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
  • C11D3/48—Medical, disinfecting agents, disinfecting, antibacterial, germicidal or antimicrobial compositions
• • A—HUMAN NECESSITIES
  • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
  • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
  • A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
• • 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
  • C11D17/0008—Detergent materials or soaps characterised by their shape or physical properties aqueous liquid non soap compositions
  • C11D17/003—Colloidal solutions, e.g. gels; Thixotropic solutions or pastes
• • 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
• • 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
  • C11D3/16—Organic compounds
  • C11D3/20—Organic compounds containing oxygen
  • C11D3/2075—Carboxylic acids-salts thereof
• • 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
  • C11D3/39—Organic or inorganic per-compounds
  • C11D3/3942—Inorganic per-compounds
• • 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
  • C11D3/39—Organic or inorganic per-compounds
  • C11D3/3947—Liquid compositions
• • C—CHEMISTRY; METALLURGY
  • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
  • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
  • C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
• • C—CHEMISTRY; METALLURGY
  • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
  • C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
  • C23G5/00—Cleaning or de-greasing metallic material by other methods; Apparatus for cleaning or de-greasing metallic material with organic solvents
  • C23G5/06—Cleaning or de-greasing metallic material by other methods; Apparatus for cleaning or de-greasing metallic material with organic solvents using emulsions

Definitions

• Solid material and gel constituting a source of hydrogen peroxide and / or acid, method of preparation and use
• the present invention relates to the gelation of an aqueous composition of hydrogen peroxide, at least one acid or a mixture thereof, which can be harmful when concentrated.
• Aqueous solutions of H 2 O 2 and acids have two main disadvantages. On the one hand, when you pour them, you can get splashes, which is a risk for the staff. On the other hand, when used to treat surfaces, they flow very (or even too much) quickly on surfaces that are not horizontal.
• CH 406123 A which recommends obtaining a stable powder, containing active and water-soluble oxygen when it is brought into contact with water, according to a process comprising mixing H 2 O 2 with sodium metasilicate in the presence of an absorbent (sodium carbonate);
• US 4313932 A which describes obtaining a powder from an H 2 O 2 generator (for example sodium peroxydisulfate), a thickener (which may be silica), a salt inorganic ammonium [e.g.
• the new technical solution developed with the present invention, comprises
• a solid material advantageously in pulverulent form, useful in particular as a source of hydrogen peroxide and / or gel acid.
• said material being characterized in that it comprises in intimate association:
• (C) an agent ensuring a homogeneous dispersion of the substance (B) in the gel resulting from the contacting with water with stirring (i) of the mixture of (A) and (B) or (ii) of said material solid.
• This material is obtained by dehydration of a gel produced by mixing with stirring of the gelling agent (A) with an aqueous solution of (B) +
• this solid material for the preparation of a gel, said use being characterized in that said material is brought into contact with water with stirring until forming a homogeneous gel, which is likely to be used in the field of hygiene, decontamination, cleaning, surface treatment including passivation, stripping, making electrolytes for batteries and accumulators , or the refining of cellulosic fibers.
• a gelling agent (A) which is a hydrophilic silica
• a method for preparing a gel from said solid material comprises bringing said material into contact with water (preferably distilled water, or better deionized water) with stirring at an angular rate of 1000 to 2500 rpm, preferably with stirring at an angular rate of 1500 to 2000 rpm, for 10 to 20 minutes.
• a gel is provided, as a new industrial product, which is obtained from a starting aqueous hydrogen peroxide solution preferably containing at most 60% w / w of H 2 O 2 .
• a hydrophilic fumed silica having a submicron granulometry, advantageously a particle size of less than or equal to
• CABOT under the CAB-O-SIL nomenclature (in particular the hydrophilic products CAB-O-SIL® L-90, LM-150, M-5, H-5, EH-5 and M-7D), which have a surface mass of 80 to 460 m 2 / g (in particular, for the 6 CAB-O-SIL mentioned above, a specific mass of 2.2 g / cm 2 ) and an average particle size of 7 to 20 mm, are particularly useful according to the present invention. invention.
• hydrophilic silica When using such a hydrophilic silica, it is imperative that the acid or acids present in B2 or B3 are free of fluorine, and that the agent C is also free of fluorine. Indeed, the presence of at least one fluorine atom in the molecule of these products would be likely to destabilize or destroy the silica of the solid material and of the gel which is involved in the preparation of said solid material or which is regenerated from said solid material.
• Hydrogen peroxide in aqueous solution which is used as a starting material, can have a practical H 2 O 2 concentration of 0.5% w / w to 60% w / w.
• this concentration of H 2 O 2 will be greater than or equal to 0.5% w / w, for example less than or equal to 8% w / w as indicated in EP 1175149 B9 cited above.
• this starting solution may have an H 2 O 2 concentration greater than or equal to 12% w / w and better still a concentration greater than or equal to 20% w / w.
• This solution may contain up to 50% w / w H 2 O 2 , or even up to 60% w / w H 2 O 2 .
