KR970070244A - Descaling method of stainless steel and chromium and / or nickel alloy steel, pickling composition and pickling waste recycling method - Google Patents

Descaling method of stainless steel and chromium and / or nickel alloy steel, pickling composition and pickling waste recycling method Download PDF

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KR970070244A
KR970070244A KR1019970013885A KR19970013885A KR970070244A KR 970070244 A KR970070244 A KR 970070244A KR 1019970013885 A KR1019970013885 A KR 1019970013885A KR 19970013885 A KR19970013885 A KR 19970013885A KR 970070244 A KR970070244 A KR 970070244A
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fluoride
nitrate
acid
sulfate
ammonium
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KR1019970013885A
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KR100230011B1 (en
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이기원
이을규
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이기원
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Priority to DE69718589T priority Critical patent/DE69718589T2/en
Priority to EP97920962A priority patent/EP0835333B9/en
Priority to US08/983,602 priority patent/US6361613B2/en
Priority to PCT/KR1997/000069 priority patent/WO1997041278A1/en
Priority to IDP971432A priority patent/ID16846A/en
Priority to JP9538753A priority patent/JP3053651B2/en
Priority to TW086105678A priority patent/TW515852B/en
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
    • C23G1/24—Cleaning or pickling metallic material with solutions or molten salts with neutral solutions
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
    • C23G1/36—Regeneration of waste pickling liquors

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  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)

Abstract

스테인레스강 및, 크롬 및/또는 니켈 합금강 제조의 열처리시 합금강의 표면에 형성된 산화 및 탄화스케일 제거방법이 개시되어 있다.A method of removing oxidized and carbide scales formed on the surface of alloy steel during heat treatment of stainless steel and chromium and / or nickel alloy steel production is disclosed.

이 방법은 질산염 및 불화물염을 필수성분으로 함유한 산세액으로 스케일이 형성된 합금강을 처리함을 포함한다.This method involves treating scaled alloy steel with a pickling solution containing nitrate and fluoride salt as essential components.

본 발명의 방법에 사용되는 산세액에 함유된 질산염 및 불화물염은 종래에 사용되던 활성이 보다 강한 질산 및 불산의 혼산과 비교해 볼 때 스케일 제거효율이 오히려 우수하고, 유해가스가 발생되지 않으며, 폐수처리가 용이할 뿐만 아니라 종래의 전처리과정을 생략할 수도 있다.The nitrate and fluoride salts contained in the pickling solution used in the method of the present invention have a rather excellent scale removal efficiency, and do not generate harmful gases, compared to the conventionally used mixed acid of nitric acid and hydrofluoric acid. Not only is the treatment easy, but the conventional pretreatment may be omitted.

산세액에는 보조성분을 함유시킬 수도 있다.The pickling solution may contain an auxiliary component.

질산염 및 불화물염을 함유한 산세조성물 및 산세폐액 재생방법이 또한 제공된다.Also provided are pickling compositions containing nitrates and fluoride salts and methods for regenerating pickling liquor.

Description

스테인레스강 및 크롬 및/또는 니켈 합금강의 스케일제거방법, 이에 사용되는 산세조성물 및 산세폐액 재생방법Descaling method of stainless steel and chromium and / or nickel alloy steel, pickling composition and pickling waste recycling method

본 내용은 요부공개 건이므로 전문내용을 수록하지 않았음As this is a public information case, the full text was not included.

제1도는 본 발명에 따라 냉각하여 산세폐액을 재생하는 방법의 실시에 사용되는 공정개략도.1 is a process schematic diagram used in the practice of a method for cooling and recovering pickling liquor according to the invention.

