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Experiments / Batch 36

Batch 36 OK

also written as LBN 36 · R-53/07032024 · 36
av
31.5
target 43.2 · -27.1% vs target
Conclusion — verbatim from the source
“Application test against violet- 27 / 23 ( Resolubility ) is good only gloss less.”
LBN 36.pdf, page 2
Aim

To develop product equivalent to reference product

Raw materials
#MaterialSourceQtyPurity %
1Surfol R-1400 (R-53/07032024)Sun shield350 gms
2Polyphosphoric acidCommercial4 gms
3Phosphorous pentaoxideCommercial4.35 gms
4Epomine SP-018Nippon60 gms100
4TolueneCommercial190 gms99
5AIBN catalystHimedia0.4 gms100
52 ethyl hexyl acrylate140 gms100
6AIBN catalyst0.64 gms100
Reaction conditions (optimized)
atmosphere: N2
Process
Step Conditions Charged What happened Results
Step 1
Phosphate ester
28112025 9076 Expt Table 2025.xls · LBN 36.pdf
temperature: 56 then 74 oC · ELN: 58-75 °Catmosphere: N2time: 4 h · ELN: 5 h
Surfol R-1400 HV-59 (R-53/07032024) 350 g
PolyPhosphoric acid 4 g
Phosphorous pentaoxide 4.35 g [Table]
Step 1) Phosphate ester- RBF with Surfol R-1400 heated to 58 deg C and then slowly added Polyphosphoric acid followed by P2O5 into it under N2 atmosphere. Digested this for 3 hrs at 70-75 deg C. Cool to RT and filter through Nylon Mesh AV-34.2 [ELN]
Expt Table remarks: After digestion cool to RT and filter through Nylon mesh [Table]
Appearance- yellowish clear [ELN]
Step-by-step (2 entries)
Time (h)Temp (°C)AtmWhat happened
56 N2 ramp start Table
4 74 N2 hold to end of digestion Table
acid_value 34.2
Step 2
Acrylate intermediate
28112025 9076 Expt Table 2025.xls · LBN 36.pdf
temperature: 68-72 oC · ELN: 65-72 °Catmosphere: N2time: 5.5 h (ELN)
Epomine SP-018 60 g
Toluene 190 ml
AIBN catalyst 0.4 g
2 ethyl hexyl acrylate 140 g (feed over 1.15 hr)
AIBN catalyst 0.64 g [Table]
Step 2) Acrylate intermediate- RBF with Epoimin SP-18 with Toluene solvent (Dissolved AIBN- 0.4 gm) heated to 66-72 deg C under N2 atmosphere. Slowly feed of 2-ethyl hexyl acylate (with dissolved AIBN- 0.64 gm) into it over 1.15 hrs and continue reaction for 3 hrs. Cool to RT removed toluene under reduced pressure. (IV-13.2) [ELN]
Initially turbid After 1 hr clear mass [Table]
Appearance- yellowish clear [ELN]
Step-by-step (3 entries)
Time (h)Temp (°C)AtmWhat happened
0.15 68-70 N2 initial hold Table
1.15 (feed) 68-72 N2 feed 2-ethyl hexyl acrylate (140 g) Table
3.5 68-72 N2 add second AIBN catalyst portion (0.64 g) Table
acid_value 31.5iodine_value 6.22iodine_value 13.2
Step 3
Neutralization
28112025 9076 Expt Table 2025.xls · LBN 36.pdf
temperature: 58-60 oC · ELN: 56-61 °Catmosphere: N2time: 2.5 hr · ELN: 3.5 h
Step - 1 Product 170 g
Step - 2 Product 30 g (feed slowly over 30 min) [Table]
Step 3) Neutralization - RBF with acrylate intermediate of step-1) (15%) heated to 56 deg C under N2 atmosphere. Slowly feed of step-2) (85%) Phosphate ester into it over 30 min and continue for 3 hrs. Cool to RT and filter through Nylon Mesh. AV- 31.5/ IV-6.22 [ELN]
Step-by-step (2 entries)
Time (h)Temp (°C)AtmWhat happened
2.5 58-60 N2 feed Step-2 product slowly over 30 min Table
Stirrer well and disperse amine Table
iodine_value 13.2acid_value 31.5iodine_value 6.22
Critical parameters — measured vs target
ParameterTargetMeasured
aminev 30.1
av 43.2 31.5
Where this record comes from
LBN 36.pdf — lab journal (primary source)
28112025 9076 Expt Table 2025.xls — researcher summary (cross-check)
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 (20 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--lbn-36--lbn-36 expt-block--36
FieldSourceExtractorConf.
