JP6802168B2 - 天然炭酸カルシウムを沈降炭酸カルシウムへ変換する方法プロセス - Google Patents
天然炭酸カルシウムを沈降炭酸カルシウムへ変換する方法プロセス Download PDFInfo
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- JP6802168B2 JP6802168B2 JP2017537499A JP2017537499A JP6802168B2 JP 6802168 B2 JP6802168 B2 JP 6802168B2 JP 2017537499 A JP2017537499 A JP 2017537499A JP 2017537499 A JP2017537499 A JP 2017537499A JP 6802168 B2 JP6802168 B2 JP 6802168B2
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- Prior art keywords
- carbonate
- calcium carbonate
- gypsum
- pcc
- ammonium
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- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 title claims description 832
- 229940088417 precipitated calcium carbonate Drugs 0.000 title claims description 341
- 238000000034 method Methods 0.000 title claims description 188
- 230000008569 process Effects 0.000 title claims description 62
- 239000010440 gypsum Substances 0.000 claims description 241
- 229910052602 gypsum Inorganic materials 0.000 claims description 241
- 239000000203 mixture Substances 0.000 claims description 166
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims description 155
- 239000001099 ammonium carbonate Substances 0.000 claims description 153
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 134
- 229910021532 Calcite Inorganic materials 0.000 claims description 126
- 238000006243 chemical reaction Methods 0.000 claims description 108
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 107
- 239000002245 particle Substances 0.000 claims description 105
- 235000012501 ammonium carbonate Nutrition 0.000 claims description 95
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 89
- 239000010459 dolomite Substances 0.000 claims description 63
- 229910000514 dolomite Inorganic materials 0.000 claims description 63
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 claims description 58
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims description 58
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 claims description 50
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid group Chemical group S(O)(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 50
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid group Chemical group C(CC(O)(C(=O)O)CC(=O)O)(=O)O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 48
- 239000000654 additive Substances 0.000 claims description 47
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims description 45
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims description 45
- 235000011130 ammonium sulphate Nutrition 0.000 claims description 45
- 239000001569 carbon dioxide Substances 0.000 claims description 43
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 43
- 235000014380 magnesium carbonate Nutrition 0.000 claims description 36
