Method of producing dimethyl sulphide |
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IPC classes for russian patent Method of producing dimethyl sulphide (RU 2457029):
 Prodrug 1,3-diamino-2-hydroxypropane derivatives / 2357962
Invention relates to the compounds of the formula
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.
 The method of obtaining single-ended diallyldisulfide / 2223265
The invention relates to a method for producing an asymmetrical diallylsulfide General formula (1): R1-S-S-R2(1) where R1=CH3C2H5n-C4H9, R2=n-C6H13the h8H17the h9H19
 A method for production of alkyl - or alkylalkoxysilane / 2220134
The invention relates to a method for producing alkyl - or alkylalkoxysilane, which can serve as extractants of noble metals, flotation reagents, additives in oils, and can be used as starting compounds for the production of biologically active compounds, alkyl - or alkylalkoxysilane interaction of the corresponding mercaptan with alkyl - or alkenylphenol in the presence of an alkaline agent
 Composition based on dimethyl disulfide / 2219168
The invention relates to a composition based on dimethyl disulfide (DMDS)
 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
 Method of producing methylmercaptan / 2394023
Present invention relates to a continuous method of producing methylmercaptan which is a valuable organic synthesis intermediate product. The proposed method involves obtaining methylmercaptan through contact of a thoroughly mixed mixture of oxides of carbon, sulphur or hydrogen sulphide and hydrogen at high temperature and pressure in the presence of a moulded solid catalyst which contains K2MoO4 as an active component, an active promoter, where the active promoter is a mixture of oxides or a mixture of sulphides or a mixture of sulphides and oxides of metals selected from a group consisting of iron, cobalt, nickel, lanthanum, cerium and manganese and optionally a carrier.
 Catalysts containing halide-containing tungstates of alkali metals for synthesis of alkylmercaptans and preparation methods thereof / 2384364
Invention relates to a catalyst which contains a tungstate of an alkali metal containing at least one halide, where the alkali metal component is selected from a group comprising Cs, Rb or the alkali metal component implies a combination of two bonded alkali metals selected from a group comprising a) potassium and caesium, b) sodium and caesium, c) rubidium and caesium, in ratio not equal to 1:1. Also disclosed is a method of preparing a supported catalyst containing a tungstate of an alkali metal and a method of producing alkylmercaptans.
 Method for synthesis of 3-(methylthio)propanal and 2-hydroxy-4(methylthio)butane nitrile / 2383531
Invention relates to a method for synthesis if 3-(methylthio)propanal and 2-hydroxy-4-(methylthio)butane nitrile through a catalytic reaction for respectively bonding methylmercaptan to acrolein and hydrocyanic acid to 3-(methylthio)propanal. In the said methods, the catalyst is heterogeneous, does not dissolve in the reaction medium and has formula (I)
 Method of activating catalyst for producing fluorine-containing hydrocarbons / 2449832
Invention relates to a method of activating a catalyst for producing fluorine-containing hydrocarbons via gas-phase hydrofluorination of halohydrocarbons. The catalyst contains chromium (III) oxide and an aluminium (III) compound, whose content ranges from 2 to 15 wt % in terms of Al2O3, and additionally contains a metal compound, where the metal Me is selected from either iron or nickel or cobalt or zinc or copper or magnesium any mixture in amount of 0.1-1.5 wt % in terms of oxides. The activation process is carried in four steps: a) drying the catalyst in a current of nitrogen at temperature 100-200°C and atmospheric pressure; b) treating the catalyst with difluorochloromethane (R-22) at temperature 300-370°C and atmospheric pressure; c) treating the catalyst with a mixture of hydrogen fluoride and nitrogen at temperature 340-370°C and atmospheric pressure, while gradually increasing hydrogen fluoride concentration in the mixture with nitrogen to 100 mol %; d) treating the catalyst with hydrogen fluoride at temperature 340-370° and pressure of up to 0.4 MPa.
