av
31.5
target 43.2 · -27.1% vs target
Conclusion — verbatim from the source
“Application test against violet- 27 / 23 ( Resolubility ) is good only gloss less.”
LBN 36.pdf, page 2
Aim
To develop product equivalent to reference product
Raw materials
| # | Material | Source | Qty | Purity % |
|---|---|---|---|---|
| 1 | Surfol R-1400 (R-53/07032024) | Sun shield | 350 gms | |
| 2 | Polyphosphoric acid | Commercial | 4 gms | |
| 3 | Phosphorous pentaoxide | Commercial | 4.35 gms | |
| 4 | Epomine SP-018 | Nippon | 60 gms | 100 |
| 4 | Toluene | Commercial | 190 gms | 99 |
| 5 | AIBN catalyst | Himedia | 0.4 gms | 100 |
| 5 | 2 ethyl hexyl acrylate | 140 gms | 100 | |
| 6 | AIBN catalyst | 0.64 gms | 100 |
Reaction conditions (optimized)
atmosphere: N2
Process
| Step | Conditions | Charged | What happened | Results | ||||||||||||||||
|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|
|
Step 1
Phosphate ester
28112025 9076 Expt Table 2025.xls · LBN 36.pdf
|
temperature: 56 then 74 oC · ELN: 58-75 °Catmosphere: N2time: 4 h · ELN: 5 h |
Surfol R-1400 HV-59 (R-53/07032024) 350 g PolyPhosphoric acid 4 g Phosphorous pentaoxide 4.35 g [Table]
|
Step 1) Phosphate ester- RBF with Surfol R-1400 heated to 58 deg C and then slowly added Polyphosphoric acid followed by P2O5 into it under N2 atmosphere. Digested this for 3 hrs at 70-75 deg C. Cool to RT and filter through Nylon Mesh AV-34.2 [ELN]
Expt Table remarks: After digestion cool to RT and filter through Nylon mesh [Table] Appearance- yellowish clear [ELN]
Step-by-step (2 entries)
|
acid_value 34.2 | ||||||||||||||||
|
Step 2
Acrylate intermediate
28112025 9076 Expt Table 2025.xls · LBN 36.pdf
|
temperature: 68-72 oC · ELN: 65-72 °Catmosphere: N2time: 5.5 h (ELN) |
Epomine SP-018 60 g Toluene 190 ml AIBN catalyst 0.4 g 2 ethyl hexyl acrylate 140 g (feed over 1.15 hr) AIBN catalyst 0.64 g [Table]
|
Step 2) Acrylate intermediate- RBF with Epoimin SP-18 with Toluene solvent (Dissolved AIBN- 0.4 gm) heated to 66-72 deg C under N2 atmosphere. Slowly feed of 2-ethyl hexyl acylate (with dissolved AIBN- 0.64 gm) into it over 1.15 hrs and continue reaction for 3 hrs. Cool to RT removed toluene under reduced pressure. (IV-13.2) [ELN]
Initially turbid After 1 hr clear mass [Table] Appearance- yellowish clear [ELN]
Step-by-step (3 entries)
|
acid_value 31.5iodine_value 6.22iodine_value 13.2 | ||||||||||||||||
|
Step 3
Neutralization
28112025 9076 Expt Table 2025.xls · LBN 36.pdf
|
temperature: 58-60 oC · ELN: 56-61 °Catmosphere: N2time: 2.5 hr · ELN: 3.5 h |
Step - 1 Product 170 g Step - 2 Product 30 g (feed slowly over 30 min) [Table]
|
Step 3) Neutralization - RBF with acrylate intermediate of step-1) (15%) heated to 56 deg C under N2 atmosphere. Slowly feed of step-2) (85%) Phosphate ester into it over 30 min and continue for 3 hrs. Cool to RT and filter through Nylon Mesh. AV- 31.5/ IV-6.22 [ELN]
Step-by-step (2 entries)
|
iodine_value 13.2acid_value 31.5iodine_value 6.22 |
Critical parameters — measured vs target
| Parameter | Target | Measured |
|---|---|---|
| aminev | 30.1 | |
| av | 43.2 | 31.5 |
Where this record comes from
LBN 36.pdf
— lab journal (primary source)
28112025 9076 Expt Table 2025.xls
— researcher summary (cross-check)
Something wrong on this page? Record a correction
Your correction is permanent: it survives every re-extraction and the field can no longer be changed by the system.
