Synthesis of multi-purpose self-adjusting catalyst of oxidation cracking of organic raw material and its application

FIELD: oil and gas industry.

SUBSTANCE: synthesis method of multi-purpose self-adjusting catalyst for liquid-phase low-temperature oxidation cracking of organic raw material, including natural biomass, is described, and it consists in the fact that iron salt FeCl3 x 6H2O is dissolved in water containing lower alcohol in concentrations required for formation of colloid system capable of peptisation, at heating up to the temperature not exceeding 100°C and constant mixing so that suspension of colloid solid particles of iron oxides containing organic impurities is obtained. The above suspension can change its activity depending on type of organic raw material and oxidiser, and at cracking of natural biomass and in case the latter represents lignine or lignine-containing biomass it has properties of ferments in relation to lignine. Method of liquid-phase low-temperature oxidising cracking of organic raw material, including natural biomass, in presence of catalyst at atmospheric pressure is described. At that, air oxygen and/or hydrogen peroxide is used as oxidiser and the above catalyst is used as catalyst.

EFFECT: high-activity catalyst of liquid-phase oxidising cracking.

8 cl, 7 dwg, 11 ex

 

The invention relates to the field of synthesis of materials, which are used as catalysts for the oxidative cracking of organic raw materials, namely the method of production of new forms of catalysts based on iron compounds for oxidative cracking of organic compounds and lignin-cellulosic biomass and other sources of natural materials.

Organic oxygen-containing compounds are valuable products and intermediates in organic synthesis. Until recently, the main ways of their industrial production was processes, the implementation of which occurred with the use of such reagents as manganese dioxide, permanganate and bichromate of potash, nitric and sulfuric acid, lye and When the stoichiometric oxidation of use massive amounts of expensive and toxic, oxidizing agents, and inevitably there are problems associated with the disposal of toxic waste.

The most promising catalytic methods for obtaining oxygen-containing compounds, based on the use as oxidant molecular oxygen and hydrogen peroxide, as both oxidant are environmentally friendly and inexpensive. Although the cost of hydrogen peroxide is higher than the cost of the oxygen in the small-capacity processes thin on the organic synthesis of the first oxidant is often preferable, since the cost of technological equipment for the oxidation of H2O2in General lower than for oxidation, which is usually carried out at elevated temperatures and pressures [R.A.Sheldon, J.Dakka. Heterogeneous catalytic oxidations in the manufacture of fine chemicals. Catalysis Today 19(1994) 215].

In nature, wood residues and most difficult to chemically breaking down the lignin is converted by microorganisms, which for the development and reproduction of necessary water containing metal ions /[1] T.K. Kirk in Microbial Degradation of Organic Compounds. V.13 (ed. Gibson D.T.) 399-438 (Marcel Dekker, Inc., New York, 1984).

[2] Boeran W., Ralph j, Baucher M., Lignin biosynthesis. Annu. Rev. Plant Biol. 54, 519-549 (2003).

[3] W. Flaig Effects of microorganins in the transformation of lignin to humic substances. // Geohim. Cosmochim. Acta - 1964, - Vol.28, - pp.1523-1535.

[4] T. K Kirk, R L Farrell Enzymatic "combustion": the microbial degradation of lignin. Annu Rev Environ. 1987; 41:465-505.

[5] P J Kersten, T.K.Kirk. Involvement of a new enzyme, glyoxal oxidase, in increasing interest among H2O2production by Phanerochaete chrysosporium. J Bacteriol. 1987 May; 169(5):2195-2201/.

The method of preparation of the catalyst and method of liquid-phase oxidation of organic compounds described in the patent of the Russian Federation 2229930. These methods are most similar to the proposed method of synthesis of the catalyst and its application. The method of preparation of known catalyst includes the process of formation of two phase titanium-silicate metastructuring materials. In the first phase, comprising preparing a mixture containing Polo is sustained fashion the charged complexes of silicon, adding compounds of titanium and adding surface-active substances (SAS) (the order of mixing is arbitrary), maintain pH in the range of 0.5 to 1.5. The second phase will cover the introduction of a portion of the alkaline solution so that the pH of the reaction mixture was maintained in the range from 1.5 to 7.0, and then the mixture is subjected to hydrothermal treatment, after which powdered solid product is separated by filtration, washed, dried and calcined. The method of liquid-phase oxidation of organic compounds, such as 2,3,6-trimethylphenol, using the obtained catalyst is carried out at a low temperature, for example 80°C., by adding the solid catalyst obtained above, acetonitrile and aqueous solution of hydrogen peroxide.

The disadvantage of this method of synthesis catalyst of liquid-phase oxidation of organic compounds is the presence of several stages of the process, the use of many components, including costly, the need to support the pH of the reaction mixture within a certain range of values, the need for filtering, washing, drying and calcination, which increases the time of preparation of the solid catalyst and its value.

The disadvantages of this method of liquid-phase oxidation is that in the oxidation of organic compounds found in the reactions is authorized mixture in a slurry form, as well as the great weight of catalyst relative to the weight of oxidizable organic compounds, and comprising tens of percent.

The present invention is to develop a one-step synthesis of a new high-level multi-function self-tuning catalyst for oxidative cracking of organic raw materials, including natural biomass, with different catalytic and physico-chemical characteristics, using cheap reagents, and the use of this catalyst in the processing of both liquid and solid forms.

According to the present invention offers a method for the synthesis of multifunctional self-tuning catalyst for low-temperature liquid-phase oxidative cracking of organic raw materials, including natural biomass, which is dissolved or suspended salt of iron in water containing a surface-active substance (surfactant), usually selected from a lower alcohol and a lower organic acid, at concentrations required for the formation capable of peptization of the colloidal system, when heated to a temperature not exceeding 100°C, and constant stirring. The result is a colloidal suspension of solid particles of iron oxide containing organic impurities, which has FPIC is the institutional capacity to modify their activity - to configure itself depending on the type of organic feedstock and oxidant and has the properties of enzymes in the cracking of natural biomass containing lignin. As iron salts used FeCl3×6H2O, and as a surfactant use ethyl alcohol and the process is conducted at a temperature of 65°C and stirring for 15 minutes. When it is desired concentration of alcohol, and salts of iron, necessary for formation capable of peptization of the colloidal system is 10 ml/l and 0.05 g/l, respectively.

