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WO2009095849A2 - Technique de purification en profondeur des gaz de synthèse et sa première application dans une usine pilote de traitement d'huiles à base de charbon - Google Patents

Technique de purification en profondeur des gaz de synthèse et sa première application dans une usine pilote de traitement d'huiles à base de charbon Download PDF

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Publication number
WO2009095849A2
WO2009095849A2 PCT/IB2009/050320 IB2009050320W WO2009095849A2 WO 2009095849 A2 WO2009095849 A2 WO 2009095849A2 IB 2009050320 W IB2009050320 W IB 2009050320W WO 2009095849 A2 WO2009095849 A2 WO 2009095849A2
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WIPO (PCT)
Prior art keywords
deep
oxygen
ppm
remove
purification technology
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Application number
PCT/IB2009/050320
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English (en)
Other versions
WO2009095849A3 (fr
Inventor
Yuhua Kong
Mailing Zhao
Hongjun Hu
Dianming Hu
Junming Chen
Xinhui Zhao
Xianhou Wang
Zhenrong Yu
Huilin Zheng
Lili Jia
Yulong Li
Xiaoding Li
Bing Xu
Yangang Huang
Lili Zhang
Qingjian Zhang
Original Assignee
Shaanxi Jin Chao Investment Corporation
Hubei Research Institute Of Chemistry
Shanghai Design Institute Of Chemical Industry
Van Der Walt, Louis, Stephanus
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Shaanxi Jin Chao Investment Corporation, Hubei Research Institute Of Chemistry, Shanghai Design Institute Of Chemical Industry, Van Der Walt, Louis, Stephanus filed Critical Shaanxi Jin Chao Investment Corporation
Priority to AU2009208699A priority Critical patent/AU2009208699B8/en
Publication of WO2009095849A2 publication Critical patent/WO2009095849A2/fr
Publication of WO2009095849A3 publication Critical patent/WO2009095849A3/fr

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
    • C01B3/50—Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification
    • C01B3/56—Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification by contacting with solids; Regeneration of used solids
    • C01B3/58—Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification by contacting with solids; Regeneration of used solids including a catalytic reaction
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
    • C01B2203/04—Integrated processes for the production of hydrogen or synthesis gas containing a purification step for the hydrogen or the synthesis gas
    • C01B2203/0435—Catalytic purification
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
    • C01B2203/04—Integrated processes for the production of hydrogen or synthesis gas containing a purification step for the hydrogen or the synthesis gas
    • C01B2203/0435—Catalytic purification
    • C01B2203/045—Purification by catalytic desulfurisation
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
    • C01B2203/04—Integrated processes for the production of hydrogen or synthesis gas containing a purification step for the hydrogen or the synthesis gas
    • C01B2203/0465—Composition of the impurity
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
    • C01B2203/04—Integrated processes for the production of hydrogen or synthesis gas containing a purification step for the hydrogen or the synthesis gas
    • C01B2203/0465—Composition of the impurity
    • C01B2203/0485—Composition of the impurity the impurity being a sulfur compound

