A method of producing methanol

 

(57) Abstract:

Usage: mainly organic synthesis for the production of methanol used as a component of motor fuel. The inventive product is methanol. B. C. CH4O, the selectivity of 50% Reagent 1: metadatabase gas. Reagent 2: oxygen-containing gas. Reaction conditions: the process carried out at the chemical exposure (heterogeneous catalytic system, the higher gaseous hydrocarbons or oxygen-containing compounds, cold oxidizer to one or more sequential stages of the direct partial oxidation of methane at 200-600C and a pressure of 2.5-1.5 MPa. 8 C.p. f-crystals, 1 Il.

The invention relates to organic chemistry, in particular to methods of producing methanol by direct oxidation of natural gas, and can be used in the chemical industry for the production of methanol used, for example, as a component of motor fuel or feedstock for production of synthetic gasoline and other motor fuels.

The number of known methods for producing methanol from methane and metastasic gases. Most of the industrial application was received by the conversion of methane into synthesis gas (CO and H2) the th equipment, large energy consumption for the conversion of methane into synthesis gas, a multi-stage process, the need for careful treatment of natural gas from sulfur compounds, the lack of profitability of small plants with a capacity of less than 2000 tons/day. So currently intensively investigated the possibility of establishing effective processes direct oxidation of methane to methanol, bypassing the stage of synthesis gas.

Closest to the present invention is a method of producing methanol, which consists in the oxidation of natural gas oxygen-containing gas at a temperature of 350-1600aboutC and a pressure of 100-150 ATM with separate feeding preheated natural gas and oxygen-containing gas in the rector [2]

However, the known method has the following disadvantages: low degree of conversion of natural gas to the target product, loss of the desired product as a result of its further oxidation to organic acids and carbon oxides, the volatility process.

The objective of the invention is to provide a highly efficient method of producing methanol, which allows to increase the degree of methane conversion in the target product (methanol, and formaldehyde and higher alcohols and Maldegem oxidation metadatareader gas, including natural gas, oxygen-containing gas, including oxygen, at elevated temperature and pressure with separate feeding into the reactor preheated metadatareader gas and oxygen-containing gas and subsequent separation of the target product, the process is carried out at the chemical effects on one or more successive stages of the direct homogeneous oxidation of methane at a temperature of 200-600aboutC and a pressure of 2.5 to 15 MPa.

Conducted in the development of the proposed method of this study revealed three main stages of the process in the reactor. The first stage is razvetvlenno-chain process, and the branching is determined only by the structure and properties of the original substances. The second stage is virodene-branched chain process, and the branching is determined by the structure and properties of intermediate products (methanol, formaldehyde, peroxides). In addition, the second stage is almost complete consumption of oxidant. The third stage is characterized thermal noncorrosive transformation of the reaction products. The second stage conditionally can be divided into two sub-phases: the substage, MIS slow accumulation of elapsed is in which there is a formation of the base products, characterized by sharp autostream process and the rise of the temperature.

Chemical reactions on the listed stages significantly different, so the solution of this problem is achieved by various types of chemical exposure at different stages or multiple stages in the reaction stream at a particular site (which corresponds to a specific point in time of the reaction) to impose any chemical (reagent, catalyst and others).

To achieve maximum yield of the target product use regulation (including automatic) point of application of the impact based on current process parameters (e.g. temperature). Also used repeated recirculation of exhaust gases from the reactor (after the separation of the target product).

In the known methods of production of methanol from metadatareader gases by direct oxidation separate chemical effect on the successive stages of the process so far has not been applied. At the same time, as research has shown, the impact on the individual stage of the process allows the best way to organize the process and optimize it from the point of view of obtaining maximum Conve from time to time.

