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"Karbondioksida merupakan gas rumah kaca yang menjadi salah satu faktor pemanasan global dan perubahan iklim secara drastis. Namun, di samping dampak negatif emisi gas CO2 secara alami maupun melalui hasil kegiatan antropogenik, CO2 dapat dimanfaatkan sebagai sumber C1 reaksi organik, salah satunya reaksi karboksilasi. Periodic Mesoporous Organosilica (PMO) merupakan material mesopori silika yang memiliki keunggulan, di antaranya memiliki ukuran pori cukup besar yang dapat memfasilitasi transfer massa dengan baik, luas permukaan besar yang memungkinkan banyak sisi katalitik, maupun integrasi dari spesi organik dan atom logam dalam kerangka PMO. Logam nikel merupakan logam yang secara luas digunakan dalam bidang katalisis, karena logam tersebut memiliki orbital d tidak terisi penuh, sehingga dapat membentuk ikatan kovalen koordinasi dan memudahkan proses pembentukan intermediet pada permukaan katalis. Pada penelitian ini, dilakukan sintesis PMO dengan prekursor 4,4’- bis(trietoksisilil)bifenil dan dilanjutkan dengan fungsionalisasi gugus amina melalui proses nitrasi dan aminasi. Selanjutnya, dilakukan imobilisasi kompleks Ni(acac)2 pada material Bph-PMO untuk digunakan sebagai katalis pada reaksi karboksilasi fenilasetilena dengan CO2. Analisis XRD menunjukkan bahwa fungsionalisasi gugus amina pada Bph-PMO tidak merubah komponen maupun struktur periodik pada Bph-PMO, begitu pula setelah nikel diimobilisasi pada Bph- PMO yang terfungsionalisasi gugus amina. Analisis FTIR Ni/NH2-Bph-PMO menunjukkan puncak serapan pada 1605 cm-1 yang mengindikasikan pembentukan ikatan C=N dari reaksi kondensasi Schiff antara gugus amina dengan C=O pada Ni(acac)2. Material Ni/NH2-Bph-PMO memiliki ukuran partikel rata-rata 420 nm, dengan pemuatan nikel 2,8% berdasarkan analisis SEM-EDX. Analisis TEM menunjukkan keberadaan struktur mesopori pada NH2-Bph-PMO. Ukuran diameter pori dan luas permukaan BET material Ni/NH2-Bph-PMO berturut-turut sebesar 3,16578 nm dan 490,742 m2/g. Uji katalitik material Ni/NH2-Bph-PMO pada karboksilasi fenilasetilena dengan CO2 dilakukan pada tiga variasi suhu, di mana kondisi optimum diperoleh pada suhu 25 °C, dengan konsentrasi produk fenil maleat 244,5899 ppm.

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ABSTRACTCarbon dioxide is a greenhouse gas that affecting global warming and produces climate change. However, aside from the negative effects of natural CO2 gas emissions and through anthropogenic activities, CO2 has been used as a source of C1 organic reactions, for example, carboxylation reaction. Periodic Mesoporous Organosilica (PMO) is a superior silica mesoporous material, which has a large pore to facilitate mass transfer, a large area that allows many catalytic sides, which also associated with organic species and metal atoms in PMO. This property supports PMO to be applied as a metal catalyst support. Nickel metal is a metal that is widely used in the catalysis field, because this metal has d orbitals and is not fully filled, so it can form covalent bonds and fasilitate process of making intermediates on the surface of the catalyst. In this study, PMO was synthesized with 4,4'-bis (triethoxysilyl) biphenyl precursor and continued with the functionalization of amine groups through nitration and amination process. Furthermore, immobilization of Ni(acac)2 complex was carried out on the Bph-PMO material to be used as a catalyst in the carboxylation reaction of phenylacetylene with CO2. Analysis of XRD shows that the functionalization of amine groups on Bph-PMO does not change the periodic structure of Bph-PMO, as well as after nickel immobilized on aminated Bph-PMO. Absorption peak at 1605 cm-1 of Ni/NH2- Bph-PMO revealed from FTIR analysis, indicating new C=N bond from Schiff condensation between amine group and C=O from Ni(acac)2. Ni/NH2-Bph-PMO material has an average particle size of 420 nm, with 2,8% nickel loading based on SEM-EDX analysis. Mesoporous structure of NH2-Bph-PMO has been proved by TEM analysis. The pore diameter size and BET surface area of Ni/NH2-Bph-PMO are 3,16578 nm and 490,742 m2/g, respectively. The catalytic test of Ni/NH2-Bph- PMO on phenylacetylene carboxylation with CO2 was carried out at three temperature variations, which shows that optimum condition was obtained at 25 °C, with a concentration of phenyl maleic product of 244,5899 ppm."

