Method for preparing methanol and other aliphatic alcohols

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

 

The invention relates to the production of lower aliphatic alcohols, in particular methanol, and can be used in chemical, petrochemical, oil refining and oil and gas industry.

There is a method of production of methanol and other aliphatic alcohols by gas-phase interaction of the hydrocarbon gas or mixture of gases with oxygen-containing gas (Patent of Ukraine # 28615 "method for the production of methanol and aliphatic alcohols", IPC 6 07 With 31/02, publ. 15.05.2002, bull. No. 5). For reasons that impede the achievement of specified following technical result is that the process is conducted at high temperatures (200-400°C) and pressure (0,25-of 9.6 MPa) in two stages with intermediate product (oxidate raw), which is then subjected to heterogeneous catalytic hydrocarbonbearing in the presence of catalysts. The process requires complex hardware design, costly and energy-intensive, and the target product has a complex structure with a large number of other organic impurities formed as a result of adverse reactions occurring at high temperatures and pressure.

There is a method of production of methanol and other aliphatic alcohols by gas-phase interaction of natural gas with oxygen-containing gas at a separate supply of natural gas and kislorodnije the containing gas into the reactor (Ed. St. formerly. The USSR №1145014, MKI 4 31/04 C 07 C, publ. 15.03.85, bull. No. 10). For reasons that impede the achievement of specified following technical result is that the methanol receive at high temperatures (500-1600° (C) and a pressure of 100-150 ATM, which requires complex and expensive equipment, and therefore, large material and energy costs. The composition of the obtained intermediate product (oxidate) is complex, it contains higher alcohols, methanol, ether and other organic impurities. The process is in two stages.

Closest to the claimed method of the same purpose is a method of production of methanol and other aliphatic alcohols by gas-phase interaction of hydrocarbon gases with water vapor under the action of ultraviolet radiation (application JP 1-096143 And "the Way of the oxidation of ethane" publ. 14.04.1989) adopted for the prototype.

For reasons that impede the achievement of the technical result when using the known method is that in the known method for obtaining aliphatic alcohols use the method of direct oxidation of ethane in which of the original hydrocarbon get a mixture of products (including impurities) with a low content of alcohol, and the resulting alcohol must be extracted from the mixture and clean, resulting in the need of material and energy-intensive equipment is s, what makes the process from a technological and economic point of view, unattractive.

The invention consists in the following.

The production of methanol and other aliphatic alcohols carried out mainly in two stages: the production of synthesis gas (carbon monoxide and hydrogen) and the subsequent oxidation synthesis gas at high temperatures and pressures in the presence of catalysts. Sophisticated instrumentation, a small degree of conversion of synthesis gas into methanol in a single pass (2-3%), the presence of significant amounts of organic impurities in methanol raw (over 4%) and the need for complex distillation separation is compensated by a high degree of knowledge and predictability of the process, so the upgrades were mainly confined to the expansion of the range of the used catalysts and technological methods of entering the synthesis gas.

The work on the production of methanol electrolytic method has not led to significant results, and receipt of methanol in the device that collects solar energy, and the means developed on its basis, have, apparently, of limited use in mind explosion and fire hazard used hydrides. In addition, the solar spectrum is quite wide and divide it into certain radiation and wavelengths for use in the same process - technical the problem, the solution which is impractical because of its intensity and complex hardware design.

The challenge is to create a new economical method of producing methanol and other aliphatic alcohols in a single phase as of individual hydrocarbons and their mixtures, including natural gas.

The technical result - obtaining methanol and other aliphatic alcohols in the gas-phase interaction of hydrocarbon gases with water vapor, namely the direct hydroxylation of the source gas or mixture of gases with water vapor in one stage, in one device, achieving high yield of the target product; receiving targeted high quality product without additives or with a minimum number of them in the case of use as a source component of natural gas; reduction of material and energy process compared to conventional industrial methods.

