JP2020502037A - 亜酸化チタンの多孔質セラミック生成物 - Google Patents
亜酸化チタンの多孔質セラミック生成物 Download PDFInfo
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- JP2020502037A JP2020502037A JP2019554029A JP2019554029A JP2020502037A JP 2020502037 A JP2020502037 A JP 2020502037A JP 2019554029 A JP2019554029 A JP 2019554029A JP 2019554029 A JP2019554029 A JP 2019554029A JP 2020502037 A JP2020502037 A JP 2020502037A
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- titanium dioxide
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- porous product
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- 239000010936 titanium Substances 0.000 title claims abstract description 64
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 18
- 229910052719 titanium Inorganic materials 0.000 title claims abstract description 18
- 239000000919 ceramic Substances 0.000 title description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 87
- 238000000034 method Methods 0.000 claims abstract description 42
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 31
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 24
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 22
- 239000000126 substance Substances 0.000 claims abstract description 20
- 239000012298 atmosphere Substances 0.000 claims abstract description 17
- 238000007493 shaping process Methods 0.000 claims abstract description 13
- 238000005245 sintering Methods 0.000 claims abstract description 13
- 230000007935 neutral effect Effects 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 230000001590 oxidative effect Effects 0.000 claims abstract description 5
- 239000000203 mixture Substances 0.000 claims description 42
- 239000011148 porous material Substances 0.000 claims description 27
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 18
- 239000006229 carbon black Substances 0.000 claims description 16
- 238000009826 distribution Methods 0.000 claims description 11
- 239000002994 raw material Substances 0.000 claims description 9
- 239000000463 material Substances 0.000 claims description 8
- 229910010272 inorganic material Inorganic materials 0.000 claims description 7
- 239000011147 inorganic material Substances 0.000 claims description 7
- 150000001340 alkali metals Chemical class 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- 229910052788 barium Inorganic materials 0.000 claims description 4
- 229910052804 chromium Inorganic materials 0.000 claims description 4
- 238000001704 evaporation Methods 0.000 claims description 4
- 229910052712 strontium Inorganic materials 0.000 claims description 4
- 229910052783 alkali metal Inorganic materials 0.000 claims description 3
- 229910052742 iron Inorganic materials 0.000 claims description 3
- 229910052748 manganese Inorganic materials 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 150000002894 organic compounds Chemical class 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- 229910000272 alkali metal oxide Inorganic materials 0.000 claims description 2
- 229910052784 alkaline earth metal Inorganic materials 0.000 claims description 2
