COMPOSITION COMPRISING A FIBROUS MATERIAL

Abstract

The present invention relates to solid compositions comprising a fibrous material of natural origin obtained from plants, wherein the fibrous material comprises micro-scaled and/or nano-scaled fibril agglomerates, and an alditol; a method to obtain such compositions; compositions obtained by this method, products comprising such compositions; and the use of such compositions as formulation aid in such products.

Claims

1. A solid composition comprising, a) a fibrous material of natural origin obtained from plants, said fibrous material containing more than 10 wt.-% xylose referred to the total weight of the fibrous material and the fibrous material comprising micro-scaled and/or nano-scaled fibril agglomerates, wherein i. the micro-scaled fibril agglomerates have an average length in the range of 500 nm-1000 μm, ii. the nano-scale fibril agglomerates have an average length in the range of 10 nm to 500 nm; and b) one or more alditols; wherein the BET specific surface area ratio of the solid composition re-dispersed in water to an aqueous suspension of the never dried fibrous material is higher than 0.75.

2. The solid composition according to claim 1, wherein the BET specific surface area of the solid composition re-dispersed in a liquid is larger than 125 m.sup.2/g.

3. The solid composition according to claim 1, wherein the fibrous material is obtained from plant pulp that has not been treated with any chemical reaction.

4. The solid composition according to claim 1, wherein the fibrous material is obtained from pulp of the Eucalyptus tree or of the Beech tree.

5. The solid composition according to claim 1, wherein the one or more alditols have a molecular weight less than 196 g/mol.

6. The solid composition according to claim 1, wherein the one or more alditols are of natural origin and obtained from plants.

7. The solid composition according to claim 1, wherein the solid composition is dispersible in a liquid selected from the group consisting of water, alcohols, oils and water-in-oil or oil-in-water emulsions, nano-emulsions and micro-emulsions.

8. The solid composition according to claim 1, wherein the alditol to fibrous material weight ratio is from 0.5 to 1.1.

9. The solid composition according to claim 1, wherein said solid composition, once dispersed in a liquid, at an effective concentration, forms a self-standing, gel-like material.

10. The solid composition according to claim 1, wherein said solid composition, once re-dispersed in water has a viscosity recovery after 300 s that is no less than 95%.

11. The solid composition according to claim 1, additionally comprising one or more polymeric additive.

12. The solid composition according to claim 1, additionally comprising one or more functional ingredients selected from the group consisting of cosmetic ingredients, personal care ingredients, drugs, dyes, nutraceuticals, fragrances and flavors, electrically conducting (nano)materials, dielectric (nano)materials, adhesives, adhesion promoters, tackifiers, surfactants different from cosmetic grade surfactants, emulsifiers, weighting agents, effervescent agents, and preservatives.

13. The solid composition according to claim 12, wherein the preservative is selected from the group consisting of sodium benzoate, potassium sorbate, benzoic acid, ethylhexyl glycerin (3-[(2-ethylhexyl)oxy]-1,2-propanediol, phenoxyethanol, pentandiol, dihydroxyacetic acid, salicylic acid, sorbic acid, benzyl alcohol, glyceryl caprylate/caprate, ethyl lauroyl arginate HCl (ethyl N2-dodecanoyl-L-argininate hydrochloride), gluconolactone, phenethyl alcohol, sodium levulinate, glyceryl caprylate, triethyl citrate, Rosmarinus officinalis (Rosemary) leaf extract, sorbitan caprylate and ([(1R)-1-[(3R,4S)-3,4-dihydroxyoxolan-2-yl]-2-hydroxyethyl] octanoate).

14. The solid composition according to claim 1, wherein the solid composition is in the form of extrudate, tablets, sponges, aerogels, xerogels, sheets, flakes, granules, pellets or powder.

