Experiments / Batch 23
Batch 23 no result yet
2024-8-04 ·
also written as Lab Batch 23 · Lab Batch23 · 23
Aim
To develop product equivalent to reference product
Observations
Appearance was clear non yellowish. (Step-A) initially found clear reaction mass, later on changed to yellowish in nature. Built viscosity at end of reaction. (Step-B) Flow able yellowish liquid. (Step-C) Expt Table remarks: Strength/gloss for C black good/ Resolubility issue i) With 3% MPA solvent and ii) without solvent; Final product: AV-42.67/amine-39.8/HV-55.32/SAP-63.5/IV-7.22
Raw materials
| # | Material | Source | Qty | Purity % |
|---|---|---|---|---|
| 1 | Sun Surfol R-1400- | FOIL | 1010 gms | 100 |
| 2 | P-Pentaoxide | FOIL | 47.16 gms | 100 |
| 3 | Epomine 018- | 90 gms | 100 | |
| 4 | 2-ethyl hexyl acrylate | 210 gms | 100 |
Reaction conditions (optimized)
atmosphere: nitrogen
Process
| Step | Conditions | Charged | What happened | Results | ||||||||||||
|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|
|
Step 1
Step A
28112025 9076 Expt Table 2025.xls · Lab Batch 23.pdf
|
temperature: 45-50; then 70-75 °C · ELN: 65-85 °Catmosphere: N2time: 0.5; then 4.5 h · ELN: 1-5 h |
Sun Surfol R-1400- HV-56 1010 g Phosphorous pentaoxide 47.16 g Epomine SP- 018 (Table, no quantity given)
|
Step- A To main reactor added Sun Surfol R-1400 under stirring and nitrogen atmosphere temp. 60 deg increased temp slowly with addition of P-Pentaoxide. Upon feed completion temp raised to 75 deg C and digested for 2-3 hrs. Appearance was clear non yellowish. Upon digestion cooled to RT. [ELN]
2024-8-04 12:17:59 [ELN remarks]
Step-by-step (2 entries)
|
acid_value 50iodine_value 49iodine_value 37.2 | ||||||||||||
|
Step 2
Step B
28112025 9076 Expt Table 2025.xls · Lab Batch 23.pdf
|
temperature: 75-81; then 78-82 °C · ELN: 55-80 °Catmosphere: N2time: 2; then 6 h · ELN: 1-8 h |
Epomine 018- 90 g (ELN) 2 ethyl hexyl acrylate 210 g
|
Step-B To main reactor added Epomine 018- reaction mass under stirring and nitrogen atmosphere temp. 75 deg Started slowly addition of 2- ethyl hexyl acrylate slowly. initially found clear reaction mass, later on changed to yellowish in nature. Built viscosity at end of reaction. [ELN]
Step-by-step (2 entries)
|
acid_value 1.1amine_value 256iodine_value 37.2 | ||||||||||||
|
Step 3
Step C
28112025 9076 Expt Table 2025.xls · Lab Batch 23.pdf
|
temperature: 60 °C · ELN: 60-65 °Catmosphere: N2time: 4 h · ELN: 1-5 h |
Step- 1 product (80) 800 g Step - 2 Product (20) 200 g
|
Step-C To main reactor added Step- B reaction mass (20%) - reaction mass under stirring and nitrogen atmosphere temp. 55 deg Started slowly addition of Step- A (80%) reaction mass in it. initially found clear reaction mass, yellowish in nature with viscosity. Mixed for 3 hrs then cooled to RT. [ELN]
Flow able yellowish liquid. [ELN remarks] Strength/gloss for C black good/ Resolubility issue i) With 3% MPA solvent and ii) without solvent [Table remarks]
Step-by-step (1 entry)
|
acid_value 42.67amine_value 39.8hydroxyl_value 55.32saponification_value 63.5iodine_value 7.22 |
Critical parameters — measured vs target
| Parameter | Target | Measured |
|---|---|---|
| aminev | 30.1 | |
| av | 43.2 |
Where this record comes from
Lab Batch 23.pdf
— lab journal (primary source)
28112025 9076 Expt Table 2025.xls
— researcher summary (cross-check)
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Field-by-field provenance (16 fields) — for auditors
2 extraction fragments · merged 2026-08-25 · 0 human-validated fields
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qwen-extract--lab-batch-23--lab-batch-23
expt-block--23
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"materials": [
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"unit": "gms",
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"purity_pct": "100"
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"action": "Step-B To main reactor added Epomine 018- reaction mass under stirring and nitrogen atmosphere temp. 75 deg Started slowly addition of 2- ethyl hexyl acrylate slowly. initially found clear reaction mass, later on changed to yellowish in nature. Built viscosity at end of reaction."
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"remarks": "Flow able yellowish liquid. AV-42.67/amine-39.8/HV-55.32 /SAP-63.5/IV-7.22"
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"verbatim": "Amine 256"
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"time_h": "4"
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"reference_value": "30.1"
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}