"Reaksi karboksilasi alkuna terminal dengan karbon dioksida (CO2) dibantu katalis dalam mempercepat reaksi untuk menghasilkan asam karboksilat. Periodic mesoporous organosilica dengan jembatan fenilena (Ph-PMO) dipilih untuk menjadi pendukung katalis karena memiliki luas permukaan yang tinggi dan diameter yang besar, sehingga mampu meningkatkan sisi aktif katalis. Sintesis Ph-PMO dilakukan menggunakan metode sol-gel dibuktikan dengan karakterisasi FTIR, XRD, TEM-EDX, BET, dan TGA. Pada analisis TEM didapatkan struktur lamellar yang menunjukkan periodisitas dari Ph-PMO dengan diameter rata-rata pori 4,9 nm. Impregnasi katalis Cu yang didukung oleh Ph-PMO dan menghasilkan Cu0 , berhasil dibuktikan melalui analisis XRD sesuai dengan JCPDS No. 04-0836. Diameter pori dengan metode BJH mengalami penurunan dari Ph-PMO menjadi Cu/PhPMO yaitu 3,8786 nm dan 3,8708 nm. Produk reaksi karboksilasi fenilasetilena dengan CO2 dengan variasi massa katalis pada kondisi optimum suhu 75oC selama 6 jam dianalisis dengan menggunakan HPLC. Hasil analisis HPLC menunjukkan kondisi optimum untuk menghasilkan asam fenilpropiolat pada massa katalis 0,2001 g dengan konsentrasi 7,3198 ppm dan asam sinamat masing-masing pada massa katalis 0,0667 g dengan konsentrasi 20,2064 ppm.

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The carboxylation reaction of a terminal alkyne with carbon dioxide (CO2) assisted by a catalyst in the reaction to produce a carboxylic acid. Periodic mesoporous organosilica with phenylene bridge (Ph-PMO) was chosen to be the catalyst support because it has a high surface area and a large diameter, to increase the active site of the catalyst. Ph-PMO synthesis was carried out using the sol-gel method as evidenced by the characterization of FTIR, XRD, TEM-EDX, BET, and TGA. In TEM analysis, we found a lamellar structure that shows the periodicity of Ph-PMO with an average pore diameter of 4,9 nm. The Cu impregnation catalyst supported by Ph-PMO and producing Cu0, was successfully proven by XRD analysis according to JCPDS No. 04-0836. The pore diameter using the BJH method decreased from Ph-PMO to Cu/Ph-PMO, namely 3,8786 nm and 3,8708 nm, respectively. The product of the carboxylation reaction of phenylacetylene with CO2 with various catalysts at an optimum temperature of 75oC for 6 hours was analyzed using HPLC. The results of HPLC analysis showed the optimum conditions to produce phenylpropiolic acid at a catalyst mass of 0,2001 g with a concentration of 7,3198 ppm and cinnamic acid respectively at a catalyst mass of 0,0667 g with a concentration of 20,2064 ppm."

