Method of producing fullerenol c84 from carbon nanocluster sulpho-adduct production wastes

FIELD: chemistry.

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. 65-90C; T. VSP. 200-250C) and high - VTP (ACC. 135-150C; 360-400C).

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.

The invention

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

http://www.sita-journal.com/files/4_v.12,%20No.3,4,2010 .pdf;

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://doctorpiter.ru/articles/1224/

http://www.pharmvesthik.ru/text/24600.html

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 60-70C. 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 60-70C.

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.



 

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