Batch 48 Q OK
Synthesis of BYK-9076 analog (Batch 48)
Step-I: Clear mass, No-Turbidity Step-II: Clear transparent Step-III: Yellowish, No foam Batch 48Q: clear transparent Mass Step I: Clear mass, No-Turbidity, AV - 52.52, MONO - 24.4 h, Diacetate - 51.76%. Step II: Clear transparent. Step III: Yellowish, No foam, AU - 44.36, Amine - 36.25. Batch 48Q: AU - 52, Amine - 31.67. Charged LUB 1010 - 178 gm Feed of P2O5 - No particles Clear mass, No-Turbidity, AV - 52.52 Charged - Sp-18 Feed of 2-ethyl hexyl Acylate over - 2 hrs. Clear transparent Charged Acylate Intermediate, feed of phosphate 85gm over 25min. clear mass Yellowish, No foam., AU - 44.36, Amine - 36.25 Charged Acylate slowly added DMS. / clear transparent Mass. slow addition of phosphate ester. AU - 52, Amine - 31.67
Step-I: Charged LUB 1010 (178 gm) at RT-50/N2, fed P2O5 over 1.5 hrs at 75-77°C/N2, held at 77°C for 1 hr. Step-II: Charged Sp-18 at 75-79°C/N2, fed 2-ethyl hexyl Acylate over 2 hrs at 78-79°C/N2, held 5.5 hrs to clear transparent. Step-III: Charged Acylate Intermediate, fed phosphate ester (85%) over 25 min at 55-59°C/N2, held 1.5 hrs. Batch 48Q: Charged Acylate Intermediate (15%) + DMS (0.5%), then phosphate (85%) at 55-75°C/N2. Step I: Phosphate ester synthesis from LUB-1010 and P2O5. Step II: Acylation of Epamine Sp-18 with 2-ethyl hexyl Acylate. Step III: Neutralization of Phosphate Ester and Acylate Intermediate. Variant Batch 48Q includes DMS.
| # | Material | Source | Qty | Purity % | Mol. wt. | Moles | Role |
|---|---|---|---|---|---|---|---|
| 1 | Vicaspin LUB 1010 (R225100845) Bu- EO-PO HV-62.3/ MW-900 ×4 | Viswaat | 178 gms | 900 | 0.197 | reactant | |
| 2 | P2O5 ×4 | Commercial | 9.357 gms | 141.94 | 0.0658 | reactant | |
| 3 | Epomine SP-018 ×3 | Nippon | 30 gms | 100 | reactant | ||
| 4 | 2 ethyl hexyl acrylate ×4 | 70 gms | 100 | 184.27 | reactant | ||
| DMS (Batch 48Q) ×3 | 0.5% % | reactant | |||||
| Phosphate Ester (Step-I) | 85 gm | reactant | |||||
| Acylate Intermediate (Step-II) | 15 gm | reactant |
| Step | Conditions | Charged | What happened | Results | ||||||||||||
|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|
|
Step 1
Phosphate ester
Lab Batch 48 Q.pdf · 9076 Exp 48-60_1.pdf
|
temperature: 58-75 °Catmosphere: N2time: 5 hrs |
Vicaspin LUB 1010 (R225100845) Bu- EO-PO HV-62.3/ MW-900 (Viswaat) 178 gms (MW 900, 0.197 mol) P2O5 (Commercial) 9.357 gms (MW 141.94, 0.0658 mol)
|
Step 1) Phosphate ester - RBF with Vicaspin LUB 1010 (R225100845) Bu- EO-PO HV-62.3/ MW-900 heated to 50 deg C and then slowly added P2O5 into it under N2 atmosphere. Digested this for 3 hrs at 70-75 deg C. Cool to RT. [ELN]
|
acid_value 52.52mono 24.44di 51.76free_acid 0.24 | ||||||||||||
|
Step 2
Acrylate intermediate
Lab Batch 48 Q.pdf · 9076 Exp 48-60_1.pdf
|
temperature: 78-82 °Catmosphere: N2time: 6.5 hrs |
Epomine SP-018 (Nippon) 30 gms (100 %) 2 ethyl hexyl acrylate 70 gms (100 %, MW 184.27)
|
