WO2014084756A1 - Procédé de préparation combinée de gaz d'hydrocarbure - Google Patents

Procédé de préparation combinée de gaz d'hydrocarbure Download PDF

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Publication number
WO2014084756A1
WO2014084756A1 PCT/RU2013/000764 RU2013000764W WO2014084756A1 WO 2014084756 A1 WO2014084756 A1 WO 2014084756A1 RU 2013000764 W RU2013000764 W RU 2013000764W WO 2014084756 A1 WO2014084756 A1 WO 2014084756A1
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Prior art keywords
gas
hydrocarbon
mercaptans
purification
regeneration
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PCT/RU2013/000764
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English (en)
Russian (ru)
Inventor
Андрей Владиславович КУРОЧКИН
Original Assignee
Kurochkin Andrei Vladislavovich
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Publication of WO2014084756A1 publication Critical patent/WO2014084756A1/fr

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
    • C10L3/00—Gaseous fuels; Natural gas; Synthetic natural gas obtained by processes not covered by subclass C10G, C10K; Liquefied petroleum gas
    • C10L3/06—Natural gas; Synthetic natural gas obtained by processes not covered by C10G, C10K3/02 or C10K3/04
    • C10L3/10—Working-up natural gas or synthetic natural gas
    • C10L3/101—Removal of contaminants
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
    • B01D53/75—Multi-step processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
    • B01D53/86—Catalytic processes
    • B01D53/8603—Removing sulfur compounds
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
    • B01D53/86—Catalytic processes
    • B01D53/8603—Removing sulfur compounds
    • B01D53/8612—Hydrogen sulfide
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2251/00—Reactants
    • B01D2251/10—Oxidants
    • B01D2251/11—Air
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2252/00—Absorbents, i.e. solvents and liquid materials for gas absorption
    • B01D2252/20—Organic absorbents
    • B01D2252/202—Alcohols or their derivatives
    • B01D2252/2023—Glycols, diols or their derivatives
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2252/00—Absorbents, i.e. solvents and liquid materials for gas absorption
    • B01D2252/20—Organic absorbents
    • B01D2252/204—Amines
    • B01D2252/20431—Tertiary amines
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2256/00—Main component in the product gas stream after treatment
    • B01D2256/24—Hydrocarbons
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/30—Sulfur compounds
    • B01D2257/304—Hydrogen sulfide
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/30—Sulfur compounds
    • B01D2257/306—Organic sulfur compounds, e.g. mercaptans
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/70—Organic compounds not provided for in groups B01D2257/00 - B01D2257/602
    • B01D2257/702—Hydrocarbons
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/80—Water
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/26—Drying gases or vapours
    • B01D53/261—Drying gases or vapours by adsorption
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/26—Drying gases or vapours
    • B01D53/263—Drying gases or vapours by absorption
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
    • C10L2290/00—Fuel preparation or upgrading, processes or apparatus therefore, comprising specific process steps or apparatus units
    • C10L2290/54—Specific separation steps for separating fractions, components or impurities during preparation or upgrading of a fuel
    • C10L2290/541—Absorption of impurities during preparation or upgrading of a fuel
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
    • Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters

