Article Cite This: Ind. Eng. Chem. Res. XXXX, XXX, XXX−XXX
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A Study of the Surface Adhesion and Rheology Properties of Cationic Conditioning Polymers Zhenyu Yuan,† Jie Wang,*,† Xiaofeng Niu,† Jun Ma,† Xue Qin,† Li Li,† Lei Shi,*,‡ Yongtao Wu,‡ and Xuhong Guo*,†,§ †
Downloaded by UNIV OF SOUTHERN INDIANA at 12:18:16:827 on May 25, 2019 from https://pubs.acs.org/doi/10.1021/acs.iecr.9b00054.
State Key Laboratory of Chemical Engineering, East China University of Science and Technology, Shanghai 200237, People’s Republic of China ‡ Firmenich Aromatics (China) Co., Ltd., Shanghai 201108, People’s Republic of China § Engineering Research Center of Materials Chemical Engineering of Xinjiang Bingtuan, Shihezi University, Xinjiang 832000, People’s Republic of China S Supporting Information *
ABSTRACT: A comparative study was carried out on the surface adhesion and rheology properties of commercial conditioning polymers: cationic guar gum (SOLVAY) and hydroxyethyl cellulose (DOW). In this study, a tailor-made JKR (Johnson, Kendall, and Roberts) instrument was applied to assess the adherence of those cationic polymers at different concentrations. It was found that the concentration, molecular weight, and cationic charge density affected the adhesion performance and rheology properties. The elastic modulus (G′) and viscous modulus (G″) of cationic polymers at different concentrations were correlated to their adhesion properties. On the basis of these results, the surface adhesion property can be controlled by using different types of cationic polymers and provide more insight toward better applications in personal care products.
1. INTRODUCTION Cationic polysaccharides with quaternary ammonium functional groups are water-soluble polymers derived from plants with unique physical-chemical properties to act as stabilizing, suspending, wetting, lubricating, and antibacterial agents.1 Because of their biocompatible and biodegradable nature, cationic polysaccharides have been extensively used in a wide range of industrial applications such as wound adhesives,2−4 hair and body care products,5,6 and film coating.7,8 A deeper knowledge about the surface adhesion properties of cationic polymers is crucial when selecting the proper one for certain applications where the interaction with the surface of target substrate determines the key performance. For instance, in hair care products, cationic conditioning polymers are required to deposit onto hair to improve its combability and to assist the © XXXX American Chemical Society
delivery of other beneficial materials including silicones and fragrances. However, most research is focused on the mechanical and swelling properties as well as the stimulation response of cationic polymers; their surface adhesion properties are still less explored. Meanwhile, the hydrophilic interactions, electrostatic interaction, or hydrogen bonding between polymers and substrates may deviate considerably from the bulk.9−11 Thus, the study of surface adhesion properties is of great significance toward better applications of cationic polysaccharides. Received: January 4, 2019 Revised: April 18, 2019 Accepted: May 20, 2019
A
DOI: 10.1021/acs.iecr.9b00054 Ind. Eng. Chem. Res. XXXX, XXX, XXX−XXX
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Industrial & Engineering Chemistry Research
2. EXPERIMENTAL SECTION 2.1. Materials. The cationic guar gums (guar hydroxypropyltrimonium chloride) were provided by SOLVAY. The cationic hydroxyethyl cellulose derivatives (polyquaternium 10) were provided by DOW. All of them were used without further treatment. The structural information on the cationic biopolymers is shown in Tables 1 and 2.34−37 The samples for
Among cationic conditioning polymers, cationic cellulose and guar gum have been paid more attention because of their natural resource abundance and commercial availability. Cellulose is a straight chain polymer consisting of anhydroglucose sugars linked by equatorial β-1,4 bonds.12 The addition of the hydroxyethyl groups on the backbone alters its crystalline structure and makes it soluble in water. Guar gum is a galactomannan polysaccharide with galactose side chains linked onto the backbone at an average molecular ratio of 1:2. The straight chains of D-mannose units are linked together by β-1,4 bonds, and D-galactose units are alternately connected through a (1−6) glycoside linkage.13 Abundant hydroxyl groups on the polymer chain make cellulose and guar gum suitable for chemical modification to install multiple cationic sites that can interact with anionic materials such as hair fibers. In this study, commercial cationically modified guar gum (SOLVAY) and hydroxyethyl cellulose (DOW) were chosen (Figure 1), and their adhesion and rheology properties were characterized by different techniques.
