WO2011018773A1 - Process for preparing metal hydroxides, hydroxyl organometals and white carbon suitable for use in ayurvedic medicine - Google Patents

Process for preparing metal hydroxides, hydroxyl organometals and white carbon suitable for use in ayurvedic medicine Download PDF

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Publication number
WO2011018773A1
WO2011018773A1 PCT/IB2010/053660 IB2010053660W WO2011018773A1 WO 2011018773 A1 WO2011018773 A1 WO 2011018773A1 IB 2010053660 W IB2010053660 W IB 2010053660W WO 2011018773 A1 WO2011018773 A1 WO 2011018773A1
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volume
subjecting
osmotic water
mixture
microwave irradiation
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PCT/IB2010/053660
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French (fr)
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Antonio Merati
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Ics Green Growing Srl
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Priority to EA201200286A priority Critical patent/EA027785B1/en
Priority to EP10759993A priority patent/EP2464360A1/en
Priority to AU2010283463A priority patent/AU2010283463B2/en
Priority to CN201080035883XA priority patent/CN102481314A/en
Publication of WO2011018773A1 publication Critical patent/WO2011018773A1/en

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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K33/00Medicinal preparations containing inorganic active ingredients
    • A61K33/24Heavy metals; Compounds thereof
    • A61K33/242Gold; Compounds thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K31/00Medicinal preparations containing organic active ingredients
    • A61K31/28Compounds containing heavy metals
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K33/00Medicinal preparations containing inorganic active ingredients
    • A61K33/24Heavy metals; Compounds thereof
    • A61K33/34Copper; Compounds thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K33/00Medicinal preparations containing inorganic active ingredients
    • A61K33/24Heavy metals; Compounds thereof
    • A61K33/38Silver; Compounds thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K33/00Medicinal preparations containing inorganic active ingredients
    • A61K33/44Elemental carbon, e.g. charcoal, carbon black
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00Nanotechnology for materials or surface science, e.g. nanocomposites
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B13/00Oxygen; Ozone; Oxides or hydroxides in general
    • C01B13/14Methods for preparing oxides or hydroxides in general
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/05Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G3/00Compounds of copper
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G5/00Compounds of silver
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G55/00Compounds of ruthenium, rhodium, palladium, osmium, iridium, or platinum
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G7/00Compounds of gold
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/30Particle morphology extending in three dimensions
    • C01P2004/32Spheres
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/60Particles characterised by their size
    • C01P2004/64Nanometer 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.

Abstract

A process is described for preparing metal hydroxides, hydroxyl organometals an 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. Specifically, this process involves an initial step of electrolysis followed by at leas five cycles of microwave irradiation with increasing intensity. Preferably, the process also includes a step of recovering the gases that are released in order to increase the yield of the final product.

Description

PROCESS FOR PREPARING METAL HYDROXIDES, HYDROXYL ORGANOMETALS AND WHITE CARBON SUITABLE FOR USE IN AYURVEDIC MEDICINE FIELD OF THE INVENTION
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.
Specifically, said process involves an initial step of electrolysis followed by at least five cycles of microwave irradiation with increasing intensity.
Preferably, the process also includes steps of recovering the gases that are released.
STATE OF THE ART
Ayurveda is the traditional medicine used in India since the 4th millennium B.C. and even today is still more widespread in the Asian sub-continent than Western medicine. The European Union, most of the Member States and the WHO count it among the non-conventional medicines whose dispensing is permitted only by qualified medical doctors.
In 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.
For cellular regeneration, in particular, metals and organometals are used in which said metals are for example silver and copper.
According to the Ayurvedic handbook 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.
