Sintesis Material Mesopori Silika dari Tetraetilortosilikat (TEOS) Menggunakan Natrium Risinoleat sebagai Template dan 3-aminopropiltrimetoksisilana (APMS) sebagai Co- Structure Directing Agent (CSDA)

Abstract

Synthesis of mesoporous silica materials has been carried out by using tetraethylorthosilicate silica (TEOS) as a silica source, sodium risinoleic as a template and a 3-aminopropyltriethoxysilane (APMS) as co-structure directing agents (CDSA). Interaction between sodium risinoleic, APMS and TEOS determines the characteristic of mesoporous silica materials. Synthesis of silica material was conducted by variation in the addition of 0.1 M HCl, TEOS addition time, addition of methanol, standing time and heating process. XRD difractogram silica material products in all cases the reaction has broaden diffraction peaks indicating amorphous material. FT-IR spectrum shows the Si-OH and Si-O-Si groups which are characteristic of the silica material. SEM and TEM image showed difference in particle size. The addition of 2 ml of HCl has the texture particles fused to form dense surface, 30 ml of HCl particles spherical dispersed and have pores, 35 ml of HCl particles spherical homogeneous forming a compact surface, 40 ml of HCl produces a mixture of particles in the form of dispersed and aggregated of spherical particles and other particles in a sheet form, 50 ml of HCl has irregular shape and size. Analysis of adsorption desorption isother (BET) shows different type of adsorption isotherm and pore size distribution that support the results of the SEM and TEM. Adsorption desorption isotherm addition of 2 ml of HCl has Type II adsorption and pore size distribution is irregular, the addition of HCl 30 ml, 35 ml, 40 ml and 50 ml has hysterisis loop Type IV characteristic og mesoporous material. shows the adsorption process occurs only in the surface layer and has irregular pore size; the addition of 30 ml, 35 ml, 40 ml of HCl show Type IV too but have a regular pore size; while the addition of 50 ml of HCl shows Type IV for mesoporous but with irregular pore size. Pore size distribution dominant in the addition of 30 ml (3.4 nm), 35 ml (3.4 nm and 3.8 nm) and 40 ml (2.2 and 3.8 nm) except for the addition of 50 ml of HCl pore size distribution is not regular. Synthesis of silica material by adding methanol without HCl and heated at C°60 for 24 hours obtained spherical particles were uniformly dispersed and adsorption desorption isotherm Type IV and dominant pore size at 3.4 nm. Extra time delay for 20 minutes TEOS obtained spherical particles of uniform and dominant pore size at 3.1 nm. The addition of methanol and HCl and allowed to stand for 2 hours obtained homogeneous spherical particle and pore size at 3.07 nm, whereas without the addition of HCl dominant pore size at 2.45 nm.

Telah dilakukan sintesis material mesopori silika dari tetraetilortosilikat (TEOS) sebagai sumber silika menggunakan natrium risinoleat sebagai template dan 3-aminopropiltrimetoksisilana (APMS) sebagai co-structure directing agents (CDSA). Sintesis material silika dibuat dengan variasi penambahan HCl 0,1 M, variasi waktu penambahan TEOS, penambahan metanol, waktu pendiaman dan pemanasan. Interaksi natrium risinoleat, APMS dan TEOS menentukan karakter material mesopori silika. Analisis XRD produk pada semua kondisi reaksi memiliki puncak difraksi yang melebar mengindikasikan material bersifat amorf. Spektrum FT-IR memiliki gugus Si-OH dan Si-O-Si merupakan karakteristik material silika. Foto SEM dan TEM menunjukkan ada perbedaan ukuran partikel. Penambahan 2 ml HCl memiliki tekstur partikel saling menyatu membentuk permukaan yang rapat, 30 ml HCl partikel spherikal terdispersi dan ada lubang pori, 35 ml HCl partikel spherikal homogen membentuk permukaan rapat, 40 ml HCl campuran partikel spherikal terdispersi dan aggregat dan berupa lembaran dan 50 ml HCl memiliki bentuk dan ukuran tidak sama. Analisis adsorpsi desorpsi isotherm (BET) menunjukkan perbedaan tipe adsorpsi isotherm dan distribusi ukuran pori mendukung hasil SEM dan TEM. Adsorpsi desorpsi isotherm penambahan 2 ml HCl memiliki adsorpsi isotherm Tipe II dan distribusi ukuran pori tidak teratur, penambahan HCl 30 ml, 35 ml, 40 ml dan 50 ml memiliki hysteresis loop Tipe IV karakteristik material mesopori. Distribusi ukuran pori dominan pada penambahan 30 ml (3,4 nm), 35 ml (3,4 nm dan 3,8 nm) dan 40 ml (2,2 dan 3,8 nm) kecuali penambahan 50 ml HCl distribusi ukuran pori tidak teratur. Sintesis material silika dengan menambah metanol tanpa HCl dan dipanaskan pada 60°C selama 24 jam diperoleh partikel sperikal terdispersi yang seragam dan adsorpsi desorpsi isotherm Tipe IV dan ukuran pori dominan 3,4 nm. Penundaan waktu penambahan TEOS selama 20 menit diperoleh partikel sperikal seragam dan ukuran pori dominan 3,1 nm. Penambahan metanol dan HCl dan didiamkan selama 2 jam diperoleh partikel sperikal homogen dan ukuran pori dominan 3,07 nm, sedangkan tanpa penambahan HCl ukuran pori dominan 2,45 nm.