Utilization of petroleum sludge wastes for increasing productivity of ordinary portland cement

Abstract

This work aims at maximum exploitation of petroleum waste sludge as additive to portland cement to prepare blended cements and hence increasing its production capacity without further firing. This will decrease the main cement industry problems involving environmental pollution such as releasing gases and high-energy consumption during industry and hence maximizes the production economics. Six batches of ordinary portland cement (OPC) mixed with different proportions of petroleum waste sludge (PWS) donated as C1 (control batch contains no PWS), C2 (contains 90 wt.% of OPC+10 wt.% of PWS), C3 (contains 80 wt.% of OPC+20 wt.% of PWS), C4 (contains 70 wt.% of OPC+30 wt.% of PWS), C4 (contains 60 wt.% of OPC+40 wt.% of PWS) and C6 (contains 50 wt.% of OPC+50 wt.% of PWS), were prepared and mixed individually with the suitable amount of mixing water. Cement mixes C2, C3 and C4 showed improved cementing and physicomechanical properties compared with pure cement (C1) with special concern of mix C4. Such improvement is due to the relatively higher surface area as well as the high content of kaolinite and quartz in the added PWS (high pozzalanity) favoring the hydration process evidenced by the increase in the cement hydration product (portlandite mineral (Ca (OH) ₂).

Keywords

Cement PWS portlandite sintering mechanical

1 Introduction

Nowadays cement industry suffers globally from a high cost and availability of its raw materials (clays (aluminum silicate) and limestone (calcium carbonate)), consumption of energy in addition to that evolution of gases during this industry which creates a serious problems to the environment, although the international demand increasing day by day for this material. Therefore, this kind of phenomena allowed the researchers and industrialists to look for the alternatives as additives to the cement to minimize the cost of these materials, saving energy and reducing the environmental hazards. This can be achieved by utilizing the field of wastes (reusing and recycling of the wastes) originate from different sources specially for those possessing a pozzolanic nature (such as aluminosilicate based minerals, petroleum waste sludge (PWS), iron slags, ceramic wastes, fumed silica, ashes of coke, barely and rice straw ... etc). Exploitations of these wastes in increasing the productivity of cement, which helps in the solving of the disposal of pollutants to the planet and adding a commercial value to the final products.

Khalill & Yousif [1] reported that the addition aluminosilicate raw materials to ordinary portland cement results in an improvement of physicochemical and mechanical properties. Khalil et al. [2] have reported improvement of cementing properties of portland cement through addition of about 20 wt. % of the ashes of either barely, rice, coal to portland cement. Many authors [1 –26], used different materials (industrial wastes, agricultural wastes and natural raw minerals) that have pozzalnic properties as additives in different proportions (up to 30 wt. %) to improve the characteristics of portland cement.

Several research works [27 –33] were carried out to study the effect of addition of different materials such as lime kaolinite, clays, fly ash and other pozzolanic additives to enhance the cement hydration process.

N. M. Khlill et al. [33] could exploitate petroleum waste sludge (the wastes produced from petroleum industry) [34 –36] in producing a high quality refractory ceramics. Many authors [37 –40] reported the feasibility of using these wastes in ceramic production in different proportions, incorporation of these wastes in cement and clayey bodies [41 –44] thus helps in elimination of dangerous material causing severe environmental problems in addition to that usage of cheap raw materials.

Many authors [45 –50] studied the possibility of utilizing petroleum waste sludge for ceramic industry, they used it together with clay, quartz and feldspar for producing densified floor tiles

Ali Benlamoudi et al. [51] could replace gypsum by petroleum waste sludge during manufacturing of ordinary portland cement depending on its relatively higher content of barite (BaSO₄).

The present work aims at benefit from the huge accumulations of petroleum waste sludge in KSA for increasing the portland cement production capacity and improve its cementing and physicomechanical properties.

2 Experimental

2.1 Materials collection

2.1.1 Portland cement (Al Arabiya Company) Western region of KSA

2.1.2 The petroleum waste sludge brought from petroleum extraction industry in Dhamam, Eastern Area of KSA. The raw material were washed and dried at 110°C, dry grounded and then passed through a 325 –mesh (45μm ASTM) sieve.

2.1.3 Analar grade methyl alcohol and dimethyl ether were used to stopp hydration at different ages (3, 7, 28 & 90 days).

