Experiments / Batch 52
Batch 52 no result yet
22/12/25 ·
also written as S 9076 # 52 · Batch-52 · ByK 9076
Aim
Handwritten lab-note for a BYK 9076 analogue batch (9076 Exp 48-60 series): Step-I phosphate ester of the polyol with P2O5, Step-II acylate/acrylate intermediate from SP-18 (or Lupasol G-20) with 2-ethyl hexyl acrylate/acylate, Step-III neutralisation of the phosphate ester with the acylate intermediate.
Observations
Step-I: slight turbidity, yellow texture Step-II: Turbidity, yellow texture; IV 24.26 at 7 hrs; IV 24 after extra Sp-18 Neutralisation: found Turbidity, then More clarity Step I: Slight turbidity, yellow texture, AV - 51.7, AV - 42.5, Monomer - 331, Dioxane - 101, Free Data 0.2 hr. Step II: Turbidity, yellow texture, IV - 24.26, IV - 24. Step III: Found Turbidity, More clarity, AV - 37, Amine - 30, SAP - 53. 100 gm LUB 1010 charged & feed of P205 complete over 10 min. @ RT. dispersion of P205 slow slight turbidity yellow texture. AV - 51.7 added, 25 gm LUB 1010 added. Sp-18 - 77.6 gm + charged / Feed of 2-ethyl Acylate over 2 hrs - Turbidity / yellow texture (continued feed) IV - 24.26 Added Sp-18 - 10 gm, IV - 24 / Cool to R. Charged Acylate 15gm, ON / feed of Phosphate Ester - 85gm over 20min / found Turbidity More clarity, AV - 37 / Amine - 30, SAP - 53
Procedure summary
Step-I: Charged LUB 1010 (100 gm) & fed P2O5 (4.8 gm) over 10 min at RT/N2, dispersion 1 hr at 77-78°C/N2, 2 hrs at 75-80°C/N2, then 1.5 hrs; added 25 gm LUB 1010. Step-II: Charged Sp-18 (77.6 gm) at 78-81°C/N2, fed 2-ethyl Acylate over 2 hrs (turbidity/yellow texture), 7 hrs IV-24.26, then added Sp-18 (10 gm) at 3.5 hrs, IV-24, cooled to RT. Neutralisation: Charged Acylate (15 gm) at 55-59°C/N2, fed Phosphate Ester (85 gm) over 20 min (found turbidity), held 3.5 hrs at 55-59°C/N2. Step I: Phosphate ester synthesis. Step II: Acylate intermediate synthesis with DBN catalyst. Step III: Neutralization.
Raw materials
| Material | Qty | Mol. wt. | Moles | Role |
|---|---|---|---|---|
| Vicasurf LUB 1010, BluePO, HV - 57.8, MW - 970.5 ×3 | 125 gm | 970.5 | 0.128 | reactant |
| P2O5 ×3 | 4.8 gm | 141.94 | 0.0338 | reactant |
| Epimine Sp-18 | 77.6 gm | - | ||
| 2 Ethyl hexyl Acylate ×2 | 181 gm | reactant | ||
| DBN Catalyst (0.2%) ×3 | 0.517 gm | 70% | catalyst | |
| Epimine Sp-18 ×2 | 87.6 gm | reactant | ||
| phosphate Ester (Step-I) | 85 gm | reactant | ||
| Acylate Intermediate (Step-II) | 15 gm | reactant |
Reaction conditions (optimized)
atmosphere: N2other: Step-I: RT-55 to 77-80°C; Step-II: 78-81°C; Neutralisation: 55-59°C; Step I: RT-55 to 75-80°C; Step II: 78-81 to 78-80°C; Step III: 55/59/42°C
Process
| Step | Conditions | Charged | What happened | Results |
|---|---|---|---|---|
|
Step 1
Step-I Phosphate Ester
9076 Exp 48-60_1.pdf
|
— | — | — | — |
|
Step 2
Step-II Acylate Intermediate
9076 Exp 48-60_1.pdf
|
— | — | — | — |
|
Step 3
step - III) Neutralisation.
