**6.1. Spectroscopic characterization**

The functional groups of the synthesized product were investigated by Fourier transform infrared spectrophotometer. The spectrums of the product confirm the existence of the carbonyl and amide functionalities. **Figures 5** and **6** show the FTIR spectra for the final product and the monomer. The peaks at 3191–3331 cm−<sup>1</sup> were due to amine group, whereas, the absorption peak at 1651 cm−<sup>1</sup> is strong and sharp and is attributed to the carbonyl (C〓O) of the carboxyl group [38]. The peaks at 2868.68 and 2909.55 and 2931.10 cm−<sup>1</sup> are assigned to υ**-**CH2 [39].

A thermal property of anionic polyacrylamide was characterized by TGA. According to **Figure 8**, crude dry particles were obtained by removing free water and solvent isothermally at 110°C. As the nonpolar solvent used to wash the products, chloroform would be expected to constitute the major part of volatile solvents since it could remain absorbed during synthesis but was not observed [42]. There are three main thermal degradations of the anionic polyacrylamide. The first degradation is at 186.53–252.51°C with a weight loss of 0.721% due to absorbed and bonded water in polyacrylamide [43]. The second degradation temperature (Td) is onset at 252.51–311.97°C with a weight loss of 8.556%. The degradation evolves ammonia from thermal imidization of polyacrylamide [44, 45] removing of unreacted monomer or absorbed solvent. The main weight loss of 19.6% onset at 390.15–487.93°C results from

**Figure 5.** FTIR spectrum of anionic polyacrylamide (APAm) induced by maghnite-Na<sup>+</sup>

Synthesis and Characterization of Polymeric Material Consisting on Acrylamide Catalyzed…

irradiation.

(5 wt%) under microwave

http://dx.doi.org/10.5772/intechopen.80033

117

degradation of the polymer chain backbone [46].

**Figure 6.** FTIR spectrum of acrylamide (Am).

The 1 H NMR spectrum of (APAm) induced by maghnite-Na<sup>+</sup> (2 wt%) under microwave irradiation was recorded in deuterated deionized water (D2 O) solution using a Bruker Avance 300 MHz Spectrometer. Chemical shifts (δ) were given in ppm with tetramethylsilane (TMS) as a standard. **Figure 7** represents 1 H NMR spectrum of APAm, which was obtained from purified polymer dispersion. The <sup>1</sup> H NMR spectrum was in accordance with the proposed structures of the product. The Methylene group of APAM was observed at 1.20–1.40 ppm and (CH) group from APAm appeared at 2.40–2.60 ppm. The strong peaks of 4.60–4.80 ppm were attributed to the solvent (D<sup>2</sup> O) [40, 41].

Synthesis and Characterization of Polymeric Material Consisting on Acrylamide Catalyzed… http://dx.doi.org/10.5772/intechopen.80033 117

**Figure 5.** FTIR spectrum of anionic polyacrylamide (APAm) induced by maghnite-Na<sup>+</sup> (5 wt%) under microwave irradiation.

**Figure 6.** FTIR spectrum of acrylamide (Am).

**5. Synthesis of polymeric material**

The reaction taking place is shown in **Scheme 2**.

**Scheme 2.** Synthesis of anionic polyacrylamide (APAm) induced by maghnite-Na<sup>+</sup>

and (2 w%) of maghnite-Na<sup>+</sup>

116 Characterizations of Some Composite Materials

**6. Results and discussion**

**6.1. Spectroscopic characterization**

absorption peak at 1651 cm−<sup>1</sup>

as a standard. **Figure 7** represents 1

purified polymer dispersion. The <sup>1</sup>

attributed to the solvent (D<sup>2</sup>

uct and the monomer. The peaks at 3191–3331 cm−<sup>1</sup>

temperature.

υ**-**CH2

The 1

[39].

nite-Na+

A solution of 2 g of acrylamide containing 0.5 M of sodium hydroxide (NaOH) was prepared

The mixture was subjected to several short burst of microwave irradiation using a microwave oven at frequency of 2.45 GHz at power output of 200 W. The reaction mixture was then submitted to microwave irradiation at 160°C and for 4 min. The mixture was cooled (4–10 min at room temperature), filtered and washed extensively with distilled water and methanol to remove any unreacted acrylamide until the washing solution became neutral and air dried.

