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← 28112025 9076 Expt Table 2025.xls · fragment 30 of 66 from this file
Original · 28112025 9076 Expt Table 2025.xls
open ↗Sheet · 28112025 9076 Expt Table 2025.converted_sheet_9076_Experiments.csv — rows 2–151 of 400
| Batch No | Step 1 | Step 2 | Step 3 | Remarks | |||||||||||||||
| Raw Materials | Reaction Conditions | Results | Raw Materials | Reaction Conditions | Results | Raw Materials | Reaction Conditions | ||||||||||||
| Name | Qty (g) | Temp. oC | Time (h) | Vac / N2 | A.V. | Other | Name | Qty (g) | Temp. oC | Time (h) | Vac / N2 | A.V. | Name | Qty (g) | Temp. oC | Time (h) | Vac / N2 | ||
| 1 | STD BYK 9076 | ||||||||||||||||||
| 2 | MPEG-350 | 300 | 35\n55\n75\n\n | 0.15\n0.5\n1-2 \n\n | N2 | 41 | During feeding of P-RM found slight exotherm Very fine yellow tincture found ,\n slight grip in viscosity found, | Step 1- Product | 152 | 35\n55\n60 | 0.15\n1\n2 | N2 | AV- 40, \nAmine value- 45 | For Carbon black pigment-Gloss, Tinting strength, Shade good \nhaving adhesion dots while cleaning Ink removal Batch 2=3<4<5 | |||||
| Phosphorous pentaoxide | 9.9 | Lupasol G-20 WF | 11 | ||||||||||||||||
| Initially found brownish dots with exotherm later on changed to pale yellow.\nIn Final product added -EHA/ Toluene/ Methoxy propyl acetate 3.33% each( by weight %) | For Carbon black pigment-Gloss, Tinting strength, Shade good \nhaving adhesion dots while cleaning Ink removal Batch 2=3<4<5 | ||||||||||||||||||
| 3 | MPEG-350 | 150 | 35 | 0.15 | |||||||||||||||
| Tripropylene glycol mono-butyl ether | 150 | 55 | 1 | N2 | 55 | Step- 1 product | 152 | 40 | 0.5 | N2 | AV-48\n | ||||||||
| Phosphorous pentaoxide | 13.2 | 60 | 2 | Lupasol G-20 WF | 13.8 | 65 | 2 | Amine value-42 | |||||||||||
| During feeding found slight exotherm ,\nVery fine yellow tincture found , slight grip in viscosity found | |||||||||||||||||||
| 4 | Vicasurf -1010 | 250 | 40 | 0.15 | Step- 1 product | 150 | 45 | 0.5 | N2 | AV-53 | |||||||||
| Butanol- 2 EO-2PO | 50 | 55 | 0.5 | N2 | 53 | Lupasol G-20 WF | 13.5 | 65 | 2.5 | Amine value-42 | |||||||||
| Phosphorous pentaoxide | 15 | 75 | 1 hr-2 hr | ||||||||||||||||
| During feeding found slight exotherm ,\nslight grip in viscosity with distinct turbidity( Not like sunflower oil) | For Carbon black pigment-Gloss, Tinting strength, Shade good \nhaving adhesion dots while cleaning Ink removal Batch 2=3<4<5 | ||||||||||||||||||
| 5 | Vicasurf -1010 | 300 | 40 | 0.15 | Step- 1 product | 152 | 40 | 0.5 | N2 | AV-38 | |||||||||
| Phosphorous pentaoxide | 10.2 | 55 | 0.5 | N2 | 38 | Lupasol G-20 WF | 7.5 | 70 | 2 | Amine value- 19 | |||||||||
| 75 | 1 hr-2 hr | ||||||||||||||||||
| Exotherm found while feed , moderate viscosity | |||||||||||||||||||
| 6 | Vicasurf -1010 | 150 | 40 | 0.5 | Step- 1 product | 170 | 40 | 0.5 | N2 | AV-38 | |||||||||
| Butanol- 2 EO-2PO | 150 | 80 | 3.5 | N2 | 42 | Lupasol G-20 WF | 7.8 | 70 | 3 | Amine value- 19 | |||||||||
| Phosphorous pentaoxide | 10.6 | ||||||||||||||||||
