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Experiments / Batch 23

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2024-8-04 · also written as Lab Batch 23 · Lab Batch23 · 23
Aim

To develop product equivalent to reference product

Observations

Appearance was clear non yellowish. (Step-A) initially found clear reaction mass, later on changed to yellowish in nature. Built viscosity at end of reaction. (Step-B) Flow able yellowish liquid. (Step-C) Expt Table remarks: Strength/gloss for C black good/ Resolubility issue i) With 3% MPA solvent and ii) without solvent; Final product: AV-42.67/amine-39.8/HV-55.32/SAP-63.5/IV-7.22

Raw materials
#MaterialSourceQtyPurity %
1Sun Surfol R-1400-FOIL1010 gms100
2P-PentaoxideFOIL47.16 gms100
3Epomine 018-90 gms100
42-ethyl hexyl acrylate210 gms100
Reaction conditions (optimized)
atmosphere: nitrogen
Process
Step Conditions Charged What happened Results
Step 1
Step A
28112025 9076 Expt Table 2025.xls · Lab Batch 23.pdf
temperature: 45-50; then 70-75 °C · ELN: 65-85 °Catmosphere: N2time: 0.5; then 4.5 h · ELN: 1-5 h
Sun Surfol R-1400- HV-56 1010 g
Phosphorous pentaoxide 47.16 g
Epomine SP- 018 (Table, no quantity given)
Step- A To main reactor added Sun Surfol R-1400 under stirring and nitrogen atmosphere temp. 60 deg increased temp slowly with addition of P-Pentaoxide. Upon feed completion temp raised to 75 deg C and digested for 2-3 hrs. Appearance was clear non yellowish. Upon digestion cooled to RT. [ELN]
2024-8-04 12:17:59 [ELN remarks]
Step-by-step (2 entries)
Time (h)Temp (°C)AtmWhat happened
0.5 45-50 Sun Surfol R-1400- HV-56, 1010 g Table
4.5 70-75 N2 Phosphorous pentaoxide, 47.16 g Table
acid_value 50iodine_value 49iodine_value 37.2
Step 2
Step B
28112025 9076 Expt Table 2025.xls · Lab Batch 23.pdf
temperature: 75-81; then 78-82 °C · ELN: 55-80 °Catmosphere: N2time: 2; then 6 h · ELN: 1-8 h
Epomine 018- 90 g (ELN)
2 ethyl hexyl acrylate 210 g
Step-B To main reactor added Epomine 018- reaction mass under stirring and nitrogen atmosphere temp. 75 deg Started slowly addition of 2- ethyl hexyl acrylate slowly. initially found clear reaction mass, later on changed to yellowish in nature. Built viscosity at end of reaction. [ELN]
Step-by-step (2 entries)
Time (h)Temp (°C)AtmWhat happened
2 75-81 stage 1 Table
6 78-82 N2 2 ethyl hexyl acrylate, 210 g Table
acid_value 1.1amine_value 256iodine_value 37.2
Step 3
Step C
28112025 9076 Expt Table 2025.xls · Lab Batch 23.pdf
temperature: 60 °C · ELN: 60-65 °Catmosphere: N2time: 4 h · ELN: 1-5 h
Step- 1 product (80) 800 g
Step - 2 Product (20) 200 g
Step-C To main reactor added Step- B reaction mass (20%) - reaction mass under stirring and nitrogen atmosphere temp. 55 deg Started slowly addition of Step- A (80%) reaction mass in it. initially found clear reaction mass, yellowish in nature with viscosity. Mixed for 3 hrs then cooled to RT. [ELN]
Flow able yellowish liquid. [ELN remarks]
Strength/gloss for C black good/ Resolubility issue i) With 3% MPA solvent and ii) without solvent [Table remarks]
Step-by-step (1 entry)
Time (h)Temp (°C)AtmWhat happened
4 60 N2 Step-1 product (80), 800 g; Step-2 Product (20), 200 g Table
acid_value 42.67amine_value 39.8hydroxyl_value 55.32saponification_value 63.5iodine_value 7.22
Critical parameters — measured vs target
ParameterTargetMeasured
aminev 30.1
av 43.2
Where this record comes from
Lab Batch 23.pdf — lab journal (primary source)
28112025 9076 Expt Table 2025.xls — researcher summary (cross-check)
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Field-by-field provenance (16 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--lab-batch-23--lab-batch-23 expt-block--23
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  "date": "2024-8-04",
  "aim": "To develop product equivalent to reference product",
  "conditions": {
    "atmosphere": "nitrogen"
  },
  "materials": [
    {
      "sr_no": "1",
      "name": "Sun Surfol R-1400-",
      "source": "FOIL",
      "quantity": "1010",
      "unit": "gms",
      "purity_pct": "100"
    },
    {
      "sr_no": "2",
      "name": "P-Pentaoxide",
      "source": "FOIL",
      "quantity": "47.16",
      "unit": "gms",
      "purity_pct": "100"
    },
    {
      "sr_no": "3",
      "name": "Epomine 018-",
      "quantity": "90",
      "unit": "gms",
      "purity_pct": "100"
    },
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      "sr_no": "4",
      "name": "2-ethyl hexyl acrylate",
      "quantity": "210",
      "unit": "gms",
      "purity_pct": "100"
    }
  ],
  "process_steps": [
    {
      "step": 1,
      "time": "1-5",
      "temperature": "65-85",
      "pressure_vacuum_n2": "Yes",
      "procedure": [
        {
          "action": "Step- A To main reactor added Sun Surfol R-1400 under stirring and nitrogen atmosphere temp. 60 deg increased temp slowly with addition of P-Pentaoxide. Upon feed completion temp raised to 75 deg C and digested for 2-3 hrs. Appearance was clear non yellowish. Upon digestion cooled to RT. AV-50"
        }
      ],
      "remarks": "2024-8-04 12:17:59"
    },
    {
      "step": 2,
