Method of preparing catalyst for obtaining diesel fuel from raw material, which contains triglycerides of fatty acids

FIELD: chemistry.

SUBSTANCE: method consists in successive application on carrier - amorphous aluminium oxide - by method of soaking with following drying and annealing of: water solution of thermally unstable salt of element, selected from the first group, including titanium, tin, zirconium, then water solution of thermally unstable salt of element, selected from the second group, including molybdenum, tungsten, and after that water solution of thermally unstable salt of element, selected from the third group, including cobalt, nickel. Obtained catalyst contains, wt %: oxide of element from the first group - 4.2-15.0, oxide of element from the second group - 12.4-14.2, oxide of element from the third group - 2.1-3.8, remaining part - aluminium oxide. After that, catalyst is activated first by soaking in hydrogen medium at temperature 450-500C, pressure 5-8 MPa for 3-4 h, then sulfidation at temperature 250-300C, pressure 5-8 MPa for 3-4 h. And sulfidation is carried out with mixture of hydrogen sulfide and hydrogen with concentration of hydrogen sulfide 10-15 vol%.

EFFECT: method makes it possible to obtain catalyst, which has increased isomerisation ability and preserves catalytic activity with respect to reaction of isomerisation for long time, which results in obtaining Diesel fuel, which has improved low-temperature properties.

4 ex

 

The invention relates to the field of production of diesel fuel from a raw material containing triglycerides of fatty acids.

A known method of producing catalyst hydrodeoxygenation described in EN 2492922, 2013, including the impregnated alumina carrier, modified carbon coating, an aqueous solution of compounds of Mo and Ni, while preparing joint impregnating solution containing a Nickel salt molybdosilicic heteropolyacids, stable two - or dragonanime organic acids (oxalic, malonic, maleic, lactic, tartaric, succinic, citric), at pH environment of 2.0 to 3.0, and is a single vacuum impregnation of the carrier at a temperature of 40C followed by heat treatment at temperatures not higher than 130C. as compounds of molybdenum and Nickel can use Ni2[Ni(OH)6Mo6O18] or Ni3.5H2[NiMo9O32].

The disadvantage of this method is the low content of Lewis sites acid sites on the catalyst. Lisovskii acid sites catalyze isomerization reactions, and their low content leads to low content in the reaction products isoparaffinic and, as a consequence, poor low-temperature properties of the obtained product.

There is a method of preparation of the catalyst for p is taking diesel fuel from raw materials of natural origin, described in EN 2429909, 2011. The method consists in the impregnation of the original calcined material, crystalline silicoaluminate with tseolitopodobnogo type structure SAPO-31, a solution of the compound of metal of group VIII is platinum and/or palladium at a rate of not more than 10.0% of the mass. metal in the final product with subsequent drying and oxidation treatment. When the oxidative preparation is carried out at a temperature not exceeding 500C., preferably at a temperature of 400-450C, with a rate of temperature rise in the furnace above 20C/min, preferably 2-5C/min

The disadvantages of this method of preparation of the catalyst are low initial attitude from/n-paraffins in the reaction products is not more than 16%, and low stability of the catalyst side product of the reaction (water), which results in reducing the activity of the catalyst (after 102 hours of catalyst ratio from/n-paraffin does not exceed 13.4 per cent).

Closest to the invention is a method for preparing a catalyst for obtaining diesel fuel hydrodeoxygenation oxygen-containing aliphatic compounds like carboxylic acids, their esters and triglycerides, which is a complex composite containing transition metals supported on a carrier (EN 2356629, 2009). The specified catalyst was prepared by impregnation of the carrier with solutions of compounds m is the metal, followed by drying and termomaslyanym metal compounds. When applying multiple components impregnation of each component is carried out either sequentially or simultaneously with other components, application of a salt of the noble metal if necessary, conduct impregnation in capacity in the last turn, thermal decomposition of metal compounds is carried out after each impregnation or in an inert atmosphere at a temperature of 400-550C, followed by reduction with hydrogen at a temperature of 300-350C, or in an oxygen environment at a temperature of 400-550C, followed by reduction with hydrogen, either directly in the environment of hydrogen at a temperature of 300-350C. the resulting catalyst contains at least a noble metal in an amount of not more than 5.0% of the mass. or contains at least Nickel or copper, or iron, or a combination of both in restored form in an amount of not more than 54.7% of the mass. and, at least, transition metals, other than those listed above, in oxide form in an amount of not more than 40% of the mass.

