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Abstrak :
Karbon mesopori telah berhasil disintesis melalui metode soft template dengan Pluronic F-127 sebagai agen pembentuk pori; phloroglucinol dan formaldehida sebagai sumber karbon. Material ini dimodifikasi lebih lanjut dengan etilendiamin (EDA) dan trietilentetramin (TETA). Struktur dan sifat dari karbon mesopori termodifikasi dikarakterisasi dengan FTIR, Analisis Luas Permukaan, EDS, XRD, dan FE-SEM. Spektra FTIR dari karbon mesopori termodifikasi gugus amina memiliki puncak serapan 3100~3600 cm-1, 1485~1579 cm-1, dan 2924 cm-1 yang merupakan karakter dari senyawa amina. Analisis unsur menunjukkan karbon mesopori termodifikasi 50% EDA dan karbon mesopori termodifikasi 50% TETA memiliki kandungan nitrogen masing-masing 23,23% dan 20,24%. Analisis luas permukaan pada karbon mesopori termodifikasi memperlihatkan berkurangnya luas permukaan, volume pori, dan diameter pori namun masih mempertahankan sifat mesoporinya. Hasil ini menunjukkan karbon mesopori telah berhasil dimodifikasi dengan gugus amina. Karbon mesopori termodifikasi gugus amina telah diuji sebagai adsorben CO 2 dan hasilnya dibandingkan dengan karbon mesopori tanpa modifikasi. Kadar CO 2 sebelum dan sesudah melewati adsorben dihitung dengan metode titrasi. Hasil eksperimen menunjukkan gugus amina telah berhasil meningkatkan kemampuan adsorpsi dari karbon mesopori.

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Mesoporous carbon has been successfully synthesized by soft templating method with Pluronic F-127 for generation of porous carbon structures; phloroglucinol and formaldehyde as carbon source. Furthermore, the mesoporous carbon was modified with ethylenediamine (EDA) and triethylenetetramine (TETA). The structure and properties of the modified mesoporous carbon were characterized by using XRD, FTIR, Surface Area Analysis, EDS, XRD, and FE-SEM. The FTIR spectra of amine-modified mesoporous carbon have peaks at 3100~3600 cm-1, 1485~1579 cm-1, and 2924 cm-1 which is characteristic of amine compounds. Elemental analysis showed that the 50% EDA-modified mesoporous carbon and 50% TETA-modified mesoporous carbon has 23.23% and 20.24% nitrogen content, respectively. Surface area analysis of this material showed surface area, pore volume, and pore diameter have decreased but still maintained mesoporous character. These results indicated mesoporous carbon has been successfully modified with amine groups. The amine-modified mesoporous carbon has been tested as CO 2 adsorbent and compared to the parent mesoporous carbon. The amount of CO 2 before and after adsorption were measured with titration method. The result showed that amine groups have successfully improved the CO 2 adsorption of mesoporous carbon.

Abstrak :
ABSTRACT
Perkembangan sains dan teknologi yang meningkat secara pesat mempengaruhi pertumbuhan ekonomi serta proses industrialisasi. Proses industrialisasi menghasilkan limbah industri yang mengandung logam berat seperti tembaga Cu. Limbah industri dapat menyebabkan pencemaran lingkungan disekitar daerah industri yang ditinggali 15 juta atau 6 dari penduduk Indonesia. Salah satu solusi untuk mengatasi permasalahan tersebut dengan menggunakan material mesopori silika Santa Barbara Amorphous SBA-15 sebagai adsorban. SBA-15 disintesis menggunakan proses sol gel menggunakan Tetraorthosilicate TEOS sebagai prekursor dan Surfaktan Pluronik 123 Triblok Kopolimer sebagai template serta 3-Chloropropyl trimethoxysilane CPTMS sebagai fungsionalisasi agen untuk memodifikasi permukaan SBA-15 agar dapat menjadi adsorban yang baik. Material tersebut dikarakterisasi oleh SAXRD dan TEM untuk mempelajari kristalinitas dan struktur pori material tersebut, FTIR untuk menunjukan kehadiran gugus organik, Brunauer Emmet Teller BET N2 uji adsorpsi isoterm pada 77 K untuk mengetahui luas permukaan pori, serta AAS untuk mengetahui konsentrasi ion setelah proses adsorpsi. Struktur kristal SBA-15 dan SBA-15 CPTMS diketahui adalah 2D heksagonal dengan struktur pori SBA-15 lebih teratur dibanding SBA-15 CPTMS. Luas permukaan SBA-15 CPTMS diketahui lebih rendah dibanding SBA-15, dengan perbandingan 711.061 m2/g dan 831.996 m2/g. Meskipun begitu, pada uji adsorpsi Tembaga, SBA-15 CPTMS memiliki kemampuan adsorpsi yang lebih tinggi.