Definitions

  • This invention relates to a deep purification technology of syngas based on coal, coke, heavy oil, residual oil or natural gas, which can remove COS and H 2 S to ⁇ 5ppb respectively, total sulfur (Ts, H 2 S + COS) ⁇ 10ppb, chlorine to ⁇ 10ppb, Fe(CO) 5 + Ni(CO) 4 to ⁇ 20ppb, oxygen to ⁇ 1 ppm, arsenic to ⁇ 20ppb.
  • the lifetime of methanol synthesis catalysts is usually 2 years, the lifetime of F-T synthesis catalysts is 8-12 months.
  • the charge of the synthesis catalysts is large, their cost are high.
  • the charge of the methanol synthesis catalyst is 100-200 tons and it costs 10-20 millions RMB, the charge of F-T synthesis catalyst is 500-1000 tons and it costs 75-150 millions RMB, consequently it is urgent to prolong the lifetime of these synthesis catalysts.
  • Sulfur-poisoning Content of Ts (H 2 S+COS) in the syngas after Rectisol is usually ⁇ 0.1 ppm, not ⁇ 0.01 ppm, when operation condition fluctuate, Ts can be increased to> 0.1 ppm. It is an important result that the lifetime of synthesis catalyst had been 3 years Lunan Methanol Plant in Shandong City (1 ⁇ 10 4 1 methanol/year) some years ago and the sulfur content of the discharged catalyst analyzed by National Quality Supervision and Test Center for Chemical Catalysts was 0.16%. Sulfur-poisoning is the characteristic of accumulation.
  • Ts of syngas must be removed to ⁇ 0.01 ppm, while chlorine must be removed to ⁇ 0.01 ppm, Fe(CO) 5 + Ni(CO) 4 must be removed to ⁇ 0.02ppm, oxygen must be removed to ⁇ 1 ppm, arsenic must be removed to ⁇ 0.02ppm, consequently it is very necessary to use the deep purification technology.
  • the invention aims to use a deep purification technology of syngas based on coal, coke, heavy oil, residual oil or natural gas, which can remove COS and H 2 S to ⁇ 5ppb respectively, total sulfur (Ts, H 2 S + COS) ⁇ 10ppb, chlorine to ⁇ 10ppb, Fe(CO) 5 + Ni(CO) 4 to ⁇ 20ppb, oxygen to ⁇ 1 ppm, arsenic to ⁇ 20ppb.
  • Ts, H 2 S + COS total sulfur
  • F-T synthesis catalyst can be prolonged from 8-12 months to 2-3 years
  • catalysts producing acetic acid, anhydride acetic acid, butyl alcohol- octyl alcohol etc. can be prolonged considerably.
  • the syngas from Rectisol based on coal, coke, heavy oil, residual oil or natural gas including 0.01 ⁇ 1 Oppm H 2 S + COS, 0.01 -5ppm chlorine, 0.02-5ppm Fe(CO) 5 + Ni(CO) 4 ,
  • No.1 deep purification tower loads EH-5 deep hydrolysis catalyst and HTS-1/HTS-2 deep fine desulfurizer, EH-5 deep hydrolysis catalyst to hydrolysis COS to H 2 S, then
  • HTS-1 or HTS-2 deep fine desulfurizer removes H 2 S to ensure COS and H 2 S ⁇ 5ppb respectively, H 2 S + COS ⁇ 10ppb.
  • No.3 deep purification tower loads CTO- 1 oxygen-removal catalyst and TAS- 1 arsenic-removal agent, CTO-1 oxygen-removal catalyst remove oxygen ⁇ 1 ppm,
  • EH-5 deep hydrolysis catalyst composed of alkaline metal (20-40%) and TiO 2 /AI 2 O 3
  • HTS-1 and HTS-2 deep fine desulfurizer composed of CuO (30-50%) and FeO
  • ET-3A protective agent composed of CaO (8-42%), ZnO (8-30%), AI 2 O 3 (10-45%) and
  • ET-3A protective agent composed of ZnO (10-30%) and CuO (3-20%), active carbon support rest.
  • CTO-1 oxygen-removal catalyst composed of CeO (1 -10%), CuO (1 -15%), MoO 3
  • TAS- 1 arsenic-removal agent composed of ZnO (25-65%), CuO (20-50%) and AI 2 O 3
  • Above deep purification technology must composed of deep hydrolysis catalyst and deep fine desulfurizer, while, according to syngas feedstock, applied condition and customer demand, need use partly or all ET-3A and ET-8A protective agent, CTO-1 oxygen-removal catalyst, TAS- 1 arsenic-removal agent.
  • composition of deep hydrolysis catalyst, deep fine desulfurizer, protective agent, oxygen-removal catalyst, arsenic-removal agent all is mass percent.
  • deep hydrolysis catalyst deep fine desulfurizer, protective agent, oxygen-removal catalyst, arsenic-removal agent all are pressured quickly to 150kg/cm 2 , then decompressed quickly to ordinary pressure, through 100 times circulation, their crush strength do not have big change, so they all can be used on 150kg/cm 2 pressure.
  • EH-5 deep hydrolysis catalyst used in the invention remove COS to ⁇ 5ppb under space velocity 6000-1200Oh “1 and 30-200 degree C
  • HTS-1 or HTS-2 deep fine desulfurizer removes H 2 S to ⁇ 5ppb under space velocity 4000-800Oh “1 and 10-250 degree C (30-150 degree C is best).
  • ET-3A protective agent used in the invention removes chlorine to ⁇ 0.01 ppm under space velocity 300Oh "1 and 10-280 degree C.
  • ET-8A protective agent used in the invention removes Fe(CO) 5 + Ni(CO) 4 to ⁇ 0.02ppm under space velocity 5000-700Oh "1 and 10-250 degree C.
  • CTO-1 oxygen-removal catalyst used in the invention removes oxygen to ⁇ 1 ppm under space velocity 3000 ⁇ 6000h ⁇ 1 and 30-300 degree C (60-200 degree C is best).
  • TAS-1 arsenic-removal agent used in the invention removes arsenic to ⁇ 0.02ppm under space velocity 3000 ⁇ 6000h ⁇ 1 and 10-160 degree C.
  • syngas feedstock coal, coke, heavy oil, residual oil or natural gas
  • used production process, product demand, above several guard or purifying agent can be used, in general, deep hydrolysis catalyst and deep fine desulfurizer must be used, oxygen-removal catalyst and chlorine-removal protective agent need be used in coal to oil plant, chlorine-removal and Fe(CO) 5 + Ni(CO) 4 - removal protective agent need be used in methanol plant, so according to different demand, above deep purification technology can composed of 3 or 2 or 1 deep purification towers.
  • the invention can be used in coal to oil, methanol, acetic acid, anhydride acetic acid, butyl alcohol- octyl alcohol, dimethyl ether and dimethyl carbonate etc. plants, especially be used in fine chemical industry plant based on coal to protect expensive catalyst, noble metal catalyst or ensure product quality.
  • toxicants content of syngas can be removed to following level: H 2 S ⁇ 5ppb, COS ⁇ 5ppb, T s ( H 2 S+COS) ⁇ 10ppb, chlorine ⁇ 10ppb, Fe(CO) 5 + Ni(CO) 4 ⁇ 20ppb, oxygen ⁇ 1 ppm, arsenic ⁇ 20ppb.
  • the life of methanol synthesis catalyst can be prolonged from 2 years (do not use the invention) to 4 years, can ensure change methanol synthesis catalyst once only every two times overhaul, taking a 660x10 3 1 methanol/year plant for instance, following economy effect can be gotten:
  • the plant will decrease a overhaul every four years, can increase 20 days production time, and produce methanol 40 ⁇ 10 3 1 (1980 tons per day), according to 500 RMB profits every ton methanol, the sum is 20 ⁇ 10 6 RMB, the benefit is 5 ⁇ 10 6 RMB per year.
  • the life of F-T synthesis catalyst can be prolonged from 8-12 months (do not use the invention) to 2-3 years, The plant will decrease 2-3 times replacements of F-T synthesis catalyst every three years, taking a 480x10 3 t oil/year plant for instance, following economy effect can be gotten:
  • Figure 1 shows flow sheet of deep purification technology for syngas based on coal, coke, heavy oil, residual oil or natural gas.
  • the syngas from Rectisol passes in order No.1 deep purification tower for deep fine sulfur-removal, No.2 deep purification tower for deep chlorine-removal and Fe(CO) 5 + Ni(CO) 4 -removal, No.3 deep purification tower for oxygen and arsenic-removal to get qualified syngas.
  • the technology was applied in Baoji 10000 ton-class coal-to-oil plant of Shanxi Jinchao Investment Corporation.
  • Came from wet desulfurization process (Vegetable tannin extract), crude syngas (its flow-rate 1000Nm 3 /h, 40-60 degree C, 0.7- 1 .0MPa, H 2 S--150mg/Nm 3 , chlorine ⁇ 1 ⁇ 10 "6 , O 2 2000 ⁇ 4000ppm) passes of ATFSR technology (Ts can be removed to 0.1 ⁇ 1 ppm) and deep purification technology (according to demand of the plant, the technology is composed of deep hydrolysis catalyst, deep fine desulfurizer, chlorine-removal protective agent and oxygen-removal catalyst), then is sent to F-T synthesis reactor, there are H 2 S 3ppb, COS 3ppb, CS 2 5ppb, chlorine 8ppb and O 2 0.8ppm in the refined syngas.
  • CS 2 content of syngas is very trace ( ⁇ 1 ppb), so it is not necessary to use deep CS 2 fine desulfurizer.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Combustion & Propulsion (AREA)
  • Inorganic Chemistry (AREA)
  • Catalysts (AREA)
  • Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)