The disadvantage of this method of preparation of the catalyst is low activity of the resulting catalyst in the reactions of hydroisomerization, which leads to a low content in the reaction products isoparaffinic and, as a consequence, poor low-temperature properties of the obtained product.

The task of the described method of preparation of the catalyst for dieseling the fuel from raw materials, containing triglycerides of fatty acids, is enhancing its effectiveness.

The task is achieved by the described method of preparation of the catalyst to obtain diesel fuel from vegetable raw materials by applying to the medium - amorphous aluminum oxide by impregnation and subsequent drying and calcination consistently aqueous solution of a thermally unstable salt of an element selected from a first group comprising titanium, tin, zirconium, and then aqueous solution of a thermally unstable salt of an element selected from a second group comprising molybdenum, tungsten, and then aqueous solution of a thermally unstable salt of an element selected from a third group including cobalt, Nickel, obtaining a catalyst containing, % mass.: oxide of an element of the first group of 4.2-15,0, the oxide of the element of the second group of 12.4-14.2 per cent, of oxide of the element of the third group of 2.1 to 3.8, the remainder alumina, followed by activation of the resulting first catalyst curing in an environment of hydrogen at a temperature of 450-500C, a pressure of 5-8 MPa, for 3-4 hours, then solifidianism at a temperature of 250-300C, a pressure of 5-8 MPa for 3-4 hours sulfatirovnie spend a mixture of hydrogen sulfide and hydrogen with the concentration of hydrogen sulfide 10-15% vol.

The technical result consists in obtaining catalysis is ora, with increased isomerizing ability and preserving the catalytic activity for the isomerization reactions for a long time, which leads, in turn, to receive diesel fuel with improved low-temperature properties due to the composition, enriched by the ISO, from raw materials containing triglycerides of fatty acids.

The described method is carried out as follows. The extrudate alumina with a specific surface area of 200-300 m2/g is impregnated with an aqueous solution of thermally unstable salt of an element selected from the group comprising titanium, tin, zirconium, and then dried and calcined at a temperature of 400-600C for 3-4 hours. When this Sol element is decomposed to the oxide of the element. Then spend the carrier impregnated with an aqueous solution of thermally unstable salt of an element selected from the group comprising molybdenum, tungsten, and then dried and calcined at a temperature of 400-600C for 3-4 hours. This is followed by impregnation with an aqueous solution of thermally unstable salt of an element selected from the group comprising cobalt, Nickel, and then dried and calcined at a temperature of 400-600C for 3-4 hours. Each of the procedures for the impregnation and calcination is carried out from one to three times depending on the desired concentration of the element in the catalysate is re. At the same time as thermally unstable salt of an element selected from the group comprising titanium, tin, zirconium is used, in particular, hydroxide, bis(ammoniacal)titanium (IV) nitrate Zirconia, sulfate, tin (IV); as thermally unstable salt of an element selected from the group comprising molybdenum, tungsten, used, in particular, ammonium molybdate, ammonium tungstate, as thermally unstable salt of an element selected from the group comprising cobalt, Nickel, is used, in particular, Nickel nitrate, cobalt nitrate. For all the above salts is sufficient compliance with the conditions of decomposition of the salt of the element at a temperature up to 600C, therefore, for the preparation of the catalyst it is possible to use other thermally unstable salts of these elements. After the final calcination, the content of oxides of the elements of the first group is 4.2-15.0% wt., oxides of elements of the second group and 12.4-14.2% of mass., oxides of elements of the third group is 2.1 to 3.8 wt. -%, the rest is aluminum oxide. This is followed by the activation of the catalyst in two stages. In the first stage, the catalyst is kept in the environment of hydrogen at a temperature of 450-500C, a pressure of 5-8 MPa within 2-3 hours. Then spend sulfatirovnie catalyst at a temperature of 250-300C, a pressure of 5-8 MPa for 3-4 hours sulfatirovnie spend a mixture of hydrogen sulfide and hydrogen with the concentration of hydrogen sulfide 10-15% vol.

