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제1편 석회석광의 부가가치향상 기술개발연구/채영배;정수복;고원식;박제신;오중환 4
ABSTRACT 6
목차 10
제1장 서론 18
제2장 연구의 배경 및 범위 20
제1절 연구의 배경 20
제2절 연구의 범위 22
제3장 국내 석회석의 분포현황 및 시료의 선정 24
제1절 국내 석회석의 분포현황 24
제2절 시료의 선정 30
제4장 옥천계 석회암층군의 석회석 31
제1절 시료의 특성 31
제2절 실험 방법 43
제3절 실험결과 및 고찰 52
제5장 조선계 대석회석암층군의 석회석 76
제1절 시료의 특성 76
제2절 실험 방법 81
제3절 실험결과 및 고찰 86
제6장 선캠브리아기 석회암층군의 석회석 99
제1절 시료의 특성 99
제2절 실험 방법 107
제3절 실험결과 및 고찰 110
제7장 정제공정의 종합 검토 124
제1절 옥천계 석회암층군 석회석의 정제공정 125
제2절 조선계 대석회암층군 석회석의 정제공정 127
제3절 선캠브리아기 석회암층군 석회석의 정제공정 128
제8장 시제품의 특성 검토 130
제1절 시제품의 특성 130
제2절 분체의 물성 평가 141
제9장 결론 145
참고문헌 147
제2편 납석의 부가가치 향상 연구/조건준;최연호;김상배;전호석;조성백 150
SUMMARY 152
목차 156
제1장 서론 166
제1절 연구의 필요성 166
제2절 연구의 목적 및 범위 167
제2장 원료광물 특성 및 이론적 고찰 168
제1절 원료광물의 현황 168
제2절 광물학적 특성 171
1. 엽납석(pyrophyllite) 171
제3절 이론적 고찰 173
1. 이론적 배경 173
2. 분쇄기 특성 174
제4절 시료 및 실험방법 175
1. 시료의 특성 175
2. 실험방법 183
제3장 충전제 제조실험 결과 및 고찰 187
제1절 분쇄실험 결과 187
1. 펄버라이져 분쇄실험 결과 187
2. 볼밀 분쇄실험 결과 189
3. 진동 밀 분쇄실험 결과 195
4. 분쇄조제(grinding aid) 첨가한 분쇄실험 결과 204
제2절 소성실험 결과 242
제4장 제오라이트 합성기술 개발 251
제1절 연구의 필요성 251
제2절 연구의 목적 및 범위 252
제3절 광물학적 특성 및 이론적 고찰 255
1. 광물학적 특성 255
2. 제올라이트의 특성 259
3. 결정화 기구 및 합성조건 263
제4절 실험방법 271
1. 규소 및 알루미늄원 271
2. 제올라이트 Y의 합성 271
3. 제올라이트 Y의 분석 273
4. 분석기기 274
제5절 실험결과 및 고찰 276
1. 시료의 특성 276
2. 반응물의 조성에 따른 영향 282
3. H₂O/Na₂O의 몰 비에 따른 영향 303
4. 숙성시간에 따른 영향 308
5. 반응시간에 따른 영향 311
제5장 결론 322
참고문헌 324
판권지 326
Table 1. Grade of limestone on the pre-Cambrian series. 26
Table 2. Grade of limestone on the Carboniferous series. 28
Table 3. Grade of limestone on the Age unknown series. 29
Table 4. Chemical analysis of Kumsan samples. 32
Table 5. Mineralogical(Mnineralogical) characteristics of rock forming minerals on Kumsan samples. 37
Table 6. Results of sieve analysis for the crushed products on Kumsan samples. 39
Table 7. Results of sieve analysis for the intermediate crushed products on Kumsan samples. 40
Table 8. Results of sieve analysis for the grinded products on Kumsan samples. 42
Table 9. Material balance of dry purification process with the crushing step on Kumsan samples. 55
Table 10. Chemical component analysis for the final products from dry purification process with the crushing step on Kumsan samples. 56
Table 11. Material balance of dry purification process with the intermediate crushing step on Kumsan samples. 59
Table 12. Chemical component analysis for the final products from dry purification process with the intermediate crushing step on Kumsan samples. 60
Table 13. Material balance of dry purification process with the grinded products on Kumsan samples. 64
Table 14. Chemical component analysis for the final products from dry purification process with the grinding step on Kumsan samples. 66
Table 15. Material balance of wet purification process on Kumsan samples. 71
Table 16. Chemical component analysis for the final products from wet purification process on Kumsan samples. 72
Table 17. Chemical component analysis of Jungsun sample. 76
Table 18. Mineralogical characteristics of rock forming minerals on Jungsun sample. 77
Table 19. Results of sieve analysis for the crushed products on Jungsun sample. 80
Table 20. Results of sieve analysis for the grinded products on Jungsun sample. 82
Table 21. Material balance of dry purification process with the crushing step on Jungsun sample. 88
Table 22. Chemical component analysis for the final products from dry purification process with the crushing step on Jungsun sample. 88
Table 23. Material balance of dry purification process with the grinding step on Jungsun sample. 89
Table 24. Chemical component analysis for the final products from dry purification process with the grinding step on Jungsun sample. 91
Table 25. Material balance of wet purification process on Jungsun sample. 96
