Batch 51 no result yet
Prepare phosphate ester, acylate intermediate, neutralised product, and blended variants (ByK-9076 equivalent)
yellow tincture Step-I: slight turbidity, yellow texture Step-II: Observed Reaction by IV analysis, Final IV 26.1 @ 5.5hrs Neutralisation: Slight Turbidity Step I: Slight turbidity, yellow texture, AU - 51.7, Final AU - 42.5, Mono - 33.1, Diols - 10.65, Free Acid - 0.26-1. Step II: Final IV - 26.1 @ 5.5hrs. Step III: Slight Turbidity, AV - 46.8. Blends: B.No-51A (AV - 23.66, Amine - 14.2), B.No-51B (AV - 31.9, Amine - 20.4). 100 gm of Vicasurf LUB 1010 added to feed of P205 over 10 min. dispersion of P205 slowly slight turbidity / yellow texture. AU - 51.7, Added 25 gm LUB 1010, Final AU - 42.5, Mono - 33.1 / Diols - 10.65, Free Acid - 0.26-1. charged SP-18 - 30 gm. heated to 75-80°C Observed Reaction by IV analysis. Final IV - 26.1 @ 5.5hrs. Charged Acrylate Intermediate - 15 gm. Feed of Phosphate Ester over 10-15 min. Slight Turbidity, AV - 46.8
Step-I: Charged Vicasurf LUB 1010 (100 gm) at RT-55/N2, fed P2O5 over 10 min, dispersion 1 hr at 77-78°C/N2, 2 hrs at 75-80°C/N2, then 1.5 hrs at 75-78°C/N2; added 25 gm LUB 1010. Step-II: Charged SP-18 (30 gm) at RT-75-78°C/N2, heated to 75-80°C, fed 2-Ethyl hexyl Acylate over 2 hrs, reaction monitored by IV to 5.5 hrs. Neutralisation: Charged Acrylate Intermediate (15 gm) at 55°C/N2, fed Phosphate Ester (85 gm) over 10-15 min at 55-59°C/N2, held 2 hrs. Blends: 51A (51 50% + Finalux 50%), 51B (51 75% + Finalux 25%), RSB-04A (RSB-04 81.8% + Finalux 9.09% + B.No-48 Acrylate 9.09%), 51C (Adepal 100%). Step I: Phosphate ester synthesis. Step II: Acylate intermediate synthesis. Step III: Neutralization. Blending of Batch 51 with Finalux, RSB-04, and Adepal.
| # | Material | Source | Qty | Mol. wt. | Moles | Role |
|---|---|---|---|---|---|---|
| 1 | i) Vicaspin LUB 1010 (R425110899/3.12.25) Bu- EO-PO HV-57.8/ MW-970.5 | Viswaat | 100 gms | - | ||
| 2 | Phosphorous pentaoxide | 4.8 gms | - | |||
| 3 | Epomine SP-018 ×4 | 30 gms | reactant | |||
| 4 | 2 ethyl hexyl acrylate ×4 | 70 gms | 184.27 | 70% | reactant | |
| Vicasurf LUB 1010, Bu-EO-PO, HV - 57.8 ×3 | 125 gm | 970.5 | 0.128 | reactant | ||
| P2O5 ×3 | 4.8 gm | 141.94 | 0.0338 | reactant | ||
| Finalux ×2 | 50% % | - | ||||
| Adepal ×2 | 100% % | - | ||||
| RSB-04 | 81.8 % | - | ||||
| B.No-48 | 9.09 % | - | ||||
| Phosphate Ester (Step-I) | 85 gm | reactant | ||||
| Acrylate Intermediate (Step-II) | 15 gm | reactant |
| Step | Conditions | Charged | What happened | Results | ||||||||||||||||||||||||||||||||||||||||
|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|
|
Step 1
Step-I) Phosphate ester
9076 Exp 48-60_1.pdf · LBN 51.pdf
|
atmosphere: N2other: Glass reactor with column and accessories; under agitation; feed of RM-II over 10 min [ELN] |
i) Vicaspin LUB 1010 (R425110899/3.12.25) Bu- EO-PO HV-57.8/ MW-970.5 (Viswaat, RM-I) 100 gms [ELN] / 125 g [Notes p9] (MW 970.5, 0.128 mol) Phosphorous pentaoxide (RM-II) 4.8 gms (MW 141.94, 0.0338 mol)
|