Catalyst efficiency is determined as follows. The feedstock containing triglycerides of fatty acids (at temperatures above their melting temperatures), mixed with hydrogen, heated to a temperature of 300-400C and served in a flow reactor with a fixed bed of the catalyst prepared by the method described above. The volumetric feed rate of 0.6 to 1.0 h-1the pressure in the reactor 7-12 MPa, the ratio of hydrogen/feedstock 600-1500 nm3/m3. In the course of the processing flow, in particular, the hydrogenation reaction of hydrodeoxygenation, hydroisomerization. As a product of the formation of n-paraffins and ISO (from fatty acid included in the composition of raw materials), propane (from glycerin, part of the raw material) and water. The product is subjected to separation in a distillation column with getting diesel, gasoline and gaseous fractions and VAT residue. As raw materials you can use vegetable oils, animal fats, lipids, microorganisms, in particular algae, cyanobacteria, bacteria, and mixtures thereof.

Example 1.

Amorphous aluminum oxide by weight 20 g with a specific surface area of 200 m2/g is impregnated with an aqueous solution of tin sulfate concentration of 20 wt. -%, then dried and calcined for 4 hours at a temperature of 400C. then spend impregnation received the CSOs carrier with an aqueous solution of ammonium molybdate concentration of 20 wt. -%, then dried and calcined for 4 hours at 400C. the above procedure is performed 2 times. Then carry out the impregnation of the received carrier with an aqueous solution of cobalt nitrate concentration of 20 wt. -%, then dried and calcined for 4 hours at 400C. the catalyst containing 4.2% of tin oxide, 13.7% of molybdenum oxide, 2.4% of cobalt oxide, the rest is aluminum oxide. The catalyst was activated first with hydrogen at a temperature of 450C, a pressure of 5 MPa for 2 hours. Then sulfiderich a mixture of hydrogen and hydrogen sulfide concentration of hydrogen sulfide 10% about. at 250C, a pressure of 5 MPa for 3 hours.

Raw materials (coconut oil) containing triglycerides of fatty acids, mixed with hydrogen, heated to a temperature of 300C and served in a flow reactor with a fixed bed of the catalyst prepared by the method described above. The volumetric feed rate of 0.6 h-1the reactor pressure is 7 MPa, the ratio of hydrogen/feedstock 600 nm3/m3.

After separation of the products of the process of getting products yield, % wt.: 4,3 hydrocarbon gases, 5,2 gasoline fraction, 79,3 diesel fraction, 11.2 balance. The ratio of ISO/n-paraffins in the diesel fraction is 21.7% of the mass. at the initial period of operation of the catalyst and 20.3% of the mass. after 120 hours of operation.

Example 2.

And ifny alumina weight 53 g with a specific surface area of 300 m 2/g is impregnated with the aqueous solution of the hydroxide bis(ammoniacal)titanium (IV) a concentration of 50 wt. -%, then dried and calcined for 3 hours at a temperature of 600C. the above procedure is performed 3 times. Then carry out the impregnation of the received carrier with an aqueous solution of ammonium tungstate concentration of 20 wt. -%, then dried and calcined for 4 hours at a temperature of 600C. the above procedure is performed 2 times. Then carry out the impregnation of the received carrier with an aqueous solution of Nickel nitrate concentration of 20 wt. -%, then dried and calcined for 3 hours at 400C. the resulting catalyst contains 15.0% titanium oxide, 12.4% of tungsten oxide, 2.9% of Nickel oxide, the rest is aluminum oxide. The catalyst was activated first with hydrogen at a temperature of 450C, a pressure of 5 MPa for 2 hours. Then sulfiderich a mixture of hydrogen and hydrogen sulfide concentration of hydrogen sulfide 10% about. at 250C, a pressure of 5 MPa for 3 hours.

