CHAPTER 4

RESULT AND DISCUSSION

4.1 CARACTERIZATION OF CATALYST

Table 4.1 shows the metal composition of spent catalyst.

Table 4.1 Metal composition of spent catalyst

Elements Atomic Extrudate Powder

(wt) (wt)
C 20.48 11.24 13.00
O 51.64 37.74 43.45
Al 14.57 17.96 15.35
Si 6.09 7.81 5.91
S 4.21 6.17 5.17
Ni 1.08 2.90 2.45
W 1.93 16.18 14.67

4.2 PRETREATMENT FOR CATALYST

De-oiling: Acetone wash was given to catalyst for oil removal. 50gm of catalyst was washed with
80ml acetone and dried in room temperature. From the de-oiling oil and soft coke is removed from
the catalyst surface.

Crushing and Screening: Extrudates of catalyst were taken in motor pestal for crushing. After
crushing, it was passed through the sieve with mesh no 40 (420 m) to get uniform particle size.
Figure 4.1 shows the powder form of catalyst.

Fig. 4.1: Powder form of spent catalyst

Decoking: Muffle furnace was used for the decoking (removal of SO2 and CO2) of catalyst
powder. The temperature in the furnace was maintained at 600 C then sample was taken in
ceramic crucible and placed into the furnace for 5hr.

These are two TGA (Thermo gravimetric analysis) curves. These curves show the weight loss with
temperature. (Figure 4.2)

Extrudate catalyst Powder catalyst

Fig. 4.2: TGA Curves

During the decoking carbon and sulphur content were removed, so that weight of catalyst was
decreases with time. Table 4.2 shows the weight loss of catalyst (extrudate and powder form)
during the different temperature for 3hr and 5hr.Table 4.2 shows the weight loss of extrudate and
powder form of catalyst when the temperature range 500C to 800C.

Table 4.2: Weight losses during decoking

Temperature(C) Time Extrudate Powder

500 0.831 0.795
600 3hr 0.824 0.750
800 0.742 0.709
500 0.773 0.825
600 5hr 0.756 0.855
800 0.742 0.839
Table: 4.3 shows the metal composition after decoking.
Table 4.3: Metal composition after decoking

Elements Atomic (Extrudate) Powder

(wt) (wt)
C 20.48 3.80 10.56
O 51.64 47.01 44.95
Al 14.57 20.19 19.66
Si 6.09 8.41 6.24
S 4.21 0.78 0
Ni 1.08 2.71 3.16
W 1.93 17.09 11.71
Figure 4.3 shows the decoking of extrudate and powder form of catalyst at 600 C.

Extrudate (600 C) Powder (600 C)

Fig. 4.3: Decoking

4.3 METAL RECOVERY PROCESSES

There are two paths for metal recovery

Metal recovery without fusion

Metal recovery with fusion

4.3.1 METAL RECOVERY WITHOUT FUSION

In leaching process take 1gm catalyst powder was contacted 100ml acid solution (10%
concentration) of HCl, H2SO4 and HNO3. Leaching experiments were conducted in a 250 ml flask
fitted with a seal to avoid evaporation loss. The contents were stirred with a magnetic stirrer at 30
C. Take samples regular time interval for to determine concentration of metals in leachate with
time for 4 hr.
The different acidic leaching is shows below. (Figure 4.4)

HCl Leachate H2SO4 Leachate HNO3 Leachate

Fig. 4.4: Acidic leachate

In leaching process. After the leaching process leachate and insoluble residue were separated. The
insoluble from the 1st stage of leaching dried and weight and again contacted with fresh acid
solution for the 2nd leaching process. Table 4.4 shows the concentration of W, Si and Al in HCl,
H2SO4 and HNO3 in 1st stage leaching.