SUMMARY OF THE INVENTION
The above object was achieved by a process for preparing metal hydroxides, hydroxyl organometals and white carbon comprising the steps of:
I) providing carbon and/or at least a metal;
II) subjecting said carbon and/or at least a metal to electrolysis in an acid solution of 15% to 25% H2O2 for a period of time of 24 to 72 hours;
III) subjecting the mixture deriving from step II) to a first cycle of treatment comprising:
a) after the addition of further acid solution of 20% to 30% H2O2, letting the mixture to settle for about 48 hours, while stirring the same about every 12 hours;
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;
c) bringing to volume by adding osmotic water and stirring;
d) repeating 3 times the steps b)-c) and then repeating the step b);
IV) subjecting the concentrated mixture deriving from step d) to a second cycle of treatment comprising:
e) adding an acid solution of 30% to 40% H2O2 and osmotic water;
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);
V) subjecting the concentrated mixture deriving from step h) to a third cycle of treatment comprising:
i) adding an acid solution of 40% to 50% H2O2 and osmotic water;
I) drying the mixture deriving from step i) by subjecting the same to microwave irradiation at a power of 600-650W;
m) bringing to volume by adding osmotic water and stirring;
n) repeating 3 times the steps l)-m) and then repeating the step I);
Vl) subjecting the concentrated mixture deriving from step n) to a fourth cycle of treatment comprising:
o) adding an acid solution of 20% H2O2 and osmotic water;
p) drying the mixture deriving from step o) by subjecting the same to microwave irradiation at a power of 700-850W;
q) bringing to volume by adding osmotic water and stirring;
r) repeating 3 times the steps p)-q) and then repeating the step p);
VII) subjecting the concentrated mixture deriving from step r) to a fifth cycle of treatment comprising:
s) adding osmotic water;
t) drying the mixture deriving from step s) by subjecting the same to microwave irradiation at a power of 1000-3000W;
u) bringing to volume by adding osmotic water and stirring;
v) repeating 6 times the steps t)-u).
In another aspect, 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.
BRIEF DESCRIPTION OF THE FIGURES
The characteristics and advantages of the present invention will be evident from the detailed description given below, from the working examples provided for illustrative and non-limiting purposes, and from the appended Figures wherein: 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.
DETAILED DESCRIPiTON OF THE INVENTION
The invention therefore relates to a process for preparing metal hydroxides, hydroxy! organometals and white carbon, comprising the steps of:
I) providing carbon and/or at least a metal;
II) subjecting said carbon and/or at least a metal to electrolysis in an acid solution of 15% to 25% H2O2 for a period of time of 24 to 72 hours;
III) subjecting the mixture deriving from step II) to a first cycle of treatment comprising:
a) after the addition of further acid solution of 20% to 30% H2O2, letting the mixture to settle for about 48 hours, while stirring the same about every 12 hours;
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;
c) bringing to volume by adding osmotic water and stirring;
d) repeating 3 times the steps b)-c) and then repeating the step b);
IV) subjecting the concentrated mixture deriving from step d) to a second cycle of treatment comprising:
e) adding an acid solution of 30% to 40% H2O2 and osmotic water;
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);
V) subjecting the concentrated mixture deriving from step h) to a third cycle of treatment comprising:
i) adding an acid solution of 40% to 50% H2O2 and osmotic water;
I) drying the mixture deriving from step i) by subjecting the same to microwave irradiation at a power of 600-650W;
m) bringing to volume by adding osmotic water and stirring;
n) repeating 3 times the steps l)-m) and then repeating the step I);
VI) subjecting the concentrated mixture deriving from step n) to a fourth cycle of treatment comprising:
o) adding an acid solution of 20% H2O2 and osmotic water;
p) drying the mixture deriving from step o) by subjecting the same to microwave irradiation at a power of 700-850W;
q) bringing to volume by adding osmotic water and stirring;
r) repeating 3 times the steps p)-q) and then repeating the step p);
VII) subjecting the concentrated mixture deriving from step r) to a fifth cycle of treatment comprising:
s) adding osmotic water;
t) drying the mixture deriving from step s) by subjecting the same to microwave irradiation at a power of 1000-3000W;
u) bringing to volume by adding osmotic water and stirring;
v) repeating 6 times the steps t)-u).