Claims (21)

표면에 스케일이 형성된 스테인레스강 및 크롬 및/또는 니켈 합금강을 질산염과 불화물염을 함유한 산세액으로 처리함을 포함하는, 스테인레스강 및 크롬 및/또는 니켈 합금강의 탄화 및 산화스케일 제거방법.A method of carbonizing and oxidizing scale of stainless steel and chromium and / or nickel alloy steel, comprising treating the stainless steel and chromium and / or nickel alloy steel having scales on the surface with a pickling solution containing nitrate and fluoride salt. 제1항에 있어서, 상기 산세액은 나아가 황산, 황산염, 인산, 인산염, 과산화물, 아민 및 아미드류, 질산, 술폰산 및 술폰산염으로 구성되는 그룹에서 선택된 보조제를 1종 이상 함유함을 특징으로 하는 방법.The method of claim 1, wherein the pickling solution further comprises at least one auxiliary agent selected from the group consisting of sulfuric acid, sulfates, phosphoric acid, phosphates, peroxides, amines and amides, nitric acid, sulfonic acid and sulfonate. . 제1항 및 제2항 중 어느 한 항에 있어서, 상기 산세액으로 처리하기 전에 전처리 공정을 거침을 특징으로 하는 방법.The method according to any one of claims 1 to 2, characterized in that it undergoes a pretreatment step before treating with the pickling solution. 제3항에 있어서, 상기 전처리 공정은 숏블라스트(Shot-Blast), 염욕(Salt bath) 침지 또는 중성염전해의 방법으로 수행됨을 특징으로 하는 방법.The method of claim 3, wherein the pretreatment is performed by shot-blast, salt bath immersion or neutral salt electrolysis. 제1항 및 제2항 중 어느 한 항에 있어서, 상기 방법은 어떠한 전처리 공정을 거치지 않음을 특징으로 하는 방법.The method of claim 1, wherein the method does not undergo any pretreatment. 제1항 및 제2항 중 어느 한 항에 있어서, 상기 질산염은 질산나트륨, 아질산나트륨, 질산바륨, 질산칼륨, 질산칼슘, 아질산칼륨 및 질산암모늄으로 구성되는 그룹에서 선택된 1종 이상이며, 상기 불화물염은 규불화암모늄, 규불화나트륨, 규불화마그네슘, 산성불화칼륨, 산성불화암모늄, 산성불화나트륨, 붕불화수소산, 붕불화암모늄, 불화칼륨, 불화나트륨, 불화바륨, 규불화칼륨 및 규불화망간으로 구성되는 그룹에서 선택된 1종 이상임을 특징으로 하는 방법.The nitrate according to any one of claims 1 and 2, wherein the nitrate is at least one selected from the group consisting of sodium nitrate, sodium nitrite, barium nitrate, potassium nitrate, calcium nitrate, potassium nitrite and ammonium nitrate. Salts include ammonium fluoride, sodium fluoride, magnesium silicate, potassium acid fluoride, acidic ammonium fluoride, acidic acid fluoride, hydrofluoric acid, ammonium fluoride, potassium fluoride, sodium fluoride, barium fluoride, potassium fluoride and manganese fluoride Method characterized in that at least one selected from the group consisting of. 제2항에 있어서, 상기 황산염은 황산마그네슘, 황산망간, 황산나트륨, 황산칼륨, 황산암모늄, 과황산암모늄 및 아황산암모늄으로 구성되는 그룹에서 선택됨을 특징으로 하는 방법.The method of claim 2, wherein the sulfate is selected from the group consisting of magnesium sulfate, manganese sulfate, sodium sulfate, potassium sulfate, ammonium sulfate, ammonium persulfate and ammonium sulfite. 제2항에 있어서, 상기 인산염은 인산나트륨, 인산암모늄, 피로인산나트륨, 산성피로인산나트륨, 인산칼슘 및 인산칼륨으로 구성되는 그룹에서 선택됨을 특징으로 하는 방법.The method of claim 2, wherein the phosphate salt is selected from the group consisting of sodium phosphate, ammonium phosphate, sodium pyrophosphate, sodium pyrophosphate, calcium phosphate and potassium phosphate. 제2항에 있어서, 상기 아민 및 아미드화합물은 헥사메틸렌디아민, 디에틸아민, 디메틸아민, 디에틸에탄올아민, 디에틸티오우레아, 디메틸티오우레아. 디에틸렌디아민, 시클로헥실아민, 황산아미노구아니딘, 에탄올아민 등으로 구성되는 그룹에서 선택됨을 특징으로 하는 방법.The method of claim 2, wherein the amine and the amide compound are hexamethylenediamine, diethylamine, dimethylamine, diethylethanolamine, diethylthiourea, dimethylthiourea. Diethylenediamine, cyclohexylamine, aminoguanidine sulfate, ethanolamine and the like. 