Classifications

• • C—CHEMISTRY; METALLURGY
  • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
  • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
  • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
• • C—CHEMISTRY; METALLURGY
  • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
  • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
  • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
  • C11D3/02—Inorganic compounds ; Elemental compounds
  • C11D3/12—Water-insoluble compounds
  • C11D3/124—Silicon containing, e.g. silica, silex, quartz or glass beads
  • C11D3/1246—Silicates, e.g. diatomaceous earth
  • C11D3/128—Aluminium silicates, e.g. zeolites
  • C11D3/1286—Stabilised aqueous aluminosilicate suspensions

Definitions

• the present invention relates to stable aqueous suspensions of zeolites.
• zeolites in detergency are well known. This use has developed in particular as a result of the at least partial substitution of zeolites for phosphates in detergents. They have been criticized, in fact, for causing eutrophication of the waters and therefore for posing ecological problems.
• Zeolites are generally used in the form of aqueous suspensions or slurries which can for example be introduced into detergent slurries which can then be atomized.
• the main object of the invention is therefore a means of obtaining an aqueous suspension of zeolite which is stable, that is to say which no longer sediments or only very shortly after several days of storage.
• a second object of the invention is a means of obtaining an aqueous suspension of zeolite which is not only stable, but which, moreover, is pumpable, that is to say which has a viscosity suitable for industrial use.
• the suspensions according to the invention comprise zeolites and they are characterized in that they also comprise a succinoglycan.
• the aqueous suspensions of zeolites further comprise a dispersant which is a siliconate and / or one of its derivatives.
• the aqueous suspensions of zeolites further comprise a dispersant which is a silicone resin.
• the zeolites used in the context of the present invention include crystalline, amorphous and mixed crystalline-amorphous, natural or synthetic zeolites.
• finely divided zeolites are used having an average diameter of primary particles of between 0.1 and 10 ⁇ m and, advantageously, between 0.5 and 5 ⁇ m, as well as a theoretical cation exchange power greater than 100 mg of CaCO3 / g of anhydrous product and preferably greater than 200 mg.
• Use is also more particularly made of zeolites of type A, X or Y and in particular 4A and 13X.
• zeolites obtained by the processes described in the French patent applications in the name of the Applicant No. 2,376,074, 2,384,716, 2,392,932, 2,528,722, the teaching of which is also incorporated herein request.
• the last reference cited refers in particular to zeolites having a speed constant, related to the surface of the zeolites per liter of solution greater than 0.15 s ⁇ 1.lm ⁇ 2, preferably greater than 0.25 and advantageously between 0.4 and 4 s ⁇ 1.lm ⁇ 2.
• These zeolites have particularly advantageous qualities in the use in detergency.
• the suspensions may have a variable zeolite concentration depending on the application. In detergency, this concentration is generally between 40 and 51% by weight.
• the pH of the suspensions is also a function of their use. Still in the detergency application, this pH expressed at 1% by weight of dry zeolite is approximately 11.
• succinoglycan is used as a stabilizing agent for zeolite suspensions.
• a succinoglycan is a polysaccharide containing succinic acid and galactose and glucose as sugars.
• the succinoglycans are generally obtained by fermentation of a medium comprising at least one carbon source assimilable by a strain or a recombinant or a mutant of this strain of the type given below: - Pseudomonas, in particular of origin NCIB 11592 - Rhizobium meliloti, in particular of origin U-27, 1021, SU-27, SU-4, SU-231, SU-255, SU-256, K 24 (R 13), A 148 (R 15), J 7017 - Rhizobium trifolii, in particular of origin J-60W - Alcaligenes faecalis of myxogenic varieties, in particular of origin 10C3,22-33 - Agrobacterium radiobacter, in particular of origin IFO 13533 - Agrobacterium rhizogenes, in particular of IFO 13259 origin - Agrobacterium tumefaciens, in particular of origin IFO 3058, A-8, A-10.
• a succinoglycan is chosen from the group of those which, after having passed the transition temperature, have an intrinsic viscosity of at least 14,000 ml / g and more particularly of at least 15,000 ml / q.