When using the suspension of the salt in a small amount of water usually add another, miscible with water, the liquid, such as ethyl alcohol in a large volume with subsequent sedimentation of particles in this alcohol solution, when mixed with a small volume of aqueous suspensions.

The invention also relates to a multifunctional catalyst, obtained in the conditions described above for the oxidative cracking of organic raw materials, including natural biomass, using as oxidant oxygen and/or hydrogen peroxide. When this catalyst, as research has shown, comprises a solid colloidal particles of iron oxides mainly in the form of several crystalline phases and molecules of alcohol and/or fragments thereof as organic impurities.

The invention also apply the method of liquid-phase low-temperature oxidative cracking of organic raw materials, including natural biomass in the presence of a catalyst at atmospheric pressure.

The difference of the proposed method against known is that as the catalyst using the above multi-function self-tuning catalyst obtained under conditions as described above, and the process is conducted at temperatures in the range from 20 to 80°C using as oxidant oxygen and/or hydrogen peroxide.

As organic raw materials can be used, for example, lemon, olive oil, peat, and natural biomass use biomass containing lignin. At the same time, the used catalyst in the cracking in respect of the lignin contained in the biomass, exhibiting the properties of the enzyme.

The advantage of the proposed method for the synthesis of the catalyst of liquid-phase oxidation of hydrocarbons is only one stage of making and using cheap reagents. However, depending on the weight proportions of iron salt/surfactant/water achieved by obtaining catalysts of oxidative cracking with various catalytic and physico-chemical characteristics, which allows for cracking, leading to a different composition of products in different reaction media from water to hydrocarbon. Thus to lainnya particles of the catalyst accelerates the reaction of oxidative cracking when replacing the water environment on alcohol and hydrocarbon, and when applied to the surface, for example, a glass substrate, depending on the environment type catalysts are changing the type of process that is manifested in form of, for example, radical and molecular types of catalysis, and chemical composition of the oxidant depending on the chemical composition of the environment, for example in aqueous suspensions as oxidant is hydrogen peroxide, and alcohol and hydrocarbon and molecular oxygen. Using the catalyst obtained according to the present invention, allows for the oxidation of lignin in the lignin-cellulosic biomass, such as sawdust, straw, etc., at low temperatures. Because in nature the cracking of lignin at low temperatures is carried out by enzymes secreted by the fungi (for example, Polystictus versicolor, Panus Tigrinus 8/18), the proposed catalyst exhibits properties similar to those of natural enzymes.

The advantages of the proposed method of liquid-phase oxidation of organic materials is the possibility of use as oxidizable organic matter insoluble in water or other liquids, solid particles of organic materials (wood, straw etc) of large enough size (units and tens of millimeters), and the use for these purposes, the proposed catalyst amount (mass %) sostav the ment of 0.001 to 0.5% by weight of organic raw materials.

Oxidation of lignin in the lignin-cellulosic biomass using hydrogen peroxide and the proposed catalyst leads to the production of pulp and valuable organic, easily recyclable substances and is the preferred process than the currently used processes using acid and alkali, resulting in huge amounts of troublesome and hazardous waste. The mechanism of the enzymatic oxidative cleavage involving hydrogen peroxide and oxygen. Thus, the catalyst of the present invention simulates natural enzymatic processes of decomposition of organic natural materials. Oxidation of limonene by oxygen by using a catalyst allows to obtain valuable products for pharmacology.

The synthesis of the catalyst of the present invention carried out by the following method.

In water at a temperature, for example 65°C, containing the additive of surface-active substances (surfactants), such as ethyl alcohol in an amount of 10 ml/l, add some salt of iron, such as FeCl3×6H2O, in concentrations sufficient for the formation of colloidal particles due to the peptization, for example, 0.05 g/L. the Mixture was kept before the formation of solid colloidal particles with constant stirring, for example for 15 minutes. Then, the resulting suspension is used in which the quality of the catalyst. Evidence of the formation of colloidal particles is the sedimentation process, allowing, for example, to concentrate the colloidal particles in small volumes of water. Water can be almost completely replaced by another, mixing with the water liquid, such as ethyl alcohol, by mixing small amounts of water suspension with large amounts of alcohol with subsequent sedimentation of particles in this alcohol solution. The size of colloidal particles, the degree of crystalline order, their catalytic activity depends on the ratio of FeCl3×6H2O/ethanol/water and temperature peptization.

Obtaining catalysts, the size of colloidal particles and their crystal structure as the examples shown in figure 1-4, where it is shown made with a transmission electron microscope pictures of catalyst particles, prepared by peptization of the particles in the mixture FeCl3×6H2O/ethanol/water at a temperature of 65°C for different ratios of the components of the mixture.

Figure 1 shows a picture of the catalyst particles obtained by the method of transmission electron microscopy, and bottom right is listed the total scale, and the scale bars. The catalyst is prepared at a temperature of 65°C and the ratio of FeCl3×6H2O/ethanol/water, equal to 0.14 g/8 ml/800 ml

Figure 2 shows Directi is fair picture of the catalyst particles, obtained by the method of powder diffraction plot with a diameter of 20 μm. The catalyst is prepared at a temperature of 65°C and the ratio of FeCl3×6H2O/ethanol/water, equal to 0.14 g/8 ml/800 ml Diffraction pattern corresponds to the crystals of alpha-Fe2O3with the possible impurity phases crystals FeO cubic system.

Figure 3 shows a picture of the catalyst particles obtained by the method of transmission electron microscopy, and bottom right is listed the total scale, and the scale bars. The catalyst is prepared at a temperature of 65°C and the ratio of FeCl3×6H2O/ethanol/water, is 0,014 g/8 ml/800 ml

Figure 4 shows the XRD pattern of the catalyst particles obtained by the method of powder diffraction plot with a diameter of 20 μm. The catalyst is prepared at a temperature of 65°C and the ratio of FeCl3×6H2O/ethanol/water, is 0,014 g/8 ml/800 ml Diffraction pattern corresponds to the crystals of alpha-Fe2O3having dimensions in the range of 2-3 nm. Blurred due to the small size of the crystals diffraction peaks allow the presence of impurities crystals of Fe3O4the cubic system crystals and beta-Fe2O3.

Figure 5 shows the spectrum of the infrared transmittance of the solid oxidation product of sawdust pine (upper curve (solid line) and the range of infrared sample of cotton cellulose (lower curve (dashed line).