• B2 substance is a mineral acid (especially a strong acid such as
• HCl, H 2 SO 4 , H 3 PO 4 or an aliphatic organic acid (in particular CH 3 CO 2 H, CH 3 CH 2 CO 2 H, a mixture CH 3 CO 2 H 2 CH 3 CO 3 H, or an ethylenically unsaturated acid ), aromatic (especially a hydroxybenzoic acid, such as 2, 3- and 4-hydroxybenzoic acids) or heterocyclic (especially a pyridinecarboxylic acid such as nicotinic, isonicotinic and picolinic acids).
• aromatic especially a hydroxybenzoic acid, such as 2, 3- and 4-hydroxybenzoic acids
• heterocyclic especially a pyridinecarboxylic acid such as nicotinic, isonicotinic and picolinic acids.
• the substance B2 will comprise at least one acid, pyridinecarboxylic acid, or will be an acid mixture comprising at least 0.1% by dry weight and better still at least 0.2% by dry weight. of pyridinecarboxylic acid relative to the dry weight of said acid mixture.
• the substance B is a mixture B3 containing hydrogen peroxide and at least one acid which is a pyridinecarboxylic acid.
• the pyridinecarboxylic acid plays here an interesting role in view of the fact that it comprises in its molecule two functional groups: a tertiary amine function and a carboxylic acid function both useful for the cohesion of the gel and the solid material of the invention .
• the agent C which ensures a homogeneous dispersion of B in the solid material and the gel is advantageously chosen from: (Cl) surfactants, (C2) sequestering agents, (C3) polyols, (C4) 5 NaOH KOH and their salts, in particular their salts with mineral acids, and (C5) mixtures thereof.
• the preferred surfactants (C1) are (i) anionic surfactants and (ii) nonionic surfactants.
• anionics mention may be made of dihexyl sodium sulphosuccinate of formula
• dialkyl analogs linear alkylsulfonates, fatty acid salts with a metal (sodium, potassium, cobalt), and sulfated castor oil; and for nonionics, polyglycol esters, polyoxyalkylenated alcohols, sorbitan esters and polyoxyalkylenated sorbitan esters.
• the sequestering agents (C2) include, in particular, substances selected from the group consisting of (i) ethylenediaminetetraacetic acid and its sodium and / or calcium salts, and (ii) benzotriazole.
• benzotriazole acts mainly as a corrosion inhibiting agent for copper and its alloys; it can also intervene as illustrated below as a sequestering agent.
• the polyols (C3) which are suitable here, are mainly C 2 -C 6 short-chain aliphatic alcohols with at least 2 and at most 6 groups
• OH especially a diol, triol, tetrol, pentol or hexol, and / or • long chain, in particular of the (polyoxyalkylene) diol type, in particular a polyethylene glycol or a polypropylene glycol.
• the polyols (C3) are interesting in terms of homogenization and stability due to the fact that they are polyfunctional products.
• the ethers and esters of these polyols are classified as non-ionic surfactants referred to above.
• the alkalis (C4) namely mainly NaOH and KOH, are favorably used to obtain a homogeneous dispersion in the solid material and in the gel. They act for this purpose as (i) pH regulators and (ii) products increasing the ionic strength of low polarity systems.
• aqueous solution that contains H 2 O 2 does not exceed a pH value greater than 8.5. Beyond this threshold, the hydrogen peroxide, which would be associated with an alkali, would become a reducing agent while it is its oxidizing properties that is sought according to the invention.
• an alkali such as NaOH or KOH will only occur if and only if it is desired to have an included pH, if necessary, between 6 and 7.5.
• agents (C) which are preferably recommended according to the invention are anionic surfactants, nonionic surfactants, polyols and mixtures thereof.
• the solid material comprises:
• the silica is, as indicated above, a hydrophilic silica having a mean granulometry in the dry state which is submicron.
• the gel to be dehydrated When forming the gel to be dehydrated according to the invention, it is recommended to stir the mixture of A with the aqueous solution of B + C, with a low angular velocity. It is recommended for this purpose a speed angular from 1000 to 2500 rpm, and preferably an angular velocity of 1500 to 2000 rpm, for 10 to 20 minutes. If the angular velocity is greater than 2500 revolutions / minute, there is a risk of destabilizing the gel formed.
• the dehydration of the gel to obtain the solid material can be carried out by an appropriate method, in particular:
• lyophilization is the most practical in the context of the invention.
• the freeze-drying phase is implemented here in a conventional manner, the sublimation phase is advantageously achieved by limiting the maximum temperature of heating under vacuum.
• Lyophilization leads to a solid powdery material, which is an advantage for the future regeneration of the gel.
• Regeneration of the gel from said material is carried out under conditions similar to those of formation of the gel to be dehydrated. These conditions are, as indicated above, stirring at an angular rate of 1000 to 2500 rpm, preferably stirring at an angular speed of 1500 to 2000 rpm for 10 to 20 minutes.
