CA2317687A1 - Bactericidal silicon dioxide doped with silver - Google Patents

Bactericidal silicon dioxide doped with silver Download PDF

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Publication number
CA2317687A1
CA2317687A1 CA002317687A CA2317687A CA2317687A1 CA 2317687 A1 CA2317687 A1 CA 2317687A1 CA 002317687 A CA002317687 A CA 002317687A CA 2317687 A CA2317687 A CA 2317687A CA 2317687 A1 CA2317687 A1 CA 2317687A1
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Prior art keywords
silver
aerosol
doped
flame
silica
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Abandoned
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CA002317687A
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French (fr)
Inventor
Helmut Mangold
Rainer Golchert
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Evonik Operations GmbH
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Degussa Huels AG
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Publication of CA2317687A1 publication Critical patent/CA2317687A1/en
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00—Use of pretreated ingredients
    • C08K9/02—Ingredients treated with inorganic substances
    • 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
    • A01N59/16—Heavy metals; Compounds thereof
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K6/00—Preparations for dentistry
    • A61K6/70—Preparations for dentistry comprising inorganic additives
    • A61K6/71—Fillers
    • A61K6/76—Fillers comprising silicon-containing compounds
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • A61K8/25—Silicon; Compounds thereof
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L2/00—Methods or apparatus for disinfecting or sterilising materials or objects other than foodstuffs or contact lenses; Accessories therefor
    • A61L2/16—Methods or apparatus for disinfecting or sterilising materials or objects other than foodstuffs or contact lenses; Accessories therefor using chemical substances
    • A61L2/23—Solid substances, e.g. granules, powders, blocks, tablets
    • A61L2/238—Metals or alloys, e.g. oligodynamic metals
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q11/00—Preparations for care of the teeth, of the oral cavity or of dentures; Dentifrices, e.g. toothpastes; Mouth rinses
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/26—Nozzle-type reactors, i.e. the distribution of the initial reactants within the reactor is effected by their introduction or injection through nozzles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
    • B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
    • B01J21/08—Silica
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
    • B01J23/48—Silver or gold
    • B01J23/50—Silver
    • B01J35/31—
    • B01J35/615—
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/0009—Use of binding agents; Moulding; Pressing; Powdering; Granulating; Addition of materials ameliorating the mechanical properties of the product catalyst
    • B01J37/0027—Powdering
    • B01J37/0054—Drying of aerosols
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/08—Heat treatment
    • B01J37/082—Decomposition and pyrolysis
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/113—Silicon oxides; Hydrates thereof
    • C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
    • C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
    • C01B33/181—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof by a dry process
    • C01B33/183—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof by a dry process by oxidation or hydrolysis in the vapour phase of silicon compounds such as halides, trichlorosilane, monosilane
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00051—Controlling the temperature
    • B01J2219/00074—Controlling the temperature by indirect heating or cooling employing heat exchange fluids
    • B01J2219/00087—Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements outside the reactor
    • B01J2219/00094—Jackets
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00051—Controlling the temperature
    • B01J2219/00074—Controlling the temperature by indirect heating or cooling employing heat exchange fluids
    • B01J2219/00105—Controlling the temperature by indirect heating or cooling employing heat exchange fluids part or all of the reactants being heated or cooled outside the reactor while recycling
    • B01J2219/00108—Controlling the temperature by indirect heating or cooling employing heat exchange fluids part or all of the reactants being heated or cooled outside the reactor while recycling involving reactant vapours
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00051—Controlling the temperature
    • B01J2219/00074—Controlling the temperature by indirect heating or cooling employing heat exchange fluids
    • B01J2219/00119—Heat exchange inside a feeding nozzle or nozzle reactor
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00051—Controlling the temperature
    • B01J2219/00157—Controlling the temperature by means of a burner
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/50—Solid solutions
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/50—Solid solutions
    • C01P2002/52—Solid solutions containing elements as dopants
    • C01P2002/54—Solid solutions containing elements as dopants one element only
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/11—Powder tap density
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/12—Surface area
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/80—Compositional purity
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/90—Other properties not specified above

Abstract

Pyrogenically prepared silica doped with silver or silver oxide is prepared by feeding an aerosol into a flame such as is used for the preparation of pyrogenic silica, mixing the aerosol homogeneously with the gas mixture before the reaction, then allowing the aerosol/gas mixture to react in a flame and separating the resulting pyrogenic silicas doped with silver or silver oxide from the gas stream in a known manner.
The pyrogenic silica doped with silver or silver oxide by means of an aerosol can be used as a bactericidal filler.

