Method of producing fullerenol c84 from carbon nanocluster sulpho-adduct production wastes
SUBSTANCE: invention relates to a novel method of producing fullerenol C84, wherein dry carbon sludge (carbon nano-cluster sulpho-adduct production wastes) is fed into Soxhlets extraction apparatus and fullerenol is extracted in form an aqueous solution of an ammonia salt of fullerenol using an ammonia solution and heating in the evaporation part of the extraction apparatus.
EFFECT: method enables to recycle sulpho-adduct production wastes to obtain fullerenol C84.
12 cl, 3 dwg
The scope of the invention
The present invention relates to the field of chemistry of nanoclusters of carbon and, in particular, to obtain fullerenol of waste production altadata of carbon nanoclusters.
The level of technology
Waste of altadata of carbon nanoclusters, for the sake of brevity hereinafter referred to as the carbon slurry, it products remaining after the extraction of altadata and sulphonic acids from the reaction mass obtained in the process of sulfonation coal tar pitch according to the technology provided by the patent application EN 2010105074 A (publication date: 20.08.2011)"Sulfoalkyl of carbon nanoclusters and method thereof" and request WIPO Patent Application WO/2011/102754 (Publication Date: August 25, 2011) "CARBON NANOCLUSTER SULFO-ADDUCT, METHOD FOR PRODUCING SAME AND USE THEREOF", alphadot of carbon nanoclusters.
Sulfoalkyl of carbon nanoclusters produced by LLC "R & d centre for Applied Nanotechnology (Saint-Petersburg) called "Astral" http://www.nanoteh.ru/production/adducts.html. While there is no technology of waste production altadata, the cost of fullerenol as proposed in the present invention, will be minimal, 3-4 orders of magnitude lower than the cost of fullerenols obtained by other technologies, in particular described in the article, Wang, C., Cheng C.-Y., Structures and stabilities of C60(OH)6and C60(OH)12fullerenols (J. Molec Struc, 1997, v.391, Issue 1-2, p.p.179-187, DI) and request US No. 2004/0048127.
Coal tar pitch, which is a raw material for producing altadata of carbon nanoclusters, get in the processing of coal tar. The main components of the pitch are multicore condensed aromatic and heterocyclic compounds, the products of polymerization and polycondensation. Pitches are spatially structured disperse systems that do not have a specific melting and solidification and melting in the interval characterized by the softening temperature. In particular, there are peck of coal medium - STP (so RASMAG. 65-90°C; T. VSP. 200-250°C) and high - VTP (ACC. 135-150°C; 360-400°C).
As it turned out, the products of sulfonation coal tar pitch concentrated sulfuric acid contains not only polycarboxylate derivatives of carbon nanoclusters (sulfoalkyl), but polyhydroxylated derived nanocluster carbon - fullerenol. The core of this fullerenol, according to mass spectrometry, is a fullerene C.
After extraction of the products of sulfonation pitch of altadata further processing of the remaining carbon slurry technology under patent applications EN 2010105074 A and WO 2011102754 A2 (WIPO Patent Application WO/2011/102754), is not provided, and this carbon is the first sludge is a waste of altadata, requiring disposal.
The carbon slurry is a fine mass of black that contains not only carbon, but a number of polyhydroxylated derived nanocluster carbon - fullerenol s.
Recently the carbon nanoclusters are increasingly used in industry. As is widely known carbon nanoclusters, you can specify soot, nanodiamonds, fullerenes, nanotubes, graphenes.
Fulleroid is a class of homologues of nanoparti with frame curved spherical (fullerene), frame curved non-spherical structures (nanotubes), bulbous structure (multilayer fullerenes) and other Fulleroid widely investigated, but they are getting at the moment is mainly the result of applying a thin plasma technology and very expensive process.
The objective of the invention is the extraction of fullerenol of waste production altadata of carbon nanoclusters (Astralene With). A homologue of fullerenol s is fullerenol C60. But the cost of fullerenol C60 derived from fullerene C60, higher cost of fullerenol s obtained by this method, at least 4 of the order. Because of the high cost fullerenol C60 only get in preparative quantities for industrial use is of he has no prospects.
This task is solved in that the proposed fullerenol slightly soluble in water, very soluble in aqueous solutions of alkalis and ammonia, and it is easily extracted from the waste of altadata, for example, water 5-7% solution of ammonia in ammonium salt.
