CN106190386B - Method for deeply removing organic sulfur from natural gas - Google Patents
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Abstract
The invention discloses a method for deeply removing organic sulfur from natural gas, which is characterized by comprising the following steps of: the method comprises the steps of carrying out wet desulphurization 1 and temperature swing adsorption 1 on natural gas containing organic sulfur to obtain a purified product, and carrying out cold blowing, pre-cold blowing, heat exchange, temperature rise, pre-temperature rise, heating, organic sulfur conversion, water cooling, wet desulphurization 2 and temperature swing adsorption 2 on regenerated gas in the temperature swing adsorption 1 process in sequence, and then mixing the regenerated gas with the purified product to serve as purified natural gas for outward transportation.
Description
Technical Field
The invention relates to the technical field of natural gas purification, in particular to a method for deeply removing organic sulfur from natural gas.
Background
At present, most of the natural gas detected in the areas contains high content of organic sulfur compounds such as hydrogen sulfide, carbonyl sulfide, carbon disulfide, methyl mercaptan, ethyl mercaptan, methyl sulfide, propyl mercaptan, butyl mercaptan, dimethyl disulfide, ethyl sulfide and thiophene. For example, the content of natural gas in northern east China is up to 17%, and the total organic sulfur content of some gas wells reaches 557.7mg/m3 (Sutianyou, Zhangjing. research on organic sulfur removal technology of high sulfur natural gas. oil and gas chemical industry, 2007, 36 (6) 470-474). These sulfur compounds not only reduce the heat capacity of natural gas but also are toxic, environmentally hazardous, unhealthy and highly corrosive, so that desulfurization of natural gas is necessary before its use or transportation.
The method for removing organic sulfur from natural gas is mainly characterized by that according to the form and content of sulfur in natural gas it utilizes analysis and calculation to define process route. At present, there are four main organic sulfur removal processes commonly used at home and abroad, namely, a hydroconversion method, a pyrolysis method, a hydrolysis method and an adsorption method. The first three processes are all to convert organic sulfur into H under the action of catalyst2S, removing by adopting other inorganic sulfur removal methods; the adsorption method is to adsorb organic sulfur in gas by adopting adsorbent, so that the content of organic sulfur in gas is qualified, and the saturated organic sulfur is difficult to regenerate at normal temperature, for example, the adsorbent is directly replaced, although the investment is less, the replacement cost of the adsorbent is high every year, the labor intensity is high during replacement, and the replaced adsorbent containing organic sulfur belongs to dangerous solid waste and is difficult to treat.
Compared with the method, the method has the advantages that the process combining adsorption and conversion is selected, organic sulfur is enriched in the adsorption bed layer, the enriched organic sulfur is regenerated and converted into inorganic sulfur through high-temperature catalysis, and then the inorganic sulfur is removed. The method has the advantages of low energy consumption, stable system, higher organic sulfur removal efficiency, effective reduction of environmental pollution and the like, and has great development prospect.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for deeply removing organic sulfur from natural gas, which can efficiently remove multi-component organic sulfur in the natural gas, such as carbonyl sulfur, carbon disulfide, methyl mercaptan, ethanethiol, methyl sulfide, propanethiol, butanethiol, dimethyl disulfide, ethyl sulfide and the like, and the total organic sulfur content in product gas after the organic sulfur is removed<20mg/Nm3。
The technical scheme adopted by the invention for solving the technical problems is as follows:
a method for removing organic sulfur from natural gas is characterized by comprising the following steps:
(a) wet desulphurization 1: removing H from natural gas containing inorganic sulfur and organic sulfur at normal temperature by a wet desulphurization method2S, making H in the desulfurized gas2S content<20mg/Nm3；
(b) Temperature swing adsorption 1: enabling the natural gas obtained in the step (a) to pass through a fixed bed layer of a special organic sulfur removal adsorbent from the top of an adsorption tower, enabling all carbonyl sulfur, carbon disulfide, methyl mercaptan, ethanethiol, methyl sulfide, propanethiol, butanethiol, dimethyl disulfide, ethanesulfide and thiophene in the natural gas to be adsorbed on the adsorbent, enabling the rest components to pass through the adsorbent and then be taken as a purified natural gas product for outward transportation, and purifying the total organic sulfur content in the natural gas<20mg/Nm3；
