PREPARATION OF MODIFIED MCM-41 PELLET FOR SIMULATION IODINE RADIOACTIVE WASTE ADSORPTION

Fajri Liestyan Rozaq S. 010700177

Background
Nuclear industry Radioactive waste (iodine-131)
Effort / attempt to maintain environmental quality

MCM-41 modified

Modified with amines

MCM-41

Modified MCM-41 pellet

Radioactive waste adsorption

Authenticity Research

Research on the MCM-41 as an adsorption material :

Chung-Kung Lee, et al.2007. Ze:Taiwan .

Application of MCM-41 for Dyes Removal from Waste Water . Yuan-

Previous studies, MCM-41 used for the absorption of the dyes, whereas, in this study MCM-41 is used to simulated radioactive waste (iodine) adsorption.

Problem Formulation

Formulation of the problem in this study were :

Can the MCM-41 be modified with amine groups by impregnation ? How is the process of making pellets of modified MCM-41? how the characters simulated radioactive waste adsorption (iodine) by the pellet of modified MCM-41?

Limitations

Limitations on this reseacrh were:

The main materials used in the process is MCM-41 and Amine groups (Diethylamine)
Waste sample used was simulated radioactive waste (iodine) solution of I 2 which dissolved in KI Characterization is carried out adsorption tests, and test with FTIR and XRD on modified MCM-41

The addition of diethylamine used is 1 mL, 2 mL, 3 mL, and 4 mL

Reflux time used is 4 hours, 6 hours, and 8 hours

Research Objective

The purpose of this study is :

Creating amine modified MCM-41 by impregnation. Making pellets from MCM-41 was modified amine. Knowing the character of adsorption of radioactive waste simulation (iodine) by the amine-modified MCM-41.

Benefits of Research

The benefits of this research were :

Amine-modified MCM-41 can be used as the adsorption of radioactive waste. With this research would be obtained information about the variables that affect the manufacture of pellets MCM-41 modified.

Theory

Waste processing industry has been a lot done in several ways, including using chemical coagulants, physically by adsorption using activated charcoal, and biologically using microbial. Many methods have been developed to solve the problem of waste in the waters, one of which is the method of adsorption. This method is one potential method, as the process was simple, it can work at low concentrations, can be recycled, and the cost required is relatively inexpensive.

Adsorption

Adsorption is a process that occurs when a fluid, liquid or gas, bonded to a solid or liquid substance (adsorbent) and finally form a thin layer or film (adsorp substance, the adsorbate) on the surface. In contrast to the absorption which is the absorption of fluid by another fluid by forming a solution.

Physisorption

Physisorption, also called physical adsorption, is a process in which the electronic structure of the atom or molecule is barely perturbed upon adsorption.

Chemisorption

Chemisorption is a sub-class of adsorption, driven by a chemical reaction occurring at the exposed surface. A new chemical species is generated at the adsorbant surface (e.g. corrosion, metallic oxidation). The strong interaction between the adsorbate and the subtrate surface creates new types of electronic bonds ionic or covalent, depending on the reactive chemical species involved

MCM-41

MCM-41 is mesoporous silica material, have hexagonal shaped and a pore diameter about 15-100 angstroms. Silica is a major component of MCM-41 MCM-41 has been used for chemical and environmental application as adsorbents, catalysts, ion exchange materials and nanofiller.

MCM 41 can be made from rice husk ash.

Diethylamine

Diethylamine is a secondary amine with CH 3 CH 2 NHCH 2 structure. Diethylamine in the form of a flammable liquid and is highly acidic. Diethylamine is soluble in water and ethanol. Diethylamine is a colorless liquid, and sometimes artifacts brown color because of impurities. Dietilamina can be made from ethanol and ammonia, and obtained simultaneously with ethylamine and triethylamine. Diethylamine is often used as a corrosion inhibitor in the production of rubber, resins, dyes and medicines. Dietilamina have a corrosive nature, when in contact with skin can cause irritation or burns.

Impregnation

According to artikata.com impregnation is saturation or compliance with the gas or liquid. According to the free dictionary by farlex impregnation is the process of totally saturating something with a substance; like "the impregnation of wood with preservative"; "the saturation of cotton with ether"

Modified MCM-41

MCM-41 modified with amine for covalent bonds amines (cationic) is needed to adsorps the iodine (anionic) ,

Pelletizing

Pelletizing is the process of compressing or molding the material into shaped pellets. Pellets of different materials including chemicals, iron ore, animal feed compounds, and more. In nuclear technology pelletizing usually done on pellet manufacture nuclear fuel for nuclear reactors. However pelletizing not only for fuel, most often we encounter the pellets to feed fish and so forth.

Hypothesis

Expected to know how to modify the MCM-41 with amines by impregnation. Expected to know how to make pellets of amine-modified MCM-41. expected pellets amines-modified MCM-41 can be used in adsorption of simulation radioactive waste (iodine).

