia nitrogen: 2% to 3% of the total nitrogen

As regards the aminogram of the protides of the fermented molasses according to the invention, the average amino acid contents can be as presented hereinafter, the ranges of the contents being given in g / kg of dry matter:

Aspartic acid: 6 - 8

Threonine: 0.5 - 3

Glutamic acid serine: 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

As a fermented by-product, fermented molasses has a low sugar content. By the term "low sugar content" is meant a fermented molasses comprising less than 5%, less than 4%, less than 3%, less than 2%, and more particularly less than 1% by weight of sugars per relative to the total mass of the dry extract. Preferably, the fermented molasses according to the invention is free of sugars.

The fermented molasses according to the invention, also referred to as raw fermented molasses, may undergo one or more chemical or physicochemical treatments. For example, fermented molasses may undergo de-packaging or demineralization. Such treatments can modify the nitrogenous composition of the fermented molasses. The de-assassification treatment consists, for example, of acidification of the crude fermented molasses with a solution of H ₂ SO ₄ , followed by neutralization with ammonia.

Treatments that can be applied to fermented molasses vary both qualitatively and quantitatively the mineral content. Thus, a crude fermented molasses can have a raw ash content of 14% to 22% by weight relative to the raw product and a

SUBSTITUTE SHEET (RULE 26) potassium from 5% to 18% by weight relative to the crude product. On the other hand, in the case of de-tasassified or demineralized fermented molasses, the raw ash content varies 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. .

Due to its high ash content, the raw fermented molasses has a density ranging from 1.10 to 1.50. Preferably, the density of the fermented molasses is from 1.20 to 1.40, and most preferably from 1.25 to 1.35.

The fermented molasses according to the invention has a viscosity of 500 mPa.s at 5000 mPa.s, preferably 1000 mPa.s at 4000 mPa.s, and a slightly acidic pH of 5 to 6.

The compressed solid composition according to the invention thus comprises crude fermented molasses or demineralized as a binding agent and / or disintegrating.

Said fermented molasses is present within the compressed solid composition in effective proportions. Effective proportions are understood to mean those which are sufficient to obtain the desired effect, namely to obtain a compressed solid composition which can in particular be transported, handled and / or stored without substantial damage and which may disintegrate during contact. with a liquid such as water.

Advantageously, the quantities used of fermented molasses raw or demineralized within the compressed solid composition according to the invention may be from 0.1% to 15% by weight, preferably from 0.5% to 5% by weight, and even more preferably from 0.5% to 1.5% by weight relative to the total weight of the compressed solid composition.

The binding properties thus brought to light of the fermented molasses make it possible to obtain a compressed solid composition having sufficient mechanical strength in order to avoid the problems of formation of fine particles during their handling. Advantageously, the fermented molasses also acts as a disintegrating agent allowing the compressed solid composition to disintegrate in contact with a liquid, and in particular in contact with water.

By means of the solid compositions compressed according to the invention, the inventors have thus identified a new way of valorization of fermented molasses but also an alternative to the use of synthetic or non-conventionally used binding agents for obtaining the compositions. solid. By way of example, mention may be made in particular of polyethylene glycol, polyvinylpyrrolidone, ethoxylated fatty alcohols, starch, hydroxyethylcellulose, gelatin or even microcrystalline cellulose.

SUBSTITUTE SHEET (RULE 26) Thus, the compressed solid composition comprising the fermented molasses according to the invention may be free of polyethylene glycol and / or polyvinylpyrrolidone and / or ethoxylated fatty alcohols and / or starch and / or hydroxyethylcellulose and / or gelatin and / or microcrystalline cellulose.

