Compounding Precipitated Silica in Elastomers – Theory and Practice

Compounding Precipitated Silica in Elastomers – Theory and Practice
اسم المؤلف
Norman Hewitt
التاريخ
14 سبتمبر 2023
المشاهدات
239
التقييم
(لا توجد تقييمات)
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Compounding Precipitated Silica in Elastomers – Theory and Practice
Norman Hewitt
Table of Contents
Acknowledgements xiii
Preface xv
Chapter 1: SILICA AS A REINFORCING FILLER
1.1 Introduction 1
1.2 Manufacture of Precipitated Silica 2
1.3 Silica and Carbon Black 3
1.4 Silica Surface Area 5
1.5 Silica Free Water 7
1.6 Silica Free Water, Affect on Visible Dispersion 11
1.7 Silica Surface Silanol Groups 12
1.8 Silica pH 16
1.9 Soluble Salts in Silica 18
1.10 Physical Form and Sensity of Silica 19
1.11 Other Silica Properties 21
1.12 Silane Treated Silicas 21
Chapter 2: COMPOUNDING PRECIPITATED SILICA IN
NATURAL RUBBER
2.1 Introduction 25
2.2 Silica and Carbon Black 25
2.3 Activation: Zinc Oxide 28
2.4 Cure Activation: Glycols 29
2.5 Acceleration with Secondary Accelerators in Normal Sulfur Systems 31
2.6 Acceleration: Single Accelerators in Normal Sulfur Systems 33
2.7 Acceleration: Single Accelerators; Vulcanizate Properties 37
2.8 Acceleration: Low Sulfur/Sulfur Donor Systems 42
2.9 Reversion 47
2.10 Antioxidant Systems: Non-staining 50
2.11 Plasticization 51
2.12 Tear Resistance 53
2.13 Tear Resistance: Contour Curve Studies of Silica Content Effects 60
2.14 Tear Resistance: Silica Primary Particle Size 64
2.15 Tear Resistance; Non-Marking Solid tires 65
2.16 Shelf Aged Stiffness and Green Strength 68
2.17 Peroxide Cure 69
2.18 Peroxide Curing: Silica Reinforcement and Structure 70
2.19 Peroxide Curing: Silica Surface Area 73
2.20 Peroxide Cure: Silane Coupling 76
2.21 Silane Coupling: Sulfur Cure Systems 77
2.22 Zinc-Free Cure Systems 78
2.23 Zinc-Free Cure Systems: Polyisoprene (IR) 79
2.24 Brass Adhesion 81viii
2.25 Brass Adhesion Mechanism 82
2.26 Adhesion to Textile Fabrics; the HRH System 83
2.27 Fabric Adhesion: Dynamic Testing 85
2.28 Heat Resistance 86
Natural Rubber Formulary 89
Chapter 3: COMPOUNDING PRECIPITATED SILICA IN
EMULSION SBR
3.1 Introduction 169
3.2 Silica and Carbon Black 169
3.3 Cure Systems: Activation with Glycols 171
3.4 Cure System: Zinc Oxide Activation 174
3.5 Cure System: Magnesium Oxide Activation 180
3.6 Cure System: Lead oxide (Litharge) Activation 181
3.7 Cure System: Stearic Acid 181
3.8 Cure Systems: Primary, Secondary Accelerators 181
3.9 Cure Systems: Single Accelerators 182
3.10 Cure Systems: Sulfur Concentration 185
3.11 Plasticization 187
3.12 Antioxidants 189
3.13 Tear Resistance: Silica Primary Particle Size 190
3.14 Tear Resistance: Silica Content 191
3.15 Fabric Adhesion 192
3.16 Heat Resistance 193
3.17 Silane Coupling 193
3.18 Silane Coupling: Competition 196
Emulsion SBR Formulary 199
Chapter 4: COMPOUNDING PRECIPITATED SILICA IN
SOLUTION SBR AND BR
4.1 Introduction 245
4.2 Silica and Carbon Black 245
4.3 Zinc-Free Cure Systems 247
4.4 Zinc-Free Cure Systems: Accelerators & Sulfur 249
4.5 Zinc-Free Cure Systems: Polymer Effects 251
4.6 Zinc-Free Cure Systems: Zinc Oxide and HMT 252
4.7 Zinc-Free Cure Systems: Effects of Additives 256
4.8 Zinc-Free Cure Systems: Sulfur Content 257
4.9 Zinc-Free Cure System: Antioxidants 259
4.10 Zinc-Free Cure Systems: Processing 260
