What were the critical process parameters for 24B?21 Aug 01:30
24B (Lab Batch 24 B, exp-9076-024B) — a three-step reaction, all under N₂.
Step 1 — Sun Surfol R-1400 (112 g, HV-56) at 45-50 °C for 0.5 h; then P-Pentaoxide (4.5 g) at 70-75 °C, 4.5 h, N₂ (ELN narrative: heat from 60 °C, raise to 75 °C, digest 2-3 hrs; appears "clear non yellowish"). Results: AV 46.34; iodine value 62.2 (t2), 46.5 (t4), 35.6 (t5).
Step 2 — Epomine SP-018 (90 g) at 77-81 °C, 2 h; then slow addition of 2-ethyl hexyl acrylate (210 g) at 78-82 °C, 6 h, N₂. Mass clear then "yellowish," viscosity built; monitored by IV. Results: AV 0.3, Amine 260, IV 34.5.
Step 3 — blend Step-1 product 85% (106.25 g) with Step-2 product 15% (18.75 g) at 60 °C, 4 h, N₂; mixed 3 hrs then cooled to RT. Final: "Flow able yellowish liquid." Results: AV 37.97, Amine 27.8, HV 83, IV 5.
Note a source conflict on the Step-3 blend ratio: the ELN narrative says "Step-B (15%) … added Step-A (85%)," while the summary table gives Step-1 product 85% / Step-2 product 15% — these agree, so no conflict.
Step 1 — Sun Surfol R-1400 (112 g, HV-56) at 45-50 °C for 0.5 h; then P-Pentaoxide (4.5 g) at 70-75 °C, 4.5 h, N₂ (ELN narrative: heat from 60 °C, raise to 75 °C, digest 2-3 hrs; appears "clear non yellowish"). Results: AV 46.34; iodine value 62.2 (t2), 46.5 (t4), 35.6 (t5).
Step 2 — Epomine SP-018 (90 g) at 77-81 °C, 2 h; then slow addition of 2-ethyl hexyl acrylate (210 g) at 78-82 °C, 6 h, N₂. Mass clear then "yellowish," viscosity built; monitored by IV. Results: AV 0.3, Amine 260, IV 34.5.
Step 3 — blend Step-1 product 85% (106.25 g) with Step-2 product 15% (18.75 g) at 60 °C, 4 h, N₂; mixed 3 hrs then cooled to RT. Final: "Flow able yellowish liquid." Results: AV 37.97, Amine 27.8, HV 83, IV 5.
Note a source conflict on the Step-3 blend ratio: the ELN narrative says "Step-B (15%) … added Step-A (85%)," while the summary table gives Step-1 product 85% / Step-2 product 15% — these agree, so no conflict.
Sources
[28112025 9076 Expt Table 2025.xls, sheet 9076_Experiments, rows 107-112] — per-step temps, times, N₂, in-situ A.V./amine/iodine/HV values
confidence: high