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 claims description 35
- 239000001095 magnesium carbonate Substances 0.000 claims description 35
- 229910000021 magnesium carbonate Inorganic materials 0.000 claims description 35
- BVCZEBOGSOYJJT-UHFFFAOYSA-N ammonium carbamate Chemical compound [NH4+].NC([O-])=O BVCZEBOGSOYJJT-UHFFFAOYSA-N 0.000 claims description 33
- KXDHJXZQYSOELW-UHFFFAOYSA-N carbonic acid monoamide Natural products NC(O)=O KXDHJXZQYSOELW-UHFFFAOYSA-N 0.000 claims description 33
- 238000010899 nucleation Methods 0.000 claims description 32
- 239000001166 ammonium sulphate Substances 0.000 claims description 30
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 28
- 229910052751 metal Inorganic materials 0.000 claims description 28
- 239000002184 metal Substances 0.000 claims description 28
- 230000032683 aging Effects 0.000 claims description 27
- 239000011575 calcium Substances 0.000 claims description 27
- 229910052791 calcium Inorganic materials 0.000 claims description 26
- 229910052943 magnesium sulfate Inorganic materials 0.000 claims description 25
- 235000019341 magnesium sulphate Nutrition 0.000 claims description 25
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 24
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 24
- 230000000996 additive effect Effects 0.000 claims description 24
- 238000004519 manufacturing process Methods 0.000 claims description 23
- 235000019738 Limestone Nutrition 0.000 claims description 21
- 239000006028 limestone Substances 0.000 claims description 21
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 20
- 239000003795 chemical substances by application Substances 0.000 claims description 18
- 238000001035 drying Methods 0.000 claims description 17
- 235000015165 citric acid Nutrition 0.000 claims description 16
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 15
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 14
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 14
- 239000011787 zinc oxide Substances 0.000 claims description 12
- 238000012545 processing Methods 0.000 claims description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 10
- 229910052799 carbon Inorganic materials 0.000 claims description 10
- 239000002270 dispersing agent Substances 0.000 claims description 10
- 239000000049 pigment Substances 0.000 claims description 10
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 claims description 10
- 235000019345 sodium thiosulphate Nutrition 0.000 claims description 10
- 238000011282 treatment Methods 0.000 claims description 10
- 230000018044 dehydration Effects 0.000 claims description 9
- 238000006297 dehydration reaction Methods 0.000 claims description 9
- 238000005549 size reduction Methods 0.000 claims description 9
- 238000004381 surface treatment Methods 0.000 claims description 9
