Composition based on dimethyl disulfide |
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IPC classes for russian patent Composition based on dimethyl disulfide (RU 2219168):
    
 The method of obtaining serosoderjaschei additives / 2181137
The invention relates to the synthesis of serosoderjaschei additives with enhanced extreme-pressure, anti-wear properties, high thermal and oxidative stability
The method of obtaining serosoderjaschei additives / 2168536
The invention relates to the field of synthesis of serosoderjaschei additives with enhanced extreme-pressure, anti-wear properties, high thermal and oxidative stability
The method of obtaining polysulfide oligomers / 2154056
The invention relates to a process for the synthesis of polysulfide oligomers used as the basis sealant, adhesive and coating materials in various industries, including optical and optoelectronic engineering
 A method of producing dimethyl sulfide / 2032664
The invention relates to the chemistry of acyclic sulfides, specifically to an improved process for the preparation of dimethyl sulfide, which can be used as odorant and the source of raw material for the synthesis of dimethyl sulfoxide
The method of producing diallylsulfide / 2017715
 The method of obtaining the odorant / 2105597
The invention relates to the purification of gases, in particular to the processes of production of odorants for natural gas from mercaptoundecanoic hydrocarbons, and may find its application in the gas industry, including for sorbent regeneration
- hydroxy -3
 ,5di-tert - butylbenzaldehyde as a stabilizer chain polymers" target="_blank"> - hydroxy -3,5di-tert - butylbenzaldehyde as a stabilizer chain polymers" align="left" vspace="30" hspace="30" /> (2-n, n-diethylaminoethyl)-4- hydroxy -3,5di-tert - butylbenzaldehyde as a stabilizer chain polymers / 2026859
- hydroxy -3
,5di-tert - butylbenzaldehyde as coagulant emulsion rubbers" target="_blank"> - hydroxy -3,5di-tert - butylbenzaldehyde as coagulant emulsion rubbers" align="left" vspace="30" hspace="30" /> (2-n,n-diethylaminoethyl)-4- hydroxy -3,5di-tert - butylbenzaldehyde as coagulant emulsion rubbers / 2026858
The invention relates to the production of synthetic rubber by emulsion polymerization method
 Method for producing organic disulfides / 2091370
The invention relates to an improved process for the preparation of organic disulfides of the General formula R-S-S-R
-dithiobis-(2,6-di-tert-butylphenol)" target="_blank">
 -dithiobis-(2,6-di-tert-butylphenol)" align="left" vspace="30" hspace="30" /> The way to obtain 4,4-dithiobis-(2,6-di-tert-butylphenol) / 2058304
The invention relates to the field of aromatic polysulfides, particularly to a method of obtaining policiales-(2,6-di-tert-butylphenol), which is used as antioxidants for high molecular weight compounds and intermediate for obtaining 2,6-di-tert-butyl-4-mercaptoethanol
 Method of oxidising mercaptans contained in hydrocarbons / 2406750
Invention relates to a method of removing mercaptans from hydrocarbons through oxidation. The method involves: a) bringing a hydrocarbon or mixture of hydrocarbons which contain one or more mercaptans of general formula R-SH, in which R is a C1-C50-aliphatic or C6-C30-aromatic hydrocarbon, into contact with a system containing iron (III), heteropolyacid, having redox properties, and water, where the heteropolyacid is selected from heteropolyacids of general formula (I): HnXVyM(12-y)O40 in which n is an integer from 4 to 6 and is equal to 3+y; X is an element selected from a group comprising P and As; y is an integer from 1 to 3; and M consists of Mo and W; b) oxidation of mercaptans to corresponding (di)sulphides as a result of the oxidative effect of iron (III), which is reduced to iron (II); c) separation of the aqueous phase from the organic phase; d) re-oxidation of iron (II) to iron (III) in a gas stream containing oxygen; e) recirculation of the system containing iron (III), heteropolyacid and water to the oxidation operation (a).