Under conventional conditions (CS), the polymer was produced with 75% yield after 5 h, if the reaction was continued the yield was 87.6% after 24 h at ambient temperature. By contrast, under microwave irradiation the material was produced with the remarkable yield 80.56% after only 2 min after the beginning of the reaction, and 92.58% after 20 min at ambient

The functional groups of the synthesized product were investigated by Fourier transform infrared spectrophotometer. The spectrums of the product confirm the existence of the carbonyl and amide functionalities. **Figures 5** and **6** show the FTIR spectra for the final prod-

300 MHz Spectrometer. Chemical shifts (δ) were given in ppm with tetramethylsilane (TMS)

structures of the product. The Methylene group of APAM was observed at 1.20–1.40 ppm and (CH) group from APAm appeared at 2.40–2.60 ppm. The strong peaks of 4.60–4.80 ppm were

the carboxyl group [38]. The peaks at 2868.68 and 2909.55 and 2931.10 cm−<sup>1</sup>

H NMR spectrum of (APAm) induced by maghnite-Na<sup>+</sup>

O) [40, 41].

diation was recorded in deuterated deionized water (D2

were due to amine group, whereas, the

(2 wt%) under microwave irra-

(2 wt%) under microwave irradiation.

O) solution using a Bruker Avance

are assigned to

is strong and sharp and is attributed to the carbonyl (C〓O) of

H NMR spectrum of APAm, which was obtained from

H NMR spectrum was in accordance with the proposed

and NaOH) was put into a flask with 100 mL and stirred to allow proper mixing.

(Algerian MMT) was then added. The mixture of (Am, magh-

A thermal property of anionic polyacrylamide was characterized by TGA. According to **Figure 8**, crude dry particles were obtained by removing free water and solvent isothermally at 110°C. As the nonpolar solvent used to wash the products, chloroform would be expected to constitute the major part of volatile solvents since it could remain absorbed during synthesis but was not observed [42]. There are three main thermal degradations of the anionic polyacrylamide. The first degradation is at 186.53–252.51°C with a weight loss of 0.721% due to absorbed and bonded water in polyacrylamide [43]. The second degradation temperature (Td) is onset at 252.51–311.97°C with a weight loss of 8.556%. The degradation evolves ammonia from thermal imidization of polyacrylamide [44, 45] removing of unreacted monomer or absorbed solvent. The main weight loss of 19.6% onset at 390.15–487.93°C results from degradation of the polymer chain backbone [46].

**6.2. Kinetics studies**

that MMT-Na+

nite-Na+

irradiation.

**Table 5** shows the effect of the amount of Magh-Na<sup>+</sup>

ried out at 160°C under effect of microwave irradiation.

The percentage moisture retains of maghnite-Na+

ture retain gradually [51].

increased with the amount of maghnite-Na+

proportional to the amount of Magh-Na+

of microwave irradiation. Indeed, using various amounts of Magh-Na+

catalyst. This phenomenon is probably the result of an increase in the number of "initiating active sites" responsible of inducing polymerization, a number that is pro rata to the amount of catalyst used a reaction [47]. In the other hand the viscosimertic molecular weight are inversely

weight, the polymerization was carried under microwave irradiation in bulk at 160°C. The polymerization should be related to their surface area. Ayat et al. obtain similar results [48]. Effect of temperature on the polymerization of anionic polyacrylamide under effect of magh-

yield reach maximum value around 160–164°C. On the other hand, with the increase in the reaction temperature above 160°C, viscosity of the obtained polymer increase and decrease the molecular weight of the polymer progressively, suggesting the possible occurrence of thermal degradation [49, 50]. On the basis these results, subsequent polymerization were car-

Am (acrylamide) and catalyst content are shown in **Figures 9**–**12**. It was observed that mois-

The decreases in moisture retain and water uptake can be attributed to the percentage of clay in the composite being limited, which reflects that the quantity of the polymer introduced in the layers reaches a limit and is enough to achieve maximum opening of the interlayer of clay and the formation of a cross-linked structure of a certain extent which prevents the insert on of water molecules [52, 53]. Finally, water resistance of these composites which as defined the decreases in moisture retain and water uptake values can be greatly improved [54, 55].

**Table 5.** Effect of amount of catalyst on polymerization yield of anionic polyacrylamide (APAm) under microwave

**Time (min) 1 2 3 4 5** Catalyst (%) 1.5 2 3 4 5 Yield (%) 15.09 34.86 52.93 77.95 84.82

**Time (min) 5 5 5 5 5** Temperature (°C) 100 130 145 160 164 Yield (%) 19.34 39.06 59.81 79.91 84.94

**Table 6.** Effect of temperature on polymerization yield of anionic polyacrylamide under microwave irradiation.

is present as the active initiator species since the number of those species by

Synthesis and Characterization of Polymeric Material Consisting on Acrylamide Catalyzed…

(5% by weight) for 5 min in microwave irradiation is shown in **Table 6**. Polymerization

on the polymerization yield under effect

http://dx.doi.org/10.5772/intechopen.80033

, thus clearly showing the effect of Mag-Na<sup>+</sup>

. This finding is in good agreement with the proposal

and APAm/maghnite-Na<sup>+</sup>

: 1.5, 2, 3, 4 and 5% yield

with increasing

as a

119

**Figure 7.** <sup>1</sup> H-NMR spectrum of anionic polyacrylamide (APAM) induced by maghnite-Na+ (5 wt%) under microwave irradiation.