Catalyst for dehydrogenation of c3-c5 paraffin hydrocarbons, method of producing said catalyst and method for dehydrogenation of c3-c5 paraffin hydrocarbons / 2448770
Invention relates to catalysts for dehydrogenation of paraffin hydrocarbons and methods of producing said catalysts, as well as methods of producing olefin hydrocarbons via catalytic dehydrogenation of corresponding C3-C5 paraffin hydrocarbons and can be used in chemical and petrochemical industry. Described is a catalyst for dehydrogenation of C3-C5 paraffin hydrocarbons, which contains chromium and potassium oxides and optionally zirconium dioxide, deposited on a solid solution of formula ZnxAl2O(3+x) where x=0.025-0.25, with a defective spinel structure. Described is a method of producing the catalyst by hydrating a precursor of the solid solution, saturating with a mixture of solutions of chromic acid, potassium chromate and a zinc salt and optionally zirconyl nitrate, followed by drying and calcination in air, wherein hydration is carried out during the saturation process. A method of dehydrogenating paraffin hydrocarbons in the presence of said catalyst is also described.
Catalyst for dehydration of paraffin hydrocarbons and method of its application / 2432203
Invention relates to chemical and petrochemical industries and may be used for heterogeneous-catalytic reactions, in particular, dehydration of paraffin hydrocarbons. Proposed catalyst comprises aluminium oxide the precursor of which is the product of thermochemical activation of hydrargillite, chromium oxide, alkaline metal oxide, and is formed in thermochemical activation of hydrargillite together with compounds of chromium and alkaline metal. Note here that catalyst comprises oxides of iron, calcium and magnesium in weight ratio Fe:Ca:Mg (in terms of oxides) equal to 0.3:1.0:0.1, formed in thermochemical activation from compounds of iron, calcium and magnesium in the following ratio of components in wt % (in terms of oxides): chromium oxide (in terms of Cr2O3) - 10.0-16.0, alkaline metal oxide - 1.2-2.0, sum of oxides of iron, calcium and magnesium - 0.05-1.5, aluminium oxide making the rest. Invention covers also method of using described catalyst for dehydration of paraffin hydrocarbons wherein mix of said catalyst with fluoaluminic catalyst "ИМ"-2201 of the following composition (in wt %) is used: chromium oxide - 13.0-14.3; alkaline metal oxide - 2.8-3.3; silicon oxide - 9.5-10.5; sum of oxides of iron, calcium and magnesium - 1.2, aluminium oxide making the rest in ratio of 1:9 to 1:1, respectively.
 Catalyst, preparation method thereof and method of decomposing chlorine-containing hydrocarbons / 2431525
Invention relates to heterogeneous catalysis. Described is a catalyst for decomposing chlorine-containing hydrocarbons or mixtures thereof, containing dispersed active particles of nickel attached to carbon fibres with diameter 0.1-0.4 mcm. Described also is a method of preparing the described catalyst, characterised by that the starting raw material for preparing said catalyst is solid articles made from nickel, for example in form of a tape, wire etc, and pairs of halogen-substituted hydrocarbons in a mixture with hydrogen are used to mould dispersed active particles from solid metal articles. Described also is a method of decomposing chlorine-containing hydrocarbons or mixtures thereof, involving catalytic conversion of thereof into carbon, hydrogen chloride and hydrogen in the presence of the described catalyst.
 Catalyst, method of its preparation and method of fluorinating halogenated hydrocarbons / 2431524
Invention relates to chemical industry, namely, to catalysts to be used in gas-phase fluorination of halogenated hydrocarbons. Proposed catalyst comprises chromium oxides, the main component, in amount of approx. 95-80 wt % wherein chromium oxidation corresponds to atomic ratio O/Cr varying from 1.6 to 2.0, and additional components of Me metal compounds selected from the group including: Al(III), Fe(III), Co(II), Ni(II), Zn(II), Mg(II) or whatever mix thereof in amount of 0.01-15.0 wt % in terms of oxides comprising water in amount of not over 3.0 wt %, anion admixtures, e.g. C, NO3 -, SO4 2- in amount of not over 0.15 wt %, carbon in amount of 0.5-5.0 wt %. It features shape of cylindrical granules with diameter of 3-10 mm, hardness of 5-40 kg/cm2, bulk density of 0.4-0.8 g/cm3, specific surface of 50-250 m2/g, pore volume making at least 0.3 cm2/g, and single-mode distribution of pore sizes in the range of 200-500 Е. Invention covers also method of producing above described catalyst and method of fluorinating halogenated hydrocarbons using said catalyst.