 Palladium-copper catalysts for homogeneous selective oxidation of thiol groups, combination and composition based on said catalysts and therapeutic treatment method / 2451010
Palladium-copper catalyst for homogeneous selective oxidation of thiols combines a functional binuclear thiolate bridge coordination compound of palladium (II) and a modifying thiolate complex of copper (I), having general formula [pd2 II(µ-SR)2(NH3)4]·{Cu1 k(SR)m} (I). SR is a residue of a thiolate ligand of glutathione or acetylcysteine, k ranges from 2 to 14, m≥3k. The invention also discloses a catalytic combination which stimulates proliferative activity, a pharmacological combination for enhancing therapeutic activity of a purine and(or) pyrimidine base or lithium ions, pharmaceutical compositions which stimulate proliferative activity, and for enhancing therapeutic activity of said bases or lithium ions, and methods for therapeutic treatment of a patient based on said catalyst.
 New cyclohexenone compounds of antrodia camphorata and their application / 2422431
Present invention refers to new compounds of formula
 Solvent composition based on organic sulphoxide with masked odour / 2485098
Invention relates to solvent compositions which contain at least one organic sulphoxide of general formula (1):
 Composition based on organic sulphide with masked odour / 2501788
Invention relates to masking the odour of organic sulphides and more specifically to alkyl or dialkyl sulphides, particularly dimethyl sulphide, as well as oxides thereof and particularly dimethyl sulphoxide by adding to said organic sulphides at least one odour masking agent which contains at least one monoester, at least one di- or triester, at least one alcohol, at least one ketone and optionally at least one terpene.
Method for modifying paraffins / 2313519
Invention relates to modification of oil paraffins, namely, to preparing sulfurous compounds used as additives in manufacturing bitumen in petroleum chemistry. Method involves interaction of paraffin with sulfur in the presence of alkaline metal persulfate or alkaline-earth metal persulfate, or ammonium persulfate. Invention provides preparing modified paraffins for a single step.
 Prodrug 1,3-diamino-2-hydroxypropane derivatives / 2357962
Invention relates to the compounds of the formula
 Method of producing dimethyl sulphide / 2457029
Invention relates to methods of producing sulphur-containing compounds, specifically dimethyl sulphide which is used as an odorant and starting material for synthesis of dimethyl sulphoxide which is used as a medicinal agent, solvent and extractant. Described is a method of producing dimethyl sulphide by converting dimethyl disulphide in the presence of methanol at atmospheric pressure and temperature 300-380°C using a catalyst containing gamma-aluminium oxide and 0.73-7.3 wt % chromium oxide. The weight ratio of methanol to dimethyl disulphide is equal to 0.8-0.9 g/g and contact time is 0.1-0.35 s.
![Method of producing 1a-methyl-1a-(3'-thioalkylprop-2'-yl)-1ah-1(9)a-homo(c<sub>60</sub>-i<sub>h</sub>)[5,6]fullerenes](http://img.russianpatents.com/img_data/1116/11161650-s.gif) Method of producing 1a-methyl-1a-(3'-thioalkylprop-2'-yl)-1ah-1(9)a-homo(c60-ih)[5,6]fullerenes / 2459805
Invention relates to organic chemistry, and specifically to a method of producing sulphur-containing homofullerenes of general formula (1):
 4-hydroxybenzamide drug derivatives / 2465271
There are presented drug derivatives wherein said derivatives contain a H2S-releasing fragment of 4-hydroxythiobenzamide which is either covalently bond with the drug, or forms a pharmaceutically acceptable salt with the antilipidemic drug.
Composition based on organic sulphide with masked odour / 2501788
Invention relates to masking the odour of organic sulphides and more specifically to alkyl or dialkyl sulphides, particularly dimethyl sulphide, as well as oxides thereof and particularly dimethyl sulphoxide by adding to said organic sulphides at least one odour masking agent which contains at least one monoester, at least one di- or triester, at least one alcohol, at least one ketone and optionally at least one terpene.
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The invention relates to a composition based on dimethyl disulfide (DMDS). DMDS is used as the source of the ingredient by a vapor-phase cracking and the sulphurization of the catalyst. To improve the smell of the product due to the presence of impurities, a composition based on DMDS comprising by weight at least 95% DMDS, less than 500 million hours of methylmercaptan, less than 100 million hours of dimethyl sulfide and up to 1% of at least one odorants representing an ester of the General formula R1-CO2R2in which R1represents the possible unsaturated, linear or branched hydrocarbon radical comprising from 1 to 4 carbon atoms, R2represents the possible unsaturated, linear, branched or cyclic hydrocarbon radical comprising from 2 to 8 carbon atoms. 7 C.p. f-crystals, 2 ill., table 1.