- 229910000287 alkaline earth metal oxide Inorganic materials 0.000 claims description 2
- 150000001342 alkaline earth metals Chemical class 0.000 claims description 2
- 239000000571 coke Substances 0.000 claims description 2
- 230000008020 evaporation Effects 0.000 claims description 2
- 229910004298 SiO 2 Inorganic materials 0.000 claims 2
- 239000000377 silicon dioxide Substances 0.000 claims 1
- 238000010438 heat treatment Methods 0.000 abstract description 9
- 229910003087 TiOx Inorganic materials 0.000 abstract 1
- 238000002360 preparation method Methods 0.000 abstract 1
- HLLICFJUWSZHRJ-UHFFFAOYSA-N tioxidazole Chemical compound CCCOC1=CC=C2N=C(NC(=O)OC)SC2=C1 HLLICFJUWSZHRJ-UHFFFAOYSA-N 0.000 abstract 1
- 239000012528 membrane Substances 0.000 description 16
- 239000000843 powder Substances 0.000 description 12
- 150000001875 compounds Chemical class 0.000 description 11
- 239000002245 particle Substances 0.000 description 11
- 238000000465 moulding Methods 0.000 description 8
- 229910010413 TiO 2 Inorganic materials 0.000 description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 6
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 6
- 229910052753 mercury Inorganic materials 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 238000001125 extrusion Methods 0.000 description 5
- 230000014759 maintenance of location Effects 0.000 description 5
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 239000000356 contaminant Substances 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 229910052786 argon Inorganic materials 0.000 description 3
- 238000000354 decomposition reaction Methods 0.000 description 3
- 238000003487 electrochemical reaction Methods 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 229910052700 potassium Inorganic materials 0.000 description 3
- 239000000376 reactant Substances 0.000 description 3
- 229910052708 sodium Inorganic materials 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- 238000000108 ultra-filtration Methods 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 238000003991 Rietveld refinement Methods 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 229910052791 calcium Inorganic materials 0.000 description 2
- 238000012512 characterization method Methods 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 238000000157 electrochemical-induced impedance spectroscopy Methods 0.000 description 2
- 238000000635 electron micrograph Methods 0.000 description 2
- 238000005469 granulation Methods 0.000 description 2
- 230000003179 granulation Effects 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000000314 lubricant Substances 0.000 description 2
- 238000009285 membrane fouling Methods 0.000 description 2
- -1 more preferably Substances 0.000 description 2
- 239000004014 plasticizer Substances 0.000 description 2
- 238000002459 porosimetry Methods 0.000 description 2
- 230000008929 regeneration Effects 0.000 description 2
- 238000011069 regeneration method Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- MTPVUVINMAGMJL-UHFFFAOYSA-N trimethyl(1,1,2,2,2-pentafluoroethyl)silane Chemical compound C[Si](C)(C)C(F)(F)C(F)(F)F MTPVUVINMAGMJL-UHFFFAOYSA-N 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- 229920003108 Methocel™ A4M Polymers 0.000 description 1
