Ulusal anahtar araştırma & geliştirme Program Bakanlığı bilim ve teknoloji Çin (2016YFB0600305), Ulusal Doğa Bilimleri Foundation of China (NOS 21573031 ve 21373038), Program tarafından sağlanan mali destek minnetle anıyoruz Dalian City (2016RD09) ve teknolojik ve daha yüksek Eğitim Enstitüsü Hong Kong (THEi SG1617105 ve THEi SG1617127) mükemmel yetenekleri için.

Uyarı: Uygun işleme yöntemlerini, özelliklerini ve bu makalede açıklanan kimyasal maddelerin toksisite ilgili malzeme güvenlik bilgi formları (MSDS) bakın. Bazı kullanılan kimyasalların toksik ve kanserojen ve özel bakımları alınmalıdır. Nanomalzemeler potansiyel güvenlik tehlikesi ve sağlık etkileri oluşturabilecek. Solunum yolu ve deri temas kaçınılmalıdır. Otoklav reaktörleri ile duman hood ve katalizör performans değerlendirme katalizör sentez gerçekleştirme gibi güvenlik önlemi uygulanmalıdır. Kişisel koruyucu donanım takılmalıdır.
1. Ni0,97Nb0.03O Nb:(Ni+Nb) molar oranları 0.03 olduğu katalizörler hazırlanması
<ol><li>Niyobyum (V) oksalat hidrat 0.161 g nikel nitrat 100 ml deiyonize suyla karıştırın bar ile donatılmış bir 250 mL üç yakalı yuvarlak alt şişesi 2.821 g ile birleştirir.</li>
	<li>50 mil ve 70 ° C çözüm Isıtma manyetik karıştırıcı kullanarak çökelti kaybolması kadar bileşikleri çözülmeye karıştırın.</li>
	<li>Sıcaklığı 80 ° C 2 ° C/dk hızında için hızla artırmak.</li>
	<li>Ni/Nb çözüm pH 9.0 ulaşıncaya kadar karışık bir temel çözüm [sulu amonyum hidroksit (50 mL, 1,0 M) ve sodyum hidroksit (50 mL, 0.2 M)] dropwise reaksiyon karışım içine ekleyin.</li>
	<li>Reaksiyon karışımı karıştırarak, sıcaklığı 120 ° c 2 ° C/dk artırmak.</li>
	<li>Reaksiyon karışımı gecede 50 devirde 120 ° C'de çözüm yeşil rengini tam ortadan kaybolması kadar ilave edin.</li>
	<li>İndüktif eşleşmiş plazma optik emisyon spektrometresi (ICP-OES) çözümlemesi için kalan Ni2 + ve çözüm Nb5 + iyonu konsantrasyonu değerlendirmek ve kalan nikel tam yağış emin olmak belgili tanımlık eriyik nitrat.</li>
	<li>Katı Büchner şişesi kullanarak filtreleme tarafından toplamak. Katı art arda kalan Na+ katyon kaldırmak için 20 dakika içinde 2 lt deiyonize su ekleyerek yıkayın.</li>
	<li>Düz bir saati cam toplamak. 110 ° c kuru fırında 12 h için katı kuru.</li>
	<li>450 ° c 5 h tüp ocağı için sentetik hava (20 mL/dk O2 ve 80 mL/dk N2) halinde katı Isıtma tarafından calcine. Kullanım yüksek sıcaklıkta tepki önce hatası için tüm Züccaciye Mağazaları kontrol edin.</li>
	<li>Calcination sonra 1 g Ni0,97Nb0.03O katalizör edinin. Hood nanocrystal reaksiyon potansiyel güvenlik tehlikesi ve Nanomalzemeler sağlığa etkileri nedeniyle gerçekleştirmek için duman ve uygun koruyucu ekipman koruyucu gözlük, eldiven, önlük gibi kullanın.</li>
</ol>2. Ni0,92Nb0,08O Nb:(Ni+Nb) molar oranları için 0,08 olduğu katalizörler hazırlanması
<ol><li>Bu yordamı 1 ilk iki adımı dışında benzer:<ol>
<li>Niyobyum (V) oksalat hidrat 100 ml deiyonize su 0.43 g geçiyoruz.</li>
		<li>Ayrı ayrı, nikel nitrat 100 ml deiyonize su 2.675 g geçiyoruz.</li>
	</ol>
</li>
</ol>3. Ni0,85Nb0,15O Nb:(Ni+Nb) molar oranları için 0,15 olduğu katalizörler hazırlanması
<ol><li>Yordam 1 ilk iki adımı dışında benzer:<ol>
<li>Niyobyum (V) oksalat hidrat 100 ml deiyonize su 0,807 g geçiyoruz.</li>
		<li>Ayrı ayrı, nikel nitrat 100 ml deiyonize su 2.472 g geçiyoruz.</li>
	</ol>
</li>
</ol>4. Ni0,80Nb0,20O Nb:(Ni+Nb) molar oranı 0,20 için olduğu katalizörler hazırlanması
<ol><li>Yordam 1 ilk iki adımı dışında benzer:<ol>