• This intrinsic viscosity is determined by the extrapolation at zero concentration of the reduced specific viscosity curve.
• succinoglycans obtained from an Agrobacterium tumefaciens I-736 strain one of its recombinants or one of its mutants.
• Agrobacterium tumefaciens strain was deposited in accordance with the Budapest Treaty with the National Collection of Culture of Microorganisms (CNCM), on March 1, 1988, where it is publicly accessible under number 1736. This strain comes from the National Collection of Phytophathogenic Bacteria and is listed under number CNBP 291 in the 1974 catalog of the curator.
• the pure culture of Agrobacterium tumefaciens I-736 can be carried out in an inclined agar tube (slant) incubated at a temperature between 26 and 32 ° C, and more generally between 28 and 32 ° C.
• the following maintenance media were considered particularly advantageous for the cultivation of Agrobacterium tumefaciens I-736: - MY Agar medium (in g / l) Soy-Peptones 5 Yeast extract 3 Malt extract 3 Glucose 10 Agar 20 - TGY Agar medium (produced by the Pasteur Institute (in g / l) Peptones 5 Yeast extract 2.5 Glucose 1 Agar 20 - Middle Bennett Agar (in g / l) Peptones 1 Meat extract 1 NZ Amine A R 2 (Produced by Sheffield Chemical Co.) Glucose 10 Agar 20 - TS Agar medium (produced by Sté Bio Mérieux) (in g / l) Bio trypcase 17 Bio soyase 3 K2HPO4 2.5 NaCl 5 Glucose 2.5 Agar 20
• the Agrobacterium tumefaciens I-736 strain can also be cultivated in a Petri dish, for example on MY agar or TGY agar medium. Under these conditions, the colonies are visible from 24 to 30 hours, and have the following characteristics, at 48 hours: - cut ; 2 to 3 mm in diameter - smooth and slightly curved appearance - very light brown-yellow color - colonies with a clear edge and less mucoid on a Petri dish than on a slant.
• the Agrobacterium tumefaciens I-736 strain can use the following sugars: - glucose - sucrose - starch hydrolysates and optionally native starch and lactose.
• Glucose and sucrose are preferred sugars.
• succinoglycan obtained from this strain comprises units derived from glucose, galactose and pyruvic, succinic and acetic acids or salts of these acids, generally in proportions molars respectively of 5-8 / 1-2 / 0.5-2 / 0.5-2 / 0.05-2 preferably of 6 -7.5 / 1 - 1.5 / 0.5 - 1/0 , 5 - 1 / 0.05-0.2 and more preferably still from 7/1 / 0.5 - 1 / 0.5 - 1 / 0.05 - 0.1.
• Said pyruvic, succinic and acetic acids are generally in the form of salts such as sodium, potassium, calcium or ammonium salts.
• succinoglycan The methods of analysis of succinoglycan which have made it possible to determine its crude formula as specified above, have as a principle the determination of the constituent elements (sugars and acids) after hydrolysis of said succinoglycan and chromatographic assays by internal or external calibration.
• succinoglycan are hydrolyzed in hermetic tubes with 5 ml of molar trifluoroacetic acid at 105 ° C for three to six hours.
• the sugar dosage is then carried out by gas chromatography with F.I.D detection, on a capillary glass column 25 m long and 0.25 mm in diameter, loaded with methylsilicone phase having a film thickness of 0.14 ⁇ .
• the carrier gas used is hydrogen, with a flow rate of 2 ml / minute.
• the dosage of pyruvic acid is carried out from a stock solution obtained by hydrolysis of 80 mg of succinoglycan using 5 ml of 4N hydrochloric acid for 1 hour at 105 ° C., then addition of 2 mg of acid ketoglutaric (constituting the internal standard) and adjustment to 25 ml by distilled water.
• the assay is then carried out by High Performance Liquid Chromatography (HPLC) using a column loaded with C18 grafted silica of 5 ⁇ in diameter, the length of which is 250 mm and the diameter of 4.6 mm.