 Catalytically inactive heat generator and perfected dehydration / 2428250
Invention relates to perfected system of layer of catalyst for dehydration in olefins production using traditional processing technologies. Catalyst layer system comprises dehydration catalyst including the following separate components bonded together a) active component selected from metal oxide of group VI and substrate selected from aluminium oxide, alumina, aluminium oxide monohydrate, aluminium oxide trihydrate, aluminium oxide-silicon oxide, aluminium apha-oxide; b) first inert material with high density and heat capacity, not capable of heat release in cyclic nonoxidising dehydration, and c) secondary component containing heat generating material and carrier suitable for application of heat release inert material thereon. Note here that said secondary material is catalytically inert to dehydration and side reactions and generates heat when subjected to reduction or regeneration. Method of adiabatic nonoxidising dehydration comprising: preparation of above described system, conduction of cyclic process, forcing raw material flow of aliphatic hydrocarbon into catalyst layer system for dehydration, dehydration of said flow, blowing through by steam and regeneration of catalyst layer.
 Method of producing olefin oligomerisation catalyst system and olefin oligomerisation method / 2412002
Invention relates to production of chromium-containing catalyst systems and use thereof in synthesis of hydrocarbons, specifically an olefin oligomerisation method. Described is a method of producing a catalyst system for trimerisation or oligomerisation of olefins, involving a step for mixing a chromium source, a nitrogen-containing ligand and alkyl aluminium in a common solvent in which alkyl aluminium is exposed to microwave radiation when producing the catalyst system. The invention also describes a method for trimerisation or oligomerisation of an olefin compound containing 2-30 carbon atoms per molecule and at least one terminal olefin double bond, involving a trimerisation or oligomerisation step in the presence of the catalyst system obtained using the method described above.
 Method of activating chromium-containing catalysts / 2410157
Described is a method of activating a chromium-containing industrial catalyst for polymerisation of olefins, involving a firs step for treatment of the catalyst which includes a time for first increase in temperature to a first required value higher than 400°C, maintaining the first temperature for a first holding period at least greater than 0; at least a second step for treatment of the catalyst which includes a time for second increase in temperature to a second required value and maintaining the second temperature for a second holding period at least greater than 0, in which the second temperature is higher than the first, the common activation cycle is less than 20 hours, and the activated catalyst contains 40% or more conversion to chromium (+6). The invention also describes a method of activating a chromium-containing industrial catalyst for polymerisation of olefins, involving at least 2 steps, in which step 1 involves instant addition of catalyst to a medium pre-heated to a first temperature between approximately 400°C and approximately 700°C, while maintaining the first temperature for approximately 1-20 hours, followed by step 2 which involves raising temperature to a second temperature value between approximately 800°C and 900°C for a period of time less than or equal to 3 hours and maintaining the second temperature for approximately 1-10 hours, where the method is realised periodically or continuously, and a method of increasing efficiency of activating an industrial chromium-containing catalyst for polymerisation of olefins, involving: instantaneous treatment of the catalyst at temperature of approximately 800°C in a first atmosphere of nitrogen or carbon oxide; maintaining temperature for not less than approximately 15 minutes; replacing the first atmosphere with anhydrous air; and maintaining temperature for an additional period of time. Described also is a method for speeding up activation the industrial chromium-containing catalyst for polymerisation of olefins, involving raising temperature of the catalyst to a first temperature lower than or equal to 800°C for less than 10 minutes and maintaining the first temperature for less than or equal to 3 hours and then raising temperature to a second temperature value in less than 15 minutes and maintaining the second temperature for less than 10 hours, where the second temperature is higher than the first, and the activation method is less than 15 hours long overall.