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conditions.atmosphereLBN 36.pdf LBN 36.pdf, pages 1-2 qwen-tasks/extract-fragment.md@unversionedhigh
materials[0]LBN 36.pdf LBN 36.pdf, pages 1-2 qwen-tasks/extract-fragment.md@unversionedhigh
materials[1]LBN 36.pdf LBN 36.pdf, pages 1-2 qwen-tasks/extract-fragment.md@unversionedhigh
materials[2]LBN 36.pdf LBN 36.pdf, pages 1-2 qwen-tasks/extract-fragment.md@unversionedhigh
materials[3]LBN 36.pdf LBN 36.pdf, pages 1-2 qwen-tasks/extract-fragment.md@unversionedhigh
materials[4]LBN 36.pdf LBN 36.pdf, pages 1-2 qwen-tasks/extract-fragment.md@unversionedhigh
materials[5]LBN 36.pdf LBN 36.pdf, pages 1-2 qwen-tasks/extract-fragment.md@unversionedhigh
materials[6]LBN 36.pdf LBN 36.pdf, pages 1-2 qwen-tasks/extract-fragment.md@unversionedhigh
materials[7]LBN 36.pdf LBN 36.pdf, pages 1-2 qwen-tasks/extract-fragment.md@unversionedhigh
process_steps[0]LBN 36.pdf LBN 36.pdf, pages 1-2 qwen-tasks/extract-fragment.md@unversionedhigh
process_steps[1]LBN 36.pdf LBN 36.pdf, pages 1-2 qwen-tasks/extract-fragment.md@unversionedhigh
process_steps[2]LBN 36.pdf LBN 36.pdf, pages 1-2 qwen-tasks/extract-fragment.md@unversionedhigh
critical_parameters[0]LBN 36.pdf LBN 36.pdf, pages 1-2 qwen-tasks/extract-fragment.md@unversionedhigh
critical_parameters[1]LBN 36.pdf LBN 36.pdf, pages 1-2 qwen-tasks/extract-fragment.md@unversionedhigh
outcomeLBN 36.pdf LBN 36.pdf, pages 1-2 qwen-tasks/extract-fragment.md@unversionedhigh
process_steps[3]28112025 9076 Expt Table 2025.xls sheet 9076_Experiments, batch block '36' qwen-tasks/extract-expt-block.md@unversionedhigh
process_steps[4]28112025 9076 Expt Table 2025.xls sheet 9076_Experiments, batch block '36' qwen-tasks/extract-expt-block.md@unversionedhigh
process_steps[5]28112025 9076 Expt Table 2025.xls sheet 9076_Experiments, batch block '36' qwen-tasks/extract-expt-block.md@unversionedhigh
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  "aim": "To develop product equivalent to reference product",
  "conclusion": "Application test against violet- 27 / 23 ( Resolubility ) is good only gloss less.",
  "conditions": {
    "atmosphere": "N2"
  },
  "materials": [
    {
      "sr_no": 1,
      "name": "Surfol R-1400 (R-53/07032024)",
      "source": "Sun shield",
      "quantity": 350,
      "unit": "gms"
    },
    {
      "sr_no": 2,
      "name": "Polyphosphoric acid",
      "source": "Commercial",
      "quantity": 4,
      "unit": "gms"
    },
    {
      "sr_no": 3,
      "name": "Phosphorous pentaoxide",
      "source": "Commercial",
      "quantity": 4.35,
      "unit": "gms"
    },
    {
      "sr_no": 4,
      "name": "Epomine SP-018",
      "source": "Nippon",
      "quantity": 60,
      "unit": "gms",
      "purity_pct": 100
    },
    {
      "sr_no": 4,
      "name": "Toluene",
      "source": "Commercial",
      "quantity": 190,
      "unit": "gms",
      "purity_pct": 99
    },
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      "sr_no": 5,
      "name": "AIBN catalyst",
      "source": "Himedia",
      "quantity": 0.4,
      "unit": "gms",
      "purity_pct": 100
    },
    {
      "sr_no": 5,
      "name": "2 ethyl hexyl acrylate",
      "quantity": 140,
      "unit": "gms",
      "purity_pct": 100
    },
    {
      "sr_no": 6,
      "name": "AIBN catalyst",
      "quantity": 0.64,
      "unit": "gms",
      "purity_pct": 100
    }
  ],
  "process_steps": [
    {
      "step": 1,
      "time_hrs": 5,
      "temperature": "58-75 °C",