Table 1. Guar Hydroxypropyltrimonium Chlorides from SOLVAY polymer Jaguar C-13S Jaguar C-162 Jaguar Excel
molecular weight (g/mol)
charge density calculated value (mequiv/g)
degree of substitution
2000000−3000000
0.6−0.8
0.10−0.13
1000000−1500000
0.6
0.10
1000000−1500000
0.6−0.8
0.10−0.13
Table 2. Cationic Hydroxyethyl Cellulose Derivatives from DOW polymer JR 30M LR 30M
concentration % by weight
molecular weight (g/mol)
viscosity (cPs)+
% nitrogen
2 2
2000000 1800000
25000−35000 25000−35000
1.5−2.2 0.8−1.1
characterizations were prepared by dissolving the polymer in water at ambient conditions. Water used in all experiments was purified by reverse osmosis and subsequent ion exchange (Millipore Milli-Q). 2.2. Rheological Measurements. Rheological measurements of all samples were performed on a Physica MCR501 (Anton Paar GmbH) stress-controlled rheometer equipped with Peltier at 25 ± 0.1 °C. A parallel plate with a diameter of 25 mm was used. The linear viscoelastic region (LVR) of samples was determined by applying the oscillatory stress in a logarithmic ramp from 0.01 to 10 Pa with six measurement points per decade at a fixed frequency of 1 Hz. The frequency sweep tests were performed using a logarithmic frequency from 0.1 to 10 Hz with 25 measurement points per decade in the LVR region. During all rheological tests, the upper plate was set at a distance of 1 mm, and a trap was used to minimize the solvent evaporation.38 2.3. JKR Measurements. All surface adhesion measurements were carried out on the tailor-made JKR instrument, and the configuration of the JKR instrument was listed in Table S1. The JKR instrument and experimental setup are shown in Figure 2. The process is as follows: (1) Choose the probe (rigid hemispherical metal indenter), initialize the parameters (automatic operating speed), and then set the control mode (pressure or displacement threshold). (2) The probe approaches and separates from the sample at a constant speed. The pressure and displacement transducer are, respectively, used for measuring the interaction force P and the relative displacement δ. (3) Quantify the adhesion energy of samples by using the data obtained in step (2). During the loading process, the probe touches the sample resulting in a level of deformation, and then moves upward to separate from the sample at the same speed. The pressure is zero before contacting, and then rises with the increase of δ, which presents unturned curve in the graph. When the probe moves upward, it will not separate with sample directly at the
Figure 1. Chemical structures of (a) guar hydroxypropyltrimonium chloride and (b) cationic hydroxyethyl cellulose.
Peel strength testing14−17 and atomic force microscopy (AFM)18−20 are common approaches for investigating the adhesion property of a wide range of materials. Peel strength testing measures the force required for peeling the substrate away from the attached rigid substrate,21,22 which is destructive and requires a large amount of sample, resulting in great energy dissipation. For AFM measurement, the contact area is limited, and the cost is high.23 Therefore, it is necessary to develop a simple measurement for surface adhesion characterization. The adhesive contact model of JKR (Johnson, Kendall, and Roberts)24 has been widely used in studying macro-25−27and microscale28−30contact phenomena. The theory provides the relation between the force and elastic potential energy produced when ideal elastomers contact. Shull and coworkers31,32 further developed the theory of JKR, and proposed the method to build the JKR surface energy instrument. On the basis of these, a JKR surface energy instrument (JKR instrument) was designed and made in our laboratory. The JKR instrument requires less amount of sample for the measurement of adhesion force on a macroscopic scale, reduces the energy dissipation, and can control the unloading precisely (μm/s). The energy required to separate the testing materials and the probe can be calculated. In addition, the study of adhesion could also help understand friction, which is strongly influenced by the adhesive properties.33 B
DOI: 10.1021/acs.iecr.9b00054 Ind. Eng. Chem. Res. XXXX, XXX, XXX−XXX
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3. RESULTS AND DISCUSSION 3.1. Influence of Cationic Guar Gum Concentration. The influence of the concentration on adhesion behavior of cationic biopolymer was quantified by JKR measurement. As shown in Figure S1, the maximum contact area was reached at the compressive force of 1 mN at different displacements. It is noted that the adhesion energy and force first increased and then decreased dramatically with the increase of the concentration (Figure 4). As shown in Figure 5, at low
Figure 2. Picture of the JKR instrument: from the front (a), from the side (b), and setup of the JKR instrument (c).
zero point position because of the adhesion of the contact surface. Instead, a reverse force (adhesion) is generated until completely separated, which presents as a downward parabola. The ideal relationship between pressure and displacement is shown in Figure 3. On the basis of these, JKR instrument can
Figure 4. Adhesion force and adhesion energy of Jaguar C-13S (a) and Jaguar C-162 (b) at different concentrations.
