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"CO2 merupakan gas yang inert, tidak beracun, tidak mudah terbakar, dan menjadi gas penyumbang terbesar dalam efek rumah kaca yang menyebabkan suhu permukaan bumi naik. Di sisi lain, kelimpahannya yang tinggi di alam menjadikan CO2 sebagai sumber karbon yang potensial dalam sintesis fine chemicals. Dalam penelitian ini dilakukan studi reaksi karboksilasi fenilasetilena dengan CO2 menggunakan katalis logam Ni terimpregnasi 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. Spektra FTIR dari karbon mesopori sebelum karbonisasi memiliki puncak serapan 3500 2800 cm-1 yang menunjukkan adanya stretching C-H dan stretcing O-H dari phloroglucinol dan formaldehida. Sedangkan setelah karbon mesopori dikarbonisasi, puncak serapan pada bilangan gelombang tersebut hilang. Karakterisasi dengan XRD menunjukkan adanya dua puncak pada 2 yakni 24,26o dan 42,76o yang menandakan puncak khas dari karbon mesopori. Analisis luas permukaan dengan BET menghasilkan isoterm adsorpsi N2 pada karbon mesopori yang menunjukkan adanya hystersis loop pada rentang P/Po sekitar 0,4-0,9 yang merupakan karakter dari karbon mesopori. Karbon mesopori hasil sintesis memiliki distribusi ukuran pori sebesar 7.2 nm yang termasuk dalam rentang material mesopori 2-50 nm . Karakterisasi dengan SEM menunjukkan bentuk yang datar dengan ukuran kristal beragam. Modifikasi support dilakukan dengan cara impregnasi logam Ni ke dalam karbon mesopori Ni@MC . Katalis Ni@MC digunakan sebagai katalis dalam reaksi karboksilasi fenilasetilena dengan CO2. Reaksi dilakukan dalam reaktor batch dengan kondisi reaksi yang bervariasi, yakni suhu 25oC, 50oC, 85oC dan waktu 8 jam, 12 jam, dan 16 jam. Hasil analisis campuran produk dengan HPLC menunjukkan terbentuknya asam sinamat sebesar 1,52 pada sampel 85oC 8jam, 2,83 pada sampel 85oC 12jam, dan 0,62 pada sampel 85oC 16jam.

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CO2 is an inert, non toxic, non flammable, and the largest contributor gas to greenhouse gases causing the earth 39 s surface temperature to rise. Its high abundance in nature makes CO2 a potential carbon source in fine chemical synthesis. In this research, carboxylation reaction of phenylacetylene with CO2 has been studied using an impregnated nickel catalyst on mesoporous carbon support. Mesoporous carbon has been successfully synthesized by soft template method using Pluronic F127 as pore forming, formaldehyde and phloroglucinol as carbon source, and HCl as acid catalyst. This material was characterized by FTIR, XRD, SEM, and BET analysis. The FTIR spectra of the mesoporous carbon before carbonization had an absorption peak of 3500 2800 cm 1 indicating the presence of stretching C H and stretching O H of phloroglucinol and formaldehyde. Meanwhile after carbonization, those peaks disappear. Characterization with XRD shows the presence of two peaks at 2 24.26 and 42.76 which denotes the typical peak of mesoporous carbon. BET Surface Area Analysis gave N2 adsorption isotherm on mesoporous carbon indicating a hysterysis loop in the P Po range 0.4 0.9 which is a character of mesoporous carbon. Synthesized mesoporous carbon had pore size distribution of 7.2 nm which is included in the mesoporous material range 2 50 nm . Characterization with SEM shows a flat shape with varying crystal sizes. Modification of support has been conducted by impregnation of Ni metal into mesoporous carbon Ni MC . The Ni MC catalyst was used as a catalyst in the carboxylation reaction of phenylacetylene with CO2. The reactions were carried out in a batch reactor under various reaction conditions at reaction temperature of 25oC, 50oC, and 85oC and for over 8, 12, and 16 hours. HPLC analysis of the product mixtures shows that cinnamic acid was formed with 1,52 yield in 85oC 8h sample, 2,83 yield in 85oC 12h sample, and 0,62 yield in 85oC 16h sample."

"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."