Table 4.4 Metal concentration in acidic leachate (1st stage)

Acids W Si Al Ni
(ppm) (ppm) (ppm) (ppm)
HCl 68.04 10.69 627.24 23.70
H2SO4 210.84 9.49 365.59 64
HNO3 385.37 10.71 429.49 42
Figure 4.5 shows the metal concentration of W, Si and Al in various acids in leachate.
Metal composition in leachate(1st stage)
HCl H2SO4 HNO3
627.235

429.488
385.373 365.585
210.837
68.043 64 23.7 42
10.6899.48810.706

W Si Al Ni
 Fig. 4.5: Metal composition in acidic leachate (1st stage)

Table 4.5 shows the weight of insoluble residue in different acids after 1st stage leaching.
Table 4.5 Insoluble residue of acidic leaching (1st stage)

Acids Insoluble Residue (gm)

HCl 0.447
H2SO4 0.524
HNO3 0.679

Table 4.6 shows the concentration of W, Si and Al in acids during the 2nd stage leaching.
Table 4.6 Metal composition in acidic leaching (2nd stage)

Acids W Si Al
(ppm) (ppm) (ppm)
HCl 3 6 105
H2SO4 11 10 510.6
HNO3 22 14 187.59

Figure 4.6 shows the metal concentration in acidic leachate in 2nd stage.

Metal concentration in leachate (2nd stage)

HCL H2SO4 HNO3

510.6

187.59
105
3 11 22 6 10 14

W Si Al

Fig. 4.6: Metal concentration in leachate (2nd stage)

Table 4.7 shows the weight of insoluble residue after 2nd stage leaching.

Table 4.1 Insoluble residue of acidic leaching (2nd stage)

Acids Insoluble Residue (gm)

HCl 0.150
H2SO4 0.336
HNO3 0.573

Figure 4.7 shows the weight of insoluble residue after the 1st and 2nd stage acidic leaching.
Insoluble Residue

0.8
0.679
0.7
0.573 HCl
0.6 0.524
0.5 0.447
0.4 0.336 H2SO4
0.3
0.2 0.15
HNO3
0.1
0
1st stage 2nd stage

Fig. 4.7: Insoluble residue of acidic leaching

Figure 4.8 shows the insoluble residue of HCl, H2SO4 and HNO3 after acidic leaching.
 HCl Residue H2SO4 Residue HNO3 Residue

Fig. 4.1: Insoluble residue

4.3.2 METAL RECOVERY WITH FUSION

Na2CO3 FUSION

Catalyst powder was fusion with Na2CO3 the ratio of catalyst to Na2CO3 was 1:1.35 at 750 C
for 4hrs in the crucible. The fusion was occur only on surface. When the mixture was taken in the
ceramic boat, it was fused and forms hard solid. The mixture was fused on boat surface because
of silica which is present in it. (Figure 0.9)
 Fig. 4.2: Fusion with Na2CO3

NaOH FUSION

The mass ratio of NaOH to catalyst powder was taken as 1.83:1. The mixture was placed in a
ceramic boat and heated in a furnace at 650 C (under access of air) for 2-4 h in muffle furnace.

Figure 4.10 shows the fused powder of catalyst.

Fig. 4.3: Fusion with NaOH

Leaching experiments were conducted in a 250 m flask fitted with a seal to avoid evaporation loss.
The contents were stirred with a magnetic stirrer. The fused mass was cooled down in a furnace
and leached with distilled water (1 g fused mass/50 ml H2O, 60 C, 200 rpm, 30 min). The insoluble
matter was filtered, dried and weighed. Figure 4.11 shows the water leaching of alkali fused
catalyst.
 Fig. 4.4: water leaching of roasted powder
Figure 4.12 shows the path for recovery of alumina by precipitation.
Characterization of catalyst
Spent catalyst Pretreatment of catalyst
Roasting with NaOH / Na2CO3 for 2hr and 4hr
Hot water leaching

Insoluble Residue
Alumina pH adjustment Ni
Recover by 2N HCl (9 pH) Si
y

Extraction (10% aliquat in kerosene) Acid Leaching

Stripping (2M NH4OH) (10% HCl)

Evaporation Nickel
Recovery

Tungsten recovery

Fig. 4.5 Path for alumina recovery

Here 1gm of catalyst powder was taken and roasted with alkali for 2hr. Roasted powder was
contact with fresh 10ml water. Three water leaching stages were followed.

