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"Sintesis karbon mesopori secara soft template dan hard template dari berbagai prekursor karbon; phloroglucinol, glukosa, dan hidrolisat tandan kosong kelapa sawit (TKKS) telah dilakukan. Pluronic F127 dan silica gel digunakan sebagai cetakan pada sintesis karbon mesopori soft template dan hard template, secara berturut-turut. Material karbon mesopori kemudian diimpregnasi dengan logam Ni dan direduksi menggunakan gas H2 sehingga membentuk Ni/mesoporous carbon (Ni/MC). Karakterisasi material dengan FTIR menunjukkan bahwa gugus organik pada soft templated mesoporous carbon (ST MC) menghilang setelah proses karbonisasi dan pada hard templated mesoporous carbon (HT MC) setelah proses desilikasi, mengindikasikan bahwa proses tersebut efektif dalam penghilangan template yang digunakan. Berdasarkan analisis SEM, material karbon memiliki morfologi seperti serpihan dengan tambahan sebaran butiran halus setelah impregnasi. Berdasarkan hasil analisis XRD untuk ST MC dan HT MC, terdapat difraksi khas karbon grafit pada 2θ 25⁰ dan 44⁰. Kemudian terdapat tambahan difraksi setelah impregnasi pada 2θ 45⁰ dan 52⁰ yang bersesuaian dengan Ni(0), mengindikasikan bahwa impregnasi berhasil dilakukan. Analisa luas permukaan menunjukkan bahwa material karbon memiliki luas permukaan dan distribusi pori yang bervariasi. Material selanjutnya digunakan sebagai katalis dalam reaksi karboksilasi fenilasetilena dengan karbon dioksida. Analsis HPLC menunjukkan hasil terbaik pada suhu reaksi 85⁰C dan waktu reaksi 8 jam dengan menggunakan katalis HT Ni/MC phloroglucinol dan garam MgCl2. Yield pembentukan produk asam fenil propiolat pada kondisi tersebut adalah 2,2 %.

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Synthesis of soft templated and hard templated mesoporous carbon from various carbon precursors; phloroglucinol, glucose, and empty palm oil shell hidrolisate, has been conducted successfully. Pluronic F127 and silica gel were used as template in the sythesis of soft and hard templated mesoporous carbon, respectively. The materials were then impregnated with Ni and reduced under H2 flow to form Ni/Mesoporous Carbon (Ni/MC). Characterization with FTIR shows that the organic groups in Soft Templated Mesoporous Carbon (ST MC) disappear after the carbonization process and in Hard Templated Mesoporous Carbon (HT MC) after the desilication process, indicating that the process is effective in template removal. Based on the SEM analysis, carbon materials have flakes-like morphology with the addition of fine grain spreads after impregnation. Based on the results of XRD analysis for ST MC and HT MC, there are a typical graphite carbon diffractions on 2θ of 25 and 44 ⁰. There are also additional diffraction peaks at 2θ of 45 and 52⁰ after impregnation which correspond with Ni(0), indicating that the Ni impregnation was successfully performed. The analysis of the surface area indicates that carbon materials have various surface area and pore distribution. The materials are subsequently used as a catalyst in the carboxylation reaction of phenylacetylene with carbon dioxide. HPLC analysis shows the best resultis obtained at reaction temperature of 85 ⁰ _C and time of 8 hour using MgCl2 salt and HT Ni/MC phloroglucinol catalyst. Yield of phenyl propiolic acid formation as product of carboxylation obtained on optimum condition is 2,2%."

"ABSTRAKKarbon dioksida (CO2) merupakan senyawa yang potensial digunakan sebagai sumber karbon dalam sintesis fine chemicals karena keberadaannya melimpah di alam, bersifat non toksik, ekonomis, dan termasuk ke dalam sumber yang dapat diperbaharui. Namun pemanfaatan CO2 secara luas masih terkendala karena sifatnya yang inert dan stabil. Oleh karena itu, keberadaan katalis sangat diperlukan dalam proses konversi CO2. Penelitian ini bertujuan untuk mensintesis Cu terimpregnasi pada karbon mesopori sebagai katalis karboksilasi fenilasetilena dengan CO2 menjadi asam karboksilat. Pembuatan karbon mesopori dilakukan dengan metode soft template menggunakan Pluronik F-127 sebagai pembentuk pori, formaldehida dan floroglusinol sebagai sumber karbon, dan HCl sebagai katalis asam. Material Cu/MC yang dihasilkan dikarakterisasi dengan FTIR, XRD, SAA, dan SEM-EDX. Analisis BET terhadap karbon mesopori menunjukkan bahwa material tersebut memiliki luas permukaan sebesar 405,8 m2/g dengan rata-rata pori sebesar 7,2 nm. Hasil analisa dengan XRD memperlihatkan puncak pada 2θ 36,62°; 43,47°; 50,63°; dan 74,19° yang mengindikasikan bahwa Cu telah berhasil terimpregnasi yang mewakili spesi Cu(0) dan Cu(I). Reaksi karboksilasi fenilasetilena dengan CO2 dilakukan dengan variasi suhu (25°C; 50°C; dan 75°C), variasi jumlah katalis (28,6; 57,2; dan 85,8 mg) dan variasi basa (Cs2CO3; K2CO3; dan Na2CO3). Hasil reaksi dianalisa dengan HPLC dan memperlihatkan %konversi terbaik terjadi pada suhu 75°C yaitu 41,32% dengan menggunakan Cs2CO3 sebagai basa, dan produk yang terbentuk diidentifikasi dengan FTIR dan LC-MS.