It is established that the process of direct partial oxidation of methane at low oxygen concentrations and high pressures, i.e., the conditions most favorable for the formation of methanol, characterized by the presence of three clear areas (see the drawing), each of which is dominated by various chemical processes. The initial stage razvetvlenno-chain acceleration reaction (section t0-t1on the curve) is characterized by the important role of homogeneous and heterogeneous reactions generation of free radicals. Theoretical and experimental studies have demonstrated a significant impact on this stage by introducing homogeneous chemical promoters, such as higher gaseous hydrocarbons (ethane, propane, and others) or oxygenated compounds (alcohols, peroxides, aldehydes), or through the use of heterogeneous catalysts for the decomposition of hydrocarbons. However, as studies have shown, this additional initiation throughout the reaction, for example by use of a catalytic reactor, even more increases the rate of oxidation of the target product and ultimately leads to the decrease of its output. It is established that such speed, the fact contributes to the overall decrease in the temperature of the remaining stages of the process, which, in turn, reduces the rate of further oxidation of the already formed methanol. Furthermore, the reduced energy consumption for preheating gases.

In the second stage of the process (t1-t2) is the accumulation of intermediate products (peroxides and aldehydes), leading to subsequent rapid warming at the end of this stage on plot (t1'-t2). Studies have shown that at the beginning of the second stage is the most effective soft catalytic effect, promotes more rapid and complete translation of the source reagents in compounds such as peroxides and aldehydes. In addition, it is shown that the introduction of the initial part of the second stage (t1-t1'the catalysts based on cobalt molybdate promotes the translation of one of the intermediate products formaldehyde in the target product methanol.

The impact on the final part of the second stage (t1'-t2must have the ultimate goal of increasing the degree of conversion of natural gas while maintaining a slight depth of oxidation in order to maintain the highest possible degree env is(oxygen or air). This technique does not lead to significant explosive heat of reaction and the associated formation of products of deep oxidation of methane monoxide and carbon dioxide, while maintaining a high degree of conversion of methane to methanol with increasing total depth of processing source metadatareader gas.

The third and final stage of the process after the consumption of one of the reagents oxygen recombination of radicals and relatively slow transformation of unstable products. Studies have shown that at this stage, as in the beginning of the second stage, the most effective introduction of specific catalysts promoting the translation formed during the previous phases of formaldehyde in the target product methanol.

It should be noted that each curve in the drawing (depending on the temperature of the process from time to time) corresponds to a certain portion of the length of the reactor.

The experiments demonstrated the fundamental volatility process partial oxidation mode cold flames. Even with complete consistency of input parameters of the process are stochastic changes in concentration and temperature profile along realda such random changes in position relative to the beginning of the reactor end of the second stage of the process, occupying a very small part of the total length of the reactor, but defines the transformation of the vast majority of all consumable methane. Any impact on this stage, for example the submission of additional portions of oxygen, it is necessary to automatically adjust to the actual current position of the zone of maximum heating.

Because of the relatively high selectivity of formation of methanol (about 50% ) is achieved only at low degrees of conversion of methane (3-5% ), rational use of Metastasio raw materials requires recirculation of unreacted part metadatareader gas after removing from it the target products.

The proposed method is as follows.

Preheated to a temperature of 200-500aboutWith natural gas under pressure from 2.5 to 15 MPa and at a flow rate of 760 nm3/h fed into the reactor, which is a pipe with a diameter of h,5 mm of steel 12X18H10T. In the mixing chamber of the natural gas is mixed with air, reducing the oxygen concentration to a value of from 1 to 4% For better mixing of the air is blown perpendicular to the gas flow. The process is controlled by the heating along the reactor thermocouples. Various the actor catalyst. At the reactor exit gases are cooled in the heat exchanger and then separated from the liquid products in the separator. Analysis of the liquid products is chromatographic.

P R I m e R 1 (comparative without chemical influence).

Process conditions: Pressure, MPa 10,0

The natural gas consumption, nm3/h 760 air Flow, nm3/h 80 Content of oxygen, about. 2 TemperatureaboutWITH 360

The composition of the reaction products:

Component methanol aldehydes water

Yield, kg/1000 nm311,36 4,10 11,9

P R I m m e R 2. The same conditions as in example 1. In the mixer additionally served formaldehyde in quantities of 1 kg/1000 nm3gas.

The composition of the reaction products:

Component m ethanol aldehydes water

Yield, kg/1000 nm312,4 12,0 4,3

P R I m e R 3. The same conditions as in example 1. In the initial section of the reactor was made of the oxide catalyst (Cr2O3).

