Classifications

• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
  • A61K33/00—Medicinal preparations containing inorganic active ingredients
  • A61K33/24—Heavy metals; Compounds thereof
  • A61K33/242—Gold; Compounds thereof
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
  • A61K31/00—Medicinal preparations containing organic active ingredients
  • A61K31/28—Compounds containing heavy metals
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
  • A61K33/00—Medicinal preparations containing inorganic active ingredients
  • A61K33/24—Heavy metals; Compounds thereof
  • A61K33/34—Copper; Compounds thereof
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
  • A61K33/00—Medicinal preparations containing inorganic active ingredients
  • A61K33/24—Heavy metals; Compounds thereof
  • A61K33/38—Silver; Compounds thereof
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
  • A61K33/00—Medicinal preparations containing inorganic active ingredients
  • A61K33/44—Elemental carbon, e.g. charcoal, carbon black
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B82—NANOTECHNOLOGY
  • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
  • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
• • C—CHEMISTRY; METALLURGY
  • C01—INORGANIC CHEMISTRY
  • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
  • C01B13/00—Oxygen; Ozone; Oxides or hydroxides in general
  • C01B13/14—Methods for preparing oxides or hydroxides in general
• • C—CHEMISTRY; METALLURGY
  • C01—INORGANIC CHEMISTRY
  • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
  • C01B32/00—Carbon; Compounds thereof
  • C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
• • C—CHEMISTRY; METALLURGY
  • C01—INORGANIC CHEMISTRY
  • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
  • C01G3/00—Compounds of copper
• • C—CHEMISTRY; METALLURGY
  • C01—INORGANIC CHEMISTRY
  • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
  • C01G5/00—Compounds of silver
• • C—CHEMISTRY; METALLURGY
  • C01—INORGANIC CHEMISTRY
  • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
  • C01G55/00—Compounds of ruthenium, rhodium, palladium, osmium, iridium, or platinum
• • C—CHEMISTRY; METALLURGY
  • C01—INORGANIC CHEMISTRY
  • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
  • C01G7/00—Compounds of gold
• • C—CHEMISTRY; METALLURGY
  • C01—INORGANIC CHEMISTRY
  • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
  • C01P2004/00—Particle morphology
  • C01P2004/30—Particle morphology extending in three dimensions
  • C01P2004/32—Spheres
• • C—CHEMISTRY; METALLURGY
  • C01—INORGANIC CHEMISTRY
  • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
  • C01P2004/00—Particle morphology
  • C01P2004/60—Particles characterised by their size
  • C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer

Definitions

• the present invention concerns a process for preparing metal hydroxides, hydroxyl organometals and white carbon.
• the purity and biocompatibility of the thus obtained substances is such that they can be used for several applications, while being particularly suitable for use in Ayurvedic medicine.
• said process involves an initial step of electrolysis followed by at least five cycles of microwave irradiation with increasing intensity.
• the process also includes steps of recovering the gases that are released.
• Ayurveda is the traditional medicine used in India since the 4 th millennium B.C. and even today is still more widespread in the Asian sub-continent than Western medicine.
• Ayurveda therapeutic use is made of medicines of plant and animal origin as well as of metals, minerals, precious and semi-precious stones. All these are used in their natural form, or treated in order to extract the full essence or to make them non-toxic, palatable, assimilable and therapeutically more potent. Certain parts of these medicines, such as alkaloids, glucose and other active principles, are not extracted for therapeutic use. According to Ayurveda each medicine possesses useful therapeutic parts which, if used alone, can produce a toxic effect. However, the same medicine contains other parts that counterbalance the toxic effects. Hence it should be noted that the whole medicine is utilized and neither the isolated parts nor chemical syntheses are used. In addition, each medicinal product has a specific mode of use in order to function at its maximum effectiveness.
• metals and organometals are used in which said metals are for example silver and copper.
• these substances are prepared by processes requiring a very long time, on average not less than two or three months. Therefore, the need was felt for processes that would significantly reduce production times without altering the beneficial effects of said substances, but possibly also increasing their biocompatibility.
• the object of the present invention is therefore to identify a process for producing metals and organometals that is more rapidly implemented, highly reproducible, and able to maintain and/or increase the properties of the treated substances, including their purity and biocompatibility.