Description

9.90149 FH/al Bactericidal silicon dioxide doped with silver The invention relates to a pyrogenically prepared silicon dioxide doped with silver or silver oxide by means of an aerosol and having bactericidal properties, and to a process for its preparation and its use. It relates also to its use in dispersions or as a filler in rubber and silicone rubber.
It is known to dope pyrogenically prepared silica in one step in a flame using a special process. (DE 96 50 500 Al).
That process is a combination of a high-temperature flame hydrolysis with a pyrolysis. That doping process is to be distinguished from the older, so-called "co-fumed process", in which the gaseous starting materials (for example SiCl4 gas and A1C13 gas) are pre-mixed and burnt together in a flame reactor.
In the doping process, an aerosol is fed into a flame in which a pyrogenic oxide is produced by flame hydrolysis, the aerosol containing a salt of the compound to be doped.
It has now been found that if silver salts dissolved in water are used as the ,starting material for the aerosol, a doped pyrogenic silica having bactericidal properties is obtained as the product.
The invention provides a pyrogenically prepared silica doped with silver or silver oxide by means of an aerosol, which silica is characterised in that the base component is a silica prepared pyrogenically in the manner of flame oxidation or, preferably, of flame hydrolysis, which silica is doped with a doping component of from 1*10-q and up to 20 wt. o, the doping amount preferably being in the range from 1 to 10,000 ppm and the doping component being a salt or a salt mixture of a silver compound or metallic silver or mixtures thereof, the BET surface area of the doped 990149 FH/al oxide being from 1 to 600 mz/g, preferably in the range from 40 to 400 m2/g.
The invention further provides a process for the preparation of the pyrogenically prepared silica doped with silver or silver oxide by means of an aerosol, which process is characterised in that an aerosol is fed into a flame such as is used for the pyrogenic preparation of silica in the manner of flame oxidation or, preferably, of flame hydrolysis, the aerosol is mixed homogeneously with the gas mixture of the flame oxidation or the flame hydrolysis before the reaction, then the aerosol/gas mixture is allowed to react in the flame and the resulting pyrogenically prepared silicas doped with silver or silver oxide are separated from the gas stream in a known manner, there being used for the preparation of the aerosol an aqueous solution containing salts or salt mixtures of silver or the metal itself in dissolved or suspended form or mixtures thereof, the aerosol being produced by atomisation by means of a two-component nozzle or by a different method of aerosol production.
The following may be used as salts: Ag(N03), Agz(SO9), Ag20, also complexed with complexing agents or ammonia.
The process of flame hydrolysis for the preparation of pyrogenic oxides is known from Ullmanns Enzyklopadie der techn. Chemie 4th edition, Vol. 21, p. 464.
The doped silicon dioxide according to the invention and the process for its preparation and use are explained and described in greater detail with reference to Figure 1 and the following example.
Figure 1 shows a diagrammatic representation of the doping apparatus. The core element of the apparatus is a burner of known type for the preparation of pyrogenic oxides. The burner is designated 1 in Figure 1.

X90149 FH/al The burner 1 consists of a central pipe 2 which opens into a nozzle 3 from which the main gas stream flows into the burner chamber, where it burns. That inner nozzle is surrounded by a further ring nozzle 4, from which (ring or secondary) hydrogen flows.
In the central pipe 2 there is a further axial pipe 5, which ends several centimetres before the nozzle of the central pipe 2. The aerosol is fed into the axial pipe 5.
The aerosol, which consists of an aqueous silver salt solution, is produced in an aerosol generator 6 (ultrasonic atomiser).
The silver saltwater aerosol produced in the aerosol generator is passed by means of a light carrier gas stream through a heating zone 7, in which the entrained water vaporises, leaving behind in the gas phase small salt crystals in finely divided form.
Example 1: Preparation of a pyrogenic silica doped With silver or silver oxide 4.44 kg/h of SiCl4 are vaporised at about 130°C and transferred to the central pipe of a burner of known type.
3 Nm3/h of (primary) hydrogen and 7.5 Nm3/h of air are additionally fed into the central pipe.
The gas mixture flows out of the inner nozzle of the burner , and burns in the burner chamber and the water-cooled flame tube adjacent thereto.
0.5 Nm3/h of (jacket or secondary) hydrogen are fed into the jacket nozzle.
12 Nm3/h of (secondary) air are additionally fed into the burner chamber.
The second gas component flows out of the axial pipe 5 into the central pipe 2.

9.90149 FH/al The second gas stream consists of an aerosol which is produced in a separate atomising unit by ultrasonic atomisation. The aerosol generator atomises 725 g/h of 5 0 aqueous silver sulfate solution. The silver sulfate aerosol is guided through a heated line with the aid of the carrier gas of 0.5 Nm3/h of air, the aqueous aerosol being converted at temperatures of about 180°C into a gas and a salt crystal aerosol.
The reaction gases and the resulting pyrogenic silica doped with silver or silver oxide are drawn through a cooling system by the application of a reduced pressure, and the particle gas stream thereby cools to about from 100 to 160°C. The solid is separated from the waste gas stream in a filter or cyclone.
The pyrogenically prepared silica doped with silver (oxide) is obtained in the form of a finely divided white powder.
In a further step, any hydrochloric acid residues still adhering to the silica. are removed therefrom at elevated temperature by treatment with air containing water vapour.
The BET surface area of the pyrogenic silica doped with silver is 206 m2/g.
The preparation conditions are summarised in Table 1, further analytical data of the silica so obtained are given in Table 2.

