JP5807284B2 - 石膏を用いた高純度硫安及び方解石の製造方法 - Google Patents
石膏を用いた高純度硫安及び方解石の製造方法 Download PDFInfo
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- JP5807284B2 JP5807284B2 JP2014521547A JP2014521547A JP5807284B2 JP 5807284 B2 JP5807284 B2 JP 5807284B2 JP 2014521547 A JP2014521547 A JP 2014521547A JP 2014521547 A JP2014521547 A JP 2014521547A JP 5807284 B2 JP5807284 B2 JP 5807284B2
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- gypsum
- ammonium sulfate
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- 239000010440 gypsum Substances 0.000 title claims description 89
- 229910052602 gypsum Inorganic materials 0.000 title claims description 89
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 title claims description 88
- 229910052921 ammonium sulfate Inorganic materials 0.000 title claims description 88
- 235000011130 ammonium sulphate Nutrition 0.000 title claims description 88
- 238000004519 manufacturing process Methods 0.000 title claims description 21
- 229910021532 Calcite Inorganic materials 0.000 title description 83
- 238000006243 chemical reaction Methods 0.000 claims description 61
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 48
- 239000002002 slurry Substances 0.000 claims description 40
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 38
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 21
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 21
- 229910021529 ammonia Inorganic materials 0.000 claims description 20
- 239000001569 carbon dioxide Substances 0.000 claims description 19
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 239000011505 plaster Substances 0.000 claims description 4
- 238000000034 method Methods 0.000 description 42
- 239000002699 waste material Substances 0.000 description 27
- 239000006227 byproduct Substances 0.000 description 14
- 238000002441 X-ray diffraction Methods 0.000 description 13
- 239000000843 powder Substances 0.000 description 13
- 238000011084 recovery Methods 0.000 description 12
- 239000000203 mixture Substances 0.000 description 11
- 238000002411 thermogravimetry Methods 0.000 description 11
- 238000007664 blowing Methods 0.000 description 10
- 230000004580 weight loss Effects 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 8
- 238000004064 recycling Methods 0.000 description 8
- 238000001035 drying Methods 0.000 description 7
- 239000002994 raw material Substances 0.000 description 7
- 239000003337 fertilizer Substances 0.000 description 6
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 description 5
- 239000001099 ammonium carbonate Substances 0.000 description 5
- 235000012501 ammonium carbonate Nutrition 0.000 description 5
- 239000007864 aqueous solution Substances 0.000 description 5
- 230000007423 decrease Effects 0.000 description 5
- 150000004683 dihydrates Chemical class 0.000 description 5
- 239000007789 gas Substances 0.000 description 5
- 239000012535 impurity Substances 0.000 description 5
- 238000002156 mixing Methods 0.000 description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 230000003247 decreasing effect Effects 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 3
- 239000007795 chemical reaction product Substances 0.000 description 3
- 238000006477 desulfuration reaction Methods 0.000 description 3
- 230000023556 desulfurization Effects 0.000 description 3
- 238000001704 evaporation Methods 0.000 description 3
- 230000008020 evaporation Effects 0.000 description 3