The feedstock (palm oil), contains triglycerides of fatty acids, mixed with hydrogen, heated to a temperature of 400C and served in a flow reactor with a fixed bed of the catalyst prepared by the method described above. The volumetric feed rate of 0.6 h-1the reactor pressure is 8 MPa, the ratio of hydrogen/feedstock 600 nm3/m3 .

After separation of the products of the process of getting products yield, % wt.: 7,6 hydrocarbon gases, 10,7 gasoline fraction, 77,2 diesel fraction, 4.5 balance. The ratio of ISO/n-paraffins in the diesel fraction is 20,3% of the mass. at the initial period of operation of the catalyst and 19.7% of the mass. after 120 hours of operation.

Example 3.

Amorphous aluminum oxide by weight of 46 g with a specific surface area of 200 m2/g is impregnated with an aqueous solution of tin sulfate concentration of 20 wt. -%, then dried and calcined for 3 hours at a temperature of 600C. the above procedure is performed 3 times. Then carry out the impregnation of the received carrier with an aqueous solution of ammonium molybdate concentration of 20 wt. -%, then dried and calcined for 3 hours at a temperature of 600C. the above procedure is performed 3 times. Then carry out the impregnation of the received carrier with an aqueous solution of cobalt nitrate concentration of 30 wt. -%, then dried and calcined for 3 hours at a temperature of 600C. the resulting catalyst contains 12.8% of the mass. tin oxide, 13.3% of the mass. molybdenum oxide, 3.8% of the mass. the cobalt oxide, the rest is aluminum oxide. The catalyst was activated first with hydrogen at a temperature of 500C, a pressure of 8 MPa for 3 hours. Then sulfiderich a mixture of hydrogen and hydrogen sulfide concentration of the second 15%vol. at a temperature of 300C, a pressure of 8 MPa in the course is e 4 hours.

Raw materials (coconut oil) containing triglycerides of fatty acids, mixed with hydrogen, heated to a temperature of 300C and served in a flow reactor with a fixed bed of the catalyst prepared by the method described above. The volumetric feed rate to 1.0 h-1the reactor pressure is 8 MPa, the ratio of hydrogen/feedstock 1500 nm3/m3.

After separation of the products of the process of getting products yield, % wt.: 3,2 hydrocarbon gases, 4,4 gasoline fraction, 82,1 diesel fraction, 10.3 balance. The ratio of ISO/n-paraffins in the diesel fraction amounts to 19.4% of the mass. at the initial period of operation of the catalyst and 18.8% of the mass. after 120 hours of operation.

Example 4.

Amorphous aluminum oxide weight 36 g with a specific surface area of 300 m2/g is impregnated with an aqueous solution of nitrate Zirconia concentration of 20 wt. -%, then dried and calcined for 4 hours at 400C. the above procedure is performed 2 times. Then carry out the impregnation of the received carrier with an aqueous solution of ammonium molybdate concentration of 20 wt. -%, then dried and calcined for 3 hours at a temperature of 600C. the above procedure is performed 3 times. Then carry out the impregnation of the received carrier with an aqueous solution of Nickel nitrate concentration of 15 wt. -%, then dried and calcined for 4 hours at temperature is 400C. The resulting catalyst contains 8.6% of zirconium oxide, 14.2% of molybdenum oxide, 2.1% of Nickel oxide, the rest is aluminum oxide. The catalyst was activated first with hydrogen at a temperature of 500C, a pressure of 8 MPa for 2 hours. Then sulfiderich a mixture of hydrogen and hydrogen sulfide concentration of the second 15% vol. in at a temperature of 300C, a pressure of 8 MPa for 3 hours.