9076 Exp 48-60_1.pdf
|
— | — | — | — |
Sample S 9076 # 52
result
Violet 23 (NC-PU ink)
| Parameter | This sample | Standard (BYK 9076 Standard) |
|---|---|---|
| Viscosity | 33 sec | 29 sec |
| Gloss | 60 | 69.4 |
| Colour Strength | 97-98.00% | 1 |
| Resolubility | 4 | 4 |
| Transparency | Opaque | Ref as std |
APP DATA- BYK 9076 equivalent.xlsx
result
Violet 27 (NC-PU ink)
| Parameter | This sample | Standard (BYK 9076 Standard) |
|---|---|---|
| Viscosity | 36 sec | 34 sec |
| Gloss | 7.2 | 7.8 |
| Colour Strength | 1 | 1 |
| Resolubility | 4 | 4 |
| Transparency | As per std | Ref as Std |
APP DATA- BYK 9076 equivalent.xlsx
result
Black (NC-PU ink)
| Parameter | This sample | Standard (BYK 9076 Standard) |
|---|---|---|
| Viscosity | 48 sec | 47 sec |
| Gloss | 46.5 | 44.6 |
| Colour Strength | 1 | 1 |
| Resolubility | 3 | 4 |
| Transparency | As per std | Ref as Std |
APP DATA- BYK 9076 equivalent.xlsx
result
Blue (NC-PU ink)
| Parameter | This sample | Standard (BYK 9076 Standard) |
|---|---|---|
| Viscosity | 35 sec | 34 sec |
| Gloss | 42.6 | 41.8 |
| Colour Strength | 1 | 1 |
| Resolubility | 3 | 4 |
| Transparency | As per std | Ref as Std |
APP DATA- BYK 9076 equivalent.xlsx
Sample unspecified sample
AV (Step-I)
51.7
AV (final Step-I)
42.5
Monomer
33.1
Dioxane
10.1
Free Data
0.2
IV (Step-II 7h)
24.26
IV (Step-II final)
24
AV (neutralisation)
37
Amine
30
SAP
53
AV - 42.5 / Monomer - 331.
Dioxane - 101.
Free Data 0.2 hr.
IV - 24.26
IV - 24
AV - 37
Amine - 30
SAP - 53
Where this record comes from
APP DATA- BYK 9076 equivalent.xlsx
— application testing
9076 Exp 48-60_1.pdf
— handwritten notebook (primary source)
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 (26 fields) — for auditors
4 extraction fragments · merged 2026-08-25 · 0 human-validated fields
Fix a wrong or missing extraction side-by-side with the original:
app-data--S 9076 # 52
qwen-extract--9076-Exp-48-60-1--batch-52
qwen-extract--9076-exp-48-60-1--batch-52
qwen-extract--9076-exp-48-60_1--batch-52
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|---|---|---|---|
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| date | 9076 Exp 48-60_1.pdf pages 10-11 | qwen-tasks/extract-fragment.md@unversioned | high |
| aim | 9076 Exp 48-60_1.pdf pages 10-11 | qwen-tasks/extract-fragment.md@unversioned | high |
| conditions.atmosphere | 9076 Exp 48-60_1.pdf pages 10-11 | qwen-tasks/extract-fragment.md@unversioned | high |
| materials[0] | 9076 Exp 48-60_1.pdf pages 10-11 | qwen-tasks/extract-fragment.md@unversioned | medium |
| materials[1] | 9076 Exp 48-60_1.pdf pages 10-11 | qwen-tasks/extract-fragment.md@unversioned | medium |
| materials[2] | 9076 Exp 48-60_1.pdf pages 10-11 | qwen-tasks/extract-fragment.md@unversioned | medium |
| materials[3] | 9076 Exp 48-60_1.pdf pages 10-11 | qwen-tasks/extract-fragment.md@unversioned | medium |
| materials[4] | 9076 Exp 48-60_1.pdf pages 10-11 | qwen-tasks/extract-fragment.md@unversioned | medium |
| samples[1] | 9076 Exp 48-60_1.pdf pages 10-11 | qwen-tasks/extract-fragment.md@unversioned | high |
| procedure_summary | 9076 Exp 48-60_1.pdf Page 9-10 | qwen-tasks/extract-fragment.md@direct-v1 | high |
| observations | 9076 Exp 48-60_1.pdf pages 9-10 | qwen-tasks/extract-fragment.md@unversioned | high |
| materials[5] | 9076 Exp 48-60_1.pdf Page 9-10 | qwen-tasks/extract-fragment.md@direct-v1 | high |
| materials[6] | 9076 Exp 48-60_1.pdf Page 9-10 | qwen-tasks/extract-fragment.md@direct-v1 | high |
| materials[7] | 9076 Exp 48-60_1.pdf Page 9-10 | qwen-tasks/extract-fragment.md@direct-v1 | high |
