JP7128546B2 - リチウム鉱石から炭酸リチウムを調製するための方法およびシステム - Google Patents
リチウム鉱石から炭酸リチウムを調製するための方法およびシステム Download PDFInfo
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- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims description 52
- 229910052744 lithium Inorganic materials 0.000 title claims description 52
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 title claims description 52
- 229910052808 lithium carbonate Inorganic materials 0.000 title claims description 52
- 238000000034 method Methods 0.000 title claims description 49
- INHCSSUBVCNVSK-UHFFFAOYSA-L lithium sulfate Inorganic materials [Li+].[Li+].[O-]S([O-])(=O)=O INHCSSUBVCNVSK-UHFFFAOYSA-L 0.000 claims description 65
- RBTVSNLYYIMMKS-UHFFFAOYSA-N tert-butyl 3-aminoazetidine-1-carboxylate;hydrochloride Chemical compound Cl.CC(C)(C)OC(=O)N1CC(N)C1 RBTVSNLYYIMMKS-UHFFFAOYSA-N 0.000 claims description 59
- 238000001914 filtration Methods 0.000 claims description 41
- 238000005342 ion exchange Methods 0.000 claims description 24
- 239000012528 membrane Substances 0.000 claims description 20
- 239000012141 concentrate Substances 0.000 claims description 15
- 238000001223 reverse osmosis Methods 0.000 claims description 13
- 239000000047 product Substances 0.000 claims description 12
- 238000000108 ultra-filtration Methods 0.000 claims description 12
- 239000002244 precipitate Substances 0.000 claims description 11
- 239000003513 alkali Substances 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 6
- 239000000243 solution Substances 0.000 claims description 5
- 239000012047 saturated solution Substances 0.000 claims description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 3
- 239000000725 suspension Substances 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 description 21
- 238000005374 membrane filtration Methods 0.000 description 19
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 14
- 239000012535 impurity Substances 0.000 description 11
- 238000001471 micro-filtration Methods 0.000 description 11
- 239000011575 calcium Substances 0.000 description 10
- 230000000694 effects Effects 0.000 description 10
- 239000003456 ion exchange resin Substances 0.000 description 9
- 229920003303 ion-exchange polymer Polymers 0.000 description 9
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 8
- 238000001556 precipitation Methods 0.000 description 8
- 239000007788 liquid Substances 0.000 description 7
- 239000000126 substance Substances 0.000 description 6
- 239000012467 final product Substances 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 229910003002 lithium salt Inorganic materials 0.000 description 3
- 159000000002 lithium salts Chemical class 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000010979 pH adjustment Methods 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 239000013618 particulate matter Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- -1 Fe 2+ Chemical class 0.000 description 1
- 229910052822 amblygonite Inorganic materials 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000003480 eluent Substances 0.000 description 1
- 238000010828 elution Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000013100 final test Methods 0.000 description 1
- 229910052629 lepidolite Inorganic materials 0.000 description 1
- 238000001728 nano-filtration Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000009287 sand filtration Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 229910021642 ultra pure water Inorganic materials 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