Abstract

L'invention se rapporte à une technique de purification en profondeur des gaz de synthèse à base de charbon, de coke, d'huile lourde, d'huile résiduelle ou de gaz naturel. Le gaz de synthèse comprenant 0,01 à 10 ppm de H2S + COS, 0,01 à 5 ppm de chlore, 0,02 à 5 ppm de composé carbonyle métallique, 1 à 5000 ppm d'oxygène, 0,02 à 2 ppm d'arsenic, traverse un catalyseur d'hydrolyse en profondeur, un dispositif de désulfuration fin en profondeur, du chlore, du Fe(CO)5 + Ni(CO)4, de l'oxygène, un agent protecteur éliminant l'arsenic ou un agent purificateur pour éliminer le mélange H2S + COS jusqu'à une quantité inférieure à 0,01 ppm (à savoir 10 ppb), le chlore jusqu'à une quantité inférieure à 0,01 ppm (à savoir 10 ppb), le composé carbonyle jusqu'à une quantité inférieure à 0,02 ppm (à savoir 20 ppb), l'oxygène jusqu'à une quantité inférieure à 1 ppm, l'arsenic jusqu'à une quantité inférieure à 0,02 ppm (à savoir 20 ppb), pour s'assurer que la durée de vie du catalyseur pour la synthèse du méthanol soit prolongée de 2 à 4-6 ans, que la durée de vie du catalyseur pour la synthèse FT puisse être prolongée de 8-12 mois à 2-3 ans, et pour que la durée de vie des catalyseurs au Pd, Pt, Rh, Au, Ag etc. produisant de l'acide acétique, de l'anhydride acétique, de l'alcool butylique, de l'alcool octylique puisse être considérablement prolongée.
PCT/IB2009/050320 2008-02-03 2009-01-27 Technique de purification en profondeur des gaz de synthèse et sa première application dans une usine pilote de traitement d'huiles à base de charbon WO2009095849A2 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AU2009208699A AU2009208699B8 (en) 2008-02-03 2009-01-27 Deep purification technology of syngas and its first application in a coal-based oil pilot plant