(c) And (3) cooling by blowing: separating purified natural gas obtained in the step (b) into 6-12% of total gas amount, performing air cooling on the adsorption tower subjected to pre-air cooling to reduce the temperature of the adsorption tower subjected to pre-air cooling to 50-80 ℃, and discharging the rest purified natural gas after pressure reduction;
(d) pre-blowing for cooling: pre-blowing the adsorption tower subjected to heating regeneration at the temperature of 70-120 ℃ to reduce the temperature of the adsorption tower from 290-340 ℃ to 150-200 ℃, wherein the temperature of pre-blown cold air is 200-260 ℃;
(e) heat exchange: exchanging heat of the pre-blown cold air in the step (d) with a heat exchanger to 340-380 ℃;
(f) and (3) heating: feeding the high-temperature regeneration gas subjected to heat exchange in the step (e) into the pre-heated adsorption tower from the bottom of the pre-heated adsorption tower, heating and regenerating the pre-heated adsorption tower to enable the temperature of a bed layer to reach 300-340 ℃, and regenerating organic sulfur adsorbed in the bed layer with the high-temperature gas;
(g) preheating: introducing the high-temperature regeneration gas in the step (f) from the bottom of a saturated adsorption tower, and pre-heating the adsorption tower which is saturated in adsorption under the normal temperature condition to raise the temperature to 220-260 ℃;
(h) heating: heating the organic sulfur-containing regenerated gas in the step (g) to 390-420 ℃ through a heater;
(i) organic sulfur conversion: enabling the heated regeneration gas in the step (h) to pass through a fixed bed reactor of an organic sulfur catalyst, converting organic sulfur into inorganic sulfur under a high-temperature catalysis condition, then exchanging heat with the pre-blown cold air in the step (e), and enabling the temperature of the regeneration gas to reach 180-220 ℃ after heat exchange;
(j) water cooling: carrying out heat exchange on the regenerated gas in the step (i) and circulating water, and cooling to 35-45 ℃;
(k) and 2, wet desulphurization: removing H in the water-cooled regeneration gas obtained in the step (j) at normal temperature by a wet desulphurization method2S, making H in the desulfurized gas2S content<6.0mg/Nm3；
(L) temperature swing adsorption 2: the regenerated gas after the wet desulphurization 2 in the step (K) is subjected to a temperature swing adsorption 1 method to further remove the organic sulfur which is not completely converted in the regenerated gas, so that the total organic sulfur content in the regenerated gas<20mg/Nm3And then incorporated into the purified natural gas for export as a product.
In the above technical solution, preferably, the wet desulfurization in step (a) and step (k) is one or more combined processes of MDEA desulfurization, LO-CAT desulfurization, EDTA complexed iron desulfurization, and sulphonamide desulfurization.
Preferably, the temperature swing adsorption in step (b) is composed of 5-8 identical adsorption towers, program control valves and pipelines, the adsorption tower is filled with a special desulfurization adsorbent, and the performance indexes of the adsorption tower require: the pore diameter is 10-20>80 percent, and the specific surface area is 1500-1800 m2(ii)/g, organic sulfur static adsorption capacity 15-20%.
Preferably, the step (L) temperature swing adsorption 2 is a small-scale plant similar to the temperature swing adsorption 1, consisting of 3 to 6 identical adsorption columns, process control valves and piping.
Preferably, the organic sulfur catalyst of step (i) is a specific catalyst with high conversion rate, and under the active condition, the conversion rate of carbonyl sulfur and carbon disulfide is more than 99%, the conversion rate of mercaptan is more than 95%, and the conversion rate of thioether is more than 25%.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) the natural gas yield is high: after the organic sulfur is regenerated by the regenerated gas, the regenerated gas is heated and catalytically converted into inorganic sulfur to be removed, and then the regenerated gas returns to the product gas, so that basically no natural gas is lost.
(2) The energy consumption is low: the heating and cooling processes of the fixed bed layer of the adsorption tower effectively utilize the thermal efficiency of the regenerated gas through multiple heat exchange, and the bed layer is heated after the high-temperature regenerated gas and the low-temperature regenerated gas after organic sulfur conversion are heated, so that the requirement of heat energy is reduced.
(3) Equipment is few, and is efficient, convenient operation: the whole device adopts the automatic program control of the program valve, no field personnel operate, and the personnel cost is saved.
(4) The organic sulfur removal efficiency is high: the overall organic sulfur removal efficiency was > 98%.