• the eluent used is a 50/50 mixture by volume of 0.02 M phosphoric acid and acetonitrile.
• the flow rate is 1.5 ml / minute.
• the detection of pyruvic acid is done by Ultraviolet at 375 nm.
• the determination of succinic acid is carried out after hydrolysis of the succinoglycan under the same conditions as those used for the determination of pyruvic acid.
• the assay is direct, by external calibration.
• the standard succinic acid solution used contains 8 mg of succinic acid in 25 ml of water.
• the HPLC technique is again used on Aminex HPX87H R columns from BIORAD R.
• the eluent is 0.01 N sulfuric acid, and the flow rate is 0.8 ml / minute.
• the detection of succinic acid is refractometric.
• acetic acid is carried out after hydrolysis of 300 to 350 mg of succinoglycan with 5 ml of 4 N trifluoroacetic acid at 120 ° C for three hours. Then 30 mg of propionic acid is added as an internal standard and assayed by gas chromatography with FID detection
• a glass column 2 m long and 3 mm in diameter is used, filled with 5% FFAP phase and 1% phosphoric acid absorbed on chromosorb G R (AW DMCS) from 80 to 100 mesh.
• the carrier gas is helium with a flow rate of 30 ml / minute.
• succinoglycans of the family described above generally also have the following properties:
• Their intrinsic viscosity is between 3000 and 25000 ml / g and more particularly between 14000 and 25000 ml / g and preferably between 15000 and 24000 ml / g.
• the intrinsic viscosity ( ⁇ ) as specified is determined by extrapolation at zero concentration of the reduced viscosity formula in which: - ⁇ is the viscosity of the solution on the Newtonian plateau - ⁇ o is the viscosity of the solvent and - C is the succinoglycan concentration, using the Huggins equation; k ′ being Huggins constant on the 1st Newtonian plateau
• the specific viscosity is measured as follows:
• a stock solution of 0.2 g / l of succinoglycan is prepared in a 0.1 M NaCl aqueous solution.
• succinoglycan at concentrations between 0.03 and 0.1 g / l by dilution of the mother solution with the 0.1 M Nacl aqueous solution.
• the measurements are then carried out at 23 ° C. using a LOW SHEAR viscometer.
• the specific viscosity curve is plotted as a function of the concentration and extrapolated to zero concentration.
• the molecular weights of these succinoglycans measured by light scattering are generally between 6.106 and 10.106, preferably between 6.5.106 and 9.5.106.
• succinoglycans also have very good rheological properties in solution in distilled water, especially at low concentrations.
• solutions at 0.1% by weight of a succinoglycan of this type in distilled water at 25 ° C have viscosities at 24 hours greater than 400 mPa.s and more particularly between 400 and 700 mPa.s; the viscosities being measured at a speed gradient of 1 s ⁇ 1 using a LOW SHEAR viscometer.
• aqueous solutions of one of these succinoglycans at pH 1.7 and at 25 ° C., have a viscosity at 24 hours of between 1000 and 2500 mPa.s, more particularly between 1400 and 2000 mPa.s, the viscosities being measured using a LOW SHEAR viscometer, at a speed gradient of 1 s ⁇ 1.
• succinoglycans from the Agrobacterium tumefaciens I-736 strain can be obtained by a process which will be described in more detail below.
• succinoglycans result from the fermentation by the aforementioned strain of a medium comprising at least one assimilable carbon source.
• the medium is conventionally innoculated by the Agrobacterium tumefaciens I-736 strain.
• the volume of the fermentation medium When the volume of the fermentation medium is large, it can advantageously be inoculated by means of an innoculum medium, seeded with a liquid preculture medium; the latter being previously seeded itself by a pure culture of Agrobacterium tumefaciens I-736.
• any medium conventionally used for this purpose can be used, and advantageously a medium of a mineral nature.
• organic source of carbon constituting the fermentation medium there may be mentioned sugars such as glucose, sucrose, starch hydrolysates, and optionally lactose or native starch, as well as mixtures of these sugars. Glucose and sucrose are preferred sugars.