Table 26. Chemical component analysis for the final products from wet purification process on Jungsun sample. 97
Table 27. Chemical analysis of Andong samples. 100
Table 28. Mineralogical characteristics of rock forming minerals on Andong sample. 104
Table 29. Results of sieve analysis for the crushed products on Andong sample. 105
Table 30. Results of sieve analysis for the grinded products on Andong sample. 106
Table 31. Material balance of dry purification process with the crushing step on Andong sample. 112
Table 32. Chemical component analysis for the final products from dry purification process with the crushing step on Andong sample. 113
Table 33. Material balance of dry purification process with the grinding step on Andong sample. 114
Table 34. Chemical component analysis for the final products from dry purification process with the grinding process on Andong sample. 116
Table 35. Material balance of wet purification process on Andong sample. 121
Table 36. Chemical component analysis for the final products from wet purification process on Andong sample. 122
Table 37. Results of each purification process on Kumsan samples. 126
Table 38. Results of each purification process on Jungsun sample. 127
Table 39. Results of each purification process on Andong sample. 128
Table 40. Density properties of the powders made on an experimental basis. 132
Table 41. Dynamic properties of the powders made on an experimental basis. 133
Table 42. Particle size distribution (Kumsan-A sample). 137
Table 43. Particle size distribution(Jungsun sample). 138
Table 44. Homogeneity of the powders made on an experimental basis. 139
Table 45. Dispersion properties of the powders made on an experimental basis. 140
Table 46. Flowability and floodability of the powders made on an experimental basis. 144
Fig. 1. Distribution map of the domestic limestone deposits. 25
Fig. 2. Deposit area of limestone on the great limestone series. 27
Fig. 3. X-ray diffraction patterns of Kumsan samples. 33
Fig. 4. Particle size distribution of each products on Kumsan-A sample 45
Fig. 5. CaO and total impurity contents of each products on Kumsan-A sample. 46
Fig. 6. Particle size distribution of each products on Kumsan-B sample 48
Fig. 7. CaO and total impurity contents of each products on Kumsan-B sample. 49
Fig. 8. Flowsheet of dry purification process with the crushing step on Kumsan samples. 54
Fig. 9. Flowsheet of dry purification process with the intermediate crushing step on Kumsan samples. 58
Fig. 10. X-ray diffraction patterns for the final products from dry purification products with the intermediate crushing step on Kumsan-A sample. 62
Fig. 11. X-ray diffraction patterns for the final products from dry purification products with the intermediate crushing step on Kumsan-B sample. 63
Fig. 12. Flowsheet of dry purification process with the grinding step on Kumsan samples. 65
Fig. 13. Flowsheet of wet purification process on Kumsan samples. 68
Fig. 14. X-ray diffraction patterns for the final products from wet purification process on Kumsan-A sample. 74
Fig. 15. X-ray diffraction patterns for the final products from wet purification process on Kumsan-B sample. 75
Fig. 16. X-ray diffraction patterns of Jungsun sample. 78
Fig. 17. Particle size distribution of each products on Jungsun sample 83
Fig. 18. CaO and total impurity contents of each products on Jungsun sample. 84
Fig. 19. Flowsheet of dry purification process with the crushing step on Jungsun sample. 87
Fig. 20. Flowsheet of dry purification process with the grinding step on Jungsun sample. 90
Fig. 21. X-ray diffraction patterns for the final products from dry purification products with the grinding step on Jungsun sample. 92