<li>Niyobyum (V) oksalat hidrat 100 ml deiyonize su 1.076 g geçiyoruz.</li>
		<li>Ayrı ayrı, nikel nitrat 100 ml deiyonize su 2.326 g geçiyoruz.</li>
	</ol>
</li>
</ol>5. kimyasal yağış yöntemini kullanarak Nb2O5 hazırlanması
<ol><li>Niobic asit (Nb2O5·nH2O) O5 parçacıklar saf Nb2' yi edinmek için 450 ° c 5 h için sentetik havada calcine. Not: burada Nb2O5·nH2O Amorphous, Nb2O5 kristal x-ışını toz kırınım (XRD) analizi ile reaksiyon tamamlanması onaylayın. Analizine göre calcination 450 ° c 5 h için tepki tamamlamak için yeterliydi.</li>
</ol>6. β-O-4 lignin modeli bileşim, 2-(2-methoxyphenoxy)-1-phenylethan-1-one sentezi
<ol><li>Bromoacetophenone (9.0 g, 45 mmol) ve 2-methoxyphenol (6,6 g, 53 mmol) dimethylformamide (DMF) 500 mL konik şişesi bir manyetik karıştırıcı ile 200 ml geçiyoruz. Uygun koruyucu ekipman ve duman hood aşındırıcı ve kanserojen kimyasallar ve Kimyasalları kullanarak tepki gerçekleştirmek için kullanın.</li>
	<li>Potasyum hidroksit (3.0 g, 53 mmol) Yukarıdaki DMF çözüm mix ve karışımı bir gecede manyetik karıştırıcı kullanarak oda sıcaklığında 50 rpm'de ilave edin.</li>
	<li>Karışım çözüm H2O 200 mL ve 600 mL Dietil eter ile ürün ayıklamak (1:3, v/v) ayırma huni kullanarak. Çözüm üst Dietil eter tabakası elde edilir.</li>
	<li>Dietil eter çözüm nem absorbe MgSO4 (10 g) ekleyin. Dietil eter çözüm filtre kağıdı ve huni kullanarak elde etmek için MgSO4 filtre.</li>
	<li>Dietil eter çözüm 0,08 MPa rotary Evaporatör kullanarak düşük basınç altında kaldırıldıktan sonra kalıntı 5 ml etanol geçiyoruz.</li>
	<li>Ürün bir 10 mL ölçek Li2 için etanol solvent yavaş yavaş buharlaşır. Sarı toz olarak (11,5 g) ürün elde etmek ve ürün verimi % 90'ı bromoacetophenone üzerinde dayalı olduğunu. 1H NMR analizi, 1H NMR (DMSO): δ 3,78 (s, 3 H, ve3), 5,54 (s, 2 H CH2), 6,82-8.01 (m, 9 H, aromatik) ppm. 17
</li>
</ol>7. Hydrodeoxygenation aromatik eter Lignin kaynaklı
Not: Seçilen lignin elde edilen aromatik eter ANISOL bu deneyde ve Ni0,92Nb0,08O. kullanımı uygun koruyucu ekipman ve duman hood kanserojen reaktifler kullanarak tepki gerçekleştirmek için katalizördür.
<ol><li>50 mL paslanmaz çelik otoklav reaktör bir ısıtıcı ve bir manyetik karıştırıcı ile donatmak.</li>
	<li>Ni0,92400 ° c 2 h H2 atmosfer basınçlı kap reaktörde 2 adımda elde edilen Nb0,08O katalizör (1 g) azaltmak ve katalizör Argon (50 mL/dk) altında bir gecede passivate.</li>
	<li>ANISOL (1.1712 g, 8 wt %) içine n-decane (20 mL) kantitatif Gaz Kromatografi (GC) analiz bir iç standart olarak n-dodecane (0.2928 g, 2 wt %) kullanımı ile çözülür.</li>
	<li>Azaltılmış katalizörler (0,1 g) hızla uzun çekim hızı ile hava (< 5 dakika) önlemek için otoklav reaktör içine tanıtmak.</li>
	<li>Otoklav reaktör mühür, H2 ile art arda (3 kez, 3 MPa basınç) hava ve atmosfer basıncı tepki karisimin ortadan kaldırmak için temizle.</li>
	<li>Karıştırma hızı 700 rpm ayarlayın.</li>
	<li>2 ° C/dk 160-210 ° c sıcaklığa istenen Isıtma sonra 3 MPa otoklav reaktöre basınç ve sıfır saat noktasını ayarlayın (t = 0). Not: 160-210 ° C sıcaklık aralığı bu raporda uygundur.</li>
	<li>Daha sonra Oda sıcaklığı 10 ° C/dk karışıma hemen serin ve deoxygenated ürünleri Gaz Kromatografi Kütle seçici bulmak ile kullanarak çözümleyebilirsiniz. 17
</li>
	<li>Lignin modeli göre aşağıdaki denklemi bileşik dönüşüm belirleyin: <img alt="Equation 1" src="/files/ftp_upload/56987/56987eq1.jpg">
</li>
	<li>Ürün selectivity aşağıdaki denklemi göre belirler: <img alt="Equation 2" src="/files/ftp_upload/56987/56987eq2.jpg">
</li>
</ol>