- 239000003546 flue gas Substances 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 229910052500 inorganic mineral Inorganic materials 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000011707 mineral Substances 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 239000007858 starting material Substances 0.000 description 3
- 239000002352 surface water Substances 0.000 description 3
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 2
- ZOMBKNNSYQHRCA-UHFFFAOYSA-J calcium sulfate hemihydrate Chemical compound O.[Ca+2].[Ca+2].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O ZOMBKNNSYQHRCA-UHFFFAOYSA-J 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 239000010871 livestock manure Substances 0.000 description 2
- 239000010452 phosphate Substances 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 238000002076 thermal analysis method Methods 0.000 description 2
- 235000019738 Limestone Nutrition 0.000 description 1
- ZRIUUUJAJJNDSS-UHFFFAOYSA-N ammonium phosphates Chemical compound [NH4+].[NH4+].[NH4+].[O-]P([O-])([O-])=O ZRIUUUJAJJNDSS-UHFFFAOYSA-N 0.000 description 1
- 239000001166 ammonium sulphate Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- FFBHFFJDDLITSX-UHFFFAOYSA-N benzyl N-[2-hydroxy-4-(3-oxomorpholin-4-yl)phenyl]carbamate Chemical compound OC1=C(NC(=O)OCC2=CC=CC=C2)C=CC(=C1)N1CCOCC1=O FFBHFFJDDLITSX-UHFFFAOYSA-N 0.000 description 1
- 230000033558 biomineral tissue development Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000000892 gravimetry Methods 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 230000003100 immobilizing effect Effects 0.000 description 1
- 239000006028 limestone Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000007039 two-step reaction Methods 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
- C22B26/20—Obtaining alkaline earth metals or magnesium
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
- B09B3/00—Destroying solid waste or transforming solid waste into something useful or harmless
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
- B09B3/00—Destroying solid waste or transforming solid waste into something useful or harmless
- B09B3/20—Agglomeration, binding or encapsulation of solid waste
- B09B3/25—Agglomeration, binding or encapsulation of solid waste using mineral binders or matrix
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/24—Sulfates of ammonium
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/18—Carbonates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/88—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by thermal analysis data, e.g. TGA, DTA, DSC
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Inorganic Chemistry (AREA)
- Geology (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Description
2NH3+H2O+CO2→(NH4)2CO3
(NH4)2CO3+CaSO4・2H2O→CaCO3+(NH4)2SO4+12KJ(吸熱反応)
2NH4(OH)+H2O+CaSO4+CO2→CaCO3+(NH4)2SO4−98KJ(発熱反応)
2NH4(OH)+xH2O+CaSO4・2H2O+CO2→CaCO3+(NH4)2SO4+yH2O
水1500ccに、アンモニア水(アンモニア含量:25%)600cc及び選鉱過程を経ていない単純乾燥した石膏500gを入れて混合し、そのスラリーを出発温度15℃で撹拌した。この際のスラリー濃度は24%であった。その後、それに二酸化炭素を5L/minの速度で吹き込みながら25分間反応させることで、方解石及び硫安を含むスラリーを製造した。
実施例1と同様に、水1500ccにアンモニア水(アンモニア含量:25%)600cc及び副産石膏500gを入れて混合し、そのスラリーを出発温度5℃で撹拌した。その後、二酸化炭素を5L/分の速度で吹き込みながら25分間反応させることで、方解石及び硫安を含むスラリーを製造した。
実施例1と同様に、水1500ccにアンモニア水(アンモニア含量:25%)600cc及び副産石膏500gを入れて混合し、そのスラリーを常温常圧で撹拌した。その後、二酸化炭素を3L/分の速度で吹き込みながら30分間反応させることで、方解石及び硫安を含むスラリーを製造した。反応後、温度は27℃増加した。
実施例1と同様に、水1500ccにアンモニア水(アンモニア含量:25%)600cc及び副産石膏500gを入れて混合し、そのスラリーを常温常圧で撹拌した。その後、二酸化炭素を10L/分の速度で吹き込みながら25分間反応させることで、方解石及び硫安を含むスラリーを製造した。
実施例1と同様に、水1000ccにアンモニア水(アンモニア含量:25%)600cc及び副産石膏500gを入れて混合し、そのスラリーを常温常圧で撹拌した。この際のスラリー濃度は31%(w/v)であった。その後、二酸化炭素を5L/分の速度で吹き込みながら25分間反応させることで、方解石及び硫安を含むスラリーを製造した。
実施例1と同様に、水2000ccにアンモニア水(アンモニア含量:25%)600cc及び副産石膏500gを入れて混合し、そのスラリーを常温常圧で撹拌した。この際のスラリー濃度は19%であった。その後、二酸化炭素を5L/分の速度で吹き込みながら25分間反応させることで、方解石及び硫安を含むスラリーを製造した。