• step III) subjecting the mixture deriving from step II) to a first cycle of treatment comprising:
• step b) concentrating the mixture deriving from step a) to about 20% of the volume thereof, by subjecting the same to microwave irradiation at a power of 200-270W;
• step f) concentrating the mixture deriving from step f) to about 5-10% of the volume thereof, by subjecting the same to microwave irradiation at a power of 400-450W; g) bringing to volume by adding osmotic water and stirring; h) repeating 4 times the steps f)-g) and then repeating the step f);
• step h) subjecting the concentrated mixture deriving from step h) to a third cycle of treatment comprising:
• step i) drying the mixture deriving from step i) by subjecting the same to microwave irradiation at a power of 600-650W;
• step p) drying the mixture deriving from step o) by subjecting the same to microwave irradiation at a power of 700-850W;
• step VII) subjecting the concentrated mixture deriving from step r) to a fifth cycle of treatment comprising:
• step t) drying the mixture deriving from step s) by subjecting the same to microwave irradiation at a power of 1000-3000W;
• the process for preparing metal hydroxides, hydroxy! organometals and white carbon further comprises a step of recovering the gases released during the concentration and drying steps so as to increase the final product yield.
• Figure 1A and Figure 1 B show the product obtained in Example 1 by the process of the invention.
• Figure 2 shows the product obtained in Example 2 by the process of the invention.
• Figure 3 shows the product obtained in Example 3 by the process of the invention.
• Figure 4 shows the product obtained in Example 4 by the process of the invention.
• Figure 5 shows the product obtained in Example 5 by the process of the invention.
• Figure 6A and Figure 6B show the product obtained in Example 6 by the process of the invention.
• Figure 7 shows the product obtained in Example 7 by the process of the invention.
• Figure 8 shows the product obtained in Example 8 by the process of the invention.
• Figure 9 shows the product obtained in Example 9 by the process of the invention.
• Figure 10 shows the product obtained in Example 10 by the process of the invention.
• Figure 11 shows the product obtained in Example 11 by the process of the invention.
• Figure 12 shows the product obtained in Example 12 by the process of the invention.
• Figure 13 shows the product obtained in Example 13 by the process of the invention.
• Figure 14 shows the product obtained in Example 14 by the process of the invention.
• Figure 15 shows the product obtained in Example 15 by the process of the invention.
• the invention therefore relates to a process for preparing metal hydroxides, hydroxy! organometals and white carbon, comprising the steps of:
• step III) subjecting the mixture deriving from step II) to a first cycle of treatment comprising:
• step b) concentrating the mixture deriving from step a) to about 20% of the volume thereof, by subjecting the same to microwave irradiation at a power of 200-270W;
• step f) concentrating the mixture deriving from step f) to about 5-10% of the volume thereof, by subjecting the same to microwave irradiation at a power of 400-450W;
• step h) subjecting the concentrated mixture deriving from step h) to a third cycle of treatment comprising:
• step i) drying the mixture deriving from step i) by subjecting the same to microwave irradiation at a power of 600-650W;
• step p) drying the mixture deriving from step o) by subjecting the same to microwave irradiation at a power of 700-850W;
• step VII) subjecting the concentrated mixture deriving from step r) to a fifth cycle of treatment comprising:
• step t) drying the mixture deriving from step s) by subjecting the same to microwave irradiation at a power of 1000-3000W;
• step V in which both microwave power and H 2 O 2 concentration are increasing, the impurities present in the starting substance are released from the elemental structure of the starting substance by absorbing the energy provided by the microwaves and then removed by the evaporating water.
• the substance purified in this manner is believed to acquire its final physico-chemical characteristics, i.e.
• the process of the invention provides that, in step v), after having repeated steps t)-u) at least twice, the gases are conveyed and collected while performing the remaining four repetitions of steps t)-u) in order to recover the product that was removed by the evaporating water.
• the gases are conveyed and collected while performing the remaining four repetitions of steps t)-u) in order to recover the product that was removed by the evaporating water.
• this recovery is particularly effective specially because it is carried out almost at the end of the whole process, i.e. when the product already has a high degree of purity. In fact at that point the gases released essentially no longer contain any impurities and so the risk of re-condensing them with consequent re- contamination of the product is very low.