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Res. 18 (5), 1-12 (2016).</li><li>Wang, K., Yang, L., Zhao, W., Cao, L., Sun, Z., Zhang, F. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=A+facile+synthesis+of+copper+nanoparticles+supported+on+an+ordered+mesoporous+polymer+as+an+efficient+and+stable+catalyst+for+solvent-free+sonogashira+coupling+Reactions.">A facile synthesis of copper nanoparticles supported on an ordered mesoporous polymer as an efficient and stable catalyst for solvent-free sonogashira coupling Reactions.</a> Green Chem. 19, 1949-1957 (2017).</li><li>Song, Y., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=High-Selectivity+Electrochemical+Conversion+of+CO2+to+Ethanol+using+a+Copper+Nanoparticle/N-Doped+Graphene+Electrode.">High-Selectivity Electrochemical Conversion of CO2 to Ethanol using a Copper Nanoparticle/N-Doped Graphene Electrode.</a> Chemistry Select. 1, 6055-6061 (2016).</li></ol>

İfşa etmek yok.

Nikel-katkılı yığın niyobyum oksit nano tanecikleri hazırlamak için yaygın yöntemlerden birini döner buharlaşma yöntemidir. 9 çeşitli basınç ve sıcaklık koşulları döner buharlaşma, Ni-Nb-O parçacıklar ticaret yağış ile solvent yavaş kaldırma işlemi sırasında istihdam ederek. Döner buharlaşma yöntemi aksine bu çalışmada bildirilen kimyasal yağış yöntemi bu gerekmez gibi solventler kaldırılması nano tanecikleri hazırlamak için artan ilgi aldı. Nanocata...

Nanokompozitlerin hazırlanması çok önemli uygulama nedeniyle artan ilgi çeşitli alanına aldı. Ni-Nb-O karışık oksit nano tanecikleri hazırlamak için gibi kuru karıştırma yöntemi,71,2,3,4,5,6 farklı yöntemler geliştirilmiştir, 8 buharlaşma yöntemi,9,10,11,12,13 sol jel yöntemi,14 termal ayrıştırma yöntemi,15 ve Auto-yanma. 16 bir tipik buharlaşma yöntem9' da metal öncüleri, uygun miktarda içeren sulu çözümler nikel nitrat hekzahidrat ve amonyum niyobyum oksalat ısıtmalı 70 ° C'de Solvent ve diğer kurutma ve calcination kaldırıldıktan sonra karışık oksit elde edildi. Bu oksit katalizörler sergi mükemmel katalitik aktivitesi ve niyobyum katyonlar NiO kafes içinde birleşme tarafından indüklenen elektronik ve yapısal düzenlenmesi ile ilgili etan oksidatif dehydrogenation (ODH) doğru seçicilik . 11 Nb ekleme etan12oksidasyon reaksiyonları için sorumludur electrophilic oksijen türleri büyük ölçüde azaltır. Sonuç olarak, bu yöntemin uzantıları karışık Ni-beni-O oksitler, farklı türde hazırlanması yapılmıştır nerede bana Li, Mg, Al, Ga, Ti ve Ta =. 13 bu metal dopants varyasyon NiO unselective ve electrophilic oksijen radikalleri alter, böylece sistematik ODH etkinlik ve seçicilik etan doğru ayarlamak bulunur. Ancak, genellikle yüzey bu oksitler nispeten alanıdır küçük (< 100 m2/g), genişletilmiş aşamasında segregasyon ve büyük Nb2O5 crystallites, oluşumu nedeniyle ve böylece onların kullandığı diğer katalitik engel uygulamaları.
Karışık oksit katalizörler hazırlamak için başka bir sık kullanılan yöntem yöntemi, katı hal taşlama yöntemi olarak da bilinir, karıştırma kurudur. Katalitik malzeme solvent içermeyen bir şekilde elde edilen, bu yöntem karışık oksit hazırlanması için umut verici bir yeşil ve sürdürülebilir alternatif sağlar. Bu yöntemle elde edilen en yüksek yüzey alanı 172 m2/g Ni80Nb20 250 ° c calcination sıcaklıkta olduğunu 8 Reaktanları iyi atom ölçeğinde karışık değil gibi Ancak, katı hal bu yöntem güvenilir değildir. Bu nedenle, kimyasal homojenliği ve belirli parçacık boyutu dağıtım ve Morfoloji daha iyi kontrol için Ni-Nb-O hazırlamak için uygun diğer yöntemleri oksit nano tanecikleri hala aranır karışık. 7
Nano tanecikleri gelişmesinde çeşitli stratejileri arasında kimyasal yağış metal iyonları tam yağış sağlar beri nanocatalysts geliştirmek için umut verici yöntemlerden birini hizmet vermektedir. Ayrıca, daha yüksek yüzey alanlarda nano tanecikleri yaygın olarak bu yöntem kullanılarak hazırlanır. Ni-Nb-O nano tanecikleri katalitik özelliklerini geliştirmek için biz burada Ni-Nb-O karışık oksit katalizörler yüksek yüzey alanı ile bir dizi sentezi için protokol kimyasal yağış yöntemi tarafından Raporu. Nb:Ni molar oranı lignin kaynaklı Organik bileşiklerin hydrodeoxygenation doğru oksitler katalitik aktivitesini belirlemede önemli bir faktör olduğunu gösterdi. 0.087 yukarıda yüksek Nb:Ni oranı ile etkin olmayan NiNb2O6 tür kuruldu. Ni0,92Nb0,08en büyük yüzey alanı (173 m2/g) vardı, O kat benzeri nanosheets yapıları sergiler ve en iyi aktivite ve seçicilik doğru ANISOL Siklokekzan için hydrodeoxygenation gösterdi.