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ABSTRACTCarbon dioxide (CO2) is a compound that has the potential to be used as carbon source in the synthesis of fine chemicals because it is abundant in nature, non-toxic, inexpensive, and is included as a renewable source. However, utilization of CO2 is stillconstrained due to its inert and stable nature. Therefore, the presence of a catalyst is needed in CO2 conversion. This study aims to synthesize impregnated Cu on mesoporous carbon (Cu/MC) as a catalyst for phenylacetylene carboxylation reaction with CO2 into carboxylic acid. The synthesis of mesoporous carbon was performed via soft template method using Pluronic F-127 as a pore forming agen, formaldehyde and phloroglucinol as carbon sources, and HCl as an acid catalyst. The Cu/MC material produced was characterized by FTIR, SAA, XRD, and SEM-EDX. BET surface area analysis of mesoporous carbon showed that the material has a surface area of 405.8 m2/g with an average pore diameter of 7,2 nm. XRD pattern of Cu/MC showed some sharp peaks at 2θ of 36.62°; 43.47°; 50.63°; and 74.19° which indicates that Cu has been successfully impregnated in the form of Cu(0) and Cu(I). Phenylacetylene carboxylation reaction with CO2 was carried out by varying reaction temperatures (25, 50, and 75 °C), the amount of catalyst (28.6, 57.2, and 85.8 mg) and the type of base (Cs2CO3, K2CO3, and Na2CO3). The reaction mixtures were analyzed by HPLC and showed that highest phenylacetylene conversion of 41% was obtained for the reaction at 75°C using Cs2CO3 as a base. The product was further identified using FTIR and LCMS."

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Pengembangan metodologi sintetis yang memanfaatkan karbon dioksida sebagai sumber karbon C1 sangat diperlukan untuk sintesis bahan kimia yang berguna, mengingat dampak negatif lingkungan dari peningkatan kadar CO₂ di atmosfer. Dalam penelitian ini, telah dilakukan studi reaksi karboksilasi fenilasetilena dengan CO₂ menggunakan katalis kompleks Ni terimobilisasi pada support karbon mesopori. Karbon mesopori telah berhasil disintesis dengan metode soft template menggunakan Pluronik F127 sebagai pembentuk pori, formaldehida dan phloroglucinol sebagai sumber karbon, dan HCl sebagai katalis asam. Material ini dikarakterisasi dengan FTIR, XRD, SEM, dan BET. Modifikasi support dilakukan dengan cara imobilisasi kompleks Ni ke dalam karbon mesopori (kompleks Ni/MC). Katalis kompleks Ni/MC digunakan sebagai katalis dalam reaksi karboksilasi fenilasetilena dengan CO₂. Reaksi dilakukan dalam reaktor dengan kondisi reaksi yang bervariasi, yakni variasi suhu (25^oC, 50^oC, 75^oC), variasi waktu (4 jam, 8 jam, dan 16 jam). Produk reaksi karboksilasi ini kemudian dianalisis dengan menggunakan HPLC untuk menentukan persen konversi. Analisis FTIR Ni(bpy)/MC menunjukan puncak pada panjang gelombang 1385 cm^-1  (C-N stretching). Analisis XRD menunjukan difraksi MC pada 24.67º dan 43.26º dan Ni(bpy)/MC pada 23.53º dan 43.56º. Analisis BET memberi informasi luas permukaan, distribusi pori, dan volume pori sebesar MC sebesar 288.7242 m²/g, 3.6136 nm, dan 0.5766 cc/g, dan Ni(bpy)/MC sebesar 348,9490 m²/g, 3.1157 nm, dan 0.3291cc/g. Analisis SEM-EDX memberi informasi morfologi permukaan MC terimobilisasi kompleks bipiridin dengan persen loading sebesar 3.26%. Analisis adsorpsi menunjukan Ni(bpy)/MC memiliki kemampuan adsorpsi CO₂ yang lebih tinggi dari MC. Konversi terbesar didapat dari Ni(bpy)/MC dengan persen konversi sebesar 94.5911% dan luas area produk sebesar 25.3846 mAU.