Table 1
The batches compositions

Batch No. Batch composition Observations

(Cement Wt.%) (Petroleum waste sludge Wt.%)

1 100 00 Control (C1)

2 90 10 C2

3 80 20 C3

4 70 30 C4

5 60 40 C5

6 50 50 C6

Batch No.	Batch composition	Observations
1	100	00	Control (C1)
2	90	10	C2
3	80	20	C3
4	70	30	C4
5	60	40	C5
6	50	50	C6

2.2 Methods

Six batches of cement-petroleum waste sludge mixes were prepared in different proportions as given in Table 1.

The suitable amount of gauging water was used to prepare pastes from each cement mix, shaped into cubic samples in steel mould, left in 100% relative humidity, demoulded after 24 days and tested at different ages of hydration (up to 90 days). The hydration behavior was studied through determining the content of water of hydration of the mixes fired at 900°C: $Hydration percent = \frac{Wt . of green sample - Wt . of ignited sample \times 100}{Wt . of ignited sample}$ (1)

2.3 Characterization

The chemical constituents and mineralogical components of cement and petroleum waste sludge were investigated using Philips X-ray fluorescence (XRF) machine and X-ray diffractometer (XRD) with Ni filtered Cu-Ka radiation operating at 30 mA and 40 kV), D8 ADVANCE (Bruker, Germany).

Optimum consistence, initial and final setting time as well as cold crushing strength were tested adopting the International Standard tests [52 –56].

The mineralogy of the hydrated samples was investigated using X-ray diffraction (XRD) technique.

The correlation between the mineralogical composition and characteristics of the hydrated cement samples was studied to reach the optimum cement mix composition compromise different outstanding characteristics and satisfy the international standards.

3 Result and discussions

3.1 Chemical constituents

XRF was used to check the chemical compositions of cement and PWS as given Table 2.

Table 2
Starting materials constitution

Starting materials Chemical composition %

Al₂O₃ BaO SiO₂ Fe₂O₃ CaO SO₃ ZrO₂ SrO TiO₂ MgO Na₂O+K₂O LOI

Cement – 7.00 24.5 4.02 63.5 0.4 – – – 0.08 0.5 3.01

PWS 0.20 39.08 28.62 0.08 9.10 2.70 2.01 1.70 1.10 0.5 – 14.91

Starting materials	Chemical composition %
Cement	–	7.00	24.5	4.02	63.5	0.4	–	–	–	0.08	0.5	3.01
PWS	0.20	39.08	28.62	0.08	9.10	2.70	2.01	1.70	1.10	0.5	–	14.91

Fig.1

A. XRD pattern of cement. B. XRD pattern of the petroleum waste sludge.

3.2 Mineral composition of starting materials

3.2.1 Cement

Figure 1(a) shows that OPC composed mainly of calcium tri-silicate (Ca₃SiO₅ –71.9 %) and calcium di-silicate (Ca₃SiO₅ –28.1 %) as given in Table 3.

3.2.2 PWS mineralogy

From Figure 1 (b) PWS consisted mainly of barite, quartz and kaolinite minerals as given in Table 4:

Table 3
Cement mineralogy

Mineral Chemical formula Percentage % Reference code

calcium trisilicate Ca₃SiO₅ 71.9 % 00-031-0301

calcium disilicate Ca₂SiO₅ 28.1 % 00-032-0148

Mineral	Chemical formula	Percentage %	Reference code
calcium trisilicate	Ca₃SiO₅	71.9 %	00-031-0301
calcium disilicate	Ca₂SiO₅	28.1 %	00-032-0148

Table 4

PWS mineralogy

Mineral	Chemical formula	Percentage %	Reference code
Barite	BaSO₄	47.0 %	00-046-1415
Quartz	SiO₂	21.7 %	00-003-0419
Kaolinite	Al₂ (Si₂O₅ (OH)₄	31.3 %	01-079-1570

3.3 PWS microstructure

As given in Table (5) and shown in Figs. (2 and 3) PWS contains a large proportion of Ba, O and S (37.69%, 24.89% and 8.97%, respectively) which reflects the presence of barite (BaSO₄) mineral. The presence of lower contents of aluminum, silicon and calcium (0.66% 1.37%, and 3.67%) refers to the presence of kaolinite and quartz minerals. Some detected residual carbon (18.01 %) are related to the technical preparation of the sample for microstructure depiction.

Table 5
Elemental composition of PWS

Element Wt. %

Barium 37.69

Aluminum 0.66

Silicon 1.37

Oxygen 24.89

Sodium 2.19

Sulphur 8.97

Calcium 3.67

Chlorine 1.74

Carbon 18.82

Element	Wt. %
Barium	37.69
Aluminum	0.66
Silicon	1.37
Oxygen	24.89
Sodium	2.19
Sulphur	8.97
Calcium	3.67
Chlorine	1.74
Carbon	18.82

Fig. 2

Microstructure of PWS.