• the concentration of organic carbon source in the fermentation medium can be between 1 and 100 g / l and preferably between 15 and 60 g / l.
• the fermentation medium can also contain at least one nitrogen source, preferably a source of organic nitrogen and optionally one or more mineral salts.
• the concentration of nitrogenous organic source in the fermentation medium can be between 3 and 80 g / l and preferably between 5 and 50 g / l.
• mineral salts which may optionally be introduced into the fermentation medium, of the sulfates such as magnesium, manganese, zinc, iron sulfates, carbonates such as calcium carbonate, the salts soluble calcium, phosphates such as potassium, sodium phosphates.
• the concentration of each of these mineral salts in the fermentation medium can vary between 0.01 and 5 g / l and preferably between 0.05 and 2 g / l.
• the fermentation medium can also contain trace elements such as traces of cobalt and / or molybdenum salts, as well as vitamins and nucleotides.
• Fermentation can be carried out at pressures between 1 and 4 bar at a temperature between 25 and 35 ° C, preferably between 28 and 32 ° C, under submerged aerobic conditions.
• the pH of the fermentation medium can be between 5 and 9 and preferably between 6 and 8.
• the pH can be adjusted, as the case may be, with a base such as soda or potash or with an acid such as acid sulfuric, phosphoric acid, hydrochloric acid or nitric acid.
• the fermentation medium placed for example in a fermentation tank or container, can advantageously be subjected to stirring.
• This agitation can be exercised for example by means of a reciprocal shaker, a gyratory shaker, a stirring mobile or a bubble column.
• the fermentation time is usually more than 30 hours, but is generally between 40 and 90 hours.
• Fermentation yields are generally greater than 40%, more particularly between 55-75% and very particularly between 60 and 75% by weight of succinoglycan produced relative to the carbon source used.
• the succinoglycan can be separated from the fermentation medium.
• the fermentation must containing the succinoglycan can advantageously be heated to temperatures between 80 and 120 ° C, for 10 to 60 minutes and preferably between 15 and 45 minutes.
• the must subjected to the above heat treatment advantageously has a pH of between 6 and 8.
• this pH can be adjusted if necessary, with a base or an acid as appropriate.
• the latter can be chosen from the bases and the acids mentioned above used for adjusting the pH of the fermentation medium.
• Suitable organic liquids according to the present invention of acetone, alcohols such as ethanol, propanol, isopropanol, butanol and tert-butanol.
• Isopropanol is more particularly preferred in the context of the present invention.
• the volume of organic liquid used is generally 2 to 3 times that of the volume of must to be treated.
• the precipitation of succinoglycan by an organic liquid can also be carried out in the presence of salts such as sulfates, chlorides or phosphates of sodium, potassium, or calcium.
• succinoglycan once precipitated, can then be separated from the organic liquid by filtration, centrifugation or spinning.
• the fibers obtained can be dehydrated, for example using acetone or an alcohol such as ethanol, propanol, isopropanol or tert-butanol.
• the weight of alcohol required to perform this dehydration operation is generally 1 to 10 times that of the fibers to be treated.
• the dehydrated fibers can undergo new centrifugation or spin filtration operations.
• the fibers can then be dried, ground and sieved to obtain a powder.
• enzymes which may be suitable for this purpose, mention may be made of proteases, mutanases, lipoproteases, cellulases and chitinases.
• Enzymatic purification can be combined or replaced by physical purification methods such as the various modes of filtration, of dialysis, or by the various techniques of chromatography.
• Fermentation musts and reconstituted aqueous solutions of succinoglycan, whether or not subjected to a purification treatment, can be concentrated. Concentration can be advantageous in certain cases, in particular insofar as transport costs can be reduced. In addition, concentrated solutions can be implemented more quickly than powders. Concentration can be achieved by techniques such as evaporation, ultrafiltration, or by diafiltration.
• succinoglycans are used, in the context of the invention, in solid form in powder or in aqueous solution.
• succinoglycan generally used from 0.001 to 2% by weight, preferably between 0.01 and 0.5% by weight of succinoglycan relative to the final suspension.