15. A method to obtain a solid composition, the method comprising the steps of: a) Providing a suspension of a fibrous material of natural origin obtained from plants, wherein the fibrous material comprises micro-scaled and/or nano-scaled fibril agglomerates, wherein the micro-scaled fibril agglomerates have an average length in the range of 500 nm-1000 μm, wherein the nano-scale fibril agglomerates have an average length in the range of 10 nm to 500 nm, and wherein the fibrous material contains more than 10 wt.-% xylose referred to the total weight of the fibrous material; b) combining one or more alditols with the suspension provided in step a) in order to form a mixture; and c) Before or after step d), adding to the mixture obtained in step b) respectively to the mixture obtained in step d) one or more polymer additives, one or more functional ingredients or a combination thereof; and d) Drying the mixture by applying a drying method involving heat, electromagnetic waves and/or vacuum in order to form the solid composition.

16. The method according to claim 15, wherein the suspension of fibrous material is obtained by performing the steps of: a) comminuting dry pulp by mechanical means; b) dispersing said comminuted pulp in a liquid; and c) further comminuting the pulp dispersed in the liquid, wherein the dry pulp is comminuted without the substantial addition of a liquid.

17. The method according to claim 15, wherein the drying method is selected from the group consisting of dehydrating, convection oven drying, freeze drying, spray drying, drum drying, bed drying, spray coating, microwave drying, infrared drying, sunlight drying and combinations therefrom.

18. (canceled)

19. The solid composition according to claim 1, wherein the residual moisture in the solid composition is 35 wt.-% or less.

20. A solid product comprising a solid composition that comprises a) a fibrous material of natural origin obtained from plants, said fibrous material containing more than 10 wt.-% xylose referred to the total weight of the fibrous material and the fibrous material comprising micro-scaled and/or nano-scaled fibril agglomerates, wherein i. the micro-scaled fibril agglomerates have an average length in the range of 500 nm-1000 μm, ii. the nano-scale fibril agglomerates have an average length in the range of 10 nm to 500 nm; and b) one or more alditols; wherein the BET specific surface area ratio of the solid composition re-dispersed in water to an aqueous suspension of the never dried fibrous material is higher than 0.75, and wherein the product is soluble or dispersible in a liquid.

21. The solid product according to claim 20, wherein the solid product is an instant soup, an instant beverage, a fragrance booster, a jellifying composition, a peeling composition, a dry personal care product, a cement composition, a plaster composition, a concrete composition, an abrasive composition, an adhesive composition, a woven or non-woven sizing composition, or a paper sizing composition.

22. A liquid or gel-like product comprising a solid composition in dispersed form, the solid composition comprising a) a fibrous material of natural origin obtained from plants, said fibrous material containing more than 10 wt.-% xylose referred to the total weight of the fibrous material and the fibrous material comprising micro-scaled and/or nano-scaled fibril agglomerates, wherein i. the micro-scaled fibril agglomerates have an average length in the range of 500 nm-1000 μm, ii. the nano-scale fibril agglomerates have an average length in the range of 10 nm to 500 nm; and b) one or more alditols wherein the BET specific surface area ratio of the solid composition re-dispersed in water to an aqueous suspension of the never dried fibrous material is higher than 0.75.

23. The liquid or gel-like product according to claim 22, wherein the product is a home care product, or a personal care product.

24. The liquid or gel-like product according to claim 23, wherein the product is a personal care product comprising: a) from 0.1 to 30 wt. % of the solid composition; b) up to 25 wt. % of one or more polyols; c) up to 5 wt. % of one or more preservatives; d) one or more functional ingredient being different from the one or more polyols mentioned under b.) and different from the one or more preservatives mentioned under c); and e) liquid to complete to 100 wt.-%; wherein the weight percentage (wt.-%) refers to the total weight of the personal care product.

25. The liquid or gel-like product according to claim 24, wherein the one or more functional ingredients are selected from the group consisting of synthetic polymers, natural polymers, solvents, polyols, surfactants, fully or partially neutralized alpha-hydroxy acids, fully or partially neutralized beta-hydroxy acids, fully or partially neutralized dicarboxylic acids, fully or partially neutralized hyaluronic acid, C10-C24 fatty acids and their salts and their esters, C10-C24 fatty alcohols and their esters, glycerin ethoxylates, proteins and peptides, collagen, glycolipids, phospholipids, sphingolipids, sterols and steroids, allantoin, caffeine, amino acids and their derivatives, quaternary amines, alkaline bases, flavonoids and isoflavonoids, polyphenols, anthocyanins, organic dyes, pigments, vitamins and their derivatives, terpenes and their derivatives, sesquiterpenes and their derivatives, triterpenes and their derivatives, ubiquinones, waxes and butters, carbohydrates and sugar alcohols, and their derivatives, mineral and vegetal particulates, bentonites, diatomea earth, kaolin, titan dioxide, plant extracts, plant juices, essential oils and/or a perfumes.