Figure 6 shows an example of the spectrum of x-ray fluorescence sample of catalyst

Analysis of the composition of the catalyst by x-ray fluorescence analysis showed that the catalyst contains, besides iron and oxygen impurity carbon in amounts greater than the oxygen content, which suggests that the molecules of alcohol and/or fragments thereof comprised in significant amounts in the catalyst composition.

The study of colloidal particles showed that the type of crystals can be different. In two cases (laboratory of Moscow state University and Institute of crystallography) the main type of crystals were found crystals of alpha-Fe2O3the cubic system with admixtures of other phases, too, the cubic system. In one case, the particles on the basis of the diffraction pattern was attributed to the composition of Fe3O4and orthorhombic symmetry and the impurity crystals of Fe(OH)3the presence of crystals of the cubic system was rejected, the color of the particle - red did not meet the crystals of Fe3O4with black color. In all three cases received the same information about the particle size.

Considering the obtained results it can be assumed that the sample is formed by colloidal particles mainly alpha-Fe2O3because the particles are red or red-brown color that matches the crystals of the LLF-Fe 2O3bright red color mixed with crystals of Fe(OH)3brown color, whereas the crystals of Fe3O4have black color. But this is not to say that in the crystalline structure of the catalyst particles always have a cubic crystal system and represent alpha-Fe2O3. This is because the crystallographic library data comparisons are given for large crystals, and the particles may have a distorted crystal lattice due to the small size of 1-2 nm, therefore, the use of library data is not completely correct. You can say that the particles consist of several crystalline phases and the proximity of the crystal parameters to some massive crystal.

While numerous data on the composition obtained by x-ray fluorescence analysis, clearly suggest that the particles are in comparable quantities of Fe, O and C, which probably represents a molecule of alcohol or its fragment. The presence of carbon may also distort the crystal structure. Figure 6 shows an example of the spectrum of x-ray fluorescence sample of the catalyst, it is seen that there are the strong lines of Fe, O, C - tens of percent. This means that the main composition contains iron, oxygen and carbon in status is ve alcohol. The elements S, Cl in this sample and other samples Si, Zn, Ca, are as random impurity concentration of the order of fractions of a percent and not essential for the catalytic properties.

Examples of the application of catalyst

Example 1.

Oxidation of sawdust pine (rough grinding, the particle size 1-3 mm)

The catalyst was prepared with a ratio of ethanol: FeCl3×6H2O=31 and peptization temperature of 65°C.

Oxidation of 4.3 g of sawdust hydrogen peroxide (6 g) was carried out at 60°C in 100 ml of water for 5 hours; the content of the catalyst based on Fe3+was 0,058%.

Conversion of solids 51%, the oxidation products are water - soluble acid (0.03 mol), simple and complex esters; the solid product is cellulose with a mixture of lignin, spent 100% of hydrogen peroxide.

Example 2.

Oxidation of sawdust pine (coarse grind. 1-3 mm)

The catalyst was prepared with a ratio of alcohol: FeCl3×6H2O=42 and peptization temperature of 70°C.

Oxidation of 3.2 g of sawdust hydrogen peroxide (5.9 g) was carried out at 60°C in 100 ml of water for 5.5 h, the content of the catalyst based on Fe3+was 0.04%, the content of lignin in the original substance was 27%.

Conversion of solids 56%, dissolved in water oxidation products are water - soluble acid (0.03 mol), simple and complex esters obtained is the result of the reaction, the solid - cellulose with lignin content is not more than 0.3%; spent 87% of hydrogen peroxide.

Example 3.

Oxidation of sawdust pine (coarse grind. 1-3 mm)

The catalyst was prepared with a ratio of alcohol: FeCl3×6H2O=42 and peptization temperature of 60°C.

Oxidation of 8 g of sawdust hydrogen peroxide (4.6 g) was carried out at 60°C in 100 ml of water for 17 hours; the content of the catalyst based on Fe3+was 0.04%.

Conversion of solids 36%, the solid oxidation product has a gray color characteristic of cellulose, the analysis of the infrared transmission spectra of the sample shows that he is a cellulose, similar to cotton cellulose, with a possible admixture of aromatic compounds, spent 99% of hydrogen peroxide.

Figure 5 shows the spectrum of infrared transmittance obtained in the experiment of the solid residue of the reaction, and the range of infrared transmittance of a sample of cotton cellulose.

Example 4.

Oxidation of sawdust pine (grinding. <0,5×0,5×0,5 mm3)

The catalyst was prepared with a ratio of alcohol: FeCl3×6H2O=40 and peptization temperature of 65°C.

Oxidation of 9.1 g of sawdust hydrogen peroxide (18 g) was carried out at 60°C in 300 ml of water for 8 hours; the content of the catalyst based on Fe3+was 0,042%. Conversion of solids 56%, solid OST the talk cellulose, cellulose acetate mixed with polycyclic acids and esters, lignin content in the solid residue does not exceed 0.5%; water-soluble oxidation products is a mixture of acids (0.13 mol), hemicellulose, polysaccharides, complex and ethers; spent 100% of hydrogen peroxide.

Example 5.

Peat oxidation

The catalyst was prepared with a ratio of alcohol: FeCl3×6H2O=138 and peptization temperature 650°C;

Oxidation of 4.5 g of peat hydrogen peroxide (1.25 g) was carried out at 60°C in 200 ml of water for 7 hours; the content of the catalyst based on Fe3+was 0.0052%.

Conversion of solids 70%, the solid residue of cellulose with carboxylic groups; water-soluble oxidation products is a mixture of acids, carboxycellulose, simple and complex esters; spent 100% of hydrogen peroxide.

Example 6.

Oxidation of olive oil (the solid residue after receipt of olive oil) (powder with dimensions of 0.2×0.2 to×0.2 mm3)

The catalyst was prepared with a ratio of alcohol: FeCl3×6H2O=51 and peptization temperature of 60°C.

Oxidation of 8 g of olive pulp with hydrogen peroxide (7.2 g) was carried out at 60°C in 100 ml of water for 35 hours; the content of the catalyst based on Fe3+was 0.022%.

Conversion of solid matter 30%spent 92% of hydrogen peroxide.

Example 7.

Oxidation of the who technical lignin.