• the metals used in the process according to the invention are transition metals such as palladium, platinum, nickel, cobalt, iridium, ruthenium and osmium.
• transition metals such as palladium, platinum, nickel, cobalt, iridium, ruthenium and osmium.
• the process proved to be particularly suitable for the treatment of these metals which, as can be seen in the working examples given hereinafter, presented extremely fine particle sizes of the order of tens or hundreds of nanometers, thus imperceptible to the touch and consequently particularly assimilable and biocompatible.
• said metals are noble metals of group 11 of the periodic table, such as copper (Cu), silver (Ag) and gold (Au).
• Cu copper
• Ag silver
• Au gold
• the latter as well as being found to be advantageously more biocompatible and assimilable by the body at the end of the process of the invention, are extremely important from the viewpoint of therapeutic use according to the teachings of Ayurvedic medicine.
• ascorbic acid or acetic acid is further added in steps II), i) and/or o) of the process.
• ascorbic acid is even more preferred, as it has been found to enhance and increase ionic exchanges in solution during microwave application. It is therefore believed to confer to the final product an improved biocompatibility and assimilability by the body.
• the process of the invention also comprises a step VIII) of separation by filtration or sedimentation following step v).
• the solution deriving from step v) can be filtered or allowed to settle so as to separate the solid product from the solution.
• step VII) can be repeated twice; the first time with microwave power at 1000-1500W, and the second time at 2500-3000W. In this manner a purer final product is obtained, having an even smaller particle size and hence an increased biocompatibility.
• thermometer a tester: a STAR TS 1025-00 digital multimeter with thermometer.
• a 10 g filament of Au (purity 23K) was subjected to electrolysis with a small graphite cylinder in 240 ml of an acid 20% H 2 O 2 solution and 1 g of laevo-rotatory vitamin C for 48 hours, applying a 150A current and a 220V voltage.
• the mixture deriving from said electrolysis comprising the thus oxidized C and Au ions, after adding 300 ml of osmotic water containing 60 ml of 25% H 2 O 2 , was left to settle for about 48 hours while stirring said mixture about every 12 hours.
• This mixture was then subjected to the first microwave irradiation cycle at a power of 250W to concentrate it to about 20% of its volume.
• the mixture thus concentrated was brought to volume with osmotic water and then stirred for several minutes. Said microwave irradiation to reduce the volume to 20% followed by osmotic water addition was repeated 3 times, after which the microwave irradiation was repeated once more.
• the mixture thus concentrated was brought to volume with osmotic water then stirred for several minutes. Said microwave irradiation to reduce the volume to 5% followed by osmotic water addition was repeated 4 times, after which microwave irradiation was repeated only once more.
• the product also had a pH of 1 with high electrical conductivity.
• Example 1 was repeated, but in this case, during all the various microwave irradiation treatments, the gases were conveyed and collected so as to also recover the gold particles, which would otherwise be lost during water evaporation. Thus 1.65 g of hydroxy-organometal of Au were obtained.
• This product illustrated in figure 2, was hygroscopic and highly water-soluble with an intense golden colour, but was reddish-brown if in a very concentrated solution. It also exhibited high electrical conductivity.
• the product was bitter-sweet and astringent in taste, and slightly more pungent than the product of Example 1.
• Example 2 was repeated, but in this case a 10 g filament of Ag was used (purity
• the final product is illustrated in figure 3, showing a magnification of the crystals obtained which are white in colour in very concentrated solutions but able to turn reddish-brown if dried at high temperatures.
• This product was hygroscopic, highly water-soluble and bitter-sweet in taste.
• Example 2 was repeated but in this case a 10 g filament of Cu was used (purity
• the final product is illustrated in figure 4, showing a magnification of the crystals obtained which are pale bluish-white in colour in very concentrated solutions but able to turn reddish-brown if dried at high temperatures.
• This product was hygroscopic, highly water-soluble and bitter astringent in taste.
• the mixture deriving from said electrolysis comprising the thus oxidized C ions, after adding 300 ml of osmotic water containing 60 ml of 20% H 2 O2, was left to settle for about 48 hours while stirring said mixture about every 12 hours.
