JP2019516662A - 高強度成形アルミナ及び該高強度成形アルミナの製造方法 - Google Patents
高強度成形アルミナ及び該高強度成形アルミナの製造方法 Download PDFInfo
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- JP2019516662A JP2019516662A JP2018561486A JP2018561486A JP2019516662A JP 2019516662 A JP2019516662 A JP 2019516662A JP 2018561486 A JP2018561486 A JP 2018561486A JP 2018561486 A JP2018561486 A JP 2018561486A JP 2019516662 A JP2019516662 A JP 2019516662A
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- alumina
- alumina powder
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- powder
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 222
- 238000004519 manufacturing process Methods 0.000 title claims description 19
- 239000000843 powder Substances 0.000 claims abstract description 141
- 238000000034 method Methods 0.000 claims abstract description 56
- 239000011230 binding agent Substances 0.000 claims abstract description 42
- 239000007788 liquid Substances 0.000 claims abstract description 40
- 238000010304 firing Methods 0.000 claims abstract description 29
- 239000012535 impurity Substances 0.000 claims abstract description 13
- 230000003311 flocculating effect Effects 0.000 claims abstract description 12
- 229910052751 metal Inorganic materials 0.000 claims abstract description 6
- 239000002184 metal Substances 0.000 claims abstract description 6
- 239000002245 particle Substances 0.000 claims description 72
- FAHBNUUHRFUEAI-UHFFFAOYSA-M hydroxidooxidoaluminium Chemical compound O[Al]=O FAHBNUUHRFUEAI-UHFFFAOYSA-M 0.000 claims description 67
- 239000002253 acid Substances 0.000 claims description 36
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 27
- 238000001354 calcination Methods 0.000 claims description 20
- 238000003801 milling Methods 0.000 claims description 18
- 229910001593 boehmite Inorganic materials 0.000 claims description 16
- 230000002776 aggregation Effects 0.000 claims description 12
- VXAUWWUXCIMFIM-UHFFFAOYSA-M aluminum;oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Al+3] VXAUWWUXCIMFIM-UHFFFAOYSA-M 0.000 claims description 8
- 238000005054 agglomeration Methods 0.000 claims description 6
- 238000004220 aggregation Methods 0.000 claims description 6
- 238000005507 spraying Methods 0.000 claims description 3
- 150000002739 metals Chemical class 0.000 abstract 1
- 239000011324 bead Substances 0.000 description 111
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 20
- 230000000052 comparative effect Effects 0.000 description 17
- 230000008569 process Effects 0.000 description 11
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 10
- 235000019253 formic acid Nutrition 0.000 description 10
- 230000000694 effects Effects 0.000 description 9
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 7
- 150000007513 acids Chemical class 0.000 description 7
- 238000001035 drying Methods 0.000 description 7
- 229910017604 nitric acid Inorganic materials 0.000 description 7