This technical result in the implementation of the invention is achieved in that in the known method of production of methanol and other aliphatic alcohols by gas-phase interaction of hydrocarbon gases with water vapor under the action of ultraviolet radiation, methanol and other aliphatic alcohols receive direct hydroxylation of hydrocarbon gas or mixture of hydrocarbon gases with water vapor, for which the source is uglevodorodnyi gas and steam or a mixture of gases and steam is served in the reaction apparatus, where the reaction mass is subjected to ultraviolet radiation in the wavelength range 240-450 nm at a temperature not lower than the temperature of vaporization, and the target product is separated from the vapor-gas mixture by condensation, and derived from the reaction zone unreacted hydrocarbon gas or mixture of gases clear of the target product by bubbling through the water and returned to the reaction apparatus, adding the source gas component in the quantity consumed.

In addition, the methanol or other aliphatic alcohols, if necessary, increase the concentration is subjected to the direct distillation.

In the present method the process of obtaining the target product, methanol or other aliphatic alcohols of individual hydrocarbon gases or their mixtures (including natural gas) are predominantly at a temperature that ensures evaporation, and under the action of ultraviolet radiation at wavelengths comparable with the energies of O-H bond of water and C-H bond of the primary atom of the hydrocarbon gas, this process is feasible even at atmospheric pressure. Under the action of ultraviolet radiation of the claimed range of 240-450 nm and a molar ratio of steam-gas, for example, (1-2):1 the reaction proceeds by a radical character according to the following scheme:

Orsodacnidae, what is the process for direct hydroxylation, and the target product is produced in one stage, and high quality, with almost no impurities, as this is not going adverse reactions common to high-temperature oxidation processes carried out at high pressure.

Experimentally proved, that the process is in accordance with the scheme when used as initial products as methane and other lower homologues of the paraffin series (ethane, propane, and others).

The high yield of the desired product (30%) is provided by the radical nature of the process, which, in turn, due to the energy parameters of the proposed range of ultraviolet radiation. The yield of the target product in relation to the original products is also influenced by the estimated ratio of the gas:couples who for different gases and, depending on the process parameters are selected (calculated) individually (see table 1). Also affects the recirculation - the return of the unreacted gases in the reaction apparatus after purification by bubbling through a water layer.

The process takes place in one stage, in one device, without the use of catalysts at relatively low temperatures and feasible even at atmospheric pressure, and for separation of the target product from the vapor-gas mixture and increase its concentration (if necessary the cost) only requires the condensation and direct distillation (distillate), i.e. material and energy costs are relatively small, which ensures absolute efficiency of the proposed method in comparison to that utilized in industry.

Thus, the above formula the features of the invention, characterizing the inventive method, a necessary and sufficient to achieve the desired technical effect.

Conducted by the applicant's analysis of the prior art, including searching by the patent and scientific and technical sources of information, and identification information about the equivalents of the claimed invention has allowed to establish that the applicant had not found the source, which is characterized by symptoms that are identical to all the essential features of the claimed invention, and also helped to identify a set of essential towards perceived by the applicant to the technical result of the distinctive features in the claimed method and set forth in the claims. Therefore, the claimed invention meets the condition of "novelty."

To verify compliance of the claimed invention, the term "inventive step", the applicant conducted an additional search of the known solutions to identify signs that match the distinctive features of the prototype of the features of the proposed method. The search results showed that the claimed invention does not follow for specialist anymoreso of the prior art, as in the prior art, a particular applicant identified the impact of ultraviolet radiation in the claimed range for the process of gas-phase interaction of hydrocarbon gases with water vapor, as well as all of the distinctive features of the claimed invention to obtain the desired technical effect.

Therefore, the claimed invention meets the condition of "inventive step".

The invention is illustrated in the table, which presents the composition of the starting components, ratio of components, the parameters of the process for production of methanol and other aliphatic alcohols for examples.

Information confirming the ability of the invention to provide the above technical result are as follows.

Method of production of methanol and other aliphatic alcohols is carried out in a reaction apparatus of the cylindrical volume, for example, 5 liters, provided with a source of ultraviolet radiation, heating element, a socket for input steam and gas flows and the withdrawal of gaseous reaction products and unreacted tail gases, instrumentation (thermocouple, flow meter and other). By means of the heating device in the reaction apparatus support temperatures the evaporation. In the device simultaneously serves the flow of hydrocarbon gas (or gas mixture) and the flux of water vapor in the estimated value and the calculated speed shown in the table. The reaction mass is subjected to UV irradiation in the wavelength range 240-450 nm with continuous supply of steam and continuous removal of the reaction products.