The composition of the reaction products:

Component methanol aldehydes water

Yield, kg/1000 nm312,6 4,8 10,5

P R I m e R 4. The same conditions as in example 1, but directly in front of the zone of maximum heating area (maximum concentration of methanol in the reactor was filed ethane in amounts of 2-10% of the water

Yield, kg/1000 nm3< / BR>
when 2% of ethane to 11.6 5,15 11,2

at 10% ethane 11,9 6,3 8,1

P R I m e R 5. The same conditions as in example 1. In the zone of maximum heat-up additionally pull air in the same volume as in the mixer (80 nm3/h).

The composition of the reaction products:

Component methanol aldehydes water

Yield, kg/1000 nm319,73 6,11 19,61

P R I m e R 6 (comparative). The conditions of example 5, but the air is supplied at the beginning of the reactor (in the mixer).

The composition of the reaction products:

Component methanol aldehydes water

Yield, kg/1000 nm317,76 1,89 20,18

P R I m e R 7. The same conditions as in example 1. In the area of the initial part of the stage of accumulation of products (t1-t2) made industrial multicomponent oxide catalyst based on cobalt molybdate (C-41).

The composition of the reaction products:

Component methanol aldehydes water

Yield, kg/1000 nm311,96 2,50 11,95

P R I m e R 8. The same conditions as in example 1, but just outside the zone of maximum heating (t2) made industrial multicomponent oxide catalyst based on cobalt molybdate (C-41).

The composition of the reaction products:

Component methanol aldehydes water

Output, and formaldehyde in quantities of 1 kg/1000 nm3gas, and in the zone of maximum heat-up additionally pull air in the same volume as in the mixer (80 nm3/h).

The composition of the reaction products:

Component methanol aldehydes water

Yield, kg/1000 nm320,2 5,2 1,3

As seen from the above examples, various types of chemical exposure lead to increased yield of methanol or aldehydes. Comparison of examples 5 and 6 shows the decisive importance of the place of application of the impact.

1. A METHOD of producing METHANOL by oxidation metadatareader gas, including natural gas, oxygen-containing gas, including oxygen, at elevated temperature and pressure with separate feeding into the reactor preheated metadatareader gas and oxygen-containing gas and subsequent separation of the target product, wherein the process is carried out at the chemical effects on one or more successive stages of the direct partial oxidation of methane at a temperature of 200 600oC and a pressure of 2.5 to 15 MPa.

2. The method according to p. 1, characterized in that the impact of exercise on the initial phase of direct partial oxidation of methane stage razvetvlenno-chain self-acceleration of the reaction. is on stage degenerate razvetvlenno-chain accumulation of intermediate products.

4. The method according to p. 1, characterized in that the impact assetsat the third phase of the process to the step noncorrosive conversion of intermediate reaction products.

5. The method according to p. 1, characterized in that the exposure is carried out by introducing into the reactor heterogeneous catalytic systems multicomponent metal oxide catalyst.

6. The method according to p. 2, characterized in that the exposure is carried out by introducing into the reactor a homogeneous chemical promoters higher gaseous hydrocarbons or oxygen-containing compounds.

7. The method according to p. 3, characterized in that the exposure is carried out by introducing into the reactor additional servings of cold oxidizer.

8. The method according to p. 1, characterized in that the application area of impact shift with regard to the current values of the output parameters of the process.

9. The method according to p. 1, characterized in that the effluent from the reactor gas after separation of the target product is re-fed to the reactor inlet (recycle).