The inventor found that after extraction from the waste of altadata nanoclusters carbon in the waste remains uncovered nanocluster carbon - fullerenol, which you can extract with aqueous solutions of alkali or ammonia in the form of salts of alkali metals or ammonia, from which you can select fullerenol acidification of solutions of salts of the acid. Fullerenol is giperarifmeticheskie polyphenols, and he has all the characteristic reactions of phenols, in particular, its allotment of alkali metal salts and ammonium salts by acidification of solutions to pH 4-6.
According to preliminary studies, the core of fullerenol according to mass spectrometry is a fullerene C (see figure 3 on page 7).
Fullerenol C soluble in water slightly soluble in alcohol, forming a yellow solution in dimethylformamide (DMF), forming a red-brown solution. Sodium and ammonium salts of fullerenol C represent the crystalline compounds of black (Figure 1), dissolve well who are in the water, forming solutions of black (Figure 2), and dimethylformamide.
The author obtained fullerenol s can be used:
a) as a modifier of epoxy composites:
the results of the research epoxy composites modified soluble adducts of carbon nanoclusters. Taisin, Advisor to the Russian Academy of architecture, doctor of technical Sciences, Professor; Antennomeres, Ph.D., Professor, "STC Application of Nanotechnologies", St. Petersburg; Sunkistem, graduate of the Mordovian state University; AAS, researcher "STC Application of Nanotechnologies", St. Petersburg. The sodium salt of fullerenol corresponds to a sample of Nanoparticles 1" http://www.nanoclaster.ru/Rezultaty%20Rus.html;
b) as microbicides with anti-HIV activity, does not exhibit cytotoxicity:
1. Thesis (26.11.2010): Microbicides with anti-HIV activity, Gilyazova A.V. Institute of immunology. Gamaleya, Moscow. Section 6 of the abstract. The study of cytotoxicity, antiviral activity and virucidal effect of adducts of carbon nanoclusters, p.18. Fullerenol s matches pattern "ANKA ECP".
2. Water Soluble Carbon Nanoclusters as Microbicides with Anti-HIV Activity. A.Gilyazova, G.Kornilaeva, A.Ponomarev, V.Chereshnev, E.Karamov http://fiqovsky.borfig.corn/sita/12_34 aspx
3. Water Soluble Carbon Nanoclusters as Microbicides with Anti-HIV Activity. A.Gilyazova, G.Kornilaeva, A.Ponomarev, V.Chereshnev, E.Karamov. Scientific Israel, Technological Advantages
C) as the aqueous solution of fullerenol C forms with cosmetic creams stable emulsion, it is assumed that the possibility of its use as an antioxidant modifier cosmetic creams that are similar to creams, modified fullerene is produced by the British company "Zelens Dermatological Research", with antioxidant and rejuvenating properties. Studies of fullerenol has shown that it has antioxidant properties: http://www.nair-it.ru/pressabout/2011-04-08 nanonewsnet.php
http://tobolsk.neduqamnet.ru/content/v-sankt-pietierburqhie-pristupili-k-bioispytaniiam-fullierienov so it is to be used as an antioxidant additive in cosmetics. Cosmetic company "Zelens Dermatoloqical Research (http://www.arbeidshyqiene.nI/~uploads/text//Icb/LCB%202007-02-08%20HSE%20aspects%20of%20nanoparticles.pdf (see p.22) launched the creams based on fullerene C60. However, these creams (day cream Zelens, Zelens night cream Zelens eye cream) too expensive, in addition, it is generally recognized, the fullerenes are toxic compounds that are carcinogenic properties. The cost of similar creams, modified fullerenol derived from glycerol, will be much less, and conducted research at the Institute of immunology. Gamaleya (see "Thesis Microbicides with anti-HIV activity") showed no cytotoxicity at this fullerenol.