• suspensions of the invention comprising a succinoglycan of the type described above are particularly stable.
• this dispersant is chosen from the group of siliconates and their derivatives.
• Siliconates are well known products, they are salts of siliconic acid or its derivatives.
• R is a hydrocarbon residue generally of 1 to 18 carbon atoms, optionally substituted by a halogen atom, an amino group, ether, ester, epoxy, mercapto, cyano, (poly) glycol
• m is an integer or fractional number varying between 0.1 and 3
• M is an alkali metal or an ammonium or phosphonium group.
• R is a hydrocarbon residue of 1 to 10 carbon atoms and more particularly of 1 to 6 atoms.
• R can be an alkyl radical, for example methyl, ethyl, propyl, butyl, isobutyl; an alkenyl radical such as for example vinyl, an aryl radical, for example phenyl or naphthyl, an arylalkyl radical such as for example benzyl or phenylethyl, alkylaryl such as for example tolyl, xylyl, or an araryl radical such as biphenylyl.
• alkyl radical for example methyl, ethyl, propyl, butyl, isobutyl
• an alkenyl radical such as for example vinyl
• an aryl radical for example phenyl or naphthyl
• an arylalkyl radical such as for example benzyl or phenylethyl
• alkylaryl such as for example tolyl, xylyl, or an araryl radical such as biphenylyl.
• R ′ are identical or different and are hydrocarbon residues of 1 to 6 carbon atoms.
• alkaline siliconates are used.
• Alkaline earth siliconates can also be used.
• alkylsiliconates and in particular alkaline alkylsiliconates such as, for example, sodium or potassium methylsiliconates.
• alkali or alkaline earth siliconates are products, most of which are commercially available.
• silanes having 3 hydrolyzable groups such as halogen atoms, alkoxy radicals, followed by dissolution of the product obtained in a solution of a strong inorganic base in proportions such as there is at least one equivalent in base per atom of silicon (see for example US-A-2,441,422, US-A-2,441,423).
• the dispersant can also be chosen from siliconate derivatives.
• derivative products is meant here the condensation products of the products corresponding in particular to formula (1) described above, or those resulting from the at least partial polymerization into silicone compounds or polymers.
• alkali metal alkylsiliconates can be transformed into polyalkylsiloxanes, in particular by the action of carbon dioxide or other acidifying agent.
• silicone resins As a second type of dispersant suitable for the present invention, mention may also be made of silicone resins.
• silicone resins are well-known and commercially available branched organopolysiloxane polymers. They present, per molecule, at least two different motifs chosen among those of formula R3SiO 0.5 (unit M), R2SiO (unit D), RSiO 1.5 (unit T) and SiO2 (unit Q).
• radicals R are identical or different and are chosen from linear or branched alkyl radicals, these radicals more particularly having from 1 to 6 carbon atoms included, vinyl, phenyl, trifluoro-3,3,3 propyl radicals.
• alkyl radicals R of methyl, ethyl, isopropyl, tert-butyl and n-hexyl radicals.
• These resins are generally hydroxylated and in this case have a weight content of hydroxyl group of between 0.1 and 10%.
• resins examples include MQ resins, MDQ resins, TD resins and MDT resins.
• Resins having a molecular mass of less than 25,000 can be used more particularly.
• the siliconates are usually used in the form of aqueous solutions.
• the amount of siliconate used depends on the specific surface of the zeolite. This amount is usually between 0.01 and 2%, more particularly between 0.05 and 0.3% by weight relative to the final suspension. This quantity is understood for a solution at 50% by weight in water of the siliconate or derivative.
• the resins can be used in the solid state or in the form of aqueous emulsions or emulsion or solution in an organic solvent.
• the amounts used are between 0.01 and 2% by weight of solid product, more particularly between 0.05 and 0.3 relative to the final suspension.
• siliconates or derivatives and resins as defined above has the effect of considerably lowering the viscosity of the zeolite suspensions. It also makes it possible to obtain stable suspensions with a higher dry extract, for example at least 55%.
• dispersants can be used.