Fig. 3

EDX analysis of PWS.

3.4 Cementing properties

3.4.1 Consistence

Using adequate content of gauging water is very sensible to avoid the poor workability of cement paste or strength deterioration of the hardened samples.

As given in Table (6) mixes C2, C3, C4, C5 and C6 consume more contents of gauging water; 33.6, 34.4, 35.2,36,4 and 36.6% respectively compared with the C1 (32.8 %). This is correlated with the increase in the PWS content from C2 to C6.

Table 6
Consistence of cement mixes pastes

Batch No. Volume (ml) Standard water (%)

C1 82 32.8

C2 84 33.6

C3 86 34.4

C4 88 35.2

C5 91 36.4

C6 92 36.6

Batch No.	Volume (ml)	Standard water (%)
C1	82	32.8
C2	84	33.6
C3	86	34.4
C4	88	35.2
C5	91	36.4
C6	92	36.6

3.4.2 Setting time

Table (7) indicates that mixes C2 up to C6 exhibit relatively longer initial and final setting times 55–150 minutes, 140-290 minutes compared with C1 (55 minutes, 120 minutes), the higher the content PWS in the mix the longer the setting time. However all the investigated cement mixes satisfy the requirements of International standards i.e. initial setting doesn’t 45 minutes while final setting doesn’t exceed 375 minutes.

Table 7
Setting time of cement mixes

Mix No. Setting time (min.)

Initial Final

C1 45 120

C2 55 140

C3 75 150

C4 95 175

C5 130 210

C6 150 290

Mix No.	Setting time (min.)
C1	45	120
C2	55	140
C3	75	150
C4	95	175
C5	130	210
C6	150	290

3.4.3 Hydration behavior

The content of chemical combined water of cement reflects its hydration behavior. Figure 4 shows a pronounced improvement in the hydration process in C2, C3 and C4 at different ages of hydration, the contents of water of hydration range from 15–23.23 %), the hydration rate decreases in C5 and C6 in which the contents of water of hydration range between (8.00–19.58 %). This is correlated with the relatively higher PWS contents with a relatively higher surface area (4500 cm²/g) and also to its high pozzolanity due to its relatively higher content of quartz, kaolinite and barite minerals, the relatively decrease of combined water in C5, and C6 is due to their extreme deficiency of cement in such mixes (60 and 50 %).

Fig. 4

Hydration behavior of cement mixes.

3.4.4 Bulk density and apparent porosity

Fig. 5

Bulk density of the hardened mixes.

Fig. 6

Apparent porosity of the hardened mixes.

Figures (5 and 6) show a pronounced increase in the values of bulk density corresponded with a pronounced decrease in apparent porosity in mixes containing 10–30 wt. % PWS (cement mixes C2, C3 & C4) recording values of bulk density ranging from 1.942 to 2.614 g/cm³ for the mix C2, 2.09 to 2.715 g/cm³ for the mix C3 and 2.143 to 2.811 g/cm³ for the mix C4 which shows the maximum bulk density among the mixes including the control mix C1 that recorded 1.928 to 2.452 g/cm³ while cement mixes containing 40–50 % PWS (cement mixes C5 and C6) show relatively lower values of bulk density recording values of bulk density ranging from 1.835 to 2.222 g/cm³ for the mix C5 and from 1.663 to 2.012 g/cm³ for the mix C6 corresponded with relatively higher percent of apparent porosity (Fig. 6). The recorded values for the mix C6 ranging from 28.12 to 20.73 % followed by mix C5 ranging from 27.31 to 22.48 %, while the mixes C4, C3 & C2 recorded lower percent of apparent porosity as (22.51 to 18.14 %, 23.095 to 20.55% and 25.14 to 21.42 %) respectively and further more lower for the control mix C1 that recorded the values 24.62 to 18.60 % These results are correlated with the PWS addition, its relatively higher surface area makes it as a good filler that fill voids, gaps and pores in the hardened paste resulting in an improvement in the densification phenomena.

3.4.5 Mechanical strength

Figure 7 shows improved mechanical strength as either the content of PWS and age of hydration increase from 10 –30 % in the cement mixes (viz., C2, C3 & C4) when compared with the control mix C1 that gave the values (62 to 84 Kg/m²).The mechanical strength values for these mixes ranging from (63 to 86 Kg/m²) for the mix C2, (60 to 87 Kg/m²) for the mix C3 and ranging from (64 to 89 Kg/m²) for the mix C4 This improvement in mechanical properties can be explained on the following bases;

Fig. 7

Mechanical strength of the mixes.