| materials[8] | 9076 Exp 48-60_1.pdf Page 9-10 | qwen-tasks/extract-fragment.md@direct-v1 | high |
| materials[9] | 9076 Exp 48-60_1.pdf Page 9-10 | qwen-tasks/extract-fragment.md@direct-v1 | high |
| materials[10] | 9076 Exp 48-60_1.pdf pages 9-10 | qwen-tasks/extract-fragment.md@unversioned | medium |
| materials[11] | 9076 Exp 48-60_1.pdf pages 9-10 | qwen-tasks/extract-fragment.md@unversioned | medium |
| materials[12] | 9076 Exp 48-60_1.pdf pages 9-10 | qwen-tasks/extract-fragment.md@unversioned | medium |
| materials[13] | 9076 Exp 48-60_1.pdf pages 9-10 | qwen-tasks/extract-fragment.md@unversioned | medium |
| materials[14] | 9076 Exp 48-60_1.pdf pages 9-10 | qwen-tasks/extract-fragment.md@unversioned | medium |
| materials[15] | 9076 Exp 48-60_1.pdf pages 9-10 | qwen-tasks/extract-fragment.md@unversioned | medium |
| process_steps[0] | 9076 Exp 48-60_1.pdf pages 9-10 | qwen-tasks/extract-fragment.md@unversioned | medium |
| process_steps[1] | 9076 Exp 48-60_1.pdf pages 9-10 | qwen-tasks/extract-fragment.md@unversioned | medium |
| process_steps[2] | 9076 Exp 48-60_1.pdf pages 9-10 | qwen-tasks/extract-fragment.md@unversioned | medium |
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"validation": {
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"samples": [
{
"sample_id": "S 9076 # 52",
"application_tests": [
{
"test": "Violet 23",
"system": "NC-PU ink",
"conditions": "trial 30.12.2025",
"result": "Viscosity: 33 sec; Gloss: 60; Colour Strength: 97-98.00%; Resolubility: 4; Transparency: Opaque",
"vs_reference": "BYK 9076 Standard — Viscosity: 29 sec; Gloss: 69.4; Colour Strength: 1; Resolubility: 4; Transparency: Ref as std",
"file": "docs/Application data Summary/APP DATA- BYK 9076 equivalent.xlsx"
},
{
"test": "Violet 27",
"system": "NC-PU ink",
"conditions": "trial 30.12.2025",
"result": "Viscosity: 36 sec; Gloss: 7.2; Colour Strength: 1; Resolubility: 4; Transparency: As per std",
"vs_reference": "BYK 9076 Standard — Viscosity: 34 sec; Gloss: 7.8; Colour Strength: 1; Resolubility: 4; Transparency: Ref as Std",
"file": "docs/Application data Summary/APP DATA- BYK 9076 equivalent.xlsx"
},
{
"test": "Black",
"system": "NC-PU ink",
"conditions": "trial 30.12.2025",
"result": "Viscosity: 48 sec; Gloss: 46.5; Colour Strength: 1; Resolubility: 3; Transparency: As per std",
"vs_reference": "BYK 9076 Standard — Viscosity: 47 sec; Gloss: 44.6; Colour Strength: 1; Resolubility: 4; Transparency: Ref as Std",
"file": "docs/Application data Summary/APP DATA- BYK 9076 equivalent.xlsx"
},
{
"test": "Blue",
"system": "NC-PU ink",
"conditions": "trial 30.12.2025",
"result": "Viscosity: 35 sec; Gloss: 42.6; Colour Strength: 1; Resolubility: 3; Transparency: As per std",
"vs_reference": "BYK 9076 Standard — Viscosity: 34 sec; Gloss: 41.8; Colour Strength: 1; Resolubility: 4; Transparency: Ref as Std",
"file": "docs/Application data Summary/APP DATA- BYK 9076 equivalent.xlsx"
}
]
},
{
"alias": "Batch-52",
"analytical": [
{
"technique": "AV (Step-I)",
"value": "51.7"
},
{
"technique": "AV (final Step-I)",
"value": "42.5"
},
{
"technique": "Monomer",
"value": "33.1"
},
{
"technique": "Dioxane",
"value": "10.1"
},
{
"technique": "Free Data",
"value": "0.2"
},
{
"technique": "IV (Step-II 7h)",
"value": "24.26"
},
{
"technique": "IV (Step-II final)",
"value": "24"
},
{
"technique": "AV (neutralisation)",
"value": "37"
},
{
"technique": "Amine",
"value": "30"
},
{
"technique": "SAP",
"value": "53"
},
{
"verbatim": "AV - 42.5 / Monomer - 331."