• these dispersants can be used alone or in combination and even optionally in combination with the siliconates, their derivatives or the resins.
• dispersants can be chosen from the group comprising nonionic or anionic surfactants, macromolecular organic polymer compounds carrying carboxyl and / or hydroxyl groups, phosphates.
• nonionic surfactants use may generally be made of compounds obtained by condensation of alkylene oxide with an organic compound which may be aliphatic or alkylaromatic.
• alkali metal soaps alkali sulfonates, such as methylnaphthalene sulfonate, xylenesulfonate, beta-sulfoethyl esters of fatty acids, sulfates and sulfated products such as alkyl sulfates, fatty alcohols polyoxyethylenated and sulphated.
• the polymers of acrylic, hydroxyacrylic, maleic, itaconic acids, the copolymers of the acids mentioned above may be given together or with unsaturated compounds ethylenic such as ethylene, propylene, vinyl alcohol, vinyl acetate, methacrylic acid.
• unsaturated compounds ethylenic such as ethylene, propylene, vinyl alcohol, vinyl acetate, methacrylic acid.
• phosphates these can be chosen from the group of primary or secondary esters of orthophosphoric acid or one of its salts and mono or diesters of this acid or of its polyoxyethylenated salts. Mention may also be made of inorganic in particular alkaline phosphates such as pyrophosphate, tripolyphosphate, sodium hexametaphosphate.
• the zeolite suspensions according to the invention are prepared in a simple manner by introducing the additives described above into the suspension and mixture. If necessary the pH of the zeolite suspension can be adjusted to the desired value in a known manner by the addition of any suitable neutralizing agent.
• Suspensions comprising zeolites and stabilized by the systems which have just been described can be used in numerous applications.
• They can be used in the form of suspensions based essentially on zeolites and the stabilizing additives mentioned above. In this case, they can enter into the preparation of detergent compositions. They can be used in any field other than detergency for which zeolites are used, for example in stationery.
• the present invention also covers detergent compositions, in particular for liquid detergents, comprising, in addition to the suspensions based on zeolite and stabilizers of the invention, all the other additives known in detergency such as bleaching agents, foam control agents, anti-redeposition agents, perfumes, solvents, enzymes, optical agents.
• the dry extract of the suspension is given in percentage by weight of anhydrous zeolite determined by a measurement of loss on ignition at 850 ° C. for one hour.
• the pH indicated is given for an aqueous dispersion containing 1% of dry zeolite and it is measured using a high alkalinity pH electrode.
• the exchange capacity is given by the amount of calcium (expressed in mg of CaCO3) exchanged with 1 g of anhydrous zeolite at 25 ° C.
• the measurement is carried out in the following manner: 0.4 g of zeolite (expressed as anhydrous) is introduced into a solution of 5.10 ⁇ 3 mole / l CaCl2. The mixture is kept stirring for 15 minutes. After filtration, the excess calcium is dosed at pH 10 in return by EDTA in the presence of a colored indicator, black eriochrome T.
• the RHEOMAT 30 equipped with the centered measurement system B is used as rheometer.
• the measurement consists in performing a cycle in speed gradient (ascent plus descent).
• the range of speed gradient explored is between 0.0215 and 157.9 s ⁇ 1, which corresponds to rotational speeds of the mobile from 0.0476 to 350 revolutions per minute.
• the viscosities reported in the examples correspond to measurements obtained during the descent in speed gradient.
• the sedimentation is determined by introducing the zeolite suspension into graduated cylinders from 50 to 100 cc. The volumes of supernatant and decantate are measured every five days. The test pieces are left at room temperature (20 ° C) or placed in a thermostatically controlled enclosure.
• the zeolite used is a 4A zeolite with an average diameter of primary particles of 3.5 ⁇ m.
• succinoglycan used in the following examples can be prepared as follows:
• a medium Agrobacterium tumefaciens I-736 is fermented containing a medium (in g / l): CSL (corn steap liquor) 11 K2 HPO4 4 MgSO4, 7H2O 0.5 Sucrose 25 Drinking water qs 1 l
• This medium is fermented by said strain at a temperature of 28 ° C., in a 20 liter BIOLAFFITE R tank containing a useful volume of 15 liters.