It was noted in fact that the suitable combination of electrolysis steps 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, exhibits extremely improved physico-chemical characteristics. In particular, it was noted that these characteristics improve as increasing microwave power is applied, while H2O2 concentration is firstly increased then reduced, until being absent in the final step of microwave irradiation.
Without to be bound by any theory, it is believed that during the first part of the process, i.e until step V), in which both microwave power and H2O2 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. However, during the second part of the process in which the microwave power is still increasing yet the H2O2 concentration is decreasing to zero, the substance purified in this manner is believed to acquire its final physico-chemical characteristics, i.e. almost spherical particles, having particle sizes in the order of tens or hundreds of nanometers, which are very light and imperceptible to the touch and hence conveniently and advantageously far more assimilable by the body than the starting substance, when administered for therapeutic purposes.
In a preferred embodiment, 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. During the volume reduction by microwave irradiation, it was noted that a part of the product particles were removed and dispersed, thus leading to a decrease in final yield. By conveying and collecting the gases formed during microwave application it was possible to obviate said losses and thereby increase the yield.
Also, 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.
Preferably, the metals used in the process according to the invention are 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.
Preferably, said metals are noble metals of group 11 of the periodic table, such as copper (Cu), silver (Ag) and gold (Au). Indeed, 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.
In another preferred embodiment of the invention, ascorbic acid or acetic acid is further added in steps II), i) and/or o) of the process.
The use of 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.
In a further preferred embodiment, the process of the invention also comprises a step VIII) of separation by filtration or sedimentation following step v). In this respect, if obtaining the final product in solid form is preferred, the solution deriving from step v) can be filtered or allowed to settle so as to separate the solid product from the solution.
In a yet further embodiment, 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.
Working examples of the present invention are given hereinafter provided for illustrative and non-limiting purposes. EXAMPLES
Instrumentation used
For implementing the examples given below the following instruments were used:
- for the electrolysis: a portable battery charger with fast starter CLASS BOOSTER 15OA (commercially available from DECA);
- for microwave irradiation: Ulisse Olimpic microwave oven (commercially available from D.P.E. Ltd) or a PANASONIC NN GD 458 W EPG microwave oven; and
- a tester: a STAR TS 1025-00 digital multimeter with thermometer.
Example 1. Preparation of hydroxy-organometals of Au according to the present invention
A 10 g filament of Au (purity 23K) was subjected to electrolysis with a small graphite cylinder in 240 ml of an acid 20% H2O2 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% H2O2, 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 to 20% of its volume to which were added 300 ml of osmotic water containing 30% H2O2, 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 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 mixture thus concentrated to 5% of its volume to which were added 300 ml of osmotic water containing 40% H2O2 and 1 g of laevo-rotatory vitamin C, was then evaporated to dryness. A reduced product was thus obtained of appearance similar to caramel. This reduced product was brought to volume with osmotic water then stirred for several minutes. The mixture thus obtained was then subjected to the third microwave irradiation cycle at a power of 600-65OW to again evaporate it to dryness. Said addition of osmotic water and subsequent microwave irradiation to dryness were repeated 4 times.
The thus dried mixture to which were added 300 ml of osmotic water containing 20% H2O2 and 1 g of laevo-rotatory vitamin C, was then evaporated to dryness. A dark brown reduced product was thus obtained. This reduced product was brought to volume with osmotic water and then stirred for several minutes. The mixture thus obtained was then subjected to the fourth microwave irradiation cycle at a power of 700-850W to again evaporate it to dryness. Said addition of osmotic water and subsequent microwave irradiation to dryness were repeated 4 times, The thus dried mixture to which 300 ml of osmotic water were added was then evaporated to dryness. A dark reddish-brown reduced product was thus obtained. This reduced product was brought to volume with osmotic water and then stirred for several minutes. The mixture thus obtained was then subjected to the fifth microwave irradiation cycle at a power of 1000W to again evaporate it to dryness. Said addition of osmotic water and subsequent microwave irradiation to dryness were repeated 6 times.