Field-by-field provenance (20 fields) — for auditors
2 extraction fragments · merged 2026-08-25 · 0 human-validated fields
Fix a wrong or missing extraction side-by-side with the original:
qwen-extract--lbn-36--lbn-36
expt-block--36
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| conditions.atmosphere | LBN 36.pdf LBN 36.pdf, pages 1-2 | qwen-tasks/extract-fragment.md@unversioned | high |
| materials[0] | LBN 36.pdf LBN 36.pdf, pages 1-2 | qwen-tasks/extract-fragment.md@unversioned | high |
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| materials[2] | LBN 36.pdf LBN 36.pdf, pages 1-2 | qwen-tasks/extract-fragment.md@unversioned | high |
| materials[3] | LBN 36.pdf LBN 36.pdf, pages 1-2 | qwen-tasks/extract-fragment.md@unversioned | high |
| materials[4] | LBN 36.pdf LBN 36.pdf, pages 1-2 | qwen-tasks/extract-fragment.md@unversioned | high |
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| materials[6] | LBN 36.pdf LBN 36.pdf, pages 1-2 | qwen-tasks/extract-fragment.md@unversioned | high |
| materials[7] | LBN 36.pdf LBN 36.pdf, pages 1-2 | qwen-tasks/extract-fragment.md@unversioned | high |
| process_steps[0] | LBN 36.pdf LBN 36.pdf, pages 1-2 | qwen-tasks/extract-fragment.md@unversioned | high |
| process_steps[1] | LBN 36.pdf LBN 36.pdf, pages 1-2 | qwen-tasks/extract-fragment.md@unversioned | high |
| process_steps[2] | LBN 36.pdf LBN 36.pdf, pages 1-2 | qwen-tasks/extract-fragment.md@unversioned | high |
| critical_parameters[0] | LBN 36.pdf LBN 36.pdf, pages 1-2 | qwen-tasks/extract-fragment.md@unversioned | high |
| critical_parameters[1] | LBN 36.pdf LBN 36.pdf, pages 1-2 | qwen-tasks/extract-fragment.md@unversioned | high |
| outcome | LBN 36.pdf LBN 36.pdf, pages 1-2 | qwen-tasks/extract-fragment.md@unversioned | high |
| process_steps[3] | 28112025 9076 Expt Table 2025.xls sheet 9076_Experiments, batch block '36' | qwen-tasks/extract-expt-block.md@unversioned | high |
| process_steps[4] | 28112025 9076 Expt Table 2025.xls sheet 9076_Experiments, batch block '36' | qwen-tasks/extract-expt-block.md@unversioned | high |
| process_steps[5] | 28112025 9076 Expt Table 2025.xls sheet 9076_Experiments, batch block '36' | qwen-tasks/extract-expt-block.md@unversioned | high |
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"aim": "To develop product equivalent to reference product",
"conclusion": "Application test against violet- 27 / 23 ( Resolubility ) is good only gloss less.",
"conditions": {
"atmosphere": "N2"
},
"materials": [
{
"sr_no": 1,
"name": "Surfol R-1400 (R-53/07032024)",
"source": "Sun shield",
"quantity": 350,
"unit": "gms"
},
{
"sr_no": 2,
"name": "Polyphosphoric acid",
"source": "Commercial",
"quantity": 4,
"unit": "gms"
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{
"sr_no": 3,
"name": "Phosphorous pentaoxide",
"source": "Commercial",
"quantity": 4.35,
"unit": "gms"
},
{
"sr_no": 4,
"name": "Epomine SP-018",
"source": "Nippon",
"quantity": 60,
"unit": "gms",
"purity_pct": 100
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{
"sr_no": 4,
"name": "Toluene",
"source": "Commercial",
"quantity": 190,
"unit": "gms",
"purity_pct": 99
},
{
"sr_no": 5,
"name": "AIBN catalyst",
"source": "Himedia",
"quantity": 0.4,
"unit": "gms",
"purity_pct": 100
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{
"sr_no": 5,
"name": "2 ethyl hexyl acrylate",
"quantity": 140,
"unit": "gms",
"purity_pct": 100
},
{
"sr_no": 6,
"name": "AIBN catalyst",
"quantity": 0.64,
"unit": "gms",
"purity_pct": 100
}
],
"process_steps": [
{
"step": 1,
"time_hrs": 5,
"temperature": "58-75 °C",
"pressure": "N2",
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{
"action": "Step 1) Phosphate ester- RBF with Surfol R-1400 heated to 58 deg C and then slowly added Polyphosphoric acid followed by P2O5 into it under N2 atmosphere. Digested this for 3 hrs at 70-75 deg C. Cool to RT and filter through Nylon Mesh AV-34.2"
}
],
"remarks": "Appearance- yellowish clear",
"results": [
{
"type": "AV",
"value": "34.2",
"verbatim": "AV-34.2",
"parameter": "unlabelled"
}
]
},
{
"step": 2,
"time_hrs": 5.5,
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"action": "Step 2) Acrylate intermediate- RBF with Epoimin SP-18 with Toluene solvent ( Dissolved AIBN- 0.4 gm) heated to 66-72 deg C under N2 atmosphere. Slowly feed of 2-ethyl hexyl acylate (with dissolved AIBN- 0.64 gm) into it over 1.15 hrs and continue reaction for 3 hrs. Cool to RT removed toluene under reduced pressure. ( IV-13.2)"
