PILOT PLANT STUDIES ON HYDROFINISHING OF BN SLACK WAX

Studies on Hydrofinishing of Bright Neutral Slack Wax carried out in pilot plant unit, as
there is substantial scope of value addition. Hence studies were conducted in Hydro
treating pilot plant with BN slack wax as feed over Grace wax hydrofinishing Catalyst at
varied operating conditions. The objective of the present work can be summarized as
following

• To optimize the process conditions for BN slack wax hydrofinishing so as to meet

the product quality requirements in line with imported Soft micro wax.

• To study the stability of the catalyst for processing Heavy waxes like BN.

EXPERIMENTAL DETAILS

The hydrofinishing studies were carried out in a high-pressure trickle bed reactor unit
procured from Vinci Technologies, France. The catalyst bed was diluted with small size
carborundum particles in 1:1 volume ratio to ensure uniform gas and liquid distribution
across the catalyst bed and proper wetting of catalyst with reactants.

Feedstock used: Bright Neutral Slack Wax collected from the dewaxing unit was used
for the pilot plant trails. The feedstock characteristics are given in Table 1.

Catalyst: Wax hydrofinishing catalyst collected from wax HyFi unit was used for pilot
plant evaluation. The catalyst is of Co-Mo/Al2O3 type.

Experimental Conditions: The experimental runs were carried out at a constant

pressure of 54 kg/cm2 and H2/HC ratio of 150 lit/lit with the reaction temperature varying
from 270-320oC. The evaluations with above operating conditions were carried out at
two different LHSV of 0.8 and 1.2 h-1. The details of experimental conditions studied are
summarized in Table 2.
Prior to catalyst evaluation in pilot plant reactor, the catalyst sample was dried and
sulfided using diesel spiked with Dimethyl Disulfide (DMDS) as per standard procedure.

The hydrofinished pilot plant products were characterized in detail to study the extent of
color removal, color stability, oil content and other important property of soft micro wax
namely hardness. The typical properties of commercial soft micro wax are presented in
Table 3. The quality of hydrofinished BN Slack Wax at varied operating conditions
namely LHSV of 0.8 and 1.2 h-1 is presented in Table 4 and 5.

Hydro Finishing of BN slack wax after Deoiling

As the Oil content of BN slack is high (about 35%), the deoiling was carried out prior to
Hydrofinishing. The following typical deoiling conditions were used in lab scale deoiling
unit for obtaining waxes for further hydrofinishing.

Feed BN slack wax

Solvent: MIBK
Solvent/ Feed ratio: 5:1
Deoiling Temperature: 150C

The deoiled BN slack was hydrofinished in pilot plant reactor under typical operating
conditions of 2800C, 54 Kg Pressure and 0.8 LHSV.to determine the Wax quality.

The Characteristics of soft wax obtained after Hydrofinishing of Deoiled BN wax was
compared with the characteristics of Soft wax obtained directly from BN slack wax
Hydrofinishing. (See Table 6)

Results and Discussions

 • ASTM color of the product wax reduces only up to 1.5 from a feed color of 5.0
even with enhanced severity of Hydrofinishing.

• With high oil content in Slack wax, the hydrofinished product color still remains in
ASTM colour scale only (above 0.5). The colour of the imported Micro Soft Wax
is in the lower scale of Saybolt measurement.

• The oil content of hydrofinished wax reduces very marginally under varied
operating conditions and remained above 32%.

• The Penetration of Hydrofinished Slack wax is very high and the reduction in oil
content is necessary to reduce it below desired value of 25.

• The changes in Penetration against the oil content in Wax feed for Hydrofinishing
is shown in Fig 3.

• The hydro finished product from deoiled BN wax compares well with the market
quality of Soft Micro wax with respect to Hardness (Penetration) and Colour (See
Table 6)

Conclusions

The BN slack wax not exceeding 5% of oil content is suitable for Hydrofinishing to
produce soft micro wax with Penetration less than 25 and Saybolt colour of +23
minimum.

The activity of the present catalyst is stable for processing heavier waxes like Bright
Neutral grade.
 Table 1. Characteristics of BN Slack Wax Feed

Characteristics Value
Density @ 15oC, gm/cc 0.8760
Viscosity @ 100oC, cSt 21.03
Melting point, oC 73.6
Congealing point, oC 73.0
RI @ 75oC 1.4677
ASTM Color 5.0
Color Stability, 100 oC, 24 Hrs 6.5
Asphaltenes ppm 280
Oil Content, wt.% 35.3
Penetration @ 25 oC, 1/10 mm 110
Simulated Distillation, % Off Temperature, oC
IBP 434
5 515
10 529
20 546
30 560
40 572
50 585
60 597
70 612
80 628
90 650
95 666
FBP 694