Finally, 300 ml of osmotic water were added, the mixture was reduced to half its volume and the final product was separated by filtration.
1.5 g of hydroxy-organometal of Au were obtained. This product, illustrated in Figures 1A and 1B, was hygroscopic and highly water-so\uble with an intense golden colour, but was reddish-brown if in a very concentrated solution.
The product also had a pH of 1 with high electrical conductivity.
The taste was bitter-sweet and slightly pungent.
Example 2. Preparation of hydroxy-organometals of Au according to the present invention with gas recovery
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.
Having introduced the gas recovery steps, it was possible to increase the yield of the final product as well as to obtain finer final particles.
Example 3. Preparation of hydroxy-organometals of Ag according to the present invention
Example 2 was repeated, but in this case a 10 g filament of Ag was used (purity
99.8%).
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 4. Preparation of hydroxy-organometals of Cu according to the present invention
Example 2 was repeated but in this case a 10 g filament of Cu was used (purity
99.5%).
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.
Example 5. Preparation of white carbon according to the present invention
Two small graphite cylinders were subjected to electrolysis in 240 ml of an acid
20% H2O2 solution for 48 hours, applying a 150A current and a 220V voltage.
The mixture deriving from said electrolysis comprising the thus oxidized C ions, after adding 300 ml of osmotic water containing 60 ml of 20% H2O2, 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.
The mixture thus concentrated to 20% of its volume to which were added 300. ml of osmotic water containing 40% H2O2, 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 mixture thus concentrated to 5% of its volume to which were added 300 ml of osmotic water containing 50% H2O2, was then evaporated to dryness. This dried mixture was brought to volume with osmotic water and then stirred for several minutes. The mixture thus obtained was then subjected to the third microwave irradiation cycle at a power of 600-650W to again evaporate it to dryness. Said addition of osmotic water and subsequent microwave irradiation to dryness were repeated 4 times.
The thus dried mixture to which were added 300 ml of osmotic water containing 20% H2O2, was evaporated to dryness. A white reduced product was thus obtained. This dried mixture was brought to volume with osmotic water and then stirred for several minutes. The mixture thus obtained was then subjected to the fourth microwave irradiation cycle at a power of 700-850W to again evaporate it to dryness. Said addition of osmotic water and subsequent microwave irradiation to dryness were repeated 4 times.
The thus dried mixture, to which were added 300 ml of osmotic water, was then evaporated to dryness. This dried mixture was brought to volume with osmotic water and then stirred for several minutes. The mixture thus obtained was then subjected to the fifth microwave irradiation cycle at a power of 1000W to again evaporate it to dryness. Said addition of osmotic water and subsequent microwave irradiation to dryness were repeated 6 times.
Finally, 300 ml of osmotic water were added, the mixture was reduced to half its volume and the final product was separated by sedimentation. 1 g of white carbon was obtained. This product appeared in the form of a white crystalline powder as illustrated in Figure 5, it being highly water-soluble and white in colour.
The product also had a high electrical conductivity.
Example 6. Preparation of white carbon according to the present invention
Example 5 was repeated, but in this case 1 g of ascorbic acid was also added to every aqueous solution comprising H2O2.
The presence of ascorbic acid was considered to promote and increase ionic exchanges in solution during microwave application; this confers to the final product an improved biocompatibility and assimilability by the body. The final product is illustrated in Figures 6A and 6B.
Example 7. Preparation of white carbon nanotubes according to the present invention
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.
After 20-25 days, the formation of white carbon nanotubes was observed, as illustrated in Figure 7.
Example 8. Preparation of white carbon nanotubes according to the present invention
Example 7 was repeated but in this case, 1 g of ascorbic acid was further added to every aqueous solution comprising H2O2.