The relatively higher surface are of PWS results in a dense and well packed matrix that leads to good mechanical properties.

The high pozzolanity of PWS and is relatively higher content of quartz and kaolinite assist the hydration process and hence improved mechanical strength.

The presence of considerable content of barium decreases the nucleation barrier of hydration which accelerate the hydration process and hence improved mechanical properties.

On increasing the PWS up to 40–50 % i.e., (C5 & C6) their mechanical values ranging from (51 to 76 Kg/m²) for the C5 and the values (52 to 71 Kg/m²) for the mix C6. This leads to negative effect on mechanical properties as a result of decreasing the combined water and poor densification of such mixes.

3.5 Phase composition of the hydrated cement pastes

3.5.1 (a) XRD data

Figure (8–13) show XRD patterns of the hydrates cement mixes compared with the anhydrous samples. As shown In Fig. (8), C1, the intensity of C3S and C2S diminishes as the hydration proceeds (from 3 to 90days of hydration) this is corresponded with the appearance of the new peaks characterizing Ca(OH)₂ (portlandite) mineral, which is an indication of the progress of hydration process. Figures 9–13, show a pronounced decrease in the anhydrous phases (C3S and C2S) with pronounced increase in the intensity of the hydration product (portlandite) as the contentment of PWS increases from 10–30 %, cement mixes 2–4, beyond which a decrease in the intensity of the portlandite peak is observed, these observations the confirm the combined water, densification and mechanical strength findings.

Fig. 8

XRD pattern of the hardened cement C1.

Fig. 9

XRD pattern of the hardened cement mix C2.

Fig. 10

XRD pattern of the hardened cement mix C3.

Fig. 11

XRD pattern of the hardened cement mix C4.

Fig. 12

XRD pattern of the hardened cement mix C5.

Fig. 13

XRD pattern of the hardened cement mix C6.

Fig. 14

SEM of C4 after 90 days of hydration.

Fig. 15

EDX analysis of C4 after 90 days of hydration.

3.5.2 (b) Morphology and EDAX analysis

The microstructure of one selected sample (C4 hydrated up to 90 days) was depicted and analyzed using SEM attached with EDAX unit. Figure (14) shows a dense microstructure of the hardened tested sample in which calcium tri-silicate (C₃S) and portlandite (P) crystals are agglomerated and twined with each other forming a compact and dense microstructure which explains the outstanding cementing and physico-mechanical behavior of such sample. S. J. Barnet et al and Run-Sheng L et al. [57, 58] found that amounts of acicular calcium silicate hydrate honeycomb appears on the surface of the particles. It first grows in a diffuse manner, then densifies. The EDX analysis shown in Fig. (15) and Table (8) indicates that the depicted area is rich in calcium (29.78 %) and oxygen (54.59%) in addition to silicon (5.86 %) which confirm the XRD data attributing the improvement in cement mix properties to the progress of hydration process evidenced by the formation of the hydration product Ca(OH)₂ (portlandite mineral).

Table 8
EDX analysis data of cement of C4 after 90 days of hydration

Element Weight %

O 54.59

Al 2.00

Si 5.86

S 2.05

Ca 29.78

Mg 1.35

Fe 1.38

Cu 2.19

Totals 100.00

Element	Weight %
O	54.59
Al	2.00
Si	5.86
S	2.05
Ca	29.78
Mg	1.35
Fe	1.38
Cu	2.19
Totals	100.00

4 Conclusion

The cementing and physico-mechanical properties of ordinary portland cement could be improved through addition of 10–30 wt. % of PWS. The relatively higher surface area and recognized mineral composition (high pozzolanity) of PWS enhances the hydration process which reflected on the properties of the cement.

Footnotes

Acknowledgment

This article entitled “Utilization of petroleum sludge wastes for increasing productivity of ordinary Portland cement” contains the results and findings of a research project that is funded by Deanship of Research & Post-graduate of University of Jeddah Grant No. (UJ-02-059-DR).

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Starting materials	Chemical composition %
	Al₂O₃	BaO	SiO₂	Fe₂O₃	CaO	SO₃	ZrO₂	SrO	TiO₂	MgO	Na₂O+K₂O	LOI
Cement	–	7.00	24.5	4.02	63.5	0.4	–	–	–	0.08	0.5	3.01
PWS	0.20	39.08	28.62	0.08	9.10	2.70	2.01	1.70	1.10	0.5	–	14.91

Mix No.	Setting time (min.)
Initial	Final
C1	45	120
C2	55	140
C3	75	150
C4	95	175
C5	130	210
C6	150	290

Utilization of petroleum sludge wastes for increasing productivity of ordinary portland cement

Abstract

Keywords

1 Introduction

2 Experimental

2.1 Materials collection

2.1.1 Portland cement (Al Arabiya Company) Western region of KSA

2.1.2 The petroleum waste sludge brought from petroleum extraction industry in Dhamam, Eastern Area of KSA. The raw material were washed and dried at 110°C, dry grounded and then passed through a 325 –mesh (45μm ASTM) sieve.