Step 2) Acrylate intermediate - RBF with Epomine SP-018 heated to 78-81 deg C under N2 atmosphere. Slowly feed of 2-ethyl hexyl acrylate over 2 hrs and continue reaction for 5 hrs. Monitoring of reaction done by IV. Cool to RT. Above said reaction acrylate mass (15%) in RBF with N2 @ 65-75, feed of DMS-0.5 % @ 1 hrs, cool to RT - clear yellow brown liquid. [ELN]
Appearance - yellowish clear [ELN remarks]
|
iodine_value 26.1 | ||||||||||||
|
Step 3
Neutralization / Batch-48Q (rework from above batch)
Lab Batch 48 Q.pdf · 9076 Exp 48-60_1.pdf
|
temperature: 55-75 then 55-60 °C (Notes rows) · ELN: 56-61 °Catmosphere: N2 (ELN) · Notes: atmosphere cell not writtentime: 0.5 + 2.5 h (Notes rows) · ELN: 3.5 hrs |
Rm. from above batch (quantity not written) [Notes] Acrylate Intermediate 15 g [Notes] DMS (dimethyl sulphate) 0.5 g [Notes] Phosphate (ester) 85 g [Notes]
|
Step 3) Neutralization - RBF with acrylate intermediate of above step-2) heated to 56 deg C under N2 atmosphere. Slowly feed of step-1) 85% Phosphate ester into it over 30 min and continue for 3 hrs. Cool to RT and filter through Nylon Mesh. [ELN]
Tested on Violet 23 resolubility ok [ELN]
Step-by-step (2 entries)
|
acid_value 52amine_value 31.67iodine_value 3.48SAP 84.9HV 38.6 | ||||||||||||
|
Step 4
Batch 48Q (RM from above Batch)
9076 Exp 48-60_1.pdf
|
— |
Acylate Intermediate DMS phosphate
|
— | — |
| Parameter | Target | Measured |
|---|---|---|
| aminev | 30.1 | 31.6 |
| av | 43.2 | 52 |
| Parameter | This sample | Standard (BYK 9076 Standard) |
|---|---|---|
| Viscosity | 30 sec | 29 sec |
| Gloss | 60.3 | 62.9 |
| Colour Strength | 98-99.00% | 1 |
| Resolubility | 5 | 4 |
| Transparency | Opaque | Ref as Std |
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Field-by-field provenance (38 fields) — for auditors
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| process_steps[6] | 9076 Exp 48-60_1.pdf pages 1-3 | qwen-tasks/extract-fragment.md@unversioned | medium |
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},
"materials[1].molecular_wt": {
"validated_by": "Claude direct analysis (Rishi-authorized 2026-08-21)",
"date": "2026-08-21"
},
"materials[1].moles": {
"validated_by": "Claude direct analysis (Rishi-authorized 2026-08-21)",
"date": "2026-08-21"
},
"materials[3].molecular_wt": {
"validated_by": "Claude direct analysis (Rishi-authorized 2026-08-21)",
"date": "2026-08-21"
},
"aim": {
"validated_by": "FOIL review",
"date": "2026-08-25"
}
},
"corrections_applied": [
"corr-0024",
"corr-0025",
"corr-0026",
"corr-0027",
"corr-0028",
"corr-0046"
]
},
"aim": "Synthesis of BYK-9076 analog (Batch 48)",
"conclusion": "Tested on Violet 23 resolubility ok",
"conditions": {
"atmosphere": "N2",
"other": "Step-I: RT-50 to 77°C; Step-II: 75-81°C; Step-III: 55-59°C; Batch 48Q: 55-75°C; Step I: RT-50 to 77°C; Step II: 75-79 to 77-81°C; Step III: RT-55-59 to 55-60°C"
},
"materials": [
{
"sr_no": 1,
"name": "Vicaspin LUB 1010 (R225100845) Bu- EO-PO HV-62.3/ MW-900",
"source": "Viswaat",
"quantity": 178,
"unit": "gms",
"molecular_wt": "900",
"moles": "0.197"
},
{
"sr_no": 2,
"name": "P2O5",
"source": "Commercial",
"quantity": 9.357,
"unit": "gms",
"molecular_wt": "141.94",
"moles": "0.0658"
},
{
"sr_no": 3,
"name": "Epomine SP-018",
"source": "Nippon",
