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INVENTION
Patent of the Russian Federation RU2159214
SYNTHETIC JEWELRY-FACING MALAKHIT AND METHOD OF ITS RECEIVING
Applicant's Name: Closed Joint Stock Company "Jenavi"
Name of the inventor: Protopopov EH .; Protopopova VS; Sokolov VV; Petrov TG; Nardov A.V.
The name of the patentee: Closed Joint Stock Company "Jenavi"
Address for correspondence: 197136, St. Petersburg, and / I 88, Novoseltseva OV
Starting date of the patent: 2000.02.09
Use: synthetic stones for the jewelry industry and arts and crafts. The basic carbonic copper is dissolved in an aqueous solution of ammonium carbonate at an excess molar content of ammonia of 1.5-8 times with respect to the mole content of carbon dioxide. The resulting solution is evaporated at 40-95 ° C at a variable rate. A polycrystalline aggregate of synthetic malachite is formed. Synthetic malachite contains basic carbonated copper and impurities with the following ratio of components, weight. % Of Cu 2 [CO 3] (OH 2) - 99,99-99,5; Impurities - 0,01-0,50. In this synthetic malachite impurity contains Fe 2 O 3 and Na 2 O, synthetic malachite density of 3.9-4.1 g / cm3, a Mohs hardness - 4.0 microhardness - 216-390 kg / mm 2, The maximum spectrum of reflection of the surface of synthetic malachite is 490-525 nm, the wear resistance of synthetic malachite is 105-150% in comparison with the wear resistance of natural malachite, and the polishing of synthetic malachite with respect to the polishability of natural malachite is 105-150%. Synthetic malachite contains alternating light and dark green layers, and its surface in reflected light exhibits a pluss moiré effect.
DESCRIPTION OF THE INVENTION
The group of inventions refers to the manufacture of synthetic jewelry and ornamental stones for the jewelry industry and decorative and applied art.
Inventions can be used in the manufacture and restoration of interiors of apartments and buildings, jewelry, costume jewelery, souvenirs, objects of decorative and applied art.
Malachite is a mineral carbonates class of chemical composition of Cu 2 [CO 3] (OH) 2 or CuCO 3 · Cu (OH) 2 containing 71.9% CuO (57.4% Cu), 19.9% CO 2, 8,2% H 2 O and up to 10% impurities in the form of CaO, Fe 2 O 3, SiO 2. Crystallizes in a monoclinic system, crystals are rare and have a needle or prismatic appearance. Typically hidden and fine crystalline kidney-like filaments, stalactite-like aggregates, rhythmically banded with a radial-fibrous structure.
The color of natural dense malachite is bright green, bluish-green to dark, sometimes brownish-green. Changing the color of the different zones and layers of malachite creates a weird pattern on the slices and polished planes. The brilliance of the aggregates is silky (plicate malachite), velvety, dull, in crystals - diamond, transforming into glass. The Mohs mineralogical hardness is 3.5 - 4.0; density of 3900-4100 kg / m 3.
In nature, malachite is found in the near-surface oxidation zone of sulfide copper ores. Large accumulations of dense malachite are very rare and are formed by replacement of limestone copper sulphate solution in the oxidation zone of large deposits of copper, which accounts for the presence of malachite natural impurities in the form of CaO, Fe 2 O 3, SiO 2. Usually found in small amounts in the dispersed state in the form of raids, primings, small accumulations, earthy masses in a mixture with other hypergenic minerals. Only dense clusters of malachite weighing up to 50 tons (Mednorudnyansk, Nizhny Tagil, Gumeshevsky mines in the Urals) are occasionally encountered [TSB, p. 276].
Dense, zoned concentric malachite in the form of large enough masses is of great value as a beautiful ornamental stone used for jewelry and decorative art products (inserts, beads, table tops, vases, facing of columns, etc.).
There are large deposits of malachite in Zaire, in the south of Australia, in Kazakhstan and in the USA. The deposits of malachite in the Urals (Mednorudnya and Gumeshevsky mines) are almost completely developed now.
In this regard, there is an urgent problem of developing technologies for obtaining synthetic jewelry and ornamental malachite, similar in its performance to natural malachite.
Known methods of producing synthetic gemstones materials, consisting of the crystallization of salt melts or high-temperature aqueous solutions [N. I. Kornilov, Yu. P. Solodova. Jewelry stones. - Moscow: Nedra, 1987, p. 259-276]. However, for these methods unsuitable malachite as malachite decomposes at 100-110 o C without melting and the water practically insoluble.
Methods are known for the production of single crystals of malachite under conditions of low-temperature hydrothermal synthesis [Ruszala P., Kostiner E. The hydrothermal synthesis of single crystals of ozurite and malachite. J. Cryst Growth. 1974 / 26. N 1, s. 155-156].