제1항 및 제2항 중 어느 한 항에 있어서, 상기 질산염, 불화물염 및 보조제는 이들 성분들을 각각 또는 이들을 함께 조합한 혼합물 형태로 처리됨을 특징으로하는 방법.3. The method of claim 1, wherein the nitrate, fluoride salt, and adjuvants are treated in the form of a mixture of each of these components or a combination thereof. 질산염 및 불화물염을 포함하여 이루어지는 스테인레스강 및 크롬 및/또는 니켈 합금강의 표면에 형성된 스케일 제거용 산세조성물.A descaling pickling composition formed on the surface of stainless steel and chromium and / or nickel alloy steel including nitrate and fluoride salts. 제11항에 있어서, 상기 조성물중 질산염 및 불화물염은 질산이온과 불산이온의 몰당량비를 기준으로 1:9-0:1로 조성됨을 특징으로 하는 산세조성물.12. The pickling composition according to claim 11, wherein the nitrate and fluoride salt in the composition is 1: 9-0: 1 based on the molar equivalent ratio between nitrate ions and fluoride ions. 제1항 및 제2항 중 어느 한 항에 있어서, 상기 질산염은 질산나트륨, 아질산나트륨, 질산바륨, 질산칼륨, 질산칼슘, 아질산칼륨 및 질산암모늄으로 구성되는 그룹에서 선택된 1종 이상이며, 상기 불화물염은 규불화암모늄, 규불화나트륨, 규불화마그네슘, 산성불화칼륨, 산성불화암모늄, 산성불화나트륨, 붕불화수소산, 붕불화암모늄, 불화칼륨, 불화나트륨, 불화바륨, 규불화칼륨 및 규불화망간으로 구성되는 그룹에서 선택된 1종 이상임을 특징으로 하는 조성물.The nitrate according to any one of claims 1 and 2, wherein the nitrate is at least one selected from the group consisting of sodium nitrate, sodium nitrite, barium nitrate, potassium nitrate, calcium nitrate, potassium nitrite and ammonium nitrate. Salts include ammonium fluoride, sodium fluoride, magnesium silicate, potassium acid fluoride, acidic ammonium fluoride, acidic acid fluoride, hydrofluoric acid, ammonium fluoride, potassium fluoride, sodium fluoride, barium fluoride, potassium fluoride and manganese fluoride Compositions characterized in that at least one selected from the group consisting of. 제11항에 있어서, 상기 산처리 조성물은 나아가 황산, 황산염, 인산, 인산염, 과산화물, 아민 및 아미드류, 질산, 술폰산 및 술폰산염으로 구성되는 그룹에서 선택된 보조제를 1종 이상 함유함을 특징으로 하는 산처리조성물.The method of claim 11, wherein the acid treatment composition further comprises at least one auxiliary agent selected from the group consisting of sulfuric acid, sulfate, phosphoric acid, phosphate, peroxide, amines and amides, nitric acid, sulfonic acid and sulfonate. Acid treatment composition. 제14항에 있어서, 상기 황산염으로는 황산마그네슘, 황산망간, 황산나트륨, 황산칼륨, 황산암모늄, 과황산암모늄 및 아황산암모늄으로 구성되는 그룹에서 선택됨을 특징으로 하는 조성물.15. The composition of claim 14, wherein the sulfate is selected from the group consisting of magnesium sulfate, manganese sulfate, sodium sulfate, potassium sulfate, ammonium sulfate, ammonium persulfate and ammonium sulfite. 제14항에 있어서, 상기 인산염은 인산나트륨, 인산암모늄, 피로인산나트륨, 산성피로인산나트륨, 인산칼슘 및 인산칼륨으로 구성되는 그룹에서 선택됨을 특징으로 하는 조성물.15. The composition of claim 14, wherein the phosphate salt is selected from the group consisting of sodium phosphate, ammonium phosphate, sodium pyrophosphate, sodium pyrophosphate, calcium phosphate and potassium phosphate. 제14항에 있어서, 상기 아민 및 아미드화합물은 헥사메틸렌디아민, 디에틸아민, 디메틸아민, 디에틸에탄올아민, 디에틸티오우레아, 디메틸티오우레아. 