- 238000010304 firing Methods 0.000 claims description 8
- 239000000872 buffer Substances 0.000 claims description 7
- 239000003623 enhancer Substances 0.000 claims description 7
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims description 7
- 239000000347 magnesium hydroxide Substances 0.000 claims description 7
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims description 7
- 239000004579 marble Substances 0.000 claims description 7
- 239000000377 silicon dioxide Substances 0.000 claims description 7
- 239000002562 thickening agent Substances 0.000 claims description 6
- 239000000080 wetting agent Substances 0.000 claims description 6
- 235000011007 phosphoric acid Nutrition 0.000 claims description 4
- 239000006184 cosolvent Substances 0.000 claims description 3
- 239000013530 defoamer Substances 0.000 claims 1
- 238000000518 rheometry Methods 0.000 claims 1
- 235000010216 calcium carbonate Nutrition 0.000 description 105
- 239000013078 crystal Substances 0.000 description 57
- 239000000047 product Substances 0.000 description 52
- 239000000463 material Substances 0.000 description 48
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 45
- 239000011162 core material Substances 0.000 description 44
- 239000002253 acid Substances 0.000 description 43
- 238000001878 scanning electron micrograph Methods 0.000 description 41
- 239000000243 solution Substances 0.000 description 38
- 229910052500 inorganic mineral Inorganic materials 0.000 description 36
- 235000010755 mineral Nutrition 0.000 description 36
- 239000011707 mineral Substances 0.000 description 36
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 34
- 239000002002 slurry Substances 0.000 description 33
- 238000007792 addition Methods 0.000 description 32
- 239000004067 bulking agent Substances 0.000 description 30
- 238000000576 coating method Methods 0.000 description 28
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 27
- -1 chalk Substances 0.000 description 27
- 239000003546 flue gas Substances 0.000 description 27
- 239000007789 gas Substances 0.000 description 26
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 description 24
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 23
- 229910021529 ammonia Inorganic materials 0.000 description 22
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 22
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 21
- 239000000908 ammonium hydroxide Substances 0.000 description 20
- 239000011248 coating agent Substances 0.000 description 19
- 229910052749 magnesium Inorganic materials 0.000 description 19
- 239000011777 magnesium Substances 0.000 description 19
- 238000009826 distribution Methods 0.000 description 17
- 239000007787 solid Substances 0.000 description 17
- 239000012535 impurity Substances 0.000 description 16