 

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The development of a synthetic methodology that utilizes carbon dioxide as a source of C1 carbon is indispensable for the synthesis of useful chemicals, due to the negative effects to environmental by increased levels of CO₂ in the atmosphere. In this research, carboxylation reaction of phenylacetylene with CO₂ has been carried out using nickel immobilized at mesoporous carbon as catalyst support. Mesoporous carbon has been successfully synthesized using soft template method with Pluronik F127 as a pore-forming, formaldehyde and phloroglucinol as carbon source, and HCl as acid catalyst. Material was characterized by FTIR, XRD, SEM, and BET. Modification of support was done by immobilizing nickel complex at mesoporous carbon (Ni complex/MC). Ni complex/MC was then used as a catalyst in carboxylation reaction of phenylacetylene with CO₂. The reactions were carried out in reactor with various conditions, such as temperature (25^oC, 50^oC, 75^oC), and time (4 hours, 8 hours, 16 hours). The result of carboxylation reactions were analyzed by HPLC to determine conversion. FTIR analysis of Ni(bpy)/MC showed a peak at a wavelength of 1385 cm^-1 (C-N stretching). XRD analysis showed MC diffraction at 24.67º and 43.26º and Ni(bpy)/MC at 23.53º and 43.56º. BET analysis gave information about the surface area, pore distribution, and pore volume of MC of 288.7242 m²/g, 3.6136 nm, and 0.5766 cc/g, and Ni(bpy)/MC of 348.9490 m²/g, 3.1157 nm, and 0, 3291 cc/g. SEM-EDX analysis gave information about the surface morphology of the MC is immobilized by the bipyridine complex with loading of 3.26%. Adsorption analysis shows that Ni(bpy)/MC has higher CO₂ adsorption ability than MC. The highest conversion is shown by Ni(bpy)/MC 8h at 25ºC with conversion of 94.5911% and product area of 25.3846 mAU.

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"Carbon dioxide is a renewable C1 resource for synthesis chemicals. CO2 in carboxylation reactions requires catalysts Ni complex for CO2 activation. However, the use of Ni complex homogeneous catalysts in the reaction is still less efficient due to the difficult in separating the product and catalyst. Therefore, it is necessary to heterogenize the Ni complex in solid supporting such as mesoporous carbon. In this research, a carboxylation reaction with CO2 was tested using a Ni catalyst that was functionalized with phenanthroline (phen) ligand impregnated on the solid support of mesoporous carbon. Soft template method has been successfully used in mesoporous carbon synthesis with phloroglucinol and formaldehyde prekursors as a carbon source, Pluronic F127 as a structural directing agent, and HCl as an acid catalyst. Modification of the catalyst was carried out by impregnation of Ni from Ni(NO3)2.6H2O which was then functionalized with phenanthroline (phen) ligands into mesoporous carbon to form Ni-phen/MC catalysts. Mesoporous carbon material (MC) and Ni-phen/MC are characterized by FT-IR, XRD, SEM-EDX, and SAA. The results of SAA characterization showed that the pore diameter of MC was 6.7174 nm and Ni-phen/MC was 5.08 nm which indicate that the material was mesoporous. Ni-phen/MC material was then used as a heterogeneous catalyst in the carboxylation reaction of phenylacetylene with CO2. The reaction were carried out in several variations of conditions, temperature variations (25oC, 50oC and 75oC), time variations (4 hours, 8 hours and 16 hours), variations in catalyst types (MC, Ni-phen and Ni-phen/MC). Based on the results of the reaction, the optimum conditions was obtained at 25oC for 8 hour of reaction time using Ni-phen/MC catalyst. The main product of the carboxylation reaction is identified by the HPLC instrument, while the remaining catalyst that has been used in the reaction was identified using the FT-IR instrument.Carbon dioxide is a renewable C1 resource for synthesis chemicals. CO2 in carboxylation reactions requires catalysts Ni complex for CO2 activation. However, the use of Ni complex homogeneous catalysts in the reaction is still less efficient due to the difficult in separating the product and catalyst. Therefore, it is necessary to heterogenize the Ni complex in solid supporting such as mesoporous carbon. In this research, a carboxylation reaction with CO2 was tested using a Ni catalyst that was functionalized with phenanthroline (phen) ligand impregnated on the solid support of mesoporous carbon. Soft template method has been successfully used in mesoporous carbon synthesis with phloroglucinol and formaldehyde prekursors as a carbon source, Pluronic F127 as a structural directing agent, and HCl as an acid catalyst. Modification of the catalyst was carried out by impregnation of Ni from Ni(NO3)2.6H2O which was then functionalized with phenanthroline (phen) ligands into mesoporous carbon to form Ni-phen/MC catalysts. Mesoporous carbon material (MC) and Ni-phen/MC are characterized by FT-IR, XRD, SEM-EDX, and SAA. The results of SAA characterization showed that the pore diameter of MC was 6.7174 nm and Ni-phen/MC was 5.08 nm which indicate that the material was mesoporous. Ni-phen/MC material was then used as a heterogeneous catalyst in the carboxylation reaction of phenylacetylene with CO2. The reaction were carried out in several variations of conditions, temperature variations (25oC, 50oC and 75oC), time variations (4 hours, 8 hours and 16 hours), variations in catalyst types (MC, Ni-phen and Ni-phen/MC). Based on the results of the reaction, the optimum conditions was obtained at 25oC for 8 hour of reaction time using Ni-phen/MC catalyst. The main product of the carboxylation reaction is identified by the HPLC instrument, while the remaining catalyst that has been used in the reaction was identified using the FT-IR instrument."

