WO2008020092A1 - Improvements introduced into patent p200500389 for 'personalized synthetic diamond of different colours, obtained from (living or dead) human or animal keratin and production method thereof' - Google Patents

Improvements introduced into patent p200500389 for 'personalized synthetic diamond of different colours, obtained from (living or dead) human or animal keratin and production method thereof' Download PDF

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Publication number
WO2008020092A1
WO2008020092A1 PCT/ES2007/000193 ES2007000193W WO2008020092A1 WO 2008020092 A1 WO2008020092 A1 WO 2008020092A1 ES 2007000193 W ES2007000193 W ES 2007000193W WO 2008020092 A1 WO2008020092 A1 WO 2008020092A1
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WIPO (PCT)
Prior art keywords
carbon
sample
carbonization
placenta
umbilical cord
Prior art date
Application number
PCT/ES2007/000193
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Spanish (es)
French (fr)
Inventor
Ramón MARTÍN PARRONDO
Dmitri Bagriantsev
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Instituto De Monocristales, S.L.
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Publication date
Priority claimed from ES200602162A external-priority patent/ES2301379B2/en
Application filed by Instituto De Monocristales, S.L. filed Critical Instituto De Monocristales, S.L.
Publication of WO2008020092A1 publication Critical patent/WO2008020092A1/en

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Classifications

    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/02Elements
    • C30B29/04Diamond
    • AHUMAN NECESSITIES
    • A44HABERDASHERY; JEWELLERY
    • A44CPERSONAL ADORNMENTS, e.g. JEWELLERY; COINS
    • A44C17/00Gems or the like
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J3/00Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
    • B01J3/06Processes using ultra-high pressure, e.g. for the formation of diamonds; Apparatus therefor, e.g. moulds or dies
    • B01J3/062Processes using ultra-high pressure, e.g. for the formation of diamonds; Apparatus therefor, e.g. moulds or dies characterised by the composition of the materials to be processed
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/25Diamond
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/25Diamond
    • C01B32/26Preparation
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2203/00Processes utilising sub- or super atmospheric pressure
    • B01J2203/06High pressure synthesis
    • B01J2203/0605Composition of the material to be processed
    • B01J2203/0625Carbon
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2203/00Processes utilising sub- or super atmospheric pressure
    • B01J2203/06High pressure synthesis
    • B01J2203/065Composition of the material produced
    • B01J2203/0655Diamond
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2203/00Processes utilising sub- or super atmospheric pressure
    • B01J2203/06High pressure synthesis
    • B01J2203/0675Structural or physico-chemical features of the materials processed
    • B01J2203/068Crystal growth

Definitions

  • the present invention relates to improvements introduced in
  • the invention patent P 200500389 improvements consisting in using as raw material for obtaining said diamond, instead of the human or animal keratin, tissues or parts of the umbilical cord and / or the placenta of any person or animal, alive or dead .
  • the object of the invention is to obtain large mono-crystals of cultured diamond (diamond obtained in the laboratory by means of crystal cultivation techniques), of the type Ib, Ha and Nb, from the carbon from the aforementioned tissues.
  • the diamond which is the crystalline cubic form of carbon, was first obtained in the laboratory in the 1950s, from carbon of mineral origin. Since then there have been many advances in the field of synthesis of diamond monocrystals, these advances have led to the industrial use of diamond due to its unique physical and chemical characteristics.
  • the diamond is the hardest substance known to man that, together with its great thermal conductivity and chemical inertia Ie make it suitable for precision machining applications, heatsink heat, surgical instruments, radiation detectors, laser optics, among many other applications.
  • these tissues are what form the umbilical cord and the placenta of humans and mammals in general.
  • Figure 1. Shows a functional diagram of the complete process for obtaining the cultured diamond according to the improvements object of the present invention, using the strong acid method.
  • Figure 2 - Finally shows a representation similar to the previous figure but in which the carbonization process is carried out with the help of a muffle furnace.
  • the carbonization processes used are, as in Ia main patent, the strong acid method, the muffle furnace method or the bunsen burner, torch or similar method.
  • the sample (1), of the umbilical cord and / or placenta is subjected to a maceration (3) in excess of strong and hot acid (boiling normally between 5 and 40 minutes and in general no more than 120 minutes), the H 2 SCM, HCl or another acid mixture of strong acids being able to be used as strong acid Do not oxidize carbon during use.
  • the macerated sample is subjected to a decantation phase (6), to a filtering phase (7) or a spin phase
  • the dry residue thus obtained is between 2.5% and 3.0% by weight of which on average 45.15% by weight is free carbon after treated with chromic mixture.
  • the sample of umbilical cord and / or placenta (T) tissue is also used, either directly or through a previous pressing phase ( 2 1 ), optional, it is introduced in a muffle furnace (3), in a crucible of mullita or any other refractory material with an outlet of gases and vapors. Said exit must prevent or at least hinder
  • This muffle furnace (3) working at a temperature between 500 and 1500 0 C, but optionally the sample can be subjected to a graphitization furnace (4) with much higher temperatures, between 1800 and 3000 ° n V- / .