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 15
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 15
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 15
- 239000000123 paper Substances 0.000 description 15
- 150000007513 acids Chemical class 0.000 description 14
- 239000010949 copper Substances 0.000 description 14
- 239000000945 filler Substances 0.000 description 14
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 13
- 150000002500 ions Chemical class 0.000 description 13
- 239000010410 layer Substances 0.000 description 13
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 13
- 235000021355 Stearic acid Nutrition 0.000 description 12
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 12
- 239000000376 reactant Substances 0.000 description 12
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- 230000015572 biosynthetic process Effects 0.000 description 11
- 235000011132 calcium sulphate Nutrition 0.000 description 11
- 238000001914 filtration Methods 0.000 description 11
- 229910052712 strontium Inorganic materials 0.000 description 11
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 10
- 229910052788 barium Inorganic materials 0.000 description 10
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 10
- 238000005538 encapsulation Methods 0.000 description 10
- 239000012530 fluid Substances 0.000 description 10
- LIKBJVNGSGBSGK-UHFFFAOYSA-N iron(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Fe+3].[Fe+3] LIKBJVNGSGBSGK-UHFFFAOYSA-N 0.000 description 10
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- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 6
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- 229910019142 PO4 Inorganic materials 0.000 description 5
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 5
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- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 4
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- 230000006911 nucleation Effects 0.000 description 3
- BWOROQSFKKODDR-UHFFFAOYSA-N oxobismuth;hydrochloride Chemical compound Cl.[Bi]=O BWOROQSFKKODDR-UHFFFAOYSA-N 0.000 description 3
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- IGLNJRXAVVLDKE-UHFFFAOYSA-N rubidium atom Chemical compound [Rb] IGLNJRXAVVLDKE-UHFFFAOYSA-N 0.000 description 3
- 238000007873 sieving Methods 0.000 description 3
- ADZWSOLPGZMUMY-UHFFFAOYSA-M silver bromide Chemical compound [Ag]Br ADZWSOLPGZMUMY-UHFFFAOYSA-M 0.000 description 3
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 description 3
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Classifications
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- C01F5/00—Compounds of magnesium
