Precipitation Polymerization in Acetic Acid: Synthesis of Monodisperse Cross-Linked Poly(divinylbenzene) Microspheres

Qing, Yan; Bai, Yaowen; Meng, Zhe; Yang, Wantai

doi:10.1021/jp711324a

Cited by 55 publications

(59 citation statements)

References 31 publications

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“…Meanwhile, the yield depends on the surfactant concentration in the solution, which is in line with the yield of poly(divinylbenzene) microspheres in surfactant solutions, [35] indicating that the yield of PDMS microspheres not only depends on the external mechanical energy input to the turbulent system, but also to the surfactant concentration in the solution. [36] 100%…”

Section: Pdms Microsphere Size Distribution From Experimentssupporting

confidence: 61%

Polydimethylsiloxane microspheres with poly(methyl methacrylate) coating: Modelling, preparation, and characterization

Ma¹,

Hansen

Hvilsted³

et al. 2015

Can J Chem Eng

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Abstract:Polydimethylsiloxane (PDMS) microspheres are prepared by mixing homogeneous dispersions of vinyl-functional PDMS and a curing agent using mechanical stirring in a series of aqueous solutions, and curing at 80 ℃ for 2 h. In order to verify the experimental diameter and size distributions of the PDMS microspheres, the Hinze-Kolmogorov theory is applied to predict the mean diameter, and a population balance model as well as the maximum entropy formalism are used to describe the size distribution. Close agreement is found between experimental and theoretical results. Furthermore, vinyl functional PDMS microspheres were coated with poly(methyl methacrylate) (PMMA) by spin coating with different concentrations of PMMA 1 solutions. The quality of the resulting PMMA shell is investigated using rheological measurements at 50 ℃ with a time-sweep procedure. The results strongly suggest that PMMA-coated PDMS microspheres react around 20 times slower than the uncoated ones, and that the PMMA shell significantly hinders the reaction between the PDMS microsphere and cross-linker. Thus the thin PMMA shells are very efficient in protecting the reactive PDMS microspheres, since the PMMA shell forms an impermeable barrier up to 50 ℃.

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Section: Pdms Microsphere Size Distribution From Experimentssupporting

confidence: 61%

Polydimethylsiloxane microspheres with poly(methyl methacrylate) coating: Modelling, preparation, and characterization

Ma¹,

Hansen

Hvilsted³

et al. 2015

Can J Chem Eng

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“…26 The pumpkin-like particles in acetic acid were caused by a prolonged nucleation, including the homocoagulation of primary nuclei into the final nuclei. Solventswollen gel layers at the particle surfaces acted as steric stabilizers.…”

Section: Resultsmentioning

confidence: 99%

Precipitation Polymerization in Acetic Acid: Study of the Solvent Effect on the Morphology of Poly(divinylbenzene)

et al. 2009

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This paper reports on two important results regarding the precipitation polymerization of poly(divinylbenzene) (PDVB) in acetic acid (HAc). (1) Acetic acid is a novel kind of solvent worthy of investigation because it is amphipathic and innoxious. Thus, two kinds of model solvents, methyl ethyl ketone (MEK) and n-heptane, were selected to investigate the solvent effect on the particle morphology of PDVB-55 during precipitation polymerization in acetic acid. Monodisperse PDVB-55 microspheres were obtained with an MEK content of 30 vol % and a DVB loading of 2 vol %. Odd-shaped particles were found to almost disappear when MEK was added. For MEK contents up to 90 vol %, space-filling macrogels consisting of small particles with diameters of around 10 nm were obtained. More homocoagulated particles were produced when n-heptane was added, for which concentrations up to 50 vol % gave rise to cauliflower-like particles. Thus, in the acetic acid system, microspheres, pumpkin-like particles, macrogels, and coagulum could be successfully obtained. (2) The preparation of nonpolar PDVB-55 particles could be more predictable. For the first time-based on the regulation of former studies--the regularity of the dispersive term (delta(d)) on the particle morphology for a PDVB precipitation polymerization system was reported. The three-dimensional Hansen solubility parameters were utilized to perfect the regularity of the Hildebrand solubility parameter. Microspheres or particles were formed in the range of moderate delta values for both parameters, i.e., delta = 20.2-24.3 MPa1/2 or delta = 16 MPa1/2. What was even more important, delta(d) was found to be around 15.4 MPa1/2, and delta(h) should be below 13.5 MPa1/2. Cyclohexane, cyclohexanone, n-butyl acetate, and 1,4-dioxane were used to verify this regularity, and positive results were obtained. Stable, uniform, and well-separated PDVB-55 microspheres and particles were produced as a result of interaction forces between oligomers, polymers, and solvent.

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“…However, the absence of stabilizer restricts the number of monomers and solvents. In addition, the concentration of the monomer is much lower (usually less than 3 wt.-% [13] ) to avoid particle agglomeration during the course of the polymerization.…”

Section: Introductionmentioning

confidence: 99%

Preparation of Monodisperse and Anion‐Charged Polystyrene Microspheres Stabilized with Polymerizable Sodium Styrene Sulfonate by Dispersion Polymerization

Zhang

Cao

Yang

2010

Macro Chemistry & Physics

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A novel dispersion polymerization system to produce “clean” polystyrene (PS) particles, using a polymerizable sodium styrene sulfonate (NaSS) as stabilizer, and a mixture of methanol/water (MeOH/H2O) as the reaction medium was investigated. The effects of the polymerization parameters, such as the methanol/water ratio in the medium, the concentration of the stabilizer, the initiator and the monomer on the resulting particles were studied. By observing the morphological changes of the PS particles by SEM and analyzing the surface chemical composition of these particles by XPS, it is found that this system had the following unique features: as little as 0.05 wt.‐% of NaSS (based on styrene as opposed to 5 wt.‐% for a routine dispersion polymerization system) was enough to prepare stable latex with monodisperse particles; as high as 20 vol.‐% of monomer (as opposed to 5 wt.‐% for polymerization system in the absence of surfactants) could be added into the polymerization system to produce monodisperse particles; surface‐charged and monodisperse particles with average diameters of approximately 470–1600 nm could be directly obtained.

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Precipitation Polymerization in Acetic Acid: Synthesis of Monodisperse Cross-Linked Poly(divinylbenzene) Microspheres

Cited by 55 publications

References 31 publications

Polydimethylsiloxane microspheres with poly(methyl methacrylate) coating: Modelling, preparation, and characterization

Polydimethylsiloxane microspheres with poly(methyl methacrylate) coating: Modelling, preparation, and characterization

Precipitation Polymerization in Acetic Acid: Study of the Solvent Effect on the Morphology of Poly(divinylbenzene)

Preparation of Monodisperse and Anion‐Charged Polystyrene Microspheres Stabilized with Polymerizable Sodium Styrene Sulfonate by Dispersion Polymerization

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