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- C01D15/00—Lithium compounds
- C01D15/08—Carbonates; Bicarbonates
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- B01D61/02—Reverse osmosis; Hyperfiltration ; Nanofiltration
- B01D61/04—Feed pretreatment
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- B01D61/145—Ultrafiltration
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- B01D2311/04—Specific process operations in the feed stream; Feed pretreatment
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01D61/025—Reverse osmosis; Hyperfiltration
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- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
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Description
本発明はリチウム塩の製造プロセスの技術分野に関する。具体的には、リチウム鉱石から炭酸リチウムを調製するための方法およびシステムに関する。
炭酸リチウムを調製するための原料は、主に塩湖のかん水およびリチウム鉱石に分けられる。近年、中国では塩湖のリチウム資源の採掘が積極的に行われているが、資源や技術などの要因に制限され、開発速度が比較的遅い。そのため、現在、中国では、リチウム鉱石からリチウムを抽出する手法が主流となっている。リチウム鉱石とは、通常、リチウム鉱石、レピドライト、アンブリゴナイトなどのリチウム含有鉱石を指す。
本発明の主な目的は、リチウム鉱石から炭酸リチウムを調製する従来技術のプロセスでは製品の品質が低いという問題を解決するために、リチウム鉱石から炭酸リチウムを調製するための方法およびシステムを提供することである。
1)リチウム鉱石の精鉱を用い、硫酸リチウム溶出液を調製する工程、
2)硫酸リチウム溶出液にアルカリを添加してPHを9~10に調整し、硫酸リチウム溶出液中のFe2+、Al3+を沈殿させる工程、
3)工程2)で得られた硫酸リチウム溶出液をろ過し、硫酸リチウム溶出液中のFe2+、Al3+の沈殿物を除去する工程、
4)ろ過で得られた硫酸リチウム溶出液をイオン交換法で処理し、硫酸リチウム溶出液中のCa2+、Mg2+を除去する工程、
5)続いて、得られる濃縮液中のFe2+の濃度<0.0005%、Al3+の濃度<0.0005%、Ca2+の濃度<0.0024%、Mg2+の濃度<0.0040%、且つ、硫酸リチウムの濃度が15~20%となるように、イオン交換処理で得られた硫酸リチウム溶出液を膜濃縮して硫酸リチウム溶出液の濃縮液を得る工程、および、
6)工程5)で得られた硫酸リチウム溶出液の濃縮液に炭酸ナトリウム飽和溶液を添加して炭酸リチウムを沈殿させ、炭酸リチウム沈殿物をろ過分離した後、該炭酸リチウム沈殿物を熱水で洗浄し、乾燥させ、炭酸リチウム完成品を得る工程を含む、
リチウム鉱石から炭酸リチウムを調製するための方法を提供することにある。
本発明の一部を構成する図面は、本発明に対する理解を補助するためのものである。図面に開示の内容、および、それに関する明細書中の記載は、本発明の解釈に資するためのものであるが、本発明を限定するものではない。
2:イオン交換装置
3:前処理装置
4:限外ろ過膜ろ過装置
5:ディスクチューブ逆浸透膜ろ過装置
6:Li2SO4溶出液産出システム
7:リチウム沈殿システム
8:乾燥システム
〔具体的な実施形態〕
以下、図面を参照しながら、本発明を明確かつ完全に説明する。本分野の当業者は、これらの説明に基づき本発明を実現することができる。図面を参照しながら本発明を説明する前に、特に以下のことを述べておく。
1)リチウム鉱石の精鉱を用い、硫酸リチウム溶出液を調製する工程、
2)硫酸リチウム溶出液にアルカリを添加してPHを9~10に調整し、硫酸リチウム溶出液中のFe2+、Al3+を沈殿させる工程、
3)工程2)で得られた硫酸リチウム溶出液をろ過し、硫酸リチウム溶出液中のFe2+、Al3+の沈殿物を除去する工程、
4)ろ過で得られた硫酸リチウム溶出液をイオン交換法で処理し、硫酸リチウム溶出液中のCa2+、Mg2+を除去する工程、
5)続いて、得られる濃縮液中のFe2+の濃度<0.0005%、Al3+の濃度<0.0005%、Ca2+の濃度<0.0024%、Mg2+の濃度<0.0040%、且つ、硫酸リチウムの濃度が15~20%となるように、イオン交換処理で得られた硫酸リチウム溶出液を膜濃縮して硫酸リチウム溶出液の濃縮液を得る工程、および、
6)工程5)で得られた硫酸リチウム溶出液の濃縮液に炭酸ナトリウム飽和溶液を添加して炭酸リチウムを沈殿させ、炭酸リチウム沈殿物をろ過分離した後、該炭酸リチウム沈殿物を熱水で洗浄し、乾燥させ、炭酸リチウム完成品を得る工程を含む。
リチウム鉱石の精鉱を用い、硫酸リチウム溶出液を調製した後、硫酸リチウム溶出液に大量のアルカリを添加することのみにより、不純物を除去する。
リチウム鉱石の精鉱を用い、硫酸リチウム溶出液を調製した後、イオン交換法で炭酸リチウム溶出液中の不純物を除去する。
本発明に係る、リチウム鉱石から炭酸リチウムを調製するための方法を実施する。
1 精密ろ過装置
2 イオン交換装置
3 前処理装置
4 限外ろ過膜ろ過装置
5 ディスクチューブ逆浸透膜ろ過装置
6 Li2SO4溶出液産出システム
7 リチウム沈殿システム
8 乾燥システム
Claims (3)
- 1)リチウム鉱石の精鉱を用い、硫酸リチウム溶出液を調製する工程、
2)硫酸リチウム溶出液にアルカリを添加してpHを9~10に調整し、硫酸リチウム溶出液中のFe2+、Al3+を沈殿させる工程、
3)工程2)で得られた硫酸リチウム溶出液をろ過し、硫酸リチウム溶出液中のFe2+、Al3+の沈殿物を除去する工程、
4)ろ過で得られた硫酸リチウム溶出液をイオン交換法で処理し、硫酸リチウム溶出液中のCa2+、Mg2+を除去する工程、
5)続いて、得られる濃縮液中のFe2+の濃度<0.0005%、Al3+の濃度<0.0005%、Ca2+の濃度<0.0024%、Mg2+の濃度<0.0040%、且つ、硫酸リチウムの濃度が15~20%となるよう、イオン交換処理で得られた硫酸リチウム溶出液を膜濃縮して硫酸リチウム溶出液の濃縮液を得る工程、および、
6)工程5)で得られた硫酸リチウム溶出液の濃縮液に炭酸ナトリウム飽和溶液を添加して炭酸リチウムを沈殿させ、炭酸リチウム沈殿物をろ過分離した後、該炭酸リチウム沈殿物を熱水で洗浄し、乾燥させ、炭酸リチウム完成品を得る工程を含むことを特徴とする、
リチウム鉱石から炭酸リチウムを調製するための方法。 - 工程5)において、硫酸リチウム溶出液を濃縮する前に、先に硫酸リチウム溶出液中の懸濁物を除去し、且つ、硫酸リチウム溶出液のpHを調整することを特徴とする、
請求項1に記載のリチウム鉱石から炭酸リチウムを調製するための方法。 - 工程5)における膜濃縮のプロセスは、限外ろ過膜によるろ過、および、逆浸透によるろ過を含むことを特徴とする、
請求項1に記載のリチウム鉱石から炭酸リチウムを調製するための方法。
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