The invention relates to organic sulfides, in particular dimethyl disulfide.
Dimethyl disulfide (DMDS) has a strong irritating odor due in part to the availability of highly odorous impurities and partially due to the inherent DMDS garlic and ethereal odor. This strong smell deters the growth of the use of this product in asnom cracking. Compared with other compounds used in these cases, for example, tert-ankylosauridae, DMDS has numerous advantages, in particular a high sulfur content (68%) and non-coking decomposition (CH4H2S). In addition, in these cases, the action DMDS in General leads to better results compared to other products, such as tert-alkyltrimethyl. However, these and other products are significantly less strong odor that enables easier handling compared to DMDS.
Among the synthesis methods DMDS a particularly effective and economical is the oxidation of mercaptan sulfur according to reaction: This oxidation of mercaptan sulfur catalyzed with an organic or inorganic homogeneous or heterogeneous basic agents, periodic or continuous mode, accompanied by the production of hydrogen sulfide and dimethyldisulfide (CH3SxCH3), in which the number of sulfur atoms x is greater than 2. In the production DMDS by this method with high yield and limited DMPS (dimethyldisulfide with the number of sulfur atoms more than 2), according to Europe is haunted by the area of the intermediate degassing followed by the distillation zone. Although this way and reach a high yield and selectivity by DMDS, it turns out that such a process leads to the formation of a significant amount of mercaptan (approximately 4000 million h (ppm) and very small amounts of dimethyl sulfide (approximately 300 million h) generated from the mercaptan used or produced during the synthesis DMDS, which remain in the finished product. The presence of these volatile impurities leads to the fact that the smell DMDS increases, it becomes very unpleasant and irritating and causes significant difficulties when using this product.
To disguise the smell of organic polysulfides, in U.S. patent 5559271 recommended to add a number of odorants, such as, for example, vanillin or ethylvanillin. Although its General formula includes DMDS, this patent largely directed to the processing of heavy polysulfides, such as, for example, di-tert-nonidentically. The application of this method to DMDS not possible to disguise its sickening and very unpleasant smell.
It was found that in the particular case DMDS introduction odorants only effective if used DMDS has the preferably comprises by weight less than 200 million h mercaptan and less than 50 million hours of dimethyl sulfide. Also found that the most effective fragrances are not those specified in the aforementioned U.S. patent, and compounds selected from esters corresponding to the General formula: R1CO2R2(I) where R1represents the possible unsaturated, linear or branched hydrocarbon radical comprising from 1 to 4 carbon atoms, and R2represents the possible unsaturated, linear, branched or cyclic hydrocarbon radical comprising from 2 to 8 carbon atoms.
The subject of the invention, therefore, is a composition based on DMDS, characterized in that the composition comprises by weight at least 95% dimethyl disulfide, not more than 500 million hours of mercaptan (MM), not more than 100 million hours of dimethyl sulfide (DMS) and up to 1% of at least one connection-odorants, preferably ester that meets the General formula (I).
In the context of the present invention can use any method known to the specialists in a specific field of technology, to obtain DMDS with low content of volatile impurities, such as MM and DMS. However, in the case DMDS with a high content of MM and DMS osobennosti deleting MM and VHI, while conventional methods reduce odor usually based on the removal of residual mercaptans by carrying out a specific reaction of the functional group of the mercaptan with the output component, such as a base or oxide alkene in the presence of a base, and have no effect on LCA contained in DMDS.
DMDS with distilled so light fractions containing preferably less than 200 million h MM and less than 50 million h ICH is used for preparation of stock that meets the present invention, by simply introducing at least one connection odorants.
Since one of the main advantages DMDS in its applications is the high content of sulfur (68%), excessively high number of odorants in such composition would lead to a relative reduction of sulfur content and thus would reduce the advantage of this product. The maximum content of perfumes (fragrances) is therefore set to 1%, but it is preferable that its content ranged from 0.1 to 0.5%, and more preferably the content of odorants in the amount equal to about 0.2%.