Step- I) - RM- I heated to 50 deg C under N2; feed of RM - II over 10 min. [ELN]
Step-by-step (9 entries)
|
acid_value 51.7acid_value_final 42.5mono 33-1Bioops 10.65free_acid 0.24-1 | ||||||||||||||||||||||||||||||||||||||||
|
Step 2
Step-II) Acrylate intermediate
9076 Exp 48-60_1.pdf · LBN 51.pdf
|
atmosphere: N2 |
Epomine SP-018 30 gms [ELN] (30 % [Notes p9]) 2 ethyl hexyl acrylate 70 gms [ELN] (70 %, MW 184.27 [Notes p9])
|
raised temperature to 75-8 deg C under agitation// yellow tincture [ELN]
Step-by-step (6 entries)
|
acid_value 56.7mono 40.54di 59.1free_acid 0.837iodine_value_final 26.1iodine_value 24 | ||||||||||||||||||||||||||||||||||||||||
|
Step 3
Step-III) Neutralisation
9076 Exp 48-60_1.pdf
|
atmosphere: N2 |
Phosphate Est. / Step I [Notes p7, weight cell not legible] / Phosphate ester (Step-I product) 85 g = 85 % [Notes p9] Acrylate Intermediate Step II 15 g = 15 % [Notes p7 and p9]
|
Handwritten analysis block below Step-III (Notes p8): 'Bending B.NO-STA-1) B.No-51-501. AV-23.66 findux = 501. Amine-14.2 G-1812'; 'B.N0-51B= DB.N0.57-751÷7AU-31.9, 11 Final -251 Active-20.4, G-1812'; 'B. No → RSB-O4 ↑, RSB~O4, 11) Final x-4.09÷12, 6÷1812'; '111 B.NO.48 - 9.09÷, Acetate, ppE- - Adipate -1001.' yellow tincture [ELN]
Step-by-step (5 entries)
|
acid_value 46.8acid_value 37amine_value 30SAP 53 | ||||||||||||||||||||||||||||||||||||||||
|
Step 4
Blending
9076 Exp 48-60_1.pdf
|
— | — | — | — |
Something wrong on this page? Record a correction
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},
"date": "17/12/25",
"aim": "Prepare phosphate ester, acylate intermediate, neutralised product, and blended variants (ByK-9076 equivalent)",
"conditions": {
"temperature": "45-50 deg C, then raised to 75-80 deg C",
"time": "0.5 hrs, then 3.5 hrs",
"atmosphere": "N2",
"other": "Glass reactor with column and accessories; under agitation; feed of RM-II over 10 min; Step-I: RT-55 to 77-80°C; Step-II: 75-81°C; Neutralisation: 55-59°C; Step I: RT-55 to 75-80°C; Step II: RT-75-78 to 75-81°C; Step III: 55 to 55-59°C"
},
"materials": [
{
"sr_no": 1,
"name": "i) Vicaspin LUB 1010 (R425110899/3.12.25) Bu- EO-PO HV-57.8/ MW-970.5",
"source": "Viswaat",
"quantity": "100",
"unit": "gms",
"role": "unknown",
"role_verbatim": "RM-I"
},
{
"sr_no": 2,
"name": "Phosphorous pentaoxide",
"quantity": "4.8",
"unit": "gms",
"role": "unknown",
"role_verbatim": "RM-II"
},
{
"sr_no": 3,
"name": "Epomine SP-018",
"quantity": "30",
"unit": "gms"
},
{
"sr_no": 4,
"name": "2 ethyl hexyl acrylate",
"quantity": "70",
"unit": "gms"
},
{
"name": "Vicasurf LUB 1010 / Bu-EO-PO",
"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": "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": "Finalux",
"quantity": "50%",
"unit": "%",
"role": "unknown",
"role_verbatim": "blend component (51A, 51B)"
},
{
"name": "Adepal",
"quantity": "100%",
"unit": "%",
"role": "unknown",
"role_verbatim": "blend component (51C)"
},
{
"name": "Vicasurf LUB 1010",
"quantity": "125",
"unit": "gm",
"role": "reactant",
"notes": "Bu-EO-PO, HV - 57.8"
},
{