- 229910052594 sapphire Inorganic materials 0.000 description 7
- 239000010980 sapphire Substances 0.000 description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 238000010899 nucleation Methods 0.000 description 6
- 239000012798 spherical particle Substances 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
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- 239000006185 dispersion Substances 0.000 description 4
- 238000011065 in-situ storage Methods 0.000 description 4
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 4
- 239000000969 carrier Substances 0.000 description 3
- 230000007423 decrease Effects 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 230000006872 improvement Effects 0.000 description 3
- 238000010902 jet-milling Methods 0.000 description 3
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- 238000007780 powder milling Methods 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- 239000007921 spray Substances 0.000 description 3
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 description 2
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 description 2
- 238000010923 batch production Methods 0.000 description 2
- 150000001735 carboxylic acids Chemical class 0.000 description 2
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- 238000000280 densification Methods 0.000 description 2
- 239000004310 lactic acid Substances 0.000 description 2
- 235000014655 lactic acid Nutrition 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000012856 packing Methods 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 238000001694 spray drying Methods 0.000 description 2
- 239000011975 tartaric acid Substances 0.000 description 2
- 235000002906 tartaric acid Nutrition 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- ZZBAGJPKGRJIJH-UHFFFAOYSA-N 7h-purine-2-carbaldehyde Chemical compound O=CC1=NC=C2NC=NC2=N1 ZZBAGJPKGRJIJH-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 229910001570 bauxite Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000010410 dusting Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 230000009969 flowable effect Effects 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000010309 melting process Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- -1 spheres Substances 0.000 description 1
- 238000005563 spheronization Methods 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
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- C01F7/023—Grinding, deagglomeration or disintegration
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Abstract
Description
本出願は、2016年5月23日に出願された米国特許出願第62/340,048号明細書への優先権を主張し、前記明細書の開示は引用することにより全ての目的のために本明細書に取り込まれる。
例えばビーズ、球、球状粒子又は凝集体の形態の高強度成形アルミナは、油田化学担体、触媒支持体及び触媒、耐火物及びポリマーのための充填剤並びに油田使用のためのプロッパント粒子のような多数の用途に用いられる。高い嵩密度を有する成形アルミナは、るつぼ溶融法(crucible melting processes)による合成サファイアの製造に用いられる。
本発明の1つの局面に従い:
i)ミキサー付きシャフトを含む凝集装置中にアルミナ粉末を供給すること、
ii)アルミナ粉末が凝集装置のシャフトの長さに沿って移動するときにその上に液体結合剤を噴霧して成形アルミナを形成すること、
iii)成形アルミナを焼成すること
を含み、前記凝集装置は、シャフトの長さに沿ってアルミナ粉末を移動させる(displace)ことができる、高強度成形アルミナの製造方法を提供する。
る021面上の寸法測定値を指す。D50値により「メジアン」を意味し、全ての粒子の50%が記載される寸法より小さく、且つ50%が記載される寸法より大きいことを意味する。粒度D50値はMalvern Mastersizer 2000粒度分析器を用いるレーザー散乱により決定される。適したアルミナの例はSasolのCatapal(登録商標) B、Catapal(登録商標) C1、Catapal(登録商標)
D及び35Å〜190Åの結晶子寸法を有する超高純度アルミナ(Ultra High Purity Alumina)である。
間の焼成時間が好ましい。
i)1.20g/ml以上、好ましくは1.65g/mlを超えるゆるみ嵩密度
ii)10m2/g未満、好ましくは5m2/g未満の表面積
iii)5ppm未満、好ましくは3ppm未満そして最も好ましくは2.5ppm未満の個別の金属の不純物、及び、合計で9ppm未満、好ましくは7ppm未満の不純物;並びに
iv)12000psiを超える圧縮強さ(crush strength)
の1つ、2つ以上又は全て、好ましくは2つ以上そして最も好ましくは全てを含む。
i)1.20g/ml以上、好ましくは1.650g/mlを超えるゆるみ嵩密度
ii)10m2/g未満、好ましくは5m2/g未満の表面積
iii)5ppm未満、好ましくは3ppm未満そして最も好ましくは2.5ppm未満の個別の金属の不純物及び合計で9ppm未満、好ましくは7ppm未満の不純物;並びに
iv)12000psiを超える圧縮強さ
の1つ、2つ以上又は全て、好ましくは2つ以上そして最も好ましくは全てを含む成形アルミナを提供する。
本発明は、中心シャフトを有する凝集装置中にアルミナ粉末を供給し、アルミナ粉末が凝集装置のシャフトの長さに沿って移動するときにその上に液体結合剤を噴霧し、成形アルミナを形成することによる高強度成形アルミナの製造方法を記載する。アルミナは凝集体、ビーズ、球状粒子又はそれらの組み合わせの形態にあることができる。成形アルミナは次いで焼成される。
るアルミナの場合、酸機能がすでに粉末供給材料中で与えられているので、液体結合剤として水のみが用いられる場合がある。しかしながら、本発明は必要なら追加の酸を加えることを排除しない。加えられる酸は液体結合剤の5重量%、好ましくは4重量%以下の場合がある。
液体結合剤中の酸としてギ酸又は硝酸を用いる。
021面上の47Åの結晶子寸法及び40ミクロンの粒度D50値を有するアルミナ粉末、Catapal(登録商標) Bアルミナを用いた。ジェットミル微粉砕(jet milling)によりアルミナを30ミクロンの平均粒度D50値に微粉砕した。4%以下の濃度に希釈されたギ酸及び水が液体結合剤を構成した。アルミナ粉末及び液体結合剤にピンミキサーを通過させ、製造されるビーズを続いてスクリーニングしてサイズで区分し、1450℃で10時間焼成し、それらをアルファアルミナ凝集体/ビーズに転換した。
出発Catapal(登録商標) Bアルミナ粉末粒度を、本発明に従いアルミナ粉末を10ミクロンの平均粒度D50値にジェットミル微粉砕することにより微粉砕する以外は、実施例1と同じ方法を用いた。
400Åの結晶子寸法を有するCatapal(登録商標) 200アルミナを用いる以外は実施例1と同じ方法に従った。Catapal(登録商標) 200は400Åの結晶子寸法を有するのでそれは微粉砕されなかった。Catapal(登録商標) 200アルミナはその中に導入されたギ酸を有し、従ってこのその場のギ酸は粉末供給材料の一部として与えられた。液体結合剤は水のみであった。粉末粒度D50値は40ミクロンであった。
微粉砕Catapal Bを25%の比でCatapal(登録商標) 200と配合した。微粉砕Catapal Bは4ミクロンの粒度を有した。ビーズは酸で処理されなかった。液体結合剤は水及び1%ギ酸のブレンドであった。図13は配合された材料の嵩密度を含み、図12は圧縮強さを含む。
021面上の47Åの結晶子寸法及び40ミクロンの粒度D50値を有するアルミナ粉末、微粉砕されないCatapal(登録商標) Bアルミナを用いた。4%以下の濃度に希釈されたギ酸及び水が液体結合剤を構成した。アルミナ粉末及び液体結合剤にピンミキサーを通過させ、製造されるビーズを続いてスクリーニングしてサイズで区分し、1450℃で10時間焼成し、それらをアルファアルミナ凝集体/ビーズに転換した。
ビーズを1600℃で10時間焼成する以外は比較例1と同じ方法を用いた。
021面上の47Åの結晶子寸法及び40ミクロンの粒度D50値を有するアルミナ粉末、微粉砕されないCatapal(登録商標) Bアルミナを用いた。液体結合剤は2.5%以下の濃度に希釈された硝酸及び水であった。アルミナ粉末及び液体結合剤にピンミキサーを通過させ、製造されるビーズを続いてスクリーニングしてサイズで区分し、1600℃で10時間焼成し、それらをアルファアルミナ凝集体/ビーズに転換した。
出発アルミナが微粉砕されないDiapal(登録商標) 15N4アルミナ(186Å)である以外は実施例1と同じ方法を用いた。この製品はその製造の間にアルミナ中に導入された硝酸を有する。この実施例では、アルミナ粉末中に酸が存在するので、液体結合剤として水のみを用いた。粉末粒度D50値は40ミクロンであった。
Catapal(登録商標) Bアルミナを77Åの結晶子寸法を有するCatapal(登録商標) Dアルミナに置き換える以外は、実施例1と同じ方法に従った。粉末粒度D50値は40ミクロンであった。
における焼成(比較例1)は、微粉砕されないCatapal(登録商標) Bアルミナの1600℃における焼成(比較例2及び3)より低い強度を与えることが容易にわかる。比較例2と比較例3の間のさらなる比較は、ギ酸及び硝酸が同じ焼成温度において類似の強度のビーズを与えることを示す。
7Å)により示される通り、異なる結晶子寸法を有する粉末に関して類似であった。
アルミナのデータと油田破砕操作(fracturing operation)のために用いられる市販のプロッパントとの比較を図11に示す。プロッパントの強度の範囲をグラフ上で斜線部分により示し、それは引用することにより記載事項が全ての目的のた