According to a particular embodiment, the fermented molasses can be adjuvanted in particular to present particular physical properties. Thus, the molasses may be adjuvanted with a compound selected from the group comprising cellulose derivatives such as carboxymethylcellulose, hemicelluloses, lignins, ethyl cellulose, methyl cellulose, hydroxypropyl cellulose, hydroxypropyl methylcellulose, derivatives thereof. of friend give as e starch of wheat, maize, cassava, tapioca, potato, rice, dextrins and other modified starches, dextrans, sugar derivatives like glucose, fructose, lactose, the sucrose, sucrose, sorbitol, glycerol, natural gums such as diutan, gelan, xanthan, carrageenan, pectins, alginates, chitosan, gum arabic, tragacanth, locust bean, acacia, agar agar, guar, production by-products such as beet pulp, chicory pulp, dried or uncooked apple pomace, sugarcane bagasse, citrus pulp, fruit juice waste, production waste of gums, starch wastes, mineral derivatives, smectites, bentonites and other silica-derived clays, lime, magnesia and the like from the same family as well as mixtures of several of these compounds. Preferably, the fermented molasses is adjuvanted with carboxymethylcellulose. The amounts of compounds for adjuvanting the fermented molasses can range from 0.1% to 2%, preferably from 0.1% to 1%, more preferably from 0.1% to 0.5%. The percentages being expressed by dry weight relative to the total dry weight of the fermented molasses adjuvanted.

The compressed solid composition may also include one or more additives. The additives may be selected from the additives known to those skilled in the art such as, for example, effervescent agents, detergents, sequestering agents, pelletizing additives, bleaching agents, polymers, surfactants, flow agents stabilizing agents, anti-foaming agents, coloring agents or lubricating agents.

As examples of stabilizing agents, mention may be made of parahydroxybenzoic acid esters such as methylparaben and propylparaben, alcohols such as chlorobutanol, benzyl alcohol and phenylethyl alcohol, phenols such as phenol and cresol, sulphite salts such as sodium bisulfite and sodium sulphite, edetic acid salts such as sodium edetate and tetrasodium edetate, and hydrogenated oils, sesame, chondroitin-sodium sulphate, dibutylhydroxytoluene, adipic acid,

SUBSTITUTE SHEET (RULE 26) ascorbic acid, L-ascorbate stearic acid esters, sodium L-ascorbate, L-aspartic acid, sodium L-aspartate, acetyltryptophan sodium, acetanilide, aprotinin solution, aminoethylsulfonic acid, aminoacetic acid, DL-alanine, L-alanine, benzalkonium chloride, sorbic acid.

By way of example of lubricating agents, mention may be made of stearic acids such as stearic acid, calcium stearate and magnesium stearate, waxes such as white beeswax and carnauba wax, sulphates such as sodium sulphate, silicic acid compounds such as magnesium silicate and light silicic anhydride, lauryl sulphates such as sodium lauryl sulphate, cocoa butter, carmellose calcium, carmellose sodium, callopeptide, hydrated silicon dioxide, hydrated amorphous silicon oxide, dry aluminum hydroxide gel, glycerin, light liquid paraffin, hydrogenated oil, synthetic aluminum silicate, sesame, wheat starch, talc, macrogols, phosphoric acid.

By way of example of a detergent agent, mention may be made of polyacrylates, acrylic / maleic copolymers, monomeric polycarbonates such as citrates, gluconates, oxydisuccinate, mono- and tri-succinates glycerols, carboxymethyloxysuccinates, carboxymethyloxymalonates, dipicolinates and hydroxyethyliminodiacetates.

According to a particular embodiment, the compressed solid composition may also comprise at least one active ingredient, at least one filler and optionally at least one additive that may be chosen from effervescent agents, detergent agents, sequestering agents and pelletizing additives. bleaching agents, polymers, surfactants, flow agents, stabilizing agents, anti-foaming agents, coloring agents or lubricating agents. According to this particular embodiment, the compressed solid composition may be in tablet form and finds application in the field of washing and / or household cleaning, agricultural and industrial. As an example of washing and / or household cleaning we can mention the washing machine such as washing in particular in a dishwasher.

According to one 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 especially of between 6% and 8%. .

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 between 60 N and 80 N, and especially between 70 N and 75 N .

SUBSTITUTE SHEET (RULE 26) 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 preferably less than 2.

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

According to another particular embodiment, the compressed solid composition comprising fermented molasses as a binding agent and / or disintegrant is in the form of an effervescent cleaning roller for toilets, dishwasher tablets, tablets calcium hypochlorite for pool, granulated fertilizer.

As examples of compressed solid composition that may be in the form of a multilayer tablet, and especially a multilayer dishwasher tablet, mention may be made of the composition given in the table below:

SUBSTITUTE SHEET (RULE 26)

Another object of the invention is the use of fermented molasses as a binding and / or disintegrating agent for the manufacture of a compressed solid composition for non-oral use.