Figure 3. Ideal relationship between pressure and displacement.
instantly measure pressure (P) and displacement (δ), and the adhesion energy (UJKR) can be calculated through the integration of the displacement−pressure curve of the closed area (eq 1):20,39 UJKR =
∫ Pdδ
Figure 5. Change of surface adhesion zone with the increase of polymer.
(1)
polymer concentration, the system presented good flowability with low cross-linking degree and had the longest free polymer chains on the surface, but there were few polymer chains in contact with probe. Increasing polymer concentration caused the increase in adhesion force (or energy?). Above the critical concentration, the degree of polymer chain entanglement was also enhanced significantly as well as the system moduli. However, the surface adhesion zone decreased with short free
In all experiments, the velocity of spherical indenter (radius of curvature = 3 mm) was set to be 3 μm/s. Samples were prepared by casting a 3 mm thick layer of polymer gel onto a glass slide. The bead initially made contact with the sample with the applied specific force as the control mode. All measurements were carried out at ambient temperature in a transparent cover to minimize the loss of water and repeated at least three times. C
DOI: 10.1021/acs.iecr.9b00054 Ind. Eng. Chem. Res. XXXX, XXX, XXX−XXX
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Industrial & Engineering Chemistry Research polymer chains on surface.40−42 All of these led to a maximum point in both adhesion energy and force. To assess their cohesion performance, the viscoelastic behavior of each concentration was studied at a constant strain of 1% (chosen in the LVR). As shown in Figure 6, G′
Figure 7. Compressive load−displacement curves of samples Jaguar C-13S (Mw 2 000 000−3 000 000), Jaguar C-162 (Mw 1 000 000− 1 500 000), and Jaguar Excel (1 000 000−1 500 000) at concentrations of 10 wt % (a) and 18 wt % (b).
In addition, their elastic modulus and viscous modulus were also investigated (Figure S2). At concentration of 10 wt %, G′ and G″ of Jaguar C-13S were higher than those of Jaguar C162 and Jaguar Excel at low frequencies, which was due to the high cross-linking degree caused by the large molecular weight of Jaguar C-13S. At concentration of 18 wt %, all samples presented gel-like structures, and G″ had a narrow gap between three samples within the entire frequency range. 3.3. Influence of Charge Density of Cationic Hydroxyethyl Cellulose. As shown in Figure 8a, JR 30M with higher charge density presented excellent adhesion property, and its adhesion energy was calculated to be 146.2 × 10−9 J, which is 14 times larger than LR 30M (9.9 × 10−9 J). For polymers of similar Mw but different charge densities, the higher charge density polymer yields stronger adhesion. However, when the concentration was increased to 33 wt %, only little difference between JR 30M and LR 30M was observed (Figure 8b). The concentration effect can also be seen from Table 3. For JR 30M, when the concentration increased from 18 to 33 wt %, the increase of cross-linking degree contributed to the decrease of the adhesion energy. At high polymer concentration, the system presented gel-like behavior with shorter free polymer chain on the surface, which limited the mobility of polymer chains. For LR 30M, no obvious changes were observed when the concentration increased. The G′ and G″ of JR 30M and LR 30M were shown in Figure S2. The G′ was higher than G″ in the range of 0.1−10 Hz, no cross section was observed, and they all presented gellike structures. G′ and G″ of JR 30M with higher nitrogen content were higher than those of LR 30M, which is consistent with the JKR results. However, at higher concentration of 33 wt %, G′ and G″ of JR 30M were still much higher than those
Figure 6. Elastic modulus (G′) and viscous modulus (G″) as a function of the frequency at different concentrations of Jaguar C-13S (a) and Jaguar C-162 (b).
and G″ of Jaguar C-13S and Jaguar C-162 increased monotonically with concentration. It was also observed that for all concentrations of Jaguar C-13S and Jaguar C-162, G′ was higher than G″, and no cross section was displayed between G′ and G″ throughout the whole range of frequency, which can be explained by the formation of a gel-like structure. The results are inconsistent with the JKR result, which has a maximum point of adhesion energy. Although the high concentration will increase the physical cross-linking of network, its effects on the cohesion and adhesion properties were different. 3.2. Influence of Cationic Guar Gum Molecular Weight. Samples of Jaguar C-13S, Jaguar C-162, and Jaguar Excel have similar degrees of substitution but different molecular weights. As shown in Figure 7, the adhesion energy at 10 and 18 wt % follows the order of Jaguar Excel > Jaguar C162 > Jaguar C-13S. However, the unloading curve of Jaguar Excel could not complete even at 10 wt % as the high surface adhesion exceeded the measurable range of JKR. The results indicate that Jaguar Excel with lower molecular weight is beneficial to the adhesion property due to the large adhesion zone with less entanglement of polymer chains. It was also found that Jaguar Excel presented good adhesion property over a wide range of concentrations. D
DOI: 10.1021/acs.iecr.9b00054 Ind. Eng. Chem. Res. XXXX, XXX, XXX−XXX
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Figure 9. Adhesion energy of cationic guar gum and hydroxyethyl cellulose at concentration of 18 wt %.