}
],
"remarks": "Appearance- yellowish clear",
"results": [
{
"type": "IV",
"value": "13.2",
"verbatim": "IV-13.2",
"parameter": "unlabelled"
}
]
},
{
"step": 3,
"time_hrs": 3.5,
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"procedure": [
{
"action": "Step 3) Neutralization - RBF with acrylate intermediate of step-1) (15%) heated to 56 deg C under N2 atmosphere. Slowly feed of step-2) (85%) Phosphate ester into it over 30 min and continue for 3 hrs. Cool to RT and filter through Nylon Mesh. AV- 31.5/ IV-6.22"
}
],
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{
"type": "AV",
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"parameter": "unlabelled"
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}
]
},
{
"step": 1,
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"name": "Surfol R-1400 HV-59 (R-53/07032024)",
"qty": "350 g",
"role": "reactant",
"verbatim": "i) Surfol R-1400 HV-59 (R-53/07032024)"
},
{
"name": "PolyPhosphoric acid",
"qty": "4 g",
"role": "reactant",
"verbatim": "ii) PolyPhosphoric acid"
},
{
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"qty": "4.35 g",
"role": "reactant",
"verbatim": "ii) Phosphorous pentaoxide"
}
],
"procedure": [
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"verbatim": "56"
},
{
"seq": 2,
"temperature": "74 oC",
"time_h": "4",
"atmosphere": "N2",
"verbatim": "74 / 4 / N2"
}
],
"conditions": {
"temperature": "56 then 74 oC",
"atmosphere": "N2",
"time_h": "4 h"
},
"results": [
{
"parameter": "acid_value",
"value": "34.2",
"unit": "as printed",
"verbatim": "34.2"
}
],
"remarks": "Expt Table remarks: After digestion cool to RT and filter through Nylon mesh"
},
{
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"qty": "60 gm",
"role": "reactant",
"verbatim": "i) Epomine SP- 018"
},
{
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"role": "solvent",
"verbatim": "ii) Toluene"
},
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"qty": "0.4 gm",
"role": "catalyst",
"verbatim": "iii) AIBN catalyst"
},
{
"name": "2 ethyl hexyl acrylate",
"qty": "140 gm",
"role": "reactant",
"addition": "feed over 1.15 hr at 68-72 oC under N2 (cell layout shows staged feed, not start-of-step charge)",
"verbatim": "iv) 2 ethyl hexyl acrylate"
},
{
"name": "AIBN catalyst",
"qty": "0.64 gm",
"role": "catalyst",
"verbatim": "v) AIBN catalyst"
}
],
"procedure": [
{
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"temperature": "68-70 oC",
"time_h": "0.15",
"verbatim": "68-70 / 0.15"
},
{
"seq": 2,
"temperature": "68-72 oC",
"time_h": "1.15 hr feed",
"atmosphere": "N2",
"action": "feed 2 ethyl hexyl acrylate (140 gm)",
"verbatim": "68-72 / 1.15\n hr feed / N2 / Feed"
},
{
"seq": 3,
"temperature": "68-72 oC",
"time_h": "3.5",
"atmosphere": "N2",
"action": "add second AIBN catalyst portion (0.64 gm)",
"verbatim": "68-72 / 3.5 / N2"
}
],
"conditions": {
"temperature": "68-72 oC",
"atmosphere": "N2"
},
"results": [
{
"parameter": "acid_value",
"value": "31.5",
"verbatim": "AV-31.5"
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{
"parameter": "iodine_value",
"value": "6.22",
"verbatim": "IV-6.22"
}
],
"observations": [
"Initially turbid After 1 hr clear mass"
]
},
{
"step": 3,
"materials": [
{
"name": "Step - 1 Product",
"qty": "170 gm",
"role": "intermediate",
"verbatim": "Step - 1 Product"
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{
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"qty": "30 gm",
"role": "intermediate",
"addition": "feed slowly over 30 min",
"verbatim": "Step - 2 Product "
}
],
"procedure": [
{
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"action": "feed Step-2 product slowly over 30 min",
"temperature": "58-60 oC",
"time_h": "2.5",
"atmosphere": "N2",
"verbatim": "58-60 / 2.5 hr / N2 / Feed slowly \nover 30 min"
},
{
"seq": 2,
"action": "Stirrer well and disperse amine",
"verbatim": "Stirrer well and\n disperse amine"
}
],
"conditions": {
"temperature": "58-60 oC",
"atmosphere": "N2",
"time_h": "2.5 hr"
},
"results": [
{
"parameter": "iodine_value",
"value": "13.2",
"verbatim": "IV-13.2"
}
]
}
],
"critical_parameters": [
{
"no": 1,
"parameter": "aminev",
"reference_value": "30.1"
},
{
"no": 2,
"parameter": "av",
"reference_value": "43.2",
"value": "31.5"
}
],
"outcome": {
"status": "ok",
"basis": "Application test against violet- 27 / 23 ( Resolubility ) is good only gloss less.",
"citation": "LBN 36.pdf, page 2"
}
}