<table><tbody><tr><td>Niobium(V) oxalate hydrate, 98%</td><td>Alfa</td><td>L04481902</td><td></td></tr><tr><td>Nickel nitrate hexahydrate, 99%</td><td>Aladdin</td><td>N108891</td><td></td></tr><tr><td>Sodium hydroxide, 98%</td><td>Aladdin</td><td>S111501</td><td></td></tr><tr><td>Ammonium hydroxide, 23-25%</td><td>Aladdin</td><td>A112077</td><td></td></tr><tr><td>Anisole, 99%</td><td>Sinopharm</td><td>81001728</td><td></td></tr><tr><td>Diphenyl ether, 98%</td><td>Aladdin</td><td>D110644</td><td></td></tr><tr><td>Phenol, 98%</td><td>Sinopharm</td><td>100153008</td><td></td></tr><tr><td>2-Methoxyphenol, 98%</td><td>Sinopharm</td><td>30114526</td><td></td></tr><tr><td>Vanillin, 99.5%</td><td>Sinopharm</td><td>69024316</td><td></td></tr><tr><td>Potassium hydroxide, AR</td><td>Aladdin</td><td>P112284</td><td></td></tr><tr><td>N,N-Dimethylformamide, 99.5%</td><td>Sinopharm</td><td>40016462</td><td></td></tr><tr><td>2-Bromoacetophenone,98%</td><td>Aladdin</td><td>B103328</td><td></td></tr><tr><td>Diethyl ether,99.5%</td><td>Sinopharm</td><td>10009318</td><td></td></tr><tr><td>Decane,98%</td><td>Aladdin</td><td>D105231</td><td></td></tr><tr><td>Dodecane,99%</td><td>Aladdin</td><td>D119697</td><td></td></tr><tr><td>Niobic acid</td><td>CBMM</td><td>1313968</td><td></td></tr><tr><td>Heating and Drying Oven</td><td></td><td></td><td>DHG Series (shanghai jinghong laboratory instrument co. ltd)</td></tr><tr><td>Autoclave Reactor</td><td></td><td></td><td>CJF-0.05&amp;mdash;0.1L (Dalian Tongda Equipment Technology Development Co., Ltd)</td></tr><tr><td>Tube&amp;nbsp;furnace</td><td></td><td></td><td>SK2-1-10/12 (Luoyang Huaxulier Electric Stove Co., Ltd)</td></tr><tr><td>Heating magnetic stirrer</td><td></td><td></td><td>DF-101 (Yu Hua Instrument Co. Ltd.)</td></tr><tr><td>Rotary evaporator</td><td></td><td></td><td>RE-3000A (Shanghai Yarong Biochemical Instrument Factory)</td></tr><tr><td>Synthetic air</td><td></td><td></td><td></td></tr><tr><td>Hydrogen gas</td><td></td><td></td><td></td></tr><tr><td>Argon gas</td><td></td><td></td><td></td></tr></tbody></table>

chemical precipitation method for the synthesis of nb2o5 modified bulk nickel catalysts with high specific surface area

Biz bir yöntemi NixNb1-xO katalizörler sünger benzeri ve kat benzeri taşınımı ile sentezi için göstermek. Nb:Ni oranı, NixNb1-xO nano tanecikleri farklı atom besteleri ile bir dizi değişen tarafından (x = 0,03 0,08, 0,15 ve 0,20) kimyasal yağış tarafından hazırlanmıştır. Bu NixNb1-xO katalizörler x-ışını kırınım, x-ışını photoelectron spektroskopisi ve tarama elektron mikroskobu ile karakterizedir. Ni0,97Nb0.03O sünger benzeri ve kat benzeri görünümünü ve Ni0,92Nb0,08O NiO yüzey ve toplu ile karşılaştırıldığında bu NixNb1-xO katalizörler büyük yüzey alanı çalışmada ortaya NiO. 173 m2/g maksimum yüzey alanı Ni0,92Nb0,08O katalizörler için elde edilebilir. Buna ek olarak, katalitik hydroconversion sentezlenmiş Ni0,92Nb0,08O katalizörler kullanarak lignin türevi bileşiklerin araştırdık.