26. Use of the solid composition according to claim 1 to improve the stability, and the rheological and mechanical properties of liquid products.

Description

DESCRIPTION OF THE FIGURES

[0101] FIG. 1 shows self-standing gels obtained from the aqueous suspension of the never dried fibrous material and from a solid composition re-dispersed in water according to the present invention at an active matter content of 3 wt.-%.

[0102] FIG. 2 shows a self-standing gel of solid composition 2.1 re-dispersed in glycerin at an active matter concentration of 3 wt.-%.

EXAMPLES

[0103] Example 1 Preparation of solid compositions according to the present invention and comparative example

[0104] A series of solid compositions were prepared by incorporating a known amount of dispersion agent into 500 ml of an aqueous suspension of never dried fibrous material comprising 3 wt.-% active matter (Celova®, ex Weidmann Fiber Technology by Weidmann Electrical AG), under high shear mixing during 5 minutes with a rotor-stator mixer (Ultra Turrax) operating at 10,000 rpm. About 150 to 200 g of these mixtures were placed in an aluminum tray and air dried in an oven at a temperature of 90° C. until the weight of the tray reached a constant value, in order to obtain a dry cake which was reduced in the form of a powder (variant 1). Another method for drying the mixtures was to immerse the aluminum tray in liquid nitrogen followed by freeze-drying (variant 2) in order to obtain flakes.

[0105] Sample 5.1 to 6.1 (comparative example) were prepared by employing various amounts of maltodextrin as dispersion agent. Maltodextrin was previously dissolved in water at a concentration of 20 wt.-%. The compositions of these samples are given in Table 1.

[0106] Samples 1.1 to 4.1 (examples according to the present invention) were prepared by employing various amounts of glycerin 99.8% or xylitol as dispersion agent. Furthermore, a known amount of xanthan gum (Rheocare XGN, ex BASF) was added to sample 3.1 after the dispersion agent was mixed with the aqueous suspension of never dried fibrous material. The compositions after drying of these samples are given in Table 1.

[0107] For sample 7.1 an aqueous suspension of never dried fibrous material was provided with an active matter content of 3 wt.-%.

TABLE-US-00001 TABLE 1 Solid compositions of samples 1.1 to 6.1 Solid Composition Drying Fibrous Xanthan Sample Method material Glycerin Xylitol gum Maltodextrin 1.1 Oven 1 0.75 1.2 Freeze 1 0.75 Drying 2.1 Freeze 1 1 Drying 3.1 Freeze 1 0.9 0.1 Drying 4.1 Oven 1 1 5.1 Freeze 1 1 Drying 6.1 Oven 1 1.5

TABLE-US-00002 TABLE 2 Composition of sample 7.1 Composition Sample Drying method Fibrous material Water 7.1 Never dried 3 97

Example 2 Measurement of the BET Specific Surface Area after Re-Dispersion in Water

[0108] A known amount of selected solid composition samples 1.1 to 6.1 were admixed with water with a glass stick and dispersed in water by using a rotor-stator mixer (Ultra Turrax) operating first at 9000 rpm for 3 minutes and then at 14000 rpm for 3 minutes. The sample 7.1 is an aqueous suspension of never dried fibrous material comprising 3 wt.-% of active matter so no re-dispersion in water was necessary for the BET specific surface area measurement.

[0109] The BET specific surface area of these samples was measured after having treated the samples as described hereinabove.