The fermented molasses is as defined above. The use of fermented molasses as a binding and / or disintegrating agent in a compressed solid composition is doubly advantageous. On the one hand, the use according to the invention makes it possible to propose a new recovery route for molasses which until now was solely intended for spreading or for animal feed. On the other hand, the use according to the invention allows the substitution of synthetic binders conventionally used and thus obtain compressed solid compositions that are more respectful of the environment.

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

The compressed solid composition may be as defined above and may be in the form of a single-layer or multilayer tablet, a roller, a tablet, a granule, a pellet or a pellet. Preferably, the compressed solid composition is in the form of a single-layer or multilayer tablet.

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

The fermented molasses according to the invention can also be used as such in a binder and / or disintegrating composition containing one or more other constituents of any kind, including binding or suitable, for example, to increase the mechanical strength of the final product, in particular an agglomerate, or to minimize the phenomena of erosion that may be experienced by said agglomerate during its handling or storage. The fermented molasses is as defined above.

According to a particular embodiment, the binder composition according to the invention may also comprise a curing agent, that is to say able to further improve the binding power.

SUBSTITUTE SHEET (RULE 26) According to a particular embodiment, the fermented molasses can be adjuvanted in particular to present particular physical properties. Thus, the molasses may be adjuvanted with a compound chosen from the group comprising cellulose derivatives such as carboxymethylcellulose, lignins, hemicelluloses, ethyl cellulose, methyl cellulose, hydroxypropyl cellulose, hydroxypropyl methylcellulose, derivatives thereof. starch products such as starch from wheat, maize, cassava, tapioca, potato, rice, dextrins and other modified starches, dextrans, sugar derivatives such as glucose, fructose, lactose, sucrose, sucrose, sorbitol, glycerol, natural gums such as diutan, gelan, xanthan, carrageenan, pectins, alginates, chitosan, gum arabic, tragacanth, locust bean, acacia, agar agar, guar, production derivatives such as beet pulp, chicory pulp, dried or uncooked apple pomace, sugarcane bagasse, citrus pulp, fruit juice waste, gum production waste, the dec starch hoes, mineral drifts, smectites, bentonites and other silica-derived clays, lime, magnesia and the like from the same family as well as mixtures of several of these compounds.

Another subject of the invention relates to a method of manufacturing a compressed solid composition for non-oral use comprising the following steps:

1) supply of an active ingredient, a filler and optionally at least one additive chosen from effervescent agents, detergent agents, sequestering agents, pelletizing additives, bleaching agents, polymers, surfactants, flow agents, stabilizing agents, anti-foaming agents, coloring agents or lubricating agents.

2) incorporation of molasses fermented compounds provided in the previous step to obtain a mixture,

3) compacting said mixture to obtain said compressed solid composition.

The first step of the process therefore consists in providing an active material, a filler and optionally at least one additive chosen from effervescent agents, detergent agents, sequestering agents, pelletizing additives, bleaching agents, polymers, surfactants, flow agents, stabilizing agents, anti-foaming agents, coloring agents or lubricating agents. The active ingredient and the filler are selected by those skilled in the art depending on the desired application for the compressed solid composition.

The fermented molasses is then incorporated in a second step to the compounds provided according to the first step of the process so as to obtain a mixture. Fermented molasses is

SUBSTITUTE SHEET (RULE 26) as defined above, namely in particular the coproduct obtained by fermentation of molasses. The amounts of molasses to be incorporated according to this step may be from 0.1% to 15% by weight, preferably from 0.5% to 5% by weight, and still more preferably from 0.5% to 1.5% by weight. weight relative to the total weight of the mixture.

The incorporation step may be performed by techniques known to those skilled in the art which result in obtaining a mixture. Thus, the incorporation step may for example be obtained by spray age.

Finally, the third step of the process according to the invention consists of a compaction step that can be carried out according to the techniques known to those skilled in the art resulting in the compression or agglomeration of the mixture prepared in the previous step. Thus, the compacting step may for example be carried out by pressure-compaction on a rotary press, by pelletizing, by granulation, by nodulation, by extrusion or by atomization. For example, the compression-compaction compaction step can be implemented via a rotary press. The compacting step thus makes it possible to obtain a compressed solid composition that can be in several forms, for example a single-layer or multilayer tablet, a roller, a tablet, a granule, a pellet or a pellet.

The method according to the invention may also comprise a drying step after the incorporation and / or compaction step.