| For Carbon black/ Red/ White pigment-Gloss, Tinting strength, Shade good \nhaving adhesion dots while cleaning Ink | |||||||||||||||||||
| 7 | Vicasurf -1010 | 200 | 40 | 0.5 | N2 | 19 | Step- 1 product | 200 | 45 | 0.5 | N2 | AV-19 | |||||||
| Phosphorous pentaoxide | 5.2 | 75 | 3 | Slight exotherm while feeding ,\nAppearance- viscous good flow, found particles | Lupasol G-20 WF - 2EO- 2 PO | 9.6 | 70 | 3 | Amine value- 42 | ||||||||||
| Found exotherm and and slight turbidity! | |||||||||||||||||||
| 8 | Vicasurf -1010 | 300 | 40 | 0.5 | Step- 1 product | 300 | 40 | 0.5 | N2 | AV-35 | |||||||||
| Phosphorous pentaoxide | 10.5 | 75 | 3 | N2 | 36.5 | Lupasol G-20 WF | 7.5 | 75 | 3 | Amine value- 14 | |||||||||
| 9- I | Batch -8 Step-II | 95 | 45 | 2 | |||||||||||||||
| 5% Polymer (Bondex - Jeson polymer emulsion - Upon water removal) | 5 | 50 | 1 | N2 | AV-40.5\nAmine value-13 | Viscous transparent mass, less flowability\n than reference sample. AV-40.5 | |||||||||||||
| 9- II | Batch -8 Step-II | 90 | 45 | 2 | N2 | Tested on Red pigment found\n better result than earlier and very finely inferior than standard(5% less) while other parameters gloss, tinting sterngth good. | |||||||||||||
| 5% Polymer (Bondex - Jeson polymer emulsion - Upon water removal) | 10 | 50 | 1 | N2 | AV- 39.2\nAmine value-12.1 | more Viscous less transparent mass, very less flowability than reference sample.\nAV-39.2\nadded -EHA/ Toluene/ Methoxy propyl acetate 3.33% each( by weight %) | |||||||||||||
| 10 | Vicasurf -1010 (HV-115-120) | 230 | 60 | 1 | Clear reaction mass, \nno charing/residue in mass | Epomine SP- 018 | 105 | 68 | 2 | Step 1- product -80 | 248 gm % | 60 | 0.5 | Initial feed of Step 10 B slowly\n found clear transparent mass ( still 20%) then slowly\n increased turbidity. Upon total feed reaction mass became viscous non flowable yellowish white mass.\nAV-55 | |||||
| Polyphosphpric acid | 15.2 | 75 | 3 | N2 | 183 | 2 ethyl hexyl acrylate | 245 | 78 | 4 | N2 | 257 | Step-2 Product -20% | 62 gm % | 62 | 3 | ||||
| Tested sample and found good results likely resolubility/ tinting strenghth/ gloss etc. with respect to reference product. | |||||||||||||||||||
| 11 | Vicasurf -1010 (HV-115-120) | 300 | 40 | 0.15 | Epomine SP- 018 | 105 | 68 | 2\n | Step- 1 product (80) | 160 | 60 | 1 | AV-36.7 | ||||||
| Phosphorous pentaoxide | 10.5 | 55 | 0.5 | N2 | 38 | 2 ethyl hexyl acrylate | 245 | 78 | 4 | N2 | 257 | Step - 2 Product (20) | 40 | 65 | 3 | N2 | Amine value- 37 | ||
| 75 | 1 hr- 2 hr | ||||||||||||||||||
| 12 | Butanol EO - ( Unitop- 25.05.23) | 184 | 60 | 1 | Epomine SP- 018 | 105 | 68 | 2\n | Step- 1 product (80) | 160 | 60 | 1 | AV-38.9 | ||||||
| Polyphosphpric acid | 15.2 | 62 | 3 | N2 | 99 | 2 ethyl hexyl acrylate | 245 | 78 | 4 | N2 | 215 | Step - 2 Product (20) | 40 | 65 | 3 | N2 | Amine value-36 | ||
| 13 | Butanol EO - 150 gm ( Unitop- Dated 25.05.23) | 150 | 70 | 1 | Epomine SP- 018 | 105 | 68 | 2 | Amine-215 | Step- 1 product (80) | 160 | 60 | 1 | AV-32 | |||||
| Phosphorous pentaoxide | 4.4 | 75 | 3 | N2 | 34 | 2 ethyl hexyl acrylate | 245 | 78 | 4 | N2 | Step - 2 Product (20) | 40 | 65 | 3 | N2 | Amine value-33 | |||