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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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"Polistirena, polimer yang terdiri dari stirena monomer, banyak digunakan sebagai bahan baku utama dalam produksi wadah makanan. Namun sejumlah kecil fenilasetilena dalam stirena dapat meracuni katalis yang digunakan dalam proses polimerisasi stirena. Karena itu, diperlukan cara untuk menghilangkannya. Salah satunya dengan mengubahnya menjadi stirena menggunakan metode hidrogenasi selektif. Karbon mesopori (MC) telah berhasil disintesis melalui metode soft template menggunakan phloroglucinol dan formaldehida sebagai prekursor karbon dan pluronic F127 sebagai template mesopori. Karbon mesopori kemudian dimodifikasi menjadi katalis bimetalik Ni-Co (NiCo/MC), dilanjutkan reduksi selama 4 jam pada suhu 400°C di bawah aliran gas H2. Katalis dikarakterisasi menggunakan FTIR, XRD, SEM-EDX, SAA dan TEM. Karbon mesopori dan bimetalik NiCo/MC kemudian digunakan sebagai katalis dalam hidrogenasi selektif fenilasetilena pada suhu 303 K dan 323 K selama 5 jam dengan gas H2 sebagai reduktor. Karbon mesopori yang dimodifikasi menjadu monometalik Ni (Ni/MC) juga diuji sebagai pembanding. Produk reaksi diukur menggunakan GC-FID. Hasil penelitian menunjukkan bahwa katalis NiCo/MC memberikan %yield sebesar 1,42% dan 1,33% untuk reaksi masing-masing pada 303 dan 323 K. Sedangkan katalis Ni/MC memberikan hasil yang lebih tinggi 4% untuk reaksi pada suhu 323 K.

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Polystyrene, a polymer composed of styrene monomer, is widely used as the main raw material in food container production. However trace quantities of phenylacetylene in styrene can poison the catalyst used in the styrene polymerization process. Therefore, it is necessary remove it, for instant by catalytically converting it to styrene using selective hydrogenation method. Mesoporous carbon (MC) has been successfully synthesized via soft template method using phloroglucinol and formaldehyde as carbon precursors, and pluronic F127 as mesopore template. The as-synthesized MC then impregnated with bimetallic Ni-Co(NiCo/MC), followed by reduction for 4 hour at 400 °C under a flow of H2. The catalysts were characterized using FTIR, XRD, SEM-EDX, SAA and TEM. Both MC and bimetallic NiCo/MC then were used as catalysts in phenylacetylene selective hydrogenation at 303 K and 323 K for 5 h with H2 as the reducing agent. The as-synthesized MC modified monometallic Ni (Ni/MC) was also tested as comparison. The reaction product was measured using gas chromatography with flame ionization detector. The results show that the NiCo/MC catalyst gives a yield of 1.42% and 1.33% for the reaction at 303 and 323 K, respectively. Whereas Ni/MC catalyst gives a higher yield of 4% for the reaction at 323 K."

"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%."

"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."

"Alkuna merupakan hidrokarbon tak jenuh yang memiliki setidaknya satu ikatan rangkap tiga C C yang berperan penting sebagai bahan baku untuk menghasilkan berbagai senyawa organik yang bermanfaat dengan membentuk ikatan baru C-C, C-H atau C-X. Proses hidrogenasi alkuna menjadi senyawa alkena sangat penting dalam sintesis senyawa organik khususnya di bidang industri polimer. Dalam penelitian ini dilakukan hidrogenasi pada senyawa difenilasetilena sebagai model senyawa alkuna dengan menggunakan NaBH4 sebagai sumber hidrogen serta katalis bimetalik NiCo yang diembankan pada karbon mesopori sebagai penyangga katalis. Karbon mesopori disintesis dengan metode cetakan lunak menggunakan surfaktan pluronik F-127 sebagai template organik, phloroglucinol dan formaldehida sebagai prekursor karbon, serta HCl sebagai katalis asam. Karbon mesopori kemudian dimodifikasi dengan penambahan bimetalik NiCo dengan metode impregnasi basah menggunakan Ni(NO3)2.6H2O dan Co(NO3)2.6H2O sebagai prekursor. Hasil sintesis karbon mesopori, Ni/MC dan NiCo/MC kemudian dikarakterisasi menggunakan FTIR, XRD, SEM-EDX, TEM dan SAA. Berdasakan analisis SAA didapatkan diameter pori MC, Ni/MC dan NiCo/MC berturut-turut sebesar 12,8 nm, 13,4 nm dan 12,7 nm yang menunjukan katalis berukuran mesopori. Reaksi hidrogenasi difenilasetilena dilakukan dengan variasi waktu (2 jam, 4 jam dan 6 jam) dan variasi suhu (30oC dan 50oC). Sisa katalis yang digunakan dikarakterisasi menggunakan FTIR, sedangkan produk hasil reaksi kemudian dikarakterisasi menggunakan GCMS. Hasil analisis menunjukan kondisi optimum diperoleh pada suhu 50oC selama 4 jam dengan persen konversi sebesar 37,6% dan persen yield sebesar 62,3% untuk cis-stilbene dan 9,2% untuk trans-stilbene dengan selektivitas terhadap pembentukan cis-stilbene sebesar 87,1%.