"Pemanfaatan bahan bakar fosil, batu bara, minyak, serta gas alam yang kaya akan karbon semakin marak digunakan guna keberlangsungan hidup manusia. Pemanfaatan bahan-bahan tersebut juga turut andil dalam peningkatan konsentrasi CO₂ di atmosfir. Meningkatnya emisi CO₂ menyebabkan turut meningkatnya suhu bumi dan perubahan iklim yang disebabkan oleh ‘efek rumah kaca’. Sehingga, konversi CO₂ menjadi senyawa yang lebih bermanfaat sangatlah diperlukan. Dalam penelitian ini, dilakukan sintesis dan karakterisasi karbon mesopori termodifikasi NiZn sebagai katalis heterogen reaksi karboksilasi asetilena dengan CO₂. Karbon mesopori disintesis dengan metode soft template menggunakan surfaktan pluronik F127 sebagai template organik, serta phloroglucinol sebagai prekursor karbon. Karbon mesopori kemudian dimodifikasi dengan logam nikel dan seng (NiZn/MC) dengan metode deposisi-presipitasi homogen, dilanjutkan dengan reduksi dengan aliran gas H₂ (30 ml per menit) selama 90 menit pada suhu 400 ^oC. Pola difraksi XRD menunjukkan puncak-puncak pada 2q sekitar 31,79^o; 34,54^o; 36,31^o; 44,04^o; 51,51^o; 56,51^o; 62,22^o; dan 75,68^o yang mengindikasikan terdapatnya spesi NiZn dan ZnO. Berdasarkan hasil EDX, material karbon mesopori berhasil dimodifikasi dengan logam nikel dan seng dengan persen loading 11,68%, untuk nikel dan 8,69% untuk logam seng. Katalis NiZn/MC kemudian digunakan sebagai katalis heterogen dalam reaksi karboksilasi asetilena dengan CO₂. Reaksi dilakukan dalam reaktor batch dengan kondisi reaksi yang bervariasi, yakni tekanan 1,5 bar; 2,5 bar; dan 3,5 bar. Asam akrilat, sebagai produk yang diinginkan, tidak terdeteksi pada analisis dengan HPLC. Namun, terdeteksi spesi yang lebih polar pada waktu retensi 3 menit, di mana kondisi optimum terjadi pada tekanan 2,5 bar.

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Utilization of fossil fuel, charcoal, oil, and natural gases, which are carbon-rich materials, is widely used for human sustainability. However, utilization of such materials contributes to higher atmospheric CO₂ concentration. The increase of CO₂ emission leads to higher temperature and climate change ea t ‘green house effect’. Therefore, conversion of CO₂ to value-added chemicals has drawn many attentions. In this research, carboxylation reaction of acetylene and CO₂ has been carried out using mesoporous carbon modified by nickel and zinc metals as heterogeneous catalyst. Mesoporous carbon has been successfully synthesized using soft template method with pluronic F127 as template and phloroglucinol as carbon precursor. Mesoporous carbon was then modified with nickel and zinc (NiZn/MC) using homogeneous deposition precipitation method, followed by reduction for 90 mins at 400 ^oC under a flow of H₂ (30 ml/min). XRD diffraction pattern showed peaks for 2q around 31.79^o, 34.54^o, 36.31^o, 44.04^o, 51.51^o, 56.51^o, 62.22^o, and 75.68^o which indicate the presence of NiZn and ZnO. EDX result revealed that mesoporous carbon material has been successfully modified by nickel and zinc metals, with 11.68% and 8.69% metal loadings for nickel and zinc, respectively. NiZn/MC catalyst was then used for carboxylation reaction of acetylene with CO₂. The reactions were carried out in batch reactor with varied pressure, 1.5 bar, 2.5 bar, and 3.5 bar. Acrylic acid, as the desired product, was not observed in analysis with HPLC. However, more polar species was noticed at retention time of 3 minutes, where optimum pressure was found to ea t 2.5 bar."