Fig. 22. Flowsheet of wet purification process on Jungsun sample. 94
Fig. 23. X-ray diffraction patterns for the final products from wet purification process on Jungsun sample. 98
Fig. 24. X-ray diffraction patterns of Andong sample. 101
Fig. 25. Particle size distribution of each products on Andong sample 108
Fig. 26. CaO and total impurity contents of each products on Andong sample. 109
Fig. 27. Flowsheet of dry purification process with the crushing step on Andong sample. 111
Fig. 28. Flowsheet of dry purification process with the grinding step on Andong sample. 115
Fig. 29. X-ray diffraction patterns for the final products from dry purification products with the grinding Andong sample. 118
Fig. 30. Flowsheet of wet purification process on Andong sample. 119
Fig. 31. X-ray diffraction patterns for the final products from dry purification process on Andong sample. 123
Fig. 32. Particle size distribution of the powders made on an experimental basis(Kumsan-A sample). 135
Fig. 33. Particle size distribution of the powders made on an experimental basis(Jungsun sample). 136
Photo. 1. Photographs of polarizing(polaizing) microscope(Kumsan-A). 34
Photo. 2. Photographs of polarizing(polaizing) microscope(Kumsan-B). 35
Photo. 3. Photographs of polarizing(polaizing) microscope(Jungsun). 79
Photo. 4. Photographs of polarizing(polaizing) microscope(Andong) 102
Photo. 5. Photographs of non-coating/coating on Kumsan-A(a) and Jungsun(b) sample. 142
Table 1. Reserve of amalgatolite in Korea 168
Table 2. The grouping and chemical components of amalgatolite 169
Table 3. The quality standards of amalgatolite products 171
Table 4. Chemical components analysis on samples 176
Table 5. Particle size analysis of pulverized samples 188
Table 6. Chemical analysis on roasted samples 194
Table 7. The result of size reduction ratio as a function of grinding time by vibrating mill 202
Table 8. The oil adsorption rate as a function of grinding aids 236
Table 9. Chemical analysis on heat treated samples 243
Table 10. Synthesis content of zeolite A, X and Y. 269
Table 11. The effect of SiO₂/Al₂O₃ mole ratio of reaction mixture on the synthesis zeolite Y 282
Table 12. The effect of SiO₂/Al₂O₃ mole ratio of reaction mixture on the synthesis zeolite Y 284
Table 13. The effect of Na₂O/SiO₂ mole ratio of reaction mixture on the synthesis zeolite Y 290
Table 14. The effect of H₂O/Na₂O mole ratio of reaction mixture on the synthesis zeolite Y 303
Table 15. The effect of aging time on the synthesis zeolite Y 308
Table 16. The effect of aging time on the synthesis zeolite Y 311
Table 17. The effect of aging time on the synthesis zeolite Y 311
Table 18. The effect of reaction time on the synthesis zeolite Y 312
Fig. 1. Structure of pyrophyllite 172
Fig. 2. X-ray diffraction patterns on samples 177
Fig. 3. DTA curves of Bu Nam sample 181
Fig. 4. DTA curves of Bu Gok sample 182
Fig. 5. The effect of grinding time on particle size ground by ball mill 191
Fig. 6. Particle size analysis of Bu Gok sample ground for 180min. by ball mill 192
Fig. 7. Particle size analysis of Bu Nam sample ground for 180min. by ball mill 193
Fig. 8. The effect of grinding time on particle size ground by ball mill 196
Fig. 9. Particle size analysis of Bu Gok roasted at 650℃ sample ground for 180min. by ball mill 197
Fig. 10. Particle size analysis of Bu Nam roasted at 570℃ sample ground for 180min. by ball mill 198
Fig. 11. The effect of grinding time on particle size ground by by vibrating mill for roasted samples. 199
Fig. 12. Particle size analysis on Bu Gok sample ground for 180min. by vibrating mill 200
Fig. 13. Particle size analysis on Bu Nam sample ground for 180min. by vibrating mill 201
Fig. 14. The effect of grinding time on particle size ground by vibrating mill for roasted samples. 203