**Figure 8.** Thermogravimetric curve of the APAm, obtained after samples treated isothermally at 110°C for 20 min.

## **6.2. Kinetics studies**

**Figure 7.** <sup>1</sup>

118 Characterizations of Some Composite Materials

irradiation.

H-NMR spectrum of anionic polyacrylamide (APAM) induced by maghnite-Na+ (5 wt%) under microwave

**Figure 8.** Thermogravimetric curve of the APAm, obtained after samples treated isothermally at 110°C for 20 min.

**Table 5** shows the effect of the amount of Magh-Na<sup>+</sup> on the polymerization yield under effect of microwave irradiation. Indeed, using various amounts of Magh-Na+ : 1.5, 2, 3, 4 and 5% yield increased with the amount of maghnite-Na+ , thus clearly showing the effect of Mag-Na<sup>+</sup> as a catalyst. This phenomenon is probably the result of an increase in the number of "initiating active sites" responsible of inducing polymerization, a number that is pro rata to the amount of catalyst used a reaction [47]. In the other hand the viscosimertic molecular weight are inversely proportional to the amount of Magh-Na+ . This finding is in good agreement with the proposal that MMT-Na+ is present as the active initiator species since the number of those species by weight, the polymerization was carried under microwave irradiation in bulk at 160°C. The polymerization should be related to their surface area. Ayat et al. obtain similar results [48].

Effect of temperature on the polymerization of anionic polyacrylamide under effect of maghnite-Na+ (5% by weight) for 5 min in microwave irradiation is shown in **Table 6**. Polymerization yield reach maximum value around 160–164°C. On the other hand, with the increase in the reaction temperature above 160°C, viscosity of the obtained polymer increase and decrease the molecular weight of the polymer progressively, suggesting the possible occurrence of thermal degradation [49, 50]. On the basis these results, subsequent polymerization were carried out at 160°C under effect of microwave irradiation.

The percentage moisture retains of maghnite-Na+ and APAm/maghnite-Na<sup>+</sup> with increasing Am (acrylamide) and catalyst content are shown in **Figures 9**–**12**. It was observed that moisture retain gradually [51].

The decreases in moisture retain and water uptake can be attributed to the percentage of clay in the composite being limited, which reflects that the quantity of the polymer introduced in the layers reaches a limit and is enough to achieve maximum opening of the interlayer of clay and the formation of a cross-linked structure of a certain extent which prevents the insert on of water molecules [52, 53]. Finally, water resistance of these composites which as defined the decreases in moisture retain and water uptake values can be greatly improved [54, 55].


**Table 5.** Effect of amount of catalyst on polymerization yield of anionic polyacrylamide (APAm) under microwave irradiation.


**Table 6.** Effect of temperature on polymerization yield of anionic polyacrylamide under microwave irradiation.

**Figure 9.** The percentage moisture retains values of acrylamide (Am) obtained including different percentages of (Am).

**Figure 11.** The percentage moisture retains values of maghnite-Na+, Am and APAm obtained including different

Synthesis and Characterization of Polymeric Material Consisting on Acrylamide Catalyzed…

http://dx.doi.org/10.5772/intechopen.80033

121

and APAm/maghnite-Na<sup>+</sup>

obtained including

percentages of Am, maghnite-Na+ and APAm.

**Figure 12.** The percentage moisture retains values of maghnite-Na+

different percentages of Am.

**Figure 10.** The percentage moisture retains values of maghnite-Na+ obtained including different percentages of maghnite.

Synthesis and Characterization of Polymeric Material Consisting on Acrylamide Catalyzed… http://dx.doi.org/10.5772/intechopen.80033 121

**Figure 11.** The percentage moisture retains values of maghnite-Na+, Am and APAm obtained including different percentages of Am, maghnite-Na+ and APAm.

**Figure 9.** The percentage moisture retains values of acrylamide (Am) obtained including different percentages of (Am).

obtained including different percentages of maghnite.

**Figure 10.** The percentage moisture retains values of maghnite-Na+

120 Characterizations of Some Composite Materials

**Figure 12.** The percentage moisture retains values of maghnite-Na+ and APAm/maghnite-Na<sup>+</sup> obtained including different percentages of Am.