990149 FH/al Table 1 Experimental conditions in the preparation of pyrogenic silica doped with silver (oxide) SiCl9 Primary Sec. Hz HZ Salt Aerosol Air BET

air air core jacket solu- amount aeros. m2/g Nm3/h Nm3/h Nm3/h Nm3/h tion kg/h Nm3/h kg/h 4.44 7.5 12 3 0.5 50 0.725 0.5 206 aqueous AgZS04 5 Explanation: Primary air = amount of air in the central pipe; Sec. air = secondary air; H2 core = hydrogen in the central pipe; Aerosol amount = mass flow rate of the salt solution converted into aerosol form; Air aerosol = amount of carrier gas (air) for the aerosol;
Table 2 Analytical data BET pH value Tamped Ag20 4g sus. density content mz/g g/1 wt.~ , Example 206 4.13 24 1.72 Explanation: pH 4~ sus. - pH value of the 4 o aqueous suspension Advantages of the silica according to the invention The silica according to the invention has bactericidal properties.

Claims (3)

1. Pyrogenically prepared silica doped with silver or silver oxide, characterised in that the base component is a silica prepared pyrogenically in the manner of flame oxidation or, preferably, of flame hydrolysis, which silica has been doped with a doping component of from 0.0001 wt.% (= 1x10 -4 wt.%) and up to 20 wt.%, the doping amount preferably being in the range from 1 to 10,000 ppm and the doping component being a salt or a salt mixture of silver or a suspension of a silver compound or metallic silver or mixtures thereof, the BET
surface area of the doped oxide being from 1 to 600 m2/g, preferably in the range from 40 to 400 m2/g.
2. Process for the preparation of pyrogenic oxides doped with silver or silver oxide, characterised in that an aerosol is fed into a flame such as is used for the preparation of pyrogenic silica in the manner of flame oxidation or, preferably, of flame hydrolysis, the aerosol is mixed homogeneously with the gas mixture of the flame oxidation or the flame hydrolysis before the reaction, then the aerosol/gas mixture is allowed to react in a flame and the resulting pyrogenic silicas doped with silver or silver oxide are separated from the gas stream in a known manner, there being used as the starting material for the aerosol a salt solution containing salts or salt mixtures of silver or the metal itself in dissolved or suspended form or mixtures thereof, the aerosol being produced by atomisation by means of a two-component nozzle or by a different method of aerosol production, preferably by an aerosol generator by means of ultrasonic atomisation.
3. Use of the pyrogenic silica doped with silver or silver oxide by means of an aerosol as a bactericidal filler especially in the production of paints or coatings, in the paper industry, as a catalytically active substance, as a starting material for the preparation of dispersions, as a polishing material (CMP applications), as a ceramics base material, in the electronics industry, as a filler for polymers, as a starting material for the production of glass or glass coatings or glass fibres, as a release auxiliary even at high temperatures, in the cosmetics industry, as an absorber material, as an additive in the silicone and rubber industry, for adjusting the rheology of liquid systems, for heat protection stabilisation, as a heat insulating material, as a flow auxiliary, as a filler in the dental industry, as an adjuvant in the pharmaceuticals industry, in the paints industry.
CA002317687A 1999-09-09 2000-09-07 Bactericidal silicon dioxide doped with silver Abandoned CA2317687A1 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE19943057.8 1999-09-09
DE19943057A DE19943057A1 (en) 1999-09-09 1999-09-09 Bactericidal, silver-doped silicon dioxide

Publications (1)

Publication Number Publication Date
CA2317687A1 true CA2317687A1 (en) 2001-03-09

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CA002317687A Abandoned CA2317687A1 (en) 1999-09-09 2000-09-07 Bactericidal silicon dioxide doped with silver

Country Status (11)

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US (2) US6423331B1 (en)
EP (1) EP1083146B1 (en)
JP (1) JP3745208B2 (en)
AT (1) ATE236854T1 (en)
CA (1) CA2317687A1 (en)
DE (2) DE19943057A1 (en)
DK (1) DK1083146T3 (en)
ES (1) ES2191588T3 (en)
IL (1) IL138349A0 (en)
NO (1) NO20004484L (en)
TW (1) TW524774B (en)

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Publication number Priority date Publication date Assignee Title
WO2012158702A2 (en) * 2011-05-16 2012-11-22 Basf Se An antimicrobial metal composite
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US6872402B2 (en) 2005-03-29
US20030235624A1 (en) 2003-12-25
EP1083146B1 (en) 2003-04-09
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