A method for manufacturing a synthetic malachite as individual particles and their co-precipitation with a small amount of uniformly dispersed bismuth used as nuclei for the subsequent growth at elevated temperatures and subsequent conversion into a copper acetylene complex used as a etilinirovaniya catalyst [US patent N 4107082, B 01 J 27/20, 15/08/78].
Agglomerates of malachite crystals are known and their preparation, containing 1-7% (BiO) 2 CuCO 3 and 0,5-3,5% SiO 2, having a mean size of 15 microns, used as catalysts in chemical processes [US patent N 4536491, The 01 J 21/20, C 04 C 33/04, 20.08.85].
There is a method of production of malachite or malahitopodobnyh products, including grinding natural malachite to particles of 10-100 microns, the powder distribution in a transparent varnish, painting them are manufactured items, drying and coating the surface patterns or masks that reproduce the texture of natural malachite [Patent EP N 0856363, B 05 D 5/05, B 44 F 9/04, 1998-08-05].
By these methods it is not possible to obtain malachite, suitable for use as a jewelry and ornamental material.
The closest in technical essence and achieved using technical result (the prototype) a process for producing polycrystalline malachite comprising dissolving carbonate of copper in an aqueous solution of ammonium carbonate containing an equal molar proportion of ammonium and carbonate ion, followed by evaporation of the solution under heating, whereby get loose sediment polycrystalline malachite [Chirvinsky PN artificial production of minerals in the XIX century. - Kiev. University, 1903-1906].
The disadvantage of this method of the prototype, but also all other known methods is the inability to obtain a dense material, similar in its characteristics to natural malachite and suitable for use in jewelry and ornamental purposes.
In particular, the disadvantages of the prototype method are a weak fusion between individual crystals and spherulites in the resulting polycrystalline malachite deposit, its high porosity and low mechanical strength (after drying the sediment is easily rubbed with fingers), which makes it unsuitable for jewelry-ornamental purposes. Another drawback of the known method is the uniformity of the resulting precipitate having a pale green color, unlike the dense polycrystalline aggregate of natural malachite, whose jewelry-ornamental varieties are characterized by the presence of alternating bright light green and dark green strips or layers.
The main technical problem (the inventive task that has not been solved to date), which inhibits the expansion of the use of malachite in jewelry and decorative and decorative purposes, is that the methods known up to now do not allow the production of synthetic dense polycrystalline malachite similar in physicomechanical and Consumer properties of natural jewelry and ornamental malachite.
The aim of the group of inventions (the required technical result achieved when using the invention) is to provide opportunities for synthetic dense polycrystalline jewelry and semi-precious malachite, which is characterized by alternating light-green and dark green stripes with a contrasting color transitions between the layers, and do not differ in their physical and mechanical and jewelry - artistic properties of the best varieties of jewelry and ornamental varieties of natural malachite.
The goal and the required technical result is achieved in that the synthetic gemstones, malachite, which is a polycrystalline aggregate containing Cu 2 basic carbonic copper (CO 3] (OH) 2 and impurities, according to the invention synthetic malachite contains basic carbonic copper and impurities at the next Ratio of components, weight%:
Cu 2 [CO 3] (OH) 2 - 99,99-99,5
Impurities - 0,01 - 0,50
In this synthetic malachite as impurities comprises Fe 2 O 3 and Na 2 O, synthetic malachite density of 3.9 - 4.1 g / cm3, a Mohs hardness of 4.0, the microhardness of 216 - 390 kg / mm 2, the maximum Spectrum of the reflection of synthetic malachite 490-525 nm, the wear resistance of synthetic malachite is 105-150% in comparison with the wear resistance of natural malachite, and the polishability of synthetic malachite in relation to the polishability of natural malachite is 105-150%.
In this case, synthetic malachite contains alternating light green and dark green layers, and its surface in reflected light exhibits a "pluss" (moire) effect.
A characteristic feature of synthetic malachite is its production by dissolving the basic carbonic copper in an aqueous solution of ammonium carbonate containing an excess mole content of ammonia with respect to the mole content of carbon dioxide and then evaporating the solution upon heating to form a synthetic polycrystalline aggregate, whereupon the intercrystalline space of synthetic malachite contains a residual Ammonium ion.
The aim and the required technical result are achieved by the fact that by the method for producing synthetic jewelry and ornamental malachite comprising dissolving the basic carbonic copper in an aqueous solution of ammonium carbonate and then evaporating the resulting solution to form a polycrystalline aggregate of synthetic malachite, according to the invention, the dissolution of basic copper carbonate In an aqueous solution of ammonium carbonate is carried out at an excess molar content of ammonia of 1.5-8 times with respect to the mole content of carbon dioxide.