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B14/00—Use of inorganic materials as fillers, e.g. pigments, for mortars, concrete or artificial stone; Treatment of inorganic materials specially adapted to enhance their filling properties in mortars, concrete or artificial stone
- C04B14/02—Granular materials, e.g. microballoons
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- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/02—Compounds of alkaline earth metals or magnesium
- C09C1/021—Calcium carbonates
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- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/63—Inorganic compounds
- D21H17/67—Water-insoluble compounds, e.g. fillers, pigments
- D21H17/675—Oxides, hydroxides or carbonates
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- B01D2251/404—Alkaline earth metal or magnesium compounds of calcium
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- B01D2251/606—Carbonates
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- 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
- B01D53/46—Removing components of defined structure
- B01D53/48—Sulfur compounds
- B01D53/50—Sulfur oxides
- B01D53/501—Sulfur oxides by treating the gases with a solution or a suspension of an alkali or earth-alkali or ammonium compound
- B01D53/502—Sulfur oxides by treating the gases with a solution or a suspension of an alkali or earth-alkali or ammonium compound characterised by a specific solution or suspension
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- C08K3/24—Acids; Salts thereof
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- C08K2003/265—Calcium, strontium or barium carbonate
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- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
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Description
本PCT国際出願は、2015年1月14日付で出願された米国仮特許出願第62/103,425号、2015年3月3日付で出願された同第62/127,687号、2015年3月12日付で出願された同第62/132,385号、及び2015年8月18日付で出願された同第62/206,594号(これら全ての主題の全体が引用することにより本明細書の一部をなす)の優先権の利益を主張するものである。
本開示は、煙道ガスを脱硫するプロセスであって、i)二酸化硫黄を含む煙道ガスを、SO2分離剤(sequestrating agent)で洗浄して、煙道ガス脱硫石膏と硫酸マグネシウムを含む水溶液とを含む懸濁液を得ること、ii)煙道ガス脱硫石膏を硫酸マグネシウム溶液から分離すること、iii)少なくとも1つの炭酸塩と硫酸マグネシウム溶液とを反応させて、マグネサイトの形態であってもよい炭酸マグネシウムを得ること、およびiv)炭酸マグネシウム又はマグネサイトを単離することからなるプロセスに関する。
本明細書で使用される場合、「沈降炭酸カルシウム」又は「PCC」は、その組成形態、純度、形態、粒径及び他の特徴(例えば粒径分布、表面積、立方度等)に関して特注であってもよい、様々な沈殿技法及び方法を用いて合成的に製造される炭酸カルシウム材料を指す。このため、沈降炭酸カルシウムは製造方法、並びに上述の及び以下により十分に説明される様々な組成/特徴の両方の点で天然炭酸カルシウム又は天然炭酸カルシウム含有鉱物(大理石、石灰石、チョーク、ドロマイト、貝殻等)又は重質炭酸カルシウム(粉砕した天然炭酸カルシウム)とは異なる。
本開示では、石膏から沈降炭酸カルシウムへの変換は、方法A〜方法I又はそれらの組合せを用いて達成される。方法及びプロセスパラメーターの選択により沈降炭酸カルシウムの構造、例えば結晶多形及び粒径の制御が可能となる。以下は方法A〜方法Iの概要である。
この方法は、以下を含む:
i. 生石膏を、硝酸、硫酸又はリン酸を含むが、これらに限定されない鉱酸で処理して、脱硫プロセスから残存する任意の未反応の炭酸カルシウム又は炭酸マグネシウムを消費すること。石膏に添加する鉱酸の量は、任意に未反応の炭酸塩の量のモル当量であるか、又は過剰である。
ii. 鉱酸で処理した石膏と炭酸アンモニウムとを0℃〜60℃又は8℃〜50℃の範囲の低温で3分間〜300分間又は5分間〜250分間反応させて、バテライト結晶構造、カルサイト結晶構造、アラゴナイト結晶構造、非晶質炭酸カルシウム、又はそれらの混合物若しくはブレンドの炭酸カルシウムを作製すること。