},
{
"verbatim": "Dioxane - 101."
},
{
"verbatim": "Free Data 0.2 hr."
},
{
"verbatim": "IV - 24.26"
},
{
"verbatim": "IV - 24"
},
{
"verbatim": "AV - 37"
},
{
"verbatim": "Amine - 30"
},
{
"verbatim": "SAP - 53"
}
],
"sample_id": "unspecified sample"
}
],
"date": "22/12/25",
"aim": "Handwritten lab-note for a BYK 9076 analogue batch (9076 Exp 48-60 series): Step-I phosphate ester of the polyol with P2O5, Step-II acylate/acrylate intermediate from SP-18 (or Lupasol G-20) with 2-ethyl hexyl acrylate/acylate, Step-III neutralisation of the phosphate ester with the acylate intermediate.",
"conditions": {
"atmosphere": "N2",
"other": "Step-I: RT-55 to 77-80°C; Step-II: 78-81°C; Neutralisation: 55-59°C; Step I: RT-55 to 75-80°C; Step II: 78-81 to 78-80°C; Step III: 55/59/42°C"
},
"materials": [
{
"name": "Vicasurf LUB 1010 / BluePO",
"quantity": "125",
"unit": "gm",
"role": "unknown",
"molecular_wt": "970.5",
"moles": "0.128",
"notes": "HV-57.8",
"role_verbatim": "polyol"
},
{
"name": "P2O5",
"quantity": "4.8",
"unit": "gm",
"role": "unknown",
"molecular_wt": "141.94",
"moles": "0.0338",
"role_verbatim": "phosphorylating agent"
},
{
"name": "Epimine Sp-18",
"quantity": "77.6",
"unit": "gm",
"role": "unknown",
"notes": "initial charge; 10 gm added later",
"role_verbatim": "amine"
},
{
"name": "2 Ethyl hexyl Acylate",
"quantity": "181",
"unit": "gm",
"role": "unknown",
"role_verbatim": "acylating agent"
},
{
"name": "DBN Catalyst (0.2%)",
"quantity": "0.517",
"unit": "gm",
"role": "catalyst"
},
{
"name": "Vicasurf LUB 1010",
"quantity": "125",
"unit": "gm",
"role": "reactant",
"notes": "BluePO, HV - 57.8, MW - 970.5"
},
{
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"quantity": "4.8",
"unit": "gm",
"role": "reactant"
},
{
"name": "Epimine Sp-18",
"quantity": "87.6",
"unit": "gm",
"role": "reactant"
},
{
"name": "2 Ethyl hexyl Acylate",
"quantity": "181",
"unit": "gm",
"role": "reactant"
},
{
"name": "DBN Catalyst",
"quantity": "0.517",
"unit": "gm",
"role": "catalyst",
"notes": "0.2%"
},
{
"name": "Vicasurf LUB 1010, BluePO, HV - 57.8, MW - 970.5",
"quantity": "125",
"unit": "gm",
"molecular_weight": "970.5",
"moles": "0.128",
"role": "reactant"
},
{
"name": "P205",
"quantity": "4.8",
"unit": "gm",
"molecular_weight": "141.94",
"moles": "0.0338",
"role": "reactant"
},
{
"name": "Epimine Sp-18",
"quantity": "87.6",
"unit": "gm",
"percentage": "30%",
"role": "reactant"
},
{
"name": "DBN Catalyst (0.2%)",
"quantity": "0.517",
"unit": "gm",
"molecular_weight": "184.27",
"moles": "70%",
"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"
}
],
"procedure_summary": "Step-I: Charged LUB 1010 (100 gm) & fed P2O5 (4.8 gm) over 10 min at RT/N2, dispersion 1 hr at 77-78°C/N2, 2 hrs at 75-80°C/N2, then 1.5 hrs; added 25 gm LUB 1010. Step-II: Charged Sp-18 (77.6 gm) at 78-81°C/N2, fed 2-ethyl Acylate over 2 hrs (turbidity/yellow texture), 7 hrs IV-24.26, then added Sp-18 (10 gm) at 3.5 hrs, IV-24, cooled to RT. Neutralisation: Charged Acylate (15 gm) at 55-59°C/N2, fed Phosphate Ester (85 gm) over 20 min (found turbidity), held 3.5 hrs at 55-59°C/N2.\n\nStep I: Phosphate ester synthesis. Step II: Acylate intermediate synthesis with DBN catalyst. Step III: Neutralization.",