Table 4.8 shows the metal concentration in three stages of water leaching.

Table 4.2 Metal concentration in water leachate

 Water leaching stage W Al
(ppm) (ppm)
1st 5120 2415
2nd 1202 81
3rd 352 42
Mixed leachate 4590 2820

Figure 4.13 shows the metal concentration in water leachate in three stages.
Metal recovery
8000 7578
7000 6322.56
6000
5000
4000
3000 Tungsten
22512230
2000 Alumina
1000 595
170.94 70 90
0
1st 2nd 3rd Mixed leachate
Stage

Fig. 4.6 Metal concentration in water leachate

Table 4.9 shows the weight of insoluble residue of the three water leaching stages.

Table 4.3 Insoluble solid after water leaching

Stage Insoluble solid (gm)

1st 0.430
2nd 0.313
3rd 0.231

Here 1gm of catalyst powder was taken and roasted with alkali for 4hr. Roasted powder was
contact with 10ml fresh water. Three water leaching stages were followed.

Table 4.10 shows the concentration of metal in three water leaching stages.
Table 4.4 Metal concentration in water leachate
 Stage W Al
(ppm) (ppm)
1st 4890 2752
2nd 796 103
3rd 156 66

Figure 4.14 shows the metal concentration in three water leaching stages

Metal recovery
5000 4590
4500
4000
3500
2820
3000
2500
2000 Tungsten
1500 Alumina
1000 796
500 103 156 66
0
1st 2nd 3rd
Stage

Fig. 4.7 Metal concentration in water leachate

Table 4.11 shows the weight of insoluble residue of three water leaching stages.

Table 4.5 Insoluble residue from water leaching

Stage Insoluble solid (gm)

1st 0.411
2nd 0.283
3rd 0.248

Figure 4.15 shows the insoluble residue after three water leaching stages
 Insoluble residue after water leaching
0.6

0.4

0.2

0
1st 2nd 3rd
2 hr 4 hr

Fig. 4.8 Insoluble residue after water leaching

When 2 gm of catalyst is roasted with alkali for 2 hr. Roasting powder was contact with 50ml
fresh water. Three water stages were applied.

Table 4.12 shows the metal concentration in water leachate in three water leaching stages.
Table 4.6 Metal concentration in water leachate

Water leaching stages W (ppm) Al (ppm)

st
1 7578 6322.56
nd
2 595 170.94
rd
3 70 90
Mixed leachate 2251 2230
Figure 4.16 shows the metal concentration in water leachate

Metal concentration
8000

6000

4000

2000

0
1st 2nd 3rd Mixed leachate
W Al

Figure 4.9 Metal concentration

Table 4.13 shows the insoluble residue after water leaching.
 Table 4.7 Insoluble residue

Water leaching stage Insoluble Residue (gm)

1st 2.920
2nd 1.339
3rd 1.006

Figure 4.17 shows the insoluble residue after three water leaching.

Insoluble Residue
3.5
3
2.5
2
1.5
1
0.5
0
1st 2nd 3rd
Insoluble Residue

Figure 4.10 Insoluble residue

Figure 4.18 shows the path for alumina recovery by precipitation.

 Characterization of catalyst
Spent catalyst Pretreatment of catalyst
Roasting with NaOH / Na2CO3 for 2hr and 4hr
Hot water leaching

Alumina pH adjustment
Recovery by 2N HCl (9 pH),
5M NH4OH add at 70 C

Extraction (10% aliquat in kerosene)

Stripping (2M NH4OH)

Evaporation

Tungsten recovery

Fig. 4.11 Path for alumina recovery

After the three stages of water leaching, mix the all leachate for the extraction. For the alumina
recovery pH was maintained up to 9. The pH of water leachate was 11.98 (basic solution). So that
pH is adjust by adding 2N HCl solution. After the pH adjusted up to 9, leachate was heated up to
70 C. Then NH4OH was added to the leachate solution for alumina precipitation.