The presence of ascorbic acid was considered to promote and increase ionic exchanges in solution during microwave application. The nanotubes were noted as being more defined and better structured than the nanotubes obtained in
Example 5, as is clearly illustrated in Figure 8.
Example 9. Preparation of silver hydroxide according to the present invention
Two 1O g filaments of Ag (purity 99.8%) were subjected to electrolysis in 240 ml of an acid 20% H2O2 solution for 48 hours, applying a 150A current and a 220V voltage.
The mixture deriving from said electrolysis comprising the thus oxidized Ag ions, after adding 300 ml of osmotic water containing 60 mi of 20% H2O2, 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 to 20% of its volume to which were added 300 ml of osmotic water containing 30% H2O2, 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 mixture thus concentrated to 5% of its volume, to which were added 300 ml of osmotic water containing 30% H2O2, was then evaporated to dryness. This dried mixture was brought to volume with osmotic water then stirred for several minutes. The mixture thus obtained was then subjected to the third microwave irradiation cycle at a power of 600-650W to again evaporate it to dryness. Said addition of osmotic water and subsequent microwave irradiation to dryness were repeated 4 times.
The thus dried mixture to which were added 300 ml of osmotic water containing 20% H2O2, was then evaporated to dryness. Said dried mixture was brought to volume with osmotic water and then stirred for several minutes. The mixture thus obtained was then subjected to the fourth microwave irradiation cycle at a power of 700-850W to again evaporate it to dryness. Said addition of osmotic water and subsequent microwave irradiation to dryness were repeated 4 times.
The thus dried mixture to which were added 300 ml of osmotic water was then dried. This dried mixture was brought to volume with osmotic water and then stirred for several minutes. The mixture thus obtained was then subjected to the fifth microwave irradiation cycle at a power of 1000W to again evaporate it to dryness. Said addition of osmotic water and subsequent microwave irradiation to dryness were repeated 6 times.
Finally, 300 ml of osmotic water were added, the mixture was reduced to half its volume and the final product was separated by sedimentation.
1 g of silver hydroxide was thus obtained.
As illustrated in Figure 9, the final product appeared in the form of nanospheres.
The product was sweet and slightly astringent to taste.
Example 10. Preparation of silver and gold hydroxide according to the present invention
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.
The two solutions were then combined for subjection to the subsequent microwave irradiation treatments.
In this manner, Ag and Au hydroxides were obtained, as illustrated in Figure 10, which were pale yellowish-white in colour, imperceptible to the touch and sweetly astringent in taste.
Example 11. Preparation of silver and copper hydroxide according to the present invention
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.
The two solutions were then combined for subjection to the subsequent microwave irradiation treatments.
A fine powder was obtained which was opaque and pale bluish-white in colour, as illustrated in Figure 11.
Alternatively, in step VII), 2 mg of pure S were added after three repetitions.
The formation of an extremely light and imperceptible powder was noted which was light turquoise-green in colour and bitter astringent and slightly pungent in taste.
Example 12. Preparation of palladium hydroxide according to the present invention
Example 9 was repeated, but in this case a filament of palladium was used.
A fine powder which was light greyish-white in colour was obtained, as illustrated in Figure 12.
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.
A fine powder which was light greyish-white in colour was obtained, as illustrated in Figure 13.
Example 14. Preparation of hydroxy-organometals of Au vehicled by white carbon nanotubes according to the present invention
1.5 g of hydroxy-organometal crystals of Au obtained in Example 1 or Examples 2 and 3 g of white carbon nanotubes obtained in Example 7 or Example 8 were mixed in 300 ml of osmotic water and stirred for several minutes.
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.
It was left to settle as with the nanotube preparation, in the absence of vibrations or tremors for 20-25 days at about 25° C.
Finally there was noted the formation of nanotubes presenting the hydroxy- organometals of Au within them, as illustrated in Figure 14.
