WO2011112693A2 - Removal of selenium from refinery wastewater - Google Patents

Removal of selenium from refinery wastewater Download PDF

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Publication number
WO2011112693A2
WO2011112693A2 PCT/US2011/027711 US2011027711W WO2011112693A2 WO 2011112693 A2 WO2011112693 A2 WO 2011112693A2 US 2011027711 W US2011027711 W US 2011027711W WO 2011112693 A2 WO2011112693 A2 WO 2011112693A2
Authority
WO
WIPO (PCT)
Prior art keywords
liquid
amount
selenium
ppm
ferric salt
Prior art date
Legal status (The legal status 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 status listed.)
Ceased
Application number
PCT/US2011/027711
Other languages
English (en)
French (fr)
Other versions
WO2011112693A3 (en
Inventor
Daniel E. Schwarz
Jitendra T. Shah
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
ChampionX LLC
Original Assignee
Nalco Co LLC
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
Priority to AU2011224425A priority Critical patent/AU2011224425B2/en
Priority to CN201180013277.2A priority patent/CN102791638B/zh
Priority to BR112012022753-0A priority patent/BR112012022753B1/pt
Priority to NZ602343A priority patent/NZ602343A/xx
Priority to KR1020127023689A priority patent/KR101818954B1/ko
Priority to JP2012557207A priority patent/JP5791639B2/ja
Priority to MX2012010442A priority patent/MX2012010442A/es
Priority to EP11753993.2A priority patent/EP2545006B1/en
Application filed by Nalco Co LLC filed Critical Nalco Co LLC
Priority to CA2792614A priority patent/CA2792614C/en
Priority to SG2012067039A priority patent/SG183994A1/en
Publication of WO2011112693A2 publication Critical patent/WO2011112693A2/en
Publication of WO2011112693A3 publication Critical patent/WO2011112693A3/en
Anticipated expiration legal-status Critical
Priority to ZA2012/06877A priority patent/ZA201206877B/en
Ceased legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/72—Treatment of water, waste water, or sewage by oxidation
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F9/00—Multistage treatment of water, waste water or sewage
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
    • C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
    • C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
    • C02F1/5245—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents using basic salts, e.g. of aluminium and iron
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/58—Treatment of water, waste water, or sewage by removing specified dissolved compounds
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/58—Treatment of water, waste water, or sewage by removing specified dissolved compounds
    • C02F1/62—Heavy metal compounds
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/72—Treatment of water, waste water, or sewage by oxidation
    • C02F1/722—Oxidation by peroxides
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/72—Treatment of water, waste water, or sewage by oxidation
    • C02F1/76—Treatment of water, waste water, or sewage by oxidation with halogens or compounds of halogens
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/72—Treatment of water, waste water, or sewage by oxidation
    • C02F1/78—Treatment of water, waste water, or sewage by oxidation with ozone
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/10—Inorganic compounds
    • C02F2101/20—Heavy metals or heavy metal compounds
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
    • C02F2103/18—Nature of the water, waste water, sewage or sludge to be treated from the purification of gaseous effluents