| 14 | Vicasurf 1010 (HV-115-120) | 300 | 60 | 1 | Epomine SP- 018 | 105 | 68 | 2 | Amine-224 | Step- 1 product (80) | 160 | 60 | 1 | Tested sample and found good results likely resolubility/ tinting strenghth/ gloss etc. with respect to reference product.\nAV-37.6 \nAmine- 35.3 | |||||
| Phosphorous pentaoxide | 9.5 | 80 | 4 | N2 | 33 | 2 ethyl hexyl acrylate | 245 | 78 | 4 | N2 | Step - 2 Product (20) | 40 | N2 | ||||||
| 15 | Vicasurf 1010 (HV-115-120) | 970 | 60 | 1 | Epomine SP- 018 | 129.5 | 68 | 2 | Step- 1 product (80) | 200 | 65 | 1 | |||||||
| Phosphorous pentaoxide | 35.45 | 80 | 3 | N2 | 38.3 | 2 ethyl hexyl acrylate | 302.16 \n(0.001 % Hydroquinone) | 78 | 5 | N2 | Amine 209 | Step - 2 Product (20) | 800 | 75 | 2 | N2 | AV-34.2 | ||
| 16 | Vicasurf 1010 (HV-115-120) | 970 | 55 | 1 | Epomine SP- 018 | 129.5 | 68 | 2 | Step- 1 product (80) | 200 | 65 | 1 | While feeding of acrylate stirring off for 2 min, more viscous , | ||||||
| Phosphorous pentaoxide | 34.2 | 80 | 3 | N2 | 37.8 | 2 ethyl hexyl acrylate | 302.16 | 78-80 | 8 | N2 | Amine-210 | Step - 2 Product (20) | 800 | 75 | 2 | N2 | Application test slightly\n inferior to reference product.\nAV-36.7\n Amine-34.8 | ||
| 17 | Vicasurf 1010 (HV-115-120) | 450 | 65 | 2 hrs | N2 | AV-44\n | Epomine SP- 018 | 60 | 75 | 2 hrs | amine - 263/ | Step- 1 product (78) | 78 | 60 | 2 hrs | AV-41.5/ SAP- 80 | |||
| Polyphosphoric acid | 16.18 | 75 | 3.5 hrs | Final AV-48 \nSAP-81/ HV-120 | 2 ethyl hexyl acrylate | 140 | 80 | 4.5 hrs | N2 | SAP- 197/\n HV-170/IV-42 | Step - 2 Product (20) | 20 | 65 | 5 hrs | N2 | IV-12/HV-136.5/ \nAmine value-42.195 | |||
| 18 | Butanol EO/PO BEP-55 (110 gm HV-88) Unitop RM | 110 | 60 | 1 hrs | 47 | Step-1 Product | 110 | 58 | 1 hr | AV-37 | |||||||||
| Phosphorous pentaoxide | 2.53 | 65 | 4 hrs | N2 | Lupasol G-20 WF | 5.2 | 61 | 3 hr | N2 | Amine value-29/ | |||||||||
| 19 | Vicasurf 1010 (HV-115-120) | 300 | 40 | 0.15 | Step-1 Product | 50 | |||||||||||||
| Phosphorous pentaoxide | 10.5 | 55 | 0.5 | Lupasol G-20 WF | 2 | 55 | 2 | Amine-35 | |||||||||||
| 75 | 2 hrs | N2 | 38 | LLP ( Liquid paraffin ) 0.2 gm | 0.2 | N2 | AV-32 | ||||||||||||
| 20 | Butanol EO - PO\nHV-56 | 226 | 45 | 0.7 | Step- 1 product (80) | 160 | 60 | 6 | N2 | AV-35.6\nAmine-14 | |||||||||
| Phosphorous pentaoxide | 8.24 | 68-75 | 4.5 | N2 | 37 | Epomine SP- 018 | 90 | 80-82 | 6 | Step - 2 Product (20) | 40 | ||||||||
| 2 ethyl hexyl acrylate | 210 | 80-83 | 2 | N2 | Amine-259 | ||||||||||||||
| Amine-40.56 | |||||||||||||||||||
| AV-42.56 | |||||||||||||||||||
| 21 | Butanol EO - PO - 300 gm (Sunshield)\nHV-56 | 300 | 40 | 1 | Epomine SP- 018 | 90 | 80-82 | 6 | Step- 1 product (80) | 160 | 60 | 605 | Strength/gloss for \nC black good/ Resolubility issue | ||||||
| Phosphorous pentaoxide | 13.7 | 65-75 | 4.5 | N2 | AV-46.86 | 2 ethyl hexyl acrylate | 210 | 80-83 | 2 | N2 | 256 | Step - 2 Product (20) | 40 | N2 | |||||
| Iodine Value | Time | ||||||||||||||||||
| 70 | 2 | ||||||||||||||||||