Figure 4.19 show the alumina precipitation during the pH adjustment in leachate.
 Fig. 4.12: Alumina precipitations
Precipitation of alumina was removed by filtration or centrifuge. Precipitate was collected, dried
and weight. From the EDS analysis determine the concentration of alumina in precipitation.
Table 4.14 shows the metal concentration in leachate after precipitation. (Adding NH4OH)

Table 4.8 Metal concentration in leachate after precipitation

pH W Al
(ppm) (ppm)
8 1599 4
9 1685 35
10 2107 256
2 1334 24
Figure 4.20 shows the W and Al concentration in leachate after precipitation

Metal concentration
3000

2000

1000

0
8 9 10 2
W Al

Fig. 4.13 Metal concentration in leachate after precipitation

Figure 4.21 shows the powder of precipitation form during the pH adjustment.
 Fig. 4.14: Alumina recovery
Table 4.15 shows the metal composition in precipitation at various pH.

Table 4.9 Metal composition in precipitation

Element pH Weight% Atomic%

Al 6 14.91 14.34
W (Without adding NH4OH) 10.28 1.45
Al 8 7.29 6.55
W (Adding NH4OH) 5.61 0.74
Al 9 2.02 2.22
W (Adding NH4OH) 1.02 0.16
Al 10 10.54 8.70
W (Adding NH4OH) 6.95 0.80
Al 2 2.74 2.69
W (Adding NH4OH) 8.36 1.21

Figure 4.22 shows the metal composition in precipitates after pH adjustment.

 Metal composition in precipitates
20
15
10
5
0
Al W
6 8 9 10

Fig. 4.15 Metal composition in precipitates

EXTRACTION
In extraction process 10% Aliquat 336 in kerosene was used as an extractant (Figure 4.23)

Fig. 4.16: Extracant: Aliquat 336

Initial pH of leachate solution was 11.94 which adjusted by 2N HCl solution up to 2.20. For the
extraction process ratio of organic phase to aqueous phase was same. Organic phase and aqueous
phase were contacted and shaking for 20-30 min on shaker. After this phases were separated by
separating funnel. (Figure 4.24)
 Fig. 4.17: Separation of organic phase and aqueous
pH was increases of aqueous phase because of extraction process. Collected the sample for the
analysis. Again pH was adjusted by HCl and contacted the organic phase to aqueous phases.

Table 4.16 shows the metal concentration during the 1st stage of extraction.

Table 4.10 Metal concentration during extraction

Initial pH W recovery Al recovery

pH (ppm) (ppm)
1 6 2.07 28 6
2 (without adding NH4OH) 2.12 26 5
3 2.02 25 9
1 9 2.05 41 19
2 (Adding NH4OH) 2.20 41 28
st
Figure 4.25 shows the metal concentration during 1 stage of extraction when pH was 6.

Extraction
30
28 28
26 26
25 Tungsten (1st satge)
24
22
1 2 3

Fig. 4.18 Metal concentration during extraction

2nd stage extraction:

For the 2nd stage of extraction, take an aqueous phase from the 1st stage leaching and aqueous phase
contact with the fresh extractant. Here the ratio of organic phase to aqueous phase was 1. Both
phases were contacted and shaking for the 20-30 min on shaker. Phases were separated by
separating funnel. Table 4.15 shows the metal concentration in 2nd stage of extraction.

Table 4.17 shows the metal concentration in aqueous phase after 2nd stage extraction.
Table 4.11 Metal concentration in extraction

Initial pH pH W recovery (ppm)

6 (without adding NH4OH) 2.11 53

STRIPPING

Organic phase and aqueous phase were separated from the extraction process. Organic phase was
contacted with 2M NH4OH, shake for 20 min on shaker. After stripping organic phase and aqueous
phase were separated by separating funnel.

Figure 4.26 shows the aqueous phase after the stripping process.