Tools and Materials

Tools

Materials

Reflux tools Analytic balance Volume pipette Burette compacting tool

MCM-41 Amine groups ( diethylamine ) Potassium Iodide (KI) Iodine (I 2 ) Aquadest

FTIR
XRD

Ammonium Chloride (NH 4 Cl)

Hydrochloric acid (HCl)

working diagram
MCM 41 Dietilamin Impregnansi (reflux) 70oC Diethylamine variation

Characterized by FTIR and XRD

MCM-41 modified

Pelletizing

Adsorption test

Analyzed with UV-VIS

Result and Discussion

Determination of the addition of diethylamine and time of reflux

Effect of variations in the addition of diethylamine (DEA) and reflux time on adsorption efficiency

Volume of DEA

4 hours reflux (%)

6 hours reflux (%)

8 hours reflux (%)

1 mL 2 mL 3 mL

83,48 83,46 86,56

87.4 92,17 93

74,3 75,37 75,37

4 mL

88,24

90,4

77,13

95 93 90 87.4 92.17 90.4 88.24

efisiensi (%)

85

86.56 83.46
83.48 reflux 4 jam reflux 6 jam reflux 8 jam 77.13

80

75 74.3 70 0 0.5 1 1.5

75.37 75.37

2 2.5 Diethilamin (mL)

3.5

4.5

The best time for reflux is 6 hours

adsorption efficiency increased from 4 hours to 6 hours, but fell at reflux 8 hours because the amine group attached to the MCM-41 were partially destroyed

the more the addition of diethylamine then the efficiency of adsorption of MCM-41 modified is greater. This is because the amine group attached to the MCM-41 more. Amine groups (cations) serves to bind Cl-(anion)

Pelletizing of modified MCM -41

Adsorption material used is formed into pellets, because adsorption treatment using pellet easier. In addition, the handling process of desorption in the form of pellets is easier than in powder form. During the MCM-41 still in the form of powder, powder puff in the air more easily, so easily scattered. Pelletizing procedure

To apply the adsorbent of the present invention to such as cyclic adsorption process, it must be formed into a stable, mechanically strong form.
In the case of pellet form, the adsorbent is mixed with a suitable inert or active secondary material as a binder

I2 adsorption results with pellets of modified MCM-41

1 hour adsorption
Volume of DEA 3 mL 4 mL Co (ppm) Ca (ppm) Efficiency (%) 73.79 74.92 Adsorption capacity (ppm/g) 58.52 58.67

50 50

13.09 12.53

24 hours adsorption
Volume of DEA 3 mL 4 mL Co (ppm) Ca (ppm) Efficiency (%) 75,53 76,32 Adsorptio n capacity (ppm/g) 62,02 61,58

50 50

12.23 11.83

known that the concentration of I 2 simulated waste has decreased from 50 ppm to about 12 ppm. This indicates that I 2 has adsorp on MCM-41 amine-modified pellet. This is consistent with the initial hypothesis that the pellets are expected amine modified MCM-41 can be used in the simulation of adsorption of radioactive waste in the form of iodine. Also that the adsorption efficiency and adsorption capacity for 1 hour and 24 hours is not too much difference. This indicates that the process of adsorption of MCM-41 pellet fast enough. Within an hour, 70% I 2 has adsorp into MCM-41 modified. After 24 hours, no change in the percentage of adsorp I 2 significantly.

ch a r a c t erization o f mo d i fied M C M - 41 FTI R r e su lt o f M o d ified M C M -4 1

can be seen that the amine group has grafted on MCM41. Amine groups from both FTIR results at a frequency of 1640 cm-1. Amine group on the addition of 4 mL diethylamine (picture below) has a transmittance of 24.08%, while the addition of 3 ml diethylamine (picture above) has a transmittance of 25.27%. If the % transmittance smaller, the greater of absorbance. Absorbance indicates the number of diethylamine is added to the MCM-41. Group Si-O-Si can be shown in the frequency of 463 cm-1 and 1086 cm-1. Group Si-O-Si is a functional group typical of MCM-41.

X R D r e su l t o f M C M - 41 a n d mo d i fied M C M - 41

characterization by XRD is used only to prove the presence of structural changes between the MCM41 are not modified with amine-modified MCM-41. Based on the Figure, it can be seen very clearly the difference between the XRD results of MCM-41 with amine-modified MCM-41. If the results of XRD diffraction patterns of MCM41 with amine-modified MCM-41 compared, it is clear that the grafting amine (modification) on MCM-41 greatly affects the crystal structure of MCM-41, as indicated by the changed of the graph.

Conclusion and advice

Conclusion :

MCM-41 can be modified with amine groups by impregnation with best DEA addition were 3 mL and 4 mL The process of making pellets amine-modified MCM-41 can be done

It has been tested that modified MCM-41 pellet can adsorb iodine in simulated radioactive waste about 50ppm/g till 60 ppm/g

Advice :

For further research, should do a more detailed variation on the addition diethilamin on MCM-41 modification.

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