| 37.2 | 5.5 | ||||||||||||||||||
| Solvent Blend | |||||||||||||||||||
| LBN 21A) LBN 21 +3% AMP | |||||||||||||||||||
| LBN 21B) LBN 21 +2% IPA | |||||||||||||||||||
| LBN 21 C) LBN21 A + 2% mix xylene | |||||||||||||||||||
| Solvent Blend | |||||||||||||||||||
| LBN 21D) LBN 21 +4% mix xylene | |||||||||||||||||||
| LBN 21E) LBN 21D +1% MIBK | |||||||||||||||||||
| LBN 21F) LBN 21 +2% ethyl cellosolve | |||||||||||||||||||
| 22 | BEP (1450) - (Esteem indusry) | 150 | 50 | 0.5 | Step- 1 product | 157 | 43.7 | ||||||||||||
| Phosphorous pentaoxide | 7.09 | 70-75 | 5 | N2 | 42 | Epoimine SP-018 - | 4.9 gm | 60 | 4.5 | N2 | |||||||||
| Solvent Blend | |||||||||||||||||||
| LBN 22 A) LBN 22 + 2 ethyl hexyl acrylate 3% + Xylene 1.44 % + MPA 0.6%+2 ethyl hexanol - 1.4 % | |||||||||||||||||||
| 23 | |||||||||||||||||||
| Sun Surfol R-1400- \nHV-56 | 1010 | 45-50 | 0.5 | Epomine SP- 018 | 90 | 75-81 | 2 | Step- 1 product (80) | 800 | Strength/gloss for \nC black good/ Resolubility issue\ni) With 3% MPA solvent and ii) without solvent | |||||||||
| Phosphorous pentaoxide | 47.16 | 70-75 | 4.5 | N2 | 49.5 | 2 ethyl hexyl acrylate | 210 | 78-82 | 6 | N2 | AV-1.1/ Amine 256\n/IV-37.2 | Step - 2 Product (20) | 200 | 60 | 4 | N2 | |||
| Iodine value | Time | AV-42.67/amine-39.8/HV-55.32\n/SAP-63.5/IV-7.22 | |||||||||||||||||
| 49 | 4 | ||||||||||||||||||
| 37.2 | 5.5 | ||||||||||||||||||
| 24A | Sun Surfol R-1400- \nHV-56 | 1010 | 45-50 | 0.5 | Epomine SP- 018 | 90 | 77-81 | 2 | Step- 1 product (85) | 106.25 | 60 | 4 | Pigment Green- Strength / Gloss inferior\nPigment Black & Red- All properties good. | ||||||
| Phosphorous pentaoxide | 47.16 | 70-75 | 4.5 | N2 | 49.5 | 2 ethyl hexyl acrylate | 210 | 78-82 | 6 | N2 | AV-1.1/ Amine 256\n/IV-37.2 | Step - 2 Product (15) | 18.75 | N2 | AV-53/Amine-29.5/\n HV-65/SAP-85.9/IV-6.5 | ||||
| Iodine value | Time | ||||||||||||||||||
| 49 | 4 | ||||||||||||||||||
| 37.2 | 5.5 | ||||||||||||||||||
| 24B | Sun Surfol R-1400- HV-56 | 112 | 45-50 | 0.5 | Epomine SP- 018 | 90 | 77-81 | 2 | Step- 1 product (85) | 106.25 | |||||||||
| Phosphorous pentaoxide | 4.5 | 70-75 | 4.5 | N2 | 46.34 | 2 ethyl hexyl acrylate | 210 | 78-82 | 6 | N2 | AV-0.3/\n Amine 260/IV-34.5 | Step - 2 Product (15) | 18.75 | 60 | 4 | N2 | Pigment Green- Strength / Gloss inferior\nPigment Black, Red, Violet, Blue - All properties good. | ||
| Iodine value | Time | AV-37.97/\nAmine-27.8/HV-83/IV-5. | |||||||||||||||||
| 62.2 | 2 | ||||||||||||||||||
| 46.5 | 4 | ||||||||||||||||||
| 35.6 | 5 | ||||||||||||||||||
| 24 C | Sun Surfol R-1400- HV-58 | 450 | 45-50 | 0.5 | AV- 39.8 | Yellowish floable liq AV adjusted to 39.8\n(180 gmAV-46.6+37.3 gm R-1400 to AV-39.8) | Epomine SP- 018 | 90 | 74-82 | 2 | Step- 1 product (85) | 170 | 58-60 | Feed 20 min | Pigment Black, Red, Green, Blue - All properties good | ||||
| Phosphorous pentaoxide | 22.03 | 70-75 | 4.5 | N2 | Phosphate ester- Mono- 12/ Di- 75/\nFree acid- 0.3 | 2 ethyl hexyl acrylate | 210 | 78-82 | 6 | N2 | AV- 0.2 \n / Amine - 265 \n /IV-34.5 | Step - 2 Product (15) | 30 | 60 | 4 | N2 | Pigment Green/ Violet - Strength / Gloss inferior | ||