In the reaction zone under the action of ultraviolet radiation is the process for direct hydroxylation of methane or other hydrocarbon gases water vapor with the formation of aliphatic alcohols.

The obtained gas-vapor mixture containing 30% of methanol or other aliphatic alcohol, is passed through a condenser for separation of the target product, and if necessary increase of its concentration through the distiller. Unreacted gases are cleaned by bubbling through the water, add the gas component in the quantity consumed to maintain the original estimated ratio of steam:gas and returned to the reaction apparatus. The process is easily adjustable, running is a simple feed gas and steam flows, stop their termination.

The invention is illustrated in the examples.

Example 1 (positive).

In the reaction apparatus in which the temperature is maintained at 100°With, at the same time serves as a continuous flow of methane and tanoy couples ratio of 1:1 at a rate of 12 l/h. As a source of ultraviolet radiation is used lamp type DPT-100, providing radiation with a wavelength of 240-450 nm, irradiation carried out luminous flux 5500 lumens.

In the reaction zone in the reaction hydroxylation 16% of the gas mixture is converted into the target product is methanol, which is isolated from the gas mixture by condensation, and unreacted "tail" gas is passed through the bubbler and return in the reaction apparatus by adding methane to the quantity consumed. The composition of the obtained aqueous solution determined by chromatographic analysis.

The composition of the aqueous solution of methanol:

methanol is 8.25%,

dimethyl ether - 0,0012%,

organic food - no,

water - the rest.

The obtained target product is subjected to distillation to improve concentration.

Example 2 (positive).

In the reaction apparatus, which supports a temperature of 100°With, at the same time serves vapor and methane in the estimated ratio of 2:1 with a speed of 18 l/h. As a source of ultraviolet radiation is used the lamp DPT-100, providing ultraviolet radiation of a wavelength of 240-450 nm and a luminous flux 5500 LM. In the reaction zone in the reaction hydroxylation 9% gas mixture is converted into methanol, and the rest remains without ISM is of high value. Target product - methanol is recovered from the vapor-gas mixture by condensation. Unreacted "tail" gas purified from methanol by bubbling through the water, add the methane in the quantity consumed, and return in the reaction apparatus. The composition of the aqueous solution of methanol determine chromatographic analysis.

The composition of the obtained aqueous solution of methanol;

methanol is 4.5%,

dimethyl ether is 0.0001%,

organic impurities - no,

water - the rest.

The resulting solution of methanol is subjected to distillation to improve concentration.

Example 3 (negative).

In the reaction apparatus in which the temperature is maintained at 100°With, at the same time serves methane and steam in the estimated ratio of 3:1 with a speed of 24 l/h. As a source of ultraviolet radiation is used the lamp DPT-100, providing radiation of a wavelength of 240-450 nm and a luminous flux 5500 LM. In the reaction zone in the reaction hydroxylation 4% gas mixture is converted to methanol, the rest remains unchanged. The formed methanol allocate the condensation of vapor-gas mixture and reacted "tail" gas is washed and fed into the reaction apparatus by adding methane to the quantity consumed.

The resulting aqueous solution analyzed by GC is I.

The composition of the aqueous solution of methanol:

methanol - to 2.15%,

dimethyl ether is missing,

organic food - no,

water - the rest.

Example 4 (negative).

In the reaction apparatus according to example 1-3 serves both methane and steam in the estimated ratio of 2:1 with a speed of 18 l/h. As a source of ultraviolet radiation is used lamp type DPT-100, which provides radiation with wavelengths of 240-450 nm and a luminous flux 5500 LM at a constant flow of methane gas and the selection of the reaction products. In the reaction zone in the reaction hydroxylation 16% of the gas mixture is converted to methanol, and unreacted methane is partially reacts with the formation of side products. Target product - methanol is recovered from the vapor-gas mixture by condensation, and unreacted methane washed by bubbling back into the reaction apparatus by adding methane to the quantity consumed. The resulting aqueous solution of methanol analyze chromatographic method.

The composition of the solution of methanol:

methanol - 8,05%,

dimethyl ether - 0,11%,

organic impurities is 0.05%,

water - the rest.