The catalyst was prepared with a ratio of alcohol: FeCl3×6H2O=480 and peptization temperature of 70°C.

Oxidation of 4.5 g of lignin by hydrogen peroxide (5 g) was carried out at 60°C in 100 ml of water for 8 hours; the content of the catalyst based on Fe3+was 0,0026%.

Conversion of lignin 22,2%, the oxidation products are water - soluble acid (0.014 mol), ethers; spent 68.4% of hydrogen peroxide.

Example 8.

Oxidation of technical lignin

The catalyst was prepared with a ratio of alcohol: FeCl3×6H2O=100 and peptization temperature of 60°C.

Oxidation of 4.5 g of lignin by hydrogen peroxide (4.5 g) was carried out at 60°C in 100 ml of water for 5 hours; the content of the catalyst based on Fe3+was 0,027%.

Conversion of lignin 33%, the oxidation products are water - soluble acid (or 0.027 mol), ethers and esters; spent 63% of hydrogen peroxide.

Examples o catalyst

Example 9.

Oxidation of limonene - natural olefin (1 methyl-4 Isopropenyl-cyclohexen)

The catalyst was prepared with a ratio of alcohol: FeCl3×6H2O=178 and the peptization temperature of 70°C.

Oxidation of a 15%solution of limonene in the tetrachloride with oxygen was carried out at 60°C for 2.5 hours; compared the oxidation without catalyst and with catalyst, the content of which in terms of Fe3+was the 2·10 -5M/4 ml or 0,0062%.

Without catalyst, the conversion of 0.15%, the oxidation product - limonene hydroperoxide; catalyst: conversion of 1%, the oxidation products are alcohol and ketone (carvon) - valuable products for perfumes. The catalyst in the first 20 minutes the reaction was adsorbiroval on the glass wall of the reactor and the acceleration of the conversion occurred in the conditions of interaction of the reaction mixture with an immobilized on the glass wall of the catalyst.

During the reaction twice (80 min and 180 min) were added to portions of the acceptor radical 2.2"-bis[2-(n-dimethylaminophenyl)indan-1,3-dion (Limpisuree, Dagroove, Animalorigin, Oticaine. Kinetic model for the oxidation of limonene, Izv. Academy of Sciences, Ser. chem., 2008, No. 1, pp. 80-86) with the aim of becoming inactive connection radicals that are produced during the reaction. In both cases, there was complete cessation of absorption of oxygen at 25 and 40 min depending on the concentration of the acceptor, after passing these time intervals the rate of absorption of oxygen returned to their previous values.

Example 10.

Oxidation of natural palm oil

Palm oil contained 1,1·10-3M β-carotene and α-tocopherol - 1,1·10-2M α-tocopherol is a strong antioxidant and effective acceptors radicals.

The catalyst was prepared with a ratio of alcohol: FeCl3×6H2O=132 and peptization temperature of 70°C.

About Islena oil oxygen was carried out at 60°C for 5 hours; compared the oxidation without catalyst and with catalyst, the content of which in terms of Fe3+was 0.3%.

Without catalyst, the conversion of palm oil was 0%, with catalyst: conversion of 0.1%, the oxidation products - mainly alcohols. The content of inhibitors of radical oxidation of β-carotene and α-tocopherol did not change, which means that the oxidation is not a radical mechanism similar enzymatic reactions in the presence of monooxygenase.

Example 11.

The preparation of the catalyst: to 600 ml of tap water at a temperature of 70°C was added 6 ml of 96% ethanol and 0,084 g of salt FeCl3×6H2O, a mixture of 20 minutes was stirred.

The conditions of reaction: oxidation of 8 g of pine sawdust with a catalyst obtained by the hydrolysis of 0,084 g of salt FeCl3×6H2O, and hydrogen peroxide in the amount of 1.5 g was carried out at 60°C in 400 ml of water for 10 hours with constant stirring. After 10 hours the whole of the hydrogen peroxide was consumed (see figure 1, curve 1). In the drawing, the abscissa is the time (min); ordinate is the concentration of hydrogen peroxide (H2O2- M (mol·liter-1). The kinetics of consumption of hydrogen peroxide was characterized by a high rate in the first 250 minutes of the process and a slower speed at a late stage.

In the reaction in water FASEB dissolved form emerged oxidation products of biomass, containing functional group, HE, -C-OH, -C(O)OH, C=O, typical for organic surface-active agents (surfactants). As the main oxidation product registered D-glyceric aldehyde (H-C(O)-CH(OH)-CH2OH) and cellulose acetate.

Was prepared with a new portion of the catalyst: to 600 ml of tap water at a temperature of 70°C was added 0,084 g of salt FeCl3×6H2O, a mixture of 20 minutes was stirred.

The conditions of the reaction: suspension with the catalyst obtained by the hydrolysis of 0,084 g of salt FeCl3×6H2O, and 2.8 g of hydrogen peroxide was added to the reaction mixture obtained after the reaction for 10 hours.

The kinetics of consumption of hydrogen peroxide in the case of the catalyst obtained by the hydrolysis of 0,084 g of salt FeCl3×6H2O without adding alcohol to the solution, was characterized by low speed at an initial stage and a sharp increase in the rate of late-stage process (see figure 1, curve 2). All the amount of hydrogen peroxide was consumed after 8 hours.

The aqueous phase of the reaction mixture after 8 hours contained mainly Glyoxylic acid.

At this stage of the experiment, it was shown that for the preparation of the catalyst can be use D-glyceric aldehyde and organic surfactants, contain oxygen.

To verify communication between Akti is the activity of the catalyst and the method of its preparation process of oxidative cracking was continued.

The preparation of the catalyst: to 600 ml of tap water at a temperature of 70°C was added 6 ml of 96% ethanol and 0,084 g of salt FeCl3×6H2O, a mixture of 20 minutes was stirred.

The conditions of the reaction: suspension of catalyst particles obtained by the hydrolysis of 0,084 g of salt FeCl3×6H2O adding alcohol to the solution, and 1.5 g of hydrogen peroxide were added to the reaction mixture obtained after the reaction. The kinetics of consumption of hydrogen peroxide was similar to the kinetics registered to begin the process of oxidative cracking: high speed in the first 250 minutes of the process and a slower speed at a later stage (see Fig.7, curve 3). All the amount of hydrogen peroxide was consumed in 8 hours.