"Kenaikan sejumlah besar CO₂ mengakibatkan konsentrasi CO₂ semakin meningkat di atmosfer secara terus-menerus yang menyebabkan terjadinya perubahan iklim. Pengembangan reaksi katalitik terbarukan diperlukan untuk mentransformasi CO₂ menjadi produk yang lebih bermanfaat. Pada penelitian ini, telah dilakukan uji reaksi karboksilasi fenilasetilena dengan CO₂ menggunakan katalis Ni(acac)₂, NiCl₂ dan Ni(DBU)₂ yang terimpregnasi pada penyangga karbon mesopori. Material karbon mesopori, Ni(acac)₂/ MC, NiCl₂/ MC dan Ni(DBU)₂/ MC dikarakterisasi dengan FT-IR, XRD, SAA dan SEM-EDS. Karbon mesopori telah berhasil disintesis menggunakan metode soft template dibuktikan dengan hasil  analisa XRD yang menunjukkan pola difraksi secara khas pada material karbon pada 25,68^o dan 43,26^o dengan indeks Miller (002) dan (100). Proses impregnasi  pada Ni(acac)₂, NiCl₂ dan Ni(DBU)₂  pada penyangga karbon mesopori telah berhasil ditunjukkan dengan analisa FT-IR dimana pada spektrum Ni(acac)₂/ MC, NiCl₂/ MC dan Ni(DBU)₂/ MC menghasilkan spektrum yang sama dengan MC dikarenakan senyawa terimpregnasi telah masuk ke dalam pori sehingga mengakibatkan tidak terdeteksinya gugus fungsi yang ada pada senyawa-senyawa tersebut. Hasil karakterisasi SAA menunjukkan bahwa ketiga katalis heterogen termasuk ke dalam material mesopori. Radius pori yang diperoleh pada ketiga senyawa yaitu  Ni(acac)₂/ MC sebesar 3,288 nm, NiCl₂/ MC sebesar 4,799 nm, dan Ni(DBU)₂/ MC sebesar 4,763 nm. Uji daya adsorpsi dan uji reaksi karboksilasi fenilasetilena dengan CO₂ dengan katalis heterogen Ni(acac)₂/ MC, NiCl₂/ MC dan Ni(DBU)₂/ MC telah dilakukan dan membuktikan bahwa katalis Ni(acac)2/ MC memiliki daya adsorpsi lebih baik dan menghasilkan produk fenil maleat lebih banyak dibanding dengan katalis NiCl₂/ MC dan Ni(DBU)₂/ MC.

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The continuous increase of CO₂ concentrations in the atmosphere for decades has influenced the global climate change. The development of renewable catalytic reactions is needed to transform CO₂ into more useful products. In this research, phenylacetylene carboxylation reaction with CO₂ was tested using catalysts Ni(acac)₂, NiCl₂ and Ni(DBU)₂ which were impregnated on the mesoporous carbon support. Mesoporous carbon materials, Ni(acac)₂ / MC, NiCl₂ / MC , and Ni(DBU)₂ / MC are characterized by FT-IR, XRD, SAA and SEM-EDS. Mesoporous carbon was successfully synthesized using soft template method which showed typical diffraction patterns of carbon materials which were 25.68^o and 43.26^o with the Miller index of (002) and (100), respectively. The impregnation process in Ni(acac)₂, NiCl₂ and Ni(DBU)₂ in mesoporous carbon support has been successfully proven by FT-IR analysis in which Ni(acac)₂ / MC, NiCl₂ / MC, and Ni(DBU)₂ / MC have similiar IR-spectrum to MC IR-spectrum because the compounds have been substituted into the pore so that no functional groups were detected in the samples. The results of the SAA characterization showed that the three heterogeneous catalysts belong to compounds that have meso-sized pores. The pore radius obtained in the three materials were 3,288 nm for Ni(acac)₂ / MC, 4,799 nm for NiCl₂ / MC, and 4,763 nm for Ni(DBU)₂ / MC. Adsorption test and phenylacetylene carboxylation reaction test with CO₂ with heterogeneous catalyst Ni(acac)₂ / MC, NiCl₂ / MC and Ni(DBU)₂ / MC have been carried out and proved the Ni(acac)₂ / MC catalyst had better adsorption performance and produced more phenyl maleate product compared to NiCl₂ / MC and Ni(DBU)₂ / MC catalysts."