• This mixture was then subjected to the first microwave irradiation cycle at a power of 250W to concentrate it to about 30% of its volume.
• the mixture thus concentrated was brought to volume with osmotic water and then stirred for several minutes. Said microwave irradiation to reduce the volume to 20% followed by osmotic water addition was repeated 3 times, after which microwave irradiation was repeated only once more.
• ml of osmotic water containing 40% H 2 O 2 was then subjected to the second microwave irradiation cycle at a power of 400-450W to concentrate it to about 5% of its volume.
• the mixture thus concentrated was brought to volume with osmotic water and then stirred for several minutes. Said microwave irradiation to reduce the volume to 5% followed by osmotic water addition was repeated 4 times, after which microwave irradiation was repeated only once more.
• the product also had a high electrical conductivity.
• Example 5 was repeated, but in this case 1 g of ascorbic acid was also added to every aqueous solution comprising H 2 O 2 .
• Example 5 was repeated, except that the final sedimentation step was carried out at a constant temperature between 25 and 28°C in a sealed glass container placed in such a manner as not to be subjected to even a minimal vibration or tremor.
• Example 7 was repeated but in this case, 1 g of ascorbic acid was further added to every aqueous solution comprising H 2 O 2 .
• nanotubes were noted as being more defined and better structured than the nanotubes obtained in
• the mixture deriving from said electrolysis comprising the thus oxidized Ag ions, after adding 300 ml of osmotic water containing 60 mi of 20% H 2 O 2 , was left to settle for about 48 hours while stirring said mixture about every 12 hours.
• This mixture was then subjected to the first microwave irradiation cycle at a power of 250W to concentrate it to about 20% of its volume.
• the mixture thus concentrated was brought to volume with osmotic water and then stirred for several minutes. Said microwave irradiation to reduce the volume to 20% followed by osmotic water addition was repeated 3 times, after which microwave irradiation was repeated only once more.
• the mixture thus concentrated was brought to volume with osmotic water and then stirred for several minutes. Said microwave irradiation to reduce the volume to 5% followed by osmotic water addition was repeated 4 times, after which microwave irradiation was repeated only once more.
• the product was sweet and slightly astringent to taste.
• Example 9 was repeated, but in this case, in parallel and separately to the electrolysis of silver, an electrolysis of gold was also carried out.
• Example 9 was repeated, but in this case, in parallel and separately to the electrolysis of silver, an electrolysis of copper was also carried out.
• step VII 2 mg of pure S were added after three repetitions.
• Example 9 was repeated, but in this case a filament of palladium was used.
• Example 13 Preparation of indium hydroxide according to the present invention Example 9 was repeated but in this case a filament of iridium was used.
• Example 14 Preparation of hydroxy-organometals of Au vehicled by white carbon nanotubes according to the present invention
• the thus obtained mixture was subjected to a first treatment by microwave irradiation at a power of 700-850W to reduce the volume by half, and then to a second treatment by microwave irradiation at a power of 1000W to reduce the volume by half.
• Example 15 Preparation of gold hydroxide according to the present invention Example 14 was repeated, but in this case the mixture was composed of 65% white carbon and 35% hydroxy-organometal of Au crystals in 300 ml of osmotic water. This mixture was subjected to a first microwave irradiation treatment at a power of 700-850W until the volume was reduced by half, then to a second microwave irradiation treatment at a power of 1000W until the volume was reduced by half.
• the entire mixture was microwave irradiated at a power of 700-850W until the volume was reduced by half, then brought to volume with osmotic water. This treatment was repeated a further five times.
• the mixture was then allowed to settle as with the nanotube preparation, in the absence of vibrations or tremors for 10-15 days at about 25°C.
• the process enables metal hydroxides, hydroxyl organometals and white carbon to be produced in a highly reproducible manner, while at the same time significantly reducing production times without altering the beneficial effects of said substances, indeed advantageously increasing the biocompatibility and assimilability by the body when administering for therapeutic purposes.
• the suitable combination of an electrolysis step and subsequent microwave irradiation treatments enables a final product to be obtained which, independently of the starting substance, i.e. metals or carbon or both, presents much improved physico-chemical characteristics, as shown above.

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• 2009
  • 2009-08-13 IT ITMI2009A001479A patent/IT1395170B1/it active
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