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ABSTRACT
The high development of science and technology affects the economic growth and industrialization process. The industrialization process produces industrial waste which contain heavy metal such as copper Cu. This industrial waste can harm the environment surronding industrial areas where 15 million or 6 of the Indonesian population live. In order to overcome this problem, mesoporous silica material Santa Barbara Amorphous 15 SBA 15 is used as an adsorbent. SBA 15 was synthesized through sol gel process using tetraorthosilicate as precursor, Pluronic 123 triblock copolymer as template, and 3 chloropropyl trimethoxysilane CPTMS as functionalized agent. CPTMS was used to modify the SBA 15 surface in order to improve the materials as adsorbent. The materials were characterized using SAXRD and TEM to study material rsquo s cristallinity and pore structure, the presence of organic group was examined using FTIR, the surface area of SBA 15 and SBA 15 CPTMS were characterized using Brunauer Emmett Teller BET N2 adsorption isotherm test at 77 K, and the ions concentration in solution after adsorption process was determined using AAS. The crystal structure of SBA 15 and SBA 15 CPTMS was found 2D heksagonal with a more regular SBA 15 pore structure than SBA 15 CPTMS. The surface area of SBA 15 CPTMS was found to be lower than SBA 15, 711.061 m2 g in comparison to 831.996 m2 g. However, in copper adsorption test, it was found that SBA 15 CPTMS has higher adsorption ability.

Abstrak :
ABSTRAK
Karbon 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.

Abstrak :
Pada pemerosesan industri tekstil banyak menggunakan air, zat pewarna juga bahan kimia campuran yang berdampak pada timbulnya limbah cair tekstil [1]. Salah satu komponen limbah berbahaya yang terkandung dalam limbah cair tekstil adalah logam-logam berat seperti kadmium (Cd), timbal (Pb), tembaga (Cu), dan seng (Zn) [1]. Contoh langkah untuk mencegah pencemaran logam berat cair adalah menggunakan material mesopori silika seperti SBA-15 karena memiliki luas permukaan, diameter, serta volume pori yang besar serta struktur heksagonal teratur sehingga dapat diaplikasikan sebagai adsorben logam berat. Pada penelitian ini, dilakukan analisis studi kepustakaan sintesis mesopori SBA-15 dengan metode sol-gel serta fungsionalisasi CPTMS yang telah berhasil dilakukan dan dilanjutkan menganalisis kemampuan serapannya pada logam berat kadmium (Cd), tembaga (Cu), seng (Zn), dan timbal (Pb). Tipikalnya, menyintesis SBA-15 dilakukan menggunakan Tetraethyl Orthosilicate (TEOS) sebagai prekursor dan Triblock Copolymer Pluronic 123 (P-123) sebagai surfaktan. Kemudian, hasil produk SBA-15 dilakukan fungsionalisasi CPTMS dengan metode post grafting. Hasil karakterisasi memperlihatkan, pada perhitungan BET dibanding sampel SBA-15 murni, sampel SBA-15 CPTMS mengalami penurunan parameter diameter pori dari 29,203 menjadi 28,521 Å, volume pori dari 265,161 menjadi 199,694 cm3/gr dan luas permukaan spesifik dari 831,996 menjadi 711,061 m2/gr, pada pengujian SAXS, sampel SBA-15 CPTMS tidak terdapat perbedaan signifikan dengan SBA-15 dengan tetap memperlihatkan puncak bidang (100), bidang (110) dan bidang 200, pada pengamatan TEM, sampel SBA-15 CPTMS tetap mempertahankan bentuk heksagonalnya, dan pada pengujian FTIR, terlihat adanya gugus klorida (-Cl) pada gelombang 500 cm 1 yang menunjukkan proses fungsionalisasi CPTMS berhasil dilakukan. Sementara, hasil pengujian serapan logam berat dengan AAS memperlihatkan fungsionalisasi CPTMS tidak memiliki selektivitas yang baik pada logam berat kadmium (Cd) dan seng (Zn) karena penurunan nilai persentase penyerapan. Namun, perhitungan kapasitas adsorpsi memperlihatkan bahwa diseluruh sampel pengujian logam berat terjadi peningkatan kapasitas adsoprsi sampel SBA-15 CPTMS bila dibandingkan dengan SBA-15 murni.