Fig. 15. The effect of methanol amount on particle size ground by ball mill 205
Fig. 16. Particle size analysis on Bu Gok sample ground by ball mill for 180min. added methanol 206
Fig. 17. Particle size analysis on Bu Nam sample ground by ball mill for 180min. added methanol 207
Fig. 18. The effect of methanol amount on particle size ground by vibrating mill 209
Fig. 19. Particle size analysis on Bu Gok sample ground by vibrating mill for 180min. added methanol 210
Fig. 20. Particle size analysis on Bu Nam sample ground by vibrating mill for 180min. added methanol 211
Fig. 21. The effect of kerosene amount on particle size ground by ball mill 213
Fig. 22. Particle size analysis on Bu Gok sample ground by ball mill for 180min. added kerosen 214
Fig. 23. Particle size analysis on Bu Nam sample ground by ball mill for 180min. added kerosen 215
Fig. 24. The effect of kerosen amount on particle size ground by vibrating mill 216
Fig. 25. Particle size analysis on Bu Gok sample ground by vibrating mill for 180min. added kerosen 217
Fig. 26. Particle size analysis on Bu Nam sample ground by vibrating mill for 180min. added kerosen 218
Fig. 27. The effect of oleic acid on particle size ground by ball mill 220
Fig. 28. Particle size analysis on Bu Gok sample ground by ball mill for 180min. added oleic acid 221
Fig. 29. Particle size analysis on Bu Nam sample ground by ball mill for 180min. added oleic acid 222
Fig. 30. The effect of oleic acid amount on particle size ground by vibrating mill 224
Fig. 31. Particle size analysis on Bu Gok sample ground by vibrating mill for 180min. added oleic acid 225
Fig. 32. Particle size analysis on Bu Nam sample ground by vibrating mill for 180min. added oleic acid 226
Fig. 33. The effect of mixture of oleic acid and methanol on particle size ground by ball mill 228
Fig. 34. Particle size analysis on Bu Gok sample ground by ball mill for 180min. added oleic acid and methanol 229
Fig. 35. Particle size analysis on Bu Nam sample ground by ball mill for 180min. added oleic acid and methanol 230
Fig. 36. The effect of mixture of oleic acid and methanol on particle size ground by vibrating mill 232
Fig. 37. Particle size analysis on Bu Gok sample ground by vibrating mill for 180min. added oleic acid and methanol 233
Fig. 38. Particle size analysis on Bu Nam sample ground by vibrating mill for 180min. added oleic acid and methanol 234
Fig. 39. Particle size analysis on Bu Gok sample ground by ball mill for 180min. added 0.6wt.% oleic acid and methanol 238
Fig. 40. Particle size analysis on Bu Nam sample ground by ball mill for 180min. added 0.6wt.% oleic acid and methanol 239
Fig. 41. Particle size analysis on Bu Gok sample ground by vibrating mill for 180min. added 0.6wt.% oleic acid and methanol 240
Fig. 42. Particle size analysis on Bu Nam sample ground by vibrating mill for 180min. added 0.6wt.% oleic acid and methanol 241
Fig. 43. XRD on Bu Gok sample as a function(funtion) of roasting temperature 245
Fig. 44. XRD on Bu Nam sample as a function(funtion) of roasting temperature 247
Fig. 45. The effect of roast temperature on whiteness. 250
Fig. 46. A composition of the structure of kaolinite, dickite and macrite viewed on the left-hand along the b axis and on the right-hand along the a axis; the c axis is always vertical. 257
Fig. 47. DTA curves of various kaolin group. 258
Fig. 48. The polyhedral units comprising the structure of zeolite A. 261
Fig. 49. The sodalite structure illustrating the total face sharing of each cage to give a space-filling structure. 261
Fig. 50. Features of the faujasite structure.... 262
Fig. 51. The type II 26-hedron cavity of the faujasite structure. 262
Fig. 52. Crystallization curve of zeolite X. 264
Fig. 53. Flowsheet. 272
