Improved homopolymer separation to enable the application of 1H NMR and HPLC for the determination of the reaction parameters of the graft copolymerization of acrylic acid onto starch

Witono, Judy Retti; Marsman, Jan Henk; Noordergraaf, Inge-Willem; Heeres, Hero J.; Janssen, Ljj Jos

doi:10.1016/j.carres.2013.01.017

Cited by 29 publications

(32 citation statements)

References 38 publications

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“…The reaction was run for 2 h at 40 • C. Samples from the reaction product were analyzed for the grafting parameters using a method of analysis involving complete homopolymer separation and quantitative analysis by HPLC and 1 H NMR. The method was especially developed for this project and has been reported in full detail before (Witono, Marsman, Noordergraaf, Heeres, & Janssen, 2013). However, the complete separation of crosslinked homopolymer from the product is more difficult than in the system without crosslinker.…”

Section: Preparation and Characterization Of The Neutralized Graft Comentioning

confidence: 99%

Water absorption, retention and the swelling characteristics of cassava starch grafted with polyacrylic acid

Witono

Noordergraaf

Heeres

et al. 2014

Carbohydrate Polymers

165

103

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Section: Preparation and Characterization Of The Neutralized Graft Comentioning

confidence: 99%

Water absorption, retention and the swelling characteristics of cassava starch grafted with polyacrylic acid

Witono

Noordergraaf

Heeres

et al. 2014

Carbohydrate Polymers

165

103

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“…In order to evaluate this, acetone was used to extract the unreacted lignin from lignin-AA polymer samples extracted from the reaction medium in soxhlet extractor for 12 h. In this case, the unreacted lignin can be extracted from the lignin-AA polymer as kra lignin is soluble in acetone, but lignin-AA polymer is insoluble. 27,28 Initially, a certain amount (about 2.0-2.5 g) of sample, M 0 , was maintained in a pre-extracted lter paper, and then the samples were extracted with acetone for 12 h. Aer the extraction, the sample was air-dried and then dried in an oven at 105 C for 12 h. The nal mass of the sample, M 1 , was weighed and the percentage of unreacted lignin was calculated using eqn (3):…”

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confidence: 99%

Novel pathway to produce high molecular weight kraft lignin–acrylic acid polymers in acidic suspension systems

et al. 2018

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Kraft lignin (KL) produced in kraft pulping process has a low molecular weight and solubility, which limits its application in industry. For the first time, KL was polymerized with acrylic acid (AA) in an acidic aqueous suspension system to produce a water soluble lignin-AA polymer with a high molecular weight in this work. The polymerization reaction was carried out using K 2 S 2 O 8 as an initiator, and the influence of reaction conditions on the carboxylate group content and molecular weight of resultant lignin polymers was systematically investigated. The mechanism of polymerization of KL and AA was discussed Compared with polyAA, the lignin-AA polymer was a more efficient flocculant for aluminium oxide suspension, which shows its potential to be used as a green flocculant in industry.

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“…For a proper characterization of the grafted starch, homopolymer have to be removed e.g., by Soxhlet extraction [1,2]. An alternative, elaborate but satisfactory, method has been developed in our laboratory [14]. After centrifugation-precipitation of the grafted starch from acetone solvent that keeps the homopolymer in solution, the grafting percentage (GP) and the graft efficiency (GE) were determined with 1 H-NMR.…”

Section: Analytical Procedures and Aspectsmentioning

confidence: 99%

“…After centrifugation-precipitation of the grafted starch from acetone solvent that keeps the homopolymer in solution, the grafting percentage (GP) and the graft efficiency (GE) were determined with 1 H-NMR. The amount of grafted polyacrylic acid onto starch was measured by integrating the relevant peaks in the NMR-spectrum [1,14]. From that result and the confirmed establishment of full monomer conversion [14] the amount of formed homopolymer and thus the grafting efficiency could be calculated.…”

Section: Analytical Procedures and Aspectsmentioning

confidence: 99%

“…The amount of grafted polyacrylic acid onto starch was measured by integrating the relevant peaks in the NMR-spectrum [1,14]. From that result and the confirmed establishment of full monomer conversion [14] the amount of formed homopolymer and thus the grafting efficiency could be calculated. Some authors use gravimetry to determine the grafting results, as discussed in more detail by Meimoun et al [2] and by Fanta et al [1,10].…”

Section: Analytical Procedures and Aspectsmentioning

confidence: 99%

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Free-Radical Graft Polymerization onto Starch as a Tool to Tune Properties in Relation to Potential Applications. A Review

2018

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Abstract:Grafting of acrylic monomers onto the renewable feedstock starch via free radical polymerizations has been investigated for many years. Many potential applications have been studied, such as superabsorbents, flocculants, thickening agents and so forth. It is expected that size and spacing of the grafts have a large influence on the performance of such polymers. Yet, information upon the structure-property relationships is only scarcely found in literature. Moreover, there is no clear overview of how reaction variables can be used to influence the grafted structure. In this review, an assessment has been made of the relation between the architecture of the grafts and potential applications. Then, from a selection of relevant literature data it is demonstrated that reaction variables such as the relative concentrations of initiator and monomer, have a large impact on the average size and spacing of the grafts. The emergence of controlled radical polymerizations, like Atom Transfer Radical Polymerization (ATRP) and Reversible Addition-Fragmentation chain Transfer (RAFT), is discussed, both the current status and future prospects. These methods are promising in the future of starch grafting, especially for systems where homopolymer formation may be a problem. Nevertheless, higher costs and other related issues make these advanced methods more suitable in high added-value products.

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Improved homopolymer separation to enable the application of 1H NMR and HPLC for the determination of the reaction parameters of the graft copolymerization of acrylic acid onto starch

Cited by 29 publications

References 38 publications

Water absorption, retention and the swelling characteristics of cassava starch grafted with polyacrylic acid

Water absorption, retention and the swelling characteristics of cassava starch grafted with polyacrylic acid

Novel pathway to produce high molecular weight kraft lignin–acrylic acid polymers in acidic suspension systems

Free-Radical Graft Polymerization onto Starch as a Tool to Tune Properties in Relation to Potential Applications. A Review

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