  • a scraping phase is carried out, either dry (5) or wet (6), in the second case accompanied by a final phase (7) of drying.
  • Sample M3 1 sample of animal placenta (dog species) is prepared. The sample is introduced into 10 x 65 mm mullite capsules. The carbonization temperature is 650 0 C.
  • the tissue or sample of umbilical cord and / or placenta (pressed or not) is introduced into a distillation flask (or distillation tool).
  • the output of gases and vapors can be with or without a vapor trap. This arrangement must prevent or at least hinder the entry of additional oxygen to the existing one when the sample to be carbonized is introduced. In this way the oxidation of carbon is avoided.
  • Oxyacetylene or hydrogen torches can also be used provided that the flask is replaced by refractory tools that allow a higher temperature to be reached.
  • the experience A is performed with human umbilical cord using the round flat bottom flask with an adapter to introduce a water trap while the experience B is performed human umbilical cord with a distillation flask to which a Teflon plug
  • the dried residue is treated with chromic mixture, in order to eliminate the non-reactive organic matter residues.
  • the weight percentage of carbon is obtained after treatment with chromic mixture and subsequent washing.
  • the temperature gradient is adjusted between 10 and 50 ° and all crystals are characterized by being amber yellow and the shape of the octahedral crystal or octahedral cube, the nitrogen concentration is between 50 and 150 parts per million and the metal inclusions are concentrated in the area of the initial seed, the results are shown in Ia Table I.
  • the temperature gradient is adjusted between 10 and 40 °.
  • the color of the diamond crystals is regulated by the thickness H of the membrane and
  • the amount of sensor present in the mixture For blue, 50 ppm of elemental B is included. Crystals up to 4.5 carats by weight and different colorations have been obtained. In all crystals metal inclusions are found in the area of the seed.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Carbon And Carbon Compounds (AREA)

Abstract

The improvements consist in the use, as raw material for obtaining the cultivated diamond, of tissues from the umbilical cord and/or the placenta of humans or animals, be these living or dead, subjecting said tissues to a carbonization process, which, as in the main patent, may be a carbonization by strong acid, a carbonization by Mufla oven or a carbonization by Bunsen burner, blowtorch or the like, the first case yielding the carbon by means of decantation, filtration or centrifugation and in the other cases by means of a mechanical dry scraping process or, optionally, wet scraping followed by drying.

Description

MEJORAS INTRODUCIDAS EN LA PATENTE DE INVENCIÓN P200500389 POR "DIAMANTE SINTÉTICO DE DISTINTOS COLORES PERSONALIZADO A PARTIR DE QUERATINA HUMANA O ANIMAL fVIVO O MUERTO). PROCEDIMIENTO PARA IMPROVEMENTS INTRODUCED IN THE PATENT OF INVENTION P200500389 BY "SYNTHETIC DIAMOND OF DIFFERENT CUSTOM COLORS FROM HUMAN KERATIN OR FIVIVE OR DEAD ANIMAL). PROCEDURE FOR
SU FABRICACIÓN"YOUR MANUFACTURE "
D E S C R I P C I Ó ND E S C R I P C I Ó N
OBJETO DE LA INVENCIÓNOBJECT OF THE INVENTION
La presente invención se refiere a unas mejoras introducidas enThe present invention relates to improvements introduced in
Ia patente de invención P 200500389, mejoras consistentes en utilizar como materia prima para Ia obtención de dicho diamante, en lugar de Ia queratina humana o animal, tejidos o partes del cordón umbilical y/o Ia placenta de cualquier persona o animal, vivo o muerto.The invention patent P 200500389, improvements consisting in using as raw material for obtaining said diamond, instead of the human or animal keratin, tissues or parts of the umbilical cord and / or the placenta of any person or animal, alive or dead .
El objeto de Ia invención es obtener grandes mono-cristales de diamante cultivado (diamante obtenido en laboratorio mediante técnicas de cultivo de cristales), del tipo Ib, Ha y Nb, a partir del carbono proveniente de los tejidos anteriormente citados.The object of the invention is to obtain large mono-crystals of cultured diamond (diamond obtained in the laboratory by means of crystal cultivation techniques), of the type Ib, Ha and Nb, from the carbon from the aforementioned tissues.
ANTECEDENTES DE LA INVENCIÓNBACKGROUND OF THE INVENTION
El diamante, que es Ia forma cúbica cristalina del carbono, se obtuvo por primera vez en el laboratorio en Ia década de los 50, a partir de carbono de origen mineral. Desde entonces ha habido muchos avances en el campo de Ia síntesis de los monocristales de diamante, estos avances han propiciado el uso industrial del diamante debido a sus características singulares tanto físicas como químicas.The diamond, which is the crystalline cubic form of carbon, was first obtained in the laboratory in the 1950s, from carbon of mineral origin. Since then there have been many advances in the field of synthesis of diamond monocrystals, these advances have led to the industrial use of diamond due to its unique physical and chemical characteristics.