"Periodic Mesoporous Organosilica atau PMO yang mengandung jembatan organik berupa bifenilena (Bph-PMO) telah berhasil disintesis melalui metode sol-gel dengan pendekatan Evaporation Induced Self-Assembly (EISA). Variasi jumlah surfaktan yang ditambahkan memberikan pengaruh terhadap karakteristik Bph-PMO yang terbentuk berupa peningkatan luas permukaan seiring meningkatnya jumlah surfaktan yang ditambahkan. Pengembanan Bph-PMO dengan nanopartikel nikel melalui metode impregnasi menggunakan NiCl2 sebagai prekursor nikel dan direduksi menggunakan NaBH4 berhasil dilakukan yang dibuktikan dengan karakterisasi TEM-EDX dan adanya penurunan luas permukaan berdasarkan perhitungan BET setelah dilakukannya impregnasi. Uji adsorpsi 15% gas CO2 menggunakan instrumentasi GC-TCD membuktikan pengaruh luas permukaan terhadap kapasitas adsorpsi. Kapasitas adsorpsi pada suhu ruang meningkat seiring bertambahnya jumlah surfaktan dimana selaras dengan luas permukaan yang cenderung meningkat pula. Setelah dilakukannya impregnasi dengan logam nikel, kapasitas adsorpsi menurun dikarenakan adanya penurunan luas permukaan. Namun, penurunan kapasitas adsorpsi tidak sesignifikan penurunan luas permukaan. Hal ini menunjukkan adanya pengaruh dari aktivitas nanopartikel nikel itu sendiri.

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The focus of this research was evaluate the CO2 adsorption activity of PMO synthesized from biphenylene-bridged organosilane with non-ionic surfactant Pluronic F127 and then the material (called Bph-PMO) was impregnated with nickel metal to increase the active site of the adsorbent and the interaction with CO2. Increasing amount of surfactant has an effect on its surface area. The impregnation method was used NiCl2 as nickel precursor and NaBH4 as reducing agent was succesfully carried out by TEM-EDX and decreased in surface area based on BET calculation. GC-TCD instrumentation was used to evaluate the adsorption of 15% CO2. It shows the effect of surface area on the adsorption capacity of the material. After impregnation with nickel metal, the adsorption capacity decreased due to its surface area. However, the decrease in adsorption capacity was not as significant as the decrease in surface area. This shows the influence of the nickel nanoparticles activitiy itself."

"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."

"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."

"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 dioksida (CO2) merupakan gas rumah kaca utama yang mendorong perubahan iklim dan pengasaman laut. Walaupun demikian CO2 juga dapat menjadi sumber daya C1 yang berlimpah, tidak beracun, tidak mudah terbakar, dan dapat diperbaharui. Karena itu, konversi gas CO2 menjadi bahan kimia yang bernilai menjadi topik hangat untuk diteliti lebih dalam. Pada penelitian ini dilakukan penelitian terkait reaksi hidrokarboksilasi difenilasetilena dengan CO2 menggunakan katalis homogen utama yaitu Nickel(II) bis(acetylacetonate)bipyridine atau Ni(acac)2(bpy). Reaksi dilakukan dalam reaktor dengan kondisi yang bervariasi, yakni variasi banyaknya ligan bipiridin, variasi jenis sumber proton (metanol dan NaBH4), dan variasi jenis pelarut (DMF dan metanol). Reaksi dengan variasi kondisi optimal dilakukan variasi suhu (5℃, 27℃, 60℃) dan variasi waktu untuk mengetahui kondisi terbaik dari reaksi hidrokarboksilasi difenilasetilena. Selain itu, dianalisis terkait pengaruh preparasi katalis secara insitu dibandingkan dengan katalis hasil sintesis terhadap reaksi hidrokarboksilasi difenilasetilena. Produk dari reaksi hidrokarboksilasi yang diharapkan adalah asam α-fenilsinamat. Analisis HPLC terbaik ditunjukan oleh variasi banyaknya ligan dengan perbandingan Ni:bpy sebesar 1:1 dengan menggunakan pelarut DMF, sumber proton metanol, dan suhu reaksi 5℃ yang memberikan persen yield asam α-fenilsinamat sebesar 3,24%.