In this solution-evaporation basic carbonate of copper in an aqueous solution of ammonium carbonate with an excess ammonia is carried out at a temperature of 40 - 95 o C, preferably at 60 - 80 o C, and evaporating the solution basic carbonate of copper in an aqueous solution of ammonium carbonate with an excess ammonia is carried out with a variable Speed with the possibility of obtaining synthetic malachite with alternating light green and dark green layers, and in order to provide the possibility of obtaining contrasting color transitions between the layers of synthetic malachite upon transition to the growth of the next layer, the rate of evaporation of the solution of the basic carbonic copper in an aqueous solution of ammonium carbonate is changed in excess Ammonia by at least 1.2 times compared with the rate of evaporation during crystallization of the previous layer of synthetic malachite.
Confirmation of the effectiveness of inventions, the possibility of industrial implementation of inventions and the possibility of practical achievement of the required technical result are confirmed by the following examples of implementation of inventions.
In the manufacture of jewelry and ornamental synthetic malachite of the invention uses a powdered basic carbonic copper Cu 2 (OH) 2 CO 3 in accordance with GOST 8927-79, ammonium carbonate (NH 4)2 CO 3 in accordance with GOST 3770-78 and 25% aqueous ammonia solution NH 4 OH in accordance with GOST 3760-79.
Example 1
Basic carbonic copper Cu 2 (OH) 2 CO 3 dissolved in a solution of ammonium carbonate (NH 4)2 CO 3 containing a molar excess of ammonia NH 3 with respect to the molar content of carbon dioxide CO 2. The molar content of ammonia relative to the mole content of carbon dioxide for the conditions of this example 1.5. The mixture was stirred until the basic copper carbonate dissolved completely. Evaporation of the solution was carried out at a temperature of 40 o C. For alternating light and dark green bars evaporation process was carried out with a variable speed, variable change in the range of 1.2 times with respect to the evaporation rate at the preceding stage receiving light or a dark strip (layer ). The evaporation process was continued until the release of ammonia vapors ceased. The termination of ammonia vapors indicates the complete decomposition of copper-carbonate ammonium complexes formed during the dissolution of the basic carbonic copper in a solution of ammonium carbonate, which leads to the formation of a dense polycrystalline aggregate of basic carbonic copper, which is a synthetic and ornamental synthetic malachite. After the evaporation process was complete, the remaining aqueous part was separated from the synthetic malachite and analyzed for compliance with the parameters of the reference malachite sample, presented in ICDD database, No. 41-1390.
The indices of the synthetic malachite prepared according to Example 1 are shown in Table 1.
Example 2
The conditions of Example 2 are similar to those of Example 1, but the molar ratio of ammonia to the molar carbon dioxide content for the conditions of this example was 4.0.
The values of the synthetic malachite obtained in Example 2 are shown in Table 1.
Example 3
The conditions of Example 3 are similar to those of Example 1, but the ratio of the mole fraction of ammonia to the mole content of carbon dioxide for the conditions of this example was 8.0.
The values of the synthetic malachite obtained in Example 3 are shown in Table 1.
Example 4
Conditions similar to those of Example 3 of Example 1, but the molar ratio of ammonia to carbon dioxide molar content conditions for this example was 4, and evaporation was carried out at a temperature of 60 o C.
The indices of the synthetic malachite prepared in Example 4 are shown in Table 1.
Example 5
Conditions similar to those of Example 5 Examples 1 and 4, but the evaporation was performed at a temperature of 80 o C.
The values of the synthetic malachite obtained in Example 5 are shown in Table 1.
Example 6
Conditions similar to those of Example 6 Examples 1 and 4, but the evaporation was performed at a temperature of 95 o C.
The values of the synthetic malachite obtained in Example 6 are shown in Table 1.
In addition, X-ray diffractometric studies have shown the identity of the X-ray patterns of natural and synthetic malachite.
Virtually all optical constants of synthetic malachite are analogous to the optical constants of natural malachite.
And like natural malachite, the synthetic malachite in the reducing flame melts and gives the copper kings. Moistened HCl, synthetic malachite stains the flame in blue. When heated in a glass tube, synthetic malachite liberates water and turns black, dissolves in hydrochloric acid with hiss.
Thus, the inventions make it possible to obtain synthetic malachite with the physicochemical properties characteristic of natural malachite, but synthetic malachite differs from natural by increased microhardness, increased wear resistance and better polishability, which is explained by a lower content of impurities and other qualitative composition of impurities.