4.11 Zinc-Free Systems: Plasticizers 262
4.12 Zinc-Free Systems: Additive Plasticizers 263
4.13 Silane Coupling: Pretreated Silica 264
4.14 Silane Coupling 265
4.15 Zinc-Free Cure Systems: Surface Area Effects 268ix
4.16 Zinc-Free Cure Systems: Trouser Tear Strength 271
4.17 Zinc-Free Cure Systems ; Silica Content 272
4.18 Zinc-Free Cure Systems: Durometer Equivalents 274
Solution SBR and BR Formulary 277
Chapter 5:COMPOUNDING PRECIPITATED SILICA IN
EPDM
5.1 Introduction 311
5.2 Silica and Carbon Black 311
5.3 Acceleration Systems 314
5.4 Low Sulfur Systems with Donors 315
5.5 Activation: Oxides and Glycols 317
5.6 Antioxidants: Heat Resistance 318
5.7 Zinc-Free Cure Systems 319
5.8 Silane Coupling 323
5.9 Silica Surface Area 325
5.10 Peroxide Cure Systems 328
5.11 Processing 329
5.12 Adhesion to Brass 330
5.13 Fabric Adhesion 333
5.14 Adhesion to Zinc (Galvanized) Coatings 336
5.15 Compression Fatigue Life 338
EPDM Formulary 345
Chapter 6: COMPOUNDING PRECIPITATED SILICA IN
NEOPRENE
6.1 Introduction 387
6.2 NSM (Type W) Neoprene: Oxide Crosslinking 388
6.3 NSM Neoprene (W): Organic Acceleration 389
6.4 NSM Neoprene: Glycol Activation 390
6.5 NSM Neoprene: Plasticization 391
6.6 NSM Neoprene: Silica and Black 392
6.7 Silica Surface Area 395
6.8 NSM Neoprene: Silane Coupling 396
6.9 NSM Neoprene: Fabric Adhesion 398
6.10 NSM Neoprene: Brass Adhesion 400
6.11 NSM Neoprene: Water Absorption 403
6.12 Sulfur Modified (SM) Neoprene: Cure Systems 404
6.13 SM Neoprene: Glycol Activation 407
6.14 SM Neoprene: Retarding Scorch 407
6.15 SM Neoprene: Silane Coupling 407
6.16 SM Neoprene: Processing 408
6.17 SM Neoprene: Silica Surface Area Effects 410
6.18 SM Neoprene: Silica Free Water Content 410
6.19 SM Neoprene: Cord and Fabric Adhesion 411x
6.20 SM Neoprene: Brass Adhesion 414
Neoprene Formulary 416
Chapter 7: COMPOUNDING PRECIPITATED SILICA IN
NITRILE
7.1 Introduction 445
7.2 Silica and Carbon Black 445
7.3 Silica Surface Area 449
7.4 NBR/PVC Blends 452
7.5 Acceleration: Sulfur Content 452
7.6 Accelerators 453
7.7 Activators 456
7.8 Silane Coupling 460
7.9 Peroxide Curing 462
7.10 Processing 464
7.11 Zinc-Free Cure Systems 465
7.12 Phenolic Resins 469
7.13 NBR Adhesion to Brass 470
7.14 NBR Adhesion to Fabric 472
Nitrile Formulary 475
Appendix A: COMPOUNDING BASICS
A.1 The Compound 517
A.2 The Formula 517
A.3 Design of Formulas 518
A.4 Formula Mixing 520
A.5 Dispersion 520
A.6 Processing Properties 521
A.7 Physical Properties 522
A.8 Silica Surface Area 524
Appendix B: COMPOUNDING MATERIALS
B.1 Elastomers 527
B.2 Natural Rubber (NR) 528
B.3 Styrene-Butadiene Rubber (SBR) 530
B.4 Polybutadiene Rubber (BR) 531
B.5 Ethylene Propylene Rubbers (EPM, EPDM) 532
B.6 Neoprene (CR) 533
B.7 Nitrile Rubber (NBR) 533
B.8 Sulfur-Based Cure Systems 534
B.9 Non-Sulfur Cure Systems 537
B.10 Antidegradants 538
B.11 Other Additives 542xi
Appendix C: RUBBER PROCESSING
C.1 Mastication 545
C.2 Masterbatching 545
C.3 Remilling 546
C.4 Finish Mixing 546
C.5 Extruding 546
C.6 Calendering 547
C.7 Vulcanization 547
Appendix D: PHYSICAL TESTING OF RUBBER
D.1 Processability 551
D.2 Vulcanizate Tests 555
D.3 Weather and Ozone Resistance Tests 562
D.4 Accelerated Aging Tests 564
D.5 Fluid Resistance Tests 565
D.6 Low-Temperature Properties Tests 566
Appendix E: COMMON COMPOUNDING ABBREVIATIONS 569
INDEX 573
INDEX
Index Terms Links
A