(5) Environmental protection, safety, running cost are low: no waste gas and waste liquid are discharged, the adsorbent is repeatedly recycled for 3-5 years, and is periodically recycled and replaced by a manufacturer.
Drawings
FIG. 1 is a block flow diagram of embodiment 1 of the present invention.
FIG. 2 is a process flow diagram of the present invention.
Wherein, the names corresponding to the reference numbers in the attached figure 2 are:
1-27-pipelines, T-1001A-F-adsorption towers, T-1002-organic sulfur conversion towers, T-1003-desulfurization towers, E1001 AB-heat exchangers, E1002 AB-preheaters, E1003 AB-heaters, E1004-coolers, V1001-gas-liquid separators, TSA-temperature swing adsorption complete equipment and Kv 1001-kV 1010A-F-program control valves.
Detailed Description
The present invention will be described in further detail with reference to examples and drawings, but the present invention is not limited to these examples.
Example 1
(1) The raw material gas composition (mol%) is: 92.20% of methane, 0.12% of ethane, 0.01% of propane, 0.01% of isobutane, 0.01% of n-butane, 6.74% of carbon dioxide, 0.09% of nitrogen, 0.01% of hydrogen, 460ppm of hydrogen sulfide, 64.50ppm of carbonyl sulfide, 1.04ppm of carbon disulfide, 85.10ppm of methyl mercaptan, 13.8ppm of ethyl mercaptan, 8.58ppm of methyl sulfide, 15.00ppm of propyl mercaptan, 1.00ppm of butyl mercaptan, 0.01ppm of dimethyl disulfide, 0.01ppm of ethyl sulfide and 0.01ppm of thiophene, the pressure: 3.5MPa, temperature: 30 ℃, gas amount: 350kmol/H, passing through LO-CAT desulfurizing tower, H in gas2S content of 6mg/Nm3。
(b) Enabling the natural gas subjected to inorganic sulfur removal to pass through a fixed bed layer of a special organic sulfur removal adsorbent, so that all carbonyl sulfur, carbon disulfide, methyl mercaptan, ethanethiol, methyl sulfide, propanethiol, butanethiol, dimethyl disulfide, ethanesulfide and thiophene in the natural gas are adsorbed on the adsorbent, wherein the natural gas passing through an adsorption tower comprises the following components: 98.15% of methane, 0.13% of ethane, 0.01% of propane, 0.01% of isobutane, 0.01% of n-butane, 1.44% of carbon dioxide, 0.09% of nitrogen, 0.01% of hydrogen, 4.0ppm of hydrogen sulfide, 4.0ppm of carbonyl sulfide, 0ppm of carbon disulfide, 4.66ppm of methyl mercaptan, 0.50ppm of ethyl mercaptan, 0ppm of methyl sulfide, 0.50ppm of propyl mercaptan, 0.04ppm of butyl mercaptan, 0ppm of dimethyl disulfide, 0ppm of ethyl sulfide and 0ppm of thiophene, and is used as an export product of purified natural gas, the total organic sulfur content of the purified natural gas is 9.7ppm,<20mg/Nm3。
(c) and separating the purified natural gas by 29.6kmol/h, and performing blow cooling on the adsorption tower subjected to pre-blow cooling, so that the temperature of the adsorption tower subjected to pre-blow cooling is reduced to 52.4 ℃, the temperature of regenerated gas is subjected to heat exchange to 120 ℃, and the rest purified natural gas is discharged after being decompressed to 3.29 Mpa.
(d) And pre-blowing and cooling the adsorption tower subjected to heating regeneration by using the regeneration gas of 120 ℃ to reduce the temperature of the adsorption tower from 310 ℃ to 160 ℃, and exchanging heat for the pre-blown and cooled regeneration gas to 260 ℃.
(e) Then the regenerated gas at 260 ℃ and the high-temperature gas converted from the organic sulfur in the heat exchanger exchange heat to 360 ℃, and then the preheating adsorption tower is heated and regenerated, so that the temperature of the bed layer reaches 310 ℃, and the organic sulfur adsorbed in the bed layer is regenerated along with the high-temperature gas.
(f) The regenerated high-temperature regenerated gas containing organic sulfur enters from the bottom of the saturated adsorption tower, and the adsorption tower saturated in adsorption under normal temperature is preheated to 220 ℃.