Así, el diamante es Ia sustancia más dura conocida por el hombre que, junto con su gran conductividad térmica e inercia química Ie hacen apto para aplicaciones de mecanizado de precisión, disipador de calor, instrumental quirúrgico, detectores de radiación, óptica para láser, entre otras múltiples aplicaciones.Thus, the diamond is the hardest substance known to man that, together with its great thermal conductivity and chemical inertia Ie make it suitable for precision machining applications, heatsink heat, surgical instruments, radiation detectors, laser optics, among many other applications.
Sin embargo, sus aplicaciones en el mundo de Ia joyería y en general del lujo, se han visto restringidas históricamente. Las principales restricciones para su uso como gema han sido en un principio de los primeros diamantes cultivados, que eran de color amarillo y también posteriormente un cierto escepticismo debido a su carácter no natural. Es decir, determinados mercados Ie son de muy difícil penetración, puesto que compite directamente con muchas piedras naturales y cultivadas, incluido el propio diamante natural.However, its applications in the world of jewelry and in general luxury have been historically restricted. The main restrictions for its use as a gem have been in the beginning of the first cultured diamonds, which were yellow in color and also later a certain skepticism due to their unnatural character. That is, certain markets are very difficult to penetrate, since it competes directly with many natural and cultured stones, including the natural diamond itself.
Por otra parte, es incuestionable que el diamante ejerce una fuerte atracción actualmente en los mercados, debido a su exclusividad y alto precio.On the other hand, it is unquestionable that the diamond currently has a strong attraction in the markets, due to its exclusivity and high price.
Todos los seres vivos y el ser humano en particular fijan, a partir del medio en el que viven, carbono en sus tejidos mediante un complejo sistema de reacciones bio-químicas. Este carbono está formando multitud de compuestos orgánicos (hidratos de carbono, grasas, aminoácidos, etc).All living beings and the human being in particular fix, from the environment in which they live, carbon in their tissues through a complex system of biochemical reactions. This carbon is forming a multitude of organic compounds (carbohydrates, fats, amino acids, etc.).
Pero en general, existen muy pocos tejidos a partir de los cuales pueda extraerse dicho carbono ya fijado por el ser vivo, en cantidad suficiente sin que se dañe a este o sin que se incurra en un proceso excesivamente engorroso o complicado para extraer el carbono.But in general, there are very few tissues from which said carbon already fixed by the living being can be extracted, in sufficient quantity without damage to it or without incurring an excessively cumbersome or complicated process to extract the carbon.
Hasta el momento, esto solo se había conseguido a partir de carbono procedente de las cenizas de seres fallecidos, mediante un proceso de purificación del grafito procedente de dichas cenizas. Esta práctica, sin embargo, puede tener un alcance comercial limitado, ya que es necesario esperar el fallecimiento y posterior incineración del ser del que se desea un recuerdo o un presente en forma de cristal y además tiene cierta reprobación moral por parte de determinados colectivos, por ejemplo, aquellos colectivos que censuran Ia comercialización posterior de los productos de Ia incineración.So far, this had only been achieved from carbon from the ashes of deceased beings, through a process of purification of graphite from these ashes. This practice, however, may have a limited commercial scope, since it is necessary to wait for the death and subsequent incineration of the being of which a memory or a present in the form of a crystal is desired and also has some moral reprobation on the part of certain groups, for example, those groups that censor subsequent commercialization of the products of the incineration.
El propio solicitante es titular de Ia patente de invención española P 200500389, en Ia que se describe un diamante sintético de distintos colores, personalizado a partir de queratina humana o animal, tanto en seres vivos como muertos, consistente en una carbonización de Ia queratina, como por ejemplo Ia existente en el pelo y en las uñas, y sometiendo posteriormente Ia queratina carbonizada a un proceso de alta presión y temperatura.The applicant himself is the holder of the Spanish invention patent P 200500389, in which a synthetic diamond of different colors is described, customized from human or animal keratin, both in living and dead beings, consisting of a carbonization of the keratin, as for example the one existing in the hair and nails, and subsequently subjecting the carbonized keratin to a process of high pressure and temperature.
DESCRIPCIÓN DE LA INVENCIÓNDESCRIPTION OF THE INVENTION
Sorprendentemente se ha llegado a Ia conclusión de que es posible extraer carbono de tejidos que han formado parte de un proceso especialmente importante de Ia vida de los seres vivos, concretamente Ia gestación.Surprisingly, it has been concluded that it is possible to extract carbon from tissues that have been part of an especially important process in the life of living beings, specifically gestation.
Específicamente estos tejidos son los que forman el cordón umbilical y Ia placenta del ser humano y de los mamíferos en general.Specifically, these tissues are what form the umbilical cord and the placenta of humans and mammals in general.
Puesto que tales tejidos contienen cantidades apreciables de proteínas, grasas y otros compuestos biológicos con base del carbono, esto hace que dichos tejidos constituyan una fuente de carbono fácil y asequible.Since such tissues contain appreciable amounts of proteins, fats and other biological compounds based on carbon, this makes these tissues an easy and affordable source of carbon.