abrasion resistance 1 4 5 8 10 13
16 18 25 27 41 52
53 64 66 67 74 77
79 80 81 169 174 175
177 182 189 192 195 196
197 245 248 249 250 251
253 257 259 262 265 266
269 270 271 272 274 319
323 392 446 449 460 461
462 463 469 519 523
abrasion index 18 22 48 58 78 171
180 182 184 190 248 251
252 256 258 259 260 261
268 270 272 312 323 328
408 409 411 449 456 462
465 558
abrasives 544
accelerated aging 564
accelerator blends, natural rubber 41
Index Terms Links
accelerator bloom 322
accelerators 535
EPDM 314
nitrile 453
secondary, emulsion SBR 181 182
secondary, in natural rubber 31
single, in emulsion SBR 182
single, in natural rubber 33
single, natural rubber properties 37
solution BR 249
solution SBR 249
activators 535
nitrile 456
agglomerates, silica 6
aging resistance 522
aging resistance, natural rubber 41
air oven test 564
antidegradants 538
antioxidants 539
emulsion SBR 189
non-staining 50
primary 539
secondary 539
solution BR 260
solution SBR 260
antiozonants 541Index Terms Links
B
Banbury mixers 545
BET surface area 5 524
blowing agents 543
BR, solution 245 531
accelerators 249
antioxidants 260
glycol 256
HMT 254
plasticizers 262
processing 261
silane coupling 265
silica content 272
silica surface area 269
sulfur 257
TBBS 258
trouser tear 271
zinc oxide 252
zinc-free cure 247
brass adhesion 82
disc fatigue 81
EPDM 331
natural rubber 81
neoprene, NSM 400Index Terms Links
brass adhesion (Cont.)
neoprene, SM 414
nitrile 470
brittleness temperature 567
building tack 329 529 548
neoprene, SM 410
C
calendaring 547
carbon black, structure 3
surface activity 3
Charpy impact 561
chemical resistance 524 565
Ciptane 22 48 64 186 264 265
267 272 274 396 461
colors 543
compression fatigue 561
EPDM 339
compression set 522 557
continuous curing 550
contour curves 60 182 339 393 403 446
471
cord adhesion, neoprene, SM 411
Cord Compression Fatigue 81
coupling mechanism, silane 21Index Terms Links
CR, properties 533
crosslink length 537
crosslinks, in natural rubber 34
CTAB surface area 5 524
cure index 553
cure rate 521
cure rate index 554
cure retardation 179
cure, sulfur-based 534
cut growth resistance 524
cut resistance 65
D
DeMattia flex test 561
difunctional compound cure 538
disc fatigue, brass adhesion 81
discrimination 81
interfacial separation 81
discrimination, disk fatigue 81
dithiocarbamates 536
dry heat curing 549
dry silica 8 11Index Terms Links
durometer 9 10 49 50 65 177
185 186 191 245 248 256
261 262 264 267 269 274
311 312 318 319 323 329
330 338 340 341 387 389
395 400 407 410 445 459
467 522 555
durometer equivalents 274
dynamic adhesion 399
dynamic modulus 41 66 74 171 251 266
269 272 312 324 341 393
396 452 456 468 523
E
elasticity 528
elastomer structures 527
elongation 27 40 41 54 55 56
69 86 169 174 185 189
193 194 250 260 269 315
318 319 323 328 329 389
398 400 410 446 450 453
456 461 462 469 472 555
elongation, ultimate 522Index Terms Links
emulsion SBR 169
antioxidants 189
fabric adhesion 192
glycol 171
heat resistance 193
lead oxide 181
magnesium oxide 180
plasticizers 187
silane coupling 193 196
trouser tear 190
zinc oxide 174
EPDM 311
accelerators 314
brass adhesion 331
compression fatigue 339
fabric adhesion 333
galvanized adhesion 336
glycol 318
heat resistance 318
magnesium oxide 318
peroxide cure 328
processing 329
properties 532
silane coupling 323Index Terms Links
EPDM (Cont.)