• the preparation of the solid material it is carried out according to a process comprising the steps of: (1) contacting with stirring • a gelling agent (A), which is a hydrophilic silica pyrogenous, with
• An aqueous solution of a mixture of a substance (B) which may be harmful in aqueous solution which is chosen from the group consisting of (B1) hydrogen peroxide,
• An agent (C) chosen from the group consisting of (C1) anionic and nonionic surfactants, (C2) sequestering agents, (C3) polyols, (C4) NaOH or KOH, and (C5) mixtures thereof; then (2) lyophilize the gel thus obtained.
• the solid material acts as an intermediate product that can be used in the preparation of the final gel.
• a gel is prepared according to a process comprising the steps of: (1) contacting with stirring
• a gelling agent (A) which is a pyrogenic hydrophilic silica
• An aqueous solution of a mixture of a substance (B) which may be harmful in aqueous solution which is chosen from the group consisting of
• step (2 °) put in contact with demineralized water, with stirring, the powder obtained at the end of step (2 °) to obtain at the time of use a gel identical or equivalent to that of the from step (1 °).
• the powder and the gel according to the invention are particularly useful, topically, in therapeutics and cosmetics vis-à-vis dermatitis, dermatoses (especially mycoses), particularly vis-à-vis unsightly conditions due to bacterial strains (in particular Staphylococcus aureus and Propionibacterium acnes), fungal (in particular Candidd) or viral strains (in particular Herpes simplex virus).
• bacterial strains in particular Staphylococcus aureus and Propionibacterium acnes
• fungal in particular Candidd
• viral strains in particular Herpes simplex virus
• Example 1 Manufacture of a powder material from an aqueous solution of H 2 O 2 at 50% w / w
• This powder retains all the oxidizing properties of hydrogen peroxide and found the same physical and chemical properties of the original gel after addition with stirring of 550 g of demineralized water of conductivity 1 ⁇ S.cm -1 .
• Example 2 Manufacture of a Powdered Material from a 50% w / w aqueous H 2 O 2 Solution to Strip and Pass Stainless Steels to the Following Formulation Prepared from an Aqueous Solution of H 2 O 2 at 50% w / w:
• Picolinic acid 2 g Ethylene glycol 2 g 80 g of pyrogenic hydrophilic silica are added with stirring at an angular speed of 2000 rpm until a homogeneous gel is formed.
• the gel thus obtained is lyophilized under partial pressure until 570 g of stable powder is obtained.
• This powder retains all the oxidizing properties of hydrogen peroxide and found the same physical and chemical properties of the original gel after addition with stirring of 430 g of deionized water of conductivity 1 ⁇ S.cm "1 .
• EXAMPLE 3 Manufacture of a Powdered Material from a 35% aqueous H 2 O 2 solution for pickling-brightening copper and its alloys to the following formulation made from an aqueous solution of H 2 O 2 to 35% w / w:
• Benzotriazole 30 g 60 g of hydrophilic fumed silica are added with stirring at an angular speed of 2000 rpm until a homogeneous gel is formed.
• the gel thus obtained is lyophilized under reduced pressure to obtain 140 g of stable powder.
• This powder retains all the oxidizing properties of hydrogen peroxide and found the same physical and chemical properties of the original gel after stirring addition of 860 g of deionized water of conductivity 1 ⁇ S.cm "1 .
• benzotriazole acts as a sequestering agent on the one hand and as a corrosion inhibitor on copper on the other hand.
• a portion of the benzotriazole was replaced by a C3 polyol.
• Example 4 Manufacture of a Powdered Material from a 35% w / w aqueous solution of H 2 O 2 for pickling-brightening copper and its alloys To the following formulation made from an aqueous solution of H 2 O 2 at 35% w / w: 720 g water
• Benzotriazole 28 g 60 g of hydrophilic fumed silica are added with stirring at 2000 rpm until a homogeneous gel is formed.
• the gel thus obtained is lyophilized under reduced pressure to obtain 140 g of stable powder.
• This powder retains all the oxidizing properties of hydrogen peroxide and found the same physical and chemical properties of the original gel after stirring addition of 860 g of deionized water of conductivity 1 ⁇ S.cm "1 .
• Example 5 Manufacture of a powdered material from a 1% w / w aqueous H 2 O 2 solution for antimycotic use
• Ethylene Glycol 2 g is added 70 g of hydrophilic fumed silica with stirring at an angular speed of 2000 rev / min until a homogeneous gel is formed.
• the gel thus obtained is lyophilized under partial pressure until a stable storage powder is obtained.
• This powder was applied once a day for 15 days on the zone of a mycosis of the feet of 6 patients. At the end of the 15-day treatment, the feet of all patients no longer had fungal infection.

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• 2005
  • 2005-07-28 EP EP05793058A patent/EP2097502A1/de not_active Withdrawn
  • 2005-07-28 WO PCT/FR2005/001975 patent/WO2006018549A1/fr not_active Ceased

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