| Iodine value | Time | AV- 35.56 \n /Amine-29.79 | |||||||||||||||||
| 62.2 | 2 | ||||||||||||||||||
| 46.5 | 4 | ||||||||||||||||||
| 35.6 | 5 | ||||||||||||||||||
| 24 CR | Sun Surfol R-1400- HV-58 | 850 | 45-50 | 0.5 | Yellowish floable liq AV adjusted to 39.8\n(180 gmAV-46.6+37.3 gm R-1400 to AV-39.8) | Epomine SP- 018 | 90 | 74-82 | 2 | Step- 1 product (85) | 483 | feed 25 min | Pigment Black, Red, Orange, \nyellow, white Blue - All properties good | ||||||
| Phosphorous pentaoxide | 39.5 | 70-75 | 4.5 | N2 | 39.8 | Phosphate ester- Mono- 12/ Di- 75/\nFree acid- 0.3 | 2 ethyl hexyl acrylate | 210 | 78-82 | 6 | N2 | AV- 0.2 \n / Amine -265/ IV-34.5 | Step - 2 Product (15) | 85.23 | 60 | 4 | N2 | AV- 35.43 \n /Amine-31.1 | |
| Iodine value | Time | ||||||||||||||||||
| 35.6 | 5 | ||||||||||||||||||
| 24 CR2 | Sun Surfol R-1400- HV-58 | 1700 | 45-50 | 0.5 | Epomine SP- 018 | 150 | 74-82 | 2 | Step- 1 product (85) | 1700 | 55-58 | 35 min | |||||||
| Phosphorous pentaoxide | 68.77 | 70-75 | 4.5 | N2 | 39.7 | Yellowish floable liq AV adjusted to 39.7\n(180 gmAV-46.6+37.3 gm R-1400 to AV-39.7) | 2 ethyl hexyl acrylate | 350 | 78-82 | 6 | N2 | AV- 0.2 \n / Amine -255 \n /IV-34 | Step - 2 Product (15) | 300 | 58-60 | 4 | N2 | AV- 35.25 \n /Amine-30.9 | |
| Iodine value | Time | ||||||||||||||||||
| Phosphate ester- Mono- 08/ Di- 81/\nFree acid- 0.25 | 70 | 2 | |||||||||||||||||
| 56 | 4 | ||||||||||||||||||
| 35 | 5.5 | ||||||||||||||||||
| 25- I | Sun Surfol R-1400- HV-56 | 160 | 35 | 0.5 | Phosphate ester- Mono- 9.7/ Di-40.16/\nFree acid- 0.29 | Epomine SP- 018 | 150 | 74-82 | 2 | Step- 1 product (80) | 80 | 60 | Feed 2 hrs | ||||||
| Polyphosphoric acid \n(AV-46 matching) | 5.714 | 55-60 | 4.5 | N2 | 46 | 2 ethyl hexyl acrylate | 350 | 78-82 | 6 | N2 | AV- 0.2 \n / Amine -255 \n /IV-34 | Step - 2 Product (20) | 20 | 60 | 4 | N2 | Found turbid mass/non uniform | ||
| Iodine value | Time | ||||||||||||||||||
| 70 | 2 | ||||||||||||||||||
| 56 | 4 | ||||||||||||||||||
| 35 | 5.5 | ||||||||||||||||||
| 25-II | Sun Surfol R-1400- HV-56 | 150 | 40 | 0.5 | Epomine SP- 018 | 150 | 74-82 | 2 | Step- 1 product (80) | 80 | 60 | Feed 2 hrs | AV-98.65 | ||||||
| Polyphosphoric acid \n(Quantity as per patent) | 12.39 | 55-60 | 4.5 | N2 | 115 | 2 ethyl hexyl acrylate | 350 | 78-82 | 6 | N2 | AV- 0.2 \n / Amine -255 \n /IV-34 | Step - 2 Product (20) | 20 | 60 | 4 | N2 | Amine -32.18\nIR PPA/P2O5 matching (mailed) | ||
| Iodine value | Time | after 2 hr found turbid mass/non uniform | |||||||||||||||||
| 70 | 2 | ||||||||||||||||||
| 56 | 4 | ||||||||||||||||||
| 35 | 5.5 | ||||||||||||||||||
| 25-A | Sun Surfol R-1400- HV-56 | 100 | 40 | 0.5 | Epomine SP- 018 | 150 | 74-82 | 2 | Step- 1 product (80) | 80 | 60 | Feed 2 hrs | |||||||
| PPA:P2O5 (20:80) | 1.071 \ngm :1.98gm | 55-60 | 4.5 | N2 | 45.75 | Phosphate ester- Mono- 14.5/ Di-61.37/\nFree acid- 0.42 | 2 ethyl hexyl acrylate | 350 | 78-82 | 6 | N2 | AV- 0.2 \n / Amine -255 \n /IV-34 | Step - 2 Product (20) | 20 | 60 | 4 | N2 | After 2 hr feed slight turbidity /yellowish flowable liq | |