From the above examples 1-4, it follows that the increase in the number of steam leads to the reduction of impurities in the target product, but practically does not effect the output of methanol, and the decrease in its concentration in methanol raw is only due to the dilution water. The reduction of the same amount of steam causes the occurrence of side reactions with the formation of dimethyl ether and other organic impurities.

Example 5 (positive).

In the reaction apparatus in which the temperature is maintained at 100°With, at the same time serves as a continuous flow of methane and steam in the estimated ratio of 1:1 with a speed of 24 l/h. As a source of ultraviolet radiation is used the lamp PTA-250, providing radiation of a wavelength of 240-450 nm, and the irradiation is carried out luminous flux 12500 LM at a constant feed gas mixture and the constant selection of the reaction products. In the reaction zone in the reaction hydroxylation 34% gas mixture is converted into methanol, and the rest remains unchanged. The formed methanol produce condensation, and unreacted "tail gas after washing the return from methanol in the reaction apparatus by adding methane to the quantity consumed. The resulting solution of methanol analyze chromatographic method.

The composition of the obtained solution of methanol:

methanol is 17.2%,

dimethyl ether is 0.001%,

organic impurities - no,

water - the rest.

The resulting solution of methanol is subjected to distillation for the avicenia his concentration.

Example 6 (positive).

In the reaction apparatus in which the temperature is maintained at 100°With, at the same time serves methane and steam in the estimated ratio of 1:1 at 42 l/h. As a source of ultraviolet radiation is used the lamp PTA-1000, providing ultraviolet radiation with wavelengths of 240-450 nm and a luminous flux 45000 LM at a constant feed gas mixture and the removal of reaction products.

In the reaction zone in the reaction hydroxylation 61% of the gas mixture is converted to methanol, the rest remains unchanged. The formed methanol is recovered from the vapor-gas mixture by condensation, and unreacted "tail gas after washing the return from methanol in the reaction apparatus by adding methane to the quantity consumed. The resulting aqueous solution of methanol analyze chromatographic method.

The composition of the aqueous solution of methanol:

methanol is 30.5%,

dimethyl ether is 0.0015%,

organic impurities - no,

water - the rest.

The resulting solution of methanol is subjected to distillation to increase the concentration.

From the above examples 1.5 and 6 it follows that the radiation energy is one of the main technological parameters. When using more powerful sources of UV radiation, the degree of transformation against the melt is proportional to the energy of the radiation, and we can say, when using ultraviolet radiation sources capable of emitting a given spectral range with sufficient light output, can be achieved 100%degree of conversion of gas-vapor stream to methanol.

Example 7 (positive).

In the reaction apparatus in which the temperature is maintained at 100°With, at the same time serves as a continuous flow of propane and steam are calculated in the ratio of 1:1 with a speed of 24 l/h. As a source of ultraviolet radiation is used the lamp DPS-250, providing radiation of a wavelength of 240-450 nm and a luminous flux 12500 LM. The irradiation is carried out at a constant flow of propane and steam and continuous removal of the reaction products. Passing through the reaction apparatus, 46% of the gas mixture becomes propanol, and the rest remains unchanged. Formed propanol produce condensation, and unreacted "tail gas after washing from propanol served in the reaction apparatus by adding propane to the quantity consumed. The resulting aqueous solution of propanol analyze chromatographic method.

The composition of the aqueous solution of propanol:

propanol - 23,2%,

organic impurities - no,

water - the rest.

An aqueous solution of propanol is subjected to distillation to increase the concentration.

Example 8 (I will put the AUX).

In the reaction apparatus in which the temperature is maintained at 100°With, at the same time serves as a continuous flow of butane and steam in the estimated ratio of 1:1 with a speed of 24 l/h. As a source of ultraviolet radiation is used the lamp DRSH-250, giving a radiation wavelength of 240-450 nm and a luminous flux 12500 LM. The irradiation was carried out with continuous supply of steam and continuous withdrawal of the reaction products. In the reaction zone in the reaction hydroxylation 58% of the gas mixture is converted into butanol, and the rest remains unchanged. The resulting butanol produce condensation, and unreacted gas after washing from butanol by bubbling through a water layer returned to the reaction apparatus by adding butane in the quantity consumed.