Detailed description of the invention
With the Hoi carbon sludge (waste of altadata of carbon nanoclusters) download and extractor type to conventional Soxhlet extractions and extracted fullerenol, in the form of an aqueous solution of ammonium salt of fullerenol, ammonia solution concentration of 7-10%, by heating it in the evaporating section of the extractor. As extraction with an aqueous solution of ammonium salt of fullerenol of the extraction part flows into the evaporator (flask, cube and so on) and turns black (like the solution shown in figure 2 on page 3). Extraction stops when the solution in the extraction part of the extractor becomes colorless and transparent. All insoluble in aqueous ammoniacal solution components carbon sludge - carbon, aromatic organics remain in the extraction part. Then extract ammonium salt of fullerenol from the evaporator extractor is poured into the container with water and acidified with a solution of sulfuric acid to slightly acid environment (pH of 6.8 to 6.5). This reaction is characteristic of an entire class of phenols, including for fullerenol C, which also belongs to the class of phenols, as giperarifmeticheskie polyphenols s(HE)n. Upon acidification of a solution of the acid extract is the formation of fullerenol in the form of flakes. After a short sludge solution is separated into soluble in water sludge fullerenol dark brown color and almost transparent aqueous solution containing excess acid and ammonium sulfate. With settled sludge carefully drained off (decanted) water part of the filter, and the comfort of the sediment. The residue, representing fullerenol C, thoroughly washed with water and dried at a temperature of 60-70°C. If not clean, dry fullerenol s representing a fine crystalline precipitate dark brown, sequentially washed with benzene or toluene, then acetone and water. Then again dried and milled.
1. The method of receiving fullerenol s, wherein the dry carbon sludge (waste of altadata nanoclusters carbon) is loaded into the extractor type to conventional Soxhlet extractions and extracted fullerenol in the form of an aqueous solution of ammonium salt of fullerenol ammonia solution, heating it in the evaporating section of the extractor.
2. The method according to claim 1, wherein the ammonia solution has a concentration of 7-10%.
3. The method according to claim 1, in which, as extraction, an aqueous solution of ammonium salt of fullerenol of the extraction part flows into the evaporator.
4. The method according to claim 1, wherein the extraction is stopped when the solution in the extraction part of the extractor becomes colorless and transparent.
5. The method according to claim 1, in which all insoluble in aqueous ammoniacal solution components carbon sludge: carbon, aromatic organics remain in the extraction part.
6. The method according to claim 1, wherein the extract ammonium salt of fullerenol from the evaporator of the extras is ktora poured into a container of water and acidified with a solution of sulfuric acid to slightly acid environment (pH of 6.8 to 6.5).
7. The method according to claim 1, in which upon acidification of a solution of the acid extract is the formation of fullerenol in the form of flakes.
8. The method according to claim 1, in which after a short sludge solution is separated into soluble in water sludge fullerenol dark brown color and almost transparent aqueous solution containing excess acid and ammonium sulfate.
9. The method according to claim 1, in which settled sludge is carefully drained off (decanted) the water part and filter the precipitate.
10. The method according to claim 1, wherein the precipitate, representing fullerenol C, thoroughly washed with water and dried at a temperature of 60-70°C.
11. The method according to claim 1, wherein fullerenol s is a partially soluble in water, soluble in alcohol and in dimethylformamide (DMF), the product contained in the waste production altadata of carbon nanoclusters.
12. The method according to claim 1, wherein if not clean, dry fullerenol s representing a fine crystalline precipitate dark brown, sequentially washed with benzene or toluene, then acetone and water, after which it is again dried and milled.
SUBSTANCE: present invention relates to a method for desalination of phenol resin and apparatus to that end. The disclosed method involves mixing starting components - phenol resin, diisopropyl ether, water and concentrated sulphuric acid at temperature 20-60°C, phase separation of the mixture into a top organic layer, which is a mixture of desalinated phenol resin and ether, and a bottom aqueous layer with subsequent removal of the aqueous layer and distillation of ether from the organic layer and obtaining desalinated phenol resin, wherein the obtained ether is fed to the step for mixing components. The starting components are used in the following weight ratio: resin : ether : water : sulphuric acid = 1 : (0.2-0.6) : (0.7-1.0) : (0.007-0.018), wherein mixing is carried out in turbulent conditions.
EFFECT: present invention enables to obtain desalinated resin with high degree of purity while reducing the cost of the process and the obtained product.
13 cl, 24 ex, 6 tbl, 2 dwg
SUBSTANCE: process includes resorcinol extraction with organic solvent tributyl phosphate (TBPh). The well-milled hard foamed polyurethane (FPU) will be modified at that with tributyl phosphate in the mass ratio FPU:TBPh = 1:(2.0-2.5), the extraction will be performed prior to establishing the interphase balance with subsequent isolation of organic phase from the water phase.