We can mention only for illustration and not as limiting examples of esters that meet the General formula (I): butylacetate. Isoamylase, 2-methylbutylamine, isoamylamine, benzoylacetate and their mixtures are particularly preferred. Esters (I) can also be used in combination with orthophthalate corresponding to the General formula: where each of the symbols R3and R4the same or different, represents a possible unsaturated, linear, branched or cyclic hydrocarbon radical, comprising from 1 to 8 carbon atoms. In particular, as a non-limiting example of compound (II) can be mentioned diethylacetal.
Typical composition conforming to the present invention, includes, in wt.%: Isoamylase - 0.1 Diethylacetal - 0,1 DMDS with distilled light fraction - 99,8Another typical composition conforming to the present invention, includes, in wt.%: Isoamyl ether acetic acid - 0,05 2 - Methylbutylamine - 0,03 Benzoylacetate - 0.02 Diethylacetal - 0,1 DMDS with distilled light fraction - 99,8 The following examples illustrate the invention but do not restrict it. EXAMPLE 1: Synthesis of dimethyl disulfide according to the method described in the patent EP 0446109 A. EQUIPMENT: Fig.1 shows a plan of the used setup, including DV and - this reactor with a stirrer, and the final stage reactor is a tubular reactor with a fixed bed. System degassing is located between the two reactors, and this system consists of a fitted jacket and a receiver 2, equipped with a stirrer, over which is mounted a column of cooling, allowing you to re-condense the mercaptan, which can be carried out with hydrogen sulfide, before deleting it. This installation is equipped with a pump located between the outlet of the crystallizer 2 and the inlet of the reactor 3 the final stage of the process that allows you to enter in the reactor liquid product processed in the crystallizer. Column degassing 4 is used for complete removal of H2S dissolved in the liquid leaving the reactor 3. Distillation column 5 allows you to separate most of the excess of the mercaptan with the purpose of recycling it through the pipe 22 into the reactor 1. Column 6 makes possible the separation of the remaining portion of dimethyldisulfide (DMPS) for the purpose of recycling them into the reactor ili reactor 1. B. METHODOLOGY: methyl mercaptan (MM) in liquid form is fed into the reactor 1 under pressure through a pipe 11 with a flow rate of 960 g/h of Liquid sulfur fed into the reactor 1 through the pipe 10 with a flow rate of 160 g/h (MM/S=4 (molar.)) is W 5.5 bar (0.55 MPa), and the temperature of the 40oC. the Reaction mixture at the outlet of the reactor 1 has the following composition by weight, excluding N2S and the excess mercaptan: DMDS 85%, DMPS 15%. This reaction mixture is then serves for processing in the crystallizer 2 via the pipe 14. After processing this mixture, freed from H2S, is fed through a pipe 17 into the reactor 3 the final stage of the process, which contains a load of dry resin A21 in the number 94, Relative to the reactor pressure is 5.5 bar (0.55 MPa), and temperature 40oC. At the outlet of the reactor 3 mixture has the following composition by weight, excluding H2S and the excess mercaptan: DMDS TO 98.5% DMPS of 1.5%. Then through the pipe 18 this mixture is served in the degasser 4 for subtracting from the H2S, formed in the reactor 3 during reverse transformation of dimethyldisulfide when interacting with the mercaptan with getting DMDS. After passing through the column degassing 4 the mixture is fed through the pipe 21 into the first distillation column 5 to remove almost all of the excess mercaptan. The mercaptan can be retalitate through the pipe 22 to be input to the reactor 1 reagents. At the outlet from the column 5 of the mixture through the pipe 23 serves to the second distillation column 6, where in the lower part of the colon is clitatii in the reactor 1. DMDS, in the end selected from the upper part of the column 6 through the pipe 24 and called AndAboutin subsequent examples, the test for odor intensity, has the following mass composition: - DMDS: 99,3% - DES: 3000 million hours MM: 4000 million hours - LCA: 300 million hours EXAMPLE 2: Purification of disulfide ethane, obtained by the method described in the patent EP 0446109 The synthesis procedure is the same as described in example 1, except that DMDS emerging from the column 6 through the pipe 24, is fed into a third distillation column 7 (see scheme in Fig.2), where