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
  • C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
  • C11D17/0047—Detergents in the form of bars or tablets
  • C11D17/0065—Solid detergents containing builders
  • C11D17/0073—Tablets
  • C11D17/0086—Laundry tablets
• • 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
  • C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
  • C11D17/0047—Detergents in the form of bars or tablets
  • C11D17/0065—Solid detergents containing builders
  • C11D17/0073—Tablets
  • C11D17/0091—Dishwashing tablets
• • 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
  • C11D3/04—Water-soluble compounds
  • C11D3/06—Phosphates, including polyphosphates

Definitions

• the subject of the present invention is tablets of compacted detergent or anti-scale composition particles; these can be implemented for carrying out washing operations in a washing machine or dishwasher.
• the Applicant has found that the presence of a higher amount of water in the NaTPP consisting mainly of phase I, makes it possible to avoid the transfer of water present in the tablet to this NaTPP, thus preventing the risks of heating of the tablet with disintegration of sensitive constituents such as enzymes in particular.
• the presence of a greater quantity of water makes it possible to multiply the number of germs of hydrated NaTPP and thus facilitates the disintegration and the dissolution of the tablet.
• a first subject of the invention consists of tablets of detergent or anti-limescale composition comprising compacted particles based on sodium tripolyphosphate having a high content in phase I and water distributed homogeneously in said sodium tripolyphosphate, said tablets being characterized in that said sodium tripolyphosphate present in the tablet or in a region of the tablet,
• phase I contains from 70% to 100%, preferably from 80% to 98% by weight of phase I relative to all the phases of anhydrous sodium tripolyphosphates
• * contains from 7% to 16%, preferably from 8 to 12% of its weight of water, at least 50%, preferably from 70% to 90% of this water being in the form of water of crystallization.
• Said sodium tripolyphosphate containing from 70% to 100% by weight of phase I and from 7 to 16% of water can represent from 5% to 100%, preferably of the order of 10% to 90% by weight ( expressed in sec) relative to the weight of the tablet (in sec) or the region of the tablet in which it is located.
• the NaTPP consisting at least mainly of phase I used for the production of the tablets of the invention, can be obtained according to a three-step process stages, spray drying of a sodium orthophosphate liquor, calcination in NaTPP anhydride phase I and hydration.
• the spray drying step can be carried out in a known manner, for example using a nozzle or turbine atomizer, using a sodium orthophosphate liquor having a dry extract which may be on the order of 50% to 70%, preferably on the order of 60% by weight, and a pore-forming element, in particular ammonium carbonate, injected into the orthophosphate liquor at the spray head; the content of ammonium carbonate introduced can be of the order of 0.1 to 0.6, by weight (expressed in dry) per 100 parts of orthophosphate (expressed in dry).
• the inlet temperature of the attack gases depends on the size of the atomizer and the flow rates of the fluids; this can be of the order of 500 to 600 ° C.
• the gas outlet temperature can be between 120 and 200 ° C, preferably 140 and 160 ° C.
• the orthophosphate particles thus obtained generally have a residual humidity of less than 5% by weight; their density is of the order of 0.25 g / cm 3 to 0.45 g / cm 3 , preferably of the order of 0.35 g / cm 3 ; their median diameter is generally between 200 and 400 ⁇ m, preferably of the order of 300 ⁇ m.
• the calcination operation can be carried out in a known manner, for example in a rotary furnace with direct co-current flame, the product being directly cooled after calcination.
• the sodium orthophosphate introduced can be calcined in approximately 30 minutes to one hour, up to a temperature of 450 to 600 ° C, preferably 490 to 530 ° C.
• the product thus obtained is a NaTPP powder consisting mainly of phase I (of the order of 70 to 100%); it has a particle size of the order of 250 to 450 ⁇ m, preferably of the order of 350 ⁇ m; its density is of the order of 0.4 g / cm 3 to 0.65 g / cm 3 , preferably of the order of 0.55 g / cm 3 .
• the NaTPP powder is then hydrated by spraying water, for example in a drum, a rapid mixer or a fluidized bed, fitted with sprayers of the bi-fluid nozzle type generating droplets of the order of 20 ⁇ m to 300 ⁇ m, preferably of the order of 100 ⁇ m, until a water content ("water of hydration") of the NaTPP in the particles is obtained of the order of 7 to 16%.