| Iodine value | Time | AV-37.69\nAmine-40.72 | |||||||||||||||||
| 70 | 2 |
Extracted values
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Experiment: exp-9076-027B
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Process steps
| Step | Charged | What happened | Results | ||||||||||||||||||||
|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|
|
Step 1
temperature 40 oC atmosphere N2 time_h Feed 0.4 (h); 4.5 h hold on N2
|
Vicasurf-1010 · 1700
Phosphorous pentaoxide · 64.09
|
|
AV 38.1 unlabelled
|
||||||||||||||||||||
|
Step 2
temperature 79-81 oC (feed) then 81-82 oC (hold) atmosphere N2 (hold stage) time_h Feed 2 h; 6 h hold
|
Epomine SP- 018 · 105
2 ethyl hexyl acrylate · 245
|
|
AV 0.35 unlabelled
Amine 272 unlabelled
IV 27.5 unlabelled
|
||||||||||||||||||||
|
Step 3
temperature 54-56 oC (feed) then 57-58 oC (hold) atmosphere N2 (hold stage) time_h Feed 25 min; 4 h hold
|
Step- 1 product (80%) AV-38.1 · 280
Step - 2 Product (20) · 70
|
|
AV 33.7 unlabelled
Amine 42.3 unlabelled
|
[
{
"conditions": {
"atmosphere": "N2",
"temperature": "40 oC",
"time_h": "Feed 0.4 (h); 4.5 h hold on N2"
},
"materials": [
{
"name": "Vicasurf-1010",
"qty_g": 1700,
"role": "unknown",
"role_verbatim": "raw",
"verbatim": "Vicasurf-1010 1700"
},
{
"name": "Phosphorous pentaoxide",
"qty_g": 64.09,
"role": "unknown",
"role_verbatim": "raw",
"verbatim": "Phosphorous pentaoxide 64.09"
}
],
"procedure": [
{
"action": "charge",
"seq": 1,
"verbatim": "Vicasurf-1010 1700; Phosphorous pentaoxide 64.09 charged at start of step"
},
{
"action": "feed",
"seq": 2,
"temperature": "40 oC",
"time_h": "Feed 0.4",
"verbatim": "40 / Feed 0.4"
},
{
"action": "hold",
"atmosphere": "N2",
"seq": 3,
"temperature": "40 oC",
"time_h": 4.5,
"verbatim": "N2 / 4.5 h"
}
],
"remarks": "Found 0.1% crystal upon filter",
"results": [
{
"parameter": "AV",
"unit": "unlabelled",
"value": "38.1",
"verbatim": "38.1 (A.V. column)"
}
],
"step": 1
},
{
"conditions": {
"atmosphere": "N2 (hold stage)",
"temperature": "79-81 oC (feed) then 81-82 oC (hold)",
"time_h": "Feed 2 h; 6 h hold"
},
"materials": [
{
"name": "Epomine SP- 018",
"qty_g": 105,
"role": "unknown",
"role_verbatim": "raw",
"verbatim": "Epomine SP- 018 105"
},
{
"name": "2 ethyl hexyl acrylate",
"qty_g": 245,
"role": "unknown",
"role_verbatim": "raw",
"verbatim": "2 ethyl hexyl acrylate 245"
}
],
"procedure": [
{
"action": "charge",
"seq": 1,
"temperature": "79-81 oC",
"time_h": "Feed",
"verbatim": "Epomine SP- 018 105; 2 ethyl hexyl acrylate 245 charged at 79-81 oC, Feed 2 h"
},
{
"action": "hold",
"atmosphere": "N2",
"seq": 2,
"temperature": "81-82 oC",
"time_h": 6,
"verbatim": "81-82 / 6 / N2"
}
],
"remarks": "",
"results": [
{
"parameter": "AV",
"unit": "unlabelled",
"value": "0.35",
"verbatim": "AV- 0.35"
},
{
"parameter": "Amine",
"unit": "unlabelled",
"value": "272",
"verbatim": "Amine - 272"
},
{
"parameter": "IV",
"unit": "unlabelled",
"value": "27.5",
"verbatim": "IV-27.5"
}
],
"step": 2
},
{
"conditions": {