"quantity": 30,
"unit": "gms",
"purity_pct": 100
},
{
"sr_no": 4,
"name": "2 ethyl hexyl acrylate",
"quantity": 70,
"unit": "gms",
"purity_pct": 100,
"molecular_wt": "184.27"
},
{
"name": "Vicalpin - LUB-1010 Bu-Eo-Po",
"quantity": "178",
"unit": "gm",
"role": "unknown",
"molecular_wt": "900",
"moles": "0.197",
"notes": "HV-62.3",
"role_verbatim": "polyol"
},
{
"name": "P2O5",
"quantity": "9.35",
"unit": "gm",
"role": "unknown",
"molecular_wt": "141.94",
"moles": "0.0658",
"role_verbatim": "phosphorylating agent"
},
{
"name": "Epamine Sp-18",
"quantity": "30",
"unit": "gm",
"role": "unknown",
"role_verbatim": "amine"
},
{
"name": "2-ethyl hexyl Acylate",
"quantity": "70",
"unit": "gm",
"role": "unknown",
"molecular_wt": "184.27",
"role_verbatim": "acylating agent"
},
{
"name": "DMS",
"quantity": "0.5%",
"unit": "%",
"role": "unknown",
"role_verbatim": "co-solvent (Batch 48Q)"
},
{
"name": "Vicalpin - LUB-1010",
"quantity": "178",
"unit": "gm",
"role": "reactant",
"notes": "Bu-Eo-Po - MW=900, HV-62.3"
},
{
"name": "P2O5",
"quantity": "9.35",
"unit": "gm",
"role": "reactant"
},
{
"name": "Epamine Sp-18",
"quantity": "30",
"unit": "gm",
"role": "reactant"
},
{
"name": "2-ethyl hexyl Acylate",
"quantity": "70",
"unit": "gm",
"role": "reactant"
},
{
"name": "DMS",
"quantity": "0.5",
"unit": "%",
"role": "unknown",
"notes": "Used in Batch 48Q",
"role_verbatim": "additive"
},
{
"name": "Vicalpin - LUB-1010, Bu-Eo-Po, MW=900, HV-62.3",
"quantity": "178",
"unit": "gm",
"molecular_weight": "900",
"moles": "0.197",
"role": "reactant"
},
{
"name": "P2O5",
"quantity": "9.35",
"unit": "gm",
"molecular_weight": "141.94",
"moles": "0.0658",
"role": "reactant"
},
{
"name": "2-ethyl hexyl Acylate",
"quantity": "70",
"unit": "gm",
"molecular_weight": "184.27",
"role": "reactant"
},
{
"name": "Phosphate Ester (Step-I)",
"quantity": "85",
"unit": "gm",
"percentage": "85%",
"role": "reactant"
},
{
"name": "Acylate Intermediate (Step-II)",
"quantity": "15",
"unit": "gm",
"percentage": "15%",
"role": "reactant"
},
{
"name": "DMS (Batch 48Q)",
"quantity": "0.5%",
"unit": "gm",
"percentage": "0.5%",
"role": "reactant"
}
],
"process_steps": [
{
"step": 1,
"time": "5 hrs",
"temperature": "58-75 °C",
"procedure": [
{
"action": "Step 1) Phosphate ester- RBF with Vicaspin LUB 1010 (R225100845) Bu- EO-PO HV-62.3/ MW-900 heated to 50 deg C and then slowly added P2O5 into it under N2 atmosphere. Digested this for 3 hrs at 70-75 deg C. Cool to RT AV-52.52"
}
],
"remarks": "Mono-24.44 / Di- 51.76/ Free acid-0.24",
"results": [
{
"measurement": "AV",
"value": "52.52",
"verbatim": "Cool to RT AV-52.52",
"parameter": "unlabelled"
}
]
},
{
"step": 2,
"time": "6.5 hrs",
"temperature": "78-82 °C",
"procedure": [
{
"action": "Step 2) Acrylate intermediate- RBF with Epomine SP- 018 heated to 78-81 deg C under N2 atmosphere. Slowly feed of 2-ethyl hexyl acrylate over 2 hrs and continue reaction for 5 hrs. Monitoring of reaction done by IV. IV-26.1 @ 5.5 hrs Cool to RT Above said reaction acrylate mass (15%) in RBF with N2 @ 65-75 feed of DMS-0.5 % @1 hrs cool to RT clear yellow brown liquid."