The feedstock (palm oil), contains triglycerides of fatty acids, mixed with hydrogen, heated to a temperature of 400C and served in a flow reactor with a fixed bed of the catalyst prepared by the method described above. The volumetric feed rate to 1.0 h-1the reactor pressure is 7 MPa, the ratio of hydrogen/feedstock 1500 nm3/m3.

After separation of the products of the process of getting products yield, % wt.: 5,1 hydrocarbon gases, 7,1 gasoline fraction, 79,7 diesel fraction, 8.1 balance. The ratio of ISO/n-paraffins in the diesel fraction of 29.1% of the mass. at the initial period of operation of the catalyst and 27.2% of the mass. after 120 hours of operation.

Thus, the described method of preparation of a catalyst to obtain diesel fuel from vegetable raw materials allows to obtain a catalyst having high isomerizing ability and preserving the catalytic activity for the isomerization reactions during long the straps.

The preparation method of catalyst for receiving diesel fuel from a raw material containing triglycerides of fatty acids, by applying to the medium - amorphous aluminum oxide by impregnation and subsequent drying and calcination consistently aqueous solution of a thermally unstable salt of an element selected from a first group comprising titanium, tin, zirconium, and then aqueous solution of a thermally unstable salt of an element selected from a second group comprising molybdenum, tungsten, and then aqueous solution of a thermally unstable salt of an element selected from a third group including cobalt, Nickel, obtaining a catalyst containing, wt.%: the oxide of the element of the first group - 4,2-15,0, the oxide of the element of the second group - 12,4-14,2, the oxide of the third element group is 2.1 to 3.8 other - aluminium oxide, with subsequent activation of the resulting first catalyst curing in an environment of hydrogen at a temperature of 450-500C, a pressure of 5-8 MPa for 3-4 h, then solifidianism at a temperature of 250-300C, a pressure of 5-8 MPa for 3-4 h, and sulfatirovnie spend a mixture of hydrogen sulfide and hydrogen with the concentration of hydrogen sulfide 10-15 vol.%.



 

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11 cl, 4 dwg, 1 ex

FIELD: chemistry.

SUBSTANCE: invention relates to a method where at the first step, a starting mixture containing water vapour and oxygenates such as methanol and/or dimethyl ether is converted on a catalyst to olefins and said olefin mixture is separated on a separating apparatus into a stream rich in C1-C4 hydrocarbons and a stream rich in C5+ hydrocarbons. The stream rich in C5+ hydrocarbons is separated into a stream rich in C5- and C6- hydrocarbons and a petrol product stream rich in C7+ hydrocarbons, wherein the stream rich in C5- and C6- hydrocarbons is partially esterified with methanol and the obtained ester is added to the petrol product stream. The invention also relates to an apparatus for producing synthetic fuel.

EFFECT: low content of olefins in synthetic fuel.

14 cl, 1 dwg, 2 ex

FIELD: oil and gas industry.

SUBSTANCE: hydrofining method to obtain hydrocarbon compositions includes hydrofining of mixture that contains component (A) - gas oil in quantity from 20 up to 95 wt %; component (A1) - benzene in quantity from 1 up to 40 wt %; component (B) of biologic origin containing fatty acid esters, probably including freed fatty acids; quantity of biologic component is from 4 up to 60 wt %. Moreover all percent ratios are referred to total weight of all components. Hydrocarbon composition (C) has been also claimed; this composition can be used as propellant and/or fuel; it is obtained by hydrofining method; it has cetane number more than 50, density of 820-845 kg/m3, content of polyaromatic compositions less than 1 by wt % in regard to total weight of hydrocarbon compound and total content of polyaromatic compositions less than 20 be wt % in regard to total weight of the composition.

EFFECT: obtaining hydrocarbon composition with improved low-temperature properties.

39 cl, 4 tbl, 2 ex

FIELD: chemistry.