"Material karbon mesopori berhasil disintesis melalui metode soft template dengan menggunakan formaldehida dan floroglusinol sebagai sumber karbon, pluronic F127 sebagai SDA, dan asam klorida sebagai katalis. Dilakukan pengujian awal terhadap karbon mesopori hasil sintesis sebagai adsorben zat warna Acid Red 119. Proses sintesis karbon mesopori melibatkan reaksi polimerisasi formaldehida dengan floroglusinol pada soft template F127 dalam pelarut etanol:air. Analisis termal gravimetri menunjukkan kestabilan termal karbon mesopori hingga mencapai suhu 900 0C. Karakterisasi dengan XRD menunjukkan adanya dua puncak pada 2θ = 22,020 dan 2θ = 42,420 yang menandakan material karbon. Isoterm adsorpsi N2 pada karbon mesopori menunjukkan adanya hystersis loop pada rentang P/P0 sekitar 0,45-0,85 yang merupakan karakter dari padatan mesopori. Karbon mesopori hasil sintesis memiliki ukuran diameter pori yang seragam, yaitu sebesar 8,863 nm. Karakterisasi dengan SEM menunjukkan bentuk grass-like dengan ukuran yang seragam. Variasi kondisi adsorpsi yaitu konsentrasi awal, pH, dan waktu kontak dilakukan untuk menentukan kondisi optimum adsorpsi Acid Red 119 pada karbon mesopori. Kondisi optimum adsorpsi Acid Red 119 dengan menggunakan 10 mg karbon mesopori tercapai pada pH 3 dengan waktu kontak selama 60 menit dan kosentrasi awal larutan sebesar 200 ppm. Karbon mesopori hasil sintesis memiliki kapasitas adsorpsi (Qe) sebesar 217,7389 mg/g. Pemodelan isoterm adsorpsi Freundlich sangat sesuai untuk menjelaskan proses adsorpsi zat warna Acid Red 119 pada karbon mesopori dengan nilai konstanta Freundlich (Kf) sebesar 9,8946 L/g. Daya adsorpsi karbon mesopori hasil sintesis lebih besar dibandingkan karbon aktif komersial, yaitu 1,53 kali lipat.

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Mesoporous carbon material was successfully synthesized through soft-template method by using formaldehyde and phloroglucinol as carbon sources, pluronic F127 as SDA, and hydrochloric acid as catalyst. Preliminary test as adsorbent was carried out to adsorption of Acid Red 119 dyes. The synthesis process of mesoporous carbon involved polymerization of formaldehyde with phloroglucinol in soft-template F127 with the mixture of ethanol and water solvent. The thermogravimetric analysis showed resulted mesoporus carbon is stable up to 900 0C. XRD characterization resulted two identity peaks at 2θ = 22.020 and 2θ = 42.420 as the evidence of carbon material structure. The isotherm of N2 adsorption in mesoporous carbon exhibited hysterisis loop in P/P0 of 0.45-0.85 range which indicates the character of mesoporous solid material. This material has homogeneous pore sizes of 8.863 nm. SEM images showed the uniform grass-like structures on the surface of the bulk carbon. Adsorption conditions, i.e. contact time, intial dye concentration, and pH solution were studied to evaluate the optimum condition of Acid Red 119 adsorption onto mesoporous carbon. The optimum condition of Acid Red 119 adsorption using 10 mg of mesoporous carbon was reached at pH 3 for 60 minutes and 200 ppm of initial dye concentration. The adsorption capacity (Qe) of synthesized mesoporous carbon reaches 217.7389 mg/g. The adsorption of Acid Red 119 into mesoporous carbon can be described by Freundlich isotherm adsorption with the Freundlich constant (Kf) value of 9.8946 L/g. Adsorption capacity of mesoporous carbon is 1.53 times higher than that of commercial activated carbon."