      "pressure": "N2",
      "procedure": [
        {
          "action": "Step 1) Phosphate ester- RBF with Surfol R-1400 heated to 58 deg C and then slowly added Polyphosphoric acid followed by P2O5 into it under N2 atmosphere. Digested this for 3 hrs at 70-75 deg C. Cool to RT and filter through Nylon Mesh AV-34.2"
        }
      ],
      "remarks": "Appearance- yellowish clear",
      "results": [
        {
          "type": "AV",
          "value": "34.2",
          "verbatim": "AV-34.2",
          "parameter": "unlabelled"
        }
      ]
    },
    {
      "step": 2,
      "time_hrs": 5.5,
      "temperature": "65-72 °C",
      "pressure": "N2",
      "procedure": [
        {
          "action": "Step 2) Acrylate intermediate- RBF with Epoimin SP-18 with Toluene solvent ( Dissolved AIBN- 0.4 gm) heated to 66-72 deg C under N2 atmosphere. Slowly feed of 2-ethyl hexyl acylate (with dissolved AIBN- 0.64 gm) into it over 1.15 hrs and continue reaction for 3 hrs. Cool to RT removed toluene under reduced pressure. ( IV-13.2)"
        }
      ],
      "remarks": "Appearance- yellowish clear",
      "results": [
        {
          "type": "IV",
          "value": "13.2",
          "verbatim": "IV-13.2",
          "parameter": "unlabelled"
        }
      ]
    },
    {
      "step": 3,
      "time_hrs": 3.5,
      "temperature": "56-61 °C",
      "pressure": "N2",
      "procedure": [
        {
          "action": "Step 3) Neutralization - RBF with acrylate intermediate of step-1) (15%) heated to 56 deg C under N2 atmosphere. Slowly feed of step-2) (85%) Phosphate ester into it over 30 min and continue for 3 hrs. Cool to RT and filter through Nylon Mesh. AV- 31.5/ IV-6.22"
        }
      ],
      "results": [
        {
          "type": "AV",
          "value": "31.5",
          "verbatim": "AV- 31.5",
          "parameter": "unlabelled"
        },
        {
          "type": "IV",
          "value": "6.22",
          "verbatim": "IV-6.22",
          "parameter": "unlabelled"
        }
      ]
    },
    {
      "step": 1,
      "materials": [
        {
          "name": "Surfol R-1400 HV-59 (R-53/07032024)",
          "qty": "350 g",
          "role": "reactant",
          "verbatim": "i) Surfol R-1400 HV-59    (R-53/07032024)"
        },
        {
          "name": "PolyPhosphoric acid",
          "qty": "4 g",
          "role": "reactant",
          "verbatim": "ii) PolyPhosphoric acid"
        },
        {
          "name": "Phosphorous pentaoxide",
          "qty": "4.35 g",
          "role": "reactant",
          "verbatim": "ii) Phosphorous pentaoxide"
        }
      ],
      "procedure": [
        {
          "seq": 1,
          "temperature": "56 oC",
          "verbatim": "56"
        },
        {
          "seq": 2,
          "temperature": "74 oC",
          "time_h": "4",
          "atmosphere": "N2",
          "verbatim": "74 / 4 / N2"
        }
      ],
      "conditions": {
        "temperature": "56 then 74 oC",
        "atmosphere": "N2",
        "time_h": "4 h"
      },
      "results": [
        {
          "parameter": "acid_value",
          "value": "34.2",
          "unit": "as printed",
          "verbatim": "34.2"
        }
      ],
      "remarks": "Expt Table remarks: After digestion cool to RT and filter through Nylon mesh"
    },
    {
      "step": 2,
      "materials": [
        {
          "name": "Epomine SP- 018",
          "qty": "60 gm",
          "role": "reactant",