SUBSTANCE: method comprises the following basic operations. a) producing mixtures of fatty acid alkyl esters and glycerine by trans- esterification, starting from lipid-based vegetable or animal materials and from lower alcohols or bioalcohols in excess; b) separating the mixtures obtained from the said operation a) of trans-esterification into a phase based on raw glycerine and a phase containing said mixtures of fatty acid alkyl esters and the excess amount of lower alcohols or bioalcohols; the method being characterised by that said starting lipid-based vegetable or animal materials include one or more of the following ingredients: i) raw vegetable oil; ii) refined vegetable oil; iii) used edible oil and/or animal fats and by that said ingredients undergo the following preliminary treatment steps before said operation a) of transesterification: 1) said ingredient i), raw vegetable oil, is subjected to preliminary cleaning and refinement in order to remove impurities and to neutralise and fractionate the oil by cooling, and then drying the refined oil thus obtained; 2) said ingredient ii), refined vegetable oil, is subjected to preliminary drying; 3) said ingredient iii), used edible oil and/or animal fats, is subjected to a preliminary cleaning, drying and then esterification of the free fatty acids contained therein, by addition of lower alcohols or bioalcohols; the obtained product based on fatty acid alkyl esters is mixed in a proportion of not more than 20% with dried refined oil obtained from treatments 1) or 2) above. Said preliminary treatments are performed in corresponding three sections for preliminary treatment of material, said sections being used together or alternatively to each other. The invention also relates to a biofuel or biofuel mixture.

EFFECT: method is extremely flexible with respect to providing raw material and provides high flexibility with respect to applicability of the obtained product.

15 cl, 1 ex, 1 tbl, 3 dwg

FIELD: chemistry.

SUBSTANCE: gasoline mixture contains at least 20 vol. % isobutanol, where the volume ratio of the mixture, which evaporates at temperature of up to about 93C (200F), is at least 35 vol. %. The invention also relates to a method of producing said gasoline mixture.

EFFECT: obtaining a gasoline mixture having good cold start and warm-up driveability performance.

7 cl, 5 dwg

FIELD: chemistry.

SUBSTANCE: method of producing bio-oil fuel from lignocellulose material, the method comprising the following steps: (a) solvating hemicellulose from lignocellulose material using a solvent, (b) removing the solvated hemicellulose from the solid substance remaining after step (a); and (c) solvating lignin and cellulose from the solid substance remaining after step (a) using a solvent at reaction temperature of 180-350C and reaction pressure of 8-26 MPa, where the step (c) of solvating lignin and cellulose yields bio-oil.

EFFECT: improving use of the energy-producing potential of lignin and cellulose.

28 cl, 13 tbl, 6 dwg, 7 ex

FIELD: chemistry.

SUBSTANCE: invention relates to novel areas of using a certain type of diesel fuel component and methods of improving performance of a turbo charged diesel engine. In particular, the invention relates to use of a viscosity increasing component in a diesel fuel composition to improve acceleration performance, at low engine speeds from 1200 to 2200 rpm, of a turbo charged diesel engine into which the fuel composition is added or will be added, or a vehicle driven by said engine. The invention also relates to a method of operating a turbo charged diesel engine and/or a vehicle driven by such an engine, which involves feeding a diesel fuel composition, containing said viscosity increasing component, into the engine.

EFFECT: improved performance of a turbo charged diesel engine.

12 cl, 22 tbl, 3 ex

FIELD: chemistry.

SUBSTANCE: method of biodiesel production is realised by the re-etherification in mixing natural oil, alcohol and a catalyst and following separation of the target product. The method is characterised by the fact that at the first stage of the re-etherification iron sulphate (II) is applied as the catalyst, after which iron sulphate and precipitated glycerol are separated and the mixture of alcohol, oil and ethers of fatty acids are supplied to the second stage of the re-etherification, at which as the catalyst used is an enzyme - lipase, immobilised on the surface, after which glycerol and the enzyme catalyst are separated and the mixture of alcohol and biodiesel is directed to a stage of the target product separation.

EFFECT: method makes it possible to simplify the process of the re-etherification reaction and increase the completeness of the reaction process.

6 cl, 1 tbl

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