(g) The regenerated gas containing organic sulfur after heat exchange is heated to 390 ℃ by a heater and then enters a fixed bed reactor of an organic sulfur catalyst, carbonyl sulfur and carbon disulfide mainly generate hydrolysis reaction to generate inorganic sulfur under the high-temperature catalysis condition, methyl mercaptan, ethanethiol, methyl sulfide, propyl mercaptan, butyl mercaptan, dimethyl disulfide and ethyl sulfide mainly generate thermal cracking reaction to generate inorganic sulfur, meanwhile, methyl mercaptan and methyl sulfide also generate hydrogenation reaction with a small amount of hydrogen in natural gas to generate inorganic sulfur, the temperature of the regenerated gas after conversion of the organic sulfur is 384.3 ℃, the pressure is 3.37 MPa, and the gas quantity: 36.72kmol/h, the regeneration gas composition (mol%) is: 79.30% of methane, 0.03% of ethane, 0% of propane, 0% of isobutane, 0% of n-butane, 14.38% of carbon dioxide, 0.08% of nitrogen, 0.9% of hydrogen, 0.17% of hydrogen sulfide, 4.0ppm of carbonyl sulfide, 0ppm of carbon disulfide, 0ppm of methyl mercaptan, 0ppm of ethanethiol, 0ppm of methyl sulfide, 0ppm of propanethiol, 0ppm of butanethiol, 0ppm of dimethyl disulfide, 0ppm of ethylsulfide and 0ppm of thiophene, and cooling the regenerated gas in the gas (e) process to normal temperature through circulating water after heat exchange and cooling.
(h) After the regenerated gas cooled to normal temperature passes through an LO-CAT desulfurizing tower, most of hydrogen sulfide and a small amount of carbon dioxide are removed, and then purified regenerated gas components (mol%) obtained through gas separation are as follows: 86.16% of methane, 0.03% of ethane, 0% of propane, 0% of isobutane, 0% of n-butane, 12.50% of carbon dioxide, 0.08% of nitrogen, 0.9% of hydrogen, 19.0ppm of hydrogen sulfide, 4.0ppm of carbonyl sulfide, 0ppm of carbon disulfide, 0ppm of methyl mercaptan, 0ppm of ethyl mercaptan, 0ppm of methyl sulfide, 0ppm of propyl mercaptan, 0ppm of butyl mercaptan, 0ppm of dimethyl disulfide, 0ppm of ethyl sulfide and 0ppm of thiophene, the pressure: 3.34MPa, temperature: 40.5 ℃, gas amount: 33.72 kmol/h.
(i) The purified regenerated gas is subjected to temperature swing adsorption 2, organic sulfur in the regenerated gas is further removed, and then the purified regenerated gas and the purified natural gas are jointly used as products for outward transportation to obtain the pressure of the products for outward transportation: 3.29MPa, temperature: 30.7 ℃, gas amount: 333.03kmol/h, the components (mol%) of the product gas are methane 96.93%, ethane 0.12%, propane 0.01%, isobutane 0.01%, n-butane 0.01%, carbon dioxide 2.56%, nitrogen 0.09%, hydrogen 0.1%, hydrogen sulfide 5.0ppm, carbonyl sulfur 4.0ppm, carbon disulfide 0ppm, methyl mercaptan 5.0ppm, ethanethiol 1.0ppm, methyl sulfide 0ppm, propyl mercaptan 1.0ppm, butyl mercaptan 0ppm, dimethyl disulfide 0.01ppm, ethyl sulfide 0.01ppm and thiophene 0.01ppm, the product meets the national standard of GB17820-2012 natural gas for total sulfur<60mg/m3Hydrogen sulfide<6 mg/m3A class of product requirements。
The temperature swing adsorption 1 is completed by at least 5 adsorption towers through five steps of adsorption, preheating, heating, preheating blowing and cooling respectively, and the 5 adsorption towers are staggered in time to form a complete circulation system so that a product and regenerated gas are continuously output; the temperature swing adsorption 2 is completed by at least 3 adsorption towers through three steps of adsorption, temperature rise and temperature reduction, and the 3 adsorption towers are staggered in time to form a complete circulating system so that purified regeneration gas and product regeneration gas are continuously output.
