Synthesis and characterization of hydrophilic and spherical poly(glycerol dimethacrylate-co-glycerol-1,3-diglycerolate diacrylate) microbeads

Figures & data

Table 1. Experimental conditions for suspension copolymerization of GDGDA with GDMA.

GDMA (mL)	GDGDA (mL)	CycOH (mL)	MAA (mL)	DMAEM (mL)	SR (rpm)
1	3	4	–	–	500
2	2	4	–	–	500
3	1	4	–	–	500
4	0	4	–	–	500
2	2	2	–	–	500
2	2	3	–	–	500
2	2	4	–	–	500
2	2	5	–	–	500
2	2	6	–	–	500
2	2	4	–	–	250
2	2	4	–	–	500
2	2	4	–	–	750
2	2	4	–	–	1000
1.5	1.5	4	1	–	500
1.5	1.5	4	–	1	500

Table 2. The physical properties of ingredients used in the suspension polymerization system.

Ingredient	Density^a (g/mL, 25 °C)	Molecular weight^a (g/gmol)	Surface tension^b (dyn/cm)	Viscosity (cP, 20 °C)	Solubility parameter (cal/cm^3)^1/2
GDMA	1.12	228.24	36.64	85^a(25 °C)	10.02^e
GDGDA	1.237	348.35	48.51	8000–12000^a (25 °C)	ND
MAA	1.015	86.09	30.92	1.40 ^a	11.20^d
DMAEM	0.933	157.21	29.09	1.60^a	ND
Cyc-OH	0.948	100.2	32.50	50.2^c	11.40^d
WATER	1.00	18.015	72.27	1.00	23.4
^aTaken from supplier catalog.^bTaken from [30].^cTaken from [25].^dTaken from [31].^eTaken from [32].ND: not determined.

Figure 1 Effect of monomer composition on the size distribution of poly(GDMA-co-GDGDA) beads.

Table 3. The effect of GDMA/GDGDA volume ratio on the microbead yield, average size, and size distribution of poly(GDMA-co-GDGDA) beads.

GDMA (mL)/GDGDA (mL)	Microbead yield (wt%)	D p (μm)	SD (μm)	CV
1/3	97.4	180	67.8	37.7
2/2	99.4	248	61.8	24.9
3/1	98.3	191	60.0	31.5
4/0	97.3	231	43.6	18.8

Figure 2 Optical micrographs of poly(GDMA-co-GDGDA) beads synthesized with different GDMA/GDGDA ratios. GDMA/GDGDA ratios (mL/mL) are: (A) 1/3, (B) 2/2, (C) 3/1 and (D) 4/0. Original magnification: 125×.

Figure 3 ESRs of poly(GDMA-GDGDA) gel beads synthesized with different GDMA/GDGDA volume ratios at different pHs.

Table 4. The effect of stirring rate on the microbead yield, average size, and size distribution of poly(GDMA-co-GDGDA) beads.

Stirring rate (rpm)	Microbead yield (wt%)	D p (μm)	SD (μm)	CV
250	98.1	278	64.7	30.3
500	99.4	248	61.8	24.9
750	95.6	34	10.0	29.3
1000	98.6	24	7.8	32.9

Figure 4 Effect of stirring rate on the size distribution of poly(GDMA-co-GDGDA) beads.

Figure 5 Optical micrographs of poly(GDMA-co-GDGDA) beads with different stirring rates. Stirring rates: (A) 250, (B) 500, (C) 750, and (D) 1000 rpm, respectively. Original magnification: 125×.

Figure 6 ESRs of poly(GDMA-co-GDGDA) gel beads synthesized with different stirring rates at different pH values.

Table 5. The effect of amount of diluent on the microbead yield, average size, and size distribution of poly(GDMA-co-GDGDA) beads.

Cyclohexanol (mL)	Microbead yield (wt%)	D p (μm)	SD (μm)	CV
2	98.5	292	68.0	23.3
3	97.9	240	50.3	21.0
4	99.4	248	61.8	24.9
5	96.8	234	58.0	24.8
6	98.2	276	68.7	24.9

Figure 7 The effect of amount of diluent on the size distribution of poly(GDMA-co-GDGDA) gel beads.

Figure 8 Optical micrographs of poly(GDMA-co-GDGDA) beads synthesized with different amounts of diluent. Amounts of diluent: (A) 2, (B) 3, (C) 4, and (D) 5 mL respectively. Original Magnification 125×.

Figure 9 ESRs of poly(GDMA-co-GDGDA) gel beads synthesized with different amounts of diluent at different pH values.

Table 6. The effect of functional monomer type on the microbead yield, average size, and size distribution of terpolymer beads including GDMA, GDGDA, and functional monomer.

Functional monomer	Microbead yield (wt%)	D p (μm)	SD (μm)	CV
None	99.4	248	61.8	24.9
MAA	86.8	106	12.7	12.0
DMAEM	65.7	33	8.38	25.3

Figure 10 The effect of functional monomer type on the size distribution of terpolymer microbeads including GDMA, GDGDA, and functional monomer.

Figure 11 Optical micrographs of terpolymer beads synthesized with different functional monomers. Functional monomers: (A) None, (B) MAA, and (C) DMAEM. Original Magnification 125× for (A) and (B) and 500× for (C).

Figure 12 ESRs of terpolymer gel beads synthesized with different functional monomers at different pH values.

http://www.chemspider.com/Chemical-Structure.67171.html (GDMA); http://www.chemspider.com/Chemical-Structure.3807655.html (GDGDA); http://www.chemspider.com/Chemical-Structure.3951.html (MAA); http://www.chemspider.com/Chemical-Structure.16879.html (DMAEM); http://www.chemspider.com/Chemical-Structure.7678.html (Cyc-OH); http://www.chemspider.com/Chemical-Structure.937.html (H2O).

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