Dado que es costumbre de muchos padres conservar los restos deshidratados del cordón umbilical que se desprende del bebé a los pocos días de su nacimiento, indudablemente resulta mucho más atractivo conservar dichos restos transformados en un diamante cultivado. Otros los mas, tiran en cambio dichos restos por ser poco manejables en el entorno doméstico y poco prácticos a pesar de que poseer una fuerte carga emocional para tales padres, por Io que constituyen un recuerdo escasamente atractivo, que sin embargo sufre un giro total cuando se convierte en un diamante cultivado. Por lo demás Ia extracción del carbono de estos tejidos se lleva a cabo por el mismo proceso de Ia patente P 200500389, es decir mediante carbonización de los mismos y sometimiento posterior a alta presión y temperatura para obtener el pretendido diamante cultivado que, como anteriormente se ha dicho, poseerá un alto valor sentimental para las personas de las que las que proceden dichos tejidos, sus familiares y entorno.Since it is the custom of many parents to keep the dehydrated remains of the umbilical cord that emerges from the baby within a few days of birth, it is undoubtedly much more attractive to keep these remains transformed into a cultured diamond. Others, however, throw these remains because they are not manageable in the domestic environment and impractical despite having a strong emotional burden for such parents, so they constitute a scarcely attractive memory, which nevertheless undergoes a total turn when It becomes a cultured diamond. Moreover, the extraction of carbon from these tissues is carried out by the same process of patent P 200500389, that is to say by carbonization of the same and subsequent subjugation at high pressure and temperature to obtain the intended cultured diamond which, as previously He said, it will have a high sentimental value for the people from whom these tissues come, their relatives and their environment.
No obstante existe Ia posibilidad de extraer el carbono de otras partes del cuerpo humano o animal, que Io contengan.However, there is the possibility of extracting carbon from other parts of the human or animal body, which contain it.
DESCRIPCIÓN DE LOS DIBUJOSDESCRIPTION OF THE DRAWINGS
Para complementar Ia descripción que se está realizando y con objeto de ayudar a una mejor comprensión de las características del invento, de acuerdo con un ejemplo preferente de realización práctica del mismo, se acompaña como parte integrante de dicha descripción, un juego de dibujos en donde con carácter ilustrativo y no limitativo, se ha representado lo siguiente:To complement the description that is being made and in order to help a better understanding of the characteristics of the invention, according to a preferred example of practical realization thereof, a set of drawings is attached as an integral part of said description. In an illustrative and non-limiting manner, the following has been represented:
La figura 1.- Muestra un diagrama funcional del proceso completo para la obtención del diamante cultivado de acuerdo con las mejoras objeto de Ia presente invención, utilizando el método por ácido fuerte.Figure 1.- Shows a functional diagram of the complete process for obtaining the cultured diamond according to the improvements object of the present invention, using the strong acid method.
La figura 2 - Muestra, finalmente, una representación similar a Ia figura anterior pero en Ia que el proceso de carbonización se lleva a cabo con el concurso de un horno de mufla.Figure 2 - Finally shows a representation similar to the previous figure but in which the carbonization process is carried out with the help of a muffle furnace.
REALIZACIÓN PREFERENTE DE LA INVENCIÓNPREFERRED EMBODIMENT OF THE INVENTION
Los procesos de carbonización que se utilizan son, como en Ia patente principal, el método por ácido fuerte, el método por horno de mufla o el método por mechero bunsen, soplete o similar.The carbonization processes used are, as in Ia main patent, the strong acid method, the muffle furnace method or the bunsen burner, torch or similar method.
En el método por ácido fuerte, el mostrado en Ia figura 1 , Ia muestra (1 ), del cordón umbilical y/o placenta, bien directamente o bien a través de una fase previa de prensado (2), opcional, se somete a una maceración (3) en exceso de ácido fuerte y caliente (a ebullición normalmente entre 5 y 40 minutos y en general no más de 120 minutos), pudiendo utilizarse como ácido fuerte el H2SCM, HCl o bien otro ácido mezcla de ácidos fuertes que no oxide el carbono durante su empleo.In the strong acid method, the one shown in Figure 1, the sample (1), of the umbilical cord and / or placenta, either directly or through a previous phase of pressing (2), optional, is subjected to a maceration (3) in excess of strong and hot acid (boiling normally between 5 and 40 minutes and in general no more than 120 minutes), the H 2 SCM, HCl or another acid mixture of strong acids being able to be used as strong acid Do not oxidize carbon during use.
La muestra macerada, bien de forma concentrada (4) o bien mediante una fase (5) de neutralización del ácido o dilución del mismo hasta conseguir una solución ligeramente acida, se somete a una fase de decantación (6), a una fase de filtrado (7) o a una fase de centrifugadoThe macerated sample, either in a concentrated form (4) or by means of a phase (5) of neutralization of the acid or dilution thereof until a slightly acid solution is obtained, is subjected to a decantation phase (6), to a filtering phase (7) or a spin phase
(8), tal como muestra también el. diagrama de Ia figura 1 , para proceder seguidamente a una fase de lavado (9) tras Ia que opcionalmente puede repetirse el centrifugado (8) y en cualquier caso el proceso culmina con una fase de secado (10) del producto.(8), as the . diagram of Figure 1, to then proceed to a washing phase (9) after which the centrifugation (8) can optionally be repeated and in any case the process culminates with a drying phase (10) of the product.