The invention will be better understood with the aid of the examples which follow, which are intended to be purely illustrative and in no way limit the scope of the protection.

EXAMPLES

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

Friability test: This test consists of measuring the loss of mass of the compressed solid composition after rotations in a drum at 25 rotations / min for 2 minutes. This test is implemented via the FT2 machine distributed by SOTAX. The friability is determined according to the formula below:

F (%) = [(ml-m2) / (ml)] x 100

in which ml corresponds to the mass of the composition before the rotations, and m2 to the mass of the composition after rotations.

Disintegration: This test consists in measuring the disintegration time of the compressed solid composition in a liquid medium. Fe test is implemented by an apparatus performing

SUBSTITUTE SHEET (RULE 26) movements back and forth in full immersion. To do this, the compressed solid composition is placed in a basket and is reciprocated per minute in a beaker filled with water heated to 30 ° C ± 1 ° C.

The first to-and-fro corresponds to T ₀ and when there is no more solid composition residue compressed in the basket, the time elapsed since T ₀ corresponds to the disintegration time. The value of the disintegration time is given in minutes, and corresponds to the average of 5 measurements.

Hardness: The hardness is calculated using a Synergie 100 traction machine (MTS) and Test works 4 software and corresponds to the force required to break the compressed solid composition. The hardness is expressed in Newton (N) and corresponds to the average of 5 measurements.

Dust rate: The measurement is carried out via the DustMon L machine and DustMon L software according to the manufacturer's recommendations. The measurement consists of evaluating the concentration of dust of a mass of compressed solid composition during its fall at the time of its passage in front of a laser beam. The value is given in dust area.

Dry matter content: Karl Fisher method

EXAMPLE 1 Preparation of a compressed solid composition for non-oral use comprising fermented molasses as a binder and / or disintegrant.

For this example, the compressed solid composition is in the form of a multilayer tablet composed of a first layer, an intermediate layer and a third layer.

A mixture of fermented molasses of beet and cane is used. The mixture contains about 90% fermented beet molasses and about 10% fermented cane molasses. Fermented molasses has a dry matter content of 60%. This fermented molasses is then adjuvanted with carboxymethylcellulose in an amount (dry / dry) of 0.2%.

The adjuvanted fermented molasses is mixed in an amount (dry / dry) with other compounds to obtain the first and third layer of the tablet. The compositions of all the layers of the tablet are listed below:

SUBSTITUTE SHEET (RULE 26)

Each composition is then compacted one on the other by means of a rotary press so as to obtain a compressed solid composition in the form of a multilayer tablet.

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

TABLE 1

SUBSTITUTE SHEET (RULE 26) The compressed solid composition according to the invention has good mechanical properties and can thus be easily handled and transported without breaking or generating significant amounts of fines. It also has a disintegration time compatible with applications in the cleaning field for which disintegration times of less than 12 min (based on the protocol described above) are generally sought.

COMPARATIVE EXAMPLE 1 Preparation of a compressed solid composition for non-oral use comprising polyethylene glycol (PEG) as a binding and / or disintegrating agent.

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

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

SUBSTITUTE SHEET (RULE 26)

Each composition is then compacted according to the same protocol as Example 1 by means of a rotary press so as to obtain a solid composition compressed in the form of a multilayer tablet.

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:

TABLE 2

The mechanical properties obtained with compressed solid compositions called "classical" PEG-based, are comparable with the solid compositions compressed according to the invention based on fermented molasses as binding agent and / or disintegrating.

Thus, as demonstrated by this comparison, the use of fermented molasses according to the invention as a binder and / or disintegrant is also a good alternative to the chemical binders conventionally used while allowing a new product recovery route. until then only intended for spreading or animal feeding.

EXAMPLE 2 Demonstration of the binding effect of the fermented molasses according to the invention.

The purpose of this example is to demonstrate the good binding properties of fermented molasses according to the invention.

A- Products used:

Carbon Black: ENSACO® (Imerys Company); Granulometry: Dv10 = 3.15 mih Dv50 = 11.8 mih; Dv90 = 33.7 mih.

Binder solution 1: fermented cane molasses with a solids content of 60%.

SUBSTITUTE SHEET (RULE 26) Binder solution 2: a mixture containing 90% fermented beet molasses, 10% fermented cane molasses and having a solids content of 60%. Binder solution 3 (control): Bretax C (lignosulfonate, Burgo Company). Bretax C is a known binder of the market.