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.
Separately, 5% of a 46% urea solution and 2% of H2O2 were added to osmotic water. Said mixture was subjected to microwave irradiation treatment at a power of 700-850W until evaporated to dryness, then brought to volume with osmotic water. This treatment was repeated a further five times until the mixture was dry. At this point, the first mixture was added to the dry urea product and stirred.
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.
Finally there was noted the formation of nanotubes presenting the hydroxy- organometals of Au within them, as illustrated in Figure 15, they being different in appearance and shape from those obtained in the preceding examples.
*****
From the detailed description and the given examples, the advantages ensuing from the process of the present invention are evident. In particular, 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. It was found that 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.
Furthermore, it was possible to optimize the yield by conveying and recovering the products from the gases emitted during the last microwave irradiation step thus increasing overall efficiency of the process without affecting the cost-effectiveness of its implementation.

Claims

1. Process for the preparation of metal hydroxides, hydroxyl organometals and white carbon, comprising the steps of:
I) providing carbon and/or at least a metal;
II) subjecting said carbon and/or at least a metal to electrolysis in an acid solution of 15% to 25% H2O2 for a period of time of 24 to 72 hours;
III) subjecting the mixture deriving from step II) to a first cycle of treatment comprising:
a) after the addition of further acid solution of 20% to 30% H2O2, letting the mixture to settle for about 48 hours, while stirring the same about every 12 hours;
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;
c) bringing to volume by adding osmotic water and stirring;
d) repeating 3 times the steps b)-c) and then repeating the step b);
IV) subjecting the concentrated mixture deriving from step d) to a second cycle of treatment comprising:
e) adding an acid solution of 30% to 40% H2O2 and osmotic water;
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);
V) subjecting the concentrated mixture deriving from step h) to a third cycle of treatment comprising:
i) adding an acid solution of 40% to 50% H2O2 and osmotic water;
I) drying the mixture deriving from step i) by subjecting the same to microwave irradiation at a power of 600-650W;
m) bringing to volume by adding osmotic water and stirring;
n) repeating 3 times the steps l)-m) and then repeating the step I);
Vl) subjecting the concentrated mixture deriving from step n) to a fourth cycle of treatment comprising:
o) adding an acid solution of 20% H2O2 and osmotic water;
p) drying the mixture deriving from step o) by subjecting the same to microwave irradiation at a power of 700-850W;
q) bringing to volume by adding osmotic water and stirring;
r) repeating 3 times the steps p)-q) and then repeating the step p);
VII) subjecting the concentrated mixture deriving from step r) to a fifth cycle of treatment comprising:
s) adding osmotic water;
t) drying the mixture deriving from step s) by subjecting the same to microwave irradiation at a power of 1000-3000W;
u) bringing to volume by adding osmotic water and stirring;
v) repeating 6 times the steps t)-u).
2. Process according to claim 1 , wherein in the step v), after twice repetitions of steps t)-u), a step of gas conveying and collecting is carried out during the remaining four repetitions of steps t)-u) for recovering product taken away by the evaporating water.
3. Process according to claim 1 or 2, wherein said at least a metal is a transition metal.
4. Process according to claim 3, wherein said at least a metal is a metal of the group 11 of the periodic table of elements.
5. Process according to anyone of claims 1-4, wherein in the acid solution of H2O2 of steps II), i) and/or o) ascorbic acid or acetic acid is further added.
6. Process according to anyone of claims 1-5, further comprising a step VIII) of separation by filtration or settlement, subsequent to step v).
7. Process according to anyone of claims 1-6, wherein the step VII) is repeated twice, the first time the microwave power is of 1000-1500W, whereas the second time is of 2500-3000W.
PCT/IB2010/053660 2009-08-13 2010-08-13 Process for preparing metal hydroxides, hydroxyl organometals and white carbon suitable for use in ayurvedic medicine WO2011018773A1 (en)

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