Los resultados obtenidos son:The results obtained are:
Disolución 100% de H2SO4 (96%):100% solution of H 2 SO 4 (96%):
Se toman 50 mL de H2SO4 (96%) .50 mL of H 2 SO 4 (96%) are taken.
Se prepara 1 muestra de cordón umbilical humano (alrededor de 10,0 g en total) y se añaden a Ia disolución en un vaso de precipitado de 10O mL1 sample of human umbilical cord (about 10.0 g in total) is prepared and added to the solution in a 10O mL beaker
Se calienta durante 30 minutos en Ia placa eléctrica de 500 a 1000 W, al final se comprueba, introduciendo una varilla de vidrio dentro del vaso, que no queden restos de muestra sin disolver.It is heated for 30 minutes in the electric plate of 500 to 1000 W, at the end it is checked, by introducing a glass rod into the vessel, that there are no remains of undissolved sample.
El residuo seco así obtenido se encuentra entre el 2,5% y el 3,0% en peso del cual en promedio el 45,15% en peso es carbono libre después de tratado con mezcla crómica.The dry residue thus obtained is between 2.5% and 3.0% by weight of which on average 45.15% by weight is free carbon after treated with chromic mixture.
En el caso de utilizar el método por horno de mufla y tal como muestra Ia figura 2, se parte igualmente de Ia muestra de tejido del cordón umbilical y/o placenta (T), que bien directamente o a través de una fase de prensado previo (21), opcional, se introduce en un horno de mufla (3), en un crisol de mullita o cualquier otro material refractario con salida de gases y vapores. Dicha salida debe impedir o al menos dificultarIn the case of using the muffle furnace method and as shown in Figure 2, the sample of umbilical cord and / or placenta (T) tissue is also used, either directly or through a previous pressing phase ( 2 1 ), optional, it is introduced in a muffle furnace (3), in a crucible of mullita or any other refractory material with an outlet of gases and vapors. Said exit must prevent or at least hinder
Ia entrada de oxígeno adicional al ya existente cuando se introduzca Ia muestra a carbonizar, de manera que se evite Ia oxidación del carbón.The entry of additional oxygen to the existing one when the sample to be carbonized is introduced, so that the oxidation of the carbon is avoided.
Este horno de mufla (3) trabaja a una temperatura comprendida entre 500 y 1500 0C, pero opcionalmente Ia muestra puede ser sometida a un horno de grafitización (4) con temperaturas mucho más altas, comprendidas entre 1800 y 3000 °n V-/ .This muffle furnace (3) working at a temperature between 500 and 1500 0 C, but optionally the sample can be subjected to a graphitization furnace (4) with much higher temperatures, between 1800 and 3000 ° n V- / .
Bien a su salida del horno de mufla (3) o del horno de grafitización (4), se lleva a cabo una fase de raspado, bien en seco (5) o bien en húmedo (6), en el segundo caso acompañado de una fase final (7) de secado.Either at the exit of the muffle furnace (3) or the graffiti furnace (4), a scraping phase is carried out, either dry (5) or wet (6), in the second case accompanied by a final phase (7) of drying.
EJEMPLO:EXAMPLE:
A continuación se indica una serie de datos del experimento realizado para conseguir Ia carbonización de Ia muestra objetivo por calentamiento.A series of data of the experiment performed to achieve the carbonization of the target sample by heating is indicated below.
Primera experiencia , Muestra MI : en un vaso de precipitado deFirst experience, Sample MI: in a beaker of
100 mi introducimos Ia muestra de cordón umbilical humano y sin tapar se realiza Ia carbonización hasta 500 0C. Los datos de esta primera experiencia son:100 ml we introduce the human umbilical cord sample and uncovered the carbonization up to 500 0 C. The data of this first experience are:
- Peso inicial de muestra, Ml : 15,652 g - Peso final de muestra, Ml : 0,508 g- Initial sample weight, Ml: 15,652 g - Final sample weight, Ml: 0.508 g
- Pérdida: 15,144 g.- Loss: 15,144 g.
- % Pérdida: 96,75%-% Loss: 96.75%
- % Residuo Seco: 3,25 %.-% Dry Waste: 3.25%.
Después de realizar el tratamiento con mezcla crómica, se ha obtenido el siguiente porcentaje de C libre: 40,99.After performing the chromic mixture treatment, the following percentage of free C has been obtained: 40.99.
