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Experiments / Batch 60

Batch 60 no result yet

1/4/26 · also written as Batch NO-60 · 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: Brown particles, slight foam, AV-52, Residue - sticks on wall. Step II: Yellowish tincture, clear mass, IU - 32.3, IU - 17.6. Step III: Foaming, turbidity, Non Uniform mass, AU - 43, Amine 25.7. Charged - LUB 1010 - 200 gm Feed of P205 - 10 gm Over 10-15 min. / slow dispersion. Brown particles, slight foam /, AV-52, Residue - sticks on wall Charged Lupasol-G-20 15gm. Feed of (Acrylate + AIBN) mix started Yellowish tincture / clear mass, Yellowish - clear mass. IU - 32.3 / clear mass. IU - 17.6 -, clear mass / yellow tincture. Charged Acrylate - 15gm. Feed of phosphate Ester - 7 min. foaming / turbidity, Non Uniform. mass., AU - 43 / Amine 25.7

Procedure summary

Step I: Phosphate ester synthesis. Step II: Acylate intermediate synthesis using Lupasop G-20 and AIBN. Step III: Neutralization.

Raw materials
MaterialQtyMolesRole
Vicarex LUB 1010, Bu-12PO-10Eo, MW-942.22 / MW 59.52 ×2200 gmreactant
P205 ×210.04 gmreactant
Lupasop G-20 ×275 gmreactant
2-Ethyl hexyl Acylate ×2225 gm75%reactant
AIBN (0.05%) ×20.15 gmcatalyst
phosphate Ester (Step-I)85 gmreactant
Acrylate Intermediate (Step-II)15 gmreactant
Reaction conditions (optimized)
atmosphere: N2other: Step I: RT-50 to 77-80°C; Step II: RT-50/78-81°C; Step III: RT-55 to 55-57°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 unspecified sample
AV-52
IU - 32.3
IU - 17.6 -
AU - 43
Amine 25.7
Where this record comes from
9076 Exp 48-60_1.pdf — handwritten notebook (primary source) · linked by a person
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 (21 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--9076-exp-48-60-1--batch-60 qwen-extract--9076-exp-48-60_1--batch-no-60
FieldSourceExtractorConf.
date9076 Exp 48-60_1.pdf Page 27-28 qwen-tasks/extract-fragment.md@direct-v1high
aim9076 Exp 48-60_1.pdf Page 27-28 qwen-tasks/extract-fragment.md@direct-v1high
conditions.atmosphere9076 Exp 48-60_1.pdf Page 27-28 qwen-tasks/extract-fragment.md@direct-v1high
materials[0]9076 Exp 48-60_1.pdf Page 27-28 qwen-tasks/extract-fragment.md@direct-v1high
materials[1]9076 Exp 48-60_1.pdf Page 27-28 qwen-tasks/extract-fragment.md@direct-v1high
materials[2]9076 Exp 48-60_1.pdf Page 27-28 qwen-tasks/extract-fragment.md@direct-v1high
materials[3]9076 Exp 48-60_1.pdf Page 27-28 qwen-tasks/extract-fragment.md@direct-v1high
materials[4]9076 Exp 48-60_1.pdf Page 27-28 qwen-tasks/extract-fragment.md@direct-v1high
procedure_summary9076 Exp 48-60_1.pdf Page 27-28 qwen-tasks/extract-fragment.md@direct-v1high
observations9076 Exp 48-60_1.pdf pages 24-28 qwen-tasks/extract-fragment.md@unversionedhigh
materials[5]9076 Exp 48-60_1.pdf pages 24-28 qwen-tasks/extract-fragment.md@unversionedmedium
materials[6]9076 Exp 48-60_1.pdf pages 24-28 qwen-tasks/extract-fragment.md@unversionedmedium
materials[7]9076 Exp 48-60_1.pdf pages 24-28 qwen-tasks/extract-fragment.md@unversionedmedium
materials[8]9076 Exp 48-60_1.pdf pages 24-28 qwen-tasks/extract-fragment.md@unversionedmedium
materials[9]9076 Exp 48-60_1.pdf pages 24-28 qwen-tasks/extract-fragment.md@unversionedmedium
materials[10]9076 Exp 48-60_1.pdf pages 24-28 qwen-tasks/extract-fragment.md@unversionedmedium
materials[11]9076 Exp 48-60_1.pdf pages 24-28 qwen-tasks/extract-fragment.md@unversionedmedium
process_steps[0]9076 Exp 48-60_1.pdf pages 24-28 qwen-tasks/extract-fragment.md@unversionedmedium
process_steps[1]9076 Exp 48-60_1.pdf pages 24-28 qwen-tasks/extract-fragment.md@unversionedmedium
process_steps[2]9076 Exp 48-60_1.pdf pages 24-28 qwen-tasks/extract-fragment.md@unversionedmedium
samples[0]9076 Exp 48-60_1.pdf pages 24-28 qwen-tasks/extract-fragment.md@unversionedhigh
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    }
  ],
  "validation": {
    "validated_fields": {},
    "corrections_applied": []
  },
  "date": "1/4/26",
  "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-50 to 77-80°C; Step II: RT-50/78-81°C; Step III: RT-55 to 55-57°C"
  },
  "materials": [
    {
      "name": "Vicarex LUB 1010",
      "quantity": "200",
      "unit": "gm",
      "role": "reactant",
      "notes": "Bu-12PO-10Eo, MW-942.22 / MW 59.52"
    },
    {
      "name": "P205",
      "quantity": "10.04",
      "unit": "gm",
      "role": "reactant"
    },
    {
      "name": "Lupasop G-20",
      "quantity": "75",
      "unit": "gm",
      "role": "reactant"
    },
    {
      "name": "2-Ethyl hexyl Acylate",
      "quantity": "225",
      "unit": "gm",