"observations": "Step-I: slight turbidity, yellow texture\nStep-II: Turbidity, yellow texture; IV 24.26 at 7 hrs; IV 24 after extra Sp-18\nNeutralisation: found Turbidity, then More clarity\n\nStep I: Slight turbidity, yellow texture, AV - 51.7, AV - 42.5, Monomer - 331, Dioxane - 101, Free Data 0.2 hr.\nStep II: Turbidity, yellow texture, IV - 24.26, IV - 24.\nStep III: Found Turbidity, More clarity, AV - 37, Amine - 30, SAP - 53.\n\n100 gm LUB 1010 charged & feed of P205 complete over 10 min. @ RT.\ndispersion of P205 slow\nslight turbidity\nyellow texture. AV - 51.7 added, 25 gm LUB 1010 added.\nSp-18 - 77.6 gm + charged / Feed of 2-ethyl Acylate over 2 hrs - Turbidity / yellow texture\n(continued feed)\nIV - 24.26\nAdded Sp-18 - 10 gm, IV - 24 / Cool to R.\nCharged Acylate 15gm, ON / feed of Phosphate Ester - 85gm over 20min / found Turbidity\nMore clarity, AV - 37 / Amine - 30, SAP - 53",
"process_steps": [
{
"name": "Step-I Phosphate Ester",
"process": [
{
"time": "0.2 hrs",
"temperature": "RT-55 / N2",
"observation": "100 gm LUB 1010 charged & feed of P205 complete over 10 min. @ RT."
},
{
"time": "1 hrs.",
"temperature": "77-78 / N2",
"observation": "dispersion of P205 slow"
},
{
"time": "2 hrs",
"temperature": "75-80 / N2",
"observation": "slight turbidity"
},
{
"time": "1.5 hrs.",
"temperature": "75-80 / N2",
"observation": "yellow texture. AV - 51.7 added, 25 gm LUB 1010 added."
}
],
"measurements": [
{
"verbatim": "AV - 42.5 / Monomer - 331."
},
{
"verbatim": "Dioxane - 101."
},
{
"verbatim": "Free Data 0.2 hr."
}
],
"step": 1
},
{
"name": "Step-II Acylate Intermediate",
"process": [
{
"time": "0.5",
"temperature": "78-81 / N2",
"observation": "Sp-18 - 77.6 gm + charged / Feed of 2-ethyl Acylate over 2 hrs - Turbidity / yellow texture"
},
{
"time": "2 hrs",
"temperature": "78-81 / N2",
"observation": "(continued feed)"
},
{
"time": "7 hrs",
"temperature": "78-80 / N2",
"observation": "IV - 24.26"
},
{
"time": "3.5 hrs",
"temperature": "78-81 / N2",
"observation": "Added Sp-18 - 10 gm, IV - 24 / Cool to R."
}
],
"measurements": [
{
"verbatim": "IV - 24.26"
},
{
"verbatim": "IV - 24"
}
],
"step": 2,
"materials": {}
},
{
"name": "step - III) Neutralisation.",
"process": [
{
"time": "0.5",
"temperature": "55/59/42",
"observation": "Charged Acylate 15gm, ON / feed of Phosphate Ester - 85gm over 20min / found Turbidity"
},
{
"time": "3.5",
"temperature": "55/59/42",
"observation": "More clarity, AV - 37 / Amine - 30, SAP - 53"
}
],
"measurements": [
{
"verbatim": "AV - 37"
},
{
"verbatim": "Amine - 30"
},
{
"verbatim": "SAP - 53"
}
],
"step": 3
}
]
}