• this water content is of the order of 8 to 12%.
• this hydration step is carried out by spraying an aqueous solution of a base or a basic salt, such as sodium hydroxide, potassium hydroxide, aqueous solutions of alkali metal silicates, of tripolyphosphate sodium ... Mention may in particular be made of the spraying of an aqueous solution of NaTPP preferably containing less than 20 ppm of Ca or Mg, so as to form "nucleis" of NaTPP, 6H 2 0.
• a base or a basic salt such as sodium hydroxide, potassium hydroxide, aqueous solutions of alkali metal silicates, of tripolyphosphate sodium ...
• Mention may in particular be made of the spraying of an aqueous solution of NaTPP preferably containing less than 20 ppm of Ca or Mg, so as to form "nucleis" of NaTPP, 6H 2 0.
• a second embodiment consists in carrying out the hydration step by spraying with an aqueous solution of a wetting agent such as nonionic surfactants such as polyethoxylated fatty alcohols, or of a sequestering agent such as the salts of polyacetic acids (ethylenediaminetetraacetates ...), polyphosphonates (ethane 1-hydroxy-1, 1-diphosphonates, methylene salts diphosphonates ).
• a wetting agent such as nonionic surfactants such as polyethoxylated fatty alcohols, or of a sequestering agent such as the salts of polyacetic acids (ethylenediaminetetraacetates ...), polyphosphonates (ethane 1-hydroxy-1, 1-diphosphonates, methylene salts diphosphonates ).
• said tablets also comprise at least one other sodium tripolyphosphate, for example a sodium tripolyphosphate having a phase I content of less than 70%, or a tripolyphosphate consisting mainly or completely of phase II.
• at least one other sodium tripolyphosphate for example a sodium tripolyphosphate having a phase I content of less than 70%, or a tripolyphosphate consisting mainly or completely of phase II.
• said other sodium tripolyphosphate is a sodium tripolyphosphate having a phase II content of at least 70% relative to all of the anhydrous phases of sodium tripolyphosphate, and a water content which can range from 0 to 15 %, preferably of the order of 5 to 10%.
• Said other sodium tripolyphosphate may be present in the tablets of the invention in an amount such that the total amount of NaTPP in the tablets is of the order of 5 to 100%, preferably from 10 to 90% depending on the use sought. .
• the tablets which are the subject of the invention can be detergent tablets for washing machines or dishwashers, as well as anti-limescale tablets. They can have one or two or even several regions.
• said sodium tripolyphosphate containing from 70% to 100% by weight of phase I and from 7 to 16% of water is preferably located in the two regions of the tablet.
• the amount of said sodium tripolyphosphate containing from 70% to 100% by weight of phase I and from 7 to 16% of water may represent from 5% to 80%, preferably of the order of 10% to 60% by weight (expressed in sec) relative to the weight of the tablet (in dry) or of the region of the tablet in which it is located.
• tripolyphosphates having a phase I content of less than 70%, or tripolyphosphates consisting mainly or completely of phase II, in particular tripolyphosphates consisting of at least 70% of phase II relative to all of the anhydrous phases and having a water content of 0 to 15%, preferably of the order of 5 to 10%; these can be present in the tablets in an amount such that the total amount of NaTPP in the tablets is of the order of 5 to 60%, preferably from 10 to 50% other or organic mineral builders, in amounts up to 50% by weight, such as
• the water-soluble salts of carboxylic polymers or copolymers such as the water-soluble salts of polycarboxylic acids with a molecular mass of the order of 2,000 to 100,000, obtained by polymerization or copolymerization of ethylenically unsaturated carboxylic acids such as acrylic acid, acid or maleic anhydride, fumaric acid, itaconic acid, mesaconic acid, citraconic acid, methylenemalonic acid, and in particular polyacrylates of molecular mass of the order of 2,000 to 10,000 (US-A-3,308,067), copolymers of acrylic acid and maleic anhydride with a molecular mass of the order of 5,000 to 75,000 (EP-A-66,915)
• polycarboxymethylated derivatives of glutamic acid such as N, N-bis (carboxymethyl) glutamic acid and its salts, especially of sodium
• glutamic acid such as N, N-bis (carboxymethyl) glutamic acid and its salts, especially of sodium
• agents such as anionic surfactants (in amounts of the order of 0 to 20%) such as.
