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Experiments / Batch 48 Q

Batch 48 Q OK

29/10/25 · also written as LBN 48 Q · S 9076 #48Q · Batch- NO - 48 · ByK-9076 · Batch - 48Q · BYK-9076
aminev
31.6
target 30.1 · +5.0% vs target
av
52
target 43.2 · +20.4% vs target
Conclusion — verbatim from the source
“Tested on Violet 23 resolubility ok”
Lab Batch 48 Q.pdf, page 2
Aim

Synthesis of BYK-9076 analog (Batch 48)

Observations

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

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. 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.

Raw materials
#MaterialSourceQtyPurity %Mol. wt.MolesRole
1Vicaspin LUB 1010 (R225100845) Bu- EO-PO HV-62.3/ MW-900 ×4Viswaat178 gms9000.197reactant
2P2O5 ×4Commercial9.357 gms141.940.0658reactant
3Epomine SP-018 ×3Nippon30 gms100reactant
42 ethyl hexyl acrylate ×470 gms100184.27reactant
DMS (Batch 48Q) ×30.5% %reactant
Phosphate Ester (Step-I)85 gmreactant
Acylate Intermediate (Step-II)15 gmreactant
Reaction conditions (optimized)
atmosphere: N2other: 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
Process
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)
Time (h)Temp (°C)AtmWhat happened
0.5 55-75 Charged Acrylate; DMS added / clean transport Notes
2.5 55-60 Slow addition of phosphate; 'Etfo.' Notes
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
Critical parameters — measured vs target
ParameterTargetMeasured
aminev 30.1 31.6
av 43.2 52
Sample S 9076 #48Q
result Violet 23 (NC-PU ink)
ParameterThis sampleStandard (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
APP DATA- BYK 9076 equivalent.xlsx
Sample unspecified sample
AV 44.36
Amine 36.25
MONO 24.4 h
Diacetate 51.76%
AU 52
Amine 31.67
AV - 52.52
MONO - 24.4 h
Diacetate - 51.76%.
AU - 44.36
Amine - 36.25
AU - 52
Amine - 31.67
Where this record comes from
Lab Batch 48 Q.pdf — lab journal (primary source)
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 (38 fields) — for auditors
5 extraction fragments · merged 2026-08-25 · 6 human-validated fields
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        "human_checked": true
      },
      "process_steps[6]": {
        "source_file": "pdf/9076 Data for Raven POC project/Handwritten  notes/9076 Exp 48-60_1.pdf",
        "extractor": "qwen-tasks/extract-fragment.md",
        "extractor_version": "unversioned",
        "extracted_date": "",
        "locator": "pages 1-3",
        "confidence": "medium",
        "human_checked": true
      }
    },
    "last_merged": "2026-08-25"
  },
  "documents": [
    {
      "file": "pdf/9076 Data for Raven POC project/Old ELN/Lab Batch 48 Q.pdf",
      "role": "eln_report",
      "link_basis": "alias match: LBN 48 Q",
      "link_status": "rule"
    },
    {
      "file": "docs/Application data Summary/APP DATA- BYK 9076 equivalent.xlsx",
      "role": "application_test",
      "link_basis": "alias match: S 9076 #48Q",
      "link_status": "rule"
    },
    {
      "file": "pdf/9076 Data for Raven POC project/Handwritten  notes/9076 Exp 48-60_1.pdf",
      "role": "handwritten_notes",
      "link_basis": "alias match: Batch- NO - 48",
      "link_status": "rule"
    }
  ],
  "validation": {
    "validated_fields": {
      "materials[0].molecular_wt": {
        "validated_by": "Claude direct analysis (Rishi-authorized 2026-08-21)",
        "date": "2026-08-21"
      },
      "materials[0].moles": {
        "validated_by": "Claude direct analysis (Rishi-authorized 2026-08-21)",
        "date": "2026-08-21"
      },
      "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"
}