EFFECT: process enables one to enhance the concentrating coefficient and reduce expenditure of the organic solvent tributyl phosphate.
1 tbl, 2 ex
SUBSTANCE: invention relates to organic chemistry, more specifically to a method of producing 2-aminoethanesulfonic acid by reacting 2-aminoethylsulphuric acid with excess sodium sulphate in an aqueous solution and boiling for 20 hours with subsequent separation of the desired product from mineral salts through electrodialysis at temperature 30-45°C and constant current density of 1.2-3.0 A/dm2.
EFFECT: reduced power consumption of the process and intensification of the technology with high current output of the product.
1 cl, 4 ex
SUBSTANCE: invention relates to compound of general formula , where R represents unsaturated linear or branched hydrocarbon chain of atoms. Invention also relates to application of said compounds as means for inhibition of platelet aggregation.
EFFECT: obtaining novel compound, characterised by high rate of reaction with sulphur-containing groups of atoms of platelet components, actively inhibiting platelet activity, possessing high stability.
2 cl, 1 tbl, 6 dwg, 6 ex
SUBSTANCE: invention relates to production of primers and can be used in production of electric detonators without priming explosives, that are safe to charge and safe to handle. The low-sensitive explosive compound contains (in wt %): blasting explosive 70-95 and nano-metal 5-30. The blasting explosive used is dinitrodiamino ethylene and the nano-metal used is nano-copper or nano-silver.
EFFECT: compound has low potential hazard in making electric detonators and low probability of unauthorised triggering by mechanical or electromagnetic action, provides stable detonation with parameters that are sufficient for reliable secondary priming.
3 cl, 5 ex
SUBSTANCE: invention relates to a method of modifying the surface of an inorganic oxide. The method involves treating an inorganic oxide with a water-soluble nickel (II) salt to form nickel (II) oxide nanoparticles on the surface of the inorganic oxide. The inorganic oxide and an alkali are successively added to the aqueous nickel (II) salt solution preheated to 50-90°C. When the obtained mixture cools down, a solution of sodium tetrahydroborate in an aliphatic alcohol is then added. An "aliphatic alcohol - water" azeotropic mixture is then distilled from the obtained product. The product is held at 70-90°C and then successively washed in water and twice in aliphatic alcohol. The separated precipitate is held in air until nickel is completely oxidised to nickel (II). The inorganic oxide used is aluminium oxide or silicon oxide.
EFFECT: low power consumption of the process.
SUBSTANCE: method of producing nanocomposite with double shape memory based on monocrystal of ferromagnetic alloy Co35Ni35AI30 comprises primary annealing of monocrystal at 1330-1340°C for 8.5 h in inert gas. Then, tempering is carried out in water. Secondary annealing is carried in two steps. Note here that monocrystal is placed at test machine clamps; vacuum of 10-2-10-3 Pa is created to heat it to intermediate temperature of 200°C. Then, compressive strength of 100-120 MPa is applied in direction  in monocrystal to be heated to 400°C at the rate of 10-20°C/min and held thereat for 0.5 h and cooled to 200°C, thereafter load being removed. Now cooling is performed to room temperature at the rate of 10-20°C/min.
EFFECT: higher mechanical and functional properties, material with double shape memory and high-temperature superelasticity.
1 tbl, 1 ex
SUBSTANCE: invention can be used to produce protective coatings for pipelines in oil, gas, oil and gas refining, mining and chemical industry. Carbon nanotubes are fed into molten stearic acid via ultrasonic dispersion. The obtained mixture is then mixed with a polymer - high-pressure polyethylene or suspended polyvinyl chloride. The mixture is heat-treated and articles are moulded.
EFFECT: simple process of producing the composite, high wear resistance of the composite.
SUBSTANCE: invention relates to material science. The method of producing a polytetrafluoroethylene-based antifrictional polymer composite involves preliminary physical and chemical treatment of ultrafine detonation diamond powder, mechanical dispersion of the mixture of powdered polytetrafluoroethylene and ultrafine detonation diamond, pressing and sintering the composite in an inert medium. Physical and chemical treatment of the ultrafine detonation diamond powder involves heating therein in an inert medium at temperature of 700-800°C for 20-30 minutes with continuous removal of gaseous thermal desorption products until removal of oxygen-containing surface groups, characterised by an absorption band in infrared spectra with a maximum in the wave number range of 1730 - 1850 cm-1.