The weight of the dry solid residue amounted to 1.98 g (25% of the original weight of sawdust).

The experiment shows that the activity of the catalyst depends on the type of surfactant and ethanol is one of the representatives of the organic substances contain carbon, hydrogen and oxygen.

Clarification of the concept of "self-configuring catalyst

More than 25 years ago Gscom was suggested catalysts as self-tuning systems, in which the stationary state of the catalyst surface is formed during the catalytic process. This fundamental is th idea on the one hand, stimulated much experimental and theoretical work in the field of heterogeneous catalysis, and has required the development of a fundamentally new experimental approach to the study of heterogeneous contacts during catalysis methods in situ (Vev "Lomonosov readings", Ser. "Chemistry", Moscow, 20-26 April, 9 (2000)).

Shown in the application example 10, demonstrate the property of the catalyst to self-control. The oxidation of palm oil in a hydrophobic environment (example 10) the dispersion and colloidal dissolution of the catalyst was carried out thanks to the presence of oil private surfactants (phospholipids, mono - and diacylglycerol). In this example, it is shown that the oxidation of the oil with colloidal catalyst can be used as an oxidant dissolved oxygen, not hydrogen peroxide, as in the other examples, where the oxidation was carried out in the aquatic environment.

The concept of adaptability is illustrated in examples 1-8 (water + hydrogen peroxide + biomass) and examples 9, 10.

These examples show that the catalyst prepared according to the same scheme, being placed in a different environment - water, palm oil (with its surfactant), citric in carbon tetrachloride (without surfactant), directs the oxidation process by different mechanisms depending on the environment and oxidant:

a) in the aquatic environment what about the radical-molecular mechanism using hydrogen peroxide as oxidant;

b) on the molecular mechanism (example 10 palm oil) using gaseous oxygen as the oxidant; the dispersion and colloidal dissolution of the catalyst is carried out thanks to the presence of oil private surfactants (phospholipids, mono - and diacylglycerol);

in) free radical (example 9 oxidation of limonene in carbon tetrachloride) with the generation of free radicals and also using gaseous oxygen as the oxidant.

Thus, the catalyst being placed in different liquid environments, provides oxidation due to different mechanisms, i.e. its oxidative activity is retained due to a change in the oxidation mechanism. This can be called self-adjustment, because the catalyst was prepared according to the same scheme.

Clarification of the concept of "multifunctional catalyst"

The proposed catalyst performs several functions:

a) - catalyzed decomposition of hydrogen peroxide with the formation of active radicals and partially with oxygen;

b) - catalyzed oxidative cracking of biomass of different nature in water (examples 1-8);

- activation of gaseous molecular oxygen and its connection to palm oil; lack of spending inhibitor of free-radical oxidation in oil - tocopherol indicates Nera is ically molecular mechanism of fixation of oxygen in the oil.

d) free-radical oxidation of limonene by molecular oxygen in the solution of carbon tetrachloride (example 9).

The oxidation straw hydrogen peroxide is a radical mechanism of catalysis, and the iron oxides are partially dissolved and transferred in ionic form, and then in the form of oxalates of iron - catalysts. The application did not mention it because, in our opinion, there are plenty of examples 1-10 to show the versatility (use of several types of oxidizers) and simonetripodi (change of catalysis mechanism depending on the environment).

By definition, catalysis means speeding up the process. Known catalysts tied to any environment: enzymes are active only within a narrow pH range and temperature and only in the aquatic environment, catalytic oil cracking synthesis lose activity in the presence of water and dissolved metals, etc. of the Catalyst prepared in a certain way, loses its activity during the transition, for example, from hydrophilic liquid to hydrophobic (water to oil oil). In our case the catalyst in different environments with different oxidants on the form (gas, liquid), and composition (oxygen, hydrogen peroxide) performs the function of oxidation of polymers and macromolecules (cellulose, lignin), molecules of a small mass - lemon, m the SLA. Moreover, the oxidation catalyst (example 10) is selectivity in the composition of palm oil is oxidized oil, but not tocopherol and carotene - organic molecules, known acceptors radicals and oxidation inhibitors (carotene - provitamin a, tocopherol - vitamin E).

1. The method of synthesis of multifunctional self-tuning catalyst for low-temperature liquid-phase oxidative cracking of organic raw materials, including natural biomass, which consists in the fact that the dissolved iron salt FeCl3·6H2O in water containing a lower alcohol, at concentrations required for the formation capable of peptization of the colloidal system, when heated to a temperature not exceeding 100°C., and stirring to obtain a suspension of colloidal solid particles of iron oxide containing organic impurities, which has the ability to alter their activity depending on the type of organic feedstock and oxidant, and when the cracking of natural biomass and when the latter is lignin or lignin-containing biomass, has the properties of enzymes in relation to lignin.

2. The method according to claim 1, characterized in that as the lower alcohol use ethyl alcohol and the process is conducted at a temperature of 65°C and stirring for 15 minutes

3. The method according to claim 1 or 2, distinguished by the different topics the concentration of alcohol and iron salts, necessary for formation capable of peptization of the colloidal system is 10 ml/l and 0.05 g/l, respectively.

4. Multi-function self-tuning of the catalyst, obtained in the conditions according to any one of claims 1 to 3, for the oxidative cracking of organic raw materials, including natural biomass using as oxidant oxygen and/or hydrogen peroxide.

5. The catalyst according to claim 4, containing colloidal particles of iron oxides in the form of several crystalline phases and molecules of alcohol and/or fragments thereof as organic impurities.

6. The method of liquid-phase low-temperature oxidative cracking of organic raw materials, including natural biomass, in the presence of a catalyst at atmospheric pressure, characterized in that as the oxidant use oxygen and/or hydrogen peroxide as the catalyst use multi-function self-tuning catalyst according to any one of claims 4 or 5, and the process is conducted at a temperature of from 20 to 80°C.

7. The method according to claim 6, characterized in that as organic raw materials use lemon, olive oil, peat.

8. The method according to claim 6, characterized in that the quality of the natural biomass use lignin or biomass containing lignin, for example lignosellus m is cel, while the catalyst in the cracking against lignin has the properties of enzymes.



 

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15 cl, 8 dwg, 3 tbl, 6 ex

FIELD: textile, paper.

