JP6494803B2 - フェライト金属酸化物触媒の製造方法 - Google Patents
フェライト金属酸化物触媒の製造方法 Download PDFInfo
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- 239000003054 catalyst Substances 0.000 title claims description 104
- 229910000859 α-Fe Inorganic materials 0.000 title claims description 38
- 229910044991 metal oxide Inorganic materials 0.000 title claims description 36
- 150000004706 metal oxides Chemical class 0.000 title claims description 36
- 238000004519 manufacturing process Methods 0.000 title claims description 34
- 238000001354 calcination Methods 0.000 claims description 53
- KAKZBPTYRLMSJV-UHFFFAOYSA-N Butadiene Chemical compound C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 0.000 claims description 50
- 239000002243 precursor Substances 0.000 claims description 28
- YIXJRHPUWRPCBB-UHFFFAOYSA-N magnesium nitrate Chemical compound [Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YIXJRHPUWRPCBB-UHFFFAOYSA-N 0.000 claims description 24
- VXNZUUAINFGPBY-UHFFFAOYSA-N 1-Butene Chemical compound CCC=C VXNZUUAINFGPBY-UHFFFAOYSA-N 0.000 claims description 21
- 239000000843 powder Substances 0.000 claims description 16
- MVFCKEFYUDZOCX-UHFFFAOYSA-N iron(2+);dinitrate Chemical compound [Fe+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MVFCKEFYUDZOCX-UHFFFAOYSA-N 0.000 claims description 12
- 239000012159 carrier gas Substances 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 7
- 239000002798 polar solvent Substances 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical group O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 239000011541 reaction mixture Substances 0.000 claims description 6
- 238000005979 thermal decomposition reaction Methods 0.000 claims description 6
- 239000012153 distilled water Substances 0.000 claims description 5
- 239000007789 gas Substances 0.000 claims description 5
- ZTERWYZERRBKHF-UHFFFAOYSA-N magnesium iron(2+) oxygen(2-) Chemical compound [Mg+2].[O-2].[Fe+2].[O-2] ZTERWYZERRBKHF-UHFFFAOYSA-N 0.000 description 26
- 230000000052 comparative effect Effects 0.000 description 22
- 230000000694 effects Effects 0.000 description 14
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 11
- 238000006243 chemical reaction Methods 0.000 description 9
- 239000000243 solution Substances 0.000 description 8
- 239000011777 magnesium Substances 0.000 description 7
- 230000004580 weight loss Effects 0.000 description 7
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 6
- 229910052749 magnesium Inorganic materials 0.000 description 6
- 238000005839 oxidative dehydrogenation reaction Methods 0.000 description 6
- 239000000376 reactant Substances 0.000 description 6
- 239000013078 crystal Substances 0.000 description 5
- 230000003247 decreasing effect Effects 0.000 description 5
- 238000002347 injection Methods 0.000 description 5
- 239000007924 injection Substances 0.000 description 5
- 229910052742 iron Inorganic materials 0.000 description 5
- 229910002651 NO3 Inorganic materials 0.000 description 4
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 4