EFFECT: invention improves tribological properties of the composite and uniformity of its properties on a sample volume.
3 cl, 5 tbl, 5 ex
SUBSTANCE: invention can be used in powder metallurgy, particularly in producing ultrafine powdered materials based on tungsten carbides used as precursors in production of hard alloys. The method of producing ultrafine powder of a mixture of tungsten carbide and cobalt metal involves producing ultrafine powder of a mixture of tungsten and cobalt oxides by neutralising an aqueous solution of corresponding inorganic salts in the presence of soot, and subsequent carbidisation, carried out by reduction in a current of an inert gas at a rate of 4.5-5.0 l/h at temperature of 1150-1250°C.
EFFECT: obtaining ultrafine powder of tungsten carbide and cobalt metal with particle size of about 300 nm.
2 cl, 2 ex
SUBSTANCE: invention relates to chemical industry. Fullerene-containing soot is mixed with a liquid which reacts with fullerenes in the soot, e.g. with an aqueous alkali solution with concentration of at least 0.5 wt % selected from KOH, NaOH, Ba(OH)2 and/or hydrogen peroxide H2O2, with ratio thereof to soot of 1:(20-300) ml/g. The obtained mixture is mixed with a solution of a catalyst for hydroxylation of fullerenes - tetrabutylammonium hydroxide with concentration of 5-20 wt % in volume ratio to the mixture of 1:(100-400). After mixing, the mixture is filtered to separate spent soot from the obtained solution, in which a salting out agent is added, e.g. methanol CH2OH, or a mixture of propanol n-C3H7OH, diethyl ether C2H5OC2H5 and n hexane C6H6. The mixture of fullerenols precipitates, and the precipitate is washed in a Soxhlet apparatus, after which the dry mixture of fullerenols is separated.
EFFECT: invention simplifies and reduces the cost of the process, increases safety by excluding aromatic solvents.
FIELD: process engineering.
SUBSTANCE: invention relates to electronics and nanotechnology and cab be used in production of composite containing laminar graphite- and molybdenum sulphide-based materials. TEG or oxidised graphite and thiomolybdate are used as initial compounds. Note here that thiomolybdate is decomposed in the mix with TEG or oxidised graphite at heating or subjected to decomposition in solution with acid medium. Formed product containing TEG or oxidised graphite and precursor of molybdenum sulphide are flushed and heated in vacuum to 350-1000°C to obtain composite including molybdenum sulphide on graphite layers pile of composition MoxSy, where x=1-3, y=2-4. Note also that TEG or oxidised graphite are pre-dispersed while molybdenum precursor represents molybdenum tri-sulphide.
EFFECT: possibility to vary size, morphology and phase composition of nanoparticles on graphite surface.
4 dwg, 5 ex
SUBSTANCE: in the method of producing nanoring arrays, comprising a substrate with deposited polystyrene spheres, with a metal layer deposited thereafter, followed by etching, the substrate used being ordered porous films, and the arrangement of the nanorings is determined by the arrangement of pores in the film material using self-organisation techniques.
EFFECT: cheap, reproducible and controlled formation or ordered nanoring arrays.
8 cl, 3 dwg
SUBSTANCE: described is a method of modifying electrochemical catalysts on a carbon support, involving performing modification in a vacuum chamber equipped with a controlled source of a stream of atoms or ionised atoms of the modifying material, a device for feeding inert gas and a holder for the processed catalyst; the modified surface of the obtained catalyst on a carbon support is treated with a stream of atoms or ionised atoms of the modifying material, wherein the synthesised catalyst is placed on a fine carbon support using an open porosity porous substrate mounted on the holder, made from an inert material, pneumatically linked to the device for automatically feeding gas; inert gas is blown through the porous substrate to form pseudo-fluidised layer of particles of a carbon support with the modified catalyst over the substrate; the catalyst is then treated with a stream of atoms or ionised atoms of the modified material.
EFFECT: high efficiency of modifying electrochemical catalysts and operational characteristics thereof.