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Carbon dioxide (CO2) is a major greenhouse gas driving climate change and ocean acidification. However, CO2 can also be an abundant, non-toxic, non-flammable, and renewable C1 resource. Therefore, the conversion of CO2 gas into valuable chemicals is a hot topic for further research. In this study, a research was conducted on the hydrocarboxylation reaction of diphenylacetylene with CO2 using Nickel(II) bis(acetylacetonate)bipyridine (Ni(acac)2(bpy)) as main homogeneous catalyst. The reaction was carried out in a reactor with various conditions, namely variations in the number of bipyridine ligands, variations in the type of proton source (methanol and NaBH4), and variations in the type of solvent (DMF and methanol). The reaction with optimal conditions was carried out with variations in temperature (5℃, 27℃, 60℃) and time variations to determine the best condition of the hydrocarboxylation reaction. In addition, it was analyzed regarding the effect of in situ preparation of the catalyst compared to the synthesized catalyst on the diphenylacetylene hydrocarboxylation reaction. The expected product of the hydrocarboxylation reaction is α-phenylcinnamic acid. The best HPLC analysis was shown by variation in the number of bipyridine (Ni:bpy = 1:1) using DMF solvent, methanol as proton source, at reaction temperature of 5℃ which give an α-phenylcinnamic acid yield of 3,24%."

"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%."

"Studi perbandingan katalis Cu/CeO2/Al2O3 dan Cu/ZnO/Al2O3 menjadi topik menarik untuk diteliti karena memiliki perbedaan konversi dan selektifitas terhadap produk alkohol. Katalis Cu/CeO2/Al2O3 dan Cu/ZnO/Al2O3 berhasil disintesis dan diuji kinerja katalisisnya dalam reaktor dengan perbandingan laju alir CO2:H2 sebesar 1:3 dengan suhu 250oC, 300oC dan 350oC. Penelitian ini bertujuan untuk melihat efektifitas dari kedua katalis dalam menghasilkan metanol dan ingin diketahui pengaruh pemberian beberapa variasi suhu. Hasil sintesis katalis dikarakterisasi menggunakan instrument SEM, XRD dan BET. Hasil reaksi hidrogenasi juga dikarakterisasi menggunakan VOC meter, IRGA dan GC-MS. Produk hasil hidrogenasi CO2 menggunakan katalis Cu-CeO2 menunjukkan konsentrasi senyawa organik secara beturut sebesar 4,7 ppm, 8,6 ppm dan 10,1 ppm dengan CO2 terkonversi sebesar 81,68%, 87,35% dan 90,14%, serta kromatogram GC-MS mengindikasikan senyawa metanol. Sedangkan dengan penggunaan katalis Cu-ZnO, didapatkan konsentrasi senyawa organik berturut sebesar 0,5 ppm, 1,0 ppm dan 2,4 ppm dengan CO2 terkonversi sebesar 81,46%, 81,58% dan 84,16%. Hasil tersebut menunjukan bahwa katalis Cu/CeO2/Al2O3 lebih efektif dalam menghidrogenasi CO2 menjadi metanol.

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Comparative studies of Cu/CeO2/Al2O3 and Cu/ZnO/Al2O3 catalysts is an interesting topic to research because of the differences of their conversion rates and selectivity to produce alcohol. Cu/CeO2/Al2O3 and Cu/ZnO/Al2O3 catalysts were successfully synthesized and the performances has been tested in a reactor with the ratio flow rate of CO2:H2 which is 1:3 temperatures of 250oC, 300oC dan 350oC. This study aimed to determine the abilities of both catalyst in producing metanol and to find the effect of several temperature variations. The characterizations of the synthesized catalysts were performed using SEM, XRD and BET instruments. The results of the hydrogenation reaction were also characterized using a VOC meter, IRGA and GC-MS. Products resulting from hydrogenation of CO2 using a Cu-CeO2 catalyst showed concentrations of organic compounds of 4.7 ppm, 8.6 ppm and 10.1 ppm with converted CO2 of 81.68%, 87.35% and 90.14% and GC-MS chromatograms indicates a methanol compound. Meanwhile, with the use of Cu-ZnO catalyst, the concentration of organic compounds was obtained, respectively, 0.5 ppm, 1.0 ppm and 2.4 ppm with converted CO2 of 81.46%, 81.58% and 84.16%. These results indicate that the Cu/CeO2/Al2O3 catalyst is more effective in hydrogenating CO2 into methanol."