Segunda experiencia. Muestra M2: en este caso se coloca un vidrio de reloj de diámetro tapando el vaso de precipitado, se obtienen los siguientes resultados, Ia temperatura es también 5000C:Second Experience Sample M2: in this case a diameter watch glass is placed covering the beaker, the following results are obtained, the temperature is also 500 0 C:
- Peso inicial de muestra, M2: 10,968 g- Initial sample weight, M2: 10,968 g
- Peso final de muestra, M2: 0,373 g - Pérdida: 10,595 g- Final sample weight, M2: 0.373 g - Loss: 10.595 g
- % Pérdida: 96,59%-% Loss: 96.59%
% Residuo Seco: 3,4%% Dry Waste: 3.4%
Después de realizar el tratamiento con mezcla crómica, se ha obtenido el siguiente porcentaje de C libre: 40,68After performing the chromic mixture treatment, the following percentage of free C was obtained: 40.68
Tercera experiencia. Muestra M3: se preparan 1 muestra de placenta animal (especie perro). La muestra se introduce en cápsulas de mullita de 10 X 65 mm. La temperatura de carbonización es 6500C .Third experience Sample M3: 1 sample of animal placenta (dog species) is prepared. The sample is introduced into 10 x 65 mm mullite capsules. The carbonization temperature is 650 0 C.
El resultado es:The result is:
- Peso inicial de muestra, M3: 1 1 ,033 g- Initial sample weight, M3: 1 1, 033 g
- Peso final de muestra, M3: 0,331 g- Final sample weight, M3: 0.331 g
- Pérdida: ! 0,702 g - % Pérdida: 97,00 %- Lost: ! 0.702 g -% Loss: 97.00%
- % Residuo Seco: 3,00%-% Dry Waste: 3.00%
Después de realizar el tratamiento con mezcla crómica, se ha obtenido el siguiente porcentaje de C libre: 44,86 Cuadro resumenAfter performing the treatment with chromic mixture, the following percentage of free C was obtained: 44.86 Summary table
Figure imgf000009_0001
Figure imgf000009_0001
Finalmente en el método de mechero bunsen, soplete o similar, se establecen las siguientes fases operativas:Finally, in the bunsen burner, torch or similar method, the following operational phases are established:
Se introduce el tejido o muestra de cordón umbilical y/o placenta (prensado o no) en un matraz de destilación (o útil de destilación). La salida de gases y vapores pueden ser con o sin trampa de vapores. Esta disposición debe impedir o al menos dificultar Ia entrada de oxigeno adicional al ya existente cuando se introduce Ia muestra a carbonizar. De esta forma se evita Ia oxidación del carbono.The tissue or sample of umbilical cord and / or placenta (pressed or not) is introduced into a distillation flask (or distillation tool). The output of gases and vapors can be with or without a vapor trap. This arrangement must prevent or at least hinder the entry of additional oxygen to the existing one when the sample to be carbonized is introduced. In this way the oxidation of carbon is avoided.
Se calienta mediante mechero bunsen o similar con llama preferentemente reductora hasta conseguir Ia carbonización total de Ia muestra. También pueden emplearse sopletes de oxiacetileno o de hidrogeno a condición de sustituir el matraz por útiles refractarios que permiten alcanzar mayor temperatura.It is heated by means of a bunsen burner or similar with a preferably reducing flame until the total carbonization of the sample is achieved. Oxyacetylene or hydrogen torches can also be used provided that the flask is replaced by refractory tools that allow a higher temperature to be reached.
- Se recupera el carbono, mediante:- Carbon is recovered, by:
Proceso mecánico de raspado en secoMechanical dry scraping process
Proceso de raspado en húmedo seguido de secado. Ejemplo: Lα carbonización de muestra objetivo con bunsen después de los experimentos llevados a cabo, han dado los siguientes resultados.Wet scraping process followed by drying. Example: Lα carbonization of target sample with bunsen after the experiments carried out, have given the following results.
Se realizan dos experiencias, Ia experiencia A se realiza con cordón umbilical humano utilizando el matraz redondo de fondo plano con un adaptador para introducir una trampa con agua mientras que Ia experiencia B se realiza cordón umbilical humano con un matraz de destilación al que se adapta un tapón de teflón. El residuo seco se trata con mezcla crómica, con objeto de eliminar los restos de materia orgánica no reaccionantes. El porcentaje en peso del carbono se obtiene después del tratamiento con mezcla crómica y su lavado posterior.Two experiences are carried out, the experience A is performed with human umbilical cord using the round flat bottom flask with an adapter to introduce a water trap while the experience B is performed human umbilical cord with a distillation flask to which a Teflon plug The dried residue is treated with chromic mixture, in order to eliminate the non-reactive organic matter residues. The weight percentage of carbon is obtained after treatment with chromic mixture and subsequent washing.