SUBSTANCE: method includes chopped straw impregnation in a reactor and maceration with aqueous solutions of sodium hydroxide with concentration of 20-30 g/l in a unit of Na2O at the temperature of 30-80°C. The method is carried out at the ratio of the solution weight to the dry chopped straw equal to 7:1. The impregnated chopped straw is maintained at the specified temperature for 30 min. The leaking liquid phase is extracted. Heated water is added to the mass, the mass temperature is increased up to 96°C, and boiling is executed at this temperature for 2 hours and 30 min.

EFFECT: higher yield of cellulose, reduced duration of process, its simplification and reduction of power inputs.

1 dwg, 1 tbl

FIELD: machine building.

SUBSTANCE: device for continuous bleaching cellulose containing semi-finished products consists of vertical hollow container of "pipe-in-pipe" type, of receiving unit, of bleaching unit, of flush unit and of unloading unit. The receiving unit is made in form of a loading element, a cutting-off or rotary gate and a pneumatic chamber with a branch connected with a pulsator. The pneumatic chamber is connected with the bleaching unit. The bleaching unit is made in form of a rotating internal pipe with orifices in its lower part. Also, a mixing device is secured along whole length of external surface of the internal pipe. The mixing device corresponds to a screw-type of a spiral-type band, or a rod, or blades. The flush unit is made as an external pipe with a bottom. The pipe is stationary fixed on a foundation. In the middle part of the pipe there is made a branch, while in a lower part there are made a process hatch and a branch. The unloading unit corresponds to a coaxial hollow cylinder attached to the external pipe; the cylinder has two bottoms. An internal bottom has orifices and is connected with an off-take chute. A branch withdrawing spent fluid is attached to an external bottom. Inside the coaxial hollow cylinder there is installed a device for target product wringing and unloading. This device is equipped with at least one scraper (s) in form of a rod(s) rigidly attached with its one end to the internal pipe. On another end the rod has a blade(s) with controlled angle of incline.

EFFECT: increased operational reliability of device.

4 cl, 2 dwg

FIELD: textile, paper.

SUBSTANCE: method includes two stages of rice straw boiling. The first boiling stage is carried out in the alkaline medium with subsequent separation of cellulose-containing product, the second stage of boiling is carried out in the acid medium by mixture of peracetic acid (PAA), acetic acid and hydrogen peroxide in presence of a stabiliser, such as a mixture of organic phosphonates. At the same time the second stage of boiling is carried out in presence of ozone with a flow rate of 2-4 g/hr.

EFFECT: reduced flow of composition based on PAA, higher yield of finished product, reduced content of lignin and increased whiteness indices.

2 cl, 1 tbl

FIELD: textile, paper.

SUBSTANCE: method includes two stages of rice straw boiling. The first boiling stage is carried out in the alkaline medium with subsequent separation of cellulose-containing product, the second stage of boiling is carried out in the acid medium by mixture of peracetic acid (PAA), acetic acid and hydrogen peroxide in presence of a stabiliser, such as a mixture of organic phosphonates. At the same time the second stage of boiling is carried out in presence of ozone with a flow rate of 2-4 g/hr.

EFFECT: reduced flow of composition based on PAA, higher yield of finished product, reduced content of lignin and increased whiteness indices.

2 cl, 1 tbl

FIELD: textile, paper.

SUBSTANCE: method includes two stages of rice straw boiling. The first boiling stage is carried out in the alkaline medium with subsequent separation of cellulose-containing product, the second stage of boiling is carried out in the acid medium by mixture of peracetic acid (PAA), acetic acid and hydrogen peroxide in presence of a stabiliser, such as a mixture of organic phosphonates. At the same time the second stage of boiling is carried out in presence of ozone with a flow rate of 2-4 g/hr.

EFFECT: reduced flow of composition based on PAA, higher yield of finished product, reduced content of lignin and increased whiteness indices.

2 cl, 1 tbl

FIELD: textile, paper.

SUBSTANCE: in accordance with preferable versions of this invention realisation, method and device are provided for continuous production of cellulose mass from suspension produced from ground hard wood, by means of its treatment at the first stage of boiling under conditions sufficient to reduce content of syringice acid (s-ligning) in hard wood compared to content of guaiac ligning in it (g-ligning), and subsequent treatment of suspension of ground hard wood at the second stage of boiling under conditions sufficient to reduce content of g-lignin that remain in it after the first stage of boiling.

EFFECT: reduced amount of cellulose mass wastes with specified Kapp number.

18 cl, 2 dwg, 1 ex

FIELD: textile, paper.

SUBSTANCE: in accordance with preferable versions of this invention realisation, method and device are provided for continuous production of cellulose mass from suspension produced from ground hard wood, by means of its treatment at the first stage of boiling under conditions sufficient to reduce content of syringice acid (s-ligning) in hard wood compared to content of guaiac ligning in it (g-ligning), and subsequent treatment of suspension of ground hard wood at the second stage of boiling under conditions sufficient to reduce content of g-lignin that remain in it after the first stage of boiling.

EFFECT: reduced amount of cellulose mass wastes with specified Kapp number.

18 cl, 2 dwg, 1 ex

FIELD: textile, paper.

SUBSTANCE: in accordance with preferable versions of this invention realisation, method and device are provided for continuous production of cellulose mass from suspension produced from ground hard wood, by means of its treatment at the first stage of boiling under conditions sufficient to reduce content of syringice acid (s-ligning) in hard wood compared to content of guaiac ligning in it (g-ligning), and subsequent treatment of suspension of ground hard wood at the second stage of boiling under conditions sufficient to reduce content of g-lignin that remain in it after the first stage of boiling.

EFFECT: reduced amount of cellulose mass wastes with specified Kapp number.

18 cl, 2 dwg, 1 ex

FIELD: oil and gas production.

SUBSTANCE: invention refers to procedure for cracking heavy fractions of oil. The procedure consists in thermal treatment of source raw stock in an active zone by exposure it to high frequency plasma. In volume of the active zone there is generated high frequency plasma with intensity 0.05÷0.2 Wt·cm2·and value of plasma carrier frequency from 106 Hz to 108 Hz. Raw stock is subjected to preliminary heating before treatment in the active zone. According to another version of the procedure low frequency plasma with intensity 0.05÷0.2 Wt·cm2 and value of plasma carrier frequency from 102 Hz to 105 Hz is generated in volume of the active zone; and raw stock is subjected to preliminary heating before treatment in the active zone. The invention also refers to the plasma reactor for cracking heavy fractions of oil and heavy oil residues.