"Sintesis Periodic Mesoporous Organosilica dengan jembatan biphenylene telah berhasil dilakukan menggunakan metode sol gel dengan kehadiran surfaktan sebagai template. Selanjutnya fungsionalisasi Bph-PMO dengan gugus amina telah berhasil dilakukan dengan dua langkah reaksi kimia yaitu reaksi nitrasi menggunakan HNO3 65%/H2SO4 96% dan reduksi menggunakan menggunakan SnCl2/HCl 37%. Hasil sintesis kemudian dikarakterisasi menggunakan FTIR, XRD, dan TEM EDX. Karakterisasi TEM mengkonfirmasi struktur material Bph-PMO memiliki struktur mesopori 2D hekasogonal dengan periodisitas molekuler, setelah difungsionalisasi dengan ukuran rata-rata diamater partikel sebesar 223.7 nm. Modifikasi permukaan pada NH2-Bph-PMO dengan nanopartikel perak telah dilakukan dengan metode impregnasi dan reduksi menggunakan AgNO3 sebagai prekursor perak dan NaBH4 sebagai agen pereduksi. Hasil karakterisasi XRD mengkonfirmasi keberadaan nanopartikel perak pada nilai 2θ = 38.1o, 44.2o, 64.5o dan 77,4o. Perhitungan besar ukuran kristal rata-rata dari nanopartikel perak dalam Ag/NH2-Bph-PMO adalah 8,05 nm berdasarkan persamaan Debye- Scherer. Kemampuan adsorpsi CO2 pada material Bph-PMO, NH2-Bph-PMO dan Ag/NH2-Bph-PMO ditentukan menggunakan metode titrimetri. Banyaknya CO2 yang teradsorpsi selama 15 menit dari masing masing material adalah 33.44, 8.392, dan 16.4 mmol. Reaksi karboksilasi fenilasetilena dengan CO2 dilakukan dengan variasi suhu (25oC, 50oC, dan 70oC). Hasil reaksi dianalisa menggunakan HPLC dan menunjukkan %konversi terbaik pada suhu 50oC yaitu 46.74%.

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Synthesis of Biphenyl Periodic Mesoporous Organosilica (Bph-PMO) has been successfully carried out using the sol gel method in the presence of surfactants as a template. Furthermore, the functionalization of Bph-PMO with an amine group has been successfully carried out with two steps of a chemical reaction, nitration reaction (HNO3 65%/H2SO4 96%) and reduction (SnCl2/HCl 37%). Results of the synthesis were characterized using FTIR, XRD, and TEM EDX. TEM characterization confirmed that Bph-PMO material having a 2D hekasogonal mesoporous structure with molecular periodicity, after functionalized the material have average particle size of 223.7 nm. Surface modification of NH2-Bph-PMO with silver nanoparticles has been carried out by impregnation and reduction method using AgNO3 as a silver precursor and NaBH4 as a reducing agent. The result of XRD characterization confirmed the presence of silver nanoparticles at 2θ = 38.1o, 44.2o, 64.5o and 77.4o. Based of Debye-Scherer Calculation the average crystal size of silver nanoparticles in Ag/NH2-Bph-PMO is 8.05 nm. The capacity adsorption of CO2 on Bph-PMO, NH2-Bph-PMO and Ag/NH2-Bph-PMO materials was determined using the titrimetry method. The amount of CO2 adsorbed for 15 minutes from each material is 33.44, 8,392 and 16.4 mmol. The carboxylation reaction of phenyl acetylene with CO2 was carried out with variation of temperature (25oC, 50oC, and 70oC). The results of the reaction were analyzed using HPLC and showed the best conversion at 50oC at 46.74%."