Definitions

  • the invention relates to the preparation of hydrocarbon gas, in particular to methods of purification from moisture, C 5+ hydrocarbons, mercaptans and hydrogen sulfide, and may find application in the oil and gas, oil and gas processing, as well as the petrochemical industry in preparation for transport or for use as fuel gas .
  • Oxidation is carried out in an alkaline environment with oxygen or air at elevated pressure, at room temperature or elevated temperature, in the presence of a homogeneous or heterogeneous transition metal catalyst.
  • a known group of methods for cleaning gases from mercaptans [RF Patent N ° SU 1272542, IPC B01D53 / 14, publ. 04/27/1997, RF Patent ⁇ SU1341807, IPC B01D53 / 14, B01D53 / 48, publ. 04/27/1997, RF Patent Jfe SU1681434, IPC B01D53 / 14, B01D53 / 48, publ. 04/27/1997] which describes alkaline-free methods for purifying hydrocarbon gas from mercaptans by oxidizing them with elemental sulfur to organic di- and polysulfides in medium liquid high-boiling hydrocarbon fraction in the presence of a catalyst - organic compounds containing a tertiary nitrogen atom.
  • the proposed methods do not provide for the purification of hydrocarbon gas from heavy hydrocarbons, hydrogen sulfide and water vapor, and also lead to gas pollution by vapors of a high boiling hydrocarbon fraction.
  • Known methods have the following disadvantages: low yield of the prepared gas due to losses of components of the feed gas with low-pressure weathering and / or regeneration gases, the complexity of the technology due to the need for separate utilization of by-products of each of the used cleaning stages, high energy costs during absorption or adsorption gas purification from heavy hydrocarbons and mercaptans, consumption of chemicals during alkaline utilization of mercaptan-containing regeneration gases, environmental pollution of the environment through water effluents of alkaline utilization of mercaptan-containing regeneration gases, and emissions into the atmosphere of products of combustion of low-pressure weathering gases and exhaust gas from the stage of utilization of hydrogen sulfide-containing regeneration gas to produce sulfur.
  • the objective of the invention is to increase the yield of prepared gas, simplifying the technology, reducing its material and energy consumption, reducing environmental pollution by water effluents and gas emissions of harmful substances.
  • the specified technical result is achieved by the fact that in the method of complex preparation of hydrocarbon gas, including multi-stage purification from heavy hydrocarbons, mercaptans, hydrogen sulfide and drying, to obtain purified gas and regeneration gases, as well as the utilization of acid regeneration gas to produce sulfur and exhaust gas, a feature is preliminary mixing of hydrocarbon gas with a mixture of regeneration gases and exhaust gas and subsequent absorption purification by chemisorbent to obtain an organic phase, water, and pre-purified gas, sent for further purification by known methods, while a hydrocarbon solution of sulfur, organic di- and polysulfides, as well as a catalytic amount of organic a compound containing a tertiary nitrogen atom, which is obtained by mixing the organic phase with sulfur in an amount providing complete oxidative conversion of mercaptans.
  • Mercaptans that dissolve in chemisorbent react with dissolved sulfur and sulfur dioxide, usually present in the exhaust gas, by known reactions catalyzed by compounds with a tertiary nitrogen atom to form disulfides and polysulfides - components of chemisorbent.
  • sulfur is consumed in the chemisorbent, its amount is replenished, for example, with sulfur obtained from the utilization of acid gas, and an excess amount of the organic phase is removed from the unit.
  • An organic compound with a tertiary nitrogen atom can have any phase state, and the optimal concentration of the catalyst in chemisorbent depends on its nature (for example, for ⁇ , ⁇ '-tetramethyldipropylenetriamine - 0.5-3.0% of the mass).
  • Pre-mixing the hydrocarbon gas with a mixture of regeneration gases and exhaust gas allows to completely prevent losses and increase the yield of prepared hydrocarbon gas due to the recirculation of regeneration gases and exhaust gas into the stream of gas to be purified.
  • the absorption treatment of the resulting gas mixture with chemisorbent to obtain the organic phase and water allows the main amount of heavy hydrocarbons and mercaptans to be removed from the gas to be cleaned and thereby reduce energy consumption and reduce the weight and size characteristics and metal consumption of the equipment at the stage of topping, as well as remove reaction water from the installation, formed during the utilization of acid gas.
  • chemisorbent by mixing the organic phase with sulfur in an amount that ensures the complete oxidative conversion of mercaptans makes it possible to purify the gas using by-products of its purification - heavy hydrocarbons, organic di- and polysulfides, and sulfur, which reduces the material consumption of the process.
  • the method is as follows.
  • Hydrocarbon gas (I) is mixed with a mixture of (II) regeneration gases and exhaust gas, and subjected to absorption purification by mixing with chemisorbent (III), as well as a nitrogen-containing organic compound - catalyst (IV), and subsequent separation of the mixture in a cooled separator 1 into gas (V), the aqueous phase (VI) and the organic phase (VII).