디에틸렌디아민, 시클로헥실아민, 황산아미노구아니딘, 에탄올아민 등으로 구성되는 그룹에서 선택됨을 특징으로 하는 조성물.15. The method of claim 14, wherein the amine and amide compound is hexamethylenediamine, diethylamine, dimethylamine, diethylethanolamine, diethylthiourea, dimethylthiourea. And diethylenediamine, cyclohexylamine, aminoguanidine sulfate, ethanolamine and the like. 표면에 산화 및 탄화스케일이 형성된 스테인레스강 및 크롬 및/또는 니켈 합금강을 산처리조내에서 질산염 및 불화물염을 함유하고 있는 산세액으로 처리하여 강표면의 스케일을 제거하는 단계; 상기 단계에서 발생되는 산세폐액을 여과하여 고형상의 산화철과 슬러지를 분리·제거하는 단계; 상기 산화철과 슬러지를 분리하고 남은 여액을 냉각시켜 여액중에 용해되어 있는 금속이온을 금속염으로 석출시켜 분리·제거하는 단계; 및 상기 금속염이 분리·제거된 산세액을 상기 산처리조로 회귀시키는 단계;를 포함하는 산세폐액 재생방법.Descaling the steel surface by treating stainless steel and chromium and / or nickel alloy steel having oxidized and carbonized scales on the surface with a pickling solution containing nitrate and fluoride salt in an acid treatment tank; Filtering and washing the pickling waste liquid generated in the step to separate and remove solid iron oxide and sludge; Separating the iron oxide and the sludge and cooling the remaining filtrate to precipitate and separate and remove metal ions dissolved in the filtrate with a metal salt; And returning the pickling solution from which the metal salt has been separated and removed to the acid treatment tank. 제19항에 있어서, 상기 산세액은 나아가 황산, 황산염, 인산, 인산염, 과산화물, 아민 및 아미드류, 질산, 술폰산 및 술폰산염으로 구성되는 그룹에서 선택된 보조제를 1종 이상 포함함을 특징으로 하는 방법.The method of claim 19, wherein the pickling solution further comprises at least one auxiliary agent selected from the group consisting of sulfuric acid, sulfates, phosphoric acid, phosphates, peroxides, amines and amides, nitric acid, sulfonic acid and sulfonate. . 표면에 산화 및 탄화스케일이 형성된 스테인레스강을 산처리조내에서 질산염 및 불화물염을 함유하고 있는 산세액으로 처리하여 강표면의 스케일을 제거하는 단계; 상기 산처리에 따라 발생되는 산세폐액을 여과하여 고형상의 산화철과 슬러지를 분리·제거하는 단계; 이온교환수지를 이용하여 상기 산화철과 슬러지를 분리하고 남은 여액중에 용해되어 있는 금속이온을 흡착하여 분리·제거하는 단계; 및 상기 금속염이 분리·제거된 산세액을 상기 산처리조로 회귀시키는 단계;를 포함하는 산세폐액 재생방법.Removing the scale of the steel surface by treating the stainless steel on which the oxidation and carbonization scales are formed on the surface with a pickling solution containing nitrate and fluoride salt in an acid treatment tank; Filtering and removing the pickling waste liquid generated by the acid treatment to remove and remove solid iron oxide and sludge; Separating and removing the iron oxide and the sludge by using an ion exchange resin to adsorb and separate the metal ions dissolved in the remaining filtrate; And returning the pickling solution from which the metal salt has been separated and removed to the acid treatment tank. 제20항에 있어서, 상기 산세액은 나아가 황산, 황산염, 인산, 인산염, 과산화물, 아민 및 아미드류, 질산, 술폰산 및 술폰산염으로 구성되는 그룹에서 선택된 보조제를 1종 이상 포함함을 특징으로 하는 방법.The method of claim 20, wherein the pickling solution further comprises at least one auxiliary agent selected from the group consisting of sulfuric acid, sulfates, phosphoric acid, phosphates, peroxides, amines and amides, nitric acid, sulfonic acid and sulfonate. . ※ 참고사항 : 최초출원 내용에 의하여 공개하는 것임.※ Note: The disclosure is based on the initial application.
KR1019970013885A 1996-04-29 1997-04-15 Descaling method for stainless steel and cr or/and ni alloy steel, and composition of pickling solution and recyling method of pickling waste solution KR100230011B1 (en)