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In the textile industry, production process is widely used water, dyes and chemicals that have an impact on the emergence of textile liquid waste [1]. Examples of hazardous waste components contained in textile liquid waste are heavy metals mainly derived from colouring agents such as cadmium (Cd), lead (Pb), copper (Cu), and zinc (Zn) [1]. Efforts that can be made to prevent the water pollution containing liquid heavy metals is to use silica mesoporous materials such as SBA-15 because it has a large surface area, pore diameter, pore volume and ordered hexagonal structure so that it can be applied as heavy metals adsorbents. In this research, an analysis of the literature review of SBA-15 mesoporous materials synthesis using sol-gel method and CPTMS functionalization has been successfully carried out and continued by analysing its adsorption ability in heavy metals such as cadmium (Cd), copper (Cu), zinc (Zn), and lead (Pb). Typically, synthesizing SBA-15 is carried out using Tetraethyl Orthosilicate (TEOS) as a precursor and Triblock Copolymer Pluronic 123 (P-123) as a surfactant. Then, the results of the SBA-15 product were carried out CPTMS functionalization with the post grafting method. The characterization results show, in the BET calculation compared to pure SBA-15 samples, SBA-15 CPTMS samples decreased pore diameter parameters from 29,203 to 28,521 Å, pore volume from 265,161 to 199,694 cm3/gr and specific surface area from 831,996 to 711,061 m2/gr, in the SAXS test, the SBA-15 CPTMS sample was not significantly different from the SBA-15 while still showing peak plane (100), plane (110) and plane (200), on TEM observations, SBA-15 CPTMS samples remained maintaining its hexagon shape, and in the FTIR test, a chloride group (-Cl) in the 500 cm-1 wave showed a successful CPTMS functionalization. Meanwhile, the results of heavy metal adsorption testing with AAS showed that CPTMS functionalization did not have good selectivity on cadmium (Cd) and zinc (Zn) heavy metals due to a decrease in the percentage of adsorption. However, the adsorption capacity calculation shows that throughout the heavy metal test sample there is an increase in the adsorption capacity of the SBA-15 CPTMS sample when compared to the pure SBA-15.

Abstrak :
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. ...... 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.

Abstrak :
ABSTRAK
Emisi CO2 telah meningkat secara dramatis dalam dekade terakhir yang menyebabkan efek samping pada lingkungan. Konversi CO2 menjadi senyawa kimia lain merupakan tantangan untuk mengurangi efek samping dari masalah ini. Ada beberapa teknik yang dapat mengurangi CO2 di alam seperti teknologi CCU (Carbon Capture and Utilization). Karbon mesopori yang memiliki luas permukaan besar dan ukuran pori dapat digunakan sebagai bahan penyerap CO2 dan bahan pendukung katalis. Ni metal memiliki beberapa keunggulan, seperti memiliki harga murah, aktivitas tinggi, dan berlimpah di alam. Dalam penelitian ini, efek karbon mesopori yang dimodifikasi oleh senyawa etilendiamin dan diimpregnasii dengan nanopartikel Ni (Ni @ EDA MC) sebagai katalis untuk hidrogenasi CO2 menjadi metana. Karbon mesopori yang dimodifikasi dikarakterisasi dengan FTIR, XRD, SEM-EDX, dan BET. Modifikasi proses hidrogenasi juga dilakukan (MC @ EDA) menggunakan ethylenediamine sebelum impregnasi. Dengan menggunakan katalis karbon mesopori yang diimpregnasi, CO2 dapat diserap dan dikonversi secara berurutan ke bahan kimia lainnya seperti metana. Katalis-katalis ini diuji dalam reaktor batch dengan variasi suhu (400, 500, dan 600oC), waktu (30, 60, 90 menit), dan jumlah katalis. Selanjutnya, analisis produk hidrogenasi menggunakan GC-TCD dengan menggunakan kolom porapak Q di bawah tekanan gas CO2 dan H2 masing-masing 1 bar.

