EXPERIMENT 4: DISTILLATION TITLE: Continuous Distillation Column ABTRACT The main purpose of this experiment is to separate two components

of a miscible liquidliquid mixture by using a distillation column. The method used in the experiment is fractional distillation or distillation with refux using the continuous distillation column. Digital refractometer is used to measure the brix degree in percentage of the product collected from various product streams. Then the refractive index can be obtained from the brix and refractive index table of ethanol. After that, from the refractive index we can found the concentration through the refractive index vs. concentration graph. From the results, we can notice that at the product stream V3, the concentration of ethanol increase over time whereas for the product stream V2, the concentration of ethanol decreases over time. As a conclusion, the two miscible liquid which is ethanol and water is separated after the distillation process.

OBJECTIVE To separate two components of a miscible liquid-liquid mixture by using a distillation column.

INTRODUCTION Continuous distillation is a process used in industry to separate chemical compounds. It works using the principles of distillation which separating mixtures of liquids into their individual components based on differences in volatility or boiling point of components in a boiling liquid mixture, but is particularly useful in dealing with large volumes of industrial chemicals by allowing distillation to happen without interruption. Continuous distillation feed a mixture of 2 substances in 1 feed stream is separated into 2 product streams, distillate (top product) and bottoms (residue). The more volatile

component will vaporize first and is removed in the distillate stream and the less volatile component will remain in the bottoms stream. The bottoms stream is in liquid phase, while the distillate stream is produced by condensing the vapour phase. A modern approach to continuous distillation uses cylindrical columnstills manufactured in stainless steel. Distillation columns are made of several trays where each tray is a level of the column where descending liquid meets the ascending vapours. There is two separate areas in the column which are stripping column and enrichment column. The stripping section is located at the lower part of the distillation column or below the feed point whereas the enrichment section is located at the upper part of the distillation column or above the feed point. The stripping section is also known as the rectifying section. Continuous distillation uses this principle to separate and purify industrial chemicals. A column, or tower, is filled with feed, the mixture to be purified. The mixture is then heated. When a mixture of chemicals is boiled, the substances with the lowest boiling points will undergo a change of state from liquid to gas and rise as vapor. As they rise, however, they also cool because the vapor will passed through a device known as a condenser, which consists of a sealed tube surrounded by a hollow area filled with coolant. As the vapor is cooled, it condenses back from a gas into a liquid and runs down the tube into a container. This progressively purifies the mixture and allows for more specific and controlled separation of the various compounds. The chemical vapors are run through separate condensers and into receiving vessels. The desired substance can be separated out from a liquid mixture using this process by controlling the temperature of the boiler.

A:

Vapour

injection

B: Vinasses extraction C: D: Reflux injection. E: Vapour extraction Feed point

F: Heat exchange device which cools extracted vapours [E] and heats then incoming feed[C] and reflux[D]. Stripping area is situated between B and C,

Enrichment area is situated between C and E.

Figure 1: Diagram of continuous distillation columns EQUIPMENTS AND MATERIALS 1. Distillation column 2. Refractometer 3. Beaker 4. Ethanol-Water Mixture

EXPERIMENTAL PROCEDURES 1. A mixture of ethanol and water were made and the refractive index of the initial mixture was recorded. 2. The mixture is boiled in the reboiler section of the distillation column. 3. A sample was collected from product stream (V3)and 4. The refractive index was recorded. 5. The concentration was recorded. 6. A sample was collected from bottom stream (V2) and 7. The refractive index was recorded.

8. The concentration was recorded. 9. All ethanol was determined whether had been distilled off.

RESULTS Time taken for the distillation process = 15 minutes (complete in 5 times) Refrative index of mixture (initial) = 4.1 % = 1.3361 nD Refractive index of product (ethanol) collected = 16.3% = 1.3442nD Refractive index of mixture in the reboiler at the end of the experiment= 3.9% = 1.3353 nD Table 1: Brix and refractive index of ethanol conversion chart % (w/w) 0.50 1.00 2.00 3.00 4.00 5.00 6.00 7.00 8.00 9.00 10.00 12.00 Ethanol 1.3333 1.3336 1.3342 1.3348 1.3354 1.3360 1.3367 1.3374 1.3381 1.3388 1.3395 1.3410

14.00 16.00 18.00 20.00 24.00 28.00 32.00 36.00 40.00 44.00 48.00 52.00 56.00 60.00 64.00 68.00 72.00 76.00 80.00 84.00 88.00 92.00 96.00 100.00 (Retrived

1.3425 1.3440 1.3455 1.3469 1.3498 1.3524 1.3546 1.3566 1.3583 1.3598 1.3610 1.3621 1.3630 1.3638 1.3644 1.3650 1.3654 1.3657 1.3658 1.3656 1.3653 1.3646 1.3636 1.3614 from

http://faculty.weber.edu/ewalker/Chem2990/Chem%202990%20Refractive%20Index%2 0Readings.pdf)

