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Experiments / Batch 55

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21/1/26 · also written as Batch-55 · BYK 9076 · Batch-55D
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: Yellowish Brownish appearance, No particles, clear mass, AV-52.85, Mono - 18.39, Di - 72.44, Free Acid - 0.3. Step II: HV - 27.5 / 5.5 hrs, Clear yellowish mass. Step III: Slight foam, Turbidity. Blend 55D: AV - 26.12, Avine - 12.86. BEP-1100M charged - 150 gm Feed of P205 - 8.68 gm, Disperse well., Yellowish Brownish appearance, No particles / clear mass, AV-52.85 / Mono - 18.39, Di - 72.44, Free Acid - 0.3 Charged Sp-18 - 72.8 gm Feed of 2-Ethyl hexyl Acylate / 2 hrs HV - 27.5 / 5.5 hrs., Clear yellowish mass charged Acrylate - 15 gm, feed of phosphate ester - 85 gm Over 15-20 min Slight foam / Turbidity.

Procedure summary

Step I: Phosphate ester synthesis using BEP-1100M. Step II: Acylate intermediate synthesis. Step III: Neutralization. Blend 55D created.

Raw materials
MaterialQtyMolesRole
BEP-1100M, BuEO-PO/Block Copolymers Esters, HV - 50.85 (crossed out) ×2150 gm0.182reactant
P205 ×28.68 gm0.0611reactant
Epamine Sp-18 ×272.8 gmreactant
2-Ethyl hexyl Acylate ×2169.1 gm70%reactant
BEP-10050 %-
Phosphate Ester (Step-II)85 gmreactant
Acrylate Intermediate (Step-II)15 gmreactant
Reaction conditions (optimized)
atmosphere: N2other: Step I: RT-50 to 75-80°C; Step II: 75-79 to 77-81°C; Step III: 55 to 55-56°C
Process
Step Conditions Charged What happened Results
Step 1
Step-I Phosphate Esters
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
Step 4
Batch-55D Blending
9076 Exp 48-60_1.pdf
B.NO 55
BEP-100
Sample unspecified sample
AV-52.85
Mono - 18.39
Di - 72.44
Free Acid - 0.3
HV - 27.5 / 5.5 hrs.
AV - 26.12
Avine - 12.86
Where this record comes from
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 (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-55 qwen-extract--9076-exp-48-60_1--batch-55
FieldSourceExtractorConf.
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conditions.atmosphere9076 Exp 48-60_1.pdf Page 17-18 qwen-tasks/extract-fragment.md@direct-v1high
materials[0]9076 Exp 48-60_1.pdf Page 17-18 qwen-tasks/extract-fragment.md@direct-v1high
materials[1]9076 Exp 48-60_1.pdf Page 17-18 qwen-tasks/extract-fragment.md@direct-v1high
materials[2]9076 Exp 48-60_1.pdf Page 17-18 qwen-tasks/extract-fragment.md@direct-v1high
materials[3]9076 Exp 48-60_1.pdf Page 17-18 qwen-tasks/extract-fragment.md@direct-v1high
materials[4]9076 Exp 48-60_1.pdf Page 17-18 qwen-tasks/extract-fragment.md@direct-v1high
procedure_summary9076 Exp 48-60_1.pdf Page 17-18 qwen-tasks/extract-fragment.md@direct-v1high
observations9076 Exp 48-60_1.pdf pages 16-17 qwen-tasks/extract-fragment.md@unversionedhigh
materials[5]9076 Exp 48-60_1.pdf pages 16-17 qwen-tasks/extract-fragment.md@unversionedmedium
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materials[8]9076 Exp 48-60_1.pdf pages 16-17 qwen-tasks/extract-fragment.md@unversionedmedium
materials[9]9076 Exp 48-60_1.pdf pages 16-17 qwen-tasks/extract-fragment.md@unversionedmedium
materials[10]9076 Exp 48-60_1.pdf pages 16-17 qwen-tasks/extract-fragment.md@unversionedmedium
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samples[0]9076 Exp 48-60_1.pdf pages 16-17 qwen-tasks/extract-fragment.md@unversionedhigh
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      "link_basis": "alias match: Batch-55",
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  "validation": {
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    "corrections_applied": []
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  "date": "21/1/26",
  "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 75-80°C; Step II: 75-79 to 77-81°C; Step III: 55 to 55-56°C"
  },
  "materials": [
    {
      "name": "BEP-1100M",
      "quantity": "150",
      "unit": "gm",
      "role": "reactant",
      "notes": "BuEO-PO/Block Copolymers Esters"
    },
    {
      "name": "P205",
      "quantity": "8.68",
      "unit": "gm",
      "role": "reactant"
    },
    {
      "name": "Epamine Sp-18",
      "quantity": "72.8",
      "unit": "gm",
      "role": "reactant"
    },
    {
      "name": "2-Ethyl hexyl Acylate",
      "quantity": "169.1",
      "unit": "gm",
      "role": "reactant"
    },
    {
      "name": "BEP-100",
      "quantity": "50",
      "unit": "%",
      "role": "unknown",
      "notes": "Used in Batch-55D",