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ABSTRACT
The emissions of CO2 have been dramatically increased within the last decade causing the side-effects on the environment. Conversion of CO2 into other chemical compounds is a challenging to reduce the side-effect of these critical issues. There are some techniques that can reduce CO2 in nature such as CCU (Carbon Capture and Utilization) technology. Mesoporous carbon which has a large surface area and pore size can be used as CO2 adsorbent and catalyst support material. Ni metal has several advantages, such as having low prices, high activity, and abundant in nature. In this research, the effect of mesoporous carbon modified by ethylendiamine compound and impregnated with Ni nanoparticles (Ni@ EDA MC) as catalyst for the hydrogenation of CO2 to methane was investigated. Modified mesoporous carbon was characterized by FTIR, XRD, SEM-EDX, and BET. Modification of hydrogenation process was also carried out (MC@ EDA) using ethylenediamine before impregnation. By using impregnated mesoporous carbon catalysts, CO2 can be adsorbed and converted sequentially to other value added chemicals such as methane. These catalysts were tested in the batch reactor with variation of temperature (400, 500, and 600oC), time (30, 60, 90 minutes), and amount of catalyst. Furthermore, the analysis of hydrogenation product was carried out by GC-TCD using porapak Q column under CO2 and H2 gas pressure of 1 bar each.

Abstrak :
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.

Abstrak :

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.

Abstrak :
Konsentrasi CO2 di dalam atmosfer yang terus meningkat menjadi perhatian bagi peneliti untuk mengkonversi CO2 menjadi senyawa yang lebih ramah lingkungan serta bermanfaat. Dalam penelitian ini, dilakukan studi adsorpsi dan reaksi karboksilasi untuk mengkonversi CO2 menggunakan substrat fenilasetilena, katalis heterogen Cu/MC, dan basa Cs2CO3 pada suhu 75˚C. Hasil sintesis karbon mesopori (MC) dikarakterisasi dengan FTIR dan SEMEDX- Mapping. Hasil FTIR MC memperlihatkan proses karbonisasi yang belum sempurna, ditandai dengan adanya peak C-O dan O-H. Namun hasil SEM-EDX-Mapping memperlihat struktur pori yang cukup seragam dengan komposisi unsur C mencapai 86.01% dan unsur O mencapai 13.99%. Hasil sintesis Cu/MC dikarakterisasi dengan FTIR dan SEM-EDX yang menunjukkan bertambahnya gugus C=C terkonjugasi sehingga komposisi C meningkat menjadi 82,34%, sementara komposisi O sekitar 15,34%, dan komposisi Cu sekitar 02,32%. Hasil karboksilasi fenilasetilena dengan CO2 menunjukan terbentuknya produk asam-3-fenil propiolat namun dalam jumlah yang sangat sedikit. Dalam penelitian ini juga diuji sifat adsorpsi fenilasetilena pada Cu/MC dan adsorpsi fenilasetilena pada MC dengan adanya penambahan basa Cs2CO3. Berdasarkan hasil HPLC uji adsorpsi fenilasetilena, diketahui bahwa adsorpsi fenilasetilena pada Cu/MC lebih baik daripada adsorpsi fenilasetilena pada MC. ......Concentration of CO2 in the atmosphere that continues to increase is a concern for researchers to convert CO2 into compounds that are more environmentally friendly and useful. In this research, study of phenylethethylene adsorption and carboxylation reaction were carried out. The carboxylation reaction to convert CO2 required phenylacetylene as substrate, Cu/MC as heterogeneous catalyst, and Cs2CO3 as base (source of nucleophile). The carboxylation reactions were carried out at 75˚C. The results of mesoporous carbon synthesis (MC) were characterized by FTIR and SEM-EDX-Mapping. The FTIR MC results show that the carbonization process is not perfect, characterized by the peak C-O and O-H. But the SEM-EDX-Mapping results show a fairly uniform pore structure with the composition of element C reaching 86.01% and element O reaching 13.99%. The results of Cu/MC synthesis were characterized by FTIR and SEM-EDX which showed an increase in the conjugated C = C group so that the composition of C increased to 82.34%, while the composition of O was around 15.34%, and the composition of Cu was around 02.32%. The carboxylation of phenylacetylene with CO2 showed the formation of acid-3-phenyl propiolic products but in very small amounts. In this study also tested the properties of phenylacetylene adsorption on Cu/MC and phenylacetylene adsorption on MC with the addition of Cs2CO3 base. Based on the results of HPLC phenylacetylene adsorption test, it is known that the adsorption of phenylacetylene in Cu/MC is better than phenylacetylene adsorption on MC.

Abstrak :
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%. ......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%.