iii. 任意に得られる炭酸カルシウムを乾燥又は湿潤状態で焼鈍して、所望の多形又は多形混合物を形成すること。
この方法は、以下を含む:
i. 生石膏を硝酸、硫酸又はリン酸を含むが、これらに限定されない鉱酸で処理して、脱硫プロセスから残存する任意の未反応の炭酸カルシウム又は炭酸マグネシウムを消費すること。石膏に添加する鉱酸の量は、任意に未反応の炭酸塩の量に対して等モルである。
ii. 重質炭酸カルシウム(GCC)又はPCCのいずれかに由来するカルサイト(又はアラゴナイト)を、鉱酸で処理した石膏にシードとして添加し、炭酸アンモニウムと0℃〜60℃又は8℃〜50℃の範囲の低温で3分間〜300分間又は5分間〜250分間反応させて、得られるものから炭酸カルシウムを添加することなく種々の優勢形態(例えば、結晶又は非晶質)の炭酸カルシウムを作製すること。カルサイトは菱面体晶又は偏三角面体晶であり得る。
この方法は、以下を含む:
i. 炭酸カルシウムを生石膏に添加して、明確に規定される炭酸カルシウムと硫酸カルシウムとの混合物を得ること。
ii. 石膏及び炭酸カルシウムの混合物と炭酸アンモニウムとを0℃〜60℃又は8℃〜50℃の範囲の低温で3分間〜300分間又は5分間〜250分間反応させて、得られるものから炭酸カルシウムを添加することなく種々の優勢結晶構造の炭酸カルシウムを作製すること。
この方法は、以下を含む:
i. 上記方法B又は方法Cのプロセスによってシーディングされた石膏を調製し、ここでドロマイト、ドロマイト質炭酸塩(dolomitic carbonate)、硫酸マグネシウム、水酸化マグネシウム、チタニア(TiO2)、シリカ(SiO2)若しくは酸化亜鉛(例えばZnO)、又はそれらの混合物を炭酸カルシウムの代わりにシードとして添加すること。
ii. シーディングされた石膏と炭酸アンモニウムとを反応させて、バテライト結晶構造、カルサイト結晶構造、アラゴナイト結晶構造、非晶質炭酸カルシウム、又はそれらの混合物若しくはブレンドの炭酸カルシウムを作製すること。
この方法は、以下を含む:
i. 添加剤を石膏に添加して、斜方晶若しくは偏三角面体晶カルサイト、バテライト、アラゴナイト、非晶質炭酸カルシウム又はそれらのブレンドを含むが、これらに限定されない他の規定の炭酸カルシウムの多形及び粒径を得る、方法A、方法B、方法C又は方法Dのプロセス。
この方法は、以下を含む:
i. 重炭酸アンモニウムの量がカルバミン酸アンモニウム濃度以上となり、反応時にカルサイト又はカルサイト−バテライトブレンドが得られるように、炭酸アンモニウムが炭酸アンモニウム、カルバミン酸アンモニウム及び重炭酸アンモニウムの混合物を含む、方法A〜方法Eのプロセス。
この方法は、以下を含む:
i. 重炭酸アンモニウムの量がカルバミン酸アンモニウム濃度以下となり、反応時にバテライト又はバテライト−カルサイトブレンドが得られるように、炭酸アンモニウムが炭酸アンモニウム、カルバミン酸アンモニウム及び重炭酸アンモニウムの混合物を含む、方法A〜方法Eのプロセス。
この方法は、以下を含む:
i. 炭酸アンモニウムを水酸化アンモニウムとCO2との反応によって作製する、方法A〜方法Gのプロセス。石膏スラリーに導入する炭酸アンモニウムはpHを適合させたものであり、及び/又は得られる多形及び粒径に影響を与えるために過剰なCO2が用いられる。
この方法は、以下を含む:
i. 金属炭酸塩を炭酸アンモニウムの代わりに石膏との反応に使用する、方法A〜方法Eのプロセス。
ii. 方法A〜方法EのFGD石膏と金属炭酸塩とを反応させて、バテライト結晶構造、カルサイト結晶構造又はカルサイト−バテライト−アラゴナイト結晶構造ブレンドの炭酸カルシウムを作製すること。
別の態様によると、本開示は、石膏とシード、鉱酸又はその両方とを含む混合物と少なくとも1つの炭酸塩源とを反応させて、沈降炭酸カルシウムを作製することを含む、石膏を沈降炭酸カルシウムへと変換するプロセスに関する。反応物及びシード及び/又は鉱酸により沈降炭酸カルシウムの結晶多形及び/又は粒径が制御され、沈降炭酸カルシウムはカルサイトの形態であり、カルサイトはバテライト多形から変換されることなく反応物から直接作製される。
第1の態様によると、本開示は、石膏とシード、鉱酸又はその両方とを含む混合物と少なくとも1つの炭酸塩源とを反応させて、沈降炭酸カルシウムを作製することを含む、石膏を沈降炭酸カルシウムへと変換するプロセスに関する。反応物及びシード及び/又は鉱酸により沈降炭酸カルシウムの結晶多形及び/又は粒径が制御され、沈降炭酸カルシウムはアラゴナイトの形態であり、アラゴナイトはバテライト多形から変換されることなく反応物から直接作製される。
第2の態様によると、本開示は、i)石膏及びii)シード、又は10℃〜60℃若しくは18℃〜45℃若しくはより好ましくは25℃〜35℃の反応温度からなる群から選択される少なくとも1つのプロセス条件を準備することと、石膏と少なくとも1つの炭酸塩源とを反応させて、沈降炭酸カルシウムをバテライトの形態で作製することとを含む、石膏を沈降炭酸カルシウムへと変換するプロセスに関する。反応物及びシード及び/又はプロセス条件によりバテライトの粒径が制御される。
本開示では、PCC組成物の結晶含量は、例えば走査型電子顕微鏡又はX線回折を用いる目視検査によって容易に決定することができる。かかる決定は結晶形の特定に基づくものであってもよく、当業者に既知である。
本開示は、バテライト多形を有する沈降炭酸カルシウム化合物に関する。本書に記載されるバテライト沈降炭酸カルシウムは、これまで既知のバテライト沈降炭酸カルシウムと比較して粒径分布(PSD)、峻度及びBET表面積等の新規の構造的特徴を有する。バテライトの特徴については下記表3を参照されたい。
或る特定の実施形態によると、本開示は、その実施形態の1つ以上における本明細書に記載のバテライト、カルサイト及び/又はアラゴナイト沈降炭酸カルシウム化合物の商業的用途に関する。
石膏又は他の硫酸塩を、固形分35%の水又は30%〜35%硫酸アンモニウム溶液中でスラリー化した。炭酸アンモニウムを、反応のために高温で水に1:1.7の(石膏:炭酸アンモニウム)モル比をもたらす濃度で溶解した。代替的な炭酸塩供給材料は、反応のために室温で水に1:1.7の(硫酸塩:炭酸塩)モル比をもたらす量で溶解した。硫酸塩スラリーと炭酸塩溶液とを混合し、少なくとも10分間反応させた。次いで、スラリーを濾過し、スラリーケーキを水で洗浄した。反応ケーキ及びデカントした液体をFTIR、DSC、SEM、Sedigraph及びBET表面積分析によって化学的及び物理的に分析した。このプロセスに関与する反応を表1及び表2に記載する。