}
],
"remarks": "Appearance- yellowish clear",
"results": [
{
"measurement": "IV",
"value": "26.1",
"verbatim": "IV-26.1 @ 5.5 hrs",
"parameter": "unlabelled"
}
]
},
{
"step": 3,
"time": "3.5 hrs",
"temperature": "56-61 °C",
"procedure": [
{
"action": "Step 3) Neutralization - RBF with acrylate intermediate of above step-2) heated to 56 deg C under N2 atmosphere. Slowly feed of step-1) 85% Phosphate ester into it over 30 min and continue for 3 hrs. Cool to RT and filter through Nylon Mesh."
}
],
"remarks": "AV-52/Amine-31.67 /IV-3.48/SAP-84.9/HV-38.6 Tested on Violet 23 resolubility ok",
"results": [
{
"measurement": "AV",
"value": "52",
"verbatim": "AV-52",
"parameter": "unlabelled"
},
{
"measurement": "Amine",
"value": "31.67",
"verbatim": "Amine-31.67",
"parameter": "unlabelled"
},
{
"measurement": "IV",
"value": "3.48",
"verbatim": "IV-3.48",
"parameter": "unlabelled"
},
{
"measurement": "SAP",
"value": "84.9",
"verbatim": "SAP-84.9",
"parameter": "unlabelled"
},
{
"measurement": "HV",
"value": "38.6",
"verbatim": "HV-38.6",
"parameter": "unlabelled"
}
]
},
{
"name": "Step-I Phosphate Ester",
"process": [
{
"time": "0.5",
"temperature": "RT-50 / N2",
"observation": "Charged LUB 1010 - 178 gm"
},
{
"time": "1.5",
"temperature": "RT-75-77 / N2",
"observation": "Feed of P2O5 - No particles"
},
{
"time": "1 hrs",
"temperature": "77 - N2",
"observation": "Clear mass, No-Turbidity, AV - 52.52"
}
],
"measurements": [
{
"verbatim": "AV - 52.52"
},
{
"verbatim": "MONO - 24.4 h"
},
{
"verbatim": "Diacetate - 51.76%."
}
],
"step": 1
},
{
"name": "Step-II Acylate Intermediate",
"process": [
{
"time": "0.5",
"temperature": "75-79 / N2",
"observation": "Charged - Sp-18"
},
{
"time": "2 hrs.",
"temperature": "78-79 / N2",
"observation": "Feed of 2-ethyl hexyl Acylate over - 2 hrs."
},
{
"time": "5.5 hrs.",
"temperature": "77-81 / N2",
"observation": "Clear transparent"
}
],
"step": 2
},
{
"name": "Step-III Neutralisation",
"process": [
{
"time": "0.5",
"temperature": "RT-55-59/N2",
"observation": "Charged Acylate Intermediate, feed of phosphate 85gm over 25min."
},
{
"time": "1.5 hrs.",
"temperature": "55-58/N2",
"observation": "clear mass"
},
{
"time": "1 hrs",
"temperature": "55-57/N2",
"observation": "Yellowish, No foam., AU - 44.36, Amine - 36.25"
}
],
"measurements": [
{
"verbatim": "AU - 44.36"
},
{
"verbatim": "Amine - 36.25"
}
],
"step": 3
},
{
"name": "Batch 48Q (RM from above Batch)",
"materials": [
{
"name": "Acylate Intermediate",
"percentage": "15%"
},
{
"name": "DMS",
"percentage": "0.5%"
},
{
"name": "phosphate",
"percentage": "85%"
}
],
"process": [
{
"time": "0.5",
"temperature": "55-75 -",
"observation": "Charged Acylate"
},
{
"time": "0.5",
"observation": "slowly added DMS. / clear transparent Mass."