• the medium is subjected to stirring at 400 revolutions / min obtained by means of RUSHTON R type mobiles.
• the medium is aerated under an air flow of 825 l / h.
• the must is heat treated at 90 ° C for 30 min.
• IPA isopropyl alcohol
• the fibers from the precipitation are then dehydrated twice in the presence of 1200 ml of IPA.
• the fibers are then wrung, shredded and dried in an oven at 85 ° C.
• the collected dry matter is crushed and sieved.
• a cream-colored product powder is then obtained.
• the suspension contains 45% by weight of zeolite.
• Table 1 Example 1 2 3 comparative. Succinoglycan% by weight relative to the suspension 0.1 0.05 0 pH 11.48 11.48 11.52 Sedimentation supernatant% volume 20 ° C 50 ° C 20 ° C 20 ° C 50 ° C 5 days 0 2 ⁇ 1 16 21 10 days ⁇ 1 2 2.5 18 23 15 days 1 2 3 20 23 % Volume decantate 5 days 0 0 0 60 60 10 days 0 0 0 60 77 15 days 0 0 "1 80 77
• RHODORSIL 51 T the quantities indicated are in percentages by weight for a 50% aqueous solution of siliconate.
• Resin A is a resin of the type described above for which R is a methyl radical. This resin is used here in the dry or solid state. It is marketed by the Applicant in the form of an emulsion under the reference RHODORSIL 865 A.
• Example 8 is a low quantity example of succinoglycan.
• Example 9 a resin "Resin B” is used which is a resin of the type described above in which R is methyl.
• This resin is used here in the dry state. It is marketed by the Applicant in the form of an emulsion and under the reference RHODORSIL 878 A.
• Example 10 describes the use as a dispersant of a nonionic surfactant of the sucroglyceride type sold by the Applicant under the name CELYNOL X8063.
• Example 11 describes the use as a dispersant of a nonionic surfactant of the ethoxylated tristirylphenol type sold under the name SOPROPHOR S25, sold by the Applicant.
• Example 12 relates to a dispersant of the anionic surfactant type which is a phosphated ethoxylated tristyrylphenol marketed under the name SOPROPHOR FL, marketed by the Applicants.
• Examples 13 to 14 relate to acrylic polymers.
• Polymer 1 is an acrylic homopolymer with a mass of 2000.
• Polymer 2 is an acrylic-maleic copolymer with a mass of 70,000 and an acrylic / maleic ratio of 60/40.
• Example 8 9 Suspension% anhydrous zeolite 49.6 49.3 Exchange capacity 295 Succinoglycan in% by weight relative to the suspension 0.02 0.12 Dispersant% by weight relative to the suspension Siliconate 0.2 Resin B 0.2 pH of the suspension 10.67 11.49 Rheology Viscosity (poises) at 4.74s ⁇ 1 13.3 14 at 32s ⁇ 1 6.9 12.6 Sedimentation Supernatant in% of volume 5 days 1 5 10 days 5 15 days 2 5 Decantate in% of volume 5 days 2.5 0 10 days 0 15 days 0 Example 10 11 12 13 14 Suspension% anhydrous zeolite 49.3 49.3 49.3 49.3 49.3 Exchange capacity Succinoglycan in% by weight relative to the suspension 0.04 0.04 0.04 0.08 0.08 Dispersant% by weight relative to the suspension CELANOL 0.2 SOPROPHOR S25 0.2 SOPROPHOR FL 0.2 POLYMER 1 0.2 POLYMER 2 0.2

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• 1989
  • 1989-10-09 FR FR8913139A patent/FR2652820B1/fr not_active Expired - Fee Related
• 1990
  • 1990-10-05 CA CA002027011A patent/CA2027011A1/fr not_active Abandoned
  • 1990-10-05 BR BR909005014A patent/BR9005014A/pt not_active Application Discontinuation
  • 1990-10-05 EP EP90402758A patent/EP0422997A1/de not_active Withdrawn
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