• alkyl esters sulfonates of formula R-CH (SO 3 M) -COOR ', where R represents an alkyl radical in C 8 -C 20 , preferably in C 10 -C 16 , R' an alkyl radical in CC 6 , preferably in CC 3 and M an alkali cation (sodium, potassium, lithium), substituted or unsubstituted ammonium (methyl-, dimethyl-, trimethyl-, tetramethylammonium, dimethylpiperidinium ...) or derived from an alkanolamine (monoethanolamine, diethanolamine, triethanolamine ...);
• alkyl sulphates of formula ROSO 3 M where R represents a C 5 -C 24 , preferably C 10 -C 18 , alkyl or hydroxyalkyl radical, M representing a hydrogen atom or a cation of the same definition as above, as well as their ethoxylenated (OE) and / or propoxylenated (OP) derivatives, having on average from 0.5 to 30 units, preferably from 0.5 to 10 OE and / or OP units;
• the sulfonated alkylamides of formula RCONHR'OSO 3 M in which R represents a C 2 -C 22 , preferably C 6 -C 20 , alkyl radical, R ′ a C 2 -C 3 alkyl radical, M representing a d atom hydrogen or a cation of the same definition as above, as well as their ethoxylenated (OE) and / or propoxylenated (OP) derivatives, having on average from 0.5 to 60 OE and / or OP units;
• the salts of C 8 -C 24 preferably C 14 -C 20 saturated or unsaturated fatty acids, C 9 -C 20 alkylbenzenesulfonates, C 8 -C 22 primary or secondary alkylsulfonates, alkylglycerol sulfonates, sulfonated polycarboxylic acids described in GB-A-1 082 179, paraffin sulfonates, N-acyl N-alkyltaurates, alkylphosphates, isethionates, alkylsuccinamates, alkylsulfosuccinates, monoesters or diesters of sulfosuccinates, N-acyl sarcosinates , alkyl glycoside sulfates, polyethoxycarboxylates, the cation being an alkali metal (sodium, potassium, lithium), a substituted or unsubstituted ammonium residue (methyl-, dimethyl
• sophorolipids such as those in acid or lactone form, derived from 17-hydroxyoctadecenic acid; non-ionic surfactants (in amounts of the order of 0 to 30%) such as polyoxyalkylenated (polyethoxyethylenated, polyoxypropylenated, polyoxybutylenated) alkylphenols in which the alkyl substituent is C 6 -C 12 and containing from 5 to 25 oxyalkyiene units ; by way of example, mention may be made of the TRITON X-45, X-114, X-100 or X-102 sold by Rohm & Haas Cy., the IGEPAL NP2 to NP17 from RH ⁇ NE-POULENC;
• polyoxyalkylenated C 8 -C 22 aliphatic alcohols containing from 1 to 25 oxyalkyiene units oxyethylene, oxypropylene
• TERGITOL 15-S-9 TERGITOL 24-L-6 NMW marketed by Union Carbide Corp.
• NEODOL 45-9 NEODOL 23-65
• NEODOL 45-7 NEODOL 45-4 marketed by Shell Chemical Cy
• KYRO EOB marketed by The Procter & Gamble Cy
• BASF a polyoxyalkylenated C 8 -C 22 aliphatic alcohols containing from 1 to 25 oxyalkyiene units (oxyethylene, oxypropylene)
• TERGITOL 15-S-9 TERGITOL 24-L-6 NMW marketed by Union Carbide Corp.