- 239000006227 byproduct Substances 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 230000007423 decrease Effects 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 238000000975 co-precipitation Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000006104 solid solution Substances 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- IAQRGUVFOMOMEM-UHFFFAOYSA-N butene Natural products CC=CC IAQRGUVFOMOMEM-UHFFFAOYSA-N 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000003384 imaging method Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000002429 nitrogen sorption measurement Methods 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 238000005118 spray pyrolysis Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 239000013585 weight reducing agent Substances 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/78—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with alkali- or alkaline earth metals
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/61—Surface area
- B01J35/613—10-100 m2/g
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/0009—Use of binding agents; Moulding; Pressing; Powdering; Granulating; Addition of materials ameliorating the mechanical properties of the product catalyst
- B01J37/0027—Powdering
- B01J37/0045—Drying a slurry, e.g. spray drying
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/04—Mixing
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/082—Decomposition and pyrolysis
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C5/00—Preparation of hydrocarbons from hydrocarbons containing the same number of carbon atoms
- C07C5/42—Preparation of hydrocarbons from hydrocarbons containing the same number of carbon atoms by dehydrogenation with a hydrogen acceptor
- C07C5/48—Preparation of hydrocarbons from hydrocarbons containing the same number of carbon atoms by dehydrogenation with a hydrogen acceptor with oxygen as an acceptor
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C2523/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group C07C2521/00
- C07C2523/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group C07C2521/00 of the iron group metals or copper
- C07C2523/74—Iron group metals
- C07C2523/745—Iron
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C2523/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group C07C2521/00
- C07C2523/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group C07C2521/00 of the iron group metals or copper
- C07C2523/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group C07C2521/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups C07C2523/02 - C07C2523/36
- C07C2523/78—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group C07C2521/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups C07C2523/02 - C07C2523/36 with alkali- or alkaline earth metals or beryllium
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Catalysts (AREA)
- Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Description
硝酸鉄(Fe(NO3)3・6H2O、SAMCHUN、98.5%、20.5kg)と硝酸マグネシウム(Mg(NO3)2・6H2O、SAMCHUN、98%、6.5kg)を蒸留水に溶解させ、撹拌しながら、マグネシウムおよび鉄が2:1のモル比で含有された溶液を製造した。製造された溶液を時間当たり3Lずつ空気(3気圧)をキャリアガスとして750℃の反応器の内部に噴霧しながら触媒粉末を製造した。製造された触媒粉末を貯蔵槽に運搬した後、500℃で3時間か焼して、マグネシウム−鉄酸化物触媒を製造した。
か焼温度を550℃に設定したことを除いて、前記実施例1と同じ条件下にマグネシウム−鉄酸化物触媒を製造した。
か焼温度を600℃に設定したことを除いて、前記実施例1と同じ条件下にマグネシウム−鉄酸化物触媒を製造した。
前記実施例1と同じ条件でマグネシウム−鉄酸化物触媒を製造するが、か焼段階を省略した。
か焼温度を650℃に設定したことを除いて、前記実施例1と同じ条件下にマグネシウム−鉄酸化物触媒を製造した。
前記実施例1〜3および比較例1〜2によって製造されたマグネシウム−鉄酸化物触媒の結晶構造を確認するために、40kV、40mA条件でNi−Filterを使用するX線回折分析器(Siemens D−5005、Cukα=1.5418ÅA)でXRD分析を行い、その結果を図2に示した。図2を参照すると、触媒の製造条件に関係なく、マグネシウム−鉄酸化物触媒の結晶構造がスピネル構造であることを確認した。
か焼時間を2時間に設定したことを除いて、前記実施例1と同じ条件下にマグネシウム−鉄酸化物触媒を製造した。
か焼時間を1時間に設定したことを除いて、前記実施例1と同じ条件下にマグネシウム−鉄酸化物触媒を製造した。