 

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SUBSTANCE: method involves partial oxidation of an alkane contained in a gaseous crude stream, which contains an alkane, with oxygen contained in an oxygen-containing crude stream. Said method involves: forming a reactor system, having a back-mixing reaction chamber with injection mixing, which is connected to a tubular flow reactor, wherein said back-mixing reaction chamber with injection mixing ensures dwell time from about 0.05 s to about 1.5 s; feeding said crude stream containing alkanes and said oxygen-containing crude stream into said back-mixing reaction chamber with injection mixing; initiating formation of alkyl free radicals in said back-mixing reaction chamber with injection mixing to obtain a product stream from the back-mixing reaction chamber with injection mixing, containing oxygen, said alkane and at least a portio of said alkyl free radicals; feeding the product stream obtained in the back-mixing reaction chamber with injection mixing into the tubular flow reactor; and converting said product stream obtained in the back-mixing reaction chamber with injection mixing into said alkyl oxygenate in said tubular flow reactor; where said alkane is selected from group consisting of methane, ethane, propane and butane.

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34 cl, 2 ex, 36 dwg

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1 ex, 1 dwg

FIELD: chemistry.

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4 cl, 15 ex

FIELD: chemistry.

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13 ex

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3 ex

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12 cl, 3 tbl, 3 dwg

FIELD: organic chemistry, chemical technology.

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FIELD: organic chemistry, chemical technology.

SUBSTANCE: invention relates to a new method for preparing methanol and other aliphatic alcohols by gas-phase interaction of hydrocarbon gases with water vapor under effect of ultraviolet radiation. Methanol and other aliphatic alcohols are prepared by direct hydroxylation of hydrocarbon gas or mixture of hydrocarbon gases with water vapor. For this aim hydrocarbon gas and vapor or mixture of gases and vapor are fed into reactor wherein the reaction mass is subjected for effect of ultraviolet radiation in wavelength range 240-450 nm at temperature lower vapor formation point. The end product is isolated from vapor-gaseous mixture by condensation and unreacted gas or mixture of gases removed from the reaction zone is purified from the end product by bubbling through water layer and recovered into reactor by adding the parent gaseous component in the amount equal to consumed one. The process is carried out for a single stage and can be realized under atmosphere pressure. Invention can be used in chemical, petroleum chemical, petroleum processing and petroleum and gas extracting industry.

EFFECT: improved preparing method.

2 cl, 1 tbl, 8 ex

FIELD: industrial organic synthesis.

SUBSTANCE: invention relates to improved process of producing methanol from purge gas produced in basic methanol or ammonia synthesis. Process comprises dispensing compressed carbon dioxide into basic synthesis purge gas, heating resultant gas mixture to starting synthesis temperature, passing thus heated gas through methanol synthesis catalyst, cooling reacted gas, recovering condensed crude methanol, and separating non-condensed gas stream into return stream and purge stream, the former being designed for mixing with basic synthesis purge gas stream and passed to one or two circulation jet compressors. Circulation is effected by energy provide either by (i) pressure of basic synthesis purge gas, which is supplied to jet compressor and further dispensed into compressed carbon dioxide stream, or by (ii) pressure of compressed carbon dioxide, which is dispensed into jet compressor and then introduced into basic synthesis purge gas stream, or by (iii) pressure of basic synthesis purge gas and pressure of indicated compressed carbon dioxide, both being supplied to one or two jet compressors. Ammonia or methanol production purge gas is successfully used for production of methanol without utilizing additional hydrogen-containing streams.

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4 cl, 5 dwg, 1 tbl, 4 ex

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SUBSTANCE: invention relates to copper-containing catalysts for low-temperature synthesis of methanol in fluidized bed at median pressure and provides catalyst, whose preparation involves impregnation and which contains oxides of copper, zinc, chromium, magnesium, aluminum, boron, and barium and has following molar ratio: CuO:ZnO:Cr2O3, MgO:Al2O3:B2O3:BaO = 1:0.3:(0.014-0.038):(0.047-0.119):(0.05-0.1):(0.007-0.014):(0.0292-0.054).

EFFECT: increased mechanical strength and wear resistance of catalyst.

1 tbl

FIELD: industrial organic synthesis catalysts.

SUBSTANCE: invention relates to copper-containing catalysts for low-temperature synthesis of methanol in fluidized bed at low pressure and provides a wear-resistant catalyst, whose preparation involves impregnation and which contains oxides of copper, zinc, chromium, magnesium, aluminum, and boron and has following molar ratio: CuO:ZnO:Cr2O3, MgO:Al2O3:B2O3 = 1:0.3:(0.15-0.2):(0.1-0.025):(0.25-0.3):(0.08-0.1).