Definitions

  • This invention relates to compositions of matter and methods of using them to remove selenium from fluids.
  • Selenium compounds are reported to comprise 0.9 ppm of the earth's crust.
  • Selenium is an important as a trace mineral used to make the enzyme glutathione peroxidase, which is involved in fat metabolism and therefore is found in many living organisms. It is commonly found in various amounts in crude oil, coal, and other fossil fuels originating from the decomposed organic matter or leached out of the nearby minerals.
  • selenium is known to be highly toxic and it can cause harm even in small quantities. Harmful effects include dermatitis, central nervous system disturbance, nephrosis, hemorrhagic necrosis of the pancreas and adrenal cortex, and when in large enough dosages, death. As a result, many localities have limited the permissible amount of selenium in domestic supplies of water at 10 ppb. As a result, wastewater produced from activity involving selenium-containing materials is difficult to dispose of. In addition, because of its toxicity, even these strict standards may be uniformly further limited in the future.
  • At least one embodiment of the invention is directed towards a method of removing selenium from a liquid comprising the steps of: adding an oxidant to the liquid, adjusting the liquid's pH to below 7.5, adding ferric salt in an amount such that less than a quarter of selenium in the liquid precipitates, and adding a dithiocarbamate material to the liquid in an amount such that the amount of dithiocarbamate groups in the material (in ppm) is greater than the amount of ferric salt (in ppm).
  • the dithiocarbamate material may be selected from the group consisting of PDTC, DTC, and any combination thereof.
  • the liquid may be water.
  • the water may be sour stripper water.
  • the pH may be lowered by the addition of sulfuric acid, HC1, H3PO4, and any combination thereof.
  • the ferric salt may be selected from the group consisting of ferric sulfate, ferric chloride, ferrous sulfate, ferrous chloride, and any combination thereof.
  • the ferric salt may be added in an amount of between 1-300 ppm.
  • the dithiocarbamate material may be between 50% to 300% of the amount (in ppm) of ferric salt added to the liquid.
  • the method may comprise adding a sulfur bearing coagulant to the liquid. The method may reduce the amount of selenium in the liquid from more than 1000 ppb to less than 40 ppb.
  • the oxidant may be selected from the list consisting of hydrogen peroxide, ozone, KMn0 4 , NaClO, C10 2 , peracetic acid, sodium percarbonate, carbamide peroxide, sodium persulfate, and any combination thereof.
  • FIG. 1 is a flowchart illustrating one embodiment of the inventive method.
  • PDTC means poly dithiocarbamate which includes all forms of polymers which have dithiocarbamate functional groups present.
  • DTC dithiocarbamate
  • Senite means a selenium bearing composition of matter having a chemical formula of HSeC .
  • Standard Water means a liquid waste product produced as a byproduct of chemical, and more typically petrochemical, processing.
  • Stripping refers to a process that removes byproducts, such as ammonia and hydrogen sulfide, along with a portion of water from a liquid stream. Stripping is commonly performed in a distillation column in which the liquid stream flows down the column and gas flows up the column to "strip" off contaminants from the liquid. "Stripper Sour Water” means sour water that has been run through a stripper process.
  • Washwater means water generated from any industrial plant or industrial process the byproducts therefrom.
  • selenium is removed from a selenium containing liquid by a method comprising the steps of: adding an oxidant to the liquid, adjusting the liquid's pH to below 7 (preferably 6), adding ferric salt in an amount such that less than a quarter of selenium in the liquid precipitates and adding a poly dithiocarbamate material to the liquid in an amount such that the amount of poly dithiocarbamate material (in ppm) is greater than the amount of ferric salt (in ppm).
  • the oxidant is selected from the list consisting of hydrogen peroxide ozone, KMn0 4 , NaClO, C10 2 , peracetic acid, sodium percarbonate, carbamide peroxide, sodium persulfate, and any combination thereof.
  • the pH is lowered by the addition of an acid selected from the list consisting of sulfuric acid HC1, H 3 P0 4 , and any combination thereof.
  • the ferric salt is selected from the group consisting of ferric sulfate, ferric chloride, ferrous sulfate, ferrous chloride, and any combination thereof.
  • the ferric salt is added in an amount of between 1-300 ppm.
  • the poly dithiocarbamate material is between 50% to 300% of the amount (in ppm) of ferric salt added to the liquid.
  • the pH, pE, voltage potential, and SHE standard hydrogen electrode
  • the pH, pE, voltage potential, and SHE standard hydrogen electrode
  • the water is stripper sour water from an oil refinery.
  • the selenium removal is a particular accomplishment as the repeated passage of the sour water through a distillation column results in an ever-increasing concentration of selenium in the sour water.
  • sour stripper water is generally highly reducing so most of the selenium is in the form of selenite, selenocyanates and other organic selenium species. Successive experimentation has shown that the inventive method effectively removes more than 95% of the selenium in stripper sour water.
  • the ratio of iron material to PDTC is important and must be tuned for each water source.
  • the ratio of iron material to PDTC is 1 :4 mols of iron sulfate to mols of dithiocarbamate functional groups (using a 10% actives iron sulfate solution).
  • the ratio of iron material to PDTC is 1 :2.
  • the ideal range falls between the two examples and is entirely water dependant.
  • the above methods are performed using DTC in the place of PDTC.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Removal Of Specific Substances (AREA)
  • Treatment Of Water By Oxidation Or Reduction (AREA)
  • Separation Of Suspended Particles By Flocculating Agents (AREA)
  • Paper (AREA)
PCT/US2011/027711 2010-03-10 2011-03-09 Removal of selenium from refinery wastewater Ceased WO2011112693A2 (en)

Priority Applications (11)

Application Number Priority Date Filing Date Title
MX2012010442A MX2012010442A (es) 2010-03-10 2011-03-09 Eliminacion de selenio de aguas residuales de refineria.
BR112012022753-0A BR112012022753B1 (pt) 2010-03-10 2011-03-09 método de retirada de selênio de um líquido
NZ602343A NZ602343A (en) 2010-03-10 2011-03-09 Removal of selenium from refinery wastewater
KR1020127023689A KR101818954B1 (ko) 2010-03-10 2011-03-09 정제 폐수로부터 셀레늄의 제거
JP2012557207A JP5791639B2 (ja) 2010-03-10 2011-03-09 製油所廃液からセレンの除去
EP11753993.2A EP2545006B1 (en) 2010-03-10 2011-03-09 Removal of selenium from refinery wastewater
CA2792614A CA2792614C (en) 2010-03-10 2011-03-09 Removal of selenium from refinery wastewater
AU2011224425A AU2011224425B2 (en) 2010-03-10 2011-03-09 Removal of selenium from refinery wastewater
CN201180013277.2A CN102791638B (zh) 2010-03-10 2011-03-09 从炼油废水中除去硒
SG2012067039A SG183994A1 (en) 2010-03-10 2011-03-09 Removal of selenium from refinery wastewater
ZA2012/06877A ZA201206877B (en) 2010-03-10 2012-09-13 Removal of selenium from refinery wastewater