水酸化アンモニウム及びCO2からの炭酸アンモニウム作製に関与する反応のために、硫酸塩を上記のように周囲温度及び圧力でスラリー化した。水酸化アンモニウムを、混合物を反応器に投入する直前に硫酸塩スラリーに添加した。反応器を覆った後、選択温度まで撹拌しながら加熱又は冷却した。CO2を撹拌しながら最低1時間反応器にバブリングした。1時間の反応時間の後、スラリーのごく一部を取り出し、PCCへの完全な変換をフェノールフタレイン色変化によって確認した。反応の完了時に、スラリーを反応器から取り出し、濾過し、洗浄し、上記のように分析した。このプロセスに関与する反応を表1に記載する。
幾つかの実施形態によると、本開示に開示される方法の1つ以上を用いて、PCCをコア材料に沈殿させることができる。例えば、PCCにより有益な特性をコア材料に付与する表面層又はコーティングを形成することができる。プロセスは、幾つかの実施形態では、コア材料を溶液から沈殿させるために用いることができ、ここで沈殿するコア材料はPCC層又はコーティングを有する。「層」又は「コーティング」という単語の使用は、コア材料の表面の少なくとも一部に形成される沈降炭酸カルシウム相を含むことが理解される。幾つかの実施形態では、PCC層又はコーティングはコア材料の表面の半分又は実質的に全てを覆うことができる。コア材料は、炭酸カルシウムでコーティングされた組成物のコアを形成することができる。
例示的な炭酸カルシウムでコーティングされたヘマタイトを、硫酸カルシウムを炭酸アンモニウム溶液と反応させることによって調製した。まず、シグマアルドリッチ社製の6.30グラムの硫酸カルシウムを250mLの水と25℃で30分間混合し、スラリーを形成した。次に、20グラムのヘマタイトをスラリーに添加し、混合して、84.5重量%対15.5重量%のヘマタイトとPCCとの特定の比率を維持した。次いで、5.97グラムの炭酸アンモニウムを250mLの水に溶解し、即座にスラリーに添加した。最終混合物を1時間混合し、PCCをヘマタイト上に沈殿させた。混合後に混合物を濾過し、洗浄して、過剰な硫酸アンモニウムを除去した。PCCでコーティングされたヘマタイトを含有する得られるケーキを回収した。
Claims (22)
- 天然炭酸カルシウムを沈降炭酸カルシウムへと変換する方法であって、
前記天然炭酸カルシウムを硫酸塩で処理して、石膏を作製することと、
前記石膏と少なくとも1つの炭酸塩源とを反応させて、沈降炭酸カルシウムを作製することと、
を含む、方法。 - 前記炭酸塩源が炭酸アンモニウム、重炭酸アンモニウム、カルバミン酸アンモニウム、炭酸カルシウム、ドロマイト、金属炭酸塩及び二酸化炭素からなる群から選択される少なくとも1つである、請求項1に記載の方法。
- 前記石膏と前記炭酸塩源とのモル比が1:1.1〜1:3である、請求項1に記載の方法。
- 前記炭酸塩源が炭酸アンモニウム、カルバミン酸アンモニウム及び重炭酸アンモニウムの炭酸塩混合物であり、該炭酸塩混合物において重炭酸アンモニウムの量がカルバミン酸アンモニウム又は炭酸アンモニウムの量以上である、請求項1に記載の方法。
- 前記炭酸塩源が炭酸アンモニウム、カルバミン酸アンモニウム及び重炭酸アンモニウムの炭酸塩混合物であり、該炭酸塩混合物において重炭酸アンモニウムの量がカルバミン酸アンモニウム又は炭酸アンモニウムの量未満である、請求項1に記載の方法。
- 前記硫酸塩が硫酸である、請求項1に記載の方法。
- 前記天然炭酸カルシウムを、該天然炭酸カルシウム中に存在するカルシウムのモル当量以上のモル当量の硫酸で処理する、請求項6に記載の方法。
- 前記天然炭酸カルシウムが石灰石、大理石又はチョークである、請求項1に記載の方法。
- 前記石灰石がドロマイト質石灰石であり、処理により石膏及び硫酸マグネシウムが作製される、請求項8に記載の方法。
- 前記硫酸マグネシウムと少なくとも1つの炭酸塩源とを反応させて、表面積が20m2/g以上の炭酸マグネシウムを作製することを更に含む、請求項9に記載の方法。
- 前記炭酸マグネシウムがマグネサイト形態である、請求項10に記載の方法。
- 反応前又は反応中に前記石膏にシードをシーディングして、前記沈降炭酸カルシウムの結晶多形及び粒径を制御することを更に含む、請求項1に記載の方法。
- 前記シードが炭酸カルシウム、ドロマイト、ドロマイト質炭酸塩、硫酸マグネシウム、水酸化マグネシウム、チタニア、シリカ及び酸化亜鉛からなる群から選択される少なくとも1つである、請求項12に記載の方法。
- 前記シードが前記石膏に対して10wt%を超えない、請求項12に記載の方法。
- 前記シードが前記石膏に対して少なくとも10wt%である、請求項12に記載の方法。
- 少なくとも1つの添加剤を前記石膏に添加すること、
を更に含み、前記添加剤が緩衝剤、分散剤、増粘剤、固化防止剤、消泡剤、レオロジー剤、湿潤剤、共溶媒、明度エンハンサー若しくは明度ダンプナー、又は顔料であり、
前記添加剤の重量%が前記石膏に対して0.5%〜10%の範囲である、請求項1に記載の方法。 - 前記添加剤がクエン酸、リン酸、硫酸アンモニウム又はチオ硫酸ナトリウムである、請求項16に記載の方法。
- 前記沈降炭酸カルシウムを脱水、乾燥、エージング、表面処理、サイズ減少及び選鉱からなる群から選択される少なくとも1つの方法によって加工して、加工炭酸カルシウムを作製することを更に含む、請求項1に記載の方法。
- 前記沈降炭酸カルシウムがバテライトであり、前記加工炭酸カルシウムがカルサイト、アラゴナイト又は多形のブレンドである、請求項18に記載の方法。
- 前記天然炭酸カルシウムが焼成されていない、請求項1に記載の方法。
- カーボンフットプリントが天然炭酸カルシウムの焼成を伴うプロセスに対して少なくとも5%低減する、請求項20に記載の方法。
- 低減されたカーボンフットプリントを有する沈降炭酸カルシウムを作製する方法であって、
天然炭酸カルシウムを、石膏中間体を介して第1の沈降炭酸カルシウムへと変換すること、
を含み、変換により、天然炭酸カルシウムを第2の沈降炭酸カルシウムへと変換するために天然炭酸カルシウムの焼成を含むプロセスから放出される第2の量の二酸化炭素よりも少ない第1の量の二酸化炭素が放出される、方法。
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