Fig. 54. X-ray diffraction curve of standard sample(Linde SK 40). 275
Fig. 55. Particle size analysis of agalmatolite. 277
Fig. 56. TGA curve of agalmatolite. 278
Fig. 57. DTA curve of agalmatolite. 279
Fig. 58. X-ray diffraction patterns of agalmatolite and calcined and acid treated agalmatolite. 280
Fig. 59. Crystallization and SiO₂/Al₂O₃ mole ratio curve of synthesized zeolite Y on SiO₂/Al₂O₃ mole ratio of reaction mixture. Na₂O/SiO₂=0.5, H₂O/Na₂O=40, aging time=48hours, reaction time=48hours. 283
Fig. 60. X-ray diffraction curve of synthesized zeolite Y on SiO₂/Al₂O₃ mole ratio of reaction mixture. Na₂O/SiO₂=0.5, H₂O/Na₂O=40, aging time=48hours, reaction time=48hours. 285
Fig. 61. SEM micrographs of synthesized zeolite Y on SiO₂/Al₂O₃ mole ratio of reaction mixture. SiO₂/Al₂O₃=8(a), 10(b), 13(c), 16(d), 19(e). Na₂O/SiO₂=0.5, H₂O/Na₂O=40, aging time=48hours, reaction time=48hours. 286
Fig. 62. Crystallization and SiO₂/Al₂O₃ mole ratio curve of synthesized zeolite Y on SiO₂/Al₂O₃ mole ratio of reaction mixture. Na₂O/SiO₂=0.5, H₂O/Na₂O=40, aging time=48hours, reaction time=48hours. 289
Fig. 63. Crystallization and SiO₂/Al₂O₃ mole ratio curve of synthesized zeolite Y on Na₂O/SiO₂ mole ratio of reaction mixture. SiO₂/Al₂O₃=13, H₂O/Na₂O=40, aging time=48hours, reaction time=48hours. 291
Fig. 64. X-ray diffraction patterns of synthesized zeolite Y on Na₂O/SiO₂ mole ratio of reaction mixture. SiO₂/Al₂O₃=13, H₂O/Na₂O=40, aging time=48hours, reaction time=48hours. 293
Fig. 65. SEM micrographs on Na₂O/SiO₂=0.8(a), 0.7(b), 0.6(c), 0.5(d), 0.4(e), 0.3(f). SiO₂/Al₂O₃=13, H₂O/Na₂O=40, aging time=48hours, reaction time=48hours. 294
Fig. 66. X-ray diffraction patterns of Linde SK 40(a) and synthesized zeolite Y(b). SiO₂/Al₂O₃=13, Na₂O/SiO₂=0.6, H₂O/Na₂O=40, aging time=48hours, reaction time=48hours. 297
Fig. 67. SEM micrographs of Linde SK 40(a), calcined and acid treated amalgatolite(b), synthesized zeolite Y(c), zeolite P(d). SiO₂/Al₂O₃=13, Na₂O/SiO₂=0.6, H₂O/Na₂O=40, aging time=48hours, reaction time=48hours. 298
Fig. 68. The effect of the Na₂O/SiO₂ mole ratio of reaction mixture on the composition(compositon) of the synthesized zeolite Y. 301
Fig. 69. Crystallization and SiO₂/Al₂O₃ mole ratio curve of synthesized zeolite Y on H₂O/Na₂Omole ratio of reaction mixture. SiO₂/Al₂O₃=13, Na₂O/SiO₂=0.4, aging time=48hours, reaction time=48hours. 305
Fig. 70. X-ray diffraction curve of synthesized zeolite Y on H₂O/Na₂O mole ratio of reaction mixture. SiO₂/Al₂O₃=13, Na₂O/SiO₂=0.4, aging time=48hours, reaction time=48hours. 307
Fig. 71. Crystallization and SiO₂/Al₂O₃ mole ratio curve of synthesized zeolite Y on aging time. SiO₂/Al₂O₃=13, Na₂O/SiO₂=0.4, H₂O/Na₂O=40, reaction time=48hours. 310
Fig. 72. Crystallization and SiO₂/Al₂O₃ mole ratio curve of synthesized zeolite Y on reaction time. SiO₂/Al₂O₃=13, Na₂O/SiO₂=0.5, H₂O/Na₂O=40, aging time=24hours. 314
Fig. 73. SEM micrographs of synthesized zeolite Y on the reaction time 40hr(a), 48hr(b), 56hr(c), 64hr(d). aging time=24hours, SiO₂/Al₂O₃=13, Na₂O/SiO₂=0.5, H₂O/Na₂O=40. 315
Fig. 74. Crystallization and SiO₂/Al₂O₃ mole ratio curve of synthesized zeolite Y on reaction time. aging time=32hours, SiO₂/Al₂O₃=13, Na₂O/SiO₂=0.5, H₂O/Na₂O=40. 317
Fig. 75. SEM micrographs of synthesized zeolite Y on the reaction time 40hr(a), 48hr(b), 56hr(c), 64hr(d). aging time=32hours, SiO₂/Al₂O₃=13, Na₂O/SiO₂=0.5, H₂O/Na₂O=40. 318
Fig. 76. Crystallization and SiO₂/Al₂O₃ mole ratio curve of synthesized zeolite Y on reaction time. aging time=32hours. SiO₂/Al₂O₃=13, Na₂O/SiO₂=0.4, H₂O/Na₂O=40, 320
Fig. 77. Crystallization and SiO₂/Al₂O₃ mole ratio curve of synthesized zeolite Y on reaction time. aging time=48hours, SiO₂/Al₂O₃=13, Na₂O/SiO₂=0.4, H₂O/Na₂O=40. 321
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