2.1.3 Analar grade methyl alcohol and dimethyl ether were used to stopp hydration at different ages (3, 7, 28 & 90 days).

Table 1 The batches compositions Batch No. Batch composition Observations (Cement Wt.%) (Petroleum waste sludge Wt.%) 1 100 00 Control (C1) 2 90 10 C2 3 80 20 C3 4 70 30 C4 5 60 40 C5 6 50 50 C6

3 Result and discussions

3.1 Chemical constituents

Table 2 Starting materials constitution Starting materials Chemical composition % Al2O3 BaO SiO2 Fe2O3 CaO SO3 ZrO2 SrO TiO2 MgO Na2O+K2O LOI Cement – 7.00 24.5 4.02 63.5 0.4 – – – 0.08 0.5 3.01 PWS 0.20 39.08 28.62 0.08 9.10 2.70 2.01 1.70 1.10 0.5 – 14.91

3.2.1 Cement

3.2.2 PWS mineralogy

Table 3 Cement mineralogy Mineral Chemical formula Percentage % Reference code calcium trisilicate Ca3SiO5 71.9 % 00-031-0301 calcium disilicate Ca2SiO5 28.1 % 00-032-0148

Table 5 Elemental composition of PWS Element Wt. % Barium 37.69 Aluminum 0.66 Silicon 1.37 Oxygen 24.89 Sodium 2.19 Sulphur 8.97 Calcium 3.67 Chlorine 1.74 Carbon 18.82

3.4.1 Consistence

Table 6 Consistence of cement mixes pastes Batch No. Volume (ml) Standard water (%) C1 82 32.8 C2 84 33.6 C3 86 34.4 C4 88 35.2 C5 91 36.4 C6 92 36.6

Table 7 Setting time of cement mixes Mix No. Setting time (min.) Initial Final C1 45 120 C2 55 140 C3 75 150 C4 95 175 C5 130 210 C6 150 290

3.5.1 (a) XRD data

Table 8 EDX analysis data of cement of C4 after 90 days of hydration Element Weight % O 54.59 Al 2.00 Si 5.86 S 2.05 Ca 29.78 Mg 1.35 Fe 1.38 Cu 2.19 Totals 100.00

Footnotes

Acknowledgment

References

Table 1
The batches compositions

Batch No. Batch composition Observations

(Cement Wt.%) (Petroleum waste sludge Wt.%)

1 100 00 Control (C1)

2 90 10 C2

3 80 20 C3

4 70 30 C4

5 60 40 C5

6 50 50 C6

Table 2
Starting materials constitution

Starting materials Chemical composition %

Al₂O₃ BaO SiO₂ Fe₂O₃ CaO SO₃ ZrO₂ SrO TiO₂ MgO Na₂O+K₂O LOI

Cement – 7.00 24.5 4.02 63.5 0.4 – – – 0.08 0.5 3.01

PWS 0.20 39.08 28.62 0.08 9.10 2.70 2.01 1.70 1.10 0.5 – 14.91

Table 3
Cement mineralogy

Mineral Chemical formula Percentage % Reference code

calcium trisilicate Ca₃SiO₅ 71.9 % 00-031-0301

calcium disilicate Ca₂SiO₅ 28.1 % 00-032-0148

Table 5
Elemental composition of PWS

Element Wt. %

Barium 37.69

Aluminum 0.66

Silicon 1.37

Oxygen 24.89

Sodium 2.19

Sulphur 8.97

Calcium 3.67

Chlorine 1.74

Carbon 18.82

Table 6
Consistence of cement mixes pastes

Batch No. Volume (ml) Standard water (%)

C1 82 32.8

C2 84 33.6

C3 86 34.4

C4 88 35.2

C5 91 36.4

C6 92 36.6

Table 7
Setting time of cement mixes

Mix No. Setting time (min.)

Initial Final

C1 45 120

C2 55 140

C3 75 150

C4 95 175

C5 130 210

C6 150 290

Table 8
EDX analysis data of cement of C4 after 90 days of hydration

Element Weight %

O 54.59

Al 2.00

Si 5.86

S 2.05

Ca 29.78

Mg 1.35

Fe 1.38

Cu 2.19

Totals 100.00