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US12/721,139 2010-03-10
US12/721,139 US8282835B2 (en) 2010-03-10 2010-03-10 Removal of selenium from refinery wastewater

Publications (2)

Publication Number Publication Date
WO2011112693A2 true WO2011112693A2 (en) 2011-09-15
WO2011112693A3 WO2011112693A3 (en) 2012-01-05

Family

ID=44558954

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/US2011/027711 Ceased WO2011112693A2 (en) 2010-03-10 2011-03-09 Removal of selenium from refinery wastewater

Country Status (15)

Country Link
US (1) US8282835B2 (enExample)
EP (1) EP2545006B1 (enExample)
JP (1) JP5791639B2 (enExample)
KR (1) KR101818954B1 (enExample)
CN (1) CN102791638B (enExample)
AR (1) AR080392A1 (enExample)
AU (1) AU2011224425B2 (enExample)
BR (1) BR112012022753B1 (enExample)
CA (1) CA2792614C (enExample)
MX (1) MX2012010442A (enExample)
NZ (1) NZ602343A (enExample)
SG (1) SG183994A1 (enExample)
TW (1) TWI561477B (enExample)
WO (1) WO2011112693A2 (enExample)
ZA (1) ZA201206877B (enExample)

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WO2017070345A1 (en) * 2015-10-21 2017-04-27 The Texas A & M University System Methods for treating selenocyanate in wastewater

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PL2812100T3 (pl) * 2012-02-06 2020-11-02 Nalco Company Kontrola korozji w systemach mokrego płukania gazów spalinowych
KR101798316B1 (ko) * 2013-06-28 2017-11-15 미츠비시 히타치 파워 시스템즈 칸쿄 솔루션 가부시키가이샤 셀레늄 제거 방법 및 셀레늄 제거 장치
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JP6204146B2 (ja) * 2013-10-16 2017-09-27 三菱重工業株式会社 排水処理方法及び排水処理装置
CN104556540B (zh) * 2013-10-22 2016-11-16 中国石油化工股份有限公司 一种含硒废水的处理方法
CN104556543B (zh) * 2013-10-29 2017-02-08 中国石油化工股份有限公司 一种含硒废水的处理方法
PL3068733T3 (pl) * 2013-11-11 2020-05-18 Nalco Company Sposób usuwania selenu ze strumieni ścieków
CN105712569B (zh) * 2014-12-05 2018-04-10 中国石油化工股份有限公司 一种含硒废水的深度处理方法
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US11084743B2 (en) 2015-10-21 2021-08-10 Texas A&M University System Method for removal of recalcitrant selenium species from wastewater
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Cited By (3)

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Publication number Priority date Publication date Assignee Title
WO2017070345A1 (en) * 2015-10-21 2017-04-27 The Texas A & M University System Methods for treating selenocyanate in wastewater
US11235994B2 (en) 2015-10-21 2022-02-01 The Texas A & M University System Methods for treating selenocyanate in wastewater
US11987512B2 (en) 2015-10-21 2024-05-21 The Texas A&M University System Methods for treating selenocyanate in wastewater

Also Published As

Publication number Publication date
JP2013522008A (ja) 2013-06-13
KR101818954B1 (ko) 2018-01-17
JP5791639B2 (ja) 2015-10-07
MX2012010442A (es) 2013-02-26
EP2545006A2 (en) 2013-01-16
CN102791638B (zh) 2014-10-22
TW201144236A (en) 2011-12-16
AR080392A1 (es) 2012-04-04
AU2011224425B2 (en) 2015-09-03
AU2011224425A1 (en) 2012-09-27
CA2792614A1 (en) 2011-09-15
TWI561477B (en) 2016-12-11
US8282835B2 (en) 2012-10-09
SG183994A1 (en) 2012-10-30
WO2011112693A3 (en) 2012-01-05
CA2792614C (en) 2018-03-27
KR20130073867A (ko) 2013-07-03
BR112012022753A2 (pt) 2019-09-10
BR112012022753B1 (pt) 2021-05-25
ZA201206877B (en) 2013-05-29
EP2545006A4 (en) 2014-12-31
NZ602343A (en) 2013-08-30
EP2545006C0 (en) 2025-03-19
EP2545006B1 (en) 2025-03-19
CN102791638A (zh) 2012-11-21
US20110220583A1 (en) 2011-09-15

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