Table 2. Experimental Conditions used in Pilot Plant Unit

Condition Value
o
Temperature, C 270, 280, 290, 300, 310, 320
Operating pressure, kg/cm2 54
LHSV, h-1 0.8, 1.2
H2/HC ratio, lit/lit 150
 Table 3. Typical properties of Soft Micro Wax

Test Description Method Min. Max. Typical

Results

-
Viscosity, SUS @ 210 F D 2161 90 112.5

Gravity, API, 60F D 4052 - - 30.7

Pounds per Gallon # D 1250 - - 7.263

60F
Flash, COC, C (F) D 92 282(540) - 307(585)

Color (Saybolt) D 156 23 - 25

Melting point, F D127 137 - 154.5

Oil Content, % D 721 - - 7.2

Needle Penetration @ D 1321 - 15 >15

77 Deg F
Total Extractables, wt% D 3235 10 30 22.3
 Table 4. Characteristics of Hydrofinished BN Slack Wax

LHSV – 0.8 h-1 Pressure – 54 kg/cm2

H2/HC ratio – 150 lit/lit

Characteristics Value
o o o
270 C 280 C 290 C 300 oC 310 oC 320 oC

Density @ 15oC, gm/cc 0.8755 0.8746 0.8737 0.8733 0.8720 0.8716

Viscosity @ 100oC, cSt 20.19 19.87 19.81 19.53 19.45 19.32

Melting point, oC 75.1 75.5 75.7 76.0 76.1 76.3

Congealing point, oC 74.5 74.5 75.0 75.0 75.0 75.5

RI @ 75oC 1.4661 1.4659 1.4657 1.4655 1.4651 1.4645

ASTM Color* < 2.0 < 2.0 < 2.0 1.5 1.5 1.5

Color Stability, 100 oC, 3.5 3.5 3.0 2.5 2.0 2.0
24 Hrs
Asphaltenes <100 <100 <100 <100 <100 <100

Oil Content, wt.% 34.9 34.2 33.8 33.1 32.9 32.7

Penetration@25oC, 1/10 107 106 107 107 105 105

mm
Simulated Distillation, %
Off
10 505 528 529 521 523 527

30 554 561 562 558 563 559

50 584 588 581 586 578 580

70 617 619 620 616 623 614

90 658 661 655 657 653 659

95 674 679 678 674 683 671

* Saybolt colour exceeds the measurement range and hence only ASTM Color is
reported.
 Table 5. Characteristics of Hydrofinished BN Slack Wax

LHSV – 1.2 h-1 Pressure – 54 kg/cm2

H2/HC ratio – 150 lit/lit

Characteristics Value
o o o
270 C 280 C 290 C 300 oC 310 oC 320 oC

Density @ 15oC, gm/cc 0.8748 0.8739 0.8736 0.8735 0.8729 0.8728

Viscosity @ 100oC, cSt 20.27 19.96 19.92 19.88 19.76 19.74

Melting point, oC 74.6 73.4 73.5 73.6 73.7 73.7

Congealing point, oC 74.0 73.2 73.0 73.1 73.2 73.3

RI @ 75oC 1.4672 1.4660 1.4655 1.4651 1.4650 1.4647

ASTM Color* 2.5 2.0 2.0 2.0 1.5 1.5

Color Stability, 100 oC, 3.0 3.5 3.0 2.5 2.0 2.0
24 Hrs
Asphaltenes <100 <100 <100 <100 <100 <100

Oil Content, wt.% 34.4 34.6 33.8 34 33.7 33.1

Penetration@25oC, 1/10 106 102 104 103 101 101

mm
Simulated Distillation, %
Off
10 521 518 519 523 517 517

30 563 567 566 565 558 566

50 589 594 592 589 586 590

70 621 630 627 624 628 624

90 657 665 659 666 665 663

95 677 683 679 684 687 685

* Saybolt colour exceeds the measurement range and hence only ASTM Color is
reported.
 Table 6. Effect of hydrofinishing on the quality of deoiled BN Slack Wax

Conditions Temp : 280oC Pressure : 54 kg

LHSV : 0.8 /h H2/Oil :150

Property Deoiled Feed Hydrofinished Direct

product from Hydrofinishing
deoiled wax of Slack wax
Density @ 15oC, gm/cc 0.8722 0.8711 0.8746

Viscosity @ 100oC, cSt 17.55 16.89 19.87

Melting point, oC 78.5 79.0 75.5

Congealing point, oC 78.0 78.4 74.5

RI @ 75oC 1.4665 1.4559 1.4659

ASTM Color <0.5 - <2.0

Asphaltenes <100 <100 <100

Color (Saybolt) - 27 -

Oil Content, wt.% 4.37 4.22 34.2

Penetration @ 77 Deg F 24 23 106

UV absorption

280-289 nm 0.61 0.065 -

290-299 nm 0.35 0.041 -

300-359 nm 0.29 0.027 -

360-400 nm 0.11 0.003 -