[0110] A parameter named “recovery” was calculated (Equation 2) from the measured data to easily compare the changes of the properties of the re-dispersed samples (1.1-6.1) to the properties of the never dried sample (7.1). The term “recovery” has been used in the application to define the change of the BET specific surface area as well as the change of viscosity in comparison to a suspension of never dried fibrous material. The term “recovery” could be also used for the comparison of other characteristic parameters of a dried and re-dispersed sample to the suspension of never dried fibrous material.

[00002]$\begin{array}{cc}\mathrm{Calculation}\mathrm{of}\mathrm{recovery}\mathrm{in}\mathrm{function}\mathrm{of}a\mathrm{specific}\mathrm{parameter}P\mathrm{for}\mathrm{never}\mathrm{dried}\mathrm{fibrous}\mathrm{material}\mathrm{as}\mathrm{well}\mathrm{as}\mathrm{the}\mathrm{solid}\mathrm{composition}.& \mathrm{Equation}2\end{array}$$\mathrm{Recovery}\left(P\right)\left[\%\right]=\frac{P\left(\mathrm{solid}\mathrm{composition}\right)}{P\left(\mathrm{never}\mathrm{dried}\mathrm{fibrous}\mathrm{material}\right)}\times 100\%$

[0111] In table 3, the recovery shows the change in the BET specific surface area of the aqueous suspension of never dried fibrous material to the re-dispersed samples 1.1-6.1. The recovery is the ratio of the BET specific surface area of the fibrous material comprised in the solid compositions re-dispersed in water to the BET specific surface area of the aqueous suspension of never dried fibrous material. The results are reported in Table 3.

TABLE-US-00003 TABLE 3 BET specific surface areas (SSA) of selected samples 1.1 to 6.1 after re-dispersion in water and of sample 7.1 as reference comprising the never-dried material. Sample SSA [m.sup.2/g] SSA Recovery [%] 1.1 250 85.0 1.2 293 99.7 2.1 251 85.4 3.1 304 103.4 4.1 264 91.0 5.1 220 74.8 6.1 179 60.9 7.1 294 —

[0112] Table 3 shows that the recovery of the BET specific surface area is much higher for samples comprising low molecular weight alditols (1.1-4.1) in comparison to samples comprising the currently known dispersion agent maltodextrin. Even at higher maltodextrin concentrations (6.1) the desired recovery of more than 75% cannot be reached.

Example 3 Impact of the BET Specific Surface Area of the Fibrous Material Comprised in the Solid Composition on the Stability of Emulsions

[0113] In this example, a series of emulsions have been prepared using samples 1.2, 6.1 and 7.1. The resulting emulsions are called Emulsion 1.2, Emulsion 6.1 and Emulsion 7.1 comprising a defined amount of active matter (Celova®, ex Weidmann). The composition of the formulations as well as the concentration of the active matter within the formulations are described in table 4.

[0114] In regard to the preparation of the emulsions described in table 4, following steps have been performed:

[0115] 1. Preparation of water phase A [0116] Weigh the solid compositions (samples 2.1 and sample 6.1) in deionized water in separate beakers accordingly. Weigh necessary amount of sample 7.1 in a third beaker. Beakers with water phase A are kept under stirring until the suspensions look homogeneous.

[0117] 2. Addition of water phase B to water phase A [0118] All ingredients of water phase B except deionized water are added to the beakers containing water phase A accordingly and are kept under stirring until the suspensions look homogeneous. Then deionized water was added to the beakers accordingly, again under continuous stirring and until homogeneous.

[0119] 3. Heating of water phase (A+B) [0120] The water phase A+B, prepared in step 2 is heated up to <75° C. while stirring.

[0121] 4. Preparation of oil phase [0122] Weigh the ingredients of oil phase in separate beakers. Prepare a water bath at 80° C. and place the beakers carefully and under stirring into the water bath so that no water enters the beaker until the oil phase has been melt and a clear liquid has been formed.

[0123] 5. Mixing of oil phase and water phase (A+B) [0124] The oil phase is added to the water phase (A+B) under continuous stirring to create whitish emulsions. Finally, the emulsion was homogenized at 4,000 rpm for 2 minutes.