Each of the binder solutions is used to be sprayed onto the carbon black and allow it to granulate.

B- Dry granulation

The carbon black is disposed in the tank (5L) of the pilot shear mixer in which the stirring member is rotated.

For each binder solution, a mass quantity of 5% by weight relative to the weight of the carbon black is sprayed inside the vessel by means of a bi-fluid nozzle so as to allow the granulation of the carbon black.

The parameters of the pilot mixer are as follows:

Linear speed: 14.1 m / s,

- Spray rate: 5 g / min,

Pulsed pressure: 0, 1 bar.

The various tests carried out are shown in Table 3 below:

TABLE 3

C - Granulometric analyzes:

For each of the tests, the obtained carbon black granules were analyzed by laser granulometry to analyze the effect of each binder solution.

Apparatus used for the measurement:

Mastersizer 3000 (Malvern Company)

Accessory Aero S.

Operational parameters:

Dry way,

Pressure: 0.5 bar,

FIRE I LLE OF REM PLACEM ENT (RULE 26) White measurement time: 30 seconds,

Measurement time: 60 seconds.

D - Results of granulometric analyzes:

TABLE 4

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

This example thus demonstrates the very good binding properties of the fermented molasses according to the invention and the fact that the latter can advantageously be used in compressed solid compositions as a binding agent.

EXAMPLE 3 Demonstration of the binding and disintegrating effect of the fermented molasses according to the invention.

Fermented molasses is used in this example to granulate a fermented cane molasses powder. The products implemented are listed below:

A - Products used:

- fermented cane molasses powder with a dry matter content of 97%.

Fermented molasses 1: fermented cane molasses with a solids content of 60%.

Fermented molasses 2: mixture of fermented molasses of beet and cane. The mixture contains about 90% fermented beet molasses and about 10% fermented cane molasses. Fermented molasses has a dry matter content of 60%. This fermented molasses is then adjuvanted with carboxymethylcellulose in an amount (dry / dry) of 0.2%.

SUBSTITUTE SHEET (RULE 26) Fermented molasses 1 and 2 are used as a binder and / or disintegrating composition on fermented cane molasses powder. The fermented molasses are used to granulate the powder and thus obtain compressed solid compositions. The granules obtained were then analyzed. B - Granulometric analysis:

Apparatus used for the measurement of laser granulometry: Mastersizer 3000 (Malvern Company) as previously.

The fermented cane molasses powder has been analyzed by laser granulometry and has the following characteristics:

- Dv10 = 18.1 mih,

Dv50 = 77.5 mih,

- Dv90 = 234 mih,

distribution width (span) = 2,788.

C - Tests performed

Trial 1:

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

TABLE 5

1501.4 g of molasses powder fermented cane is disposed 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 rate of liquid molasses solution 1 spray / fermented raw cane molasses powder is 10%.

Analysis of the granules obtained:

The granules obtained were analyzed under the same conditions as the fermented cane molasses powder and have the following characteristics:

Dv10 = 62.4 mih,

Dv50 = 166 pm,

SUBSTITUTE SHEET (RULE 26) Dv90 = 629 mih,

distribution width (span) = 3,442.

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

Trial 2:

For this test, the granulator is the same as that of test 1 and the operating conditions are the same except for the setting of the mixer which is set at 600 U / min.

1500 g of fermented cane molasses powder is placed in the granulator and the granulation is carried out with 5% of a molasses liquid solution 2. The quantity of solution sprayed is 75 g and the proportion of spray solution / powder of raw cane molasses is 5%.

Analysis of the granules obtained:

The granules obtained were analyzed under the same conditions as the fermented cane molasses powder has the following characteristics:

Dv10 = 55.4 mih,

Dv50 = 127 mih,

Dv90 = 305 mih,

distribution width (span) = 1.965.

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

B - Wettability test

The wettability of the granules obtained in tests 1 and 2 is compared with 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 while launching the stopwatch,

- Stop the stopwatch when the sample is completely wet.

The results are shown below in Table 6:

TABLE 6

SUBSTITUTE SHEET (RULE 26) The duration here expresses the time required for the different samples to arrive at the passage of the air / water interface.