- Cuadro resumen:- Summary table:
Figure imgf000010_0001
Figure imgf000010_0001
A continuación se preparan diversas cápsulas de reacción de alta presión y alta temperatura cuya fuente de carbono es el carbono obtenido por estos procedimientos y se someten dichas cápsulas al proceso de alta presión y alta temperatura, reivindicado en las patentes n° PCT/ES2005/000463 y n° PCT/ES2005/000462 y los resultados obtenidos son los siguientes donde se designa por "Biocarbono" al carbono procedente de tejido o partes de origen humano o animal. En este caso de cordón umbilical humano. Designamos como "Biodiamante" al diamante cultivado obtenido a partir de Biocarbono"Various high pressure and high temperature reaction capsules are then prepared whose carbon source is the carbon obtained by these processes and said capsules are subjected to the high pressure and high temperature process, claimed in patents No. PCT / ES2005 / 000463 and PCT / ES2005 / 000462 and the results obtained are the following where "Biocarbon" refers to carbon from tissue or parts of human or animal origin. In this case of human umbilical cord. We designate as "Biodiamante" the cultured diamond obtained from Biocarbon "
Para el crecimiento de cristales amarillos de biodiamante de color ámbar tipo I b se emplean los parámetros siguientes:For the growth of yellow crystals of amber biodiamante type I b the following parameters are used:
Se ajusta el gradiente de temperatura entre 10 y 50 ° y todos los cristales se caracterizan por ser de color amarillo ámbar y forma del cristal octaédrica o cubo octaédrico, Ia concentración de nitrógeno está entre 50 y 150 partes por millón y las inclusiones metálicas se concentran en Ia zona de Ia semilla inicial, los resultados se exponen en Ia Tabla I.The temperature gradient is adjusted between 10 and 50 ° and all crystals are characterized by being amber yellow and the shape of the octahedral crystal or octahedral cube, the nitrogen concentration is between 50 and 150 parts per million and the metal inclusions are concentrated in the area of the initial seed, the results are shown in Ia Table I.
TABLATABLE
Figure imgf000011_0001
Figure imgf000011_0001
*4 semillas por cápsula (crecimiento simultáneo de 4 cristales) **lnternational Gemological lnstitute (IGI)* 4 seeds per capsule (simultaneous growth of 4 crystals) ** International Gemological Institute (IGI)
Con los mismos parámetros empleados para los biodiamantes de color amarillo ámbar se han cultivado cristales de color amarillo canary y de color verde. Los resultados se muestran en Ia Tabla II. 007/000193With the same parameters used for amber yellow biodiamonds, canary yellow and green crystals have been grown. The results are shown in Table II. 007/000193
11eleven
Tabla IITable II
Figure imgf000012_0001
Figure imgf000012_0001
*lnternational Gemological lnstitute (IGI)* International Gemological Institute (IGI)
Para el crecimiento de cristales ligeramente coloreados o blancos tipo Il a y azules tipo Hb se emplean los parámetros siguientes:For the growth of slightly colored or white crystals type Il a and blue type Hb the following parameters are used:
Se ajusta el gradiente de temperatura entre 10 y 40°. El color de los cristales del diamante se regula mediante el grosor H de Ia membrana yThe temperature gradient is adjusted between 10 and 40 °. The color of the diamond crystals is regulated by the thickness H of the membrane and
Ia cantidad de captador presente en Ia mezcla. Para el azul se incluye 50 ppm de B elemental. Se han obtenido cristales hasta 4,5 quilates en peso y diferentes coloraciones. En todos los cristales se encuentran inclusiones metálicas en Ia zona de Ia semilla.The amount of sensor present in the mixture. For blue, 50 ppm of elemental B is included. Crystals up to 4.5 carats by weight and different colorations have been obtained. In all crystals metal inclusions are found in the area of the seed.
Tales inclusiones no impiden su aplicación comercial, los resultados se exponen en Ia Tabla III Tabla IIISuch inclusions do not prevent their commercial application, the results are shown in Table III Table III
Figure imgf000013_0001
Figure imgf000013_0001
*lntemational Gemological lnstitute (IGI) * lntemational Gemological lnstitute (IGI)

Claims

R E I V I N D I C A C I O N E S R E I V I N D I C A C I O N E S
Ia.- Mejoras introducidas en Ia patente de invención P200500389 por "Diamante sintético de distintos colores personalizado a partir de queratina humana o animal (vivo o muerto). Procedimiento para su fabricación", caracterizadas porque consisten en utilizar, como materia prima para Ia obtención del carbono a transformar en diamante, cordón umbilical y/o placenta humana o animal.I to .- Improvements to patent of invention P200500389 Ia by "synthetic diamond custom colors different from human or animal keratin (dead or alive). Process for manufacturing", wherein consist in using, as raw material for Ia Obtaining the carbon to be transformed into diamond, umbilical cord and / or human or animal placenta.
2a.- Mejoras, según reivindicación Ia, caracterizadas porque Ia carbonización del cordón umbilical y/o Ia placenta se lleva a cabo por métodos de carbonización de ácido fuerte, por horno de mufla o mediante mechero bunsen, soplete o similar.2 .- Improvements according to claim I, wherein the carbonization cord and / or placenta Ia is carried out by methods carbonization strong acid, muffle furnace or by bunsen burner blowtorch or similar.