In general, taking into account the novelty and non-obviousness of inventions, the materiality of all general and particular features of inventions, shown in the "SUMMARY OF THE INVENTION" section, and the feasibility of the invention shown in the section "Examples of realization of inventions", a confident solution of the tasks and obtaining a new technical result, the claimed group Inventions, in our opinion, meets all the requirements for the protection afforded to inventions.
The analysis shows that all common and particular features of inventions are significant, as each of them is necessary, and all together they are not only sufficient to achieve the purpose of inventions, but also allow the group of inventions to be realized in an industrial way.
In addition, an analysis of the set of essential features of a group of inventions and the technical result achieved using them shows the existence of a single inventive concept, a close and inextricable link between inventions and the purpose of the method directly for the production of synthetic jewelry and ornamental malachite, which makes it possible to combine the two inventions in one application.
CLAIM
1. A synthetic gemstones malachite, which is a polycrystalline aggregate containing basic carbonic copper Cu 2 [CO 3] (OH) 2 and impurities, characterized in that the synthetic malachite contains a basic carbonic copper and impurities at the following ratio, wt.% :
Cu 2 [CO 3] (OH) 2 - 99.99 - 99.5
Impurities - 0,01 - 0,50
2. Synthetic malachite according to claim 1, characterized in that the synthetic malachite impurity contain Fe 2 O 3 and Na 2 O.
3. Synthetic malachite according to claim 1 or 2, characterized in that the synthetic malachite density of 3.9 - 4.1 g / cm 3.
4. Synthetic malachite according to any one of claims 1 to 3, characterized in that the hardness of the synthetic malachite according to Mohs is 4.
5. A synthetic malachite as claimed in any one of claims 1 - 4, characterized in that the microhardness of synthetic malachite is 216 - 390 kg / mm 2.
6. Synthetic malachite according to any one of claims 1 to 5, characterized in that the maximum of the reflection spectrum of synthetic malachite is 490-525 nm.
7. Synthetic malachite according to any one of claims 1 to 6, characterized in that the wear resistance of synthetic malachite is 105-150% compared to the wear resistance of natural malachite.
8. Synthetic malachite according to any one of claims 1 to 7, characterized in that the polishability of synthetic malachite with respect to the polishability of natural malachite is 105-150%.
9. A synthetic malachite according to any one of claims 1 to 8, characterized in that the synthetic malachite comprises alternating light and dark green layers.
10. A synthetic malachite according to any one of claims 1 to 9, characterized in that the surface of the synthetic malachite in reflected light exhibits a pluss moiré effect.
11. A synthetic malachite according to any one of claims 1 to 10, characterized in that it is obtained by dissolving the basic carbonic copper in an aqueous solution of ammonium carbonate containing an excess molar amount of ammonia relative to the mole content of carbon dioxide and then evaporating the resulting solution at Heating to form a polycrystalline aggregate of synthetic malachite.
12. Synthetic malachite according to any one of claims 1 to 11, characterized in that the intercrystalline space of the synthetic malachite contains a residual ammonium ion.
13. A method for producing synthetic jewelry and ornamental malachite comprising dissolving the basic carbonic copper in an aqueous solution of ammonium carbonate and then evaporating the solution to form a polycrystalline aggregate of synthetic malachite, characterized in that dissolution of the basic copper carbonate in an aqueous solution of ammonium carbonate is carried out at an excess mole content of ammonia With respect to the mole content of carbon dioxide.
14. The process of claim 13, wherein dissolving the basic carbonic copper in an aqueous solution of ammonium carbonate is carried out at an excess molar ammonia content of 1.5 to 8 times with respect to the mole content of carbon dioxide.
15. The method according to any one of claims 13 - 14, characterized in that the evaporation of the basic copper carbonate in an aqueous solution of ammonium carbonate solution is carried out at 40 - 95 o C.
16. The method according to claim 15, characterized in that the evaporation of the basic copper carbonate in an aqueous solution of ammonium carbonate solution is preferably carried out at 60 - 80 o C.
17. A process according to any one of claims 13 to 16, characterized in that the solution of basic copper carbonate is evaporated in an aqueous solution of ammonium carbonate at a variable rate, with the possibility of producing synthetic malachite with alternating light and dark green layers.
18. The method according to claim 17, characterized in that, in order to provide the possibility of obtaining contrasting color transitions between the layers of synthetic malachite upon transition to the growth of the next layer, the rate of evaporation of the solution of the basic carbonic copper in an aqueous solution of ammonium carbonate is changed by at least 1.2 times Compared with the rate of evaporation during crystallization of the previous layer of synthetic malachite.
19. A method according to any one of claims 13 to 18, characterized in that a synthetic malachite according to any one of claims 1 to 12 is obtained.
print version
Date of publication 03.01.2007gg
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