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Organic Laboratory III

Faculty of Chemistry, HUS

May 2010

Vietnam National University, HanoiCollege of Sciences

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ContentsContents

Introduction

Experimental

Results

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IntroductionIntroductiony Biodiesel (BDF) show large potential as diesel substitutes due to itssustainable properties and its low emission of GHS.

y BDF is synthesized by transesterification of vegetable and animal oils.

Catalytic transesterification have been applied so farAcid (H2SO4)Alkali (NaOH, KOH) Enzymes

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IntroductionIntroductiony Purposes:

y Produce BDF from fish oil

y Apply co-solvent associated with alkalitransesterification method into BDF production.

y Employ central composite orthogonal design to optimizethe BDF production

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IntroductionIntroductionyOriginality

y Use co-solvent method.

y

Generate the oil-rich one-phase system.y Use central composite orthogonal model to design optimized

experiments

y Simultaneously analysis the effect of factors

y an active experiment has a successive property, or, each next stage

is projected and designed based on results of a previous series oftrials;

y From a mathematical point of view, a classical experiment offerspartial effect, while the active one gives the total effect, for with itall factors are simultaneously varying in the experiment.

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ExperimentalExperimentaly Chemicals

y Potassium hydroxide KOH

y Acetone

y Methanol

y H3PO4

y Equipments:y HPLC (Shimazu)

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Experimental-P

rocedureExperimental-P

rocedure1. Derive a CC matrixy x1: time

y x2:temperature

y

x3: wt% of KOHy x4: molar ratio

MeOH:oil

y y: yeild of reaction

Exp No Exp Name Run Order x1 x2 x3 x4 y

1 N1 13 5 30 0.5 3

2 N2 2 30 30 0.5 3

3 N3 21 5 60 0.5 3

4 N4 8 30 60 0.5 3

5 N5 1 5 30 1.5 3

6 N6 24 30 30 1.5 3

7 N7 23 5 60 1.5 3

8 N8 3 30 60 1.5 3

9 N9 5 5 30 0.5 6

10 N10 19 30 30 0.5 6

11 N11 4 5 60 0.5 6

12 N12 17 30 60 0.5 6

13 N13 9 5 30 1.5 6

14 N14 20 30 30 1.5 6

15 N15 10 5 60 1.5 6

16 N16 26 30 60 1.5 6

17 N17 14 -7.5 45 1 4.5

18 N18 11 42.5 45 1 4.5

19 N19 25 17.5 15 1 4.5

20 N20 12 17.5 75 1 4.5

21 N21 18 17.5 45 0 4.5

22 N22 7 17.5 45 2 4.5

23 N23 6 17.5 45 1 1.5

24 N24 22 17.5 45 1 7.5

25 N25 15 17.5 45 1 4.5

26 N26 16 17.5 45 1 4.5

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Experimental-P

rocedureExperimental-P

rocedure2. Carry out experiments:y weighting a specific amount of fish oil and pour into a 250ml

spherical flask A.

y Pipetting a specific volume of acetone into the oil-containing

spherical flask A under a controlled temperature and a stiringspeed of 400rpm.

y Dissolve a specific weigh of KOH in a flask B containing a specificvolume of methanol.

y Rapidly pour the mixture in the flask B into the flask A.

y Wait for a certain amount of time.

y Take 2-3ml of the product and put into a glass tube containingH2O and 5% H3PO4 solution.

y Analyse the results using HPLC equipment.

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ExperimentalExperimentaly Data Exp No Exp Name Run Order Incl/Excl x1 x2 x3 x4 y1 N1 13 Incl 5 30 0.5 3 42.142 N2 2 Incl 30 30 0.5 3 86.53

3 N3 10 Incl 5 60 0.5 3 87.71

4 N4 25 Incl 30 60 0.5 3 98

5 N5 1 Incl 5 30 1.5 3 82.28

6 N6 12 Incl 30 30 1.5 3 81.79

7 N7 26 Incl 5 60 1.5 3 94.22

8 N8 22 Incl 30 60 1.5 3 98.13

9 N9 5 Incl 5 30 0.5 6 93.22

10 N10 16 Incl 30 30 0.5 6 99.07

11 N11 19 Incl 5 60 0.5 6 96.96

12 N12 6 Incl 30 60 0.5 6 98.54

13 N13 15 Incl 5 30 1.5 6 97.51

14 N14 14 Incl 30 30 1.5 6 100

15 N15 24 Incl 5 60 1.5 6 98.85

16 N16 17 Incl 30 60 1.5 6 100

17 N17 27 Excl -7.5 45 1 4.5

18 N18 4 Incl 42.5 45 1 4.5 99.1

19 N19 21 Incl 17.5 15 1 4.5 9820 N20 18 Incl 17.5 75 1 4.5 99.37

21 N21 9 Incl 17.5 45 0 4.5 55.86

22 N22 20 Incl 17.5 45 2 4.5 99.84

23 N23 23 Incl 17.5 45 1 1.5 83.72

24 N24 11 Incl 17.5 45 1 7.5 99.95

25 N25 3 Incl 17.5 45 1 4.5 98.78

26 N26 8 Incl 17.5 45 1 4.5 98.4

27 N27 7 Incl 17.5 45 1 4.5 98.01

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ResultsResults

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Thanks for your attention!Thanks for your attention!