3a.- Mejoras, según reivindicación 2a, caracterizadas porque con el método de ácido fuerte se establecen las siguientes fases operativas:3 .- Improvements according to claim 2, characterized in that the strong acid method the following operational steps are established:
- Se macera el tejido o muestra del cordón umbilical y/o placenta (prensado o no), en exceso de ácido fuerte y caliente (a ebullición entre 5 y 40 minutos.- The tissue or sample of the umbilical cord and / or placenta (pressed or not) is macerated, in excess of strong and hot acid (boiling for 5 to 40 minutes.
Se neutraliza el ácido o se diluye hasta conseguir una solución ligeramente acida, o bien sin neutralizar se separa el carbono de Ia disolución mediante decantación, filtrado o centrifugado.The acid is neutralized or diluted until a slightly acidic solution is obtained, or without neutralizing the carbon is separated from the solution by decantation, filtration or centrifugation.
- Lavado- Washed
Secado.Drying
4a.- Mejoras, según reivindicación 2a, caracterizadas por que en el método de horno de mufla se establecen las siguientes fases operativas:4 .- Improvements according to claim 2, characterized by the following operational steps are established in the muffle furnace method:
Se introduce el tejido o muestra con cordón umbilical y/o placentaThe tissue or sample with umbilical cord and / or placenta is introduced
(prensado o no) en un crisol de mullita o cualquier otro material refractario, con salida de gases. Dicha salida debe impedir o al menos dificultar Ia entrada de oxigeno adicional al ya existente cuando se introduzca Ia muestra a carbonizar. De esta forma se evita Ia oxidación del carbono.(pressed or not) in a mullite crucible or any other refractory material, with gas outlet. Such exit must prevent or at less hinder the entry of additional oxygen to the existing one when the sample to be carbonized is introduced. In this way the oxidation of carbon is avoided.
- Se aumenta Ia temperatura hasta conseguir Ia carbonización de Ia muestra (entre 500 0C y 1500 0C). En hornos con atmósfera reductora y crisol de grafito (u otro) puede continuarse el calentamiento obteniéndose Ia conversión del carbono a Ia forma de grafito ( entre 18000C y 30000C).- The temperature is increased until the carbonization of the sample is achieved (between 500 0 C and 1500 0 C). In furnaces with reducing atmosphere and graphite crucible (or other) heating can be continued, obtaining the conversion of carbon to the graphite form (between 1800 0 C and 3000 0 C).
Se recupera el carbono mediante proceso mecánico de raspado en seco o raspado en húmedo, seguido de una fase de secado.Carbon is recovered by mechanical dry scraping or wet scraping process, followed by a drying phase.
5a.- Mejoras , según reivindicación 2a, caracterizadas porque en el método de mechero bunsen o similar se establecen las siguientes bases operativas:5 .- Improvements according to claim 2, wherein the following operational bases are set in the method of Bunsen burner or similar:
Se introduce el tejido o muestra con cordón umbilical y/o placenta (prensado o no) en un matraz de destilación (o útil de destilación). La salida de gases o vapores puede ser con o sin trampa de vapores. Esta disposición debe impedir o al menos dificultar Ia entrada de oxigeno adicional al ya existente cuando se introduce Ia muestra a carbonizar. De esta forma se evita Ia oxidación del carbono.The tissue or sample with umbilical cord and / or placenta (pressed or not) is introduced into a distillation flask (or distillation tool). The output of gases or vapors can be with or without a vapor trap. This arrangement must prevent or at least hinder the entry of additional oxygen to the existing one when the sample to be carbonized is introduced. In this way the oxidation of carbon is avoided.
Se calienta mediante mechero bunsen o similar con llama preferentemente reductora hasta conseguir Ia carbonización total de Ia muestra. También pueden emplearse sopletes de oxiacetileno o de hidrogeno a condición de sustituir el matraz por útiles refractarios que permiten alcanzar mayor temperatura.It is heated by means of a bunsen burner or similar with a preferably reducing flame until the total carbonization of the sample is achieved. Oxyacetylene or hydrogen torches can also be used provided that the flask is replaced by refractory tools that allow a higher temperature to be reached.
Se recupera el carbono mediante proceso mecánico de raspado en seco o raspado en húmedo, seguido de una fase de secado.Carbon is recovered by mechanical dry scraping or wet scraping process, followed by a drying phase.
HOJA DE SUSTITUCIÓN (REGLA 26) SUBSTITUTE SHEET (RULE 26)
PCT/ES2007/000193 2006-08-08 2007-04-04 Improvements introduced into patent p200500389 for 'personalized synthetic diamond of different colours, obtained from (living or dead) human or animal keratin and production method thereof' WO2008020092A1 (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2004076058A1 (en) * 2003-02-25 2004-09-10 1061803 Alberta Ltd. Method of encapsulating material from humans or animals in a natural gemstone and its product
WO2005110917A1 (en) * 2004-04-14 2005-11-24 Hatleberg John N Synthetic diamonds prepared from organic materials

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2004076058A1 (en) * 2003-02-25 2004-09-10 1061803 Alberta Ltd. Method of encapsulating material from humans or animals in a natural gemstone and its product
WO2005110917A1 (en) * 2004-04-14 2005-11-24 Hatleberg John N Synthetic diamonds prepared from organic materials

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