Figure 8. Compressive load−displacement curves of JR 30M and LR 30M at 18 wt % (a); and compressive load−displacement curves of JR 30M and LR 30M at 33 wt % (b).
Table 3. Adhesion Force and Adhesion Energy of Samples at 33 wt % adhesion force (mN)
adhesion energy (10−9 J)
polymer
18 wt %
33 wt %
18 wt %
33 wt %
JR 30M LR 30M
1.34 0.30
0.14 0.20
146.2 9.9
3.3 6.6
of LR 30M. This is due to the high cross-linking degree caused by the electrostatic, hydrogen bonding and also the entanglement of polymer chains. 3.4. Comparison of Adhesion Energy for All Samples at Concentration of 18 wt %. The adhesion energy of all samples at concentration of 18 wt % was also investigated (Figure 9). It can be seen that at high concentration, cationic guar gum and hydroxyethyl cellulose displayed similar adhesion properties. This was probably because in the gellike state, the polymers presented a limited surface adhesion zone, which may attenuate the impact caused by the structural differences. Moreover, the surface adhesion energy of these samples varies from 3.3 × 10−9 to 134.7 × 10−9 J, which provides a wide range for the application in different fields. 3.5. Reproducibility of JKR Measurement. The reproducibility was significantly influenced by the evaporation of water during the testing due to the concentration change of the system. So we also applied a trap and controlled the testing time to diminish the evaporation effect. As shown in Figure 10, the measurement was repeated three times under the same conditions, and the load−displacement curve coincided well during the test. Besides, there was no significant difference in the calculated adhesion force and adhesion energy in Table S2, so the tailor-made JKR instrument showed good reproducibility.
Figure 10. Repeatability of Jaguar C-162 at 8 wt % (a) and Jaguar Excel at 18 wt % (b).
4. CONCLUSIONS Surface adhesion properties of cationic guar gum and hydroxyethyl cellulose derivatives in water were investigated by the tailor-made JKR instrument and a rheometer. The compressive load−displacement curves presented good reproducibility, and the adhesion energy was obtained through the integration of enclosed curves. The concentration effect on cationic guar gum showed a maximum value, which is different from the rheological results. As compared to cationic guar gum Jaguar 13S and Jaguar C162, Jaguar Excel with lower molecular weight showed higher adhesion force and energy due to weaker intermolecular chain interaction. The adhesion power was also significantly influenced by the cationic charge density. JR 30M had the highest adhesion energy of 134.7 × 10−9 J as E
DOI: 10.1021/acs.iecr.9b00054 Ind. Eng. Chem. Res. XXXX, XXX, XXX−XXX
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compared to other cationic polysaccharides at a high concentration of 18 wt %. In summary, the study of adhesion and rheology properties of a series of commercial cationic polymers provides more details for choosing the optimal cationic polymers in personal care products and other applications. Besides, the JKR measurement provides a convenient and effective approach for studying the surface adhesion property of polymers.
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ASSOCIATED CONTENT
S Supporting Information *
The Supporting Information is available free of charge on the ACS Publications website at DOI: 10.1021/acs.iecr.9b00054. Rheology measurements and fundamental information on JKR instrument; compressive load−displacement curves of samples Jaguar C-13S and Jaguar C-162; rheology results of Jaguar C-13S, Jaguar C-162, and Jaguar Excel; GPC results of Jaguar C-162 and Jaguar Excel; rheology results of JR 30M and LR 30M; and adhesion force and adhesion energy values of Jaguar C162 and Jaguar Excel (PDF)
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AUTHOR INFORMATION
Corresponding Authors
*E-mail:
[email protected]. *E-mail: lei.rocky.shi@firmenich.com. *E-mail:
[email protected]. ORCID
Jie Wang: 0000-0003-2227-1971 Li Li: 0000-0001-5100-734X Xuhong Guo: 0000-0002-1792-8564 Notes
The authors declare no competing financial interest.
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ACKNOWLEDGMENTS We gratefully thank NSFC Grants (51403062, 51273063, and 21476143), the Fundamental Research Funds for the Central Universities, and the 111 Project Grant (B08021) for financial support of this work.
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DOI: 10.1021/acs.iecr.9b00054 Ind. Eng. Chem. Res. XXXX, XXX, XXX−XXX