- KEXCKZCLTTUBOQ-UHFFFAOYSA-N Putrol Natural products CCC1C(O)CC2(C)CCC3(C)C(=CCC4C5(C)CCCC(C)(C)C5CCC34C)C12 KEXCKZCLTTUBOQ-UHFFFAOYSA-N 0.000 description 1
- 229910008484 TiSi Inorganic materials 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 239000003242 anti bacterial agent Substances 0.000 description 1
- 239000002260 anti-inflammatory agent Substances 0.000 description 1
- 229940088710 antibiotic agent Drugs 0.000 description 1
- 239000012300 argon atmosphere Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000002902 bimodal effect Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 150000001721 carbon Chemical class 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000000748 compression moulding Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000001627 detrimental effect Effects 0.000 description 1
- 238000003618 dip coating Methods 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000008240 homogeneous mixture Substances 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 239000010955 niobium Substances 0.000 description 1
- 229910000484 niobium oxide Inorganic materials 0.000 description 1
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000006259 organic additive Substances 0.000 description 1
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- BPUBBGLMJRNUCC-UHFFFAOYSA-N oxygen(2-);tantalum(5+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ta+5].[Ta+5] BPUBBGLMJRNUCC-UHFFFAOYSA-N 0.000 description 1
- CHWRSCGUEQEHOH-UHFFFAOYSA-N potassium oxide Chemical compound [O-2].[K+].[K+] CHWRSCGUEQEHOH-UHFFFAOYSA-N 0.000 description 1
- 229910001950 potassium oxide Inorganic materials 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000004626 scanning electron microscopy Methods 0.000 description 1
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 1
- 229910001948 sodium oxide Inorganic materials 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 229910001936 tantalum oxide Inorganic materials 0.000 description 1
- 239000012855 volatile organic compound Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
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Abstract
Description
(a)少なくとも一つの二酸化チタン源、炭素を含有する還元剤、及び好ましくは水のような溶媒と混合された、任意の一つ又は複数の有機物質、例えば、結合剤、可塑剤、潤滑剤などを含む原料を混合すること;
(b)例えば、押出成形、加圧成形、テープ成形、又は造粒によって、生成物を成形すること;
(c)任意に、特に工程(a)の間に有機物質が使用されたときに、一つ又は複数の有機物質を高い割合で除去するのに十分な温度であって、還元剤の蒸発温度よりも低い温度で、空気又は酸化雰囲気下で熱処理を行うこと;
(d)例えば、1150℃を超えるが、1430℃を超えない温度で、中性雰囲気又は還元雰囲気下で焼結を行うこと。
− この生成物を構成する材料は、一般式TiOxに対応しており、ここで、xの値が1.6〜1.9、好ましくは1.75〜1.85である;
− 細孔径分布が、およそ単峰性である:
− 細孔のメジアン径d50が、0.5〜5μm、特に1〜2.5μmである;
− 開放気孔率が、34%を上回る。
1)難分解性の生成物中に存在する結晶相を、X線回折によって特徴付けた。得られた結果を表に示す。これらの表において、PPは、一つ又は複数の主となる相を指し、PMは、一つ又は複数の少量の相を指す。本発明の意味するところにおいて、相は、生成物の全重量の少なくとも25%を占めるときに「主となる」相と見なされる。相は、生成物の重量の5%を超えるが25%未満の量を占めるとき、特に、生成物の重量の5%を超えるが20%未満の量を占めるとき、好ましくは、生成物の重量の5%を超えるが15%未満の量を占めるときに、「少量の」相と見なされ、少量の相の重量の合計は、通常、生成物の重量の50%未満であり、好ましくは、生成物の重量の30%未満、さらには20%未満である。
− 実施例1では、カーボンブラックの水準が、必要とされるマグネリ相を得るためには不十分である。
− 実施例8及び9では、二酸化チタン源が、粉末状のルチルである。
− 実施例14では、焼結するための熱処理の温度が高すぎる。