volatile impurities, such as methyl mercaptan and dimethyl sulfide, is removed from the upper part of the column through the pipe 27. DMDS selected from the lower part of the column through a pipe 28 has the following mass composition: - DMDS: 99,7% - DES: 3000 million hours - MM:<100 million hours - LCA:<50 million hours This cleared DMDS, hereafter referred to as Boand the sample DMDS AAboutobtained in example 1 were tested for the presence of odor. 8 people invited to this test, unanimously recognized the significant improvement of the odor sample BoDMDS compared with sample AaboutDMDS, nevertheless it also reported that garlic ethereal odor remained DMDS sample BboBoobtained in example 2. Complete dissolution of vanillin was observed after one hour at 25oC. the thus Obtained sample was denoted as B1. EXAMPLE 4 The vanilla used in example 3 was replaced by 2000 million h by weight of ethylvanillin (3 ethoxy-4-hydroxybenzaldehyde). Its dissolution was observed after one hour at 25oC. the thus Obtained sample was designated as a2. Examples 5 and 6 illustrate the obtaining of compounds based DMDS, whose smell is masked preferred products in accordance with the present invention. EXAMPLE 5 2000 million h of a mixture consisting by weight of from 50% Solidaritate and 50% of diethylacetamide added to 100 g DMDS sample Boobtained in example 2. Since this mixture was liquid, dissolution occurred immediately at the 25oC. the thus Obtained sample was designated as a3. EXAMPLE 6 The mixture used in example 5 was replaced with a 2000 million h of a mixture having the following mass composition, %: Isoamylase - 25 Diethylacetal - 50 2-Methylbutylamine - 15 Benzoylacetate - 10 Dissolve this mixture in Bohappened instantly at 25oC. the thus Obtained sample was designated to test performed by the group of 8 persons referred to in example 2. These 8 people were asked to evaluate the samples in points from 0 to 5 in accordance with a preferred scent to 0 score corresponded to the composition with the least preferred scent, 5 - composition with a most preferred scent, and points 1, 2, 3 and 4 to classify intermediate levels. The results presented in the table. It is easy to see that the smell of compositions B1B2In3and B4always preferred the smell of composition B0and that the sum of the scores obtained for composition B4very close to the maximum possible value (40). The members of the expert group, also indicated that they preferred a "fruity" odor compounds In3and B4"vanilla garlic" smell inherent in the compositions In1and In2. Comparative examples 7-11 illustrate the necessity of removing the most volatile impurities from DMDS order to obtain significant deodorizing effect. EXAMPLE 7 Example 3 was repeated (flavoring vanillin), but 100 g DMDS sample B0replaced by 100 g DMDS with neolignans light fraction samples A0prepared in example 1. The obtained sample was designated as A1. A B0(DMDS, purified from volatile impurities, without odorants) odour composition And1from crude DMDS and vanilla. EXAMPLE 8 The experiment was carried out in accordance with methods described in example 7, but the vanilla was replaced by ethylvanillin. 8 members of the expert group chose the odor of the sample In0smell obtained in this sample (A2). EXAMPLE 9 The experiment was carried out in accordance with methods described in example 7, but the vanilla was replaced by menthol. The smell of pattern In members of the group are still preferred the smell obtained in this sample (A3). EXAMPLE 10 The experiment was carried out in accordance with methods described in example 7, but the vanilla was replaced by a mixture of perfumes specified in example 5. The obtained sample was denoted as a4. All 8 members of the Commission preferred the smell of composition B0the smell of the sample And4. EXAMPLE 11 The experiment was carried out in accordance with methods described in example 7, but the vanilla was replaced by a mixture of perfumes specified in example 6. The obtained sample was denoted as a5. The smell of sample B0members also prefer the smell of a sample And the5.
where each of R3and R4identical or different - possibly unsaturated linear, branched or cyclic hydrocarbon radical, comprising from 1 to 8 carbon atoms.
6. Composition under item 5, in which orthophthalate is diety is with 0.05% Solidaritate, 0.03% of 2-methylbutyrate, 0,02% benzoylacetate and 0.1% diethylacetamide.
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