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FIELD: chemistry. SUBSTANCE: 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. EFFECT: high efficiency of the process of producing dimethyl sulphide. 12 ex, 1 tbl
The invention relates to methods for sulfur-containing compounds, specifically to dimethyl sulfide, is used as the odorant and the source of raw material for the synthesis of dimethyl sulfoxide, which is used as a drug, solvent, extractant. Available and cheap raw materials for the synthesis of dimethyl sulfide may be dimethyl disulfide produced in large quantities when cleaning gases from mercaptans. When gas-phase decomposition of dimethyl disulfide in a nitrogen atmosphere, with a small admixture of hydrogen at a temperature of 200°C, contact time 0.06-0.12 C in the presence of aluminum oxide, pure or modified sulfides of Nickel, cobalt, molybdenum, cobaltmolybdenum or michelwolverine conversion of dimethyl disulfide 35-45% dimethyl sulphide is formed with selectivity 22-44% (US 5493058, B01J 27/043, SS 321/04, SS 319/06, 20.02.1996). The disadvantage of this method is the low selectivity of the formation of dimethyl sulfide. In the presence of a catalyst containing 10.0-18.5 wt.% sulfide of cobalt supported on alumina, at atmospheric pressure, the temperature 200-330°C, feed rate of 50-250 mmol of dimethyl sulfide per hour per 1 g of catalyst selectivity for dimethyl sulphide equal 44-56% (of the Russian Federation No. 2368418, B01J 21/04, SS S/14, 37.09.2009). The disadvantage of this method is the low selectivity for dimethyl sulphide. Most near them to the technical nature of the invention is a method of producing dimethyl sulfide conversion of dimethyl disulfide in the presence of a catalyst (70% gamma + 30% hee-phase aluminum oxide), at atmospheric pressure and a temperature of 250-400°C with the addition to the reaction mixture of methanol in the amount of 0.17-0.82 g per 1 g of dimethyl disulfide. When the conversion of the disulfide 70-91% selectivity for dimethyl sulfide is 66-95% (of the Russian Federation No. 2402529, SS 321/04, 27.10.2009. The disadvantage of this method is low productivity, which is 0.8-19.8 mmol of dimethyl sulfide per hour per 1 g of catalyst. The objective of the invention is to provide a method of producing dimethyl sulfide, which allows to obtain the dimethyl sulfide with a high performance. The task is solved in that the receipt of dimethyl sulfide from dimethyl disulfide is carried out in an environment of helium at atmospheric pressure, at a temperature of 300-380°C with the addition to the reaction mixture of methanol, in the presence of a catalyst, which is used as the oxide of chromium (Cr2O3)incurred in the amount of 0.73-7.3 wt.% on gamma-alumina (γ-Al2O3). The catalyst prepared according to the patent of the Russian Federation 2032664, 10.04.1995 impregnation on the capacity of gamma-alumina in an aqueous solution of chromic anhydride, followed by drying at a temperature of 100-110°C. and calcining in a stream of dry air at a temperature of 490-510°C. According to IKS-research on the catalyst surface IG2About3/γ-Al2About3contains the main centers of moderate strength and acid centers - strong the roton, strong Lisovskii acid centers of the ions of aluminum A13+and average power from ions of chromium, in the form of a solid solution of chromium with the carrier and dispersed chromium oxide, which is proved by the methods of x-ray analysis, electron microscopy and high resolution temperature-programmed recovery. Under the action of these active centers dimethyl disulfide decomposes communication S-S with the formation of Metacity groups (CH3S), but the conversion of methanol leads to the appearance on the surface metaxylene groups (CH3O). The catalyst is prepared by impregnation capacity of gamma-alumina in an aqueous solution of chromic anhydride, followed by drying at a temperature of 100-110°C. and calcining in a stream of dry air at a temperature of 490-510°C. Dimethyl sulphide is produced by transformation of a mixture of dimethyl disulfide with methanol in the presence of the oxide catalyst (chromium oxide (CR2About3)incurred in the amount of 0.73-7.3 wt.