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Alkynes are unsaturated hydrocarbons that have at least one C≡C triple bond which plays an important role as raw material for producing various useful organic compounds by forming new C-C, C-H or C-X bonds. The hydrogenation process of alkenes to become alkenes is very important in the synthesis of organic compounds, especially in the polymer industry. In this study, hydrogenation was carried out on diphenylacetylene compounds as a model for alkyne compounds using NaBH4 as a source of hydrogen as well. NiCo bimetallic catalyst which is carried on mesoporous carbon as catalyst support. Mesoporous carbon was synthesized by the soft mold method using pluronic F-127 surfactant as an organic template, phloroglucinol and formaldehyde as carbon precursors, and HCl as an acid catalyst. Mesoporous carbon was then modified by adding bimetallic NiCo by wet impregnation method using Ni(NO3)2.6H2O and Co (NO3) 2.6H2O as precursors. The results of the synthesis of mesoporous carbon, Ni / MC and NiCo / MC were then characterized using FTIR, XRD, SEM-EDX, TEM and SAA. Based on the SAA analysis, it was found that the pore diameters of MC, Ni / MC and NiCo / MC were 12.8 nm, 13.4 nm and 12.7 nm respectively, which indicated the mesoporous size of the catalyst. The hydrogenation reaction of diphenylacethylene was carried out with variations in time (2 hours, 4 hours and 6 hours) and temperature variations (30oC and 50oC). The remaining catalyst used was characterized using FTIR, while the reaction product was characterized using GCMS. The results of the analysis showed that the optimum conditions were obtained at 50oC for 4 hours with a percent conversion of 37.6% and yield of 62.3% for cis-stilbene and 9.2% for trans-stilbene with a selectivity to the formation of cis-stilbene of 87,1%."

"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%."

"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."

"ABSTRAKKarbon mesopori telah berhasil disintesis dengan metode soft template menggunakan phloroglucinol dan formaldehida sebagai sumber karbon dan Pluronic F127 sebagai template. Material kemudian diimpregnasi dengan Ni II dilanjutkan dengan reduksi dengan H2 sehingga terbentuk nanopartikel Ni yang terimpregnasi dalam karbon mesopori. Analisis dengan XRD menunjukkan difraksi pada 25 dan 44o yang merupakan difraksi dari karbon grafitik. Selain itu difraksi pada 45 dan 52o menunjukkan keberadaan Ni 0 . Analisis EDX mengungkap kandungan Ni dalam beberapa karbon mesopori sebesar 0,1 hingga 24 . Analisis luas permukaan memberi informasi karbon mesopori memiliki luas permukaan sebesar 387,7 m2/g dan pori 7,4 nm. Impregnasi dengan Ni akan memperkecil luas permukaan maupun ukuran pori. Analisis dengan XPS mengonfimasi keberadaan Ni dengan bilangan oksidasi nol. Material digunakan sebagai katalis untuk reaksi hidrogenasi CO2. Reaksi hanya dapat berlangsung jika terdapat Ni 0 sebagai pusat aktif pada karbon mesopori. Semakin banyak Ni 0 semakin besar konversinya meskipun tidak berpengaruh terhadap persen hasil yield . Konversi terbesar didapat dari katalis Ni-MC 30 dengan konversi dan yield berturut-turut 94,6 dan 3,5 pada suhu 673 K.

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ABSTRACT Mesoporous Carbon has been successfully synthesized via soft template method using phlroglucinol and formaldehyde as carbon precursors and Pluronic F127 as template. The material was impregnated with Ni II and reduced with H2 to obtainNi metal. XRD analysis showed diffraction peaks on 25 and 44o which are characteristic of graphitic carbon. In addition, diffraction on 45 and 52o showed the existence of Ni 0 . EDX analysis showed the Ni content in mesoporous carbon, that was 0.1 to 24 . Surface area analysis gave information about surface area of 387.7 m2 g and pore diameter of 7.4 nm. Ni impregnation is presumed to reduce both surface area and pore diameter of mesoporous carbon. XPS analysis confirmed zero oxidation state of Ni. This material was used as catalyst for CO2 hydrogenation reaction. This reaction gave product only in the presence of Ni. The higher the Ni content the higher the conversion though the yield is unchanged. The highest conversion is shown by Ni MC 30 with conversion of 94.6 and yield of 3.5 at 673 K."