"Gas rumah kaca seperti karbon dioksida merupakan gas yang melimpah di alam sehingga diperlukan cara untuk mengkonversi CO2. Namun, CO2 bersifat stabil secara termodinamika dan kinetika sehingga diperlukan bantuan logam bervalensi rendah contohnya Ni(0) atau Pd(0) untuk dapat bereaksi. Pada penelitian ini digunakan ZSM-5 hirarki terimpregnasi logam nikel sebagai katalis reaksi karboksilasi bertekanan antara fenilasetilena dengan karbon dioksida menjadi asam sinamat. ZSM-5 hirarki dianggap mampu menjadi penyangga katalis logam Ni dikarenakan ZSM-5 hirarki memiliki selektivitas dan transport massa yang baik. ZSM-5 Hirarki disintesis menggunakan metode double template yaitu TPAOH sebagai pengarah struktur MFI dan PDD-AM sebagai pengarah mesopori. Impregnasi logam nikel dilakukan menggunakan metode impregnasi basah dengan reduksi oleh aliran gas hidrogen. Karakterisasi material ZSM-5 hirarki dan Ni/ZSM-5 hirarki dilakukan dengan menggunakan XRD, FTIR, XRF, SEM-EDS dan SAA. Analisa XRD menunjukkan ZSM-5 telah berhasil disintesis. Analisa FTIR menunjukkan dekomposisi template melalui kalsinasi telah berhasil. Pencitraan SEM menunjukkan morfologi material dengan bentuk coffin like-shaped yang merupakan ciri khas ZSM-5. Hasil analisa EDS menunjukkan persen loading Ni dalam ZSM-5 sebesar 1,4 %. Sedangkan analisa XRF menunjukkan persen loading Ni dalam ZSM-5 sebesar 3,325 % yang mengindikasikan logam Ni telah masuk ke dalam pori ZSM-5. Analisa BET menunjukkan adanya hysteresis loop yang mengindikasikan adanya pori berukuran meso. Reaksi karboksilasi bertekanan fenilasetilena dilakukan dalam reaktor batch dengan variasi tekanan CO2 (1, 3, 5, 7 bar) dan suhu (85, 100, dan 125 C). Berdasarkan analisa terhadap campuran produk didapat tekanan CO2 optimum sebesar 3 bar dan suhu optimum pada 85 C.

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Carbon dioxide is one of greenhouse gases which is abundant in nature, therefore efforts are needed to reduce its concentration through CO2 conversion. However, CO2 is thermodynamically and kinetically stable, so it needs low valent metals such as Ni (0) or Pd (0) to help CO2 to react. In this study, the hierarchical ZSM-5 impregnated nickel metal was used as a catalyst for pressurized carboxylation reactions between phenylacetylene and carbon dioxide to cinnamic acid. Hierarchical ZSM-5 is assumed capable for supporting Ni metal catalysts because it has good selectivity and mass transport. Hierarchical ZSM-5 was synthesized using the double template method with TPAOH as structure directing agent for MFI and PDD-AM as mesoporous directing agent. Impregnation of nickel was carried out using a wet impregnation method with reduction by the hydrogen gas flow. Material characterization of hierarchical ZSM-5 and Ni/ZSM-5 was carried out using XRD, FTIR, XRF, SEM-EDS and SAA. XRD analysis shows that ZSM-5 has been successfully synthesized.

FTIR analysis showed that the template decomposition through calcination was successful. SEM imaging of the material shows a coffin-like morphology, which is a characteristic of the ZSM-5. The EDS analysis results shows 1.4% Ni in ZSM-5. While the XRF analysis shows 3.325 % Ni in ZSM-5 of which indicates that Ni has entered the ZSM-5 pores. BET analysis shows a hysteresis loop that indicates mesoporous. Pressurized carboxylation reaction of phenylacetylene were carried out in batch reactors with variations of CO2 pressure (1, 3, 5, 7 bar) and temperature (85, 100, and 125 125 C). Based on the analysis of products with HPLC, the optimal CO2 pressure was obtained at 3 bar and the optimal temperature at 85 C."

"Karbon mesopori telah disintesis dengan menggunakan metode soft-templating dengan menggunakan phloroglucinol sebagai prekursor karbon dan pluronic F127 sebagai template untuk membentuk pori dengan ukuran meso pada struktur karbon. Karbon mesopori kemudian diimpregnasi dengan logam nikel, dengan menggunakan Ni NO3 2. Setelah diimpregnasi, material selanjutnya diuji kemampuan katalisisnya untuk reaksi asetilen dengan CO2. Reaktor yang digunakan adalah lsquo;batch reactor rsquo; dari gelas kaca. Hasil BET membuktikan adanya hysteresis loop dan isotherm adsorpsi tipe IV dengan diameter pori sebesar 7,46 nm. Dengan instrumen EDX dibuktikan bahwa impregnasi nikel berhasil dengan masing-masing persen nikel untuk reduksi dengan etilen glikol pelarut air 34,48, etilen glikol pelarut air:etanol 0,02, NaBH4 0,9 dan gas H2 1,73. Pola XRD dari karbon mesopori yang direduksi dengan NaBH4 dan H2 menunjukan tidak ada perubahan pada struktur karbon mesopori, puncak 2 = 24,44 dan 43,18 hal ini membuktikan bahwa impregnasi logam tidak merubah struktur karbon mesopori. Pada uji aplikasinya, hasil analisa HPLC menunjukan puncak untuk baru pada waktu retensi 3,625 menit. Kondisi optimum didapatkan pada suhu 25 dan waktu 3 jam.