% on gamma-alumina γ-Al2About3), at atmospheric pressure, the temperature of 300-380°C, the weight ratio of methanol and dimethyldisulfide 0.8-0.9 g/g, when the contact time is preferably 0.1-0.35 C. According to IKS-research on the catalyst surface IG2About3/γ-Al2About3contains strong proton, lisowska acid sites and the basic price is ture moderate strength. Under their influence dimethyl disulfide decomposes communication S-S with the formation of Metacity groups (CH3S), but the conversion of methanol leads to the appearance on the surface metaxylene groups (CH3O). Involving acid-base centers, a surface complex, including CH3S and CH3O-group. Decomposition of this intermediate are dimethyl sulfide and water: (CH3)2S2+2CH3HE=2(CH3)2S+2H2O The combination of acid-base centers optimum strength and ease of methoxylation surface with methanol provide high performance formation of dimethyl sulfide in the catalytic decomposition of dimethyl disulfide in the presence of methanol. Synthesis of dimethyl sulfide is carried out at atmospheric pressure in a flow setup. Helium from a balloon with a certain velocity is passed through the temperature-controlled fountain offering - the first with dimethyl disulfide, and the second with methanol. A mixture of dimethylsulfide, methanol and helium at a ratio of 0.8-0.9 g of methanol per 1 g of dimethyl disulfide at a certain temperature comes filled with catalyst reactor, heated instantaneous oven. The reactor is connected via castigados faucet with chromatograph LHM-MD. Periodically (every 45 minutes) using the two-way tap selected sample is gazoobraznykh products for analysis. The results of the analysis to calculate the conversion of dimethyl disulfide, the product yield and selectivity of the formation of dimethyl sulfide in % relative output of dimethyl sulfide to the conversion of dimethyl disulfide. The contact time in seconds equal to the ratio of the amount of catalyst (in cm3to gas flow rate in cm3/s at room temperature and atmospheric pressure. The invention is illustrated by the following examples. Example 1 The catalyst composition of 0.73 wt.%. CR2About3/Al2About3prepared by impregnation of the carrier by capacity. To do this, 98.5 g of γ-Al2About3impregnated with a solution containing 1.46 g of chromic anhydride (SGAs3) in 100 ml of distilled water. The mixture was kept in air for 12 h, then dried at T=100-110°C for 5 hours and Then the catalyst is placed in a heated furnace reactor and calcined in a stream of dry air at T=500°C for 5 hours Through the catalyst at atmospheric pressure, T=350°C, contact time is 0.53 with miss helium, a mixture of dimethyl disulfide with methanol containing 0.81 g of methanol per 1 g of dimethyl disulfide. Conversion of dimethyl disulfide is 85%, the selectivity to dimethyl sulfide 91%, the productivity of the process 11.4 mmol of dimethyl sulfide per hour per 1 g of catalyst. Example 2 The catalyst composition is 1.5 wt.% rsub> 2About3/Al2About3prepared analogously to catalyst according to example 1, except that 97 g of aluminum oxide impregnated with a solution containing 3.0 g SGAs3in 116 ml of distilled water, and calcined in air flow at T=490°C for 5 hours Through the catalyst pass the mixture under the same conditions as in example 1, except that the contact time is 0.25 s, the ratio of methanol to dimethyl disulfide 0.90 g/year Conversion of dimethyl disulfide 88%, the selectivity to dimethyl sulfide 93%, the productivity of the process is equal to 27.2 mmol of dimethyl sulfide per hour per 1 g of catalyst. Example 3 The catalyst composition of 2.2 wt.