めに本明細書の内容となるHarris,J.T.,Finite Element Modeling of Particle Failure in Stressed Particles Bes,M.S.Thesis,Engineering,Mechanics,Pennsylvania State University(2008)により記載されている市販の焼結ボーキサイト及びシリカ−アルミナプロッパントビーズに関する強度値の範囲を表す。40ミクロンの平均粉末直径の粒度D50値を有し、1450℃で焼成されるCatapal(登録商標) Bアルミナから製造されるビーズは、いずれの直径においても代表的なプロッパントの型より有意に低い平均圧縮強さを有する。これはグラフの最下部における曲線により示される。1600℃に焼成温度を上昇させると、グラフ上の上部の曲線により示される通り、市販のプロッパントの範囲内である強度が得られる。
アルミナの純度はサファイア製造に関する決定的な問題である。表IIはa)出発アルミナ粉末、b)高純度ベーマイトのジェットミル微粉砕及び高せん断凝集装置における成形により製造される非焼成ビーズ及びc)焼成後のビーズに関する金属不純物分析を示す。本発明の方法を介して生成物の汚染が起こらないか又は非常に少ないことがわかる。この可能な汚染の低いレベルは、ビーズの成形方法を合成サファイア製造方法のための高い嵩密度のるつぼ充填物の製造に適したものとしている。
Claims (17)
- 高強度成形アルミナの製造方法であって:
i)ミキサー付きシャフトを含む凝集装置中にアルミナ粉末を供給すること、
ii)前記アルミナ粉末が前記凝集装置のシャフトの長さに沿って移動するときに前記アルミナ粉末の上に液体結合剤を噴霧して成形アルミナを形成すること、及び
iii)前記成形アルミナを焼成すること
を含み、
前記凝集装置は、シャフトの長さに沿ってアルミナ粉末を移動させることができる、方法。 - 前記アルミナ粉末が水酸化酸化アルミニウム(AlOOH)、ベーマイト又は擬ベーマイトを含む、請求項1に記載の方法。
- 前記アルミナ粉末が35Å〜190Åの結晶子寸法及び40ミクロン以上の粒度D50値を有する、請求項1又は2に記載の方法。
- 前記アルミナ粉末が300Å〜500Åの結晶子寸法を有する、請求項1又は2に記載の方法。
- 前記アルミナ粉末が、35Å〜190Åの結晶子寸法及び40ミクロン以上の粒度D50値を有するアルミナ粉末と、300Å〜500Åの結晶子寸法を有するアルミナ粉末との組み合わせである、請求項1又は2に記載の方法。
- 35Å〜190Åの結晶子寸法及び40ミクロン以上の粒度D50値を有する前記アルミナ粉末を凝集装置中に供給する前に、そのようなアルミナ粉末を微粉砕して40ミクロン未満の平均粒度D50値を有するアルミナ粉末を製造する初期ステップを含む、請求項3又は5に記載の方法。
- 35Å〜190Åの結晶子寸法及び40ミクロン以上の粒度D50値を有する前記アルミナ粉末を30ミクロンの平均粒度D50値に微粉砕する、請求項6に記載の方法。
- 35Å〜190Åの結晶子寸法及び40ミクロン以上の粒度D50値を有する前記アルミナ粉末を10ミクロン以下の平均粒度D50値に微粉砕する、請求項6に記載の方法。
- 35Å〜190Åの結晶子寸法及び40ミクロン以上の粒度D50値を有するアルミナ粉末を40ミクロン未満の平均粒度D50値に微粉砕して微粉砕アルミナ粉末を形成し、該微粉砕アルミナ粉末を微粉砕する必要のない300Å〜500Åの結晶子寸法を有するアルミナ粉末と組み合わせる初期ステップを含む、請求項1〜8のいずれか1つに記載の方法。
- アルミナ製造法の一部として前記アルミナ粉末がアルミナ粉末中に導入された酸を含む、請求項1〜9のいずれか1つに記載の方法。
- 前記液体結合剤が水を含む、請求項10に記載の方法。
- 前記液体結合剤が水及び酸を含む、請求項1〜10のいずれか1つに記載の方法。
- アルミナ粉末対液体結合剤の比が重量に基づいて1.5:1〜15:1である、請求項1〜12のいずれか1つに記載の方法。
- 前記アルミナ粉末対液体結合剤の比が1.8:1〜10:1である、請求項13に記載の方法。
- 焼成温度が1250℃〜1700℃であり、1時間〜40時間にわたり焼成を行う、請求項1〜14のいずれか1つに記載の方法。
- 請求項1〜15の方法に従って製造され、以下の性質:
i)1.20g/ml以上、好ましくは1.65g/mlを超えるゆるみ嵩密度、
ii)10m2/g未満、好ましくは5m2/g未満の表面積、
iii)5ppm未満、好ましくは3ppm未満、そして最も好ましくは2.5ppm未満の個別の金属の不純物、及び、合計で9ppm未満、好ましくは7ppm未満の不純物、並びに
iv)12000psiを超える圧縮強さ
の少なくとも1つを有する、高強度成形アルミナ。 - 以下の性質:
i)1.20g/ml以上、好ましくは1.650g/mlを超えるゆるみ嵩密度、
ii)10m2/g未満、好ましくは5m2/g未満の表面積、
iii)5ppm未満、好ましくは3ppm未満、そして最も好ましくは2.5ppm未満の個別の金属の不純物、及び、合計で9ppm未満、好ましくは7ppm未満の不純物;並びに
iv)12000psiを超える圧縮強さ
の少なくとも1つを含む、成形アルミナ。
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CN109476550A (zh) | 2019-03-15 |
US11884594B2 (en) | 2024-01-30 |
WO2017205286A1 (en) | 2017-11-30 |
WO2017205286A9 (en) | 2018-02-15 |
CA3024172A1 (en) | 2017-11-30 |
RU2759835C2 (ru) | 2021-11-18 |
US20210403383A1 (en) | 2021-12-30 |
JP7042754B2 (ja) | 2022-03-28 |
RU2018144008A3 (ja) | 2020-10-07 |
US20190210926A1 (en) | 2019-07-11 |
RU2018144008A (ru) | 2020-06-25 |
US11091396B2 (en) | 2021-08-17 |
KR102366730B1 (ko) | 2022-02-22 |
EP3464215A1 (en) | 2019-04-10 |
KR20190026685A (ko) | 2019-03-13 |
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