The refractive index is calculated by using the brix and refractive index of ethanol conversion table through interpolation: For refrative index of mixture (initial): = x=1.3361 nD For refractive index of product (ethanol) collected: = X= 1.3442 nD For refractive index of mixture in the reboiler at the end of the experiment: = X=1.3353 nD

Table 2: Refractive index for product stream V3 Time (min) 3.00 6.00 9.00 12.00 15.00 Brix (%) 16.8 17.1 17.7 17.9 18.1 Refractive index (nD) 1.3446 1.3448 1.3453 1.3454 1.3456

Calculation for the refractive index of product stream V3 For 3 min, = X= 1.3456 nD For 6 min, = X= 1.3454 nD For 9 min, = X= 1.3453 nD For 12 min, = X= 1.3448 nD For 15 min, = X= 1.3446 nD

Table 3: Refractive index for product stream V2 Time (min) 3.00 6.00 9.00 12.00 15.00 Brix (%) 4.4 3.9 3.6 3.1 2.7 Refractive index (nD) 1.3356 1.3353 1.3352 1.3349 1.3346

Calculation for the refractive index of product stream V2 For 3 min, = X= 1.3356 nD For 6 min, = X= 1.3353 nD For 9 min, = X= 1.3352 nD For 12 min, = X= 1.3349 nD

For 15 min, = X= 1.3346 nD

Table 4: Concentration and refractive index of ethanol conversion table Ethanol

Concentration vs. refractive index (20C) % by wt. 0.00 0.50 1.00 1.50 2.00 2.50 3.00 3.50 4.00 4.50 5.00 5.50 6.00 6.60 7.00 7.50 8.00 8.50 9.00 nD 1.3330 1.3333 1.3336 1.3339 1.3342 1.3345 1.3348 1.3351 1.3354 1.3357 1.3360 1.3364 1.3367 1.3370 1.3374 1.3377 1.3381 1.3384 1.3388

9.50 10.00 11.00 12.00 13.00 14.00 15.00 16.00 17.00 18.00 19.00 20.00 22.00 24.00 26.00 28.00 30.00 32.00 34.00 36.00 38.00 40.00 42.00 44.00 46.00 48.00 50.00 52.00 54.00 56.00

1.3392 1.3395 1.3403 1.3410 1.3417 1.3425 1.3432 1.3440 1.3447 1.3455 1.3462 1.3469 1.3484 1.3498 1.3511 1.3524 1.3535 1.3546 1.3557 1.3566 1.3575 1.3583 1.3590 1.3598 1.3604 1.3610 1.3616 1.3621 1.3626 1.3630

58.00 60.00 62.00 64.00 66.00 68.00 70.00 72.00 74.00 76.00 78.00 80.00 82.00 84.00 86.00 88.00 90.00 92.00 94.00 96.00 98.00 100.00

1.3634 1.3638 1.3641 1.3644 1.3647 1.3650 1.3652 1.3654 1.3655 1.3657 1.3657 1.3658 1.3657 1.3656 1.3655 1.3653 1.3650 1.3646 1.3642 1.3636 1.3630 1.3614

Sensitivity: % Retrieved

0.0650 from

http://us.mt.com/us/en/home/supportive_content/application_editorials/Ethanol_re_e.htm l

Refractive index (nD) against concentration of ethanol (w/w%) graph

1.3700

Refractive index (nD)

1.3600 1.3500 1.3400 1.3300 1.3200 1.3100 0.00 1.50 3.00 4.50 6.00 7.50 9.00

17.00

92.00

11.00

14.00

20.00

26.00

32.00

38.00

44.00

50.00

56.00

62.00

68.00

74.00

80.00

86.00

Concentration of ethanol (w/w%)

Figure 2: Graph of refractive index of ethanol vs. concentration of ethanol

From the table or conversion chart of refractive index of ethanol vs. concentration of ethanol, Table 5: Concentration of product stream V3 Time (min) 3.00 6.00 9.00 12.00 15.00 Refractive index (nD) 1.3446 1.3448 1.3453 1.3454 1.3456 Concentration (w/w %) 16.86 17.13 17.75 17.88 18.14

98.00

Table 6: Concentration of product stream V Time (min) 3.00 6.00 9.00 12.00 15.00 Refractive index (nD) 1.3356 1.3353 1.3352 1.3349 1.3346 Concentration (w/w %) 4.33 3.83 3.67 3.17 2.67

Refractive index against concentration graph

1.3458 1.3456

Refractive index (nD)

1.3454 1.3452 1.345 1.3448 1.3446 1.3444 1.3442 1.344 16.86 17.13 17.75 17.88 18.14

Concentration (w/w %)

Figure 3: Graph of refractive index vs. concentration graph for product stream V3

Refractive index against concentration graph

1.3358

Refractive index (nD)

1.3356 1.3354 1.3352 1.335 1.3348 1.3346 1.3344 1.3342 1.334 4.33 3.83 3.67 3.17 2.67

Concentration (w/w %)

Figure 4: Graph of refractive index vs. concentration graph for product stream V2