EFFECT: increased efficiency of processing source raw stock, including heavy hydrocarbons, into motor fuel; increased depth of treatment of source raw stock due to maximal area of plasma contact with vapour-gas phase of raw stock; reduced power consumption per unit of product.

8 cl, 1 tbl, 2 dwg

FIELD: oil and gas production.

SUBSTANCE: here is disclosed procedure for processing oil containing fractions. The procedure consists in thermal cracking the fractions out of a source liquid phase at atmospheric pressure and in production of finish products out of generated gaseous substance. The procedure also consists in exposure of source raw stock to generated magnetic field, and in successive separation of gaseous substance to condensed liquid and non-condensed vapour-like constituents. In the procedure there is used alternate and rotating magnetic field. It influences treated volume of liquid phase directly during thermal cracking in a cavity of the cracking unit. Processed volume proper functions as a connecting link locking magnetic flow in used circuit. Also, intensity of alternate magnetic field is measured in thickness of layers present in the unit of treated oil containing fractions and equals to 1×104 ÷ 1×106 a/m; the range of frequencies of applied magnetic field is within limits 40-70 Hz; temperature of their heating is within the range 45°-65°C, while time of processing is 0.06-0.18 hours. Also, here is disclosed the device for processing oil containing fractions. The device consists of the cracking unit designed for holding volumes of source raw stock and of a unit for extraction of finish products. The latter includes a tank-accumulator, a refluxer-distiller for cooling and condensation of gaseous substance produced at cracking, and a source of heat power supply for heating treated raw stock to specified process temperature. The device further consists of a generator of magnetic field electrically coupled with an external power source. The generator produces alternate rotating magnetic field in volume of treated raw stock corresponding to the locking connecting link in the applied magnetic system of specified frequency and intensity. The generator corresponds to a closed circuit consisting of interconnected magnetic-conducting plates, in bodies of which there are arranged three electric windings of a coil each connected to one of phases of an external three-phase power source supplying alternate electric current. Notably, one set of plates, generating magnetic circuit, has a through slot wherein there is positioned the cracking unit proper containing processed oil fractions.

EFFECT: processing oil and its heavy constituents to light oil products at low power expenditures, simple process and embodiment; implementation of procedure at low capital cost and short period of preproduction.

2 cl, 3 ex, 1 dwg

FIELD: oil and gas production.

SUBSTANCE: here is disclosed procedure for extraction of hydrocarbons out of hydrocarbon containing stock, such as coal, boghead coal, pyro-shale, oil-bearing sand rock, natural bitumen, bituminous rock, and residual oil products. The procedure consists in contacting said stock with carbon dioxide. Also, modes of overcritical and pre-critical states of CO2 are alternately changed. Owing to that, the process of extraction progresses at lower pressure within the range of 55-90 at and temperature in the range of 20-40°C. The process is characterised with higher selectivity to hydrocarbons dissolution.

EFFECT: processing stock with low contents of hydrocarbons and increased efficiency of complex treatment of hydrocarbon containing stock.

3 ex, 1 dwg

FIELD: oil and gas production.

SUBSTANCE: here is disclosed system for processing hydrocarbons produced out of oil. The system consists of a unit for catalytic cracking, where into there are supplied hydrocarbons produced out of oil and wherein there are particles of catalyst, in essence, of uniform dimension in a fluidised state. Coke is deposited on particles of catalyst. Further, the system consists of a reducing reactor for regeneration of mixture out of catalyst particles and particles of metal oxide used as oxygen carriers. Present particles of metal oxide have in essence similar dimension, but different from dimension of catalyst particles. The reducing reactor is fed with solid fuel and catalyst particles with deposited coke. Solid fuel and coke are combusted in the reactor to ensure regeneration of catalyst particles further directed to the unit for catalytic cracking. The system includes an oxidising reactor where oxygen carrier is oxidised. Oxygen carrier circulates between the reducing and oxidising reactors.

EFFECT: reduced expenditures for trapping carbon dioxide and for production of steam generating electric power.

15 cl, 1 dwg

FIELD: oil and gas production.

SUBSTANCE: invention refers to procedure for catalytic conversion of hydrocarbons. The procedure consists in contacting source hydrocarbons with catalyst of hydrocarbon conversion to ensure reaction of catalytic cracking in a reactor. Further, products of reaction are withdrawn from the reactor and are divided into fractions to produce light olefines, gasoline, diesel fuel, heavy diesel fuel and other saturated low-molecule hydrocarbons. Also, catalyst of hydrocarbons conversion contains (of total weight of catalyst): 1-60 % wt of mixture of zeolite, 5-99 % wt of heat-resistant non-organic oxide and 0-70 % wt of clay. Mixture of zeolite contains (from total weight of mixture): 1-75 % wt of beta-zeolite modified with phosphorus and transition metal M, 25-99 % wt of zeolite with MF-structure and 0-74 % wt of zeolite of large pores. Waterless chemical composition of beta-zeolite modified with phosphorus and transition metal M is of the following kind: (0-0.3)Na2O·(0.5-10)Al2O3·(1.3-10)P2O5·(0.7-15)MxOy·(64-97)SiO2 (in brackets there are indicated wt percents of oxides) where transition metal M is one or several metals chosen from a group consisting of Fe, Co, Ni, Cu, Mn, Zn and Sn; x is number of atoms of transition metal M, and y is number ensuring valence corresponding to a degree of transition metal M oxidation.

EFFECT: increased conversion of hydrocarbons of oil and higher output of light olefines, particularly, propylene.

17 cl, 43 ex, 8 tbl

FIELD: oil and gas production.

SUBSTANCE: invention refers to procedure improving fluidity characteristics of hydrocarbon stock. The procedure consists in division of hydrocarbon stock to the first and second raw stock flows, and in processing the first stock flow possessing at least one property out of density number in degrees of API below 18, viscosity above 10000 sCt (38°C) and chilling temperature above 20°C. Further, the procedure consists in cracking the first stock flow with fresh catalyst, thus forming cracking flow and dead catalyst and in regenerating dead catalyst with production of fresh catalyst, in recirculation of the said fresh catalyst; and in mixing at least part of cracking flow with the second stock flow. The invention also refers to the unit for realization of the procedure improving fluidity characteristics of hydrocarbon raw stock.