silica surface area 326
sulfur 315
sulfur donors 315
zinc adhesion 336
zinc oxide 317
zinc-free cure 319
EPM, properties 532
EP rubbers, properties 532
extension modulus 47 180 522
extruding 546
extrusion swell 447
F
fabric adhesion
emulsion SBR 192
EPDM 333
neoprene, NSM 398
neoprene, SM 411
nitrile 472
Fade-Ometer 563
filler dispersion 520
finish mixing 546
flame retardants 543Index Terms Links
flat belting cure 549
flex resistance 561
flex-crack resistance 561
flexometer 38 42 44 55 56 58
61 65 78 169 177 180
185 251 272 312 323 562
fluid resistance 316 565
formula, rubber 517
free water, silica 7
effect on peroxide cure 8
effect on sulfur cure 10
effect on visible dispersion 11
G
galvanized adhesion, EPDM 336
glycol
emulsion SBR 171
natural rubber 29
EPDM 318
neoprene, NSM 390
neoprene, SM 407
solution BR 256
solution SBR 256Index Terms Links
green strength 68
guanidine 33 34 53 181 249 250
389 536
H
hardness 5 8 9 12 25 27
29 30 47 28 50 52
56 57 58 61 65 66
68 69 71 72 74 78
79 170 171 174 184 186
189 191 197 248 249 253
256 260 261 262 266 272
274 312 326 328 330 337
387 391 392 393 398 400
406 410 412 414 447 450
456 459 460 467 469 522
555
hardness equivalents 274Index Terms Links
heat build-up 4 13 27 31 33 37
38 41 42 43 44 51
54 55 56 57 58 60
61 64 65 66 67 69
74 77 78 79 81 174
180 181 185 196 251 261
265 269 272 274 312 323
339 389 392 396 410 413
459 460 461 462 523 561
heat resistance 35 40 41 44 45 79
86 87 169 171 174 185
193 253 262 311 314 315
316 317 318 323 326 328
387 392 396 445 452 453
454 462 557
emulsion SBR 193
EPDM 318
natural rubber 86
HMT, solution BR 254
HMT, solution SBR 254
hot air cure 550Index Terms Links
I
impact resistance 560
impact strength 560
interfacial separation, disk fatigue 81
Izod impact 560
L
lead oxide, emulsion SBR 181
light transmission 175
Liquid Cure Medium 550
M
magnesium oxide
emulsion SBR 180
EPDM 318
neoprene, NSM 388
neoprene, SM 404
masterbatching 545
mastication 545
maximum torque 554
MDR 23 65 79 174 263Index Terms Links
mercaptosilane 4 21 56 66 76 77
87 171 182 189 193 194
264 265 266 274 311 312
314 319 323 340 387 393
396 398 407 408 460
metal oxide cure 538
methacryloxysilane 328
microwave cure 550
minimum torque 553
modulus 27 30 31 33 34 48
49 65 67 69 70 71
72 74 76 77 78 79
169 174 176 177 181 183
186 188 190 191 196 197
245 246 247 248 249 250
252 253 255 256 257 260
261 264 265 266 269 274
312 319 323 326 337 389
392 395 398 400 406 407
408 410 414 445 449 460
462 463 467 469 470 472
modulus, dynamic 41 66 74 171 251 266
269 272 312 324 341 393
396 452 456 468 523Index Terms Links
modulus, extension 47 180 522
Monsanto fatigue tester 561
Mooney cure time 553
Mooney scorch 552
Mooney viscometer 68 521 551
Mooney viscosity 27 65 189 251 261 388
551
N
natural rubber 25
brass adhesion 81
heat resistance 86
peroxide cure 69
plasticizers 51
properties 528
textile adhesion 83
zinc-free cure 78
NBR, properties 533
NBS abrader 558
Neoprene 387
neoprene, NSM 387
brass adhesion 400
fabric adhesion 398Index Terms Links
neoprene, NSM (Cont.)