• ethoxylated amines containing from 5 to 30 ethoxylated units; . alkoxylated amidoamines containing from 1 to 50, preferably from 1 to 25, very particularly from 2 to 20 oxyalkylene units (preferably oxyethylene;. amine oxides such as C 10 -C 18 alkyl oxides dimethylamines, alkoxy oxides C 8 -C 22 ethyl dihydroxy ethylamines; alkoxylated terpene hydrocarbons such as ethoxylated and / or propoxylated - or ⁇ -pinenes, containing from 1 to 30 oxyethylene and / or oxypropylene units;
• alkylpolyglycosides obtainable by condensation (for example by acid catalysis) of glucose with primary fatty alcohols (US-A-3,598,865; US-A-4,565,647; EP-A-132,043; EP-A-132 046 ...) having a C 20 -C 20 , preferably C 8 -C 18 alkyl group, as well as an average number of glucose units of the order of 0.5 to 3, preferably of the order of 1.1 to 1.8 per mole of alkylpolyglycoside (APG); we can mention in particular those presenting
• GLUCOPON 600 EC ® GLUCOPON 600 CSUP ®
• GLUCOPON 650 EC ® GLUCOPON 225 CSUP ®
• agents such as cellulose derivatives such as cellulose hydroxyethers, methylcellulose, ethylcellulose, hydroxypropyl methylcellulose, hydroxybutyl methylcellulose
• agents such as cellulose derivatives such as cellulose hydroxyethers, methylcellulose, ethylcellulose, hydroxypropyl methylcellulose, hydroxybutyl methylcellulose
• polyvinyl esters grafted on polyalkylene trunks such as polyvinylacetates grafted on polyoxyethylene trunks (EP-A-219 048) polyvinyl alcohols polyester copolymers based on ethylene terephthalate
• polyoxyethylene and / or polyoxypropylene of the order of 1/10 to 10/1, the polyoxyethylene and / or polyoxypropylene units having a molecular weight of in the range of 250 to 10,000, with a molecular weight of the copolyester in the range of 1,000 to 100,000
• - terephthalic copolyester oligomers with a sulfonated, sulfoaroyl polyalkyleneoxyalkyl ending and optionally containing sulfoisophthaloyl units in their chain (US-A-4,721,580; US-A-5,415,807; US-A-4,877,896; US-A-5 182,043; US-A-5,599,782; US-A-4,764,289; EP-A-311,342; WO 92/04433; WO 97/42293) - sulfonated terephthalic copolyesters of molecular weight less than 20,000, obtained for example from a diester of terephthalic acid, isophthalic acid, a diester of sulfoisophthalic acid and a diol, ethylene glycol in particular (WO 95/32997)
• polyesters-polyurethanes obtained by reaction of a polyester with a molecular weight of 300-4,000 obtained from a diester of terephthalic acid, optionally a diester of sulfoisophthalic acid and a diol, onto a prepolymer with terminal isocyanate groups obtained from a polyoxyethylene glycol with a molecular mass of 600-4,000 and a diisocyanate (US-A-4,201,824)
• anti-redeposition agents in amounts of about 0.01-10% by weight for a powdered detergent composition, agents such as - ethoxylated monoamines or polyamines, polymers of ethoxylated amines (US-A-4,597,898, EP-A-11,984)
• the polyvinylpyrrolidones of bleaching agents in an amount of about 0.1-20%, preferably 1-10% of the weight of said detergent powder composition, such as
• - perborates such as sodium perborate monohydrate or tetrahydrate - peroxygen compounds such as sodium carbonate peroxyhydrate, pyrophosphate peroxyhydrate, urea peroxyhyd failed, sodium peroxide, sodium persulfate
• percarboxylic acids and their salts such as magnesium monoperoxyphthalate hexahydrate, magnesium metachloroperbenzoate, 4-nonylamino-4-oxoperoxybutyric acid, 6-nonyiamino-6-oxoperoxycaproic acid, diperoxydodecanedioic acid, nonylamide of peroxysuccinic acid, decyldiperoxysuccinic acid, preferably combined with a bleach activator generating in situ in the washing medium, a peroxycarboxylic acid; among these activators, there may be mentioned, tetraacetylethylene diamine, tetraacetyl methylene diamine, tetraacetyl glycoluryl, sodium p-acetoxybenzene sulfonate, pentaacetyl glucose, octaacetyl lactose, ...