      "time": "1-8",
      "temperature": "55-80",
      "pressure_vacuum_n2": "Yes",
      "procedure": [
        {
          "action": "Step-B To main reactor added Epomine 018- reaction mass under stirring and nitrogen atmosphere temp. 75 deg Started slowly addition of 2- ethyl hexyl acrylate slowly. initially found clear reaction mass, later on changed to yellowish in nature. Built viscosity at end of reaction."
        }
      ],
      "remarks": "AV-1.1/ Amine 256 /IV-37.2"
    },
    {
      "step": 3,
      "time": "1-5",
      "temperature": "60-65",
      "pressure_vacuum_n2": "Yes",
      "procedure": [
        {
          "action": "Step-C To main reactor added Step- B reaction mass (20%) - reaction mass under stirring and nitrogen atmosphere temp. 55 deg Started slowly addition of Step- A (80%) reaction mass in it. initially found clear reaction mass, yellowish in nature with viscosity. Mixed for 3 hrs then cooled to RT."
        }
      ],
      "remarks": "Flow able yellowish liquid. AV-42.67/amine-39.8/HV-55.32 /SAP-63.5/IV-7.22"
    },
    {
      "name": "Step 1",
      "materials": [
        {
          "name": "Sun Surfol R-1400-  \nHV-56",
          "quantity": 1010,
          "unit": "g",
          "role": "reactant"
        },
        {
          "name": "Phosphorous pentaoxide",
          "quantity": 47.16,
          "unit": "g",
          "role": "reactant"
        },
        {
          "name": "Epomine SP- 018",
          "role": "reactant"
        }
      ],
      "procedure": [
        {
          "seq": 1,
          "temperature": "45-50",
          "time_h": 0.5,
          "verbatim": "Sun Surfol R-1400-  HV-56, 1010 g, 45-50 oC, 0.5 h"
        },
        {
          "seq": 2,
          "temperature": "70-75",
          "time_h": 4.5,
          "atmosphere": "N2",
          "verbatim": "Phosphorous pentaoxide, 47.16 g, 70-75 oC, 4.5 h, N2"
        }
      ],
      "conditions": {
        "temperature": "45-50; then 70-75",
        "atmosphere": "N2",
        "time_h": "0.5; then 4.5"
      },
      "results": [
        {
          "parameter": "A.V.",
          "value": 49.5,
          "verbatim": "49.5"
        },
        {
          "parameter": "Iodine value",
          "value": 49,
          "at_time_h": 4,
          "verbatim": "Iodine value 49, Time 4"
        },
        {
          "parameter": "Iodine value",
          "value": 37.2,
          "at_time_h": 5.5,
          "verbatim": "Iodine value 37.2, Time 5.5"
        }
      ],
      "step": 1
    },
    {
      "name": "Step 2",
      "materials": [
        {
          "name": "90",
          "role": "reactant"
        },
        {
          "name": "2 ethyl hexyl acrylate",
          "quantity": 210,
          "unit": "g",
          "role": "reactant"
        }
      ],
      "procedure": [
        {
          "seq": 1,
          "temperature": "75-81",
          "time_h": 2,
          "verbatim": "90, 75-81, 2 (column positions: Name=90, Qty=75-81, Temp=2)"
        },
        {
          "seq": 2,
          "temperature": "78-82",
          "time_h": 6,
          "atmosphere": "N2",
          "verbatim": "2 ethyl hexyl acrylate, 210 g, 78-82 oC, 6 h, N2"
        }
      ],
      "conditions": {
        "temperature": "75-81; then 78-82",
        "atmosphere": "N2",
        "time_h": "2; then 6"
      },
      "results": [
        {
          "parameter": "A.V.",
          "value": 1.1,
          "verbatim": "AV-1.1"
        },
        {
          "parameter": "Amine value",
          "value": 256,
          "verbatim": "Amine 256"
        },
        {
          "parameter": "Iodine value",
          "value": 37.2,
          "verbatim": "IV-37.2"
        }
      ],
      "step": 2
    },
    {
      "name": "Step 3",
      "materials": [
        {
          "name": "Step-  1 product  (80)",
          "quantity": 800,
          "unit": "g",
          "role": "intermediate"
        },
        {
          "name": "Step -  2 Product  (20)",
          "quantity": 200,
          "unit": "g",
          "role": "intermediate"
        }
      ],
      "procedure": [
        {
          "seq": 1,
          "temperature": "60",
          "time_h": 4,
          "atmosphere": "N2",
          "verbatim": "Step-1 product (80), 800 g; Step-2 Product (20), 200 g; 60 oC, 4 h, N2"
        }
      ],
      "conditions": {
        "temperature": "60",
        "atmosphere": "N2",
        "time_h": "4"
      },
      "results": [],
      "step": 3
    }
  ],
  "critical_parameters": [
    {
      "parameter": "aminev",
      "reference_value": "30.1"
    },
    {
      "parameter": "av",
      "reference_value": "43.2"
    }
  ],
  "observations": "Appearance was clear non yellowish. (Step-A)\ninitially found clear reaction mass, later on changed to yellowish in nature. Built viscosity at end of reaction. (Step-B)\nFlow able yellowish liquid. (Step-C)\n\nExpt Table remarks: Strength/gloss for C black good/ Resolubility issue i) With 3% MPA solvent and ii) without solvent; Final product: AV-42.67/amine-39.8/HV-55.32/SAP-63.5/IV-7.22"
}