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

C - Disintegration test

The disintegration test is carried out on the granules obtained in test 1 and 2 above in order to highlight the disintegrating effect of fermented molasses. The test is carried out according to the following protocol:

- Take 10 g of the sample to be tested and sieve it so as to recover the sieved fraction 180-125 mih.

Take the sieve including the sieved fraction 180-125 mih and place it on top of a 2 L beaker,

Add 400 mL of distilled water at 20 ° C so that the screen soaks on the surface, - Agitate at about 300 rpm.

The evolution of the weight of the whole is followed over time as soon as the first mL of distilled water is added. This makes it possible to translate the decrease in the weight of the sample as a function of time.

The results are shown in Table 7 below:

TABLE 7

SUBSTITUTE SHEET (RULE 26) The positive values at the beginning of the test reflect the water absorption of the granules. Over time, the results show that under the action of water, the granules obtained from the fermented molasses according to the invention can completely disintegrate, thus demonstrating the disintegrating effect of said fermented molasses.

In conclusion, this example thus demonstrates the binding and disintegrating properties of the fermented molasses according to the invention. Indeed, its implementation allows to obtain compressed solid compositions in the form of granules, said granules can then disintegrate under the action of water.

SUBSTITUTE SHEET (RULE 26)

Claims

A compressed solid composition for non-oral use characterized in that it comprises fermented molasses as a binding and / or disintegrating agent.

2. Compressed solid composition for non-oral use according to claim 1, characterized in that fermented molasses is obtained by fermentation of beet molasses, cane molasses or a mixture of molasses of beet and cane.

3. Compressed solid composition for non-oral use according to claims 1 or 2, characterized in that the fermented molasses has a solids content of between 50% and 80%.

Compressed solid composition for non-oral use according to one of claims 1 to

3, characterized in that the fermented molasses comprises less than 5%, and preferably less than 1% by weight of sugars relative to the total mass of the dry extract.

5. Compressed solid composition for non-oral use according to one of claims 1 to

4, characterized in that the fermented molasses is adjuvanted with carboxymethylcellulose.

6. Compressed solid composition for non-oral use according to claim 5, characterized in that the amount (dry / dry) of carboxymethylcellulose is from 0.1% to 2%, preferably from 0.1% to 1%, more preferably from 0.1% to 0.5%.

7. Compressed solid composition for non-oral use according to one of claims 1 to

6, characterized in that the fermented molasses has a viscosity of 500 to 5000 mPa.s.

Compressed solid composition for non-oral use according to one of claims 1 to

Characterized in that it comprises an active material, a filler and optionally at least one additive chosen from effervescent agents, detergent agents, sequestering agents, pelletizing additives, bleaching agents, polymers, surfactants, flow agents, stabilizing agents, anti-foaming agents, coloring agents and lubricating agents.

9. Compressed solid composition for non-oral use according to one of claims 1 to

8, characterized in that it is in the form of a single layer or multilayer tablet, a roller, a tablet, a granule, a pellet or a pellet.

10. Compressed solid composition for non-oral use according to one of claims 1 to

9, characterized in that it is free of polyethylene glycol and / or microcrystalline cellulose and / or polyvinylpyrrolidone and / or starch, and / or hydroxyethylcellulose and / or gelatin.

11. Use of a compressed solid composition for non-oral use according to one of claims 1 to 10 for washing in a dishwasher.

12. Use of fermented molasses as a binding and / or disintegrating agent for the manufacture of a compressed solid composition for non-oral use.

13. Use according to claim 12, characterized in that the fermented molasses is present in the compressed solid composition for non-oral use in an amount by weight of 0.1% to 15% relative to the total weight of the composition.

14. Binder and / or disintegrating composition characterized in that it comprises at least molten fermented as binding agent.

A method of making a compressed solid composition for non-oral use comprising the steps of:

supply of an active ingredient, a filler and optionally at least one additive chosen from effervescent agents, detergent agents, sequestering agents, pelletizing additives, bleaching agents, polymers, surfactants, agents flow, stabilizing agents, anti-foaming agents, coloring agents or lubricating agents,

incorporation of fermented molasses with the compounds provided in the previous step in order to obtain a mixture,

compacting said mixture to obtain said compressed solid composition.

16. The manufacturing method according to claim 15, characterized in that the incorporation step is carried out by spray.

17. The manufacturing method according to claim 15 or 16, characterized in that the compaction step is performed on a rotary press.