EFFECT: oil product with good fluidity characteristics such as low chilling temperature, high density in degrees of API and low viscosity.

9 cl, 4 ex, 9 tbl, 2 dwg

FIELD: oil and gas production.

SUBSTANCE: invention refers to procedure for production of heavy oil. The procedure consists in mixing material containing heavy oil with solvent including bio-diesel, in forming mixture and in dividing mixture into a phase of solvent enriched with heavy oil and into a residual phase of sand. Also, the invention refers to another procedure for production of heavy oil.

EFFECT: production of hydrocarbons and mixtures of hydrocarbons such as heavy oil.

13 cl, 6 ex, 5 dwg

FIELD: chemistry.

SUBSTANCE: invention relates to a method of producing light olefins, involving bringing starting material - hydrocarbon oil into contact with a conversion catalyst in a catalytic conversion reactor having one or more reaction zones for conducting the reaction, where the starting material in form of hydrocarbon oil undergoes catalytic conversion in the presence of an inhibitor, and reagent vapour which arbitrarily contains the inhibitor is removed from coke deposited on the catalyst, and the desired article, which contains ethylene and propylene, is obtained by separating reagent vapour. The catalyst is separated from coke and restored for reuse in the reactor, where the ratio of the inhibitor to the starting material is 0.001-15 wt %. The inhibitor is a substance capable of producing hydrogen or has reducing capacity or has adsorption capacity on the active centre of acid catalysts and mixtures thereof, where the substance capable of producing hydrogen or containing hydrogen is hydrogen, tetradihydronaphthalene, decalin, dry catalytic cracking gas, dry coke gas and mixtures thereof. The substance with reducing capacity is carbon oxide and the substance with adsorption capacity on the active centre of acid catalysts is methanol, ethyl alcohol, ammonia, pyridine and mixtures thereof.

EFFECT: use of present method enables inhibition of further conversion of light olefins, which increases output of end products.

21 cl, 7 ex, 3 tbl, 2 dwg

FIELD: oil and gas production.

SUBSTANCE: invention refers to procedure for hydrocarbon stock catalytic cracking at fine dispersed catalyst for production of target products. The procedure consists in contacting raw stock and catalyst in a direct flow reactor. Successively spent catalyst is stripped from entrained hydrocarbons in a stripping column by processing catalyst with steam under stepped-counter flow conditions and with implementation of conic ring-like and disk partitions. Part of steam passes through orifices in the partitions. Steam is directed via nozzle orifices made on one or three lower partitions at amount of 10-45% of its consumption into the stripper. Also, steam from the nozzle orifices is exhausted at distance from partition surface equal to 0.04-0.09 of diametre of the stripper.

EFFECT: increased degree of catalyst stripping, raised stability of catalyst circulation, reduced thermo-steam deactivation of catalyst and increased output of cracking target products.

5 ex, 1 tbl, 2 dwg

FIELD: chemistry.

SUBSTANCE: invention relates to a method of increasing output of light olefin hydrocarbons from hydrocarbon material through catalytic cracking, involving (a) feeding hydrocarbon material in form of naphtha or kerosene and water vapour into a catalytic cracking furnace, where the hydrocarbon material undergoes a catalytic cracking reaction in the presence of a catalyst; (b) regenerating the catalyst used in the catalytic cracking reaction through continuous or periodic regeneration, and repeated use of (recycling) of the regenerated catalyst in the catalytic cracking furnace: (c) fast cooling, compression and separation of the catalytic cracking reaction product in order to separate and extract hydrogen, methane and C2-C3 olefin hydrocarbons and to separate into a stream containing C2-C3 paraffin hydrocarbons and a stream which contains C4+ hydrocarbons; (d) feeding the stream which contains C2-C3 paraffin hydrocarbons into the furnace for recycling, where the stream is converted to C2-C3 olefin hydrocarbons through a thermal cracking reaction, and recycling the converted C2-C3 olefin hydrocarbons to the fast cooling step; (e) recycling at least a portion of the C4-C5 hydrocarbons of the stream which contains C4+ hydrocarbons to the catalytic cracking reaction step, where the output of ethylene and propylene obtained through catalytic cracking of recycled C4-C5 hydrocarbons is higher than the output of ethylene and propylene obtained through catalytic cracking of naphtha or kerosene, wherein the catalytic cracking reaction is carried out at temperature 500-750°C and weight ratio of naphtha or kerosene to water vapour is equal to 0.01-10 and the dwell time of naphtha or kerosene is equal to 0.1-600 seconds and the weight ratio of the catalyst to naphtha or kerosene of the hydrocarbons is equal to 1-100.

EFFECT: high output of light olefins.

4 cl, 4 ex, 8 tbl, 2 dwg

FIELD: chemistry.

SUBSTANCE: invention relates to chemical industry and specifically to obtaining composite anticorrosion coating materials meant for protecting rusty metal surfaces from corrosion, applied directly onto the rusty metal surface, and obtaining a base - sorption materials from products of processing natural organic compounds of plant origin. The method of obtaining a base for composite anticorrosion coating material involves using cut high density wood as raw material which undergoes hydrolysis with 0.5-0.8% sulphuric acid solution, washing and pressing the hydrolysate, its ammonolysis which is carried out with a mixture containing ammounium hydroxide, sodium citrate, sodium hydroxide, citric acid sodium, water, repeated washing and pressing the ammoniated product, separation into fractions, drying the product to 5-15% moisture content. The product is activated in the presence of ammonium hydroxide, amine additives, catalyst and water, followed by grinding and activation with a composition containing ammonium hydroxide, amine additives, catalysts and water at normal pressure and temperature of 100-150°C until achieving 5-15% moisture content of the product and particle size of 1-10 mcm. The method of obtaining composite anticorrosion coating material involves preparation of a mixture of binding substance and a base for composite anticorrosion coating material, mechanical activation and dispersion of the composition with filler pigments, treatment in the chamber of an apparatus with a vortex layer of ferromagnetic particles, colouring and dilution with diluents-solvents. The material is taken for bottling and packaging.

EFFECT: method enables to shorten the time for obtaining the material and power consumption, while obtaining high-quality anticorrosion coating complex material.

10 cl

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