X-ışını kırınım (XRD) desenleri (Resim 1 ve Şekil 2), bahis yüzey alanlarını, sıcaklık programlanmış azaltma ile hidrojen hidrojen (H2- TPR), elektron mikroskobu (SEM) bir enerji dağıtıcı x-ışını (EDX ile donatılmış tarama ) Çözümleyicisi, x-ışını photoelectron spektroskopisi (XPS) toplanan nano tanecikleri için NiO, Ni-Nb-O ve Nb2O5 oksitler17</...

Watch this Scientific Journal Video about Chemical Precipitation Method for the Synthesis of Nb2O5 Modified Bulk Nickel Catalysts with High Specific Surface Area at JoVE.com

Chemical Precipitation Method for the Synthesis of Nb2O5 Modified Bulk Nickel Catalysts with High Specific Surface Area

Sünger benzeri ve kat benzeri Ni1-xNbxO nano tanecikleri kimyasal yağış tarafından sentezi için bir protokol sunulmuştur.

Nb2O5 sentezi için kimyasal yağış yöntemi toplu nikel katalizör yüksek belirli yüzey alanı ile modifiye

We demonstrate a method for the synthesis of NixNb1-xO catalysts with sponge-like and fold-like nanostructures. By varying the Nb:Ni ratio, a series of ...

chemical-precipitation-method-for-synthesis-nb2o5-modified-bulk

Research

JoVE Journal

Chemistry

Chemical Precipitation Method for the Synthesis of Nb2O5 Modified Bulk Nickel Catalysts with High Specific Surface Area

11.8K Görüntüleme.  Dalian University of Technology. Sünger benzeri ve kat benzeri Ni1-xNbxO nano tanecikleri kimyasal yağış tarafından sentezi için bir protokol sunulmuştur.

Video: Chemical Precipitation Method for the Synthesis of Nb2O5 Modified Bulk Nickel Catalysts with High Specific Surface Area

Reverse Microemulsion-mediated Synthesis of Monometallic and Bimetallic Early Transition Metal Carbide and Nitride Nanoparticles

A reverse microemulsion is used to encapsulate monometallic or bimetallic early transition metal oxide nanoparticles in microporous silica shells. The silica-encapsulated metal oxide nanoparticles are then carburized in a methane/hydrogen atmosphere at temperatures over 800 &#176;C to form silica-encapsulated early transition metal carbide nanoparticles. During the carburization process, the silica shells prevent the sintering of adjacent carbide nanoparticles while also preventing the deposition of excess surface carbon. Alternatively, the silica-encapsulated metal oxide nanoparticles can be nitridized in an ammonia atmosphere at temperatures over 800 &#176;C to form silica-encapsulated early transition metal nitride nanoparticles. By adjusting the reverse microemulsion parameters, the thickness of the silica shells, and the carburization/nitridation conditions, the transition metal carbide or nitride nanoparticles can be tuned to various sizes, compositions, and crystal phases. After carburization or nitridation, the silica shells are then removed using either a room-temperature aqueous ammonium bifluoride solution or a 0.1 to 0.5 M NaOH solution at 40-60 &#176;C. While the silica shells are dissolving, a high surface area support, such as carbon black, can be added to these solutions to obtain supported early transition metal carbide or nitride nanoparticles. If no high surface area support is added, then the nanoparticles can be stored as a nanodispersion or centrifuged to obtain a nanopowder.

A &#8220;removable ceramic coating method&#8221; is presented in visual format for the synthesis of non-sintered and metal-terminated monometallic and bimetallic early transition metal carbide and nitride nanoparticles with tunable sizes and crystal structures.

Monometalik ve Bimetalik Erken Geçiş Metal Carbide ve Nitrür Nanopartiküller Ters Mikroemülsiyon aracılı sentezi

A reverse microemulsion is used to encapsulate monometallic or bimetallic early transition metal oxide nanoparticles in microporous silica shells. The ...

Kimya

Two-way Valorization of Blast Furnace Slag: Synthesis of Precipitated Calcium Carbonate and Zeolitic Heavy Metal Adsorbent

The aim of this work is to present a zero-waste process for storing CO2 in a stable and benign mineral form while producing zeolitic minerals with sufficient heavy metal adsorption capacity. To this end, blast furnace slag, a residue from iron-making, is utilized as the starting material. Calcium is selectively extracted from the slag by leaching with acetic acid (2 M CH3COOH) as the extraction agent. The filtered leachate is subsequently physico-chemically purified and then carbonated to form precipitated calcium carbonate (PCC) of high purity (&lt;2 wt% non-calcium impurities, according to ICP-MS analysis). Sodium hydroxide is added to neutralize the regenerated acetate. The morphological properties of the resulting calcitic PCC are tuned for its potential application as a filler in papermaking. In parallel, the residual solids from the extraction stage are subjected to hydrothermal conversion in a caustic solution (2 M NaOH) that leads to the predominant formation of a particular zeolitic mineral phase (detected by XRD), namely analcime (NaAlSi2O6&#8729;H2O). Based on its ability to adsorb Ni2+, as reported from batch adsorption experiments and ICP-OES analysis, this product can potentially be used in wastewater treatment or for environmental remediation applications.