− 実施例15では、有機化合物を取り除くための熱処理の温度が高すぎ、これは、一部の還元剤の除去をもたらす。
− ルチル相は、本発明による生成物を構成する材料に望ましい多孔率をもたらさないので、二酸化チタン源として、二酸化チタンのアナターゼ型を、少なくとも55重量%を超える割合で使用することが必要である;
− 還元剤の必要な量は、望ましいマグネリ相を得るために調整しなければならない;
− 有機物質の存在下に、空気又は酸化雰囲気下での熱処理を、酸化チタンの還元剤の蒸発温度を下回る温度で行わなければならず、例えば、還元剤がカーボンブラックであるときには、450℃を下回る温度で行わなければならない;
− 本発明による方法で得られた生成物は、34%を超えるか又はこれに等しい多孔率を有する;
− 細孔径分布は、単峰性であり、かつマイクロメーターの位である。
Claims (16)
- 以下の工程を含む、一般式TiOxで示され、xの値が1.6〜1.9である、本質的に、一つ又は複数の亜酸化チタンからなる多孔質生成物の製造方法:
(a)少なくとも一つの二酸化チタン源、炭素を含有する還元剤、及び好ましくは水のような溶媒と混合された、任意の一つ又は複数の有機物質を含む原料を混合すること;
(b)生成物を成形すること;
(c)任意に、特に工程(a)の間に有機物質が使用されたときに、一つ又は複数の前記有機物質を高い割合で除去するのに十分な温度であって、前記還元剤の蒸発温度よりも低い温度で、空気又は酸化雰囲気下で熱処理を行うこと;
(d)例えば、1150℃を超えるが、1430℃を超えない温度で、中性又は還元雰囲気下で焼結を行うこと;
ここで、二酸化チタン源は、少なくとも55重量%のアナターゼからなる。 - 前記多孔質生成物が、xの値が1.6〜1.9、好ましくは、1.75〜1.85である一般式TiOxに相当するように、前記還元剤の量を調整する、請求項1に記載の方法。
- 前記初期混合物が、前記二酸化チタン源として、90重量%を超えるアナターゼを含み、好ましくは、アナターゼ型のみを含む、請求項1又は2に記載の方法。
- 炭素を含有する前記還元剤が、カーボンブラック、コークス、又は少なくとも50重量%の炭素、若しくは少なくとも70重量%の炭素、若しくは80重量%の炭素を含有する任意のその他の有機化合物から選択される、請求項1〜3のいずれか一項に記載の方法。
- 前記還元剤が、カーボンブラックである、請求項1〜4のいずれか一項に記載の方法。
- 前記初期混合物が、二酸化チタンの全重量に対して、1.5〜5.0重量%の炭素を含む、請求項1〜5のいずれか一項に記載の方法。
- 工程(d)が、中性雰囲気下で行われる、請求項1〜6のいずれか一項に記載の方法。
- 工程(d)が、還元雰囲気下で行われる、請求項1〜6のいずれか一項に記載の方法。
- 前記原料の混合物が、少なくとも90重量%のアナターゼ型の二酸化チタン、及び少なくとも3重量%のカーボンブラックを含有し、かつ前記焼結温度を、好ましくは、中性雰囲気下で、1300℃〜1450℃に調整する、請求項1〜8のいずれか一項に記載の方法。
- 前記多孔質生成物は、本質的に、Ti4O7及び/又はTi5O9から選択されるマグネリ相からなる、請求項1〜9のいずれか一項に記載の方法。
- 前記原料の初期混合物が、全無機物質の重量の5.0%を下回る量で、二酸化チタン以外の無機物質を含む、請求項1〜10のいずれか一項に記載の方法。
- 前記原料の初期混合物が、二酸化チタン以外の無機物質を含み、前記無機物質が、SiO2であるシリカ;Nb2O5若しくはTa2O5、V2O5、ZrO2である酸化物;又はBa、Sr、Mn、Cr、Feの酸化物;又はアルカリ金属若しくはアルカリ土類金属の酸化物;からなる群から選択される、請求項1〜11のいずれか一項に記載の方法。
- 以下の特徴を有する、多孔質生成物:
− 前記生成物を構成する材料は、一般式TiOxに対応しており、ここで、xの値が1.6〜1.9、好ましくは1.75〜1.85である;
− 細孔径分布が、およそ単峰性である:
− 細孔のメジアン径d50が、0.5〜5μmである;
− 開放気孔率が、34%を上回る。 - Ti4O7、Ti5O9、Ti6O11、又はこれらの相の少なくとも2つの混合物から選択されるマグネリ相を、合計で、90重量%を超えて含んでいる、請求項13に記載の多孔質生成物。
- 細孔のメジアン径d50が、1〜2.5μmである、請求項13又は14に記載の多孔質生成物。
- 全無機物質の重量の5.0%を下回る量で、二酸化チタン以外の無機物質をさらに含み、追加の前記無機物質が、SiO2であるシリカ;Nb2O5若しくはTa2O5、V2O5、ZrO2である酸化物;Ba、Sr、Mn、Cr、Feの酸化物;又はアルカリ金属若しくはアルカリ土類金属の酸化物;からなる群から選択される、請求項13〜15のいずれか一項に記載の多孔質生成物。
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WO2020041712A1 (en) * | 2018-08-23 | 2020-02-27 | Evoqua Water Technologies Llc | System and method for electrochemical oxidation of polyfluoroalkyl substances in water |
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EP3558895A1 (fr) | 2019-10-30 |
RU2019122413A (ru) | 2021-01-22 |
AU2017383345B2 (en) | 2022-12-01 |
US10934218B2 (en) | 2021-03-02 |
MX2019007318A (es) | 2019-08-16 |
AU2017383345A1 (en) | 2019-07-04 |
FR3060554B1 (fr) | 2022-04-01 |
EP3558895B1 (fr) | 2023-09-13 |
KR102478403B1 (ko) | 2022-12-19 |
CA3046408A1 (fr) | 2018-06-28 |
RU2753684C2 (ru) | 2021-08-19 |
DK3558895T3 (da) | 2023-10-30 |
CN110088062A (zh) | 2019-08-02 |
FR3060554A1 (fr) | 2018-06-22 |
BR112019010813A2 (pt) | 2019-10-01 |
CN110088062B (zh) | 2022-07-29 |
RU2019122413A3 (ja) | 2021-02-08 |
JP7084940B2 (ja) | 2022-06-15 |
KR20190090811A (ko) | 2019-08-02 |
US20190315661A1 (en) | 2019-10-17 |
WO2018115749A1 (fr) | 2018-06-28 |
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