"name": "P205",
"quantity": "4.8",
"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": "Finalux",
"quantity": "50",
"unit": "%",
"role": "unknown",
"notes": "Used in B.No-51A and B.No-51B",
"role_verbatim": "blend_component"
},
{
"name": "RSB-04",
"quantity": "81.8",
"unit": "%",
"role": "unknown",
"notes": "Used in B.No-RSB-04A",
"role_verbatim": "blend_component"
},
{
"name": "B.No-48",
"quantity": "9.09",
"unit": "%",
"role": "unknown",
"notes": "Used in B.No-RSB-04A",
"role_verbatim": "blend_component"
},
{
"name": "Adepal",
"quantity": "100",
"unit": "%",
"role": "unknown",
"notes": "Used in B.No-51C",
"role_verbatim": "blend_component"
},
{
"name": "Vicasurf LUB 1010, Bu-EO-PO, HV - 57.8",
"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": "Epamine SP 18",
"quantity": "30",
"unit": "gm",
"percentage": "30%",
"role": "reactant"
},
{
"name": "2-Ethyl hexyl Acylate",
"quantity": "70",
"unit": "gm",
"molecular_weight": "184.27",
"moles": "70%",
"role": "reactant"
},
{
"name": "Phosphate Ester (Step-I)",
"quantity": "85",
"unit": "gm",
"percentage": "85%",
"role": "reactant"
},
{
"name": "Acrylate Intermediate (Step-II)",
"quantity": "15",
"unit": "gm",
"percentage": "15%",
"role": "reactant"
}
],
"process_steps": [
{
"step": 1,
"time_hrs": "0.5",
"temp_c": "45-50",
"pressure": "N2",
"procedure": [
{
"action": "Step- I) - RM- I heated to 50 deg C under N2; feed of RM - II over 10 min"
}
]
},
{
"step": 2,
"time_hrs": "3.5",
"temp_c": "75-80",
"pressure": "N2",
"procedure": [
{
"action": "raised temperature to 75-8 deg C under agitation// yellow tincture AV-56.7 Mono-40.54 / Di- 59.1/ Free acid-0.837"
}
]
},
{
"name": "Step-I Phosphate Ester (Chemical Composition)",
"process": [
{
"time": "0.2 hrs",
"temperature": "RT - 55 / N2",
"observation": "100 gm of Vicasurf LUB 1010 added to feed of P205 over 10 min."
},
{
"time": "1 hrs.",
"temperature": "77-78 / N2",
"observation": "dispersion of P205 slowly"
},
{
"time": "2 hrs.",
"temperature": "75-80 / N2",
"observation": "slight turbidity / yellow texture."
},
{
"time": "1.5 hrs.",
"temperature": "75-78 / N2",
"observation": "AU - 51.7, Added 25 gm LUB 1010, Final AU - 42.5, Mono - 33.1 / Diols - 10.65, Free Acid - 0.26-1."
}
],
"measurements": [
{
"verbatim": "AU - 51.7"
},
{
"verbatim": "Final AU - 42.5"
},
{
"verbatim": "Mono - 33.1 / Diols - 10.65"
},
{
"verbatim": "Free Acid - 0.26-1."
}
],
"step": 1
},
{
"name": "Step-II Acylate Intermediate",
"process": [
{
"time": "0.2",
"temperature": "RT - 75-78 / N2",
"observation": "charged SP-18 - 30 gm. heated to 75-80°C"
},
{
"time": "5.5hrs.",
"temperature": "75-81°C / N2",
"observation": "Observed Reaction by IV analysis. Final IV - 26.1 @ 5.5hrs."
}
],
"measurements": [
{
"verbatim": "Final IV - 26.1 @ 5.5hrs."
}
],
"step": 2
},
{
"name": "Step-III Neutralisation",
"process": [
{
"time": "0.2",
"temperature": "55 / N2",
"observation": "Charged Acrylate Intermediate - 15 gm."
},
{
"time": "0.5",
"temperature": "55-59 / N2",
"observation": "Feed of Phosphate Ester over 10-15 min."