The resulting aqueous solution of butanol analyze chromatographic method.

The composition of the aqueous solution of butanol:

butanol was 29.6%,

organic impurities - no,

water - the rest.

An aqueous solution of butanol is subjected to distillation.

From the above examples 6, 7 and 8 it follows that the reaction is cleavage of the C-H bond, as these communications more accessible to the action of reagents, which is confirmed by the absence in samples of by-products. Radicals with the free electron secondary atom formed easier than the PE the primary, and therefore, ceteris paribus, the output of aliphatic alcohols from methanol to butanol increases.

Example 9 (positive).

In the reaction apparatus, which supports a temperature of 100°With, at the same time serves couples and natural gas of the following composition: methane - 92,52%, ethane - 3,96%, propane - 1,0%, butane - 0,1%, inert gases (CO2) - 2,42% in the estimated ratio of 1:1 with a speed of 24 l/h. As a source of ultraviolet radiation is used the lamp DRSH - 250, which gives the radiation wavelength 240-450 nm and a luminous flux 12500 LM. In the hydroxylation reactions of 35.2% of the gas mixture is converted into alcohol, the rest remains unchanged. The resulting alcohols are the condensation and unreacted "tail" gas washed from alcohols and return in the reaction apparatus by adding natural gas to the quantity consumed. The resulting aqueous solution of alcohols analyze chromatographic method.

The composition of the mixture obtained aliphatic alcohols:

methanol - 15,72%,

ethanol - 1,2%,

propanol - 0,6%,

butanol - 0,08%,

organic impurities - 0,0014%,

water - the rest.

With increasing pressure and temperature and in the presence of catalysts used in the reactions photochemical synthesis (for example, ZnO, TiO2), the formation of aliphatic alcohols hasten the is, the degree of conversion of gas-vapor mixture per cycle increases to 25-40%, the overall yield of the target product is 75-95% depending on the structure of the original products. However, a special advantage is that the process is feasible at a relatively low temperature and atmospheric pressure. The method is economical, requires relatively low capital investment and meets the requirements of environmental protection.

Thus, the presented data suggest the implementation of the use of the claimed method the following cumulative conditions:

- a means of embodying the inventive method in its implementation, is intended for use in industry, namely in the chemical, petrochemical, oil refining and oil and gas industry;

for the inventive method, it is described in the independent clause sets out the claims, confirmed the possibility of its implementation using the steps described in the application of tools and methods.

Therefore, the claimed invention meets the condition of "industrial applicability".

Table
IndicatorsThe placeholderExamples
12 456789
The composition of the gas componentnatural gasmethanemethanemethanemethanemethanemethanepropaneBhutannatural gas
The ratio of steam and
gas combined-cycle4:11:12:13:11:21:11:11:11:11:1
mixture
The consumption of steam and gas121824182442242424
mixture, l/h#x0200A;
Power light55005500550055001250045000125001250012500
flood lamp, LM
Conversion rate
steam-flow (2,2-3,51694163461465835,2
one pass), %
Composition
condensing
product %
Alcohol87,48,254,52,158,0517,230,523,229,617,6
Diethyl ether2,5-3,00,00120,0001-0,110,0010,0015---
Other organicof 4.5-5.6---0,05----0,0014
products
H2Oto 3.6791,748895,499997,85 91,7982,79969,4985of 76.870,482,4986

1. Method of production of methanol and other aliphatic alcohols by gas-phase interaction of hydrocarbon gases with water vapor under the action of ultraviolet radiation, characterized in that the methanol and other aliphatic alcohols receive direct hydroxylation of hydrocarbon gas or mixture of hydrocarbon gases with water vapor, for which the source of hydrocarbon gas and steam or a mixture of gases and steam is served in the reaction apparatus where the reaction mass is subjected to ultraviolet radiation in the wavelength range 240-450 nm at a temperature not lower than the temperature of vaporization, and the target product is separated from the vapor-gas mixture by condensation, and derived from the reaction zone unreacted gas or mixture of gases clear of the target product by bubbling through the water and returned to the reaction apparatus, adding the source gas component in the quantity consumed.

2. The method according to claim 1, characterized in that the methanol or other aliphatic alcohol, if necessary, increase the concentration is subjected to the direct distillation.



 

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