      "role_verbatim": "blend_component"
    },
    {
      "name": "BEP-1100M, BuEO-PO/Block Copolymers Esters, HV - 50.85 (crossed out)",
      "quantity": "150",
      "unit": "gm",
      "molecular_weight": "820",
      "moles": "0.182",
      "role": "reactant"
    },
    {
      "name": "P205",
      "quantity": "8.68",
      "unit": "gm",
      "molecular_weight": "141.94",
      "moles": "0.0611",
      "role": "reactant"
    },
    {
      "name": "Epamine Sp-18",
      "quantity": "72.8",
      "unit": "gm",
      "percentage": "30%",
      "role": "reactant"
    },
    {
      "name": "2-Ethyl hexyl Acylate",
      "quantity": "169.1",
      "unit": "gm",
      "molecular_weight": "184.27",
      "moles": "70%",
      "role": "reactant"
    },
    {
      "name": "Phosphate Ester (Step-II)",
      "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 using BEP-1100M. Step II: Acylate intermediate synthesis. Step III: Neutralization. Blend 55D created.",
  "observations": "Step I: Yellowish Brownish appearance, No particles, clear mass, AV-52.85, Mono - 18.39, Di - 72.44, Free Acid - 0.3.\nStep II: HV - 27.5 / 5.5 hrs, Clear yellowish mass.\nStep III: Slight foam, Turbidity.\nBlend 55D: AV - 26.12, Avine - 12.86.\n\nBEP-1100M charged - 150 gm\nFeed of P205 - 8.68 gm, Disperse well., Yellowish Brownish appearance, No particles / clear mass, AV-52.85 / Mono - 18.39, Di - 72.44, Free Acid - 0.3\nCharged Sp-18 - 72.8 gm\nFeed of 2-Ethyl hexyl Acylate / 2 hrs\nHV - 27.5 / 5.5 hrs., Clear yellowish mass\ncharged Acrylate - 15 gm, feed of phosphate ester - 85 gm Over 15-20 min\nSlight foam / Turbidity.",
  "process_steps": [
    {
      "name": "Step-I Phosphate Esters",
      "process": [
        {
          "time": "0.5 hrs",
          "temperature": "RT-50/N2",
          "observation": "BEP-1100M charged - 150 gm"
        },
        {
          "time": "4.5 hrs",
          "temperature": "75-80/N2",
          "observation": "Feed of P205 - 8.68 gm, Disperse well., Yellowish Brownish appearance, No particles / clear mass, AV-52.85 / Mono - 18.39, Di - 72.44, Free Acid - 0.3"
        }
      ],
      "measurements": [
        {
          "verbatim": "AV-52.85"
        },
        {
          "verbatim": "Mono - 18.39"
        },
        {
          "verbatim": "Di - 72.44"
        },
        {
          "verbatim": "Free Acid - 0.3"
        }
      ],
      "step": 1,
      "materials": {}
    },
    {
      "name": "Step-II Acylate Intermediate",
      "process": [
        {
          "time": "0.5",
          "temperature": "75-79 / N2",
          "observation": "Charged Sp-18 - 72.8 gm"
        },
        {
          "time": "2 hrs",
          "temperature": "77-81 / N2",
          "observation": "Feed of 2-Ethyl hexyl Acylate / 2 hrs"
        },
        {
          "time": "5.5",
          "temperature": "77-81 / N2",
          "observation": "HV - 27.5 / 5.5 hrs., Clear yellowish mass"
        }
      ],
      "measurements": [
        {
          "verbatim": "HV - 27.5 / 5.5 hrs."
        }
      ],
      "step": 2
    },
    {
      "name": "Step-III Neutralisation",
      "process": [
        {
          "time": "0.5",
          "temperature": "55 / N2",
          "observation": "charged Acrylate - 15 gm, feed of phosphate ester - 85 gm Over 15-20 min"
        },
        {
          "time": "2.5",
          "temperature": "55-56 / N2",
          "observation": "Slight foam / Turbidity."
        }
      ],
      "step": 3
    },
    {
      "name": "Batch-55D Blending",
      "materials": [
        {
          "name": "B.NO 55",
          "percentage": "50%"
        },
        {
          "name": "BEP-100",
          "percentage": "50%"
        }
      ],
      "measurements": [
        {
          "verbatim": "AV - 26.12"
        },
        {
          "verbatim": "Avine - 12.86"
        }
      ],
      "step": 4
    }
  ],
  "samples": [
    {
      "id": "Batch-55",
      "analytical": [
        {
          "verbatim": "AV-52.85"
        },
        {
          "verbatim": "Mono - 18.39"
        },
        {
          "verbatim": "Di - 72.44"
        },
        {
          "verbatim": "Free Acid - 0.3"
        },
        {
          "verbatim": "HV - 27.5 / 5.5 hrs."
        },
        {
          "verbatim": "AV - 26.12"
        },
        {
          "verbatim": "Avine - 12.86"
        }
      ],
      "sample_id": "unspecified sample"
    }
  ]
}