},
{
"time": "2 hrs.",
"temperature": "55-58 / N2",
"observation": "Slight Turbidity, AV - 46.8"
}
],
"measurements": [
{
"verbatim": "AV - 46.8"
}
],
"step": 3
},
{
"name": "Blending",
"blends": [
{
"id": "B.No-51A",
"components": [
{
"name": "B.No-51",
"percentage": "50%"
},
{
"name": "Finalux",
"percentage": "50%"
}
],
"measurements": [
{
"verbatim": "AV - 23.66"
},
{
"verbatim": "Amine - 14.2"
}
]
},
{
"id": "B.No-51B",
"components": [
{
"name": "B.No-51",
"percentage": "75%"
},
{
"name": "Finalux",
"percentage": "25%"
}
],
"measurements": [
{
"verbatim": "AV - 31.9"
},
{
"verbatim": "Amine - 20.4"
}
]
},
{
"id": "B.No-RSB-04A",
"components": [
{
"name": "RSB-04",
"percentage": "81.8%"
},
{
"name": "Finalux",
"percentage": "9.09%"
},
{
"name": "B.No-48",
"percentage": "9.09%",
"note": "Acrylate"
}
],
"measurements": []
},
{
"id": "B.No-51C PP6",
"components": [
{
"name": "Adepal",
"percentage": "100%"
}
],
"measurements": []
}
],
"step": 4
}
],
"observations": "yellow tincture\n\nStep-I: slight turbidity, yellow texture\nStep-II: Observed Reaction by IV analysis, Final IV 26.1 @ 5.5hrs\nNeutralisation: Slight Turbidity\n\nStep I: Slight turbidity, yellow texture, AU - 51.7, Final AU - 42.5, Mono - 33.1, Diols - 10.65, Free Acid - 0.26-1.\nStep II: Final IV - 26.1 @ 5.5hrs.\nStep III: Slight Turbidity, AV - 46.8.\nBlends: B.No-51A (AV - 23.66, Amine - 14.2), B.No-51B (AV - 31.9, Amine - 20.4).\n\n100 gm of Vicasurf LUB 1010 added to feed of P205 over 10 min.\ndispersion of P205 slowly\nslight turbidity / yellow texture.\nAU - 51.7, Added 25 gm LUB 1010, Final AU - 42.5, Mono - 33.1 / Diols - 10.65, Free Acid - 0.26-1.\ncharged SP-18 - 30 gm. heated to 75-80°C\nObserved Reaction by IV analysis. Final IV - 26.1 @ 5.5hrs.\nCharged Acrylate Intermediate - 15 gm.\nFeed of Phosphate Ester over 10-15 min.\nSlight Turbidity, AV - 46.8",
"samples": [
{
"alias": "Batch-51",
"analytical": [
{
"technique": "AU",
"value": "51.7"
},
{
"technique": "AV (final)",
"value": "42.5"
},
{
"technique": "Mono",
"value": "33.1"
},
{
"technique": "Diols",
"value": "10.65"
},
{
"technique": "Free Acid",
"value": "0.26"
},
{
"technique": "IV",
"value": "26.1"
},
{
"technique": "AV (neutralisation)",
"value": "46.8"
},
{
"technique": "AV",
"value": "23.66"
},
{
"technique": "Amine",
"value": "14.2"
},
{
"technique": "AV",
"value": "31.9"
},
{
"technique": "Amine",
"value": "20.4"
},
{
"verbatim": "AU - 51.7"
},
{
"verbatim": "Final AU - 42.5"
},
{
"verbatim": "Mono - 33.1 / Diols - 10.65"
},
{
"verbatim": "Free Acid - 0.26-1."
},
{
"verbatim": "Final IV - 26.1 @ 5.5hrs."
},
{
"verbatim": "AV - 46.8"
},
{
"verbatim": "B.No-51A: B.No-51 - 50% / Finalux - 50%: AV - 23.66, Amine - 14.2"
},
{
"verbatim": "B.No-51B: B.No-51 - 75% / Finalux - 25%: AV - 31.9, Amine - 20.4"
},
{
"verbatim": "B.No-RSB-04A: RSB-04 - 81.8% / Finalux - 9.09% / B.No-48 - 9.09% (Acrylate)"
},
{
"verbatim": "B.No-51C PP6 - Adepal — 100%."
}
],
"sample_id": "unspecified sample"
}
],
"procedure_summary": "Step-I: Charged Vicasurf LUB 1010 (100 gm) at RT-55/N2, fed P2O5 over 10 min, dispersion 1 hr at 77-78°C/N2, 2 hrs at 75-80°C/N2, then 1.5 hrs at 75-78°C/N2; added 25 gm LUB 1010. Step-II: Charged SP-18 (30 gm) at RT-75-78°C/N2, heated to 75-80°C, fed 2-Ethyl hexyl Acylate over 2 hrs, reaction monitored by IV to 5.5 hrs. Neutralisation: Charged Acrylate Intermediate (15 gm) at 55°C/N2, fed Phosphate Ester (85 gm) over 10-15 min at 55-59°C/N2, held 2 hrs. Blends: 51A (51 50% + Finalux 50%), 51B (51 75% + Finalux 25%), RSB-04A (RSB-04 81.8% + Finalux 9.09% + B.No-48 Acrylate 9.09%), 51C (Adepal 100%).\n\nStep I: Phosphate ester synthesis. Step II: Acylate intermediate synthesis. Step III: Neutralization. Blending of Batch 51 with Finalux, RSB-04, and Adepal."
}