  • the chemisorbent absorbs sulfur vapor and aerosol, the main amount of heavy hydrocarbons and mercaptans, and partially sulfur dioxide from a mixture of gases (I) and (II).
  • chemisorbent Mercaptans dissolved in chemisorbent react in the presence of a catalyst with sulfur and sulfur dioxide according to known reactions with the formation of disulfides and polysulfides - components of chemisorbent.
  • a chemisorbent is prepared by adding a catalyst and liquid sulfur (dotted line in the diagram) to the recycled part of the organic phase (VIII). The balance part of the organic phase (VII) is removed from the installation.
  • Gas (V) after purification by chemisorbent is purified from the remaining heavy hydrocarbons and mercaptans in a known manner (for example, by adsorption or absorption purification) on the topping unit for 2 s obtaining stripped gas (IX) and fatty gas regeneration (X).
  • the stripped gas (IX) is then purified from hydrogen sulfide in a known manner (for example, by adsorption or amine purification) on the desulfurization unit 3 to obtain a desulfurized stripped gas (XI) and an acidic regeneration gas (XII).
  • the desulfurized stripped gas (XI) is dried in a known manner (for example, by adsorption or glycol drying) on the drying unit 4 to obtain the prepared gas (XIII) discharged from the plant and a regeneration gas (XIV) containing water vapor.
  • the regeneration acid gas (XII) is disposed of in a known manner on the catalytic unit 5 by catalytic oxidation of hydrogen sulfide with an oxygen-containing gas (XV), for example, air, to produce sulfur (XVI) and exhaust gas (XVII) containing sulfur vapor, reaction water, unreacted hydrogen sulfide and sulfur dioxide, which is sent for mixing with the regeneration gases (X) and (XIV).
  • XV oxygen-containing gas
  • a method for complex preparation of hydrocarbon gases including preliminary purification of hydrocarbon gas mixed with regeneration gases and exhaust gas of the stage of utilization of acid gas of regeneration by absorption with a chemisorbent, which is a hydrocarbon solution of sulfur, disulfides, polysulfides and catalytic the amount of an organic compound containing a tertiary nitrogen atom, with further oxidation of the absorbed mercaptans with sulfur to form m chemisorbent component, followed by additional purification gas from heavy hydrocarbons and mercaptans, hydrogen sulfide and water vapor, and recycling a stream of purified gas mixture regeneration gas and the exhaust gas recycling the acidic regeneration step of gas.
  • a chemisorbent which is a hydrocarbon solution of sulfur, disulfides, polysulfides and catalytic the amount of an organic compound containing a tertiary nitrogen atom
  • the claimed invention meets the patentability criterion of "novelty.”
  • b The authors' studies proved that sequential purification of hydrocarbon gas by absorption by chemisorbent based on the products of sulfur oxidation of mercaptans, topping (removal of heavy hydrocarbons), desulfurization and drying, with recirculation of topping and drying regeneration gases, and acid gas exhaust gas allows the hydrocarbon to be cleaned efficiently. gas from heavy hydrocarbons, mercaptans, hydrogen sulfide and water vapor, as well as utilize regeneration gases, preventing pollution of the environment s.
  • the claimed invention meets the patentability criterion of "inventive step”.
  • the invention is illustrated by the following example.
  • Example 1 Hydrocarbon gas composition,% vol .: oxygen 0.03, nitrogen 10.90, carbon dioxide 0.28, methane 70, 10, ethane 5.61, propane 4.02, n-butane 2.65, isobutane 1, 14, isopentane 1, 35, pentane and higher 2.06, hydrogen sulfide 1, 64, mercaptans 0.24, with a humidity corresponding to a dew point of 25 ° C, in order to prepare for transport, they are mixed in a stream with regeneration gases, exhaust gas and chemisorbent, and separated at 30 ° C.
  • the separated gas is sequentially stripped on sibunite synthetic carbon adsorbent, purified from hydrogen sulfide by adsorption with a 50% aqueous solution of methyldiethanolamine, and dried on a composite absorbent.
  • the regeneration gases of the topping and drying stages are recycled to the hydrocarbon gas to be purified, and the acid gas of the regeneration is purified from hydrogen sulfide by direct oxidation with oxygen at an elevated temperature in the presence of a solid catalyst mixed with a stoichiometric amount of air and recirculated exhaust gas.
  • Liquid sulfur is separated from the oxidation products at 130 ° C, the exhaust gas is partially recirculated, and the balance part is mixed with the gas to be purified.
  • Part of the liquid sulfur is periodically added to the organic phase, separated during gas separation from the mixture with chemisorbent, containing 0.5% of the mass.
  • chemisorbent containing 0.5% of the mass.
  • the prepared gas has a composition,% vol.: Oxygen, nitrogen 1 1, 60, carbon dioxide 0.21, methane 74.3, ethane 5.95, propane 3.94, n-butane 1, 88, isobutane 1, 06 , isopentane 1, 06, n-pentane and higher ot, hydrogen sulfide 0.002, mercaptans ot, and a water dew point of -60 ° C, which meets the requirements of STO 089-2010.
  • the proposed method can find application in the oil and gas, oil and gas processing, as well as the petrochemical industry.
  • the claimed invention meets the patentability criterion of "industrial applicability”.