• percarbonates such as magnesium monoperoxyphthalate hexahydrate, magnesium metach
• fluorescent agents in quantity of about 0.05-1.2% by weight, agents such as stilbene derivatives, pyrazoline, coumarin, fumaric acid, cinnamic acid, azoles, methinecyanins, thiophenes, ... foam suppressants, in amounts up to '' at 5% by weight, agents such as
• - polyorganosiloxane oils or resins optionally combined with silica particles, softening agents, in amounts of about 0.5-10% by weight, agents such as clays of enzymes in amounts up to 5 mg by weight, preferably of the order of 0.05-3 mg of active enzyme / g of detergent composition, enzymes such as proteases, amylases, lipases, cellulases, peroxidases (US-A-3553139, US-A-4101457, US-A-4 507 219, US-A-4 261 868) and other additives such as
• - buffering agents or fillers such as sodium sulphate, carbonates or bicarbonates of alkaline earth metals.
• the amount of said sodium tripolyphosphate containing from 70% to 100% by weight of phase I and from 7 to 16% of water can represent from 10% to 90% in weight (expressed in sec) relative to the weight of the tablet (in sec) or of the region of the tablet in which it is located.
• the other additives which may be present in the dishwasher tablets one can mention
• tripolyphosphates having a phase I content of less than 70%, or tripolyphosphates consisting mainly or totally of phase II, in particular tripolyphosphates consisting of at least 70% phase II compared to all of the anhydrous phases and having a water content of 0 to 15%, preferably of the order of 5 to 10%; these can be present in the tablets in an amount such that the total amount of NaTPP in the tablets is of the order of 20 to 80%.
• alkalizing additives or sequestering agents which are soluble in the washing medium such as. hexametaphosphates of alkali metals, ammonium or alkanolamines
• alkali metal silicates (0 to 30% by weight).
• alkali metal carbonates (0 to 30% by weight)
• water-soluble polyphosphonates (1-hydroxy-1-ethane, 1-diphosphonates, methylene salts diphosphonates, ...)
• the water-soluble salts of carboxylic polymers or copolymers such as the water-soluble salts of polycarboxylic acids with a molecular weight of about 2,000 to 100,000, obtained by polymerization or copolymerization of carboxylic acids ethylenically unsaturated such as acrylic acid, maleic acid or anhydride, fumaric acid, itaconic acid, mesaconic acid, citraconic acid, methylenemalonic acid, and very particularly polyacrylates with a molecular mass of the order of 2,000 to 10,000 (US-A- 3,308,067), the copolymers of acrylic acid and maleic anhydride with a molecular mass of the order of 5,000 to 75,000 (EP-A-66,915)
• polycarboxylate ethers oxidisuccinic acid and its salts, monosuccinic acid tartrate and its salts, disuccinic acid tartrate and its salts
• citric acid and its salts citric acid and its salts, mellitic acid, succinic acid and their salts.
• polyacetic acid salts ethylenediaminetetraacetates, nitrilotriacetates,
• succinic C 5 -C 20 alkyl acids and their salts (2-dodecenylsuccinates, lauryl succinates, 7)
• polyacetal carboxylic esters polyaspartic acid, polyglutamic acid and their salts
• polycarboxymethylated derivatives of glutamic acid such as N, N- bis (carboxymethyl) glutamic acid and its salts, especially of sodium] or other amino acids
• bleaching agents such as perborates and percarbonates of alkali metals (0 to 20%) associated with a bleaching activator (tetraacetylethylene diamine) (up to 10%) and possibly associated with a bleaching catalyst (organometallic manganese complexes, cobalt %) (0 to 1%)
• polyoxyalkylenated C 8 -C 22 aliphatic alcohols containing from 1 to 25 oxyalkyiene units oxyethylene, oxypropylene
• TERGITOL 15-S-9 polyoxyalkylenated C 8 -C 22 aliphatic alcohols containing from 1 to 25 oxyalkyiene units (oxyethylene, oxypropylene); by way of example, mention may be made of TERGITOL 15-S-9, TERGITOL 24-L-6 NMW sold by Union Carbide Corp., NEODOL 45-9, NEODOL 23-65, NEODOL 45-7, NEODOL 45-4 marketed by Shell Chemical Cy, KYRO EOB marketed by The Procter & Gamble Cy, SYNPERONIC A3 to A9 from ICI, RHODASURF IT, DB and B from RHONE-POULENC, PLURAFAC LF 403 marketed by BASF; . the products resulting from the condensation of ethylene oxide or propylene oxide with propy
• products resulting from the condensation of ethylene oxide or propylene oxide with ethylenediamine such as TETRONIC sold by BASF;
• ethoxylated amines containing from 5 to 30 ethoxylated units; . alkoxylated amidoamines containing from 1 to 50, preferably from 1 to 25, very particularly from 2 to 20 oxyalkylene units (preferably oxyethylene;
• amine oxides such as C 10 -C 18 alkyl oxides dimethylamines, C 8 -C 22 alkoxy oxides ethyl dihydroxy ethyiamines;
• alkoxylated terpene hydrocarbons such as ethoxylated and / or propoxylated ⁇ - or ⁇ -pinenes, containing from 1 to 30 oxyethylene and / or oxypropylene units;
• the amount of said sodium tripolyphosphate containing from 70% to 100% by weight of phase I and from 7 to 16% of water can represent from 10% to 100%, from preferably from 20 to 90% by weight (expressed in sec) relative to the weight of the tablet (in dry) or of the region of the tablet in which it is located.