          "verbatim": "i)  Epomine SP- 018"
        },
        {
          "name": "Toluene",
          "qty": "190 ml",
          "role": "solvent",
          "verbatim": "ii) Toluene"
        },
        {
          "name": "AIBN catalyst",
          "qty": "0.4 gm",
          "role": "catalyst",
          "verbatim": "iii) AIBN catalyst"
        },
        {
          "name": "2 ethyl hexyl acrylate",
          "qty": "140 gm",
          "role": "reactant",
          "addition": "feed over 1.15 hr at 68-72 oC under N2 (cell layout shows staged feed, not start-of-step charge)",
          "verbatim": "iv)   2 ethyl hexyl acrylate"
        },
        {
          "name": "AIBN catalyst",
          "qty": "0.64 gm",
          "role": "catalyst",
          "verbatim": "v)  AIBN catalyst"
        }
      ],
      "procedure": [
        {
          "seq": 1,
          "temperature": "68-70 oC",
          "time_h": "0.15",
          "verbatim": "68-70 / 0.15"
        },
        {
          "seq": 2,
          "temperature": "68-72 oC",
          "time_h": "1.15 hr feed",
          "atmosphere": "N2",
          "action": "feed 2 ethyl hexyl acrylate (140 gm)",
          "verbatim": "68-72 / 1.15\n hr feed / N2 / Feed"
        },
        {
          "seq": 3,
          "temperature": "68-72 oC",
          "time_h": "3.5",
          "atmosphere": "N2",
          "action": "add second AIBN catalyst portion (0.64 gm)",
          "verbatim": "68-72 / 3.5 / N2"
        }
      ],
      "conditions": {
        "temperature": "68-72 oC",
        "atmosphere": "N2"
      },
      "results": [
        {
          "parameter": "acid_value",
          "value": "31.5",
          "verbatim": "AV-31.5"
        },
        {
          "parameter": "iodine_value",
          "value": "6.22",
          "verbatim": "IV-6.22"
        }
      ],
      "observations": [
        "Initially turbid After 1 hr clear mass"
      ]
    },
    {
      "step": 3,
      "materials": [
        {
          "name": "Step - 1 Product",
          "qty": "170 gm",
          "role": "intermediate",
          "verbatim": "Step - 1 Product"
        },
        {
          "name": "Step -  2 Product ",
          "qty": "30 gm",
          "role": "intermediate",
          "addition": "feed slowly over 30 min",
          "verbatim": "Step -  2 Product "
        }
      ],
      "procedure": [
        {
          "seq": 1,
          "action": "feed Step-2 product slowly over 30 min",
          "temperature": "58-60 oC",
          "time_h": "2.5",
          "atmosphere": "N2",
          "verbatim": "58-60 / 2.5 hr / N2 / Feed  slowly \nover 30 min"
        },
        {
          "seq": 2,
          "action": "Stirrer well and disperse amine",
          "verbatim": "Stirrer well and\n disperse amine"
        }
      ],
      "conditions": {
        "temperature": "58-60 oC",
        "atmosphere": "N2",
        "time_h": "2.5 hr"
      },
      "results": [
        {
          "parameter": "iodine_value",
          "value": "13.2",
          "verbatim": "IV-13.2"
        }
      ]
    }
  ],
  "critical_parameters": [
    {
      "no": 1,
      "parameter": "aminev",
      "reference_value": "30.1"
    },
    {
      "no": 2,
      "parameter": "av",
      "reference_value": "43.2",
      "value": "31.5"
    }
  ],
  "outcome": {
    "status": "ok",
    "basis": "Application test against violet- 27 / 23 ( Resolubility ) is good only gloss less.",
    "citation": "LBN 36.pdf, page 2"
  }
}