"atmosphere": "N2 (hold stage)",
"temperature": "54-56 oC (feed) then 57-58 oC (hold)",
"time_h": "Feed 25 min; 4 h hold"
},
"materials": [
{
"name": "Step- 1 product (80%) AV-38.1",
"qty_g": 280,
"role": "intermediate",
"verbatim": "Step- 1 product (80%) AV-38.1 280"
},
{
"name": "Step - 2 Product (20)",
"qty_g": 70,
"role": "intermediate",
"verbatim": "Step - 2 Product (20) 70"
}
],
"procedure": [
{
"action": "charge",
"seq": 1,
"temperature": "54-56 oC",
"time_h": "Feed 25 min",
"verbatim": "Step- 1 product (80%) 280; Step - 2 Product (20) 70 charged at 54-56 oC, Feed 25 min"
},
{
"action": "hold",
"atmosphere": "N2",
"seq": 2,
"temperature": "57-58 oC",
"time_h": 4,
"verbatim": "57-58 / 4 / N2"
}
],
"remarks": "Initially after 10 min feed\n found turbidity in white mass; After over night mass became clear.",
"results": [
{
"parameter": "AV",
"unit": "unlabelled",
"value": "33.7",
"verbatim": "AV- 33.7"
},
{
"parameter": "Amine",
"unit": "unlabelled",
"value": "42.3",
"verbatim": "Amine-42.3"
}
],
"step": 3
}
]
observations high
Expt Table remarks: Found 0.1% crystal upon filter (Step 1); Initially after 10 min feed found turbidity in white mass (Step 3); After over night mass became clear (Step 3). Stray measurement outside the fixed columns (Iodine value / Time block, positionally under Step 2 'Other'): 68.5 at 2, 41 at 4, 27.5 at 5.5 — parameter unconfirmed (IV assumed from header); not dropped.
More actions — correct a value · link · ignore
History (1)
| Action | Field | Value | Date |
|---|---|---|---|
| verify | 2026-08-20 |
Raw fragment JSON
{
"fragment_id": "expt-block--27b",
"source_file": "docs/Project Expt Report/28112025 9076 Expt Table 2025.xls",
"derived_from": "ocr/28112025 9076 Expt Table 2025.converted/28112025 9076 Expt Table 2025.converted_sheet_9076_Experiments.csv",
"locator": "sheet 9076_Experiments, batch block '27 B'",
"extractor": "qwen-tasks/extract-expt-block.md",
"target_aliases": [
"27 B"
],
"document_role": "summary_table",
"payload": {
"record_type": "synthesis",
"process_steps": [
{
"step": 1,
"materials": [
{
"name": "Vicasurf-1010",
"qty_g": 1700,
"role": "unknown",
"verbatim": "Vicasurf-1010 1700",
"role_verbatim": "raw"
},
{
"name": "Phosphorous pentaoxide",
"qty_g": 64.09,
"role": "unknown",
"verbatim": "Phosphorous pentaoxide 64.09",
"role_verbatim": "raw"
}
],
"procedure": [
{
"seq": 1,
"action": "charge",
"verbatim": "Vicasurf-1010 1700; Phosphorous pentaoxide 64.09 charged at start of step"
},
{
"seq": 2,
"temperature": "40 oC",
"action": "feed",
"verbatim": "40 / Feed 0.4",
"time_h": "Feed 0.4"
},
{
"seq": 3,
"atmosphere": "N2",
"time_h": 4.5,
"temperature": "40 oC",
"action": "hold",
"verbatim": "N2 / 4.5 h"
}
],
"conditions": {
"temperature": "40 oC",
"atmosphere": "N2",
"time_h": "Feed 0.4 (h); 4.5 h hold on N2"
},
"results": [
{
"parameter": "AV",
"value": "38.1",
"unit": "unlabelled",
"verbatim": "38.1 (A.V. column)"
}
],
"remarks": "Found 0.1% crystal upon filter"
},
{
"step": 2,
"materials": [
{
"name": "Epomine SP- 018",
"qty_g": 105,
"role": "unknown",