Claims (3)
1. A method for deeply removing organic sulfur from natural gas is characterized by comprising the following steps: the method comprises the following steps:
(a) wet desulphurization 1: removing H from natural gas containing inorganic sulfur and organic sulfur at normal temperature by a wet desulphurization method2S, making H in the desulfurized gas2S content<6.0mg/Nm3；
(b) Temperature swing adsorption 1: enabling the natural gas obtained in the step (a) to pass through a fixed bed layer of a special organic sulfur removal adsorbent from the top of an adsorption tower, enabling all carbonyl sulfur, carbon disulfide, methyl mercaptan, ethanethiol, methyl sulfide, propanethiol, butanethiol, dimethyl disulfide, ethanesulfide and thiophene in the natural gas to be adsorbed on the adsorbent, enabling the rest components to pass through the adsorbent and then be taken as a purified natural gas product for outward transportation, and purifying the total organic sulfur content in the natural gas<20mg/Nm3；
(c) And (3) cooling by blowing: separating purified natural gas obtained in the step (b) into 6-12% of total gas amount, performing air cooling on the adsorption tower subjected to pre-air cooling to reduce the temperature of the adsorption tower subjected to pre-air cooling to 50-80 ℃, and discharging the rest purified natural gas after pressure reduction;
(d) pre-blowing for cooling: pre-blowing the adsorption tower subjected to heating regeneration by using the cold blowing gas with the temperature of 70-120 ℃ obtained in the step (c) to cool the adsorption tower, so that the temperature of the adsorption tower is reduced from 290-340 ℃ to 150-200 ℃, and the temperature of the pre-blown cold gas is subjected to heat exchange to 200-260 ℃;
(e) heat exchange: exchanging heat of the pre-blown cold air in the step (d) with a heat exchanger to 340-380 ℃;
(f) and (3) heating: feeding the high-temperature regeneration gas subjected to heat exchange in the step (e) into the pre-heated adsorption tower from the bottom of the pre-heated adsorption tower, heating and regenerating the pre-heated adsorption tower to enable the temperature of a bed layer to reach 300-340 ℃, and regenerating organic sulfur adsorbed in the bed layer with the high-temperature gas;
(g) preheating: introducing the high-temperature regeneration gas in the step (f) from the bottom of a saturated adsorption tower, and pre-heating the adsorption tower which is saturated in adsorption under the normal temperature condition to raise the temperature to 220-260 ℃;
(h) heating: heating the organic sulfur-containing regenerated gas in the step (g) to 390-420 ℃ through a heater;
(i) organic sulfur conversion: enabling the heated regeneration gas in the step (h) to pass through a fixed bed reactor of an organic sulfur catalyst, converting organic sulfur into inorganic sulfur under a high-temperature catalysis condition, then exchanging heat with the pre-blown cold air in the step (e), and enabling the temperature of the regeneration gas to reach 180-220 ℃ after heat exchange;
(j) water cooling: carrying out heat exchange on the regenerated gas in the step (i) and circulating water, and cooling to 35-45 ℃;
(k) and 2, wet desulphurization: removing H in the water-cooled regeneration gas obtained in the step (j) at normal temperature by a wet desulphurization method2S, making H in the desulfurized gas2S content<6.0mg/Nm3；
(L) temperature swing adsorption 2: the regenerated gas after the wet desulphurization 2 in the step (K) is subjected to a temperature swing adsorption 1 method to further remove the organic sulfur which is not completely converted in the regenerated gas, so that the total organic sulfur content in the regenerated gas<20mg/Nm3Then the purified natural gas is merged into the product for output,
wherein the content of the first and second substances,
the temperature swing adsorption 1 in the step (b) is composed of 5-8 identical adsorption towers, program control valves and pipelines, the adsorption towers are filled with special organic sulfur removal adsorbents, and the performance indexes of the adsorption towers require that: the specific surface area is 1500-1800 m2(ii)/g, the organic sulfur static adsorption capacity is 15-20%.
2. The method for deeply removing organic sulfur from natural gas according to claim 1, characterized in that: the wet desulphurization in the step (a) and the step (k) is one or more combined processes of MDEA desulphurization, LO-CAT desulphurization, EDTA complex iron desulphurization and sulphonamide desulphurization.
3. The method for deeply removing organic sulfur from natural gas according to claim 1, characterized in that: the organic sulfur catalyst in the step (i) is a special catalyst with high conversion rate, and under the active condition, the conversion rate of carbonyl sulfur and carbon disulfide is more than 99 percent, the conversion rate of mercaptan is more than 95 percent, and the conversion rate of thioether is more than 25 percent.
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