% CR2About3/Al2About3prepared analogously to catalyst according to example 1, except that 95 g of aluminum oxide impregnated with a solution containing 4.4 g SGAs3in 114 ml of distilled water, and calcined in air flow at T=510°C for 5 hours Through the catalyst pass the mixture under the same conditions as in example 1, except that the contact time is equal to 0.15 and the ratio of methanol and dimethyl disulfide equal to 0.85 g/year Conversion of dimethyl disulfide 86%, the selectivity to dimethyl sulfide 93%, the productivity of the process is equal to 43.0 mmol of dimethyl sulfide per hour per 1 g of catalyst. Example 4 The catalyst composition of 4.4 wt.% CR2About3/Al2About 3prepared analogously to catalyst according to example 1, except that 91 g of aluminum oxide impregnated with a solution containing 8.7 g SGAs3in 140 ml of distilled water. Through the catalyst pass the mixture under the same conditions as in example 1, except that the contact time is equal to 0.13, the ratio of methanol and dimethyl sulfide 0.80 g/year Conversion of dimethyl disulfide 80%, the selectivity to dimethyl sulfide 97%, the productivity of the process is equal to 44.8 mmol of dimethyl sulfide per hour per 1 g of catalyst. Example 5 The catalyst composition of 7.3 wt.% CR2About3/Al2About3prepared analogously to catalyst according to example 1, except that 85 g of aluminum oxide impregnated with a solution containing 14.6 g SGAs3in 103 ml of distilled water. Through the catalyst pass the mixture under the same conditions as in example 1, except that the contact time is equal to 0.17 and the ratio of methanol and dimethyl disulfide is equal to 0.82. Conversion of dimethyl disulfide 90%, the selectivity to dimethyl sulfide 86%, the productivity of the process is equal to 35.0 mmol of dimethyl sulfide per hour per 1 g of catalyst. Example 6 The catalyst composition of 14.6 wt.% CR2About3/Al2About3prepared analogously to catalyst according to example 1, except that 71 g of aluminum oxide impregnated with a solution containing 29. g SGAs 3in 85 ml of distilled water. Through the catalyst pass the mixture under the same conditions as in example 1, except that the contact time is equal to 0.18 and the ratio of methanol and dimethyl disulfide is equal to 0.87. Conversion of dimethyl disulfide 96%, the selectivity to dimethyl sulfide 84%, the productivity of the process is equal to 27.6 mmol of dimethyl sulfide per hour per 1 g of catalyst. Examples 7-12 Similar to example 3 is repeated with the difference that the catalyst calcined at T=500°C and through it pass the mixture of dimethyl disulfide with helium with the addition of 0.80-0.90 g of methanol, 1 g of dimethyl disulfide, the contact time is 0.05-0.55 and temperature 280-380°C. Examples 1 and 6 show that the decrease of the content in the catalyst CR2About3less than 1.5 wt.% and the increase above 7.3 wt.% reduces the performance of the process. Example 7 shows that with decreasing temperature below 300°C is not reached significant effect of improving the performance of the process. Example 10 illustrates that when the contact time is less than 0.1 with at and achieve high performance dimethyl sulfide, but conversion of dimethyl disulfide low. Thus, compared with the results of the prototype the proposed method allows for an increase in 3-14 times the performance of the process of obtaining dimethyl sulfide due to add and to the reaction mixture of methanol and use as a catalyst of chromium oxide, put in the number of 0.73-7.3 wt.% on gamma-alumina.
A method of producing dimethyl sulfide conversion of dimethyl disulfide in the presence of methanol using an oxide catalyst at atmospheric pressure, the temperature of 300-380°C, characterized in that the use of catalyst containing 0,73 of 7.3 wt.% chromium oxide Cr2O3and gamma-aluminum oxide - the rest, the weight ratio of methanol to dimethyl disulfide is 0.8-0.9 g/g, the contact time of 0.1 to 0.35 C.
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