glycol 390
magnesium oxide 388
plasticizers 391
silane coupling 396
silica surface area 395
water absorption 403
zinc oxide 388
neoprene, properties 533
neoprene, SM 387
brass adhesion 414
building tack 410
cord adhesion 411
fabric adhesion 411
glycol 407
magnesium oxide 404
processing 408
scorch 407
silane coupling 407
silica free water 410
silica surface area 410
zinc oxide 404
nerve 521Index Terms Links
nitrile 445
accelerators 453
activators 456
brass adhesion 470
fabric adhesion 472
peroxide curing 462
phenolic resins 469
processing 464
properties 533
PVC blends 452
silane coupling 460
silica surface area 449
sulfur content 452
zinc-free cure 465
nitrogen surface area 524
O
odorants 543
ODR 34 37
oil resistance 566
oils 542
open steam curing 549
oscillating disk rheometer 553Index Terms Links
outdoor exposure 562
oxidative deterioration 565
ozone 563
ozone resistance 541 562
P
pendulum rebound 523
permanent set 523
peroxide cure 537
EPDM 328
natural rubber 69
peroxide cure, nitrile 462
pH, silica 16
phenolic resins, nitrile 469
physical testing 551
PICO abrader 559
PICO abrasion 50 52 58 61 65 79
175 182 189 250 259 260
261 268 270 328 456 465
pilling 175
plasticizers
emulsion SBR 187
natural rubber 51
neoprene, NSM 391Index Terms Links
plasticizers (Cont.)
solution BR 262
solution SBR 262
polybutadiene 408
properties 531
polyisoprene, zinc-free cure 79
pore volume 21
precipitated silica, manufacture 2
press curing 548
primary antioxidants 539
structures 540
processing aids 542
processing
EPDM 329
neoprene, SM 408
nitrile 464
solution BR 261
solution SBR 261
R
rate of cure 547
refractive index 21
reinforcement 4Index Terms Links
reinforcement potential 3
remilling 546
residual salt, silica 403
resilience 41 61 62 64 69 70
71 76 177 185 252 269
272 274 312 323 392 393
414 449 461 467 523 547
retarders, scorch 407 414 536
reversion 34 47 48 49 50 77
521
natural rubber 47 48
reversion resistance, natural rubber 49
rolling resistance 27
Ross flex test 561
rubber formula 517
design 518
mixing 520
elastic behavior 519
plastic behavior 519
S
SBR, emulsion 169
antioxidants 189
fabric adhesion 192Index Terms Links
SBR, emulsion (Cont.)
glycol 171
heat resistance 193
lead oxide 181
magnesium oxide 180
plasticizers 187
silane coupling 193 196
trouser tear 190
zinc oxide 164
SBR cure, sulfur concentration 185
SBR properties 530
SBR, solution 245
accelerators 249
antioxidants 260
glycol 256
HMT 254
plasticizers 262
processing 261
silane coupling 265
silica content 272
silica surface area 269
sulfur 257
TBBS 258Index Terms Links
SBR, solution (Cont.)
trouser tear 271
zinc-free cure 247
zinc oxide 252
scorch retarders 407 414 536
scorch safety 29 31 37 41 42 51
65 78 181 182 184 185
186 187 195 246 249 251
253 254 255 259 261 314
316 318 320 330 389 391
402 405 406 407 408 410
414 453 462 521
scorch, neoprene, SM 407
secondary antioxidants 539
secondary antioxidants, structures 541
shelf aged stiffening 68
shrinkage 521
silane coupling 21
emulsion SBR 193 196
EPDM 323
natural rubber 76 77
neoprene, NSM 396
neoprene, SM 407
nitrile 460Index Terms Links
solution BR 265
solution SBR 265
silanol 4 5 12 28 51 52
53 72 83 175 179 193
194 196 197 255 265 269
338 392 396 398 460 467
geminal 14
isolated 14
vicinal 14
silica agglomerates 6
silica content
solution BR 272
solution SBR 272
trouser tear 191
silica free water 7
neoprene, SM 410
silica gel 3
silica particle size, tear strength 64 190
silica pH 16
effects 17
silica structure 5 12
natural rubber 70Index Terms Links
silica surface area 5
neoprene, NSM 395
EPDM 326
natural rubber 73
neoprene, SM 410
nitrile 449
solution BR 269
solution SBR 269
silica, vs carbon black
emulsion SBR 169
EPDM 311
natural rubber 25
nitrile 445
NSM neoprene 392
solution SBR 245
silica
density 19
dry 8
physical forms 20
pore volume 21
pretreated 264
reaction with zinc 13
refractive index 21
residual salt 403Index Terms Links
silica (Cont.)