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Health & Medical Sciences (AREA)
  • Biomedical Technology (AREA)
  • Analytical Chemistry (AREA)
  • Organic Chemistry (AREA)
  • Gas Separation By Absorption (AREA)

Abstract

L'invention concerne un procédé de préparation de gaz d'hydrocarbure et notamment des procédés d'élimination de l'humidité, des hydrocarbures С5+, des mercaptans et d'hydrogène sulfuré, et peut s'utiliser dans l'industrie pétrolière et gazeuse, dans la transformation de gaz et de pétrole ainsi que dans l'industrie pétrochimique lors de la préparation au transport ou pour l'utilisation en qualité de gaz combustible. On propose un procédé de préparation combinée de gaz d'hydrocarbure comprenant l'élimination des hydrocarbures lourds, des mercaptans, de l'hydrogène sulfuré et le séchage, avec obtention de gaz purifié et de gaz régénérés, ainsi que le recyclage du gaz régénéré avec obtention de soufre et de gaz sortant, le gaz d'hydrocarbure étant préalablement mélangé à un mélange de gaz régénérés et de gaz sortant et soumis à une purification par absorption par un agent de sorption chimique, avec obtention de phase organique, d'eau et de gaz préalablement purifié envoyé au stade de purification ultérieure. En outre, on utilise en tant qu'agent de sorption chimique une solution d'hydrocarbure de soufre, de di- et polysulfures organiques et d'une quantité catalytique d'un composé organique comprenant un atome tertiaire d'azote qui est obtenu par le mélange d'une phase organique avec du soufre assurant une transformation par oxydation complète des mercaptans. Le résultat technique obtenu grâce à la mise en oeuvre de l'invention consiste en un plus grand rendement de gaz préparé, une simplification de la technologie, une baisse de la consommation de matériaux et de l'énergie du processus, une baisse de la part des métaux dans l'équipement, une réduction de la pollution de l'environnement par les effluents aqueux basiques et les rejets gazeux polluants.
PCT/RU2013/000764 2012-09-10 2013-09-03 Procédé de préparation combinée de gaz d'hydrocarbure WO2014084756A1 (fr)

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RU2012138830 2012-09-10
RU2012138830/05A RU2509597C1 (ru) 2012-09-10 2012-09-10 Способ комплексной подготовки углеводородного газа

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RU2571126C1 (ru) * 2014-10-27 2015-12-20 Андрей Владиславович Курочкин Способ подготовки сероводород- и меркаптансодержащего попутного нефтяного газа

Citations (4)

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Publication number Priority date Publication date Assignee Title
RU2239593C1 (ru) * 2003-10-07 2004-11-10 Институт катализа им. Г.К. Борескова СО РАН Способ разложения сероводорода и/или меркаптанов
EA200900511A1 (ru) * 2006-10-05 2009-08-28 Шелл Интернэшнл Рисерч Маатсхаппий Б.В. Способ удаления меркаптанов
US7780933B2 (en) * 2005-07-08 2010-08-24 Chiyoda Corporation Method of removing sulfur compounds from natural gas
US20120216678A1 (en) * 2009-08-11 2012-08-30 Frank Haiko Geuzebroek Absorbent composition and process for removing co2 and/or h2s from a gas comprising co2 and/or h2s

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SU1089799A1 (ru) * 1982-04-08 1996-01-27 Всесоюзный научно-исследовательский институт углеводородного сырья Способ очистки газов от сернистых соединений
CA1339890C (fr) * 1989-05-26 1998-06-02 Vijay Kumar Chopra Methode pour eliminer un gaz acide dans un melange gazeux qui en renferme
EP1116511A1 (fr) * 2000-01-17 2001-07-18 Gastec N.C. Procédé pour éliminer des composés sulfurés de mélanges gazeux
EP1338557B1 (fr) * 2000-10-18 2005-03-23 Jgc Corporation Procede et appareil destines a eliminer un compose sulfure a partir d'un gaz contenant de l'hydrogene sulfure, du mercaptan, du dioxyde de carbone et un hydrocarbure aromatique
RU2395329C2 (ru) * 2007-11-19 2010-07-27 Общество С Ограниченной Ответственностью "Газпром Трансгаз-Кубань" Способ осушки и очистки природного газа

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RU2239593C1 (ru) * 2003-10-07 2004-11-10 Институт катализа им. Г.К. Борескова СО РАН Способ разложения сероводорода и/или меркаптанов
US7780933B2 (en) * 2005-07-08 2010-08-24 Chiyoda Corporation Method of removing sulfur compounds from natural gas
EA200900511A1 (ru) * 2006-10-05 2009-08-28 Шелл Интернэшнл Рисерч Маатсхаппий Б.В. Способ удаления меркаптанов
US20120216678A1 (en) * 2009-08-11 2012-08-30 Frank Haiko Geuzebroek Absorbent composition and process for removing co2 and/or h2s from a gas comprising co2 and/or h2s

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