か焼温度を450℃に設定したことを除いて、前記実施例1と同じ条件下にマグネシウム−鉄酸化物触媒を製造した。
か焼時間を30分に設定したことを除いて、前記実施例1と同じ条件下にマグネシウム−鉄酸化物触媒を製造した。
か焼時間を5時間に設定したことを除いて、前記実施例1と同じ条件下にマグネシウム−鉄酸化物触媒を製造した。
前記実施例1〜5および比較例1〜5によって製造されたマグネシウム−鉄酸化物触媒の表面積を分析するために、体積式窒素吸着測定装置(Quantachrome、ASiQ AGC/TCD)を利用して窒素吸着量を測定した後、BET式を利用して表面積を計算し、その結果を下記表1に示した。
前記実施例1および比較例1によって製造されたマグネシウム−鉄酸化物触媒の粒度および形状を分析するために、イメージング顕微鏡(ICAMSCOPE、SOMTECH)を利用してイメージを観察し、その結果を図3に示した。
前記実施例1〜5および比較例1〜5によって製造されたマグネシウム−鉄酸化物触媒をステンレス反応器に充填し、空気を注入しながら370℃で活性化させた。反応物であるC4混合物(n−ブテン):空気:スチームの混合比が5.2体積%:17.2体積%:77.6体積%である混合気体を、400h−1の空間速度(GHSV、Gas Hourly Space Velocity)で前記反応器を通過するように流しながら、1,3−ブタジエンを製造した。n−ブテンの転換率、1、3−ブタジエンの選択度、および1,3−ブタジエンの収率をそれぞれ下記数式1〜3を利用して計算し、その結果を下記表2に示した。
Claims (11)
- (a)マグネシウム硝酸塩前駆体および鉄硝酸塩前駆体を極性溶媒に溶解させて、前駆体溶液を製造する段階と、
(b)前記前駆体溶液をキャリアガスを利用して反応器の内部に噴霧しながら熱分解させて、触媒粉末を形成する段階と、
(c)前記触媒粉末を貯蔵槽に運搬した後、前記貯蔵槽でか焼する段階と、を含むフェライト金属酸化物触媒の製造方法であって、
前記(c)段階で、前記か焼する段階の温度が500℃〜600℃であることを特徴とする、フェライト金属酸化物触媒の製造方法。 - 前記(a)段階で、前記マグネシウム硝酸塩前駆体および前記鉄硝酸塩前駆体がそれぞれ硝酸マグネシウムおよび硝酸鉄であることを特徴とする、請求項1に記載のフェライト金属酸化物触媒の製造方法。
- 前記(a)段階で、前記極性溶媒が蒸留水であることを特徴とする、請求項1または2に記載のフェライト金属酸化物触媒の製造方法。
- 前記(b)段階で、前記キャリアガスが空気であることを特徴とする、請求項1〜3のいずれか1項に記載のフェライト金属酸化物触媒の製造方法。
- 前記(b)段階で、前記空気の圧力が2気圧〜4気圧であることを特徴とする、請求項4に記載のフェライト金属酸化物触媒の製造方法。
- 前記(b)段階で、前記熱分解温度が500℃〜900℃であることを特徴とする、請求項1〜5のいずれか1項に記載のフェライト金属酸化物触媒の製造方法。
- 前記(c)段階で、前記か焼が1時間〜4時間行われることを特徴とする、請求項1〜6のいずれか1項に記載のフェライト金属酸化物触媒の製造方法。
- 請求項1〜7のいずれか1項に記載の製造方法により製造されたフェライト金属酸化物触媒を反応器に充填する段階と、
前記反応器にn−ブテンを含有する反応混合物を注入して通過させる段階と、を含む1,3−ブタジエンの製造方法。 - 前記反応混合物がn−ブテン4〜12体積%、空気16〜30体積%、およびスチーム60〜80体積%を含むことを特徴とする、請求項8に記載の1,3−ブタジエンの製造方法。
- 前記反応混合物を100h−1〜700h−1の空間速度(GHSV、Gas Hourly Space Velocity)で注入することを特徴とする、請求項8または9に記載の1,3−ブタジエンの製造方法。
- 前記反応器の温度を300℃〜500℃に調節することを特徴とする、請求項8〜10のいずれか1項に記載の1,3−ブタジエンの製造方法。
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KR10-2015-0079758 | 2015-06-05 | ||
KR1020150079758A KR101701973B1 (ko) | 2015-06-05 | 2015-06-05 | 페라이트 금속 산화물 촉매의 제조방법 |
PCT/KR2015/008657 WO2016195162A1 (ko) | 2015-06-05 | 2015-08-19 | 페라이트 금속 산화물 촉매의 제조방법 |
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US (1) | US9943831B2 (ja) |
JP (1) | JP6494803B2 (ja) |
KR (1) | KR101701973B1 (ja) |
CN (1) | CN107771101B (ja) |
DE (1) | DE112015006597T5 (ja) |
MY (1) | MY173112A (ja) |
PH (1) | PH12017502194A1 (ja) |
SG (1) | SG11201710009TA (ja) |
WO (1) | WO2016195162A1 (ja) |
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KR101884928B1 (ko) * | 2017-03-28 | 2018-08-30 | 금호석유화학 주식회사 | 금속산화물 촉매, 그 제조방법, 및 이를 이용한 알코올의 제조방법 |
KR102353146B1 (ko) * | 2018-03-13 | 2022-01-18 | 주식회사 엘지화학 | 페라이트계 코팅 촉매의 제조방법 및 이를 이용한 부타디엔의 제조방법 |
KR20190118345A (ko) * | 2018-04-10 | 2019-10-18 | 주식회사 엘지화학 | 금속 복합 촉매의 제조방법 및 이에 의해 제조된 금속 복합 촉매 |
KR102568103B1 (ko) * | 2018-09-21 | 2023-08-17 | 주식회사 엘지화학 | 1,3-부타디엔의 제조방법 |
KR102564957B1 (ko) * | 2018-09-21 | 2023-08-07 | 주식회사 엘지화학 | 1,3-부타디엔의 제조방법 |
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KR100956421B1 (ko) * | 2007-12-24 | 2010-05-06 | 엠파워(주) | 분무 열분해 방법을 이용한 탄소나노튜브용 촉매 제조장치및 촉매 제조방법 |
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KR101503295B1 (ko) * | 2013-04-02 | 2015-03-18 | 한국기계연구원 | 분무열분해에 의한 나노 형태의 3원계 알루미늄 산화물 코어 분말의 제조방법 |
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SG11201710009TA (en) | 2018-01-30 |
KR101701973B1 (ko) | 2017-02-03 |
WO2016195162A1 (ko) | 2016-12-08 |
MY173112A (en) | 2019-12-27 |
US9943831B2 (en) | 2018-04-17 |
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