      "role": "reactant"
    },
    {
      "name": "AIBN",
      "quantity": "0.15",
      "unit": "gm",
      "role": "catalyst",
      "notes": "0.05%"
    },
    {
      "name": "Vicarex LUB 1010, Bu-12PO-10Eo, MW-942.22 / MW 59.52",
      "quantity": "200",
      "unit": "gm",
      "molecular_weight": "942.22",
      "role": "reactant"
    },
    {
      "name": "P205",
      "quantity": "10.04",
      "unit": "gm",
      "molecular_weight": "141.94",
      "role": "reactant"
    },
    {
      "name": "Lupasop G-20",
      "quantity": "75",
      "unit": "gm",
      "percentage": "25%",
      "role": "reactant"
    },
    {
      "name": "2-Ethyl hexyl Acylate",
      "quantity": "225",
      "unit": "gm",
      "molecular_weight": "184.27",
      "moles": "75%",
      "role": "reactant"
    },
    {
      "name": "AIBN (0.05%)",
      "quantity": "0.15",
      "unit": "gm",
      "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"
    }
  ],
  "procedure_summary": "Step I: Phosphate ester synthesis. Step II: Acylate intermediate synthesis using Lupasop G-20 and AIBN. Step III: Neutralization.",
  "observations": "Step I: Brown particles, slight foam, AV-52, Residue - sticks on wall.\nStep II: Yellowish tincture, clear mass, IU - 32.3, IU - 17.6.\nStep III: Foaming, turbidity, Non Uniform mass, AU - 43, Amine 25.7.\n\nCharged - LUB 1010 - 200 gm\nFeed of P205 - 10 gm Over 10-15 min. / slow dispersion.\nBrown particles, slight foam /, AV-52, Residue - sticks on wall\nCharged Lupasol-G-20 15gm.\nFeed of (Acrylate + AIBN) mix started\nYellowish tincture / clear mass, Yellowish - clear mass.\nIU - 32.3 / clear mass.\nIU - 17.6 -, clear mass / yellow tincture.\nCharged Acrylate - 15gm.\nFeed of phosphate Ester - 7 min.\nfoaming / turbidity, Non Uniform. mass., AU - 43 / Amine 25.7",
  "process_steps": [
    {
      "name": "Step-I phosphate Ester",
      "process": [
        {
          "time": "0.5",
          "temperature": "RT-50 / N2",
          "observation": "Charged - LUB 1010 - 200 gm"
        },
        {
          "time": "1.5",
          "temperature": "RT-75 / N2",
          "observation": "Feed of P205 - 10 gm Over 10-15 min. / slow dispersion."
        },
        {
          "time": "1.5",
          "temperature": "77-80 / N2",
          "observation": "Brown particles, slight foam /, AV-52, Residue - sticks on wall"
        }
      ],
      "measurements": [
        {
          "verbatim": "AV-52"
        }
      ],
      "step": 1
    },
    {
      "name": "Step-II Acylate Intermediate",
      "process": [
        {
          "time": "0.5",
          "temperature": "RT-50/N2, 78-81",
          "observation": "Charged Lupasol-G-20 15gm."
        },
        {
          "time": "1.5",
          "temperature": "78-81/N2",
          "observation": "Feed of (Acrylate + AIBN) mix started"
        },
        {
          "time": "1.5",
          "temperature": "78-81/N2 -",
          "observation": "Yellowish tincture / clear mass, Yellowish - clear mass."
        },
        {
          "time": "4.1",
          "temperature": "78-81/N2",
          "observation": "IU - 32.3 / clear mass."
        },
        {
          "time": "3 hrs.",
          "temperature": "78-81/N2",
          "observation": "IU - 17.6 -, clear mass / yellow tincture."
        }
      ],
      "measurements": [
        {
          "verbatim": "IU - 32.3"
        },
        {
          "verbatim": "IU - 17.6 -"
        }
      ],
      "step": 2
    },
    {
      "name": "Step-III Neutralisation -",
      "process": [
        {
          "time": "0.5",
          "temperature": "RT-55/N2",
          "observation": "Charged Acrylate - 15gm."
        },
        {
          "time": "1.5",
          "temperature": "55-58/N2 -",
          "observation": "Feed of phosphate Ester - 7 min."
        },
        {
          "time": "1 hrs",
          "temperature": "55-57/N2",
          "observation": "foaming / turbidity, Non Uniform. mass., AU - 43 / Amine 25.7"
        }
      ],
      "measurements": [
        {
          "verbatim": "AU - 43"
        },
        {
          "verbatim": "Amine 25.7"
        }
      ],
      "step": 3
    }
  ],
  "samples": [
    {
      "id": "Batch NO-60",
      "analytical": [
        {
          "verbatim": "AV-52"
        },
        {
          "verbatim": "IU - 32.3"
        },
        {
          "verbatim": "IU - 17.6 -"
        },
        {
          "verbatim": "AU - 43"
        },
        {
          "verbatim": "Amine 25.7"
        }
      ],
      "sample_id": "unspecified sample"
    }
  ]
}