"verbatim": "Epomine SP- 018 105",
"role_verbatim": "raw"
},
{
"name": "2 ethyl hexyl acrylate",
"qty_g": 245,
"role": "unknown",
"verbatim": "2 ethyl hexyl acrylate 245",
"role_verbatim": "raw"
}
],
"procedure": [
{
"seq": 1,
"action": "charge",
"temperature": "79-81 oC",
"verbatim": "Epomine SP- 018 105; 2 ethyl hexyl acrylate 245 charged at 79-81 oC, Feed 2 h",
"time_h": "Feed"
},
{
"seq": 2,
"temperature": "81-82 oC",
"time_h": 6,
"atmosphere": "N2",
"action": "hold",
"verbatim": "81-82 / 6 / N2"
}
],
"conditions": {
"temperature": "79-81 oC (feed) then 81-82 oC (hold)",
"atmosphere": "N2 (hold stage)",
"time_h": "Feed 2 h; 6 h hold"
},
"results": [
{
"parameter": "AV",
"value": "0.35",
"unit": "unlabelled",
"verbatim": "AV- 0.35"
},
{
"parameter": "Amine",
"value": "272",
"unit": "unlabelled",
"verbatim": "Amine - 272"
},
{
"parameter": "IV",
"value": "27.5",
"unit": "unlabelled",
"verbatim": "IV-27.5"
}
],
"remarks": ""
},
{
"step": 3,
"materials": [
{
"name": "Step- 1 product (80%) AV-38.1",
"qty_g": 280,
"role": "intermediate",
"verbatim": "Step- 1 product (80%) AV-38.1 280"
},
{
"name": "Step - 2 Product (20)",
"qty_g": 70,
"role": "intermediate",
"verbatim": "Step - 2 Product (20) 70"
}
],
"procedure": [
{
"seq": 1,
"action": "charge",
"temperature": "54-56 oC",
"verbatim": "Step- 1 product (80%) 280; Step - 2 Product (20) 70 charged at 54-56 oC, Feed 25 min",
"time_h": "Feed 25 min"
},
{
"seq": 2,
"temperature": "57-58 oC",
"time_h": 4,
"atmosphere": "N2",
"action": "hold",
"verbatim": "57-58 / 4 / N2"
}
],
"conditions": {
"temperature": "54-56 oC (feed) then 57-58 oC (hold)",
"atmosphere": "N2 (hold stage)",
"time_h": "Feed 25 min; 4 h hold"
},
"results": [
{
"parameter": "AV",
"value": "33.7",
"unit": "unlabelled",
"verbatim": "AV- 33.7"
},
{
"parameter": "Amine",
"value": "42.3",
"unit": "unlabelled",
"verbatim": "Amine-42.3"
}
],
"remarks": "Initially after 10 min feed\n found turbidity in white mass; After over night mass became clear."
}
],
"observations": "Expt Table remarks: Found 0.1% crystal upon filter (Step 1); Initially after 10 min feed found turbidity in white mass (Step 3); After over night mass became clear (Step 3). Stray measurement outside the fixed columns (Iodine value / Time block, positionally under Step 2 'Other'): 68.5 at 2, 41 at 4, 27.5 at 5.5 — parameter unconfirmed (IV assumed from header); not dropped.",
"stray_results": [
{
"parameter": "unlabelled",
"value": 68.5,
"time": "2",
"verbatim": "Iodine value / Time: 68.5 at 2"
},
{
"parameter": "unlabelled",
"value": 41,
"time": "4",
"verbatim": "Iodine value / Time: 41 at 4"
},
{
"parameter": "unlabelled",
"value": 27.5,
"time": "5.5",
"verbatim": "Iodine value / Time: 27.5 at 5.5"
}
]
},
"field_confidence": {
"target_aliases": "high",
"step1_materials": "high",
"step1_conditions": "high",
"step1_results_AV": "medium",
"step2_materials": "high",
"step2_conditions": "medium",
"step2_results": "high",
"step3_materials": "high",
"step3_conditions": "medium",
"step3_results": "high",
"observations": "high",
"stray_results": "low"
}
}