Fig. 4.19: stripping

Table 4.18 shows the metal concentration in aqueous phase after stripping process.

Table 4.12 Metal concentration after stripping

Initial pH pH W recovery (ppm) Al recovery (ppm)

6 2.43 227 14
(without adding NH4OH)
9 2.35 354 32
(Adding NH4OH)

After the stripping, aqueous phase separated. When the solution is slowly evaporated, crystals form
in the solution. (Figure 4.27)

Fig. 4.20: Ammonium peratungstate

When aqueous phase of stripping was evaporated (40ml), only 0.005 gm solid obtained from it.
Metal composition was determine by EDX analysis.

Table 4.19 shows the metal composition of ammonium peratungstate.

Table 4.13 Metal composition (Without adding NH4OH)

Element Weight% Atomic%

W 0.83 0.15
Na 5.14 7.28
Si 2.58 2.99
Cl 86.51 79.52
O 4.94 10.06
Table 4.19 shows the metal composition after evaporation
Table 4.14 Metal composition (Adding NH4OH)

Element Weight% Atomic%

Al 52.03 65.28
Cl 33.59 32.07
W 14.38 2.65

4.3.3 RECOVERY OF Ni FROM INSOLUBLE RESIDUE

When the water leaching step was performed, Ni and Si are insoluble in the water. For the recovery
of Ni from the insoluble residue, acid leaching was done. Here 1 gm residue was contacted with
HCl (10% concentration). The contents were stirred with a magnetic stirrer at 30 C. Samples
were collected at regular time interval to determine concentration of metals in leachate.
Table 4.20 shows the Ni concentration in leachate with time.
Table 0.15 Ni concentration in leachate

Time ppm
30 min 115
1 hr 107
2 hr 125
3 hr 118
4 hr 98
Figure 4.28 shows the Ni concentration in leachate with time.

Ni concentration in leachate
150

100

50

0
30 min 1 hr 2 hr 3 hr 4 hr
ppm

Fig. 4.21: Ni concentration

Leachate and insoluble residue were separated. The residue after leaching shown in the
Figure 4.29. Metal composition in solid residue was determine by EDS analysis.

Figure 4.22: Insoluble residue after Ni leaching

Table 4.22 shows the metal concentration in insoluble residue after the acidic leaching.

Table 4.16 Metal composition in insoluble residue

Element Weight% Atomic% Compound%

Al 12.82 11.83 24.23
Si 13.40 11.87 28.66
Ni 18.23 7.73 23.20
 CHAPTER 5

CONCLUSION AND FUTURE SCOPE

The total recycling process demonstrated its ability to reduce hazardous waste disposal to the zero
limit and save natural resources with economic benefits. The recovered metals such as Mo. V, Ni
and Co could be used in steel manufacture and the alumina could be used for the manufacture of
refractories, ceramics and abrasives.

APT- Ferrotungsten, W chemicals, W metal, WC

Cemented tungsten carbides are currently used extensively in various industries, especially in
manufacturing industries where WC is used to make a variety of hard metals. Cemented tungsten
carbides are commonly used in the production of cutting tools for machining processes, wear
resistant parts, and similar industrial uses.
APT can be calcined under reducing conditions to form tungsten blue oxide, which is a mixture of
tungsten oxides and other constituents; calcined under oxidizing conditions to form tungsten
trioxide; decomposed by hydrochloric acid to form tungstic acid; or subjected to partial thermal
decomposition to form ammonium metatungstate. Tungsten blue oxide is the most commonly used
starting material to make tungsten metal powder which is used to make tungsten alloys, carbide
powder, and metal. Tungsten trioxide can be used to make tungsten metal powder and is also used
as a yellow pigment. Tungstic acid is used to make tungsten chemicals and ultrafine tungsten metal
and tungsten carbide powders. Ammonium metatungstate is used to make tungsten chemicals and
catalysts (Lassner and Schubert, 1999, p. 208-215).
 CHAPTER 6

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