},
{
"time": "2.5",
"temperature": "55-60 -",
"observation": "slow addition of phosphate ester. AU - 52, Amine - 31.67"
}
],
"measurements": [
{
"verbatim": "AU - 52"
},
{
"verbatim": "Amine - 31.67"
}
],
"step": 4
}
],
"critical_parameters": [
{
"parameter": "aminev",
"reference_value": "30.1",
"value": "31.6"
},
{
"parameter": "av",
"reference_value": "43.2",
"value": "52"
}
],
"outcome": {
"status": "ok",
"basis": "Tested on Violet 23 resolubility ok",
"citation": "Lab Batch 48 Q.pdf, page 2"
},
"samples": [
{
"sample_id": "S 9076 #48Q",
"application_tests": [
{
"test": "Violet 23",
"system": "NC-PU ink",
"conditions": "trial 05.11.2025",
"result": "Viscosity: 30 sec; Gloss: 60.3; Colour Strength: 98-99.00%; Resolubility: 5; Transparency: Opaque",
"vs_reference": "BYK 9076 Standard — Viscosity: 29 sec; Gloss: 62.9; Colour Strength: 1; Resolubility: 4; Transparency: Ref as Std",
"file": "docs/Application data Summary/APP DATA- BYK 9076 equivalent.xlsx"
}
]
},
{
"alias": "Batch-48",
"analytical": [
{
"technique": "AV",
"value": "44.36"
},
{
"technique": "Amine",
"value": "36.25"
},
{
"technique": "MONO",
"value": "24.4 h"
},
{
"technique": "Diacetate",
"value": "51.76%"
},
{
"technique": "AU",
"value": "52"
},
{
"technique": "Amine",
"value": "31.67"
},
{
"verbatim": "AV - 52.52"
},
{
"verbatim": "MONO - 24.4 h"
},
{
"verbatim": "Diacetate - 51.76%."
},
{
"verbatim": "AU - 44.36"
},
{
"verbatim": "Amine - 36.25"
},
{
"verbatim": "AU - 52"
},
{
"verbatim": "Amine - 31.67"
}
],
"sample_id": "unspecified sample"
}
],
"date": "29/10/25",
"procedure_summary": "Step-I: Charged LUB 1010 (178 gm) at RT-50/N2, fed P2O5 over 1.5 hrs at 75-77°C/N2, held at 77°C for 1 hr. Step-II: Charged Sp-18 at 75-79°C/N2, fed 2-ethyl hexyl Acylate over 2 hrs at 78-79°C/N2, held 5.5 hrs to clear transparent. Step-III: Charged Acylate Intermediate, fed phosphate ester (85%) over 25 min at 55-59°C/N2, held 1.5 hrs. Batch 48Q: Charged Acylate Intermediate (15%) + DMS (0.5%), then phosphate (85%) at 55-75°C/N2.\n\nStep I: Phosphate ester synthesis from LUB-1010 and P2O5. Step II: Acylation of Epamine Sp-18 with 2-ethyl hexyl Acylate. Step III: Neutralization of Phosphate Ester and Acylate Intermediate. Variant Batch 48Q includes DMS.",
"observations": "Step-I: Clear mass, No-Turbidity\nStep-II: Clear transparent\nStep-III: Yellowish, No foam\nBatch 48Q: clear transparent Mass\n\nStep I: Clear mass, No-Turbidity, AV - 52.52, MONO - 24.4 h, Diacetate - 51.76%.\nStep II: Clear transparent.\nStep III: Yellowish, No foam, AU - 44.36, Amine - 36.25.\nBatch 48Q: AU - 52, Amine - 31.67.\n\nCharged LUB 1010 - 178 gm\nFeed of P2O5 - No particles\nClear mass, No-Turbidity, AV - 52.52\nCharged - Sp-18\nFeed of 2-ethyl hexyl Acylate over - 2 hrs.\nClear transparent\nCharged Acylate Intermediate, feed of phosphate 85gm over 25min.\nclear mass\nYellowish, No foam., AU - 44.36, Amine - 36.25\nCharged Acylate\nslowly added DMS. / clear transparent Mass.\nslow addition of phosphate ester. AU - 52, Amine - 31.67"
}