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Application Number Priority Date Filing Date Title
CN200810046867.5 2008-02-03
CN2008100468675A CN101224871B (zh) 2008-02-03 2008-02-03 合成气的深度净化方法

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WO2009095849A3 WO2009095849A3 (fr) 2009-12-10

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ZA (1) ZA200900792B (fr)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2013067287A1 (fr) * 2011-11-03 2013-05-10 Fluor Technologies Corporation Conversion de composés organiques du souffre en sulfure d'hydrogène dans un effluent de réacteur de synthèse d'alcool mixte
CN104624197A (zh) * 2015-01-30 2015-05-20 武汉科林精细化工有限公司 一种脱氧脱硫双功能精脱硫剂及其制备方法

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CN102219186B (zh) * 2010-04-15 2012-11-14 中国石油化工股份有限公司 合成气中羰基铁和羰基镍的脱除方法
CN102259835B (zh) 2011-06-20 2013-03-27 中国科学院广州能源研究所 一种基于熔融盐特性的粗合成气净化提质方法
CN102390807B (zh) * 2011-08-10 2013-02-13 西南化工研究设计院 一种铜系净化剂
CN103372369A (zh) * 2012-04-13 2013-10-30 中国石油化工股份有限公司 一种脱除合成气中微量杂质的方法及合成气的应用
CN103372364A (zh) * 2012-04-13 2013-10-30 中国石油化工股份有限公司 一种脱除合成气中羰基金属化合物的方法
CN102814160A (zh) * 2012-08-20 2012-12-12 西南化工研究设计院有限公司 一种脱除合成气中羰基铁、镍的净化剂及其制备和应用
CN103432896B (zh) * 2013-08-23 2015-09-09 西南化工研究设计院有限公司 一种脱除合成气等还原性气体中杂质氧的净化剂及其制备和应用
CN105776138A (zh) * 2016-04-25 2016-07-20 张家港市华昌新材料科技有限公司 一种合成气净化的方法
CN110272021B (zh) * 2018-03-13 2021-04-13 国家能源投资集团有限责任公司 甲醇催化剂保护剂及其制备方法
KR20210018932A (ko) * 2018-06-12 2021-02-18 할도르 토프쉐 에이/에스 저-철 촉매를 사용한 메탄올 제조 과정
CN110052113A (zh) * 2019-05-23 2019-07-26 河南开祥精细化工有限公司 一种用于降低低压反应尾气中羰基镍含量的方法
CN113562698A (zh) * 2021-06-29 2021-10-29 湖北宜化化工股份有限公司 一种原料气脱氧净化的方法
CN113999085B (zh) * 2021-12-02 2023-12-22 西安元创化工科技股份有限公司 一种烃类原料深度净化方法

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MY140997A (en) * 2004-07-22 2010-02-12 Shell Int Research Process for the removal of cos from a synthesis gas stream comprising h2s and cos

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2013067287A1 (fr) * 2011-11-03 2013-05-10 Fluor Technologies Corporation Conversion de composés organiques du souffre en sulfure d'hydrogène dans un effluent de réacteur de synthèse d'alcool mixte
CN104624197A (zh) * 2015-01-30 2015-05-20 武汉科林精细化工有限公司 一种脱氧脱硫双功能精脱硫剂及其制备方法

Also Published As

Publication number Publication date
AU2009208699B8 (en) 2014-09-11
AU2009208699A8 (en) 2014-09-11
CN101224871A (zh) 2008-07-23
ZA200900792B (en) 2009-12-30
WO2009095849A3 (fr) 2009-12-10
AU2009208699B2 (en) 2014-05-01
AU2009208699A1 (en) 2009-08-06
CN101224871B (zh) 2011-02-16

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