A protocol for the parallel production of precipitated calcium carbonate and zeolitic material from blast furnace slag via mineral carbonation and alkaline hydrothermal conversion, respectively, is presented. The performance of the zeolitic material towards nickel adsorption is tested.

Yüksek Fırın Cüruf iki yönlü Valorizasyon: çöktürülmüş Kalsiyum Karbonat ve Zeolitik Ağır Metal Adsorban Sentezi

The aim of this work is to present a zero-waste process for storing CO2 in a stable and benign mineral form while producing zeolitic minerals with ...

Mühendislik

Simple Methods for the Preparation of Non-noble Metal Bulk-electrodes for Electrocatalytic Applications

The rock material pentlandite with the composition Fe4.5Ni4.5S8 was synthesized via high temperature synthesis from the elements. The structure and composition of the material was characterized via powder X-ray diffraction (PXRD), M&#246;ssbauer spectroscopy (MB), scanning electron microscopy (SEM), differential scanning calorimetry (DSC) and energy dispersive X-ray spectroscopy (EDX). Two preparation methods of pentlandite bulk electrodes are presented. In the first approach a piece of synthetic pentlandite rock is directly contacted via a wire ferrule. The second approach utilizes pentlandite pellets, pressed from finely ground powder, which is immobilized in a Teflon casing. Both electrodes, whilst being prepared by an additive-free method, reveal high durability during electrocatalytic conversions in comparison to common drop-coating methods. We herein showcase the striking performance of such electrodes to accomplish the hydrogen evolution reaction (HER) and present a standardized method to evaluate the electrocatalytic performance by electrochemical and gas chromatographic methods. Furthermore, we report stability tests via potentiostatic methods at an overpotential of 0.6 V to explore the material limitations of the electrodes during electrolysis under industrial relevant conditions.

A facile preparation method of electrodes using the bulk material Fe4.5Ni4.5S8 is presented. This method provides an alternative technique to conventional electrode fabrication and describes prerequisites for unconventional electrode materials including a straightforward electrocatalytic testing method.

Elektrokatalitik Uygulamalar İçin Asal Olmayan Metal Dökme Elektrodların Hazırlanması İçin Basit Yöntemler

The rock material pentlandite with the composition Fe4.5Ni4.5S8 was synthesized via high temperature synthesis from the elements. The structure and ...

Synthesis of Platinum-nickel Nanowires and Optimization for Oxygen Reduction Performance

Platinum-nickel (Pt-Ni) nanowires were developed as fuel cell electrocatalysts, and were optimized for the performance and durability in the oxygen reduction reaction. Spontaneous galvanic displacement was used to deposit Pt layers onto Ni nanowire substrates. The synthesis approach produced catalysts with high specific activities and high Pt surface areas. Hydrogen annealing improved Pt and Ni mixing and specific activity. Acid leaching was used to preferentially remove Ni near the nanowire surface, and oxygen annealing was used to stabilize near-surface Ni, improving durability and minimizing Ni dissolution. These protocols detail the optimization of each post-synthesis processing step, including hydrogen annealing to 250 &#176;C, exposure to 0.1 M nitric acid, and oxygen annealing to 175 &#176;C. Through these steps, Pt-Ni nanowires produced increased activities more than an order of magnitude than Pt nanoparticles, while offering significant durability improvements. The presented protocols are based on Pt-Ni systems in the development of fuel cell catalysts. These techniques have also been used for a variety of metal combinations, and can be applied to develop catalysts for a number of electrochemical processes.

&#160; The protocol describes the synthesis and electrochemical testing of platinum-nickel nanowires. Nanowires were synthesized by the galvanic displacement of a nickel nanowire template. Post-synthesis processing, including hydrogen annealing, acid leaching, and oxygen annealing were used to optimize nanowire performance and durability in the oxygen reduction reaction.

Platin-nikel Nanowires ve oksijen azaltma performansı için en iyi duruma getirme sentezi

Platinum-nickel (Pt-Ni) nanowires were developed as fuel cell electrocatalysts, and were optimized for the performance and durability in the oxygen ...

Synthesis and Performance Characterizations of Transition Metal Single Atom Catalyst for Electrochemical CO2 Reduction

This protocol presents both the synthesis method of the Ni single atom catalyst, and the electrochemical testing of its catalytic activity and selectivity in aqueous CO2 reduction. Different from traditional metal nanocrystals, the synthesis of metal single atoms involves a matrix material that can confine those single atoms and prevent them from aggregation. We report an electrospinning and thermal annealing method to prepare Ni single atoms dispersed and coordinated in a graphene shell, as active centers for CO2 reduction to CO. During the synthesis, N dopants play a critical role in generating graphene vacancies to trap Ni atoms. Aberration-corrected scanning transmission electron microscopy and three-dimensional atom probe tomography were employed to identify the single Ni atomic sites in graphene vacancies. Detailed setup of electrochemical CO2 reduction apparatus coupled with an on-line gas chromatography is also demonstrated. Compared to metallic Ni, Ni single atom catalyst exhibit dramatically improved CO2 reduction and suppressed H2 evolution side reaction.