soluble salts 18
types 1
slab cure 549
solid tires 65
soluble salts 18
soluble zinc 192
solution BR 245
accelerators 249
antioxidants 260
glycol 256
HMT 254
plasticizers 262
processing 261
silane coupling 265
silica content 272
silica surface area 269
sulfur 257
TBBS 258
trouser tear 271
zinc oxide 252
zinc-free cure 247Index Terms Links
solution SBR 245
accelerators 249
antioxidants 260
glycol 256
HMT 254
plasticizers 262
processing 261
silane coupling 265
silica content 272
silica surface area 269
sulfur 257
TBBS 258
trouser tear 271
zinc oxide 252
zinc-free cure 247
state of cure 521 547
stress-strain 555
structure, carbon black 3
structure, silica 5 12
styrene-butadiene
rubber, properties 530
sulfonamide 31 33 34 35 181 184
185 195 247 249 250 253
314 453 470 536Index Terms Links
sulfur concentration, SBR cure 185
sulfur content, nitrile 452
sulfur donors 43
EPDM 315
natural rubber 42
sulfur 535
EPDM 315
solution BR 257
solution SBR 257
sulfur-based cure systems 534
surface activity, carbon black 3
surface area
BET 5 524
CTAB 5 524
nitrogen 524
silica 5
T
Taber abrader 547
tackifiers 543
TBBS 258
TBTD 58Index Terms Links
tear resistance 39 53 54 60 64 67
169 190 191 251 269 459
463 469 547
contour curves 60
tear strength 1 4 25 27 40 41
42 44 52 54 55 56
57 58 60 61 64 66
67 69 74 76 77 78
80 171 179 180 185 190
191 192 258 259 261 265
269 271 272 311 312 314
335 337 392 395 400 410
445 447 449 461 462 470
471 522 547
mixing procedures 67
silica particle size 64 190
temperature retraction 567
tensile strength 1 4 25 27 30 31
76 86 174 176 180 181
185 188 189 248 249 256
260 261 274 314 315 318
319 323 326 330 335 407
410 445 522 555
Tension Fatigue test 85 399 412
test tube aging 564Index Terms Links
tetrabutylthiuram disulfide 58
textile adhesion, natural rubber 83
textile adhesion, tension fatigue 85
thiuram 33 37 48 49 58 180
181 182 186 249 250 253
314 319 387 402 407 453
454 470 471 453
torsional stiffness 567
trouser tear 27 40 54 56 59 61
65 78 86 171 174 179
181 186 189 190 191 197
261 265 269 271 272 316
329 395 452 461 547
emulsion SBR 190
silica content 191
solution BR 271
solution SBR 271
U
ultimate dispersion 20
ultimate elongation 522Index Terms Links
V
viscoelastic ranking 56
viscoelastic series 461
vulcanization 534 547
W
water absorption, neoprene, NSM 403
water sensitivity 19
weather resistance 562
weathering 562
Weather-Ometer 563
Winkleman tear 547
Z
zinc adhesion, EPDM 336
zinc attachment to silanols 28
zinc reaction with silica 13
zinc-free cure
EPDM 319
natural rubber 78
nitrile 465
polyisoprene 79
solution BR 247
solution SBR 247Index Terms Links
zinc oxide
emulsion SBR 174
natural rubber 28
emulsion SBR 174
EPDM 317
natural rubber 28
neoprene, NSM 388
neoprene, SM 404
solution BR 252
solution SBR 252

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