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Mesoporous carbon has been synthesized using the soft templating method using phloroglucinol as carbon precursor and pluronic F127 as a template to form meso size pores on carbon structure. The mesoporous carbon is then impregnated with nickel metal, using Ni NO3 2. After impregnation, the material was further tested for its catalysis capacity for acetylene reactions with CO2. The reactor used is a 39 batch reactor 39 made of glass. The BET results prove the existence of hysteresis loop and IV type adsorption isotherm with a pore diameter of 7.46 nm. With EDX instrument it is proved that nickel impregnation succeeds with each percent of nickel, reduction using ethylene glycol with water as the solvent 34,48, ethylene glycol with water ethanol as the solvent 0,02, NaBH4 0,9 and H2 gas 1,73. XRD patterns of mesoporous carbon reduced with NaBH4 and H2 showed no change in mesoporous carbon structure, peak 2 24.44 and 43.18 This proves that metal impregnation does not alter the mesoporous carbon structure. In the application test, HPLC analysis shows a new peak at retention time of 3,625 minutes. The optimum condition was obtained at 25 and 3 hours."

"Karbon mesopori berhasil disintesis menggunakan metode template lunak dengan Pluronic F-127 sebagai agen struktural; phloroglucinol dan formaldehida sebagai prekursor karbon. Karbon mesopori yang berhasil disintesis kemudian dimodifikasi menggunakan etilendiamin, yang kemudian diimpregnasi dengan nanopartikel Ni. Hasil modifikasi dan impregnasi tersebut dikarakterisasi dengan FTIR, SEM-EDX, BET, dan XRD. Pengujian kapasitas adsorpsi MC, Ni-MC, MC-EDA, dan Ni-EDA MC dilakukan dengan mengalirkan gas CO2 selama 5, 10, dan 15 menit untuk melihat kemampuan adsorpsi CO2. Bahan Ni-MC dan Ni-EDA MC kemudian digunakan sebagai katalis dalam reaksi Hidrogenasi, yaitu reaksi antara molekul hidrogen (H2) dengan unsur atau senyawa lain yang melibatkan suatu katalis. Reaksi hanya dapat berlangsung jika terdapat Ni(0) sebagai pusat aktif pada karbon mesopori. Berbagai parameter katalis yang digunakan meliputi; variasi suhu, variasi jumlah katalis, dan variasi waktu. Proses reaksi hidrogenasi menggunakan reaktor aliran dan dianalisis menggunakan instrumen GC-TCD. % rendemen yang diperoleh dari katalis Ni-MC dan Ni-EDA MC berturut-turut adalah 3,54% dan 3,86% pada suhu 873 K. Pada variasi jumlah katalis, % rendemen diperoleh bahan Ni-MC dengan massa katalis 0,02 g sebesar 4,37% sedangkan Ni-EDA MC diperoleh % rendemen sebesar 4,45% dengan massa katalis 0,03 gr. Untuk melihat hambatan katalis dilakukan dengan variasi waktu. Bahan Ni-MC optimum diuji selama 30 menit dengan rendemen 13,32%, sedangkan MC Ni-EDA optimum pada rentang waktu 40 menit dengan rendemen 13,26%.

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Mesoporous carbon was successfully synthesized using the soft template method with Pluronic F-127 as a structural agent; phloroglucinol and formaldehyde as carbon precursors. The successfully synthesized mesoporous carbon was then modified using ethylenediamine, which was then impregnated with Ni nanoparticles. The results of these modifications and impregnations were characterized by FTIR, SEM-EDX, BET, and XRD. The adsorption capacity of MC, Ni-MC, MC-EDA, and Ni-EDA MC was tested by flowing CO2 gas for 5, 10, and 15 minutes to see the CO2 adsorption ability. Ni-MC and Ni-EDA MC materials are then used as catalysts in Hydrogenation reactions, namely reactions between hydrogen molecules (H2) with other elements or compounds involving a catalyst. The reaction can only take place if there is Ni(0) as the active center on the mesoporous carbon. Various parameters of the catalyst used include; variations in temperature, variations in the amount of catalyst, and variations in time. The hydrogenation reaction process uses a flow reactor and is analyzed using the GC-TCD instrument. The % yields obtained from Ni-MC and Ni-EDA MC catalysts were 3.54% and 3.86% at a temperature of 873 K, respectively. In the variation of the amount of catalyst, the % yield was obtained for Ni-MC material with a catalyst mass of 0.02 g of 4.37% while Ni-EDA MC obtained % yield of 4.45% with a catalyst mass of 0.03 g. To see the catalyst resistance is done with time variations. The optimum Ni-MC material was tested for 30 minutes with a yield of 13.32%, while the optimum Ni-EDA MC was tested for a period of 40 minutes with a yield of 13.26%."