Synthesis and Performance Characterizations of Transition Metal Single Atom Catalyst for Electrochemical CO2 Reduction

Here, we present a protocol for the synthesis and electrochemical testing of transition metal single atoms coordinated in graphene vacancies as active centers for selective carbon dioxide reduction to carbon monoxide in aqueous solutions.

Sentez ve elektrokimyasal CO2 azaltılması için geçiş metalleri tek Atom katalizör performans karakterizasyonu

This protocol presents both the synthesis method of the Ni single atom catalyst, and the electrochemical testing of its catalytic activity and selectivity ...

A Continuous-flow Photocatalytic Reactor for the Precisely Controlled Deposition of Metallic Nanoparticles

In this work, a novel photocatalytic reactor for the pulsed and controlled excitation of the photocatalyst and the precise deposition of metallic nanoparticles is developed. Guidelines for the replication of the reactor and its operation are provided in detail. Three different composite systems (Pt/graphene, Pt/TiO2, and Au/TiO2) with monodisperse and uniformly distributed particles are produced by this reactor, and the photodeposition mechanism, as well as the synthesis optimization strategy, are discussed. The synthesis methods and their technical aspects are described comprehensively. The role of the ultraviolet (UV) dose (in each excitation pulse) on the photodeposition process is investigated and the optimum values for each composite system are provided.

For a continuous and scalable synthesis of noble-metal-based nanocomposites, a novel photocatalytic reactor is developed and its structure, operation principles, and product quality optimization strategies are described.

Metalik nano tanecikleri tam kontrollü birikimi için sürekli akış Fotokatalitik reaktör

In this work, a novel photocatalytic reactor for the pulsed and controlled excitation of the photocatalyst and the precise deposition of metallic ...

Tuning the Acidity of Pt/ CNTs Catalysts for Hydrodeoxygenation of Diphenyl Ether

We herein present a method for the synthesis of HNbWO6, HNbMoO6, HTaWO6 solid acid nanosheet modified Pt/CNTs. By varying the weight of various solid acid nanosheets, a series of Pt/xHMNO6/CNTs with different solid acid compositions (x = 5, 20 wt%; M = Nb, Ta; N = Mo, W) have been prepared by carbon nanotube pretreatment, protonic exchange, solid acid exfoliation, aggregation and finally Pt particles impregnation. The Pt/xHMNO6/CNTs are characterized by X-ray diffraction, scanning electron microscopy, transmission electron microscopy and NH3-temperature programmed desorption. The study revealed that HNbWO6 nanosheets were attached on CNTs, with some edges of the nanosheets being bent in shape. The acid strength of the supported Pt catalysts increases in the following order: Pt/CNTs &#60; Pt/5HNbWO6/CNTs &#60; Pt/20HNbMoO6/CNTs &#60; Pt/20HNbWO6/CNTs &#60; Pt/20HTaWO6/CNTs. In addition, the catalytic hydroconversion of lignin-derived model compound: diphenyl ether using the synthesized Pt/20HNbWO6 catalyst has been investigated.

A protocol for the synthesis of HNbWO6, HNbMoO6, HTaWO6 solid acid nanosheet modified Pt/CNTs is presented.

Difenil Eterhidrodeoksijenasyonu için Pt/ CNTs Katalizörlerinin Asitliğini Değiştirme

We herein present a method for the synthesis of HNbWO6, HNbMoO6, HTaWO6 solid acid nanosheet modified Pt/CNTs. By varying the weight of various solid acid ...

Preparation of Silver-Palladium Alloyed Nanoparticles for Plasmonic Catalysis under Visible-Light Illumination

Localized surface plasmon resonance (LSPR) in plasmonic nanoparticles (NPs) can accelerate and control the selectivity of a variety of molecular transformations. This opens possibilities for the use of visible or near-IR light as a sustainable input to drive and control reactions when plasmonic nanoparticles supporting LSPR excitation in these ranges are employed as catalysts. Unfortunately, this is not the case for several catalytic metals such as palladium (Pd). One strategy to overcome this limitation is to employ bimetallic NPs containing plasmonic and catalytic metals. In this case, the LSPR excitation in the plasmonic metal can contribute to accelerate and control transformations driven by the catalytic component. The method reported herein focuses on the synthesis of bimetallic silver-palladium (Ag-Pd) NPs supported on ZrO2 (Ag-Pd/ZrO2) that acts as a plasmonic-catalytic system. The NPs were prepared by co-impregnation of corresponding metal precursors on the ZrO2 support followed by simultaneous reduction leading to the formation of bimetallic NPs directly on the ZrO2 support. The Ag-Pd/ZrO2 NPs were then used as plasmonic catalysts for the reduction of nitrobenzene under 425 nm illumination by LED lamps. Using gas chromatography (GC), the conversion and selectivity of the reduction reaction under the dark and light irradiation conditions can be monitored, demonstrating the enhanced catalytic performance and control over selectivity under LSPR excitation after alloying non-plasmonic Pd with plasmonic metal Ag. This technique can be adapted to a wide range of molecular transformations and NPs compositions, making it useful for the characterization of the plasmonic catalytic activity of different types of catalysis in terms of conversion and selectivity.