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DE69718589T DE69718589T2 (en) 1996-04-29 1997-04-29 Pickling solution for the descaling of iron-based alloys
EP97920962A EP0835333B9 (en) 1996-04-29 1997-04-29 Pickling solution used for removing scales on iron-based alloys
US08/983,602 US6361613B2 (en) 1996-04-29 1997-04-29 Method for pickling mettalic surface, pickling solutions therefor, and process for regenerating spent pickling solutions
PCT/KR1997/000069 WO1997041278A1 (en) 1996-04-29 1997-04-29 A method for pickling metallic surface, pickling solutions therefor, and process for regenerating spent pickling solutions
IDP971432A ID16846A (en) 1996-04-29 1997-04-29 METHODS FOR ACIDING THE PRESERVATION OF THE METALIC SURFACE OF ITS ACQUISITION, AND THE PROCESS FOR THE REGENERATION OF THE PRETTY ACID SOLUTION USED
JP9538753A JP3053651B2 (en) 1996-04-29 1997-04-29 Acid cleaning method for metal surface, acid cleaning liquid, and method for regenerating cleaning waste liquid
TW086105678A TW515852B (en) 1996-04-29 1997-04-29 A method for pickling metallic surface, pickling solutions therefor, and process for regenerating spent pickling solutions

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* Cited by examiner, † Cited by third party
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KR100415261B1 (en) * 1998-03-26 2004-03-26 이기원 Electronic display device and cleaning and etching composition for substrate
KR100839730B1 (en) * 2005-11-25 2008-06-19 엔쏜 인코포레이티드 Method and device for the purification of process solutions
KR20200004642A (en) * 2018-07-04 2020-01-14 바이켐 주식회사 Scaling cleaning agent for removing scaling of aluminum alloy which is generated during heat treatment and heat treatment method of aluminum alloy using the same

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KR100742865B1 (en) * 2001-09-06 2007-07-26 주식회사 포스코 Method For Seperating and Analyzing Strong Acid In Chemical Polishing Solution
KR101091154B1 (en) * 2009-11-10 2011-12-09 한국원자력연구원 Method for chemical decontamination of surface of radioactive metal waste using acid/acid salt mixture
KR101958416B1 (en) 2018-10-04 2019-03-14 (주)신광 Automatic pickling apparatus for stainless steel
KR102013528B1 (en) * 2018-10-10 2019-10-21 (주)스템코코리아 Composition for cleaning stainless steel and method of cleaning stainless steel using the same

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100415261B1 (en) * 1998-03-26 2004-03-26 이기원 Electronic display device and cleaning and etching composition for substrate
KR100839730B1 (en) * 2005-11-25 2008-06-19 엔쏜 인코포레이티드 Method and device for the purification of process solutions
KR20200004642A (en) * 2018-07-04 2020-01-14 바이켐 주식회사 Scaling cleaning agent for removing scaling of aluminum alloy which is generated during heat treatment and heat treatment method of aluminum alloy using the same

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