TABLE-US-00004 TABLE 4 Cosmetic formulation used to test the impact of the BET specific surface area of the fibrous material comprised in the solid composition on the stability of known stable emulsion Concentration in wt.-% Emulsion Emulsion Emulsion Phase Ingredient name Supplier 1.2 6.1 7.1 Water A Deionized water — 39.1 34.7 Water A Solid composition sample 1.2 Weidmann 2.4 Water A Solid composition sample 6.1 Weidmann 6.8 Water A Reference sample 7.1 Weidmann 45.0 Water B Deionized water — 38.7 38.7 35.1 Water B Glycerine 99.8% — 1.8 1.8 1.8 Water B A-Leen 5 Minasolve 2.7 2.7 2.7 Oil Sunflower oil — 10.8 10.8 10.8 Oil Cutina GMS-SE BASF 4.5 4.5 4.5 100.0 100.0 100.0 Active matter in formulation [%] 1.35 2.7 1.35

[0125] The quality of the emulsions obtained was assessed by optical microscopy 48 hours after the preparation of the emulsions. It is known by a person skilled in the art that oil in water emulsions are expected to show a better long-term stability the smaller and the more homogeneous the droplet size distribution is. These images are reported in Table 5 as a function of the BET specific surface areas measured in Example 2.

[0126] The microscopic images in Table 5 demonstrate that the emulsions obtained by a suspension of never dried fibrous material (7.1) as well as by the solid composition comprising glycerin (1.2) show a small and homogeneous droplet size distribution. In comparison the emulsion obtained with sample 6.1, which was prepared with double the amount of active matter due to the low recovery of SSA and viscosity, shows no homogenous droplet size distribution and coalescence of droplets has occurred. These results show that the recovery plays an essential role in the quality of an oil in water emulsion.

Example 4 Impact of the BET Specific Surface Area of the Fibrous Material Comprised in the Solid Composition on Viscosity and Visco-Stability of Liquid Dispersions Comprising Dispersed Solid Compositions

[0127] The viscosity of selected solid composition samples was measured at 20° C. by using a viscometer IKA Rotavisc hi-vi I, equipped with a VAN-SP3 spindle operating at 1 rpm. Both the initial viscosity measured after 25 s and the variation of the viscosity over time (120 s, 300 s) were measured, in order to provide an estimate of the visco-stability of the dispersion.

[0128] The viscosity values, at t=30 s, t=120 s and t=300 s, are given in mPas in Table 6. Furthermore, the recovery of the viscosity of the re-dispersed solid composition in comparison to the suspension of never dried fibrous material (sample 7.1) is shown. As in Example 2, recovery is defined by the ratio between the viscosity of the solid composition re-dispersed in water to the viscosity of the suspension of never dried fibrous material at an equivalent active matter concentration of 2 wt.-%.

TABLE-US-00005 TABLE 6 Viscosity in mPas of selected samples that were re-dispersed in water as a function of time in comparison to the suspension of never dried fibrous material. Viscosity [mPas] Viscosity Recovery [%] after after after after after after Sample 30 s 120 s 300 s 30 s 120 s 300 s 1.1 149′800 134′820 105′930 108.0 107.7 108.8 1.2 180′830 167′990 141′070 130.3 134.2 144.9 2.1 194′740 172′270 136′960 140.4 137.6 140.7 3.1 182′970 177′620 173′340 122.1 131.7 163.6 4.1 192′600 167′990 146′590 138.8 134.2 150.5 5.1 132′680 112′350  83′460 95.6 89.7 85.7 6.1 110′210  95′230  70′620 79.4 76.1 72.5 7.1 138′740 125′190  97′370 — — —

[0129] Table 6 shows that only solid compositions comprising alditols (1.1-4.1) can preserve or even improve the viscosity in comparison to the reference sample (7.1). Samples comprising maltodextrin (5.1, 6.1) show lower viscosity values compared to the suspension of never dried fibrous material (7.1) at equivalent active matter concentration.

Example 5 Redispersion of Solid Composition in Glycerin

[0130] A known amount of solid composition 2.1 was re-dispersed in glycerin by mixing by hand. The mixture results in a self-standing gel-like material similar to the solid composition re-dispersed in water as shown in FIG. 2.