• tripolyphosphates having a phase I content of less than 70%, or tripolyphosphates consisting mainly or totally of phase II, in particular tripolyphosphates consisting of at least 70% phase II compared to all of the anhydrous phases and having a water content of 0 to 15%, preferably of the order of 5 to 10%; these can be present in the tablets in an amount such that the total amount of NaTPP in the tablets is of the order of 30 to 99%, preferably from 50 to 90%.
• - sodium hexametaphosphate (0 to 10%)
• alkali metal carbonates (0 to 30%)
• crystalline or amorphous aluminosilicates of alkali metals or ammonium (0 to 30%)
• - water-soluble polyphosphonates (1-hydroxy-1, 1-ethane-diphosphonates, methylene diphosphonate salts, etc.) (0 to 5%)
• - water-soluble salts of carboxylic polymers or copolymers such as the salts water-soluble polycarboxylic acids of molecular weight of the order of 2,000 to 100,000, obtained by polymerization or copolymerization of ethylenically unsaturated carboxylic acids such as acrylic acid, maleic acid or anhydride, fumaric acid, itaconic acid, mesaconic acid, acid citraconic, methylenemalonic acid, and especially polyacrylates, copolymers of acrylic acid and maleic anhydride
• the tablets which are the subject of the invention can be obtained in a conventional manner by pressing in a mold the desired quantity of a particulate composition containing the various constituents of said tablets.
• the density of the tablets can be of the order of 0.9 to 2 g / cm 3 , depending on the use sought.
• the gas inlet temperature is 500 ° C; the outlet temperature is 150 ° C.
• the product obtained, with a density of 0.35 g / cm 3 is then calcined up to 520 ° C. in a co-current rotary oven with direct flame.
• the NaTPP obtained has the following characteristics: * a rate of phase I of 87% relative to all of the anhydrous phases
• a third part is hydrated in a fast Lôdige mixer batchwise by spraying with water, so as to obtain an NaTPP having different "hydration" rates:
• a fourth part is hydrated by spraying water continuously in a COMESSA fluidized bed (from COMESSA), the powder flow rate is 50 to 100 kg / h, so as to obtain an NaTPP having different "hydration" rates:
• the dissolution rate (VD) of each tablet is carried out by monitoring the conductivity of the water. This determines the time required for the dissolution of 90% of the tablet. The results are shown in Table 1. Test 2
• the dissolution rate and the longitudinal tensile strength t in Pascal of each tablet are measured.

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• 1998
  • 1998-10-09 FR FR9812682A patent/FR2784392B1/fr not_active Expired - Fee Related
• 1999
  • 1999-10-01 CN CN99811953A patent/CN1323342A/zh active Pending
  • 1999-10-01 RU RU2001112111/04A patent/RU2213132C2/ru not_active IP Right Cessation
  • 1999-10-01 WO PCT/FR1999/002343 patent/WO2000022090A1/fr not_active Application Discontinuation
  • 1999-10-01 EP EP99946276A patent/EP1119606A1/de not_active Withdrawn
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• 2001
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