EFFECT: increased mechanical strength and wear resistance of catalyst.

1 tbl

FIELD: industrial organic synthesis catalysts.

SUBSTANCE: invention relates to copper-containing catalysts for low-temperature synthesis of methanol in fluidized bed at high pressure and provides catalyst, whose preparation involves impregnation and which contains oxides of copper, zinc, chromium, magnesium, aluminum, boron, and barium and has following molar ratio: CuO:ZnO:Cr2O3, MgO:Al2O3:B2O3:BaO = 1:(0.7-1.1):(0.086-0.157):(0.05-0.15):(0.125-0.2):(0.018-0.029):(0.04-0.075).

EFFECT: increased mechanical strength and wear resistance of catalyst.

1 tbl

FIELD: industrial organic synthesis and chemical engineering .

SUBSTANCE: invention relates to a process of producing liquid oxygenates, including methanol, C2-C4-alcohols, formaldehyde, lower organic acids, or mixtures thereof, and to installation for implementation the process. Process comprises successively supplying natural gas from complex gas preparation plant to a series of "gas-gas" heat exchangers and into annular space of at least one tubular reaction zone of reactor, wherein natural gas is heated to temperature of the beginning of reaction, whereupon heated gas is passed to the entry of the tubular reaction zone mixer, into which compressed air or oxygen is also injected to provide gas-phase oxidation in reaction zone of reactor. Resulting reaction mixture is discharged from reactor into a series of "gas-liquid" and "gas-gas" heat exchangers, wherein reaction mixture is cooled to ambient temperature and sent to separator, wherefrom liquid phase is passed through lower carboxylic acid recovery vessel to the system of rectification columns to isolate the rest of mixture components, whereas leaving gas is recycled to complex gas preparation plant. More specifically, oxidation is carried out within temperature range 240 to 450°C and pressure from 2 to 10 MPa at residence time of reaction mixture in reactor 2-6 sec and oxidant concentration 2 to 15 wt %. In reactor having mixers hollow and at least one tubular reaction zones, required temperature is maintained constant throughout all length of tubular reaction zone and at entries for compressed air or oxygen in mixers of each of tubular reaction zones and hollow reaction zone. Liquid oxygenate production plant is composed of aforesaid complex gas preparation plant, a series of "gas-gas" heat exchanger to heat natural gas, reactor, a series of "gas-liquid" and "gas-gas" heat exchangers to cool reaction mixture obtained in reactor, gas-liquid separator, lower carboxylic acid recovery vessel, and system of rectification columns to isolate the rest of products.

EFFECT: enabled implementation of the process directly near gas and gas condensate deposits, increased conversion of methane per one passage through reactor, and increased yield of oxygenates due to improved design of plant.

6 cl, 1 dwg, 1 tbl

FIELD: chemical industry; methods of production of hydrogen and a methanol.

SUBSTANCE: the invention is pertaining to the method of production of the industrial hydrogen and methanol from the converted gas consisting mainly of CO2, H2. The method of production of hydrogen and methanol from the converted gas containing carbon oxides and hydrogen includes the synthesis of methanol. For execution of the methanol synthesis feed the converted gas with the volumetric ratio of H2-CO2/CO+CO2, equal to 2.03-5.4, which is conducted in the reactor system including the flow reactor or the cascade of the floe reactors and / or the reactor with the recycle of the gas mixture with production of methanol, the unreacted gas and the blow-down gas. At that the mixture of the unreacted and converted gases is fed for purification from carbon carbon dioxide with its extraction and batch feeding of the carbon dioxide into the converted gas delivered for the synthesis of methanol. The blow-down gases are subjected to the fine purification from the impurities with production of hydrogen. The invention allows to upgrade the method due to maximum usage of the carbon dioxide.

EFFECT: the invention ensures improvement of the method of production of hydrogen and a methanol due to maximum usage of the carbon dioxide.

2 cl, 1 dwg, 1 tbl, 5 ex

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