実施例1と同様に、水1500ccにアンモニア水(アンモニア含量:25%)900cc及び副産石膏780gを入れて混合し、そのスラリーを常温常圧で撹拌した。この際のスラリー濃度は33%であった。その後、二酸化炭素を5L/分の速度で吹き込みながら25分間反応させることで、方解石及び硫安を含むスラリーを製造した。
実施例1と同様に、水1500ccにアンモニア水(アンモニア含量:25%)900cc及び副産石膏780gを入れて混合し、そのスラリーを常温常圧で撹拌した。その後、二酸化炭素を9L/分の速度で吹き込みながら25分間反応させることで、方解石及び硫安を含むスラリーを製造した。
S110 廃石膏を100メッシュ以下に原料として準備する段階
S120 廃石膏、アンモニア水、及び水の量を秤量してスラリーに混合する段階
S130 上記スラリーを二酸化炭素と反応させることで石膏を炭酸化させて、水溶液状の硫安を製造する段階
S140 製造された方解石と水溶液状の硫安とを分離する段階
S150、S160 分離された方解石と水溶液状の硫安をそれぞれ独立して乾燥又は結晶化することで粉末を得る段階
Claims (4)
- 水、アンモニア水、及び石膏を混合したスラリーに、石膏1g当たりに8〜20cc/minの流量で供給される二酸化炭素を添加して炭酸化反応させる段階を含み、前記スラリーの濃度は20〜28(w/v)%であり、石膏100重量部に対して、25重量%のアンモニアを含有するアンモニア水が100〜150重量部混合される、純度が95%以上である、方解石及び硫安の製造方法。
- 前記スラリーは、石膏100重量部に対して、前記アンモニア水以外に180〜350重量部の水が混合されることを特徴とする、請求項1に記載の方解石及び硫安の製造方法。
- 前記スラリーの初期反応温度は5〜18℃であることを特徴とする、請求項1に記載の方解石及び硫安の製造方法。
- 前記炭酸化反応は常温常圧の条件で行われることを特徴とする、請求項1〜3のいずれか一項に記載の方解石及び硫安の製造方法。
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
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KR20110070317 | 2011-07-15 | ||
KR10-2011-0070317 | 2011-07-15 | ||
PCT/KR2012/005591 WO2013012214A2 (ko) | 2011-07-15 | 2012-07-13 | 석고를 이용한 고순도 황안 및 방해석의 제조 방법 |
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JP2014520754A JP2014520754A (ja) | 2014-08-25 |
JP5807284B2 true JP5807284B2 (ja) | 2015-11-10 |
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Country Status (6)
Country | Link |
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US (1) | US9200347B2 (ja) |
JP (1) | JP5807284B2 (ja) |
KR (1) | KR101452371B1 (ja) |
CN (1) | CN103874658B (ja) |
DE (1) | DE112012002980B4 (ja) |
WO (1) | WO2013012214A2 (ja) |
Families Citing this family (15)
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CN104854251B (zh) * | 2012-08-10 | 2017-03-01 | 斯帕斯坦技术有限责任公司 | 用于将fgd石膏转化为硫酸铵和碳酸钙的方法 |
JP2014189416A (ja) * | 2013-03-26 | 2014-10-06 | Yoshizawa Lime Industry | マグネシウムを含む溶液及び炭酸カルシウムの製造方法 |
CN103224246B (zh) * | 2013-05-09 | 2015-05-27 | 中化重庆涪陵化工有限公司 | 一种化学石膏制硫铵反应料浆浓缩和余热余氨回收方法 |
KR101482017B1 (ko) * | 2013-05-23 | 2015-01-14 | 한국지질자원연구원 | Co2 포집 중간 생성물을 이용한 탈황 석고의 탄산화 반응으로부터의 순수 방해석 합성 방법 |
KR102044792B1 (ko) * | 2013-08-19 | 2019-11-15 | 재단법인 포항산업과학연구원 | 이산화탄소 흡수 공정과 연계된 광물탄산화 공정 |
US9505629B2 (en) | 2013-08-19 | 2016-11-29 | Korea Institute Of Geoscience And Mineral Resources | Method of preparing calcium carbonate using direct carbonation reaction |
KR101490389B1 (ko) * | 2013-08-19 | 2015-02-05 | 한국지질자원연구원 | 배연 탈황석고로부터 바테라이트의 제조방법 |
CN103495587B (zh) * | 2013-09-22 | 2015-06-10 | 清华大学 | 一种石膏类材料表面包覆碳酸钙的方法 |
KR101518008B1 (ko) * | 2014-05-22 | 2015-05-06 | 한국지질자원연구원 | 황산암모늄의 제조방법 |
CN104096707B (zh) * | 2014-06-27 | 2016-09-14 | 武汉钢铁(集团)公司 | 半干法脱硫灰资源化利用方法 |
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CN107500329A (zh) * | 2017-08-10 | 2017-12-22 | 青阳县永诚钙业有限责任公司 | 一种基于石膏废料生产方解石的方法 |
CN107583466A (zh) * | 2017-09-27 | 2018-01-16 | 四川恒泰环境技术有限责任公司 | 一种将湿法脱硫石膏直接转化为硫酸铵和碳酸钙并循环利用的方法 |
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EP4299523A1 (en) * | 2022-06-30 | 2024-01-03 | SABIC Global Technologies B.V. | Knh4so4, caco3, cacl2 fertilizer |
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CN103874658B (zh) | 2016-04-27 |
DE112012002980B4 (de) | 2019-06-27 |
WO2013012214A2 (ko) | 2013-01-24 |
CN103874658A (zh) | 2014-06-18 |
KR20130009705A (ko) | 2013-01-23 |
JP2014520754A (ja) | 2014-08-25 |
US20140161692A1 (en) | 2014-06-12 |
WO2013012214A3 (ko) | 2013-03-14 |
KR101452371B1 (ko) | 2014-10-21 |
US9200347B2 (en) | 2015-12-01 |
DE112012002980T5 (de) | 2014-05-22 |
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