Presented here is a protocol for the synthesis of silver-palladium (Ag-Pd) alloy nanoparticles (NPs) supported on ZrO2 (Ag-Pd/ZrO2). This system allows for harvesting energy from visible light irradiation to accelerate and control molecular transformations. This is illustrated by nitrobenzene reduction under light irradiation catalyzed by Ag-Pd/ZrO2 NPs.

Görünür-Işık Aydınlatması Altında Plazmonik Kataliz için Gümüş-Paladyum Alaşımlı Nanopartiküllerin Hazırlanması

Localized surface plasmon resonance (LSPR) in plasmonic nanoparticles (NPs) can accelerate and control the selectivity of a variety of molecular ...

Synthesis of Metal Nanoparticles Supported on Carbon Nanotube with Doped Co and N Atoms and its Catalytic Applications in Hydrogen Production

A method for facile synthesis of nanostructured catalysts supported on carbon nanotubes with atomically dispersed cobalt and nitrogen dopant is presented herein. The novel strategy is based on a facile one-pot pyrolysis treatment of cobalt (II) acetylacetonate and nitrogen-rich organic precursors under Ar atmosphere at 800 &#176;C, resulting in the formation of Co- and N- co-doped carbon nanotube with earthworm-like morphology. The obtained catalyst was found to have a high density of defect sites, as confirmed by Raman spectroscopy. Here, cobalt (II) nanoparticles were stabilized on the atomically dispersed cobalt- and nitrogen-doped carbon nanotubes. The catalyst was confirmed to be effective in the catalytic hydrolysis of ammonia borane, in which the turnover frequency was 5.87 mol H2&#183;molCo-1&#183;min-1, and the specific hydrogen generation rate was determined to be 2447 mL H2&#183;gCo-1&#183;min-1. A synergistic function between the Co nanoparticle and the doped carbon nanotubes was proposed for the first time in the catalytic hydrolysis of ammonia borane reaction under a mild condition. The resulting hydrogen production with its high energy density and minimal refueling time could be suitable for future development as energy sources for mobile and stationary applications such as road trucks and forklifts in transport and logistics.

Here, we present a protocol to synthesize Co nanoparticles supported on carbon nanotubes with Co- and N- dopants for hydrogen productions.

Karbon Nanotüp Üzerinde Katkılı Co ve N Atomları ile Desteklenen Metal Nanopartiküllerin Sentezi ve Hidrojen Üretiminde Katalitik Uygulamaları

A method for facile synthesis of nanostructured catalysts supported on carbon nanotubes with atomically dispersed cobalt and nitrogen dopant is presented ...

Nikel Hidroksit Nanotabakaların Mikrodalga Sentezi ve Karakterizasyonu

Effect of Microwave Synthesis Conditions on the Structure of Nickel Hydroxide Nanosheets

A protocol for rapid, microwave-assisted hydrothermal synthesis of nickel hydroxide nanosheets under mildly acidic conditions is presented, and the effect of reaction temperature and time on the material&#39;s structure is examined. All reaction conditions studied result in aggregates of layered &#945;-Ni(OH)2 nanosheets. The reaction temperature and time strongly influence the structure of the material and product yield. Synthesizing &#945;-Ni(OH)2 at higher temperatures increases the reaction yield, lowers the interlayer spacing, increases crystalline domain size, shifts the frequencies of interlayer anion vibrational modes, and lowers the pore diameter. Longer reaction times increase reaction yields and result in similar crystalline domain sizes. Monitoring the reaction pressure in situ shows that higher pressures are obtained at higher reaction temperatures. This microwave-assisted synthesis route provides a rapid, high-throughput, scalable process that can be applied to the synthesis and production of a variety of transition metal hydroxides used for numerous energy storage, catalysis, sensor, and other applications.

Yazar Spotlight: Nikel Hidroksit Nanotabakalarının Hızlı, Mikrodalga Destekli Hidrotermal Sentezi 

Nickel hydroxide nanosheets are synthesized by a microwave-assisted hydrothermal reaction. This protocol demonstrates that the reaction temperature and time used for microwave synthesis affects the reaction yield, crystal structure, and local coordination environment.

Mikrodalga Sentez Koşullarının Nikel Hidroksit Nano Levhaların Yapısına Etkisi

A protocol for rapid, microwave-assisted hydrothermal synthesis of nickel hydroxide nanosheets under mildly acidic conditions is presented, and the effect ...

Nb₂O₅ sentezi için kimyasal yağış yöntemi toplu nikel katalizör yüksek belirli yüzey alanı ile modifiye

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